data_CSD0796rLT _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 N2 Ni O4.50' _chemical_formula_weight 697.42 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 44.5471(15) _cell_length_b 11.9193(5) _cell_length_c 12.5427(4) _cell_angle_alpha 90 _cell_angle_beta 96.780(3) _cell_angle_gamma 90 _cell_volume 6613.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9613 _cell_measurement_theta_min 2.6260 _cell_measurement_theta_max 28.2030 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.401 _exptl_crystal_F_000 2912 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.090 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 0.636 _shelx_estimated_absorpt_T_min 0.945 _shelx_estimated_absorpt_T_max 0.994 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.46659 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source 'Microfocus rotating anode X-ray tube' _diffrn_source_type 'Rigaku MicroMax-007HF' _diffrn_source_power 50 _diffrn_source_current 24 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_radiation_monochromator 'Confocal Max Flux optic' _diffrn_detector_type 'PILATUS 200K' _diffrn_measurement_device_type '1/4chi goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 5.8140 _diffrn_reflns_number 28776 _diffrn_reflns_av_unetI/netI 0.0522 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 59 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.446 _diffrn_reflns_theta_max 28.951 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.850 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.850 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.850 _diffrn_reflns_point_group_measured_fraction_full 0.987 _reflns_number_total 7433 _reflns_number_gt 5375 _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 'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)' _computing_cell_refinement 'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.12b (Rigaku OD, 2015)' _computing_structure_solution 'Sir2019' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'shelXle (Hübschle, Sheldrick and Dittirch, 2011)' _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _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^)+(0.0534P)^2^+14.1224P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7433 _refine_ls_number_parameters 494 _refine_ls_number_restraints 194 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 C1 C 0.59264(5) 0.8726(2) 0.34863(19) 0.0172(5) Uani 1 1 d . . . . . N1 N 0.60989(4) 0.81828(16) 0.28541(15) 0.0148(4) Uani 1 1 d . . . . . O1 O 0.64283(4) 0.99210(14) 0.13354(13) 0.0167(3) Uani 1 1 d . U . . . Ni1 Ni 0.61510(2) 0.84578(3) 0.12679(2) 0.01444(10) Uani 1 1 d . . . . . C2 C 0.57653(6) 0.9770(2) 0.30838(19) 0.0202(5) Uani 1 1 d . . . . . H2B H 0.555195 0.959774 0.286108 0.030 Uiso 1 1 calc R U . . . H2C H 0.585759 1.006326 0.246933 0.030 Uiso 1 1 calc R U . . . H2F H 0.578051 1.033292 0.365700 0.030 Uiso 1 1 calc R U . . . N2 N 0.64955(4) 0.72677(16) 0.16289(15) 0.0144(4) Uani 1 1 d . . . . . O2 O 0.62812(4) 0.91021(15) -0.01806(14) 0.0233(4) Uani 1 1 d . . . . . C3 C 0.58944(5) 0.8330(2) 0.45239(19) 0.0179(5) Uani 1 1 d . . . . . H3 H 0.577131 0.873727 0.495790 0.021 Uiso 1 1 calc R U . . . O3 O 0.57139(4) 0.90607(14) 0.07171(13) 0.0192(4) Uani 1 1 d . . . . . C4 C 0.60361(5) 0.7373(2) 0.49248(18) 0.0169(5) Uani 1 1 d . . . . . O4 O 0.58361(4) 0.72829(14) 0.06267(13) 0.0192(4) Uani 1 1 d . . . . . C5 C 0.62349(5) 0.6827(2) 0.42784(18) 0.0158(5) Uani 1 1 d . . . . . C6 C 0.64233(6) 0.5908(2) 0.46600(19) 0.0200(5) Uani 1 1 d . . . . . H6 H 0.640581 0.560091 0.534885 0.024 Uiso 1 1 calc R U . . . C7 C 0.66254(6) 0.5470(2) 0.40583(19) 0.0209(5) Uani 1 1 d . . . . . H7 H 0.674770 0.485725 0.432898 0.025 Uiso 1 1 calc R U . . . C8 C 0.66590(5) 0.5910(2) 0.30246(19) 0.0172(5) Uani 1 1 d . . . . . C9 C 0.68798(5) 0.5499(2) 0.24007(19) 0.0183(5) Uani 1 1 d . . . . . C10 C 0.68963(5) 0.5977(2) 0.14191(19) 0.0171(5) Uani 1 1 d . . . . . H10 H 0.704125 0.570739 0.098289 0.021 Uiso 1 1 calc R U . . . C11 C 0.67032(5) 0.6859(2) 0.10430(18) 0.0156(5) Uani 1 1 d . . . . . C12 C 0.67396(6) 0.7376(2) -0.00201(19) 0.0222(6) Uani 1 1 d . . . . . H12G H 0.689512 0.696881 -0.035428 0.033 Uiso 1 1 calc R U . . . H12H H 0.680020 0.816284 0.008377 0.033 Uiso 1 1 calc R U . . . H12I H 0.654722 0.733672 -0.048662 0.033 Uiso 1 1 calc R U . . . C13 C 0.64737(5) 0.6794(2) 0.26090(18) 0.0149(5) Uani 1 1 d . . . . . C14 C 0.62591(5) 0.7273(2) 0.32564(18) 0.0154(5) Uani 1 1 d . . . . . C15 C 0.59928(5) 0.6924(2) 0.60013(19) 0.0174(5) Uani 1 1 d . . . . . C16 C 0.60494(6) 0.7606(2) 0.69037(19) 0.0206(5) Uani 1 1 d . . . . . H16 H 0.611680 0.835533 0.682989 0.025 Uiso 1 1 calc R U . . . C17 C 0.60078(6) 0.7195(2) 0.7910(2) 0.0237(6) Uani 1 1 d . . . . . H17 H 0.604498 0.766500 0.852338 0.028 Uiso 1 1 calc R U . . . C18 C 0.59121(6) 0.6101(2) 0.8024(2) 0.0256(6) Uani 1 1 d . . . . . H18 H 0.588368 0.582273 0.871498 0.031 Uiso 1 1 calc R U . . . C19 C 0.58577(6) 0.5412(2) 0.7135(2) 0.0269(6) Uani 1 1 d . . . . . H19 H 0.579285 0.466011 0.721461 0.032 Uiso 1 1 calc R U . . . C20 C 0.58979(6) 0.5820(2) 0.6128(2) 0.0225(6) Uani 1 1 d . . . . . H20 H 0.586070 0.534593 0.551763 0.027 Uiso 1 1 calc R U . . . C21 C 0.70943(6) 0.4605(2) 0.2823(2) 0.0257(6) Uani 1 1 d . . . . . C22 C 0.73297(7) 0.4872(3) 0.3637(3) 0.0367(7) Uani 1 1 d . . . . . H22 H 0.735045 0.561887 0.389909 0.044 Uiso 1 1 calc R U . . . C23 C 0.75296(7) 0.4060(3) 0.4053(3) 0.0406(8) Uani 1 1 d . . . . . H23 H 0.768767 0.423751 0.460359 0.049 Uiso 1 1 calc R U . . . C24 C 0.74961(7) 0.2991(3) 0.3659(2) 0.0367(7) Uani 1 1 d . . . . . H24 H 0.763567 0.243278 0.394105 0.044 Uiso 1 1 calc R U . . . C25 C 0.72719(8) 0.2693(3) 0.2880(2) 0.0396(8) Uani 1 1 d . . . . . H25 H 0.725285 0.194086 0.262993 0.048 Uiso 1 1 calc R U . . . C26 C 0.70663(7) 0.3536(3) 0.2451(2) 0.0346(7) Uani 1 1 d . . . . . H26 H 0.690880 0.335124 0.190129 0.042 Uiso 1 1 calc R U . . . C27 C 0.64405(5) 0.9826(2) 0.03759(19) 0.0180(3) Uani 1 1 d . U . . . C28 C 0.66640(6) 1.0505(2) -0.0151(2) 0.0217(6) Uani 1 1 d . . . . . C29 C 0.68375(6) 1.1321(2) 0.0431(2) 0.0272(6) Uani 1 1 d . . . . . H29 H 0.680507 1.147953 0.115126 0.033 Uiso 1 1 calc R U . . . C30 C 0.70572(6) 1.1901(2) -0.0039(2) 0.0300(6) Uani 1 1 d . . . . . H30 H 0.717465 1.245846 0.035935 0.036 Uiso 1 1 calc R U . . . C31 C 0.71060(6) 1.1674(3) -0.1079(2) 0.0310(7) Uani 1 1 d . . . . . H31 H 0.725810 1.206923 -0.139619 0.037 Uiso 1 1 calc R U . . . C32 C 0.69335(6) 1.0870(2) -0.1663(2) 0.0282(6) Uani 1 1 d . . . . . H32 H 0.696766 1.071535 -0.238215 0.034 Uiso 1 1 calc R U . . . C33 C 0.67126(6) 1.0291(2) -0.1211(2) 0.0248(6) Uani 1 1 d . . . . . H33 H 0.659340 0.974646 -0.162050 0.030 Uiso 1 1 calc R U . . . C34 C 0.56464(6) 0.8070(2) 0.04207(18) 0.0184(5) Uani 1 1 d . . . . . C35 C 0.53434(6) 0.7831(2) -0.01877(19) 0.0220(6) Uani 1 1 d . . . . . C36 C 0.51524(6) 0.8712(3) -0.0522(2) 0.0293(7) Uani 1 1 d . . . . . H36 H 0.521316 0.946160 -0.035465 0.035 Uiso 1 1 calc R U . . . C37 C 0.48723(6) 0.8504(3) -0.1100(2) 0.0386(8) Uani 1 1 d . . . . . H37 H 0.474092 0.910936 -0.132306 0.046 Uiso 1 1 calc R U . . . C38 C 0.47859(7) 0.7412(3) -0.1348(2) 0.0430(9) Uani 1 1 d . . . . . H38 H 0.459563 0.726742 -0.175061 0.052 Uiso 1 1 calc R U . . . C39 C 0.49738(7) 0.6536(3) -0.1014(3) 0.0459(9) Uani 1 1 d . . . . . H39 H 0.491219 0.578738 -0.118330 0.055 Uiso 1 1 calc R U . . . C40 C 0.52545(7) 0.6737(3) -0.0429(2) 0.0344(7) Uani 1 1 d . . . . . H40 H 0.538385 0.612831 -0.019760 0.041 Uiso 1 1 calc R U . . . O1S O 0.500000 0.7834(10) 0.250000 0.082(2) Uani 0.5 2 d DS TU P A 1 C1S C 0.5246(2) 0.7033(8) 0.2917(9) 0.066(2) Uani 0.5 1 d D U P A 1 H1SA H 0.525374 0.692239 0.370175 0.079 Uiso 0.5 1 calc R U P A 1 H1SB H 0.544649 0.728940 0.274517 0.079 Uiso 0.5 1 calc R U P A 1 C2S C 0.5143(2) 0.5964(8) 0.2293(9) 0.058(2) Uani 0.5 1 d D U P A 1 H2SA H 0.512589 0.606150 0.150475 0.069 Uiso 0.5 1 calc R U P A 1 H2SB H 0.526847 0.529976 0.251685 0.069 Uiso 0.5 1 calc R U P A 1 O1S' O 0.5154(3) 0.6120(12) 0.3051(11) 0.068(2) Uani 0.25 1 d D U P B -2 C1S' C 0.5322(4) 0.6985(14) 0.2657(19) 0.069(3) Uani 0.25 1 d D U P B -2 H1SC H 0.535891 0.683849 0.190685 0.083 Uiso 0.25 1 calc R U P B -2 H1SD H 0.551750 0.708954 0.310747 0.083 Uiso 0.25 1 calc R U P B -2 C2S' C 0.5114(4) 0.8005(18) 0.273(2) 0.072(3) Uani 0.25 1 d D U P B -2 H2SX H 0.518241 0.865305 0.232647 0.086 Uiso 0.25 1 calc R U P B -2 H2SY H 0.510361 0.822812 0.348294 0.086 Uiso 0.25 1 calc R U P B -2 C3S' C 0.4798(4) 0.7552(14) 0.2190(19) 0.063(3) Uani 0.25 1 d D U P B -2 H3SA H 0.462697 0.785846 0.253327 0.075 Uiso 0.25 1 calc R U P B -2 H3SB H 0.476664 0.769568 0.140697 0.075 Uiso 0.25 1 calc R U P B -2 C4S' C 0.4856(5) 0.6286(17) 0.246(2) 0.069(3) Uani 0.25 1 d D U P B -2 H4SA H 0.469939 0.600598 0.288639 0.082 Uiso 0.25 1 calc R U P B -2 H4SB H 0.484138 0.584873 0.178029 0.082 Uiso 0.25 1 calc R U P B -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 C1 0.0171(12) 0.0159(13) 0.0179(11) -0.0038(10) -0.0009(9) -0.0023(10) N1 0.0153(10) 0.0140(10) 0.0142(9) -0.0005(8) -0.0012(8) 0.0002(8) O1 0.0162(5) 0.0147(5) 0.0187(4) -0.0012(4) 0.0000(4) 0.0001(4) Ni1 0.01612(16) 0.01332(16) 0.01314(15) 0.00103(13) -0.00137(11) 0.00032(13) C2 0.0257(14) 0.0165(13) 0.0181(12) -0.0006(11) 0.0014(10) 0.0041(11) N2 0.0168(10) 0.0125(10) 0.0134(9) -0.0004(8) -0.0009(8) -0.0024(8) O2 0.0257(10) 0.0216(10) 0.0215(9) 0.0001(8) -0.0015(7) -0.0027(8) C3 0.0174(12) 0.0196(13) 0.0165(11) -0.0047(10) 0.0016(9) 0.0006(10) O3 0.0181(9) 0.0188(9) 0.0196(8) -0.0010(8) -0.0021(7) -0.0004(7) C4 0.0188(12) 0.0179(13) 0.0137(11) -0.0022(10) 0.0003(9) -0.0017(10) O4 0.0185(9) 0.0188(9) 0.0196(8) -0.0005(8) -0.0010(7) -0.0011(7) C5 0.0164(12) 0.0158(12) 0.0149(11) 0.0001(10) 0.0003(9) -0.0019(10) C6 0.0229(13) 0.0215(14) 0.0154(11) 0.0037(11) 0.0019(10) 0.0022(11) C7 0.0225(13) 0.0196(13) 0.0204(12) 0.0073(11) 0.0010(10) 0.0053(11) C8 0.0170(12) 0.0175(13) 0.0167(11) 0.0009(10) 0.0002(9) -0.0009(10) C9 0.0171(12) 0.0184(13) 0.0190(12) -0.0003(11) 0.0012(9) 0.0006(10) C10 0.0175(12) 0.0170(13) 0.0171(11) -0.0028(10) 0.0026(9) -0.0018(10) C11 0.0171(12) 0.0144(12) 0.0149(11) -0.0027(10) -0.0005(9) -0.0037(10) C12 0.0302(14) 0.0182(13) 0.0188(12) 0.0016(11) 0.0060(10) 0.0007(11) C13 0.0155(12) 0.0145(12) 0.0141(11) -0.0009(10) -0.0003(9) -0.0025(10) C14 0.0150(12) 0.0146(12) 0.0157(11) -0.0003(10) -0.0023(9) -0.0015(10) C15 0.0166(12) 0.0193(13) 0.0162(11) 0.0005(10) 0.0013(9) 0.0032(10) C16 0.0229(13) 0.0199(13) 0.0187(12) 0.0000(11) 0.0015(10) 0.0011(11) C17 0.0241(14) 0.0306(16) 0.0156(12) -0.0020(12) -0.0008(10) 0.0065(12) C18 0.0242(14) 0.0345(16) 0.0184(12) 0.0109(12) 0.0045(10) 0.0082(13) C19 0.0296(15) 0.0243(15) 0.0282(14) 0.0049(12) 0.0093(11) 0.0002(12) C20 0.0252(14) 0.0225(14) 0.0204(12) -0.0032(11) 0.0057(10) -0.0035(11) C21 0.0241(14) 0.0311(16) 0.0237(13) 0.0085(12) 0.0103(11) 0.0107(12) C22 0.0269(16) 0.0349(18) 0.0461(18) 0.0072(15) -0.0043(13) 0.0027(13) C23 0.0287(17) 0.047(2) 0.0447(18) 0.0072(17) -0.0016(14) 0.0053(15) C24 0.0324(17) 0.045(2) 0.0346(16) 0.0062(15) 0.0111(13) 0.0162(15) C25 0.053(2) 0.0364(18) 0.0313(16) -0.0065(14) 0.0129(14) 0.0153(16) C26 0.0458(18) 0.0346(17) 0.0226(14) 0.0000(13) 0.0001(12) 0.0111(15) C27 0.0171(6) 0.0158(6) 0.0204(5) 0.0000(5) -0.0001(5) 0.0006(5) C28 0.0228(14) 0.0170(13) 0.0245(13) 0.0025(11) -0.0008(10) 0.0024(11) C29 0.0316(15) 0.0254(15) 0.0247(13) -0.0029(12) 0.0036(11) -0.0028(12) C30 0.0287(16) 0.0256(15) 0.0352(15) -0.0017(13) 0.0020(12) -0.0077(12) C31 0.0262(15) 0.0337(17) 0.0336(15) 0.0067(14) 0.0048(12) -0.0028(13) C32 0.0298(15) 0.0332(17) 0.0215(13) 0.0019(12) 0.0024(11) 0.0033(13) C33 0.0279(15) 0.0221(14) 0.0231(13) 0.0040(12) -0.0023(11) 0.0000(12) C34 0.0201(13) 0.0217(13) 0.0132(11) 0.0027(10) 0.0013(9) 0.0000(11) C35 0.0168(13) 0.0324(16) 0.0168(12) -0.0021(12) 0.0022(10) -0.0048(11) C36 0.0212(14) 0.0395(18) 0.0262(14) 0.0060(13) -0.0015(11) -0.0030(12) C37 0.0210(15) 0.064(2) 0.0298(15) 0.0109(16) -0.0024(11) -0.0024(15) C38 0.0196(15) 0.079(3) 0.0298(16) -0.0113(17) -0.0003(12) -0.0132(17) C39 0.0278(17) 0.057(2) 0.053(2) -0.0249(18) 0.0039(14) -0.0163(17) C40 0.0254(15) 0.0374(18) 0.0405(17) -0.0123(14) 0.0035(12) -0.0063(13) O1S 0.077(5) 0.083(4) 0.087(4) 0.000 0.012(4) 0.000 C1S 0.041(4) 0.080(4) 0.077(4) -0.011(4) 0.006(3) -0.018(3) C2S 0.043(3) 0.050(4) 0.079(4) -0.008(3) 0.006(3) 0.000(3) O1S' 0.059(4) 0.069(4) 0.079(5) 0.006(4) 0.014(4) 0.004(4) C1S' 0.053(4) 0.077(4) 0.078(5) -0.010(4) 0.008(4) -0.008(4) C2S' 0.060(5) 0.075(5) 0.079(5) -0.012(4) 0.002(5) -0.023(4) C3S' 0.055(5) 0.061(5) 0.070(5) -0.004(5) -0.004(5) -0.017(4) C4S' 0.060(4) 0.068(5) 0.079(5) -0.003(4) 0.011(4) -0.012(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 C1 N1 1.335(3) . ? C1 C3 1.407(3) . ? C1 C2 1.494(3) . ? N1 C14 1.362(3) . ? N1 Ni1 2.0565(19) . ? O1 C27 1.216(3) . ? O1 Ni1 2.1330(16) . ? Ni1 O4 2.0760(17) . ? Ni1 N2 2.100(2) . ? Ni1 O3 2.1138(16) . ? Ni1 O2 2.1155(18) . ? Ni1 C34 2.415(2) . ? Ni1 C27 2.432(3) . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C2 H2F 0.9800 . ? N2 C11 1.340(3) . ? N2 C13 1.366(3) . ? O2 C27 1.272(3) . ? C3 C4 1.371(3) . ? C3 H3 0.9500 . ? O3 C34 1.263(3) . ? C4 C5 1.426(3) . ? C4 C15 1.486(3) . ? O4 C34 1.269(3) . ? C5 C14 1.403(3) . ? C5 C6 1.428(3) . ? C6 C7 1.346(4) . ? C6 H6 0.9500 . ? C7 C8 1.423(3) . ? C7 H7 0.9500 . ? C8 C13 1.401(3) . ? C8 C9 1.414(3) . ? C9 C10 1.366(3) . ? C9 C21 1.487(4) . ? C10 C11 1.404(3) . ? C10 H10 0.9500 . ? C11 C12 1.495(3) . ? C12 H12G 0.9800 . ? C12 H12H 0.9800 . ? C12 H12I 0.9800 . ? C13 C14 1.443(3) . ? C15 C16 1.392(3) . ? C15 C20 1.396(4) . ? C16 C17 1.387(3) . ? C16 H16 0.9500 . ? C17 C18 1.384(4) . ? C17 H17 0.9500 . ? C18 C19 1.384(4) . ? C18 H18 0.9500 . ? C19 C20 1.385(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C26 1.357(4) . ? C21 C22 1.411(4) . ? C22 C23 1.376(4) . ? C22 H22 0.9500 . ? C23 C24 1.369(5) . ? C23 H23 0.9500 . ? C24 C25 1.359(5) . ? C24 H24 0.9500 . ? C25 C26 1.422(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.496(4) . ? C28 C29 1.394(4) . ? C28 C33 1.396(4) . ? C29 C30 1.386(4) . ? C29 H29 0.9500 . ? C30 C31 1.374(4) . ? C30 H30 0.9500 . ? C31 C32 1.384(4) . ? C31 H31 0.9500 . ? C32 C33 1.378(4) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.497(3) . ? C35 C36 1.385(4) . ? C35 C40 1.387(4) . ? C36 C37 1.389(4) . ? C36 H36 0.9500 . ? C37 C38 1.383(5) . ? C37 H37 0.9500 . ? C38 C39 1.373(5) . ? C38 H38 0.9500 . ? C39 C40 1.394(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? O1S C1S 1.501(8) . ? O1S C1S 1.501(8) 2_655 ? C1S C2S 1.537(8) . ? C1S H1SA 0.9900 . ? C1S H1SB 0.9900 . ? C2S C2S 1.432(19) 2_655 ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? O1S' C1S' 1.397(10) . ? O1S' C4S' 1.456(10) . ? C1S' C2S' 1.538(10) . ? C1S' H1SC 0.9900 . ? C1S' H1SD 0.9900 . ? C2S' C3S' 1.579(9) . ? C2S' H2SX 0.9900 . ? C2S' H2SY 0.9900 . ? C3S' C4S' 1.561(10) . ? C3S' H3SA 0.9900 . ? C3S' H3SB 0.9900 . ? C4S' H4SA 0.9900 . ? C4S' H4SB 0.9900 . ? 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 C1 C3 121.0(2) . . ? N1 C1 C2 119.4(2) . . ? C3 C1 C2 119.6(2) . . ? C1 N1 C14 118.6(2) . . ? C1 N1 Ni1 129.49(16) . . ? C14 N1 Ni1 111.79(15) . . ? C27 O1 Ni1 88.74(15) . . ? N1 Ni1 O4 96.83(7) . . ? N1 Ni1 N2 81.19(8) . . ? O4 Ni1 N2 94.08(7) . . ? N1 Ni1 O3 99.52(7) . . ? O4 Ni1 O3 63.15(7) . . ? N2 Ni1 O3 157.21(7) . . ? N1 Ni1 O2 164.25(7) . . ? O4 Ni1 O2 98.82(7) . . ? N2 Ni1 O2 99.38(7) . . ? O3 Ni1 O2 86.06(7) . . ? N1 Ni1 O1 102.88(7) . . ? O4 Ni1 O1 158.22(7) . . ? N2 Ni1 O1 97.98(7) . . ? O3 Ni1 O1 103.99(6) . . ? O2 Ni1 O1 61.39(6) . . ? N1 Ni1 C34 100.92(8) . . ? O4 Ni1 C34 31.69(8) . . ? N2 Ni1 C34 125.76(8) . . ? O3 Ni1 C34 31.51(8) . . ? O2 Ni1 C34 91.54(7) . . ? O1 Ni1 C34 132.73(8) . . ? N1 Ni1 C27 132.73(8) . . ? O4 Ni1 C27 130.16(7) . . ? N2 Ni1 C27 97.96(8) . . ? O3 Ni1 C27 98.04(7) . . ? O2 Ni1 C27 31.52(7) . . ? O1 Ni1 C27 30.00(7) . . ? C34 Ni1 C27 116.26(8) . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C2 H2F 109.5 . . ? H2B C2 H2F 109.5 . . ? H2C C2 H2F 109.5 . . ? C11 N2 C13 118.1(2) . . ? C11 N2 Ni1 131.46(16) . . ? C13 N2 Ni1 110.20(15) . . ? C27 O2 Ni1 88.10(14) . . ? C4 C3 C1 121.7(2) . . ? C4 C3 H3 119.1 . . ? C1 C3 H3 119.1 . . ? C34 O3 Ni1 87.51(14) . . ? C3 C4 C5 117.5(2) . . ? C3 C4 C15 122.0(2) . . ? C5 C4 C15 120.6(2) . . ? C34 O4 Ni1 89.05(15) . . ? C14 C5 C4 117.8(2) . . ? C14 C5 C6 119.4(2) . . ? C4 C5 C6 122.6(2) . . ? C7 C6 C5 121.0(2) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 121.2(2) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C13 C8 C9 118.2(2) . . ? C13 C8 C7 119.7(2) . . ? C9 C8 C7 122.1(2) . . ? C10 C9 C8 118.0(2) . . ? C10 C9 C21 121.3(2) . . ? C8 C9 C21 120.7(2) . . ? C9 C10 C11 121.2(2) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? N2 C11 C10 121.6(2) . . ? N2 C11 C12 119.6(2) . . ? C10 C11 C12 118.8(2) . . ? C11 C12 H12G 109.5 . . ? C11 C12 H12H 109.5 . . ? H12G C12 H12H 109.5 . . ? C11 C12 H12I 109.5 . . ? H12G C12 H12I 109.5 . . ? H12H C12 H12I 109.5 . . ? N2 C13 C8 123.0(2) . . ? N2 C13 C14 117.7(2) . . ? C8 C13 C14 119.2(2) . . ? N1 C14 C5 123.1(2) . . ? N1 C14 C13 117.3(2) . . ? C5 C14 C13 119.5(2) . . ? C16 C15 C20 119.1(2) . . ? C16 C15 C4 119.9(2) . . ? C20 C15 C4 121.0(2) . . ? C17 C16 C15 120.2(2) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 120.2(2) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 120.2(2) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C15 120.5(2) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? C26 C21 C22 119.4(3) . . ? C26 C21 C9 121.4(3) . . ? C22 C21 C9 119.2(3) . . ? C23 C22 C21 120.6(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 118.7(3) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C25 C24 C23 122.9(3) . . ? C25 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? C24 C25 C26 118.2(3) . . ? C24 C25 H25 120.9 . . ? C26 C25 H25 120.9 . . ? C21 C26 C25 120.3(3) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? O1 C27 O2 121.2(2) . . ? O1 C27 C28 119.8(2) . . ? O2 C27 C28 118.8(2) . . ? O1 C27 Ni1 61.26(13) . . ? O2 C27 Ni1 60.39(13) . . ? C28 C27 Ni1 169.30(18) . . ? C29 C28 C33 119.2(3) . . ? C29 C28 C27 120.2(2) . . ? C33 C28 C27 120.5(2) . . ? C30 C29 C28 120.1(3) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C31 C30 C29 120.3(3) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 119.9(3) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C33 C32 C31 120.5(3) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C28 120.0(3) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? O3 C34 O4 120.1(2) . . ? O3 C34 C35 119.8(2) . . ? O4 C34 C35 120.1(2) . . ? O3 C34 Ni1 60.98(12) . . ? O4 C34 Ni1 59.26(12) . . ? C35 C34 Ni1 175.48(17) . . ? C36 C35 C40 119.9(3) . . ? C36 C35 C34 119.7(2) . . ? C40 C35 C34 120.5(3) . . ? C35 C36 C37 120.3(3) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C38 C37 C36 119.6(3) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C39 C38 C37 120.3(3) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 120.5(3) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C35 C40 C39 119.5(3) . . ? C35 C40 H40 120.3 . . ? C39 C40 H40 120.3 . . ? C1S O1S C1S 101.1(9) . 2_655 ? O1S C1S C2S 100.8(8) . . ? O1S C1S H1SA 111.6 . . ? C2S C1S H1SA 111.6 . . ? O1S C1S H1SB 111.6 . . ? C2S C1S H1SB 111.6 . . ? H1SA C1S H1SB 109.4 . . ? C2S C2S C1S 92.4(8) 2_655 . ? C2S C2S H2SA 113.2 2_655 . ? C1S C2S H2SA 113.2 . . ? C2S C2S H2SB 113.2 2_655 . ? C1S C2S H2SB 113.2 . . ? H2SA C2S H2SB 110.6 . . ? C1S' O1S' C4S' 102.2(18) . . ? O1S' C1S' C2S' 102.2(16) . . ? O1S' C1S' H1SC 111.3 . . ? C2S' C1S' H1SC 111.3 . . ? O1S' C1S' H1SD 111.3 . . ? C2S' C1S' H1SD 111.3 . . ? H1SC C1S' H1SD 109.2 . . ? C1S' C2S' C3S' 102.5(17) . . ? C1S' C2S' H2SX 111.3 . . ? C3S' C2S' H2SX 111.3 . . ? C1S' C2S' H2SY 111.3 . . ? C3S' C2S' H2SY 111.3 . . ? H2SX C2S' H2SY 109.2 . . ? C4S' C3S' C2S' 97.1(15) . . ? C4S' C3S' H3SA 112.3 . . ? C2S' C3S' H3SA 112.3 . . ? C4S' C3S' H3SB 112.3 . . ? C2S' C3S' H3SB 112.3 . . ? H3SA C3S' H3SB 109.9 . . ? O1S' C4S' C3S' 111.0(16) . . ? O1S' C4S' H4SA 109.4 . . ? C3S' C4S' H4SA 109.4 . . ? O1S' C4S' H4SB 109.4 . . ? C3S' C4S' H4SB 109.4 . . ? H4SA C4S' H4SB 108.0 . . ? 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 C3 C1 N1 C14 -4.1(3) . . . . ? C2 C1 N1 C14 176.0(2) . . . . ? C3 C1 N1 Ni1 172.59(17) . . . . ? C2 C1 N1 Ni1 -7.4(3) . . . . ? N1 C1 C3 C4 -0.4(4) . . . . ? C2 C1 C3 C4 179.5(2) . . . . ? C1 C3 C4 C5 4.1(3) . . . . ? C1 C3 C4 C15 -177.4(2) . . . . ? C3 C4 C5 C14 -3.3(3) . . . . ? C15 C4 C5 C14 178.1(2) . . . . ? C3 C4 C5 C6 172.1(2) . . . . ? C15 C4 C5 C6 -6.5(4) . . . . ? C14 C5 C6 C7 0.6(4) . . . . ? C4 C5 C6 C7 -174.7(2) . . . . ? C5 C6 C7 C8 0.2(4) . . . . ? C6 C7 C8 C13 -1.7(4) . . . . ? C6 C7 C8 C9 176.9(2) . . . . ? C13 C8 C9 C10 -1.1(3) . . . . ? C7 C8 C9 C10 -179.6(2) . . . . ? C13 C8 C9 C21 176.6(2) . . . . ? C7 C8 C9 C21 -2.0(4) . . . . ? C8 C9 C10 C11 0.8(4) . . . . ? C21 C9 C10 C11 -176.9(2) . . . . ? C13 N2 C11 C10 -0.6(3) . . . . ? Ni1 N2 C11 C10 -173.83(17) . . . . ? C13 N2 C11 C12 -178.3(2) . . . . ? Ni1 N2 C11 C12 8.5(3) . . . . ? C9 C10 C11 N2 0.1(4) . . . . ? C9 C10 C11 C12 177.8(2) . . . . ? C11 N2 C13 C8 0.3(3) . . . . ? Ni1 N2 C13 C8 174.87(18) . . . . ? C11 N2 C13 C14 177.2(2) . . . . ? Ni1 N2 C13 C14 -8.2(2) . . . . ? C9 C8 C13 N2 0.6(4) . . . . ? C7 C8 C13 N2 179.2(2) . . . . ? C9 C8 C13 C14 -176.3(2) . . . . ? C7 C8 C13 C14 2.3(3) . . . . ? C1 N1 C14 C5 4.8(3) . . . . ? Ni1 N1 C14 C5 -172.37(18) . . . . ? C1 N1 C14 C13 -171.9(2) . . . . ? Ni1 N1 C14 C13 10.9(3) . . . . ? C4 C5 C14 N1 -1.1(3) . . . . ? C6 C5 C14 N1 -176.6(2) . . . . ? C4 C5 C14 C13 175.6(2) . . . . ? C6 C5 C14 C13 0.0(3) . . . . ? N2 C13 C14 N1 -1.7(3) . . . . ? C8 C13 C14 N1 175.4(2) . . . . ? N2 C13 C14 C5 -178.5(2) . . . . ? C8 C13 C14 C5 -1.5(3) . . . . ? C3 C4 C15 C16 -55.1(3) . . . . ? C5 C4 C15 C16 123.3(3) . . . . ? C3 C4 C15 C20 125.4(3) . . . . ? C5 C4 C15 C20 -56.2(3) . . . . ? C20 C15 C16 C17 -0.9(4) . . . . ? C4 C15 C16 C17 179.6(2) . . . . ? C15 C16 C17 C18 0.5(4) . . . . ? C16 C17 C18 C19 0.0(4) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C18 C19 C20 C15 -0.1(4) . . . . ? C16 C15 C20 C19 0.6(4) . . . . ? C4 C15 C20 C19 -179.9(2) . . . . ? C10 C9 C21 C26 -76.0(4) . . . . ? C8 C9 C21 C26 106.4(3) . . . . ? C10 C9 C21 C22 104.7(3) . . . . ? C8 C9 C21 C22 -72.9(3) . . . . ? C26 C21 C22 C23 -0.1(4) . . . . ? C9 C21 C22 C23 179.2(3) . . . . ? C21 C22 C23 C24 0.3(5) . . . . ? C22 C23 C24 C25 -0.7(5) . . . . ? C23 C24 C25 C26 0.9(5) . . . . ? C22 C21 C26 C25 0.2(4) . . . . ? C9 C21 C26 C25 -179.0(3) . . . . ? C24 C25 C26 C21 -0.6(5) . . . . ? Ni1 O1 C27 O2 7.3(2) . . . . ? Ni1 O1 C27 C28 -167.8(2) . . . . ? Ni1 O2 C27 O1 -7.4(2) . . . . ? Ni1 O2 C27 C28 167.8(2) . . . . ? O1 C27 C28 C29 -6.1(4) . . . . ? O2 C27 C28 C29 178.7(2) . . . . ? Ni1 C27 C28 C29 -98.6(10) . . . . ? O1 C27 C28 C33 170.5(2) . . . . ? O2 C27 C28 C33 -4.7(4) . . . . ? Ni1 C27 C28 C33 78.1(10) . . . . ? C33 C28 C29 C30 -0.6(4) . . . . ? C27 C28 C29 C30 176.1(2) . . . . ? C28 C29 C30 C31 -0.2(4) . . . . ? C29 C30 C31 C32 0.6(4) . . . . ? C30 C31 C32 C33 -0.1(4) . . . . ? C31 C32 C33 C28 -0.8(4) . . . . ? C29 C28 C33 C32 1.1(4) . . . . ? C27 C28 C33 C32 -175.6(2) . . . . ? Ni1 O3 C34 O4 4.3(2) . . . . ? Ni1 O3 C34 C35 -174.9(2) . . . . ? Ni1 O4 C34 O3 -4.3(2) . . . . ? Ni1 O4 C34 C35 174.8(2) . . . . ? O3 C34 C35 C36 6.9(4) . . . . ? O4 C34 C35 C36 -172.2(2) . . . . ? O3 C34 C35 C40 -173.8(2) . . . . ? O4 C34 C35 C40 7.1(4) . . . . ? C40 C35 C36 C37 -0.1(4) . . . . ? C34 C35 C36 C37 179.1(2) . . . . ? C35 C36 C37 C38 -0.5(4) . . . . ? C36 C37 C38 C39 0.8(5) . . . . ? C37 C38 C39 C40 -0.5(5) . . . . ? C36 C35 C40 C39 0.5(4) . . . . ? C34 C35 C40 C39 -178.8(3) . . . . ? C38 C39 C40 C35 -0.2(5) . . . . ? C1S O1S C1S C2S 20.5(5) 2_655 . . . ? O1S C1S C2S C2S -57.5(10) . . . 2_655 ? C4S' O1S' C1S' C2S' 48(2) . . . . ? O1S' C1S' C2S' C3S' -48(2) . . . . ? C1S' C2S' C3S' C4S' 27(2) . . . . ? C1S' O1S' C4S' C3S' -31(3) . . . . ? C2S' C3S' C4S' O1S' 1(2) . . . . ? _refine_diff_density_max 1.038 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.074 _shelx_res_file ; TITL ICIQ 223a-21 CSD0796rLT 20211013 in C2/c CSD0796rLT.res created by SHELXL-2018/3 at 12:51:17 on 15-Dec-2021 REM C2/c (#15 in standard setting) CELL 0.71073 44.547151 11.919296 12.542655 90.0000 96.7798 90.0000 ZERR 8.00 0.001497 0.000482 0.000368 0.0000 0.0027 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O NI UNIT 336 272 16 36 8 TEMP -173.120 SIZE 0.09 0.06 0.01 L.S. 15 ACTA CONF BOND $H LIST 4 OMIT -22 8 9 OMIT -6 0 2 OMIT 0 0 2 OMIT -8 0 2 OMIT -1 1 1 FMAP 2 PLAN 20 WGHT 0.053400 14.122400 FVAR 0.07749 C1 1 0.592645 0.872645 0.348635 11.00000 0.01714 0.01593 = 0.01794 -0.00381 -0.00092 -0.00231 N1 3 0.609885 0.818279 0.285411 11.00000 0.01534 0.01403 = 0.01423 -0.00054 -0.00118 0.00023 SIMU 0.0005 O1 C27 ISOR 0.001 C27 ISOR 0.0005 O1 O1 4 0.642828 0.992096 0.133543 11.00000 0.01618 0.01474 = 0.01874 -0.00123 0.00002 0.00012 NI1 5 0.615102 0.845778 0.126786 11.00000 0.01612 0.01332 = 0.01314 0.00103 -0.00137 0.00032 C2 1 0.576526 0.976981 0.308383 11.00000 0.02575 0.01653 = 0.01810 -0.00058 0.00141 0.00415 AFIX 137 H2B 2 0.555195 0.959774 0.286108 11.00000 -1.50000 H2C 2 0.585759 1.006326 0.246933 11.00000 -1.50000 H2F 2 0.578051 1.033292 0.365700 11.00000 -1.50000 AFIX 0 N2 3 0.649551 0.726773 0.162894 11.00000 0.01675 0.01248 = 0.01345 -0.00043 -0.00090 -0.00244 O2 4 0.628120 0.910207 -0.018061 11.00000 0.02568 0.02161 = 0.02148 0.00011 -0.00147 -0.00268 C3 1 0.589438 0.833036 0.452395 11.00000 0.01739 0.01963 = 0.01651 -0.00472 0.00164 0.00057 AFIX 43 H3 2 0.577131 0.873727 0.495790 11.00000 -1.20000 AFIX 0 O3 4 0.571387 0.906074 0.071714 11.00000 0.01814 0.01883 = 0.01955 -0.00097 -0.00214 -0.00039 C4 1 0.603612 0.737261 0.492476 11.00000 0.01884 0.01789 = 0.01371 -0.00217 0.00029 -0.00169 O4 4 0.583608 0.728294 0.062665 11.00000 0.01848 0.01879 = 0.01961 -0.00051 -0.00100 -0.00112 C5 1 0.623490 0.682695 0.427838 11.00000 0.01644 0.01577 = 0.01495 0.00015 0.00033 -0.00194 C6 1 0.642330 0.590808 0.466001 11.00000 0.02285 0.02153 = 0.01540 0.00373 0.00192 0.00220 AFIX 43 H6 2 0.640581 0.560091 0.534885 11.00000 -1.20000 AFIX 0 C7 1 0.662539 0.547035 0.405833 11.00000 0.02251 0.01957 = 0.02040 0.00731 0.00102 0.00533 AFIX 43 H7 2 0.674770 0.485725 0.432898 11.00000 -1.20000 AFIX 0 C8 1 0.665902 0.590951 0.302456 11.00000 0.01696 0.01750 = 0.01666 0.00095 0.00019 -0.00094 C9 1 0.687977 0.549877 0.240065 11.00000 0.01712 0.01837 = 0.01905 -0.00030 0.00121 0.00063 C10 1 0.689634 0.597676 0.141907 11.00000 0.01746 0.01703 = 0.01706 -0.00277 0.00257 -0.00176 AFIX 43 H10 2 0.704125 0.570739 0.098289 11.00000 -1.20000 AFIX 0 C11 1 0.670319 0.685864 0.104298 11.00000 0.01707 0.01437 = 0.01486 -0.00274 -0.00051 -0.00368 C12 1 0.673957 0.737636 -0.002014 11.00000 0.03021 0.01822 = 0.01882 0.00164 0.00600 0.00074 AFIX 137 H12G 2 0.689512 0.696881 -0.035428 11.00000 -1.50000 H12H 2 0.680020 0.816284 0.008377 11.00000 -1.50000 H12I 2 0.654722 0.733672 -0.048662 11.00000 -1.50000 AFIX 0 C13 1 0.647374 0.679449 0.260895 11.00000 0.01554 0.01445 = 0.01412 -0.00091 -0.00030 -0.00252 C14 1 0.625907 0.727280 0.325642 11.00000 0.01501 0.01458 = 0.01570 -0.00029 -0.00229 -0.00145 C15 1 0.599281 0.692404 0.600135 11.00000 0.01659 0.01934 = 0.01619 0.00052 0.00134 0.00316 C16 1 0.604944 0.760618 0.690372 11.00000 0.02291 0.01992 = 0.01867 -0.00005 0.00147 0.00113 AFIX 43 H16 2 0.611680 0.835533 0.682989 11.00000 -1.20000 AFIX 0 C17 1 0.600776 0.719480 0.791046 11.00000 0.02405 0.03061 = 0.01559 -0.00202 -0.00076 0.00654 AFIX 43 H17 2 0.604498 0.766500 0.852338 11.00000 -1.20000 AFIX 0 C18 1 0.591207 0.610094 0.802420 11.00000 0.02424 0.03455 = 0.01837 0.01089 0.00445 0.00821 AFIX 43 H18 2 0.588368 0.582273 0.871498 11.00000 -1.20000 AFIX 0 C19 1 0.585765 0.541160 0.713478 11.00000 0.02961 0.02429 = 0.02824 0.00495 0.00928 0.00023 AFIX 43 H19 2 0.579285 0.466011 0.721461 11.00000 -1.20000 AFIX 0 C20 1 0.589793 0.582035 0.612752 11.00000 0.02523 0.02247 = 0.02040 -0.00324 0.00570 -0.00353 AFIX 43 H20 2 0.586070 0.534593 0.551763 11.00000 -1.20000 AFIX 0 C21 1 0.709431 0.460470 0.282317 11.00000 0.02405 0.03114 = 0.02373 0.00849 0.01027 0.01067 C22 1 0.732974 0.487185 0.363664 11.00000 0.02695 0.03494 = 0.04615 0.00716 -0.00434 0.00265 AFIX 43 H22 2 0.735045 0.561887 0.389909 11.00000 -1.20000 AFIX 0 C23 1 0.752960 0.405985 0.405320 11.00000 0.02865 0.04720 = 0.04469 0.00718 -0.00155 0.00534 AFIX 43 H23 2 0.768767 0.423751 0.460359 11.00000 -1.20000 AFIX 0 C24 1 0.749607 0.299072 0.365856 11.00000 0.03245 0.04476 = 0.03458 0.00624 0.01106 0.01618 AFIX 43 H24 2 0.763567 0.243278 0.394105 11.00000 -1.20000 AFIX 0 C25 1 0.727185 0.269261 0.288045 11.00000 0.05306 0.03645 = 0.03130 -0.00654 0.01290 0.01530 AFIX 43 H25 2 0.725285 0.194086 0.262993 11.00000 -1.20000 AFIX 0 C26 1 0.706634 0.353647 0.245106 11.00000 0.04583 0.03457 = 0.02259 -0.00004 0.00009 0.01114 AFIX 43 H26 2 0.690880 0.335124 0.190129 11.00000 -1.20000 AFIX 0 C27 1 0.644052 0.982593 0.037586 11.00000 0.01714 0.01580 = 0.02045 -0.00002 -0.00006 0.00057 C28 1 0.666400 1.050498 -0.015071 11.00000 0.02280 0.01701 = 0.02447 0.00246 -0.00080 0.00241 C29 1 0.683749 1.132099 0.043143 11.00000 0.03164 0.02538 = 0.02473 -0.00295 0.00358 -0.00276 AFIX 43 H29 2 0.680507 1.147953 0.115126 11.00000 -1.20000 AFIX 0 C30 1 0.705724 1.190126 -0.003892 11.00000 0.02874 0.02564 = 0.03517 -0.00172 0.00202 -0.00772 AFIX 43 H30 2 0.717465 1.245846 0.035935 11.00000 -1.20000 AFIX 0 C31 1 0.710605 1.167422 -0.107890 11.00000 0.02620 0.03368 = 0.03355 0.00669 0.00484 -0.00280 AFIX 43 H31 2 0.725810 1.206923 -0.139619 11.00000 -1.20000 AFIX 0 C32 1 0.693351 1.086980 -0.166323 11.00000 0.02977 0.03316 = 0.02152 0.00192 0.00240 0.00330 AFIX 43 H32 2 0.696766 1.071535 -0.238215 11.00000 -1.20000 AFIX 0 C33 1 0.671259 1.029094 -0.121100 11.00000 0.02786 0.02214 = 0.02310 0.00397 -0.00234 -0.00003 AFIX 43 H33 2 0.659340 0.974646 -0.162050 11.00000 -1.20000 AFIX 0 C34 1 0.564636 0.807013 0.042073 11.00000 0.02006 0.02168 = 0.01320 0.00275 0.00134 0.00002 C35 1 0.534339 0.783115 -0.018767 11.00000 0.01677 0.03243 = 0.01678 -0.00214 0.00218 -0.00476 C36 1 0.515238 0.871180 -0.052161 11.00000 0.02118 0.03952 = 0.02622 0.00605 -0.00155 -0.00297 AFIX 43 H36 2 0.521316 0.946160 -0.035465 11.00000 -1.20000 AFIX 0 C37 1 0.487231 0.850432 -0.109957 11.00000 0.02098 0.06377 = 0.02980 0.01088 -0.00237 -0.00240 AFIX 43 H37 2 0.474092 0.910936 -0.132306 11.00000 -1.20000 AFIX 0 C38 1 0.478591 0.741208 -0.134762 11.00000 0.01961 0.07879 = 0.02976 -0.01126 -0.00034 -0.01322 AFIX 43 H38 2 0.459563 0.726742 -0.175061 11.00000 -1.20000 AFIX 0 C39 1 0.497385 0.653581 -0.101414 11.00000 0.02780 0.05675 = 0.05287 -0.02492 0.00387 -0.01633 AFIX 43 H39 2 0.491219 0.578738 -0.118330 11.00000 -1.20000 AFIX 0 C40 1 0.525449 0.673655 -0.042912 11.00000 0.02537 0.03736 = 0.04047 -0.01231 0.00346 -0.00631 AFIX 43 H40 2 0.538385 0.612831 -0.019760 11.00000 -1.20000 AFIX 0 SIMU 0.01 O1S > C4S' DELU 0.01 O1S > C4S' ISOR 0.01 O1S > C4S' DFIX 1.43 0.01 O1S C1S DFIX 1.54 0.01 C1S C2S DFIX -2.1 0.02 O1S C2S PART 1 O1S 4 0.500000 0.783354 0.250000 10.25000 0.07706 0.08323 = 0.08681 0.00000 0.01241 0.00000 C1S 1 0.524633 0.703306 0.291681 10.50000 0.04124 0.07958 = 0.07668 -0.01132 0.00569 -0.01784 AFIX 23 H1SA 2 0.525374 0.692239 0.370175 10.50000 -1.20000 H1SB 2 0.544649 0.728940 0.274517 10.50000 -1.20000 AFIX 0 C2S 1 0.514312 0.596394 0.229346 10.50000 0.04313 0.05027 = 0.07930 -0.00836 0.00635 0.00013 AFIX 23 H2SA 2 0.512589 0.606150 0.150475 10.50000 -1.20000 H2SB 2 0.526847 0.529976 0.251685 10.50000 -1.20000 AFIX 0 DFIX 1.43 0.01 O1S' C1S' DFIX 1.54 0.01 C1S' C2S' DFIX 1.54 0.01 C2S' C3S' DFIX 1.54 0.01 C3S' C4S' DFIX 1.43 0.01 C4S' O1S' DFIX -2.1 0.02 O1S' C2S' PART -2 O1S' 4 0.515372 0.612011 0.305140 10.25000 0.05900 0.06899 = 0.07893 0.00599 0.01433 0.00356 C1S' 1 0.532159 0.698454 0.265699 10.25000 0.05317 0.07672 = 0.07832 -0.01005 0.00797 -0.00820 AFIX 23 H1SC 2 0.535891 0.683849 0.190685 10.25000 -1.20000 H1SD 2 0.551750 0.708954 0.310747 10.25000 -1.20000 AFIX 0 C2S' 1 0.511355 0.800510 0.272759 10.25000 0.06034 0.07507 = 0.07919 -0.01243 0.00221 -0.02281 AFIX 23 H2SX 2 0.518241 0.865305 0.232647 10.25000 -1.20000 H2SY 2 0.510361 0.822812 0.348294 10.25000 -1.20000 AFIX 0 C3S' 1 0.479838 0.755193 0.218958 10.25000 0.05478 0.06144 = 0.06954 -0.00375 -0.00428 -0.01704 AFIX 23 H3SA 2 0.462697 0.785846 0.253327 10.25000 -1.20000 H3SB 2 0.476664 0.769568 0.140697 10.25000 -1.20000 AFIX 0 C4S' 1 0.485625 0.628554 0.245581 10.25000 0.05992 0.06767 = 0.07907 -0.00349 0.01065 -0.01154 AFIX 23 H4SA 2 0.469939 0.600598 0.288639 10.25000 -1.20000 H4SB 2 0.484138 0.584873 0.178029 10.25000 -1.20000 PART 0 REM O1S' 4 0.485866 0.604487 0.229057 0.22868 10.03000 REM C1S' 1 0.490945 0.793832 0.231365 0.18536 10.03000 REM C2S' 1 0.527598 0.686864 0.284544 0.39912 10.03000 REM C3S' 1 0.481149 0.629027 0.178195 0.21857 10.03000 REM C4S' 1 0.485273 0.600082 0.279027 0.39239 10.03000 REM PART 0 REM O1S 4 0.500000 0.789443 0.250000 10.50000 0.37583 0.12015 = REM 0.17247 0.00000 0.17346 0.00000 REM C1S 1 0.514147 0.606663 0.255294 11.00000 0.03969 0.05367 = REM 0.30453 0.03738 0.01250 0.00174 REM AFIX 23 REM H1SA 2 0.521162 0.585056 0.186149 11.00000 -1.20000 REM H1SB 2 0.521607 0.549511 0.309295 11.00000 -1.20000 REM AFIX 0 REM C2S 1 0.525790 0.703761 0.285001 11.00000 0.06124 0.19369 = REM 0.11121 -0.03739 -0.01359 -0.03407 REM AFIX 23 REM H2SA 2 0.543882 0.719728 0.248675 11.00000 -1.20000 REM H2SB 2 0.531535 0.706101 0.363663 11.00000 -1.20000 REM part 1 REM C1S 1 0.472794 0.292706 -0.276165 21.00000 0.06064 REM O1S 4 0.484690 0.390635 -0.286007 21.00000 0.12200 REM C2S 1 0.500000 0.201735 -0.250000 20.50000 0.04730 REM PART 2 REM C1S' 1 0.527940 0.317907 -0.182801 -21.00000 0.17477 REM C2S' 1 0.516213 0.230249 -0.220940 -21.00000 0.07495 REM C3S' 1 0.514719 0.400044 -0.277769 -21.00000 0.04772 REM PART 0 REM AFIX 0 REM AFIX 0 ! chuebsch want to keep this here!! REM ##### AFIX 0 HKLF 4 REM ICIQ 223a-21 CSD0796rLT 20211013 in C2/c REM wR2 = 0.116191, GooF = S = 1.02592, Restrained GooF = 1.03888 for all data REM R1 = 0.044978 for 5375 Fo > 4sig(Fo) and 0.076184 for all 7433 data REM 494 parameters refined using 194 restraints END WGHT 0.0534 14.1226 REM Highest difference peak 1.038, deepest hole -0.659, 1-sigma level 0.074 Q1 1 0.6464 1.0070 0.0970 11.00000 0.05 1.04 Q2 1 0.6374 0.9947 0.1609 11.00000 0.05 0.74 Q3 1 0.6863 0.3285 0.2338 11.00000 0.05 0.74 Q4 1 0.7043 0.2205 0.2646 11.00000 0.05 0.69 Q5 1 0.7310 0.4227 0.3088 11.00000 0.05 0.59 Q6 1 0.6991 0.4177 0.2480 11.00000 0.05 0.43 Q7 1 0.5494 0.7952 0.0199 11.00000 0.05 0.42 Q8 1 0.7386 0.2317 0.3369 11.00000 0.05 0.41 Q9 1 0.5310 0.6568 0.3590 11.00000 0.05 0.40 Q10 1 0.7422 1.0464 -0.0679 11.00000 0.05 0.37 Q11 1 0.5265 0.6573 0.3237 11.00000 0.05 0.37 Q12 1 0.7508 0.3621 0.3299 11.00000 0.05 0.34 Q13 1 0.6406 0.7190 0.2990 11.00000 0.05 0.34 Q14 1 0.6794 0.5784 0.2822 11.00000 0.05 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7 146.388 4.33770 1 -1 5 7 138.625 4.36085 1 -1 -5 7 134.283 4.12384 3 -1 -5 6 0.22365 0.56209 3 -1 -5 6-1.03424 1.41873 2 -1 5 6 0.54546 0.92457 1 1 -5 -6-0.57271 0.45664 2 1 5 -6-1.69411 1.17082 2 -1 5 6 0.17317 0.94295 1 -1 5 6 0.30042 0.77178 2 1 5 -6 0.02398 0.56611 3 -1 -5 5 3.13364 0.49123 3 1 -5 -5 2.71061 0.39652 2 -1 5 5 3.56627 0.67889 2 1 5 -5 3.93923 0.63005 3 -1 -5 5 3.08863 1.24616 2 -1 -5 4 7.64229 1.23750 2 1 5 -4 7.56940 0.65370 3 1 5 -4 6.55489 1.09657 2 -1 -5 4 7.84202 0.50872 3 1 -5 -4 7.86861 0.47147 2 -1 5 4 6.24486 0.88947 1 -1 5 4 6.45454 0.89537 1 -1 5 4 8.83416 0.63877 2 -1 5 3 33.4760 1.28980 1 1 5 -3 27.5191 0.91125 1 1 5 -3 31.6469 1.08996 3 1 5 -3 30.1359 0.94870 1 -1 5 3 29.9346 1.02362 2 -1 -5 3 33.8823 1.49447 2 -1 5 3 31.8398 1.28637 1 1 5 -3 31.5514 1.50952 2 -1 5 2 7.83466 0.44886 2 1 5 -2 8.88897 0.99607 2 -1 -5 2 8.41418 0.97169 2 1 5 -2 8.65701 0.55728 1 1 5 -2 9.35386 0.64647 3 -1 5 2 8.75502 0.79172 1 -1 5 2 7.25962 0.80410 1 1 5 -2 8.29485 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224.232 6.59893 2 -1 5 -5 231.570 6.83763 2 1 -5 6 65.0385 2.42460 2 1 5 6 55.3112 2.10853 1 -1 5 -6 56.7052 1.79219 3 1 5 6 55.9458 1.98319 2 1 -5 6 57.5781 1.78533 3 -1 5 -6 60.4483 2.30077 2 -1 -5 -6 57.2119 1.84178 2 1 5 6 65.4474 2.11729 1 1 5 7 5.36583 1.01831 1 1 5 7 3.95302 0.99496 1 -1 -5 -7 4.41512 0.54551 2 1 -5 7 4.28822 0.56472 3 -1 5 -7 5.88153 1.20769 2 -1 5 -8 4.06804 1.26165 2 1 5 8 3.30798 1.07174 1 1 -5 8 2.41978 0.67658 3 -1 -5 -8 3.66382 0.60069 2 1 5 8 2.76050 1.09719 1 -1 5 -9 71.7210 2.85413 2 1 5 9 73.6743 2.75220 1 1 5 9 76.9732 2.71578 1 -1 -5 -9 75.1346 2.42845 2 1 5 10 4.86200 1.27273 1 -1 5 -10 5.80691 1.48017 2 -1 -5 -10 5.16176 0.78527 2 1 5 11 25.4392 1.74303 1 -1 5 -11 19.8758 1.85631 2 -1 -5 -11 24.3941 1.21616 2 -1 5 -12 6.63367 1.63988 2 -1 -5 -12 3.69315 0.92920 2 1 5 12 5.22463 1.60047 1 -1 -5 -13 107.370 3.50920 2 -1 5 -13 104.214 3.94511 2 1 5 13 109.832 3.94999 1 -1 5 -14 4.69587 1.74279 2 1 7 -14 0.58352 2.04543 2 1 -7 -14 3.15431 1.02809 2 1 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30.1190 1.63336 2 -1 -7 3 31.2057 1.49455 2 1 7 -3 32.6927 1.06048 1 1 7 -3 31.1362 1.13492 1 -1 7 2 36.1621 1.51023 1 1 7 -2 36.6914 1.28928 1 1 7 -2 38.0896 1.35932 1 1 7 -2 35.7528 1.36965 3 -1 7 2 38.3377 1.45022 1 -1 7 2 40.0934 1.24419 2 1 7 -2 39.7454 1.72397 2 -1 7 1 71.6195 2.38013 1 -1 7 1 72.2248 2.33545 1 1 7 -1 72.2495 2.32499 3 1 7 -1 73.9238 2.32681 1 1 7 -1 73.5156 2.28533 1 1 7 -1 72.1967 2.52231 2 1 7 0 315.940 9.22078 1 -1 7 0 313.181 9.26073 1 -1 7 0 320.863 9.32864 2 -1 7 0 314.872 9.22208 1 1 7 0 311.342 9.33468 2 1 7 0 321.559 9.25422 1 -1 7 -1 5.60571 0.88469 2 1 7 1 4.97038 0.63866 1 -1 7 -1 4.88086 0.72162 1 1 7 1 5.14828 0.61101 1 -1 7 -1 4.97148 0.62089 1 1 7 2 106.136 3.38281 1 1 7 2 104.884 3.34720 1 -1 7 -2 104.898 3.51364 2 -1 7 -2 112.109 3.28220 1 1 7 2 110.183 3.20367 2 -1 7 -2 104.240 3.27416 3 -1 7 -2 106.224 3.21578 1 1 -7 3 5.39466 1.02118 2 -1 7 -3 6.21769 0.48948 1 1 7 3 6.25304 0.89331 1 1 7 3 6.20050 0.51602 2 1 7 3 5.76924 0.86400 1 -1 7 -3 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1.91163 2 -1 9 -11 2.01279 2.00913 2 -1 9 -12-0.87049 2.07067 2 -1 9 -13 2.45683 2.14451 2 1 11 -11 3.62663 2.36146 2 1 11 -10-0.28941 2.27508 2 1 11 -8 1.78887 2.13584 2 -1 11 7 25.1776 1.94986 1 1 11 -7 20.0360 2.38276 2 1 11 -6 2.65043 2.02138 2 -1 11 6 3.30142 1.50537 1 1 11 -5-1.43956 1.96108 2 -1 11 5-1.79932 1.53299 1 1 11 -4 18.0557 2.05017 2 -1 11 4 19.8583 1.69749 1 1 11 -3 16.4689 1.23511 3 1 11 -3 17.4973 1.95781 2 -1 11 3 18.5331 1.55595 1 -1 11 2 0.74094 0.89017 1 1 11 -2 0.83063 0.97781 3 -1 11 2-0.66400 1.15150 1 -1 11 2 0.71443 1.12090 2 1 11 -2 0.53865 1.55295 2 1 11 -2 1.46268 1.07750 1 1 11 -1 0.11132 0.96774 3 -1 11 1 2.27808 1.12487 2 1 11 -1 0.61993 0.88152 1 -1 11 1 0.95720 0.92354 1 -1 11 1 0.69033 1.09318 1 1 11 -1-0.35420 1.43367 2 1 11 -1 0.91254 1.12438 1 -1 11 0-1.56586 1.19218 1 -1 11 0-0.04576 1.21739 2 1 11 0 0.09389 1.12784 1 -1 11 0 0.34914 0.88428 3 1 11 0 0.04647 1.25249 2 1 11 0 0.88515 0.92969 1 -1 11 0 0.79175 0.92228 1 1 11 0-0.19981 0.89251 3 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170.082 4.84683 3 -2 2 1 168.358 4.81300 2 -2 -2 1 174.454 4.91736 2 2 2 -1 170.819 4.85193 3 -2 -2 1 160.043 4.81148 1 2 2 0 309.884 9.05394 1 -2 2 0 326.663 9.06377 2 -2 -2 0 313.930 9.05349 1 -2 2 0 308.658 9.06709 1 2 -2 0 315.600 9.06448 1 2 -2 1 145.809 4.32297 1 -2 -2 -1 150.388 4.36007 1 -2 2 -1 142.902 4.40579 2 2 -2 1 148.172 4.40121 2 -2 2 -1 155.852 4.32539 1 2 -2 2 42.6344 1.54203 2 -2 -2 -2 40.1863 1.23248 2 -2 2 -2 38.4307 1.46779 2 -2 2 -3 29.8093 1.24945 2 2 2 3 29.4000 1.15200 1 2 -2 3 32.4472 0.97312 3 -2 2 -3 26.9107 0.90010 1 -2 2 -3 30.7009 0.93599 3 -2 -2 -3 30.3544 0.98560 2 2 -2 3 29.8698 1.42348 2 -2 2 -4 11.2792 0.92445 2 -2 -2 -4 14.6441 0.64248 2 2 2 4 14.5254 0.85489 1 2 -2 4 13.2080 0.55155 1 -2 -2 -4 11.5863 0.82151 1 2 -2 4 14.1719 0.70493 3 -2 2 -4 13.3329 0.53091 1 2 -2 4 14.7528 1.20420 2 -2 -2 -5 128.232 3.87317 1 2 -2 5 129.889 3.80407 3 2 -2 5 130.719 3.73087 1 -2 2 -5 126.353 3.73136 1 -2 -2 -5 125.810 3.80384 2 -2 2 -5 129.955 3.93671 2 2 -2 5 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3.99198 0.34301 1 -2 4 8 4.56672 0.98279 1 2 4 -8 5.77198 1.23785 2 -2 -4 8 4.71565 0.93918 3 2 -4 -8 5.00829 0.63458 2 -2 4 8 5.14554 1.03719 1 -2 4 7 42.8593 1.74950 1 2 -4 -7 42.8519 1.49560 2 2 4 -7 41.9087 1.92385 2 -2 4 7 44.8804 1.74416 1 2 4 -7 43.8367 1.52033 3 -2 -4 7 44.1519 1.59534 3 -2 4 7 42.3875 1.71462 2 2 4 -6 144.342 4.54978 2 2 -4 -6 140.430 4.24375 2 -2 -4 6 142.112 4.27312 3 -2 4 6 139.234 4.34495 2 2 4 -6 143.747 4.26095 3 -2 4 6 150.183 4.40422 1 -2 -4 6 143.695 4.60915 2 -2 4 6 141.140 4.41611 1 -2 -4 5 64.3175 2.28895 2 -2 -4 5 51.1346 1.65908 3 -2 4 5 47.6067 1.70756 2 2 -4 -5 48.3643 1.58395 2 -2 4 5 54.1044 1.82520 1 2 4 -5 48.8313 2.01305 2 -2 4 5 45.3042 1.81266 1 2 4 -5 49.7392 1.66356 3 -2 -4 4 12.7315 1.33095 2 2 4 -4 12.1951 0.75441 3 2 4 -4 13.3003 1.11339 2 -2 4 4 12.1441 0.72211 2 2 -4 -4 12.6631 0.56265 2 -2 -4 4 13.8543 0.71682 3 -2 4 3 95.2691 2.85518 2 2 4 -3 94.5975 3.12327 2 -2 -4 3 97.4875 2.86317 3 2 -4 -3 96.9897 2.82648 2 -2 -4 3 103.906 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1.83229 2 -21 7 5 15.1248 1.58493 1 -21 -7 5 12.3385 0.83785 1 21 7 -5 13.5910 1.07212 1 -21 7 4 11.0420 0.71000 2 21 -7 -4 12.4963 1.34199 1 21 7 -4 13.7960 1.47367 3 -21 7 4 12.8838 1.52386 1 21 7 -4 12.2052 1.05958 1 21 7 -4 12.6375 1.61970 2 -21 -7 4 13.0088 0.87212 1 -21 7 3 78.3851 2.86239 1 21 7 -3 73.8314 2.84620 3 21 7 -3 80.3719 2.55864 1 -21 7 3 75.3741 2.31872 2 21 7 -3 83.3424 3.03031 2 -21 -7 3 76.9162 2.47476 1 21 -7 -3 76.1615 2.76543 1 -21 7 3 72.8278 2.28737 2 -21 7 2 25.0230 0.84885 2 21 -7 -2 28.2377 1.55537 1 21 7 -2 31.2572 1.64001 3 21 7 -2 28.5351 1.33021 1 -21 7 2 28.5144 1.65349 3 21 7 -2 26.6996 1.69184 2 -21 7 2 24.4867 0.93769 2 -21 -7 2 27.3724 1.20376 1 -21 7 2 27.3371 1.66296 1 -21 7 1 42.1967 1.32943 2 21 7 -1 48.8233 1.77119 1 21 7 -1 51.2235 2.04074 3 -21 7 1 50.5733 1.98732 3 -21 -7 1 49.2608 1.70309 1 21 7 -1 48.5965 2.05691 2 -21 7 1 53.5760 2.00701 1 21 -7 -1 50.3343 1.94022 1 -21 7 0 2.61040 1.17010 1 21 7 0-0.63644 1.10099 3 -21 7 0 1.44463 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27.2376 1.69585 3 -21 -7 -6 29.8143 1.63224 1 -21 7 -7 19.0637 1.27206 2 21 7 7 20.9108 1.60757 3 21 7 8 7.57391 1.45571 3 -21 7 -8 7.26343 1.17598 2 21 7 9 8.29394 1.52184 3 -21 7 -9 4.55104 1.20838 2 -21 7 -10 10.9223 1.36266 2 -21 7 -11 16.7107 1.57191 2 -21 7 -12 5.03648 1.47079 2 -21 9 8 41.3173 2.52285 1 21 9 -8 42.4108 2.38823 3 21 9 -7-0.59230 1.74458 3 -21 9 7 0.10865 1.76801 1 21 9 -6 13.6456 1.76895 3 -21 9 6 12.6179 1.85018 1 21 9 -5 9.54952 1.64404 3 -21 9 5 7.94783 1.72707 1 21 9 -4 2.42250 1.52987 3 -21 9 4 1.64729 1.57713 1 -21 -9 4 2.06027 0.85786 1 21 9 -3-0.74793 1.46988 3 21 9 -3 0.61179 1.04701 1 -21 9 3 1.07426 1.56805 1 -21 -9 3 0.32106 0.88904 1 21 9 -2 25.6418 1.39194 1 21 9 -2 24.0543 1.76502 3 -21 9 2 25.4672 1.84028 1 -21 -9 2 26.5952 1.33085 1 21 -9 -2 24.3238 1.62004 1 21 9 -1 9.37823 1.49655 3 21 9 -1 10.7377 1.17140 1 21 -9 -1 9.56858 1.35552 1 -21 9 1 9.10112 1.58076 1 -21 -9 1 8.10568 1.04762 1 21 9 0 30.5533 1.55606 1 21 -9 0 30.3131 1.62943 1 21 9 0 27.9348 1.85407 3 -21 -9 0 29.7086 1.45876 1 -21 9 0 27.8326 1.77884 1 -21 9 -1 0.23533 1.29796 1 21 9 1 0.83652 1.41299 3 -21 -9 -1 1.34349 1.03545 1 21 9 1 0.72374 1.14645 1 21 -9 1 0.87010 1.18292 1 21 9 2 2.88987 1.35757 3 -21 -9 -2 3.89438 1.17075 1 21 -9 2 2.74272 1.17005 1 -21 9 -2 2.14079 1.24271 1 -21 9 -3 7.95590 1.04578 2 21 9 3 6.15120 1.45174 3 -21 -9 -3 9.83735 1.27645 1 -21 9 -3 9.31316 1.21161 1 21 9 4 36.2588 1.98482 3 -21 9 -4 30.6254 1.59444 1 -21 -9 -4 38.2491 1.79842 1 -21 -9 -5 28.1830 1.70231 1 -21 -9 -6 6.59186 1.40018 1 21 9 7 1.90750 1.54020 3 21 9 8 54.5728 2.60960 3 21 9 9 8.08833 1.73392 3 21 9 10 1.44471 1.78849 3 21 11 -9 28.8636 3.03092 2 21 11 -8 8.72667 2.63670 2 21 11 -7 1.29818 2.49875 2 21 11 -6 2.50059 1.89907 3 21 11 -6 0.66797 2.48146 2 -21 11 5 59.9049 2.84919 1 21 11 -5 49.8772 2.74380 3 21 11 -5 63.6646 3.31283 2 -21 11 4-0.05353 1.80543 1 21 11 -4 4.43760 2.24539 2 21 11 -4 0.63807 1.76374 3 21 11 -3 8.38782 1.75329 3 -21 11 3 8.45652 1.93044 1 21 11 -3 9.49083 2.14514 2 21 11 -2 5.06660 1.70035 3 -21 11 2 3.38870 1.82116 1 21 11 -2 3.83264 1.96508 2 21 11 -1 8.88020 1.77169 3 -21 11 1 9.35798 1.82738 1 -21 -11 1 7.90064 1.26180 1 21 11 -1 6.51625 1.82194 2 21 11 0 1.28251 1.57755 3 -21 11 0 1.34490 1.63770 1 -21 -11 0 1.52173 1.24596 1 21 11 0-0.67730 1.66563 2 -21 11 -1 6.09818 1.59016 1 21 11 1 1.93008 1.59745 3 -21 -11 -1 3.97167 1.29219 1 21 11 1 2.39052 1.57822 2 21 11 2 2.15265 1.61876 3 -21 -11 -2 0.89549 1.28281 1 21 11 2 0.71031 1.51386 2 21 11 3 22.4488 1.88870 3 -21 -11 -3 21.8936 1.71155 1 21 11 4 7.32175 1.75365 3 -21 -11 -4 8.64691 1.51344 1 21 11 5 4.61463 1.73747 3 21 11 6-0.11864 1.68299 3 21 11 7 21.8228 2.05138 3 21 13 -6-6.04963 2.84608 2 21 13 -5 6.99781 2.72188 2 21 13 -4 55.2519 3.42249 2 21 13 -3 0.52577 1.97948 3 21 13 -2 0.35222 1.88775 3 -21 13 2-0.65669 2.15571 1 21 13 -2-1.24159 2.29965 2 21 13 -1 2.98707 2.14345 2 21 13 -1-0.41547 1.90400 3 21 13 0 9.40920 1.97562 3 21 13 0 8.77297 2.06831 2 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1 22 0 -6 2.15081 1.04726 1 22 0 -6 2.15449 1.07420 3 -22 0 6 1.84763 1.20644 2 22 0 -6 1.01302 0.97175 2 -22 0 5 0.84551 0.94866 1 -22 0 5-2.32893 1.39999 3 -22 0 5 0.02503 1.09979 2 22 0 -5 1.59250 0.90302 2 22 0 -5-0.15610 0.99641 1 22 0 -4 70.9248 2.48553 1 -22 0 4 72.2159 2.43297 1 -22 0 4 70.8580 2.38415 2 22 0 -4 67.3135 2.39443 2 -22 0 3 0.45953 1.23032 3 22 0 -3 1.40648 1.03561 1 22 0 -3-0.22737 1.05798 3 -22 0 3-0.39310 0.73875 2 22 0 -3 1.05834 0.84183 2 -22 0 3 0.57214 0.86431 1 -22 0 2 115.933 3.76567 3 -22 0 2 118.599 3.65094 1 22 0 -2 115.743 3.59980 2 22 0 -2 116.901 3.72584 1 22 0 -2 115.597 3.77125 3 -22 0 1 0.07228 1.06017 3 22 0 -1 0.20154 0.93445 3 -22 0 1 1.25974 0.85830 1 22 0 -1 0.04332 0.66205 2 -22 0 0 162.451 4.95909 3 22 0 0 161.909 4.69747 2 22 0 0 162.367 4.98918 3 -22 0 -1-0.78838 0.89615 3 22 0 1 0.17898 0.94122 3 22 0 1 0.05600 0.37403 2 22 0 1-1.25040 0.98956 1 -22 0 -2 50.5690 1.84158 1 -22 0 -2 55.7816 1.86430 3 22 0 2 50.7816 1.91059 3 22 0 2 51.2319 1.93822 1 22 0 2 51.8640 1.64820 2 22 0 3-0.55530 0.56635 2 22 0 3-1.13824 0.84421 3 -22 0 -3-0.18659 0.35165 2 22 0 3 0.11509 0.92312 1 -22 0 -3 0.19131 0.75326 1 22 0 4 85.7935 2.67782 2 22 0 4 86.8132 2.83462 1 22 0 4 81.5159 2.78552 3 -22 0 -4 86.1102 2.57328 2 -22 0 -4 84.4024 2.76949 1 -22 0 -5 0.70869 0.78686 1 22 0 5-0.50386 0.77854 2 22 0 5 1.78351 0.84907 3 -22 0 -5-0.28422 0.43951 2 22 0 5-0.86269 0.94922 1 22 0 6 5.29834 0.87144 3 -22 0 -6 5.52094 0.58169 2 22 0 6 5.88095 1.04352 1 -22 0 -6 5.67403 0.85493 1 22 0 7-0.20312 0.83642 3 -22 0 -7-0.09057 0.58395 2 22 0 7 0.48964 1.04037 1 -22 0 -7 0.82041 0.89621 1 22 0 8 82.8030 2.81655 1 22 0 8 83.8243 2.75267 3 -22 0 -8 77.0969 2.59299 2 -22 0 -8 80.0235 2.74771 1 22 0 9 1.48756 1.01288 3 22 0 9-0.79794 1.19054 1 -22 0 -9-1.56523 0.77940 2 -22 0 -9-0.52442 1.04510 1 22 0 10 3.06693 1.10616 3 -22 0 -10 3.20658 0.84321 2 -22 0 -10 4.94599 1.17400 1 -22 0 -11 1.64813 0.91546 2 -22 0 -11 0.42903 1.23681 1 -22 0 -12 1.45771 0.99758 2 -22 0 -12 2.48985 1.36027 1 -22 0 -13-0.33433 1.07604 2 22 2 -15 13.6269 2.05064 2 22 2 -14 2.94080 1.76671 2 22 -2 -14 0.88856 1.27155 2 22 -2 -13 25.5299 1.60598 2 22 2 -13 25.1786 2.08894 2 22 2 -13 21.6344 1.91763 3 -22 2 13 26.1314 2.11193 1 22 -2 -12 33.8511 1.73734 2 22 2 -12 31.9884 2.11339 2 22 2 -12 28.4449 2.01719 3 -22 2 12 31.3098 2.19196 1 22 2 -11 6.77746 1.66134 2 -22 -2 11 6.65244 1.32096 1 22 -2 -11 7.55659 1.18838 2 22 2 -11 6.95368 1.52021 3 -22 2 11 8.59756 1.69366 1 22 2 -10 4.46520 1.55051 2 -22 -2 10 3.12321 1.20047 1 22 -2 -10 2.84224 1.03673 2 22 2 -10 5.11407 1.43556 3 22 -2 -10 1.33794 1.36104 3 22 2 -10 4.18313 1.11053 1 -22 2 10 2.03129 1.50024 1 22 -2 -10 1.84813 1.33333 1 22 -2 -9 80.6891 2.71645 2 -22 2 9 79.3442 2.97463 1 22 2 -9 80.9807 2.70395 1 22 2 -9 77.5470 3.03086 3 22 -2 -9 77.7850 2.93795 3 -22 -2 9 76.5811 2.72422 1 22 -2 -9 76.8507 2.83587 1 22 2 -9 79.8088 3.02180 2 22 -2 -8 20.9986 1.42831 1 22 -2 -8 22.0710 1.18919 2 22 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2 4.67625 2.37999 3 53 -1 2 1.98740 2.28122 3 53 1 4 2.89567 2.44367 3 53 -3 -6 1.20839 2.32918 3 53 3 -5 4.88534 2.56930 3 53 3 -4 4.38579 2.61393 3 53 -3 -4 3.19914 2.23839 3 53 3 -3 7.96288 2.53958 3 53 -3 -3 9.03850 2.30721 3 53 3 -2 11.1943 2.60371 3 53 -3 -2 13.1186 2.34178 3 53 3 -1 1.31769 2.50046 3 53 -3 -1 2.94848 2.25353 3 53 3 0 13.2897 2.54197 3 53 -3 0 11.3197 2.32125 3 53 3 1 1.67608 2.41761 3 53 3 2 3.39700 2.42160 3 53 3 3-1.33545 2.51786 3 53 3 4 5.18175 2.46078 3 53 3 5 2.99495 2.60198 3 53 -5 -6 2.13660 2.14197 3 53 -5 -5 3.85584 2.15572 3 53 -5 -4 3.71457 2.09575 3 53 -5 -3 28.3997 2.48946 3 53 5 -1-3.48535 2.66484 3 53 5 0-5.68900 2.72317 3 54 0 -6 10.7822 2.63291 3 54 0 -5-2.75130 2.50527 3 54 0 -4 5.39806 2.45180 3 54 0 -3-3.12420 2.37170 3 54 0 -2 14.9547 2.57334 3 54 0 -1 1.44956 2.33928 3 54 0 0 12.3024 2.53580 3 54 0 1 2.07075 2.34525 3 54 0 2 49.5056 3.15885 3 54 0 3-1.51676 2.51730 3 54 -2 -6 1.20635 2.39064 3 54 2 -5 6.03546 2.68543 3 54 -2 -5 3.13088 2.44921 3 54 2 -4 3.58115 2.49218 3 54 -2 -4 0.91670 2.34638 3 54 2 -3 10.0794 2.54396 3 54 2 -2 4.87731 2.52326 3 54 -2 -2 3.94919 2.36364 3 54 2 -1 1.71229 2.42574 3 54 -2 -1 4.07889 2.40512 3 54 2 0 2.65332 2.47725 3 54 -2 0 2.10285 2.20117 3 54 2 1-1.19140 2.47480 3 54 -2 1-1.09296 2.34043 3 54 2 3 6.19396 2.45944 3 54 2 4-0.69163 2.54857 3 54 -4 -6-2.60012 2.43134 3 54 -4 -5 3.09775 2.24690 3 54 -4 -4 0.21101 2.24206 3 54 4 -3 2.48574 2.65832 3 54 -4 -3 4.95244 2.30001 3 54 4 -2 23.8682 2.87681 3 54 -4 -2 24.8751 2.54281 3 54 4 -1 0.08660 2.57983 3 54 4 0 13.2073 2.64498 3 54 4 1 13.8281 2.75813 3 54 4 2 11.3897 2.67102 3 54 -6 -5 1.84196 2.26063 3 54 -6 -4 1.76970 2.23209 3 55 1 -5 14.9143 2.79220 3 55 -1 -5 15.2992 2.63421 3 55 1 -4 9.24384 2.69405 3 55 -1 -4 5.80447 2.48887 3 55 1 -3 0.66512 2.52426 3 55 -1 -3-0.15799 2.39996 3 55 1 -2-0.90062 2.46382 3 55 -1 -2 0.15504 2.41299 3 55 1 -1-0.56390 2.51712 3 55 -1 -1 4.08380 2.40152 3 55 1 0-2.06294 2.51967 3 55 -1 0-3.82998 2.47038 3 55 1 1 5.25083 2.58961 3 55 -1 1 1.52052 2.33993 3 55 1 2 4.11274 2.52114 3 55 1 3 42.9530 3.21439 3 55 -3 -5 7.97333 2.42989 3 55 3 -3-4.93413 2.74187 3 55 -3 -3-0.36615 2.33658 3 55 3 -2 12.9370 2.78789 3 55 -3 -2 20.0538 2.55568 3 55 3 -1-0.25709 2.54502 3 55 -3 -1 3.20390 2.26714 3 55 3 0-0.33896 2.58982 3 55 3 1 5.17142 2.60989 3 55 3 2 4.79159 2.61271 3 55 3 3-4.34708 2.66553 3 55 -5 -5 26.7678 2.65291 3 55 -5 -4 3.77496 2.27753 3 56 0 -4 7.71064 2.72446 3 56 0 -3-1.41428 2.51900 3 56 0 -2 5.59572 2.56473 3 56 0 -1 0.23793 2.52730 3 56 0 0 1.48429 2.45170 3 56 0 1 1.54281 2.55046 3 56 0 2 5.24487 2.55569 3 56 -2 -5 3.73428 2.55408 3 56 -2 -4 0.94866 2.45354 3 56 2 -3-3.57748 2.71052 3 56 -2 -3-1.70566 2.43750 3 56 2 -2-2.66430 2.59569 3 56 2 -1 2.71109 2.60151 3 56 -2 -1-0.29721 2.45970 3 56 2 0 9.37022 2.70401 3 56 -2 0 9.11420 2.49763 3 56 2 1-3.06545 2.64912 3 56 2 2 7.12721 2.73585 3 56 2 3 16.4334 2.89167 3 56 -4 -4 18.5590 2.57444 3 56 -4 -3 0.64056 2.34349 3 56 -4 -2 1.04846 2.31637 3 57 -1 -4 0.41707 2.55330 3 57 -1 -3 0.32731 2.55169 3 57 1 -2 1.69854 2.65273 3 57 1 -1 2.67767 2.63748 3 57 -1 -1 2.28635 2.55682 3 57 1 0 2.56140 2.64227 3 57 1 1 33.2593 3.05534 3 57 -1 1 33.0536 2.93093 3 57 1 2 2.66398 2.62174 3 57 1 3 6.07935 2.77623 3 57 -3 -4 13.5119 2.66779 3 57 -3 -3 1.21340 2.32449 3 57 -3 -2 11.3366 2.49265 3 58 0 -2 16.1795 2.86235 3 58 0 -1-1.89176 2.66696 3 58 0 0-2.99858 2.57135 3 58 0 1-1.27892 2.63560 3 58 -2 -3 29.2649 2.96176 3 58 -2 -1 3.00499 2.47154 3 58 -4 -3-0.88267 2.46959 3 59 -1 0 2.55743 2.53611 3 59 -3 -2 10.1006 2.67514 3 0 0 0 0.00 0.00 0 TITL ICIQ 223a-21 CSD0796rLT 20211013 in C2/c REM C2/c (#15 in standard setting) CELL 0.71073 44.484681 11.904969 12.540416 90.0000 96.7799 90.0000 ZERR 8.00 0.001079 0.000335 0.000320 0.0000 0.0022 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N O Ni UNIT 320.00 240.00 16.00 32.00 8.00 TREF HKLF 4 END ; _shelx_hkl_checksum 87736