# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_wag342 #TrackingRef 'wag342.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H72 Cl8 Mn4 N16 O3' _chemical_formula_weight 1724.83 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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 9.650(5) _cell_length_b 12.313(7) _cell_length_c 17.436(10) _cell_angle_alpha 87.08(4) _cell_angle_beta 76.79(3) _cell_angle_gamma 87.47(3) _cell_volume 2013.1(19) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 2398 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 20.81 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 882 _exptl_absorpt_coefficient_mu 0.934 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6524 _exptl_absorpt_correction_T_max 0.9816 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26842 _diffrn_reflns_av_R_equivalents 0.2127 _diffrn_reflns_av_sigmaI/netI 0.2176 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6950 _reflns_number_gt 3403 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. Asymm unit contains half of the tetrametallic complex plus half a MeOH and 0.75 and 0.25 occupancy water molecules of solvation. Other half is generated by inversion. Tetranuclear complex, [Mn(II)4 (LMe)2 (mu2-Cl)2 (Cl)6].MeOH.2H2O, features a central double-Cl- bridge; other Cl- are terminal. In each ligand only one of the two pockets binds in the usual tetradentate fashion, the other binds in a terdentate manner, with the pyrimidine N absent from the coord sphere. Very weak dataset indeed so refinement remarkably good under the circumstances. Data cutoff at 0.84A resolution using SHEL. OMIT 0 0 1 as behind beamstop. All non-H ANIS but DELU and SIMU applied to all atoms (default std devs) and 4 atoms required strong ISOR restraints too. All H calc and ride except on water molecules where they were found and AFIX 01'ed, and on the methanol molecule where AFIX 147 was used to locate the H atom but it was then AFIX 01'ed. H-bonds present. ; _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^)+(0.1840P)^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 6950 _refine_ls_number_parameters 491 _refine_ls_number_restraints 490 _refine_ls_R_factor_all 0.2197 _refine_ls_R_factor_gt 0.1191 _refine_ls_wR_factor_ref 0.3486 _refine_ls_wR_factor_gt 0.2866 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 1.16396(17) 0.51827(13) 0.41551(10) 0.0345(5) Uani 1 1 d U . . Mn2 Mn 0.68475(18) 1.14844(14) 0.20942(11) 0.0425(6) Uani 1 1 d U . . C1 C 0.7746(12) 0.9858(9) 0.3439(7) 0.040(2) Uani 1 1 d U . . C2 C 0.8440(13) 0.9059(9) 0.3819(7) 0.045(3) Uani 1 1 d U . . H2 H 0.8702 0.9193 0.4298 0.054 Uiso 1 1 calc R . . C3 C 0.8730(11) 0.8082(9) 0.3483(7) 0.035(2) Uani 1 1 d U . . N11 N 0.8427(9) 0.7902(7) 0.2777(5) 0.038(2) Uani 1 1 d U . . C4 C 0.7761(12) 0.8725(9) 0.2430(7) 0.043(3) Uani 1 1 d U . . N15 N 0.7429(9) 0.9715(7) 0.2746(6) 0.0381(19) Uani 1 1 d U . . C5 C 0.7399(13) 0.8499(9) 0.1682(7) 0.041(2) Uani 1 1 d U . . C6 C 0.8279(15) 0.7851(10) 0.1165(7) 0.056(3) Uani 1 1 d U . . H6 H 0.9126 0.7542 0.1287 0.067 Uiso 1 1 calc R . . C7 C 0.7948(16) 0.7642(11) 0.0467(8) 0.063(4) Uani 1 1 d U . . H7 H 0.8598 0.7215 0.0099 0.076 Uiso 1 1 calc R . . C8 C 0.6660(16) 0.8044(11) 0.0276(8) 0.060(3) Uani 1 1 d U . . H8 H 0.6407 0.7864 -0.0196 0.072 Uiso 1 1 calc R . . C9 C 0.5787(14) 0.8717(9) 0.0820(8) 0.052(3) Uani 1 1 d U . . H9 H 0.4937 0.9031 0.0705 0.062 Uiso 1 1 calc R . . C10 C 0.6133(12) 0.8937(9) 0.1524(8) 0.046(3) Uani 1 1 d U . . H10 H 0.5514 0.9381 0.1894 0.055 Uiso 1 1 calc R . . C11 C 0.9436(11) 0.7148(9) 0.3865(7) 0.037(2) Uani 1 1 d U . . H11A H 0.9862 0.7450 0.4271 0.045 Uiso 1 1 calc R . . H11B H 0.8681 0.6657 0.4144 0.045 Uiso 1 1 calc R . . N12 N 1.0543(9) 0.6485(7) 0.3357(5) 0.0355(19) Uani 1 1 d U . . C12 C 1.1702(12) 0.7121(9) 0.2863(7) 0.039(2) Uani 1 1 d U . . C14 C 1.2760(11) 0.7403(9) 0.3388(7) 0.039(2) Uani 1 1 d U . . C15 C 1.3299(12) 0.8397(9) 0.3367(8) 0.048(3) Uani 1 1 d U . . H15 H 1.2991 0.8971 0.3054 0.057 Uiso 1 1 calc R . . C16 C 1.4296(13) 0.8589(10) 0.3797(8) 0.050(3) Uani 1 1 d U . . H16 H 1.4688 0.9286 0.3780 0.060 Uiso 1 1 calc R . . C17 C 1.4715(12) 0.7718(10) 0.4261(7) 0.046(3) Uani 1 1 d U . . H17 H 1.5415 0.7807 0.4556 0.056 Uiso 1 1 calc R . . C18 C 1.4094(12) 0.6757(9) 0.4274(7) 0.042(3) Uani 1 1 d U . . H18 H 1.4395 0.6165 0.4574 0.051 Uiso 1 1 calc R . . N13 N 1.3060(9) 0.6585(7) 0.3881(6) 0.039(2) Uani 1 1 d U . . C22 C 0.9996(13) 0.5789(9) 0.2849(7) 0.042(3) Uani 1 1 d U . . H22A H 0.9110 0.5462 0.3158 0.051 Uiso 1 1 calc R . . H22B H 0.9746 0.6245 0.2413 0.051 Uiso 1 1 calc R . . C24 C 1.0983(12) 0.4921(9) 0.2515(7) 0.041(3) Uani 1 1 d U . . C25 C 1.0899(14) 0.4480(10) 0.1837(8) 0.054(3) Uani 1 1 d U . . H25 H 1.0172 0.4731 0.1578 0.065 Uiso 1 1 calc R . . C26 C 1.1878(15) 0.3648(10) 0.1504(8) 0.058(3) Uani 1 1 d U . . H26 H 1.1833 0.3329 0.1026 0.070 Uiso 1 1 calc R . . C27 C 1.2938(12) 0.3316(10) 0.1929(7) 0.044(3) Uani 1 1 d U . . H27 H 1.3654 0.2786 0.1723 0.052 Uiso 1 1 calc R . . C28 C 1.2915(12) 0.3753(9) 0.2612(7) 0.039(2) Uani 1 1 d U . . H28 H 1.3590 0.3489 0.2903 0.047 Uiso 1 1 calc R . . N14 N 1.1968(9) 0.4562(7) 0.2916(5) 0.0357(19) Uani 1 1 d U . . Cl1 Cl 0.9426(3) 0.4026(2) 0.45035(17) 0.0376(7) Uani 1 1 d U . . Cl2 Cl 1.3375(3) 0.3956(2) 0.45730(18) 0.0423(8) Uani 1 1 d U . . C31 C 0.7346(12) 1.0929(9) 0.3802(7) 0.041(2) Uani 1 1 d U . . H31A H 0.6323 1.0941 0.4067 0.049 Uiso 1 1 calc R . . H31B H 0.7896 1.1018 0.4209 0.049 Uiso 1 1 calc R . . N16 N 0.7615(9) 1.1841(7) 0.3223(6) 0.0415(19) Uani 1 1 d U . . C32 C 0.6794(13) 1.2811(9) 0.3558(8) 0.049(3) Uani 1 1 d U . . H32A H 0.7251 1.3104 0.3954 0.059 Uiso 1 1 calc R . . H32B H 0.5820 1.2600 0.3830 0.059 Uiso 1 1 calc R . . C34 C 0.6701(12) 1.3687(10) 0.2930(8) 0.047(2) Uani 1 1 d U . . C35 C 0.6523(13) 1.4760(11) 0.3118(9) 0.058(3) Uani 1 1 d U . . H35 H 0.6483 1.4986 0.3636 0.070 Uiso 1 1 calc R . . C36 C 0.6405(13) 1.5488(11) 0.2507(10) 0.064(3) Uani 1 1 d U . . H36 H 0.6276 1.6242 0.2604 0.077 Uiso 1 1 calc R . . C37 C 0.6471(16) 1.5149(11) 0.1764(10) 0.069(4) Uani 1 1 d U . . H37 H 0.6406 1.5658 0.1345 0.083 Uiso 1 1 calc R . . C38 C 0.6632(14) 1.4056(11) 0.1642(9) 0.063(3) Uani 1 1 d U . . H38 H 0.6679 1.3813 0.1128 0.076 Uiso 1 1 calc R . . N17 N 0.6727(11) 1.3321(8) 0.2218(7) 0.052(2) Uani 1 1 d U . . C42 C 0.9157(12) 1.2053(10) 0.2974(8) 0.047(3) Uani 1 1 d U . . H42A H 0.9281 1.2826 0.2795 0.056 Uiso 1 1 calc R . . H42B H 0.9599 1.1922 0.3432 0.056 Uiso 1 1 calc R . . C44 C 0.9892(12) 1.1354(9) 0.2331(8) 0.045(2) Uani 1 1 d U . . C45 C 1.1284(12) 1.0914(10) 0.2284(8) 0.048(3) Uani 1 1 d U . . H45 H 1.1769 1.1017 0.2690 0.057 Uiso 1 1 calc R . . C46 C 1.1925(14) 1.0329(11) 0.1634(8) 0.057(3) Uani 1 1 d U . . H46 H 1.2854 1.0017 0.1600 0.069 Uiso 1 1 calc R . . C47 C 1.1250(13) 1.0191(11) 0.1040(8) 0.053(3) Uani 1 1 d U . . H47 H 1.1690 0.9784 0.0595 0.064 Uiso 1 1 calc R . . C48 C 0.9904(14) 1.0665(10) 0.1107(8) 0.053(3) Uani 1 1 d U . . H48 H 0.9431 1.0588 0.0692 0.063 Uiso 1 1 calc R . . N18 N 0.9249(10) 1.1219(8) 0.1719(6) 0.045(2) Uani 1 1 d U . . Cl3 Cl 0.4447(3) 1.1194(2) 0.2891(2) 0.0556(9) Uani 1 1 d U . . Cl4 Cl 0.6520(4) 1.1558(3) 0.0749(2) 0.0621(10) Uani 1 1 d U . . O50 O 0.774(2) 0.3251(18) -0.0675(13) 0.090(7) Uani 0.50 1 d PU . . H50 H 0.7935 0.3281 -0.0237 0.108 Uiso 0.50 1 d P . . C50 C 0.640(3) 0.379(2) -0.0671(14) 0.051(6) Uani 0.50 1 d PU . . H50A H 0.5647 0.3265 -0.0544 0.061 Uiso 0.50 1 calc PR . . H50B H 0.6425 0.4142 -0.1191 0.061 Uiso 0.50 1 calc PR . . H50C H 0.6220 0.4350 -0.0273 0.061 Uiso 0.50 1 calc PR . . O70 O 0.1542(14) 1.1657(8) 0.4283(7) 0.059(3) Uani 0.75 1 d P . . H70X H 0.1028 1.2254 0.4327 0.070 Uiso 0.75 1 d P . . H70Y H 0.2292 1.1537 0.3917 0.070 Uiso 0.75 1 d P . . O60 O 0.951(3) 0.478(3) 0.0152(18) 0.044(9) Uani 0.25 1 d P A -1 H60X H 0.9194 0.5371 0.0361 0.053 Uiso 0.25 1 d P B -1 H60Y H 0.9068 0.4516 -0.0158 0.053 Uiso 0.25 1 d P C -1 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 Mn1 0.0181(9) 0.0318(9) 0.0573(11) 0.0022(8) -0.0181(8) 0.0057(7) Mn2 0.0230(10) 0.0353(10) 0.0762(13) 0.0012(9) -0.0277(9) 0.0046(8) C1 0.029(6) 0.035(5) 0.057(6) -0.002(4) -0.016(5) 0.006(5) C2 0.045(7) 0.035(5) 0.059(7) -0.004(5) -0.022(6) 0.014(5) C3 0.016(5) 0.034(5) 0.052(6) -0.004(5) -0.002(5) 0.011(4) N11 0.025(5) 0.033(5) 0.053(5) 0.003(4) -0.009(4) 0.008(4) C4 0.035(7) 0.030(5) 0.068(6) 0.000(4) -0.022(5) 0.002(5) N15 0.019(4) 0.037(4) 0.062(5) 0.001(3) -0.017(4) 0.005(4) C5 0.042(7) 0.028(5) 0.054(6) 0.000(4) -0.013(5) 0.014(5) C6 0.059(8) 0.053(7) 0.057(7) -0.006(5) -0.025(6) 0.040(6) C7 0.064(8) 0.063(9) 0.064(7) -0.018(6) -0.020(7) 0.029(7) C8 0.068(9) 0.055(8) 0.066(8) -0.011(6) -0.033(7) 0.010(7) C9 0.046(7) 0.039(7) 0.078(8) -0.006(6) -0.031(6) 0.004(5) C10 0.025(6) 0.041(7) 0.075(7) -0.018(6) -0.018(5) 0.015(5) C11 0.018(5) 0.038(5) 0.057(6) -0.003(4) -0.014(4) 0.014(4) N12 0.020(4) 0.032(4) 0.059(6) -0.004(3) -0.018(4) 0.008(3) C12 0.032(6) 0.035(6) 0.051(6) -0.001(4) -0.015(4) 0.001(4) C14 0.019(5) 0.034(5) 0.066(7) 0.001(5) -0.018(5) 0.007(4) C15 0.029(7) 0.042(6) 0.080(8) 0.013(6) -0.029(6) -0.007(5) C16 0.035(7) 0.042(6) 0.080(9) 0.004(6) -0.030(6) -0.005(5) C17 0.032(7) 0.048(6) 0.067(8) 0.002(6) -0.029(6) -0.004(5) C18 0.024(6) 0.036(5) 0.073(8) 0.001(6) -0.025(5) 0.004(5) N13 0.018(4) 0.040(4) 0.061(5) 0.007(4) -0.019(4) -0.001(3) C22 0.035(6) 0.033(6) 0.068(7) -0.005(4) -0.032(5) 0.006(4) C24 0.035(6) 0.032(5) 0.065(6) 0.002(4) -0.031(5) 0.005(4) C25 0.051(8) 0.049(7) 0.072(8) -0.011(5) -0.034(6) 0.026(6) C26 0.062(9) 0.048(7) 0.073(8) -0.013(6) -0.038(7) 0.022(6) C27 0.025(6) 0.047(7) 0.061(7) -0.005(5) -0.016(5) 0.013(5) C28 0.026(6) 0.041(6) 0.052(6) 0.004(5) -0.016(5) 0.009(5) N14 0.018(4) 0.036(5) 0.055(5) 0.005(4) -0.016(4) 0.001(3) Cl1 0.0222(14) 0.0393(15) 0.0559(17) -0.0020(13) -0.0190(13) 0.0011(12) Cl2 0.0252(15) 0.0391(15) 0.0664(19) 0.0107(14) -0.0225(14) 0.0061(12) C31 0.021(6) 0.041(5) 0.060(6) -0.006(4) -0.008(5) 0.012(5) N16 0.020(4) 0.040(4) 0.068(5) -0.005(4) -0.018(4) 0.008(4) C32 0.027(6) 0.039(5) 0.084(7) -0.007(5) -0.019(6) 0.009(5) C34 0.017(5) 0.044(4) 0.081(6) -0.009(4) -0.015(5) 0.008(5) C35 0.032(6) 0.050(5) 0.098(7) -0.008(5) -0.027(6) 0.005(5) C36 0.020(6) 0.045(6) 0.126(9) 0.004(6) -0.018(8) 0.003(6) C37 0.053(9) 0.047(6) 0.115(8) 0.029(7) -0.038(9) -0.017(7) C38 0.046(8) 0.049(5) 0.101(8) 0.016(6) -0.034(7) -0.005(7) N17 0.033(5) 0.040(4) 0.090(6) 0.007(4) -0.031(5) 0.002(4) C42 0.020(4) 0.048(6) 0.076(6) -0.003(4) -0.019(4) 0.004(4) C44 0.025(5) 0.038(6) 0.075(7) 0.000(5) -0.019(5) -0.006(5) C45 0.019(5) 0.051(7) 0.075(7) 0.002(5) -0.013(5) -0.005(5) C46 0.032(7) 0.061(8) 0.081(8) -0.001(6) -0.020(6) 0.005(6) C47 0.027(6) 0.064(8) 0.070(7) 0.002(6) -0.014(6) -0.001(6) C48 0.045(6) 0.051(8) 0.063(7) 0.009(5) -0.016(5) 0.001(6) N18 0.026(4) 0.049(6) 0.062(5) 0.008(4) -0.015(4) -0.002(4) Cl3 0.0210(15) 0.0370(16) 0.114(3) 0.0016(17) -0.0272(16) 0.0047(13) Cl4 0.058(2) 0.055(2) 0.086(2) 0.0068(18) -0.0465(19) 0.0027(17) O50 0.038(11) 0.095(16) 0.113(16) 0.058(13) 0.020(11) 0.005(11) C50 0.040(12) 0.058(16) 0.051(14) 0.032(12) -0.005(12) -0.022(11) O70 0.068(9) 0.032(6) 0.068(8) 0.004(5) -0.004(6) 0.014(6) O60 0.014(17) 0.06(2) 0.06(2) -0.018(17) -0.007(16) 0.011(17) _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 Mn1 N13 2.217(9) . y Mn1 N14 2.277(9) . y Mn1 Cl2 2.416(3) . y Mn1 N12 2.434(8) . y Mn1 Cl1 2.554(4) 2_766 y Mn1 Cl1 2.559(3) . y Mn2 N18 2.273(10) . y Mn2 N17 2.277(10) . y Mn2 N16 2.324(9) . y Mn2 Cl4 2.434(4) . y Mn2 Cl3 2.445(4) . y Mn2 N15 2.507(9) . y C1 N15 1.334(14) . ? C1 C2 1.391(15) . ? C1 C31 1.489(16) . ? C2 C3 1.355(15) . ? C2 H2 0.9500 . ? C3 N11 1.359(14) . ? C3 C11 1.513(14) . ? N11 C4 1.366(13) . ? C4 N15 1.358(14) . ? C4 C5 1.468(16) . ? C5 C6 1.354(16) . ? C5 C10 1.393(15) . ? C6 C7 1.365(17) . ? C6 H6 0.9500 . ? C7 C8 1.421(19) . ? C7 H7 0.9500 . ? C8 C9 1.396(19) . ? C8 H8 0.9500 . ? C9 C10 1.386(16) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N12 1.468(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N12 C22 1.460(13) . ? N12 C12 1.474(14) . ? C12 C14 1.579(15) . ? C14 C15 1.347(15) . ? C14 N13 1.355(13) . ? C15 C16 1.382(15) . ? C15 H15 0.9500 . ? C16 C17 1.412(16) . ? C16 H16 0.9500 . ? C17 C18 1.347(15) . ? C17 H17 0.9500 . ? C18 N13 1.362(13) . ? C18 H18 0.9500 . ? C22 C24 1.452(16) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C24 C25 1.347(16) . ? C24 N14 1.350(13) . ? C25 C26 1.415(17) . ? C25 H25 0.9500 . ? C26 C27 1.428(16) . ? C26 H26 0.9500 . ? C27 C28 1.327(16) . ? C27 H27 0.9500 . ? C28 N14 1.364(14) . ? C28 H28 0.9500 . ? Cl1 Mn1 2.554(4) 2_766 ? C31 N16 1.462(14) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? N16 C32 1.473(14) . ? N16 C42 1.483(14) . ? C32 C34 1.513(17) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C34 N17 1.337(16) . ? C34 C35 1.371(17) . ? C35 C36 1.379(19) . ? C35 H35 0.9500 . ? C36 C37 1.37(2) . ? C36 H36 0.9500 . ? C37 C38 1.370(19) . ? C37 H37 0.9500 . ? C38 N17 1.333(16) . ? C38 H38 0.9500 . ? C42 C44 1.476(17) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C44 N18 1.371(14) . ? C44 C45 1.413(16) . ? C45 C46 1.382(18) . ? C45 H45 0.9500 . ? C46 C47 1.364(17) . ? C46 H46 0.9500 . ? C47 C48 1.383(17) . ? C47 H47 0.9500 . ? C48 N18 1.316(16) . ? C48 H48 0.9500 . ? O50 C50 1.43(3) . ? O50 H50 0.8282 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O70 H70X 0.8650 . ? O70 H70Y 0.8619 . ? O60 H60X 0.8464 . ? O60 H60Y 0.8422 . ? 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 N13 Mn1 N14 98.7(3) . . y N13 Mn1 Cl2 95.1(2) . . y N14 Mn1 Cl2 96.3(2) . . y N13 Mn1 N12 73.7(3) . . y N14 Mn1 N12 71.0(3) . . y Cl2 Mn1 N12 161.0(2) . . y N13 Mn1 Cl1 88.3(3) . 2_766 y N14 Mn1 Cl1 164.2(2) . 2_766 y Cl2 Mn1 Cl1 97.15(11) . 2_766 y N12 Mn1 Cl1 97.7(2) . 2_766 y N13 Mn1 Cl1 162.7(2) . . y N14 Mn1 Cl1 86.2(2) . . y Cl2 Mn1 Cl1 100.91(11) . . y N12 Mn1 Cl1 92.5(2) . . y Cl1 Mn1 Cl1 83.15(11) 2_766 . y N18 Mn2 N17 99.6(4) . . y N18 Mn2 N16 76.8(3) . . y N17 Mn2 N16 72.2(3) . . y N18 Mn2 Cl4 93.9(3) . . y N17 Mn2 Cl4 95.4(3) . . y N16 Mn2 Cl4 162.6(3) . . y N18 Mn2 Cl3 156.4(3) . . y N17 Mn2 Cl3 94.8(3) . . y N16 Mn2 Cl3 90.1(3) . . y Cl4 Mn2 Cl3 103.34(14) . . y N18 Mn2 N15 73.6(3) . . y N17 Mn2 N15 143.3(3) . . y N16 Mn2 N15 71.1(3) . . y Cl4 Mn2 N15 120.8(2) . . y Cl3 Mn2 N15 83.7(2) . . y N15 C1 C2 122.7(11) . . ? N15 C1 C31 117.5(9) . . ? C2 C1 C31 119.8(10) . . ? C3 C2 C1 117.7(11) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 N11 121.5(10) . . ? C2 C3 C11 121.7(10) . . ? N11 C3 C11 116.8(9) . . ? C3 N11 C4 117.8(9) . . ? N15 C4 N11 123.1(10) . . ? N15 C4 C5 120.1(9) . . ? N11 C4 C5 116.8(10) . . ? C1 N15 C4 117.1(9) . . ? C1 N15 Mn2 111.9(7) . . ? C4 N15 Mn2 129.2(7) . . ? C6 C5 C10 121.0(11) . . ? C6 C5 C4 119.9(10) . . ? C10 C5 C4 119.2(11) . . ? C5 C6 C7 120.0(12) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C6 C7 C8 122.0(13) . . ? C6 C7 H7 119.0 . . ? C8 C7 H7 119.0 . . ? C9 C8 C7 116.4(12) . . ? C9 C8 H8 121.8 . . ? C7 C8 H8 121.8 . . ? C10 C9 C8 121.5(11) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C5 119.1(11) . . ? C9 C10 H10 120.4 . . ? C5 C10 H10 120.4 . . ? N12 C11 C3 118.1(9) . . ? N12 C11 H11A 107.8 . . ? C3 C11 H11A 107.8 . . ? N12 C11 H11B 107.8 . . ? C3 C11 H11B 107.8 . . ? H11A C11 H11B 107.1 . . ? C22 N12 C11 113.8(9) . . ? C22 N12 C12 108.4(9) . . ? C11 N12 C12 114.0(9) . . ? C22 N12 Mn1 102.8(6) . . ? C11 N12 Mn1 110.2(6) . . ? C12 N12 Mn1 106.9(6) . . ? N12 C12 C14 108.3(9) . . ? C15 C14 N13 121.9(10) . . ? C15 C14 C12 122.5(9) . . ? N13 C14 C12 115.5(9) . . ? C14 C15 C16 120.6(11) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 118.1(11) . . ? C15 C16 H16 121.0 . . ? C17 C16 H16 121.0 . . ? C18 C17 C16 118.0(10) . . ? C18 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? C17 C18 N13 123.8(10) . . ? C17 C18 H18 118.1 . . ? N13 C18 H18 118.1 . . ? C14 N13 C18 117.0(9) . . ? C14 N13 Mn1 118.9(7) . . ? C18 N13 Mn1 123.3(7) . . ? C24 C22 N12 114.2(9) . . ? C24 C22 H22A 108.7 . . ? N12 C22 H22A 108.7 . . ? C24 C22 H22B 108.7 . . ? N12 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C25 C24 N14 121.4(11) . . ? C25 C24 C22 121.0(10) . . ? N14 C24 C22 117.6(10) . . ? C24 C25 C26 120.9(11) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C25 C26 C27 116.1(12) . . ? C25 C26 H26 121.9 . . ? C27 C26 H26 121.9 . . ? C28 C27 C26 119.5(11) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 N14 123.1(10) . . ? C27 C28 H28 118.4 . . ? N14 C28 H28 118.4 . . ? C24 N14 C28 118.8(10) . . ? C24 N14 Mn1 115.1(8) . . ? C28 N14 Mn1 125.3(7) . . ? Mn1 Cl1 Mn1 96.85(11) 2_766 . ? N16 C31 C1 112.5(10) . . ? N16 C31 H31A 109.1 . . ? C1 C31 H31A 109.1 . . ? N16 C31 H31B 109.1 . . ? C1 C31 H31B 109.1 . . ? H31A C31 H31B 107.8 . . ? C31 N16 C32 109.3(9) . . ? C31 N16 C42 111.3(9) . . ? C32 N16 C42 111.3(9) . . ? C31 N16 Mn2 111.1(7) . . ? C32 N16 Mn2 106.7(6) . . ? C42 N16 Mn2 107.1(7) . . ? N16 C32 C34 111.8(11) . . ? N16 C32 H32A 109.3 . . ? C34 C32 H32A 109.3 . . ? N16 C32 H32B 109.3 . . ? C34 C32 H32B 109.3 . . ? H32A C32 H32B 107.9 . . ? N17 C34 C35 124.7(12) . . ? N17 C34 C32 114.9(11) . . ? C35 C34 C32 120.3(12) . . ? C34 C35 C36 115.6(14) . . ? C34 C35 H35 122.2 . . ? C36 C35 H35 122.2 . . ? C37 C36 C35 121.5(14) . . ? C37 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? C36 C37 C38 118.2(14) . . ? C36 C37 H37 120.9 . . ? C38 C37 H37 120.9 . . ? N17 C38 C37 122.5(15) . . ? N17 C38 H38 118.8 . . ? C37 C38 H38 118.8 . . ? C38 N17 C34 117.5(12) . . ? C38 N17 Mn2 125.1(10) . . ? C34 N17 Mn2 117.4(8) . . ? C44 C42 N16 112.1(9) . . ? C44 C42 H42A 109.2 . . ? N16 C42 H42A 109.2 . . ? C44 C42 H42B 109.2 . . ? N16 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? N18 C44 C45 118.9(12) . . ? N18 C44 C42 118.3(10) . . ? C45 C44 C42 122.5(11) . . ? C46 C45 C44 118.5(12) . . ? C46 C45 H45 120.7 . . ? C44 C45 H45 120.7 . . ? C47 C46 C45 121.3(12) . . ? C47 C46 H46 119.3 . . ? C45 C46 H46 119.3 . . ? C46 C47 C48 117.7(13) . . ? C46 C47 H47 121.2 . . ? C48 C47 H47 121.2 . . ? N18 C48 C47 123.0(13) . . ? N18 C48 H48 118.5 . . ? C47 C48 H48 118.5 . . ? C48 N18 C44 120.5(11) . . ? C48 N18 Mn2 124.3(8) . . ? C44 N18 Mn2 111.5(8) . . ? C50 O50 H50 109.9 . . ? O50 C50 H50A 109.5 . . ? O50 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O50 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? H70X O70 H70Y 125.1 . . ? H60X O60 H60Y 118.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N15 C1 C2 C3 -3.6(17) . . . . ? C31 C1 C2 C3 177.3(11) . . . . ? C1 C2 C3 N11 3.6(17) . . . . ? C1 C2 C3 C11 -177.8(10) . . . . ? C2 C3 N11 C4 -2.8(15) . . . . ? C11 C3 N11 C4 178.5(10) . . . . ? C3 N11 C4 N15 1.9(16) . . . . ? C3 N11 C4 C5 -177.9(10) . . . . ? C2 C1 N15 C4 2.7(16) . . . . ? C31 C1 N15 C4 -178.2(10) . . . . ? C2 C1 N15 Mn2 -163.4(9) . . . . ? C31 C1 N15 Mn2 15.7(12) . . . . ? N11 C4 N15 C1 -1.8(16) . . . . ? C5 C4 N15 C1 177.9(10) . . . . ? N11 C4 N15 Mn2 161.5(8) . . . . ? C5 C4 N15 Mn2 -18.8(15) . . . . ? N18 Mn2 N15 C1 87.4(8) . . . . ? N17 Mn2 N15 C1 3.3(10) . . . . ? N16 Mn2 N15 C1 6.0(7) . . . . ? Cl4 Mn2 N15 C1 172.0(7) . . . . ? Cl3 Mn2 N15 C1 -86.2(7) . . . . ? N18 Mn2 N15 C4 -76.6(9) . . . . ? N17 Mn2 N15 C4 -160.7(9) . . . . ? N16 Mn2 N15 C4 -158.0(10) . . . . ? Cl4 Mn2 N15 C4 8.0(10) . . . . ? Cl3 Mn2 N15 C4 109.8(9) . . . . ? N15 C4 C5 C6 145.0(12) . . . . ? N11 C4 C5 C6 -35.2(17) . . . . ? N15 C4 C5 C10 -36.4(17) . . . . ? N11 C4 C5 C10 143.4(11) . . . . ? C10 C5 C6 C7 2(2) . . . . ? C4 C5 C6 C7 -179.7(12) . . . . ? C5 C6 C7 C8 -3(2) . . . . ? C6 C7 C8 C9 4(2) . . . . ? C7 C8 C9 C10 -3(2) . . . . ? C8 C9 C10 C5 1.7(19) . . . . ? C6 C5 C10 C9 -1.0(19) . . . . ? C4 C5 C10 C9 -179.6(11) . . . . ? C2 C3 C11 N12 -138.6(11) . . . . ? N11 C3 C11 N12 40.1(14) . . . . ? C3 C11 N12 C22 -71.1(13) . . . . ? C3 C11 N12 C12 53.9(12) . . . . ? C3 C11 N12 Mn1 174.0(7) . . . . ? N13 Mn1 N12 C22 141.0(8) . . . . ? N14 Mn1 N12 C22 35.6(7) . . . . ? Cl2 Mn1 N12 C22 85.6(10) . . . . ? Cl1 Mn1 N12 C22 -133.0(7) 2_766 . . . ? Cl1 Mn1 N12 C22 -49.6(7) . . . . ? N13 Mn1 N12 C11 -97.3(7) . . . . ? N14 Mn1 N12 C11 157.2(7) . . . . ? Cl2 Mn1 N12 C11 -152.8(6) . . . . ? Cl1 Mn1 N12 C11 -11.4(7) 2_766 . . . ? Cl1 Mn1 N12 C11 72.1(7) . . . . ? N13 Mn1 N12 C12 27.0(7) . . . . ? N14 Mn1 N12 C12 -78.5(7) . . . . ? Cl2 Mn1 N12 C12 -28.4(11) . . . . ? Cl1 Mn1 N12 C12 113.0(6) 2_766 . . . ? Cl1 Mn1 N12 C12 -163.6(6) . . . . ? C22 N12 C12 C14 -152.4(8) . . . . ? C11 N12 C12 C14 79.8(10) . . . . ? Mn1 N12 C12 C14 -42.2(9) . . . . ? N12 C12 C14 C15 -136.2(12) . . . . ? N12 C12 C14 N13 41.9(13) . . . . ? N13 C14 C15 C16 6(2) . . . . ? C12 C14 C15 C16 -175.6(12) . . . . ? C14 C15 C16 C17 -1(2) . . . . ? C15 C16 C17 C18 -1.6(19) . . . . ? C16 C17 C18 N13 -2(2) . . . . ? C15 C14 N13 C18 -9.4(18) . . . . ? C12 C14 N13 C18 172.5(10) . . . . ? C15 C14 N13 Mn1 160.7(10) . . . . ? C12 C14 N13 Mn1 -17.4(13) . . . . ? C17 C18 N13 C14 7.1(18) . . . . ? C17 C18 N13 Mn1 -162.5(10) . . . . ? N14 Mn1 N13 C14 62.1(9) . . . . ? Cl2 Mn1 N13 C14 159.3(9) . . . . ? N12 Mn1 N13 C14 -5.1(8) . . . . ? Cl1 Mn1 N13 C14 -103.7(9) 2_766 . . . ? Cl1 Mn1 N13 C14 -43.2(15) . . . . ? N14 Mn1 N13 C18 -128.4(9) . . . . ? Cl2 Mn1 N13 C18 -31.2(9) . . . . ? N12 Mn1 N13 C18 164.4(10) . . . . ? Cl1 Mn1 N13 C18 65.8(9) 2_766 . . . ? Cl1 Mn1 N13 C18 126.3(9) . . . . ? C11 N12 C22 C24 -163.4(10) . . . . ? C12 N12 C22 C24 68.7(12) . . . . ? Mn1 N12 C22 C24 -44.3(11) . . . . ? N12 C22 C24 C25 -154.9(12) . . . . ? N12 C22 C24 N14 26.1(15) . . . . ? N14 C24 C25 C26 -2(2) . . . . ? C22 C24 C25 C26 178.8(12) . . . . ? C24 C25 C26 C27 0(2) . . . . ? C25 C26 C27 C28 3.0(18) . . . . ? C26 C27 C28 N14 -4.0(18) . . . . ? C25 C24 N14 C28 1.6(16) . . . . ? C22 C24 N14 C28 -179.5(10) . . . . ? C25 C24 N14 Mn1 -168.4(10) . . . . ? C22 C24 N14 Mn1 10.5(13) . . . . ? C27 C28 N14 C24 1.7(16) . . . . ? C27 C28 N14 Mn1 170.5(9) . . . . ? N13 Mn1 N14 C24 -95.3(8) . . . . ? Cl2 Mn1 N14 C24 168.5(7) . . . . ? N12 Mn1 N14 C24 -26.0(7) . . . . ? Cl1 Mn1 N14 C24 20.2(14) 2_766 . . . ? Cl1 Mn1 N14 C24 67.9(7) . . . . ? N13 Mn1 N14 C28 95.4(8) . . . . ? Cl2 Mn1 N14 C28 -0.7(8) . . . . ? N12 Mn1 N14 C28 164.8(9) . . . . ? Cl1 Mn1 N14 C28 -149.0(8) 2_766 . . . ? Cl1 Mn1 N14 C28 -101.3(8) . . . . ? N13 Mn1 Cl1 Mn1 -61.2(9) . . . 2_766 ? N14 Mn1 Cl1 Mn1 -168.3(2) . . . 2_766 ? Cl2 Mn1 Cl1 Mn1 96.00(12) . . . 2_766 ? N12 Mn1 Cl1 Mn1 -97.5(2) . . . 2_766 ? Cl1 Mn1 Cl1 Mn1 0.0 2_766 . . 2_766 ? N15 C1 C31 N16 -40.8(14) . . . . ? C2 C1 C31 N16 138.3(11) . . . . ? C1 C31 N16 C32 161.8(9) . . . . ? C1 C31 N16 C42 -74.8(12) . . . . ? C1 C31 N16 Mn2 44.3(10) . . . . ? N18 Mn2 N16 C31 -103.1(7) . . . . ? N17 Mn2 N16 C31 152.1(8) . . . . ? Cl4 Mn2 N16 C31 -162.0(7) . . . . ? Cl3 Mn2 N16 C31 57.1(7) . . . . ? N15 Mn2 N16 C31 -26.2(7) . . . . ? N18 Mn2 N16 C32 137.9(8) . . . . ? N17 Mn2 N16 C32 33.1(7) . . . . ? Cl4 Mn2 N16 C32 78.9(11) . . . . ? Cl3 Mn2 N16 C32 -61.9(7) . . . . ? N15 Mn2 N16 C32 -145.2(8) . . . . ? N18 Mn2 N16 C42 18.6(7) . . . . ? N17 Mn2 N16 C42 -86.2(7) . . . . ? Cl4 Mn2 N16 C42 -40.3(12) . . . . ? Cl3 Mn2 N16 C42 178.8(7) . . . . ? N15 Mn2 N16 C42 95.5(7) . . . . ? C31 N16 C32 C34 -164.6(10) . . . . ? C42 N16 C32 C34 72.1(12) . . . . ? Mn2 N16 C32 C34 -44.4(10) . . . . ? N16 C32 C34 N17 30.1(14) . . . . ? N16 C32 C34 C35 -153.4(11) . . . . ? N17 C34 C35 C36 -1.9(19) . . . . ? C32 C34 C35 C36 -178.0(11) . . . . ? C34 C35 C36 C37 -0.3(19) . . . . ? C35 C36 C37 C38 1(2) . . . . ? C36 C37 C38 N17 0(2) . . . . ? C37 C38 N17 C34 -2(2) . . . . ? C37 C38 N17 Mn2 175.7(10) . . . . ? C35 C34 N17 C38 3.0(18) . . . . ? C32 C34 N17 C38 179.3(11) . . . . ? C35 C34 N17 Mn2 -174.9(10) . . . . ? C32 C34 N17 Mn2 1.4(13) . . . . ? N18 Mn2 N17 C38 90.0(11) . . . . ? N16 Mn2 N17 C38 162.7(11) . . . . ? Cl4 Mn2 N17 C38 -4.9(11) . . . . ? Cl3 Mn2 N17 C38 -108.8(10) . . . . ? N15 Mn2 N17 C38 165.4(9) . . . . ? N18 Mn2 N17 C34 -92.4(8) . . . . ? N16 Mn2 N17 C34 -19.7(8) . . . . ? Cl4 Mn2 N17 C34 172.7(8) . . . . ? Cl3 Mn2 N17 C34 68.8(8) . . . . ? N15 Mn2 N17 C34 -17.0(12) . . . . ? C31 N16 C42 C44 84.8(12) . . . . ? C32 N16 C42 C44 -153.1(10) . . . . ? Mn2 N16 C42 C44 -36.8(11) . . . . ? N16 C42 C44 N18 43.9(14) . . . . ? N16 C42 C44 C45 -142.6(11) . . . . ? N18 C44 C45 C46 -2.3(18) . . . . ? C42 C44 C45 C46 -175.7(11) . . . . ? C44 C45 C46 C47 1.2(19) . . . . ? C45 C46 C47 C48 1(2) . . . . ? C46 C47 C48 N18 -1(2) . . . . ? C47 C48 N18 C44 0.1(19) . . . . ? C47 C48 N18 Mn2 -156.7(10) . . . . ? C45 C44 N18 C48 1.6(17) . . . . ? C42 C44 N18 C48 175.4(11) . . . . ? C45 C44 N18 Mn2 161.2(9) . . . . ? C42 C44 N18 Mn2 -25.1(12) . . . . ? N17 Mn2 N18 C48 -130.0(9) . . . . ? N16 Mn2 N18 C48 161.0(10) . . . . ? Cl4 Mn2 N18 C48 -33.8(9) . . . . ? Cl3 Mn2 N18 C48 103.3(11) . . . . ? N15 Mn2 N18 C48 87.2(10) . . . . ? N17 Mn2 N18 C44 71.4(8) . . . . ? N16 Mn2 N18 C44 2.4(7) . . . . ? Cl4 Mn2 N18 C44 167.5(7) . . . . ? Cl3 Mn2 N18 C44 -55.3(12) . . . . ? N15 Mn2 N18 C44 -71.5(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O60 H60Y O50 0.84 2.39 3.19(4) 158.9 . O70 H70X Cl1 0.86 2.61 3.472(11) 178.0 1_465 O70 H70Y Cl3 0.86 2.45 3.311(12) 179.1 . _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.124 _refine_diff_density_min -1.114 _refine_diff_density_rms 0.179 _database_code_depnum_ccdc_archive 'CCDC 921843' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_wag343 #TrackingRef 'wag343.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78.40 H94.60 Cl8 N16 Ni4 O6.90' _chemical_formula_weight 1889.94 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.9160(15) _cell_length_b 12.3755(14) _cell_length_c 15.7457(19) _cell_angle_alpha 77.888(4) _cell_angle_beta 73.973(3) _cell_angle_gamma 83.045(3) _cell_volume 2177.1(5) _cell_formula_units_Z 1 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 4472 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 22.60 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 1.158 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7686 _exptl_absorpt_correction_T_max 0.8015 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28904 _diffrn_reflns_av_R_equivalents 0.0752 _diffrn_reflns_av_sigmaI/netI 0.1099 _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 -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.61 _reflns_number_total 8754 _reflns_number_gt 4940 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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. {[Ni4LMe2Cl4]Cl4.6.4MeOH.0.5H2O} half of this in the asymm. unit and the other half symmetry generated by center of inversion. Methanol molecules of solvation: two are full occup. (i.e O50,C50 and O60,C60), one is half occup. (o70, c70), and one is diordered over two sites in the same region of space 0.3:0.4 occup., for O80 c80 and o81 c81 respectively. All SAMEd to O50 C50. One 1/4 occup. water molecule, O90, is also present. All non H atoms ANIS. All H calc + ride, except for O90 where the H's were found from the map and AFIX 01'ed. H-bonding network is present involving the lattice chloride counter ions, the methanols and water of solvation. ; _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^)+(0.1049P)^2^+5.1242P] 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 8754 _refine_ls_number_parameters 563 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1397 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2324 _refine_ls_wR_factor_gt 0.1977 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.19094(7) 0.28942(7) 0.34819(6) 0.0287(3) Uani 1 1 d . . . Ni2 Ni 0.05892(7) 0.54968(8) 0.69914(6) 0.0310(3) Uani 1 1 d . . . C1 C 0.3136(5) 0.4369(6) 0.4100(5) 0.0298(16) Uani 1 1 d . . . C2 C 0.3365(5) 0.5145(6) 0.4508(4) 0.0289(15) Uani 1 1 d . . . H2 H 0.4049 0.5543 0.4254 0.035 Uiso 1 1 calc R . . C3 C 0.2597(5) 0.5349(5) 0.5294(4) 0.0267(15) Uani 1 1 d . . . N15 N 0.1642(4) 0.4780(4) 0.5685(4) 0.0270(12) Uani 1 1 d . . . C4 C 0.1514(5) 0.3960(6) 0.5283(4) 0.0282(15) Uani 1 1 d . . . C5 C 0.0614(5) 0.3151(6) 0.5775(4) 0.0283(15) Uani 1 1 d . . . C6 C 0.0978(6) 0.2051(6) 0.6017(5) 0.0344(16) Uani 1 1 d . . . H6 H 0.1785 0.1820 0.5846 0.041 Uiso 1 1 calc R . . C7 C 0.0182(6) 0.1289(6) 0.6503(5) 0.0373(17) Uani 1 1 d . . . H7 H 0.0437 0.0539 0.6679 0.045 Uiso 1 1 calc R . . C8 C -0.1009(6) 0.1630(6) 0.6735(5) 0.0373(17) Uani 1 1 d . . . H8 H -0.1569 0.1105 0.7053 0.045 Uiso 1 1 calc R . . C9 C -0.1361(6) 0.2704(6) 0.6508(5) 0.0352(17) Uani 1 1 d . . . H9 H -0.2170 0.2929 0.6681 0.042 Uiso 1 1 calc R . . C10 C -0.0569(5) 0.3486(6) 0.6028(5) 0.0315(16) Uani 1 1 d . . . H10 H -0.0829 0.4241 0.5874 0.038 Uiso 1 1 calc R . . N11 N 0.2197(4) 0.3763(5) 0.4474(4) 0.0279(13) Uani 1 1 d . . . C11 C 0.3907(5) 0.4136(6) 0.3217(5) 0.0308(16) Uani 1 1 d . . . H11A H 0.3738 0.4716 0.2722 0.037 Uiso 1 1 calc R . . H11B H 0.4737 0.4160 0.3209 0.037 Uiso 1 1 calc R . . N12 N 0.3718(4) 0.3046(4) 0.3070(3) 0.0269(12) Uani 1 1 d . . . C12 C 0.4112(6) 0.2955(7) 0.2096(5) 0.0383(18) Uani 1 1 d . . . H12A H 0.4940 0.2663 0.1954 0.046 Uiso 1 1 calc R . . H12B H 0.4065 0.3702 0.1723 0.046 Uiso 1 1 calc R . . N13 N 0.2251(5) 0.2182(5) 0.2339(4) 0.0334(14) Uani 1 1 d . . . C14 C 0.3378(6) 0.2203(6) 0.1856(5) 0.0380(18) Uani 1 1 d . . . C15 C 0.3803(7) 0.1643(7) 0.1164(5) 0.046(2) Uani 1 1 d . . . H15 H 0.4607 0.1661 0.0849 0.055 Uiso 1 1 calc R . . C16 C 0.3084(8) 0.1054(7) 0.0918(5) 0.050(2) Uani 1 1 d . . . H16 H 0.3373 0.0680 0.0424 0.060 Uiso 1 1 calc R . . C17 C 0.1916(7) 0.1016(7) 0.1411(6) 0.047(2) Uani 1 1 d . . . H17 H 0.1388 0.0611 0.1266 0.057 Uiso 1 1 calc R . . C18 C 0.1552(7) 0.1586(6) 0.2115(5) 0.0417(19) Uani 1 1 d . . . H18 H 0.0761 0.1551 0.2460 0.050 Uiso 1 1 calc R . . Cl1 Cl -0.01386(13) 0.27503(14) 0.39154(11) 0.0310(4) Uani 1 1 d . . . Cl2 Cl 0.14543(13) 0.47186(15) 0.26383(12) 0.0336(4) Uani 1 1 d . . . C22 C 0.4239(5) 0.2147(6) 0.3652(5) 0.0338(17) Uani 1 1 d . . . H22A H 0.4322 0.2435 0.4171 0.041 Uiso 1 1 calc R . . H22B H 0.5033 0.1925 0.3309 0.041 Uiso 1 1 calc R . . N14 N 0.2376(4) 0.1333(5) 0.4105(4) 0.0293(13) Uani 1 1 d . . . C24 C 0.3548(5) 0.1153(6) 0.3993(5) 0.0299(15) Uani 1 1 d . . . C25 C 0.4036(6) 0.0095(6) 0.4229(5) 0.0370(18) Uani 1 1 d . . . H25 H 0.4860 -0.0028 0.4137 0.044 Uiso 1 1 calc R . . C26 C 0.3325(6) -0.0787(7) 0.4598(5) 0.0422(19) Uani 1 1 d . . . H26 H 0.3652 -0.1513 0.4770 0.051 Uiso 1 1 calc R . . C27 C 0.2119(6) -0.0583(6) 0.4710(5) 0.0375(17) Uani 1 1 d . . . H27 H 0.1607 -0.1165 0.4965 0.045 Uiso 1 1 calc R . . C28 C 0.1683(5) 0.0492(6) 0.4441(5) 0.0313(16) Uani 1 1 d . . . H28 H 0.0866 0.0632 0.4500 0.038 Uiso 1 1 calc R . . C31 C 0.2831(5) 0.6183(6) 0.5783(4) 0.0314(16) Uani 1 1 d . . . H31A H 0.3686 0.6232 0.5662 0.038 Uiso 1 1 calc R . . H31B H 0.2485 0.6921 0.5563 0.038 Uiso 1 1 calc R . . N16 N 0.2324(5) 0.5857(5) 0.6753(4) 0.0305(13) Uani 1 1 d . . . C32 C 0.2292(6) 0.6813(6) 0.7217(5) 0.0356(17) Uani 1 1 d . . . H32A H 0.3070 0.6847 0.7318 0.043 Uiso 1 1 calc R . . H32B H 0.2114 0.7514 0.6827 0.043 Uiso 1 1 calc R . . N17 N 0.0462(5) 0.6165(5) 0.8135(4) 0.0350(14) Uani 1 1 d . . . C34 C 0.1396(6) 0.6693(6) 0.8092(5) 0.0380(18) Uani 1 1 d . . . C35 C 0.1500(7) 0.7144(7) 0.8799(5) 0.049(2) Uani 1 1 d . . . H35 H 0.2178 0.7511 0.8746 0.059 Uiso 1 1 calc R . . C36 C 0.0617(8) 0.7054(7) 0.9572(6) 0.055(2) Uani 1 1 d . . . H36 H 0.0665 0.7381 1.0054 0.066 Uiso 1 1 calc R . . C37 C -0.0356(7) 0.6481(7) 0.9650(5) 0.048(2) Uani 1 1 d . . . H37 H -0.0969 0.6390 1.0188 0.058 Uiso 1 1 calc R . . C38 C -0.0402(6) 0.6047(6) 0.8914(5) 0.0397(18) Uani 1 1 d . . . H38 H -0.1059 0.5655 0.8957 0.048 Uiso 1 1 calc R . . C42 C 0.2961(5) 0.4857(6) 0.7174(5) 0.0337(16) Uani 1 1 d . . . H42A H 0.3301 0.5077 0.7614 0.040 Uiso 1 1 calc R . . H42B H 0.3617 0.4606 0.6700 0.040 Uiso 1 1 calc R . . N18 N 0.1077(5) 0.3979(5) 0.7625(4) 0.0339(14) Uani 1 1 d . . . C44 C 0.2212(6) 0.3897(6) 0.7644(5) 0.0354(17) Uani 1 1 d . . . C45 C 0.2687(6) 0.2925(6) 0.8083(5) 0.0405(18) Uani 1 1 d . . . H45 H 0.3476 0.2876 0.8115 0.049 Uiso 1 1 calc R . . C46 C 0.2006(7) 0.2037(7) 0.8469(5) 0.046(2) Uani 1 1 d . . . H46 H 0.2319 0.1370 0.8768 0.056 Uiso 1 1 calc R . . C47 C 0.0848(7) 0.2135(6) 0.8413(5) 0.0404(18) Uani 1 1 d . . . H47 H 0.0361 0.1533 0.8663 0.049 Uiso 1 1 calc R . . C48 C 0.0433(7) 0.3121(6) 0.7989(5) 0.0401(18) Uani 1 1 d . . . H48 H -0.0356 0.3191 0.7955 0.048 Uiso 1 1 calc R . . Cl3 Cl 0.56215(14) 0.71526(15) 0.42423(12) 0.0370(4) Uani 1 1 d . . . Cl4 Cl 0.2644(3) 0.9213(2) -0.0406(2) 0.0914(10) Uani 1 1 d . . . O50 O 0.3493(5) 0.9060(5) -0.2418(5) 0.0694(19) Uani 1 1 d D . . H50 H 0.3494 0.9242 -0.1933 0.083 Uiso 1 1 calc R . . C50 C 0.2707(8) 0.9795(8) -0.2829(7) 0.068(3) Uani 1 1 d D . . H50A H 0.1907 0.9713 -0.2448 0.081 Uiso 1 1 calc R . . H50B H 0.2756 0.9622 -0.3418 0.081 Uiso 1 1 calc R . . H50C H 0.2913 1.0559 -0.2905 0.081 Uiso 1 1 calc R . . O60 O 0.4352(5) 0.7620(8) 0.2716(5) 0.088(3) Uani 1 1 d D . . H60 H 0.4644 0.7557 0.3154 0.105 Uiso 1 1 calc R . . C60 C 0.4452(10) 0.8709(11) 0.2218(7) 0.108(5) Uani 1 1 d D . . H60A H 0.3804 0.9193 0.2498 0.130 Uiso 1 1 calc R . . H60B H 0.4423 0.8714 0.1601 0.130 Uiso 1 1 calc R . . H60C H 0.5197 0.8976 0.2208 0.130 Uiso 1 1 calc R . . O70 O 0.4008(7) 0.5188(8) -0.1122(5) 0.026(2) Uani 0.50 1 d PD . . H70 H 0.3834 0.5831 -0.1010 0.031 Uiso 0.50 1 calc PR . . C70 C 0.3616(13) 0.4461(13) -0.0393(10) 0.053(5) Uani 0.50 1 d PD . . H70A H 0.3950 0.3719 -0.0488 0.063 Uiso 0.50 1 calc PR . . H70B H 0.2761 0.4478 -0.0255 0.063 Uiso 0.50 1 calc PR . . H70C H 0.3844 0.4642 0.0111 0.063 Uiso 0.50 1 calc PR . . O80 O 0.4150(12) 0.6463(12) 0.1727(11) 0.034(4) Uani 0.30 1 d PD A 1 H80 H 0.4354 0.6933 0.1961 0.041 Uiso 0.30 1 calc PR A 1 C80 C 0.344(3) 0.699(2) 0.1172(16) 0.043(7) Uani 0.30 1 d PD A 1 H80A H 0.3893 0.7065 0.0542 0.052 Uiso 0.30 1 calc PR A 1 H80B H 0.3160 0.7725 0.1312 0.052 Uiso 0.30 1 calc PR A 1 H80C H 0.2772 0.6548 0.1269 0.052 Uiso 0.30 1 calc PR A 1 O81 O 0.3633(9) 0.6889(10) -0.0046(7) 0.030(3) Uani 0.40 1 d PD B 2 H81 H 0.3468 0.7575 -0.0161 0.036 Uiso 0.40 1 calc PR B 2 C81 C 0.319(3) 0.650(2) 0.0858(12) 0.078(9) Uani 0.40 1 d PD B 2 H81A H 0.3370 0.6994 0.1206 0.093 Uiso 0.40 1 calc PR B 2 H81B H 0.3545 0.5753 0.1021 0.093 Uiso 0.40 1 calc PR B 2 H81C H 0.2340 0.6468 0.0991 0.093 Uiso 0.40 1 calc PR B 2 O90 O 0.0146(18) 1.0241(18) 0.0493(13) 0.049(6) Uani 0.25 1 d P . . H90X H 0.0837 0.9958 0.0250 0.059 Uiso 0.25 1 d P . . H90Y H 0.0422 1.0814 0.0092 0.059 Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0163(4) 0.0347(5) 0.0379(5) -0.0084(4) -0.0112(4) 0.0007(3) Ni2 0.0183(4) 0.0372(6) 0.0391(5) -0.0069(4) -0.0113(4) 0.0004(4) C1 0.012(3) 0.037(4) 0.044(4) -0.012(3) -0.013(3) 0.004(3) C2 0.012(3) 0.034(4) 0.037(4) 0.000(3) -0.007(3) 0.003(3) C3 0.017(3) 0.026(4) 0.037(4) 0.000(3) -0.013(3) 0.002(3) N15 0.017(3) 0.029(3) 0.038(3) -0.005(3) -0.012(2) -0.001(2) C4 0.010(3) 0.041(4) 0.034(4) -0.006(3) -0.010(3) 0.008(3) C5 0.013(3) 0.033(4) 0.039(4) -0.006(3) -0.007(3) -0.003(3) C6 0.023(4) 0.040(4) 0.040(4) -0.005(4) -0.007(3) -0.005(3) C7 0.036(4) 0.032(4) 0.043(4) -0.005(4) -0.009(3) -0.003(3) C8 0.025(4) 0.046(5) 0.042(4) -0.003(4) -0.007(3) -0.018(3) C9 0.014(3) 0.048(5) 0.044(4) -0.003(4) -0.011(3) -0.005(3) C10 0.023(3) 0.033(4) 0.042(4) -0.006(3) -0.017(3) 0.001(3) N11 0.019(3) 0.033(3) 0.031(3) -0.006(3) -0.009(2) 0.008(2) C11 0.017(3) 0.033(4) 0.043(4) -0.008(3) -0.009(3) 0.001(3) N12 0.027(3) 0.030(3) 0.025(3) -0.008(3) -0.008(2) 0.000(2) C12 0.029(4) 0.049(5) 0.034(4) -0.008(4) -0.005(3) -0.003(3) N13 0.029(3) 0.031(3) 0.046(4) -0.009(3) -0.019(3) 0.003(3) C14 0.030(4) 0.041(5) 0.043(4) -0.001(4) -0.016(3) 0.000(3) C15 0.048(5) 0.048(5) 0.050(5) -0.021(4) -0.015(4) -0.003(4) C16 0.066(6) 0.046(5) 0.041(5) -0.011(4) -0.016(4) -0.002(4) C17 0.050(5) 0.046(5) 0.060(5) -0.016(4) -0.034(4) 0.002(4) C18 0.034(4) 0.045(5) 0.055(5) -0.010(4) -0.026(4) 0.003(3) Cl1 0.0177(8) 0.0359(10) 0.0408(10) -0.0050(8) -0.0111(7) -0.0023(7) Cl2 0.0204(8) 0.0391(10) 0.0411(10) -0.0046(8) -0.0102(7) -0.0010(7) C22 0.015(3) 0.049(5) 0.040(4) -0.013(4) -0.009(3) 0.003(3) N14 0.017(3) 0.037(3) 0.039(3) -0.011(3) -0.013(2) 0.003(2) C24 0.020(3) 0.036(4) 0.036(4) -0.009(3) -0.011(3) 0.003(3) C25 0.018(3) 0.048(5) 0.048(4) -0.013(4) -0.013(3) 0.003(3) C26 0.026(4) 0.051(5) 0.052(5) -0.013(4) -0.018(3) 0.008(3) C27 0.021(4) 0.042(5) 0.046(4) -0.006(4) -0.004(3) -0.003(3) C28 0.017(3) 0.040(4) 0.039(4) -0.004(3) -0.013(3) -0.003(3) C31 0.020(3) 0.039(4) 0.035(4) -0.005(3) -0.008(3) -0.003(3) N16 0.028(3) 0.029(3) 0.040(3) -0.006(3) -0.018(3) -0.003(2) C32 0.028(4) 0.044(5) 0.042(4) -0.019(4) -0.015(3) 0.000(3) N17 0.030(3) 0.039(4) 0.039(3) -0.012(3) -0.014(3) 0.008(3) C34 0.034(4) 0.038(4) 0.048(5) -0.013(4) -0.018(3) 0.002(3) C35 0.050(5) 0.058(6) 0.043(5) -0.021(4) -0.013(4) -0.002(4) C36 0.061(6) 0.056(6) 0.049(5) -0.016(5) -0.014(4) 0.004(5) C37 0.042(5) 0.065(6) 0.036(4) -0.020(4) 0.000(3) 0.002(4) C38 0.031(4) 0.038(5) 0.044(4) -0.002(4) -0.007(3) 0.006(3) C42 0.018(3) 0.046(5) 0.038(4) -0.008(4) -0.010(3) 0.004(3) N18 0.030(3) 0.041(4) 0.034(3) -0.012(3) -0.011(3) 0.003(3) C44 0.033(4) 0.045(5) 0.031(4) -0.015(4) -0.009(3) 0.004(3) C45 0.032(4) 0.041(5) 0.043(4) -0.002(4) -0.009(3) 0.008(3) C46 0.043(5) 0.046(5) 0.047(5) -0.010(4) -0.014(4) 0.016(4) C47 0.049(5) 0.037(5) 0.036(4) -0.004(4) -0.011(4) -0.006(4) C48 0.040(4) 0.043(5) 0.038(4) -0.012(4) -0.011(3) 0.001(4) Cl3 0.0220(8) 0.0450(11) 0.0463(10) -0.0108(9) -0.0140(7) 0.0060(7) Cl4 0.147(3) 0.0504(15) 0.113(2) -0.0223(16) -0.094(2) 0.0093(16) O50 0.031(3) 0.060(4) 0.105(6) -0.017(4) -0.003(3) 0.012(3) C50 0.063(6) 0.069(7) 0.076(7) -0.031(6) -0.024(5) 0.020(5) O60 0.034(4) 0.168(8) 0.056(4) 0.013(5) -0.022(3) -0.024(4) C60 0.067(7) 0.162(14) 0.064(7) 0.011(8) -0.012(6) 0.047(8) O70 0.029(5) 0.041(6) 0.010(4) 0.006(4) -0.011(3) -0.018(4) C70 0.046(10) 0.050(10) 0.080(12) 0.007(10) -0.051(9) -0.025(8) O80 0.020(8) 0.034(10) 0.051(10) -0.003(8) -0.021(7) 0.002(7) C80 0.09(2) 0.026(16) 0.012(12) 0.005(11) -0.018(12) 0.006(14) O81 0.020(6) 0.031(7) 0.030(6) 0.006(5) -0.002(5) 0.006(5) C81 0.10(2) 0.045(16) 0.061(18) 0.000(14) 0.010(15) 0.032(15) O90 0.052(13) 0.056(15) 0.043(12) 0.012(11) -0.019(10) -0.044(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N14 2.061(6) . y Ni1 N13 2.086(6) . y Ni1 N12 2.092(5) . y Ni1 N11 2.192(5) . y Ni1 Cl1 2.3638(17) . y Ni1 Cl2 2.449(2) . y Ni2 N18 2.032(6) . y Ni2 N16 2.082(5) . y Ni2 N17 2.096(6) . y Ni2 Cl2 2.3766(17) 2_566 y Ni2 N15 2.380(5) . y Ni2 Cl1 2.4238(19) 2_566 y C1 N11 1.347(8) . ? C1 C2 1.353(9) . ? C1 C11 1.504(9) . ? C2 C3 1.372(9) . ? C2 H2 0.9500 . ? C3 N15 1.340(8) . ? C3 C31 1.502(9) . ? N15 C4 1.347(8) . ? C4 N11 1.361(8) . ? C4 C5 1.494(9) . ? C5 C6 1.385(10) . ? C5 C10 1.391(8) . ? C6 C7 1.373(10) . ? C6 H6 0.9500 . ? C7 C8 1.399(10) . ? C7 H7 0.9500 . ? C8 C9 1.349(10) . ? C8 H8 0.9500 . ? C9 C10 1.386(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 N12 1.468(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N12 C22 1.477(8) . ? N12 C12 1.500(8) . ? C12 C14 1.517(10) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N13 C18 1.335(9) . ? N13 C14 1.349(9) . ? C14 C15 1.360(10) . ? C15 C16 1.367(11) . ? C15 H15 0.9500 . ? C16 C17 1.395(11) . ? C16 H16 0.9500 . ? C17 C18 1.379(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? Cl1 Ni2 2.4238(19) 2_566 ? Cl2 Ni2 2.3766(17) 2_566 ? C22 C24 1.484(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? N14 C28 1.334(9) . ? N14 C24 1.356(8) . ? C24 C25 1.385(10) . ? C25 C26 1.390(11) . ? C25 H25 0.9500 . ? C26 C27 1.397(9) . ? C26 H26 0.9500 . ? C27 C28 1.392(10) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C31 N16 1.466(9) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? N16 C42 1.501(9) . ? N16 C32 1.508(8) . ? C32 C34 1.483(10) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? N17 C34 1.336(9) . ? N17 C38 1.360(9) . ? C34 C35 1.385(10) . ? C35 C36 1.366(11) . ? C35 H35 0.9500 . ? C36 C37 1.395(12) . ? C36 H36 0.9500 . ? C37 C38 1.392(10) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C42 C44 1.510(10) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? N18 C48 1.321(9) . ? N18 C44 1.351(9) . ? C44 C45 1.396(10) . ? C45 C46 1.378(11) . ? C45 H45 0.9500 . ? C46 C47 1.395(10) . ? C46 H46 0.9500 . ? C47 C48 1.369(10) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? O50 C50 1.416(9) . ? O50 H50 0.8400 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? O60 C60 1.410(11) . ? O60 H60 0.8400 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? O70 C70 1.312(13) . ? O70 H70 0.8400 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? O80 C80 1.392(16) . ? O80 H80 0.8400 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? O81 C81 1.378(15) . ? O81 H81 0.8400 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? O90 H90X 0.8712 . ? O90 H90Y 0.8732 . ? 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 N14 Ni1 N13 84.8(2) . . y N14 Ni1 N12 83.4(2) . . y N13 Ni1 N12 82.6(2) . . y N14 Ni1 N11 95.6(2) . . y N13 Ni1 N11 159.8(2) . . y N12 Ni1 N11 77.41(19) . . y N14 Ni1 Cl1 97.71(15) . . y N13 Ni1 Cl1 96.80(16) . . y N12 Ni1 Cl1 178.66(16) . . y N11 Ni1 Cl1 103.14(14) . . y N14 Ni1 Cl2 175.76(16) . . y N13 Ni1 Cl2 91.54(17) . . y N12 Ni1 Cl2 94.02(16) . . y N11 Ni1 Cl2 87.11(15) . . y Cl1 Ni1 Cl2 84.80(6) . . y N18 Ni2 N16 85.9(2) . . y N18 Ni2 N17 90.6(2) . . y N16 Ni2 N17 80.5(2) . . y N18 Ni2 Cl2 97.87(17) . 2_566 y N16 Ni2 Cl2 172.66(16) . 2_566 y N17 Ni2 Cl2 93.15(16) . 2_566 y N18 Ni2 N15 82.4(2) . . y N16 Ni2 N15 73.68(19) . . y N17 Ni2 N15 153.6(2) . . y Cl2 Ni2 N15 112.96(13) 2_566 . y N18 Ni2 Cl1 173.75(17) . 2_566 y N16 Ni2 Cl1 91.77(16) . 2_566 y N17 Ni2 Cl1 94.79(17) . 2_566 y Cl2 Ni2 Cl1 85.09(6) 2_566 2_566 y N15 Ni2 Cl1 91.33(14) . 2_566 y N11 C1 C2 121.0(6) . . ? N11 C1 C11 116.8(6) . . ? C2 C1 C11 122.2(6) . . ? C1 C2 C3 119.1(6) . . ? C1 C2 H2 120.4 . . ? C3 C2 H2 120.4 . . ? N15 C3 C2 122.0(6) . . ? N15 C3 C31 116.9(6) . . ? C2 C3 C31 121.0(6) . . ? C3 N15 C4 115.8(6) . . ? C3 N15 Ni2 108.4(4) . . ? C4 N15 Ni2 135.8(4) . . ? N15 C4 N11 124.9(6) . . ? N15 C4 C5 118.6(6) . . ? N11 C4 C5 116.3(6) . . ? C6 C5 C10 119.6(6) . . ? C6 C5 C4 118.8(5) . . ? C10 C5 C4 121.5(6) . . ? C7 C6 C5 120.6(6) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 119.4(7) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C9 C8 C7 120.0(6) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 121.4(6) . . ? C8 C9 H9 119.3 . . ? C10 C9 H9 119.3 . . ? C9 C10 C5 119.0(6) . . ? C9 C10 H10 120.5 . . ? C5 C10 H10 120.5 . . ? C1 N11 C4 116.6(6) . . ? C1 N11 Ni1 109.5(4) . . ? C4 N11 Ni1 132.5(4) . . ? N12 C11 C1 111.1(6) . . ? N12 C11 H11A 109.4 . . ? C1 C11 H11A 109.4 . . ? N12 C11 H11B 109.4 . . ? C1 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C11 N12 C22 111.0(5) . . ? C11 N12 C12 112.2(6) . . ? C22 N12 C12 113.1(5) . . ? C11 N12 Ni1 106.5(4) . . ? C22 N12 Ni1 106.5(4) . . ? C12 N12 Ni1 107.1(4) . . ? N12 C12 C14 112.3(6) . . ? N12 C12 H12A 109.1 . . ? C14 C12 H12A 109.1 . . ? N12 C12 H12B 109.1 . . ? C14 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? C18 N13 C14 117.5(6) . . ? C18 N13 Ni1 128.0(5) . . ? C14 N13 Ni1 113.7(4) . . ? N13 C14 C15 122.1(7) . . ? N13 C14 C12 115.3(6) . . ? C15 C14 C12 122.5(7) . . ? C14 C15 C16 120.6(8) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C17 118.3(7) . . ? C15 C16 H16 120.9 . . ? C17 C16 H16 120.9 . . ? C18 C17 C16 117.9(7) . . ? C18 C17 H17 121.1 . . ? C16 C17 H17 121.1 . . ? N13 C18 C17 123.6(7) . . ? N13 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? Ni1 Cl1 Ni2 95.46(7) . 2_566 ? Ni2 Cl2 Ni1 94.46(7) 2_566 . ? N12 C22 C24 114.0(5) . . ? N12 C22 H22A 108.7 . . ? C24 C22 H22A 108.7 . . ? N12 C22 H22B 108.7 . . ? C24 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C28 N14 C24 120.2(6) . . ? C28 N14 Ni1 126.2(4) . . ? C24 N14 Ni1 112.5(4) . . ? N14 C24 C25 120.3(6) . . ? N14 C24 C22 116.2(6) . . ? C25 C24 C22 123.5(6) . . ? C24 C25 C26 120.3(6) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 118.5(7) . . ? C25 C26 H26 120.8 . . ? C27 C26 H26 120.8 . . ? C28 C27 C26 118.6(7) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? N14 C28 C27 122.1(6) . . ? N14 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? N16 C31 C3 110.1(6) . . ? N16 C31 H31A 109.6 . . ? C3 C31 H31A 109.6 . . ? N16 C31 H31B 109.6 . . ? C3 C31 H31B 109.6 . . ? H31A C31 H31B 108.2 . . ? C31 N16 C42 113.1(5) . . ? C31 N16 C32 110.0(6) . . ? C42 N16 C32 109.9(5) . . ? C31 N16 Ni2 109.7(4) . . ? C42 N16 Ni2 107.9(4) . . ? C32 N16 Ni2 106.0(4) . . ? C34 C32 N16 111.2(6) . . ? C34 C32 H32A 109.4 . . ? N16 C32 H32A 109.4 . . ? C34 C32 H32B 109.4 . . ? N16 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 N17 C38 118.2(6) . . ? C34 N17 Ni2 114.0(5) . . ? C38 N17 Ni2 127.6(5) . . ? N17 C34 C35 122.5(7) . . ? N17 C34 C32 115.4(6) . . ? C35 C34 C32 122.0(7) . . ? C36 C35 C34 119.3(8) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C35 C36 C37 119.7(8) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C38 C37 C36 117.9(7) . . ? C38 C37 H37 121.0 . . ? C36 C37 H37 121.0 . . ? N17 C38 C37 122.3(7) . . ? N17 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? N16 C42 C44 114.5(5) . . ? N16 C42 H42A 108.6 . . ? C44 C42 H42A 108.6 . . ? N16 C42 H42B 108.6 . . ? C44 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C48 N18 C44 119.8(6) . . ? C48 N18 Ni2 128.0(5) . . ? C44 N18 Ni2 112.2(5) . . ? N18 C44 C45 120.1(7) . . ? N18 C44 C42 119.4(6) . . ? C45 C44 C42 120.5(6) . . ? C46 C45 C44 119.7(7) . . ? C46 C45 H45 120.1 . . ? C44 C45 H45 120.1 . . ? C45 C46 C47 118.9(7) . . ? C45 C46 H46 120.6 . . ? C47 C46 H46 120.6 . . ? C48 C47 C46 118.2(7) . . ? C48 C47 H47 120.9 . . ? C46 C47 H47 120.9 . . ? N18 C48 C47 123.3(7) . . ? N18 C48 H48 118.4 . . ? C47 C48 H48 118.4 . . ? C50 O50 H50 109.5 . . ? O50 C50 H50A 109.5 . . ? O50 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? O50 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C60 O60 H60 109.5 . . ? O60 C60 H60A 109.5 . . ? O60 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? O60 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C70 O70 H70 109.5 . . ? O70 C70 H70A 109.5 . . ? O70 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? O70 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C81 O81 H81 109.5 . . ? O81 C81 H81A 109.5 . . ? O81 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? O81 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? H90X O90 H90Y 80.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 C1 C2 C3 -3.0(10) . . . . ? C11 C1 C2 C3 177.2(6) . . . . ? C1 C2 C3 N15 2.0(10) . . . . ? C1 C2 C3 C31 178.4(6) . . . . ? C2 C3 N15 C4 3.1(9) . . . . ? C31 C3 N15 C4 -173.5(5) . . . . ? C2 C3 N15 Ni2 -178.2(5) . . . . ? C31 C3 N15 Ni2 5.3(7) . . . . ? N18 Ni2 N15 C3 -112.8(4) . . . . ? N16 Ni2 N15 C3 -24.9(4) . . . . ? N17 Ni2 N15 C3 -37.0(7) . . . . ? Cl2 Ni2 N15 C3 151.8(4) 2_566 . . . ? Cl1 Ni2 N15 C3 66.6(4) 2_566 . . . ? N18 Ni2 N15 C4 65.5(6) . . . . ? N16 Ni2 N15 C4 153.5(6) . . . . ? N17 Ni2 N15 C4 141.4(6) . . . . ? Cl2 Ni2 N15 C4 -29.8(6) 2_566 . . . ? Cl1 Ni2 N15 C4 -115.1(6) 2_566 . . . ? C3 N15 C4 N11 -7.8(9) . . . . ? Ni2 N15 C4 N11 173.9(4) . . . . ? C3 N15 C4 C5 167.9(5) . . . . ? Ni2 N15 C4 C5 -10.4(9) . . . . ? N15 C4 C5 C6 -115.7(7) . . . . ? N11 C4 C5 C6 60.4(8) . . . . ? N15 C4 C5 C10 61.3(8) . . . . ? N11 C4 C5 C10 -122.6(7) . . . . ? C10 C5 C6 C7 0.2(10) . . . . ? C4 C5 C6 C7 177.2(6) . . . . ? C5 C6 C7 C8 1.4(11) . . . . ? C6 C7 C8 C9 -2.2(11) . . . . ? C7 C8 C9 C10 1.4(11) . . . . ? C8 C9 C10 C5 0.2(10) . . . . ? C6 C5 C10 C9 -1.0(10) . . . . ? C4 C5 C10 C9 -178.0(6) . . . . ? C2 C1 N11 C4 -1.2(9) . . . . ? C11 C1 N11 C4 178.7(5) . . . . ? C2 C1 N11 Ni1 167.0(5) . . . . ? C11 C1 N11 Ni1 -13.1(7) . . . . ? N15 C4 N11 C1 7.0(9) . . . . ? C5 C4 N11 C1 -168.8(5) . . . . ? N15 C4 N11 Ni1 -157.9(5) . . . . ? C5 C4 N11 Ni1 26.3(8) . . . . ? N14 Ni1 N11 C1 110.6(4) . . . . ? N13 Ni1 N11 C1 20.5(8) . . . . ? N12 Ni1 N11 C1 28.7(4) . . . . ? Cl1 Ni1 N11 C1 -150.1(4) . . . . ? Cl2 Ni1 N11 C1 -66.1(4) . . . . ? N14 Ni1 N11 C4 -83.7(6) . . . . ? N13 Ni1 N11 C4 -173.8(6) . . . . ? N12 Ni1 N11 C4 -165.6(6) . . . . ? Cl1 Ni1 N11 C4 15.6(6) . . . . ? Cl2 Ni1 N11 C4 99.6(6) . . . . ? N11 C1 C11 N12 -19.1(8) . . . . ? C2 C1 C11 N12 160.8(6) . . . . ? C1 C11 N12 C22 -73.4(6) . . . . ? C1 C11 N12 C12 159.0(5) . . . . ? C1 C11 N12 Ni1 42.1(6) . . . . ? N14 Ni1 N12 C11 -134.8(4) . . . . ? N13 Ni1 N12 C11 139.6(4) . . . . ? N11 Ni1 N12 C11 -37.6(4) . . . . ? Cl2 Ni1 N12 C11 48.6(4) . . . . ? N14 Ni1 N12 C22 -16.3(4) . . . . ? N13 Ni1 N12 C22 -101.9(4) . . . . ? N11 Ni1 N12 C22 81.0(4) . . . . ? Cl2 Ni1 N12 C22 167.1(4) . . . . ? N14 Ni1 N12 C12 104.9(4) . . . . ? N13 Ni1 N12 C12 19.4(4) . . . . ? N11 Ni1 N12 C12 -157.8(5) . . . . ? Cl2 Ni1 N12 C12 -71.7(4) . . . . ? C11 N12 C12 C14 -148.1(6) . . . . ? C22 N12 C12 C14 85.4(7) . . . . ? Ni1 N12 C12 C14 -31.6(7) . . . . ? N14 Ni1 N13 C18 81.5(6) . . . . ? N12 Ni1 N13 C18 165.5(6) . . . . ? N11 Ni1 N13 C18 173.6(6) . . . . ? Cl1 Ni1 N13 C18 -15.7(6) . . . . ? Cl2 Ni1 N13 C18 -100.6(6) . . . . ? N14 Ni1 N13 C14 -87.8(5) . . . . ? N12 Ni1 N13 C14 -3.8(5) . . . . ? N11 Ni1 N13 C14 4.3(9) . . . . ? Cl1 Ni1 N13 C14 175.0(5) . . . . ? Cl2 Ni1 N13 C14 90.1(5) . . . . ? C18 N13 C14 C15 0.0(11) . . . . ? Ni1 N13 C14 C15 170.5(6) . . . . ? C18 N13 C14 C12 176.0(6) . . . . ? Ni1 N13 C14 C12 -13.5(8) . . . . ? N12 C12 C14 N13 31.1(9) . . . . ? N12 C12 C14 C15 -152.9(7) . . . . ? N13 C14 C15 C16 1.7(12) . . . . ? C12 C14 C15 C16 -174.0(8) . . . . ? C14 C15 C16 C17 -1.9(13) . . . . ? C15 C16 C17 C18 0.5(12) . . . . ? C14 N13 C18 C17 -1.4(11) . . . . ? Ni1 N13 C18 C17 -170.3(6) . . . . ? C16 C17 C18 N13 1.2(12) . . . . ? N14 Ni1 Cl1 Ni2 -173.20(15) . . . 2_566 ? N13 Ni1 Cl1 Ni2 -87.57(17) . . . 2_566 ? N11 Ni1 Cl1 Ni2 89.16(16) . . . 2_566 ? Cl2 Ni1 Cl1 Ni2 3.36(6) . . . 2_566 ? N13 Ni1 Cl2 Ni2 93.27(16) . . . 2_566 ? N12 Ni1 Cl2 Ni2 175.94(14) . . . 2_566 ? N11 Ni1 Cl2 Ni2 -106.91(14) . . . 2_566 ? Cl1 Ni1 Cl2 Ni2 -3.42(6) . . . 2_566 ? C11 N12 C22 C24 143.7(6) . . . . ? C12 N12 C22 C24 -89.2(7) . . . . ? Ni1 N12 C22 C24 28.2(6) . . . . ? N13 Ni1 N14 C28 -82.9(5) . . . . ? N12 Ni1 N14 C28 -166.0(6) . . . . ? N11 Ni1 N14 C28 117.4(5) . . . . ? Cl1 Ni1 N14 C28 13.3(5) . . . . ? N13 Ni1 N14 C24 85.0(4) . . . . ? N12 Ni1 N14 C24 1.9(4) . . . . ? N11 Ni1 N14 C24 -74.7(4) . . . . ? Cl1 Ni1 N14 C24 -178.8(4) . . . . ? C28 N14 C24 C25 0.0(9) . . . . ? Ni1 N14 C24 C25 -168.7(5) . . . . ? C28 N14 C24 C22 -177.4(6) . . . . ? Ni1 N14 C24 C22 13.9(7) . . . . ? N12 C22 C24 N14 -29.4(8) . . . . ? N12 C22 C24 C25 153.3(6) . . . . ? N14 C24 C25 C26 -1.3(10) . . . . ? C22 C24 C25 C26 175.9(7) . . . . ? C24 C25 C26 C27 1.0(11) . . . . ? C25 C26 C27 C28 0.5(10) . . . . ? C24 N14 C28 C27 1.6(10) . . . . ? Ni1 N14 C28 C27 168.7(5) . . . . ? C26 C27 C28 N14 -1.9(10) . . . . ? N15 C3 C31 N16 27.1(8) . . . . ? C2 C3 C31 N16 -149.5(6) . . . . ? C3 C31 N16 C42 70.6(6) . . . . ? C3 C31 N16 C32 -166.1(5) . . . . ? C3 C31 N16 Ni2 -49.9(6) . . . . ? N18 Ni2 N16 C31 122.5(4) . . . . ? N17 Ni2 N16 C31 -146.3(5) . . . . ? N15 Ni2 N16 C31 39.2(4) . . . . ? Cl1 Ni2 N16 C31 -51.7(4) 2_566 . . . ? N18 Ni2 N16 C42 -1.1(4) . . . . ? N17 Ni2 N16 C42 90.1(4) . . . . ? N15 Ni2 N16 C42 -84.4(4) . . . . ? Cl1 Ni2 N16 C42 -175.3(4) 2_566 . . . ? N18 Ni2 N16 C32 -118.8(4) . . . . ? N17 Ni2 N16 C32 -27.5(4) . . . . ? N15 Ni2 N16 C32 157.9(5) . . . . ? Cl1 Ni2 N16 C32 67.0(4) 2_566 . . . ? C31 N16 C32 C34 157.3(6) . . . . ? C42 N16 C32 C34 -77.5(7) . . . . ? Ni2 N16 C32 C34 38.8(6) . . . . ? N18 Ni2 N17 C34 98.9(5) . . . . ? N16 Ni2 N17 C34 13.1(5) . . . . ? Cl2 Ni2 N17 C34 -163.2(5) 2_566 . . . ? N15 Ni2 N17 C34 24.9(8) . . . . ? Cl1 Ni2 N17 C34 -77.9(5) 2_566 . . . ? N18 Ni2 N17 C38 -75.7(6) . . . . ? N16 Ni2 N17 C38 -161.5(6) . . . . ? Cl2 Ni2 N17 C38 22.2(6) 2_566 . . . ? N15 Ni2 N17 C38 -149.7(5) . . . . ? Cl1 Ni2 N17 C38 107.5(6) 2_566 . . . ? C38 N17 C34 C35 -1.7(11) . . . . ? Ni2 N17 C34 C35 -176.9(6) . . . . ? C38 N17 C34 C32 -178.8(6) . . . . ? Ni2 N17 C34 C32 6.1(8) . . . . ? N16 C32 C34 N17 -30.8(9) . . . . ? N16 C32 C34 C35 152.2(7) . . . . ? N17 C34 C35 C36 -0.2(12) . . . . ? C32 C34 C35 C36 176.6(8) . . . . ? C34 C35 C36 C37 2.1(13) . . . . ? C35 C36 C37 C38 -1.9(13) . . . . ? C34 N17 C38 C37 1.8(11) . . . . ? Ni2 N17 C38 C37 176.2(5) . . . . ? C36 C37 C38 N17 0.0(12) . . . . ? C31 N16 C42 C44 -121.8(6) . . . . ? C32 N16 C42 C44 114.8(6) . . . . ? Ni2 N16 C42 C44 -0.3(7) . . . . ? N16 Ni2 N18 C48 -176.9(6) . . . . ? N17 Ni2 N18 C48 102.7(6) . . . . ? Cl2 Ni2 N18 C48 9.4(6) 2_566 . . . ? N15 Ni2 N18 C48 -102.9(6) . . . . ? N16 Ni2 N18 C44 2.5(4) . . . . ? N17 Ni2 N18 C44 -77.9(5) . . . . ? Cl2 Ni2 N18 C44 -171.2(4) 2_566 . . . ? N15 Ni2 N18 C44 76.6(4) . . . . ? C48 N18 C44 C45 -2.9(10) . . . . ? Ni2 N18 C44 C45 177.6(5) . . . . ? C48 N18 C44 C42 176.1(6) . . . . ? Ni2 N18 C44 C42 -3.4(7) . . . . ? N16 C42 C44 N18 2.5(9) . . . . ? N16 C42 C44 C45 -178.5(6) . . . . ? N18 C44 C45 C46 2.2(11) . . . . ? C42 C44 C45 C46 -176.7(6) . . . . ? C44 C45 C46 C47 -0.2(11) . . . . ? C45 C46 C47 C48 -1.2(11) . . . . ? C44 N18 C48 C47 1.6(10) . . . . ? Ni2 N18 C48 C47 -179.1(5) . . . . ? C46 C47 C48 N18 0.5(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O50 H50 Cl4 0.84 2.33 3.088(8) 149.8 . O60 H60 Cl3 0.84 2.27 3.100(6) 170.5 . O80 H80 O60 0.84 1.60 2.400(17) 158.0 . O70 H70 O81 0.84 2.15 2.890(15) 146.5 . O81 H81 Cl4 0.84 2.15 2.974(11) 166.7 . O90 H90X Cl4 0.87 2.29 3.16(2) 179.2 . _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 26.61 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.060 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.128 _database_code_depnum_ccdc_archive 'CCDC 921844' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_wag345 #TrackingRef 'wag345.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H79 Cl8 Cu4 N16 O4.50' _chemical_formula_weight 1790.28 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 12.727(4) _cell_length_b 13.733(2) _cell_length_c 13.977(2) _cell_angle_alpha 118.696(8) _cell_angle_beta 99.214(12) _cell_angle_gamma 98.490(12) _cell_volume 2042.8(8) _cell_formula_units_Z 1 _cell_measurement_temperature 92(2) _cell_measurement_reflns_used 7037 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 26.40 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 917 _exptl_absorpt_coefficient_mu 1.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6151 _exptl_absorpt_correction_T_max 0.8772 _exptl_absorpt_process_details 'SCALE (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 92(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa Apex II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42552 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 26.40 _reflns_number_total 8310 _reflns_number_gt 7025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2006)' _computing_cell_refinement 'APEX2 & SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2006)' _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. [Cu(II)4 (LMe)2 (mu-Cl)2 (Cl)4]Cl2 .(3.5H2O) .(MeOH) Half of this in asym unit; other half generated by -1. All non-H ANIS. All H calc and ride except those on O of water which were found, HIMP'ed, then AFIX 01'ed whilst U(H)=1.2U(O). Lattice chloride ion was disordered (0.50:0.25:0.25 for Cl22, Cl21, Cl20). H2O and MeOH are all partial occupancy and disordered. This region of solvent was modelled as well as possible, in preference to resorting to SQUEEZE, however the residual peaks occur in this region. H-bonds are present between solvents, between solvents and lattice Cl- and between solvents and terminal Cl-. ; _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^)+(0.0824P)^2^+6.9150P] 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 8310 _refine_ls_number_parameters 524 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.095 _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 Cu1 Cu 0.94312(4) 0.86819(4) 0.37229(4) 0.02217(15) Uani 1 1 d . . . Cu2 Cu 0.78879(4) 0.21727(4) 0.17885(4) 0.02541(16) Uani 1 1 d . . . C1 C 0.7335(4) 0.4698(4) 0.2097(4) 0.0301(10) Uani 1 1 d . . . C2 C 0.7108(4) 0.5391(4) 0.1662(4) 0.0323(10) Uani 1 1 d . . . H2 H 0.6388 0.5282 0.1250 0.039 Uiso 1 1 calc R . . C3 C 0.7991(4) 0.6245(4) 0.1864(4) 0.0334(11) Uani 1 1 d . . . N11 N 0.9015(4) 0.6374(3) 0.2402(3) 0.0335(9) Uani 1 1 d . . . C4 C 0.9156(4) 0.5651(4) 0.2778(4) 0.0306(10) Uani 1 1 d . . . N15 N 0.8342(3) 0.4841(3) 0.2677(3) 0.0289(8) Uani 1 1 d . . . C5 C 1.0289(4) 0.5730(4) 0.3309(4) 0.0318(10) Uani 1 1 d . . . C6 C 1.1189(5) 0.6308(4) 0.3163(4) 0.0409(12) Uani 1 1 d . . . H6 H 1.1078 0.6704 0.2771 0.049 Uiso 1 1 calc R . . C7 C 1.2250(5) 0.6301(5) 0.3596(6) 0.0519(15) Uani 1 1 d . . . H7 H 1.2861 0.6679 0.3480 0.062 Uiso 1 1 calc R . . C8 C 1.2420(5) 0.5754(5) 0.4188(6) 0.0552(16) Uani 1 1 d . . . H8 H 1.3148 0.5759 0.4484 0.066 Uiso 1 1 calc R . . C9 C 1.1538(5) 0.5200(4) 0.4352(5) 0.0472(14) Uani 1 1 d . . . H9 H 1.1657 0.4836 0.4777 0.057 Uiso 1 1 calc R . . C10 C 1.0471(5) 0.5172(4) 0.3896(4) 0.0388(11) Uani 1 1 d . . . H10 H 0.9861 0.4767 0.3989 0.047 Uiso 1 1 calc R . . C11 C 0.7855(5) 0.7103(4) 0.1511(4) 0.0394(12) Uani 1 1 d . . . H11A H 0.8384 0.7120 0.1068 0.047 Uiso 1 1 calc R . . H11B H 0.7101 0.6863 0.1018 0.047 Uiso 1 1 calc R . . N12 N 0.8043(3) 0.8277(3) 0.2506(3) 0.0269(8) Uani 1 1 d . . . C12 C 0.7120(4) 0.8376(4) 0.3044(4) 0.0347(11) Uani 1 1 d . . . H12A H 0.6420 0.7876 0.2460 0.042 Uiso 1 1 calc R . . H12B H 0.7060 0.9180 0.3411 0.042 Uiso 1 1 calc R . . C14 C 0.7313(4) 0.8026(4) 0.3918(4) 0.0315(10) Uani 1 1 d . . . C15 C 0.6472(5) 0.7621(6) 0.4246(5) 0.0484(14) Uani 1 1 d . . . H15 H 0.5727 0.7531 0.3906 0.058 Uiso 1 1 calc R . . C16 C 0.6718(5) 0.7346(6) 0.5076(5) 0.0489(14) Uani 1 1 d . . . H16 H 0.6146 0.7070 0.5314 0.059 Uiso 1 1 calc R . . C17 C 0.7800(4) 0.7477(4) 0.5546(4) 0.0365(11) Uani 1 1 d . . . H17 H 0.7989 0.7291 0.6113 0.044 Uiso 1 1 calc R . . C18 C 0.8609(4) 0.7886(4) 0.5180(4) 0.0269(9) Uani 1 1 d . . . H18 H 0.9359 0.7974 0.5502 0.032 Uiso 1 1 calc R . . N13 N 0.8371(3) 0.8161(3) 0.4385(3) 0.0236(7) Uani 1 1 d . . . C22 C 0.8274(4) 0.9123(4) 0.2135(4) 0.0302(10) Uani 1 1 d . . . H22A H 0.8162 0.9868 0.2686 0.036 Uiso 1 1 calc R . . H22B H 0.7765 0.8838 0.1388 0.036 Uiso 1 1 calc R . . C24 C 0.9445(4) 0.9276(3) 0.2063(4) 0.0280(9) Uani 1 1 d . . . C25 C 0.9797(5) 0.9579(4) 0.1333(4) 0.0346(11) Uani 1 1 d . . . H25 H 0.9290 0.9681 0.0831 0.041 Uiso 1 1 calc R . . C26 C 1.0897(5) 0.9731(4) 0.1347(4) 0.0376(12) Uani 1 1 d . . . H26 H 1.1157 0.9937 0.0852 0.045 Uiso 1 1 calc R . . C27 C 1.1615(4) 0.9581(4) 0.2085(4) 0.0360(11) Uani 1 1 d . . . H27 H 1.2374 0.9679 0.2103 0.043 Uiso 1 1 calc R . . C28 C 1.1217(4) 0.9285(4) 0.2799(4) 0.0315(10) Uani 1 1 d . . . H28 H 1.1712 0.9188 0.3312 0.038 Uiso 1 1 calc R . . N14 N 1.0148(3) 0.9133(3) 0.2786(3) 0.0254(8) Uani 1 1 d . . . Cl3 Cl 1.09654(9) 0.90930(9) 0.50219(9) 0.0271(2) Uani 1 1 d . . . C31 C 0.6433(4) 0.3742(4) 0.1929(4) 0.0318(10) Uani 1 1 d . . . H31A H 0.6435 0.3824 0.2673 0.038 Uiso 1 1 calc R . . H31B H 0.5713 0.3818 0.1622 0.038 Uiso 1 1 calc R . . N16 N 0.6547(3) 0.2569(3) 0.1147(3) 0.0244(7) Uani 1 1 d . . . C32 C 0.5582(4) 0.1724(4) 0.1025(4) 0.0269(9) Uani 1 1 d . . . H32A H 0.5479 0.0970 0.0334 0.032 Uiso 1 1 calc R . . H32B H 0.4907 0.1989 0.0955 0.032 Uiso 1 1 calc R . . C34 C 0.5781(4) 0.1604(3) 0.2055(4) 0.0253(9) Uani 1 1 d . . . C35 C 0.4938(4) 0.1239(4) 0.2411(4) 0.0318(10) Uani 1 1 d . . . H35 H 0.4191 0.1096 0.2037 0.038 Uiso 1 1 calc R . . C36 C 0.5198(4) 0.1084(4) 0.3324(4) 0.0356(11) Uani 1 1 d . . . H36 H 0.4631 0.0822 0.3576 0.043 Uiso 1 1 calc R . . C37 C 0.6304(4) 0.1319(4) 0.3865(4) 0.0329(10) Uani 1 1 d . . . H37 H 0.6503 0.1221 0.4492 0.039 Uiso 1 1 calc R . . C38 C 0.7104(4) 0.1697(4) 0.3469(4) 0.0298(9) Uani 1 1 d . . . H38 H 0.7858 0.1871 0.3842 0.036 Uiso 1 1 calc R . . N17 N 0.6849(3) 0.1826(3) 0.2576(3) 0.0255(7) Uani 1 1 d . . . C42 C 0.6661(4) 0.2406(4) 0.0047(4) 0.0285(9) Uani 1 1 d . . . H42A H 0.6237 0.2858 -0.0159 0.034 Uiso 1 1 calc R . . H42B H 0.6363 0.1585 -0.0550 0.034 Uiso 1 1 calc R . . C44 C 0.7862(4) 0.2795(4) 0.0131(4) 0.0275(9) Uani 1 1 d . . . C45 C 0.8215(4) 0.3239(4) -0.0508(4) 0.0335(10) Uani 1 1 d . . . H45 H 0.7700 0.3323 -0.1018 0.040 Uiso 1 1 calc R . . C46 C 0.9345(5) 0.3559(4) -0.0379(4) 0.0377(12) Uani 1 1 d . . . H46 H 0.9613 0.3857 -0.0808 0.045 Uiso 1 1 calc R . . C47 C 1.0064(4) 0.3436(4) 0.0375(4) 0.0378(12) Uani 1 1 d . . . H47 H 1.0836 0.3660 0.0481 0.045 Uiso 1 1 calc R . . C48 C 0.9660(4) 0.2985(4) 0.0979(4) 0.0319(10) Uani 1 1 d . . . H48 H 1.0162 0.2896 0.1494 0.038 Uiso 1 1 calc R . . N18 N 0.8575(3) 0.2672(3) 0.0854(3) 0.0263(8) Uani 1 1 d . . . Cl4 Cl 0.94303(9) 0.22260(9) 0.28506(10) 0.0306(2) Uani 1 1 d . . . Cl5 Cl 0.72193(9) -0.00070(9) 0.01292(9) 0.0283(2) Uani 1 1 d . . . O50 O 0.5393(9) -0.3586(9) 0.0123(12) 0.098(4) Uani 0.50 1 d P . . H50X H 0.5117 -0.3745 0.0579 0.117 Uiso 0.50 1 d P . . H50Y H 0.5470 -0.4250 -0.0307 0.117 Uiso 0.50 1 d P . . O60 O 0.4849(6) -0.4643(7) -0.4511(7) 0.052(2) Uani 0.50 1 d P . . H60X H 0.4260 -0.4902 -0.4427 0.062 Uiso 0.50 1 d P . . H60Y H 0.4740 -0.5045 -0.5244 0.062 Uiso 0.50 1 d P . . O70 O 0.7144(8) -0.2592(6) -0.0868(7) 0.058(2) Uani 0.50 1 d P A 1 H70 H 0.7156 -0.1885 -0.0599 0.069 Uiso 0.50 1 d P B 1 C70 C 0.7242(11) -0.3033(10) -0.1878(8) 0.052(3) Uani 0.50 1 d PU A 1 H70C H 0.6525 -0.3517 -0.2415 0.063 Uiso 0.50 1 calc PR A 1 H70A H 0.7772 -0.3502 -0.1976 0.063 Uiso 0.50 1 calc PR A 1 H70B H 0.7506 -0.2418 -0.2018 0.063 Uiso 0.50 1 calc PR A 1 O80 O 0.5902(11) -0.4350(14) -0.2624(11) 0.042(3) Uani 0.25 1 d PU C 2 H80X H 0.5915 -0.4756 -0.2304 0.050 Uiso 0.25 1 d P D 2 H80Y H 0.5555 -0.4458 -0.3245 0.050 Uiso 0.25 1 d P E 2 Cl20 Cl 0.4445(7) -0.3828(7) 0.1413(6) 0.064(2) Uani 0.25 1 d P F 1 Cl21 Cl 0.4036(5) -0.4286(7) 0.1510(5) 0.0405(15) Uani 0.25 1 d P G 2 O90 O 0.3989(7) -0.0188(7) 0.4506(7) 0.054(2) Uani 0.50 1 d P . . H90X H 0.4652 -0.0051 0.4847 0.065 Uiso 0.50 1 d P . . H90Y H 0.3537 0.0033 0.4933 0.065 Uiso 0.50 1 d P . . Cl22 Cl 0.5931(2) 0.1440(2) 0.6684(3) 0.0516(7) Uani 0.50 1 d P . . 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 Cu1 0.0297(3) 0.0186(3) 0.0226(3) 0.0125(2) 0.0099(2) 0.0079(2) Cu2 0.0273(3) 0.0262(3) 0.0259(3) 0.0155(2) 0.0088(2) 0.0063(2) C1 0.044(3) 0.017(2) 0.031(2) 0.0112(18) 0.018(2) 0.0088(19) C2 0.049(3) 0.021(2) 0.025(2) 0.0102(18) 0.013(2) 0.006(2) C3 0.057(3) 0.018(2) 0.020(2) 0.0080(17) 0.010(2) 0.002(2) N11 0.053(3) 0.0176(17) 0.0215(18) 0.0067(15) 0.0097(17) -0.0008(17) C4 0.052(3) 0.020(2) 0.019(2) 0.0086(17) 0.0156(19) 0.0059(19) N15 0.045(2) 0.0156(17) 0.0246(18) 0.0087(15) 0.0147(17) 0.0051(16) C5 0.047(3) 0.017(2) 0.024(2) 0.0048(17) 0.014(2) 0.0047(19) C6 0.059(3) 0.024(2) 0.037(3) 0.010(2) 0.025(2) 0.010(2) C7 0.053(4) 0.035(3) 0.065(4) 0.018(3) 0.033(3) 0.015(3) C8 0.054(4) 0.030(3) 0.071(4) 0.014(3) 0.020(3) 0.020(3) C9 0.059(4) 0.023(2) 0.048(3) 0.013(2) 0.007(3) 0.011(2) C10 0.050(3) 0.024(2) 0.034(3) 0.013(2) 0.005(2) 0.003(2) C11 0.064(3) 0.020(2) 0.025(2) 0.0125(19) 0.000(2) -0.004(2) N12 0.036(2) 0.0223(18) 0.0281(19) 0.0185(16) 0.0058(16) 0.0041(15) C12 0.028(2) 0.042(3) 0.045(3) 0.032(2) 0.005(2) 0.005(2) C14 0.034(2) 0.029(2) 0.038(3) 0.022(2) 0.008(2) 0.0079(19) C15 0.035(3) 0.067(4) 0.066(4) 0.051(3) 0.016(3) 0.010(3) C16 0.044(3) 0.066(4) 0.064(4) 0.052(3) 0.024(3) 0.014(3) C17 0.052(3) 0.035(3) 0.040(3) 0.028(2) 0.023(2) 0.017(2) C18 0.038(2) 0.022(2) 0.028(2) 0.0167(18) 0.0134(19) 0.0108(18) N13 0.0318(19) 0.0191(16) 0.0236(18) 0.0127(15) 0.0095(15) 0.0082(14) C22 0.041(3) 0.027(2) 0.034(2) 0.023(2) 0.013(2) 0.0107(19) C24 0.043(3) 0.0158(19) 0.028(2) 0.0122(17) 0.0135(19) 0.0088(18) C25 0.055(3) 0.025(2) 0.035(3) 0.020(2) 0.020(2) 0.013(2) C26 0.060(3) 0.023(2) 0.037(3) 0.017(2) 0.026(2) 0.009(2) C27 0.045(3) 0.022(2) 0.038(3) 0.011(2) 0.024(2) 0.008(2) C28 0.041(3) 0.023(2) 0.034(2) 0.0136(19) 0.017(2) 0.0109(19) N14 0.035(2) 0.0158(16) 0.0259(18) 0.0097(15) 0.0127(15) 0.0083(15) Cl3 0.0307(5) 0.0247(5) 0.0303(5) 0.0161(4) 0.0091(4) 0.0111(4) C31 0.042(3) 0.021(2) 0.039(3) 0.017(2) 0.019(2) 0.0100(19) N16 0.0305(19) 0.0196(17) 0.0272(18) 0.0150(15) 0.0093(15) 0.0053(15) C32 0.027(2) 0.025(2) 0.033(2) 0.0191(19) 0.0076(18) 0.0026(17) C34 0.031(2) 0.0184(19) 0.027(2) 0.0119(17) 0.0070(17) 0.0057(17) C35 0.032(2) 0.029(2) 0.036(2) 0.019(2) 0.009(2) 0.0031(19) C36 0.044(3) 0.029(2) 0.038(3) 0.020(2) 0.017(2) 0.004(2) C37 0.046(3) 0.029(2) 0.029(2) 0.018(2) 0.013(2) 0.011(2) C38 0.036(2) 0.029(2) 0.028(2) 0.0158(19) 0.0095(19) 0.0122(19) N17 0.033(2) 0.0212(17) 0.0235(18) 0.0123(15) 0.0084(15) 0.0071(15) C42 0.035(2) 0.026(2) 0.031(2) 0.0194(19) 0.0094(19) 0.0077(18) C44 0.039(2) 0.0182(19) 0.027(2) 0.0108(17) 0.0144(19) 0.0079(18) C45 0.049(3) 0.025(2) 0.029(2) 0.0154(19) 0.015(2) 0.008(2) C46 0.055(3) 0.025(2) 0.030(2) 0.012(2) 0.021(2) 0.001(2) C47 0.042(3) 0.032(2) 0.028(2) 0.008(2) 0.017(2) -0.001(2) C48 0.033(2) 0.028(2) 0.025(2) 0.0084(19) 0.0097(19) 0.0019(19) N18 0.033(2) 0.0177(16) 0.0228(18) 0.0066(14) 0.0105(15) 0.0029(15) Cl4 0.0298(5) 0.0301(5) 0.0335(6) 0.0182(5) 0.0061(4) 0.0077(4) Cl5 0.0326(6) 0.0211(5) 0.0290(5) 0.0121(4) 0.0078(4) 0.0043(4) O50 0.068(7) 0.060(7) 0.122(10) 0.029(7) -0.018(7) 0.009(5) O60 0.037(4) 0.043(4) 0.051(5) 0.006(4) 0.008(4) 0.016(3) O70 0.089(7) 0.028(4) 0.056(5) 0.022(4) 0.017(5) 0.020(4) C70 0.078(7) 0.046(5) 0.020(4) 0.001(4) 0.005(4) 0.049(5) O80 0.035(6) 0.069(8) 0.027(6) 0.020(5) 0.016(5) 0.038(6) Cl20 0.055(5) 0.069(5) 0.040(4) 0.011(3) -0.019(3) 0.038(4) Cl21 0.026(3) 0.078(5) 0.023(2) 0.026(3) 0.015(2) 0.021(3) O90 0.062(5) 0.058(5) 0.065(6) 0.042(5) 0.034(4) 0.021(4) Cl22 0.0362(13) 0.0483(15) 0.090(2) 0.0539(16) 0.0100(14) 0.0061(11) _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 Cu1 N14 1.981(4) . y Cu1 N13 1.985(4) . y Cu1 N12 2.040(4) . y Cu1 Cl3 2.2322(13) . y Cu2 N17 1.993(4) . y Cu2 N18 1.998(4) . y Cu2 N16 2.065(4) . y Cu2 Cl4 2.2321(13) . y Cu2 Cl5 2.6480(13) . y C1 N15 1.334(6) . ? C1 C2 1.392(6) . ? C1 C31 1.508(6) . ? C2 C3 1.382(7) . ? C3 N11 1.336(7) . ? C3 C11 1.501(6) . ? N11 C4 1.347(6) . ? C4 N15 1.339(6) . ? C4 C5 1.476(7) . ? C5 C10 1.381(7) . ? C5 C6 1.393(7) . ? C6 C7 1.391(9) . ? C7 C8 1.372(9) . ? C8 C9 1.376(9) . ? C9 C10 1.393(8) . ? C11 N12 1.488(6) . ? N12 C12 1.482(6) . ? N12 C22 1.494(5) . ? C12 C14 1.512(6) . ? C14 N13 1.343(6) . ? C14 C15 1.374(7) . ? C15 C16 1.388(8) . ? C16 C17 1.372(8) . ? C17 C18 1.383(6) . ? C18 N13 1.341(5) . ? C22 C24 1.502(7) . ? C24 N14 1.347(6) . ? C24 C25 1.383(6) . ? C25 C26 1.380(8) . ? C26 C27 1.379(8) . ? C27 C28 1.381(7) . ? C28 N14 1.341(6) . ? C31 N16 1.497(5) . ? N16 C42 1.479(6) . ? N16 C32 1.485(5) . ? C32 C34 1.512(6) . ? C34 N17 1.348(6) . ? C34 C35 1.379(6) . ? C35 C36 1.389(7) . ? C36 C37 1.396(7) . ? C37 C38 1.383(7) . ? C38 N17 1.340(6) . ? C42 C44 1.509(6) . ? C44 N18 1.337(6) . ? C44 C45 1.394(6) . ? C45 C46 1.396(7) . ? C46 C47 1.373(8) . ? C47 C48 1.381(7) . ? C48 N18 1.340(6) . ? O60 O60 1.404(15) 2_644 ? O70 C70 1.278(13) . ? O90 Cl22 1.758(9) 2_656 ? Cl22 O90 1.758(9) 2_656 ? 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 N14 Cu1 N13 165.64(16) . . y N14 Cu1 N12 82.33(15) . . y N13 Cu1 N12 83.35(15) . . y N14 Cu1 Cl3 97.02(12) . . y N13 Cu1 Cl3 97.32(11) . . y N12 Cu1 Cl3 178.59(12) . . y N17 Cu2 N18 163.54(16) . . y N17 Cu2 N16 81.38(14) . . y N18 Cu2 N16 82.23(15) . . y N17 Cu2 Cl4 97.44(11) . . y N18 Cu2 Cl4 97.99(12) . . y N16 Cu2 Cl4 164.83(11) . . y N17 Cu2 Cl5 89.29(11) . . y N18 Cu2 Cl5 92.83(10) . . y N16 Cu2 Cl5 92.33(10) . . y Cl4 Cu2 Cl5 102.80(4) . . y N15 C1 C2 122.6(4) . . ? N15 C1 C31 116.8(4) . . ? C2 C1 C31 120.6(5) . . ? C3 C2 C1 116.1(5) . . ? N11 C3 C2 122.4(4) . . ? N11 C3 C11 115.7(4) . . ? C2 C3 C11 122.0(5) . . ? C3 N11 C4 117.1(4) . . ? N15 C4 N11 124.7(5) . . ? N15 C4 C5 117.3(4) . . ? N11 C4 C5 118.0(4) . . ? C1 N15 C4 116.9(4) . . ? C10 C5 C6 119.2(5) . . ? C10 C5 C4 120.4(4) . . ? C6 C5 C4 120.3(5) . . ? C7 C6 C5 119.7(5) . . ? C8 C7 C6 120.6(6) . . ? C7 C8 C9 120.0(6) . . ? C8 C9 C10 119.9(6) . . ? C5 C10 C9 120.6(5) . . ? N12 C11 C3 111.6(4) . . ? C12 N12 C11 111.8(4) . . ? C12 N12 C22 113.9(4) . . ? C11 N12 C22 108.1(3) . . ? C12 N12 Cu1 106.6(3) . . ? C11 N12 Cu1 111.2(3) . . ? C22 N12 Cu1 105.0(3) . . ? N12 C12 C14 110.1(4) . . ? N13 C14 C15 121.3(4) . . ? N13 C14 C12 115.7(4) . . ? C15 C14 C12 123.0(4) . . ? C14 C15 C16 119.5(5) . . ? C17 C16 C15 119.0(5) . . ? C16 C17 C18 118.8(5) . . ? N13 C18 C17 122.1(4) . . ? C18 N13 C14 119.2(4) . . ? C18 N13 Cu1 126.7(3) . . ? C14 N13 Cu1 114.0(3) . . ? N12 C22 C24 108.4(4) . . ? N14 C24 C25 121.7(5) . . ? N14 C24 C22 115.4(4) . . ? C25 C24 C22 122.9(4) . . ? C26 C25 C24 118.8(5) . . ? C27 C26 C25 119.4(4) . . ? C26 C27 C28 119.2(5) . . ? N14 C28 C27 121.6(5) . . ? C28 N14 C24 119.2(4) . . ? C28 N14 Cu1 127.1(3) . . ? C24 N14 Cu1 113.6(3) . . ? N16 C31 C1 113.3(4) . . ? C42 N16 C32 112.6(3) . . ? C42 N16 C31 112.7(3) . . ? C32 N16 C31 107.2(3) . . ? C42 N16 Cu2 106.1(3) . . ? C32 N16 Cu2 104.1(2) . . ? C31 N16 Cu2 113.8(3) . . ? N16 C32 C34 108.8(3) . . ? N17 C34 C35 121.8(4) . . ? N17 C34 C32 115.2(4) . . ? C35 C34 C32 122.9(4) . . ? C34 C35 C36 119.0(4) . . ? C35 C36 C37 119.1(4) . . ? C38 C37 C36 118.6(4) . . ? N17 C38 C37 122.0(4) . . ? C38 N17 C34 119.4(4) . . ? C38 N17 Cu2 126.9(3) . . ? C34 N17 Cu2 113.4(3) . . ? N16 C42 C44 109.4(4) . . ? N18 C44 C45 121.7(4) . . ? N18 C44 C42 115.5(4) . . ? C45 C44 C42 122.8(4) . . ? C44 C45 C46 118.3(5) . . ? C47 C46 C45 119.0(4) . . ? C46 C47 C48 119.8(5) . . ? N18 C48 C47 121.3(5) . . ? C44 N18 C48 119.8(4) . . ? C44 N18 Cu2 114.3(3) . . ? C48 N18 Cu2 125.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N15 C1 C2 C3 0.0(7) . . . . ? C31 C1 C2 C3 179.8(4) . . . . ? C1 C2 C3 N11 2.8(7) . . . . ? C1 C2 C3 C11 -175.9(4) . . . . ? C2 C3 N11 C4 -1.9(6) . . . . ? C11 C3 N11 C4 176.9(4) . . . . ? C3 N11 C4 N15 -2.0(6) . . . . ? C3 N11 C4 C5 176.2(4) . . . . ? C2 C1 N15 C4 -3.5(6) . . . . ? C31 C1 N15 C4 176.7(4) . . . . ? N11 C4 N15 C1 4.6(6) . . . . ? C5 C4 N15 C1 -173.5(4) . . . . ? N15 C4 C5 C10 -14.0(6) . . . . ? N11 C4 C5 C10 167.8(4) . . . . ? N15 C4 C5 C6 162.0(4) . . . . ? N11 C4 C5 C6 -16.3(6) . . . . ? C10 C5 C6 C7 0.9(7) . . . . ? C4 C5 C6 C7 -175.1(4) . . . . ? C5 C6 C7 C8 -1.6(8) . . . . ? C6 C7 C8 C9 0.4(9) . . . . ? C7 C8 C9 C10 1.4(8) . . . . ? C6 C5 C10 C9 1.0(7) . . . . ? C4 C5 C10 C9 176.9(4) . . . . ? C8 C9 C10 C5 -2.1(8) . . . . ? N11 C3 C11 N12 -67.9(6) . . . . ? C2 C3 C11 N12 110.9(5) . . . . ? C3 C11 N12 C12 -72.8(5) . . . . ? C3 C11 N12 C22 161.0(4) . . . . ? C3 C11 N12 Cu1 46.3(5) . . . . ? N14 Cu1 N12 C12 -153.2(3) . . . . ? N13 Cu1 N12 C12 25.7(3) . . . . ? N14 Cu1 N12 C11 84.6(3) . . . . ? N13 Cu1 N12 C11 -96.5(3) . . . . ? N14 Cu1 N12 C22 -32.0(3) . . . . ? N13 Cu1 N12 C22 146.9(3) . . . . ? C11 N12 C12 C14 87.9(5) . . . . ? C22 N12 C12 C14 -149.2(4) . . . . ? Cu1 N12 C12 C14 -33.9(4) . . . . ? N12 C12 C14 N13 26.5(6) . . . . ? N12 C12 C14 C15 -155.1(5) . . . . ? N13 C14 C15 C16 0.0(9) . . . . ? C12 C14 C15 C16 -178.3(6) . . . . ? C14 C15 C16 C17 -0.4(10) . . . . ? C15 C16 C17 C18 0.3(9) . . . . ? C16 C17 C18 N13 0.3(7) . . . . ? C17 C18 N13 C14 -0.7(6) . . . . ? C17 C18 N13 Cu1 -176.8(3) . . . . ? C15 C14 N13 C18 0.5(7) . . . . ? C12 C14 N13 C18 179.0(4) . . . . ? C15 C14 N13 Cu1 177.1(4) . . . . ? C12 C14 N13 Cu1 -4.4(5) . . . . ? N14 Cu1 N13 C18 168.2(5) . . . . ? N12 Cu1 N13 C18 163.8(4) . . . . ? Cl3 Cu1 N13 C18 -14.9(4) . . . . ? N14 Cu1 N13 C14 -8.1(7) . . . . ? N12 Cu1 N13 C14 -12.4(3) . . . . ? Cl3 Cu1 N13 C14 168.8(3) . . . . ? C12 N12 C22 C24 157.0(4) . . . . ? C11 N12 C22 C24 -78.1(5) . . . . ? Cu1 N12 C22 C24 40.7(4) . . . . ? N12 C22 C24 N14 -30.0(5) . . . . ? N12 C22 C24 C25 151.9(4) . . . . ? N14 C24 C25 C26 0.3(7) . . . . ? C22 C24 C25 C26 178.3(4) . . . . ? C24 C25 C26 C27 -0.1(7) . . . . ? C25 C26 C27 C28 -0.3(7) . . . . ? C26 C27 C28 N14 0.5(7) . . . . ? C27 C28 N14 C24 -0.3(6) . . . . ? C27 C28 N14 Cu1 178.8(3) . . . . ? C25 C24 N14 C28 -0.1(6) . . . . ? C22 C24 N14 C28 -178.2(4) . . . . ? C25 C24 N14 Cu1 -179.3(3) . . . . ? C22 C24 N14 Cu1 2.6(5) . . . . ? N13 Cu1 N14 C28 -166.2(5) . . . . ? N12 Cu1 N14 C28 -161.8(4) . . . . ? Cl3 Cu1 N14 C28 17.0(4) . . . . ? N13 Cu1 N14 C24 13.0(7) . . . . ? N12 Cu1 N14 C24 17.4(3) . . . . ? Cl3 Cu1 N14 C24 -163.9(3) . . . . ? N15 C1 C31 N16 -69.3(5) . . . . ? C2 C1 C31 N16 110.9(5) . . . . ? C1 C31 N16 C42 -53.0(5) . . . . ? C1 C31 N16 C32 -177.5(4) . . . . ? C1 C31 N16 Cu2 67.9(4) . . . . ? N17 Cu2 N16 C42 -154.1(3) . . . . ? N18 Cu2 N16 C42 27.4(3) . . . . ? Cl4 Cu2 N16 C42 119.2(4) . . . . ? Cl5 Cu2 N16 C42 -65.2(2) . . . . ? N17 Cu2 N16 C32 -35.1(3) . . . . ? N18 Cu2 N16 C32 146.4(3) . . . . ? Cl4 Cu2 N16 C32 -121.7(4) . . . . ? Cl5 Cu2 N16 C32 53.8(3) . . . . ? N17 Cu2 N16 C31 81.3(3) . . . . ? N18 Cu2 N16 C31 -97.2(3) . . . . ? Cl4 Cu2 N16 C31 -5.3(6) . . . . ? Cl5 Cu2 N16 C31 170.2(3) . . . . ? C42 N16 C32 C34 156.3(3) . . . . ? C31 N16 C32 C34 -79.1(4) . . . . ? Cu2 N16 C32 C34 41.8(4) . . . . ? N16 C32 C34 N17 -27.3(5) . . . . ? N16 C32 C34 C35 155.8(4) . . . . ? N17 C34 C35 C36 -0.7(7) . . . . ? C32 C34 C35 C36 175.9(4) . . . . ? C34 C35 C36 C37 1.0(7) . . . . ? C35 C36 C37 C38 -0.1(7) . . . . ? C36 C37 C38 N17 -1.1(7) . . . . ? C37 C38 N17 C34 1.4(6) . . . . ? C37 C38 N17 Cu2 -171.9(3) . . . . ? C35 C34 N17 C38 -0.5(6) . . . . ? C32 C34 N17 C38 -177.3(4) . . . . ? C35 C34 N17 Cu2 173.7(3) . . . . ? C32 C34 N17 Cu2 -3.2(4) . . . . ? N18 Cu2 N17 C38 -158.9(5) . . . . ? N16 Cu2 N17 C38 -164.1(4) . . . . ? Cl4 Cu2 N17 C38 0.6(4) . . . . ? Cl5 Cu2 N17 C38 103.4(4) . . . . ? N18 Cu2 N17 C34 27.4(7) . . . . ? N16 Cu2 N17 C34 22.3(3) . . . . ? Cl4 Cu2 N17 C34 -173.0(3) . . . . ? Cl5 Cu2 N17 C34 -70.2(3) . . . . ? C32 N16 C42 C44 -150.5(4) . . . . ? C31 N16 C42 C44 88.0(4) . . . . ? Cu2 N16 C42 C44 -37.2(4) . . . . ? N16 C42 C44 N18 30.6(5) . . . . ? N16 C42 C44 C45 -150.3(4) . . . . ? N18 C44 C45 C46 0.0(7) . . . . ? C42 C44 C45 C46 -179.0(4) . . . . ? C44 C45 C46 C47 -0.7(7) . . . . ? C45 C46 C47 C48 1.0(7) . . . . ? C46 C47 C48 N18 -0.6(7) . . . . ? C45 C44 N18 C48 0.4(6) . . . . ? C42 C44 N18 C48 179.5(4) . . . . ? C45 C44 N18 Cu2 174.0(3) . . . . ? C42 C44 N18 Cu2 -6.9(5) . . . . ? C47 C48 N18 C44 0.0(6) . . . . ? C47 C48 N18 Cu2 -172.9(3) . . . . ? N17 Cu2 N18 C44 -17.2(7) . . . . ? N16 Cu2 N18 C44 -12.0(3) . . . . ? Cl4 Cu2 N18 C44 -176.7(3) . . . . ? Cl5 Cu2 N18 C44 80.0(3) . . . . ? N17 Cu2 N18 C48 156.0(5) . . . . ? N16 Cu2 N18 C48 161.2(4) . . . . ? Cl4 Cu2 N18 C48 -3.5(4) . . . . ? Cl5 Cu2 N18 C48 -106.8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O80 H80Y O60 0.84 1.73 2.570(16) 178.6 . O90 H90X Cl22 0.85 2.46 3.131(10) 136.6 . O70 H70 Cl5 0.85 2.26 3.108(7) 178.9 . O50 H50X Cl21 0.87 2.31 3.169(16) 167.9 . O50 H50Y Cl20 0.85 2.36 3.209(14) 173.8 2_645 O50 H50Y Cl21 0.85 2.18 3.006(14) 165.5 2_645 O80 H80X Cl21 0.87 2.09 2.956(17) 179.1 2_645 O90 H90X O90 0.85 1.72 2.566(18) 177.8 2_656 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.56 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.912 _refine_diff_density_min -0.545 _refine_diff_density_rms 0.139 _database_code_depnum_ccdc_archive 'CCDC 921845'