data_compound_4 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H78 Cl20 N12 Ni O12 S6' _chemical_formula_sum 'C96 H78 Cl20 N12 Ni O12 S6' _chemical_formula_weight 2551.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_H-M_alt 'R -3 :H' _space_group_name_Hall '-R 3' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 24.6475(9) _cell_length_b 24.6475(9) _cell_length_c 15.8565(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 8342.3(7) _cell_formula_units_Z 3 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8832 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 29.74 _exptl_crystal_description 'prism' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.524 _exptl_crystal_F_000 3894 _exptl_transmission_factor_min 0.9117 _exptl_transmission_factor_max 1.0000 _exptl_crystal_size_max 0.249 _exptl_crystal_size_mid 0.217 _exptl_crystal_size_min 0.168 _exptl_absorpt_coefficient_mu 0.831 _shelx_estimated_absorpt_T_min 0.820 _shelx_estimated_absorpt_T_max 0.873 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.9117 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(Sheldrick, 2000)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD diffractometer 01-670-03' _diffrn_measurement_method '\w-scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 60395 _diffrn_reflns_av_unetI/netI 0.0326 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.300 _diffrn_reflns_theta_max 30.043 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 5428 _reflns_number_gt 3067 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX2 v2012.10.0(Bruker, 2012)' _computing_cell_refinement 'APEX2 v2012.10.0(Bruker, 2012)' _computing_data_reduction 'SAINT V8.27B (Bruker, 2012)' _computing_structure_solution 'SHELXS-2012 (Bruker, 2013)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'XP V 5.1 (Bruker, 1998)' _computing_publication_material 'CIFTAB V 2013/2 (Sheldrick, 2013)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1667P)^2^+23.1849P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5428 _refine_ls_number_parameters 394 _refine_ls_number_restraints 759 _refine_ls_R_factor_all 0.1474 _refine_ls_R_factor_gt 0.0958 _refine_ls_wR_factor_ref 0.3285 _refine_ls_wR_factor_gt 0.2764 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 1.133 _refine_ls_shift/su_mean 0.043 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.6667 0.3333 0.8333 0.0464(3) Uani 1 6 d S T P . . Cl1 Cl 0.6667 0.3333 0.48932(19) 0.1201(11) Uani 1 3 d S T P . . N1 N 0.61900(16) 0.36576(17) 0.7550(2) 0.0578(8) Uani 1 1 d . U . . . C2 C 0.5912(2) 0.3403(2) 0.6821(3) 0.0634(9) Uani 1 1 d . U . . . H2 H 0.5867 0.3031 0.6608 0.076 Uiso 1 1 calc R U . . . O2 O 0.3241(12) 0.5763(7) 0.6769(10) 0.252(7) Uani 0.738(11) 1 d . U P A 1 O2B O 0.313(4) 0.576(2) 0.575(3) 0.282(10) Uani 0.262(11) 1 d . U P A 2 N3 N 0.5705(2) 0.3743(2) 0.6435(2) 0.0722(9) Uani 1 1 d . U . . . C4 C 0.5850(3) 0.4240(3) 0.6931(4) 0.0813(12) Uani 1 1 d . U . . . H4 H 0.5759 0.4557 0.6821 0.098 Uiso 1 1 calc R U . . . C5 C 0.6155(2) 0.4194(2) 0.7628(4) 0.0746(11) Uani 1 1 d . U . . . H5 H 0.6311 0.4477 0.8074 0.090 Uiso 1 1 calc R U . . . C6 C 0.5355(4) 0.3528(5) 0.5623(7) 0.0803(18) Uani 0.738(11) 1 d D U P A 1 H6A H 0.5447 0.3226 0.5363 0.096 Uiso 0.738(11) 1 calc R U P A 1 H6AB H 0.5502 0.3883 0.5244 0.096 Uiso 0.738(11) 1 calc R U P A 1 O1 O 0.4520(4) 0.3727(4) 0.5802(6) 0.0916(17) Uani 0.738(11) 1 d D U P A 1 C7 C 0.4644(4) 0.3227(4) 0.5731(6) 0.0841(15) Uani 0.738(11) 1 d D U P A 1 H7 H 0.4447 0.3000 0.5209 0.101 Uiso 0.738(11) 1 calc R U P A 1 C8 C 0.4371(6) 0.2768(4) 0.6451(6) 0.0794(14) Uani 0.738(11) 1 d D U P A 1 Cl2 Cl 0.4555(3) 0.1928(3) 0.5564(3) 0.1117(12) Uani 0.738(11) 1 d D U P A 1 C9 C 0.4306(6) 0.2171(4) 0.6445(6) 0.0840(16) Uani 0.738(11) 1 d D U P A 1 C10 C 0.4048(5) 0.1765(4) 0.7114(6) 0.0851(17) Uani 0.738(11) 1 d D U P A 1 H10 H 0.4016 0.1372 0.7102 0.102 Uiso 0.738(11) 1 calc R U P A 1 Cl3 Cl 0.3492(2) 0.1422(2) 0.8631(3) 0.1061(13) Uani 0.738(11) 1 d D U P A 1 C11 C 0.3839(6) 0.1949(4) 0.7802(6) 0.0863(18) Uani 0.738(11) 1 d D U P A 1 C12 C 0.3892(6) 0.2528(5) 0.7830(7) 0.089(2) Uani 0.738(11) 1 d D U P A 1 H12 H 0.3741 0.2641 0.8296 0.107 Uiso 0.738(11) 1 calc R U P A 1 C13 C 0.4159(7) 0.2934(5) 0.7194(6) 0.084(2) Uani 0.738(11) 1 d D U P A 1 H13 H 0.4208 0.3332 0.7236 0.100 Uiso 0.738(11) 1 calc R U P A 1 Cl4 Cl 0.2619(3) 0.3163(3) 0.6700(6) 0.144(3) Uani 0.738(11) 1 d D U P A 1 C14 C 0.3227(8) 0.3901(4) 0.6372(14) 0.1040(19) Uani 0.738(11) 1 d D U P A 1 S1 S 0.3206(3) 0.4553(3) 0.6621(5) 0.1187(15) Uani 0.738(11) 1 d D U P A 1 C15 C 0.3727(5) 0.3991(4) 0.5915(8) 0.0913(15) Uani 0.738(11) 1 d D U P A 1 C16 C 0.4087(4) 0.4658(5) 0.5717(7) 0.0973(19) Uani 0.738(11) 1 d D U P A 1 H16 H 0.4437 0.4832 0.5368 0.117 Uiso 0.738(11) 1 calc R U P A 1 C17 C 0.3862(5) 0.4997(5) 0.6094(7) 0.102(2) Uani 0.738(11) 1 d D U P A 1 H17 H 0.4054 0.5431 0.6060 0.123 Uiso 0.738(11) 1 calc R U P A 1 C18 C 0.3865(4) 0.3521(5) 0.5615(7) 0.0938(17) Uani 0.738(11) 1 d D U P A 1 H18A H 0.3793 0.3463 0.5012 0.113 Uiso 0.738(11) 1 calc R U P A 1 H18B H 0.3595 0.3124 0.5892 0.113 Uiso 0.738(11) 1 calc R U P A 1 C6B C 0.5420(11) 0.3722(14) 0.564(2) 0.084(3) Uani 0.262(11) 1 d D U P A 2 H6BA H 0.5537 0.3509 0.5229 0.101 Uiso 0.262(11) 1 calc R U P A 2 H6BB H 0.5560 0.4144 0.5444 0.101 Uiso 0.262(11) 1 calc R U P A 2 O1B O 0.4542(12) 0.3826(10) 0.5969(16) 0.090(2) Uani 0.262(11) 1 d D U P A 2 C7B C 0.4706(11) 0.3369(10) 0.5763(14) 0.086(2) Uani 0.262(11) 1 d D U P A 2 H7B H 0.4517 0.3191 0.5215 0.103 Uiso 0.262(11) 1 calc R U P A 2 C8B C 0.4450(17) 0.2839(10) 0.6391(15) 0.085(2) Uani 0.262(11) 1 d D U P A 2 Cl2B Cl 0.4702(10) 0.2120(9) 0.5335(10) 0.138(4) Uani 0.262(11) 1 d D U P A 2 C9B C 0.4408(18) 0.2259(11) 0.6265(14) 0.090(3) Uani 0.262(11) 1 d D U P A 2 C10B C 0.4186(15) 0.1807(10) 0.6886(14) 0.087(3) Uani 0.262(11) 1 d D U P A 2 H10B H 0.4197 0.1439 0.6813 0.105 Uiso 0.262(11) 1 calc R U P A 2 Cl3B Cl 0.3647(8) 0.1325(7) 0.8379(10) 0.117(4) Uani 0.262(11) 1 d D U P A 2 C11B C 0.3946(18) 0.1910(10) 0.7615(15) 0.090(3) Uani 0.262(11) 1 d D U P A 2 C12B C 0.4006(19) 0.2482(11) 0.7779(15) 0.089(3) Uani 0.262(11) 1 d D U P A 2 H12B H 0.3874 0.2554 0.8295 0.107 Uiso 0.262(11) 1 calc R U P A 2 C13B C 0.425(2) 0.2938(11) 0.7201(16) 0.087(3) Uani 0.262(11) 1 d D U P A 2 H13B H 0.4302 0.3328 0.7327 0.104 Uiso 0.262(11) 1 calc R U P A 2 Cl4B Cl 0.2784(9) 0.3124(6) 0.6774(12) 0.108(3) Uani 0.262(11) 1 d D U P A 2 C14B C 0.3248(18) 0.3894(8) 0.640(4) 0.096(3) Uani 0.262(11) 1 d D U P A 2 S1B S 0.3091(8) 0.4454(7) 0.6705(14) 0.095(2) Uani 0.262(11) 1 d D U P A 2 C15B C 0.3767(11) 0.4104(9) 0.592(2) 0.091(2) Uani 0.262(11) 1 d D U P A 2 C16B C 0.4138(9) 0.4783(10) 0.6052(19) 0.097(3) Uani 0.262(11) 1 d D U P A 2 H16B H 0.4563 0.5025 0.5932 0.116 Uiso 0.262(11) 1 calc R U P A 2 C17B C 0.3783(11) 0.5014(8) 0.637(2) 0.101(3) Uani 0.262(11) 1 d D U P A 2 H17B H 0.3914 0.5438 0.6399 0.121 Uiso 0.262(11) 1 calc R U P A 2 C18B C 0.3990(11) 0.3730(13) 0.5501(16) 0.091(2) Uani 0.262(11) 1 d D U P A 2 H18C H 0.4099 0.3863 0.4920 0.110 Uiso 0.262(11) 1 calc R U P A 2 H18D H 0.3669 0.3291 0.5507 0.110 Uiso 0.262(11) 1 calc R U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0473(4) 0.0473(4) 0.0446(6) 0.000 0.000 0.0236(2) Cl1 0.1447(18) 0.1447(18) 0.0709(15) 0.000 0.000 0.0723(9) N1 0.0594(18) 0.0619(18) 0.0567(17) 0.0040(14) 0.0013(14) 0.0337(15) C2 0.066(2) 0.076(2) 0.0528(19) 0.0059(17) -0.0023(16) 0.039(2) O2 0.43(2) 0.161(10) 0.231(13) -0.007(10) 0.006(16) 0.196(13) O2B 0.44(2) 0.186(13) 0.238(16) -0.008(14) 0.005(19) 0.170(16) N3 0.070(2) 0.095(2) 0.0612(18) 0.0167(16) 0.0019(15) 0.0486(19) C4 0.084(3) 0.082(3) 0.091(3) 0.015(2) -0.008(2) 0.051(2) C5 0.080(3) 0.075(3) 0.085(3) -0.002(2) -0.007(2) 0.051(2) C6 0.083(3) 0.100(4) 0.061(3) 0.018(3) -0.005(2) 0.048(3) O1 0.080(3) 0.095(3) 0.100(4) 0.010(3) -0.012(3) 0.044(3) C7 0.078(3) 0.097(3) 0.078(3) 0.010(3) -0.015(2) 0.045(3) C8 0.070(3) 0.090(3) 0.078(3) 0.004(2) -0.015(2) 0.039(3) Cl2 0.132(3) 0.115(3) 0.097(2) -0.0076(18) 0.0023(17) 0.069(3) C9 0.078(4) 0.092(3) 0.076(3) 0.002(2) -0.013(3) 0.038(3) C10 0.079(4) 0.089(3) 0.080(3) 0.004(3) -0.017(3) 0.036(3) Cl3 0.096(2) 0.104(2) 0.085(2) 0.0199(16) -0.0089(14) 0.0260(15) C11 0.079(4) 0.094(3) 0.075(3) 0.006(3) -0.015(3) 0.034(3) C12 0.080(5) 0.098(3) 0.081(3) 0.001(3) -0.011(3) 0.038(3) C13 0.074(5) 0.091(3) 0.087(3) 0.006(2) -0.014(3) 0.043(3) Cl4 0.101(3) 0.137(3) 0.131(4) -0.026(3) 0.014(3) 0.012(2) C14 0.096(3) 0.118(3) 0.076(3) -0.005(3) -0.008(3) 0.038(3) S1 0.109(3) 0.133(3) 0.087(2) -0.023(2) 0.0056(19) 0.040(2) C15 0.083(3) 0.110(3) 0.083(3) 0.015(3) -0.017(2) 0.050(3) C16 0.093(3) 0.112(3) 0.088(4) 0.008(3) -0.001(3) 0.053(3) C17 0.105(4) 0.113(3) 0.088(4) 0.003(3) 0.001(3) 0.054(3) C18 0.080(3) 0.102(4) 0.102(4) 0.022(3) -0.016(3) 0.048(3) C6B 0.081(4) 0.103(5) 0.071(4) 0.022(4) -0.008(3) 0.048(4) O1B 0.081(4) 0.100(4) 0.091(5) 0.013(4) -0.013(4) 0.046(4) C7B 0.079(3) 0.099(4) 0.081(4) 0.016(3) -0.015(3) 0.045(3) C8B 0.075(4) 0.094(3) 0.081(3) 0.011(3) -0.020(3) 0.039(3) Cl2B 0.166(10) 0.130(9) 0.106(6) -0.005(5) 0.004(6) 0.063(7) C9B 0.084(5) 0.094(4) 0.084(4) 0.007(3) -0.019(4) 0.040(4) C10B 0.080(5) 0.091(4) 0.088(5) 0.005(4) -0.024(4) 0.040(4) Cl3B 0.110(7) 0.114(5) 0.099(6) 0.024(5) -0.025(5) 0.035(5) C11B 0.080(5) 0.096(4) 0.084(4) 0.007(4) -0.020(4) 0.036(4) C12B 0.077(6) 0.100(4) 0.083(4) 0.006(4) -0.014(4) 0.038(4) C13B 0.074(6) 0.095(4) 0.086(4) 0.008(3) -0.015(4) 0.038(4) Cl4B 0.130(8) 0.088(4) 0.089(5) -0.002(4) 0.001(6) 0.043(5) C14B 0.095(4) 0.107(3) 0.082(4) -0.002(4) -0.004(4) 0.047(3) S1B 0.094(4) 0.103(3) 0.086(4) -0.006(3) 0.002(3) 0.047(3) C15B 0.085(4) 0.110(4) 0.085(4) 0.009(4) -0.010(3) 0.053(3) C16B 0.091(4) 0.114(4) 0.086(5) 0.003(5) -0.002(4) 0.051(4) C17B 0.100(5) 0.113(4) 0.087(5) -0.002(4) 0.003(5) 0.050(4) C18B 0.081(4) 0.104(5) 0.094(5) 0.013(4) -0.010(4) 0.050(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.121(3) 2_655 ? Ni1 N1 2.121(3) 17_556 ? Ni1 N1 2.121(3) . ? Ni1 N1 2.121(3) 18_546 ? Ni1 N1 2.121(3) 3_665 ? Ni1 N1 2.121(3) 16_656 ? N1 C2 1.330(6) . ? N1 C5 1.374(6) . ? C2 N3 1.328(6) . ? C2 H2 0.9300 . ? N3 C4 1.345(7) . ? N3 C6B 1.43(3) . ? N3 C6 1.493(12) . ? C4 C5 1.374(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.535(9) . ? C6 H6A 0.9700 . ? C6 H6AB 0.9700 . ? O1 C7 1.416(9) . ? O1 C18 1.459(8) . ? C7 C8 1.508(9) . ? C7 H7 0.9800 . ? C8 C9 1.397(9) . ? C8 C13 1.430(9) . ? Cl2 C9 1.746(8) . ? C9 C10 1.378(10) . ? C10 C11 1.377(11) . ? C10 H10 0.9300 . ? Cl3 C11 1.743(7) . ? C11 C12 1.367(11) . ? C12 C13 1.340(9) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? Cl4 C14 1.760(9) . ? C14 C15 1.348(10) . ? C14 S1 1.682(9) . ? S1 C17 1.655(10) . ? C15 C18 1.443(11) . ? C15 C16 1.458(12) . ? C16 C17 1.353(13) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C6B C7B 1.534(12) . ? C6B H6BA 0.9700 . ? C6B H6BB 0.9700 . ? O1B C7B 1.414(12) . ? O1B C18B 1.462(11) . ? C7B C8B 1.507(11) . ? C7B H7B 0.9800 . ? C8B C9B 1.396(12) . ? C8B C13B 1.433(11) . ? Cl2B C9B 1.750(11) . ? C9B C10B 1.379(12) . ? C10B C11B 1.377(14) . ? C10B H10B 0.9300 . ? Cl3B C11B 1.741(10) . ? C11B C12B 1.368(13) . ? C12B C13B 1.339(12) . ? C12B H12B 0.9300 . ? C13B H13B 0.9300 . ? Cl4B C14B 1.760(11) . ? C14B C15B 1.348(12) . ? C14B S1B 1.682(11) . ? S1B C17B 1.655(13) . ? C15B C18B 1.447(13) . ? C15B C16B 1.466(14) . ? C16B C17B 1.359(15) . ? C16B H16B 0.9300 . ? C17B H17B 0.9300 . ? C18B H18C 0.9700 . ? C18B H18D 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 180.0 2_655 17_556 ? N1 Ni1 N1 89.19(13) 2_655 . ? N1 Ni1 N1 90.81(13) 17_556 . ? N1 Ni1 N1 90.81(13) 2_655 18_546 ? N1 Ni1 N1 89.19(13) 17_556 18_546 ? N1 Ni1 N1 90.81(13) . 18_546 ? N1 Ni1 N1 89.19(13) 2_655 3_665 ? N1 Ni1 N1 90.81(14) 17_556 3_665 ? N1 Ni1 N1 89.19(13) . 3_665 ? N1 Ni1 N1 180.0 18_546 3_665 ? N1 Ni1 N1 90.81(13) 2_655 16_656 ? N1 Ni1 N1 89.19(13) 17_556 16_656 ? N1 Ni1 N1 180.0 . 16_656 ? N1 Ni1 N1 89.19(13) 18_546 16_656 ? N1 Ni1 N1 90.81(13) 3_665 16_656 ? C2 N1 C5 105.5(4) . . ? C2 N1 Ni1 125.6(3) . . ? C5 N1 Ni1 128.6(3) . . ? N3 C2 N1 111.8(4) . . ? N3 C2 H2 124.1 . . ? N1 C2 H2 124.1 . . ? C2 N3 C4 107.2(4) . . ? C2 N3 C6B 136.0(14) . . ? C4 N3 C6B 116.6(14) . . ? C2 N3 C6 120.5(6) . . ? C4 N3 C6 132.2(5) . . ? N3 C4 C5 107.5(4) . . ? N3 C4 H4 126.2 . . ? C5 C4 H4 126.2 . . ? N1 C5 C4 107.9(5) . . ? N1 C5 H5 126.0 . . ? C4 C5 H5 126.0 . . ? N3 C6 C7 113.1(7) . . ? N3 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? N3 C6 H6AB 108.9 . . ? C7 C6 H6AB 109.0 . . ? H6A C6 H6AB 107.8 . . ? C7 O1 C18 111.3(6) . . ? O1 C7 C8 112.6(6) . . ? O1 C7 C6 106.3(6) . . ? C8 C7 C6 114.8(6) . . ? O1 C7 H7 107.6 . . ? C8 C7 H7 107.6 . . ? C6 C7 H7 107.6 . . ? C9 C8 C13 116.2(6) . . ? C9 C8 C7 123.9(7) . . ? C13 C8 C7 119.9(6) . . ? C10 C9 C8 121.9(7) . . ? C10 C9 Cl2 118.7(6) . . ? C8 C9 Cl2 119.4(6) . . ? C11 C10 C9 118.9(7) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C12 C11 C10 121.0(7) . . ? C12 C11 Cl3 120.6(7) . . ? C10 C11 Cl3 118.4(6) . . ? C13 C12 C11 120.6(8) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C8 121.3(7) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? C15 C14 S1 115.5(6) . . ? C15 C14 Cl4 124.4(7) . . ? S1 C14 Cl4 120.0(5) . . ? C17 S1 C14 91.5(5) . . ? C14 C15 C18 127.5(8) . . ? C14 C15 C16 107.0(8) . . ? C18 C15 C16 125.3(8) . . ? C17 C16 C15 113.2(8) . . ? C17 C16 H16 123.4 . . ? C15 C16 H16 123.4 . . ? C16 C17 S1 112.4(7) . . ? C16 C17 H17 123.8 . . ? S1 C17 H17 123.8 . . ? C15 C18 O1 108.5(7) . . ? C15 C18 H18A 109.9 . . ? O1 C18 H18A 110.1 . . ? C15 C18 H18B 110.0 . . ? O1 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? N3 C6B C7B 108.4(19) . . ? N3 C6B H6BA 110.1 . . ? C7B C6B H6BA 110.1 . . ? N3 C6B H6BB 109.9 . . ? C7B C6B H6BB 109.9 . . ? H6BA C6B H6BB 108.4 . . ? C7B O1B C18B 111.6(13) . . ? O1B C7B C8B 111.9(12) . . ? O1B C7B C6B 106.3(12) . . ? C8B C7B C6B 116.0(12) . . ? O1B C7B H7B 107.5 . . ? C8B C7B H7B 107.4 . . ? C6B C7B H7B 107.4 . . ? C9B C8B C13B 116.3(10) . . ? C9B C8B C7B 125.2(11) . . ? C13B C8B C7B 118.5(11) . . ? C10B C9B C8B 121.4(11) . . ? C10B C9B Cl2B 118.6(10) . . ? C8B C9B Cl2B 119.8(10) . . ? C11B C10B C9B 119.0(11) . . ? C11B C10B H10B 120.5 . . ? C9B C10B H10B 120.5 . . ? C12B C11B C10B 120.9(11) . . ? C12B C11B Cl3B 120.2(12) . . ? C10B C11B Cl3B 118.4(11) . . ? C13B C12B C11B 120.2(12) . . ? C13B C12B H12B 119.9 . . ? C11B C12B H12B 119.9 . . ? C12B C13B C8B 121.6(12) . . ? C12B C13B H13B 119.2 . . ? C8B C13B H13B 119.2 . . ? C15B C14B S1B 114.4(9) . . ? C15B C14B Cl4B 125.8(12) . . ? S1B C14B Cl4B 119.5(10) . . ? C17B S1B C14B 91.5(7) . . ? C14B C15B C18B 127.0(13) . . ? C14B C15B C16B 106.7(13) . . ? C18B C15B C16B 125.1(13) . . ? C17B C16B C15B 111.5(11) . . ? C17B C16B H16B 124.3 . . ? C15B C16B H16B 124.2 . . ? C16B C17B S1B 112.4(10) . . ? C16B C17B H17B 123.7 . . ? S1B C17B H17B 123.9 . . ? C15B C18B O1B 106.4(13) . . ? C15B C18B H18C 110.6 . . ? O1B C18B H18C 110.2 . . ? C15B C18B H18D 110.5 . . ? O1B C18B H18D 110.4 . . ? H18C C18B H18D 108.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C2 N3 0.1(5) . . . . ? Ni1 N1 C2 N3 -173.9(3) . . . . ? N1 C2 N3 C4 -0.4(6) . . . . ? N1 C2 N3 C6B 175.0(14) . . . . ? N1 C2 N3 C6 -177.6(5) . . . . ? C2 N3 C4 C5 0.5(6) . . . . ? C6B N3 C4 C5 -175.9(11) . . . . ? C6 N3 C4 C5 177.2(6) . . . . ? C2 N1 C5 C4 0.2(6) . . . . ? Ni1 N1 C5 C4 174.0(3) . . . . ? N3 C4 C5 N1 -0.4(6) . . . . ? C2 N3 C6 C7 100.9(7) . . . . ? C4 N3 C6 C7 -75.5(9) . . . . ? C18 O1 C7 C8 -73.3(10) . . . . ? C18 O1 C7 C6 160.2(8) . . . . ? N3 C6 C7 O1 80.1(8) . . . . ? N3 C6 C7 C8 -45.0(10) . . . . ? O1 C7 C8 C9 165.5(11) . . . . ? C6 C7 C8 C9 -72.7(13) . . . . ? O1 C7 C8 C13 -14.2(13) . . . . ? C6 C7 C8 C13 107.6(12) . . . . ? C13 C8 C9 C10 0.5(18) . . . . ? C7 C8 C9 C10 -179.3(10) . . . . ? C13 C8 C9 Cl2 -179.9(10) . . . . ? C7 C8 C9 Cl2 0.4(16) . . . . ? C8 C9 C10 C11 1.1(17) . . . . ? Cl2 C9 C10 C11 -178.6(9) . . . . ? C9 C10 C11 C12 -0.8(16) . . . . ? C9 C10 C11 Cl3 178.1(9) . . . . ? C10 C11 C12 C13 -1.2(18) . . . . ? Cl3 C11 C12 C13 179.9(10) . . . . ? C11 C12 C13 C8 2.9(19) . . . . ? C9 C8 C13 C12 -2.5(18) . . . . ? C7 C8 C13 C12 177.3(11) . . . . ? C15 C14 S1 C17 1.9(18) . . . . ? Cl4 C14 S1 C17 -177.6(16) . . . . ? S1 C14 C15 C18 -180.0(12) . . . . ? Cl4 C14 C15 C18 0(3) . . . . ? S1 C14 C15 C16 -4(2) . . . . ? Cl4 C14 C15 C16 175.2(17) . . . . ? C14 C15 C16 C17 5.4(17) . . . . ? C18 C15 C16 C17 -178.9(10) . . . . ? C15 C16 C17 S1 -4.2(13) . . . . ? C14 S1 C17 C16 1.5(13) . . . . ? C14 C15 C18 O1 -133.2(18) . . . . ? C16 C15 C18 O1 51.9(14) . . . . ? C7 O1 C18 C15 164.6(8) . . . . ? C2 N3 C6B C7B 94.3(19) . . . . ? C4 N3 C6B C7B -90.6(17) . . . . ? C18B O1B C7B C8B -97(3) . . . . ? C18B O1B C7B C6B 135(2) . . . . ? N3 C6B C7B O1B 91(2) . . . . ? N3 C6B C7B C8B -34(2) . . . . ? O1B C7B C8B C9B 165(3) . . . . ? C6B C7B C8B C9B -73(4) . . . . ? O1B C7B C8B C13B -18(4) . . . . ? C6B C7B C8B C13B 104(3) . . . . ? C13B C8B C9B C10B 1(5) . . . . ? C7B C8B C9B C10B 178(3) . . . . ? C13B C8B C9B Cl2B -174(3) . . . . ? C7B C8B C9B Cl2B 3(5) . . . . ? C8B C9B C10B C11B 6(5) . . . . ? Cl2B C9B C10B C11B -179(3) . . . . ? C9B C10B C11B C12B -9(5) . . . . ? C9B C10B C11B Cl3B 178(3) . . . . ? C10B C11B C12B C13B 5(6) . . . . ? Cl3B C11B C12B C13B 178(3) . . . . ? C11B C12B C13B C8B 2(6) . . . . ? C9B C8B C13B C12B -5(6) . . . . ? C7B C8B C13B C12B 178(3) . . . . ? C15B C14B S1B C17B -10(5) . . . . ? Cl4B C14B S1B C17B 164(4) . . . . ? S1B C14B C15B C18B -174(3) . . . . ? Cl4B C14B C15B C18B 11(8) . . . . ? S1B C14B C15B C16B 18(5) . . . . ? Cl4B C14B C15B C16B -156(5) . . . . ? C14B C15B C16B C17B -19(4) . . . . ? C18B C15B C16B C17B 173(3) . . . . ? C15B C16B C17B S1B 12(4) . . . . ? C14B S1B C17B C16B -2(4) . . . . ? C14B C15B C18B O1B -108(5) . . . . ? C16B C15B C18B O1B 58(4) . . . . ? C7B O1B C18B C15B 164.8(17) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C2 H2 N1 0.93 2.56 3.056(6) 113.8 2_655 C6 H6A Cl2 0.97 2.85 3.416(10) 117.9 . C7 H7 Cl3 0.98 3.04 3.813(11) 136.4 13_556 C12 H12 Cl4 0.93 2.88 3.761(14) 159.3 5 C6B H6BA Cl2B 0.97 2.99 3.46(3) 111.0 . C10B H10B Cl4B 0.93 2.76 3.66(2) 164.3 13_556 C18B H18C Cl4B 0.97 2.58 3.42(3) 145.2 9_554 C18B H18D Cl3B 0.97 2.87 3.78(3) 156.9 13_556 C18B H18D Cl4B 0.97 2.84 3.27(3) 107.8 . _refine_diff_density_max 0.687 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.088 _shelx_res_file ; compound_4.res created by SHELXL-2014/7 TITL 163NOP17_0m_a.res in R-3 REM Old TITL 163NOP17_0m in R-3 REM SHELXT solution in R-3 REM R1 0.268, Rweak 0.044, Alpha 0.059, Orientation as input REM Formula found by SHELXT: C84 N18 O12 S6 Cl20 Ni CELL 0.71073 24.6475 24.6475 15.8565 90.000 90.000 120.000 ZERR 3.000 0.0009 0.0009 0.0006 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H N O S CL NI UNIT 288 234 36 36 18 60 3 OMIT -1 1 1 OMIT -2 2 2 OMIT -5 7 6 OMIT -5 9 1 OMIT -9 13 2 OMIT -2 12 4 OMIT -15 10 2 OMIT -1 2 0 OMIT 2 8 3 OMIT 0 6 0 TEMP 25.000 SIZE 0.168 0.217 0.249 L.S. 40 ACTA CONF EQIV $2 -y+1, x-y, z HTAB C2 N1_$2 HTAB C6 Cl2 EQIV $6 -x+2/3, -y+1/3, -z+4/3 HTAB C7 Cl3_$6 EQIV $7 -y+2/3, x-y+1/3, z+1/3 HTAB C12 Cl4_$7 HTAB C6B Cl2B HTAB C10B Cl4B_$6 EQIV $9 -x+y+1/3, -x+2/3, z-1/3 HTAB C18B Cl4B_$9 HTAB C18B Cl3B_$6 HTAB C18B Cl4B BOND $H LIST 4 FMAP 2 PLAN 10 WGHT 0.166700 23.184900 FVAR 0.15673 0.26245 NI1 7 0.666667 0.333333 0.833333 10.16667 0.04727 0.04727 = 0.04462 0.00000 0.00000 0.02364 CL1 6 0.666667 0.333333 0.489324 10.33333 0.14466 0.14466 = 0.07092 0.00000 0.00000 0.07233 SIMU 0.01 N1 > C18B DELU 0.005 N1 > C18B N1 3 0.619004 0.365759 0.755007 11.00000 0.05937 0.06193 = 0.05671 0.00402 0.00128 0.03373 C2 1 0.591164 0.340278 0.682123 11.00000 0.06581 0.07598 = 0.05280 0.00586 -0.00227 0.03884 AFIX 43 H2 2 0.586695 0.303116 0.660763 11.00000 -1.20000 AFIX 0 PART 1 O2 4 0.324124 0.576292 0.676869 -21.00000 0.42932 0.16054 = 0.23128 -0.00674 0.00556 0.19568 PART 2 O2B 4 0.313176 0.576384 0.575030 21.00000 0.44069 0.18559 = 0.23778 -0.00838 0.00548 0.16959 PART 0 N3 3 0.570522 0.374333 0.643547 11.00000 0.06977 0.09536 = 0.06121 0.01674 0.00187 0.04864 C4 1 0.584958 0.424032 0.693072 11.00000 0.08432 0.08170 = 0.09077 0.01532 -0.00768 0.05110 AFIX 43 H4 2 0.575908 0.455737 0.682119 11.00000 -1.20000 AFIX 0 C5 1 0.615511 0.419445 0.762805 11.00000 0.07996 0.07472 = 0.08517 -0.00217 -0.00716 0.05072 AFIX 43 H5 2 0.631078 0.447690 0.807405 11.00000 -1.20000 AFIX 0 PART 1 C6 1 0.535548 0.352766 0.562258 -21.00000 0.08269 0.09984 = 0.06106 0.01772 -0.00540 0.04760 AFIX 23 H6A 2 0.544716 0.322607 0.536308 -21.00000 -1.20000 H6AB 2 0.550190 0.388284 0.524408 -21.00000 -1.20000 AFIX 0 O1 4 0.451964 0.372718 0.580208 -21.00000 0.07987 0.09476 = 0.10016 0.00989 -0.01237 0.04368 C7 1 0.464389 0.322673 0.573055 -21.00000 0.07842 0.09704 = 0.07785 0.00951 -0.01487 0.04465 AFIX 13 H7 2 0.444662 0.299990 0.520926 -21.00000 -1.20000 AFIX 0 C8 1 0.437149 0.276776 0.645057 -21.00000 0.07007 0.08952 = 0.07772 0.00369 -0.01502 0.03922 CL2 6 0.455452 0.192811 0.556449 -21.00000 0.13186 0.11534 = 0.09700 -0.00761 0.00228 0.06851 C9 1 0.430648 0.217109 0.644476 -21.00000 0.07769 0.09203 = 0.07631 0.00239 -0.01327 0.03805 C10 1 0.404828 0.176451 0.711411 -21.00000 0.07889 0.08873 = 0.08003 0.00379 -0.01682 0.03617 AFIX 43 H10 2 0.401580 0.137208 0.710183 -21.00000 -1.20000 AFIX 0 CL3 6 0.349170 0.142182 0.863095 -21.00000 0.09640 0.10425 = 0.08543 0.01986 -0.00892 0.02601 C11 1 0.383909 0.194927 0.780180 -21.00000 0.07871 0.09370 = 0.07473 0.00638 -0.01465 0.03424 C12 1 0.389189 0.252816 0.783028 -21.00000 0.07966 0.09779 = 0.08146 0.00113 -0.01091 0.03825 AFIX 43 H12 2 0.374079 0.264113 0.829584 -21.00000 -1.20000 AFIX 0 C13 1 0.415924 0.293421 0.719384 -21.00000 0.07447 0.09137 = 0.08650 0.00630 -0.01387 0.04270 AFIX 43 H13 2 0.420782 0.333248 0.723619 -21.00000 -1.20000 AFIX 0 CL4 6 0.261873 0.316324 0.670002 -21.00000 0.10129 0.13671 = 0.13091 -0.02593 0.01386 0.01213 C14 1 0.322742 0.390091 0.637209 -21.00000 0.09632 0.11816 = 0.07646 -0.00517 -0.00768 0.03781 S1 5 0.320641 0.455337 0.662088 -21.00000 0.10859 0.13331 = 0.08733 -0.02264 0.00564 0.04038 C15 1 0.372687 0.399107 0.591534 -21.00000 0.08300 0.10967 = 0.08311 0.01494 -0.01694 0.04959 C16 1 0.408735 0.465760 0.571743 -21.00000 0.09345 0.11220 = 0.08840 0.00837 -0.00128 0.05300 AFIX 43 H16 2 0.443701 0.483169 0.536751 -21.00000 -1.20000 AFIX 0 C17 1 0.386209 0.499722 0.609388 -21.00000 0.10516 0.11340 = 0.08787 0.00303 0.00064 0.05422 AFIX 43 H17 2 0.405407 0.543124 0.606031 -21.00000 -1.20000 AFIX 0 C18 1 0.386520 0.352056 0.561516 -21.00000 0.08007 0.10244 = 0.10159 0.02157 -0.01633 0.04758 AFIX 23 H18A 2 0.379275 0.346317 0.501215 -21.00000 -1.20000 H18B 2 0.359502 0.312380 0.589174 -21.00000 -1.20000 AFIX 0 PART 2 SAME 0.01 0.02 C6 > C18 SIMU 0.01 C6B > C18B DELU 0.005 C6B > C18B C6B 1 0.541984 0.372216 0.564344 21.00000 0.08150 0.10318 = 0.07081 0.02171 -0.00820 0.04844 AFIX 23 H6BA 2 0.553650 0.350934 0.522882 21.00000 -1.20000 H6BB 2 0.556043 0.414403 0.544407 21.00000 -1.20000 AFIX 0 O1B 4 0.454177 0.382630 0.596918 21.00000 0.08138 0.09974 = 0.09119 0.01267 -0.01315 0.04643 C7B 1 0.470649 0.336899 0.576266 21.00000 0.07878 0.09903 = 0.08111 0.01570 -0.01538 0.04529 AFIX 13 H7B 2 0.451703 0.319124 0.521469 21.00000 -1.20000 AFIX 0 C8B 1 0.444967 0.283931 0.639111 21.00000 0.07541 0.09404 = 0.08059 0.01091 -0.01991 0.03891 CL2B 6 0.470150 0.211961 0.533514 21.00000 0.16561 0.12959 = 0.10574 -0.00501 0.00425 0.06339 C9B 1 0.440798 0.225922 0.626470 21.00000 0.08437 0.09388 = 0.08440 0.00653 -0.01923 0.03955 C10B 1 0.418561 0.180713 0.688556 21.00000 0.08007 0.09058 = 0.08769 0.00460 -0.02444 0.03955 AFIX 43 H10B 2 0.419705 0.143854 0.681325 21.00000 -1.20000 AFIX 0 CL3B 6 0.364729 0.132469 0.837942 21.00000 0.11021 0.11436 = 0.09888 0.02355 -0.02476 0.03489 C11B 1 0.394624 0.190956 0.761453 21.00000 0.07979 0.09589 = 0.08387 0.00730 -0.02043 0.03628 C12B 1 0.400620 0.248166 0.777949 21.00000 0.07684 0.09981 = 0.08256 0.00591 -0.01441 0.03824 AFIX 43 H12B 2 0.387393 0.255413 0.829512 21.00000 -1.20000 AFIX 0 C13B 1 0.425488 0.293780 0.720053 21.00000 0.07446 0.09516 = 0.08556 0.00815 -0.01499 0.03790 AFIX 43 H13B 2 0.430227 0.332768 0.732678 21.00000 -1.20000 AFIX 0 CL4B 6 0.278384 0.312446 0.677396 21.00000 0.12998 0.08775 = 0.08911 -0.00249 0.00093 0.04261 C14B 1 0.324810 0.389412 0.639621 21.00000 0.09486 0.10687 = 0.08169 -0.00172 -0.00431 0.04719 S1B 5 0.309079 0.445406 0.670541 21.00000 0.09390 0.10325 = 0.08587 -0.00593 0.00234 0.04735 C15B 1 0.376743 0.410385 0.591842 21.00000 0.08504 0.10976 = 0.08491 0.00858 -0.00968 0.05344 C16B 1 0.413812 0.478250 0.605160 21.00000 0.09145 0.11378 = 0.08599 0.00287 -0.00246 0.05141 AFIX 43 H16B 2 0.456331 0.502472 0.593218 21.00000 -1.20000 AFIX 0 C17B 1 0.378262 0.501351 0.637148 21.00000 0.09965 0.11254 = 0.08703 -0.00210 0.00316 0.04967 AFIX 43 H17B 2 0.391359 0.543842 0.639949 21.00000 -1.20000 AFIX 0 C18B 1 0.398959 0.372989 0.550088 21.00000 0.08082 0.10426 = 0.09422 0.01301 -0.01047 0.05033 AFIX 23 H18C 2 0.409864 0.386261 0.491959 21.00000 -1.20000 H18D 2 0.366884 0.329076 0.550705 21.00000 -1.20000 PART 0 rem CL1 6 0.666667 0.333333 0.488792 10.33333 0.14592 0.14592 = REM ##### REM ##### AFIX 0 HKLF 4 REM 163NOP17_0m_a.res in R-3 REM R1 = 0.0958 for 3067 Fo > 4sig(Fo) and 0.1474 for all 5428 data REM 394 parameters refined using 759 restraints END WGHT 0.1667 23.1849 REM Highest difference peak 0.687, deepest hole -0.508, 1-sigma level 0.088 Q1 1 0.3376 0.5002 0.6506 11.00000 0.05 0.69 Q2 1 0.4182 0.0925 0.6337 11.00000 0.05 0.60 Q3 1 0.4184 0.2995 0.7684 11.00000 0.05 0.58 Q4 1 0.2606 0.3658 0.6448 11.00000 0.05 0.55 Q5 1 0.4496 0.3630 0.5198 11.00000 0.05 0.53 Q6 1 0.4203 0.2023 0.5407 11.00000 0.05 0.48 Q7 1 0.6567 0.3658 0.4725 11.00000 0.05 0.42 Q8 1 0.4818 0.2651 0.5394 11.00000 0.05 0.37 Q9 1 0.5575 0.4070 0.5835 11.00000 0.05 0.37 Q10 1 0.5969 0.4146 0.6572 11.00000 0.05 0.35 ; _shelx_res_checksum 9109 _shelx_hkl_file ; 1 1 0 -0.20 0.30 1 1 0 -0.20 0.10 -2 1 0 0.00 0.10 -2 1 0 -0.10 0.40 1 -2 0 -0.20 0.30 1 -2 0 1.20 0.40 1 -2 0 -0.20 0.40 1 -2 0 -0.10 0.10 1 1 0 0.00 0.20 1 1 0 -0.10 0.20 1 1 0 0.20 0.20 1 1 0 -0.20 0.30 -2 1 0 0.10 0.40 -2 1 0 1.80 0.60 -1 2 0 0.50 0.40 2 -1 0 -0.20 0.40 2 -1 0 -0.20 0.10 -1 -1 0 0.20 0.30 -1 2 0 0.80 0.30 -1 2 0 0.10 0.10 -1 -1 0 -0.50 0.30 -1 -1 0 0.00 0.40 2 -1 0 0.10 0.30 -1 2 0 0.00 0.10 -1 2 0 -0.20 0.40 -1 2 0 0.60 0.60 -3 3 0 413.46 19.20 -3 3 0 421.06 18.20 -3 3 0 409.46 18.40 -3 3 0 407.76 17.30 0 -3 0 422.66 19.20 -3 3 0 382.76 19.10 3 0 0 420.26 17.10 3 0 0 454.35 17.60 3 0 0 402.16 19.20 3 -3 0 437.06 19.20 -3 0 0 415.36 19.20 -3 0 0 428.16 19.30 0 3 0 440.36 18.00 0 3 0 433.16 19.30 0 3 0 406.86 19.10 0 3 0 429.86 17.90 -3 0 0 415.46 18.60 -4 2 0 65.99 2.90 2 2 0 55.39 3.50 2 -4 0 45.40 3.60 2 2 0 49.70 3.70 -4 2 0 63.09 4.10 -4 2 0 63.39 4.20 -4 2 0 65.69 4.30 2 2 0 55.59 3.40 2 2 0 51.49 4.00 2 -4 0 52.29 4.10 2 -4 0 48.00 3.80 2 2 0 51.29 4.00 -2 4 0 55.69 4.10 -2 4 0 46.40 3.80 -2 4 0 47.30 3.60 -2 4 0 45.90 3.10 -2 4 0 46.60 3.70 4 -2 0 60.59 4.10 -2 -2 0 46.30 3.80 -2 -2 0 48.30 3.90 -5 1 0 1430.06 61.99 1 4 0 1448.26 64.39 1 4 0 1435.56 64.49 4 -5 0 1513.35 64.19 1 4 0 1517.35 60.19 4 -5 0 1504.65 64.39 -5 1 0 1519.75 64.69 1 4 0 1445.96 59.39 1 4 0 1447.76 59.29 -4 5 0 1527.65 61.99 5 -1 0 1372.46 57.99 -4 5 0 1409.06 57.79 5 -1 0 1381.76 58.59 -1 -4 0 1474.65 62.19 -1 -4 0 1504.15 64.49 -4 5 0 1450.25 64.29 -4 5 0 1600.44 64.59 -4 5 0 1538.25 60.79 1 -5 0 1181.38 54.09 1 -5 0 1245.38 54.09 -5 4 0 1260.57 49.10 1 -5 0 1218.08 52.39 -5 4 0 1202.48 54.29 4 1 0 1185.08 49.80 -5 4 0 1212.58 52.09 -5 4 0 1253.77 51.09 4 1 0 1309.27 49.50 -5 4 0 1222.68 54.29 -1 5 0 1180.18 50.09 -4 -1 0 1302.57 54.49 5 -4 0 1224.58 54.19 -1 5 0 1219.08 54.19 -1 5 0 1234.28 50.99 -4 -1 0 1219.88 52.39 -4 -1 0 1305.57 50.59 -1 5 0 1156.48 53.99 5 -4 0 1278.57 54.19 -6 3 0 313.87 14.90 3 -6 0 319.77 15.60 -6 3 0 309.37 15.30 3 -6 0 318.97 15.60 3 3 0 311.67 14.40 3 3 0 315.77 16.00 3 3 0 299.07 14.40 3 -6 0 324.67 15.80 3 3 0 313.37 14.80 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8.50 -10 14 0 140.69 9.90 -10 14 0 105.19 9.70 14 -4 0 111.19 9.70 7 7 0 111.59 9.90 7 -14 0 100.59 8.80 -14 7 0 120.09 6.20 -14 7 0 105.69 9.90 -14 7 0 118.49 9.10 7 -14 0 102.29 9.70 7 7 0 91.29 8.80 7 7 0 108.49 8.60 -14 7 0 112.89 9.20 -14 7 0 105.89 9.40 -7 14 0 103.39 9.50 -7 14 0 99.49 9.40 -7 14 0 105.39 9.00 14 -7 0 111.89 6.50 -7 14 0 124.59 9.30 -7 -7 0 110.39 9.70 -7 14 0 91.19 6.80 14 -7 0 104.09 9.10 -7 -7 0 110.39 10.00 -14 10 0 427.36 24.00 10 4 0 473.05 22.10 -14 10 0 431.56 23.50 -14 10 0 459.75 24.90 10 4 0 453.75 25.30 4 -14 0 436.86 24.60 10 4 0 449.66 23.20 4 -14 0 434.66 24.20 -14 10 0 483.35 20.50 -14 10 0 421.36 24.90 -4 14 0 457.65 25.00 -10 -4 0 446.96 24.70 -10 -4 0 417.46 22.10 -4 14 0 423.36 23.50 -4 14 0 463.45 24.00 -4 14 0 486.95 25.10 14 -10 0 438.06 24.30 1 -14 0 72.89 10.20 -14 13 0 52.29 8.70 -14 13 0 47.40 8.30 -14 13 0 42.90 6.80 1 -14 0 40.60 8.00 -14 13 0 50.89 6.40 13 1 0 41.10 7.20 -14 13 0 34.10 6.80 13 1 0 54.49 8.10 13 1 0 46.50 4.70 14 -13 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15 -15 0 371.46 22.40 2 14 0 58.19 9.20 -16 2 0 56.89 8.10 2 14 0 54.09 9.10 -16 2 0 56.39 10.20 2 14 0 52.19 8.80 -16 2 0 63.49 10.80 2 14 0 56.89 8.50 -2 -14 0 49.99 7.70 16 -2 0 51.19 7.60 -14 16 0 50.99 9.70 -14 16 0 43.90 8.40 16 -2 0 43.70 4.00 -2 -14 0 55.49 10.00 -14 16 0 56.39 8.90 -14 16 0 40.20 7.40 16 -2 0 57.49 10.10 -14 16 0 48.60 7.10 -16 5 0 195.98 14.70 -16 5 0 205.28 10.00 11 -16 0 204.88 14.00 11 -16 0 188.68 14.70 5 11 0 212.88 15.30 5 11 0 210.78 14.40 -16 5 0 215.58 15.70 5 11 0 217.88 13.40 5 11 0 199.38 13.90 16 -5 0 196.68 12.00 -5 -11 0 192.18 14.90 -11 16 0 184.58 13.60 16 -5 0 215.18 14.80 -5 -11 0 202.08 14.80 -11 16 0 219.08 10.50 -11 16 0 188.08 14.50 -11 16 0 204.98 13.60 -11 16 0 193.88 14.70 -16 8 0 81.69 9.80 -16 8 0 62.79 5.70 8 8 0 68.69 9.30 8 -16 0 58.99 6.80 -16 8 0 59.09 4.00 8 8 0 66.99 8.70 8 -16 0 62.99 9.80 8 8 0 59.09 8.80 -16 8 0 53.79 8.80 -16 8 0 90.19 11.40 -8 16 0 66.59 9.40 -8 -8 0 58.59 9.80 -8 16 0 54.19 5.20 16 -8 0 60.79 4.60 -8 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11.40 4.40 17 -1 0 6.30 1.80 -1 -16 0 6.50 5.60 -16 17 0 6.50 4.70 -17 4 0 90.19 10.30 4 13 0 109.59 10.30 4 13 0 104.19 9.20 4 13 0 101.19 10.70 -17 4 0 100.89 10.40 4 13 0 97.39 10.10 13 -17 0 115.39 11.40 -17 4 0 80.89 5.30 -13 17 0 109.09 10.80 17 -4 0 104.19 9.90 -13 17 0 60.69 8.70 -4 -13 0 82.79 11.90 -13 17 0 111.59 11.00 17 -4 0 102.29 8.40 -13 17 0 102.79 5.70 -4 -13 0 107.09 10.00 -13 17 0 119.89 11.20 -17 7 0 270.07 18.30 7 10 0 288.27 18.00 -17 7 0 267.77 19.10 -17 7 0 270.37 17.30 7 10 0 268.97 18.90 10 -17 0 291.87 17.90 10 -17 0 302.17 19.30 -17 7 0 276.37 13.00 7 10 0 289.57 16.60 7 10 0 300.87 17.50 -7 -10 0 284.47 19.40 17 -7 0 294.37 18.30 17 -7 0 293.57 14.80 -10 17 0 286.17 19.00 -10 17 0 270.77 18.30 -10 17 0 290.07 17.60 -10 17 0 320.87 14.80 -10 17 0 286.27 17.70 -17 10 0 88.79 5.40 7 -17 0 91.69 6.00 10 7 0 90.79 9.90 -17 10 0 85.09 8.90 10 7 0 91.09 9.50 7 -17 0 108.39 10.70 7 -17 0 70.79 7.50 -17 10 0 74.59 6.10 10 7 0 98.09 8.50 -17 10 0 82.29 9.60 -17 10 0 82.29 11.20 -7 17 0 79.89 11.30 -7 17 0 88.99 11.60 -7 17 0 81.89 7.20 -7 17 0 76.79 7.00 -7 17 0 88.79 11.40 -10 -7 0 89.99 12.30 -10 -7 0 85.39 7.60 17 -10 0 83.49 8.20 17 -10 0 76.59 4.80 -10 -7 0 98.09 9.90 -17 13 0 26.90 7.50 -17 13 0 26.50 6.90 13 4 0 20.70 6.00 4 -17 0 21.80 6.70 -17 13 0 24.30 6.70 13 4 0 10.40 4.60 -17 13 0 21.30 3.70 13 4 0 21.60 4.70 4 -17 0 27.70 5.20 -4 17 0 24.60 7.10 -4 17 0 23.60 6.70 -13 -4 0 30.60 5.80 -4 17 0 26.00 5.90 -13 -4 0 24.60 7.30 -13 -4 0 29.40 7.80 -4 17 0 27.00 7.50 1 -17 0 18.40 5.30 -17 16 0 7.00 2.60 16 1 0 10.20 4.80 16 1 0 3.30 4.60 -17 16 0 -1.90 4.10 16 1 0 8.50 2.60 -17 16 0 6.50 5.00 -17 16 0 8.10 5.10 1 -17 0 17.60 6.80 -1 17 0 19.30 6.40 -1 17 0 15.00 5.60 -1 17 0 12.60 5.80 -1 17 0 7.00 4.20 -16 -1 0 8.20 3.50 -16 -1 0 10.00 5.70 3 15 0 17.00 6.50 3 15 0 16.00 6.30 -18 3 0 4.00 3.40 3 15 0 8.80 4.50 -18 3 0 5.50 5.00 -18 3 0 13.00 5.40 3 15 0 17.20 6.40 -15 18 0 11.00 3.70 -15 18 0 13.70 5.90 -15 18 0 0.50 4.60 -3 -15 0 6.00 5.50 18 -3 0 9.50 4.30 -15 18 0 9.50 5.50 18 -3 0 9.20 3.70 -18 6 0 86.59 9.80 -18 6 0 93.29 10.50 6 12 0 76.69 10.30 12 -18 0 72.69 11.40 6 12 0 80.09 8.20 6 12 0 91.09 10.00 -18 6 0 78.59 8.30 6 12 0 91.99 12.30 -6 -12 0 94.29 9.40 -12 18 0 90.29 8.90 -12 18 0 93.99 5.80 -12 18 0 89.29 12.50 -6 -12 0 81.89 12.20 18 -6 0 94.79 8.90 18 -6 0 79.39 7.10 -12 18 0 97.39 13.40 -18 9 0 8.20 4.70 9 9 0 13.70 4.90 9 -18 0 10.10 5.10 -18 9 0 7.50 4.80 9 9 0 13.30 5.60 9 9 0 12.70 5.60 -18 9 0 14.50 5.70 18 -9 0 8.50 2.00 -9 -9 0 -0.50 2.80 -9 18 0 15.60 5.80 -9 -9 0 6.60 5.40 -9 -9 0 6.90 3.20 -9 18 0 11.60 3.40 -9 18 0 11.90 5.10 -9 18 0 10.90 6.00 18 -9 0 10.00 3.40 12 6 0 232.58 14.10 -18 12 0 204.28 15.50 -18 12 0 203.48 16.20 12 6 0 204.38 14.90 -18 12 0 192.88 10.60 6 -18 0 201.38 16.00 12 6 0 229.98 16.50 6 -18 0 195.08 11.70 -18 12 0 203.78 15.10 -6 18 0 215.18 15.60 -12 -6 0 201.38 16.20 -6 18 0 188.88 15.30 -6 18 0 226.88 13.50 -6 18 0 183.68 14.80 -12 -6 0 203.68 15.70 -12 -6 0 223.58 13.80 3 -18 0 27.80 7.90 -18 15 0 29.60 7.60 15 3 0 26.30 7.10 -18 15 0 26.60 4.20 15 3 0 33.00 5.50 3 -18 0 30.50 5.40 -18 15 0 28.70 7.50 15 3 0 26.60 6.50 -18 15 0 28.70 8.00 -15 -3 0 32.30 6.30 -3 18 0 31.80 7.80 -15 -3 0 30.20 8.10 -3 18 0 29.80 6.70 -3 18 0 31.00 7.80 -3 18 0 36.20 8.60 -18 18 0 8.80 5.70 -18 18 0 8.80 3.40 0 -18 0 12.00 6.80 0 -18 0 8.90 4.40 18 0 0 10.00 4.80 -18 18 0 7.10 6.30 -18 18 0 9.00 5.10 0 18 0 1.20 5.20 -18 0 0 11.20 5.70 0 18 0 8.00 4.70 0 18 0 6.50 5.10 0 18 0 3.70 4.10 -18 0 0 10.10 4.10 2 17 0 21.20 6.60 2 17 0 22.10 6.60 -19 2 0 15.90 6.90 -19 2 0 12.20 4.40 2 17 0 15.80 7.20 2 17 0 19.30 6.00 19 -2 0 19.50 5.90 -2 -17 0 14.80 5.10 -17 19 0 11.50 6.30 -17 19 0 25.10 5.80 -2 -17 0 18.70 7.40 -17 19 0 17.70 6.70 -17 19 0 16.80 6.60 5 14 0 103.19 9.70 -19 5 0 92.29 12.90 5 14 0 104.89 11.40 5 14 0 98.89 12.40 -19 5 0 98.29 11.30 14 -19 0 108.99 14.30 5 14 0 123.69 14.90 -14 19 0 94.39 10.90 -14 19 0 109.39 14.30 -14 19 0 100.89 9.70 -5 -14 0 101.99 14.30 19 -5 0 112.29 8.90 8 11 0 10.70 5.50 11 -19 0 9.70 5.50 -19 8 0 9.80 5.20 8 11 0 10.20 5.80 -19 8 0 5.70 4.10 -19 8 0 16.30 5.50 8 11 0 4.30 4.40 -11 19 0 9.90 2.30 -8 -11 0 5.80 5.00 -11 19 0 11.10 5.20 19 -8 0 5.70 2.30 -11 19 0 9.50 5.30 -8 -11 0 6.30 3.70 -11 19 0 -0.30 3.40 11 8 0 51.39 10.20 -19 11 0 50.89 9.80 8 -19 0 54.69 4.90 -19 11 0 47.20 9.30 11 8 0 60.29 8.60 -19 11 0 61.49 9.80 8 -19 0 62.99 11.00 11 8 0 52.69 9.40 -11 -8 0 61.99 10.70 -8 19 0 58.19 7.60 -8 19 0 55.99 9.70 -11 -8 0 43.70 8.60 -11 -8 0 71.19 7.10 -8 19 0 63.19 10.60 -8 19 0 54.09 9.40 -19 14 0 5.10 4.70 14 5 0 2.30 4.20 -19 14 0 0.40 3.90 14 5 0 -3.30 2.30 14 5 0 0.60 2.70 -19 14 0 -0.50 3.30 5 -19 0 -0.20 4.10 -19 14 0 -0.50 0.80 5 -19 0 -0.30 2.40 -5 19 0 2.90 1.20 -14 -5 0 -0.70 3.30 -5 19 0 -1.30 4.50 -14 -5 0 3.80 5.00 -5 19 0 -0.90 3.40 -14 -5 0 0.00 2.00 -5 19 0 -2.50 3.80 2 -19 0 8.40 4.70 -19 17 0 4.20 2.20 17 2 0 9.60 5.30 -19 17 0 18.80 7.20 -19 17 0 9.90 5.80 2 -19 0 8.10 5.90 17 2 0 12.20 3.20 -19 17 0 7.80 5.40 -2 19 0 4.10 4.90 -17 -2 0 10.80 7.00 -17 -2 0 6.30 3.60 -2 19 0 5.70 4.30 -2 19 0 5.10 5.20 -2 19 0 8.80 5.30 -20 1 0 87.09 8.60 1 19 0 84.89 12.40 -20 1 0 85.19 13.60 1 19 0 92.89 14.90 1 19 0 87.49 12.30 1 19 0 72.59 12.00 20 -1 0 83.59 11.20 -19 20 0 67.69 12.40 -1 -19 0 68.59 11.90 -1 -19 0 85.59 11.30 -19 20 0 86.49 13.50 -19 20 0 72.29 6.90 -19 20 0 86.19 13.50 4 16 0 -2.10 4.20 4 16 0 -0.60 3.40 4 16 0 4.20 5.10 4 16 0 0.00 3.30 -20 4 0 -1.00 4.20 -20 4 0 0.00 2.70 -20 4 0 5.30 4.70 16 -20 0 -5.40 3.90 -16 20 0 -0.60 0.80 -16 20 0 -1.70 3.40 20 -4 0 -0.50 3.10 -4 -16 0 -0.60 4.00 -16 20 0 1.90 4.60 -16 20 0 -4.90 3.00 -20 7 0 235.78 18.50 7 13 0 240.88 17.00 13 -20 0 233.38 18.20 7 13 0 250.67 18.70 -20 7 0 250.77 18.60 7 13 0 243.28 17.40 7 13 0 234.28 15.80 -20 7 0 216.08 16.00 -13 20 0 236.88 16.50 -13 20 0 245.48 18.40 -7 -13 0 260.57 19.40 20 -7 0 279.07 14.60 -13 20 0 225.38 17.80 -20 10 0 30.50 8.30 -20 10 0 31.10 8.50 -20 10 0 32.00 7.70 10 -20 0 28.10 7.90 10 10 0 32.40 7.00 10 10 0 27.40 7.50 10 10 0 29.50 7.10 -10 -10 0 48.10 7.30 -10 -10 0 43.00 8.90 -10 -10 0 28.60 8.30 -10 20 0 32.60 7.80 -10 20 0 24.60 7.50 -10 20 0 34.50 8.30 -10 20 0 39.10 5.80 13 7 0 32.10 6.60 -20 13 0 43.30 8.90 13 7 0 37.30 8.40 -20 13 0 35.80 8.80 7 -20 0 40.40 9.40 7 -20 0 45.20 6.20 13 7 0 33.90 7.60 -20 13 0 24.90 7.70 -7 20 0 31.50 8.00 -13 -7 0 41.70 6.90 -7 20 0 30.90 8.10 -13 -7 0 32.70 9.70 -13 -7 0 31.70 7.70 -7 20 0 27.60 7.80 -7 20 0 34.40 6.60 16 4 0 52.39 9.50 -20 16 0 37.50 9.20 4 -20 0 41.90 7.30 -20 16 0 49.10 9.80 16 4 0 49.50 7.20 -20 16 0 58.19 11.20 4 -20 0 39.20 9.60 16 4 0 39.90 8.40 -4 20 0 34.60 8.00 -16 -4 0 46.90 10.60 -16 -4 0 38.30 8.70 -16 -4 0 40.30 7.40 -4 20 0 39.90 8.90 -4 20 0 49.10 10.00 -4 20 0 48.40 8.80 -20 19 0 5.50 4.50 -20 19 0 0.80 4.60 1 -20 0 -0.50 4.70 1 -20 0 -3.10 3.50 -20 19 0 1.80 1.70 19 1 0 0.40 3.70 -20 19 0 0.80 3.20 -19 -1 0 2.10 2.80 -1 20 0 3.10 4.50 -1 20 0 0.30 4.30 -1 20 0 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5.80 -8 22 0 1.50 2.50 -8 22 0 -1.40 3.70 17 5 0 -0.90 4.40 -22 17 0 -2.30 3.60 5 -22 0 -0.90 5.10 -22 17 0 -1.10 4.80 -22 17 0 -2.30 2.50 5 -22 0 -2.40 2.70 -5 22 0 3.50 4.80 -17 -5 0 2.00 5.40 -17 -5 0 -1.60 2.10 -5 22 0 2.60 5.20 -5 22 0 8.30 5.10 -5 22 0 1.50 3.40 2 -22 0 15.30 6.10 2 -22 0 18.00 7.60 -22 20 0 17.20 6.50 20 2 0 6.10 5.20 -22 20 0 16.70 7.10 -22 20 0 13.20 7.10 -2 22 0 11.50 5.80 -20 -2 0 9.20 2.50 -20 -2 0 8.70 6.90 -2 22 0 13.30 5.40 -2 22 0 6.20 5.80 -2 22 0 12.50 6.30 1 22 0 12.60 6.00 1 22 0 16.30 6.50 1 22 0 12.80 4.60 1 22 0 13.80 6.30 -23 1 0 16.90 7.70 -1 -22 0 13.30 6.50 -22 23 0 19.20 6.40 -1 -22 0 11.00 7.30 -22 23 0 24.30 8.20 -22 23 0 15.10 7.60 23 -1 0 17.30 6.10 -23 4 0 15.80 7.20 4 19 0 31.20 8.10 19 -23 0 32.80 8.80 -23 4 0 20.00 6.40 4 19 0 26.30 8.20 -23 4 0 18.90 5.10 4 19 0 34.60 8.20 4 19 0 29.30 8.60 -4 -19 0 33.20 9.70 -4 -19 0 27.60 7.80 -19 23 0 23.40 5.90 -19 23 0 36.40 8.30 -19 23 0 28.20 8.80 23 -4 0 16.20 4.60 7 16 0 5.30 4.20 -23 7 0 2.70 4.90 7 16 0 4.10 5.10 7 16 0 4.40 5.50 7 16 0 0.70 3.30 16 -23 0 -3.10 3.70 -23 7 0 0.80 1.20 -23 7 0 3.40 3.80 -16 23 0 0.90 4.20 -16 23 0 1.80 5.40 -16 23 0 0.80 3.00 -7 -16 0 0.00 4.70 10 13 0 -4.30 5.00 10 13 0 -0.40 4.00 -23 10 0 5.00 4.80 10 13 0 2.40 3.50 13 -23 0 2.10 4.40 -23 10 0 4.40 4.30 -23 10 0 -0.10 4.70 -10 -13 0 10.30 4.00 -13 23 0 -1.60 3.20 -13 23 0 5.80 4.30 -10 -13 0 1.70 5.20 -13 23 0 2.20 5.60 13 10 0 13.40 6.30 -23 13 0 26.60 7.50 13 10 0 19.50 6.50 -23 13 0 16.50 6.20 13 10 0 22.80 6.40 10 -23 0 29.40 8.50 -23 13 0 15.20 7.00 -13 -10 0 22.50 5.30 -10 23 0 11.50 6.40 -13 -10 0 23.60 8.20 -10 23 0 32.40 9.00 -10 23 0 15.30 7.00 -10 23 0 27.20 4.90 7 -23 0 -4.30 4.30 7 -23 0 2.10 2.40 16 7 0 -1.40 4.20 -23 16 0 1.50 3.70 -23 16 0 0.60 4.90 -23 16 0 3.00 4.90 16 7 0 4.60 3.20 -16 -7 0 -4.50 1.50 -7 23 0 9.30 3.60 -16 -7 0 5.70 5.70 -7 23 0 -1.90 3.90 -7 23 0 -3.90 2.40 -7 23 0 -4.20 4.00 4 -23 0 19.40 7.70 -23 19 0 18.70 7.30 -23 19 0 12.30 6.00 -23 19 0 14.30 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11.50 7.40 -15 24 0 16.10 7.60 -15 24 0 8.90 5.50 12 12 0 67.59 10.60 12 -24 0 68.19 11.80 -24 12 0 47.70 10.40 -24 12 0 71.79 12.40 12 12 0 72.19 12.10 -24 12 0 53.59 9.90 -12 24 0 70.49 12.20 -12 24 0 49.80 10.20 -12 24 0 46.50 10.30 -12 -12 0 68.09 6.90 -12 -12 0 50.79 11.40 15 9 0 11.90 6.80 15 9 0 8.30 4.50 -24 15 0 15.90 6.10 -24 15 0 24.70 8.00 9 -24 0 21.40 7.20 -24 15 0 9.70 4.70 -9 24 0 19.70 7.40 -9 24 0 11.70 5.30 -15 -9 0 20.40 5.30 -9 24 0 26.40 5.40 -15 -9 0 17.90 8.50 -9 24 0 13.00 6.80 6 -24 0 1.60 4.10 6 -24 0 1.70 5.60 -24 18 0 4.70 5.80 -24 18 0 0.80 3.90 -24 18 0 1.20 4.40 18 6 0 4.20 5.90 -18 -6 0 -1.70 6.00 -6 24 0 2.30 4.70 -6 24 0 -1.10 1.10 -6 24 0 4.20 3.70 -6 24 0 -2.00 4.70 -24 21 0 46.70 10.90 3 -24 0 43.50 8.90 -24 21 0 47.00 10.40 21 3 0 29.20 8.50 3 -24 0 39.50 10.80 -24 21 0 42.20 10.30 -3 24 0 45.60 9.20 -3 24 0 43.00 11.20 -3 24 0 28.10 7.90 -21 -3 0 36.90 10.20 -3 24 0 36.50 9.20 0 -24 0 5.70 4.70 -24 24 0 10.00 4.00 -24 24 0 6.50 5.80 0 -24 0 11.20 6.10 -24 24 0 8.90 6.30 24 0 0 5.20 4.30 0 24 0 12.30 5.80 0 24 0 4.80 5.00 -24 0 0 11.80 4.30 0 24 0 1.80 4.90 0 24 0 8.80 3.70 -24 0 0 4.70 6.00 -25 2 0 7.30 5.60 2 23 0 7.90 6.10 2 23 0 6.40 6.40 2 23 0 0.40 1.90 2 23 0 14.30 5.60 23 -25 0 11.70 7.10 -2 -23 0 7.10 6.10 -23 25 0 10.10 5.70 -23 25 0 7.80 5.20 -23 25 0 3.50 3.10 -2 -23 0 10.60 6.80 -25 5 0 6.70 2.40 5 20 0 4.50 5.30 -25 5 0 -1.70 2.80 5 20 0 0.60 2.80 5 20 0 1.90 3.30 5 20 0 -5.50 4.20 20 -25 0 6.00 5.50 -5 -20 0 -5.20 4.30 -20 25 0 -2.80 2.30 -20 25 0 3.70 6.10 -5 -20 0 -2.40 3.90 -20 25 0 1.10 2.50 -25 8 0 13.70 7.00 8 17 0 17.40 7.20 17 -25 0 22.40 8.00 -25 8 0 13.00 4.60 8 17 0 18.10 4.90 8 17 0 24.40 7.60 8 17 0 18.90 7.50 -17 25 0 21.00 6.30 -17 25 0 18.90 5.70 -17 25 0 9.30 6.40 -8 -17 0 21.10 8.70 -8 -17 0 14.20 7.20 11 14 0 24.80 8.00 -25 11 0 30.60 9.30 -25 11 0 28.50 7.60 14 -25 0 28.30 8.30 -25 11 0 30.90 9.10 11 14 0 30.10 8.10 -14 25 0 27.40 9.00 -11 -14 0 21.70 8.40 -14 25 0 25.10 8.20 -14 25 0 12.90 6.50 -11 -14 0 19.00 4.50 -25 14 0 10.10 5.30 -25 14 0 5.10 5.60 14 11 0 7.50 6.60 -25 14 0 5.50 4.30 14 11 0 19.00 5.60 11 -25 0 0.80 4.30 -14 -11 0 2.10 5.50 -11 25 0 4.80 3.50 -11 25 0 13.10 5.70 -11 25 0 4.30 5.50 17 8 0 20.10 7.60 8 -25 0 9.60 2.90 8 -25 0 14.10 7.20 -25 17 0 23.60 7.60 -25 17 0 2.80 4.60 -25 17 0 9.30 6.20 -8 25 0 17.80 5.90 -8 25 0 8.40 3.10 -8 25 0 14.40 6.50 -8 25 0 11.20 6.50 -17 -8 0 19.90 8.30 -25 20 0 4.70 3.30 5 -25 0 4.90 6.20 -25 20 0 6.20 5.50 5 -25 0 2.30 4.20 20 5 0 -0.60 4.30 -25 20 0 -0.80 4.60 -5 25 0 -3.30 5.50 -5 25 0 -3.50 2.80 -5 25 0 5.80 4.70 -5 25 0 -0.50 2.60 -20 -5 0 -3.10 4.80 2 -25 0 8.50 5.50 -25 23 0 0.70 5.00 23 2 0 3.80 5.00 -25 23 0 9.00 2.90 -25 23 0 11.70 6.60 2 -25 0 4.30 4.90 -2 25 0 1.40 5.50 -23 -2 0 9.10 4.50 -2 25 0 6.80 5.60 -2 25 0 9.00 5.60 -2 25 0 8.60 4.20 -23 -2 0 3.50 5.10 1 25 0 5.00 4.90 1 25 0 5.00 6.00 -26 1 0 5.80 5.40 1 25 0 2.40 2.90 25 -26 0 -1.30 5.40 -1 -25 0 3.20 6.60 -1 -25 0 -3.20 4.90 -25 26 0 6.70 5.60 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3.10 15 8 4 8.10 5.20 15 8 4 9.50 5.10 -5 20 -4 126.29 11.50 -5 20 -4 111.59 12.10 -15 -5 -4 113.29 12.90 -15 -5 -4 104.89 11.30 -5 20 -4 111.99 11.30 -5 20 -4 127.99 13.30 15 5 4 103.29 10.40 -20 15 4 120.39 13.40 15 5 4 101.49 14.00 -20 15 4 138.89 12.10 5 -20 4 120.19 12.60 15 5 4 132.19 12.80 -20 15 4 111.09 11.90 5 -20 4 130.39 10.60 -15 -2 -4 42.30 8.70 -2 17 -4 39.60 8.80 -15 -2 -4 47.30 9.00 -2 17 -4 39.90 9.10 -2 17 -4 61.59 10.50 -2 17 -4 54.79 8.50 15 2 4 40.40 7.90 15 2 4 58.19 11.20 2 -17 4 55.39 10.00 -17 15 4 35.10 8.00 -17 15 4 34.40 3.60 -17 15 4 47.80 10.90 2 -17 4 62.99 10.70 -17 15 4 42.90 8.10 2 -17 4 50.59 7.80 15 2 4 34.50 7.60 1 14 -4 319.87 20.70 -15 1 -4 314.37 20.60 1 14 -4 309.87 17.30 -15 1 -4 308.57 19.30 1 14 -4 313.47 19.60 -15 1 -4 303.17 19.60 1 14 -4 301.57 19.40 -14 15 4 320.77 20.10 -1 -14 4 341.47 20.80 -14 15 4 304.57 18.90 -1 -14 4 324.37 20.90 -1 -14 4 289.37 16.90 -14 15 4 308.97 20.80 15 -1 4 316.47 20.60 15 -1 4 291.77 18.50 -14 15 4 302.47 16.80 -14 15 4 347.97 19.10 15 -1 4 287.17 17.40 4 11 -4 14.60 5.20 4 11 -4 23.50 6.30 -15 4 -4 18.80 5.40 -15 4 -4 15.90 5.80 -15 4 -4 14.40 4.30 4 11 -4 14.60 3.40 4 11 -4 9.80 4.10 -15 4 -4 7.60 4.30 -4 -11 4 11.40 5.40 -11 15 4 9.50 5.30 -11 15 4 6.80 3.40 -11 15 4 9.40 4.20 -11 15 4 11.90 2.40 -11 15 4 12.10 5.40 15 -4 4 8.90 4.80 -11 15 4 14.40 4.20 -4 -11 4 18.20 4.80 15 -4 4 16.20 4.60 -4 -11 4 13.50 5.40 -15 7 -4 168.18 13.70 8 -15 -4 179.98 14.50 -15 7 -4 182.08 13.60 7 8 -4 185.08 12.10 -15 7 -4 186.28 11.40 7 8 -4 173.88 13.30 -15 7 -4 190.38 12.00 7 8 -4 166.28 12.90 -8 15 4 174.28 11.70 -7 -8 4 186.68 13.90 15 -7 4 146.69 10.70 -7 -8 4 174.78 11.50 -8 15 4 170.78 10.40 15 -7 4 171.98 13.80 -7 -8 4 176.58 13.90 -8 15 4 161.58 11.80 -8 15 4 159.48 13.10 -8 15 4 189.28 12.70 10 5 -4 240.28 16.20 -15 10 -4 253.37 14.60 -15 10 -4 238.08 16.60 -15 10 -4 238.18 14.50 5 -15 -4 227.28 16.80 -15 10 -4 225.88 16.80 10 5 -4 255.07 16.00 10 5 -4 253.27 13.80 15 -10 4 217.38 12.90 15 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4.30 -15 7 5 6.10 2.80 -15 7 5 7.90 3.10 -15 7 5 2.60 4.10 7 8 5 -1.00 3.70 8 -15 5 -2.20 3.40 -15 7 5 5.90 3.50 -9 -7 -5 44.00 8.50 -7 16 -5 55.29 10.10 -9 -7 -5 31.20 7.30 -7 16 -5 36.30 7.30 -7 16 -5 41.40 7.70 16 -9 -5 40.00 3.50 9 7 5 40.50 8.70 7 -16 5 36.00 6.80 -16 9 5 34.60 7.00 7 -16 5 39.70 5.80 -16 9 5 40.10 8.80 -16 9 5 33.40 5.90 9 7 5 35.30 7.10 9 7 5 46.60 8.70 7 -16 5 37.90 7.50 -16 9 5 32.10 5.70 -4 13 -5 18.10 5.10 -4 13 -5 17.30 4.90 13 -9 -5 25.10 3.30 -9 -4 -5 24.60 6.40 -9 -4 -5 22.30 5.50 -9 -4 -5 18.20 4.40 -4 13 -5 22.20 5.80 -4 13 -5 26.80 5.80 -13 9 5 29.00 7.00 9 4 5 19.40 5.50 -13 9 5 20.70 1.90 9 4 5 11.00 3.00 4 -13 5 10.20 4.80 -13 9 5 23.00 5.00 9 4 5 14.90 5.50 4 -13 5 20.90 5.00 4 -13 5 23.20 4.70 -13 9 5 20.70 4.90 -13 9 5 22.10 5.00 9 4 5 11.50 4.60 -1 10 -5 43.60 7.20 -9 -1 -5 30.40 6.20 -1 10 -5 48.40 7.40 -1 10 -5 49.60 5.90 -9 -1 -5 39.30 6.10 10 -9 -5 37.10 3.40 -1 10 -5 37.80 6.40 -10 9 5 43.40 7.90 -10 9 5 31.90 3.50 -10 9 5 32.60 5.80 9 1 5 44.90 7.60 1 -10 5 37.80 6.30 9 1 5 38.00 6.80 1 -10 5 43.60 5.90 1 -10 5 39.60 6.80 9 1 5 34.60 6.20 -10 9 5 42.80 5.60 9 1 5 35.70 5.80 1 -10 5 41.20 6.30 -10 9 5 38.90 5.40 2 7 -5 1907.01 79.99 2 7 -5 1943.81 86.29 -9 2 -5 1897.41 86.19 2 7 -5 1897.11 78.09 -9 2 -5 1941.21 80.99 -9 2 -5 1880.31 81.89 2 7 -5 1918.21 79.59 -7 9 5 1971.10 81.39 9 -2 5 1922.41 86.69 9 -2 5 1950.40 86.69 -2 -7 5 2041.00 86.79 -7 9 5 2106.99 78.09 -2 -7 5 1877.61 86.49 -7 9 5 1695.23 78.19 -7 9 5 2038.30 84.09 9 -2 5 1780.82 79.39 9 -2 5 1839.82 79.69 -2 -7 5 2015.60 73.19 -9 5 -5 795.72 35.90 5 4 -5 844.22 35.10 -9 5 -5 776.42 37.10 -9 5 -5 796.12 38.80 4 -9 -5 846.72 38.40 5 4 -5 823.32 38.20 -9 5 -5 787.82 34.60 5 4 -5 820.62 36.10 -5 -4 5 705.03 38.20 -4 9 5 824.12 36.00 -4 9 5 812.82 37.00 -5 -4 5 776.62 37.30 9 -5 5 754.92 39.10 9 -5 5 819.42 35.70 -4 9 5 804.72 36.00 9 -5 5 775.52 39.00 -5 -4 5 792.52 38.40 -4 9 5 824.12 35.10 -4 9 5 795.52 35.80 -9 8 -5 1.80 1.40 -9 8 -5 -0.80 2.20 1 -9 -5 0.30 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-3 2 22 -11.90 4.20 -2 2 -22 9.00 5.30 2 0 -22 5.80 4.30 2 0 -22 -0.40 3.50 0 -2 -22 -0.20 3.10 -2 2 -22 1.10 3.20 0 -2 -22 -4.20 3.00 2 -2 22 -4.40 5.10 -2 0 22 -2.70 5.20 -3 -2 -22 -0.50 3.10 5 -3 -22 -1.50 3.10 -3 -2 -22 8.60 5.20 -2 5 -22 -1.60 2.70 5 -3 -22 4.20 2.40 -2 5 -22 -2.40 3.30 -5 3 22 3.10 5.40 2 -5 22 1.90 6.50 1 2 -22 -2.80 2.60 -3 1 -22 0.60 3.30 1 2 -22 3.00 3.90 -3 1 -22 -6.00 2.90 2 -3 -22 -2.80 2.90 2 -3 -22 8.80 5.40 -1 -2 22 -2.30 5.80 -3 4 -22 4.70 2.80 4 -1 -22 5.80 4.00 -1 -3 -22 -4.30 3.30 -3 4 -22 5.50 5.00 -1 -3 -22 1.50 3.20 4 -1 -22 -3.70 3.10 -4 1 22 1.50 5.10 3 -4 22 -3.50 5.80 0 4 -22 -1.70 3.00 -4 0 -22 3.70 3.90 -4 0 -22 0.00 3.00 4 -4 -22 4.70 3.20 0 4 -22 -2.10 2.50 4 -4 -22 4.40 3.80 0 -4 22 -7.60 6.10 3 1 -22 -1.70 3.40 1 -4 -22 -4.20 3.10 -4 3 -22 5.10 3.80 -4 3 -22 -0.30 3.80 3 1 -22 -4.80 3.40 1 -4 -22 -1.90 3.00 -3 -1 22 1.20 6.80 3 -5 -22 2.50 2.80 3 -5 -22 1.90 3.50 2 3 -22 0.70 3.40 2 3 -22 11.60 4.40 -5 2 -22 3.60 3.70 -5 2 -22 6.20 4.50 -2 -3 22 0.40 5.70 -5 5 -22 7.20 4.70 0 -5 -22 6.60 4.70 -5 0 22 0.60 5.60 5 -5 22 -2.70 5.50 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 6324