# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Augustin Madalan' _publ_contact_author_email madalin.madalan@g.unibuc.ro loop_ _publ_author_name 'Andrei Cucos' 'Andrei Ursu' 'Augustin M. Madalan' 'Carine Duhayon' 'Jean-Pascal Sutter' 'Marius Andruh' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 809434' #TrackingRef 'C1a_au3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Cl N5 Ni2 O12' _chemical_formula_weight 887.60 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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 11.5278(15) _cell_length_b 12.7865(15) _cell_length_c 15.6274(17) _cell_angle_alpha 65.755(9) _cell_angle_beta 74.110(9) _cell_angle_gamma 65.063(9) _cell_volume 1890.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8693 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 26.00 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7762 _exptl_absorpt_correction_T_max 0.8379 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15709 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.1068 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 26.04 _reflns_number_total 7153 _reflns_number_gt 4021 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The geometrical restrains were used for the refinement of the ammonium ion. The N-H bond distance were restrained according to [R.J.C. Brown, J.Mol.Struct.(1995) 345, 77.] ; _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^)+(0.0263P)^2^+0.0000P] 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 7153 _refine_ls_number_parameters 525 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1276 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.929 _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 C1 C 0.7307(7) 0.5222(5) 0.9657(4) 0.103(2) Uani 1 1 d . . . H1A H 0.8196 0.4704 0.9605 0.154 Uiso 1 1 calc R . . H1B H 0.6909 0.5323 0.9150 0.154 Uiso 1 1 calc R . . H1C H 0.6871 0.4853 1.0251 0.154 Uiso 1 1 calc R . . C2 C 0.7546(5) 0.6447(5) 1.0359(3) 0.0589(15) Uani 1 1 d . . . C3 C 0.8069(6) 0.5451(5) 1.1120(4) 0.0743(17) Uani 1 1 d . . . H3 H 0.8232 0.4667 1.1136 0.089 Uiso 1 1 calc R . . C4 C 0.8351(7) 0.5589(7) 1.1851(4) 0.095(2) Uani 1 1 d . . . H4 H 0.8731 0.4901 1.2345 0.114 Uiso 1 1 calc R . . C5 C 0.8080(6) 0.6733(7) 1.1861(3) 0.0787(19) Uani 1 1 d . . . H5 H 0.8252 0.6823 1.2370 0.094 Uiso 1 1 calc R . . C6 C 0.7537(5) 0.7781(6) 1.1095(3) 0.0561(14) Uani 1 1 d . . . C7 C 0.7276(5) 0.7658(5) 1.0322(3) 0.0491(13) Uani 1 1 d . . . C8 C 0.7163(5) 0.8951(7) 1.1161(4) 0.0663(17) Uani 1 1 d . . . H8 H 0.7283 0.8972 1.1717 0.080 Uiso 1 1 calc R . . C9 C 0.6149(6) 1.1141(6) 1.0730(4) 0.083(2) Uani 1 1 d . . . H9A H 0.6643 1.1085 1.1170 0.100 Uiso 1 1 calc R . . H9B H 0.5260 1.1288 1.1016 0.100 Uiso 1 1 calc R . . C10 C 0.6224(6) 1.2157(6) 0.9834(4) 0.081(2) Uani 1 1 d . . . H10A H 0.7075 1.2211 0.9684 0.098 Uiso 1 1 calc R . . H10B H 0.5595 1.2930 0.9889 0.098 Uiso 1 1 calc R . . C11 C 0.5555(5) 1.2774(5) 0.8328(4) 0.0566(15) Uani 1 1 d . . . H11 H 0.5410 1.3559 0.8300 0.068 Uiso 1 1 calc R . . C12 C 0.5311(4) 1.2665(4) 0.7527(3) 0.0445(12) Uani 1 1 d . . . C13 C 0.4841(5) 1.3724(4) 0.6759(4) 0.0603(15) Uani 1 1 d . . . H13 H 0.4697 1.4487 0.6779 0.072 Uiso 1 1 calc R . . C14 C 0.4596(5) 1.3655(4) 0.5990(4) 0.0596(15) Uani 1 1 d . . . H14 H 0.4296 1.4368 0.5486 0.071 Uiso 1 1 calc R . . C15 C 0.4791(4) 1.2510(4) 0.5943(3) 0.0463(13) Uani 1 1 d . . . H15 H 0.4623 1.2464 0.5413 0.056 Uiso 1 1 calc R . . C16 C 0.5237(4) 1.1459(4) 0.6700(3) 0.0332(10) Uani 1 1 d . . . C17 C 0.5517(4) 1.1503(4) 0.7508(3) 0.0338(10) Uani 1 1 d . . . C18 C 0.5303(5) 1.0164(4) 0.5920(3) 0.0488(13) Uani 1 1 d . . . H18A H 0.4438 1.0629 0.5763 0.073 Uiso 1 1 calc R . . H18B H 0.5487 0.9312 0.6045 0.073 Uiso 1 1 calc R . . H18C H 0.5897 1.0446 0.5401 0.073 Uiso 1 1 calc R . . C19 C -0.0262(6) 1.1922(6) 0.0768(4) 0.082(2) Uani 1 1 d . . . H19A H 0.0342 1.1709 0.0252 0.124 Uiso 1 1 calc R . . H19B H -0.0472 1.2772 0.0665 0.124 Uiso 1 1 calc R . . H19C H -0.1032 1.1779 0.0806 0.124 Uiso 1 1 calc R . . C20 C 0.0610(4) 0.9959(5) 0.1925(3) 0.0414(11) Uani 1 1 d . . . C21 C 0.0458(5) 0.9336(6) 0.1448(4) 0.0629(16) Uani 1 1 d . . . H21 H 0.0116 0.9766 0.0875 0.076 Uiso 1 1 calc R . . C22 C 0.0816(6) 0.8052(7) 0.1824(5) 0.080(2) Uani 1 1 d . . . H22 H 0.0715 0.7638 0.1496 0.096 Uiso 1 1 calc R . . C23 C 0.1303(6) 0.7423(6) 0.2650(5) 0.0753(19) Uani 1 1 d . . . H23 H 0.1561 0.6573 0.2880 0.090 Uiso 1 1 calc R . . C24 C 0.1432(5) 0.8039(4) 0.3183(4) 0.0495(13) Uani 1 1 d . . . C25 C 0.1099(4) 0.9317(4) 0.2813(3) 0.0354(10) Uani 1 1 d . . . C26 C 0.1820(5) 0.7349(4) 0.4101(4) 0.0558(16) Uani 1 1 d . . . H26 H 0.2066 0.6502 0.4294 0.067 Uiso 1 1 calc R . . C27 C 0.2333(5) 0.6981(5) 0.5611(4) 0.0666(18) Uani 1 1 d . . . H27A H 0.2106 0.6254 0.5844 0.080 Uiso 1 1 calc R . . H27B H 0.3263 0.6730 0.5553 0.080 Uiso 1 1 calc R . . C28 C 0.1705(5) 0.7693(5) 0.6264(3) 0.0684(17) Uani 1 1 d . . . H28A H 0.0827 0.7711 0.6487 0.082 Uiso 1 1 calc R . . H28B H 0.2175 0.7327 0.6806 0.082 Uiso 1 1 calc R . . C29 C 0.1770(5) 0.9605(6) 0.6133(4) 0.0658(17) Uani 1 1 d . . . H29 H 0.1870 0.9235 0.6773 0.079 Uiso 1 1 calc R . . C30 C 0.1689(4) 1.0850(6) 0.5714(4) 0.0533(14) Uani 1 1 d . . . C31 C 0.1804(5) 1.1451(8) 0.6251(4) 0.081(2) Uani 1 1 d . . . H31 H 0.1955 1.1024 0.6879 0.097 Uiso 1 1 calc R . . C32 C 0.1696(6) 1.2647(9) 0.5858(6) 0.099(3) Uani 1 1 d . . . H32 H 0.1776 1.3032 0.6219 0.119 Uiso 1 1 calc R . . C33 C 0.1468(5) 1.3296(6) 0.4931(5) 0.082(2) Uani 1 1 d . . . H33 H 0.1396 1.4115 0.4670 0.098 Uiso 1 1 calc R . . C34 C 0.1347(5) 1.2739(5) 0.4392(4) 0.0540(14) Uani 1 1 d . . . C35 C 0.1449(4) 1.1494(5) 0.4767(4) 0.0437(12) Uani 1 1 d . . . C36 C 0.1195(6) 1.4517(5) 0.2996(5) 0.096(2) Uani 1 1 d . . . H36A H 0.0590 1.5048 0.3335 0.145 Uiso 1 1 calc R . . H36B H 0.0993 1.4833 0.2360 0.145 Uiso 1 1 calc R . . H36C H 0.2051 1.4473 0.2984 0.145 Uiso 1 1 calc R . . N1 N 0.6669(4) 1.0002(5) 1.0522(3) 0.0552(13) Uani 1 1 d . . . N2 N 0.5954(4) 1.1893(4) 0.9080(3) 0.0522(11) Uani 1 1 d . . . N3 N 0.1861(4) 0.7799(3) 0.4683(3) 0.0441(11) Uani 1 1 d . . . N4 N 0.1719(4) 0.8932(4) 0.5726(3) 0.0509(11) Uani 1 1 d . . . N5 N 0.7524(3) 0.8316(3) 0.7751(2) 0.0324(8) Uani 1 1 d D . . Ni1 Ni 0.63437(6) 1.02451(6) 0.93399(4) 0.03956(19) Uani 1 1 d . . . Ni2 Ni 0.15260(6) 0.94221(5) 0.44669(4) 0.03258(17) Uani 1 1 d . . . O1 O 0.7226(4) 0.6391(3) 0.9607(3) 0.0721(12) Uani 1 1 d . . . O2 O 0.6809(3) 0.8574(3) 0.9577(2) 0.0511(9) Uani 1 1 d . . . O3 O 0.5961(3) 1.0467(2) 0.81934(19) 0.0351(7) Uani 1 1 d . . . O4 O 0.5430(3) 1.0316(3) 0.6736(2) 0.0456(8) Uani 1 1 d . . . O5 O 0.0294(3) 1.1190(3) 0.1627(2) 0.0565(10) Uani 1 1 d . . . O6 O 0.1204(3) 0.9959(2) 0.3237(2) 0.0324(7) Uani 1 1 d . . . O7 O 0.1327(3) 1.1033(3) 0.4205(2) 0.0406(8) Uani 1 1 d . . . O8 O 0.1122(3) 1.3321(3) 0.3455(3) 0.0629(10) Uani 1 1 d . . . O14 O 0.4680(8) 0.4464(5) 0.1908(6) 0.220(4) Uani 1 1 d . . . H1N H 0.741(5) 0.785(4) 0.8482(7) 0.15(3) Uiso 1 1 d D . . H2N H 0.673(3) 0.913(2) 0.757(3) 0.16(3) Uiso 1 1 d D . . H3N H 0.837(2) 0.851(4) 0.756(3) 0.16(3) Uiso 1 1 d D . . H4N H 0.758(5) 0.776(4) 0.739(3) 0.16(3) Uiso 1 1 d D . . Cl1 Cl 0.51598(16) 0.32341(13) 0.24101(12) 0.0728(4) Uani 1 1 d . . . O11 O 0.5192(6) 0.3034(7) 0.3339(4) 0.183(3) Uani 1 1 d . . . O12 O 0.6434(5) 0.2738(7) 0.2004(4) 0.165(3) Uani 1 1 d . . . O13 O 0.4349(5) 0.2730(4) 0.2319(4) 0.1215(18) 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 C1 0.173(7) 0.051(4) 0.090(5) 0.000(3) -0.063(5) -0.040(4) C2 0.079(4) 0.054(3) 0.035(3) 0.003(2) -0.018(3) -0.026(3) C3 0.095(5) 0.068(4) 0.045(3) 0.005(3) -0.030(3) -0.026(3) C4 0.111(6) 0.102(6) 0.050(4) 0.006(4) -0.027(4) -0.039(5) C5 0.081(4) 0.124(6) 0.031(3) -0.012(3) -0.025(3) -0.038(4) C6 0.054(3) 0.090(4) 0.029(3) -0.020(3) 0.003(2) -0.035(3) C7 0.048(3) 0.072(4) 0.031(3) -0.012(3) -0.006(2) -0.030(3) C8 0.064(4) 0.126(6) 0.030(3) -0.031(3) -0.003(3) -0.050(4) C9 0.106(5) 0.125(6) 0.073(4) -0.071(4) 0.015(4) -0.069(5) C10 0.099(5) 0.108(5) 0.090(5) -0.077(4) 0.005(4) -0.054(4) C11 0.056(3) 0.053(3) 0.080(4) -0.044(3) 0.009(3) -0.026(3) C12 0.043(3) 0.034(3) 0.060(3) -0.020(2) -0.002(2) -0.016(2) C13 0.060(4) 0.035(3) 0.079(4) -0.018(3) -0.002(3) -0.014(3) C14 0.059(3) 0.030(3) 0.063(3) 0.004(2) -0.013(3) -0.007(2) C15 0.036(3) 0.044(3) 0.043(3) -0.003(2) -0.004(2) -0.013(2) C16 0.037(3) 0.030(2) 0.035(2) -0.0096(19) -0.005(2) -0.015(2) C17 0.032(2) 0.032(2) 0.039(2) -0.016(2) 0.001(2) -0.0114(19) C18 0.055(3) 0.057(3) 0.041(3) -0.023(2) -0.015(2) -0.013(3) C19 0.090(5) 0.092(5) 0.053(3) -0.002(3) -0.035(3) -0.026(4) C20 0.038(3) 0.056(3) 0.041(3) -0.027(2) 0.004(2) -0.023(2) C21 0.058(4) 0.100(5) 0.056(3) -0.044(3) 0.006(3) -0.042(3) C22 0.093(5) 0.108(6) 0.094(5) -0.080(5) 0.024(4) -0.064(4) C23 0.093(5) 0.066(4) 0.096(5) -0.049(4) 0.022(4) -0.055(4) C24 0.051(3) 0.044(3) 0.072(3) -0.034(3) 0.007(3) -0.027(2) C25 0.027(2) 0.041(3) 0.046(3) -0.023(2) 0.003(2) -0.015(2) C26 0.044(3) 0.030(3) 0.083(4) -0.014(3) 0.006(3) -0.017(2) C27 0.053(3) 0.044(3) 0.062(4) 0.019(3) -0.020(3) -0.008(3) C28 0.045(3) 0.074(4) 0.048(3) 0.012(3) -0.010(3) -0.015(3) C29 0.033(3) 0.117(6) 0.039(3) -0.030(3) 0.000(2) -0.020(3) C30 0.033(3) 0.097(5) 0.046(3) -0.045(3) 0.001(2) -0.021(3) C31 0.047(3) 0.165(7) 0.065(4) -0.079(5) 0.004(3) -0.035(4) C32 0.076(5) 0.177(8) 0.119(6) -0.127(6) 0.021(4) -0.059(5) C33 0.058(4) 0.117(5) 0.121(6) -0.101(5) 0.019(4) -0.038(4) C34 0.044(3) 0.067(4) 0.077(4) -0.055(3) 0.003(3) -0.021(3) C35 0.025(2) 0.069(3) 0.053(3) -0.044(3) 0.004(2) -0.014(2) C36 0.106(5) 0.047(3) 0.158(6) -0.048(4) -0.012(5) -0.036(4) N1 0.055(3) 0.097(4) 0.047(3) -0.045(3) 0.005(2) -0.044(3) N2 0.059(3) 0.066(3) 0.056(3) -0.042(2) 0.004(2) -0.030(2) N3 0.036(2) 0.031(2) 0.049(2) -0.0039(19) -0.001(2) -0.0089(18) N4 0.031(2) 0.066(3) 0.039(2) -0.005(2) -0.0013(19) -0.015(2) N5 0.049(2) 0.0263(18) 0.0257(17) -0.0099(14) -0.0025(16) -0.0166(17) Ni1 0.0445(4) 0.0550(4) 0.0355(4) -0.0270(3) 0.0018(3) -0.0252(3) Ni2 0.0283(3) 0.0330(3) 0.0314(3) -0.0054(3) -0.0055(3) -0.0102(3) O1 0.126(3) 0.041(2) 0.051(2) 0.0026(17) -0.040(2) -0.030(2) O2 0.069(2) 0.055(2) 0.039(2) -0.0148(17) -0.0139(19) -0.028(2) O3 0.0476(18) 0.0330(17) 0.0320(15) -0.0150(13) -0.0073(14) -0.0153(15) O4 0.067(2) 0.0376(19) 0.0393(18) -0.0136(14) -0.0217(17) -0.0153(17) O5 0.066(2) 0.053(2) 0.043(2) -0.0090(17) -0.0249(18) -0.011(2) O6 0.0448(18) 0.0266(16) 0.0333(16) -0.0109(13) -0.0107(14) -0.0152(14) O7 0.047(2) 0.0405(19) 0.0437(19) -0.0222(15) -0.0099(16) -0.0137(16) O8 0.080(3) 0.041(2) 0.084(3) -0.0293(19) -0.014(2) -0.0258(19) O14 0.274(8) 0.058(4) 0.353(10) -0.006(5) -0.165(8) -0.064(5) Cl1 0.0811(11) 0.0578(9) 0.0952(11) -0.0233(8) -0.0336(9) -0.0272(8) O11 0.173(6) 0.328(10) 0.124(5) -0.129(6) -0.005(4) -0.115(6) O12 0.098(4) 0.260(8) 0.161(5) -0.109(5) -0.018(4) -0.047(5) O13 0.151(4) 0.113(4) 0.149(5) -0.027(3) -0.050(4) -0.089(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.429(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.359(6) . ? C2 C3 1.380(7) . ? C2 C7 1.424(7) . ? C3 C4 1.363(8) . ? C3 H3 0.9300 . ? C4 C5 1.367(8) . ? C4 H4 0.9300 . ? C5 C6 1.416(7) . ? C5 H5 0.9300 . ? C6 C7 1.404(7) . ? C6 C8 1.412(8) . ? C7 O2 1.306(6) . ? C8 N1 1.301(7) . ? C8 H8 0.9300 . ? C9 N1 1.459(7) . ? C9 C10 1.481(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.487(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.279(6) . ? C11 C12 1.425(7) . ? C11 H11 0.9300 . ? C12 C13 1.404(7) . ? C12 C17 1.414(6) . ? C13 C14 1.350(7) . ? C13 H13 0.9300 . ? C14 C15 1.415(7) . ? C14 H14 0.9300 . ? C15 C16 1.383(6) . ? C15 H15 0.9300 . ? C16 O4 1.362(5) . ? C16 C17 1.414(6) . ? C17 O3 1.315(5) . ? C18 O4 1.420(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O5 1.422(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O5 1.354(5) . ? C20 C21 1.378(7) . ? C20 C25 1.422(6) . ? C21 C22 1.407(8) . ? C21 H21 0.9300 . ? C22 C23 1.338(9) . ? C22 H22 0.9300 . ? C23 C24 1.429(7) . ? C23 H23 0.9300 . ? C24 C25 1.403(6) . ? C24 C26 1.420(7) . ? C25 O6 1.304(5) . ? C26 N3 1.279(7) . ? C26 H26 0.9300 . ? C27 C28 1.483(7) . ? C27 N3 1.483(6) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N4 1.461(6) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N4 1.289(7) . ? C29 C30 1.423(8) . ? C29 H29 0.9300 . ? C30 C35 1.406(7) . ? C30 C31 1.411(7) . ? C31 C32 1.357(9) . ? C31 H31 0.9300 . ? C32 C33 1.376(10) . ? C32 H32 0.9300 . ? C33 C34 1.370(7) . ? C33 H33 0.9300 . ? C34 O8 1.385(6) . ? C34 C35 1.416(7) . ? C35 O7 1.304(5) . ? C36 O8 1.426(6) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? N1 Ni1 1.860(4) . ? N2 Ni1 1.846(4) . ? N3 Ni2 1.841(4) . ? N4 Ni2 1.850(4) . ? N5 H1N 1.051(15) . ? N5 H2N 1.049(15) . ? N5 H3N 1.05(3) . ? N5 H4N 1.05(3) . ? Ni1 O3 1.842(3) . ? Ni1 O2 1.866(3) . ? Ni2 O6 1.843(3) . ? Ni2 O7 1.850(3) . ? O14 Cl1 1.373(5) . ? Cl1 O11 1.375(6) . ? Cl1 O13 1.402(4) . ? Cl1 O12 1.413(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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.3(5) . . ? O1 C2 C7 114.3(4) . . ? C3 C2 C7 120.3(6) . . ? C4 C3 C2 121.6(6) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 120.4(6) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 119.8(6) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C8 120.5(5) . . ? C7 C6 C5 120.7(6) . . ? C8 C6 C5 118.7(5) . . ? O2 C7 C6 124.5(5) . . ? O2 C7 C2 118.4(5) . . ? C6 C7 C2 117.1(5) . . ? N1 C8 C6 126.7(5) . . ? N1 C8 H8 116.7 . . ? C6 C8 H8 116.7 . . ? N1 C9 C10 108.4(4) . . ? N1 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? N1 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C9 C10 N2 107.4(4) . . ? C9 C10 H10A 110.2 . . ? N2 C10 H10A 110.2 . . ? C9 C10 H10B 110.2 . . ? N2 C10 H10B 110.2 . . ? H10A C10 H10B 108.5 . . ? N2 C11 C12 126.2(5) . . ? N2 C11 H11 116.9 . . ? C12 C11 H11 116.9 . . ? C13 C12 C17 119.8(5) . . ? C13 C12 C11 119.6(5) . . ? C17 C12 C11 120.6(4) . . ? C14 C13 C12 121.2(5) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 120.7(5) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 118.8(5) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? O4 C16 C15 123.6(4) . . ? O4 C16 C17 114.8(3) . . ? C15 C16 C17 121.7(4) . . ? O3 C17 C16 118.4(4) . . ? O3 C17 C12 123.8(4) . . ? C16 C17 C12 117.8(4) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C20 C21 124.9(5) . . ? O5 C20 C25 114.6(4) . . ? C21 C20 C25 120.5(5) . . ? C20 C21 C22 120.2(6) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 120.5(5) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 121.0(6) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C26 121.5(4) . . ? C25 C24 C23 119.4(5) . . ? C26 C24 C23 119.0(5) . . ? O6 C25 C24 124.1(4) . . ? O6 C25 C20 117.6(4) . . ? C24 C25 C20 118.3(4) . . ? N3 C26 C24 125.3(5) . . ? N3 C26 H26 117.4 . . ? C24 C26 H26 117.4 . . ? C28 C27 N3 106.7(4) . . ? C28 C27 H27A 110.4 . . ? N3 C27 H27A 110.4 . . ? C28 C27 H27B 110.4 . . ? N3 C27 H27B 110.4 . . ? H27A C27 H27B 108.6 . . ? N4 C28 C27 106.5(4) . . ? N4 C28 H28A 110.4 . . ? C27 C28 H28A 110.4 . . ? N4 C28 H28B 110.4 . . ? C27 C28 H28B 110.4 . . ? H28A C28 H28B 108.6 . . ? N4 C29 C30 127.3(5) . . ? N4 C29 H29 116.4 . . ? C30 C29 H29 116.4 . . ? C35 C30 C31 120.0(6) . . ? C35 C30 C29 119.6(5) . . ? C31 C30 C29 120.4(6) . . ? C32 C31 C30 120.5(6) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 120.7(6) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C34 C33 C32 120.2(7) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 O8 124.1(6) . . ? C33 C34 C35 121.5(6) . . ? O8 C34 C35 114.5(4) . . ? O7 C35 C30 125.2(5) . . ? O7 C35 C34 117.6(5) . . ? C30 C35 C34 117.2(5) . . ? O8 C36 H36A 109.5 . . ? O8 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? O8 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C8 N1 C9 121.1(5) . . ? C8 N1 Ni1 126.3(4) . . ? C9 N1 Ni1 112.2(4) . . ? C11 N2 C10 119.4(5) . . ? C11 N2 Ni1 127.1(4) . . ? C10 N2 Ni1 113.4(4) . . ? C26 N3 C27 120.4(5) . . ? C26 N3 Ni2 126.8(4) . . ? C27 N3 Ni2 112.6(4) . . ? C29 N4 C28 121.3(5) . . ? C29 N4 Ni2 125.7(4) . . ? C28 N4 Ni2 112.8(4) . . ? H1N N5 H2N 109(3) . . ? H1N N5 H3N 109(3) . . ? H2N N5 H3N 109(3) . . ? H1N N5 H4N 109(3) . . ? H2N N5 H4N 109(3) . . ? H3N N5 H4N 109(3) . . ? O3 Ni1 N2 94.25(17) . . ? O3 Ni1 N1 177.58(16) . . ? N2 Ni1 N1 86.6(2) . . ? O3 Ni1 O2 85.64(13) . . ? N2 Ni1 O2 177.56(17) . . ? N1 Ni1 O2 93.58(19) . . ? N3 Ni2 O6 94.81(17) . . ? N3 Ni2 N4 86.3(2) . . ? O6 Ni2 N4 175.76(16) . . ? N3 Ni2 O7 175.35(15) . . ? O6 Ni2 O7 84.66(13) . . ? N4 Ni2 O7 94.57(18) . . ? C2 O1 C1 117.3(4) . . ? C7 O2 Ni1 128.0(3) . . ? C17 O3 Ni1 128.1(3) . . ? C16 O4 C18 118.9(3) . . ? C20 O5 C19 119.0(4) . . ? C25 O6 Ni2 126.8(3) . . ? C35 O7 Ni2 127.3(3) . . ? C34 O8 C36 117.2(4) . . ? O14 Cl1 O11 111.3(5) . . ? O14 Cl1 O13 105.6(4) . . ? O11 Cl1 O13 112.2(4) . . ? O14 Cl1 O12 108.5(5) . . ? O11 Cl1 O12 108.2(4) . . ? O13 Cl1 O12 111.1(4) . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 26.04 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.304 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.057 # Attachment 'C1b_au2.cif' data_shelxlC1b _database_code_depnum_ccdc_archive 'CCDC 809435' #TrackingRef 'C1b_au2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 F6 N5 Ni2 O8 P' _chemical_formula_weight 933.12 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 11.6795(12) _cell_length_b 12.8729(14) _cell_length_c 15.7482(19) _cell_angle_alpha 66.151(9) _cell_angle_beta 73.257(9) _cell_angle_gamma 64.351(8) _cell_volume 1933.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7354 _cell_measurement_theta_min 2.80 _cell_measurement_theta_max 26.80 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8314 _exptl_absorpt_correction_T_max 0.8945 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14849 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.1256 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 26.81 _reflns_number_total 7767 _reflns_number_gt 4019 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The geometrical restrains were used for the refinement of the ammonium ion. The N-H bond distance were restrained according to [R.J.C. Brown, J.Mol.Struct.(1995) 345, 77.] ; _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^)+(0.0284P)^2^+0.0000P] 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 7767 _refine_ls_number_parameters 539 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1366 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 0.892 _refine_ls_restrained_S_all 0.891 _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 C1 C 0.4659(4) 0.4931(4) 0.4065(4) 0.0468(13) Uani 1 1 d . . . H1A H 0.4465 0.5780 0.3938 0.070 Uiso 1 1 calc R . . H1B H 0.5525 0.4475 0.4200 0.070 Uiso 1 1 calc R . . H1C H 0.4082 0.4652 0.4595 0.070 Uiso 1 1 calc R . . C2 C 0.4751(4) 0.3598(4) 0.3312(3) 0.0352(10) Uani 1 1 d . . . C3 C 0.5206(4) 0.2582(4) 0.4040(4) 0.0478(13) Uani 1 1 d . . . H3 H 0.5376 0.2652 0.4552 0.057 Uiso 1 1 calc R . . C4 C 0.5420(5) 0.1430(4) 0.4027(4) 0.0601(15) Uani 1 1 d . . . H4 H 0.5707 0.0740 0.4535 0.072 Uiso 1 1 calc R . . C5 C 0.5205(5) 0.1328(4) 0.3263(5) 0.0603(16) Uani 1 1 d . . . H5 H 0.5370 0.0562 0.3245 0.072 Uiso 1 1 calc R . . C6 C 0.4741(4) 0.2358(4) 0.2509(4) 0.0481(13) Uani 1 1 d . . . C7 C 0.4490(4) 0.3532(4) 0.2514(3) 0.0354(10) Uani 1 1 d . . . C8 C 0.4536(5) 0.2227(5) 0.1704(5) 0.0583(15) Uani 1 1 d . . . H8 H 0.4708 0.1438 0.1732 0.070 Uiso 1 1 calc R . . C9 C 0.3941(7) 0.2763(7) 0.0219(5) 0.090(2) Uani 1 1 d . . . H9A H 0.4616 0.2011 0.0156 0.108 Uiso 1 1 calc R . . H9B H 0.3125 0.2651 0.0382 0.108 Uiso 1 1 calc R . . C10 C 0.3951(7) 0.3750(7) -0.0654(5) 0.094(2) Uani 1 1 d . . . H10A H 0.3458 0.3767 -0.1065 0.112 Uiso 1 1 calc R . . H10B H 0.4824 0.3626 -0.0966 0.112 Uiso 1 1 calc R . . C11 C 0.2909(5) 0.5916(7) -0.1083(4) 0.0707(18) Uani 1 1 d . . . H11 H 0.2820 0.5863 -0.1631 0.085 Uiso 1 1 calc R . . C12 C 0.2488(5) 0.7123(6) -0.1033(4) 0.0594(15) Uani 1 1 d . . . C13 C 0.1975(6) 0.8141(8) -0.1795(4) 0.088(2) Uani 1 1 d . . . H13 H 0.1862 0.8019 -0.2304 0.105 Uiso 1 1 calc R . . C14 C 0.1637(7) 0.9303(7) -0.1806(5) 0.096(2) Uani 1 1 d . . . H14 H 0.1286 0.9970 -0.2309 0.115 Uiso 1 1 calc R . . C15 C 0.1836(6) 0.9457(6) -0.1042(4) 0.0758(18) Uani 1 1 d . . . H15 H 0.1631 1.0242 -0.1046 0.091 Uiso 1 1 calc R . . C16 C 0.2316(5) 0.8503(5) -0.0295(4) 0.0567(14) Uani 1 1 d . . . C17 C 0.2671(5) 0.7275(5) -0.0252(4) 0.0481(13) Uani 1 1 d . . . C18 C 0.2394(7) 0.9773(5) 0.0441(5) 0.089(2) Uani 1 1 d . . . H18A H 0.2576 0.9715 0.1019 0.133 Uiso 1 1 calc R . . H18B H 0.1529 1.0320 0.0352 0.133 Uiso 1 1 calc R . . H18C H 0.2975 1.0075 -0.0070 0.133 Uiso 1 1 calc R . . C21 C 0.8985(6) 0.0498(4) 0.6863(5) 0.084(2) Uani 1 1 d . . . H21A H 0.9163 0.0184 0.7496 0.126 Uiso 1 1 calc R . . H21B H 0.9640 0.0000 0.6511 0.126 Uiso 1 1 calc R . . H21C H 0.8168 0.0488 0.6864 0.126 Uiso 1 1 calc R . . C22 C 0.8713(4) 0.2315(5) 0.5536(4) 0.0542(15) Uani 1 1 d . . . C23 C 0.8574(5) 0.1789(6) 0.4986(5) 0.078(2) Uani 1 1 d . . . H23 H 0.8666 0.0972 0.5223 0.094 Uiso 1 1 calc R . . C24 C 0.8300(6) 0.2464(9) 0.4087(6) 0.098(3) Uani 1 1 d . . . H24 H 0.8181 0.2107 0.3726 0.117 Uiso 1 1 calc R . . C25 C 0.8202(5) 0.3641(8) 0.3722(5) 0.088(2) Uani 1 1 d . . . H25 H 0.8048 0.4081 0.3105 0.106 Uiso 1 1 calc R . . C26 C 0.8332(4) 0.4210(6) 0.4274(4) 0.0579(15) Uani 1 1 d . . . C27 C 0.8584(4) 0.3567(5) 0.5182(4) 0.0430(13) Uani 1 1 d . . . C28 C 0.8233(4) 0.5466(6) 0.3866(4) 0.0676(18) Uani 1 1 d . . . H28 H 0.8119 0.5848 0.3237 0.081 Uiso 1 1 calc R . . C29 C 0.8313(5) 0.7327(5) 0.3774(4) 0.0731(18) Uani 1 1 d . . . H29A H 0.7855 0.7693 0.3238 0.088 Uiso 1 1 calc R . . H29B H 0.9190 0.7293 0.3550 0.088 Uiso 1 1 calc R . . C30 C 0.7684(6) 0.8053(5) 0.4425(5) 0.077(2) Uani 1 1 d . . . H30A H 0.6758 0.8332 0.4476 0.092 Uiso 1 1 calc R . . H30B H 0.7933 0.8757 0.4201 0.092 Uiso 1 1 calc R . . C31 C 0.8145(5) 0.7656(4) 0.5946(5) 0.0600(16) Uani 1 1 d . . . H31 H 0.7874 0.8499 0.5770 0.072 Uiso 1 1 calc R . . C32 C 0.8540(4) 0.6977(4) 0.6846(4) 0.0527(14) Uani 1 1 d . . . C33 C 0.8652(6) 0.7578(6) 0.7379(6) 0.077(2) Uani 1 1 d . . . H33 H 0.8396 0.8423 0.7160 0.093 Uiso 1 1 calc R . . C34 C 0.9131(6) 0.6937(7) 0.8210(6) 0.087(2) Uani 1 1 d . . . H34 H 0.9199 0.7347 0.8551 0.105 Uiso 1 1 calc R . . C35 C 0.9522(5) 0.5668(6) 0.8555(4) 0.0699(18) Uani 1 1 d . . . H35 H 0.9872 0.5233 0.9113 0.084 Uiso 1 1 calc R . . C36 C 0.9383(4) 0.5064(5) 0.8061(4) 0.0466(12) Uani 1 1 d . . . C37 C 0.8897(4) 0.5689(4) 0.7198(3) 0.0377(11) Uani 1 1 d . . . C38 C 1.0323(6) 0.3102(6) 0.9146(4) 0.088(2) Uani 1 1 d . . . H38A H 1.0521 0.2259 0.9247 0.132 Uiso 1 1 calc R . . H38B H 0.9748 0.3322 0.9672 0.132 Uiso 1 1 calc R . . H38C H 1.1098 0.3233 0.9078 0.132 Uiso 1 1 calc R . . F1 F 0.4140(4) 0.7859(3) 0.2356(4) 0.1225(19) Uani 1 1 d . . . F2 F 0.6229(4) 0.7166(4) 0.2347(5) 0.157(2) Uani 1 1 d . . . F3 F 0.5034(7) 0.7919(6) 0.3412(4) 0.195(3) Uani 1 1 d . . . F4 F 0.6094(4) 0.8950(3) 0.2311(4) 0.1243(18) Uani 1 1 d . . . F5 F 0.4039(4) 0.9627(3) 0.2273(5) 0.164(3) Uani 1 1 d . . . F6 F 0.5317(6) 0.8795(6) 0.1243(4) 0.181(2) Uani 1 1 d . . . N1 N 0.4144(4) 0.3075(4) 0.0961(4) 0.0538(12) Uani 1 1 d . . . N2 N 0.3386(4) 0.4924(5) -0.0459(4) 0.0593(13) Uani 1 1 d . . . N3 N 0.8290(4) 0.6106(4) 0.4297(3) 0.0560(12) Uani 1 1 d . . . N4 N 0.8125(4) 0.7221(4) 0.5358(4) 0.0540(12) Uani 1 1 d . . . N5 N 0.2371(3) 0.6677(3) 0.2302(3) 0.0404(9) Uani 1 1 d D . . Ni1 Ni 0.36738(6) 0.47241(6) 0.07097(5) 0.04137(19) Uani 1 1 d . . . Ni2 Ni 0.84825(5) 0.56084(5) 0.55375(5) 0.03634(17) Uani 1 1 d . . . O1 O 0.4518(3) 0.4759(3) 0.3267(2) 0.0459(9) Uani 1 1 d . . . O2 O 0.4041(3) 0.4541(2) 0.1845(2) 0.0376(8) Uani 1 1 d . . . O3 O 0.3127(3) 0.6386(3) 0.0490(2) 0.0491(9) Uani 1 1 d . . . O4 O 0.2544(4) 0.8592(3) 0.0475(3) 0.0687(12) Uani 1 1 d . . . O5 O 0.8960(3) 0.1722(3) 0.6444(3) 0.0622(11) Uani 1 1 d . . . O6 O 0.8709(3) 0.4007(3) 0.5760(2) 0.0424(8) Uani 1 1 d . . . O7 O 0.8813(3) 0.5064(2) 0.6750(2) 0.0338(7) Uani 1 1 d . . . O8 O 0.9739(3) 0.3824(3) 0.8328(3) 0.0565(10) Uani 1 1 d . . . P1 P 0.51148(15) 0.83811(12) 0.23542(13) 0.0618(4) Uani 1 1 d . . . H1N H 0.325(2) 0.596(3) 0.245(3) 0.15(3) Uiso 1 1 d D . . H4N H 0.165(3) 0.632(3) 0.247(3) 0.15(3) Uiso 1 1 d D . . H3N H 0.244(4) 0.718(3) 0.1586(8) 0.086(18) Uiso 1 1 d D . . H2N H 0.214(4) 0.725(3) 0.270(3) 0.17(3) Uiso 1 1 d 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 C1 0.055(3) 0.051(3) 0.043(3) -0.021(2) -0.017(3) -0.014(2) C2 0.033(2) 0.031(2) 0.041(3) -0.016(2) -0.004(2) -0.0087(19) C3 0.039(3) 0.050(3) 0.054(3) -0.017(3) -0.005(3) -0.016(2) C4 0.059(3) 0.033(3) 0.070(4) -0.006(3) -0.007(3) -0.012(2) C5 0.057(3) 0.036(3) 0.085(5) -0.027(3) -0.005(3) -0.010(2) C6 0.043(3) 0.040(3) 0.066(4) -0.029(3) 0.007(3) -0.017(2) C7 0.033(2) 0.035(2) 0.042(3) -0.021(2) -0.001(2) -0.0110(19) C8 0.058(3) 0.050(3) 0.082(5) -0.042(3) 0.008(3) -0.025(3) C9 0.114(6) 0.111(6) 0.093(6) -0.075(5) -0.002(5) -0.050(5) C10 0.126(6) 0.129(6) 0.072(5) -0.075(5) 0.018(5) -0.067(5) C11 0.069(4) 0.130(6) 0.039(4) -0.039(4) -0.001(3) -0.053(4) C12 0.055(3) 0.098(4) 0.031(3) -0.020(3) -0.003(3) -0.036(3) C13 0.085(5) 0.146(6) 0.038(3) -0.016(4) -0.024(3) -0.049(5) C14 0.102(5) 0.107(5) 0.056(4) 0.012(4) -0.039(4) -0.036(4) C15 0.088(4) 0.075(4) 0.048(4) 0.007(3) -0.030(4) -0.027(3) C16 0.063(4) 0.063(4) 0.044(3) -0.008(3) -0.017(3) -0.025(3) C17 0.049(3) 0.070(4) 0.030(3) -0.009(3) -0.008(2) -0.031(3) C18 0.137(6) 0.047(3) 0.093(5) -0.003(3) -0.054(5) -0.036(3) C21 0.102(5) 0.042(3) 0.126(6) -0.031(4) -0.029(5) -0.028(3) C22 0.039(3) 0.074(4) 0.073(4) -0.054(3) 0.003(3) -0.019(3) C23 0.056(4) 0.113(5) 0.104(6) -0.088(5) 0.006(4) -0.028(3) C24 0.067(4) 0.177(8) 0.118(7) -0.116(7) 0.012(4) -0.057(5) C25 0.043(3) 0.193(8) 0.064(4) -0.085(5) 0.004(3) -0.040(4) C26 0.030(3) 0.105(5) 0.046(3) -0.040(4) 0.006(2) -0.024(3) C27 0.028(2) 0.069(3) 0.047(3) -0.037(3) -0.003(2) -0.015(2) C28 0.028(3) 0.126(6) 0.037(3) -0.025(4) -0.003(2) -0.021(3) C29 0.051(3) 0.081(4) 0.042(3) 0.024(3) -0.011(3) -0.022(3) C30 0.057(4) 0.055(4) 0.068(5) 0.024(3) -0.014(4) -0.013(3) C31 0.041(3) 0.027(3) 0.093(5) -0.014(3) 0.011(3) -0.013(2) C32 0.041(3) 0.042(3) 0.085(4) -0.034(3) 0.008(3) -0.021(2) C33 0.080(4) 0.064(4) 0.115(6) -0.058(4) 0.020(4) -0.044(3) C34 0.098(5) 0.112(6) 0.104(6) -0.081(5) 0.030(5) -0.069(4) C35 0.070(4) 0.115(5) 0.064(4) -0.058(4) 0.010(3) -0.053(4) C36 0.046(3) 0.060(3) 0.047(3) -0.030(3) 0.004(2) -0.026(2) C37 0.029(2) 0.040(3) 0.047(3) -0.021(2) 0.005(2) -0.0161(19) C38 0.104(5) 0.103(5) 0.054(4) -0.006(4) -0.031(4) -0.040(4) F1 0.115(3) 0.075(2) 0.206(6) -0.019(3) -0.073(3) -0.051(2) F2 0.123(3) 0.116(3) 0.258(7) -0.103(4) -0.101(4) 0.020(3) F3 0.309(8) 0.276(7) 0.076(4) -0.038(4) -0.011(5) -0.200(6) F4 0.099(3) 0.103(3) 0.200(6) -0.047(3) -0.051(3) -0.045(2) F5 0.094(3) 0.072(3) 0.346(10) -0.093(4) -0.044(4) -0.015(2) F6 0.218(6) 0.234(6) 0.107(5) -0.020(5) -0.040(5) -0.117(5) N1 0.061(3) 0.068(3) 0.059(3) -0.047(3) 0.006(3) -0.031(2) N2 0.067(3) 0.088(4) 0.050(3) -0.041(3) 0.001(3) -0.040(3) N3 0.030(2) 0.073(3) 0.045(3) -0.002(2) -0.010(2) -0.014(2) N4 0.036(2) 0.038(2) 0.070(4) -0.008(2) 0.001(2) -0.0113(19) N5 0.058(2) 0.0280(19) 0.036(2) -0.0106(17) -0.0037(19) -0.0172(18) Ni1 0.0459(4) 0.0591(4) 0.0372(4) -0.0309(3) 0.0049(3) -0.0274(3) Ni2 0.0270(3) 0.0365(3) 0.0358(4) -0.0034(3) -0.0046(3) -0.0103(3) O1 0.068(2) 0.0385(18) 0.042(2) -0.0147(15) -0.0204(18) -0.0188(16) O2 0.0479(18) 0.0332(17) 0.0375(18) -0.0194(15) -0.0058(16) -0.0125(14) O3 0.070(2) 0.054(2) 0.031(2) -0.0130(17) -0.0140(19) -0.0253(18) O4 0.114(3) 0.045(2) 0.049(2) 0.0036(18) -0.037(2) -0.033(2) O5 0.071(2) 0.050(2) 0.086(3) -0.040(2) -0.007(2) -0.0260(18) O6 0.0442(19) 0.0457(19) 0.043(2) -0.0195(17) -0.0072(17) -0.0157(15) O7 0.0395(16) 0.0267(16) 0.0390(19) -0.0134(15) -0.0065(14) -0.0120(13) O8 0.066(2) 0.060(2) 0.045(2) -0.0175(19) -0.022(2) -0.0145(18) P1 0.0694(10) 0.0469(8) 0.0812(12) -0.0184(8) -0.0313(9) -0.0205(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.425(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.358(6) . ? C2 O1 1.373(5) . ? C2 C7 1.418(6) . ? C3 C4 1.401(6) . ? C3 H3 0.9300 . ? C4 C5 1.363(8) . ? C4 H4 0.9300 . ? C5 C6 1.391(7) . ? C5 H5 0.9300 . ? C6 C7 1.411(5) . ? C6 C8 1.441(7) . ? C7 O2 1.301(5) . ? C8 N1 1.270(7) . ? C8 H8 0.9300 . ? C9 C10 1.447(9) . ? C9 N1 1.485(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.487(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.261(7) . ? C11 C12 1.441(8) . ? C11 H11 0.9300 . ? C12 C17 1.406(6) . ? C12 C13 1.407(8) . ? C13 C14 1.366(8) . ? C13 H13 0.9300 . ? C14 C15 1.391(8) . ? C14 H14 0.9300 . ? C15 C16 1.350(7) . ? C15 H15 0.9300 . ? C16 O4 1.371(6) . ? C16 C17 1.427(7) . ? C17 O3 1.307(6) . ? C18 O4 1.433(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 O5 1.432(6) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 O5 1.370(7) . ? C22 C23 1.374(6) . ? C22 C27 1.429(7) . ? C23 C24 1.374(11) . ? C23 H23 0.9300 . ? C24 C25 1.351(10) . ? C24 H24 0.9300 . ? C25 C26 1.415(7) . ? C25 H25 0.9300 . ? C26 C27 1.374(8) . ? C26 C28 1.443(8) . ? C27 O6 1.317(5) . ? C28 N3 1.293(7) . ? C28 H28 0.9300 . ? C29 N3 1.459(6) . ? C29 C30 1.487(8) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N4 1.503(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 N4 1.271(7) . ? C31 C32 1.418(8) . ? C31 H31 0.9300 . ? C32 C33 1.414(7) . ? C32 C37 1.421(6) . ? C33 C34 1.362(10) . ? C33 H33 0.9300 . ? C34 C35 1.397(8) . ? C34 H34 0.9300 . ? C35 C36 1.380(6) . ? C35 H35 0.9300 . ? C36 O8 1.371(6) . ? C36 C37 1.407(7) . ? C37 O7 1.313(5) . ? C38 O8 1.407(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? F1 P1 1.552(3) . ? F2 P1 1.544(4) . ? F3 P1 1.515(6) . ? F4 P1 1.578(4) . ? F5 P1 1.533(4) . ? F6 P1 1.588(6) . ? N1 Ni1 1.845(4) . ? N2 Ni1 1.862(5) . ? N3 Ni2 1.842(5) . ? N4 Ni2 1.846(4) . ? N5 H1N 1.05(3) . ? N5 H4N 1.05(3) . ? N5 H3N 1.05(2) . ? N5 H2N 1.05(3) . ? Ni1 O3 1.857(3) . ? Ni1 O2 1.858(3) . ? Ni2 O7 1.843(3) . ? Ni2 O6 1.855(3) . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 124.3(4) . . ? C3 C2 C7 121.5(4) . . ? O1 C2 C7 114.2(4) . . ? C2 C3 C4 120.6(5) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 119.5(5) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.6(4) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 121.0(5) . . ? C5 C6 C8 119.7(4) . . ? C7 C6 C8 119.4(5) . . ? O2 C7 C6 124.9(4) . . ? O2 C7 C2 118.4(3) . . ? C6 C7 C2 116.7(4) . . ? N1 C8 C6 126.8(5) . . ? N1 C8 H8 116.6 . . ? C6 C8 H8 116.6 . . ? C10 C9 N1 108.3(5) . . ? C10 C9 H9A 110.0 . . ? N1 C9 H9A 110.0 . . ? C10 C9 H9B 110.0 . . ? N1 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? C9 C10 N2 109.4(5) . . ? C9 C10 H10A 109.8 . . ? N2 C10 H10A 109.8 . . ? C9 C10 H10B 109.8 . . ? N2 C10 H10B 109.8 . . ? H10A C10 H10B 108.2 . . ? N2 C11 C12 126.6(5) . . ? N2 C11 H11 116.7 . . ? C12 C11 H11 116.7 . . ? C17 C12 C13 120.6(6) . . ? C17 C12 C11 119.8(5) . . ? C13 C12 C11 119.5(5) . . ? C14 C13 C12 121.7(6) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C13 C14 C15 117.9(6) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? C16 C15 C14 122.1(6) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C15 C16 O4 124.9(5) . . ? C15 C16 C17 121.8(5) . . ? O4 C16 C17 113.3(4) . . ? O3 C17 C12 124.8(5) . . ? O3 C17 C16 119.2(4) . . ? C12 C17 C16 115.9(5) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O5 C22 C23 124.4(6) . . ? O5 C22 C27 114.9(4) . . ? C23 C22 C27 120.7(6) . . ? C22 C23 C24 120.3(7) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 120.6(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.3(7) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 120.6(6) . . ? C27 C26 C28 120.2(5) . . ? C25 C26 C28 119.2(6) . . ? O6 C27 C26 125.7(5) . . ? O6 C27 C22 116.8(5) . . ? C26 C27 C22 117.5(5) . . ? N3 C28 C26 125.7(5) . . ? N3 C28 H28 117.2 . . ? C26 C28 H28 117.2 . . ? N3 C29 C30 107.1(5) . . ? N3 C29 H29A 110.3 . . ? C30 C29 H29A 110.3 . . ? N3 C29 H29B 110.3 . . ? C30 C29 H29B 110.3 . . ? H29A C29 H29B 108.6 . . ? C29 C30 N4 106.4(4) . . ? C29 C30 H30A 110.5 . . ? N4 C30 H30A 110.5 . . ? C29 C30 H30B 110.5 . . ? N4 C30 H30B 110.5 . . ? H30A C30 H30B 108.6 . . ? N4 C31 C32 126.1(5) . . ? N4 C31 H31 116.9 . . ? C32 C31 H31 116.9 . . ? C33 C32 C31 119.6(5) . . ? C33 C32 C37 119.3(6) . . ? C31 C32 C37 120.9(4) . . ? C34 C33 C32 120.9(6) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 120.6(5) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 119.5(6) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? O8 C36 C35 124.6(5) . . ? O8 C36 C37 113.6(4) . . ? C35 C36 C37 121.7(5) . . ? O7 C37 C36 119.0(4) . . ? O7 C37 C32 123.1(4) . . ? C36 C37 C32 117.9(4) . . ? O8 C38 H38A 109.5 . . ? O8 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O8 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C8 N1 C9 119.0(5) . . ? C8 N1 Ni1 127.0(3) . . ? C9 N1 Ni1 113.9(4) . . ? C11 N2 C10 120.9(5) . . ? C11 N2 Ni1 127.0(4) . . ? C10 N2 Ni1 111.7(4) . . ? C28 N3 C29 119.8(5) . . ? C28 N3 Ni2 127.0(4) . . ? C29 N3 Ni2 113.0(4) . . ? C31 N4 C30 120.5(5) . . ? C31 N4 Ni2 127.0(4) . . ? C30 N4 Ni2 112.4(4) . . ? H1N N5 H4N 109(3) . . ? H1N N5 H3N 109(3) . . ? H4N N5 H3N 109(3) . . ? H1N N5 H2N 109(3) . . ? H4N N5 H2N 109(3) . . ? H3N N5 H2N 109(3) . . ? N1 Ni1 O3 177.30(19) . . ? N1 Ni1 O2 94.12(17) . . ? O3 Ni1 O2 85.45(12) . . ? N1 Ni1 N2 86.6(2) . . ? O3 Ni1 N2 93.93(19) . . ? O2 Ni1 N2 176.94(19) . . ? N3 Ni2 O7 175.49(16) . . ? N3 Ni2 N4 86.7(2) . . ? O7 Ni2 N4 94.39(18) . . ? N3 Ni2 O6 94.06(18) . . ? O7 Ni2 O6 85.22(13) . . ? N4 Ni2 O6 175.49(17) . . ? C2 O1 C1 118.4(4) . . ? C7 O2 Ni1 127.7(2) . . ? C17 O3 Ni1 127.6(3) . . ? C16 O4 C18 117.5(4) . . ? C22 O5 C21 117.4(4) . . ? C27 O6 Ni2 127.0(3) . . ? C37 O7 Ni2 127.7(3) . . ? C36 O8 C38 118.4(4) . . ? F3 P1 F5 96.9(4) . . ? F3 P1 F2 87.8(4) . . ? F5 P1 F2 175.3(4) . . ? F3 P1 F1 94.1(3) . . ? F5 P1 F1 89.9(2) . . ? F2 P1 F1 90.7(2) . . ? F3 P1 F4 88.1(3) . . ? F5 P1 F4 89.0(2) . . ? F2 P1 F4 90.2(2) . . ? F1 P1 F4 177.7(3) . . ? F3 P1 F6 175.4(4) . . ? F5 P1 F6 87.2(4) . . ? F2 P1 F6 88.1(3) . . ? F1 P1 F6 87.9(3) . . ? F4 P1 F6 89.9(3) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 26.81 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.431 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.059 # Attachment 'C1c_cs6.cif' data_shelxlC1c _database_code_depnum_ccdc_archive 'CCDC 809436' #TrackingRef 'C1c_cs6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H44 Cl N5 Ni2 O13' _chemical_formula_weight 1015.72 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 13.7451(5) _cell_length_b 14.0632(5) _cell_length_c 22.8343(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.607(3) _cell_angle_gamma 90.00 _cell_volume 4392.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27549 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.20 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.991 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6559 _exptl_absorpt_correction_T_max 0.8628 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53676 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 28.38 _reflns_number_total 10989 _reflns_number_gt 8113 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The geometrical restrains were used for the refinement of the ammonium ion. The N-H bond distance were restrained according to [R.J.C. Brown, J.Mol.Struct.(1995) 345, 77.] ; _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^)+(0.0555P)^2^+0.0000P] 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 10989 _refine_ls_number_parameters 613 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1060 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 C1 C 0.2768(2) 0.1989(3) 0.28412(13) 0.0610(8) Uani 1 1 d . . . H1A H 0.3410 0.1968 0.2711 0.092 Uiso 1 1 calc R . . H1B H 0.2674 0.1445 0.3084 0.092 Uiso 1 1 calc R . . H1C H 0.2698 0.2559 0.3064 0.092 Uiso 1 1 calc R . . C2 C 0.10985(19) 0.2008(2) 0.24458(11) 0.0437(6) Uani 1 1 d . . . C3 C 0.0765(2) 0.2116(3) 0.29876(13) 0.0621(8) Uani 1 1 d . . . H3 H 0.1210 0.2150 0.3321 0.075 Uiso 1 1 calc R . . C4 C -0.0232(3) 0.2175(3) 0.30441(14) 0.0782(11) Uani 1 1 d . . . H4 H -0.0447 0.2249 0.3415 0.094 Uiso 1 1 calc R . . C5 C -0.0891(2) 0.2127(3) 0.25660(13) 0.0647(9) Uani 1 1 d . . . H5 H -0.1555 0.2180 0.2609 0.078 Uiso 1 1 calc R . . C6 C -0.05719(19) 0.1997(2) 0.19975(11) 0.0438(6) Uani 1 1 d . . . C7 C 0.04335(18) 0.19202(18) 0.19320(10) 0.0386(5) Uani 1 1 d . . . C8 C -0.12882(18) 0.1989(2) 0.15055(11) 0.0429(6) Uani 1 1 d . . . H8 H -0.1936 0.2075 0.1578 0.051 Uiso 1 1 calc R . . C9 C -0.18785(17) 0.18972(19) 0.04980(11) 0.0407(5) Uani 1 1 d . . . C10 C -0.28444(19) 0.2146(2) 0.05586(14) 0.0524(7) Uani 1 1 d . . . H10 H -0.3037 0.2308 0.0925 0.063 Uiso 1 1 calc R . . C11 C -0.3512(2) 0.2146(3) 0.00649(15) 0.0628(8) Uani 1 1 d . . . H11 H -0.4160 0.2310 0.0099 0.075 Uiso 1 1 calc R . . C12 C -0.3227(2) 0.1905(3) -0.04775(15) 0.0672(9) Uani 1 1 d . . . H12 H -0.3686 0.1901 -0.0805 0.081 Uiso 1 1 calc R . . C13 C -0.2270(2) 0.1669(2) -0.05409(13) 0.0557(7) Uani 1 1 d . . . H13 H -0.2080 0.1521 -0.0910 0.067 Uiso 1 1 calc R . . C14 C -0.15937(18) 0.16552(19) -0.00487(11) 0.0416(5) Uani 1 1 d . . . C15 C -0.0218(2) 0.1130(2) -0.05083(11) 0.0449(6) Uani 1 1 d . . . H15 H -0.0646 0.1068 -0.0848 0.054 Uiso 1 1 calc R . . C16 C 0.0771(2) 0.0895(2) -0.05538(11) 0.0440(6) Uani 1 1 d . . . C17 C 0.1048(3) 0.0596(2) -0.11036(13) 0.0586(8) Uani 1 1 d . . . H17 H 0.0580 0.0556 -0.1425 0.070 Uiso 1 1 calc R . . C18 C 0.1993(3) 0.0364(2) -0.11681(13) 0.0622(8) Uani 1 1 d . . . H18 H 0.2166 0.0158 -0.1531 0.075 Uiso 1 1 calc R . . C19 C 0.2701(2) 0.0436(2) -0.06915(13) 0.0545(7) Uani 1 1 d . . . H19 H 0.3346 0.0275 -0.0738 0.065 Uiso 1 1 calc R . . C20 C 0.2458(2) 0.07422(19) -0.01518(12) 0.0448(6) Uani 1 1 d . . . C21 C 0.14732(19) 0.09732(18) -0.00641(10) 0.0392(5) Uani 1 1 d . . . C22 C 0.4091(2) 0.0599(3) 0.02919(17) 0.0693(9) Uani 1 1 d . . . H22A H 0.4469 0.0710 0.0662 0.104 Uiso 1 1 calc R . . H22B H 0.4349 0.0973 -0.0009 0.104 Uiso 1 1 calc R . . H22C H 0.4122 -0.0063 0.0192 0.104 Uiso 1 1 calc R . . C23 C 0.4668(2) 0.4242(3) 0.21439(18) 0.0766(11) Uani 1 1 d . . . H23A H 0.5038 0.4050 0.1829 0.115 Uiso 1 1 calc R . . H23B H 0.4829 0.3839 0.2479 0.115 Uiso 1 1 calc R . . H23C H 0.4822 0.4890 0.2248 0.115 Uiso 1 1 calc R . . C24 C 0.30212(18) 0.44148(19) 0.23601(12) 0.0431(6) Uani 1 1 d . . . C25 C 0.3293(2) 0.4715(2) 0.29228(13) 0.0492(6) Uani 1 1 d . . . H25 H 0.3953 0.4767 0.3052 0.059 Uiso 1 1 calc R . . C26 C 0.2594(2) 0.4946(2) 0.33071(12) 0.0533(7) Uani 1 1 d . . . H26 H 0.2788 0.5154 0.3687 0.064 Uiso 1 1 calc R . . C27 C 0.1632(2) 0.4862(2) 0.31187(12) 0.0515(7) Uani 1 1 d . . . H27 H 0.1167 0.4991 0.3378 0.062 Uiso 1 1 calc R . . C28 C 0.13233(19) 0.45830(19) 0.25340(11) 0.0415(5) Uani 1 1 d . . . C29 C 0.20155(17) 0.43606(18) 0.21408(11) 0.0382(5) Uani 1 1 d . . . C30 C 0.03083(19) 0.4573(2) 0.23527(12) 0.0445(6) Uani 1 1 d . . . H30 H -0.0112 0.4700 0.2638 0.053 Uiso 1 1 calc R . . C31 C -0.11188(18) 0.4471(2) 0.16843(13) 0.0470(6) Uani 1 1 d . . . C32 C -0.1796(2) 0.4689(3) 0.20782(17) 0.0671(9) Uani 1 1 d . . . H32 H -0.1597 0.4792 0.2474 0.081 Uiso 1 1 calc R . . C33 C -0.2767(2) 0.4748(3) 0.1868(2) 0.0805(11) Uani 1 1 d . . . H33 H -0.3228 0.4891 0.2127 0.097 Uiso 1 1 calc R . . C34 C -0.3069(2) 0.4599(3) 0.1285(2) 0.0756(11) Uani 1 1 d . . . H34 H -0.3730 0.4639 0.1155 0.091 Uiso 1 1 calc R . . C35 C -0.2405(2) 0.4390(2) 0.08894(17) 0.0616(8) Uani 1 1 d . . . H35 H -0.2611 0.4298 0.0493 0.074 Uiso 1 1 calc R . . C36 C -0.14164(18) 0.43184(19) 0.10949(14) 0.0464(6) Uani 1 1 d . . . C37 C -0.0806(2) 0.39641(19) 0.01833(13) 0.0492(6) Uani 1 1 d . . . H37 H -0.1448 0.4023 0.0017 0.059 Uiso 1 1 calc R . . C38 C -0.0092(2) 0.3728(2) -0.01999(12) 0.0488(6) Uani 1 1 d . . . C39 C -0.0400(3) 0.3578(2) -0.08070(13) 0.0627(9) Uani 1 1 d . . . H39 H -0.1055 0.3653 -0.0944 0.075 Uiso 1 1 calc R . . C40 C 0.0256(3) 0.3328(3) -0.11871(14) 0.0732(10) Uani 1 1 d . . . H40 H 0.0048 0.3234 -0.1583 0.088 Uiso 1 1 calc R . . C41 C 0.1236(3) 0.3213(2) -0.09863(14) 0.0674(9) Uani 1 1 d . . . H41 H 0.1677 0.3039 -0.1251 0.081 Uiso 1 1 calc R . . C42 C 0.1567(2) 0.3351(2) -0.04035(13) 0.0545(7) Uani 1 1 d . . . C43 C 0.0903(2) 0.36219(19) 0.00088(11) 0.0457(6) Uani 1 1 d . . . C44 C 0.3235(3) 0.3029(3) -0.05439(19) 0.0833(12) Uani 1 1 d . . . H44A H 0.3859 0.2974 -0.0318 0.125 Uiso 1 1 calc R . . H44B H 0.3260 0.3528 -0.0829 0.125 Uiso 1 1 calc R . . H44C H 0.3076 0.2439 -0.0742 0.125 Uiso 1 1 calc R . . C45 C 0.3754(6) 0.5220(7) 0.0668(4) 0.181(3) Uani 1 1 d . . . H45A H 0.3938 0.5591 0.0344 0.271 Uiso 1 1 calc R . . H45B H 0.3855 0.4558 0.0592 0.271 Uiso 1 1 calc R . . H45C H 0.4148 0.5403 0.1021 0.271 Uiso 1 1 calc R . . Cl1 Cl -0.05440(6) 0.67881(7) 0.32063(4) 0.0651(2) Uani 1 1 d . . . N1 N -0.11092(14) 0.18698(15) 0.09623(9) 0.0378(4) Uani 1 1 d . . . N2 N -0.05867(15) 0.14231(15) -0.00372(9) 0.0395(4) Uani 1 1 d . . . N3 N -0.00872(14) 0.44040(16) 0.18254(10) 0.0411(5) Uani 1 1 d . . . N4 N -0.06417(15) 0.41066(15) 0.07479(10) 0.0430(5) Uani 1 1 d . . . N5 N 0.27034(16) 0.24338(19) 0.11766(11) 0.0501(6) Uani 1 1 d D . . Ni1 Ni 0.00934(2) 0.15788(2) 0.070213(13) 0.03403(8) Uani 1 1 d . . . Ni2 Ni 0.05728(2) 0.40944(2) 0.117914(14) 0.03687(8) Uani 1 1 d . . . O1 O 0.20576(13) 0.19807(16) 0.23450(8) 0.0503(5) Uani 1 1 d . . . O2 O 0.07842(12) 0.17727(13) 0.14291(7) 0.0403(4) Uani 1 1 d . . . O3 O 0.12940(12) 0.12478(13) 0.04616(7) 0.0418(4) Uani 1 1 d . . . O4 O 0.31031(14) 0.08600(16) 0.03372(9) 0.0565(5) Uani 1 1 d . . . O5 O 0.36471(13) 0.41634(18) 0.19590(10) 0.0614(6) Uani 1 1 d . . . O6 O 0.17981(12) 0.41237(14) 0.15896(8) 0.0443(4) Uani 1 1 d . . . O7 O 0.12572(13) 0.37641(14) 0.05535(8) 0.0465(4) Uani 1 1 d . . . O8 O 0.25072(17) 0.32455(18) -0.01622(10) 0.0669(6) Uani 1 1 d . . . O9 O -0.0801(2) 0.5869(2) 0.34019(13) 0.0903(9) Uani 1 1 d . . . O10 O 0.0071(3) 0.6712(3) 0.27558(17) 0.1260(14) Uani 1 1 d . . . O11 O -0.0011(3) 0.7266(3) 0.36959(15) 0.1114(11) Uani 1 1 d . . . O12 O -0.1361(2) 0.7342(3) 0.30505(17) 0.1128(11) Uani 1 1 d . . . O13 O 0.2840(3) 0.5367(4) 0.0734(3) 0.164(2) Uani 1 1 d . . . H13A H 0.2626 0.4919 0.0912 0.247 Uiso 1 1 calc R . . H2N H 0.3450(7) 0.242(3) 0.1325(16) 0.15(2) Uiso 1 1 d D . . H1N H 0.230(2) 0.212(3) 0.1495(13) 0.15(2) Uiso 1 1 d D . . H3N H 0.247(3) 0.3141(11) 0.1109(19) 0.20(3) Uiso 1 1 d D . . H4N H 0.258(3) 0.206(3) 0.0780(10) 0.17(2) Uiso 1 1 d 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 C1 0.0573(16) 0.076(2) 0.0473(16) -0.0052(15) -0.0084(13) -0.0020(15) C2 0.0502(14) 0.0460(15) 0.0352(12) -0.0036(11) 0.0050(10) -0.0023(12) C3 0.0626(17) 0.089(2) 0.0352(14) -0.0101(15) 0.0053(12) -0.0024(17) C4 0.073(2) 0.128(4) 0.0370(15) -0.0140(19) 0.0190(14) -0.003(2) C5 0.0536(16) 0.097(3) 0.0469(16) -0.0068(17) 0.0221(13) -0.0028(17) C6 0.0456(13) 0.0498(15) 0.0375(12) -0.0019(11) 0.0110(10) -0.0016(11) C7 0.0465(13) 0.0376(13) 0.0323(11) -0.0015(10) 0.0074(9) 0.0006(10) C8 0.0397(12) 0.0464(15) 0.0444(13) 0.0002(11) 0.0129(10) -0.0048(11) C9 0.0384(12) 0.0382(13) 0.0451(13) 0.0038(10) 0.0019(10) -0.0057(10) C10 0.0397(13) 0.0565(18) 0.0609(17) 0.0044(14) 0.0041(12) -0.0045(12) C11 0.0420(14) 0.072(2) 0.073(2) 0.0103(17) -0.0020(14) -0.0041(14) C12 0.0538(17) 0.082(2) 0.062(2) 0.0141(17) -0.0146(14) -0.0044(16) C13 0.0570(16) 0.063(2) 0.0453(15) 0.0063(14) -0.0056(12) -0.0050(14) C14 0.0433(12) 0.0390(13) 0.0418(13) 0.0042(11) 0.0004(10) -0.0066(11) C15 0.0543(14) 0.0469(16) 0.0326(12) -0.0006(10) 0.0006(10) -0.0071(12) C16 0.0580(15) 0.0401(14) 0.0342(12) -0.0028(10) 0.0068(10) -0.0052(12) C17 0.074(2) 0.066(2) 0.0366(14) -0.0112(13) 0.0094(13) -0.0113(16) C18 0.079(2) 0.068(2) 0.0439(15) -0.0187(14) 0.0234(15) -0.0091(17) C19 0.0634(17) 0.0496(17) 0.0547(17) -0.0080(13) 0.0264(14) 0.0005(14) C20 0.0525(14) 0.0400(15) 0.0435(14) -0.0029(11) 0.0122(11) 0.0031(11) C21 0.0518(13) 0.0324(12) 0.0345(11) -0.0004(10) 0.0092(10) -0.0013(11) C22 0.0485(16) 0.085(3) 0.077(2) -0.0045(19) 0.0187(15) 0.0131(16) C23 0.0353(14) 0.107(3) 0.087(3) -0.027(2) -0.0002(15) 0.0005(16) C24 0.0401(12) 0.0430(14) 0.0449(14) -0.0035(11) -0.0023(10) -0.0003(11) C25 0.0482(14) 0.0469(16) 0.0495(15) -0.0039(12) -0.0107(11) -0.0002(12) C26 0.0668(18) 0.0530(18) 0.0378(13) -0.0058(12) -0.0062(12) 0.0022(14) C27 0.0629(17) 0.0523(17) 0.0394(13) -0.0061(12) 0.0058(12) 0.0015(13) C28 0.0447(13) 0.0404(14) 0.0392(12) -0.0023(10) 0.0037(10) 0.0013(11) C29 0.0395(12) 0.0362(13) 0.0379(12) -0.0028(10) -0.0020(9) 0.0002(10) C30 0.0420(13) 0.0487(16) 0.0440(14) -0.0031(11) 0.0097(10) 0.0013(11) C31 0.0358(12) 0.0420(15) 0.0634(17) 0.0013(12) 0.0054(11) -0.0028(11) C32 0.0404(14) 0.083(3) 0.079(2) -0.0082(19) 0.0127(14) -0.0027(15) C33 0.0388(15) 0.095(3) 0.111(3) -0.010(2) 0.0195(18) -0.0010(17) C34 0.0337(14) 0.077(3) 0.116(3) 0.006(2) 0.0019(17) -0.0028(14) C35 0.0431(14) 0.0580(19) 0.081(2) 0.0067(16) -0.0079(14) -0.0059(13) C36 0.0360(12) 0.0363(14) 0.0663(17) 0.0049(12) 0.0020(11) -0.0038(10) C37 0.0498(14) 0.0382(15) 0.0560(16) 0.0087(12) -0.0120(12) -0.0102(12) C38 0.0631(17) 0.0379(14) 0.0425(14) 0.0054(11) -0.0098(12) -0.0130(12) C39 0.088(2) 0.0506(19) 0.0441(16) 0.0098(13) -0.0187(15) -0.0163(16) C40 0.120(3) 0.059(2) 0.0377(15) 0.0030(14) -0.0060(18) -0.021(2) C41 0.109(3) 0.053(2) 0.0414(15) -0.0009(13) 0.0153(17) -0.0118(18) C42 0.079(2) 0.0423(15) 0.0431(14) 0.0016(12) 0.0123(13) -0.0098(14) C43 0.0641(16) 0.0348(14) 0.0375(13) 0.0024(10) 0.0020(11) -0.0064(12) C44 0.100(3) 0.073(2) 0.085(3) -0.002(2) 0.053(2) 0.007(2) C45 0.166(8) 0.229(10) 0.138(6) 0.027(6) -0.030(5) 0.030(7) Cl1 0.0560(4) 0.0715(6) 0.0718(5) -0.0045(4) 0.0267(4) 0.0020(4) N1 0.0375(10) 0.0373(11) 0.0388(10) 0.0021(8) 0.0048(8) -0.0038(8) N2 0.0469(11) 0.0352(11) 0.0358(10) 0.0015(8) 0.0016(8) -0.0043(9) N3 0.0363(10) 0.0392(12) 0.0481(12) -0.0006(9) 0.0049(9) 0.0001(8) N4 0.0413(10) 0.0350(11) 0.0509(12) 0.0048(9) -0.0045(9) -0.0044(9) N5 0.0418(11) 0.0566(15) 0.0529(13) -0.0098(11) 0.0088(10) 0.0024(10) Ni1 0.03733(15) 0.03555(16) 0.02940(14) 0.00025(12) 0.00421(11) -0.00037(13) Ni2 0.03462(14) 0.03753(17) 0.03771(16) -0.00097(13) -0.00029(11) -0.00143(13) O1 0.0455(9) 0.0675(13) 0.0367(9) -0.0084(9) -0.0015(7) 0.0002(9) O2 0.0384(8) 0.0535(11) 0.0293(8) -0.0033(7) 0.0049(6) 0.0020(7) O3 0.0439(9) 0.0516(11) 0.0303(8) -0.0039(7) 0.0064(7) 0.0049(8) O4 0.0439(10) 0.0759(15) 0.0511(11) -0.0088(10) 0.0109(8) 0.0140(10) O5 0.0343(9) 0.0882(17) 0.0609(12) -0.0207(12) 0.0007(8) 0.0000(10) O6 0.0357(8) 0.0575(12) 0.0393(9) -0.0105(8) 0.0009(7) 0.0029(8) O7 0.0472(10) 0.0545(12) 0.0374(9) -0.0028(8) 0.0026(7) -0.0011(8) O8 0.0706(14) 0.0782(17) 0.0548(12) -0.0050(11) 0.0219(11) 0.0029(12) O9 0.113(2) 0.0764(19) 0.0866(19) -0.0068(15) 0.0370(17) -0.0263(16) O10 0.148(3) 0.112(3) 0.136(3) 0.024(2) 0.103(3) 0.032(2) O11 0.114(2) 0.113(3) 0.102(2) 0.001(2) -0.0129(19) -0.037(2) O12 0.0703(17) 0.135(3) 0.133(3) 0.029(2) 0.0124(17) 0.0266(18) O13 0.097(3) 0.225(6) 0.168(4) 0.088(4) -0.005(3) -0.027(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 C1 O1 1.421(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.361(3) . ? C2 C3 1.369(4) . ? C2 C7 1.420(3) . ? C3 C4 1.392(5) . ? C3 H3 0.9300 . ? C4 C5 1.350(5) . ? C4 H4 0.9300 . ? C5 C6 1.422(4) . ? C5 H5 0.9300 . ? C6 C7 1.409(3) . ? C6 C8 1.420(4) . ? C7 O2 1.305(3) . ? C8 N1 1.299(3) . ? C8 H8 0.9300 . ? C9 C14 1.387(4) . ? C9 C10 1.393(4) . ? C9 N1 1.423(3) . ? C10 C11 1.383(4) . ? C10 H10 0.9300 . ? C11 C12 1.377(5) . ? C11 H11 0.9300 . ? C12 C13 1.378(4) . ? C12 H12 0.9300 . ? C13 C14 1.387(4) . ? C13 H13 0.9300 . ? C14 N2 1.420(3) . ? C15 N2 1.300(3) . ? C15 C16 1.412(4) . ? C15 H15 0.9300 . ? C16 C21 1.408(4) . ? C16 C17 1.412(4) . ? C17 C18 1.362(5) . ? C17 H17 0.9300 . ? C18 C19 1.391(5) . ? C18 H18 0.9300 . ? C19 C20 1.377(4) . ? C19 H19 0.9300 . ? C20 O4 1.366(3) . ? C20 C21 1.426(4) . ? C21 O3 1.307(3) . ? C22 O4 1.420(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 O5 1.430(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O5 1.363(3) . ? C24 C25 1.369(4) . ? C24 C29 1.426(3) . ? C25 C26 1.401(4) . ? C25 H25 0.9300 . ? C26 C27 1.354(4) . ? C26 H26 0.9300 . ? C27 C28 1.416(4) . ? C27 H27 0.9300 . ? C28 C29 1.406(3) . ? C28 C30 1.416(4) . ? C29 O6 1.308(3) . ? C30 N3 1.294(3) . ? C30 H30 0.9300 . ? C31 C36 1.385(4) . ? C31 C32 1.390(4) . ? C31 N3 1.426(3) . ? C32 C33 1.376(5) . ? C32 H32 0.9300 . ? C33 C34 1.373(6) . ? C33 H33 0.9300 . ? C34 C35 1.376(5) . ? C34 H34 0.9300 . ? C35 C36 1.397(4) . ? C35 H35 0.9300 . ? C36 N4 1.420(4) . ? C37 N4 1.303(4) . ? C37 C38 1.416(4) . ? C37 H37 0.9300 . ? C38 C43 1.411(4) . ? C38 C39 1.425(4) . ? C39 C40 1.357(5) . ? C39 H39 0.9300 . ? C40 C41 1.390(6) . ? C40 H40 0.9300 . ? C41 C42 1.377(4) . ? C41 H41 0.9300 . ? C42 O8 1.363(4) . ? C42 C43 1.426(4) . ? C43 O7 1.306(3) . ? C44 O8 1.422(4) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 O13 1.297(8) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? Cl1 O12 1.385(3) . ? Cl1 O10 1.398(3) . ? Cl1 O9 1.424(3) . ? Cl1 O11 1.441(3) . ? N1 Ni1 1.856(2) . ? N2 Ni1 1.861(2) . ? N3 Ni2 1.858(2) . ? N4 Ni2 1.853(2) . ? N5 H2N 1.049(15) . ? N5 H1N 1.05(2) . ? N5 H3N 1.051(15) . ? N5 H4N 1.05(2) . ? Ni1 O3 1.8489(16) . ? Ni1 O2 1.8503(16) . ? Ni2 O7 1.8450(18) . ? Ni2 O6 1.8462(17) . ? O13 H13A 0.8200 . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.8(2) . . ? O1 C2 C7 114.4(2) . . ? C3 C2 C7 120.7(2) . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 120.7(3) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C7 C6 C8 121.8(2) . . ? C7 C6 C5 120.0(2) . . ? C8 C6 C5 118.1(2) . . ? O2 C7 C6 123.8(2) . . ? O2 C7 C2 118.5(2) . . ? C6 C7 C2 117.7(2) . . ? N1 C8 C6 125.1(2) . . ? N1 C8 H8 117.4 . . ? C6 C8 H8 117.4 . . ? C14 C9 C10 120.4(2) . . ? C14 C9 N1 114.2(2) . . ? C10 C9 N1 125.4(2) . . ? C11 C10 C9 118.9(3) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.8(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C14 119.3(3) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C9 C14 C13 120.0(2) . . ? C9 C14 N2 113.6(2) . . ? C13 C14 N2 126.4(2) . . ? N2 C15 C16 126.2(2) . . ? N2 C15 H15 116.9 . . ? C16 C15 H15 116.9 . . ? C21 C16 C17 120.4(3) . . ? C21 C16 C15 120.9(2) . . ? C17 C16 C15 118.7(3) . . ? C18 C17 C16 120.7(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.7(3) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? O4 C20 C19 125.1(3) . . ? O4 C20 C21 114.0(2) . . ? C19 C20 C21 120.9(3) . . ? O3 C21 C16 125.2(2) . . ? O3 C21 C20 117.6(2) . . ? C16 C21 C20 117.2(2) . . ? O4 C22 H22A 109.5 . . ? O4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 H23A 109.5 . . ? O5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O5 C24 C25 125.3(2) . . ? O5 C24 C29 113.8(2) . . ? C25 C24 C29 120.8(2) . . ? C24 C25 C26 121.2(3) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 119.2(3) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 121.1(3) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C29 C28 C30 121.3(2) . . ? C29 C28 C27 120.3(2) . . ? C30 C28 C27 118.3(2) . . ? O6 C29 C28 124.5(2) . . ? O6 C29 C24 118.3(2) . . ? C28 C29 C24 117.2(2) . . ? N3 C30 C28 125.9(2) . . ? N3 C30 H30 117.1 . . ? C28 C30 H30 117.1 . . ? C36 C31 C32 120.7(3) . . ? C36 C31 N3 113.7(2) . . ? C32 C31 N3 125.6(3) . . ? C33 C32 C31 118.4(4) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C34 C33 C32 121.3(3) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 120.9(3) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C34 C35 C36 118.7(3) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C31 C36 C35 120.0(3) . . ? C31 C36 N4 114.1(2) . . ? C35 C36 N4 125.8(3) . . ? N4 C37 C38 125.8(3) . . ? N4 C37 H37 117.1 . . ? C38 C37 H37 117.1 . . ? C43 C38 C37 121.5(2) . . ? C43 C38 C39 119.9(3) . . ? C37 C38 C39 118.6(3) . . ? C40 C39 C38 120.5(3) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 C41 120.1(3) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C42 C41 C40 121.4(3) . . ? C42 C41 H41 119.3 . . ? C40 C41 H41 119.3 . . ? O8 C42 C41 125.9(3) . . ? O8 C42 C43 113.9(2) . . ? C41 C42 C43 120.2(3) . . ? O7 C43 C38 124.3(3) . . ? O7 C43 C42 117.8(3) . . ? C38 C43 C42 117.8(3) . . ? O8 C44 H44A 109.5 . . ? O8 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? O8 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O13 C45 H45A 109.5 . . ? O13 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? O13 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O12 Cl1 O10 112.8(2) . . ? O12 Cl1 O9 111.8(2) . . ? O10 Cl1 O9 110.4(2) . . ? O12 Cl1 O11 106.0(2) . . ? O10 Cl1 O11 108.0(3) . . ? O9 Cl1 O11 107.6(2) . . ? C8 N1 C9 120.8(2) . . ? C8 N1 Ni1 126.28(18) . . ? C9 N1 Ni1 112.81(16) . . ? C15 N2 C14 121.1(2) . . ? C15 N2 Ni1 125.86(19) . . ? C14 N2 Ni1 113.08(16) . . ? C30 N3 C31 121.1(2) . . ? C30 N3 Ni2 126.09(18) . . ? C31 N3 Ni2 112.83(18) . . ? C37 N4 C36 121.2(2) . . ? C37 N4 Ni2 125.7(2) . . ? C36 N4 Ni2 113.03(18) . . ? H2N N5 H1N 109(2) . . ? H2N N5 H3N 109(2) . . ? H1N N5 H3N 109(2) . . ? H2N N5 H4N 109(2) . . ? H1N N5 H4N 109(2) . . ? H3N N5 H4N 109(2) . . ? O3 Ni1 O2 84.78(7) . . ? O3 Ni1 N1 177.78(9) . . ? O2 Ni1 N1 94.32(8) . . ? O3 Ni1 N2 94.85(8) . . ? O2 Ni1 N2 178.08(9) . . ? N1 Ni1 N2 86.11(9) . . ? O7 Ni2 O6 83.68(8) . . ? O7 Ni2 N4 95.27(9) . . ? O6 Ni2 N4 177.61(9) . . ? O7 Ni2 N3 178.11(9) . . ? O6 Ni2 N3 94.79(8) . . ? N4 Ni2 N3 86.30(10) . . ? C2 O1 C1 117.8(2) . . ? C7 O2 Ni1 127.72(15) . . ? C21 O3 Ni1 126.94(16) . . ? C20 O4 C22 117.2(2) . . ? C24 O5 C23 116.6(2) . . ? C29 O6 Ni2 127.26(15) . . ? C43 O7 Ni2 127.23(18) . . ? C42 O8 C44 118.1(3) . . ? C45 O13 H13A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.38 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.325 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.052 # Attachment 'C2_au6.cif' data_shelxlC2 _database_code_depnum_ccdc_archive 'CCDC 809437' #TrackingRef 'C2_au6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H84 Cl3 N11 Ni4 O28' _chemical_formula_weight 1892.69 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 '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 14.8436(13) _cell_length_b 15.6993(12) _cell_length_c 17.3575(13) _cell_angle_alpha 97.492(6) _cell_angle_beta 97.828(7) _cell_angle_gamma 91.792(7) _cell_volume 3968.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12892 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 25.00 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.125 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7725 _exptl_absorpt_correction_T_max 0.8083 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30184 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.1179 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.39 _diffrn_reflns_theta_max 25.21 _reflns_number_total 13028 _reflns_number_gt 7130 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The geometrical restrains were used for the refinement of the ammonium ion. The N-H bond distance were restrained according to [R.J.C. Brown, J.Mol.Struct.(1995) 345, 77.] ; _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^)+(0.0330P)^2^+0.0000P] 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 13028 _refine_ls_number_parameters 1111 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1251 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 0.899 _refine_ls_restrained_S_all 0.897 _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 C1 C -0.0939(5) 0.3492(4) 0.5043(4) 0.088(2) Uani 1 1 d . . . H1A H -0.1280 0.3466 0.4529 0.132 Uiso 1 1 calc R . . H1B H -0.0599 0.4034 0.5179 0.132 Uiso 1 1 calc R . . H1C H -0.1350 0.3436 0.5418 0.132 Uiso 1 1 calc R . . C2 C 0.0225(4) 0.2752(3) 0.5741(3) 0.0476(15) Uani 1 1 d . . . C3 C 0.0332(5) 0.3349(4) 0.6411(4) 0.0663(19) Uani 1 1 d . . . H3 H 0.0013 0.3850 0.6420 0.080 Uiso 1 1 calc R . . C4 C 0.0916(5) 0.3201(4) 0.7069(4) 0.077(2) Uani 1 1 d . . . H4 H 0.0984 0.3606 0.7517 0.092 Uiso 1 1 calc R . . C5 C 0.1383(5) 0.2483(4) 0.7072(4) 0.0709(19) Uani 1 1 d . . . H5 H 0.1777 0.2400 0.7517 0.085 Uiso 1 1 calc R . . C6 C 0.1279(4) 0.1853(3) 0.6403(3) 0.0491(15) Uani 1 1 d . . . C7 C 0.0710(4) 0.1984(3) 0.5722(3) 0.0425(14) Uani 1 1 d . . . C8 C 0.1759(4) 0.1087(4) 0.6451(4) 0.0546(16) Uani 1 1 d . . . H8 H 0.2135 0.1041 0.6917 0.066 Uiso 1 1 calc R . . C9 C 0.2261(5) -0.0302(4) 0.6009(4) 0.070(2) Uani 1 1 d . . . H9A H 0.2865 -0.0205 0.5875 0.084 Uiso 1 1 calc R . . H9B H 0.2318 -0.0404 0.6552 0.084 Uiso 1 1 calc R . . C10 C 0.1785(4) -0.1042(4) 0.5492(4) 0.071(2) Uani 1 1 d . . . H10A H 0.1291 -0.1267 0.5732 0.086 Uiso 1 1 calc R . . H10B H 0.2202 -0.1495 0.5399 0.086 Uiso 1 1 calc R . . C11 C 0.1353(4) -0.1243(3) 0.4092(4) 0.0532(16) Uani 1 1 d . . . H11 H 0.1613 -0.1774 0.4098 0.064 Uiso 1 1 calc R . . C12 C 0.0910(4) -0.1051(3) 0.3369(4) 0.0513(16) Uani 1 1 d . . . C13 C 0.0888(5) -0.1664(4) 0.2676(4) 0.0680(19) Uani 1 1 d . . . H13 H 0.1212 -0.2159 0.2701 0.082 Uiso 1 1 calc R . . C14 C 0.0407(5) -0.1534(5) 0.1989(5) 0.079(2) Uani 1 1 d . . . H14 H 0.0406 -0.1941 0.1549 0.095 Uiso 1 1 calc R . . C15 C -0.0089(5) -0.0803(4) 0.1928(4) 0.070(2) Uani 1 1 d . . . H15 H -0.0425 -0.0723 0.1452 0.084 Uiso 1 1 calc R . . C16 C -0.0076(4) -0.0202(4) 0.2577(4) 0.0542(16) Uani 1 1 d . . . C17 C 0.0432(4) -0.0294(3) 0.3307(3) 0.0444(14) Uani 1 1 d . . . C18 C -0.1227(5) 0.0635(5) 0.1949(4) 0.094(3) Uani 1 1 d . . . H18A H -0.1501 0.1177 0.2048 0.141 Uiso 1 1 calc R . . H18B H -0.1687 0.0177 0.1878 0.141 Uiso 1 1 calc R . . H18C H -0.0943 0.0620 0.1483 0.141 Uiso 1 1 calc R . . C21 C 0.1364(4) 0.4398(3) 0.4764(3) 0.0595(18) Uani 1 1 d . . . H21A H 0.0940 0.4554 0.4343 0.089 Uiso 1 1 calc R . . H21B H 0.1866 0.4816 0.4886 0.089 Uiso 1 1 calc R . . H21C H 0.1066 0.4380 0.5219 0.089 Uiso 1 1 calc R . . C22 C 0.2310(4) 0.3236(3) 0.5062(3) 0.0367(13) Uani 1 1 d . . . C23 C 0.2614(4) 0.3639(4) 0.5813(3) 0.0539(16) Uani 1 1 d . . . H23 H 0.2390 0.4164 0.5990 0.065 Uiso 1 1 calc R . . C24 C 0.3248(4) 0.3263(4) 0.6299(3) 0.0632(18) Uani 1 1 d . . . H24 H 0.3454 0.3541 0.6801 0.076 Uiso 1 1 calc R . . C25 C 0.3579(4) 0.2490(4) 0.6054(3) 0.0577(17) Uani 1 1 d . . . H25 H 0.4003 0.2241 0.6390 0.069 Uiso 1 1 calc R . . C26 C 0.3281(4) 0.2071(3) 0.5298(3) 0.0395(13) Uani 1 1 d . . . C27 C 0.2646(3) 0.2445(3) 0.4787(3) 0.0352(13) Uani 1 1 d . . . C28 C 0.3634(4) 0.1265(3) 0.5052(3) 0.0496(15) Uani 1 1 d . . . H28 H 0.4042 0.1043 0.5421 0.060 Uiso 1 1 calc R . . C29 C 0.3887(6) -0.0002(4) 0.4201(5) 0.120(4) Uani 1 1 d . . . H29A H 0.4543 0.0108 0.4289 0.144 Uiso 1 1 calc R . . H29B H 0.3737 -0.0388 0.4563 0.144 Uiso 1 1 calc R . . C30 C 0.3640(6) -0.0385(5) 0.3472(4) 0.107(3) Uani 1 1 d . . . H30A H 0.3351 -0.0943 0.3490 0.128 Uiso 1 1 calc R . . H30B H 0.4183 -0.0480 0.3224 0.128 Uiso 1 1 calc R . . C31 C 0.2758(4) -0.0195(4) 0.2264(4) 0.0597(17) Uani 1 1 d . . . H31 H 0.3001 -0.0704 0.2069 0.072 Uiso 1 1 calc R . . C32 C 0.2130(4) 0.0189(3) 0.1730(3) 0.0517(16) Uani 1 1 d . . . C33 C 0.1884(5) -0.0220(4) 0.0944(4) 0.073(2) Uani 1 1 d . . . H33 H 0.2139 -0.0735 0.0780 0.087 Uiso 1 1 calc R . . C34 C 0.1287(6) 0.0132(5) 0.0435(4) 0.080(2) Uani 1 1 d . . . H34 H 0.1133 -0.0145 -0.0076 0.096 Uiso 1 1 calc R . . C35 C 0.0896(5) 0.0900(4) 0.0660(3) 0.0679(19) Uani 1 1 d . . . H35 H 0.0488 0.1134 0.0300 0.081 Uiso 1 1 calc R . . C36 C 0.1109(4) 0.1314(4) 0.1406(3) 0.0467(15) Uani 1 1 d . . . C37 C 0.1738(4) 0.0968(3) 0.1962(3) 0.0421(14) Uani 1 1 d . . . C38 C 0.0078(5) 0.2418(4) 0.1164(4) 0.076(2) Uani 1 1 d . . . H38A H -0.0119 0.2940 0.1428 0.115 Uiso 1 1 calc R . . H38B H -0.0434 0.2014 0.1004 0.115 Uiso 1 1 calc R . . H38C H 0.0336 0.2540 0.0710 0.115 Uiso 1 1 calc R . . C41 C 0.4291(4) 0.4112(3) 0.4547(3) 0.0605(18) Uani 1 1 d . . . H41A H 0.3895 0.4583 0.4574 0.091 Uiso 1 1 calc R . . H41B H 0.4909 0.4330 0.4585 0.091 Uiso 1 1 calc R . . H41C H 0.4235 0.3789 0.4973 0.091 Uiso 1 1 calc R . . C42 C 0.4566(4) 0.2862(3) 0.3697(3) 0.0399(13) Uani 1 1 d . . . C43 C 0.5191(4) 0.2595(4) 0.4262(3) 0.0546(16) Uani 1 1 d . . . H43 H 0.5272 0.2886 0.4771 0.066 Uiso 1 1 calc R . . C44 C 0.5708(4) 0.1886(4) 0.4077(4) 0.0675(19) Uani 1 1 d . . . H44 H 0.6128 0.1706 0.4464 0.081 Uiso 1 1 calc R . . C45 C 0.5601(4) 0.1463(4) 0.3344(4) 0.0629(19) Uani 1 1 d . . . H45 H 0.5950 0.0995 0.3225 0.075 Uiso 1 1 calc R . . C46 C 0.4958(4) 0.1726(3) 0.2750(3) 0.0446(14) Uani 1 1 d . . . C47 C 0.4426(3) 0.2430(3) 0.2919(3) 0.0347(13) Uani 1 1 d . . . C48 C 0.4862(4) 0.1242(3) 0.1993(4) 0.0595(18) Uani 1 1 d . . . H48 H 0.5235 0.0782 0.1920 0.071 Uiso 1 1 calc R . . C49 C 0.4238(6) 0.0801(4) 0.0653(4) 0.097(3) Uani 1 1 d . . . H49A H 0.4845 0.0723 0.0516 0.116 Uiso 1 1 calc R . . H49B H 0.3984 0.0244 0.0725 0.116 Uiso 1 1 calc R . . C50 C 0.3700(6) 0.1116(5) 0.0050(4) 0.102(3) Uani 1 1 d . . . H50A H 0.3281 0.0657 -0.0230 0.123 Uiso 1 1 calc R . . H50B H 0.4086 0.1291 -0.0315 0.123 Uiso 1 1 calc R . . C51 C 0.2550(5) 0.2149(4) -0.0167(3) 0.0630(18) Uani 1 1 d . . . H51 H 0.2438 0.1866 -0.0678 0.076 Uiso 1 1 calc R . . C52 C 0.2027(4) 0.2862(4) 0.0013(3) 0.0506(15) Uani 1 1 d . . . C53 C 0.1359(5) 0.3075(5) -0.0595(4) 0.072(2) Uani 1 1 d . . . H53 H 0.1280 0.2753 -0.1090 0.087 Uiso 1 1 calc R . . C54 C 0.0843(5) 0.3754(5) -0.0437(4) 0.082(2) Uani 1 1 d . . . H54 H 0.0393 0.3885 -0.0826 0.098 Uiso 1 1 calc R . . C55 C 0.0969(5) 0.4261(4) 0.0291(4) 0.074(2) Uani 1 1 d . . . H55 H 0.0621 0.4737 0.0376 0.089 Uiso 1 1 calc R . . C56 C 0.1603(4) 0.4064(4) 0.0883(3) 0.0495(15) Uani 1 1 d . . . C57 C 0.2159(4) 0.3359(4) 0.0748(3) 0.0437(14) Uani 1 1 d . . . C58 C 0.1221(5) 0.5235(4) 0.1797(4) 0.076(2) Uani 1 1 d . . . H58A H 0.1405 0.5495 0.2329 0.114 Uiso 1 1 calc R . . H58B H 0.0594 0.5034 0.1732 0.114 Uiso 1 1 calc R . . H58C H 0.1293 0.5651 0.1448 0.114 Uiso 1 1 calc R . . C61 C 0.6377(5) 0.4098(5) 0.3075(3) 0.078(2) Uani 1 1 d . . . H61A H 0.6211 0.4550 0.3450 0.117 Uiso 1 1 calc R . . H61B H 0.7001 0.4194 0.3004 0.117 Uiso 1 1 calc R . . H61C H 0.6303 0.3555 0.3262 0.117 Uiso 1 1 calc R . . C62 C 0.5932(4) 0.3485(4) 0.1731(3) 0.0479(15) Uani 1 1 d . . . C63 C 0.6540(4) 0.2856(4) 0.1783(4) 0.0628(18) Uani 1 1 d . . . H63 H 0.6902 0.2822 0.2258 0.075 Uiso 1 1 calc R . . C64 C 0.6620(5) 0.2259(4) 0.1122(5) 0.082(2) Uani 1 1 d . . . H64 H 0.7009 0.1810 0.1169 0.099 Uiso 1 1 calc R . . C65 C 0.6138(4) 0.2332(4) 0.0419(4) 0.0667(18) Uani 1 1 d . . . H65 H 0.6214 0.1948 -0.0020 0.080 Uiso 1 1 calc R . . C66 C 0.5518(4) 0.2993(3) 0.0348(3) 0.0456(14) Uani 1 1 d . . . C67 C 0.5391(4) 0.3584(3) 0.1002(3) 0.0416(14) Uani 1 1 d . . . C68 C 0.5060(4) 0.3089(3) -0.0420(3) 0.0462(15) Uani 1 1 d . . . H68 H 0.5194 0.2708 -0.0842 0.055 Uiso 1 1 calc R . . C69 C 0.4162(4) 0.3764(3) -0.1394(3) 0.0482(15) Uani 1 1 d . . . H69A H 0.4169 0.3221 -0.1732 0.058 Uiso 1 1 calc R . . H69B H 0.4549 0.4186 -0.1570 0.058 Uiso 1 1 calc R . . C70 C 0.3214(4) 0.4057(4) -0.1412(3) 0.0526(16) Uani 1 1 d . . . H70A H 0.3041 0.4334 -0.1875 0.063 Uiso 1 1 calc R . . H70B H 0.2789 0.3572 -0.1422 0.063 Uiso 1 1 calc R . . C71 C 0.2603(4) 0.5254(3) -0.0691(3) 0.0454(15) Uani 1 1 d . . . H71 H 0.2203 0.5263 -0.1151 0.054 Uiso 1 1 calc R . . C72 C 0.2510(4) 0.5874(3) -0.0035(3) 0.0417(14) Uani 1 1 d . . . C73 C 0.1865(4) 0.6510(4) -0.0123(4) 0.0632(18) Uani 1 1 d . . . H73 H 0.1482 0.6496 -0.0596 0.076 Uiso 1 1 calc R . . C74 C 0.1802(4) 0.7139(4) 0.0477(4) 0.0662(19) Uani 1 1 d . . . H74 H 0.1358 0.7540 0.0420 0.079 Uiso 1 1 calc R . . C75 C 0.2391(4) 0.7193(3) 0.1176(3) 0.0541(16) Uani 1 1 d . . . H75 H 0.2361 0.7646 0.1573 0.065 Uiso 1 1 calc R . . C76 C 0.3014(4) 0.6585(3) 0.1284(3) 0.0425(14) Uani 1 1 d . . . C77 C 0.3073(4) 0.5892(3) 0.0690(3) 0.0375(13) Uani 1 1 d . . . C78 C 0.3811(4) 0.7376(3) 0.2462(3) 0.0618(18) Uani 1 1 d . . . H78A H 0.4252 0.7295 0.2901 0.093 Uiso 1 1 calc R . . H78B H 0.3260 0.7565 0.2647 0.093 Uiso 1 1 calc R . . H78C H 0.4046 0.7802 0.2182 0.093 Uiso 1 1 calc R . . Cl1 Cl -0.07699(11) 0.39538(10) 0.28236(9) 0.0613(4) Uani 1 1 d . . . Cl2 Cl 0.30977(13) 0.61312(14) 0.40010(10) 0.0812(6) Uani 1 1 d . . . Cl3 Cl 0.59218(11) 0.90398(8) 0.21075(9) 0.0561(4) Uani 1 1 d . . . N1 N 0.1709(3) 0.0453(3) 0.5893(3) 0.0482(12) Uani 1 1 d . . . N2 N 0.1424(3) -0.0736(3) 0.4744(3) 0.0494(12) Uani 1 1 d . . . N3 N 0.3448(3) 0.0810(3) 0.4373(3) 0.0487(13) Uani 1 1 d . . . N4 N 0.3018(3) 0.0099(3) 0.2988(3) 0.0503(13) Uani 1 1 d . . . N5 N 0.4293(3) 0.1392(3) 0.1392(3) 0.0513(13) Uani 1 1 d . . . N6 N 0.3180(3) 0.1844(3) 0.0314(3) 0.0533(13) Uani 1 1 d . . . N7 N 0.4481(3) 0.3660(2) -0.0570(2) 0.0406(11) Uani 1 1 d . . . N8 N 0.3206(3) 0.4677(3) -0.0688(2) 0.0401(11) Uani 1 1 d . . . N11 N 0.0370(3) 0.2063(3) 0.3595(3) 0.0469(11) Uani 1 1 d D . . N12 N 0.2138(3) 0.3315(3) 0.2872(3) 0.0455(11) Uani 1 1 d D . . N13 N 0.3920(3) 0.4693(3) 0.2307(3) 0.0477(12) Uani 1 1 d D . . Ni1 Ni 0.10413(5) 0.03683(4) 0.48960(4) 0.03873(19) Uani 1 1 d . . . Ni2 Ni 0.26831(4) 0.10967(4) 0.35225(4) 0.03465(18) Uani 1 1 d . . . Ni3 Ni 0.35136(5) 0.22739(4) 0.13549(4) 0.03806(19) Uani 1 1 d . . . Ni4 Ni 0.40478(5) 0.44578(4) 0.01395(4) 0.03282(18) Uani 1 1 d . . . O1 O -0.0325(3) 0.2806(2) 0.5051(2) 0.0578(11) Uani 1 1 d . . . O2 O 0.0599(2) 0.1451(2) 0.5060(2) 0.0434(9) Uani 1 1 d . . . O3 O 0.0414(2) 0.0311(2) 0.3891(2) 0.0465(10) Uani 1 1 d . . . O4 O -0.0566(3) 0.0534(3) 0.2592(2) 0.0685(13) Uani 1 1 d . . . O5 O 0.1696(2) 0.3560(2) 0.45297(19) 0.0468(10) Uani 1 1 d . . . O6 O 0.2347(2) 0.21067(18) 0.40491(17) 0.0359(9) Uani 1 1 d . . . O7 O 0.1909(2) 0.1391(2) 0.26767(19) 0.0441(10) Uani 1 1 d . . . O8 O 0.0752(3) 0.2057(2) 0.1686(2) 0.0576(11) Uani 1 1 d . . . O9 O 0.4045(2) 0.3564(2) 0.38149(19) 0.0485(10) Uani 1 1 d . . . O10 O 0.3829(2) 0.27160(19) 0.24047(19) 0.0394(9) Uani 1 1 d . . . O11 O 0.2746(2) 0.3179(2) 0.13360(19) 0.0452(10) Uani 1 1 d . . . O12 O 0.1777(3) 0.4519(2) 0.1618(2) 0.0586(11) Uani 1 1 d . . . O13 O 0.5805(3) 0.4091(2) 0.2342(2) 0.0555(11) Uani 1 1 d . . . O14 O 0.4837(2) 0.42053(19) 0.09966(18) 0.0378(9) Uani 1 1 d . . . O15 O 0.3668(2) 0.53080(19) 0.08479(18) 0.0380(9) Uani 1 1 d . . . O16 O 0.3624(3) 0.6581(2) 0.1950(2) 0.0519(10) Uani 1 1 d . . . O21 O -0.1174(4) 0.3120(3) 0.2823(3) 0.1090(18) Uani 1 1 d . . . O22 O 0.0194(3) 0.3862(3) 0.2944(3) 0.1000(17) Uani 1 1 d . . . O23 O -0.0997(4) 0.4263(4) 0.2101(3) 0.1121(19) Uani 1 1 d . . . O24 O -0.1034(4) 0.4523(3) 0.3438(3) 0.116(2) Uani 1 1 d . . . O25 O 0.2602(4) 0.5350(5) 0.3517(3) 0.146(3) Uani 1 1 d . . . O26 O 0.4004(3) 0.6127(3) 0.3806(2) 0.0797(13) Uani 1 1 d . . . O27 O 0.3089(3) 0.6025(3) 0.4795(2) 0.0751(13) Uani 1 1 d . . . O28 O 0.2685(6) 0.6843(5) 0.3830(5) 0.191(4) Uani 1 1 d . . . O29 O 0.6368(4) 0.8264(3) 0.1965(3) 0.1015(18) Uani 1 1 d . . . O30 O 0.6482(3) 0.9745(3) 0.1976(3) 0.0764(13) Uani 1 1 d . . . O31 O 0.5082(3) 0.9009(3) 0.1593(3) 0.0936(16) Uani 1 1 d . . . O32 O 0.5763(4) 0.9170(3) 0.2906(3) 0.0928(16) Uani 1 1 d . . . H11N H 0.347(3) 0.500(3) 0.192(3) 0.28(6) Uiso 1 1 d D . . H1N H 0.1081(6) 0.210(3) 0.375(3) 0.11(2) Uiso 1 1 d D . . H3N H 0.019(3) 0.241(3) 0.312(2) 0.15(3) Uiso 1 1 d D . . H8N H 0.220(6) 0.317(4) 0.3449(15) 0.30(7) Uiso 1 1 d D . . H2N H 0.014(3) 0.1417(10) 0.343(3) 0.17(4) Uiso 1 1 d D . . H10N H 0.4581(16) 0.475(4) 0.216(3) 0.14(3) Uiso 1 1 d D . . H5N H 0.148(2) 0.313(4) 0.258(5) 0.34(8) Uiso 1 1 d D . . H7N H 0.262(4) 0.298(4) 0.257(5) 0.25(5) Uiso 1 1 d D . . H9N H 0.371(4) 0.4041(10) 0.226(3) 0.16(3) Uiso 1 1 d D . . H12N H 0.391(4) 0.499(3) 0.2885(13) 0.16(3) Uiso 1 1 d D . . H6N H 0.226(5) 0.3981(9) 0.288(4) 0.14(3) Uiso 1 1 d D . . H4N H 0.007(3) 0.233(3) 0.4080(19) 0.18(4) Uiso 1 1 d 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 C1 0.094(6) 0.069(4) 0.115(6) 0.026(4) 0.041(5) 0.051(4) C2 0.052(4) 0.041(3) 0.056(4) 0.011(3) 0.022(3) 0.008(3) C3 0.080(5) 0.044(3) 0.079(5) -0.006(4) 0.041(4) 0.005(3) C4 0.101(6) 0.069(5) 0.059(5) -0.011(4) 0.028(4) -0.003(4) C5 0.082(5) 0.075(4) 0.055(4) -0.001(4) 0.020(4) -0.006(4) C6 0.047(4) 0.045(3) 0.054(4) 0.000(3) 0.012(3) -0.007(3) C7 0.047(4) 0.037(3) 0.046(4) 0.006(3) 0.016(3) -0.001(3) C8 0.051(4) 0.066(4) 0.048(4) 0.014(3) 0.008(3) -0.002(3) C9 0.069(5) 0.056(4) 0.083(5) 0.028(4) -0.016(4) 0.014(3) C10 0.064(5) 0.050(4) 0.101(5) 0.027(4) -0.006(4) 0.010(3) C11 0.037(4) 0.038(3) 0.087(5) 0.008(3) 0.017(4) 0.007(3) C12 0.050(4) 0.033(3) 0.071(4) -0.007(3) 0.026(3) -0.006(3) C13 0.062(5) 0.052(4) 0.091(5) -0.011(4) 0.036(4) -0.004(3) C14 0.089(6) 0.071(5) 0.072(5) -0.019(4) 0.026(5) -0.022(4) C15 0.075(5) 0.074(5) 0.059(4) -0.001(4) 0.014(4) -0.025(4) C16 0.060(4) 0.045(3) 0.055(4) -0.003(3) 0.011(3) -0.011(3) C17 0.043(4) 0.039(3) 0.051(4) -0.004(3) 0.018(3) -0.006(3) C18 0.091(6) 0.123(6) 0.062(5) 0.027(4) -0.020(5) 0.000(5) C21 0.074(5) 0.040(3) 0.061(4) -0.009(3) 0.007(3) 0.018(3) C22 0.041(3) 0.038(3) 0.028(3) -0.002(2) 0.002(3) 0.005(2) C23 0.067(4) 0.056(3) 0.035(3) -0.008(3) 0.006(3) 0.003(3) C24 0.071(5) 0.078(4) 0.032(3) -0.009(3) -0.007(3) -0.006(4) C25 0.061(4) 0.073(4) 0.035(3) 0.011(3) -0.013(3) 0.001(3) C26 0.039(3) 0.043(3) 0.033(3) 0.004(2) -0.004(3) 0.003(3) C27 0.032(3) 0.038(3) 0.036(3) 0.005(2) 0.002(3) -0.002(2) C28 0.037(4) 0.054(3) 0.055(4) 0.016(3) -0.011(3) 0.006(3) C29 0.157(9) 0.068(5) 0.109(6) -0.024(5) -0.056(6) 0.076(5) C30 0.143(8) 0.081(5) 0.087(6) -0.013(5) -0.011(5) 0.073(5) C31 0.067(5) 0.039(3) 0.073(5) -0.007(3) 0.023(4) 0.004(3) C32 0.063(4) 0.045(3) 0.044(4) -0.008(3) 0.016(3) -0.015(3) C33 0.094(6) 0.057(4) 0.062(5) -0.018(4) 0.022(4) -0.011(4) C34 0.105(6) 0.090(5) 0.034(4) -0.021(4) 0.003(4) -0.026(5) C35 0.074(5) 0.081(5) 0.040(4) -0.003(3) -0.008(3) -0.009(4) C36 0.048(4) 0.057(4) 0.029(3) -0.002(3) -0.002(3) -0.014(3) C37 0.046(4) 0.044(3) 0.035(3) -0.001(3) 0.006(3) -0.006(3) C38 0.072(5) 0.091(5) 0.062(4) 0.019(4) -0.015(4) 0.008(4) C41 0.061(4) 0.059(4) 0.049(4) -0.022(3) -0.012(3) 0.007(3) C42 0.029(3) 0.046(3) 0.042(3) 0.004(3) -0.003(3) 0.000(2) C43 0.051(4) 0.059(4) 0.049(4) 0.009(3) -0.011(3) 0.005(3) C44 0.051(4) 0.070(4) 0.078(5) 0.018(4) -0.015(4) 0.021(3) C45 0.052(4) 0.060(4) 0.073(4) 0.008(4) -0.010(4) 0.030(3) C46 0.043(4) 0.035(3) 0.055(4) 0.002(3) 0.003(3) 0.010(3) C47 0.030(3) 0.030(3) 0.044(3) 0.008(2) -0.001(3) 0.006(2) C48 0.060(4) 0.039(3) 0.080(5) 0.002(3) 0.011(4) 0.026(3) C49 0.132(7) 0.072(5) 0.076(5) -0.032(4) 0.010(5) 0.043(5) C50 0.142(8) 0.094(6) 0.060(5) -0.022(4) -0.001(5) 0.047(5) C51 0.075(5) 0.077(4) 0.032(3) 0.000(3) 0.001(4) -0.016(4) C52 0.034(4) 0.065(4) 0.053(4) 0.016(3) 0.000(3) -0.001(3) C53 0.065(5) 0.099(5) 0.052(4) 0.017(4) 0.001(4) -0.011(4) C54 0.065(5) 0.108(6) 0.067(5) 0.021(4) -0.016(4) 0.016(5) C55 0.068(5) 0.085(5) 0.068(5) 0.023(4) -0.011(4) 0.017(4) C56 0.041(4) 0.056(3) 0.049(4) 0.019(3) -0.014(3) 0.008(3) C57 0.032(3) 0.068(4) 0.034(3) 0.018(3) 0.002(3) 0.001(3) C58 0.073(5) 0.071(4) 0.085(5) 0.013(4) 0.006(4) 0.039(4) C61 0.065(5) 0.111(5) 0.052(4) 0.017(4) -0.023(4) -0.003(4) C62 0.034(4) 0.055(4) 0.057(4) 0.018(3) 0.001(3) 0.012(3) C63 0.047(4) 0.077(4) 0.064(4) 0.021(4) -0.008(3) 0.018(3) C64 0.064(5) 0.082(5) 0.108(6) 0.034(5) 0.009(5) 0.043(4) C65 0.057(4) 0.057(4) 0.087(5) 0.007(4) 0.015(4) 0.020(3) C66 0.036(4) 0.044(3) 0.061(4) 0.016(3) 0.013(3) 0.009(3) C67 0.043(4) 0.033(3) 0.052(4) 0.013(3) 0.012(3) 0.002(3) C68 0.053(4) 0.034(3) 0.054(4) -0.003(3) 0.024(3) 0.000(3) C69 0.060(4) 0.049(3) 0.034(3) -0.007(3) 0.012(3) 0.004(3) C70 0.063(4) 0.058(3) 0.031(3) -0.011(3) 0.005(3) 0.003(3) C71 0.042(4) 0.051(3) 0.041(3) 0.013(3) -0.006(3) 0.004(3) C72 0.043(4) 0.044(3) 0.038(3) 0.003(3) 0.004(3) 0.009(3) C73 0.058(4) 0.063(4) 0.066(4) 0.003(3) -0.002(3) 0.027(3) C74 0.060(4) 0.063(4) 0.079(5) 0.014(4) 0.009(4) 0.035(3) C75 0.061(4) 0.041(3) 0.060(4) -0.004(3) 0.016(3) 0.016(3) C76 0.047(4) 0.037(3) 0.046(3) 0.004(3) 0.014(3) 0.006(3) C77 0.039(3) 0.034(3) 0.042(3) 0.007(2) 0.012(3) 0.004(2) C78 0.090(5) 0.044(3) 0.047(3) -0.011(3) 0.015(3) -0.003(3) Cl1 0.0542(11) 0.0675(10) 0.0601(10) 0.0111(8) -0.0040(8) 0.0130(8) Cl2 0.0564(12) 0.1294(16) 0.0629(12) 0.0222(11) 0.0134(10) 0.0249(11) Cl3 0.0677(11) 0.0399(8) 0.0572(10) 0.0041(7) -0.0028(9) 0.0092(7) N1 0.042(3) 0.053(3) 0.052(3) 0.018(2) 0.005(2) 0.007(2) N2 0.040(3) 0.037(2) 0.071(3) 0.005(3) 0.005(3) 0.005(2) N3 0.045(3) 0.042(2) 0.055(3) 0.003(2) -0.007(2) 0.014(2) N4 0.055(3) 0.037(2) 0.056(3) -0.002(2) 0.004(3) 0.011(2) N5 0.058(3) 0.043(3) 0.053(3) -0.004(2) 0.014(3) 0.011(2) N6 0.056(3) 0.062(3) 0.041(3) -0.004(2) 0.011(3) 0.006(3) N7 0.048(3) 0.031(2) 0.041(3) -0.002(2) 0.010(2) 0.000(2) N8 0.039(3) 0.047(3) 0.032(2) 0.003(2) -0.001(2) 0.004(2) N11 0.040(3) 0.049(3) 0.055(3) 0.015(2) 0.006(2) 0.013(2) N12 0.041(3) 0.052(3) 0.045(3) 0.011(2) 0.005(2) 0.010(2) N13 0.048(3) 0.049(3) 0.047(3) 0.009(2) 0.007(2) 0.002(2) Ni1 0.0338(4) 0.0322(3) 0.0505(4) 0.0080(3) 0.0038(3) 0.0065(3) Ni2 0.0327(4) 0.0290(3) 0.0400(4) 0.0000(3) 0.0007(3) 0.0049(3) Ni3 0.0357(4) 0.0407(4) 0.0367(4) 0.0009(3) 0.0050(3) 0.0037(3) Ni4 0.0364(4) 0.0303(3) 0.0305(4) 0.0000(3) 0.0038(3) 0.0034(3) O1 0.066(3) 0.039(2) 0.072(3) 0.0082(19) 0.017(2) 0.0286(19) O2 0.048(2) 0.0377(19) 0.046(2) 0.0072(17) 0.0073(19) 0.0124(17) O3 0.051(2) 0.0374(19) 0.050(2) 0.0006(18) 0.0037(19) 0.0115(17) O4 0.080(3) 0.072(3) 0.047(3) 0.009(2) -0.014(2) -0.003(2) O5 0.058(3) 0.0369(19) 0.041(2) -0.0062(17) -0.001(2) 0.0140(17) O6 0.041(2) 0.0338(18) 0.0280(19) -0.0038(15) -0.0075(17) 0.0092(15) O7 0.048(2) 0.047(2) 0.032(2) -0.0049(17) -0.0058(18) 0.0081(18) O8 0.061(3) 0.066(3) 0.040(2) 0.007(2) -0.015(2) 0.012(2) O9 0.048(2) 0.046(2) 0.045(2) -0.0093(17) -0.0063(19) 0.0181(18) O10 0.037(2) 0.0398(19) 0.037(2) -0.0012(16) -0.0051(18) 0.0108(16) O11 0.044(2) 0.054(2) 0.038(2) 0.0064(17) 0.0030(19) 0.0169(18) O12 0.058(3) 0.063(2) 0.053(3) 0.010(2) -0.002(2) 0.025(2) O13 0.050(3) 0.067(2) 0.047(2) 0.011(2) -0.009(2) 0.011(2) O14 0.039(2) 0.0362(19) 0.038(2) 0.0043(16) 0.0039(17) 0.0114(16) O15 0.043(2) 0.0385(18) 0.0317(19) 0.0019(15) 0.0034(17) 0.0103(17) O16 0.066(3) 0.042(2) 0.043(2) -0.0063(17) -0.001(2) 0.0110(18) O21 0.091(4) 0.071(3) 0.158(5) 0.015(3) -0.006(4) -0.002(3) O22 0.048(3) 0.139(4) 0.113(4) 0.039(3) -0.012(3) 0.012(3) O23 0.113(5) 0.151(5) 0.073(3) 0.047(3) -0.023(3) 0.043(4) O24 0.170(6) 0.086(3) 0.097(4) -0.003(3) 0.044(4) 0.036(4) O25 0.116(5) 0.217(7) 0.081(4) -0.018(4) -0.024(4) -0.041(5) O26 0.046(3) 0.123(4) 0.076(3) 0.018(3) 0.023(2) 0.015(3) O27 0.072(3) 0.105(3) 0.048(3) 0.004(2) 0.017(2) 0.001(3) O28 0.226(8) 0.194(7) 0.242(8) 0.161(6) 0.188(7) 0.161(6) O29 0.135(5) 0.051(3) 0.110(4) -0.010(3) -0.001(3) 0.036(3) O30 0.076(3) 0.062(3) 0.094(3) 0.016(2) 0.015(3) -0.002(2) O31 0.074(4) 0.097(3) 0.100(4) 0.025(3) -0.032(3) -0.004(3) O32 0.128(5) 0.093(3) 0.062(3) 0.015(3) 0.026(3) 0.019(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 C1 O1 1.434(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.369(6) . ? C2 C3 1.383(7) . ? C2 C7 1.422(7) . ? C3 C4 1.386(9) . ? C3 H3 0.9300 . ? C4 C5 1.342(9) . ? C4 H4 0.9300 . ? C5 C6 1.412(7) . ? C5 H5 0.9300 . ? C6 C7 1.398(7) . ? C6 C8 1.424(8) . ? C7 O2 1.317(6) . ? C8 N1 1.288(6) . ? C8 H8 0.9300 . ? C9 C10 1.469(8) . ? C9 N1 1.481(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N2 1.481(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.285(7) . ? C11 C12 1.409(8) . ? C11 H11 0.9300 . ? C12 C17 1.411(7) . ? C12 C13 1.436(8) . ? C13 C14 1.346(9) . ? C13 H13 0.9300 . ? C14 C15 1.392(9) . ? C14 H14 0.9300 . ? C15 C16 1.369(8) . ? C15 H15 0.9300 . ? C16 O4 1.383(7) . ? C16 C17 1.410(8) . ? C17 O3 1.300(5) . ? C18 O4 1.413(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 O5 1.447(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 O5 1.365(6) . ? C22 C23 1.382(6) . ? C22 C27 1.403(6) . ? C23 C24 1.376(8) . ? C23 H23 0.9300 . ? C24 C25 1.362(7) . ? C24 H24 0.9300 . ? C25 C26 1.396(7) . ? C25 H25 0.9300 . ? C26 C27 1.402(7) . ? C26 C28 1.421(7) . ? C27 O6 1.331(5) . ? C28 N3 1.288(6) . ? C28 H28 0.9300 . ? C29 C30 1.326(8) . ? C29 N3 1.464(7) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N4 1.461(7) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 N4 1.282(7) . ? C31 C32 1.427(8) . ? C31 H31 0.9300 . ? C32 C37 1.405(7) . ? C32 C33 1.425(8) . ? C33 C34 1.348(9) . ? C33 H33 0.9300 . ? C34 C35 1.388(9) . ? C34 H34 0.9300 . ? C35 C36 1.361(7) . ? C35 H35 0.9300 . ? C36 O8 1.357(6) . ? C36 C37 1.422(7) . ? C37 O7 1.317(5) . ? C38 O8 1.437(6) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C41 O9 1.435(5) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.372(7) . ? C42 O9 1.375(6) . ? C42 C47 1.416(7) . ? C43 C44 1.399(8) . ? C43 H43 0.9300 . ? C44 C45 1.343(8) . ? C44 H44 0.9300 . ? C45 C46 1.417(7) . ? C45 H45 0.9300 . ? C46 C47 1.402(6) . ? C46 C48 1.416(7) . ? C47 O10 1.303(5) . ? C48 N5 1.302(7) . ? C48 H48 0.9300 . ? C49 C50 1.381(9) . ? C49 N5 1.472(7) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 N6 1.459(7) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 N6 1.311(7) . ? C51 C52 1.408(8) . ? C51 H51 0.9300 . ? C52 C57 1.393(7) . ? C52 C53 1.427(8) . ? C53 C54 1.352(9) . ? C53 H53 0.9300 . ? C54 C55 1.389(9) . ? C54 H54 0.9300 . ? C55 C56 1.369(8) . ? C55 H55 0.9300 . ? C56 O12 1.366(6) . ? C56 C57 1.415(7) . ? C57 O11 1.315(6) . ? C58 O12 1.441(6) . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C61 O13 1.428(6) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 C63 1.360(7) . ? C62 O13 1.368(6) . ? C62 C67 1.432(7) . ? C63 C64 1.405(9) . ? C63 H63 0.9300 . ? C64 C65 1.348(9) . ? C64 H64 0.9300 . ? C65 C66 1.415(7) . ? C65 H65 0.9300 . ? C66 C67 1.407(7) . ? C66 C68 1.440(7) . ? C67 O14 1.296(6) . ? C68 N7 1.289(6) . ? C68 H68 0.9300 . ? C69 N7 1.476(6) . ? C69 C70 1.492(7) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 N8 1.487(6) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C71 N8 1.294(6) . ? C71 C72 1.423(7) . ? C71 H71 0.9300 . ? C72 C77 1.409(7) . ? C72 C73 1.413(7) . ? C73 C74 1.354(7) . ? C73 H73 0.9300 . ? C74 C75 1.387(8) . ? C74 H74 0.9300 . ? C75 C76 1.362(7) . ? C75 H75 0.9300 . ? C76 O16 1.370(6) . ? C76 C77 1.412(6) . ? C77 O15 1.321(5) . ? C78 O16 1.430(5) . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? Cl1 O23 1.406(5) . ? Cl1 O24 1.406(5) . ? Cl1 O21 1.423(5) . ? Cl1 O22 1.432(5) . ? Cl2 O28 1.339(5) . ? Cl2 O27 1.411(4) . ? Cl2 O26 1.432(4) . ? Cl2 O25 1.503(6) . ? Cl3 O29 1.414(4) . ? Cl3 O30 1.425(4) . ? Cl3 O31 1.427(4) . ? Cl3 O32 1.427(4) . ? N1 Ni1 1.860(4) . ? N2 Ni1 1.839(4) . ? N3 Ni2 1.849(4) . ? N4 Ni2 1.833(4) . ? N5 Ni3 1.834(4) . ? N6 Ni3 1.839(4) . ? N7 Ni4 1.833(4) . ? N8 Ni4 1.846(4) . ? N11 H1N 1.05(2) . ? N11 H3N 1.05(3) . ? N11 H2N 1.05(2) . ? N11 H4N 1.05(3) . ? N12 H8N 1.05(3) . ? N12 H5N 1.05(3) . ? N12 H7N 1.06(5) . ? N12 H6N 1.05(2) . ? N13 H11N 1.05(3) . ? N13 H10N 1.05(3) . ? N13 H9N 1.05(2) . ? N13 H12N 1.05(3) . ? Ni1 O2 1.844(3) . ? Ni1 O3 1.853(3) . ? Ni2 O6 1.842(3) . ? Ni2 O7 1.855(3) . ? Ni3 O11 1.849(3) . ? Ni3 O10 1.854(3) . ? Ni4 O15 1.849(3) . ? Ni4 O14 1.858(3) . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 126.7(5) . . ? O1 C2 C7 112.9(5) . . ? C3 C2 C7 120.4(6) . . ? C2 C3 C4 119.9(6) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 121.2(6) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 120.4(7) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 120.3(5) . . ? C7 C6 C8 121.8(5) . . ? C5 C6 C8 118.0(6) . . ? O2 C7 C6 124.7(5) . . ? O2 C7 C2 117.6(5) . . ? C6 C7 C2 117.7(5) . . ? N1 C8 C6 124.4(5) . . ? N1 C8 H8 117.8 . . ? C6 C8 H8 117.8 . . ? C10 C9 N1 106.9(5) . . ? C10 C9 H9A 110.3 . . ? N1 C9 H9A 110.3 . . ? C10 C9 H9B 110.3 . . ? N1 C9 H9B 110.3 . . ? H9A C9 H9B 108.6 . . ? C9 C10 N2 107.3(5) . . ? C9 C10 H10A 110.3 . . ? N2 C10 H10A 110.3 . . ? C9 C10 H10B 110.3 . . ? N2 C10 H10B 110.3 . . ? H10A C10 H10B 108.5 . . ? N2 C11 C12 124.6(5) . . ? N2 C11 H11 117.7 . . ? C12 C11 H11 117.7 . . ? C11 C12 C17 122.2(5) . . ? C11 C12 C13 119.6(6) . . ? C17 C12 C13 118.1(6) . . ? C14 C13 C12 121.2(6) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 121.1(6) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 119.2(7) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 O4 124.2(6) . . ? C15 C16 C17 122.2(6) . . ? O4 C16 C17 113.6(5) . . ? O3 C17 C16 118.1(5) . . ? O3 C17 C12 123.6(5) . . ? C16 C17 C12 118.2(5) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O5 C22 C23 124.7(4) . . ? O5 C22 C27 114.8(4) . . ? C23 C22 C27 120.4(5) . . ? C24 C23 C22 120.1(5) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.9(5) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 120.0(5) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C27 120.2(5) . . ? C25 C26 C28 119.2(5) . . ? C27 C26 C28 120.5(4) . . ? O6 C27 C26 124.3(4) . . ? O6 C27 C22 117.4(4) . . ? C26 C27 C22 118.3(4) . . ? N3 C28 C26 126.8(5) . . ? N3 C28 H28 116.6 . . ? C26 C28 H28 116.6 . . ? C30 C29 N3 113.2(6) . . ? C30 C29 H29A 108.9 . . ? N3 C29 H29A 108.9 . . ? C30 C29 H29B 108.9 . . ? N3 C29 H29B 108.9 . . ? H29A C29 H29B 107.8 . . ? C29 C30 N4 114.3(5) . . ? C29 C30 H30A 108.7 . . ? N4 C30 H30A 108.7 . . ? C29 C30 H30B 108.7 . . ? N4 C30 H30B 108.7 . . ? H30A C30 H30B 107.6 . . ? N4 C31 C32 126.0(5) . . ? N4 C31 H31 117.0 . . ? C32 C31 H31 117.0 . . ? C37 C32 C33 118.6(6) . . ? C37 C32 C31 121.5(5) . . ? C33 C32 C31 120.0(6) . . ? C34 C33 C32 120.6(6) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 121.2(5) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C36 C35 C34 120.4(6) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? O8 C36 C35 124.8(5) . . ? O8 C36 C37 114.7(4) . . ? C35 C36 C37 120.5(6) . . ? O7 C37 C32 123.4(5) . . ? O7 C37 C36 117.7(5) . . ? C32 C37 C36 118.9(5) . . ? O8 C38 H38A 109.5 . . ? O8 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O8 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O9 C41 H41A 109.5 . . ? O9 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O9 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 O9 124.7(5) . . ? C43 C42 C47 121.2(5) . . ? O9 C42 C47 114.1(4) . . ? C42 C43 C44 120.3(5) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 120.4(6) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 C46 120.4(5) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C47 C46 C48 121.7(5) . . ? C47 C46 C45 120.6(5) . . ? C48 C46 C45 117.7(5) . . ? O10 C47 C46 124.2(4) . . ? O10 C47 C42 118.6(4) . . ? C46 C47 C42 117.2(5) . . ? N5 C48 C46 125.1(5) . . ? N5 C48 H48 117.4 . . ? C46 C48 H48 117.4 . . ? C50 C49 N5 111.1(5) . . ? C50 C49 H49A 109.4 . . ? N5 C49 H49A 109.4 . . ? C50 C49 H49B 109.4 . . ? N5 C49 H49B 109.4 . . ? H49A C49 H49B 108.0 . . ? C49 C50 N6 113.7(5) . . ? C49 C50 H50A 108.8 . . ? N6 C50 H50A 108.8 . . ? C49 C50 H50B 108.8 . . ? N6 C50 H50B 108.8 . . ? H50A C50 H50B 107.7 . . ? N6 C51 C52 126.5(5) . . ? N6 C51 H51 116.8 . . ? C52 C51 H51 116.8 . . ? C57 C52 C51 122.1(5) . . ? C57 C52 C53 120.4(6) . . ? C51 C52 C53 117.6(6) . . ? C54 C53 C52 118.9(6) . . ? C54 C53 H53 120.6 . . ? C52 C53 H53 120.6 . . ? C53 C54 C55 121.5(6) . . ? C53 C54 H54 119.2 . . ? C55 C54 H54 119.2 . . ? C56 C55 C54 120.5(6) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? O12 C56 C55 125.0(5) . . ? O12 C56 C57 114.9(5) . . ? C55 C56 C57 120.1(6) . . ? O11 C57 C52 123.0(5) . . ? O11 C57 C56 118.3(5) . . ? C52 C57 C56 118.6(5) . . ? O12 C58 H58A 109.5 . . ? O12 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? O12 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O13 C61 H61A 109.5 . . ? O13 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O13 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C63 C62 O13 124.3(5) . . ? C63 C62 C67 121.6(5) . . ? O13 C62 C67 114.0(4) . . ? C62 C63 C64 120.2(6) . . ? C62 C63 H63 119.9 . . ? C64 C63 H63 119.9 . . ? C65 C64 C63 120.5(6) . . ? C65 C64 H64 119.8 . . ? C63 C64 H64 119.8 . . ? C64 C65 C66 120.1(6) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C67 C66 C65 121.1(5) . . ? C67 C66 C68 120.1(5) . . ? C65 C66 C68 118.6(5) . . ? O14 C67 C66 125.6(5) . . ? O14 C67 C62 118.0(5) . . ? C66 C67 C62 116.4(5) . . ? N7 C68 C66 125.2(5) . . ? N7 C68 H68 117.4 . . ? C66 C68 H68 117.4 . . ? N7 C69 C70 106.1(4) . . ? N7 C69 H69A 110.5 . . ? C70 C69 H69A 110.5 . . ? N7 C69 H69B 110.5 . . ? C70 C69 H69B 110.5 . . ? H69A C69 H69B 108.7 . . ? N8 C70 C69 106.7(4) . . ? N8 C70 H70A 110.4 . . ? C69 C70 H70A 110.4 . . ? N8 C70 H70B 110.4 . . ? C69 C70 H70B 110.4 . . ? H70A C70 H70B 108.6 . . ? N8 C71 C72 124.2(5) . . ? N8 C71 H71 117.9 . . ? C72 C71 H71 117.9 . . ? C77 C72 C73 119.2(5) . . ? C77 C72 C71 121.6(5) . . ? C73 C72 C71 119.2(5) . . ? C74 C73 C72 120.4(5) . . ? C74 C73 H73 119.8 . . ? C72 C73 H73 119.8 . . ? C73 C74 C75 120.8(5) . . ? C73 C74 H74 119.6 . . ? C75 C74 H74 119.6 . . ? C76 C75 C74 120.3(5) . . ? C76 C75 H75 119.9 . . ? C74 C75 H75 119.9 . . ? C75 C76 O16 124.7(5) . . ? C75 C76 C77 120.9(5) . . ? O16 C76 C77 114.4(4) . . ? O15 C77 C72 124.2(4) . . ? O15 C77 C76 117.5(4) . . ? C72 C77 C76 118.3(5) . . ? O16 C78 H78A 109.5 . . ? O16 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? O16 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? O23 Cl1 O24 110.6(3) . . ? O23 Cl1 O21 112.1(3) . . ? O24 Cl1 O21 109.4(4) . . ? O23 Cl1 O22 108.0(3) . . ? O24 Cl1 O22 110.6(3) . . ? O21 Cl1 O22 106.0(3) . . ? O28 Cl2 O27 111.2(4) . . ? O28 Cl2 O26 111.6(4) . . ? O27 Cl2 O26 111.3(3) . . ? O28 Cl2 O25 110.1(5) . . ? O27 Cl2 O25 106.7(3) . . ? O26 Cl2 O25 105.7(3) . . ? O29 Cl3 O30 109.9(3) . . ? O29 Cl3 O31 110.2(3) . . ? O30 Cl3 O31 108.7(3) . . ? O29 Cl3 O32 109.3(3) . . ? O30 Cl3 O32 108.4(3) . . ? O31 Cl3 O32 110.3(3) . . ? C8 N1 C9 119.2(5) . . ? C8 N1 Ni1 127.6(4) . . ? C9 N1 Ni1 113.1(4) . . ? C11 N2 C10 120.5(5) . . ? C11 N2 Ni1 127.2(4) . . ? C10 N2 Ni1 112.2(4) . . ? C28 N3 C29 120.4(5) . . ? C28 N3 Ni2 126.2(4) . . ? C29 N3 Ni2 113.3(4) . . ? C31 N4 C30 119.8(5) . . ? C31 N4 Ni2 126.8(4) . . ? C30 N4 Ni2 113.4(4) . . ? C48 N5 C49 118.7(5) . . ? C48 N5 Ni3 126.9(4) . . ? C49 N5 Ni3 114.4(4) . . ? C51 N6 C50 121.4(5) . . ? C51 N6 Ni3 125.2(4) . . ? C50 N6 Ni3 113.3(4) . . ? C68 N7 C69 119.3(4) . . ? C68 N7 Ni4 127.2(4) . . ? C69 N7 Ni4 113.3(3) . . ? C71 N8 C70 118.5(4) . . ? C71 N8 Ni4 128.2(4) . . ? C70 N8 Ni4 113.2(3) . . ? H1N N11 H3N 109(4) . . ? H1N N11 H2N 109(4) . . ? H3N N11 H2N 109(4) . . ? H1N N11 H4N 109(4) . . ? H3N N11 H4N 109(4) . . ? H2N N11 H4N 109(4) . . ? H8N N12 H5N 109(4) . . ? H8N N12 H7N 109(4) . . ? H5N N12 H7N 109(4) . . ? H8N N12 H6N 109(4) . . ? H5N N12 H6N 109(4) . . ? H7N N12 H6N 109(4) . . ? H11N N13 H10N 109(4) . . ? H11N N13 H9N 109(4) . . ? H10N N13 H9N 109(4) . . ? H11N N13 H12N 109(4) . . ? H10N N13 H12N 109(4) . . ? H9N N13 H12N 109(4) . . ? N2 Ni1 O2 176.89(19) . . ? N2 Ni1 O3 94.35(18) . . ? O2 Ni1 O3 85.29(14) . . ? N2 Ni1 N1 86.2(2) . . ? O2 Ni1 N1 94.26(18) . . ? O3 Ni1 N1 177.7(2) . . ? N4 Ni2 O6 179.27(19) . . ? N4 Ni2 N3 85.7(2) . . ? O6 Ni2 N3 94.83(16) . . ? N4 Ni2 O7 94.83(17) . . ? O6 Ni2 O7 84.64(13) . . ? N3 Ni2 O7 179.42(18) . . ? N5 Ni3 N6 86.3(2) . . ? N5 Ni3 O11 178.65(19) . . ? N6 Ni3 O11 94.85(18) . . ? N5 Ni3 O10 94.66(17) . . ? N6 Ni3 O10 178.92(19) . . ? O11 Ni3 O10 84.18(14) . . ? N7 Ni4 N8 86.34(19) . . ? N7 Ni4 O15 176.54(18) . . ? N8 Ni4 O15 94.21(16) . . ? N7 Ni4 O14 94.76(17) . . ? N8 Ni4 O14 176.50(19) . . ? O15 Ni4 O14 84.89(13) . . ? C2 O1 C1 117.3(5) . . ? C7 O2 Ni1 126.9(3) . . ? C17 O3 Ni1 127.0(3) . . ? C16 O4 C18 119.7(5) . . ? C22 O5 C21 117.4(4) . . ? C27 O6 Ni2 127.2(3) . . ? C37 O7 Ni2 127.6(3) . . ? C36 O8 C38 117.4(4) . . ? C42 O9 C41 115.5(4) . . ? C47 O10 Ni3 127.4(3) . . ? C57 O11 Ni3 128.2(3) . . ? C56 O12 C58 117.6(4) . . ? C62 O13 C61 118.2(4) . . ? C67 O14 Ni4 126.5(3) . . ? C77 O15 Ni4 126.8(3) . . ? C76 O16 C78 117.2(4) . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 25.21 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 0.587 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.063 # Attachment 'C3_au8.cif' data_shelxlC3 _database_code_depnum_ccdc_archive 'CCDC 809438' #TrackingRef 'C3_au8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H48 Cl N5 Ni2 O12' _chemical_formula_weight 991.74 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' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 13.8843(8) _cell_length_b 23.6202(10) _cell_length_c 14.7348(8) _cell_angle_alpha 90.00 _cell_angle_beta 114.441(4) _cell_angle_gamma 90.00 _cell_volume 4399.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11325 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5896 _exptl_absorpt_correction_T_max 0.7424 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35615 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 26.41 _reflns_number_total 8966 _reflns_number_gt 6280 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The geometrical restrains were used for the refinement of the disordered fragment ; _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^)+(0.1084P)^2^+1.4110P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8966 _refine_ls_number_parameters 587 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0984 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1897 _refine_ls_wR_factor_gt 0.1716 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.040 _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 C1 C 0.6265(6) 0.2483(3) 1.0869(5) 0.094(2) Uani 1 1 d . . . H1A H 0.6624 0.2580 1.0457 0.141 Uiso 1 1 calc R . . H1B H 0.6776 0.2401 1.1532 0.141 Uiso 1 1 calc R . . H1C H 0.5830 0.2795 1.0889 0.141 Uiso 1 1 calc R . . C2 C 0.5046(4) 0.1806(2) 1.0977(4) 0.0628(12) Uani 1 1 d . . . C3 C 0.5011(6) 0.2080(3) 1.1784(5) 0.0866(18) Uani 1 1 d . . . H3 H 0.5387 0.2414 1.2016 0.104 Uiso 1 1 calc R . . C4 C 0.4414(8) 0.1857(4) 1.2251(6) 0.110(3) Uani 1 1 d . . . H4 H 0.4379 0.2049 1.2789 0.132 Uiso 1 1 calc R . . C5 C 0.3880(6) 0.1366(3) 1.1940(5) 0.093(2) Uani 1 1 d . . . H5 H 0.3490 0.1219 1.2268 0.112 Uiso 1 1 calc R . . C6 C 0.3913(4) 0.1079(2) 1.1120(4) 0.0674(14) Uani 1 1 d . . . C7 C 0.4499(4) 0.1294(2) 1.0610(3) 0.0553(11) Uani 1 1 d . A . C8 C 0.3402(4) 0.0542(3) 1.0856(5) 0.0760(16) Uani 1 1 d . A . H8 H 0.3069 0.0407 1.1245 0.091 Uiso 1 1 calc R . . C9 C 0.2901(7) -0.0346(4) 0.9988(7) 0.140(4) Uani 0.40 1 d P A 1 H9 H 0.3516 -0.0587 1.0354 0.168 Uiso 0.40 1 calc PR A 1 C10 C 0.2578(8) -0.0525(4) 0.9011(9) 0.131(3) Uani 0.40 1 d P A 1 H10A H 0.1854 -0.0407 0.8620 0.157 Uiso 0.40 1 calc PR A 1 H10B H 0.2606 -0.0935 0.8988 0.157 Uiso 0.40 1 calc PR A 1 C19 C 0.2117(13) -0.0554(7) 1.0305(13) 0.084(4) Uani 0.40 1 d P A 1 H19A H 0.2310 -0.0451 1.0988 0.126 Uiso 0.40 1 calc PR A 1 H19B H 0.2074 -0.0959 1.0242 0.126 Uiso 0.40 1 calc PR A 1 H19C H 0.1442 -0.0391 0.9896 0.126 Uiso 0.40 1 calc PR A 1 C9A C 0.2901(7) -0.0346(4) 0.9988(7) 0.140(4) Uani 0.60 1 d P A 2 H9A1 H 0.3424 -0.0608 1.0429 0.168 Uiso 0.60 1 calc PR A 2 H9A2 H 0.2300 -0.0347 1.0164 0.168 Uiso 0.60 1 calc PR A 2 C10A C 0.2578(8) -0.0525(4) 0.9011(9) 0.131(3) Uani 0.60 1 d P A 2 H10C H 0.1924 -0.0309 0.8668 0.157 Uiso 0.60 1 calc PR A 2 C19A C 0.2206(8) -0.1089(4) 0.8866(9) 0.089(3) Uani 0.60 1 d P A 2 H19D H 0.1975 -0.1189 0.8177 0.133 Uiso 0.60 1 calc PR A 2 H19E H 0.1624 -0.1122 0.9055 0.133 Uiso 0.60 1 calc PR A 2 H19F H 0.2765 -0.1338 0.9269 0.133 Uiso 0.60 1 calc PR A 2 C11 C 0.3337(5) -0.0504(2) 0.7833(5) 0.0805(18) Uani 1 1 d . A . H11 H 0.2937 -0.0829 0.7584 0.097 Uiso 1 1 calc R . . C12 C 0.3950(4) -0.0308(2) 0.7332(4) 0.0664(14) Uani 1 1 d . . . C13 C 0.3986(6) -0.0634(3) 0.6540(5) 0.095(2) Uani 1 1 d . . . H13 H 0.3578 -0.0961 0.6337 0.114 Uiso 1 1 calc R . . C14 C 0.4598(8) -0.0478(3) 0.6081(5) 0.110(3) Uani 1 1 d . . . H14 H 0.4611 -0.0698 0.5562 0.132 Uiso 1 1 calc R . . C15 C 0.5220(7) 0.0012(3) 0.6373(5) 0.097(2) Uani 1 1 d . . . H15 H 0.5657 0.0111 0.6062 0.116 Uiso 1 1 calc R . . C16 C 0.5182(5) 0.0343(2) 0.7118(4) 0.0681(13) Uani 1 1 d . . . C17 C 0.4540(4) 0.0195(2) 0.7617(3) 0.0568(11) Uani 1 1 d . A . C18 C 0.6461(6) 0.0983(4) 0.7016(6) 0.102(2) Uani 1 1 d . . . H18A H 0.6809 0.1331 0.7303 0.153 Uiso 1 1 calc R . . H18B H 0.6076 0.1029 0.6310 0.153 Uiso 1 1 calc R . . H18C H 0.6978 0.0688 0.7147 0.153 Uiso 1 1 calc R . . C21 C 0.4917(7) 0.3568(3) 0.8753(7) 0.114(3) Uani 1 1 d . . . H21A H 0.5206 0.3490 0.8276 0.171 Uiso 1 1 calc R . . H21B H 0.5479 0.3589 0.9409 0.171 Uiso 1 1 calc R . . H21C H 0.4544 0.3922 0.8593 0.171 Uiso 1 1 calc R . . C22 C 0.3727(4) 0.3173(2) 0.9346(4) 0.0611(12) Uani 1 1 d . . . C23 C 0.3872(5) 0.3616(2) 1.0007(5) 0.0823(17) Uani 1 1 d . . . H23 H 0.4326 0.3911 1.0031 0.099 Uiso 1 1 calc R . . C24 C 0.3359(7) 0.3628(3) 1.0626(5) 0.101(2) Uani 1 1 d . . . H24 H 0.3464 0.3930 1.1061 0.121 Uiso 1 1 calc R . . C25 C 0.2708(7) 0.3207(3) 1.0605(5) 0.096(2) Uani 1 1 d . . . H25 H 0.2365 0.3218 1.1030 0.115 Uiso 1 1 calc R . . C26 C 0.2535(5) 0.2748(2) 0.9954(4) 0.0699(14) Uani 1 1 d . . . C27 C 0.3032(4) 0.27212(19) 0.9304(4) 0.0566(11) Uani 1 1 d . . . C28 C 0.1847(6) 0.2304(3) 0.9979(6) 0.094(2) Uani 1 1 d . . . H28 H 0.1553 0.2337 1.0440 0.113 Uiso 1 1 calc R . . C29 C 0.1141(8) 0.1411(5) 0.9797(7) 0.172(5) Uani 1 1 d D . . H29A H 0.1681 0.1161 1.0252 0.206 Uiso 1 1 calc R . . H29B H 0.0714 0.1559 1.0123 0.206 Uiso 1 1 calc R . . C30 C 0.0515(6) 0.1137(5) 0.8888(7) 0.171(6) Uani 1 1 d D . . H30 H 0.0338 0.0757 0.9038 0.206 Uiso 1 1 calc R . . C31 C 0.0959(4) 0.0700(2) 0.7509(5) 0.0812(19) Uani 1 1 d . . . H31 H 0.0488 0.0411 0.7470 0.097 Uiso 1 1 calc R . . C32 C 0.1410(4) 0.06795(19) 0.6806(4) 0.0699(16) Uani 1 1 d . . . C33 C 0.1120(5) 0.0240(2) 0.6109(6) 0.087(2) Uani 1 1 d . . . H33 H 0.0649 -0.0036 0.6126 0.104 Uiso 1 1 calc R . . C34 C 0.1512(6) 0.0208(2) 0.5414(6) 0.099(3) Uani 1 1 d . . . H34 H 0.1303 -0.0087 0.4955 0.119 Uiso 1 1 calc R . . C35 C 0.2223(5) 0.0608(2) 0.5370(4) 0.0808(18) Uani 1 1 d . . . H35 H 0.2491 0.0582 0.4888 0.097 Uiso 1 1 calc R . . C36 C 0.2531(4) 0.1050(2) 0.6057(4) 0.0644(14) Uani 1 1 d . . . C37 C 0.2134(4) 0.10950(17) 0.6788(4) 0.0559(12) Uani 1 1 d . . . C38 C 0.3615(6) 0.1460(3) 0.5316(5) 0.098(2) Uani 1 1 d . . . H38A H 0.4086 0.1774 0.5412 0.147 Uiso 1 1 calc R . . H38B H 0.3033 0.1489 0.4673 0.147 Uiso 1 1 calc R . . H38C H 0.3989 0.1113 0.5353 0.147 Uiso 1 1 calc R . . C40 C -0.0528(6) 0.1458(7) 0.8282(9) 0.266(11) Uani 1 1 d D . . H40A H -0.0927 0.1256 0.7677 0.399 Uiso 1 1 calc R . . H40B H -0.0367 0.1831 0.8124 0.399 Uiso 1 1 calc R . . H40C H -0.0936 0.1487 0.8671 0.399 Uiso 1 1 calc R . . C41 C 0.5304(4) 0.2087(2) 0.8013(4) 0.0611(12) Uani 1 1 d . . . C42 C 0.6372(5) 0.2064(3) 0.8550(6) 0.095(2) Uani 1 1 d . . . H42 H 0.6664 0.1814 0.9082 0.113 Uiso 1 1 calc R . . C43 C 0.7018(7) 0.2415(4) 0.8298(10) 0.134(4) Uani 1 1 d . . . H43 H 0.7749 0.2400 0.8650 0.160 Uiso 1 1 calc R . . C44 C 0.6568(11) 0.2788(4) 0.7521(11) 0.148(5) Uani 1 1 d . . . H44 H 0.7000 0.3030 0.7357 0.177 Uiso 1 1 calc R . . C45 C 0.5488(10) 0.2810(3) 0.6979(7) 0.128(4) Uani 1 1 d . . . H45 H 0.5196 0.3063 0.6452 0.153 Uiso 1 1 calc R . . C46 C 0.4846(6) 0.2456(2) 0.7221(5) 0.0838(18) Uani 1 1 d . . . H46 H 0.4116 0.2465 0.6858 0.101 Uiso 1 1 calc R . . Cl1 Cl -0.12433(14) -0.04238(7) 0.77384(15) 0.0849(5) Uani 1 1 d . . . N1 N 0.3359(4) 0.0229(2) 1.0130(4) 0.0705(12) Uani 1 1 d . . . N2 N 0.3282(3) -0.02761(18) 0.8592(4) 0.0696(12) Uani 1 1 d . . . N3 N 0.1600(5) 0.1865(2) 0.9422(5) 0.0859(15) Uani 1 1 d . . . N4 N 0.1131(4) 0.1078(2) 0.8209(4) 0.0791(14) Uani 1 1 d D . . N5 N 0.4623(3) 0.17315(17) 0.8291(3) 0.0597(10) Uani 1 1 d . . . H5A H 0.4672 0.1375 0.8118 0.090 Uiso 1 1 calc R . . H5B H 0.3957 0.1849 0.7979 0.090 Uiso 1 1 calc R . . H5C H 0.4821 0.1751 0.8947 0.090 Uiso 1 1 calc R . . Ni1 Ni 0.39318(4) 0.03824(2) 0.92232(4) 0.04943(17) Uani 1 1 d . A . Ni2 Ni 0.20244(5) 0.16918(2) 0.84258(5) 0.05431(18) Uani 1 1 d . . . O1 O 0.5613(3) 0.19939(16) 1.0464(3) 0.0735(10) Uani 1 1 d . . . O2 O 0.4568(2) 0.10540(13) 0.9839(2) 0.0534(7) Uani 1 1 d . . . O3 O 0.4540(2) 0.05299(13) 0.8339(2) 0.0541(7) Uani 1 1 d . . . O4 O 0.5742(3) 0.08326(17) 0.7449(3) 0.0758(10) Uani 1 1 d . . . O5 O 0.4204(3) 0.31260(16) 0.8724(3) 0.0791(11) Uani 1 1 d . . . O6 O 0.2905(3) 0.23099(13) 0.8658(2) 0.0569(8) Uani 1 1 d . . . O7 O 0.2449(2) 0.15249(12) 0.7422(2) 0.0540(7) Uani 1 1 d . . . O8 O 0.3224(3) 0.14647(16) 0.6072(3) 0.0726(10) Uani 1 1 d . . . O11 O -0.0319(7) -0.0532(4) 0.7789(12) 0.273(7) Uani 1 1 d . . . O12 O -0.1450(9) 0.0062(5) 0.7204(13) 0.307(8) Uani 1 1 d . . . O13 O -0.2045(6) -0.0789(4) 0.7195(7) 0.197(4) Uani 1 1 d . . . O14 O -0.1336(10) -0.0247(8) 0.8528(8) 0.318(9) 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 C1 0.097(5) 0.076(4) 0.103(5) -0.024(3) 0.037(4) -0.033(3) C2 0.065(3) 0.062(3) 0.058(3) 0.001(2) 0.023(2) 0.003(2) C3 0.105(5) 0.079(4) 0.078(4) -0.009(3) 0.040(4) 0.001(4) C4 0.139(7) 0.121(6) 0.089(5) -0.003(5) 0.067(5) 0.030(6) C5 0.109(5) 0.111(5) 0.091(5) 0.017(4) 0.072(4) 0.024(4) C6 0.058(3) 0.086(4) 0.066(3) 0.019(3) 0.033(3) 0.014(3) C7 0.049(2) 0.065(3) 0.051(3) 0.010(2) 0.020(2) 0.011(2) C8 0.060(3) 0.098(4) 0.079(4) 0.032(3) 0.037(3) 0.008(3) C9 0.127(7) 0.163(8) 0.101(6) 0.040(6) 0.017(5) -0.089(7) C10 0.126(7) 0.096(5) 0.188(10) -0.010(6) 0.084(7) -0.061(5) C19 0.083(10) 0.084(10) 0.104(12) 0.017(8) 0.058(9) -0.008(8) C9A 0.127(7) 0.163(8) 0.101(6) 0.040(6) 0.017(5) -0.089(7) C10A 0.126(7) 0.096(5) 0.188(10) -0.010(6) 0.084(7) -0.061(5) C19A 0.072(6) 0.060(5) 0.104(8) 0.011(5) 0.006(6) -0.019(4) C11 0.064(3) 0.052(3) 0.101(5) -0.003(3) 0.009(3) -0.010(2) C12 0.067(3) 0.059(3) 0.052(3) -0.001(2) 0.003(2) 0.006(2) C13 0.114(6) 0.073(4) 0.068(4) -0.009(3) 0.008(4) 0.007(4) C14 0.169(9) 0.083(5) 0.068(4) -0.013(3) 0.039(5) 0.021(5) C15 0.144(7) 0.084(4) 0.075(4) 0.006(3) 0.057(4) 0.026(4) C16 0.079(4) 0.065(3) 0.059(3) 0.005(2) 0.028(3) 0.015(3) C17 0.053(3) 0.057(2) 0.047(2) 0.003(2) 0.007(2) 0.009(2) C18 0.106(5) 0.121(6) 0.113(5) 0.000(4) 0.079(5) -0.007(4) C21 0.138(7) 0.075(4) 0.158(7) -0.037(4) 0.091(6) -0.055(4) C22 0.063(3) 0.049(2) 0.069(3) -0.017(2) 0.024(3) 0.001(2) C23 0.093(4) 0.059(3) 0.085(4) -0.022(3) 0.028(4) -0.004(3) C24 0.138(7) 0.080(4) 0.087(5) -0.031(4) 0.048(5) 0.005(4) C25 0.130(6) 0.087(4) 0.086(4) -0.016(4) 0.062(4) 0.014(4) C26 0.085(4) 0.062(3) 0.072(3) -0.002(2) 0.042(3) 0.010(3) C27 0.061(3) 0.050(2) 0.056(3) -0.002(2) 0.021(2) 0.008(2) C28 0.119(6) 0.084(4) 0.115(5) 0.000(4) 0.085(5) 0.010(4) C29 0.234(14) 0.140(8) 0.232(13) -0.056(9) 0.187(12) -0.078(9) C30 0.103(6) 0.295(16) 0.118(7) 0.048(8) 0.048(6) -0.095(9) C31 0.055(3) 0.061(3) 0.099(5) 0.015(3) 0.003(3) -0.015(2) C32 0.052(3) 0.042(2) 0.080(4) 0.000(2) -0.009(3) -0.002(2) C33 0.068(4) 0.051(3) 0.100(5) -0.012(3) -0.006(4) -0.007(2) C34 0.084(4) 0.050(3) 0.106(5) -0.032(3) -0.018(4) 0.003(3) C35 0.076(4) 0.066(3) 0.067(3) -0.022(3) -0.003(3) 0.016(3) C36 0.061(3) 0.048(2) 0.060(3) -0.008(2) 0.001(2) 0.006(2) C37 0.045(2) 0.041(2) 0.060(3) -0.0032(19) 0.000(2) 0.0018(17) C38 0.124(6) 0.101(5) 0.078(4) -0.006(4) 0.052(4) 0.007(4) C40 0.068(6) 0.42(3) 0.298(18) 0.211(19) 0.064(9) 0.071(10) C41 0.065(3) 0.054(3) 0.078(3) -0.009(2) 0.044(3) -0.014(2) C42 0.061(4) 0.098(5) 0.131(6) -0.020(4) 0.046(4) -0.013(3) C43 0.095(6) 0.118(7) 0.223(12) -0.060(7) 0.100(7) -0.043(5) C44 0.198(12) 0.108(7) 0.232(13) -0.072(8) 0.183(11) -0.083(8) C45 0.205(11) 0.087(5) 0.141(8) 0.001(5) 0.121(8) -0.041(6) C46 0.117(5) 0.067(3) 0.089(4) 0.003(3) 0.065(4) -0.012(3) Cl1 0.0842(10) 0.0725(9) 0.1230(13) -0.0181(8) 0.0679(10) -0.0154(7) N1 0.059(3) 0.077(3) 0.075(3) 0.023(2) 0.028(2) -0.007(2) N2 0.050(2) 0.052(2) 0.098(3) 0.003(2) 0.021(2) -0.0104(17) N3 0.092(4) 0.075(3) 0.120(4) 0.009(3) 0.073(3) -0.001(3) N4 0.061(3) 0.070(3) 0.090(3) 0.009(3) 0.015(2) -0.016(2) N5 0.058(2) 0.064(2) 0.061(2) 0.0010(19) 0.028(2) -0.0154(18) Ni1 0.0369(3) 0.0485(3) 0.0572(3) 0.0110(2) 0.0138(2) -0.0014(2) Ni2 0.0430(3) 0.0488(3) 0.0688(4) 0.0027(3) 0.0208(3) -0.0030(2) O1 0.085(3) 0.068(2) 0.068(2) -0.0157(17) 0.032(2) -0.0239(19) O2 0.0551(18) 0.0576(17) 0.0516(17) 0.0029(14) 0.0262(15) -0.0062(14) O3 0.0507(17) 0.0500(16) 0.0608(19) -0.0012(14) 0.0224(15) -0.0034(13) O4 0.088(3) 0.078(2) 0.080(3) 0.000(2) 0.053(2) 0.000(2) O5 0.087(3) 0.062(2) 0.103(3) -0.032(2) 0.053(2) -0.0290(19) O6 0.0574(18) 0.0505(16) 0.067(2) -0.0146(14) 0.0302(16) -0.0082(14) O7 0.0518(17) 0.0454(15) 0.0583(18) -0.0058(13) 0.0162(15) -0.0092(13) O8 0.079(3) 0.072(2) 0.065(2) -0.0163(18) 0.027(2) -0.0019(19) O11 0.130(6) 0.207(9) 0.54(2) -0.162(12) 0.192(10) -0.044(6) O12 0.197(10) 0.149(8) 0.49(2) 0.067(11) 0.056(12) -0.020(8) O13 0.156(6) 0.180(7) 0.263(9) -0.063(7) 0.095(7) -0.103(6) O14 0.282(13) 0.57(3) 0.173(8) -0.117(12) 0.163(9) -0.143(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.436(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.371(7) . ? C2 C3 1.372(8) . ? C2 C7 1.412(7) . ? C3 C4 1.381(11) . ? C3 H3 0.9300 . ? C4 C5 1.351(11) . ? C4 H4 0.9300 . ? C5 C6 1.403(9) . ? C5 H5 0.9300 . ? C6 C7 1.411(7) . ? C6 C8 1.425(9) . ? C7 O2 1.308(6) . ? C8 N1 1.281(8) . ? C8 H8 0.9300 . ? C9 C10 1.385(13) . ? C9 C19 1.436(15) . ? C9 N1 1.478(9) . ? C9 H9 0.9800 . ? C10 N2 1.478(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C19A H19D 0.9600 . ? C19A H19E 0.9600 . ? C19A H19F 0.9600 . ? C11 N2 1.271(8) . ? C11 C12 1.417(9) . ? C11 H11 0.9300 . ? C12 C17 1.405(7) . ? C12 C13 1.416(9) . ? C13 C14 1.339(11) . ? C13 H13 0.9300 . ? C14 C15 1.401(11) . ? C14 H14 0.9300 . ? C15 C16 1.365(8) . ? C15 H15 0.9300 . ? C16 O4 1.366(7) . ? C16 C17 1.415(8) . ? C17 O3 1.325(6) . ? C18 O4 1.433(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C21 O5 1.427(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 O5 1.339(6) . ? C22 C23 1.387(7) . ? C22 C27 1.423(7) . ? C23 C24 1.370(10) . ? C23 H23 0.9300 . ? C24 C25 1.336(11) . ? C24 H24 0.9300 . ? C25 C26 1.402(8) . ? C25 H25 0.9300 . ? C26 C27 1.394(7) . ? C26 C28 1.430(9) . ? C27 O6 1.319(5) . ? C28 N3 1.278(9) . ? C28 H28 0.9300 . ? C29 C30 1.417(13) . ? C29 N3 1.468(10) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C40 1.549(15) . ? C30 N4 1.567(10) . ? C30 H30 0.9800 . ? C31 N4 1.310(8) . ? C31 C32 1.416(9) . ? C31 H31 0.9300 . ? C32 C33 1.398(8) . ? C32 C37 1.413(7) . ? C33 C34 1.347(10) . ? C33 H33 0.9300 . ? C34 C35 1.387(10) . ? C34 H34 0.9300 . ? C35 C36 1.391(7) . ? C35 H35 0.9300 . ? C36 O8 1.367(7) . ? C36 C37 1.402(8) . ? C37 O7 1.326(5) . ? C38 O8 1.428(7) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.363(8) . ? C41 C46 1.384(8) . ? C41 N5 1.445(6) . ? C42 C43 1.380(12) . ? C42 H42 0.9300 . ? C43 C44 1.373(16) . ? C43 H43 0.9300 . ? C44 C45 1.377(15) . ? C44 H44 0.9300 . ? C45 C46 1.372(10) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? Cl1 O11 1.279(7) . ? Cl1 O14 1.292(9) . ? Cl1 O12 1.354(12) . ? Cl1 O13 1.373(6) . ? N1 Ni1 1.851(5) . ? N2 Ni1 1.845(4) . ? N3 Ni2 1.840(5) . ? N4 Ni2 1.849(4) . ? N5 H5A 0.8900 . ? N5 H5B 0.8900 . ? N5 H5C 0.8900 . ? Ni1 O3 1.855(3) . ? Ni1 O2 1.859(3) . ? Ni2 O6 1.843(3) . ? Ni2 O7 1.847(3) . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.0(5) . . ? O1 C2 C7 114.0(4) . . ? C3 C2 C7 122.0(6) . . ? C2 C3 C4 119.7(7) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 121.0(7) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C4 C5 C6 120.0(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C7 121.0(6) . . ? C5 C6 C8 118.5(6) . . ? C7 C6 C8 120.4(5) . . ? O2 C7 C6 124.9(5) . . ? O2 C7 C2 118.8(4) . . ? C6 C7 C2 116.2(5) . . ? N1 C8 C6 126.0(5) . . ? N1 C8 H8 117.0 . . ? C6 C8 H8 117.0 . . ? C10 C9 C19 105.7(10) . . ? C10 C9 N1 111.3(6) . . ? C19 C9 N1 127.4(12) . . ? C10 C9 H9 103.2 . . ? C19 C9 H9 103.2 . . ? N1 C9 H9 103.2 . . ? C9 C10 N2 109.1(6) . . ? C9 C10 H10A 109.9 . . ? N2 C10 H10A 109.9 . . ? C9 C10 H10B 109.9 . . ? N2 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C9 C19 H19A 109.5 . . ? C9 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C9 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? H19D C19A H19E 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? N2 C11 C12 126.0(5) . . ? N2 C11 H11 117.0 . . ? C12 C11 H11 117.0 . . ? C17 C12 C13 119.5(6) . . ? C17 C12 C11 121.5(5) . . ? C13 C12 C11 119.0(6) . . ? C14 C13 C12 120.8(7) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.7(7) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.8(7) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 O4 124.5(6) . . ? C15 C16 C17 121.3(6) . . ? O4 C16 C17 114.3(4) . . ? O3 C17 C12 123.5(5) . . ? O3 C17 C16 118.7(4) . . ? C12 C17 C16 117.8(5) . . ? O4 C18 H18A 109.5 . . ? O4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O5 C21 H21A 109.5 . . ? O5 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O5 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O5 C22 C23 125.1(5) . . ? O5 C22 C27 115.2(4) . . ? C23 C22 C27 119.7(5) . . ? C24 C23 C22 121.2(6) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C25 C24 C23 120.2(6) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.9(7) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 120.8(6) . . ? C27 C26 C28 120.7(5) . . ? C25 C26 C28 118.5(6) . . ? O6 C27 C26 124.9(5) . . ? O6 C27 C22 118.0(4) . . ? C26 C27 C22 117.1(4) . . ? N3 C28 C26 125.7(6) . . ? N3 C28 H28 117.1 . . ? C26 C28 H28 117.1 . . ? C30 C29 N3 99.8(7) . . ? C30 C29 H29A 111.8 . . ? N3 C29 H29A 111.8 . . ? C30 C29 H29B 111.8 . . ? N3 C29 H29B 111.8 . . ? H29A C29 H29B 109.5 . . ? C29 C30 C40 112.5(8) . . ? C29 C30 N4 111.1(6) . . ? C40 C30 N4 107.6(5) . . ? C29 C30 H30 108.5 . . ? C40 C30 H30 108.5 . . ? N4 C30 H30 108.5 . . ? N4 C31 C32 127.5(5) . . ? N4 C31 H31 116.3 . . ? C32 C31 H31 116.3 . . ? C33 C32 C37 119.6(7) . . ? C33 C32 C31 118.8(6) . . ? C37 C32 C31 121.6(5) . . ? C34 C33 C32 121.0(6) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 121.2(6) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C34 C35 C36 119.2(7) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? O8 C36 C35 123.5(6) . . ? O8 C36 C37 115.5(4) . . ? C35 C36 C37 121.1(6) . . ? O7 C37 C36 118.7(4) . . ? O7 C37 C32 123.2(5) . . ? C36 C37 C32 118.0(5) . . ? O8 C38 H38A 109.5 . . ? O8 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O8 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C30 C40 H40A 109.5 . . ? C30 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C30 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 121.6(6) . . ? C42 C41 N5 119.7(6) . . ? C46 C41 N5 118.6(5) . . ? C41 C42 C43 119.5(9) . . ? C41 C42 H42 120.3 . . ? C43 C42 H42 120.3 . . ? C44 C43 C42 119.2(9) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C43 C44 C45 121.2(8) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C46 C45 C44 119.7(9) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C41 118.8(8) . . ? C45 C46 H46 120.6 . . ? C41 C46 H46 120.6 . . ? O11 Cl1 O14 118.9(9) . . ? O11 Cl1 O12 99.8(9) . . ? O14 Cl1 O12 100.0(11) . . ? O11 Cl1 O13 117.3(6) . . ? O14 Cl1 O13 111.7(7) . . ? O12 Cl1 O13 105.5(7) . . ? C8 N1 C9 121.1(6) . . ? C8 N1 Ni1 127.1(4) . . ? C9 N1 Ni1 111.5(6) . . ? C11 N2 C10 119.3(6) . . ? C11 N2 Ni1 127.3(4) . . ? C10 N2 Ni1 113.3(5) . . ? C28 N3 C29 113.2(6) . . ? C28 N3 Ni2 127.1(5) . . ? C29 N3 Ni2 118.1(5) . . ? C31 N4 C30 126.4(6) . . ? C31 N4 Ni2 124.1(5) . . ? C30 N4 Ni2 109.0(5) . . ? C41 N5 H5A 109.5 . . ? C41 N5 H5B 109.5 . . ? H5A N5 H5B 109.5 . . ? C41 N5 H5C 109.5 . . ? H5A N5 H5C 109.5 . . ? H5B N5 H5C 109.5 . . ? N2 Ni1 N1 86.1(2) . . ? N2 Ni1 O3 94.23(19) . . ? N1 Ni1 O3 178.49(17) . . ? N2 Ni1 O2 178.89(18) . . ? N1 Ni1 O2 94.25(19) . . ? O3 Ni1 O2 85.41(13) . . ? N3 Ni2 O6 94.7(2) . . ? N3 Ni2 O7 179.50(19) . . ? O6 Ni2 O7 84.89(13) . . ? N3 Ni2 N4 84.1(2) . . ? O6 Ni2 N4 178.9(2) . . ? O7 Ni2 N4 96.2(2) . . ? C2 O1 C1 116.0(5) . . ? C7 O2 Ni1 127.0(3) . . ? C17 O3 Ni1 127.1(3) . . ? C16 O4 C18 116.7(5) . . ? C22 O5 C21 116.9(5) . . ? C27 O6 Ni2 126.7(3) . . ? C37 O7 Ni2 127.4(3) . . ? C36 O8 C38 118.3(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.904 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.070 # Attachment 'C5_max36.cif' data_max36 _database_code_depnum_ccdc_archive 'CCDC 809440' #TrackingRef 'C5_max36.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H62 Cr N11 Ni2 O10 S4' _chemical_formula_weight 1226.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' _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 10.9775(9) _cell_length_b 12.3684(9) _cell_length_c 12.8226(10) _cell_angle_alpha 63.924(5) _cell_angle_beta 69.868(6) _cell_angle_gamma 79.319(6) _cell_volume 1467.0(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3482 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 26.42 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 631 _exptl_absorpt_coefficient_mu 1.019 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7084 _exptl_absorpt_correction_T_max 0.7360 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10713 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0693 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.21 _reflns_number_total 5492 _reflns_number_gt 3658 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0614P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5492 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.1153 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _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 C1 C 0.3156(5) -0.2986(4) 0.1198(5) 0.0642(12) Uani 1 1 d . . . H1A H 0.3325 -0.2644 0.0332 0.096 Uiso 1 1 calc R . . H1B H 0.2334 -0.3361 0.1586 0.096 Uiso 1 1 calc R . . H1C H 0.3829 -0.3578 0.1417 0.096 Uiso 1 1 calc R . . C2 C 0.2908(3) -0.2370(3) 0.2795(4) 0.0455(9) Uani 1 1 d . . . C3 C 0.2713(4) -0.3516(4) 0.3682(4) 0.0659(13) Uani 1 1 d . . . H3 H 0.2710 -0.4148 0.3475 0.079 Uiso 1 1 calc R . . C4 C 0.2517(5) -0.3741(4) 0.4892(5) 0.0794(16) Uani 1 1 d . . . H4 H 0.2378 -0.4521 0.5489 0.095 Uiso 1 1 calc R . . C5 C 0.2530(5) -0.2830(4) 0.5201(4) 0.0691(14) Uani 1 1 d . . . H5 H 0.2422 -0.2995 0.6008 0.083 Uiso 1 1 calc R . . C6 C 0.2702(4) -0.1639(4) 0.4324(3) 0.0479(9) Uani 1 1 d . . . C7 C 0.2904(3) -0.1401(3) 0.3100(3) 0.0394(8) Uani 1 1 d . . . C8 C 0.2764(4) -0.0695(4) 0.4658(3) 0.0529(10) Uani 1 1 d . . . H8 H 0.2793 -0.0925 0.5444 0.063 Uiso 1 1 calc R . . C9 C 0.3000(4) 0.1270(4) 0.4435(4) 0.0538(10) Uani 1 1 d . . . H9A H 0.3761 0.1726 0.3866 0.065 Uiso 1 1 calc R . . H9B H 0.3182 0.0801 0.5205 0.065 Uiso 1 1 calc R . . C10 C 0.1859(4) 0.2150(4) 0.4616(3) 0.0533(10) Uani 1 1 d . . . C11 C 0.0846(5) 0.1553(5) 0.5834(4) 0.0824(16) Uani 1 1 d . . . H11A H 0.0523 0.0874 0.5851 0.124 Uiso 1 1 calc R . . H11B H 0.0142 0.2122 0.5942 0.124 Uiso 1 1 calc R . . H11C H 0.1234 0.1288 0.6477 0.124 Uiso 1 1 calc R . . C12 C 0.2395(7) 0.3247(5) 0.4545(5) 0.0934(18) Uani 1 1 d . . . H12A H 0.1697 0.3820 0.4655 0.140 Uiso 1 1 calc R . . H12B H 0.3019 0.3613 0.3763 0.140 Uiso 1 1 calc R . . H12C H 0.2805 0.2997 0.5171 0.140 Uiso 1 1 calc R . . C13 C 0.1226(4) 0.2550(4) 0.3597(4) 0.0599(11) Uani 1 1 d . . . H13A H 0.0568 0.1987 0.3844 0.072 Uiso 1 1 calc R . . H13B H 0.0797 0.3336 0.3484 0.072 Uiso 1 1 calc R . . C14 C 0.2372(5) 0.3651(4) 0.1521(4) 0.0573(11) Uani 1 1 d . . . H14 H 0.2069 0.4329 0.1688 0.069 Uiso 1 1 calc R . . C15 C 0.3030(4) 0.3849(4) 0.0277(4) 0.0516(10) Uani 1 1 d . . . C16 C 0.3291(5) 0.5034(4) -0.0609(4) 0.0721(14) Uani 1 1 d . . . H16 H 0.3160 0.5665 -0.0369 0.086 Uiso 1 1 calc R . . C17 C 0.3734(5) 0.5261(4) -0.1814(4) 0.0708(14) Uani 1 1 d . . . H17 H 0.3939 0.6041 -0.2389 0.085 Uiso 1 1 calc R . . C18 C 0.3882(4) 0.4336(4) -0.2186(4) 0.0562(11) Uani 1 1 d . . . H18 H 0.4156 0.4503 -0.3011 0.067 Uiso 1 1 calc R . . C19 C 0.3626(4) 0.3169(3) -0.1339(3) 0.0443(9) Uani 1 1 d . . . C20 C 0.3241(3) 0.2898(3) -0.0079(3) 0.0392(8) Uani 1 1 d . . . C21 C 0.3809(4) 0.2424(4) -0.2818(4) 0.0611(12) Uani 1 1 d . . . H21A H 0.3890 0.1674 -0.2893 0.092 Uiso 1 1 calc R . . H21B H 0.4549 0.2895 -0.3381 0.092 Uiso 1 1 calc R . . H21C H 0.3033 0.2859 -0.2993 0.092 Uiso 1 1 calc R . . C22 C -0.2591(4) 0.0700(4) 0.1621(4) 0.0544(10) Uani 1 1 d . . . C23 C 0.0237(4) 0.2747(4) -0.1617(4) 0.0638(13) Uani 1 1 d . . . N1 N 0.2783(3) 0.0443(3) 0.3980(3) 0.0445(7) Uani 1 1 d . . . N2 N 0.2164(3) 0.2616(3) 0.2429(3) 0.0467(8) Uani 1 1 d . . . N3 N -0.1661(3) 0.0388(3) 0.1063(3) 0.0553(9) Uani 1 1 d . . . N4 N 0.0150(3) 0.1736(3) -0.1098(3) 0.0514(8) Uani 1 1 d . . . N5 N 0.1009(3) 0.0232(3) 0.0973(3) 0.0630(10) Uani 1 1 d . . . H5A H 0.1216 0.0999 0.0646 0.094 Uiso 1 1 calc R . . H5B H 0.1730 -0.0236 0.0953 0.094 Uiso 1 1 calc R . . H5C H 0.0516 0.0032 0.1741 0.094 Uiso 1 1 calc R . . N6 N 0.5000 0.0000 0.0000 0.0642(15) Uani 1 2 d S . . O1 O 0.3128(3) -0.2056(2) 0.1585(3) 0.0533(7) Uani 1 1 d . . . O2 O 0.3117(2) -0.0320(2) 0.2210(2) 0.0417(6) Uani 1 1 d . . . O3 O 0.3050(2) 0.1759(2) 0.0690(2) 0.0424(6) Uani 1 1 d . . . O4 O 0.3743(3) 0.2196(3) -0.1610(2) 0.0545(7) Uani 1 1 d . . . O5W O -0.0638(12) 0.2417(17) 0.1810(15) 0.391(9) Uani 1 1 d . . . S1 S -0.39030(14) 0.11410(19) 0.24248(15) 0.1110(7) Uani 1 1 d . . . S2 S 0.03457(16) 0.41789(13) -0.2390(3) 0.1641(13) Uani 1 1 d . . . Cr1 Cr 0.0000 0.0000 0.0000 0.0364(2) Uani 1 2 d S . . Ni1 Ni 0.27795(4) 0.11362(4) 0.23519(4) 0.03597(14) 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 C1 0.075(3) 0.051(2) 0.091(3) -0.045(3) -0.040(3) 0.008(2) C2 0.0415(19) 0.036(2) 0.053(2) -0.0151(18) -0.0109(17) -0.0043(16) C3 0.070(3) 0.039(2) 0.077(3) -0.019(2) -0.012(2) -0.008(2) C4 0.103(4) 0.034(2) 0.062(3) 0.000(2) -0.003(3) -0.008(2) C5 0.089(3) 0.051(3) 0.035(2) -0.001(2) -0.005(2) 0.002(2) C6 0.055(2) 0.039(2) 0.045(2) -0.0172(18) -0.0140(17) 0.0073(17) C7 0.0388(18) 0.0346(19) 0.0399(18) -0.0116(16) -0.0124(15) 0.0021(15) C8 0.061(2) 0.057(3) 0.0340(19) -0.0172(19) -0.0148(17) 0.012(2) C9 0.058(2) 0.068(3) 0.049(2) -0.036(2) -0.0184(19) 0.003(2) C10 0.067(3) 0.051(2) 0.045(2) -0.030(2) -0.0095(19) 0.004(2) C11 0.084(3) 0.090(4) 0.054(3) -0.032(3) -0.003(2) 0.014(3) C12 0.141(5) 0.076(4) 0.085(4) -0.051(3) -0.035(4) -0.001(4) C13 0.062(3) 0.061(3) 0.054(2) -0.032(2) -0.013(2) 0.017(2) C14 0.089(3) 0.037(2) 0.055(2) -0.028(2) -0.025(2) 0.010(2) C15 0.075(3) 0.035(2) 0.046(2) -0.0183(19) -0.021(2) 0.0021(19) C16 0.118(4) 0.036(2) 0.064(3) -0.016(2) -0.036(3) -0.003(2) C17 0.107(4) 0.037(2) 0.058(3) -0.004(2) -0.030(3) -0.008(2) C18 0.069(3) 0.054(3) 0.039(2) -0.010(2) -0.0183(19) -0.004(2) C19 0.047(2) 0.045(2) 0.045(2) -0.0188(18) -0.0198(16) 0.0047(17) C20 0.047(2) 0.0329(19) 0.0365(18) -0.0114(16) -0.0164(15) 0.0005(15) C21 0.070(3) 0.077(3) 0.047(2) -0.033(2) -0.022(2) 0.001(2) C22 0.047(2) 0.058(3) 0.049(2) -0.021(2) -0.0088(19) 0.0027(19) C23 0.036(2) 0.049(3) 0.081(3) -0.016(2) -0.003(2) -0.0007(18) N1 0.0500(18) 0.0496(19) 0.0393(16) -0.0241(16) -0.0173(14) 0.0089(14) N2 0.0602(19) 0.0418(18) 0.0420(17) -0.0245(15) -0.0144(15) 0.0068(15) N3 0.0415(18) 0.057(2) 0.058(2) -0.0241(18) -0.0052(16) 0.0032(15) N4 0.0497(19) 0.0384(19) 0.0544(19) -0.0109(16) -0.0122(15) -0.0023(15) N5 0.058(2) 0.071(2) 0.068(2) -0.026(2) -0.0294(18) -0.0073(18) N6 0.062(3) 0.042(3) 0.057(3) -0.017(2) 0.010(2) 0.009(2) O1 0.0729(18) 0.0371(14) 0.0630(17) -0.0270(14) -0.0284(14) 0.0005(13) O2 0.0587(15) 0.0291(13) 0.0375(12) -0.0127(11) -0.0154(11) -0.0022(11) O3 0.0615(16) 0.0307(13) 0.0372(13) -0.0154(11) -0.0152(11) -0.0016(11) O4 0.0789(19) 0.0495(16) 0.0417(14) -0.0227(13) -0.0241(13) 0.0050(14) O5W 0.255(11) 0.67(3) 0.52(2) -0.50(2) -0.172(13) 0.122(14) S1 0.0687(9) 0.1450(16) 0.0908(11) -0.0576(11) 0.0003(8) 0.0390(9) S2 0.0739(10) 0.0375(7) 0.252(3) 0.0078(11) 0.0127(12) -0.0007(6) Cr1 0.0304(4) 0.0353(4) 0.0411(4) -0.0139(4) -0.0105(3) -0.0003(3) Ni1 0.0439(3) 0.0328(2) 0.0334(2) -0.01557(19) -0.01278(19) 0.00138(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.431(5) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.365(5) . ? C2 C3 1.370(5) . ? C2 C7 1.413(5) . ? C3 C4 1.395(7) . ? C3 H3 0.9300 . ? C4 C5 1.352(7) . ? C4 H4 0.9300 . ? C5 C6 1.404(5) . ? C5 H5 0.9300 . ? C6 C7 1.406(5) . ? C6 C8 1.429(6) . ? C7 O2 1.317(4) . ? C8 N1 1.288(5) . ? C8 H8 0.9300 . ? C9 N1 1.467(5) . ? C9 C10 1.524(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.522(6) . ? C10 C12 1.532(7) . ? C10 C13 1.537(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N2 1.474(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N2 1.289(5) . ? C14 C15 1.433(6) . ? C14 H14 0.9300 . ? C15 C20 1.394(6) . ? C15 C16 1.410(5) . ? C16 C17 1.361(7) . ? C16 H16 0.9300 . ? C17 C18 1.386(7) . ? C17 H17 0.9300 . ? C18 C19 1.380(5) . ? C18 H18 0.9300 . ? C19 O4 1.366(5) . ? C19 C20 1.417(5) . ? C20 O3 1.322(4) . ? C21 O4 1.424(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N3 1.139(5) . ? C22 S1 1.617(5) . ? C23 N4 1.133(5) . ? C23 S2 1.608(4) . ? N1 Ni1 1.877(3) . ? N2 Ni1 1.863(3) . ? N3 Cr1 1.988(3) . ? N4 Cr1 1.983(3) . ? N5 Cr1 2.061(3) . ? N5 H5A 0.8900 . ? N5 H5B 0.8900 . ? N5 H5C 0.8900 . ? O2 Ni1 1.847(3) . ? O3 Ni1 1.852(2) . ? Cr1 N4 1.983(3) 2 ? Cr1 N3 1.988(3) 2 ? Cr1 N5 2.061(3) 2 ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 125.1(4) . . ? O1 C2 C7 114.7(3) . . ? C3 C2 C7 120.2(4) . . ? C2 C3 C4 120.5(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 120.3(4) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C7 119.2(4) . . ? C5 C6 C8 120.3(4) . . ? C7 C6 C8 120.4(3) . . ? O2 C7 C6 123.5(4) . . ? O2 C7 C2 117.7(3) . . ? C6 C7 C2 118.8(3) . . ? N1 C8 C6 126.6(4) . . ? N1 C8 H8 116.7 . . ? C6 C8 H8 116.7 . . ? N1 C9 C10 114.0(3) . . ? N1 C9 H9A 108.7 . . ? C10 C9 H9A 108.7 . . ? N1 C9 H9B 108.7 . . ? C10 C9 H9B 108.7 . . ? H9A C9 H9B 107.6 . . ? C11 C10 C9 110.4(4) . . ? C11 C10 C12 111.3(4) . . ? C9 C10 C12 107.5(4) . . ? C11 C10 C13 108.7(4) . . ? C9 C10 C13 109.5(3) . . ? C12 C10 C13 109.4(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C10 113.1(3) . . ? N2 C13 H13A 109.0 . . ? C10 C13 H13A 109.0 . . ? N2 C13 H13B 109.0 . . ? C10 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? N2 C14 C15 125.7(4) . . ? N2 C14 H14 117.1 . . ? C15 C14 H14 117.1 . . ? C20 C15 C16 119.9(4) . . ? C20 C15 C14 119.9(3) . . ? C16 C15 C14 119.6(4) . . ? C17 C16 C15 120.6(5) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.3(4) . . ? C16 C17 H17 119.9 . . ? C18 C17 H17 119.9 . . ? C19 C18 C17 120.4(4) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? O4 C19 C18 124.9(4) . . ? O4 C19 C20 114.7(3) . . ? C18 C19 C20 120.3(4) . . ? O3 C20 C15 124.0(3) . . ? O3 C20 C19 117.6(3) . . ? C15 C20 C19 118.3(3) . . ? O4 C21 H21A 109.5 . . ? O4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 S1 179.2(4) . . ? N4 C23 S2 178.0(5) . . ? C8 N1 C9 118.7(3) . . ? C8 N1 Ni1 125.1(3) . . ? C9 N1 Ni1 115.7(3) . . ? C14 N2 C13 118.8(4) . . ? C14 N2 Ni1 125.4(3) . . ? C13 N2 Ni1 115.3(3) . . ? C22 N3 Cr1 174.8(4) . . ? C23 N4 Cr1 172.4(4) . . ? Cr1 N5 H5A 109.5 . . ? Cr1 N5 H5B 109.5 . . ? H5A N5 H5B 109.5 . . ? Cr1 N5 H5C 109.5 . . ? H5A N5 H5C 109.5 . . ? H5B N5 H5C 109.5 . . ? C2 O1 C1 118.2(3) . . ? C7 O2 Ni1 127.0(2) . . ? C20 O3 Ni1 126.2(2) . . ? C19 O4 C21 117.5(3) . . ? N4 Cr1 N4 180.0(3) . 2 ? N4 Cr1 N3 89.25(14) . . ? N4 Cr1 N3 90.75(14) 2 . ? N4 Cr1 N3 90.75(14) . 2 ? N4 Cr1 N3 89.25(14) 2 2 ? N3 Cr1 N3 180.0(3) . 2 ? N4 Cr1 N5 89.64(15) . . ? N4 Cr1 N5 90.36(15) 2 . ? N3 Cr1 N5 90.09(16) . . ? N3 Cr1 N5 89.91(16) 2 . ? N4 Cr1 N5 90.36(15) . 2 ? N4 Cr1 N5 89.64(15) 2 2 ? N3 Cr1 N5 89.91(16) . 2 ? N3 Cr1 N5 90.09(16) 2 2 ? N5 Cr1 N5 180.0(2) . 2 ? O2 Ni1 O3 83.27(11) . . ? O2 Ni1 N2 169.59(12) . . ? O3 Ni1 N2 92.87(12) . . ? O2 Ni1 N1 93.54(13) . . ? O3 Ni1 N1 171.08(12) . . ? N2 Ni1 N1 91.64(14) . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 26.21 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.714 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.070 # Attachment 'C7_max7b.cif' data_max7b _database_code_depnum_ccdc_archive 'CCDC 809442' #TrackingRef 'C7_max7b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H26 Au Cr N8 O4 S4' _chemical_formula_weight 855.72 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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.4463(5) _cell_length_b 16.4541(16) _cell_length_c 25.4253(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3115.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4856 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1676 _exptl_absorpt_coefficient_mu 5.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5321 _exptl_absorpt_correction_T_max 0.5791 _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE-IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20077 _diffrn_reflns_av_R_equivalents 0.1372 _diffrn_reflns_av_sigmaI/netI 0.2039 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 25.34 _reflns_number_total 5671 _reflns_number_gt 2899 _reflns_threshold_expression >2sigma(I) _computing_data_collection X-Area _computing_cell_refinement X-Area _computing_data_reduction X-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.002(12) _refine_ls_number_reflns 5671 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1246 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 0.701 _refine_ls_restrained_S_all 0.701 _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 C1 C 0.919(3) 0.4145(9) 1.0403(6) 0.085(6) Uani 1 1 d . . . H1A H 0.8214 0.3935 1.0609 0.128 Uiso 1 1 calc R . . H1B H 0.9442 0.4693 1.0509 0.128 Uiso 1 1 calc R . . H1C H 1.0236 0.3814 1.0456 0.128 Uiso 1 1 calc R . . C2 C 0.889(2) 0.3400(9) 0.9618(7) 0.063(5) Uani 1 1 d . . . C3 C 0.937(2) 0.2686(8) 0.9875(8) 0.078(6) Uani 1 1 d . . . H3 H 0.9640 0.2685 1.0232 0.094 Uiso 1 1 calc R . . C4 C 0.943(2) 0.1955(11) 0.9573(7) 0.068(5) Uiso 1 1 d . . . H4 H 0.9866 0.1481 0.9727 0.082 Uiso 1 1 calc R . . C5 C 0.890(2) 0.1944(9) 0.9088(8) 0.079(6) Uani 1 1 d . . . H5 H 0.8829 0.1444 0.8918 0.095 Uiso 1 1 calc R . . C6 C 0.8420(18) 0.2651(7) 0.8803(6) 0.047(4) Uani 1 1 d . . . C7 C 0.841(2) 0.3384(8) 0.9062(6) 0.054(4) Uani 1 1 d . . . C8 C 0.775(3) 0.2587(9) 0.8274(7) 0.076(6) Uani 1 1 d . . . H8 H 0.7527 0.2061 0.8155 0.091 Uiso 1 1 calc R . . C9 C 0.648(3) 0.2879(11) 0.7439(8) 0.097(7) Uani 1 1 d . . . H9A H 0.7234 0.2462 0.7282 0.116 Uiso 1 1 calc R . . H9B H 0.5367 0.2621 0.7541 0.116 Uiso 1 1 calc R . . C10 C 0.609(4) 0.3444(15) 0.7049(9) 0.189(16) Uani 1 1 d . . . H10A H 0.5965 0.3137 0.6725 0.227 Uiso 1 1 calc R . . H10B H 0.4904 0.3654 0.7131 0.227 Uiso 1 1 calc R . . C11 C 0.707(5) 0.4070(10) 0.6934(8) 0.168(13) Uani 1 1 d . . . H11A H 0.6467 0.4374 0.6659 0.201 Uiso 1 1 calc R . . H11B H 0.8198 0.3877 0.6791 0.201 Uiso 1 1 calc R . . C12 C 0.780(3) 0.5423(13) 0.7210(6) 0.093(7) Uani 1 1 d . . . H12 H 0.7904 0.5495 0.6849 0.112 Uiso 1 1 calc R . . C13 C 0.800(2) 0.6114(8) 0.7508(5) 0.047(4) Uani 1 1 d . . . C14 C 0.825(2) 0.6868(10) 0.7238(6) 0.065(5) Uani 1 1 d . . . H14 H 0.8370 0.6862 0.6874 0.078 Uiso 1 1 calc R . . C15 C 0.833(2) 0.7593(9) 0.7492(7) 0.070(5) Uani 1 1 d . . . H15 H 0.8375 0.8079 0.7306 0.084 Uiso 1 1 calc R . . C16 C 0.8346(18) 0.7586(7) 0.8046(7) 0.059(4) Uani 1 1 d . . . H16 H 0.8380 0.8081 0.8223 0.070 Uiso 1 1 calc R . . C17 C 0.8310(16) 0.6863(7) 0.8346(5) 0.041(4) Uiso 1 1 d . . . C18 C 0.8040(16) 0.6129(6) 0.8067(6) 0.035(3) Uani 1 1 d . . . C19 C 0.834(3) 0.7592(8) 0.9144(6) 0.083(7) Uani 1 1 d . . . H19A H 0.9296 0.7920 0.9002 0.125 Uiso 1 1 calc R . . H19B H 0.8560 0.7497 0.9511 0.125 Uiso 1 1 calc R . . H19C H 0.7221 0.7870 0.9101 0.125 Uiso 1 1 calc R . . C20 C 0.8138(16) -0.0561(8) 1.1773(5) 0.048(4) Uani 1 1 d . . . C21 C 0.8366(18) 0.1181(8) 1.0894(6) 0.043(4) Uani 1 1 d . . . C22 C 0.830(2) -0.0376(7) 0.9333(7) 0.058(5) Uani 1 1 d . . . C23 C 0.843(2) -0.2494(11) 1.0524(6) 0.058(5) Uani 1 1 d . . . Au1 Au 0.77017(8) 0.43244(3) 0.81043(2) 0.04924(15) Uani 1 1 d . . . Cr1 Cr 0.8341(3) -0.05993(14) 1.05612(9) 0.0378(6) Uani 1 1 d . . . N1 N 0.741(2) 0.3164(7) 0.7939(5) 0.071(4) Uani 1 1 d . . . N2 N 0.747(3) 0.4635(7) 0.7374(5) 0.075(4) Uani 1 1 d . . . N3 N 0.8311(16) -0.0671(9) 1.1342(5) 0.059(4) Uani 1 1 d . . . N4 N 0.8297(14) 0.0596(8) 1.0660(5) 0.059(4) Uani 1 1 d . . . N5 N 0.8334(15) -0.0477(6) 0.9775(5) 0.049(3) Uani 1 1 d . . . N6 N 0.8339(16) -0.1807(7) 1.0509(5) 0.054(4) Uani 1 1 d . . . N7 N 1.1061(12) -0.0551(6) 1.0534(4) 0.043(3) Uani 1 1 d . . . H7A H 1.1420 -0.0038 1.0568 0.065 Uiso 1 1 calc R . . H7B H 1.1441 -0.0747 1.0227 0.065 Uiso 1 1 calc R . . H7C H 1.1516 -0.0848 1.0794 0.065 Uiso 1 1 calc R . . N8 N 0.5536(12) -0.0629(9) 1.0550(5) 0.062(4) Uani 1 1 d . . . H8A H 0.5115 -0.0134 1.0483 0.093 Uiso 1 1 calc R . . H8B H 0.5132 -0.0796 1.0861 0.093 Uiso 1 1 calc R . . H8C H 0.5167 -0.0971 1.0301 0.093 Uiso 1 1 calc R . . O1 O 0.8704(13) 0.4134(5) 0.9858(4) 0.065(3) Uani 1 1 d . . . O2 O 0.7956(12) 0.4118(4) 0.8871(3) 0.047(3) Uani 1 1 d . . . O3 O 0.7995(14) 0.5481(6) 0.8355(3) 0.064(3) Uani 1 1 d . . . O4 O 0.8281(14) 0.6821(5) 0.8868(4) 0.054(3) Uani 1 1 d . . . S1 S 0.7843(10) -0.0404(3) 1.24070(17) 0.1021(19) Uani 1 1 d . . . S2 S 0.8501(7) 0.2016(3) 1.12299(19) 0.0805(16) Uani 1 1 d . . . S3 S 0.8259(9) -0.0243(2) 0.86982(17) 0.101(2) Uani 1 1 d . . . S4 S 0.8330(6) -0.3497(2) 1.05705(16) 0.0663(14) 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 C1 0.155(17) 0.057(12) 0.044(11) 0.003(9) -0.002(11) -0.012(11) C2 0.088(12) 0.043(10) 0.058(12) 0.023(9) 0.020(10) -0.011(8) C3 0.107(15) 0.029(10) 0.099(16) 0.014(9) 0.035(13) 0.008(9) C5 0.108(15) 0.023(8) 0.106(17) -0.013(9) 0.015(13) -0.023(9) C6 0.057(10) 0.017(7) 0.066(11) -0.010(7) 0.016(8) -0.014(6) C7 0.062(11) 0.037(8) 0.062(12) 0.010(8) 0.021(9) -0.003(7) C8 0.090(15) 0.055(10) 0.083(15) -0.042(9) 0.008(14) -0.033(12) C9 0.137(18) 0.061(12) 0.094(16) -0.027(12) -0.022(14) -0.020(11) C10 0.34(4) 0.14(2) 0.09(2) 0.034(17) -0.06(2) -0.18(2) C11 0.31(4) 0.105(15) 0.085(13) -0.083(14) -0.09(3) 0.09(2) C12 0.068(12) 0.18(2) 0.031(9) 0.010(11) 0.014(11) 0.026(16) C13 0.054(11) 0.045(8) 0.041(9) 0.006(7) 0.012(9) 0.015(8) C14 0.077(14) 0.083(12) 0.035(9) 0.005(9) 0.014(9) 0.022(10) C15 0.088(14) 0.036(9) 0.086(14) 0.003(9) 0.010(11) -0.014(8) C16 0.101(13) 0.023(6) 0.052(10) 0.023(7) -0.013(11) -0.005(6) C18 0.049(9) 0.019(6) 0.038(8) 0.011(6) 0.004(9) 0.000(6) C19 0.143(19) 0.047(9) 0.060(12) -0.022(8) -0.011(12) -0.015(10) C20 0.052(8) 0.037(7) 0.056(10) 0.002(8) -0.008(8) -0.007(6) C21 0.046(9) 0.032(8) 0.051(10) 0.003(7) 0.021(8) 0.000(7) C22 0.086(13) 0.026(7) 0.064(11) -0.005(7) -0.003(10) -0.003(6) C23 0.052(11) 0.092(13) 0.031(9) -0.005(9) 0.014(8) 0.018(10) Au1 0.0497(3) 0.0513(3) 0.0467(3) -0.0127(4) 0.0022(4) 0.0046(4) Cr1 0.0478(13) 0.0282(11) 0.0373(13) -0.0003(12) 0.0015(10) 0.0004(12) N1 0.069(9) 0.084(9) 0.060(9) -0.013(7) -0.011(11) -0.008(11) N2 0.088(11) 0.066(9) 0.070(9) -0.013(6) -0.013(12) 0.023(11) N3 0.079(10) 0.060(7) 0.037(7) -0.006(8) 0.013(7) -0.009(10) N4 0.044(8) 0.048(7) 0.086(10) -0.001(9) -0.001(7) -0.002(8) N5 0.067(9) 0.038(8) 0.042(7) 0.000(6) -0.010(7) -0.004(5) N6 0.047(9) 0.040(7) 0.074(10) -0.016(7) 0.003(7) 0.017(6) N7 0.062(7) 0.032(6) 0.037(7) -0.003(6) -0.004(6) -0.001(6) N8 0.028(6) 0.081(9) 0.077(9) 0.002(10) -0.004(7) 0.025(8) O1 0.107(8) 0.027(6) 0.059(7) 0.000(5) 0.002(6) -0.004(5) O2 0.056(7) 0.022(5) 0.062(6) -0.003(4) 0.007(5) -0.003(4) O3 0.073(8) 0.068(7) 0.052(6) -0.026(5) -0.005(6) 0.005(6) O4 0.086(9) 0.045(6) 0.030(6) 0.002(5) -0.006(6) 0.015(5) S1 0.122(5) 0.134(4) 0.050(3) -0.026(2) 0.018(4) -0.034(4) S2 0.119(4) 0.051(3) 0.072(3) -0.026(2) -0.005(3) 0.002(3) S3 0.210(7) 0.050(2) 0.042(3) 0.0038(19) 0.001(3) -0.008(3) S4 0.114(4) 0.032(2) 0.053(3) 0.0021(18) -0.002(3) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.432(16) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 O1 1.360(17) . ? C2 C3 1.390(18) . ? C2 C7 1.46(2) . ? C3 C4 1.43(2) . ? C3 H3 0.9300 . ? C4 C5 1.30(2) . ? C4 H4 0.9300 . ? C5 C6 1.42(2) . ? C5 H5 0.9300 . ? C6 C7 1.375(17) . ? C6 C8 1.44(2) . ? C7 O2 1.343(14) . ? C8 N1 1.300(17) . ? C8 H8 0.9300 . ? C9 C10 1.39(2) . ? C9 N1 1.52(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.29(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N2 1.485(19) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.374(19) . ? C12 N2 1.38(2) . ? C12 H12 0.9300 . ? C13 C18 1.422(18) . ? C13 C14 1.432(18) . ? C14 C15 1.357(18) . ? C14 H14 0.9300 . ? C15 C16 1.41(2) . ? C15 H15 0.9300 . ? C16 C17 1.413(16) . ? C16 H16 0.9300 . ? C17 O4 1.330(14) . ? C17 C18 1.415(16) . ? C18 O3 1.292(12) . ? C19 O4 1.451(14) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 N3 1.117(15) . ? C20 S1 1.648(14) . ? C21 N4 1.133(15) . ? C21 S2 1.621(14) . ? C22 N5 1.136(17) . ? C22 S3 1.628(17) . ? C23 N6 1.133(16) . ? C23 S4 1.657(18) . ? Au1 N2 1.933(12) . ? Au1 N1 1.968(12) . ? Au1 O2 1.987(9) . ? Au1 O3 2.019(9) . ? Cr1 N4 1.982(14) . ? Cr1 N3 1.989(12) . ? Cr1 N6 1.992(13) . ? Cr1 N5 2.010(12) . ? Cr1 N7 2.028(9) . ? Cr1 N8 2.089(9) . ? N7 H7A 0.8900 . ? N7 H7B 0.8900 . ? N7 H7C 0.8900 . ? N8 H8A 0.8900 . ? N8 H8B 0.8900 . ? N8 H8C 0.8900 . ? 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 O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.4(16) . . ? O1 C2 C7 115.1(13) . . ? C3 C2 C7 120.3(16) . . ? C2 C3 C4 117.9(18) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C5 C4 C3 120.9(16) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 123.5(15) . . ? C4 C5 H5 118.3 . . ? C6 C5 H5 118.3 . . ? C7 C6 C5 118.6(15) . . ? C7 C6 C8 120.7(14) . . ? C5 C6 C8 120.3(13) . . ? O2 C7 C6 128.0(15) . . ? O2 C7 C2 113.4(13) . . ? C6 C7 C2 118.5(14) . . ? N1 C8 C6 128.7(12) . . ? N1 C8 H8 115.6 . . ? C6 C8 H8 115.6 . . ? C10 C9 N1 119.1(16) . . ? C10 C9 H9A 107.5 . . ? N1 C9 H9A 107.5 . . ? C10 C9 H9B 107.5 . . ? N1 C9 H9B 107.5 . . ? H9A C9 H9B 107.0 . . ? C11 C10 C9 125(3) . . ? C11 C10 H10A 106.1 . . ? C9 C10 H10A 106.1 . . ? C11 C10 H10B 106.1 . . ? C9 C10 H10B 106.1 . . ? H10A C10 H10B 106.3 . . ? C10 C11 N2 116(2) . . ? C10 C11 H11A 108.2 . . ? N2 C11 H11A 108.2 . . ? C10 C11 H11B 108.2 . . ? N2 C11 H11B 108.2 . . ? H11A C11 H11B 107.4 . . ? C13 C12 N2 128.9(13) . . ? C13 C12 H12 115.6 . . ? N2 C12 H12 115.6 . . ? C12 C13 C18 124.6(12) . . ? C12 C13 C14 117.8(14) . . ? C18 C13 C14 117.5(12) . . ? C15 C14 C13 122.6(15) . . ? C15 C14 H14 118.7 . . ? C13 C14 H14 118.7 . . ? C14 C15 C16 118.0(14) . . ? C14 C15 H15 121.0 . . ? C16 C15 H15 121.0 . . ? C15 C16 C17 123.1(13) . . ? C15 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? O4 C17 C16 125.7(12) . . ? O4 C17 C18 116.9(11) . . ? C16 C17 C18 116.9(13) . . ? O3 C18 C17 115.2(12) . . ? O3 C18 C13 123.3(11) . . ? C17 C18 C13 121.2(11) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 S1 178.9(14) . . ? N4 C21 S2 179.0(14) . . ? N5 C22 S3 179.3(11) . . ? N6 C23 S4 173.7(15) . . ? N2 Au1 N1 92.4(5) . . ? N2 Au1 O2 174.5(4) . . ? N1 Au1 O2 93.1(4) . . ? N2 Au1 O3 93.6(4) . . ? N1 Au1 O3 174.0(5) . . ? O2 Au1 O3 80.9(3) . . ? N4 Cr1 N3 86.1(6) . . ? N4 Cr1 N6 176.4(5) . . ? N3 Cr1 N6 90.4(6) . . ? N4 Cr1 N5 91.5(5) . . ? N3 Cr1 N5 177.5(5) . . ? N6 Cr1 N5 91.9(5) . . ? N4 Cr1 N7 89.0(4) . . ? N3 Cr1 N7 92.7(5) . . ? N6 Cr1 N7 92.1(5) . . ? N5 Cr1 N7 88.0(4) . . ? N4 Cr1 N8 90.5(5) . . ? N3 Cr1 N8 90.1(5) . . ? N6 Cr1 N8 88.5(6) . . ? N5 Cr1 N8 89.2(5) . . ? N7 Cr1 N8 177.1(5) . . ? C8 N1 C9 114.3(14) . . ? C8 N1 Au1 123.2(10) . . ? C9 N1 Au1 121.9(11) . . ? C12 N2 C11 113.3(14) . . ? C12 N2 Au1 121.4(10) . . ? C11 N2 Au1 125.2(11) . . ? C20 N3 Cr1 165.9(15) . . ? C21 N4 Cr1 155.4(13) . . ? C22 N5 Cr1 177.1(11) . . ? C23 N6 Cr1 173.2(14) . . ? Cr1 N7 H7A 109.5 . . ? Cr1 N7 H7B 109.5 . . ? H7A N7 H7B 109.5 . . ? Cr1 N7 H7C 109.5 . . ? H7A N7 H7C 109.5 . . ? H7B N7 H7C 109.5 . . ? Cr1 N8 H8A 109.5 . . ? Cr1 N8 H8B 109.5 . . ? H8A N8 H8B 109.5 . . ? Cr1 N8 H8C 109.5 . . ? H8A N8 H8C 109.5 . . ? H8B N8 H8C 109.5 . . ? C2 O1 C1 114.8(11) . . ? C7 O2 Au1 122.2(8) . . ? C18 O3 Au1 127.0(8) . . ? C17 O4 C19 115.8(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.164 _refine_diff_density_min -1.084 _refine_diff_density_rms 0.110