# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/172 data_global #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author ; Paul H Walton Department of Chemistry University of York Heslington YORK YO10 5DD UK ; _publ_contact_author_email phw2@york.ac.uk _publ_contact_author_fax '44 1904 432516' _publ_contact_author_phone '44 1904 432580' # TITLE AND AUTHOR LIST _publ_section_title ; Syntheses and Structures of a Range of Metal Complexes with the Ligand cis,cis-1,3,5-(E,E)-tri(phenylpropenylideneamino)cyclohexane ; loop_ _publ_author_name _publ_author_address 'Greener, Bryan' ; Department of Chemistry University of York Heslington YORK YO10 5DD UK ; 'Foxon, Simon P' ; Department of Chemistry University of York Heslington YORK YO10 5DD UK ; 'Walton, Paul H' ; Department of Chemistry University of York Heslington YORK YO10 5DD UK ; _publ_requested_journal 'New Journal of Chemistry' #------------------------------------------------------------------------------- data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis,cis-1,3,5-(E,E)-tri(phenyl-propenylideneamino)cyclohexane copper sulfate, (1) {tri(phenyl-propenylideneamino)cyclohexane = (Ph-protach)} ; _chemical_name_common '[Cu(Ph-protach)(SO4)(0.5CH3OH)], (1)' _chemical_melting_point '549-549.5 K' _chemical_formula_moiety 'C33 H33 Cu N3 2+, O4 S 2-, C1.5 H6 O1.5' _chemical_formula_sum 'C34.50 H39 Cu N3 O5.5 S' _chemical_formula_weight 679.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.056(5) _cell_length_b 17.494(3) _cell_length_c 14.397(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.49(2) _cell_angle_gamma 90.00 _cell_volume 3337.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.7 _exptl_crystal_size_min 0.6 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.6170 _exptl_absorpt_correction_T_max 0.6573 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; Crystal mounted in a Lindemann tube with mother liquor ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_source_current 30 _diffrn_source_voltage 50 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -2 5 -1 -6 -2 -1 -6 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.045 _diffrn_reflns_number 6114 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5644 _reflns_number_gt 3642 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'AFC/MSC (Diffractometer Control)' _computing_cell_refinement 'AFC/MSC (Diffractometer Control)' _computing_data_reduction 'teXsan (Molecular Structure Corporation, 1992)' _computing_structure_solution 'SAPI91 (Rigaku Corporation, 1993)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics teXsan _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+3.4458P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5644 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1487 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.69259(4) 0.38745(3) 0.71113(4) 0.05234(19) Uani 1 1 d . . . S1 S 0.57076(10) 0.26144(9) 0.62493(9) 0.0740(4) Uani 1 1 d . . . O1 O 0.9057(7) 0.3995(4) 0.1366(7) 0.200(3) Uani 1 1 d . . . H1 H 0.9629 0.3816 0.1532 0.300 Uiso 1 1 calc R . . O4 O 0.6764(2) 0.2796(2) 0.6678(2) 0.0734(10) Uani 1 1 d . A . O5 O 0.5231(3) 0.2425(3) 0.6954(3) 0.1002(14) Uani 1 1 d . A . O2 O 0.5545(4) 0.3565(4) 0.6247(4) 0.0547(15) Uani 0.50 1 d P A 1 O3 O 0.5399(6) 0.2390(5) 0.5309(5) 0.074(2) Uani 0.50 1 d P A 1 O6 O 0.5048(5) 0.2941(5) 0.5364(5) 0.0641(18) Uani 0.50 1 d P A 2 O7 O 0.5836(7) 0.1745(5) 0.5884(7) 0.116(3) Uani 0.50 1 d P A 2 O8 O 0.5503(5) 0.4243(4) 0.6121(5) 0.0609(16) Uani 0.50 1 d P A 2 H8 H 0.4974 0.3904 0.6055 0.073 Uiso 0.50 1 calc PR A 2 C35 C 0.5214(9) 0.4945(6) 0.5524(8) 0.085(3) Uani 0.50 1 d P A 2 H35A H 0.4505 0.4931 0.5157 0.128 Uiso 0.50 1 calc PR A 2 H35B H 0.5588 0.4977 0.5077 0.128 Uiso 0.50 1 calc PR A 2 H35C H 0.5360 0.5383 0.5950 0.128 Uiso 0.50 1 calc PR A 2 N1 N 0.7688(3) 0.4364(2) 0.6161(2) 0.0514(9) Uani 1 1 d . A . N2 N 0.6848(3) 0.4846(2) 0.7807(3) 0.0541(9) Uani 1 1 d . A . N3 N 0.8175(2) 0.3679(2) 0.8263(3) 0.0471(9) Uani 1 1 d . A . C1 C 0.8488(3) 0.4894(3) 0.6733(3) 0.0540(11) Uani 1 1 d . . . H1A H 0.8818 0.5108 0.6289 0.065 Uiso 1 1 calc R A . C2 C 0.8032(4) 0.5553(3) 0.7144(3) 0.0602(12) Uani 1 1 d . A . H2A H 0.8514 0.5970 0.7314 0.072 Uiso 1 1 calc R . . H2B H 0.7435 0.5734 0.6628 0.072 Uiso 1 1 calc R . . C3 C 0.7742(3) 0.5356(2) 0.8049(3) 0.0546(11) Uani 1 1 d . . . H3 H 0.7578 0.5832 0.8320 0.066 Uiso 1 1 calc R A . C4 C 0.8621(3) 0.4981(3) 0.8833(3) 0.0554(12) Uani 1 1 d . A . H4A H 0.8417 0.4851 0.9394 0.066 Uiso 1 1 calc R . . H4B H 0.9173 0.5344 0.9054 0.066 Uiso 1 1 calc R . . C5 C 0.8991(3) 0.4259(3) 0.8460(3) 0.0508(11) Uani 1 1 d . . . H5 H 0.9590 0.4066 0.8979 0.061 Uiso 1 1 calc R A . C6 C 0.9278(3) 0.4447(3) 0.7547(3) 0.0563(12) Uani 1 1 d . A . H6A H 0.9414 0.3971 0.7269 0.068 Uiso 1 1 calc R . . H6B H 0.9899 0.4740 0.7756 0.068 Uiso 1 1 calc R . . C7 C 0.7551(3) 0.4299(3) 0.5243(3) 0.0549(11) Uani 1 1 d . . . H7 H 0.7987 0.4565 0.4995 0.066 Uiso 1 1 calc R A . C8 C 0.6774(3) 0.3847(3) 0.4562(3) 0.0565(11) Uani 1 1 d . A . H8 H 0.6365 0.3543 0.4801 0.068 Uiso 1 1 calc R . . C9 C 0.6622(4) 0.3850(3) 0.3601(3) 0.0626(12) Uani 1 1 d . . . H9 H 0.7079 0.4131 0.3396 0.075 Uiso 1 1 calc R A . C10 C 0.5813(4) 0.3460(3) 0.2823(3) 0.0558(11) Uani 1 1 d . A . C11 C 0.5895(4) 0.3369(3) 0.1889(4) 0.0737(15) Uani 1 1 d . . . H11 H 0.6474 0.3539 0.1776 0.088 Uiso 1 1 calc R A . C12 C 0.5139(6) 0.3033(4) 0.1135(4) 0.0917(19) Uani 1 1 d . A . H12 H 0.5206 0.2979 0.0517 0.110 Uiso 1 1 calc R . . C13 C 0.4286(6) 0.2779(4) 0.1295(4) 0.098(2) Uani 1 1 d . . . H13 H 0.3778 0.2543 0.0790 0.117 Uiso 1 1 calc R A . C14 C 0.4181(5) 0.2874(3) 0.2205(4) 0.0850(17) Uani 1 1 d . A . H14 H 0.3594 0.2711 0.2306 0.102 Uiso 1 1 calc R . . C15 C 0.4941(4) 0.3210(3) 0.2968(4) 0.0676(13) Uani 1 1 d . . . H15 H 0.4865 0.3267 0.3582 0.081 Uiso 1 1 calc R A . C16 C 0.6164(4) 0.4995(3) 0.8194(3) 0.0597(12) Uani 1 1 d . . . H16 H 0.6197 0.5462 0.8513 0.072 Uiso 1 1 calc R A . C17 C 0.5352(3) 0.4482(3) 0.8164(3) 0.0568(11) Uani 1 1 d . A . H17 H 0.5274 0.4032 0.7801 0.068 Uiso 1 1 calc R . . C18 C 0.4709(3) 0.4637(3) 0.8644(3) 0.0569(12) Uani 1 1 d . . . H18 H 0.4790 0.5106 0.8963 0.068 Uiso 1 1 calc R A . C19 C 0.3894(3) 0.4153(3) 0.8724(3) 0.0541(11) Uani 1 1 d . A . C20 C 0.3198(4) 0.4453(3) 0.9123(4) 0.0667(13) Uani 1 1 d . . . H20 H 0.3261 0.4957 0.9341 0.080 Uiso 1 1 calc R A . C21 C 0.2407(4) 0.4005(4) 0.9200(4) 0.0773(16) Uani 1 1 d . A . H21 H 0.1951 0.4212 0.9474 0.093 Uiso 1 1 calc R . . C22 C 0.2296(4) 0.3276(4) 0.8879(4) 0.0762(16) Uani 1 1 d . . . H22 H 0.1763 0.2982 0.8929 0.091 Uiso 1 1 calc R A . C23 C 0.2969(4) 0.2966(3) 0.8480(4) 0.0720(14) Uani 1 1 d . A . H23 H 0.2889 0.2462 0.8259 0.086 Uiso 1 1 calc R . . C24 C 0.3762(4) 0.3393(3) 0.8403(3) 0.0597(12) Uani 1 1 d . . . H24 H 0.4215 0.3175 0.8135 0.072 Uiso 1 1 calc R A . C25 C 0.8271(3) 0.3179(3) 0.8927(3) 0.0517(11) Uani 1 1 d . . . H25 H 0.8896 0.3142 0.9421 0.062 Uiso 1 1 calc R A . C26 C 0.7487(3) 0.2663(3) 0.8977(3) 0.0542(11) Uani 1 1 d . A . H26 H 0.6876 0.2641 0.8461 0.065 Uiso 1 1 calc R . . C27 C 0.7639(4) 0.2219(3) 0.9763(3) 0.0601(12) Uani 1 1 d . . . H27 H 0.8292 0.2215 1.0212 0.072 Uiso 1 1 calc R A . C28 C 0.6909(4) 0.1738(3) 1.0007(3) 0.0575(12) Uani 1 1 d . A . C29 C 0.7218(5) 0.1334(3) 1.0888(4) 0.0821(17) Uani 1 1 d . . . H29 H 0.7893 0.1346 1.1285 0.099 Uiso 1 1 calc R A . C30 C 0.6535(6) 0.0915(4) 1.1179(5) 0.099(2) Uani 1 1 d . A . H30 H 0.6745 0.0661 1.1781 0.118 Uiso 1 1 calc R . . C31 C 0.5561(6) 0.0872(4) 1.0589(5) 0.092(2) Uani 1 1 d . . . H31 H 0.5105 0.0584 1.0785 0.111 Uiso 1 1 calc R A . C32 C 0.5238(4) 0.1251(3) 0.9703(5) 0.0757(16) Uani 1 1 d . A . H32 H 0.4566 0.1217 0.9302 0.091 Uiso 1 1 calc R . . C33 C 0.5904(4) 0.1682(3) 0.9406(4) 0.0632(13) Uani 1 1 d . . . H33 H 0.5683 0.1935 0.8803 0.076 Uiso 1 1 calc R A . C34 C 0.8578(8) 0.3707(8) 0.1908(10) 0.221(7) Uani 1 1 d . . . H34A H 0.8510 0.3165 0.1802 0.331 Uiso 1 1 calc R . . H34B H 0.7920 0.3935 0.1736 0.331 Uiso 1 1 calc R . . H34C H 0.8947 0.3806 0.2589 0.331 Uiso 1 1 calc R . . 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 Cu 0.0415(3) 0.0707(4) 0.0453(3) -0.0118(3) 0.0150(2) -0.0156(3) S1 0.0494(7) 0.1108(12) 0.0537(7) 0.0138(8) 0.0064(6) -0.0152(7) O1 0.223(9) 0.085(4) 0.244(9) -0.008(5) 0.013(7) 0.009(5) O4 0.0493(19) 0.098(3) 0.071(2) -0.035(2) 0.0175(16) -0.0257(18) O5 0.081(3) 0.141(4) 0.076(2) 0.012(3) 0.023(2) -0.046(3) O2 0.037(3) 0.062(4) 0.059(4) -0.008(3) 0.006(3) -0.004(3) O3 0.075(5) 0.079(6) 0.055(4) -0.021(4) 0.003(4) -0.026(5) O6 0.048(4) 0.074(5) 0.056(4) 0.011(4) 0.000(3) -0.003(4) O7 0.119(7) 0.054(5) 0.124(7) -0.028(5) -0.028(6) -0.002(5) O8 0.046(4) 0.063(5) 0.066(4) -0.011(4) 0.008(3) 0.004(3) C35 0.087(8) 0.058(7) 0.093(8) 0.002(6) 0.007(6) 0.028(6) N1 0.045(2) 0.064(2) 0.045(2) -0.0050(18) 0.0160(16) -0.0069(18) N2 0.049(2) 0.065(2) 0.051(2) 0.0021(18) 0.0204(17) 0.0024(19) N3 0.041(2) 0.049(2) 0.051(2) -0.0026(17) 0.0145(16) -0.0048(16) C1 0.052(3) 0.062(3) 0.053(3) 0.000(2) 0.026(2) -0.014(2) C2 0.065(3) 0.055(3) 0.062(3) 0.003(2) 0.023(2) -0.012(2) C3 0.062(3) 0.044(3) 0.065(3) -0.009(2) 0.030(2) -0.008(2) C4 0.055(3) 0.056(3) 0.052(3) -0.012(2) 0.013(2) -0.018(2) C5 0.037(2) 0.058(3) 0.052(3) -0.003(2) 0.0067(19) -0.013(2) C6 0.044(3) 0.065(3) 0.062(3) -0.009(2) 0.020(2) -0.014(2) C7 0.049(3) 0.069(3) 0.050(3) -0.001(2) 0.021(2) -0.003(2) C8 0.051(3) 0.072(3) 0.048(2) 0.004(2) 0.019(2) 0.004(2) C9 0.060(3) 0.080(3) 0.054(3) 0.002(3) 0.027(2) 0.001(3) C10 0.063(3) 0.058(3) 0.045(2) 0.001(2) 0.016(2) 0.007(2) C11 0.091(4) 0.079(4) 0.053(3) -0.002(3) 0.027(3) 0.013(3) C12 0.133(6) 0.082(4) 0.051(3) -0.011(3) 0.018(4) 0.007(4) C13 0.122(6) 0.080(4) 0.060(4) -0.006(3) -0.013(4) -0.004(4) C14 0.082(4) 0.080(4) 0.077(4) 0.018(3) 0.005(3) -0.017(3) C15 0.077(4) 0.065(3) 0.053(3) 0.007(2) 0.012(3) -0.003(3) C16 0.065(3) 0.057(3) 0.062(3) 0.005(2) 0.027(2) 0.007(2) C17 0.056(3) 0.059(3) 0.060(3) 0.002(2) 0.027(2) 0.000(2) C18 0.057(3) 0.057(3) 0.060(3) -0.001(2) 0.025(2) 0.005(2) C19 0.050(3) 0.067(3) 0.048(2) 0.003(2) 0.020(2) 0.011(2) C20 0.060(3) 0.077(4) 0.071(3) -0.018(3) 0.032(3) 0.000(3) C21 0.068(3) 0.099(5) 0.079(4) -0.022(3) 0.044(3) -0.005(3) C22 0.063(3) 0.102(5) 0.072(3) -0.014(3) 0.032(3) -0.019(3) C23 0.072(4) 0.071(4) 0.077(4) -0.010(3) 0.031(3) -0.007(3) C24 0.057(3) 0.070(3) 0.057(3) -0.004(2) 0.025(2) 0.005(2) C25 0.042(2) 0.058(3) 0.052(3) 0.000(2) 0.0100(19) -0.002(2) C26 0.052(3) 0.058(3) 0.053(3) -0.001(2) 0.018(2) -0.010(2) C27 0.059(3) 0.060(3) 0.059(3) 0.001(2) 0.017(2) -0.005(2) C28 0.072(3) 0.058(3) 0.045(2) -0.003(2) 0.024(2) -0.007(2) C29 0.102(4) 0.082(4) 0.060(3) 0.003(3) 0.024(3) -0.022(3) C30 0.143(6) 0.098(5) 0.066(4) 0.006(3) 0.050(4) -0.027(5) C31 0.119(6) 0.092(5) 0.096(5) -0.015(4) 0.076(5) -0.033(4) C32 0.074(4) 0.077(4) 0.091(4) -0.013(3) 0.047(3) -0.015(3) C33 0.063(3) 0.071(3) 0.062(3) -0.005(3) 0.029(3) -0.005(3) C34 0.134(8) 0.315(18) 0.289(15) -0.093(13) 0.171(10) -0.038(9) _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 Cu O4 1.976(4) . ? Cu N2 1.994(4) . ? Cu O2 1.999(5) . ? Cu N3 2.001(3) . ? Cu O8 2.132(6) . ? Cu N1 2.175(3) . ? S1 O3 1.335(6) . ? S1 O6 1.422(6) . ? S1 O5 1.428(4) . ? S1 O4 1.441(3) . ? S1 O7 1.639(8) . ? S1 O2 1.679(7) . ? O1 C34 1.291(11) . ? O8 C35 1.476(12) . ? N1 C7 1.276(5) . ? N1 C1 1.477(5) . ? N2 C16 1.288(5) . ? N2 C3 1.484(5) . ? N3 C25 1.270(5) . ? N3 C5 1.486(5) . ? C1 C2 1.531(6) . ? C1 C6 1.533(6) . ? C2 C3 1.529(6) . ? C3 C4 1.517(6) . ? C4 C5 1.531(6) . ? C5 C6 1.533(6) . ? C7 C8 1.437(6) . ? C8 C9 1.328(6) . ? C9 C10 1.471(6) . ? C10 C15 1.383(7) . ? C10 C11 1.396(6) . ? C11 C12 1.372(8) . ? C12 C13 1.368(9) . ? C13 C14 1.375(9) . ? C14 C15 1.382(7) . ? C16 C17 1.442(6) . ? C17 C18 1.336(6) . ? C18 C19 1.460(6) . ? C19 C20 1.393(6) . ? C19 C24 1.398(7) . ? C20 C21 1.393(7) . ? C21 C22 1.348(8) . ? C22 C23 1.372(7) . ? C23 C24 1.377(7) . ? C25 C26 1.446(6) . ? C26 C27 1.329(6) . ? C27 C28 1.458(6) . ? C28 C29 1.388(7) . ? C28 C33 1.392(6) . ? C29 C30 1.381(8) . ? C30 C31 1.351(9) . ? C31 C32 1.374(8) . ? C32 C33 1.377(7) . ? 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 O4 Cu N2 162.22(14) . . ? O4 Cu O2 63.9(2) . . ? N2 Cu O2 109.8(2) . . ? O4 Cu N3 94.32(14) . . ? N2 Cu N3 84.81(14) . . ? O2 Cu N3 150.5(2) . . ? O4 Cu O8 95.4(2) . . ? N2 Cu O8 83.2(2) . . ? O2 Cu O8 33.5(2) . . ? N3 Cu O8 166.8(2) . . ? O4 Cu N1 101.92(14) . . ? N2 Cu N1 95.82(14) . . ? O2 Cu N1 107.2(2) . . ? N3 Cu N1 96.22(14) . . ? O8 Cu N1 90.6(2) . . ? O3 S1 O6 46.7(4) . . ? O3 S1 O5 125.5(4) . . ? O6 S1 O5 114.2(4) . . ? O3 S1 O4 116.1(4) . . ? O6 S1 O4 124.5(3) . . ? O5 S1 O4 114.0(2) . . ? O3 S1 O7 55.7(5) . . ? O6 S1 O7 101.2(5) . . ? O5 S1 O7 98.0(5) . . ? O4 S1 O7 97.7(4) . . ? O3 S1 O2 106.9(5) . . ? O6 S1 O2 63.4(4) . . ? O5 S1 O2 97.8(3) . . ? O4 S1 O2 84.4(2) . . ? O7 S1 O2 161.5(4) . . ? S1 O4 Cu 109.9(2) . . ? S1 O2 Cu 99.4(3) . . ? C35 O8 Cu 131.0(6) . . ? C7 N1 C1 117.2(4) . . ? C7 N1 Cu 132.9(3) . . ? C1 N1 Cu 109.8(2) . . ? C16 N2 C3 118.1(4) . . ? C16 N2 Cu 124.4(3) . . ? C3 N2 Cu 116.5(3) . . ? C25 N3 C5 116.4(4) . . ? C25 N3 Cu 125.8(3) . . ? C5 N3 Cu 116.7(3) . . ? N1 C1 C2 110.4(4) . . ? N1 C1 C6 109.2(4) . . ? C2 C1 C6 112.2(4) . . ? C3 C2 C1 115.1(4) . . ? N2 C3 C4 109.4(4) . . ? N2 C3 C2 112.4(4) . . ? C4 C3 C2 110.4(4) . . ? C3 C4 C5 112.6(3) . . ? N3 C5 C4 107.4(3) . . ? N3 C5 C6 112.9(3) . . ? C4 C5 C6 109.9(4) . . ? C5 C6 C1 115.8(4) . . ? N1 C7 C8 125.1(4) . . ? C9 C8 C7 122.0(5) . . ? C8 C9 C10 127.3(5) . . ? C15 C10 C11 118.1(5) . . ? C15 C10 C9 122.1(4) . . ? C11 C10 C9 119.7(5) . . ? C12 C11 C10 121.3(6) . . ? C13 C12 C11 119.8(6) . . ? C12 C13 C14 120.0(6) . . ? C13 C14 C15 120.5(6) . . ? C14 C15 C10 120.2(5) . . ? N2 C16 C17 123.9(5) . . ? C18 C17 C16 121.5(5) . . ? C17 C18 C19 127.4(5) . . ? C20 C19 C24 117.4(5) . . ? C20 C19 C18 119.5(4) . . ? C24 C19 C18 123.1(4) . . ? C19 C20 C21 120.6(5) . . ? C22 C21 C20 120.6(5) . . ? C21 C22 C23 120.0(5) . . ? C22 C23 C24 120.6(5) . . ? C23 C24 C19 120.7(5) . . ? N3 C25 C26 125.2(4) . . ? C27 C26 C25 119.9(4) . . ? C26 C27 C28 128.0(5) . . ? C29 C28 C33 118.4(5) . . ? C29 C28 C27 118.8(5) . . ? C33 C28 C27 122.7(4) . . ? C30 C29 C28 120.6(6) . . ? C31 C30 C29 120.0(6) . . ? C30 C31 C32 120.6(6) . . ? C31 C32 C33 120.3(6) . . ? C32 C33 C28 120.0(5) . . ? 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 O3 S1 O4 Cu 119.4(5) . . . . ? O6 S1 O4 Cu 65.6(5) . . . . ? O5 S1 O4 Cu -82.7(3) . . . . ? O7 S1 O4 Cu 174.9(4) . . . . ? O2 S1 O4 Cu 13.3(3) . . . . ? N2 Cu O4 S1 60.4(6) . . . . ? O2 Cu O4 S1 -12.4(3) . . . . ? N3 Cu O4 S1 146.9(2) . . . . ? O8 Cu O4 S1 -24.1(3) . . . . ? N1 Cu O4 S1 -115.8(2) . . . . ? O3 S1 O2 Cu -128.1(4) . . . . ? O6 S1 O2 Cu -145.8(4) . . . . ? O5 S1 O2 Cu 101.0(3) . . . . ? O4 S1 O2 Cu -12.5(2) . . . . ? O7 S1 O2 Cu -110.1(12) . . . . ? O4 Cu O2 S1 10.1(2) . . . . ? N2 Cu O2 S1 -151.8(2) . . . . ? N3 Cu O2 S1 -35.7(6) . . . . ? O8 Cu O2 S1 168.6(6) . . . . ? N1 Cu O2 S1 105.2(3) . . . . ? O4 Cu O8 C35 -139.1(8) . . . . ? N2 Cu O8 C35 58.8(8) . . . . ? O2 Cu O8 C35 -158.3(10) . . . . ? N3 Cu O8 C35 83.9(13) . . . . ? N1 Cu O8 C35 -37.0(8) . . . . ? O4 Cu N1 C7 44.2(5) . . . . ? N2 Cu N1 C7 -134.7(4) . . . . ? O2 Cu N1 C7 -21.9(5) . . . . ? N3 Cu N1 C7 139.9(4) . . . . ? O8 Cu N1 C7 -51.5(5) . . . . ? O4 Cu N1 C1 -138.6(3) . . . . ? N2 Cu N1 C1 42.5(3) . . . . ? O2 Cu N1 C1 155.3(3) . . . . ? N3 Cu N1 C1 -42.9(3) . . . . ? O8 Cu N1 C1 125.7(3) . . . . ? O4 Cu N2 C16 -23.6(7) . . . . ? O2 Cu N2 C16 42.1(4) . . . . ? N3 Cu N2 C16 -111.5(4) . . . . ? O8 Cu N2 C16 62.9(4) . . . . ? N1 Cu N2 C16 152.7(4) . . . . ? O4 Cu N2 C3 144.5(4) . . . . ? O2 Cu N2 C3 -149.8(3) . . . . ? N3 Cu N2 C3 56.5(3) . . . . ? O8 Cu N2 C3 -129.1(4) . . . . ? N1 Cu N2 C3 -39.2(3) . . . . ? O4 Cu N3 C25 -52.5(4) . . . . ? N2 Cu N3 C25 109.7(4) . . . . ? O2 Cu N3 C25 -12.3(6) . . . . ? O8 Cu N3 C25 84.6(10) . . . . ? N1 Cu N3 C25 -155.0(4) . . . . ? O4 Cu N3 C5 139.6(3) . . . . ? N2 Cu N3 C5 -58.2(3) . . . . ? O2 Cu N3 C5 179.8(4) . . . . ? O8 Cu N3 C5 -83.3(10) . . . . ? N1 Cu N3 C5 37.1(3) . . . . ? C7 N1 C1 C2 116.3(4) . . . . ? Cu N1 C1 C2 -61.3(4) . . . . ? C7 N1 C1 C6 -119.8(4) . . . . ? Cu N1 C1 C6 62.5(4) . . . . ? N1 C1 C2 C3 77.4(5) . . . . ? C6 C1 C2 C3 -44.7(5) . . . . ? C16 N2 C3 C4 100.4(5) . . . . ? Cu N2 C3 C4 -68.5(4) . . . . ? C16 N2 C3 C2 -136.7(4) . . . . ? Cu N2 C3 C2 54.5(4) . . . . ? C1 C2 C3 N2 -70.8(5) . . . . ? C1 C2 C3 C4 51.5(5) . . . . ? N2 C3 C4 C5 66.6(5) . . . . ? C2 C3 C4 C5 -57.5(5) . . . . ? C25 N3 C5 C4 -99.1(4) . . . . ? Cu N3 C5 C4 70.0(4) . . . . ? C25 N3 C5 C6 139.5(4) . . . . ? Cu N3 C5 C6 -51.4(4) . . . . ? C3 C4 C5 N3 -66.7(4) . . . . ? C3 C4 C5 C6 56.5(5) . . . . ? N3 C5 C6 C1 70.0(5) . . . . ? C4 C5 C6 C1 -49.9(5) . . . . ? N1 C1 C6 C5 -78.6(5) . . . . ? C2 C1 C6 C5 44.2(5) . . . . ? C1 N1 C7 C8 -176.3(4) . . . . ? Cu N1 C7 C8 0.7(7) . . . . ? N1 C7 C8 C9 174.7(5) . . . . ? C7 C8 C9 C10 -175.3(5) . . . . ? C8 C9 C10 C15 18.5(8) . . . . ? C8 C9 C10 C11 -164.7(5) . . . . ? C15 C10 C11 C12 -0.7(8) . . . . ? C9 C10 C11 C12 -177.6(5) . . . . ? C10 C11 C12 C13 -0.2(9) . . . . ? C11 C12 C13 C14 1.2(10) . . . . ? C12 C13 C14 C15 -1.4(9) . . . . ? C13 C14 C15 C10 0.5(8) . . . . ? C11 C10 C15 C14 0.5(7) . . . . ? C9 C10 C15 C14 177.3(5) . . . . ? C3 N2 C16 C17 -168.8(4) . . . . ? Cu N2 C16 C17 -1.0(6) . . . . ? N2 C16 C17 C18 174.6(4) . . . . ? C16 C17 C18 C19 -176.2(4) . . . . ? C17 C18 C19 C20 -170.0(5) . . . . ? C17 C18 C19 C24 9.1(7) . . . . ? C24 C19 C20 C21 0.3(7) . . . . ? C18 C19 C20 C21 179.4(5) . . . . ? C19 C20 C21 C22 -0.6(8) . . . . ? C20 C21 C22 C23 0.4(9) . . . . ? C21 C22 C23 C24 0.1(8) . . . . ? C22 C23 C24 C19 -0.4(8) . . . . ? C20 C19 C24 C23 0.2(7) . . . . ? C18 C19 C24 C23 -178.8(4) . . . . ? C5 N3 C25 C26 167.2(4) . . . . ? Cu N3 C25 C26 -0.7(7) . . . . ? N3 C25 C26 C27 -172.7(5) . . . . ? C25 C26 C27 C28 171.5(5) . . . . ? C26 C27 C28 C29 -178.0(5) . . . . ? C26 C27 C28 C33 0.3(8) . . . . ? C33 C28 C29 C30 -2.9(8) . . . . ? C27 C28 C29 C30 175.5(5) . . . . ? C28 C29 C30 C31 2.3(10) . . . . ? C29 C30 C31 C32 -0.8(10) . . . . ? C30 C31 C32 C33 -0.2(9) . . . . ? C31 C32 C33 C28 -0.4(8) . . . . ? C29 C28 C33 C32 1.9(7) . . . . ? C27 C28 C33 C32 -176.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.597 _refine_diff_density_min -0.519 _refine_diff_density_rms 0.062 #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis,cis-1,3,5-(E,E)-tri(phenyl-propenylideneamino)cyclohexane nickel(II) chloride tetraphenylborate, (2) {tri(phenyl-propenylideneamino)cyclohexane = (Ph-protach)} ; _chemical_name_common '[Ni(Ph-protach)(Cl)]BPh4, (2)' _chemical_melting_point '495-495.5 K' _chemical_formula_moiety 'C33 H33 Cl N3 Ni 1+, C24 H20 B 1-' _chemical_formula_sum 'C57 H53 B Cl N3 Ni' _chemical_formula_weight 884.99 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' 'Ni' 'Ni' 0.3393 1.1124 '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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.579(3) _cell_length_b 16.549(3) _cell_length_c 19.916(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.335(10) _cell_angle_gamma 90.00 _cell_volume 4845.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 0.496 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.797 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; Crystal mounted in epoxy-based glue on a glass capillary ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_source_current 30 _diffrn_source_voltage 50 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -5 -1 5 1 -1 -7 0 -6 -1 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.344 _diffrn_reflns_number 7496 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6868 _reflns_number_gt 4119 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'MSC/AFC (Diffractometer Control)' _computing_cell_refinement 'MSC/AFC (Diffractometer Control)' _computing_data_reduction '(teXsan, Molecular Structure Corporation, 1992)' _computing_structure_solution 'SAPI91 (Rigaku Corporation, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics teXsan _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0969P)^2^+3.7150P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6868 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1229 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1934 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.32612(5) 0.45147(4) 0.70689(4) 0.0557(2) Uani 1 1 d . . . Cl1 Cl 0.28603(11) 0.56165(9) 0.64261(8) 0.0752(5) Uani 1 1 d . . . N1 N 0.3109(3) 0.4389(3) 0.8016(2) 0.0573(11) Uani 1 1 d . . . N2 N 0.4531(3) 0.4093(3) 0.7350(2) 0.0640(12) Uani 1 1 d . . . N3 N 0.2756(3) 0.3423(2) 0.6751(2) 0.0569(11) Uani 1 1 d . . . C1 C 0.3459(4) 0.3617(3) 0.8382(3) 0.0632(15) Uani 1 1 d . . . H1 H 0.3373 0.3617 0.8847 0.076 Uiso 1 1 calc R . . C2 C 0.4478(4) 0.3569(3) 0.8497(3) 0.0705(16) Uani 1 1 d . . . H2A H 0.4758 0.4078 0.8695 0.085 Uiso 1 1 calc R . . H2B H 0.4744 0.3150 0.8844 0.085 Uiso 1 1 calc R . . C3 C 0.4707(4) 0.3392(3) 0.7826(3) 0.0669(15) Uani 1 1 d . . . H3 H 0.5356 0.3258 0.7964 0.080 Uiso 1 1 calc R . . C4 C 0.4161(4) 0.2676(3) 0.7424(3) 0.0709(16) Uani 1 1 d . . . H4A H 0.4278 0.2614 0.6978 0.085 Uiso 1 1 calc R . . H4B H 0.4372 0.2189 0.7701 0.085 Uiso 1 1 calc R . . C5 C 0.3140(4) 0.2751(3) 0.7266(3) 0.0651(15) Uani 1 1 d . . . H5 H 0.2850 0.2244 0.7056 0.078 Uiso 1 1 calc R . . C6 C 0.2927(4) 0.2906(3) 0.7945(3) 0.0703(16) Uani 1 1 d . . . H6A H 0.3065 0.2422 0.8236 0.084 Uiso 1 1 calc R . . H6B H 0.2281 0.3012 0.7824 0.084 Uiso 1 1 calc R . . C7 C 0.2751(4) 0.4902(4) 0.8338(3) 0.0595(14) Uani 1 1 d . . . H7 H 0.2656 0.4729 0.8752 0.071 Uiso 1 1 calc R . . C8 C 0.2492(3) 0.5699(3) 0.8114(3) 0.0572(14) Uani 1 1 d . . . H8 H 0.2458 0.5858 0.7658 0.069 Uiso 1 1 calc R . . C9 C 0.2295(3) 0.6233(3) 0.8547(3) 0.0608(14) Uani 1 1 d . . . H9 H 0.2247 0.6031 0.8969 0.073 Uiso 1 1 calc R . . C10 C 0.2149(4) 0.7100(4) 0.8425(3) 0.0635(15) Uani 1 1 d . . . C11 C 0.2080(5) 0.7573(4) 0.8978(3) 0.0825(19) Uani 1 1 d . . . H11 H 0.2106 0.7332 0.9407 0.099 Uiso 1 1 calc R . . C12 C 0.1975(6) 0.8392(6) 0.8899(5) 0.126(3) Uani 1 1 d . . . H12 H 0.1942 0.8702 0.9279 0.152 Uiso 1 1 calc R . . C13 C 0.1917(6) 0.8768(5) 0.8269(6) 0.118(3) Uani 1 1 d . . . H13 H 0.1849 0.9325 0.8220 0.142 Uiso 1 1 calc R . . C14 C 0.1962(6) 0.8290(5) 0.7707(4) 0.106(2) Uani 1 1 d . . . H14 H 0.1904 0.8527 0.7271 0.127 Uiso 1 1 calc R . . C15 C 0.2092(5) 0.7481(4) 0.7791(3) 0.0839(19) Uani 1 1 d . . . H15 H 0.2144 0.7174 0.7415 0.101 Uiso 1 1 calc R . . C16 C 0.5154(4) 0.4327(4) 0.7084(4) 0.0791(18) Uani 1 1 d . . . H16 H 0.5709 0.4059 0.7242 0.095 Uiso 1 1 calc R . . C17 C 0.5061(4) 0.4947(4) 0.6581(4) 0.0816(18) Uani 1 1 d . . . H17 H 0.4528 0.5249 0.6442 0.098 Uiso 1 1 calc R . . C18 C 0.5698(5) 0.5122(5) 0.6295(4) 0.087(2) Uani 1 1 d . . . H18 H 0.6225 0.4811 0.6437 0.105 Uiso 1 1 calc R . . C19 C 0.5637(5) 0.5769(4) 0.5772(4) 0.0819(19) Uani 1 1 d . . . C20 C 0.6397(6) 0.5928(6) 0.5568(5) 0.117(3) Uani 1 1 d . . . H20 H 0.6924 0.5625 0.5761 0.140 Uiso 1 1 calc R . . C21 C 0.6372(8) 0.6530(6) 0.5085(6) 0.137(4) Uani 1 1 d . . . H21 H 0.6885 0.6634 0.4958 0.165 Uiso 1 1 calc R . . C22 C 0.5610(9) 0.6968(6) 0.4793(6) 0.136(3) Uani 1 1 d . . . H22 H 0.5587 0.7361 0.4454 0.163 Uiso 1 1 calc R . . C23 C 0.4879(7) 0.6830(5) 0.5001(5) 0.117(3) Uani 1 1 d . . . H23 H 0.4367 0.7155 0.4821 0.140 Uiso 1 1 calc R . . C24 C 0.4873(6) 0.6228(5) 0.5465(4) 0.099(2) Uani 1 1 d . . . H24 H 0.4347 0.6127 0.5575 0.119 Uiso 1 1 calc R . . C25 C 0.2151(4) 0.3238(3) 0.6162(3) 0.0636(15) Uani 1 1 d . . . H25 H 0.1989 0.2697 0.6080 0.076 Uiso 1 1 calc R . . C26 C 0.1707(4) 0.3804(4) 0.5621(3) 0.0665(15) Uani 1 1 d . . . H26 H 0.1836 0.4351 0.5703 0.080 Uiso 1 1 calc R . . C27 C 0.1108(4) 0.3570(4) 0.4996(3) 0.0697(16) Uani 1 1 d . . . H27 H 0.1002 0.3019 0.4925 0.084 Uiso 1 1 calc R . . C28 C 0.0608(4) 0.4109(4) 0.4419(3) 0.0703(16) Uani 1 1 d . . . C29 C 0.0075(4) 0.3744(5) 0.3783(3) 0.085(2) Uani 1 1 d . . . H29 H 0.0035 0.3184 0.3743 0.102 Uiso 1 1 calc R . . C30 C -0.0395(5) 0.4238(7) 0.3213(4) 0.105(3) Uani 1 1 d . . . H30 H -0.0721 0.4002 0.2780 0.127 Uiso 1 1 calc R . . C31 C -0.0390(5) 0.5037(8) 0.3274(5) 0.114(3) Uani 1 1 d . . . H31 H -0.0740 0.5344 0.2890 0.137 Uiso 1 1 calc R . . C32 C 0.0132(5) 0.5434(5) 0.3905(5) 0.109(3) Uani 1 1 d . . . H32 H 0.0145 0.5994 0.3945 0.131 Uiso 1 1 calc R . . C33 C 0.0628(5) 0.4935(5) 0.4464(4) 0.0864(19) Uani 1 1 d . . . H33 H 0.0989 0.5175 0.4885 0.104 Uiso 1 1 calc R . . C34 C 0.2149(4) -0.0660(3) 0.5730(3) 0.0545(13) Uani 1 1 d . . . C35 C 0.2847(4) -0.1215(4) 0.5841(3) 0.0715(17) Uani 1 1 d . . . H35 H 0.3426 -0.1030 0.5885 0.086 Uiso 1 1 calc R . . C36 C 0.2709(5) -0.2052(4) 0.5890(3) 0.0822(19) Uani 1 1 d . . . H36 H 0.3196 -0.2406 0.5965 0.099 Uiso 1 1 calc R . . C37 C 0.1872(5) -0.2348(4) 0.5827(3) 0.0796(18) Uani 1 1 d . . . H37 H 0.1783 -0.2900 0.5860 0.095 Uiso 1 1 calc R . . C38 C 0.1165(5) -0.1823(4) 0.5715(3) 0.0763(17) Uani 1 1 d . . . H38 H 0.0588 -0.2018 0.5664 0.092 Uiso 1 1 calc R . . C39 C 0.1303(4) -0.0983(3) 0.5676(3) 0.0688(16) Uani 1 1 d . . . H39 H 0.0814 -0.0635 0.5613 0.083 Uiso 1 1 calc R . . C40 C 0.3346(4) 0.0571(4) 0.5901(3) 0.0654(15) Uani 1 1 d . . . C41 C 0.3796(4) 0.0514(6) 0.5402(4) 0.114(3) Uani 1 1 d . . . H41 H 0.3486 0.0302 0.4954 0.136 Uiso 1 1 calc R . . C42 C 0.4703(6) 0.0767(7) 0.5556(6) 0.153(5) Uani 1 1 d . . . H42 H 0.4967 0.0757 0.5200 0.184 Uiso 1 1 calc R . . C43 C 0.5196(5) 0.1024(5) 0.6214(7) 0.128(4) Uani 1 1 d . . . H43 H 0.5793 0.1198 0.6313 0.153 Uiso 1 1 calc R . . C44 C 0.4798(5) 0.1024(4) 0.6737(6) 0.114(3) Uani 1 1 d . . . H44 H 0.5142 0.1157 0.7202 0.137 Uiso 1 1 calc R . . C45 C 0.3892(4) 0.0828(4) 0.6573(4) 0.0810(19) Uani 1 1 d . . . H45 H 0.3632 0.0868 0.6930 0.097 Uiso 1 1 calc R . . C46 C 0.1746(4) 0.0764(3) 0.6187(3) 0.0541(13) Uani 1 1 d . . . C47 C 0.1985(5) 0.0593(4) 0.6915(3) 0.0817(19) Uani 1 1 d . . . H47 H 0.2444 0.0217 0.7110 0.098 Uiso 1 1 calc R . . C48 C 0.1575(7) 0.0952(5) 0.7357(4) 0.097(2) Uani 1 1 d . . . H48 H 0.1764 0.0821 0.7839 0.117 Uiso 1 1 calc R . . C49 C 0.0897(6) 0.1493(5) 0.7087(5) 0.104(3) Uani 1 1 d . . . H49 H 0.0630 0.1748 0.7384 0.124 Uiso 1 1 calc R . . C50 C 0.0605(5) 0.1664(4) 0.6372(4) 0.084(2) Uani 1 1 d . . . H50 H 0.0127 0.2023 0.6180 0.101 Uiso 1 1 calc R . . C51 C 0.1029(4) 0.1296(4) 0.5937(3) 0.0660(15) Uani 1 1 d . . . H51 H 0.0819 0.1415 0.5453 0.079 Uiso 1 1 calc R . . C52 C 0.1742(3) 0.0649(3) 0.4845(3) 0.0499(12) Uani 1 1 d . . . C53 C 0.1925(4) 0.1430(3) 0.4645(3) 0.0602(14) Uani 1 1 d . . . H53 H 0.2375 0.1734 0.4970 0.072 Uiso 1 1 calc R . . C54 C 0.1467(4) 0.1766(4) 0.3987(3) 0.0678(16) Uani 1 1 d . . . H54 H 0.1599 0.2288 0.3880 0.081 Uiso 1 1 calc R . . C55 C 0.0807(4) 0.1312(4) 0.3489(3) 0.0761(18) Uani 1 1 d . . . H55 H 0.0499 0.1525 0.3042 0.091 Uiso 1 1 calc R . . C56 C 0.0615(4) 0.0554(4) 0.3659(3) 0.0662(15) Uani 1 1 d . . . H56 H 0.0168 0.0252 0.3329 0.079 Uiso 1 1 calc R . . C57 C 0.1079(3) 0.0229(3) 0.4319(3) 0.0563(14) Uani 1 1 d . . . H57 H 0.0941 -0.0296 0.4415 0.068 Uiso 1 1 calc R . . B1 B 0.2257(4) 0.0329(4) 0.5668(3) 0.0526(15) Uani 1 1 d . . . 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 0.0642(5) 0.0481(4) 0.0545(4) 0.0031(3) 0.0192(3) -0.0027(3) Cl1 0.0888(11) 0.0623(9) 0.0768(10) 0.0199(7) 0.0305(8) 0.0107(8) N1 0.063(3) 0.060(3) 0.046(2) 0.000(2) 0.013(2) -0.004(2) N2 0.058(3) 0.063(3) 0.067(3) 0.001(2) 0.016(2) -0.001(2) N3 0.068(3) 0.048(3) 0.055(3) -0.006(2) 0.021(2) -0.009(2) C1 0.089(4) 0.049(3) 0.050(3) 0.007(3) 0.021(3) 0.002(3) C2 0.080(4) 0.059(3) 0.058(4) 0.010(3) 0.004(3) 0.012(3) C3 0.067(4) 0.064(4) 0.063(4) 0.008(3) 0.013(3) 0.008(3) C4 0.091(5) 0.056(3) 0.066(4) 0.000(3) 0.027(3) 0.011(3) C5 0.088(4) 0.041(3) 0.063(4) -0.002(3) 0.021(3) -0.011(3) C6 0.094(4) 0.059(4) 0.058(4) 0.005(3) 0.025(3) -0.010(3) C7 0.060(3) 0.071(4) 0.046(3) 0.000(3) 0.017(3) -0.008(3) C8 0.051(3) 0.067(4) 0.050(3) 0.003(3) 0.013(3) -0.002(3) C9 0.057(3) 0.067(4) 0.059(3) -0.002(3) 0.021(3) 0.003(3) C10 0.057(3) 0.074(4) 0.057(4) -0.004(3) 0.015(3) 0.007(3) C11 0.103(5) 0.079(5) 0.072(4) -0.006(4) 0.039(4) 0.019(4) C12 0.153(8) 0.117(7) 0.106(7) -0.034(6) 0.037(6) 0.043(6) C13 0.139(8) 0.074(5) 0.138(8) -0.001(6) 0.041(7) 0.018(5) C14 0.141(7) 0.079(5) 0.095(6) 0.023(4) 0.037(5) 0.011(5) C15 0.117(6) 0.064(4) 0.074(4) 0.001(3) 0.035(4) -0.002(4) C16 0.061(4) 0.089(5) 0.087(5) -0.004(4) 0.025(4) 0.002(3) C17 0.077(4) 0.074(4) 0.102(5) 0.007(4) 0.040(4) -0.003(4) C18 0.070(4) 0.105(5) 0.093(5) 0.000(4) 0.036(4) -0.005(4) C19 0.090(5) 0.090(5) 0.081(5) -0.011(4) 0.048(4) -0.018(4) C20 0.101(6) 0.149(8) 0.119(7) 0.020(6) 0.061(5) -0.005(5) C21 0.159(10) 0.131(8) 0.166(10) 0.032(7) 0.113(9) -0.005(7) C22 0.185(11) 0.120(8) 0.131(8) 0.012(6) 0.093(9) -0.018(8) C23 0.140(8) 0.109(7) 0.117(7) 0.024(5) 0.065(6) 0.006(6) C24 0.099(6) 0.096(6) 0.115(6) 0.009(5) 0.050(5) 0.001(5) C25 0.071(4) 0.061(4) 0.061(4) -0.013(3) 0.026(3) -0.017(3) C26 0.065(4) 0.076(4) 0.056(4) -0.005(3) 0.017(3) -0.008(3) C27 0.064(4) 0.074(4) 0.068(4) -0.002(3) 0.018(3) -0.006(3) C28 0.054(4) 0.095(5) 0.062(4) -0.007(4) 0.019(3) -0.006(3) C29 0.057(4) 0.123(6) 0.066(4) -0.007(4) 0.009(3) 0.007(4) C30 0.074(5) 0.165(9) 0.065(5) 0.000(5) 0.005(4) 0.016(6) C31 0.068(5) 0.188(10) 0.088(6) 0.060(7) 0.027(5) 0.035(6) C32 0.078(5) 0.130(7) 0.121(7) 0.035(6) 0.035(5) 0.013(5) C33 0.079(5) 0.104(6) 0.072(5) 0.011(4) 0.019(4) -0.006(4) C34 0.056(3) 0.057(3) 0.048(3) 0.004(2) 0.013(3) 0.002(3) C35 0.055(4) 0.077(4) 0.073(4) -0.001(3) 0.008(3) 0.007(3) C36 0.087(5) 0.070(4) 0.076(4) 0.002(3) 0.008(4) 0.027(4) C37 0.102(6) 0.060(4) 0.068(4) 0.014(3) 0.016(4) -0.002(4) C38 0.084(4) 0.061(4) 0.085(5) 0.016(3) 0.029(4) -0.006(4) C39 0.064(4) 0.060(4) 0.089(4) 0.011(3) 0.033(3) 0.000(3) C40 0.054(3) 0.073(4) 0.065(4) 0.019(3) 0.015(3) 0.006(3) C41 0.053(4) 0.192(9) 0.092(5) 0.045(5) 0.019(4) 0.004(5) C42 0.053(5) 0.230(12) 0.178(10) 0.118(9) 0.039(6) 0.025(6) C43 0.042(5) 0.085(6) 0.235(13) 0.036(7) 0.018(7) 0.015(4) C44 0.049(5) 0.077(5) 0.176(9) -0.043(5) -0.017(5) 0.017(4) C45 0.055(4) 0.077(4) 0.097(5) -0.020(4) 0.007(4) 0.010(3) C46 0.059(3) 0.046(3) 0.059(3) -0.003(2) 0.022(3) -0.014(3) C47 0.115(5) 0.071(4) 0.060(4) 0.001(3) 0.031(4) -0.017(4) C48 0.156(8) 0.088(5) 0.061(4) -0.010(4) 0.054(5) -0.032(5) C49 0.141(8) 0.086(6) 0.118(7) -0.026(5) 0.089(6) -0.034(5) C50 0.085(5) 0.080(5) 0.104(6) -0.018(4) 0.053(4) -0.015(4) C51 0.059(4) 0.075(4) 0.071(4) -0.010(3) 0.032(3) -0.007(3) C52 0.047(3) 0.056(3) 0.050(3) 0.001(2) 0.020(2) 0.003(2) C53 0.064(4) 0.057(3) 0.061(4) 0.000(3) 0.022(3) 0.001(3) C54 0.082(4) 0.061(4) 0.069(4) 0.016(3) 0.038(4) 0.016(3) C55 0.072(4) 0.107(5) 0.050(4) 0.017(4) 0.022(3) 0.026(4) C56 0.060(4) 0.078(4) 0.055(3) -0.001(3) 0.011(3) 0.004(3) C57 0.051(3) 0.062(3) 0.059(3) -0.004(3) 0.022(3) -0.001(3) B1 0.050(4) 0.057(4) 0.046(3) 0.002(3) 0.010(3) -0.007(3) _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 N3 1.989(4) . ? Ni1 N1 1.989(4) . ? Ni1 N2 1.995(5) . ? Ni1 Cl1 2.1964(16) . ? N1 C7 1.296(7) . ? N1 C1 1.483(6) . ? N2 C16 1.309(7) . ? N2 C3 1.465(7) . ? N3 C25 1.276(6) . ? N3 C5 1.496(7) . ? C1 C2 1.529(8) . ? C1 C6 1.533(7) . ? C2 C3 1.521(8) . ? C3 C4 1.524(8) . ? C4 C5 1.521(8) . ? C5 C6 1.517(8) . ? C7 C8 1.409(7) . ? C8 C9 1.339(7) . ? C9 C10 1.460(8) . ? C10 C11 1.385(8) . ? C10 C15 1.387(8) . ? C11 C12 1.369(11) . ? C12 C13 1.377(11) . ? C13 C14 1.391(11) . ? C14 C15 1.357(9) . ? C16 C17 1.407(9) . ? C17 C18 1.329(8) . ? C18 C19 1.476(9) . ? C19 C24 1.373(10) . ? C19 C20 1.398(9) . ? C20 C21 1.377(11) . ? C21 C22 1.347(13) . ? C22 C23 1.353(12) . ? C23 C24 1.361(10) . ? C25 C26 1.421(8) . ? C26 C27 1.342(8) . ? C27 C28 1.460(8) . ? C28 C33 1.369(9) . ? C28 C29 1.401(8) . ? C29 C30 1.394(10) . ? C30 C31 1.328(12) . ? C31 C32 1.412(12) . ? C32 C33 1.395(10) . ? C34 C35 1.384(7) . ? C34 C39 1.393(7) . ? C34 B1 1.654(8) . ? C35 C36 1.410(8) . ? C36 C37 1.360(9) . ? C37 C38 1.362(8) . ? C38 C39 1.411(8) . ? C40 C45 1.394(8) . ? C40 C41 1.396(9) . ? C40 B1 1.654(8) . ? C41 C42 1.408(11) . ? C42 C43 1.350(14) . ? C43 C44 1.378(13) . ? C44 C45 1.378(10) . ? C46 C51 1.379(7) . ? C46 C47 1.400(8) . ? C46 B1 1.663(8) . ? C47 C48 1.383(10) . ? C48 C49 1.353(11) . ? C49 C50 1.374(10) . ? C50 C51 1.392(8) . ? C52 C57 1.390(7) . ? C52 C53 1.409(7) . ? C52 B1 1.655(8) . ? C53 C54 1.383(7) . ? C54 C55 1.390(8) . ? C55 C56 1.357(8) . ? C56 C57 1.382(7) . ? 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 N3 Ni1 N1 92.73(17) . . ? N3 Ni1 N2 91.29(19) . . ? N1 Ni1 N2 96.64(19) . . ? N3 Ni1 Cl1 124.25(14) . . ? N1 Ni1 Cl1 122.66(14) . . ? N2 Ni1 Cl1 121.20(15) . . ? C7 N1 C1 118.1(5) . . ? C7 N1 Ni1 127.4(4) . . ? C1 N1 Ni1 114.6(3) . . ? C16 N2 C3 119.4(5) . . ? C16 N2 Ni1 125.6(4) . . ? C3 N2 Ni1 114.5(4) . . ? C25 N3 C5 117.3(5) . . ? C25 N3 Ni1 127.1(4) . . ? C5 N3 Ni1 115.5(3) . . ? N1 C1 C2 108.2(4) . . ? N1 C1 C6 109.9(4) . . ? C2 C1 C6 112.6(5) . . ? C3 C2 C1 114.4(5) . . ? N2 C3 C2 111.6(5) . . ? N2 C3 C4 108.9(5) . . ? C2 C3 C4 111.0(5) . . ? C5 C4 C3 114.1(5) . . ? N3 C5 C6 109.3(5) . . ? N3 C5 C4 110.9(4) . . ? C6 C5 C4 110.6(5) . . ? C5 C6 C1 113.5(5) . . ? N1 C7 C8 125.6(5) . . ? C9 C8 C7 121.1(5) . . ? C8 C9 C10 126.6(5) . . ? C11 C10 C15 117.9(6) . . ? C11 C10 C9 118.1(6) . . ? C15 C10 C9 123.9(5) . . ? C12 C11 C10 120.4(7) . . ? C11 C12 C13 121.5(7) . . ? C12 C13 C14 118.1(8) . . ? C15 C14 C13 120.4(7) . . ? C14 C15 C10 121.6(7) . . ? N2 C16 C17 126.1(6) . . ? C18 C17 C16 123.3(7) . . ? C17 C18 C19 125.3(7) . . ? C24 C19 C20 117.4(7) . . ? C24 C19 C18 124.1(6) . . ? C20 C19 C18 118.6(7) . . ? C21 C20 C19 120.5(9) . . ? C22 C21 C20 120.5(9) . . ? C21 C22 C23 119.2(9) . . ? C22 C23 C24 121.8(9) . . ? C23 C24 C19 120.5(8) . . ? N3 C25 C26 124.5(5) . . ? C27 C26 C25 121.9(6) . . ? C26 C27 C28 125.5(6) . . ? C33 C28 C29 119.0(7) . . ? C33 C28 C27 124.3(6) . . ? C29 C28 C27 116.7(6) . . ? C30 C29 C28 118.5(8) . . ? C31 C30 C29 121.6(8) . . ? C30 C31 C32 121.9(8) . . ? C33 C32 C31 116.0(8) . . ? C28 C33 C32 122.9(8) . . ? C35 C34 C39 115.5(5) . . ? C35 C34 B1 125.1(5) . . ? C39 C34 B1 119.4(5) . . ? C34 C35 C36 122.3(6) . . ? C37 C36 C35 120.7(6) . . ? C36 C37 C38 119.0(6) . . ? C37 C38 C39 120.5(6) . . ? C34 C39 C38 122.1(6) . . ? C45 C40 C41 114.5(6) . . ? C45 C40 B1 125.9(5) . . ? C41 C40 B1 119.6(6) . . ? C40 C41 C42 121.9(8) . . ? C43 C42 C41 120.9(10) . . ? C42 C43 C44 118.7(8) . . ? C43 C44 C45 120.2(8) . . ? C44 C45 C40 123.5(7) . . ? C51 C46 C47 114.1(5) . . ? C51 C46 B1 123.2(5) . . ? C47 C46 B1 122.6(5) . . ? C48 C47 C46 123.6(7) . . ? C49 C48 C47 119.7(7) . . ? C48 C49 C50 119.7(7) . . ? C49 C50 C51 119.5(7) . . ? C46 C51 C50 123.3(6) . . ? C57 C52 C53 114.5(5) . . ? C57 C52 B1 125.6(5) . . ? C53 C52 B1 119.8(5) . . ? C54 C53 C52 123.2(5) . . ? C53 C54 C55 119.1(6) . . ? C56 C55 C54 119.6(5) . . ? C55 C56 C57 120.5(6) . . ? C56 C57 C52 123.2(5) . . ? C34 B1 C40 109.8(4) . . ? C34 B1 C52 111.3(4) . . ? C40 B1 C52 108.4(4) . . ? C34 B1 C46 107.5(4) . . ? C40 B1 C46 112.2(4) . . ? C52 B1 C46 107.6(4) . . ? 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 N3 Ni1 N1 C7 -132.2(5) . . . . ? N2 Ni1 N1 C7 136.2(5) . . . . ? Cl1 Ni1 N1 C7 2.2(5) . . . . ? N3 Ni1 N1 C1 48.3(4) . . . . ? N2 Ni1 N1 C1 -43.4(4) . . . . ? Cl1 Ni1 N1 C1 -177.3(3) . . . . ? N3 Ni1 N2 C16 119.1(5) . . . . ? N1 Ni1 N2 C16 -148.0(5) . . . . ? Cl1 Ni1 N2 C16 -13.1(6) . . . . ? N3 Ni1 N2 C3 -52.5(4) . . . . ? N1 Ni1 N2 C3 40.4(4) . . . . ? Cl1 Ni1 N2 C3 175.2(3) . . . . ? N1 Ni1 N3 C25 132.3(5) . . . . ? N2 Ni1 N3 C25 -131.0(5) . . . . ? Cl1 Ni1 N3 C25 -1.0(5) . . . . ? N1 Ni1 N3 C5 -48.1(4) . . . . ? N2 Ni1 N3 C5 48.6(4) . . . . ? Cl1 Ni1 N3 C5 178.6(3) . . . . ? C7 N1 C1 C2 -119.2(5) . . . . ? Ni1 N1 C1 C2 60.4(5) . . . . ? C7 N1 C1 C6 117.4(5) . . . . ? Ni1 N1 C1 C6 -63.0(5) . . . . ? N1 C1 C2 C3 -73.9(6) . . . . ? C6 C1 C2 C3 47.8(6) . . . . ? C16 N2 C3 C2 131.8(6) . . . . ? Ni1 N2 C3 C2 -56.0(5) . . . . ? C16 N2 C3 C4 -105.4(6) . . . . ? Ni1 N2 C3 C4 66.8(5) . . . . ? C1 C2 C3 N2 72.6(6) . . . . ? C1 C2 C3 C4 -49.0(6) . . . . ? N2 C3 C4 C5 -70.3(6) . . . . ? C2 C3 C4 C5 52.9(6) . . . . ? C25 N3 C5 C6 -118.2(5) . . . . ? Ni1 N3 C5 C6 62.1(5) . . . . ? C25 N3 C5 C4 119.6(5) . . . . ? Ni1 N3 C5 C4 -60.1(5) . . . . ? C3 C4 C5 N3 66.7(6) . . . . ? C3 C4 C5 C6 -54.6(6) . . . . ? N3 C5 C6 C1 -70.1(6) . . . . ? C4 C5 C6 C1 52.2(6) . . . . ? N1 C1 C6 C5 71.4(6) . . . . ? C2 C1 C6 C5 -49.4(6) . . . . ? C1 N1 C7 C8 171.4(5) . . . . ? Ni1 N1 C7 C8 -8.1(8) . . . . ? N1 C7 C8 C9 -166.8(5) . . . . ? C7 C8 C9 C10 170.5(5) . . . . ? C8 C9 C10 C11 -170.9(6) . . . . ? C8 C9 C10 C15 7.8(9) . . . . ? C15 C10 C11 C12 -1.1(10) . . . . ? C9 C10 C11 C12 177.7(7) . . . . ? C10 C11 C12 C13 1.3(14) . . . . ? C11 C12 C13 C14 0.4(15) . . . . ? C12 C13 C14 C15 -2.2(14) . . . . ? C13 C14 C15 C10 2.4(12) . . . . ? C11 C10 C15 C14 -0.8(10) . . . . ? C9 C10 C15 C14 -179.4(7) . . . . ? C3 N2 C16 C17 175.0(6) . . . . ? Ni1 N2 C16 C17 3.7(10) . . . . ? N2 C16 C17 C18 -175.4(7) . . . . ? C16 C17 C18 C19 -179.4(6) . . . . ? C17 C18 C19 C24 -6.1(12) . . . . ? C17 C18 C19 C20 174.3(7) . . . . ? C24 C19 C20 C21 0.8(13) . . . . ? C18 C19 C20 C21 -179.6(8) . . . . ? C19 C20 C21 C22 -0.8(16) . . . . ? C20 C21 C22 C23 2.4(17) . . . . ? C21 C22 C23 C24 -3.9(16) . . . . ? C22 C23 C24 C19 3.9(14) . . . . ? C20 C19 C24 C23 -2.2(12) . . . . ? C18 C19 C24 C23 178.2(7) . . . . ? C5 N3 C25 C26 178.9(5) . . . . ? Ni1 N3 C25 C26 -1.5(8) . . . . ? N3 C25 C26 C27 176.7(5) . . . . ? C25 C26 C27 C28 178.7(5) . . . . ? C26 C27 C28 C33 -5.9(10) . . . . ? C26 C27 C28 C29 174.4(6) . . . . ? C33 C28 C29 C30 1.8(9) . . . . ? C27 C28 C29 C30 -178.4(6) . . . . ? C28 C29 C30 C31 -4.0(11) . . . . ? C29 C30 C31 C32 3.7(13) . . . . ? C30 C31 C32 C33 -1.1(12) . . . . ? C29 C28 C33 C32 0.7(10) . . . . ? C27 C28 C33 C32 -179.1(6) . . . . ? C31 C32 C33 C28 -1.1(11) . . . . ? C39 C34 C35 C36 0.6(8) . . . . ? B1 C34 C35 C36 179.9(5) . . . . ? C34 C35 C36 C37 0.1(10) . . . . ? C35 C36 C37 C38 0.1(10) . . . . ? C36 C37 C38 C39 -1.0(10) . . . . ? C35 C34 C39 C38 -1.5(8) . . . . ? B1 C34 C39 C38 179.1(5) . . . . ? C37 C38 C39 C34 1.8(9) . . . . ? C45 C40 C41 C42 -5.5(11) . . . . ? B1 C40 C41 C42 175.3(7) . . . . ? C40 C41 C42 C43 4.7(14) . . . . ? C41 C42 C43 C44 0.9(14) . . . . ? C42 C43 C44 C45 -5.2(13) . . . . ? C43 C44 C45 C40 4.3(11) . . . . ? C41 C40 C45 C44 1.1(10) . . . . ? B1 C40 C45 C44 -179.8(6) . . . . ? C51 C46 C47 C48 -3.1(9) . . . . ? B1 C46 C47 C48 179.5(6) . . . . ? C46 C47 C48 C49 0.8(11) . . . . ? C47 C48 C49 C50 1.8(11) . . . . ? C48 C49 C50 C51 -1.9(11) . . . . ? C47 C46 C51 C50 3.0(8) . . . . ? B1 C46 C51 C50 -179.6(5) . . . . ? C49 C50 C51 C46 -0.6(9) . . . . ? C57 C52 C53 C54 1.8(7) . . . . ? B1 C52 C53 C54 -174.4(5) . . . . ? C52 C53 C54 C55 -1.5(8) . . . . ? C53 C54 C55 C56 0.9(9) . . . . ? C54 C55 C56 C57 -0.9(9) . . . . ? C55 C56 C57 C52 1.4(8) . . . . ? C53 C52 C57 C56 -1.8(7) . . . . ? B1 C52 C57 C56 174.2(5) . . . . ? C35 C34 B1 C40 -10.1(7) . . . . ? C39 C34 B1 C40 169.2(5) . . . . ? C35 C34 B1 C52 109.9(6) . . . . ? C39 C34 B1 C52 -70.8(6) . . . . ? C35 C34 B1 C46 -132.5(5) . . . . ? C39 C34 B1 C46 46.8(6) . . . . ? C45 C40 B1 C34 -95.7(7) . . . . ? C41 C40 B1 C34 83.4(7) . . . . ? C45 C40 B1 C52 142.5(6) . . . . ? C41 C40 B1 C52 -38.4(7) . . . . ? C45 C40 B1 C46 23.8(8) . . . . ? C41 C40 B1 C46 -157.1(6) . . . . ? C57 C52 B1 C34 18.6(7) . . . . ? C53 C52 B1 C34 -165.6(4) . . . . ? C57 C52 B1 C40 139.5(5) . . . . ? C53 C52 B1 C40 -44.8(6) . . . . ? C57 C52 B1 C46 -98.9(6) . . . . ? C53 C52 B1 C46 76.8(6) . . . . ? C51 C46 B1 C34 -120.4(5) . . . . ? C47 C46 B1 C34 56.7(6) . . . . ? C51 C46 B1 C40 118.7(5) . . . . ? C47 C46 B1 C40 -64.1(6) . . . . ? C51 C46 B1 C52 -0.4(7) . . . . ? C47 C46 B1 C52 176.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.804 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.804 _refine_diff_density_max 0.376 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.074 #===END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis,cis-1,3,5-(E,E)-tri(phenyl-propenylideneamino)cyclohexane zinc(II) chloride tetraphenylborate, (3) {tri(phenyl-propenylideneamino)cyclohexane = (Ph-protach)} ; _chemical_name_common '[Zn(Ph-protach)(Cl)]BPh4, (3)' _chemical_melting_point 509-510 _chemical_formula_moiety 'C33 H33 Cl N3 Zn 1+, C24 H20 B 1-, 3(C H2 Cl2)' _chemical_formula_sum 'C60 H59 B Cl7 N3 Zn' _chemical_formula_weight 1146.43 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.222(10) _cell_length_b 19.097(9) _cell_length_c 10.784(10) _cell_angle_alpha 99.61(6) _cell_angle_beta 103.87(7) _cell_angle_gamma 76.73(4) _cell_volume 2941(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.7 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method ? _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; Crystal mounted with mother liquor in a Lindemann tube ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_source_current 30 _diffrn_source_voltage 50 _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -1 4 0 -4 3 1 -3 3 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.186 _diffrn_reflns_number 9459 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.06 _reflns_number_total 9028 _reflns_number_gt 5460 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'AFC/MSC (Diffractometer Control)' _computing_cell_refinement 'AFC/MSC (Diffractometer Control)' _computing_data_reduction 'teXsan (Molecular Structure Corporation, 1992)' _computing_structure_solution 'SAPI91 (Rigaku Corporation, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics teXsan _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1117P)^2^+5.0561P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9028 _refine_ls_number_parameters 649 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1414 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2276 _refine_ls_wR_factor_gt 0.1853 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.26572(5) 0.18846(4) 0.39513(7) 0.0536(3) Uani 1 1 d . . . C59 C 0.3022(15) 0.4164(9) 0.307(2) 0.283(12) Uani 1 1 d D . . H59A H 0.3540 0.3761 0.3036 0.340 Uiso 1 1 calc R . . H59B H 0.2994 0.4502 0.2473 0.340 Uiso 1 1 calc R . . Cl2 Cl 0.1882(4) 0.3888(3) 0.2960(8) 0.288(3) Uani 1 1 d D . . Cl5 Cl 0.5752(7) 0.3939(4) 0.4288(7) 0.365(5) Uani 1 1 d D . . Cl4 Cl 0.5961(7) 0.4013(4) 0.6884(6) 0.366(5) Uani 1 1 d D . . Cl1 Cl 0.39582(11) 0.22462(10) 0.48032(18) 0.0769(5) Uani 1 1 d . . . Cl6 Cl 0.9585(4) 0.4297(3) 0.3443(6) 0.233(2) Uani 1 1 d D . . Cl7 Cl 0.8263(3) 0.3494(2) 0.3405(4) 0.1984(17) Uani 1 1 d D . . N1 N 0.2116(3) 0.1898(3) 0.2042(5) 0.0567(13) Uani 1 1 d . . . N2 N 0.1461(3) 0.2320(3) 0.4576(5) 0.0508(12) Uani 1 1 d . . . N3 N 0.2505(3) 0.0862(3) 0.4038(5) 0.0579(13) Uani 1 1 d . . . C1 C 0.9257(4) 0.2783(3) 0.7981(5) 0.0479(14) Uani 1 1 d . . . C2 C 0.9701(5) 0.3072(4) 0.9181(6) 0.0661(18) Uani 1 1 d . . . H2 H 0.9917 0.2770 0.9828 0.079 Uiso 1 1 calc R . . C3 C 0.9840(6) 0.3773(4) 0.9474(8) 0.082(2) Uani 1 1 d . . . H3 H 1.0127 0.3938 1.0298 0.098 Uiso 1 1 calc R . . C4 C 0.9548(6) 0.4221(4) 0.8529(9) 0.087(2) Uani 1 1 d . . . H4 H 0.9643 0.4694 0.8707 0.105 Uiso 1 1 calc R . . C5 C 0.9118(6) 0.3974(4) 0.7322(9) 0.088(2) Uani 1 1 d . . . H5 H 0.8921 0.4279 0.6680 0.105 Uiso 1 1 calc R . . C6 C 0.8974(5) 0.3265(3) 0.7058(7) 0.0657(17) Uani 1 1 d . . . H6 H 0.8677 0.3107 0.6234 0.079 Uiso 1 1 calc R . . C7 C 0.7562(6) 0.1831(4) 0.4169(6) 0.078(2) Uani 1 1 d . . . H7 H 0.7629 0.1861 0.3346 0.094 Uiso 1 1 calc R . . C8 C 0.7390(4) 0.1768(4) 0.6605(6) 0.0608(16) Uani 1 1 d . . . H8 H 0.7309 0.1746 0.7424 0.073 Uiso 1 1 calc R . . C9 C 0.8249(4) 0.1834(3) 0.6470(5) 0.0482(14) Uani 1 1 d . . . C10 C 0.8314(5) 0.1842(4) 0.5198(6) 0.0656(17) Uani 1 1 d . . . H10 H 0.8882 0.1856 0.5035 0.079 Uiso 1 1 calc R . . C11 C 0.8322(4) 0.2169(3) 0.9710(6) 0.0582(16) Uani 1 1 d . . . H11 H 0.8107 0.2645 0.9523 0.070 Uiso 1 1 calc R . . C12 C 0.8898(4) 0.1697(3) 0.8966(5) 0.0454(13) Uani 1 1 d . . . C13 C 0.9189(4) 0.0999(3) 0.9341(5) 0.0502(14) Uani 1 1 d . . . H13 H 0.9578 0.0659 0.8889 0.060 Uiso 1 1 calc R . . C14 C 0.8369(4) 0.1264(4) 1.1040(6) 0.0617(17) Uani 1 1 d . . . H14 H 0.8197 0.1127 1.1722 0.074 Uiso 1 1 calc R . . C15 C 0.8933(4) 0.0783(3) 1.0345(6) 0.0566(15) Uani 1 1 d . . . H15 H 0.9146 0.0310 1.0545 0.068 Uiso 1 1 calc R . . C16 C 0.8058(5) 0.1961(4) 1.0705(6) 0.0672(18) Uani 1 1 d . . . H16 H 0.7665 0.2293 1.1160 0.081 Uiso 1 1 calc R . . C17 C 1.0098(4) 0.0680(3) 0.6770(6) 0.0551(15) Uani 1 1 d . . . H17 H 0.9537 0.0532 0.6449 0.066 Uiso 1 1 calc R . . C18 C 1.0085(4) 0.1398(3) 0.7375(5) 0.0455(13) Uani 1 1 d . . . C19 C 1.0947(4) 0.1587(3) 0.7735(5) 0.0538(15) Uani 1 1 d . . . H19 H 1.0985 0.2060 0.8089 0.065 Uiso 1 1 calc R . . C20 C 1.1760(4) 0.1092(4) 0.7585(6) 0.0670(18) Uani 1 1 d . . . H20 H 1.2324 0.1240 0.7846 0.080 Uiso 1 1 calc R . . C21 C 1.1731(5) 0.0388(4) 0.7056(6) 0.0639(18) Uani 1 1 d . . . H21 H 1.2273 0.0054 0.6988 0.077 Uiso 1 1 calc R . . C22 C 1.0892(4) 0.0189(3) 0.6633(6) 0.0585(16) Uani 1 1 d . . . H22 H 1.0859 -0.0280 0.6249 0.070 Uiso 1 1 calc R . . C23 C 0.6719(6) 0.1775(4) 0.4359(7) 0.077(2) Uani 1 1 d . . . H23 H 0.6215 0.1766 0.3674 0.093 Uiso 1 1 calc R . . C24 C 0.6644(5) 0.1734(4) 0.5574(8) 0.079(2) Uani 1 1 d . . . H24 H 0.6085 0.1682 0.5718 0.095 Uiso 1 1 calc R . . C25 C 0.1596(4) 0.0712(4) 0.3307(6) 0.0602(16) Uani 1 1 d . . . H25 H 0.1587 0.0204 0.3340 0.072 Uiso 1 1 calc R . . C26 C 0.1428(4) 0.0835(3) 0.1920(6) 0.0639(17) Uani 1 1 d . . . H26A H 0.0908 0.0621 0.1443 0.077 Uiso 1 1 calc R . . H26B H 0.1965 0.0579 0.1580 0.077 Uiso 1 1 calc R . . C27 C 0.0838(4) 0.1193(3) 0.3952(6) 0.0598(17) Uani 1 1 d . . . H27A H 0.0265 0.1023 0.3593 0.072 Uiso 1 1 calc R . . H27B H 0.0999 0.1140 0.4863 0.072 Uiso 1 1 calc R . . C28 C 0.0678(4) 0.1994(3) 0.3796(6) 0.0574(16) Uani 1 1 d . . . H28 H 0.0120 0.2243 0.4110 0.069 Uiso 1 1 calc R . . C29 C 0.0522(4) 0.2104(3) 0.2379(6) 0.0582(16) Uani 1 1 d . . . H29A H -0.0083 0.2012 0.1941 0.070 Uiso 1 1 calc R . . H29B H 0.0523 0.2606 0.2329 0.070 Uiso 1 1 calc R . . C30 C 0.1235(4) 0.1624(4) 0.1673(6) 0.0596(16) Uani 1 1 d . . . H30 H 0.0997 0.1645 0.0748 0.072 Uiso 1 1 calc R . . C31 C 0.2406(5) 0.2071(4) 0.1130(6) 0.0674(18) Uani 1 1 d . . . H31 H 0.2032 0.2032 0.0312 0.081 Uiso 1 1 calc R . . C32 C 0.3240(5) 0.2315(4) 0.1244(7) 0.0692(18) Uani 1 1 d . . . H32 H 0.3616 0.2402 0.2049 0.083 Uiso 1 1 calc R . . C33 C 0.3479(5) 0.2420(4) 0.0176(8) 0.079(2) Uani 1 1 d . . . H33 H 0.3054 0.2346 -0.0588 0.095 Uiso 1 1 calc R . . C34 C 0.4302(6) 0.2629(4) 0.0049(9) 0.086(2) Uani 1 1 d . . . C35 C 0.4501(7) 0.2541(5) -0.1177(10) 0.109(3) Uani 1 1 d . . . H35 H 0.4116 0.2338 -0.1883 0.131 Uiso 1 1 calc R . . C36 C 0.4879(6) 0.2908(6) 0.1060(11) 0.112(3) Uani 1 1 d . . . H36 H 0.4760 0.2956 0.1880 0.134 Uiso 1 1 calc R . . C37 C 0.1322(4) 0.2774(4) 0.5556(6) 0.0618(16) Uani 1 1 d . . . H37 H 0.0742 0.2862 0.5755 0.074 Uiso 1 1 calc R . . C38 C 0.1994(5) 0.3157(4) 0.6371(6) 0.0661(17) Uani 1 1 d . . . H38 H 0.2580 0.3074 0.6191 0.079 Uiso 1 1 calc R . . C39 C 0.1809(5) 0.3621(4) 0.7367(7) 0.0730(19) Uani 1 1 d . . . H39 H 0.1236 0.3655 0.7558 0.088 Uiso 1 1 calc R . . C40 C 0.2402(5) 0.4093(4) 0.8213(7) 0.077(2) Uani 1 1 d . . . C41 C 0.3226(6) 0.4156(4) 0.7967(8) 0.090(2) Uani 1 1 d . . . H41 H 0.3430 0.3881 0.7256 0.108 Uiso 1 1 calc R . . C42 C 0.3756(7) 0.4620(6) 0.8754(12) 0.121(3) Uani 1 1 d . . . H42 H 0.4304 0.4664 0.8565 0.145 Uiso 1 1 calc R . . C43 C 0.3471(8) 0.5009(6) 0.9803(12) 0.124(4) Uani 1 1 d . . . H43 H 0.3835 0.5313 1.0345 0.148 Uiso 1 1 calc R . . C44 C 0.2675(9) 0.4963(6) 1.0074(10) 0.132(4) Uani 1 1 d . . . H44 H 0.2482 0.5242 1.0790 0.159 Uiso 1 1 calc R . . C45 C 0.2135(6) 0.4498(5) 0.9286(8) 0.103(3) Uani 1 1 d . . . H45 H 0.1588 0.4461 0.9488 0.123 Uiso 1 1 calc R . . C46 C 0.3035(4) 0.0371(4) 0.4714(6) 0.0593(16) Uani 1 1 d . . . H46 H 0.2859 -0.0073 0.4620 0.071 Uiso 1 1 calc R . . C47 C 0.3880(4) 0.0466(4) 0.5601(6) 0.0625(17) Uani 1 1 d . . . H47 H 0.4122 0.0871 0.5603 0.075 Uiso 1 1 calc R . . C48 C 0.4328(4) -0.0013(3) 0.6423(7) 0.0644(17) Uani 1 1 d . . . H48 H 0.4107 -0.0440 0.6313 0.077 Uiso 1 1 calc R . . C49 C 0.5121(4) 0.0054(4) 0.7475(6) 0.0604(16) Uani 1 1 d . . . C50 C 0.5406(5) -0.0443(4) 0.8364(8) 0.081(2) Uani 1 1 d . . . H50 H 0.5115 -0.0836 0.8234 0.097 Uiso 1 1 calc R . . C51 C 0.5591(5) 0.0619(4) 0.7693(7) 0.081(2) Uani 1 1 d . . . H51 H 0.5429 0.0958 0.7109 0.097 Uiso 1 1 calc R . . C52 C 0.6293(6) 0.0689(5) 0.8752(8) 0.093(3) Uani 1 1 d . . . H52 H 0.6600 0.1072 0.8879 0.112 Uiso 1 1 calc R . . C53 C 0.6536(5) 0.0198(5) 0.9610(8) 0.087(2) Uani 1 1 d . . . H53 H 0.7004 0.0255 1.0330 0.104 Uiso 1 1 calc R . . C54 C 0.6111(5) -0.0377(5) 0.9444(8) 0.083(2) Uani 1 1 d . . . H54 H 0.6287 -0.0714 1.0033 0.100 Uiso 1 1 calc R . . C55 C 0.5265(10) 0.2755(7) -0.1332(15) 0.144(5) Uani 1 1 d . . . H55 H 0.5392 0.2706 -0.2147 0.173 Uiso 1 1 calc R . . C56 C 0.5846(8) 0.3044(8) -0.0277(19) 0.153(6) Uani 1 1 d . . . H56 H 0.6370 0.3181 -0.0383 0.183 Uiso 1 1 calc R . . C57 C 0.5657(8) 0.3127(7) 0.0894(14) 0.147(5) Uani 1 1 d . . . H57 H 0.6043 0.3331 0.1599 0.177 Uiso 1 1 calc R . . C58 C 0.625(2) 0.3642(8) 0.5681(15) 0.339(18) Uani 1 1 d D . . H58A H 0.6189 0.3142 0.5603 0.407 Uiso 1 1 calc R . . H58B H 0.6907 0.3636 0.5806 0.407 Uiso 1 1 calc R . . Cl3 Cl 0.2924(9) 0.4576(6) 0.4646(11) 0.449(7) Uani 1 1 d D . . C60 C 0.8563(10) 0.3994(9) 0.2627(16) 0.215(8) Uani 1 1 d D . . H60A H 0.8068 0.4411 0.2459 0.258 Uiso 1 1 calc R . . H60B H 0.8655 0.3728 0.1804 0.258 Uiso 1 1 calc R . . B1 B 0.9126(5) 0.1936(4) 0.7695(6) 0.0480(16) Uani 1 1 d . . . 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 Zn1 0.0427(4) 0.0631(5) 0.0556(4) 0.0090(3) 0.0029(3) -0.0182(3) C59 0.30(3) 0.139(14) 0.35(3) -0.079(17) 0.08(2) 0.006(15) Cl2 0.221(5) 0.151(4) 0.482(11) 0.061(5) 0.044(6) -0.033(4) Cl5 0.474(13) 0.325(9) 0.236(7) -0.004(6) 0.076(8) 0.018(8) Cl4 0.658(16) 0.298(8) 0.213(6) -0.020(5) 0.222(8) -0.137(9) Cl1 0.0493(9) 0.0899(13) 0.0911(13) 0.0141(10) -0.0044(9) -0.0309(9) Cl6 0.188(4) 0.204(5) 0.306(6) 0.038(4) 0.022(4) -0.063(4) Cl7 0.240(5) 0.177(4) 0.187(4) 0.021(3) 0.044(3) -0.059(3) N1 0.051(3) 0.066(3) 0.056(3) 0.010(3) 0.011(2) -0.016(3) N2 0.047(3) 0.057(3) 0.047(3) 0.008(2) 0.003(2) -0.013(2) N3 0.045(3) 0.067(3) 0.062(3) 0.011(3) 0.006(2) -0.015(3) C1 0.044(3) 0.051(3) 0.050(3) 0.007(3) 0.013(3) -0.007(3) C2 0.083(5) 0.060(4) 0.055(4) 0.003(3) 0.008(3) -0.022(4) C3 0.106(6) 0.065(5) 0.076(5) -0.014(4) 0.019(4) -0.033(4) C4 0.093(6) 0.055(5) 0.115(7) -0.001(5) 0.026(5) -0.023(4) C5 0.104(6) 0.065(5) 0.099(6) 0.032(4) 0.013(5) -0.017(4) C6 0.075(5) 0.054(4) 0.066(4) 0.013(3) 0.006(3) -0.012(3) C7 0.105(6) 0.081(5) 0.041(4) 0.000(3) 0.010(4) -0.014(5) C8 0.052(4) 0.075(4) 0.058(4) 0.016(3) 0.006(3) -0.019(3) C9 0.053(4) 0.048(3) 0.044(3) 0.009(3) 0.011(3) -0.007(3) C10 0.064(4) 0.077(5) 0.056(4) 0.002(3) 0.019(3) -0.012(3) C11 0.061(4) 0.057(4) 0.055(4) 0.013(3) 0.018(3) 0.002(3) C12 0.043(3) 0.055(4) 0.039(3) 0.008(3) 0.008(2) -0.009(3) C13 0.049(3) 0.057(4) 0.046(3) 0.005(3) 0.014(3) -0.008(3) C14 0.062(4) 0.078(5) 0.051(4) 0.016(3) 0.015(3) -0.016(4) C15 0.063(4) 0.059(4) 0.051(4) 0.009(3) 0.012(3) -0.015(3) C16 0.069(4) 0.077(5) 0.057(4) 0.004(3) 0.030(3) -0.001(4) C17 0.062(4) 0.057(4) 0.055(4) 0.003(3) 0.027(3) -0.017(3) C18 0.048(3) 0.052(3) 0.039(3) 0.008(3) 0.013(3) -0.010(3) C19 0.049(4) 0.061(4) 0.048(3) 0.006(3) 0.006(3) -0.009(3) C20 0.046(4) 0.092(5) 0.056(4) 0.007(4) 0.005(3) -0.007(4) C21 0.061(4) 0.070(5) 0.055(4) 0.013(3) 0.023(3) 0.011(4) C22 0.064(4) 0.056(4) 0.059(4) 0.009(3) 0.030(3) 0.000(3) C23 0.081(5) 0.075(5) 0.064(5) 0.010(4) -0.009(4) -0.017(4) C24 0.061(4) 0.092(6) 0.085(6) 0.020(4) -0.001(4) -0.027(4) C25 0.050(4) 0.062(4) 0.068(4) 0.014(3) -0.006(3) -0.024(3) C26 0.053(4) 0.066(4) 0.071(4) 0.001(3) 0.002(3) -0.023(3) C27 0.045(3) 0.068(4) 0.073(4) 0.023(3) 0.004(3) -0.022(3) C28 0.041(3) 0.072(4) 0.062(4) 0.010(3) 0.008(3) -0.018(3) C29 0.045(3) 0.061(4) 0.066(4) 0.016(3) -0.002(3) -0.013(3) C30 0.052(4) 0.079(5) 0.048(3) 0.011(3) -0.002(3) -0.026(3) C31 0.067(4) 0.081(5) 0.057(4) 0.013(3) 0.005(3) -0.025(4) C32 0.069(4) 0.079(5) 0.067(4) 0.013(4) 0.017(4) -0.022(4) C33 0.081(5) 0.087(5) 0.078(5) 0.017(4) 0.024(4) -0.020(4) C34 0.080(6) 0.084(6) 0.102(6) 0.023(5) 0.035(5) -0.012(4) C35 0.124(8) 0.106(7) 0.122(8) 0.032(6) 0.073(7) -0.008(6) C36 0.088(6) 0.140(9) 0.124(8) 0.032(7) 0.028(6) -0.039(6) C37 0.054(4) 0.069(4) 0.062(4) 0.008(3) 0.011(3) -0.014(3) C38 0.063(4) 0.070(4) 0.064(4) -0.001(4) 0.014(3) -0.015(3) C39 0.076(5) 0.072(5) 0.070(5) -0.004(4) 0.017(4) -0.021(4) C40 0.079(5) 0.078(5) 0.070(5) -0.006(4) 0.010(4) -0.022(4) C41 0.076(5) 0.087(6) 0.101(6) -0.009(5) 0.015(5) -0.020(5) C42 0.084(6) 0.110(8) 0.155(10) -0.026(7) 0.019(6) -0.029(6) C43 0.096(7) 0.110(8) 0.147(10) -0.022(7) -0.002(7) -0.042(6) C44 0.136(9) 0.133(9) 0.110(8) -0.056(7) 0.020(7) -0.047(8) C45 0.097(6) 0.123(7) 0.081(6) -0.027(5) 0.019(5) -0.036(6) C46 0.053(4) 0.061(4) 0.064(4) 0.009(3) 0.008(3) -0.016(3) C47 0.047(4) 0.061(4) 0.080(5) 0.013(3) 0.010(3) -0.011(3) C48 0.051(4) 0.054(4) 0.083(5) 0.014(3) 0.009(3) -0.003(3) C49 0.048(4) 0.063(4) 0.065(4) 0.013(3) 0.005(3) -0.002(3) C50 0.072(5) 0.072(5) 0.093(6) 0.025(4) 0.003(4) -0.008(4) C51 0.075(5) 0.079(5) 0.086(5) 0.029(4) -0.004(4) -0.019(4) C52 0.081(5) 0.103(6) 0.095(6) 0.029(5) -0.012(5) -0.035(5) C53 0.068(5) 0.098(6) 0.080(5) 0.009(5) -0.001(4) -0.006(5) C54 0.073(5) 0.087(6) 0.083(5) 0.032(4) 0.001(4) -0.001(4) C55 0.128(10) 0.136(10) 0.199(15) 0.071(10) 0.107(11) 0.022(8) C56 0.072(7) 0.148(11) 0.27(2) 0.101(13) 0.075(10) 0.008(7) C57 0.092(8) 0.198(13) 0.171(12) 0.060(10) 0.045(8) -0.024(8) C58 0.71(5) 0.128(12) 0.119(12) 0.017(10) 0.10(2) 0.04(2) Cl3 0.584(19) 0.308(10) 0.404(13) 0.132(9) -0.042(13) -0.071(11) C60 0.154(13) 0.267(19) 0.244(18) 0.167(16) 0.002(12) -0.025(13) B1 0.048(4) 0.050(4) 0.047(4) 0.008(3) 0.013(3) -0.006(3) _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 Zn1 N1 2.028(5) . ? Zn1 N3 2.039(5) . ? Zn1 N2 2.041(5) . ? Zn1 Cl1 2.188(2) . ? C59 Cl3 1.779(18) . ? C59 Cl2 1.90(2) . ? Cl5 C58 1.643(16) . ? Cl4 C58 1.486(16) . ? Cl6 C60 1.765(14) . ? Cl7 C60 1.573(13) . ? N1 C31 1.287(8) . ? N1 C30 1.492(7) . ? N2 C37 1.277(8) . ? N2 C28 1.484(7) . ? N3 C46 1.288(8) . ? N3 C25 1.483(7) . ? C1 C6 1.394(8) . ? C1 C2 1.396(8) . ? C1 B1 1.645(9) . ? C2 C3 1.375(9) . ? C3 C4 1.366(11) . ? C4 C5 1.369(11) . ? C5 C6 1.392(9) . ? C7 C23 1.376(10) . ? C7 C10 1.392(9) . ? C8 C9 1.386(8) . ? C8 C24 1.391(9) . ? C9 C10 1.402(8) . ? C9 B1 1.659(9) . ? C11 C16 1.376(8) . ? C11 C12 1.399(8) . ? C12 C13 1.401(8) . ? C12 B1 1.647(8) . ? C13 C15 1.385(8) . ? C14 C15 1.364(9) . ? C14 C16 1.383(9) . ? C17 C22 1.371(8) . ? C17 C18 1.416(8) . ? C18 C19 1.388(8) . ? C18 B1 1.656(9) . ? C19 C20 1.400(9) . ? C20 C21 1.375(9) . ? C21 C22 1.368(9) . ? C23 C24 1.359(10) . ? C25 C26 1.505(9) . ? C25 C27 1.532(9) . ? C26 C30 1.523(9) . ? C27 C28 1.525(8) . ? C28 C29 1.532(8) . ? C29 C30 1.518(9) . ? C31 C32 1.422(9) . ? C32 C33 1.346(9) . ? C33 C34 1.441(10) . ? C34 C36 1.344(12) . ? C34 C35 1.400(11) . ? C35 C55 1.371(14) . ? C36 C57 1.402(14) . ? C37 C38 1.432(9) . ? C38 C39 1.316(9) . ? C39 C40 1.471(9) . ? C40 C45 1.373(10) . ? C40 C41 1.377(11) . ? C41 C42 1.379(11) . ? C42 C43 1.350(13) . ? C43 C44 1.338(14) . ? C44 C45 1.391(12) . ? C46 C47 1.436(9) . ? C47 C48 1.334(9) . ? C48 C49 1.458(9) . ? C49 C51 1.387(9) . ? C49 C50 1.387(9) . ? C50 C54 1.392(10) . ? C51 C52 1.376(10) . ? C52 C53 1.356(11) . ? C53 C54 1.365(11) . ? C55 C56 1.383(18) . ? C56 C57 1.338(17) . ? 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 Zn1 N3 96.3(2) . . ? N1 Zn1 N2 97.1(2) . . ? N3 Zn1 N2 91.1(2) . . ? N1 Zn1 Cl1 120.20(16) . . ? N3 Zn1 Cl1 121.81(16) . . ? N2 Zn1 Cl1 123.23(15) . . ? Cl3 C59 Cl2 86.2(11) . . ? C31 N1 C30 116.8(5) . . ? C31 N1 Zn1 132.1(4) . . ? C30 N1 Zn1 111.0(4) . . ? C37 N2 C28 118.1(5) . . ? C37 N2 Zn1 129.7(4) . . ? C28 N2 Zn1 112.0(4) . . ? C46 N3 C25 117.2(5) . . ? C46 N3 Zn1 129.6(4) . . ? C25 N3 Zn1 112.8(4) . . ? C6 C1 C2 114.2(6) . . ? C6 C1 B1 123.9(5) . . ? C2 C1 B1 121.9(5) . . ? C3 C2 C1 124.5(7) . . ? C4 C3 C2 118.7(7) . . ? C3 C4 C5 120.2(7) . . ? C4 C5 C6 119.9(7) . . ? C5 C6 C1 122.5(7) . . ? C23 C7 C10 120.5(7) . . ? C9 C8 C24 123.2(6) . . ? C8 C9 C10 114.3(6) . . ? C8 C9 B1 123.9(5) . . ? C10 C9 B1 121.7(5) . . ? C7 C10 C9 122.7(6) . . ? C16 C11 C12 122.9(6) . . ? C11 C12 C13 113.7(5) . . ? C11 C12 B1 122.0(5) . . ? C13 C12 B1 124.0(5) . . ? C15 C13 C12 124.0(5) . . ? C15 C14 C16 118.3(6) . . ? C14 C15 C13 120.0(6) . . ? C11 C16 C14 121.1(6) . . ? C22 C17 C18 123.6(6) . . ? C19 C18 C17 114.1(5) . . ? C19 C18 B1 124.0(5) . . ? C17 C18 B1 121.8(5) . . ? C18 C19 C20 122.5(6) . . ? C21 C20 C19 120.5(6) . . ? C22 C21 C20 118.8(6) . . ? C21 C22 C17 120.3(6) . . ? C24 C23 C7 118.3(7) . . ? C23 C24 C8 120.9(7) . . ? N3 C25 C26 111.7(5) . . ? N3 C25 C27 108.9(5) . . ? C26 C25 C27 110.7(5) . . ? C25 C26 C30 115.5(5) . . ? C28 C27 C25 114.1(5) . . ? N2 C28 C27 110.8(5) . . ? N2 C28 C29 110.6(5) . . ? C27 C28 C29 111.0(5) . . ? C30 C29 C28 114.5(5) . . ? N1 C30 C29 110.3(5) . . ? N1 C30 C26 109.4(5) . . ? C29 C30 C26 112.8(5) . . ? N1 C31 C32 126.7(6) . . ? C33 C32 C31 119.3(7) . . ? C32 C33 C34 129.1(8) . . ? C36 C34 C35 119.1(9) . . ? C36 C34 C33 122.4(8) . . ? C35 C34 C33 118.5(9) . . ? C55 C35 C34 119.8(11) . . ? C34 C36 C57 120.8(11) . . ? N2 C37 C38 124.8(6) . . ? C39 C38 C37 122.0(7) . . ? C38 C39 C40 127.7(7) . . ? C45 C40 C41 117.6(7) . . ? C45 C40 C39 119.9(7) . . ? C41 C40 C39 122.5(7) . . ? C40 C41 C42 121.3(8) . . ? C43 C42 C41 119.4(10) . . ? C44 C43 C42 121.1(10) . . ? C43 C44 C45 120.0(10) . . ? C40 C45 C44 120.6(9) . . ? N3 C46 C47 124.3(6) . . ? C48 C47 C46 121.7(6) . . ? C47 C48 C49 127.7(6) . . ? C51 C49 C50 116.6(6) . . ? C51 C49 C48 123.5(6) . . ? C50 C49 C48 119.8(6) . . ? C49 C50 C54 122.5(7) . . ? C52 C51 C49 121.5(7) . . ? C53 C52 C51 119.8(8) . . ? C52 C53 C54 121.8(8) . . ? C53 C54 C50 117.8(7) . . ? C35 C55 C56 120.1(13) . . ? C57 C56 C55 120.1(12) . . ? C56 C57 C36 120.1(13) . . ? Cl4 C58 Cl5 121.0(14) . . ? Cl7 C60 Cl6 112.9(8) . . ? C1 B1 C12 109.8(5) . . ? C1 B1 C18 109.9(5) . . ? C12 B1 C18 108.9(5) . . ? C1 B1 C9 110.7(5) . . ? C12 B1 C9 107.8(5) . . ? C18 B1 C9 109.8(5) . . ? 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 N3 Zn1 N1 C31 -130.4(6) . . . . ? N2 Zn1 N1 C31 137.7(6) . . . . ? Cl1 Zn1 N1 C31 2.3(7) . . . . ? N3 Zn1 N1 C30 46.8(4) . . . . ? N2 Zn1 N1 C30 -45.1(4) . . . . ? Cl1 Zn1 N1 C30 179.5(3) . . . . ? N1 Zn1 N2 C37 -141.3(6) . . . . ? N3 Zn1 N2 C37 122.2(6) . . . . ? Cl1 Zn1 N2 C37 -7.8(6) . . . . ? N1 Zn1 N2 C28 44.3(4) . . . . ? N3 Zn1 N2 C28 -52.2(4) . . . . ? Cl1 Zn1 N2 C28 177.7(3) . . . . ? N1 Zn1 N3 C46 143.5(6) . . . . ? N2 Zn1 N3 C46 -119.2(6) . . . . ? Cl1 Zn1 N3 C46 11.9(6) . . . . ? N1 Zn1 N3 C25 -43.5(4) . . . . ? N2 Zn1 N3 C25 53.8(4) . . . . ? Cl1 Zn1 N3 C25 -175.1(3) . . . . ? C6 C1 C2 C3 1.5(10) . . . . ? B1 C1 C2 C3 179.2(7) . . . . ? C1 C2 C3 C4 -1.7(12) . . . . ? C2 C3 C4 C5 0.7(13) . . . . ? C3 C4 C5 C6 0.2(13) . . . . ? C4 C5 C6 C1 -0.3(12) . . . . ? C2 C1 C6 C5 -0.5(10) . . . . ? B1 C1 C6 C5 -178.2(6) . . . . ? C24 C8 C9 C10 -1.8(9) . . . . ? C24 C8 C9 B1 175.3(6) . . . . ? C23 C7 C10 C9 -3.2(11) . . . . ? C8 C9 C10 C7 3.8(9) . . . . ? B1 C9 C10 C7 -173.4(6) . . . . ? C16 C11 C12 C13 -0.8(9) . . . . ? C16 C11 C12 B1 174.1(6) . . . . ? C11 C12 C13 C15 0.4(8) . . . . ? B1 C12 C13 C15 -174.3(6) . . . . ? C16 C14 C15 C13 0.7(9) . . . . ? C12 C13 C15 C14 -0.4(9) . . . . ? C12 C11 C16 C14 1.1(10) . . . . ? C15 C14 C16 C11 -1.0(10) . . . . ? C22 C17 C18 C19 4.7(8) . . . . ? C22 C17 C18 B1 -171.6(5) . . . . ? C17 C18 C19 C20 -3.9(8) . . . . ? B1 C18 C19 C20 172.3(5) . . . . ? C18 C19 C20 C21 0.5(10) . . . . ? C19 C20 C21 C22 2.6(9) . . . . ? C20 C21 C22 C17 -1.9(9) . . . . ? C18 C17 C22 C21 -1.9(9) . . . . ? C10 C7 C23 C24 0.2(11) . . . . ? C7 C23 C24 C8 1.8(11) . . . . ? C9 C8 C24 C23 -1.0(11) . . . . ? C46 N3 C25 C26 -129.5(6) . . . . ? Zn1 N3 C25 C26 56.6(6) . . . . ? C46 N3 C25 C27 107.9(6) . . . . ? Zn1 N3 C25 C27 -66.0(5) . . . . ? N3 C25 C26 C30 -71.9(7) . . . . ? C27 C25 C26 C30 49.7(7) . . . . ? N3 C25 C27 C28 70.7(6) . . . . ? C26 C25 C27 C28 -52.5(7) . . . . ? C37 N2 C28 C27 -110.4(6) . . . . ? Zn1 N2 C28 C27 64.8(5) . . . . ? C37 N2 C28 C29 126.1(6) . . . . ? Zn1 N2 C28 C29 -58.7(5) . . . . ? C25 C27 C28 N2 -71.0(7) . . . . ? C25 C27 C28 C29 52.4(7) . . . . ? N2 C28 C29 C30 74.2(6) . . . . ? C27 C28 C29 C30 -49.3(7) . . . . ? C31 N1 C30 C29 -120.8(6) . . . . ? Zn1 N1 C30 C29 61.5(5) . . . . ? C31 N1 C30 C26 114.6(6) . . . . ? Zn1 N1 C30 C26 -63.1(5) . . . . ? C28 C29 C30 N1 -75.9(6) . . . . ? C28 C29 C30 C26 46.8(7) . . . . ? C25 C26 C30 N1 75.6(7) . . . . ? C25 C26 C30 C29 -47.6(7) . . . . ? C30 N1 C31 C32 -177.3(6) . . . . ? Zn1 N1 C31 C32 -0.2(11) . . . . ? N1 C31 C32 C33 174.8(7) . . . . ? C31 C32 C33 C34 -176.7(7) . . . . ? C32 C33 C34 C36 -15.1(14) . . . . ? C32 C33 C34 C35 165.3(8) . . . . ? C36 C34 C35 C55 -1.5(14) . . . . ? C33 C34 C35 C55 178.1(9) . . . . ? C35 C34 C36 C57 1.7(15) . . . . ? C33 C34 C36 C57 -177.9(9) . . . . ? C28 N2 C37 C38 -177.3(6) . . . . ? Zn1 N2 C37 C38 8.6(10) . . . . ? N2 C37 C38 C39 179.7(7) . . . . ? C37 C38 C39 C40 -174.4(7) . . . . ? C38 C39 C40 C45 -173.8(8) . . . . ? C38 C39 C40 C41 6.9(13) . . . . ? C45 C40 C41 C42 -1.3(14) . . . . ? C39 C40 C41 C42 178.0(8) . . . . ? C40 C41 C42 C43 1.4(16) . . . . ? C41 C42 C43 C44 -1.5(18) . . . . ? C42 C43 C44 C45 1.4(19) . . . . ? C41 C40 C45 C44 1.2(14) . . . . ? C39 C40 C45 C44 -178.1(9) . . . . ? C43 C44 C45 C40 -1.3(17) . . . . ? C25 N3 C46 C47 -171.7(6) . . . . ? Zn1 N3 C46 C47 1.0(10) . . . . ? N3 C46 C47 C48 169.2(7) . . . . ? C46 C47 C48 C49 -171.8(6) . . . . ? C47 C48 C49 C51 -6.7(11) . . . . ? C47 C48 C49 C50 169.5(7) . . . . ? C51 C49 C50 C54 1.6(11) . . . . ? C48 C49 C50 C54 -174.9(7) . . . . ? C50 C49 C51 C52 -1.2(11) . . . . ? C48 C49 C51 C52 175.1(7) . . . . ? C49 C51 C52 C53 -0.1(13) . . . . ? C51 C52 C53 C54 1.1(13) . . . . ? C52 C53 C54 C50 -0.7(12) . . . . ? C49 C50 C54 C53 -0.6(12) . . . . ? C34 C35 C55 C56 1.2(17) . . . . ? C35 C55 C56 C57 -1(2) . . . . ? C55 C56 C57 C36 1(2) . . . . ? C34 C36 C57 C56 -1.6(18) . . . . ? C6 C1 B1 C12 -144.3(6) . . . . ? C2 C1 B1 C12 38.2(7) . . . . ? C6 C1 B1 C18 96.0(7) . . . . ? C2 C1 B1 C18 -81.5(7) . . . . ? C6 C1 B1 C9 -25.5(8) . . . . ? C2 C1 B1 C9 157.1(6) . . . . ? C11 C12 B1 C1 39.2(7) . . . . ? C13 C12 B1 C1 -146.5(5) . . . . ? C11 C12 B1 C18 159.5(5) . . . . ? C13 C12 B1 C18 -26.1(7) . . . . ? C11 C12 B1 C9 -81.5(6) . . . . ? C13 C12 B1 C9 92.9(6) . . . . ? C19 C18 B1 C1 21.0(7) . . . . ? C17 C18 B1 C1 -163.0(5) . . . . ? C19 C18 B1 C12 -99.3(6) . . . . ? C17 C18 B1 C12 76.7(6) . . . . ? C19 C18 B1 C9 143.0(5) . . . . ? C17 C18 B1 C9 -41.1(7) . . . . ? C8 C9 B1 C1 -103.2(6) . . . . ? C10 C9 B1 C1 73.7(7) . . . . ? C8 C9 B1 C12 16.9(8) . . . . ? C10 C9 B1 C12 -166.2(5) . . . . ? C8 C9 B1 C18 135.3(6) . . . . ? C10 C9 B1 C18 -47.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.864 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.864 _refine_diff_density_max 0.560 _refine_diff_density_min -0.511 _refine_diff_density_rms 0.072 #===END data_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; cis,cis-1,3,5-(E,E)-tri(phenyl-propenylideneamino)cyclohexane cadmium(II) nitrate tetraphenylborate, (4) {tri(phenyl-propenylideneamino)cyclohexane = (Ph-protach)} ; _chemical_name_common '[Cd(Ph-protach)(NO3)(CH3OH)]BPh4, (4)' _chemical_melting_point '424-424.5 K' _chemical_formula_moiety 'C33 H33 Cd N3 2+, N O3 1-, C24 H20 B 1-, 2(C H4 O)' _chemical_formula_sum 'C59 H61 B Cd N4 O5' _chemical_formula_weight 1029.33 _publ_requested_journal 'test' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cd' 'Cd' -0.8075 1.2024 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.642(3) _cell_length_b 17.746(4) _cell_length_c 10.348(3) _cell_angle_alpha 99.861(19) _cell_angle_beta 105.154(17) _cell_angle_gamma 76.486(15) _cell_volume 2677.1(10) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.459 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7103 _exptl_absorpt_correction_T_max 0.8377 _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_special_details ; Crystal mounted with mother liquor in a Lindemann tube ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_source_current 30 _diffrn_source_voltage 50 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC6S' _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -4 3 4 -3 -1 -3 -6 2 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.3279 _diffrn_reflns_number 9800 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.02 _reflns_number_total 9427 _reflns_number_gt 7595 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'AFC/MSC (Diffractometer Control)' _computing_cell_refinement 'AFC/MSC (Diffractometer Control)' _computing_data_reduction 'teXsan (Molecular Structure Corporation, 1992)' _computing_structure_solution 'SAPI91 (Rigaku Corporation, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics teXsan _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+1.2060P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9427 _refine_ls_number_parameters 645 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0533 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0965 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.231712(14) 0.243041(13) 0.32522(2) 0.05246(8) Uani 1 1 d . . . O1 O 0.29224(17) 0.23313(15) 0.1372(2) 0.0769(6) Uani 1 1 d . . . O2 O 0.3488(2) 0.32229(17) 0.0902(3) 0.1005(9) Uani 1 1 d . . . O3 O 0.30299(16) 0.33694(15) 0.2738(2) 0.0769(6) Uani 1 1 d . . . O4 O 0.38508(14) 0.19123(14) 0.4311(2) 0.0726(6) Uani 1 1 d D . . H4 H 0.4261(10) 0.2038(3) 0.4125(5) 0.087 Uiso 1 1 d RD . . O5A O 0.5128(10) 0.1916(6) 0.295(3) 0.154(9) Uani 0.394(17) 1 d PD A 1 H5A H 0.4623 0.2141 0.3044 0.230 Uiso 0.394(17) 1 calc PR A 1 C59A C 0.5628(4) 0.2428(5) 0.3071(7) 0.174(3) Uani 0.394(17) 1 d PD A 1 H59A H 0.5250 0.2918 0.2839 0.261 Uiso 0.394(17) 1 calc PR A 1 H59B H 0.6034 0.2250 0.2480 0.261 Uiso 0.394(17) 1 calc PR A 1 H59C H 0.5970 0.2492 0.3986 0.261 Uiso 0.394(17) 1 calc PR A 1 O5B O 0.5403(4) 0.2251(6) 0.4089(10) 0.115(4) Uani 0.606(17) 1 d PD A 2 H5B H 0.5835 0.2234 0.4742 0.172 Uiso 0.606(17) 1 calc PR A 2 C59B C 0.5628(4) 0.2428(5) 0.3071(7) 0.174(3) Uani 0.606(17) 1 d PD A 2 H59D H 0.6165 0.2070 0.2915 0.261 Uiso 0.606(17) 1 calc PR A 2 H59E H 0.5740 0.2949 0.3265 0.261 Uiso 0.606(17) 1 calc PR A 2 H59F H 0.5145 0.2395 0.2283 0.261 Uiso 0.606(17) 1 calc PR A 2 N1 N 0.19618(16) 0.28414(14) 0.5286(2) 0.0544(6) Uani 1 1 d . . . N2 N 0.07801(15) 0.29370(14) 0.2393(3) 0.0567(6) Uani 1 1 d . . . N3 N 0.18909(16) 0.12868(14) 0.3187(2) 0.0539(6) Uani 1 1 d . . . N4 N 0.31636(16) 0.29621(16) 0.1698(3) 0.0584(6) Uani 1 1 d . . . C1 C 0.1145(2) 0.26069(18) 0.5433(3) 0.0590(7) Uani 1 1 d . . . H1 H 0.1088 0.2776 0.6365 0.071 Uiso 1 1 calc R . . C2 C 0.1230(2) 0.17221(18) 0.5188(3) 0.0618(8) Uani 1 1 d . . . H2A H 0.0800 0.1588 0.5594 0.074 Uiso 1 1 calc R . . H2B H 0.1830 0.1485 0.5659 0.074 Uiso 1 1 calc R . . C3 C 0.1077(2) 0.13544(18) 0.3717(3) 0.0590(7) Uani 1 1 d . . . H3 H 0.0978 0.0826 0.3689 0.071 Uiso 1 1 calc R . . C4 C 0.0243(2) 0.1805(2) 0.2820(4) 0.0670(8) Uani 1 1 d . . . H4A H 0.0254 0.1617 0.1886 0.080 Uiso 1 1 calc R . . H4B H -0.0290 0.1686 0.2985 0.080 Uiso 1 1 calc R . . C5 C 0.01518(19) 0.26880(19) 0.3011(3) 0.0615(8) Uani 1 1 d . . . H5 H -0.0466 0.2915 0.2560 0.074 Uiso 1 1 calc R . . C6 C 0.0297(2) 0.3018(2) 0.4507(3) 0.0643(8) Uani 1 1 d . . . H6A H 0.0325 0.3565 0.4584 0.077 Uiso 1 1 calc R . . H6B H -0.0225 0.2991 0.4824 0.077 Uiso 1 1 calc R . . C7 C 0.2393(2) 0.32496(18) 0.6276(3) 0.0613(8) Uani 1 1 d . . . H7 H 0.2202 0.3357 0.7079 0.074 Uiso 1 1 calc R . . C8 C 0.3160(2) 0.35514(18) 0.6214(3) 0.0618(8) Uani 1 1 d . . . H8 H 0.3375 0.3419 0.5432 0.074 Uiso 1 1 calc R . . C9 C 0.3571(2) 0.40079(19) 0.7217(3) 0.0663(8) Uani 1 1 d . . . H9 H 0.3358 0.4111 0.8002 0.080 Uiso 1 1 calc R . . C10 C 0.4322(2) 0.43653(19) 0.7224(3) 0.0646(8) Uani 1 1 d . . . C11 C 0.4864(2) 0.4106(2) 0.6300(4) 0.0786(10) Uani 1 1 d . . . H11 H 0.4748 0.3689 0.5648 0.094 Uiso 1 1 calc R . . C12 C 0.5567(3) 0.4455(3) 0.6331(4) 0.0924(12) Uani 1 1 d . . . H12 H 0.5929 0.4268 0.5715 0.111 Uiso 1 1 calc R . . C13 C 0.5735(3) 0.5081(3) 0.7273(5) 0.0950(13) Uani 1 1 d . . . H13 H 0.6204 0.5324 0.7284 0.114 Uiso 1 1 calc R . . C14 C 0.5215(3) 0.5346(2) 0.8193(5) 0.0989(13) Uani 1 1 d . . . H14 H 0.5333 0.5769 0.8833 0.119 Uiso 1 1 calc R . . C15 C 0.4517(3) 0.4994(2) 0.8182(4) 0.0861(11) Uani 1 1 d . . . H15 H 0.4171 0.5178 0.8820 0.103 Uiso 1 1 calc R . . C16 C 0.0434(2) 0.33199(18) 0.1376(3) 0.0591(7) Uani 1 1 d . . . H16 H -0.0181 0.3359 0.0996 0.071 Uiso 1 1 calc R . . C17 C 0.0938(2) 0.36932(17) 0.0784(3) 0.0579(7) Uani 1 1 d . . . H17 H 0.1542 0.3690 0.1199 0.069 Uiso 1 1 calc R . . C18 C 0.0581(2) 0.40415(17) -0.0324(3) 0.0592(7) Uani 1 1 d . . . H18 H -0.0005 0.3990 -0.0771 0.071 Uiso 1 1 calc R . . C19 C 0.1016(2) 0.44998(17) -0.0919(3) 0.0590(7) Uani 1 1 d . . . C20 C 0.0653(3) 0.4665(2) -0.2242(4) 0.0773(10) Uani 1 1 d . . . H20 H 0.0154 0.4465 -0.2757 0.093 Uiso 1 1 calc R . . C21 C 0.1034(4) 0.5128(3) -0.2793(5) 0.0972(14) Uani 1 1 d . . . H21 H 0.0807 0.5218 -0.3690 0.117 Uiso 1 1 calc R . . C22 C 0.1742(4) 0.5455(2) -0.2025(6) 0.1032(15) Uani 1 1 d . . . H22 H 0.1977 0.5783 -0.2390 0.124 Uiso 1 1 calc R . . C23 C 0.2105(3) 0.5299(2) -0.0718(5) 0.0915(12) Uani 1 1 d . . . H23 H 0.2586 0.5520 -0.0197 0.110 Uiso 1 1 calc R . . C24 C 0.1755(2) 0.4814(2) -0.0180(4) 0.0711(9) Uani 1 1 d . . . H24 H 0.2019 0.4694 0.0695 0.085 Uiso 1 1 calc R . . C25 C 0.2248(2) 0.06095(19) 0.2713(3) 0.0597(7) Uani 1 1 d . . . H25 H 0.1955 0.0202 0.2661 0.072 Uiso 1 1 calc R . . C26 C 0.3073(2) 0.04298(18) 0.2251(3) 0.0596(7) Uani 1 1 d . . . H26 H 0.3352 0.0835 0.2228 0.072 Uiso 1 1 calc R . . C27 C 0.3450(2) -0.02996(19) 0.1856(3) 0.0651(8) Uani 1 1 d . . . H27 H 0.3108 -0.0677 0.1776 0.078 Uiso 1 1 calc R . . C28 C 0.4331(2) -0.0576(2) 0.1536(3) 0.0673(8) Uani 1 1 d . . . C29 C 0.4944(3) -0.0093(3) 0.1713(4) 0.0837(11) Uani 1 1 d . . . H29 H 0.4795 0.0431 0.2042 0.100 Uiso 1 1 calc R . . C30 C 0.5772(3) -0.0387(4) 0.1403(4) 0.1083(15) Uani 1 1 d . . . H30 H 0.6173 -0.0058 0.1500 0.130 Uiso 1 1 calc R . . C31 C 0.6008(4) -0.1157(5) 0.0957(5) 0.133(2) Uani 1 1 d . . . H31 H 0.6576 -0.1352 0.0774 0.160 Uiso 1 1 calc R . . C32 C 0.5425(4) -0.1638(4) 0.0778(5) 0.131(2) Uani 1 1 d . . . H32 H 0.5588 -0.2161 0.0459 0.157 Uiso 1 1 calc R . . C33 C 0.4579(3) -0.1356(2) 0.1066(4) 0.0966(13) Uani 1 1 d . . . H33 H 0.4180 -0.1691 0.0944 0.116 Uiso 1 1 calc R . . C34 C -0.0471(2) 0.17036(17) -0.2004(3) 0.0546(7) Uani 1 1 d . . . C35 C 0.0220(2) 0.2110(2) -0.1827(3) 0.0605(7) Uani 1 1 d . . . H35 H 0.0078 0.2599 -0.2130 0.073 Uiso 1 1 calc R . . C36 C 0.1109(2) 0.1820(2) -0.1220(3) 0.0739(9) Uani 1 1 d . . . H36 H 0.1547 0.2116 -0.1111 0.089 Uiso 1 1 calc R . . C37 C 0.1349(3) 0.1098(3) -0.0778(3) 0.0849(12) Uani 1 1 d . . . H37 H 0.1948 0.0896 -0.0387 0.102 Uiso 1 1 calc R . . C38 C 0.0693(3) 0.0681(2) -0.0920(4) 0.0871(11) Uani 1 1 d . . . H38 H 0.0845 0.0196 -0.0602 0.105 Uiso 1 1 calc R . . C39 C -0.0190(2) 0.0969(2) -0.1529(4) 0.0761(9) Uani 1 1 d . . . H39 H -0.0619 0.0665 -0.1631 0.091 Uiso 1 1 calc R . . C40 C -0.1870(2) 0.13235(17) -0.3876(3) 0.0598(8) Uani 1 1 d . . . C41 C -0.1288(3) 0.0884(2) -0.4673(4) 0.0788(10) Uani 1 1 d . . . H41 H -0.0701 0.0969 -0.4477 0.095 Uiso 1 1 calc R . . C42 C -0.1537(4) 0.0332(2) -0.5733(4) 0.1023(15) Uani 1 1 d . . . H42 H -0.1125 0.0064 -0.6240 0.123 Uiso 1 1 calc R . . C43 C -0.2379(4) 0.0182(3) -0.6034(5) 0.1164(19) Uani 1 1 d . . . H43 H -0.2549 -0.0189 -0.6750 0.140 Uiso 1 1 calc R . . C44 C -0.2981(3) 0.0579(3) -0.5279(5) 0.1009(15) Uani 1 1 d . . . H44 H -0.3558 0.0469 -0.5474 0.121 Uiso 1 1 calc R . . C45 C -0.2731(2) 0.1155(2) -0.4204(4) 0.0741(9) Uani 1 1 d . . . H45 H -0.3150 0.1426 -0.3710 0.089 Uiso 1 1 calc R . . C46 C -0.16990(18) 0.28047(17) -0.3485(3) 0.0505(6) Uani 1 1 d . . . C47 C -0.2012(2) 0.28192(19) -0.4867(3) 0.0596(7) Uani 1 1 d . . . H47 H -0.2085 0.2352 -0.5409 0.072 Uiso 1 1 calc R . . C48 C -0.2221(2) 0.3494(2) -0.5477(3) 0.0735(9) Uani 1 1 d . . . H48 H -0.2439 0.3474 -0.6407 0.088 Uiso 1 1 calc R . . C49 C -0.2110(2) 0.4193(2) -0.4725(4) 0.0733(9) Uani 1 1 d . . . H49 H -0.2249 0.4648 -0.5135 0.088 Uiso 1 1 calc R . . C50 C -0.1789(2) 0.42102(19) -0.3352(4) 0.0706(9) Uani 1 1 d . . . H50 H -0.1702 0.4678 -0.2826 0.085 Uiso 1 1 calc R . . C51 C -0.1597(2) 0.35298(18) -0.2754(3) 0.0615(8) Uani 1 1 d . . . H51 H -0.1389 0.3557 -0.1823 0.074 Uiso 1 1 calc R . . C52 C -0.2152(2) 0.22808(18) -0.1560(3) 0.0560(7) Uani 1 1 d . . . C53 C -0.2995(2) 0.2774(2) -0.1808(3) 0.0707(9) Uani 1 1 d . . . H53 H -0.3231 0.2924 -0.2669 0.085 Uiso 1 1 calc R . . C54 C -0.3507(3) 0.3057(2) -0.0850(4) 0.0826(10) Uani 1 1 d . . . H54 H -0.4064 0.3391 -0.1072 0.099 Uiso 1 1 calc R . . C55 C -0.3183(3) 0.2841(3) 0.0419(4) 0.0895(12) Uani 1 1 d . . . H55 H -0.3514 0.3031 0.1074 0.107 Uiso 1 1 calc R . . C56 C -0.2371(3) 0.2344(3) 0.0715(4) 0.0921(12) Uani 1 1 d . . . H56 H -0.2153 0.2185 0.1573 0.110 Uiso 1 1 calc R . . C57 C -0.1862(2) 0.2068(2) -0.0257(3) 0.0786(10) Uani 1 1 d . . . H57 H -0.1308 0.1731 -0.0025 0.094 Uiso 1 1 calc R . . C58 C 0.4172(3) 0.1451(3) 0.5394(5) 0.1144(16) Uani 1 1 d . . . H58A H 0.4527 0.1726 0.6146 0.172 Uiso 1 1 calc R . . H58B H 0.4540 0.0967 0.5116 0.172 Uiso 1 1 calc R . . H58C H 0.3669 0.1348 0.5654 0.172 Uiso 1 1 calc R . . B1 B -0.1538(2) 0.2020(2) -0.2719(3) 0.0548(8) Uani 1 1 d . . . 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 Cd1 0.04756(12) 0.05756(13) 0.05893(14) 0.00868(9) 0.02042(9) -0.01298(9) O1 0.0804(16) 0.0821(16) 0.0785(15) 0.0050(13) 0.0349(13) -0.0208(13) O2 0.108(2) 0.107(2) 0.116(2) 0.0221(17) 0.0640(18) -0.0277(17) O3 0.0760(15) 0.0886(17) 0.0749(15) 0.0042(13) 0.0222(13) -0.0324(13) O4 0.0523(12) 0.0909(16) 0.0760(15) 0.0214(13) 0.0123(11) -0.0112(11) O5A 0.115(10) 0.135(9) 0.25(2) 0.026(10) 0.106(13) -0.028(7) C59A 0.107(4) 0.279(9) 0.170(6) 0.116(6) 0.020(4) -0.054(5) O5B 0.072(3) 0.160(7) 0.121(6) 0.050(6) 0.015(3) -0.024(4) C59B 0.107(4) 0.279(9) 0.170(6) 0.116(6) 0.020(4) -0.054(5) N1 0.0515(13) 0.0580(14) 0.0586(14) 0.0054(11) 0.0218(11) -0.0115(11) N2 0.0450(13) 0.0636(15) 0.0654(15) 0.0152(12) 0.0159(11) -0.0094(11) N3 0.0552(14) 0.0541(14) 0.0562(14) 0.0084(11) 0.0150(11) -0.0146(11) N4 0.0438(13) 0.0606(16) 0.0766(18) 0.0058(13) 0.0246(12) -0.0116(12) C1 0.0575(17) 0.0665(19) 0.0628(18) 0.0063(15) 0.0305(15) -0.0137(14) C2 0.0614(18) 0.0664(19) 0.0682(19) 0.0153(15) 0.0253(15) -0.0166(15) C3 0.0597(18) 0.0588(17) 0.0688(19) 0.0108(14) 0.0213(15) -0.0220(14) C4 0.0504(17) 0.081(2) 0.078(2) 0.0130(17) 0.0154(15) -0.0251(16) C5 0.0410(15) 0.074(2) 0.075(2) 0.0223(16) 0.0170(14) -0.0086(14) C6 0.0466(16) 0.073(2) 0.083(2) 0.0186(17) 0.0317(15) -0.0050(14) C7 0.0623(18) 0.0654(19) 0.0583(18) 0.0009(15) 0.0238(15) -0.0104(15) C8 0.0576(18) 0.0646(19) 0.0633(19) -0.0025(15) 0.0197(15) -0.0133(15) C9 0.0607(19) 0.069(2) 0.066(2) -0.0040(16) 0.0182(16) -0.0110(16) C10 0.0566(18) 0.0639(19) 0.067(2) 0.0024(15) 0.0055(15) -0.0125(15) C11 0.070(2) 0.083(2) 0.084(2) -0.0020(19) 0.0184(19) -0.0255(19) C12 0.076(3) 0.113(3) 0.097(3) 0.018(3) 0.020(2) -0.032(2) C13 0.075(3) 0.098(3) 0.118(4) 0.034(3) -0.001(2) -0.037(2) C14 0.096(3) 0.081(3) 0.115(3) -0.005(2) 0.006(3) -0.040(2) C15 0.079(2) 0.083(3) 0.090(3) -0.013(2) 0.015(2) -0.026(2) C16 0.0488(16) 0.0640(18) 0.0642(19) 0.0118(15) 0.0134(14) -0.0069(14) C17 0.0546(17) 0.0568(17) 0.0630(18) 0.0125(14) 0.0178(14) -0.0038(14) C18 0.0587(18) 0.0578(17) 0.0584(18) 0.0049(14) 0.0140(14) -0.0070(14) C19 0.072(2) 0.0493(16) 0.0570(17) 0.0064(13) 0.0296(15) 0.0025(14) C20 0.088(2) 0.069(2) 0.071(2) 0.0184(17) 0.0268(19) 0.0096(18) C21 0.122(4) 0.086(3) 0.091(3) 0.047(2) 0.051(3) 0.023(3) C22 0.132(4) 0.073(3) 0.131(4) 0.035(3) 0.082(4) 0.003(3) C23 0.105(3) 0.081(3) 0.110(3) 0.006(2) 0.060(3) -0.024(2) C24 0.082(2) 0.070(2) 0.071(2) 0.0022(17) 0.0353(18) -0.0167(18) C25 0.0657(19) 0.0613(19) 0.0561(17) 0.0107(14) 0.0110(15) -0.0208(15) C26 0.0678(19) 0.0557(18) 0.0566(17) 0.0060(14) 0.0148(15) -0.0147(15) C27 0.078(2) 0.0610(19) 0.0576(18) 0.0018(15) 0.0181(16) -0.0164(16) C28 0.075(2) 0.071(2) 0.0511(17) -0.0003(15) 0.0175(16) -0.0067(17) C29 0.074(2) 0.108(3) 0.065(2) 0.002(2) 0.0158(18) -0.017(2) C30 0.073(3) 0.170(5) 0.073(3) 0.008(3) 0.011(2) -0.020(3) C31 0.084(3) 0.210(7) 0.074(3) 0.000(4) 0.020(3) 0.024(4) C32 0.128(5) 0.136(5) 0.093(4) -0.023(3) 0.037(3) 0.031(4) C33 0.107(3) 0.084(3) 0.084(3) -0.014(2) 0.030(2) 0.002(2) C34 0.0598(17) 0.0621(18) 0.0413(14) 0.0033(13) 0.0107(13) -0.0141(14) C35 0.0580(18) 0.075(2) 0.0490(16) 0.0014(14) 0.0161(14) -0.0135(15) C36 0.059(2) 0.097(3) 0.065(2) 0.0032(19) 0.0162(16) -0.0158(19) C37 0.062(2) 0.124(3) 0.055(2) 0.015(2) 0.0077(16) 0.004(2) C38 0.089(3) 0.085(3) 0.075(2) 0.027(2) 0.007(2) 0.006(2) C39 0.075(2) 0.078(2) 0.072(2) 0.0199(18) 0.0020(18) -0.0158(18) C40 0.073(2) 0.0521(17) 0.0508(16) 0.0145(13) -0.0013(15) -0.0176(15) C41 0.091(3) 0.070(2) 0.067(2) 0.0005(17) 0.0077(19) -0.0169(19) C42 0.130(4) 0.073(3) 0.070(2) -0.008(2) -0.007(3) 0.000(3) C43 0.144(5) 0.063(2) 0.092(3) -0.002(2) -0.042(3) -0.007(3) C44 0.102(3) 0.073(3) 0.105(3) 0.024(2) -0.040(3) -0.037(2) C45 0.076(2) 0.067(2) 0.074(2) 0.0228(17) -0.0118(18) -0.0255(18) C46 0.0452(15) 0.0619(17) 0.0484(15) 0.0065(13) 0.0113(12) -0.0179(13) C47 0.0665(19) 0.0686(19) 0.0491(16) 0.0099(14) 0.0108(14) -0.0245(16) C48 0.086(2) 0.087(2) 0.0552(19) 0.0199(17) 0.0123(17) -0.029(2) C49 0.084(2) 0.066(2) 0.081(2) 0.0290(18) 0.0283(19) -0.0102(18) C50 0.086(2) 0.0563(19) 0.076(2) 0.0034(16) 0.0300(19) -0.0185(17) C51 0.0679(19) 0.067(2) 0.0518(17) 0.0054(14) 0.0139(14) -0.0182(16) C52 0.0576(18) 0.0655(18) 0.0501(16) 0.0118(14) 0.0072(13) -0.0245(15) C53 0.066(2) 0.086(2) 0.066(2) 0.0186(17) 0.0180(16) -0.0169(18) C54 0.076(2) 0.091(3) 0.091(3) 0.014(2) 0.036(2) -0.016(2) C55 0.084(3) 0.123(3) 0.077(3) 0.001(2) 0.036(2) -0.040(3) C56 0.090(3) 0.143(4) 0.051(2) 0.018(2) 0.0149(19) -0.035(3) C57 0.064(2) 0.121(3) 0.0545(19) 0.0215(19) 0.0081(16) -0.024(2) C58 0.092(3) 0.145(4) 0.102(3) 0.053(3) 0.009(3) -0.001(3) B1 0.0564(19) 0.064(2) 0.0459(17) 0.0103(15) 0.0046(15) -0.0204(16) _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 Cd1 N3 2.265(2) . ? Cd1 N1 2.273(2) . ? Cd1 O1 2.341(2) . ? Cd1 N2 2.351(2) . ? Cd1 O4 2.396(2) . ? Cd1 O3 2.405(2) . ? O1 N4 1.229(3) . ? O2 N4 1.268(3) . ? O3 N4 1.227(3) . ? O4 C58 1.416(5) . ? O5A C59A 1.301(12) . ? N1 C7 1.282(4) . ? N1 C1 1.484(3) . ? N2 C16 1.280(4) . ? N2 C5 1.483(4) . ? N3 C25 1.275(4) . ? N3 C3 1.486(4) . ? C1 C2 1.527(4) . ? C1 C6 1.527(4) . ? C2 C3 1.531(4) . ? C3 C4 1.528(4) . ? C4 C5 1.522(4) . ? C5 C6 1.536(5) . ? C7 C8 1.442(4) . ? C8 C9 1.325(4) . ? C9 C10 1.458(4) . ? C10 C11 1.391(5) . ? C10 C15 1.394(5) . ? C11 C12 1.373(5) . ? C12 C13 1.373(6) . ? C13 C14 1.365(6) . ? C14 C15 1.376(6) . ? C16 C17 1.439(4) . ? C17 C18 1.325(4) . ? C18 C19 1.466(4) . ? C19 C24 1.387(5) . ? C19 C20 1.392(4) . ? C20 C21 1.387(6) . ? C21 C22 1.371(7) . ? C22 C23 1.372(6) . ? C23 C24 1.376(5) . ? C25 C26 1.439(4) . ? C26 C27 1.333(4) . ? C27 C28 1.456(5) . ? C28 C33 1.385(5) . ? C28 C29 1.388(5) . ? C29 C30 1.377(6) . ? C30 C31 1.361(8) . ? C31 C32 1.348(8) . ? C32 C33 1.391(7) . ? C34 C35 1.393(4) . ? C34 C39 1.404(4) . ? C34 B1 1.645(4) . ? C35 C36 1.384(5) . ? C36 C37 1.370(5) . ? C37 C38 1.364(6) . ? C38 C39 1.376(5) . ? C40 C45 1.391(5) . ? C40 C41 1.399(5) . ? C40 B1 1.642(4) . ? C41 C42 1.378(5) . ? C42 C43 1.350(7) . ? C43 C44 1.372(7) . ? C44 C45 1.416(5) . ? C46 C47 1.389(4) . ? C46 C51 1.397(4) . ? C46 B1 1.656(4) . ? C47 C48 1.382(4) . ? C48 C49 1.368(5) . ? C49 C50 1.374(5) . ? C50 C51 1.386(4) . ? C52 C53 1.389(5) . ? C52 C57 1.393(4) . ? C52 B1 1.667(5) . ? C53 C54 1.390(5) . ? C54 C55 1.365(5) . ? C55 C56 1.361(6) . ? C56 C57 1.398(5) . ? 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 N3 Cd1 N1 90.06(9) . . ? N3 Cd1 O1 107.17(9) . . ? N1 Cd1 O1 162.05(9) . . ? N3 Cd1 N2 86.31(9) . . ? N1 Cd1 N2 83.83(9) . . ? O1 Cd1 N2 101.91(9) . . ? N3 Cd1 O4 92.10(9) . . ? N1 Cd1 O4 91.42(8) . . ? O1 Cd1 O4 83.10(9) . . ? N2 Cd1 O4 174.99(8) . . ? N3 Cd1 O3 159.91(9) . . ? N1 Cd1 O3 108.96(9) . . ? O1 Cd1 O3 53.38(9) . . ? N2 Cd1 O3 101.74(9) . . ? O4 Cd1 O3 81.30(8) . . ? N4 O1 Cd1 94.54(18) . . ? N4 O3 Cd1 91.52(17) . . ? C58 O4 Cd1 128.3(2) . . ? C7 N1 C1 119.0(2) . . ? C7 N1 Cd1 126.1(2) . . ? C1 N1 Cd1 114.88(18) . . ? C16 N2 C5 117.5(2) . . ? C16 N2 Cd1 127.5(2) . . ? C5 N2 Cd1 114.52(18) . . ? C25 N3 C3 117.4(2) . . ? C25 N3 Cd1 127.6(2) . . ? C3 N3 Cd1 114.93(18) . . ? O3 N4 O1 120.6(3) . . ? O3 N4 O2 119.5(3) . . ? O1 N4 O2 119.7(3) . . ? N1 C1 C2 111.6(2) . . ? N1 C1 C6 110.7(2) . . ? C2 C1 C6 111.4(3) . . ? C1 C2 C3 116.6(3) . . ? N3 C3 C4 110.4(2) . . ? N3 C3 C2 110.6(2) . . ? C4 C3 C2 112.2(3) . . ? C5 C4 C3 115.7(3) . . ? N2 C5 C4 112.2(2) . . ? N2 C5 C6 109.6(2) . . ? C4 C5 C6 111.7(3) . . ? C1 C6 C5 115.3(3) . . ? N1 C7 C8 123.6(3) . . ? C9 C8 C7 123.2(3) . . ? C8 C9 C10 126.9(3) . . ? C11 C10 C15 117.6(3) . . ? C11 C10 C9 122.7(3) . . ? C15 C10 C9 119.8(3) . . ? C12 C11 C10 121.3(4) . . ? C13 C12 C11 119.9(4) . . ? C14 C13 C12 120.0(4) . . ? C13 C14 C15 120.5(4) . . ? C14 C15 C10 120.7(4) . . ? N2 C16 C17 124.0(3) . . ? C18 C17 C16 123.1(3) . . ? C17 C18 C19 126.6(3) . . ? C24 C19 C20 118.3(3) . . ? C24 C19 C18 122.0(3) . . ? C20 C19 C18 119.6(3) . . ? C21 C20 C19 120.0(4) . . ? C22 C21 C20 120.5(4) . . ? C21 C22 C23 120.0(4) . . ? C22 C23 C24 119.9(4) . . ? C23 C24 C19 121.2(4) . . ? N3 C25 C26 124.7(3) . . ? C27 C26 C25 122.0(3) . . ? C26 C27 C28 127.8(3) . . ? C33 C28 C29 118.5(4) . . ? C33 C28 C27 118.9(4) . . ? C29 C28 C27 122.5(3) . . ? C30 C29 C28 120.1(4) . . ? C31 C30 C29 120.6(5) . . ? C32 C31 C30 120.3(5) . . ? C31 C32 C33 120.4(5) . . ? C28 C33 C32 120.0(5) . . ? C35 C34 C39 114.5(3) . . ? C35 C34 B1 124.9(3) . . ? C39 C34 B1 120.6(3) . . ? C36 C35 C34 122.9(3) . . ? C37 C36 C35 120.3(4) . . ? C38 C37 C36 118.9(3) . . ? C37 C38 C39 120.7(4) . . ? C38 C39 C34 122.7(4) . . ? C45 C40 C41 115.2(3) . . ? C45 C40 B1 124.6(3) . . ? C41 C40 B1 120.1(3) . . ? C42 C41 C40 123.7(4) . . ? C43 C42 C41 120.0(5) . . ? C42 C43 C44 119.7(4) . . ? C43 C44 C45 120.4(4) . . ? C40 C45 C44 121.1(4) . . ? C47 C46 C51 114.5(3) . . ? C47 C46 B1 123.9(3) . . ? C51 C46 B1 121.4(2) . . ? C48 C47 C46 123.1(3) . . ? C49 C48 C47 120.5(3) . . ? C48 C49 C50 118.8(3) . . ? C49 C50 C51 120.0(3) . . ? C50 C51 C46 123.1(3) . . ? C53 C52 C57 114.1(3) . . ? C53 C52 B1 121.6(3) . . ? C57 C52 B1 124.2(3) . . ? C52 C53 C54 124.1(3) . . ? C55 C54 C53 119.4(4) . . ? C56 C55 C54 119.2(4) . . ? C55 C56 C57 120.7(4) . . ? C52 C57 C56 122.5(4) . . ? C40 B1 C34 107.4(3) . . ? C40 B1 C46 107.2(2) . . ? C34 B1 C46 113.1(2) . . ? C40 B1 C52 113.2(2) . . ? C34 B1 C52 110.3(2) . . ? C46 B1 C52 105.7(2) . . ? 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 N3 Cd1 O1 N4 -174.40(17) . . . . ? N1 Cd1 O1 N4 -11.3(4) . . . . ? N2 Cd1 O1 N4 95.81(18) . . . . ? O4 Cd1 O1 N4 -84.33(18) . . . . ? O3 Cd1 O1 N4 -0.07(16) . . . . ? N3 Cd1 O3 N4 16.0(3) . . . . ? N1 Cd1 O3 N4 176.41(17) . . . . ? O1 Cd1 O3 N4 0.07(16) . . . . ? N2 Cd1 O3 N4 -96.14(18) . . . . ? O4 Cd1 O3 N4 87.90(18) . . . . ? N3 Cd1 O4 C58 -44.4(4) . . . . ? N1 Cd1 O4 C58 45.7(4) . . . . ? O1 Cd1 O4 C58 -151.5(4) . . . . ? N2 Cd1 O4 C58 26.9(11) . . . . ? O3 Cd1 O4 C58 154.6(4) . . . . ? N3 Cd1 N1 C7 142.8(3) . . . . ? O1 Cd1 N1 C7 -21.1(4) . . . . ? N2 Cd1 N1 C7 -131.0(3) . . . . ? O4 Cd1 N1 C7 50.7(3) . . . . ? O3 Cd1 N1 C7 -30.6(3) . . . . ? N3 Cd1 N1 C1 -37.7(2) . . . . ? O1 Cd1 N1 C1 158.4(3) . . . . ? N2 Cd1 N1 C1 48.54(19) . . . . ? O4 Cd1 N1 C1 -129.84(19) . . . . ? O3 Cd1 N1 C1 148.87(19) . . . . ? N3 Cd1 N2 C16 -129.5(3) . . . . ? N1 Cd1 N2 C16 140.0(3) . . . . ? O1 Cd1 N2 C16 -22.8(3) . . . . ? O4 Cd1 N2 C16 158.8(8) . . . . ? O3 Cd1 N2 C16 31.9(3) . . . . ? N3 Cd1 N2 C5 42.0(2) . . . . ? N1 Cd1 N2 C5 -48.4(2) . . . . ? O1 Cd1 N2 C5 148.8(2) . . . . ? O4 Cd1 N2 C5 -29.6(10) . . . . ? O3 Cd1 N2 C5 -156.6(2) . . . . ? N1 Cd1 N3 C25 -143.7(3) . . . . ? O1 Cd1 N3 C25 31.1(3) . . . . ? N2 Cd1 N3 C25 132.5(3) . . . . ? O4 Cd1 N3 C25 -52.3(3) . . . . ? O3 Cd1 N3 C25 17.8(4) . . . . ? N1 Cd1 N3 C3 38.8(2) . . . . ? O1 Cd1 N3 C3 -146.36(19) . . . . ? N2 Cd1 N3 C3 -45.03(19) . . . . ? O4 Cd1 N3 C3 130.21(19) . . . . ? O3 Cd1 N3 C3 -159.7(2) . . . . ? Cd1 O3 N4 O1 -0.1(3) . . . . ? Cd1 O3 N4 O2 174.3(3) . . . . ? Cd1 O1 N4 O3 0.1(3) . . . . ? Cd1 O1 N4 O2 -174.3(3) . . . . ? C7 N1 C1 C2 -123.0(3) . . . . ? Cd1 N1 C1 C2 57.4(3) . . . . ? C7 N1 C1 C6 112.3(3) . . . . ? Cd1 N1 C1 C6 -67.3(3) . . . . ? N1 C1 C2 C3 -77.8(3) . . . . ? C6 C1 C2 C3 46.6(3) . . . . ? C25 N3 C3 C4 -112.0(3) . . . . ? Cd1 N3 C3 C4 65.8(3) . . . . ? C25 N3 C3 C2 123.1(3) . . . . ? Cd1 N3 C3 C2 -59.1(3) . . . . ? C1 C2 C3 N3 78.4(3) . . . . ? C1 C2 C3 C4 -45.4(3) . . . . ? N3 C3 C4 C5 -78.0(3) . . . . ? C2 C3 C4 C5 46.0(3) . . . . ? C16 N2 C5 C4 112.9(3) . . . . ? Cd1 N2 C5 C4 -59.6(3) . . . . ? C16 N2 C5 C6 -122.4(3) . . . . ? Cd1 N2 C5 C6 65.1(3) . . . . ? C3 C4 C5 N2 75.4(3) . . . . ? C3 C4 C5 C6 -48.1(3) . . . . ? N1 C1 C6 C5 76.4(3) . . . . ? C2 C1 C6 C5 -48.4(3) . . . . ? N2 C5 C6 C1 -75.4(3) . . . . ? C4 C5 C6 C1 49.5(3) . . . . ? C1 N1 C7 C8 -175.9(3) . . . . ? Cd1 N1 C7 C8 3.6(4) . . . . ? N1 C7 C8 C9 176.2(3) . . . . ? C7 C8 C9 C10 -177.2(3) . . . . ? C8 C9 C10 C11 -17.8(6) . . . . ? C8 C9 C10 C15 162.0(4) . . . . ? C15 C10 C11 C12 0.2(6) . . . . ? C9 C10 C11 C12 180.0(4) . . . . ? C10 C11 C12 C13 -1.1(6) . . . . ? C11 C12 C13 C14 1.2(7) . . . . ? C12 C13 C14 C15 -0.4(7) . . . . ? C13 C14 C15 C10 -0.6(7) . . . . ? C11 C10 C15 C14 0.7(6) . . . . ? C9 C10 C15 C14 -179.1(4) . . . . ? C5 N2 C16 C17 171.0(3) . . . . ? Cd1 N2 C16 C17 -17.6(4) . . . . ? N2 C16 C17 C18 175.2(3) . . . . ? C16 C17 C18 C19 173.5(3) . . . . ? C17 C18 C19 C24 -19.4(5) . . . . ? C17 C18 C19 C20 164.1(3) . . . . ? C24 C19 C20 C21 0.5(5) . . . . ? C18 C19 C20 C21 177.0(3) . . . . ? C19 C20 C21 C22 -3.0(6) . . . . ? C20 C21 C22 C23 2.8(6) . . . . ? C21 C22 C23 C24 -0.1(6) . . . . ? C22 C23 C24 C19 -2.5(6) . . . . ? C20 C19 C24 C23 2.2(5) . . . . ? C18 C19 C24 C23 -174.2(3) . . . . ? C3 N3 C25 C26 -175.2(3) . . . . ? Cd1 N3 C25 C26 7.3(4) . . . . ? N3 C25 C26 C27 175.0(3) . . . . ? C25 C26 C27 C28 -171.4(3) . . . . ? C26 C27 C28 C33 -176.3(3) . . . . ? C26 C27 C28 C29 5.3(5) . . . . ? C33 C28 C29 C30 1.1(6) . . . . ? C27 C28 C29 C30 179.5(3) . . . . ? C28 C29 C30 C31 -1.8(6) . . . . ? C29 C30 C31 C32 1.8(8) . . . . ? C30 C31 C32 C33 -1.0(9) . . . . ? C29 C28 C33 C32 -0.3(6) . . . . ? C27 C28 C33 C32 -178.8(4) . . . . ? C31 C32 C33 C28 0.2(8) . . . . ? C39 C34 C35 C36 -0.7(4) . . . . ? B1 C34 C35 C36 -179.9(3) . . . . ? C34 C35 C36 C37 1.0(5) . . . . ? C35 C36 C37 C38 -1.4(5) . . . . ? C36 C37 C38 C39 1.7(6) . . . . ? C37 C38 C39 C34 -1.5(6) . . . . ? C35 C34 C39 C38 1.0(5) . . . . ? B1 C34 C39 C38 -179.8(3) . . . . ? C45 C40 C41 C42 1.4(5) . . . . ? B1 C40 C41 C42 -174.8(3) . . . . ? C40 C41 C42 C43 -1.2(6) . . . . ? C41 C42 C43 C44 -0.2(7) . . . . ? C42 C43 C44 C45 1.2(7) . . . . ? C41 C40 C45 C44 -0.3(5) . . . . ? B1 C40 C45 C44 175.7(3) . . . . ? C43 C44 C45 C40 -1.0(6) . . . . ? C51 C46 C47 C48 -1.0(4) . . . . ? B1 C46 C47 C48 173.9(3) . . . . ? C46 C47 C48 C49 1.2(5) . . . . ? C47 C48 C49 C50 -0.2(5) . . . . ? C48 C49 C50 C51 -0.8(5) . . . . ? C49 C50 C51 C46 1.0(5) . . . . ? C47 C46 C51 C50 -0.1(4) . . . . ? B1 C46 C51 C50 -175.1(3) . . . . ? C57 C52 C53 C54 1.7(5) . . . . ? B1 C52 C53 C54 -175.0(3) . . . . ? C52 C53 C54 C55 -0.7(6) . . . . ? C53 C54 C55 C56 -0.9(6) . . . . ? C54 C55 C56 C57 1.4(7) . . . . ? C53 C52 C57 C56 -1.2(5) . . . . ? B1 C52 C57 C56 175.4(3) . . . . ? C55 C56 C57 C52 -0.3(6) . . . . ? C45 C40 B1 C34 144.9(3) . . . . ? C41 C40 B1 C34 -39.3(4) . . . . ? C45 C40 B1 C46 -93.2(3) . . . . ? C41 C40 B1 C46 82.5(3) . . . . ? C45 C40 B1 C52 23.0(4) . . . . ? C41 C40 B1 C52 -161.3(3) . . . . ? C35 C34 B1 C40 129.1(3) . . . . ? C39 C34 B1 C40 -50.0(4) . . . . ? C35 C34 B1 C46 11.0(4) . . . . ? C39 C34 B1 C46 -168.2(3) . . . . ? C35 C34 B1 C52 -107.1(3) . . . . ? C39 C34 B1 C52 73.7(4) . . . . ? C47 C46 B1 C40 -3.2(4) . . . . ? C51 C46 B1 C40 171.4(3) . . . . ? C47 C46 B1 C34 115.1(3) . . . . ? C51 C46 B1 C34 -70.4(4) . . . . ? C47 C46 B1 C52 -124.2(3) . . . . ? C51 C46 B1 C52 50.3(3) . . . . ? C53 C52 B1 C40 -79.3(4) . . . . ? C57 C52 B1 C40 104.3(3) . . . . ? C53 C52 B1 C34 160.4(3) . . . . ? C57 C52 B1 C34 -16.0(4) . . . . ? C53 C52 B1 C46 37.8(4) . . . . ? C57 C52 B1 C46 -138.6(3) . . . . ? 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 O4 H4 O5B 0.80 1.92 2.708(6) 166.1 . O4 H4 O5A 0.80 2.00 2.732(11) 151.1 . O5A H5A O4 0.82 2.14 2.732(11) 128.9 . O5A H5A N4 0.82 2.60 3.262(18) 139.0 . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.632 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.056 #===END OF FILE