Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Vickie McKee' _publ_contact_author_address ; Chemistry Loughborough University Chemistry Department Loughborough University Loughborough Leics LE11 3TU UNITED KINGDOM ; _publ_contact_author_email V.MCKEE@LBORO.AC.UK _publ_section_title ; Dinuclear Complexes of a Pseudocalixarene Macrocycle: Structural Consequences of Intramolecular Hydrogen Bonding. ; loop_ _publ_author_name 'Vickie McKee' 'Julia Barreira Fontecha' 'Sandrine Goetz' data_test_3 _database_code_depnum_ccdc_archive 'CCDC 249422' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H80.10 Cl2 N4 O8.05 Zn2' _chemical_formula_weight 1151.79 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 13.8372(7) _cell_length_b 14.7550(7) _cell_length_c 16.8022(8) _cell_angle_alpha 103.4880(10) _cell_angle_beta 95.6630(10) _cell_angle_gamma 93.0300(10) _cell_volume 3309.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14554 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 23.83 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1217 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.697745 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 23643 _diffrn_reflns_av_R_equivalents 0.0167 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11600 _reflns_number_gt 9694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. This complex is isomorphous with the copper equivalent. The detailed structure differs in the occupancy of the solvate sites and in the 5-/6-coordinate disorder at the zinc sites. One disordered t-butylphenol group was refined with 60:40 occupancy of two positions and one with 18:15; one of the pendant alcohols showed 80:20 disorder over two positions; the ethanol solvate was modeled with partial (25:25) occupancy of two overlapping positions and the diethylether solvate molecules were each refined with 50% occupancy. No hydrogen atoms bonded to oxygen were located or included in the model. ; _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^)+(0.1388P)^2^+5.2564P] 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 11600 _refine_ls_number_parameters 805 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.2262 _refine_ls_wR_factor_gt 0.2137 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.4060(2) 0.54567(17) 0.16557(16) 0.0344(3) Uani 0.85 1 d P . . Zn1' Zn 0.4139(12) 0.5259(10) 0.1791(10) 0.053(3) Uani 0.15 1 d P . . O1W O 0.476(2) 0.435(2) 0.262(2) 0.086(8) Uiso 0.15 1 d P . . Zn2 Zn 0.4257(2) 0.79423(14) 0.16730(18) 0.0342(4) Uani 0.60 1 d P . . Zn2' Zn 0.4339(4) 0.8250(2) 0.1791(3) 0.0500(10) Uani 0.40 1 d P . . O2W O 0.5022(7) 0.9578(7) 0.2554(6) 0.062(2) Uani 0.40 1 d P . . Cl1 Cl 0.34610(7) 0.65238(7) 0.09664(6) 0.0401(3) Uani 1 1 d . . . Cl2 Cl 0.20108(10) 1.13871(10) 0.14193(10) 0.0652(4) Uani 1 1 d . . . O1 O 0.55213(19) 0.59566(19) 0.19173(18) 0.0374(6) Uani 1 1 d . . . C1 C 0.6338(3) 0.5503(3) 0.1777(2) 0.0348(8) Uani 1 1 d . . . C2 C 0.6274(3) 0.4587(3) 0.1295(2) 0.0352(8) Uani 1 1 d . B . C3 C 0.7132(3) 0.4122(3) 0.1191(3) 0.0391(9) Uani 1 1 d . . . H3 H 0.7081 0.3493 0.0877 0.047 Uiso 1 1 calc R . . C4 C 0.8046(3) 0.4541(3) 0.1525(3) 0.0424(10) Uani 1 1 d . . . C5 C 0.8978(3) 0.4041(4) 0.1377(3) 0.0543(12) Uani 1 1 d . . . C6 C 0.9701(4) 0.4271(5) 0.2141(4) 0.0785(18) Uani 1 1 d . . . H6A H 1.0288 0.3942 0.2028 0.050 Uiso 1 1 calc R . . H6B H 0.9411 0.4073 0.2588 0.050 Uiso 1 1 calc R . . H6C H 0.9873 0.4946 0.2303 0.050 Uiso 1 1 calc R . . C7 C 0.8783(5) 0.2991(5) 0.1091(6) 0.106(3) Uani 1 1 d . . . H7A H 0.9399 0.2704 0.1006 0.050 Uiso 1 1 calc R . . H7B H 0.8350 0.2834 0.0572 0.050 Uiso 1 1 calc R . . H7C H 0.8472 0.2753 0.1509 0.050 Uiso 1 1 calc R . . C8 C 0.9436(5) 0.4362(7) 0.0681(5) 0.108(3) Uani 1 1 d . . . H8A H 1.0035 0.4050 0.0580 0.050 Uiso 1 1 calc R . . H8B H 0.9589 0.5040 0.0843 0.050 Uiso 1 1 calc R . . H8C H 0.8976 0.4199 0.0178 0.050 Uiso 1 1 calc R . . C9 C 0.8081(3) 0.5473(3) 0.1970(3) 0.0437(10) Uani 1 1 d . . . H9 H 0.8699 0.5787 0.2195 0.052 Uiso 1 1 calc R . . C10 C 0.7259(3) 0.5962(3) 0.2100(3) 0.0393(9) Uani 1 1 d . . . C11 C 0.7358(3) 0.6980(3) 0.2591(3) 0.0439(10) Uani 1 1 d . . . H11A H 0.6810 0.7087 0.2930 0.053 Uiso 1 1 calc R . . H11B H 0.7969 0.7091 0.2971 0.053 Uiso 1 1 calc R . . C12 C 0.7366(3) 0.7680(3) 0.2059(3) 0.0403(9) Uani 1 1 d . . . C13 C 0.8236(3) 0.8091(3) 0.1917(3) 0.0452(10) Uani 1 1 d . . . H13 H 0.8826 0.7930 0.2169 0.054 Uiso 1 1 calc R . . C14 C 0.8294(3) 0.8734(3) 0.1421(3) 0.0448(10) Uani 1 1 d . . . C15 C 0.9276(3) 0.9163(4) 0.1275(4) 0.0547(12) Uani 1 1 d . . . C16 C 0.9722(4) 0.8444(4) 0.0637(4) 0.0647(14) Uani 1 1 d . . . H16A H 0.9283 0.8281 0.0121 0.050 Uiso 1 1 calc R . . H16B H 0.9818 0.7882 0.0842 0.050 Uiso 1 1 calc R . . H16C H 1.0351 0.8708 0.0537 0.050 Uiso 1 1 calc R . . C17 C 0.9153(4) 1.0033(4) 0.0927(5) 0.0788(19) Uani 1 1 d . . . H17A H 0.8714 0.9864 0.0412 0.050 Uiso 1 1 calc R . . H17B H 0.9789 1.0274 0.0821 0.050 Uiso 1 1 calc R . . H17C H 0.8877 1.0516 0.1327 0.050 Uiso 1 1 calc R . . C18 C 0.9951(4) 0.9433(5) 0.2073(4) 0.0766(18) Uani 1 1 d . . . H18A H 1.0574 0.9710 0.1974 0.050 Uiso 1 1 calc R . . H18B H 1.0062 0.8876 0.2281 0.050 Uiso 1 1 calc R . . H18C H 0.9653 0.9889 0.2480 0.050 Uiso 1 1 calc R . . C19 C 0.7420(3) 0.8924(3) 0.1047(3) 0.0441(10) Uani 1 1 d . . . H19 H 0.7430 0.9329 0.0682 0.053 Uiso 1 1 calc R . . C20 C 0.6512(3) 0.8542(3) 0.1184(3) 0.0379(9) Uani 1 1 d . . . C21 C 0.6482(3) 0.7934(3) 0.1711(3) 0.0363(9) Uani 1 1 d . . . O2 O 0.56333(19) 0.7580(2) 0.18713(18) 0.0381(6) Uani 1 1 d . . . C22 C 0.5663(3) 0.8750(3) 0.0699(3) 0.0387(9) Uani 1 1 d . . . H22 H 0.5783 0.9076 0.0289 0.046 Uiso 1 1 calc R . . N1 N 0.4771(3) 0.8543(2) 0.0764(2) 0.0410(8) Uani 1 1 d . B . C23 C 0.4043(3) 0.8764(4) 0.0148(3) 0.0527(12) Uani 1 1 d . . . H23A H 0.3694 0.8173 -0.0184 0.063 Uiso 1 1 calc R A 1 H23B H 0.4387 0.9058 -0.0228 0.063 Uiso 1 1 calc R A 1 C24 C 0.3314(3) 0.9401(4) 0.0515(4) 0.0575(13) Uani 0.80 1 d P B 1 H24 H 0.2890 0.9530 0.0043 0.069 Uiso 0.80 1 calc PR B 1 O3 O 0.3804(3) 1.0238(3) 0.0928(3) 0.0459(9) Uani 0.80 1 d P B 1 C24' C 0.3314(3) 0.9401(4) 0.0515(4) 0.0575(13) Uani 0.20 1 d P B 2 H24' H 0.3754 0.9839 0.0965 0.069 Uiso 0.20 1 calc PR B 2 O3' O 0.2825(14) 0.9987(15) 0.0246(13) 0.068(5) Uani 0.20 1 d P B 2 C25 C 0.2630(3) 0.8997(4) 0.1041(4) 0.0625(15) Uani 1 1 d . . . H25A H 0.2117 0.9432 0.1180 0.075 Uiso 1 1 calc R B 1 H25B H 0.2306 0.8395 0.0707 0.075 Uiso 1 1 calc R B 1 N2 N 0.3124(3) 0.8843(3) 0.1807(3) 0.0542(11) Uani 1 1 d . B . C26 C 0.2831(6) 0.9242(4) 0.2484(5) 0.089(2) Uani 1 1 d . . . H26 H 0.2363 0.9686 0.2458 0.107 Uiso 1 1 calc R B 1 C27 C 0.3131(7) 0.9094(4) 0.3298(5) 0.103(3) Uani 0.60 1 d P B 1 C28 C 0.2945(6) 0.9714(5) 0.4066(6) 0.056(2) Uani 0.60 1 d P B 1 H28 H 0.2658 1.0275 0.4024 0.067 Uiso 0.60 1 calc PR B 1 C29 C 0.3139(6) 0.9580(6) 0.4849(6) 0.058(2) Uani 0.60 1 d P B 1 C30 C 0.2823(8) 1.0215(7) 0.5627(7) 0.079(3) Uani 0.60 1 d P B 1 C31 C 0.2226(9) 1.1029(7) 0.5398(7) 0.143(4) Uani 0.60 1 d P B 1 H31A H 0.1682 1.0757 0.4977 0.050 Uiso 0.60 1 calc PR B 1 H31B H 0.2655 1.1444 0.5185 0.050 Uiso 0.60 1 calc PR B 1 H31C H 0.1974 1.1388 0.5891 0.050 Uiso 0.60 1 calc PR B 1 C32 C 0.1993(10) 0.9658(7) 0.5975(7) 0.155(5) Uani 0.60 1 d P B 1 H32A H 0.1441 0.9447 0.5546 0.050 Uiso 0.60 1 calc PR B 1 H32B H 0.1772 1.0072 0.6457 0.050 Uiso 0.60 1 calc PR B 1 H32C H 0.2260 0.9115 0.6134 0.050 Uiso 0.60 1 calc PR B 1 C33 C 0.3805(11) 1.0565(10) 0.6305(9) 0.131(6) Uani 0.60 1 d PU B 1 H33A H 0.3615 1.0936 0.6821 0.050 Uiso 0.60 1 calc PR B 1 H33B H 0.4261 1.0947 0.6084 0.050 Uiso 0.60 1 calc PR B 1 H33C H 0.4120 1.0018 0.6410 0.050 Uiso 0.60 1 calc PR B 1 C34 C 0.3648(6) 0.8816(6) 0.4926(5) 0.054(2) Uani 0.60 1 d P B 1 H34 H 0.3854 0.8723 0.5455 0.065 Uiso 0.60 1 calc PR B 1 C35 C 0.3846(8) 0.8212(4) 0.4247(4) 0.106(3) Uani 0.60 1 d P B 1 C27' C 0.3131(7) 0.9094(4) 0.3298(5) 0.103(3) Uani 0.40 1 d P B 2 C28' C 0.2186(11) 0.9484(12) 0.3727(9) 0.071(4) Uani 0.40 1 d P B 2 H28' H 0.1698 0.9789 0.3476 0.085 Uiso 0.40 1 calc PR B 2 C29' C 0.2180(12) 0.9318(14) 0.4499(11) 0.085(5) Uani 0.40 1 d P B 2 C30' C 0.1552(16) 0.987(2) 0.5130(14) 0.123(9) Uani 0.40 1 d P B 2 C31' C 0.2226(9) 1.1029(7) 0.5398(7) 0.143(4) Uani 0.40 1 d P B 2 H31D H 0.2077 1.1349 0.4956 0.050 Uiso 0.40 1 calc PR B 2 H31E H 0.2927 1.0956 0.5466 0.050 Uiso 0.40 1 calc PR B 2 H31F H 0.2033 1.1399 0.5914 0.050 Uiso 0.40 1 calc PR B 2 C32' C 0.1993(10) 0.9658(7) 0.5975(7) 0.155(5) Uani 0.40 1 d P B 2 H32D H 0.2693 0.9593 0.5969 0.050 Uiso 0.40 1 calc PR B 2 H32E H 0.1671 0.9076 0.6040 0.050 Uiso 0.40 1 calc PR B 2 H32F H 0.1885 1.0174 0.6435 0.050 Uiso 0.40 1 calc PR B 2 C33' C 0.0519(19) 0.988(2) 0.4651(18) 0.179(13) Uani 0.40 1 d PU B 2 H33D H 0.0590 1.0114 0.4160 0.050 Uiso 0.40 1 calc PR B 2 H33E H 0.0118 1.0282 0.5009 0.050 Uiso 0.40 1 calc PR B 2 H33F H 0.0205 0.9240 0.4486 0.050 Uiso 0.40 1 calc PR B 2 C34' C 0.2814(12) 0.8676(12) 0.4698(9) 0.073(4) Uani 0.40 1 d P B 2 H34' H 0.2667 0.8447 0.5159 0.088 Uiso 0.40 1 calc PR B 2 C35' C 0.3846(8) 0.8212(4) 0.4247(4) 0.106(3) Uani 0.40 1 d P B 2 C36 C 0.3693(6) 0.8383(4) 0.3448(4) 0.078(2) Uani 1 1 d . . . O4 O 0.4093(3) 0.7843(2) 0.28372(19) 0.0507(8) Uani 1 1 d . B . C37 C 0.4430(7) 0.7451(5) 0.4407(4) 0.100(3) Uani 1 1 d . . . H37A H 0.4731 0.7635 0.4987 0.120 Uiso 1 1 calc R B 1 H37B H 0.4965 0.7394 0.4053 0.120 Uiso 1 1 calc R B 1 C38 C 0.3895(5) 0.6503(4) 0.4266(3) 0.0637(14) Uani 1 1 d . B . C39 C 0.3667(4) 0.6166(4) 0.4933(3) 0.0675(15) Uani 1 1 d D . . H39 H 0.3856 0.6548 0.5471 0.081 Uiso 1 1 calc R B . C40 C 0.3178(4) 0.5297(4) 0.4857(3) 0.0633(14) Uani 1 1 d . B . C41 C 0.2973(5) 0.4954(5) 0.5623(4) 0.085(2) Uani 0.85 1 d PD B 1 C42 C 0.2358(7) 0.5629(7) 0.6145(5) 0.106(3) Uani 0.85 1 d PD B 1 H42A H 0.2229 0.5405 0.6633 0.050 Uiso 0.85 1 calc PR B 1 H42B H 0.1740 0.5668 0.5821 0.050 Uiso 0.85 1 calc PR B 1 H42C H 0.2710 0.6250 0.6319 0.050 Uiso 0.85 1 calc PR B 1 C43 C 0.2407(9) 0.4009(6) 0.5411(5) 0.118(4) Uani 0.85 1 d PD B 1 H43A H 0.2303 0.3819 0.5920 0.050 Uiso 0.85 1 calc PR B 1 H43B H 0.2775 0.3548 0.5072 0.050 Uiso 0.85 1 calc PR B 1 H43C H 0.1776 0.4046 0.5105 0.050 Uiso 0.85 1 calc PR B 1 C44 C 0.3949(7) 0.4904(9) 0.6122(6) 0.115(4) Uani 0.80 1 d PD B 1 H44A H 0.3832 0.4678 0.6611 0.050 Uiso 0.85 1 calc PR B 1 H44B H 0.4294 0.5527 0.6293 0.050 Uiso 0.85 1 calc PR B 1 H44C H 0.4346 0.4474 0.5782 0.050 Uiso 0.85 1 calc PR B 1 C41' C 0.2973(5) 0.4954(5) 0.5623(4) 0.085 Uani 0.15 1 d P B 2 C42' C 0.1877 0.4645 0.5540 0.050 Uiso 0.15 1 d P B 2 H42D H 0.1662 0.4297 0.4973 0.075 Uiso 0.15 1 d P C 2 H42E H 0.1507 0.5198 0.5678 0.075 Uiso 0.15 1 d P D 2 H42F H 0.1767 0.4244 0.5917 0.075 Uiso 0.15 1 d P E 2 C43' C 0.3490 0.4072 0.5563 0.050 Uiso 0.15 1 d P B 2 H43D H 0.3353 0.3676 0.5003 0.075 Uiso 0.15 1 d P F 2 H43E H 0.3262 0.3734 0.5955 0.075 Uiso 0.15 1 d P G 2 H43F H 0.4193 0.4235 0.5693 0.075 Uiso 0.15 1 d P H 2 C44' C 0.3224 0.5629 0.6451 0.050 Uiso 0.15 1 d PD B 2 H44D H 0.3039 0.5333 0.6884 0.075 Uiso 0.15 1 d P I 2 H44E H 0.2873 0.6191 0.6467 0.075 Uiso 0.15 1 d P J 2 H44F H 0.3927 0.5801 0.6539 0.075 Uiso 0.15 1 d P K 2 C45 C 0.2910(4) 0.4767(4) 0.4063(3) 0.0619(14) Uani 1 1 d D . . H45 H 0.2560 0.4177 0.3988 0.074 Uiso 1 1 calc R B . C46 C 0.3135(4) 0.5068(3) 0.3357(3) 0.0514(11) Uani 1 1 d . B . C47 C 0.3648(4) 0.5931(3) 0.3471(3) 0.0500(11) Uani 1 1 d D . . O5 O 0.3929(3) 0.6207(2) 0.28188(18) 0.0479(7) Uani 1 1 d . B . C48 C 0.2736(4) 0.4470(3) 0.2552(3) 0.0499(11) Uani 1 1 d . . . H48 H 0.2286 0.3963 0.2558 0.060 Uiso 1 1 calc R B . N3 N 0.2931(2) 0.4560(2) 0.1836(2) 0.0386(8) Uani 1 1 d . B . C49 C 0.2393(3) 0.3914(3) 0.1112(3) 0.0444(10) Uani 1 1 d . . . H49A H 0.2025 0.4281 0.0779 0.053 Uiso 1 1 calc R B . H49B H 0.1915 0.3510 0.1299 0.053 Uiso 1 1 calc R . . C50 C 0.3042(3) 0.3290(3) 0.0561(3) 0.0426(10) Uani 1 1 d . B . H50 H 0.2604 0.2867 0.0099 0.051 Uiso 1 1 calc R . . O6 O 0.3564(2) 0.2718(2) 0.0993(2) 0.0514(8) Uani 1 1 d . . . C51 C 0.3773(3) 0.3814(3) 0.0182(3) 0.0408(9) Uani 1 1 d . . . H51A H 0.4089 0.3359 -0.0223 0.049 Uiso 1 1 calc R B . H51B H 0.3426 0.4226 -0.0117 0.049 Uiso 1 1 calc R . . N4 N 0.4530(2) 0.4383(2) 0.08046(19) 0.0343(7) Uani 1 1 d . B . C52 C 0.5390(3) 0.4102(3) 0.0810(2) 0.0347(8) Uani 1 1 d . . . H52 H 0.5458 0.3509 0.0457 0.042 Uiso 1 1 calc R B . O61 O 0.1394(7) 1.2700(5) 0.2953(6) 0.078(3) Uani 0.25 1 d PD L 1 C62 C 0.0579(13) 1.2317(15) 0.3158(12) 0.047(5) Uani 0.25 1 d PD L 1 H62A H 0.0188 1.2804 0.3451 0.050 Uiso 0.25 1 calc PR L 1 H62B H 0.0173 1.1932 0.2665 0.050 Uiso 0.25 1 calc PR L 1 C63 C 0.091(2) 1.180(2) 0.3642(18) 0.077(7) Uiso 0.25 1 d PD L 1 H63A H 0.0365 1.1507 0.3845 0.050 Uiso 0.25 1 calc PR L 1 H63B H 0.1339 1.2192 0.4109 0.050 Uiso 0.25 1 calc PR L 1 H63C H 0.1281 1.1314 0.3334 0.050 Uiso 0.25 1 calc PR L 1 O61' O 0.1394(7) 1.2700(5) 0.2953(6) 0.078(3) Uani 0.25 1 d PD M 2 C62' C 0.104(3) 1.214(3) 0.340(2) 0.32(7) Uani 0.25 1 d PD M 2 H62C H 0.1225 1.1496 0.3224 0.050 Uiso 0.25 1 calc PR M 2 H62D H 0.1256 1.2387 0.3999 0.050 Uiso 0.25 1 calc PR M 2 C63' C 0.009(2) 1.219(3) 0.324(2) 0.097(10) Uiso 0.25 1 d PD M 2 H63D H -0.0260 1.1849 0.3566 0.050 Uiso 0.25 1 calc PR M 2 H63E H -0.0103 1.1919 0.2651 0.050 Uiso 0.25 1 calc PR M 2 H63F H -0.0057 1.2850 0.3373 0.050 Uiso 0.25 1 calc PR M 2 C71 C 0.1170(9) 0.6857(9) 0.2002(11) 0.100(5) Uani 0.50 1 d PDU . . H71A H 0.1810 0.6881 0.1801 0.050 Uiso 0.50 1 calc PR . . H71B H 0.0825 0.7394 0.1914 0.050 Uiso 0.50 1 calc PR . . H71C H 0.0791 0.6277 0.1703 0.050 Uiso 0.50 1 calc PR . . C72 C 0.1278(9) 0.6880(12) 0.2745(11) 0.114(5) Uani 0.50 1 d PDU . . H72A H 0.1679 0.7462 0.3031 0.050 Uiso 0.50 1 calc PR . . H72B H 0.1656 0.6349 0.2821 0.050 Uiso 0.50 1 calc PR . . O71 O 0.0422(9) 0.6843(9) 0.3144(6) 0.113(3) Uani 0.50 1 d PDU . . C73 C 0.026(2) 0.697(2) 0.4016(11) 0.221(14) Uani 0.50 1 d PDU . . H73A H 0.0609 0.7575 0.4325 0.050 Uiso 0.50 1 calc PR . . H73B H -0.0445 0.7042 0.4050 0.050 Uiso 0.50 1 calc PR . . C74 C 0.050(2) 0.637(2) 0.4378(14) 0.26(2) Uani 0.50 1 d PDU . . H74A H 0.0324 0.6547 0.4943 0.050 Uiso 0.50 1 calc PR . . H74B H 0.1201 0.6325 0.4391 0.050 Uiso 0.50 1 calc PR . . H74C H 0.0153 0.5771 0.4089 0.050 Uiso 0.50 1 calc PR . . C81 C 0.5932(13) 0.7524(16) 0.6701(12) 0.175(13) Uani 0.50 1 d PDU . . H81A H 0.6615 0.7605 0.6605 0.050 Uiso 0.50 1 calc PR . . H81B H 0.5558 0.7130 0.6204 0.050 Uiso 0.50 1 calc PR . . H81C H 0.5891 0.7225 0.7161 0.050 Uiso 0.50 1 calc PR . . C82 C 0.5607(12) 0.8267(15) 0.6863(13) 0.142(8) Uani 0.50 1 d PDU . . H82A H 0.5690 0.8584 0.6413 0.050 Uiso 0.50 1 calc PR . . H82B H 0.5977 0.8656 0.7374 0.050 Uiso 0.50 1 calc PR . . O81 O 0.4582(9) 0.8192(10) 0.6977(7) 0.120(4) Uani 0.50 1 d PDU . . C83 C 0.4175(11) 0.836(2) 0.7756(9) 0.204(15) Uani 0.50 1 d PDU . . H83A H 0.4354 0.7852 0.8021 0.050 Uiso 0.50 1 calc PR . . H83B H 0.4513 0.8948 0.8109 0.050 Uiso 0.50 1 calc PR . . C84 C 0.3289(11) 0.8431(15) 0.7781(9) 0.124(7) Uani 0.50 1 d PDU . . H84A H 0.3122 0.8393 0.8326 0.050 Uiso 0.50 1 calc PR . . H84B H 0.2927 0.7921 0.7359 0.050 Uiso 0.50 1 calc PR . . H84C H 0.3119 0.9032 0.7676 0.050 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0328(5) 0.0404(6) 0.0321(6) 0.0099(4) 0.0116(4) 0.0009(4) Zn1' 0.040(4) 0.068(8) 0.045(6) -0.001(4) 0.015(4) -0.009(5) Zn2 0.0283(6) 0.0414(11) 0.0383(7) 0.0167(8) 0.0108(4) 0.0059(8) Zn2' 0.0341(13) 0.060(2) 0.069(2) 0.0331(19) 0.0213(13) 0.0136(17) O2W 0.055(5) 0.060(5) 0.074(6) 0.020(5) 0.010(4) 0.002(4) Cl1 0.0364(5) 0.0489(6) 0.0386(5) 0.0168(4) 0.0073(4) 0.0027(4) Cl2 0.0606(8) 0.0593(7) 0.0807(9) 0.0220(7) 0.0228(7) -0.0024(6) O1 0.0318(14) 0.0393(15) 0.0449(16) 0.0162(12) 0.0073(12) 0.0043(11) C1 0.033(2) 0.043(2) 0.035(2) 0.0205(17) 0.0101(16) 0.0057(16) C2 0.036(2) 0.042(2) 0.0336(19) 0.0184(17) 0.0116(16) 0.0035(16) C3 0.040(2) 0.045(2) 0.040(2) 0.0197(18) 0.0141(17) 0.0081(18) C4 0.036(2) 0.054(3) 0.046(2) 0.026(2) 0.0125(18) 0.0078(18) C5 0.037(2) 0.071(3) 0.063(3) 0.026(3) 0.018(2) 0.016(2) C6 0.055(3) 0.097(5) 0.085(4) 0.023(4) -0.001(3) 0.033(3) C7 0.048(3) 0.083(5) 0.179(9) 0.008(5) 0.021(4) 0.027(3) C8 0.074(4) 0.181(9) 0.106(6) 0.081(6) 0.055(4) 0.062(5) C9 0.031(2) 0.057(3) 0.050(2) 0.029(2) 0.0036(18) 0.0000(18) C10 0.035(2) 0.046(2) 0.041(2) 0.0214(18) 0.0035(17) 0.0018(17) C11 0.036(2) 0.050(2) 0.047(2) 0.018(2) -0.0021(18) 0.0000(18) C12 0.036(2) 0.039(2) 0.048(2) 0.0104(18) 0.0087(18) 0.0028(17) C13 0.030(2) 0.041(2) 0.063(3) 0.008(2) 0.0048(19) 0.0031(17) C14 0.035(2) 0.035(2) 0.065(3) 0.010(2) 0.017(2) 0.0015(17) C15 0.031(2) 0.054(3) 0.079(3) 0.015(2) 0.016(2) -0.0022(19) C16 0.037(3) 0.081(4) 0.079(4) 0.020(3) 0.018(2) 0.003(2) C17 0.052(3) 0.065(3) 0.129(6) 0.038(4) 0.031(3) -0.009(3) C18 0.054(3) 0.084(4) 0.083(4) 0.006(3) 0.017(3) -0.027(3) C19 0.037(2) 0.037(2) 0.063(3) 0.014(2) 0.020(2) 0.0035(17) C20 0.036(2) 0.0314(19) 0.050(2) 0.0123(17) 0.0158(18) 0.0052(16) C21 0.031(2) 0.035(2) 0.046(2) 0.0101(17) 0.0118(17) 0.0034(16) O2 0.0282(13) 0.0435(15) 0.0495(16) 0.0211(13) 0.0123(12) 0.0043(11) C22 0.036(2) 0.033(2) 0.052(2) 0.0170(18) 0.0135(18) 0.0030(16) N1 0.0361(18) 0.0419(19) 0.051(2) 0.0202(16) 0.0112(15) 0.0074(15) C23 0.044(2) 0.058(3) 0.066(3) 0.035(2) 0.001(2) 0.002(2) C24 0.036(2) 0.057(3) 0.093(4) 0.044(3) 0.006(2) 0.003(2) O3 0.0361(19) 0.0379(19) 0.070(3) 0.0217(18) 0.0142(17) 0.0018(15) C24' 0.036(2) 0.057(3) 0.093(4) 0.044(3) 0.006(2) 0.003(2) O3' 0.059(11) 0.091(14) 0.077(13) 0.060(11) 0.013(9) 0.006(10) C25 0.031(2) 0.056(3) 0.115(5) 0.046(3) 0.015(3) 0.009(2) N2 0.042(2) 0.040(2) 0.092(3) 0.028(2) 0.033(2) 0.0051(16) C26 0.112(5) 0.041(3) 0.139(6) 0.037(3) 0.085(5) 0.029(3) C27 0.176(8) 0.042(3) 0.109(6) 0.018(3) 0.098(6) 0.029(4) C28 0.046(5) 0.039(4) 0.078(6) -0.006(4) 0.030(4) -0.004(3) C29 0.058(5) 0.044(4) 0.065(5) -0.011(4) 0.036(4) -0.011(4) C30 0.082(7) 0.061(6) 0.086(7) -0.016(5) 0.056(6) -0.004(5) C31 0.190(11) 0.100(7) 0.127(8) -0.025(6) 0.064(8) 0.048(7) C32 0.235(14) 0.114(7) 0.121(8) -0.006(6) 0.116(9) 0.030(8) C33 0.144(10) 0.096(8) 0.118(9) -0.058(7) 0.066(8) -0.023(7) C34 0.057(5) 0.053(5) 0.045(4) -0.006(3) 0.027(4) -0.014(4) C35 0.219(10) 0.044(3) 0.061(4) 0.003(3) 0.069(5) -0.001(4) C27' 0.176(8) 0.042(3) 0.109(6) 0.018(3) 0.098(6) 0.029(4) C28' 0.053(8) 0.086(10) 0.059(8) -0.015(7) 0.004(6) 0.023(7) C29' 0.068(10) 0.100(12) 0.075(11) -0.010(9) 0.021(8) 0.020(9) C30' 0.084(14) 0.18(3) 0.088(14) -0.004(15) 0.026(11) 0.031(15) C31' 0.190(11) 0.100(7) 0.127(8) -0.025(6) 0.064(8) 0.048(7) C32' 0.235(14) 0.114(7) 0.121(8) -0.006(6) 0.116(9) 0.030(8) C33' 0.161(17) 0.200(18) 0.168(17) 0.022(13) 0.022(13) 0.027(14) C34' 0.067(10) 0.089(11) 0.054(8) -0.002(7) 0.013(7) 0.001(8) C35' 0.219(10) 0.044(3) 0.061(4) 0.003(3) 0.069(5) -0.001(4) C36 0.134(6) 0.041(3) 0.065(3) 0.005(2) 0.052(4) 0.003(3) O4 0.066(2) 0.0462(17) 0.0427(17) 0.0096(14) 0.0239(15) 0.0051(15) C37 0.180(8) 0.076(4) 0.034(3) 0.004(3) 0.013(4) -0.036(5) C38 0.093(4) 0.061(3) 0.044(3) 0.018(2) 0.025(3) 0.005(3) C39 0.083(4) 0.080(4) 0.046(3) 0.021(3) 0.024(3) 0.013(3) C40 0.068(3) 0.080(4) 0.055(3) 0.033(3) 0.024(3) 0.012(3) C41 0.096(6) 0.114(6) 0.064(4) 0.052(4) 0.029(4) 0.019(5) C42 0.123(8) 0.152(9) 0.072(5) 0.060(6) 0.062(5) 0.030(7) C43 0.199(12) 0.101(7) 0.073(5) 0.055(5) 0.046(6) -0.017(7) C44 0.107(7) 0.182(11) 0.098(7) 0.103(8) 0.033(6) 0.043(7) C41' 0.096 0.114 0.064 0.052 0.029 0.019 C45 0.070(3) 0.068(3) 0.064(3) 0.035(3) 0.030(3) 0.014(3) C46 0.065(3) 0.049(3) 0.049(3) 0.021(2) 0.026(2) 0.009(2) C47 0.069(3) 0.049(3) 0.040(2) 0.018(2) 0.023(2) 0.010(2) O5 0.067(2) 0.0483(17) 0.0317(15) 0.0115(13) 0.0184(14) -0.0015(15) C48 0.059(3) 0.041(2) 0.060(3) 0.024(2) 0.028(2) 0.007(2) N3 0.0371(18) 0.0382(18) 0.0459(19) 0.0142(15) 0.0174(15) 0.0086(14) C49 0.030(2) 0.041(2) 0.064(3) 0.016(2) 0.0095(19) 0.0002(17) C50 0.034(2) 0.039(2) 0.054(3) 0.0101(19) 0.0038(18) 0.0018(17) O6 0.0500(18) 0.0442(17) 0.067(2) 0.0211(15) 0.0181(16) 0.0118(14) C51 0.040(2) 0.048(2) 0.034(2) 0.0096(18) 0.0032(17) 0.0026(18) N4 0.0357(18) 0.0389(17) 0.0297(16) 0.0103(13) 0.0092(13) -0.0031(14) C52 0.036(2) 0.038(2) 0.035(2) 0.0148(16) 0.0140(16) 0.0034(16) O61 0.089(6) 0.045(4) 0.096(6) -0.003(4) 0.050(5) -0.012(4) C62 0.025(8) 0.067(12) 0.054(12) 0.018(10) 0.031(8) -0.006(8) O61' 0.089(6) 0.045(4) 0.096(6) -0.003(4) 0.050(5) -0.012(4) C62' 0.61(19) 0.21(7) 0.07(3) 0.02(3) -0.14(6) -0.22(9) C71 0.060(8) 0.061(7) 0.214(14) 0.068(10) 0.093(10) 0.018(6) C72 0.048(6) 0.095(11) 0.213(15) 0.086(13) -0.027(7) -0.010(7) O71 0.109(8) 0.128(9) 0.092(6) 0.009(7) 0.003(6) -0.005(7) C73 0.20(2) 0.35(4) 0.098(11) 0.07(2) -0.045(12) -0.07(3) C74 0.26(4) 0.45(5) 0.078(14) 0.08(2) 0.003(18) 0.13(4) C81 0.123(14) 0.24(2) 0.113(14) -0.039(15) -0.086(12) 0.083(16) C82 0.116(11) 0.173(18) 0.094(12) -0.039(13) -0.014(9) -0.003(13) O81 0.135(9) 0.148(11) 0.084(7) 0.023(7) 0.048(7) 0.027(8) C83 0.105(9) 0.45(4) 0.062(8) 0.118(16) -0.023(7) -0.103(17) C84 0.109(10) 0.20(2) 0.060(8) 0.039(10) 0.013(7) -0.066(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 2.039(4) . ? Zn1 N4 2.053(4) . ? Zn1 N3 2.084(4) . ? Zn1 O1 2.084(4) . ? Zn1 Cl1 2.3035(18) . ? Zn1' N3 1.933(17) . ? Zn1' N4 1.990(18) . ? Zn1' O5 2.010(18) . ? Zn1' O1 2.092(17) . ? Zn1' O1W 2.29(3) . ? Zn1' Cl1 2.723(10) . ? Zn2 O2 2.022(4) . ? Zn2 O4 2.029(4) . ? Zn2 N1 2.099(5) . ? Zn2 N2 2.104(5) . ? Zn2 Cl1 2.311(2) . ? Zn2' N2 1.936(6) . ? Zn2' N1 2.012(6) . ? Zn2' O4 2.038(6) . ? Zn2' O2 2.098(6) . ? Zn2' O2W 2.184(10) . ? Zn2' Cl1 2.752(4) . ? O1 C1 1.356(5) . ? C1 C2 1.398(6) . ? C1 C10 1.406(6) . ? C2 C3 1.408(6) . ? C2 C52 1.452(6) . ? C3 C4 1.383(6) . ? C4 C9 1.400(7) . ? C4 C5 1.532(6) . ? C5 C6 1.507(8) . ? C5 C7 1.513(9) . ? C5 C8 1.537(8) . ? C9 C10 1.387(6) . ? C10 C11 1.528(6) . ? C11 C12 1.517(6) . ? C12 C13 1.386(6) . ? C12 C21 1.409(6) . ? C13 C14 1.404(7) . ? C14 C19 1.381(7) . ? C14 C15 1.535(6) . ? C15 C18 1.514(8) . ? C15 C16 1.524(8) . ? C15 C17 1.540(8) . ? C19 C20 1.412(6) . ? C20 C21 1.403(6) . ? C20 C22 1.451(6) . ? C21 O2 1.336(5) . ? C22 N1 1.277(5) . ? N1 C23 1.475(6) . ? C23 C24 1.494(7) . ? C24 O3 1.374(7) . ? C24 C25 1.543(7) . ? C25 N2 1.468(7) . ? N2 C26 1.269(8) . ? C26 C27 1.459(12) . ? C27 C36 1.393(10) . ? C27 C28 1.452(10) . ? C28 C29 1.378(14) . ? C29 C34 1.383(13) . ? C29 C30 1.538(11) . ? C30 C31 1.590(16) . ? C30 C32 1.610(14) . ? C30 C33 1.66(2) . ? C34 C35 1.336(10) . ? C35 C36 1.419(10) . ? C35 C37 1.477(12) . ? C28' C29' 1.38(3) . ? C29' C34' 1.40(2) . ? C29' C30' 1.55(2) . ? C30' C33' 1.57(3) . ? C36 O4 1.332(6) . ? C37 C38 1.504(9) . ? C38 C39 1.385(7) . ? C38 C47 1.403(7) . ? C39 C40 1.391(9) . ? C40 C45 1.383(8) . ? C40 C41 1.533(7) . ? C41 C43 1.511(10) . ? C41 C42 1.522(9) . ? C41 C44 1.533(10) . ? C45 C46 1.415(7) . ? C46 C47 1.388(7) . ? C46 C48 1.469(7) . ? C47 O5 1.339(5) . ? C48 N3 1.294(6) . ? N3 C49 1.466(6) . ? C49 C50 1.538(6) . ? C50 O6 1.416(5) . ? C50 C51 1.518(6) . ? C51 N4 1.476(5) . ? N4 C52 1.281(5) . ? O61 C62 1.346(16) . ? C62 C63 1.31(3) . ? C62' C63' 1.32(4) . ? C71 C72 1.234(17) . ? C72 O71 1.422(14) . ? O71 C73 1.474(16) . ? C73 C74 1.227(19) . ? C81 C82 1.190(18) . ? C82 O81 1.452(15) . ? O81 C83 1.450(14) . ? C83 C84 1.239(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 N4 154.51(16) . . ? O5 Zn1 N3 85.67(16) . . ? N4 Zn1 N3 90.12(16) . . ? O5 Zn1 O1 85.05(16) . . ? N4 Zn1 O1 85.59(16) . . ? N3 Zn1 O1 148.64(15) . . ? O5 Zn1 Cl1 97.18(13) . . ? N4 Zn1 Cl1 107.80(13) . . ? N3 Zn1 Cl1 110.60(15) . . ? O1 Zn1 Cl1 100.26(12) . . ? N3 Zn1' N4 96.5(8) . . ? N3 Zn1' O5 90.6(7) . . ? N4 Zn1' O5 172.4(10) . . ? N3 Zn1' O1 170.8(7) . . ? N4 Zn1' O1 87.0(7) . . ? O5 Zn1' O1 85.6(7) . . ? N3 Zn1' O1W 82.6(9) . . ? N4 Zn1' O1W 90.7(10) . . ? O5 Zn1' O1W 87.7(10) . . ? O1 Zn1' O1W 88.9(10) . . ? N3 Zn1' Cl1 100.2(6) . . ? N4 Zn1' Cl1 95.5(5) . . ? O5 Zn1' Cl1 85.7(5) . . ? O1 Zn1' Cl1 87.8(4) . . ? O1W Zn1' Cl1 172.9(12) . . ? O2 Zn2 O4 87.17(17) . . ? O2 Zn2 N1 85.87(17) . . ? O4 Zn2 N1 156.02(18) . . ? O2 Zn2 N2 155.32(19) . . ? O4 Zn2 N2 85.81(19) . . ? N1 Zn2 N2 91.03(18) . . ? O2 Zn2 Cl1 101.36(13) . . ? O4 Zn2 Cl1 98.58(14) . . ? N1 Zn2 Cl1 105.28(16) . . ? N2 Zn2 Cl1 103.08(17) . . ? N2 Zn2' N1 98.8(3) . . ? N2 Zn2' O4 90.1(3) . . ? N1 Zn2' O4 171.1(3) . . ? N2 Zn2' O2 175.0(3) . . ? N1 Zn2' O2 86.1(2) . . ? O4 Zn2' O2 84.9(2) . . ? N2 Zn2' O2W 86.9(3) . . ? N1 Zn2' O2W 91.8(3) . . ? O4 Zn2' O2W 89.0(3) . . ? O2 Zn2' O2W 92.7(3) . . ? N2 Zn2' Cl1 93.5(2) . . ? N1 Zn2' Cl1 93.5(2) . . ? O4 Zn2' Cl1 85.55(16) . . ? O2 Zn2' Cl1 86.49(14) . . ? O2W Zn2' Cl1 174.6(4) . . ? Zn1 Cl1 Zn2 104.80(11) . . ? Zn1 Cl1 Zn1' 1.0(4) . . ? Zn2 Cl1 Zn1' 105.1(4) . . ? Zn1 Cl1 Zn2' 106.86(14) . . ? Zn2 Cl1 Zn2' 2.44(19) . . ? Zn1' Cl1 Zn2' 107.2(4) . . ? C1 O1 Zn1 130.2(3) . . ? C1 O1 Zn1' 122.9(5) . . ? Zn1 O1 Zn1' 11.6(3) . . ? O1 C1 C2 120.4(4) . . ? O1 C1 C10 120.1(4) . . ? C2 C1 C10 119.5(4) . . ? C1 C2 C3 118.9(4) . . ? C1 C2 C52 124.5(4) . . ? C3 C2 C52 116.2(4) . . ? C4 C3 C2 122.9(4) . . ? C3 C4 C9 116.2(4) . . ? C3 C4 C5 122.4(4) . . ? C9 C4 C5 121.4(4) . . ? C6 C5 C7 109.0(5) . . ? C6 C5 C4 111.3(4) . . ? C7 C5 C4 112.6(4) . . ? C6 C5 C8 109.0(6) . . ? C7 C5 C8 106.4(6) . . ? C4 C5 C8 108.3(4) . . ? C10 C9 C4 123.4(4) . . ? C9 C10 C1 118.9(4) . . ? C9 C10 C11 120.2(4) . . ? C1 C10 C11 120.8(4) . . ? C12 C11 C10 113.8(4) . . ? C13 C12 C21 119.0(4) . . ? C13 C12 C11 120.8(4) . . ? C21 C12 C11 120.1(4) . . ? C12 C13 C14 123.7(4) . . ? C19 C14 C13 116.1(4) . . ? C19 C14 C15 122.1(4) . . ? C13 C14 C15 121.8(4) . . ? C18 C15 C16 110.2(5) . . ? C18 C15 C14 110.1(4) . . ? C16 C15 C14 108.5(4) . . ? C18 C15 C17 109.1(5) . . ? C16 C15 C17 107.3(5) . . ? C14 C15 C17 111.7(4) . . ? C14 C19 C20 122.6(4) . . ? C21 C20 C19 119.6(4) . . ? C21 C20 C22 124.0(4) . . ? C19 C20 C22 116.1(4) . . ? O2 C21 C20 121.1(4) . . ? O2 C21 C12 120.1(4) . . ? C20 C21 C12 118.8(4) . . ? C21 O2 Zn2 131.4(3) . . ? C21 O2 Zn2' 122.7(3) . . ? Zn2 O2 Zn2' 12.47(13) . . ? N1 C22 C20 127.0(4) . . ? C22 N1 C23 116.4(4) . . ? C22 N1 Zn2' 122.2(3) . . ? C23 N1 Zn2' 119.5(3) . . ? C22 N1 Zn2 125.9(3) . . ? C23 N1 Zn2 117.7(3) . . ? Zn2' N1 Zn2 12.45(13) . . ? N1 C23 C24 113.8(4) . . ? O3 C24 C23 108.0(4) . . ? O3 C24 C25 113.1(5) . . ? C23 C24 C25 115.5(4) . . ? N2 C25 C24 114.0(4) . . ? C26 N2 C25 118.4(5) . . ? C26 N2 Zn2' 120.6(5) . . ? C25 N2 Zn2' 119.9(4) . . ? C26 N2 Zn2 125.5(5) . . ? C25 N2 Zn2 116.0(3) . . ? Zn2' N2 Zn2 12.00(14) . . ? N2 C26 C27 127.3(6) . . ? C36 C27 C28 110.8(8) . . ? C36 C27 C26 124.8(5) . . ? C28 C27 C26 124.2(7) . . ? C29 C28 C27 127.2(8) . . ? C28 C29 C34 116.9(7) . . ? C28 C29 C30 124.2(9) . . ? C34 C29 C30 118.9(9) . . ? C29 C30 C31 110.6(10) . . ? C29 C30 C32 109.6(7) . . ? C31 C30 C32 100.4(9) . . ? C29 C30 C33 108.0(8) . . ? C31 C30 C33 115.4(10) . . ? C32 C30 C33 112.7(11) . . ? C35 C34 C29 119.2(9) . . ? C34 C35 C36 123.0(8) . . ? C34 C35 C37 114.3(8) . . ? C36 C35 C37 121.5(6) . . ? C28' C29' C34' 116.6(14) . . ? C28' C29' C30' 121.2(18) . . ? C34' C29' C30' 122.1(18) . . ? C29' C30' C33' 106.5(19) . . ? O4 C36 C27 120.2(6) . . ? O4 C36 C35 118.6(6) . . ? C27 C36 C35 121.2(6) . . ? C36 O4 Zn2 132.5(4) . . ? C36 O4 Zn2' 122.5(3) . . ? Zn2 O4 Zn2' 12.82(12) . . ? C35 C37 C38 116.5(8) . . ? C39 C38 C47 118.6(5) . . ? C39 C38 C37 119.7(5) . . ? C47 C38 C37 121.6(4) . . ? C38 C39 C40 123.4(6) . . ? C45 C40 C39 116.3(5) . . ? C45 C40 C41 122.9(6) . . ? C39 C40 C41 120.8(6) . . ? C43 C41 C42 106.5(7) . . ? C43 C41 C40 112.7(6) . . ? C42 C41 C40 109.9(5) . . ? C43 C41 C44 109.6(7) . . ? C42 C41 C44 109.7(7) . . ? C40 C41 C44 108.4(5) . . ? C40 C45 C46 122.9(5) . . ? C47 C46 C45 118.3(5) . . ? C47 C46 C48 124.6(4) . . ? C45 C46 C48 116.9(5) . . ? O5 C47 C46 119.7(4) . . ? O5 C47 C38 119.9(4) . . ? C46 C47 C38 120.4(4) . . ? C47 O5 Zn1' 120.4(4) . . ? C47 O5 Zn1 130.6(3) . . ? Zn1' O5 Zn1 11.9(3) . . ? N3 C48 C46 126.9(4) . . ? C48 N3 C49 117.2(4) . . ? C48 N3 Zn1' 117.3(5) . . ? C49 N3 Zn1' 122.9(6) . . ? C48 N3 Zn1 124.0(3) . . ? C49 N3 Zn1 118.4(3) . . ? Zn1' N3 Zn1 11.3(4) . . ? N3 C49 C50 114.1(3) . . ? O6 C50 C51 107.6(3) . . ? O6 C50 C49 111.7(4) . . ? C51 C50 C49 114.7(4) . . ? N4 C51 C50 112.4(3) . . ? C52 N4 C51 116.8(3) . . ? C52 N4 Zn1' 120.6(5) . . ? C51 N4 Zn1' 119.6(6) . . ? C52 N4 Zn1 126.5(3) . . ? C51 N4 Zn1 116.3(3) . . ? Zn1' N4 Zn1 11.9(3) . . ? N4 C52 C2 127.3(4) . . ? C63 C62 O61 103.2(17) . . ? C71 C72 O71 117.4(12) . . ? C72 O71 C73 132.9(15) . . ? C74 C73 O71 119(2) . . ? C81 C82 O81 112.2(19) . . ? C83 O81 C82 126.6(14) . . ? C84 C83 O81 120.7(13) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.412 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.125 data_test_2 _database_code_depnum_ccdc_archive 'CCDC 249423' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H104 Cl2 Co2 N4 O21' _chemical_formula_weight 1454.27 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 27.9433(17) _cell_length_b 13.7494(8) _cell_length_c 18.8620(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7246.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4466 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.44 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.746807 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 67304 _diffrn_reflns_av_R_equivalents 0.0937 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6669 _reflns_number_gt 4477 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 crystals are isomorphous with the nickel analog. The pendant alcohol group of the macrocycle is disordered 75:25 over two positions. The cations lie on mirror planes, as do the perchlorate anions, one of which is disordered (modeled as 45:5 % over two sites on the mirror plane), and the uncoordinated ethanol solvate molecules. Hydrogen atoms bonded to oxygen atoms were located from difference maps and not further refined. The quality of the refinement is not improved by reducing the symmetry. ; _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^)+(0.1274P)^2^+43.0433P] 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 6669 _refine_ls_number_parameters 474 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1362 _refine_ls_R_factor_gt 0.0992 _refine_ls_wR_factor_ref 0.2786 _refine_ls_wR_factor_gt 0.2476 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.092 _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 Co1 Co 0.06986(3) 0.09682(6) 0.27338(4) 0.0225(3) Uani 1 1 d . . . O1 O 0.01786(13) 0.1629(3) 0.2180(2) 0.0241(9) Uani 1 1 d . . . C1 C -0.02306(19) 0.1207(4) 0.1957(3) 0.0235(13) Uani 1 1 d . . . C2 C -0.0467(2) 0.1571(5) 0.1357(3) 0.0288(14) Uani 1 1 d . . . C3 C -0.0873(2) 0.1111(5) 0.1124(4) 0.0349(16) Uani 1 1 d . . . H3 H -0.1035 0.1377 0.0727 0.042 Uiso 1 1 calc R . . C4 C -0.1059(2) 0.0282(5) 0.1432(4) 0.0384(17) Uani 1 1 d . . . C5 C -0.1517(3) -0.0208(6) 0.1130(5) 0.056(2) Uani 1 1 d . . . C6 C -0.1492(4) -0.0326(11) 0.0359(6) 0.125(6) Uani 1 1 d . . . H6A H -0.1213 -0.0722 0.0237 0.050 Uiso 1 1 calc R . . H6B H -0.1464 0.0314 0.0135 0.050 Uiso 1 1 calc R . . H6C H -0.1784 -0.0649 0.0191 0.050 Uiso 1 1 calc R . . C7 C -0.1951(3) 0.0399(7) 0.1342(6) 0.066(3) Uani 1 1 d . . . H7A H -0.1969 0.0438 0.1860 0.050 Uiso 1 1 calc R . . H7B H -0.2243 0.0093 0.1158 0.050 Uiso 1 1 calc R . . H7C H -0.1920 0.1055 0.1145 0.050 Uiso 1 1 calc R . . C8 C -0.1588(4) -0.1223(9) 0.1429(9) 0.145(7) Uani 1 1 d . . . H8A H -0.1604 -0.1189 0.1947 0.050 Uiso 1 1 calc R . . H8B H -0.1319 -0.1637 0.1288 0.050 Uiso 1 1 calc R . . H8C H -0.1887 -0.1497 0.1245 0.050 Uiso 1 1 calc R . . C9 C -0.0835(2) -0.0044(5) 0.2049(4) 0.0372(17) Uani 1 1 d . . . H9 H -0.0967 -0.0583 0.2297 0.045 Uiso 1 1 calc R . . C10 C -0.0419(2) 0.0403(4) 0.2314(3) 0.0289(14) Uani 1 1 d . . . C11 C -0.0289(3) 0.2500 0.0996(4) 0.032(2) Uani 1 2 d S . . H11A H 0.0065 0.2500 0.0995 0.039 Uiso 1 2 calc SR . . H11B H -0.0398 0.2500 0.0496 0.039 Uiso 1 2 calc SR . . C12 C -0.0240(2) 0.0047(5) 0.2995(4) 0.0314(15) Uani 1 1 d . . . H12 H -0.0437 -0.0399 0.3247 0.038 Uiso 1 1 calc R . . N1 N 0.01595(18) 0.0283(4) 0.3282(3) 0.0291(12) Uani 1 1 d . B . C13 C 0.0242(2) -0.0088(5) 0.4010(4) 0.0390(17) Uani 1 1 d . . . H13A H -0.0030 -0.0510 0.4146 0.047 Uiso 1 1 calc R A 1 H13B H 0.0249 0.0469 0.4343 0.047 Uiso 1 1 calc R A 1 C14 C 0.0703(3) -0.0659(5) 0.4082(4) 0.0401(17) Uani 0.75 1 d P B 1 H14 H 0.0705 -0.0933 0.4573 0.048 Uiso 0.75 1 calc PR B 1 O2 O 0.0701(2) -0.1444(4) 0.3623(4) 0.0408(15) Uani 0.75 1 d P B 1 C14' C 0.0703(3) -0.0659(5) 0.4082(4) 0.0401(17) Uani 0.25 1 d P B 2 H14' H 0.0704 -0.1123 0.3674 0.048 Uiso 0.25 1 calc PR B 2 O2' O 0.0714(8) -0.125(2) 0.4698(15) 0.083(10) Uani 0.25 1 d P B 2 C15 C 0.1153(2) -0.0075(5) 0.4006(4) 0.0374(16) Uani 1 1 d . . . H15A H 0.1138 0.0488 0.4333 0.045 Uiso 1 1 calc R B 1 H15B H 0.1428 -0.0482 0.4151 0.045 Uiso 1 1 calc R B 1 N2 N 0.12356(17) 0.0281(4) 0.3287(3) 0.0281(12) Uani 1 1 d . B . C16 C 0.1630(2) 0.0053(4) 0.2986(4) 0.0322(15) Uani 1 1 d . . . H16 H 0.1827 -0.0395 0.3235 0.039 Uiso 1 1 calc R B . C17 C 0.1813(2) 0.0393(4) 0.2311(3) 0.0286(14) Uani 1 1 d . B . C18 C 0.2224(2) -0.0058(5) 0.2034(4) 0.0378(16) Uani 1 1 d . . . H18 H 0.2345 -0.0615 0.2272 0.045 Uiso 1 1 calc R B . C19 C 0.2460(2) 0.0262(5) 0.1438(4) 0.0368(17) Uani 1 1 d . B . C20 C 0.2901(3) -0.0243(6) 0.1129(6) 0.060(3) Uani 1 1 d . . . C21 C 0.3004(4) -0.1219(8) 0.1485(8) 0.141(7) Uani 1 1 d . B . H21A H 0.2721 -0.1636 0.1451 0.050 Uiso 1 1 calc R . . H21B H 0.3084 -0.1111 0.1985 0.050 Uiso 1 1 calc R . . H21C H 0.3274 -0.1535 0.1247 0.050 Uiso 1 1 calc R . . C22 C 0.3335(3) 0.0404(8) 0.1180(6) 0.074(3) Uani 1 1 d . B . H22A H 0.3613 0.0068 0.0979 0.050 Uiso 1 1 calc R . . H22B H 0.3397 0.0558 0.1679 0.050 Uiso 1 1 calc R . . H22C H 0.3277 0.1007 0.0916 0.050 Uiso 1 1 calc R . . C23 C 0.2813(3) -0.0495(7) 0.0373(7) 0.090(4) Uani 1 1 d . B . H23A H 0.2539 -0.0937 0.0341 0.050 Uiso 1 1 calc R . . H23B H 0.3097 -0.0812 0.0176 0.050 Uiso 1 1 calc R . . H23C H 0.2744 0.0100 0.0105 0.050 Uiso 1 1 calc R . . C24 C 0.2278(2) 0.1102(4) 0.1112(3) 0.0273(13) Uani 1 1 d . . . H24 H 0.2438 0.1353 0.0707 0.033 Uiso 1 1 calc R B . C25 C 0.18732(19) 0.1582(4) 0.1355(3) 0.0205(12) Uani 1 1 d . B . C26 C 0.16273(19) 0.1199(4) 0.1947(3) 0.0209(12) Uani 1 1 d . . . O3 O 0.12207(13) 0.1628(3) 0.2172(2) 0.0228(9) Uani 1 1 d . B . C27 C 0.1700(3) 0.2500 0.0986(4) 0.0216(17) Uani 1 2 d S . . H27A H 0.1816 0.2500 0.0490 0.026 Uiso 1 2 calc SR B . H27B H 0.1346 0.2500 0.0974 0.026 Uiso 1 2 calc SR . . O4 O 0.0704(2) 0.2500 0.3337(3) 0.0370(16) Uani 1 2 d S . . Cl1 Cl 0.30126(9) 0.2500 0.92065(17) 0.0373(6) Uani 0.90 2 d SP . . O11 O 0.2759(3) 0.1657(6) 0.9286(6) 0.121(3) Uani 1 1 d . . . O12 O 0.3424(4) 0.2500 0.9670(9) 0.120(6) Uani 0.90 2 d SP . . O13 O 0.3268(8) 0.2500 0.8579(9) 0.184(9) Uani 1 2 d S . . Cl1' Cl 0.2886(16) 0.2500 0.878(3) 0.073(10) Uiso 0.10 2 d SP . . O12' O 0.270(7) 0.2500 0.823(11) 0.17(7) Uiso 0.10 2 d SP . . Cl2 Cl 0.06815(8) 0.2500 0.57613(13) 0.0388(6) Uani 1 2 d S . . O21 O 0.0813(4) 0.2500 0.6482(5) 0.114(5) Uani 1 2 d S . . O22 O 0.0175(3) 0.2500 0.5691(5) 0.067(3) Uani 1 2 d S . . O23 O 0.0862(3) 0.1659(7) 0.5433(5) 0.107(3) Uani 1 1 d . . . O30 O 0.06842(15) -0.0184(3) 0.1964(2) 0.0345(11) Uani 1 1 d D . . C31 C 0.0725(3) -0.0028(6) 0.1211(4) 0.0436(18) Uani 1 1 d D . . H31A H 0.1050 -0.0221 0.1057 0.052 Uiso 1 1 calc R . . H31B H 0.0688 0.0675 0.1113 0.052 Uiso 1 1 calc R . . C32 C 0.0374(3) -0.0566(8) 0.0792(5) 0.071(3) Uani 1 1 d D . . H32A H 0.0429 -0.1266 0.0849 0.107 Uiso 1 1 calc R . . H32B H 0.0406 -0.0389 0.0291 0.107 Uiso 1 1 calc R . . H32C H 0.0051 -0.0404 0.0956 0.107 Uiso 1 1 calc R . . O40 O -0.0071(3) 0.2500 0.4204(4) 0.064(2) Uani 1 2 d SD . . C41 C -0.0591(6) 0.2500 0.4121(13) 0.195(17) Uani 1 2 d SD . . H41A H -0.0717 0.1921 0.4371 0.050 Uiso 0.50 1 calc PR . . H41B H -0.0717 0.3079 0.4371 0.050 Uiso 0.50 1 calc PR . . C42 C -0.0779(9) 0.2500 0.3444(13) 0.215(19) Uani 1 2 d SD . . H42A H -0.1123 0.2362 0.3466 0.050 Uiso 0.50 1 calc PR . . H42B H -0.0619 0.1999 0.3159 0.050 Uiso 0.50 1 calc PR . . H42C H -0.0728 0.3139 0.3226 0.050 Uiso 0.50 1 calc PR . . C52 C -0.0318(10) -0.2500 0.1792(17) 0.181(13) Uani 1 2 d S . . H52A H -0.0608 -0.2810 0.1977 0.050 Uiso 0.50 1 calc PR . . H52B H -0.0204 -0.2862 0.1377 0.050 Uiso 0.50 1 calc PR . . H52C H -0.0390 -0.1829 0.1654 0.050 Uiso 0.50 1 calc PR . . C51 C 0.0002(6) -0.2500 0.2265(11) 0.090(5) Uani 1 2 d S . . H51A H 0.0104 -0.3181 0.2345 0.050 Uiso 0.50 1 calc PR . . H51B H -0.0143 -0.2264 0.2712 0.050 Uiso 0.50 1 calc PR . . O50 O 0.0384(7) -0.1978(11) 0.2136(14) 0.157(10) Uani 0.50 1 d P . . O60 O 0.1483(2) 0.2500 0.4193(4) 0.055(2) Uani 1 2 d S . . C61 C 0.1958(4) 0.2500 0.4088(7) 0.091(6) Uani 1 2 d S . . H61A H 0.2085 0.3077 0.4340 0.050 Uiso 0.50 1 calc PR . . H61B H 0.2085 0.1923 0.4340 0.050 Uiso 0.50 1 calc PR . . C62 C 0.2161(5) 0.2500 0.3447(7) 0.078(4) Uani 1 2 d S . . H62A H 0.2476 0.2811 0.3476 0.050 Uiso 0.50 1 calc PR . . H62B H 0.1959 0.2860 0.3114 0.050 Uiso 0.50 1 calc PR . . H62C H 0.2199 0.1829 0.3282 0.050 Uiso 0.50 1 calc PR . . C72 C 0.1567(6) -0.2500 0.1155(11) 0.105(6) Uani 1 2 d S . . H72A H 0.1816 -0.2058 0.0982 0.050 Uiso 0.50 1 calc PR . . H72B H 0.1254 -0.2282 0.0982 0.050 Uiso 0.50 1 calc PR . . H72C H 0.1630 -0.3159 0.0982 0.050 Uiso 0.50 1 calc PR . . C71 C 0.1566(5) -0.2500 0.1944(9) 0.076(4) Uani 1 2 d S . . H71A H 0.1888 -0.2702 0.2107 0.050 Uiso 0.50 1 calc PR . . H71B H 0.1516 -0.1823 0.2107 0.050 Uiso 0.50 1 calc PR . . O70 O 0.1212(5) -0.3119(8) 0.2297(7) 0.071(4) Uani 0.50 1 d P . . H1O H 0.0240 0.2500 0.2066 0.050 Uiso 1 2 d S . . H3O H 0.1210 0.2500 0.2048 0.050 Uiso 1 2 d S . . H4OA H 0.0938 0.2500 0.3619 0.050 Uiso 1 2 d S . . H4OB H 0.0464 0.2500 0.3607 0.050 Uiso 1 2 d S . . H30 H 0.0609 -0.0772 0.2012 0.050 Uiso 1 1 d . . . H40 H 0.0028 0.2500 0.4617 0.050 Uiso 1 2 d S . . H50 H 0.0698 -0.2374 0.2147 0.050 Uiso 0.50 1 d P . . H70 H 0.1400 -0.2944 0.2673 0.050 Uiso 0.50 1 d P . . H60 H 0.1380 0.2500 0.4686 0.050 Uiso 1 2 d S . . 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 Co1 0.0198(4) 0.0206(4) 0.0270(4) 0.0046(3) 0.0014(3) -0.0008(3) O1 0.020(2) 0.022(2) 0.030(2) -0.0008(18) -0.0033(17) -0.0039(16) C1 0.018(3) 0.026(3) 0.027(3) -0.012(2) 0.000(2) -0.002(2) C2 0.024(3) 0.034(4) 0.028(3) -0.012(3) 0.002(3) 0.000(3) C3 0.021(3) 0.045(4) 0.038(4) -0.017(3) -0.007(3) 0.003(3) C4 0.020(3) 0.043(4) 0.052(4) -0.023(4) -0.002(3) -0.004(3) C5 0.030(4) 0.052(5) 0.085(6) -0.029(5) -0.006(4) -0.011(4) C6 0.057(6) 0.199(15) 0.118(10) -0.113(11) -0.005(6) -0.036(8) C7 0.025(4) 0.078(6) 0.095(7) -0.015(6) 0.001(4) -0.007(4) C8 0.087(9) 0.085(9) 0.26(2) -0.007(11) -0.094(11) -0.045(7) C9 0.022(3) 0.032(4) 0.057(5) -0.013(3) 0.009(3) -0.006(3) C10 0.021(3) 0.026(3) 0.040(4) -0.006(3) 0.006(3) -0.003(3) C11 0.026(5) 0.053(6) 0.018(4) 0.000 -0.007(4) 0.000 C12 0.026(3) 0.024(3) 0.044(4) 0.000(3) 0.012(3) -0.002(3) N1 0.028(3) 0.031(3) 0.028(3) 0.004(2) 0.005(2) -0.002(2) C13 0.038(4) 0.047(4) 0.032(4) 0.011(3) 0.009(3) -0.004(3) C14 0.048(4) 0.036(4) 0.037(4) 0.019(3) 0.003(3) 0.001(3) O2 0.051(4) 0.025(3) 0.046(4) 0.004(3) 0.009(3) -0.002(3) C14' 0.048(4) 0.036(4) 0.037(4) 0.019(3) 0.003(3) 0.001(3) O2' 0.053(15) 0.12(2) 0.079(18) 0.067(18) 0.003(13) 0.014(15) C15 0.041(4) 0.035(4) 0.037(4) 0.011(3) -0.008(3) 0.007(3) N2 0.025(3) 0.023(3) 0.036(3) 0.009(2) 0.000(2) -0.002(2) C16 0.033(4) 0.023(3) 0.041(4) 0.010(3) -0.007(3) 0.006(3) C17 0.027(3) 0.018(3) 0.040(4) 0.004(3) -0.003(3) -0.001(2) C18 0.033(4) 0.023(3) 0.057(4) 0.011(3) 0.001(3) 0.010(3) C19 0.018(3) 0.025(3) 0.067(5) 0.006(3) 0.007(3) 0.007(3) C20 0.035(4) 0.048(5) 0.096(7) 0.021(5) 0.032(4) 0.017(4) C21 0.101(9) 0.095(9) 0.229(16) 0.101(10) 0.117(10) 0.083(8) C22 0.023(4) 0.086(7) 0.113(8) 0.017(6) 0.006(5) 0.011(4) C23 0.054(6) 0.057(6) 0.160(12) -0.041(7) 0.049(7) 0.004(5) C24 0.022(3) 0.028(3) 0.032(3) -0.003(3) 0.000(3) 0.000(3) C25 0.019(3) 0.017(3) 0.025(3) -0.001(2) -0.001(2) -0.002(2) C26 0.014(3) 0.015(3) 0.034(3) 0.000(2) -0.001(2) -0.002(2) O3 0.021(2) 0.016(2) 0.031(2) 0.0005(17) 0.0041(17) 0.0024(16) C27 0.019(4) 0.024(4) 0.022(4) 0.000 -0.002(3) 0.000 O4 0.021(3) 0.061(5) 0.030(3) 0.000 -0.001(3) 0.000 Cl1 0.0282(13) 0.0351(15) 0.0486(18) 0.000 0.0101(13) 0.000 O11 0.066(5) 0.081(5) 0.217(11) 0.017(6) 0.001(6) -0.037(4) O12 0.077(8) 0.080(8) 0.204(17) 0.000 -0.066(10) 0.000 O13 0.26(2) 0.147(14) 0.148(14) 0.000 0.152(16) 0.000 Cl2 0.0225(11) 0.0535(15) 0.0403(13) 0.000 0.0030(10) 0.000 O21 0.076(7) 0.230(16) 0.037(5) 0.000 0.004(5) 0.000 O22 0.023(4) 0.092(7) 0.086(6) 0.000 0.006(4) 0.000 O23 0.100(6) 0.113(7) 0.109(6) -0.023(5) -0.003(5) 0.064(5) O30 0.038(3) 0.024(2) 0.041(3) -0.007(2) 0.008(2) -0.006(2) C31 0.046(4) 0.050(5) 0.035(4) -0.007(3) 0.003(3) -0.006(4) C32 0.063(6) 0.083(7) 0.067(6) -0.029(6) 0.009(5) -0.011(5) O40 0.030(4) 0.111(7) 0.052(5) 0.000 -0.002(4) 0.000 C41 0.15(3) 0.33(5) 0.10(2) 0.000 0.032(19) 0.000 C42 0.29(4) 0.13(2) 0.23(4) 0.000 0.18(4) 0.000 C52 0.16(3) 0.12(2) 0.27(4) 0.000 0.04(3) 0.000 C51 0.058(10) 0.094(13) 0.118(15) 0.000 0.024(10) 0.000 O50 0.115(14) 0.064(10) 0.29(3) 0.081(14) -0.076(16) -0.057(10) O60 0.033(4) 0.098(7) 0.034(4) 0.000 -0.003(3) 0.000 C61 0.023(6) 0.194(19) 0.055(8) 0.000 -0.001(5) 0.000 C62 0.053(8) 0.127(14) 0.054(8) 0.000 -0.005(7) 0.000 C72 0.064(10) 0.108(14) 0.142(18) 0.000 -0.029(11) 0.000 C71 0.074(10) 0.048(8) 0.107(13) 0.000 -0.025(9) 0.000 O70 0.098(10) 0.037(6) 0.078(9) 0.001(6) 0.007(8) -0.008(6) _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 Co1 O1 2.007(4) . ? Co1 O3 2.019(4) . ? Co1 N1 2.056(5) . ? Co1 N2 2.058(5) . ? Co1 O30 2.149(4) . ? Co1 O4 2.394(3) . ? O1 C1 1.349(7) . ? C1 C10 1.398(9) . ? C1 C2 1.403(9) . ? C2 C3 1.370(9) . ? C2 C11 1.531(8) . ? C3 C4 1.382(10) . ? C4 C9 1.394(10) . ? C4 C5 1.555(9) . ? C5 C6 1.464(14) . ? C5 C8 1.518(15) . ? C5 C7 1.525(11) . ? C9 C10 1.407(9) . ? C10 C12 1.464(9) . ? C11 C2 1.531(8) 7_565 ? C12 N1 1.282(8) . ? N1 C13 1.482(8) . ? C13 C14 1.515(10) . ? C14 O2 1.384(10) . ? C14 C15 1.499(10) . ? C15 N2 1.459(8) . ? N2 C16 1.279(8) . ? C16 C17 1.449(9) . ? C17 C26 1.404(8) . ? C17 C18 1.404(9) . ? C18 C19 1.377(10) . ? C19 C24 1.405(9) . ? C19 C20 1.530(9) . ? C20 C23 1.487(15) . ? C20 C22 1.506(12) . ? C20 C21 1.527(12) . ? C24 C25 1.387(8) . ? C25 C26 1.414(8) . ? C25 C27 1.520(7) . ? C26 O3 1.348(6) . ? C27 C25 1.520(7) 7_565 ? O4 Co1 2.394(3) 7_565 ? Cl1 Cl1' 0.87(5) . ? Cl1 O11 1.367(7) 7_565 ? Cl1 O11 1.367(7) . ? Cl1 O13 1.382(13) . ? Cl1 O12 1.445(12) . ? Cl1 O12' 2.0(2) . ? O11 Cl1' 1.54(3) . ? O13 Cl1' 1.14(4) . ? O13 O12' 1.7(2) . ? Cl1' O12' 1.2(2) . ? Cl1' O11 1.54(3) 7_565 ? Cl2 O23 1.406(8) 7_565 ? Cl2 O23 1.406(8) . ? Cl2 O21 1.407(10) . ? Cl2 O22 1.420(7) . ? O30 C31 1.441(8) . ? C31 C32 1.461(11) . ? O40 C41 1.462(17) . ? C41 C42 1.382(19) . ? C52 C51 1.26(3) . ? C51 O50 1.308(19) . ? O60 C61 1.343(13) . ? C61 C62 1.335(17) . ? C72 C71 1.49(2) . ? C71 O70 1.466(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co1 O3 92.66(16) . . ? O1 Co1 N1 86.50(18) . . ? O3 Co1 N1 178.52(19) . . ? O1 Co1 N2 179.11(19) . . ? O3 Co1 N2 86.89(18) . . ? N1 Co1 N2 93.9(2) . . ? O1 Co1 O30 88.20(17) . . ? O3 Co1 O30 89.42(16) . . ? N1 Co1 O30 89.34(19) . . ? N2 Co1 O30 91.0(2) . . ? O1 Co1 O4 81.57(18) . . ? O3 Co1 O4 81.37(18) . . ? N1 Co1 O4 99.7(2) . . ? N2 Co1 O4 99.1(2) . . ? O30 Co1 O4 165.85(19) . . ? C1 O1 Co1 125.5(4) . . ? O1 C1 C10 120.7(5) . . ? O1 C1 C2 119.8(5) . . ? C10 C1 C2 119.5(5) . . ? C3 C2 C1 118.9(6) . . ? C3 C2 C11 120.7(6) . . ? C1 C2 C11 120.2(6) . . ? C2 C3 C4 123.9(7) . . ? C3 C4 C9 116.5(6) . . ? C3 C4 C5 120.9(7) . . ? C9 C4 C5 122.4(7) . . ? C6 C5 C8 105.9(10) . . ? C6 C5 C7 111.0(9) . . ? C8 C5 C7 107.5(9) . . ? C6 C5 C4 112.0(7) . . ? C8 C5 C4 111.7(8) . . ? C7 C5 C4 108.7(6) . . ? C4 C9 C10 121.8(7) . . ? C1 C10 C9 119.1(6) . . ? C1 C10 C12 123.9(5) . . ? C9 C10 C12 116.7(6) . . ? C2 C11 C2 113.1(7) 7_565 . ? N1 C12 C10 125.7(6) . . ? C12 N1 C13 116.0(5) . . ? C12 N1 Co1 122.8(4) . . ? C13 N1 Co1 120.7(4) . . ? N1 C13 C14 113.2(5) . . ? O2 C14 C15 111.1(6) . . ? O2 C14 C13 110.1(6) . . ? C15 C14 C13 115.3(6) . . ? N2 C15 C14 113.7(6) . . ? C16 N2 C15 117.8(5) . . ? C16 N2 Co1 121.0(4) . . ? C15 N2 Co1 120.7(4) . . ? N2 C16 C17 128.0(6) . . ? C26 C17 C18 117.9(6) . . ? C26 C17 C16 123.6(6) . . ? C18 C17 C16 118.2(6) . . ? C19 C18 C17 123.8(6) . . ? C18 C19 C24 116.5(6) . . ? C18 C19 C20 123.6(6) . . ? C24 C19 C20 119.9(6) . . ? C23 C20 C22 109.4(8) . . ? C23 C20 C21 104.4(10) . . ? C22 C20 C21 109.8(9) . . ? C23 C20 C19 109.7(7) . . ? C22 C20 C19 110.8(7) . . ? C21 C20 C19 112.5(7) . . ? C25 C24 C19 122.9(6) . . ? C24 C25 C26 118.7(5) . . ? C24 C25 C27 120.2(6) . . ? C26 C25 C27 121.1(5) . . ? O3 C26 C17 120.3(5) . . ? O3 C26 C25 119.7(5) . . ? C17 C26 C25 120.0(5) . . ? C26 O3 Co1 125.3(3) . . ? C25 C27 C25 112.2(6) 7_565 . ? Co1 O4 Co1 123.3(3) . 7_565 ? Cl1' Cl1 O11 83.6(16) . 7_565 ? Cl1' Cl1 O11 83.6(16) . . ? O11 Cl1 O11 116.0(8) 7_565 . ? Cl1' Cl1 O13 55(3) . . ? O11 Cl1 O13 111.2(6) 7_565 . ? O11 Cl1 O13 111.2(6) . . ? Cl1' Cl1 O12 151(3) . . ? O11 Cl1 O12 110.3(5) 7_565 . ? O11 Cl1 O12 110.3(5) . . ? O13 Cl1 O12 96.2(12) . . ? Cl1' Cl1 O12' 2(7) . . ? O11 Cl1 O12' 83(3) 7_565 . ? O11 Cl1 O12' 83(3) . . ? O13 Cl1 O12' 57(6) . . ? O12 Cl1 O12' 153(6) . . ? Cl1 O11 Cl1' 34.3(17) . . ? Cl1' O13 Cl1 39(3) . . ? Cl1' O13 O12' 42(7) . . ? Cl1 O13 O12' 81(7) . . ? Cl1 Cl1' O13 86(4) . . ? Cl1 Cl1' O12' 177(10) . . ? O13 Cl1' O12' 97(10) . . ? Cl1 Cl1' O11 62(2) . 7_565 ? O13 Cl1' O11 115(2) . 7_565 ? O12' Cl1' O11 116(6) . 7_565 ? Cl1 Cl1' O11 62(2) . . ? O13 Cl1' O11 115(2) . . ? O12' Cl1' O11 116(6) . . ? O11 Cl1' O11 98(3) 7_565 . ? Cl1' O12' O13 41(7) . . ? Cl1' O12' Cl1 1(5) . . ? O13 O12' Cl1 42(5) . . ? O23 Cl2 O23 110.7(8) 7_565 . ? O23 Cl2 O21 109.4(4) 7_565 . ? O23 Cl2 O21 109.4(4) . . ? O23 Cl2 O22 108.4(4) 7_565 . ? O23 Cl2 O22 108.4(4) . . ? O21 Cl2 O22 110.5(6) . . ? C31 O30 Co1 123.7(4) . . ? O30 C31 C32 113.8(7) . . ? C42 C41 O40 118(2) . . ? C52 C51 O50 116(2) . . ? C62 C61 O60 123.7(12) . . ? O70 C71 C72 117.0(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Co1 O1 C1 139.2(4) . . . . ? N1 Co1 O1 C1 -39.6(4) . . . . ? N2 Co1 O1 C1 80(12) . . . . ? O30 Co1 O1 C1 49.8(4) . . . . ? O4 Co1 O1 C1 -140.0(4) . . . . ? Co1 O1 C1 C10 25.5(7) . . . . ? Co1 O1 C1 C2 -153.8(4) . . . . ? O1 C1 C2 C3 177.6(5) . . . . ? C10 C1 C2 C3 -1.7(9) . . . . ? O1 C1 C2 C11 -5.7(8) . . . . ? C10 C1 C2 C11 175.0(6) . . . . ? C1 C2 C3 C4 -2.1(10) . . . . ? C11 C2 C3 C4 -178.7(6) . . . . ? C2 C3 C4 C9 5.2(10) . . . . ? C2 C3 C4 C5 -179.1(6) . . . . ? C3 C4 C5 C6 47.7(11) . . . . ? C9 C4 C5 C6 -136.8(10) . . . . ? C3 C4 C5 C8 166.2(9) . . . . ? C9 C4 C5 C8 -18.3(12) . . . . ? C3 C4 C5 C7 -75.4(10) . . . . ? C9 C4 C5 C7 100.1(9) . . . . ? C3 C4 C9 C10 -4.7(10) . . . . ? C5 C4 C9 C10 179.6(6) . . . . ? O1 C1 C10 C9 -177.3(5) . . . . ? C2 C1 C10 C9 2.1(9) . . . . ? O1 C1 C10 C12 9.2(9) . . . . ? C2 C1 C10 C12 -171.4(6) . . . . ? C4 C9 C10 C1 1.2(9) . . . . ? C4 C9 C10 C12 175.2(6) . . . . ? C3 C2 C11 C2 94.3(8) . . . 7_565 ? C1 C2 C11 C2 -82.3(9) . . . 7_565 ? C1 C10 C12 N1 -14.7(10) . . . . ? C9 C10 C12 N1 171.7(6) . . . . ? C10 C12 N1 C13 173.7(6) . . . . ? C10 C12 N1 Co1 -14.7(9) . . . . ? O1 Co1 N1 C12 33.2(5) . . . . ? O3 Co1 N1 C12 -22(8) . . . . ? N2 Co1 N1 C12 -146.0(5) . . . . ? O30 Co1 N1 C12 -55.0(5) . . . . ? O4 Co1 N1 C12 114.0(5) . . . . ? O1 Co1 N1 C13 -155.5(5) . . . . ? O3 Co1 N1 C13 149(7) . . . . ? N2 Co1 N1 C13 25.3(5) . . . . ? O30 Co1 N1 C13 116.3(5) . . . . ? O4 Co1 N1 C13 -74.7(5) . . . . ? C12 N1 C13 C14 125.1(6) . . . . ? Co1 N1 C13 C14 -46.8(8) . . . . ? N1 C13 C14 O2 -58.8(8) . . . . ? N1 C13 C14 C15 68.0(8) . . . . ? O2 C14 C15 N2 57.1(8) . . . . ? C13 C14 C15 N2 -69.1(8) . . . . ? C14 C15 N2 C16 -123.4(7) . . . . ? C14 C15 N2 Co1 48.5(7) . . . . ? O1 Co1 N2 C16 26(12) . . . . ? O3 Co1 N2 C16 -33.0(5) . . . . ? N1 Co1 N2 C16 145.8(5) . . . . ? O30 Co1 N2 C16 56.4(5) . . . . ? O4 Co1 N2 C16 -113.7(5) . . . . ? O1 Co1 N2 C15 -145(12) . . . . ? O3 Co1 N2 C15 155.3(5) . . . . ? N1 Co1 N2 C15 -25.9(5) . . . . ? O30 Co1 N2 C15 -115.3(5) . . . . ? O4 Co1 N2 C15 74.6(5) . . . . ? C15 N2 C16 C17 -173.4(6) . . . . ? Co1 N2 C16 C17 14.7(9) . . . . ? N2 C16 C17 C26 14.3(11) . . . . ? N2 C16 C17 C18 -171.2(7) . . . . ? C26 C17 C18 C19 1.8(10) . . . . ? C16 C17 C18 C19 -173.1(7) . . . . ? C17 C18 C19 C24 1.6(11) . . . . ? C17 C18 C19 C20 -178.6(7) . . . . ? C18 C19 C20 C23 124.3(9) . . . . ? C24 C19 C20 C23 -55.9(10) . . . . ? C18 C19 C20 C22 -114.8(9) . . . . ? C24 C19 C20 C22 65.0(11) . . . . ? C18 C19 C20 C21 8.6(14) . . . . ? C24 C19 C20 C21 -171.7(9) . . . . ? C18 C19 C24 C25 -1.8(10) . . . . ? C20 C19 C24 C25 178.4(7) . . . . ? C19 C24 C25 C26 -1.4(9) . . . . ? C19 C24 C25 C27 178.8(6) . . . . ? C18 C17 C26 O3 176.7(6) . . . . ? C16 C17 C26 O3 -8.7(9) . . . . ? C18 C17 C26 C25 -5.0(9) . . . . ? C16 C17 C26 C25 169.5(6) . . . . ? C24 C25 C26 O3 -176.9(5) . . . . ? C27 C25 C26 O3 3.0(8) . . . . ? C24 C25 C26 C17 4.8(8) . . . . ? C27 C25 C26 C17 -175.3(5) . . . . ? C17 C26 O3 Co1 -25.7(7) . . . . ? C25 C26 O3 Co1 156.0(4) . . . . ? O1 Co1 O3 C26 -139.3(4) . . . . ? N1 Co1 O3 C26 -84(7) . . . . ? N2 Co1 O3 C26 40.0(4) . . . . ? O30 Co1 O3 C26 -51.1(4) . . . . ? O4 Co1 O3 C26 139.7(4) . . . . ? C24 C25 C27 C25 -96.9(7) . . . 7_565 ? C26 C25 C27 C25 83.2(8) . . . 7_565 ? O1 Co1 O4 Co1 -46.5(3) . . . 7_565 ? O3 Co1 O4 Co1 47.5(3) . . . 7_565 ? N1 Co1 O4 Co1 -131.4(3) . . . 7_565 ? N2 Co1 O4 Co1 132.9(3) . . . 7_565 ? O30 Co1 O4 Co1 -2.4(9) . . . 7_565 ? O11 Cl1 O11 Cl1' 80(3) 7_565 . . . ? O13 Cl1 O11 Cl1' -49(3) . . . . ? O12 Cl1 O11 Cl1' -154(3) . . . . ? O12' Cl1 O11 Cl1' 1(6) . . . . ? O11 Cl1 O13 Cl1' -65.4(6) 7_565 . . . ? O11 Cl1 O13 Cl1' 65.4(6) . . . . ? O12 Cl1 O13 Cl1' 180.000(15) . . . . ? O12' Cl1 O13 Cl1' 0.000(16) . . . . ? Cl1' Cl1 O13 O12' 0.00(2) . . . . ? O11 Cl1 O13 O12' -65.4(6) 7_565 . . . ? O11 Cl1 O13 O12' 65.4(6) . . . . ? O12 Cl1 O13 O12' 180.00(2) . . . . ? O11 Cl1 Cl1' O13 121.4(5) 7_565 . . . ? O11 Cl1 Cl1' O13 -121.4(5) . . . . ? O12 Cl1 Cl1' O13 0.00(2) . . . . ? O12' Cl1 Cl1' O13 180.0(5) . . . . ? O11 Cl1 Cl1' O12' -58.6(10) 7_565 . . . ? O11 Cl1 Cl1' O12' 58.6(10) . . . . ? O13 Cl1 Cl1' O12' 180.0(8) . . . . ? O12 Cl1 Cl1' O12' 180.0(8) . . . . ? O11 Cl1 Cl1' O11 117.2(9) . . . 7_565 ? O13 Cl1 Cl1' O11 -121.4(5) . . . 7_565 ? O12 Cl1 Cl1' O11 -121.4(5) . . . 7_565 ? O12' Cl1 Cl1' O11 58.6(8) . . . 7_565 ? O11 Cl1 Cl1' O11 -117.2(9) 7_565 . . . ? O13 Cl1 Cl1' O11 121.4(5) . . . . ? O12 Cl1 Cl1' O11 121.4(5) . . . . ? O12' Cl1 Cl1' O11 -58.6(7) . . . . ? O12' O13 Cl1' Cl1 180.000(10) . . . . ? Cl1 O13 Cl1' O12' 180.00(3) . . . . ? Cl1 O13 Cl1' O11 57(3) . . . 7_565 ? O12' O13 Cl1' O11 -123(3) . . . 7_565 ? Cl1 O13 Cl1' O11 -57(3) . . . . ? O12' O13 Cl1' O11 123(3) . . . . ? Cl1 O11 Cl1' O13 70(4) . . . . ? Cl1 O11 Cl1' O12' -177(11) . . . . ? Cl1 O11 Cl1' O11 -52.6(18) . . . 7_565 ? Cl1 Cl1' O12' O13 180.0(8) . . . . ? O11 Cl1' O12' O13 123(5) 7_565 . . . ? O11 Cl1' O12' O13 -123(5) . . . . ? O13 Cl1' O12' Cl1 180.0(19) . . . . ? O11 Cl1' O12' Cl1 -57(6) 7_565 . . . ? O11 Cl1' O12' Cl1 57(7) . . . . ? Cl1 O13 O12' Cl1' 0.00(4) . . . . ? Cl1' O13 O12' Cl1 0.00(6) . . . . ? O11 Cl1 O12' Cl1' 121.3(17) 7_565 . . . ? O11 Cl1 O12' Cl1' -121.3(19) . . . . ? O13 Cl1 O12' Cl1' 0.0(13) . . . . ? O12 Cl1 O12' Cl1' 0.0(12) . . . . ? Cl1' Cl1 O12' O13 0.0(8) . . . . ? O11 Cl1 O12' O13 121.3(7) 7_565 . . . ? O11 Cl1 O12' O13 -121.3(8) . . . . ? O12 Cl1 O12' O13 0.000(16) . . . . ? O1 Co1 O30 C31 52.6(5) . . . . ? O3 Co1 O30 C31 -40.1(5) . . . . ? N1 Co1 O30 C31 139.1(5) . . . . ? N2 Co1 O30 C31 -127.0(5) . . . . ? O4 Co1 O30 C31 9.0(10) . . . . ? Co1 O30 C31 C32 -133.8(6) . . . . ? 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 O40 H40 O22 0.82 2.07 2.887(12) 172.0 . O4 H4OA O60 0.84 1.87 2.710(9) 176.3 . O4 H4OB O40 0.84 1.87 2.713(10) 179.7 . O30 H30 O50 0.84 1.79 2.626(14) 173.6 . O50 H50 O70 1.03 1.79 2.81(2) 171.2 . O60 H60 O23 0.97 2.33 3.132(12) 139.6 . O60 H60 O23 0.97 2.33 3.132(12) 139.6 7_565 O70 H70 O13 0.92 2.04 2.947(18) 171.9 2_554 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.420 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.152 data_Complex5a _database_code_depnum_ccdc_archive 'CCDC 249424' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H104 Cl2 N4 Ni2 O21' _chemical_formula_weight 1453.83 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 27.9805(12) _cell_length_b 13.7050(6) _cell_length_c 18.8743(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7237.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21493 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.28 _exptl_crystal_description block _exptl_crystal_colour Green _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3096 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.872055 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50518 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6664 _reflns_number_gt 5805 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 crystals are isomorphous with the cobalt analog, although there appears to be an extra solvate water molecule in the cobalt complex. The pendant alcohol group of the macrocycle is disordered 75:25 over two positions. The cations lie on mirror planes, as do the perchlorate anions, one of which is disordered (modeled as 45:5 % over two sites on the mirror plane), and the uncoordinated ethanol solvate molecules. Hydrogen atoms bonded to oxygen atoms were located from difference maps and not further refined. The quality of the refinements is not improved by reducing the symmetry. ; _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^)+(0.0589P)^2^+27.7475P] 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 6664 _refine_ls_number_parameters 477 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0840 _refine_ls_R_factor_gt 0.0764 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1899 _refine_ls_goodness_of_fit_ref 1.196 _refine_ls_restrained_S_all 1.198 _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 Ni1 Ni 0.070237(19) 0.09613(4) 0.27355(3) 0.03032(19) Uani 1 1 d . . . O1 O 0.01954(10) 0.1626(2) 0.21712(16) 0.0303(7) Uani 1 1 d . . . C1 C -0.02132(15) 0.1210(3) 0.1945(2) 0.0309(10) Uani 1 1 d . . . C2 C -0.04466(16) 0.1580(4) 0.1342(2) 0.0362(11) Uani 1 1 d . . . C3 C -0.08563(17) 0.1114(4) 0.1104(3) 0.0432(12) Uani 1 1 d . . . H3 H -0.1012 0.1367 0.0697 0.052 Uiso 1 1 calc R . . C4 C -0.10498(17) 0.0298(4) 0.1430(3) 0.0482(14) Uani 1 1 d . . . C5 C -0.15091(19) -0.0188(5) 0.1135(4) 0.0644(18) Uani 1 1 d . . . C6 C -0.1481(3) -0.0291(9) 0.0354(5) 0.135(5) Uani 1 1 d . . . H6A H -0.1202 -0.0687 0.0230 0.050 Uiso 1 1 calc R . . H6B H -0.1451 0.0356 0.0137 0.050 Uiso 1 1 calc R . . H6C H -0.1771 -0.0610 0.0179 0.050 Uiso 1 1 calc R . . C7 C -0.19371(19) 0.0417(5) 0.1349(4) 0.0703(19) Uani 1 1 d . . . H7A H -0.1954 0.0454 0.1867 0.050 Uiso 1 1 calc R . . H7B H -0.2229 0.0113 0.1166 0.050 Uiso 1 1 calc R . . H7C H -0.1906 0.1076 0.1153 0.050 Uiso 1 1 calc R . . C8 C -0.1576(3) -0.1209(6) 0.1412(7) 0.149(5) Uani 1 1 d . . . H8A H -0.1593 -0.1194 0.1930 0.050 Uiso 1 1 calc R . . H8B H -0.1305 -0.1615 0.1264 0.050 Uiso 1 1 calc R . . H8C H -0.1872 -0.1483 0.1221 0.050 Uiso 1 1 calc R . . C9 C -0.08313(17) -0.0025(4) 0.2045(3) 0.0457(13) Uani 1 1 d . . . H9 H -0.0968 -0.0557 0.2296 0.055 Uiso 1 1 calc R . . C10 C -0.04115(15) 0.0416(3) 0.2309(3) 0.0352(11) Uani 1 1 d . . . C11 C -0.0267(2) 0.2500 0.0982(3) 0.0382(16) Uani 1 2 d S . . H11A H -0.0372 0.2500 0.0482 0.046 Uiso 1 2 calc SR . . H11B H 0.0087 0.2500 0.0987 0.046 Uiso 1 2 calc SR . . C12 C -0.02316(16) 0.0079(3) 0.2995(3) 0.0382(11) Uani 1 1 d . . . H12 H -0.0432 -0.0352 0.3254 0.046 Uiso 1 1 calc R . . N1 N 0.01673(13) 0.0304(3) 0.3284(2) 0.0361(9) Uani 1 1 d . B . C13 C 0.02417(18) -0.0051(4) 0.4011(3) 0.0469(13) Uani 1 1 d . . . H13A H -0.0032 -0.0467 0.4149 0.056 Uiso 1 1 calc R A 1 H13B H 0.0250 0.0513 0.4338 0.056 Uiso 1 1 calc R A 1 C14 C 0.0701(2) -0.0632(4) 0.4092(3) 0.0497(13) Uani 0.75 1 d P B 1 H14 H 0.0702 -0.0895 0.4586 0.060 Uiso 0.75 1 calc PR B 1 O2 O 0.07064(17) -0.1428(3) 0.3646(3) 0.0495(12) Uani 0.75 1 d P B 1 C14' C 0.0701(2) -0.0632(4) 0.4092(3) 0.0497(13) Uani 0.25 1 d P B 2 H14' H 0.0703 -0.1101 0.3686 0.060 Uiso 0.25 1 calc PR B 2 O2' O 0.0702(7) -0.1203(17) 0.4693(12) 0.092(7) Uani 0.25 1 d P B 2 C15 C 0.11540(18) -0.0035(4) 0.4011(3) 0.0436(12) Uani 1 1 d . . . H15A H 0.1136 0.0539 0.4329 0.052 Uiso 1 1 calc R B 1 H15B H 0.1430 -0.0435 0.4162 0.052 Uiso 1 1 calc R B 1 N2 N 0.12351(13) 0.0304(3) 0.3283(2) 0.0352(9) Uani 1 1 d . B . C16 C 0.16294(16) 0.0068(3) 0.2985(3) 0.0385(11) Uani 1 1 d . . . H16 H 0.1826 -0.0378 0.3238 0.046 Uiso 1 1 calc R B . C17 C 0.18125(15) 0.0401(3) 0.2307(2) 0.0352(10) Uani 1 1 d . B . C18 C 0.22247(17) -0.0051(4) 0.2043(3) 0.0448(13) Uani 1 1 d . . . H18 H 0.2350 -0.0598 0.2290 0.054 Uiso 1 1 calc R B . C19 C 0.24567(16) 0.0262(4) 0.1440(3) 0.0435(12) Uani 1 1 d . B . C20 C 0.2898(2) -0.0248(5) 0.1136(4) 0.0662(19) Uani 1 1 d . . . C21 C 0.3011(3) -0.1187(6) 0.1512(6) 0.160(6) Uani 1 1 d . B . H21A H 0.2733 -0.1622 0.1488 0.050 Uiso 1 1 calc R . . H21B H 0.3087 -0.1050 0.2009 0.050 Uiso 1 1 calc R . . H21C H 0.3286 -0.1501 0.1284 0.050 Uiso 1 1 calc R . . C22 C 0.3324(2) 0.0418(6) 0.1166(4) 0.081(2) Uani 1 1 d . B . H22A H 0.3603 0.0084 0.0965 0.050 Uiso 1 1 calc R . . H22B H 0.3390 0.0593 0.1660 0.050 Uiso 1 1 calc R . . H22C H 0.3258 0.1010 0.0892 0.050 Uiso 1 1 calc R . . C23 C 0.2805(2) -0.0510(6) 0.0367(5) 0.098(3) Uani 1 1 d . B . H23A H 0.2531 -0.0952 0.0339 0.050 Uiso 1 1 calc R . . H23B H 0.3088 -0.0831 0.0169 0.050 Uiso 1 1 calc R . . H23C H 0.2737 0.0085 0.0098 0.050 Uiso 1 1 calc R . . C24 C 0.22721(15) 0.1101(3) 0.1116(3) 0.0340(10) Uani 1 1 d . . . H24 H 0.2434 0.1356 0.0714 0.041 Uiso 1 1 calc R B . C25 C 0.18670(14) 0.1579(3) 0.1352(2) 0.0272(9) Uani 1 1 d . B . C26 C 0.16216(14) 0.1202(3) 0.1940(2) 0.0287(9) Uani 1 1 d . . . O3 O 0.12143(10) 0.1626(2) 0.21627(16) 0.0292(7) Uani 1 1 d . B . C27 C 0.1696(2) 0.2500 0.0982(3) 0.0280(13) Uani 1 2 d S . . H27A H 0.1815 0.2500 0.0488 0.034 Uiso 1 2 calc SR B . H27B H 0.1343 0.2500 0.0966 0.034 Uiso 1 2 calc SR . . O4 O 0.07067(16) 0.2500 0.3331(3) 0.0440(12) Uani 1 2 d S . . Cl1 Cl -0.19827(7) 0.2500 0.57964(13) 0.0468(5) Uani 0.90 2 d SP . . O11 O -0.22356(19) 0.1657(4) 0.5722(4) 0.123(2) Uani 1 1 d . . . O12 O -0.1575(4) 0.2500 0.5319(8) 0.134(5) Uani 0.90 2 d SP . . O13 O -0.1734(5) 0.2500 0.6420(6) 0.166(5) Uani 1 2 d S . . Cl1' Cl -0.2121(8) 0.2500 0.6230(13) 0.043(4) Uiso 0.10 2 d SP . . O12' O -0.233(6) 0.2500 0.663(9) 0.19(6) Uiso 0.10 2 d SP . . Cl2 Cl 0.06891(6) 0.2500 0.57652(11) 0.0517(5) Uani 1 2 d S . . O21 O 0.0805(3) 0.2500 0.6488(4) 0.121(4) Uani 1 2 d S . . O22 O 0.0177(2) 0.2500 0.5679(4) 0.075(2) Uani 1 2 d S . . O23 O 0.0871(2) 0.1666(5) 0.5445(4) 0.120(2) Uani 1 1 d . . . O30 O 0.06870(12) -0.0174(2) 0.19884(19) 0.0426(8) Uani 1 1 d . . . C31 C 0.07369(19) -0.0022(4) 0.1240(3) 0.0487(13) Uani 1 1 d . . . H31A H 0.1063 -0.0218 0.1093 0.058 Uiso 1 1 calc R . . H31B H 0.0699 0.0681 0.1136 0.058 Uiso 1 1 calc R . . C32 C 0.0378(2) -0.0589(5) 0.0814(4) 0.0677(19) Uani 1 1 d . . . H32A H 0.0419 -0.1288 0.0904 0.102 Uiso 1 1 calc R . . H32B H 0.0426 -0.0456 0.0309 0.102 Uiso 1 1 calc R . . H32C H 0.0054 -0.0391 0.0952 0.102 Uiso 1 1 calc R . . O40 O -0.0056(2) 0.2500 0.4209(4) 0.070(2) Uani 1 2 d SD . . C41 C -0.0573(7) 0.2190(12) 0.4114(10) 0.191(16) Uani 0.50 1 d PD . . H41A H -0.0609 0.1470 0.4133 0.050 Uiso 0.50 1 d P . . H41B H -0.0780 0.2500 0.4499 0.050 Uiso 1 2 d S . . C42 C -0.0761(6) 0.2500 0.3490(10) 0.171(9) Uani 1 2 d SD . . H42A H -0.1094 0.2288 0.3456 0.050 Uiso 0.50 1 calc PR . . H42B H -0.0577 0.2221 0.3096 0.050 Uiso 0.50 1 calc PR . . H42C H -0.0746 0.3214 0.3467 0.050 Uiso 0.50 1 calc PR . . C52 C -0.0357(4) -0.2500 0.1820(8) 0.111(5) Uani 1 2 d SD . . H52A H -0.0639 -0.2815 0.2027 0.050 Uiso 0.50 1 calc PR . . H52B H -0.0257 -0.2859 0.1396 0.050 Uiso 0.50 1 calc PR . . H52C H -0.0435 -0.1826 0.1691 0.050 Uiso 0.50 1 calc PR . . C51 C 0.0022(4) -0.2500 0.2325(6) 0.080(3) Uani 1 2 d SD . . H51A H 0.0099 -0.3183 0.2453 0.050 Uiso 0.50 1 calc PR . . H51B H -0.0087 -0.2164 0.2760 0.050 Uiso 0.50 1 calc PR . . O50 O 0.0449(4) -0.2029(7) 0.2068(8) 0.116(5) Uani 0.50 1 d PD . . O60 O 0.14889(18) 0.2500 0.4185(3) 0.0553(14) Uani 1 2 d S . . C61 C 0.1969(3) 0.2500 0.4082(6) 0.110(5) Uani 1 2 d S . . H61A H 0.2097 0.3079 0.4332 0.050 Uiso 0.50 1 calc PR . . H61B H 0.2097 0.1921 0.4332 0.050 Uiso 0.50 1 calc PR . . C62 C 0.2164(3) 0.2500 0.3437(5) 0.075(3) Uani 1 2 d S . . H62A H 0.2473 0.2836 0.3453 0.050 Uiso 0.50 1 calc PR . . H62B H 0.1951 0.2838 0.3106 0.050 Uiso 0.50 1 calc PR . . H62C H 0.2211 0.1826 0.3279 0.050 Uiso 0.50 1 calc PR . . C72 C 0.1555(5) -0.2500 0.1196(8) 0.125(6) Uani 1 2 d S . . H72A H 0.1800 -0.2065 0.1001 0.050 Uiso 0.50 1 calc PR . . H72B H 0.1238 -0.2271 0.1050 0.050 Uiso 0.50 1 calc PR . . H72C H 0.1606 -0.3164 0.1018 0.050 Uiso 0.50 1 calc PR . . C71 C 0.1585(4) -0.2500 0.1947(7) 0.086(3) Uani 1 2 d S . . H71A H 0.1543 -0.1822 0.2116 0.050 Uiso 0.50 1 calc PR . . H71B H 0.1910 -0.2713 0.2084 0.050 Uiso 0.50 1 calc PR . . O70 O 0.1236(3) -0.3123(6) 0.2313(5) 0.073(3) Uani 0.50 1 d P . . H1O H 0.0240 0.2500 0.2066 0.050 Uiso 1 2 d S . . H3O H 0.1210 0.2500 0.2048 0.050 Uiso 1 2 d S . . H4OA H 0.0938 0.2500 0.3619 0.050 Uiso 1 2 d S . . H4OB H 0.0464 0.2500 0.3607 0.050 Uiso 1 2 d S . . H30 H 0.0609 -0.0772 0.2012 0.050 Uiso 1 1 d . . . H40 H 0.0028 0.2500 0.4617 0.050 Uiso 1 2 d S . . H50 H 0.0698 -0.2374 0.2147 0.050 Uiso 0.50 1 d P . . H70 H 0.1400 -0.2944 0.2673 0.050 Uiso 0.50 1 d P . . H60 H 0.1380 0.2500 0.4686 0.050 Uiso 1 2 d S . . 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 0.0272(3) 0.0291(3) 0.0346(3) 0.0040(2) 0.0014(2) -0.0004(2) O1 0.0238(14) 0.0271(16) 0.0400(17) -0.0011(13) -0.0040(13) -0.0044(12) C1 0.025(2) 0.035(2) 0.033(2) -0.0110(19) 0.0016(18) -0.0013(18) C2 0.031(2) 0.047(3) 0.031(2) -0.014(2) 0.0005(19) 0.000(2) C3 0.031(2) 0.058(3) 0.041(3) -0.020(3) -0.006(2) 0.003(2) C4 0.028(2) 0.055(3) 0.062(3) -0.029(3) 0.001(2) -0.003(2) C5 0.035(3) 0.068(4) 0.090(5) -0.035(4) -0.006(3) -0.008(3) C6 0.060(5) 0.223(12) 0.123(8) -0.113(9) 0.002(5) -0.049(6) C7 0.033(3) 0.083(5) 0.094(5) -0.025(4) 0.004(3) -0.010(3) C8 0.082(6) 0.082(6) 0.282(16) -0.022(8) -0.087(8) -0.029(5) C9 0.033(2) 0.038(3) 0.066(4) -0.018(3) 0.010(2) -0.006(2) C10 0.027(2) 0.032(2) 0.046(3) -0.010(2) 0.0066(19) -0.0038(19) C11 0.034(3) 0.055(4) 0.026(3) 0.000 -0.004(3) 0.000 C12 0.033(2) 0.029(2) 0.053(3) 0.000(2) 0.011(2) -0.002(2) N1 0.034(2) 0.032(2) 0.042(2) 0.0039(18) 0.0077(17) -0.0019(17) C13 0.045(3) 0.054(3) 0.041(3) 0.015(3) 0.008(2) -0.003(3) C14 0.056(3) 0.048(3) 0.044(3) 0.021(3) 0.005(3) 0.001(3) O2 0.057(3) 0.030(2) 0.062(3) 0.006(2) 0.008(2) -0.003(2) C14' 0.056(3) 0.048(3) 0.044(3) 0.021(3) 0.005(3) 0.001(3) O2' 0.070(12) 0.099(16) 0.107(16) 0.057(14) -0.007(11) 0.001(11) C15 0.044(3) 0.046(3) 0.041(3) 0.013(2) -0.002(2) 0.005(2) N2 0.036(2) 0.032(2) 0.038(2) 0.0095(17) 0.0002(17) -0.0016(17) C16 0.035(2) 0.031(2) 0.050(3) 0.011(2) -0.004(2) 0.005(2) C17 0.031(2) 0.030(2) 0.045(3) 0.007(2) 0.000(2) 0.0011(19) C18 0.032(2) 0.033(3) 0.069(4) 0.013(2) 0.003(2) 0.010(2) C19 0.028(2) 0.035(3) 0.067(3) 0.007(3) 0.011(2) 0.008(2) C20 0.042(3) 0.052(3) 0.104(5) 0.014(4) 0.032(3) 0.024(3) C21 0.113(7) 0.105(7) 0.261(14) 0.108(8) 0.126(8) 0.084(6) C22 0.030(3) 0.105(6) 0.109(6) 0.021(5) 0.015(3) 0.015(3) C23 0.059(4) 0.067(5) 0.168(9) -0.043(5) 0.051(5) 0.007(4) C24 0.027(2) 0.033(2) 0.043(3) -0.001(2) 0.0044(19) -0.0020(19) C25 0.026(2) 0.020(2) 0.035(2) -0.0023(18) -0.0033(17) -0.0028(16) C26 0.023(2) 0.022(2) 0.041(2) -0.0008(18) -0.0011(18) -0.0015(17) O3 0.0264(15) 0.0224(15) 0.0388(17) 0.0034(13) 0.0054(13) 0.0019(12) C27 0.028(3) 0.028(3) 0.028(3) 0.000 0.001(2) 0.000 O4 0.026(2) 0.068(3) 0.038(3) 0.000 -0.003(2) 0.000 Cl1 0.0370(10) 0.0435(11) 0.0601(15) 0.000 -0.0125(10) 0.000 O11 0.065(3) 0.085(4) 0.219(8) -0.024(5) -0.001(4) -0.030(3) O12 0.092(7) 0.086(7) 0.225(14) 0.000 0.072(8) 0.000 O13 0.230(14) 0.131(9) 0.135(9) 0.000 -0.122(10) 0.000 Cl2 0.0354(9) 0.0699(13) 0.0498(11) 0.000 0.0028(8) 0.000 O21 0.074(5) 0.241(12) 0.049(4) 0.000 0.000(4) 0.000 O22 0.034(3) 0.113(6) 0.078(4) 0.000 0.005(3) 0.000 O23 0.112(5) 0.124(5) 0.124(5) -0.029(4) -0.008(4) 0.070(4) O30 0.048(2) 0.0300(17) 0.050(2) -0.0067(15) 0.0091(16) -0.0067(15) C31 0.048(3) 0.051(3) 0.048(3) -0.010(3) 0.004(2) -0.002(3) C32 0.056(4) 0.076(4) 0.071(4) -0.038(4) 0.008(3) -0.007(3) O40 0.034(3) 0.113(6) 0.064(4) 0.000 -0.003(3) 0.000 C41 0.42(5) 0.052(11) 0.098(14) 0.039(9) 0.09(2) 0.067(17) C42 0.21(2) 0.109(13) 0.20(2) 0.000 0.108(18) 0.000 C52 0.087(9) 0.102(10) 0.145(13) 0.000 0.015(9) 0.000 C51 0.058(6) 0.074(7) 0.110(9) 0.000 0.015(6) 0.000 O50 0.079(7) 0.051(5) 0.219(15) 0.032(7) -0.004(8) -0.009(5) O60 0.041(3) 0.081(4) 0.044(3) 0.000 -0.004(2) 0.000 C61 0.042(5) 0.221(17) 0.068(7) 0.000 -0.015(5) 0.000 C62 0.054(5) 0.107(8) 0.064(6) 0.000 -0.007(5) 0.000 C72 0.071(8) 0.183(16) 0.123(13) 0.000 0.023(8) 0.000 C71 0.085(8) 0.062(6) 0.111(10) 0.000 -0.010(7) 0.000 O70 0.085(6) 0.044(5) 0.090(7) -0.002(5) 0.002(5) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O1 1.994(3) . ? Ni1 O3 2.012(3) . ? Ni1 N2 2.025(4) . ? Ni1 N1 2.031(4) . ? Ni1 O30 2.101(3) . ? Ni1 O4 2.390(2) . ? O1 C1 1.347(5) . ? C1 C10 1.402(6) . ? C1 C2 1.406(7) . ? C2 C3 1.387(6) . ? C2 C11 1.518(6) . ? C3 C4 1.387(8) . ? C4 C9 1.383(8) . ? C4 C5 1.551(7) . ? C5 C6 1.482(10) . ? C5 C8 1.506(12) . ? C5 C7 1.511(8) . ? C9 C10 1.412(7) . ? C10 C12 1.465(7) . ? C11 C2 1.518(6) 7_565 ? C12 N1 1.280(6) . ? N1 C13 1.472(6) . ? C13 C14 1.519(7) . ? C14 O2 1.379(8) . ? C14 C15 1.517(7) . ? C15 N2 1.468(6) . ? N2 C16 1.279(6) . ? C16 C17 1.452(7) . ? C17 C18 1.401(6) . ? C17 C26 1.405(6) . ? C18 C19 1.379(7) . ? C19 C24 1.402(7) . ? C19 C20 1.530(7) . ? C20 C22 1.502(9) . ? C20 C21 1.503(9) . ? C20 C23 1.517(11) . ? C24 C25 1.382(6) . ? C25 C26 1.404(6) . ? C25 C27 1.520(5) . ? C26 O3 1.346(5) . ? C27 C25 1.520(5) 7_565 ? O4 Ni1 2.390(2) 7_565 ? Cl1 Cl1' 0.90(2) . ? Cl1 O11 1.362(5) . ? Cl1 O11 1.362(5) 7_565 ? Cl1 O13 1.366(9) . ? Cl1 O12 1.454(10) . ? Cl1 O12' 1.86(17) . ? O11 Cl1' 1.535(16) . ? O13 Cl1' 1.14(2) . ? O13 O12' 1.72(16) . ? Cl1' O12' 0.96(16) . ? Cl1' O11 1.535(16) 7_565 ? Cl2 O23 1.389(6) . ? Cl2 O23 1.389(6) 7_565 ? Cl2 O21 1.402(7) . ? Cl2 O22 1.443(6) . ? O30 C31 1.435(6) . ? C31 C32 1.503(8) . ? O40 C41 1.52(2) . ? C41 C42 1.358(18) . ? C52 C51 1.426(15) . ? C51 O50 1.440(12) . ? O60 C61 1.358(11) . ? C61 C62 1.332(13) . ? C72 C71 1.419(17) . ? C71 O70 1.469(13) . ? 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 Ni1 O3 90.72(12) . . ? O1 Ni1 N2 177.90(14) . . ? O3 Ni1 N2 87.21(13) . . ? O1 Ni1 N1 87.16(14) . . ? O3 Ni1 N1 177.79(14) . . ? N2 Ni1 N1 94.90(15) . . ? O1 Ni1 O30 88.02(13) . . ? O3 Ni1 O30 89.37(12) . . ? N2 Ni1 O30 91.58(15) . . ? N1 Ni1 O30 89.92(15) . . ? O1 Ni1 O4 81.47(13) . . ? O3 Ni1 O4 81.37(13) . . ? N2 Ni1 O4 98.58(15) . . ? N1 Ni1 O4 98.93(15) . . ? O30 Ni1 O4 165.86(14) . . ? C1 O1 Ni1 125.4(3) . . ? O1 C1 C10 120.6(4) . . ? O1 C1 C2 119.9(4) . . ? C10 C1 C2 119.5(4) . . ? C3 C2 C1 118.7(5) . . ? C3 C2 C11 120.8(5) . . ? C1 C2 C11 120.5(4) . . ? C2 C3 C4 123.4(5) . . ? C9 C4 C3 117.2(5) . . ? C9 C4 C5 122.0(6) . . ? C3 C4 C5 120.6(5) . . ? C6 C5 C8 105.3(8) . . ? C6 C5 C7 111.1(7) . . ? C8 C5 C7 108.6(7) . . ? C6 C5 C4 110.8(5) . . ? C8 C5 C4 112.1(6) . . ? C7 C5 C4 109.0(5) . . ? C4 C9 C10 121.8(5) . . ? C1 C10 C9 119.2(5) . . ? C1 C10 C12 122.8(4) . . ? C9 C10 C12 117.6(4) . . ? C2 C11 C2 112.3(5) . 7_565 ? N1 C12 C10 126.9(4) . . ? C12 N1 C13 116.2(4) . . ? C12 N1 Ni1 122.2(3) . . ? C13 N1 Ni1 121.2(3) . . ? N1 C13 C14 112.7(4) . . ? O2 C14 C15 110.8(5) . . ? O2 C14 C13 111.3(5) . . ? C15 C14 C13 114.5(4) . . ? N2 C15 C14 113.2(4) . . ? C16 N2 C15 117.7(4) . . ? C16 N2 Ni1 121.6(3) . . ? C15 N2 Ni1 120.3(3) . . ? N2 C16 C17 127.7(4) . . ? C18 C17 C26 118.9(4) . . ? C18 C17 C16 117.7(4) . . ? C26 C17 C16 123.1(4) . . ? C19 C18 C17 123.0(4) . . ? C18 C19 C24 116.2(4) . . ? C18 C19 C20 123.2(5) . . ? C24 C19 C20 120.6(5) . . ? C22 C20 C21 109.6(7) . . ? C22 C20 C23 108.4(6) . . ? C21 C20 C23 106.6(7) . . ? C22 C20 C19 110.4(5) . . ? C21 C20 C19 112.5(5) . . ? C23 C20 C19 109.2(5) . . ? C25 C24 C19 123.4(4) . . ? C24 C25 C26 118.8(4) . . ? C24 C25 C27 120.2(4) . . ? C26 C25 C27 121.0(4) . . ? O3 C26 C25 120.2(4) . . ? O3 C26 C17 120.3(4) . . ? C25 C26 C17 119.5(4) . . ? C26 O3 Ni1 125.1(3) . . ? C25 C27 C25 112.4(5) 7_565 . ? Ni1 O4 Ni1 123.9(2) . 7_565 ? Cl1' Cl1 O11 82.6(7) . . ? Cl1' Cl1 O11 82.6(7) . 7_565 ? O11 Cl1 O11 116.0(5) . 7_565 ? Cl1' Cl1 O13 55.9(14) . . ? O11 Cl1 O13 110.7(5) . . ? O11 Cl1 O13 110.7(5) 7_565 . ? Cl1' Cl1 O12 153.6(14) . . ? O11 Cl1 O12 110.1(4) . . ? O11 Cl1 O12 110.1(4) 7_565 . ? O13 Cl1 O12 97.7(9) . . ? Cl1' Cl1 O12' 6(5) . . ? O11 Cl1 O12' 79(2) . . ? O11 Cl1 O12' 79(2) 7_565 . ? O13 Cl1 O12' 62(5) . . ? O12 Cl1 O12' 160(5) . . ? Cl1 O11 Cl1' 35.8(8) . . ? Cl1' O13 Cl1 41.1(12) . . ? Cl1' O13 O12' 32(5) . . ? Cl1 O13 O12' 73(5) . . ? Cl1 Cl1' O12' 168(10) . . ? Cl1 Cl1' O13 83.0(18) . . ? O12' Cl1' O13 109(10) . . ? Cl1 Cl1' O11 61.6(10) . . ? O12' Cl1' O11 112(6) . . ? O13 Cl1' O11 113.3(13) . . ? Cl1 Cl1' O11 61.6(10) . 7_565 ? O12' Cl1' O11 112(6) . 7_565 ? O13 Cl1' O11 113.3(13) . 7_565 ? O11 Cl1' O11 97.6(14) . 7_565 ? Cl1' O12' O13 39(7) . . ? Cl1' O12' Cl1 6(5) . . ? O13 O12' Cl1 45(4) . . ? O23 Cl2 O23 110.7(7) . 7_565 ? O23 Cl2 O21 109.8(3) . . ? O23 Cl2 O21 109.8(3) 7_565 . ? O23 Cl2 O22 108.3(3) . . ? O23 Cl2 O22 108.3(3) 7_565 . ? O21 Cl2 O22 109.9(4) . . ? C31 O30 Ni1 123.5(3) . . ? O30 C31 C32 112.7(5) . . ? C42 C41 O40 112.5(14) . . ? C52 C51 O50 113.1(10) . . ? C62 C61 O60 122.4(9) . . ? C72 C71 O70 115.5(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ni1 O1 C1 139.3(3) . . . . ? N2 Ni1 O1 C1 129(4) . . . . ? N1 Ni1 O1 C1 -40.0(3) . . . . ? O30 Ni1 O1 C1 50.0(3) . . . . ? O4 Ni1 O1 C1 -139.5(3) . . . . ? Ni1 O1 C1 C10 25.9(5) . . . . ? Ni1 O1 C1 C2 -154.6(3) . . . . ? O1 C1 C2 C3 177.4(4) . . . . ? C10 C1 C2 C3 -3.1(6) . . . . ? O1 C1 C2 C11 -5.5(6) . . . . ? C10 C1 C2 C11 173.9(4) . . . . ? C1 C2 C3 C4 0.0(7) . . . . ? C11 C2 C3 C4 -177.0(5) . . . . ? C2 C3 C4 C9 3.4(7) . . . . ? C2 C3 C4 C5 -179.9(5) . . . . ? C9 C4 C5 C6 -138.2(7) . . . . ? C3 C4 C5 C6 45.3(8) . . . . ? C9 C4 C5 C8 -21.0(9) . . . . ? C3 C4 C5 C8 162.6(7) . . . . ? C9 C4 C5 C7 99.3(7) . . . . ? C3 C4 C5 C7 -77.2(7) . . . . ? C3 C4 C9 C10 -3.9(7) . . . . ? C5 C4 C9 C10 179.6(5) . . . . ? O1 C1 C10 C9 -177.9(4) . . . . ? C2 C1 C10 C9 2.7(6) . . . . ? O1 C1 C10 C12 8.7(7) . . . . ? C2 C1 C10 C12 -170.7(4) . . . . ? C4 C9 C10 C1 0.9(7) . . . . ? C4 C9 C10 C12 174.7(4) . . . . ? C3 C2 C11 C2 94.3(6) . . . 7_565 ? C1 C2 C11 C2 -82.7(6) . . . 7_565 ? C1 C10 C12 N1 -15.0(7) . . . . ? C9 C10 C12 N1 171.5(5) . . . . ? C10 C12 N1 C13 173.8(4) . . . . ? C10 C12 N1 Ni1 -13.8(7) . . . . ? O1 Ni1 N1 C12 32.7(4) . . . . ? O3 Ni1 N1 C12 16(4) . . . . ? N2 Ni1 N1 C12 -146.9(4) . . . . ? O30 Ni1 N1 C12 -55.3(4) . . . . ? O4 Ni1 N1 C12 113.6(4) . . . . ? O1 Ni1 N1 C13 -155.2(4) . . . . ? O3 Ni1 N1 C13 -172(4) . . . . ? N2 Ni1 N1 C13 25.2(4) . . . . ? O30 Ni1 N1 C13 116.7(4) . . . . ? O4 Ni1 N1 C13 -74.3(4) . . . . ? C12 N1 C13 C14 125.7(5) . . . . ? Ni1 N1 C13 C14 -46.8(6) . . . . ? N1 C13 C14 O2 -58.6(6) . . . . ? N1 C13 C14 C15 68.0(6) . . . . ? O2 C14 C15 N2 57.3(6) . . . . ? C13 C14 C15 N2 -69.6(6) . . . . ? C14 C15 N2 C16 -123.2(5) . . . . ? C14 C15 N2 Ni1 48.8(5) . . . . ? O1 Ni1 N2 C16 -23(4) . . . . ? O3 Ni1 N2 C16 -33.5(4) . . . . ? N1 Ni1 N2 C16 145.9(4) . . . . ? O30 Ni1 N2 C16 55.8(4) . . . . ? O4 Ni1 N2 C16 -114.3(4) . . . . ? O1 Ni1 N2 C15 165(4) . . . . ? O3 Ni1 N2 C15 154.8(4) . . . . ? N1 Ni1 N2 C15 -25.9(4) . . . . ? O30 Ni1 N2 C15 -115.9(4) . . . . ? O4 Ni1 N2 C15 73.9(4) . . . . ? C15 N2 C16 C17 -172.6(5) . . . . ? Ni1 N2 C16 C17 15.4(7) . . . . ? N2 C16 C17 C18 -171.8(5) . . . . ? N2 C16 C17 C26 13.8(8) . . . . ? C26 C17 C18 C19 0.8(8) . . . . ? C16 C17 C18 C19 -173.8(5) . . . . ? C17 C18 C19 C24 3.2(8) . . . . ? C17 C18 C19 C20 -178.1(6) . . . . ? C18 C19 C20 C22 -115.7(7) . . . . ? C24 C19 C20 C22 62.9(8) . . . . ? C18 C19 C20 C21 7.1(10) . . . . ? C24 C19 C20 C21 -174.3(7) . . . . ? C18 C19 C20 C23 125.2(6) . . . . ? C24 C19 C20 C23 -56.2(7) . . . . ? C18 C19 C24 C25 -3.2(7) . . . . ? C20 C19 C24 C25 178.0(5) . . . . ? C19 C24 C25 C26 -0.9(7) . . . . ? C19 C24 C25 C27 178.5(4) . . . . ? C24 C25 C26 O3 -177.1(4) . . . . ? C27 C25 C26 O3 3.5(6) . . . . ? C24 C25 C26 C17 5.0(6) . . . . ? C27 C25 C26 C17 -174.4(4) . . . . ? C18 C17 C26 O3 177.1(4) . . . . ? C16 C17 C26 O3 -8.6(7) . . . . ? C18 C17 C26 C25 -5.0(7) . . . . ? C16 C17 C26 C25 169.3(4) . . . . ? C25 C26 O3 Ni1 156.9(3) . . . . ? C17 C26 O3 Ni1 -25.2(5) . . . . ? O1 Ni1 O3 C26 -139.8(3) . . . . ? N2 Ni1 O3 C26 39.8(3) . . . . ? N1 Ni1 O3 C26 -123(4) . . . . ? O30 Ni1 O3 C26 -51.8(3) . . . . ? O4 Ni1 O3 C26 138.9(3) . . . . ? C24 C25 C27 C25 -96.6(5) . . . 7_565 ? C26 C25 C27 C25 82.8(6) . . . 7_565 ? O1 Ni1 O4 Ni1 -45.5(2) . . . 7_565 ? O3 Ni1 O4 Ni1 46.5(2) . . . 7_565 ? N2 Ni1 O4 Ni1 132.4(2) . . . 7_565 ? N1 Ni1 O4 Ni1 -131.3(2) . . . 7_565 ? O30 Ni1 O4 Ni1 -3.1(7) . . . 7_565 ? O11 Cl1 O11 Cl1' -78.0(12) 7_565 . . . ? O13 Cl1 O11 Cl1' 49.2(12) . . . . ? O12 Cl1 O11 Cl1' 156.1(13) . . . . ? O12' Cl1 O11 Cl1' -5(5) . . . . ? O11 Cl1 O13 Cl1' -65.1(4) . . . . ? O11 Cl1 O13 Cl1' 65.1(4) 7_565 . . . ? O12 Cl1 O13 Cl1' 180.000(5) . . . . ? O12' Cl1 O13 Cl1' 0.000(6) . . . . ? Cl1' Cl1 O13 O12' 0.000(17) . . . . ? O11 Cl1 O13 O12' -65.1(4) . . . . ? O11 Cl1 O13 O12' 65.1(4) 7_565 . . . ? O12 Cl1 O13 O12' 180.000(15) . . . . ? O11 Cl1 Cl1' O12' -58.8(4) . . . . ? O11 Cl1 Cl1' O12' 58.8(3) 7_565 . . . ? O13 Cl1 Cl1' O12' 180.00(13) . . . . ? O12 Cl1 Cl1' O12' 180.00(13) . . . . ? O11 Cl1 Cl1' O13 121.2(3) . . . . ? O11 Cl1 Cl1' O13 -121.2(3) 7_565 . . . ? O12 Cl1 Cl1' O13 0.000(6) . . . . ? O12' Cl1 Cl1' O13 180.00(3) . . . . ? O11 Cl1 Cl1' O11 117.6(6) 7_565 . . . ? O13 Cl1 Cl1' O11 -121.2(3) . . . . ? O12 Cl1 Cl1' O11 -121.2(3) . . . . ? O12' Cl1 Cl1' O11 58.8(3) . . . . ? O11 Cl1 Cl1' O11 -117.6(6) . . . 7_565 ? O13 Cl1 Cl1' O11 121.2(3) . . . 7_565 ? O12 Cl1 Cl1' O11 121.2(3) . . . 7_565 ? O12' Cl1 Cl1' O11 -58.8(3) . . . 7_565 ? O12' O13 Cl1' Cl1 180.000(5) . . . . ? Cl1 O13 Cl1' O12' 180.00(3) . . . . ? Cl1 O13 Cl1' O11 55.0(13) . . . . ? O12' O13 Cl1' O11 -125.0(13) . . . . ? Cl1 O13 Cl1' O11 -55.0(13) . . . 7_565 ? O12' O13 Cl1' O11 125.0(13) . . . 7_565 ? Cl1 O11 Cl1' O12' 169(9) . . . . ? Cl1 O11 Cl1' O13 -67.5(18) . . . . ? Cl1 O11 Cl1' O11 51.9(9) . . . 7_565 ? Cl1 Cl1' O12' O13 180.00(16) . . . . ? O11 Cl1' O12' O13 126(3) . . . . ? O11 Cl1' O12' O13 -126(3) 7_565 . . . ? O13 Cl1' O12' Cl1 180.0(3) . . . . ? O11 Cl1' O12' Cl1 -54(4) . . . . ? O11 Cl1' O12' Cl1 54(4) 7_565 . . . ? Cl1 O13 O12' Cl1' 0.00(2) . . . . ? Cl1' O13 O12' Cl1 0.00(4) . . . . ? O11 Cl1 O12' Cl1' 120.4(9) . . . . ? O11 Cl1 O12' Cl1' -120.4(9) 7_565 . . . ? O13 Cl1 O12' Cl1' 0.00(13) . . . . ? O12 Cl1 O12' Cl1' 0.00(9) . . . . ? Cl1' Cl1 O12' O13 0.00(14) . . . . ? O11 Cl1 O12' O13 120.4(8) . . . . ? O11 Cl1 O12' O13 -120.4(8) 7_565 . . . ? O12 Cl1 O12' O13 0.00(2) . . . . ? O1 Ni1 O30 C31 52.8(4) . . . . ? O3 Ni1 O30 C31 -37.9(4) . . . . ? N2 Ni1 O30 C31 -125.1(4) . . . . ? N1 Ni1 O30 C31 140.0(4) . . . . ? O4 Ni1 O30 C31 10.9(8) . . . . ? Ni1 O30 C31 C32 -134.8(4) . . . . ? 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 O40 H40 O22 0.81 2.05 2.850(9) 174.8 . O4 H4OA O60 0.85 1.87 2.718(7) 174.7 . O4 H4OB O40 0.86 1.85 2.702(8) 179.6 . O30 H30 O50 0.85 1.78 2.632(10) 179.6 . O50 H50 O70 0.86 1.85 2.705(14) 179.8 . O60 H60 O23 0.99 2.32 3.155(9) 140.9 . O60 H60 O23 0.99 2.32 3.155(9) 140.9 7_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.768 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.090 data_Complex6a _database_code_depnum_ccdc_archive 'CCDC 249425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H90 N10 Ni2 O17' _chemical_formula_weight 1388.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3462(5) _cell_length_b 31.9837(13) _cell_length_c 16.4255(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.6140(10) _cell_angle_gamma 90.00 _cell_volume 6912.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8986 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.91 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.618 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.856645 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50389 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12167 _reflns_number_gt 8067 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. One of the coordinated dmf molecules is disordered, and was refined with 70:30 occupancy of two overlapping positions (both coordinated). There was one non-coordinated and ordered dmf solvate in the lattice but the remaining solvent was too disordered for individual atoms to be resolved; it was modeled as a diffuse contribution using the PLATON SQUEEZE procedure [Sluis, 1990 #165] within the WINGX package[Farrugia, 1999 #254]. The electron density and void volume match dmf and one water molecule per asymmetric unit and these were included in the formula. The hydrogen atoms bonded to the methylenediphenol units were located and not further refined; those bonded to the pendant alcohol groups were not located. One of the alcohol oxygen atoms is disordered with 50:50 occupancy of two equivalent sites. ; _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^)+(0.1082P)^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 12167 _refine_ls_number_parameters 826 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0627 _refine_ls_wR_factor_ref 0.1922 _refine_ls_wR_factor_gt 0.1767 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.130 _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 0.08891(4) 0.181465(17) 0.06288(3) 0.02883(16) Uani 1 1 d . . . Ni2 Ni 0.41083(4) 0.202082(16) 0.00434(3) 0.02859(16) Uani 1 1 d . . . O1 O 0.16137(19) 0.23782(8) 0.07299(17) 0.0293(6) Uani 1 1 d . . . C1 C 0.1126(3) 0.27312(13) 0.0904(3) 0.0304(9) Uani 1 1 d . . . C2 C 0.0094(3) 0.27904(14) 0.0558(3) 0.0334(10) Uani 1 1 d . B . C3 C -0.0386(3) 0.31588(14) 0.0741(3) 0.0382(11) Uani 1 1 d . . . H3 H -0.1078 0.3200 0.0504 0.046 Uiso 1 1 calc R . . C4 C 0.0109(3) 0.34688(14) 0.1258(3) 0.0393(11) Uani 1 1 d . . . C5 C -0.0471(4) 0.38508(15) 0.1499(3) 0.0460(12) Uani 1 1 d . . . C6 C -0.1119(5) 0.3711(2) 0.2125(4) 0.083(2) Uani 1 1 d . . . H6A H -0.1496 0.3951 0.2290 0.125 Uiso 1 1 calc R . . H6B H -0.0681 0.3596 0.2611 0.125 Uiso 1 1 calc R . . H6C H -0.1599 0.3496 0.1878 0.125 Uiso 1 1 calc R . . C7 C -0.1101(6) 0.4047(2) 0.0758(4) 0.088(2) Uani 1 1 d . . . H7A H -0.0661 0.4130 0.0365 0.132 Uiso 1 1 calc R . . H7B H -0.1449 0.4294 0.0929 0.132 Uiso 1 1 calc R . . H7C H -0.1605 0.3845 0.0496 0.132 Uiso 1 1 calc R . . C8 C 0.0243(5) 0.4181(2) 0.1941(6) 0.104(3) Uani 1 1 d . . . H8A H 0.0690 0.4284 0.1568 0.156 Uiso 1 1 calc R . . H8B H 0.0654 0.4058 0.2432 0.156 Uiso 1 1 calc R . . H8C H -0.0156 0.4414 0.2106 0.156 Uiso 1 1 calc R . . C9 C 0.1120(3) 0.33947(14) 0.1587(3) 0.0353(10) Uani 1 1 d . . . H9 H 0.1477 0.3597 0.1947 0.042 Uiso 1 1 calc R . . C10 C 0.1635(3) 0.30350(13) 0.1411(3) 0.0300(10) Uani 1 1 d . . . C11 C 0.2738(3) 0.29758(13) 0.1808(2) 0.0279(9) Uani 1 1 d . . . H11A H 0.2862 0.2675 0.1922 0.034 Uiso 1 1 calc R . . H11B H 0.2857 0.3125 0.2344 0.034 Uiso 1 1 calc R . . C12 C 0.3495(3) 0.31328(13) 0.1283(3) 0.0307(10) Uani 1 1 d . C . C13 C 0.3917(3) 0.35222(13) 0.1424(3) 0.0332(10) Uani 1 1 d . . . H13 H 0.3729 0.3686 0.1857 0.040 Uiso 1 1 calc R . . C14 C 0.4623(3) 0.36919(13) 0.0953(3) 0.0347(10) Uani 1 1 d . . . C15 C 0.5138(3) 0.41116(14) 0.1159(3) 0.0407(11) Uani 1 1 d . . . C16 C 0.4498(5) 0.44100(18) 0.1585(5) 0.087(2) Uani 1 1 d . . . H16A H 0.4863 0.4675 0.1701 0.130 Uiso 1 1 calc R . . H16B H 0.4373 0.4285 0.2103 0.130 Uiso 1 1 calc R . . H16C H 0.3849 0.4461 0.1223 0.130 Uiso 1 1 calc R . . C17 C 0.5372(6) 0.4323(2) 0.0377(4) 0.096(3) Uani 1 1 d . . . H17A H 0.5700 0.4594 0.0521 0.144 Uiso 1 1 calc R . . H17B H 0.4737 0.4367 -0.0010 0.144 Uiso 1 1 calc R . . H17C H 0.5827 0.4145 0.0119 0.144 Uiso 1 1 calc R . . C18 C 0.6141(4) 0.40323(19) 0.1732(5) 0.079(2) Uani 1 1 d . . . H18A H 0.6487 0.4299 0.1874 0.119 Uiso 1 1 calc R . . H18B H 0.6572 0.3852 0.1454 0.119 Uiso 1 1 calc R . . H18C H 0.6008 0.3895 0.2237 0.119 Uiso 1 1 calc R . . C19 C 0.4842(3) 0.34458(14) 0.0316(3) 0.0360(10) Uani 1 1 d . . . H19 H 0.5294 0.3551 -0.0024 0.043 Uiso 1 1 calc R . . C20 C 0.4424(3) 0.30450(13) 0.0148(3) 0.0288(9) Uani 1 1 d . C . C21 C 0.3746(3) 0.28824(13) 0.0631(3) 0.0320(10) Uani 1 1 d . . . O2 O 0.3334(2) 0.24994(9) 0.04808(18) 0.0318(7) Uani 1 1 d . C . C22 C 0.4722(3) 0.28269(14) -0.0557(3) 0.0308(10) Uani 1 1 d . . . H22 H 0.5062 0.2989 -0.0912 0.037 Uiso 1 1 calc R C . N1 N 0.4571(2) 0.24411(11) -0.0746(2) 0.0312(8) Uani 1 1 d . C . C23 C 0.4858(3) 0.23075(14) -0.1534(3) 0.0369(10) Uani 1 1 d . . . H23A H 0.5228 0.2539 -0.1754 0.044 Uiso 1 1 calc R C . H23B H 0.4232 0.2254 -0.1937 0.044 Uiso 1 1 calc R . . C24 C 0.5521(4) 0.19158(16) -0.1465(3) 0.0455(12) Uani 1 1 d . C . H24 H 0.5699 0.1865 -0.2025 0.055 Uiso 1 1 calc R . . O3 O 0.6446(3) 0.19736(13) -0.0917(2) 0.0625(11) Uani 1 1 d . . . C25 C 0.5004(4) 0.15221(16) -0.1227(3) 0.0482(13) Uani 1 1 d . . . H25A H 0.4336 0.1492 -0.1588 0.058 Uiso 1 1 calc R C . H25B H 0.5423 0.1276 -0.1315 0.058 Uiso 1 1 calc R . . N2 N 0.4858(3) 0.15312(12) -0.0368(2) 0.0358(9) Uani 1 1 d . C . C26 C 0.5280(3) 0.12380(14) 0.0101(3) 0.0376(11) Uani 1 1 d . . . H26 H 0.5662 0.1037 -0.0144 0.045 Uiso 1 1 calc R C . C27 C 0.5229(3) 0.11840(13) 0.0970(3) 0.0315(10) Uani 1 1 d . C . C28 C 0.5989(3) 0.09411(14) 0.1441(3) 0.0377(11) Uani 1 1 d . . . H28 H 0.6476 0.0808 0.1169 0.045 Uiso 1 1 calc R C . C29 C 0.6059(3) 0.08877(14) 0.2281(3) 0.0370(11) Uani 1 1 d . C . C30 C 0.6959(4) 0.06502(18) 0.2771(3) 0.0519(14) Uani 1 1 d . . . C31 C 0.7929(4) 0.0907(3) 0.2731(4) 0.091(3) Uani 1 1 d . C . H31A H 0.7864 0.1184 0.2970 0.137 Uiso 1 1 calc R . . H31B H 0.8021 0.0936 0.2154 0.137 Uiso 1 1 calc R . . H31C H 0.8519 0.0763 0.3044 0.137 Uiso 1 1 calc R . . C32 C 0.6858(4) 0.0598(2) 0.3684(3) 0.0617(16) Uani 1 1 d . C . H32A H 0.6803 0.0874 0.3932 0.093 Uiso 1 1 calc R . . H32B H 0.7458 0.0453 0.3977 0.093 Uiso 1 1 calc R . . H32C H 0.6248 0.0434 0.3724 0.093 Uiso 1 1 calc R . . C33 C 0.7031(6) 0.0214(2) 0.2398(4) 0.094(3) Uani 1 1 d . C . H33A H 0.6403 0.0059 0.2420 0.141 Uiso 1 1 calc R . . H33B H 0.7609 0.0063 0.2712 0.141 Uiso 1 1 calc R . . H33C H 0.7128 0.0241 0.1822 0.141 Uiso 1 1 calc R . . C34 C 0.5296(3) 0.10771(14) 0.2646(3) 0.0351(10) Uani 1 1 d . . . H34 H 0.5314 0.1042 0.3223 0.042 Uiso 1 1 calc R C . C35 C 0.4512(3) 0.13146(12) 0.2202(3) 0.0289(9) Uani 1 1 d . C . C36 C 0.4481(3) 0.13683(12) 0.1357(3) 0.0286(9) Uani 1 1 d . . . O4 O 0.3740(2) 0.16027(9) 0.08968(17) 0.0306(7) Uani 1 1 d . C . C37 C 0.3739(3) 0.15199(13) 0.2657(3) 0.0293(9) Uani 1 1 d . . . H37A H 0.3559 0.1797 0.2404 0.035 Uiso 1 1 calc R C . H37B H 0.4062 0.1568 0.3237 0.035 Uiso 1 1 calc R . . C38 C 0.2766(3) 0.12713(12) 0.2653(2) 0.0272(9) Uani 1 1 d . C . C39 C 0.2633(3) 0.10367(12) 0.3331(3) 0.0286(9) Uani 1 1 d . . . H39 H 0.3159 0.1035 0.3799 0.034 Uiso 1 1 calc R C . C40 C 0.1749(3) 0.07989(13) 0.3359(3) 0.0320(10) Uani 1 1 d . C . C41 C 0.1658(3) 0.05507(15) 0.4151(3) 0.0383(11) Uani 1 1 d . . . C42 C 0.1847(4) 0.08397(17) 0.4896(3) 0.0504(13) Uani 1 1 d . C . H42A H 0.2521 0.0967 0.4936 0.076 Uiso 1 1 calc R . . H42B H 0.1813 0.0679 0.5398 0.076 Uiso 1 1 calc R . . H42C H 0.1328 0.1059 0.4834 0.076 Uiso 1 1 calc R . . C43 C 0.2462(4) 0.02010(16) 0.4244(3) 0.0538(14) Uani 1 1 d . C . H43A H 0.3140 0.0325 0.4286 0.081 Uiso 1 1 calc R . . H43B H 0.2334 0.0016 0.3762 0.081 Uiso 1 1 calc R . . H43C H 0.2422 0.0039 0.4745 0.081 Uiso 1 1 calc R . . C44 C 0.0603(4) 0.03491(17) 0.4095(3) 0.0518(14) Uani 1 1 d . C . H44A H 0.0478 0.0163 0.3615 0.078 Uiso 1 1 calc R . . H44B H 0.0082 0.0568 0.4037 0.078 Uiso 1 1 calc R . . H44C H 0.0575 0.0188 0.4598 0.078 Uiso 1 1 calc R . . C45 C 0.1018(3) 0.08028(13) 0.2659(3) 0.0337(10) Uani 1 1 d . . . H45 H 0.0427 0.0637 0.2652 0.040 Uiso 1 1 calc R C . C46 C 0.1104(3) 0.10407(13) 0.1952(3) 0.0301(9) Uani 1 1 d . C . C47 C 0.1987(3) 0.12844(13) 0.1959(3) 0.0280(9) Uani 1 1 d . . . O5 O 0.2083(2) 0.15359(9) 0.13257(17) 0.0314(7) Uani 1 1 d . C . C48 C 0.0305(3) 0.10099(14) 0.1235(3) 0.0356(10) Uani 1 1 d . . . H48 H -0.0154 0.0782 0.1228 0.043 Uiso 1 1 calc R C . N3 N 0.0153(2) 0.12543(11) 0.0617(2) 0.0309(8) Uani 1 1 d . B . C49 C -0.0624(3) 0.11363(15) -0.0081(3) 0.0433(12) Uani 1 1 d . . . H49A H -0.0991 0.0887 0.0073 0.052 Uiso 1 1 calc R A 1 H49B H -0.0288 0.1058 -0.0553 0.052 Uiso 1 1 calc R A 1 C50 C -0.1388(3) 0.14816(17) -0.0352(3) 0.0477(13) Uani 0.50 1 d P B 1 H50 H -0.1656 0.1574 0.0152 0.057 Uiso 0.50 1 calc PR B 1 O6 O -0.2192(5) 0.1324(2) -0.0886(5) 0.0546(19) Uani 0.50 1 d P B 1 C50' C -0.1388(3) 0.14816(17) -0.0352(3) 0.0477(13) Uani 0.50 1 d P B 2 H50' H -0.1845 0.1358 -0.0836 0.057 Uiso 0.50 1 calc PR B 2 O6' O -0.1987(5) 0.1545(2) 0.0184(4) 0.056(2) Uani 0.50 1 d P B 2 C51 C -0.0948(3) 0.18707(15) -0.0710(3) 0.0421(12) Uani 1 1 d . . . H51A H -0.0566 0.1784 -0.1149 0.050 Uiso 1 1 calc R B 1 H51B H -0.1513 0.2054 -0.0964 0.050 Uiso 1 1 calc R B 1 N4 N -0.0277(3) 0.21052(12) -0.0082(2) 0.0334(8) Uani 1 1 d . B . C52 C -0.0499(3) 0.24916(15) 0.0018(3) 0.0368(11) Uani 1 1 d . . . H52 H -0.1116 0.2591 -0.0296 0.044 Uiso 1 1 calc R B . N11 N 0.1985(3) 0.17805(16) -0.0918(3) 0.0569(12) Uani 1 1 d . . . O11 O 0.1622(4) 0.16439(12) -0.0347(3) 0.0731(13) Uani 1 1 d . C . O12 O 0.2857(2) 0.19124(11) -0.0908(2) 0.0479(9) Uani 1 1 d . C . O13 O 0.1284(5) 0.1880(2) -0.1494(4) 0.139(2) Uani 1 1 d . C . O61 O 0.0314(2) 0.19576(9) 0.17278(17) 0.0322(7) Uani 1 1 d D . . C61 C 0.0931(3) 0.20612(13) 0.2348(3) 0.0314(10) Uani 1 1 d D . . H61 H 0.1541 0.2193 0.2258 0.038 Uiso 1 1 calc R . . N61 N 0.0811(3) 0.20041(11) 0.3114(2) 0.0331(8) Uani 1 1 d D . . C62 C 0.1575(4) 0.21272(16) 0.3814(3) 0.0463(12) Uani 1 1 d D . . H62A H 0.1336 0.2056 0.4329 0.069 Uiso 1 1 calc R . . H62B H 0.1691 0.2429 0.3793 0.069 Uiso 1 1 calc R . . H62C H 0.2211 0.1979 0.3789 0.069 Uiso 1 1 calc R . . C63 C -0.0083(4) 0.17850(17) 0.3318(3) 0.0484(13) Uani 1 1 d D . . H63A H -0.0038 0.1772 0.3919 0.073 Uiso 1 1 calc R . . H63B H -0.0106 0.1501 0.3093 0.073 Uiso 1 1 calc R . . H63C H -0.0700 0.1936 0.3076 0.073 Uiso 1 1 calc R . . O71 O 0.5332(2) 0.21832(10) 0.09455(18) 0.0381(7) Uani 0.70 1 d PD C 1 C71 C 0.6215(5) 0.2137(3) 0.1079(5) 0.0419(18) Uani 0.70 1 d PD C 1 H71 H 0.6444 0.1906 0.0796 0.050 Uiso 0.70 1 calc PR C 1 N71 N 0.6938(3) 0.23385(12) 0.1536(2) 0.0400(9) Uani 0.70 1 d PD C 1 C72 C 0.7992(5) 0.2265(3) 0.1661(6) 0.065(2) Uani 0.70 1 d PD C 1 H72A H 0.8132 0.2014 0.1357 0.098 Uiso 0.70 1 calc PR C 1 H72B H 0.8242 0.2224 0.2251 0.098 Uiso 0.70 1 calc PR C 1 H72C H 0.8337 0.2505 0.1461 0.098 Uiso 0.70 1 calc PR C 1 C73 C 0.6645(6) 0.2770(3) 0.1804(6) 0.069(2) Uani 0.70 1 d PD C 1 H73A H 0.6916 0.2983 0.1472 0.104 Uiso 0.70 1 calc PR C 1 H73B H 0.6928 0.2812 0.2389 0.104 Uiso 0.70 1 calc PR C 1 H73C H 0.5903 0.2793 0.1727 0.104 Uiso 0.70 1 calc PR C 1 O71' O 0.5332(2) 0.21832(10) 0.09455(18) 0.0381(7) Uani 0.30 1 d PD C 2 C71' C 0.6122(8) 0.2383(4) 0.1022(9) 0.027(4) Uani 0.30 1 d PD C 2 H71' H 0.6126 0.2605 0.0639 0.033 Uiso 0.30 1 calc PR C 2 N71' N 0.6938(3) 0.23385(12) 0.1536(2) 0.0400(9) Uani 0.30 1 d PD C 2 C72' C 0.7107(14) 0.1940(6) 0.2040(14) 0.086(9) Uani 0.30 1 d PD C 2 H72D H 0.6504 0.1761 0.1914 0.130 Uiso 0.30 1 calc PR C 2 H72E H 0.7228 0.2009 0.2629 0.130 Uiso 0.30 1 calc PR C 2 H72F H 0.7698 0.1791 0.1901 0.130 Uiso 0.30 1 calc PR C 2 C73' C 0.7865(11) 0.2592(6) 0.1686(15) 0.067(7) Uani 0.30 1 d PD C 2 H73D H 0.8452 0.2417 0.1629 0.101 Uiso 0.30 1 calc PR C 2 H73E H 0.7954 0.2708 0.2246 0.101 Uiso 0.30 1 calc PR C 2 H73F H 0.7811 0.2821 0.1284 0.101 Uiso 0.30 1 calc PR C 2 N22 N 0.7119(4) 0.3018(3) -0.0751(5) 0.0808(19) Uani 1 1 d . . . O21 O 0.7053(4) 0.2798(4) -0.0240(5) 0.210(5) Uani 1 1 d . . . O22 O 0.7248(6) 0.2808(3) -0.1354(5) 0.173(4) Uani 1 1 d . . . O23 O 0.7006(7) 0.3354(2) -0.0718(9) 0.229(6) Uani 1 1 d . . . O81 O 0.5699(7) 0.4566(2) 0.3789(4) 0.148(3) Uani 1 1 d . . . C81 C 0.6692(8) 0.4547(3) 0.3799(7) 0.128(4) Uani 1 1 d . . . H81 H 0.7116 0.4328 0.4050 0.153 Uiso 1 1 calc R . . N81 N 0.7028(4) 0.48758(15) 0.3409(3) 0.0707(15) Uani 1 1 d . . . C82 C 0.6520(6) 0.5244(2) 0.3052(5) 0.085(2) Uani 1 1 d . . . H82A H 0.5802 0.5233 0.3112 0.127 Uiso 1 1 calc R . . H82B H 0.6574 0.5258 0.2465 0.127 Uiso 1 1 calc R . . H82C H 0.6837 0.5492 0.3336 0.127 Uiso 1 1 calc R . . C83 C 0.8130(6) 0.4844(3) 0.3363(5) 0.099(2) Uani 1 1 d . . . H83A H 0.8504 0.5059 0.3715 0.148 Uiso 1 1 calc R . . H83B H 0.8230 0.4886 0.2791 0.148 Uiso 1 1 calc R . . H83C H 0.8381 0.4567 0.3553 0.148 Uiso 1 1 calc R . . H2 H 0.2949 0.1550 0.1013 0.040 Uiso 1 1 d . . . H1 H 0.2333 0.2413 0.0593 0.040 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0230(3) 0.0305(3) 0.0316(3) 0.0018(2) 0.0005(2) 0.0014(2) Ni2 0.0254(3) 0.0292(3) 0.0310(3) 0.0005(2) 0.0042(2) 0.0043(2) O1 0.0181(14) 0.0298(16) 0.0407(17) 0.0013(13) 0.0069(12) 0.0042(12) C1 0.025(2) 0.029(2) 0.038(2) 0.0108(19) 0.0085(18) 0.0058(18) C2 0.024(2) 0.037(3) 0.041(3) 0.011(2) 0.0093(19) 0.0063(19) C3 0.028(2) 0.040(3) 0.049(3) 0.012(2) 0.013(2) 0.011(2) C4 0.038(3) 0.031(2) 0.054(3) 0.011(2) 0.021(2) 0.010(2) C5 0.044(3) 0.036(3) 0.063(3) 0.008(2) 0.023(2) 0.018(2) C6 0.105(5) 0.059(4) 0.105(5) 0.020(4) 0.071(5) 0.029(4) C7 0.121(6) 0.067(4) 0.077(4) 0.016(4) 0.015(4) 0.061(4) C8 0.076(5) 0.056(4) 0.187(9) -0.037(5) 0.041(5) 0.021(4) C9 0.038(3) 0.031(2) 0.040(3) 0.007(2) 0.013(2) 0.006(2) C10 0.026(2) 0.027(2) 0.038(2) 0.0104(19) 0.0087(18) 0.0045(18) C11 0.029(2) 0.026(2) 0.029(2) 0.0006(17) 0.0042(18) 0.0042(17) C12 0.027(2) 0.028(2) 0.036(2) 0.0037(18) 0.0033(18) 0.0057(18) C13 0.031(2) 0.030(2) 0.037(2) 0.0018(19) -0.0003(19) 0.0048(19) C14 0.029(2) 0.029(2) 0.044(3) 0.004(2) 0.001(2) 0.0017(18) C15 0.034(3) 0.035(3) 0.051(3) -0.003(2) 0.002(2) -0.005(2) C16 0.067(4) 0.046(4) 0.153(7) -0.033(4) 0.034(4) -0.016(3) C17 0.161(7) 0.054(4) 0.074(4) 0.001(3) 0.021(5) -0.063(5) C18 0.054(4) 0.055(4) 0.115(6) -0.005(4) -0.025(4) -0.012(3) C19 0.027(2) 0.038(3) 0.042(3) 0.011(2) 0.0034(19) 0.0041(19) C20 0.020(2) 0.029(2) 0.036(2) 0.0019(18) 0.0009(17) 0.0018(17) C21 0.026(2) 0.031(2) 0.038(3) 0.0043(19) 0.0013(19) 0.0057(18) O2 0.0263(15) 0.0276(16) 0.0424(17) -0.0006(13) 0.0086(13) -0.0014(12) C22 0.019(2) 0.039(3) 0.034(2) 0.008(2) 0.0032(17) 0.0034(18) N1 0.0237(18) 0.038(2) 0.032(2) -0.0017(16) 0.0032(15) 0.0079(16) C23 0.035(2) 0.044(3) 0.031(2) 0.003(2) 0.0032(19) 0.006(2) C24 0.051(3) 0.057(3) 0.031(3) 0.002(2) 0.015(2) 0.016(2) O3 0.035(2) 0.088(3) 0.066(3) 0.020(2) 0.0141(18) 0.0195(19) C25 0.065(3) 0.046(3) 0.035(3) -0.003(2) 0.014(2) 0.014(3) N2 0.037(2) 0.038(2) 0.032(2) -0.0007(17) 0.0052(16) 0.0061(17) C26 0.038(3) 0.030(2) 0.044(3) -0.006(2) 0.004(2) 0.008(2) C27 0.030(2) 0.024(2) 0.040(3) 0.0016(18) 0.0054(19) 0.0046(18) C28 0.033(2) 0.033(2) 0.050(3) 0.004(2) 0.015(2) 0.0083(19) C29 0.027(2) 0.035(3) 0.049(3) 0.009(2) 0.004(2) 0.0045(19) C30 0.034(3) 0.063(4) 0.059(3) 0.024(3) 0.012(2) 0.019(2) C31 0.037(3) 0.141(7) 0.094(5) 0.061(5) 0.005(3) 0.012(4) C32 0.047(3) 0.080(4) 0.057(3) 0.031(3) 0.005(3) 0.024(3) C33 0.120(6) 0.080(5) 0.084(5) 0.035(4) 0.026(4) 0.068(5) C34 0.029(2) 0.035(2) 0.041(3) 0.009(2) 0.0028(19) -0.0015(19) C35 0.024(2) 0.024(2) 0.037(2) 0.0027(18) -0.0024(18) -0.0033(17) C36 0.027(2) 0.020(2) 0.037(2) -0.0001(18) 0.0001(18) 0.0019(17) O4 0.0246(15) 0.0310(16) 0.0350(16) 0.0019(13) 0.0008(12) 0.0045(12) C37 0.028(2) 0.028(2) 0.030(2) -0.0048(18) -0.0010(18) 0.0001(17) C38 0.024(2) 0.026(2) 0.031(2) -0.0051(17) 0.0035(17) 0.0020(17) C39 0.029(2) 0.026(2) 0.030(2) -0.0005(18) 0.0027(18) 0.0066(18) C40 0.032(2) 0.029(2) 0.036(2) 0.0035(19) 0.0070(19) 0.0045(18) C41 0.036(2) 0.042(3) 0.037(3) 0.009(2) 0.007(2) -0.002(2) C42 0.058(3) 0.063(4) 0.032(3) 0.006(2) 0.011(2) -0.003(3) C43 0.056(3) 0.046(3) 0.060(3) 0.021(3) 0.010(3) 0.015(3) C44 0.042(3) 0.062(4) 0.052(3) 0.018(3) 0.010(2) -0.008(3) C45 0.033(2) 0.028(2) 0.041(3) 0.0045(19) 0.006(2) -0.0043(19) C46 0.030(2) 0.027(2) 0.033(2) 0.0027(18) 0.0055(18) 0.0017(18) C47 0.025(2) 0.027(2) 0.033(2) 0.0000(18) 0.0044(18) 0.0042(17) O5 0.0240(15) 0.0348(17) 0.0345(16) 0.0048(13) 0.0024(12) -0.0027(13) C48 0.028(2) 0.035(3) 0.043(3) -0.002(2) 0.003(2) -0.0062(19) N3 0.0220(18) 0.033(2) 0.035(2) 0.0018(17) -0.0012(15) 0.0012(15) C49 0.034(3) 0.045(3) 0.045(3) -0.002(2) -0.007(2) -0.006(2) C50 0.027(2) 0.055(3) 0.055(3) 0.007(3) -0.012(2) -0.008(2) O6 0.036(4) 0.043(4) 0.076(5) -0.007(4) -0.018(3) -0.007(3) C50' 0.027(2) 0.055(3) 0.055(3) 0.007(3) -0.012(2) -0.008(2) O6' 0.025(3) 0.084(6) 0.060(5) 0.027(4) 0.011(3) -0.001(3) C51 0.033(3) 0.051(3) 0.039(3) 0.005(2) -0.004(2) -0.001(2) N4 0.0243(18) 0.044(2) 0.032(2) 0.0051(17) 0.0056(15) -0.0016(16) C52 0.020(2) 0.047(3) 0.043(3) 0.015(2) 0.0028(19) 0.002(2) N11 0.045(3) 0.086(4) 0.035(2) -0.003(2) -0.006(2) -0.010(2) O11 0.116(4) 0.052(2) 0.068(3) 0.002(2) 0.062(3) -0.005(2) O12 0.0295(18) 0.050(2) 0.061(2) 0.0000(17) -0.0018(16) -0.0073(15) O13 0.105(5) 0.197(7) 0.104(5) 0.023(5) -0.010(4) -0.020(5) O61 0.0273(15) 0.0354(17) 0.0331(17) 0.0004(13) 0.0023(13) -0.0005(13) C61 0.026(2) 0.029(2) 0.039(3) -0.0005(19) 0.0079(19) 0.0008(18) N61 0.033(2) 0.036(2) 0.030(2) -0.0024(16) 0.0021(16) -0.0028(16) C62 0.041(3) 0.051(3) 0.044(3) -0.009(2) -0.001(2) -0.005(2) C63 0.044(3) 0.061(3) 0.042(3) -0.001(2) 0.010(2) -0.013(3) O71 0.0319(18) 0.0442(19) 0.0384(18) 0.0014(15) 0.0067(14) -0.0043(15) C71 0.029(4) 0.051(5) 0.047(4) -0.008(4) 0.010(3) 0.008(4) N71 0.029(2) 0.053(3) 0.038(2) -0.0034(19) 0.0041(17) -0.0050(18) C72 0.034(4) 0.092(7) 0.066(6) -0.016(6) -0.002(4) 0.000(5) C73 0.053(5) 0.076(6) 0.077(6) -0.026(5) 0.005(4) 0.007(4) O71' 0.0319(18) 0.0442(19) 0.0384(18) 0.0014(15) 0.0067(14) -0.0043(15) C71' 0.025(8) 0.005(7) 0.048(9) 0.008(7) -0.006(6) -0.004(6) N71' 0.029(2) 0.053(3) 0.038(2) -0.0034(19) 0.0041(17) -0.0050(18) C72' 0.045(11) 0.079(14) 0.113(18) 0.073(13) -0.051(11) -0.038(10) C73' 0.031(10) 0.045(12) 0.120(19) 0.037(13) -0.007(10) -0.007(9) N22 0.039(3) 0.100(5) 0.099(5) 0.043(4) -0.002(3) -0.003(3) O21 0.052(4) 0.413(16) 0.165(7) 0.132(9) 0.021(4) 0.038(6) O22 0.140(6) 0.245(10) 0.135(6) -0.053(7) 0.023(5) -0.012(6) O23 0.182(9) 0.068(5) 0.453(18) -0.056(7) 0.101(10) -0.020(5) O81 0.197(8) 0.104(5) 0.139(6) 0.029(4) 0.015(6) -0.031(5) C81 0.106(7) 0.138(9) 0.156(9) -0.068(7) 0.073(7) -0.070(6) N81 0.092(4) 0.047(3) 0.070(3) 0.013(3) 0.005(3) -0.013(3) C82 0.100(5) 0.055(4) 0.100(5) 0.025(4) 0.019(4) 0.012(4) C83 0.094(6) 0.103(6) 0.105(6) 0.015(5) 0.033(5) 0.009(5) _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 O5 2.009(3) . ? Ni1 N4 2.010(4) . ? Ni1 O1 2.039(3) . ? Ni1 N3 2.042(3) . ? Ni1 O11 2.085(4) . ? Ni1 O61 2.126(3) . ? Ni2 N2 2.033(4) . ? Ni2 N1 2.034(4) . ? Ni2 O2 2.043(3) . ? Ni2 O4 2.055(3) . ? Ni2 O71 2.079(3) . ? Ni2 O12 2.117(3) . ? O1 C1 1.358(5) . ? C1 C10 1.382(6) . ? C1 C2 1.412(6) . ? C2 C3 1.397(6) . ? C2 C52 1.446(6) . ? C3 C4 1.397(7) . ? C4 C9 1.388(6) . ? C4 C5 1.533(6) . ? C5 C7 1.496(8) . ? C5 C6 1.517(7) . ? C5 C8 1.522(9) . ? C9 C10 1.395(6) . ? C10 C11 1.519(5) . ? C11 C12 1.520(6) . ? C12 C13 1.370(6) . ? C12 C21 1.421(6) . ? C13 C14 1.423(6) . ? C14 C19 1.379(6) . ? C14 C15 1.520(6) . ? C15 C18 1.523(7) . ? C15 C16 1.526(7) . ? C15 C17 1.529(7) . ? C19 C20 1.407(6) . ? C20 C21 1.398(6) . ? C20 C22 1.463(6) . ? C21 O2 1.348(5) . ? C22 N1 1.280(5) . ? N1 C23 1.473(5) . ? C23 C24 1.527(6) . ? C24 O3 1.414(6) . ? C24 C25 1.518(7) . ? C25 N2 1.457(6) . ? N2 C26 1.282(6) . ? C26 C27 1.452(6) . ? C27 C36 1.400(6) . ? C27 C28 1.403(6) . ? C28 C29 1.378(6) . ? C29 C34 1.402(6) . ? C29 C30 1.531(6) . ? C30 C33 1.534(9) . ? C30 C32 1.536(7) . ? C30 C31 1.543(8) . ? C34 C35 1.396(6) . ? C35 C36 1.392(6) . ? C35 C37 1.519(6) . ? C36 O4 1.365(5) . ? C37 C38 1.522(6) . ? C38 C39 1.379(6) . ? C38 C47 1.410(6) . ? C39 C40 1.412(6) . ? C40 C45 1.378(6) . ? C40 C41 1.545(6) . ? C41 C42 1.521(7) . ? C41 C44 1.538(6) . ? C41 C43 1.539(6) . ? C45 C46 1.408(6) . ? C46 C47 1.411(6) . ? C46 C48 1.455(6) . ? C47 O5 1.338(5) . ? C48 N3 1.271(5) . ? N3 C49 1.462(5) . ? C49 C50 1.518(7) . ? C50 O6 1.364(7) . ? C50 C51 1.534(7) . ? C51 N4 1.456(6) . ? N4 C52 1.288(6) . ? N11 O11 1.207(5) . ? N11 O12 1.236(5) . ? N11 O13 1.254(7) . ? O61 C61 1.243(5) . ? C61 N61 1.308(5) . ? N61 C62 1.457(5) . ? N61 C63 1.469(5) . ? O71 C71 1.172(7) . ? C71 N71 1.292(7) . ? N71 C72 1.407(7) . ? N71 C73 1.520(8) . ? N22 O23 1.089(9) . ? N22 O21 1.110(9) . ? N22 O22 1.232(9) . ? O81 C81 1.325(11) . ? C81 N81 1.346(10) . ? N81 C82 1.433(8) . ? N81 C83 1.489(9) . ? 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 O5 Ni1 N4 178.28(13) . . ? O5 Ni1 O1 91.47(11) . . ? N4 Ni1 O1 87.09(13) . . ? O5 Ni1 N3 87.16(12) . . ? N4 Ni1 N3 94.34(14) . . ? O1 Ni1 N3 175.80(13) . . ? O5 Ni1 O11 83.84(15) . . ? N4 Ni1 O11 95.24(16) . . ? O1 Ni1 O11 90.99(13) . . ? N3 Ni1 O11 92.81(15) . . ? O5 Ni1 O61 88.63(11) . . ? N4 Ni1 O61 92.27(12) . . ? O1 Ni1 O61 88.52(11) . . ? N3 Ni1 O61 87.48(13) . . ? O11 Ni1 O61 172.44(15) . . ? N2 Ni2 N1 94.50(14) . . ? N2 Ni2 O2 178.10(13) . . ? N1 Ni2 O2 87.39(12) . . ? N2 Ni2 O4 84.97(13) . . ? N1 Ni2 O4 175.83(12) . . ? O2 Ni2 O4 93.17(11) . . ? N2 Ni2 O71 93.32(14) . . ? N1 Ni2 O71 90.19(13) . . ? O2 Ni2 O71 86.86(12) . . ? O4 Ni2 O71 85.71(11) . . ? N2 Ni2 O12 89.97(14) . . ? N1 Ni2 O12 85.62(13) . . ? O2 Ni2 O12 89.98(12) . . ? O4 Ni2 O12 98.51(12) . . ? O71 Ni2 O12 174.87(13) . . ? C1 O1 Ni1 121.0(2) . . ? O1 C1 C10 120.5(4) . . ? O1 C1 C2 119.8(4) . . ? C10 C1 C2 119.8(4) . . ? C3 C2 C1 118.5(4) . . ? C3 C2 C52 117.8(4) . . ? C1 C2 C52 123.7(4) . . ? C4 C3 C2 122.8(4) . . ? C9 C4 C3 116.5(4) . . ? C9 C4 C5 122.3(4) . . ? C3 C4 C5 121.0(4) . . ? C7 C5 C6 111.6(5) . . ? C7 C5 C8 108.6(5) . . ? C6 C5 C8 105.3(6) . . ? C7 C5 C4 111.3(4) . . ? C6 C5 C4 108.1(4) . . ? C8 C5 C4 111.9(4) . . ? C4 C9 C10 122.7(4) . . ? C1 C10 C9 119.7(4) . . ? C1 C10 C11 121.0(4) . . ? C9 C10 C11 119.3(4) . . ? C10 C11 C12 113.8(3) . . ? C13 C12 C21 119.8(4) . . ? C13 C12 C11 119.8(4) . . ? C21 C12 C11 120.3(4) . . ? C12 C13 C14 123.0(4) . . ? C19 C14 C13 116.0(4) . . ? C19 C14 C15 121.8(4) . . ? C13 C14 C15 122.1(4) . . ? C14 C15 C18 108.0(4) . . ? C14 C15 C16 112.8(4) . . ? C18 C15 C16 108.8(5) . . ? C14 C15 C17 110.6(4) . . ? C18 C15 C17 108.2(5) . . ? C16 C15 C17 108.4(5) . . ? C14 C19 C20 122.8(4) . . ? C21 C20 C19 120.1(4) . . ? C21 C20 C22 124.0(4) . . ? C19 C20 C22 116.0(4) . . ? O2 C21 C20 121.1(4) . . ? O2 C21 C12 120.6(4) . . ? C20 C21 C12 118.3(4) . . ? C21 O2 Ni2 122.0(2) . . ? N1 C22 C20 126.8(4) . . ? C22 N1 C23 116.1(4) . . ? C22 N1 Ni2 122.3(3) . . ? C23 N1 Ni2 121.3(3) . . ? N1 C23 C24 113.9(4) . . ? O3 C24 C25 109.3(4) . . ? O3 C24 C23 111.9(4) . . ? C25 C24 C23 114.7(4) . . ? N2 C25 C24 112.0(4) . . ? C26 N2 C25 116.7(4) . . ? C26 N2 Ni2 123.7(3) . . ? C25 N2 Ni2 119.4(3) . . ? N2 C26 C27 126.1(4) . . ? C36 C27 C28 119.2(4) . . ? C36 C27 C26 123.4(4) . . ? C28 C27 C26 117.4(4) . . ? C29 C28 C27 122.9(4) . . ? C28 C29 C34 116.2(4) . . ? C28 C29 C30 120.3(4) . . ? C34 C29 C30 123.5(4) . . ? C29 C30 C33 109.7(5) . . ? C29 C30 C32 112.2(4) . . ? C33 C30 C32 108.3(5) . . ? C29 C30 C31 107.7(4) . . ? C33 C30 C31 110.9(5) . . ? C32 C30 C31 108.1(5) . . ? C35 C34 C29 123.1(4) . . ? C36 C35 C34 118.8(4) . . ? C36 C35 C37 121.8(4) . . ? C34 C35 C37 119.3(4) . . ? O4 C36 C35 121.2(4) . . ? O4 C36 C27 119.0(4) . . ? C35 C36 C27 119.7(4) . . ? C36 O4 Ni2 120.1(2) . . ? C35 C37 C38 114.9(3) . . ? C39 C38 C47 119.5(4) . . ? C39 C38 C37 120.4(4) . . ? C47 C38 C37 120.1(4) . . ? C38 C39 C40 122.7(4) . . ? C45 C40 C39 116.6(4) . . ? C45 C40 C41 124.3(4) . . ? C39 C40 C41 119.1(4) . . ? C42 C41 C44 109.2(4) . . ? C42 C41 C43 110.0(4) . . ? C44 C41 C43 108.5(4) . . ? C42 C41 C40 109.8(4) . . ? C44 C41 C40 111.4(4) . . ? C43 C41 C40 107.8(4) . . ? C40 C45 C46 123.3(4) . . ? C45 C46 C47 118.3(4) . . ? C45 C46 C48 118.8(4) . . ? C47 C46 C48 122.8(4) . . ? O5 C47 C38 119.5(4) . . ? O5 C47 C46 121.0(4) . . ? C38 C47 C46 119.5(4) . . ? C47 O5 Ni1 122.7(2) . . ? N3 C48 C46 127.1(4) . . ? C48 N3 C49 117.7(4) . . ? C48 N3 Ni1 121.3(3) . . ? C49 N3 Ni1 120.8(3) . . ? N3 C49 C50 113.3(4) . . ? O6 C50 C49 109.7(5) . . ? O6 C50 C51 111.3(5) . . ? C49 C50 C51 114.9(4) . . ? N4 C51 C50 112.1(4) . . ? C52 N4 C51 117.2(4) . . ? C52 N4 Ni1 122.8(3) . . ? C51 N4 Ni1 119.9(3) . . ? N4 C52 C2 126.7(4) . . ? O11 N11 O12 127.8(5) . . ? O11 N11 O13 109.3(5) . . ? O12 N11 O13 120.4(5) . . ? N11 O11 Ni1 143.4(4) . . ? N11 O12 Ni2 133.7(3) . . ? C61 O61 Ni1 118.1(3) . . ? O61 C61 N61 125.5(4) . . ? C61 N61 C62 122.6(4) . . ? C61 N61 C63 121.3(4) . . ? C62 N61 C63 115.9(4) . . ? C71 O71 Ni2 138.3(4) . . ? O71 C71 N71 132.5(7) . . ? C71 N71 C72 129.2(6) . . ? C71 N71 C73 114.8(5) . . ? C72 N71 C73 114.1(6) . . ? O23 N22 O21 124.0(13) . . ? O23 N22 O22 128.2(11) . . ? O21 N22 O22 107.5(11) . . ? O81 C81 N81 111.7(11) . . ? C81 N81 C82 131.6(7) . . ? C81 N81 C83 112.4(7) . . ? C82 N81 C83 116.0(6) . . ? 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 O1 H1 O2 1.03 1.41 2.430(4) 172.9 . O4 H2 O5 1.12 1.34 2.440(4) 166.0 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.874 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.083 data_test_1 _database_code_depnum_ccdc_archive 'CCDC 249426' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H72 N6 O13 Zn2' _chemical_formula_weight 1143.92 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 41.2744(13) _cell_length_b 41.2744(13) _cell_length_c 13.2831(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 22628.8(14) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18575 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.78 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9632 _exptl_absorpt_coefficient_mu 0.914 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.891319 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 80813 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 49 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 0.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9961 _reflns_number_gt 7811 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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 coordinated nitrate and one pendant alcohol are both disordered and were modelled with 60:40 occupancy of two related positions. Hydrogen atoms bonded to oxygen were all located and not further refined except for that bound to the disordered alcohol, which was not included in the refinement. The electron density on the 4~1~ axis is likely to be an artefact. ; _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^)+(0.0607P)^2^+60.4911P] 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 9961 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1430 _refine_ls_goodness_of_fit_ref 1.231 _refine_ls_restrained_S_all 1.231 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.559719(11) 0.140173(12) 0.39865(4) 0.03961(15) Uani 1 1 d . . . Zn2 Zn 0.539921(10) 0.127306(11) 0.07213(3) 0.03409(14) Uani 1 1 d . . . O1 O 0.59248(6) 0.11858(7) 0.30222(19) 0.0372(6) Uani 1 1 d . . . C1 C 0.62230(9) 0.10895(10) 0.3356(3) 0.0343(9) Uani 1 1 d . . . C2 C 0.63889(9) 0.12863(10) 0.4047(3) 0.0363(9) Uani 1 1 d . B . C3 C 0.66949(10) 0.11871(12) 0.4373(3) 0.0434(10) Uani 1 1 d . . . H3 H 0.6809 0.1321 0.4833 0.052 Uiso 1 1 calc R C . C4 C 0.68381(10) 0.09026(12) 0.4054(3) 0.0442(11) Uani 1 1 d . . . C5 C 0.71726(11) 0.08036(14) 0.4440(3) 0.0548(13) Uani 1 1 d . . . C6 C 0.71553(13) 0.07761(15) 0.5596(4) 0.0635(14) Uani 1 1 d . . . H6A H 0.6996 0.0611 0.5782 0.095 Uiso 1 1 calc R . . H6B H 0.7090 0.0985 0.5882 0.095 Uiso 1 1 calc R . . H6C H 0.7369 0.0715 0.5860 0.095 Uiso 1 1 calc R . . C7 C 0.74146(12) 0.10584(17) 0.4126(4) 0.0763(18) Uani 1 1 d . . . H7A H 0.7346 0.1270 0.4385 0.114 Uiso 1 1 calc R . . H7B H 0.7426 0.1067 0.3389 0.114 Uiso 1 1 calc R . . H7C H 0.7628 0.1004 0.4399 0.114 Uiso 1 1 calc R . . C8 C 0.72811(14) 0.04760(16) 0.4026(4) 0.0777(18) Uani 1 1 d . . . H8A H 0.7125 0.0309 0.4225 0.117 Uiso 1 1 calc R . . H8B H 0.7495 0.0422 0.4298 0.117 Uiso 1 1 calc R . . H8C H 0.7293 0.0487 0.3290 0.117 Uiso 1 1 calc R . . C9 C 0.66620(10) 0.07144(11) 0.3377(3) 0.0400(10) Uani 1 1 d . . . H9 H 0.6754 0.0517 0.3149 0.048 Uiso 1 1 calc R C . C10 C 0.63593(9) 0.08024(10) 0.3023(3) 0.0337(9) Uani 1 1 d . . . C11 C 0.61985(9) 0.05994(10) 0.2221(3) 0.0357(9) Uani 1 1 d . . . H11A H 0.6278 0.0374 0.2264 0.043 Uiso 1 1 calc R C . H11B H 0.5961 0.0597 0.2332 0.043 Uiso 1 1 calc R . . C12 C 0.62708(9) 0.07348(9) 0.1190(3) 0.0314(8) Uani 1 1 d . . . C13 C 0.65582(9) 0.06526(10) 0.0703(3) 0.0337(9) Uani 1 1 d . . . H13 H 0.6698 0.0499 0.1014 0.040 Uiso 1 1 calc R C . C14 C 0.66503(9) 0.07858(10) -0.0221(3) 0.0365(9) Uani 1 1 d . . . C15 C 0.69719(10) 0.07030(11) -0.0742(3) 0.0444(11) Uani 1 1 d . . . C16 C 0.71545(14) 0.04346(19) -0.0213(4) 0.087(2) Uani 1 1 d . . . H16A H 0.7357 0.0391 -0.0574 0.131 Uiso 1 1 calc R . . H16B H 0.7021 0.0238 -0.0202 0.131 Uiso 1 1 calc R . . H16C H 0.7204 0.0501 0.0478 0.131 Uiso 1 1 calc R . . C17 C 0.71792(13) 0.10111(16) -0.0807(6) 0.099(3) Uani 1 1 d . . . H17A H 0.7057 0.1182 -0.1152 0.148 Uiso 1 1 calc R . . H17B H 0.7378 0.0965 -0.1185 0.148 Uiso 1 1 calc R . . H17C H 0.7235 0.1084 -0.0127 0.148 Uiso 1 1 calc R . . C18 C 0.69058(13) 0.06011(13) -0.1821(3) 0.0565(13) Uani 1 1 d . . . H18A H 0.6789 0.0775 -0.2171 0.085 Uiso 1 1 calc R . . H18B H 0.6774 0.0404 -0.1824 0.085 Uiso 1 1 calc R . . H18C H 0.7112 0.0559 -0.2165 0.085 Uiso 1 1 calc R . . C19 C 0.64376(9) 0.10002(10) -0.0659(3) 0.0368(9) Uani 1 1 d . . . H19 H 0.6491 0.1090 -0.1297 0.044 Uiso 1 1 calc R C . C20 C 0.61435(9) 0.10917(10) -0.0197(3) 0.0341(9) Uani 1 1 d . . . C21 C 0.60611(9) 0.09618(10) 0.0749(3) 0.0311(8) Uani 1 1 d . . . O2 O 0.57940(6) 0.10500(7) 0.12495(19) 0.0344(6) Uani 1 1 d . . . C22 C 0.59503(10) 0.13294(10) -0.0728(3) 0.0373(9) Uani 1 1 d . . . H22 H 0.6041 0.1415 -0.1330 0.045 Uiso 1 1 calc R C . N1 N 0.56719(8) 0.14374(8) -0.0477(2) 0.0378(8) Uani 1 1 d . B . C23 C 0.55199(11) 0.16754(11) -0.1151(3) 0.0442(10) Uani 1 1 d . . . H23A H 0.5679 0.1743 -0.1669 0.053 Uiso 1 1 calc R A 1 H23B H 0.5459 0.1870 -0.0757 0.053 Uiso 1 1 calc R A 1 C24 C 0.52202(11) 0.15413(13) -0.1667(3) 0.0505(12) Uani 0.40 1 d P B 1 H24 H 0.5286 0.1323 -0.1924 0.061 Uiso 0.40 1 calc PR B 1 O3 O 0.5117(2) 0.1696(3) -0.2449(7) 0.074(3) Uani 0.40 1 d P B 1 C24' C 0.52202(11) 0.15413(13) -0.1667(3) 0.0505(12) Uani 0.60 1 d P B 2 H24' H 0.5145 0.1718 -0.2127 0.061 Uiso 0.60 1 calc PR B 2 O3' O 0.52817(12) 0.12882(12) -0.2264(4) 0.0432(11) Uani 0.60 1 d P B 2 C25 C 0.49375(11) 0.14767(11) -0.0967(3) 0.0459(11) Uani 1 1 d . . . H25A H 0.4880 0.1682 -0.0625 0.055 Uiso 1 1 calc R B 1 H25B H 0.4749 0.1410 -0.1378 0.055 Uiso 1 1 calc R B 1 N2 N 0.49962(8) 0.12274(8) -0.0197(3) 0.0364(8) Uani 1 1 d . B . C26 C 0.47972(9) 0.09903(10) -0.0177(3) 0.0346(9) Uani 1 1 d . . . H26 H 0.4638 0.0988 -0.0692 0.042 Uiso 1 1 calc R B . C27 C 0.47856(9) 0.07238(9) 0.0540(3) 0.0301(8) Uani 1 1 d . B . C28 C 0.45979(9) 0.04557(10) 0.0270(3) 0.0353(9) Uani 1 1 d . . . H28 H 0.4487 0.0460 -0.0356 0.042 Uiso 1 1 calc R B . C29 C 0.45666(9) 0.01845(10) 0.0872(3) 0.0341(9) Uani 1 1 d . B . C30 C 0.43703(11) -0.01108(11) 0.0531(3) 0.0448(11) Uani 1 1 d . . . C31 C 0.44079(15) -0.01637(14) -0.0586(4) 0.0690(16) Uani 1 1 d . B . H31A H 0.4639 -0.0178 -0.0754 0.104 Uiso 1 1 calc R . . H31B H 0.4310 0.0018 -0.0951 0.104 Uiso 1 1 calc R . . H31C H 0.4299 -0.0366 -0.0779 0.104 Uiso 1 1 calc R . . C32 C 0.40315(14) -0.00771(19) 0.0856(7) 0.122(4) Uani 1 1 d . B . H32A H 0.4024 -0.0042 0.1585 0.182 Uiso 1 1 calc R . . H32B H 0.3912 -0.0275 0.0688 0.182 Uiso 1 1 calc R . . H32C H 0.3932 0.0108 0.0511 0.182 Uiso 1 1 calc R . . C33 C 0.45167(19) -0.04245(13) 0.0994(5) 0.087(2) Uani 1 1 d . B . H33A H 0.4741 -0.0450 0.0767 0.130 Uiso 1 1 calc R . . H33B H 0.4389 -0.0612 0.0778 0.130 Uiso 1 1 calc R . . H33C H 0.4512 -0.0409 0.1731 0.130 Uiso 1 1 calc R . . C34 C 0.47189(9) 0.01970(10) 0.1801(3) 0.0338(9) Uani 1 1 d . . . H34 H 0.4695 0.0018 0.2243 0.041 Uiso 1 1 calc R B . C35 C 0.49060(9) 0.04600(10) 0.2120(3) 0.0315(8) Uani 1 1 d . B . C36 C 0.49441(8) 0.07232(9) 0.1475(3) 0.0287(8) Uani 1 1 d . . . O4 O 0.51336(6) 0.09796(7) 0.17247(19) 0.0349(6) Uani 1 1 d . B . C37 C 0.50754(9) 0.04438(11) 0.3136(3) 0.0383(9) Uani 1 1 d . . . H37A H 0.5076 0.0216 0.3365 0.046 Uiso 1 1 calc R B . H37B H 0.5304 0.0511 0.3044 0.046 Uiso 1 1 calc R . . C38 C 0.49271(9) 0.06507(11) 0.3956(3) 0.0381(10) Uani 1 1 d . B . C39 C 0.46928(9) 0.05199(12) 0.4602(3) 0.0414(10) Uani 1 1 d . . . H39 H 0.4624 0.0303 0.4502 0.050 Uiso 1 1 calc R B . C40 C 0.45578(10) 0.06986(13) 0.5389(3) 0.0457(11) Uani 1 1 d . B . C41 C 0.42999(11) 0.05572(14) 0.6104(3) 0.0516(12) Uani 1 1 d . . . C42 C 0.39812(11) 0.07409(15) 0.5944(4) 0.0650(15) Uani 1 1 d . B . H42A H 0.3815 0.0654 0.6398 0.098 Uiso 1 1 calc R . . H42B H 0.3910 0.0714 0.5244 0.098 Uiso 1 1 calc R . . H42C H 0.4014 0.0971 0.6085 0.098 Uiso 1 1 calc R . . C43 C 0.42289(13) 0.02023(15) 0.5891(5) 0.0717(17) Uani 1 1 d . B . H43A H 0.4065 0.0123 0.6366 0.108 Uiso 1 1 calc R . . H43B H 0.4428 0.0076 0.5967 0.108 Uiso 1 1 calc R . . H43C H 0.4147 0.0179 0.5201 0.108 Uiso 1 1 calc R . . C44 C 0.44213(16) 0.0579(2) 0.7180(4) 0.101(3) Uani 1 1 d . B . H44A H 0.4258 0.0489 0.7637 0.152 Uiso 1 1 calc R . . H44B H 0.4462 0.0806 0.7353 0.152 Uiso 1 1 calc R . . H44C H 0.4623 0.0455 0.7245 0.152 Uiso 1 1 calc R . . C45 C 0.46645(10) 0.10174(13) 0.5502(3) 0.0485(12) Uani 1 1 d . . . H45 H 0.4571 0.1146 0.6021 0.058 Uiso 1 1 calc R B . C46 C 0.49017(10) 0.11567(12) 0.4891(3) 0.0440(11) Uani 1 1 d . B . C47 C 0.50309(9) 0.09690(12) 0.4094(3) 0.0410(10) Uani 1 1 d . . . O5 O 0.52577(7) 0.10923(8) 0.3475(2) 0.0453(7) Uani 1 1 d . B . C48 C 0.49964(11) 0.14835(12) 0.5118(3) 0.0481(11) Uani 1 1 d . . . H48 H 0.4865 0.1597 0.5587 0.058 Uiso 1 1 calc R B . N3 N 0.52382(9) 0.16373(10) 0.4759(3) 0.0467(9) Uani 1 1 d . B . C49 C 0.52926(12) 0.19703(13) 0.5117(4) 0.0582(13) Uani 1 1 d . . . H49A H 0.5123 0.2028 0.5613 0.070 Uiso 1 1 calc R B . H49B H 0.5275 0.2122 0.4543 0.070 Uiso 1 1 calc R . . C50 C 0.56252(12) 0.20063(13) 0.5603(4) 0.0559(13) Uani 1 1 d . B . H50 H 0.5625 0.2217 0.5977 0.067 Uiso 1 1 calc R . . O6 O 0.56551(8) 0.17541(10) 0.6336(2) 0.0652(10) Uani 1 1 d . . . C51 C 0.59107(12) 0.20143(11) 0.4878(3) 0.0506(11) Uani 1 1 d . . . H51A H 0.5865 0.2173 0.4338 0.061 Uiso 1 1 calc R B . H51B H 0.6106 0.2088 0.5244 0.061 Uiso 1 1 calc R . . N4 N 0.59762(9) 0.16949(8) 0.4418(2) 0.0392(8) Uani 1 1 d . B . C52 C 0.62683(11) 0.15944(11) 0.4439(3) 0.0402(10) Uani 1 1 d . . . H52 H 0.6423 0.1734 0.4740 0.048 Uiso 1 1 calc R B . N11 N 0.5359(4) 0.1841(4) 0.2036(14) 0.044(4) Uani 0.60 1 d P C 1 O11 O 0.55610(18) 0.1659(2) 0.2417(6) 0.075(2) Uani 0.60 1 d P C 1 O12 O 0.52474(15) 0.17350(19) 0.1197(5) 0.0645(16) Uani 0.60 1 d P C 1 O13 O 0.5238(2) 0.20499(16) 0.2496(6) 0.0742(19) Uani 0.60 1 d P C 1 N11' N 0.5449(7) 0.1800(9) 0.1917(17) 0.068(9) Uani 0.40 1 d P C 2 O11' O 0.5363(3) 0.1559(3) 0.1956(10) 0.070(4) Uani 0.40 1 d P C 2 O12' O 0.5501(6) 0.1966(2) 0.1135(7) 0.165(9) Uani 0.40 1 d P C 2 O13' O 0.5494(4) 0.1973(3) 0.2749(7) 0.090(4) Uani 0.40 1 d P C 2 N21 N 0.63780(11) 0.14091(11) 0.6874(3) 0.0529(10) Uani 1 1 d . . . O21 O 0.62003(11) 0.11831(9) 0.6630(3) 0.0799(13) Uani 1 1 d . . . O22 O 0.62606(9) 0.16862(9) 0.6965(3) 0.0698(10) Uani 1 1 d . . . O23 O 0.66646(11) 0.13654(11) 0.7053(4) 0.0864(13) Uani 1 1 d . . . O61 O 0.57153(7) 0.10770(7) 0.5200(2) 0.0420(7) Uani 1 1 d . C . C61 C 0.57644(12) 0.07321(11) 0.5175(3) 0.0496(11) Uani 1 1 d . . . H61A H 0.6000 0.0685 0.5191 0.060 Uiso 1 1 calc R C . H61B H 0.5676 0.0644 0.4538 0.060 Uiso 1 1 calc R . . C62 C 0.56016(17) 0.05683(14) 0.6054(5) 0.0786(18) Uani 1 1 d . C . H62A H 0.5640 0.0334 0.6019 0.118 Uiso 1 1 calc R . . H62B H 0.5368 0.0611 0.6030 0.118 Uiso 1 1 calc R . . H62C H 0.5691 0.0653 0.6684 0.118 Uiso 1 1 calc R . . H1 H 0.5879 0.1117 0.2334 0.040 Uiso 1 1 d . . . H4 H 0.5197 0.1015 0.2515 0.040 Uiso 1 1 d . . . H6 H 0.5908 0.1722 0.6601 0.040 Uiso 1 1 d . . . H61 H 0.5873 0.1120 0.5696 0.040 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0346(3) 0.0527(3) 0.0316(3) -0.0131(2) 0.00117(19) -0.0017(2) Zn2 0.0284(2) 0.0407(3) 0.0332(3) 0.0010(2) 0.00534(18) -0.00131(19) O1 0.0286(14) 0.0575(18) 0.0255(14) -0.0129(12) -0.0017(11) -0.0009(12) C1 0.030(2) 0.052(2) 0.0213(18) -0.0015(17) 0.0017(15) -0.0064(17) C2 0.032(2) 0.053(2) 0.0243(19) -0.0049(17) 0.0014(16) -0.0096(18) C3 0.034(2) 0.069(3) 0.027(2) -0.004(2) -0.0044(17) -0.011(2) C4 0.036(2) 0.070(3) 0.027(2) 0.005(2) -0.0035(17) -0.002(2) C5 0.039(2) 0.088(4) 0.038(3) 0.005(2) -0.011(2) 0.004(2) C6 0.054(3) 0.092(4) 0.044(3) 0.011(3) -0.015(2) 0.000(3) C7 0.037(3) 0.133(6) 0.059(3) 0.024(3) -0.011(2) -0.005(3) C8 0.055(3) 0.114(5) 0.063(4) -0.013(3) -0.019(3) 0.032(3) C9 0.040(2) 0.052(3) 0.028(2) 0.0049(18) -0.0005(17) 0.0001(19) C10 0.029(2) 0.047(2) 0.0244(19) 0.0003(17) 0.0011(15) -0.0072(17) C11 0.032(2) 0.042(2) 0.033(2) -0.0040(18) 0.0016(17) -0.0039(17) C12 0.031(2) 0.038(2) 0.0258(19) -0.0105(16) 0.0016(15) -0.0078(16) C13 0.029(2) 0.039(2) 0.033(2) -0.0130(17) 0.0000(16) -0.0046(16) C14 0.029(2) 0.050(2) 0.031(2) -0.0195(18) 0.0052(16) -0.0095(18) C15 0.033(2) 0.054(3) 0.046(2) -0.019(2) 0.0112(19) -0.0026(19) C16 0.055(3) 0.157(7) 0.050(3) 0.002(4) 0.013(3) 0.048(4) C17 0.044(3) 0.097(5) 0.155(7) -0.075(5) 0.048(4) -0.032(3) C18 0.070(3) 0.058(3) 0.042(3) -0.010(2) 0.018(2) 0.014(3) C19 0.032(2) 0.052(2) 0.027(2) -0.0093(18) 0.0054(16) -0.0079(18) C20 0.028(2) 0.048(2) 0.0262(19) -0.0079(17) 0.0026(16) -0.0062(17) C21 0.0247(18) 0.043(2) 0.0251(19) -0.0099(16) 0.0023(15) -0.0073(16) O2 0.0262(13) 0.0540(17) 0.0230(13) -0.0027(12) 0.0043(10) 0.0013(12) C22 0.035(2) 0.050(2) 0.027(2) -0.0029(18) 0.0056(17) -0.0091(18) N1 0.0338(18) 0.048(2) 0.0313(18) 0.0033(15) 0.0033(14) -0.0046(15) C23 0.043(2) 0.051(3) 0.038(2) 0.013(2) 0.0058(19) -0.003(2) C24 0.043(3) 0.067(3) 0.041(3) 0.017(2) -0.002(2) -0.001(2) O3 0.060(6) 0.093(7) 0.069(6) 0.034(5) 0.000(5) 0.007(5) C24' 0.043(3) 0.067(3) 0.041(3) 0.017(2) -0.002(2) -0.001(2) O3' 0.053(3) 0.044(3) 0.033(3) -0.003(2) -0.003(2) -0.001(2) C25 0.040(2) 0.050(3) 0.047(3) 0.013(2) 0.001(2) 0.003(2) N2 0.0299(17) 0.0397(19) 0.0395(19) 0.0052(15) 0.0014(14) 0.0025(15) C26 0.033(2) 0.043(2) 0.029(2) -0.0019(17) 0.0004(16) 0.0027(17) C27 0.0256(18) 0.038(2) 0.0260(19) -0.0033(16) 0.0025(15) 0.0003(16) C28 0.035(2) 0.047(2) 0.0244(19) -0.0048(17) -0.0031(16) -0.0049(17) C29 0.032(2) 0.040(2) 0.031(2) -0.0067(17) 0.0051(16) -0.0037(17) C30 0.047(3) 0.048(3) 0.039(2) -0.013(2) 0.0073(19) -0.017(2) C31 0.098(4) 0.063(3) 0.046(3) -0.020(3) 0.006(3) -0.032(3) C32 0.052(4) 0.119(6) 0.193(9) -0.099(6) 0.051(5) -0.043(4) C33 0.126(6) 0.048(3) 0.086(4) -0.002(3) -0.019(4) -0.018(3) C34 0.031(2) 0.039(2) 0.031(2) -0.0018(17) 0.0072(16) -0.0021(17) C35 0.0248(18) 0.044(2) 0.0253(19) -0.0016(16) 0.0042(15) 0.0034(16) C36 0.0214(18) 0.038(2) 0.0269(19) -0.0056(16) 0.0042(14) -0.0011(15) O4 0.0322(14) 0.0467(16) 0.0257(13) -0.0048(12) 0.0002(11) -0.0099(12) C37 0.028(2) 0.057(3) 0.030(2) 0.0021(19) -0.0012(16) -0.0009(18) C38 0.026(2) 0.065(3) 0.0239(19) 0.0005(19) -0.0047(15) 0.0003(18) C39 0.029(2) 0.069(3) 0.026(2) 0.0063(19) -0.0021(16) 0.0018(19) C40 0.028(2) 0.083(3) 0.027(2) 0.010(2) 0.0000(17) 0.007(2) C41 0.037(2) 0.086(4) 0.031(2) 0.015(2) 0.0055(19) 0.005(2) C42 0.040(3) 0.097(4) 0.058(3) 0.021(3) 0.021(2) 0.015(3) C43 0.054(3) 0.088(4) 0.074(4) 0.028(3) 0.025(3) 0.008(3) C44 0.081(4) 0.186(8) 0.037(3) 0.032(4) -0.005(3) -0.027(5) C45 0.036(2) 0.084(4) 0.026(2) -0.004(2) 0.0040(18) 0.011(2) C46 0.034(2) 0.072(3) 0.026(2) -0.007(2) -0.0006(17) 0.004(2) C47 0.0242(19) 0.073(3) 0.026(2) -0.0055(19) -0.0001(16) -0.0027(19) O5 0.0343(15) 0.074(2) 0.0274(14) -0.0145(14) 0.0042(12) -0.0122(14) C48 0.037(2) 0.076(3) 0.031(2) -0.013(2) 0.0024(19) 0.007(2) N3 0.044(2) 0.062(2) 0.0338(19) -0.0142(17) -0.0004(16) 0.0047(18) C49 0.058(3) 0.062(3) 0.054(3) -0.023(2) 0.002(2) 0.010(2) C50 0.059(3) 0.067(3) 0.042(3) -0.021(2) 0.007(2) -0.004(2) O6 0.054(2) 0.110(3) 0.0322(17) -0.0057(19) 0.0052(15) -0.013(2) C51 0.062(3) 0.049(3) 0.041(3) -0.013(2) 0.008(2) -0.006(2) N4 0.047(2) 0.044(2) 0.0262(17) -0.0059(15) 0.0054(15) -0.0073(16) C52 0.045(3) 0.051(3) 0.024(2) -0.0062(18) 0.0012(17) -0.015(2) N11 0.048(6) 0.030(7) 0.054(7) -0.012(5) 0.007(5) 0.007(6) O11 0.065(4) 0.097(6) 0.064(5) 0.020(5) 0.024(4) 0.024(5) O12 0.056(4) 0.079(5) 0.059(4) -0.024(4) 0.002(3) 0.001(3) O13 0.099(6) 0.051(4) 0.073(5) -0.020(4) 0.003(5) -0.005(4) N11' 0.12(2) 0.055(10) 0.034(10) -0.017(9) -0.049(13) 0.047(15) O11' 0.072(8) 0.043(6) 0.097(10) -0.037(6) 0.049(7) -0.032(5) O12' 0.43(3) 0.034(5) 0.030(5) 0.001(4) -0.007(10) -0.039(10) O13' 0.144(12) 0.089(9) 0.036(5) -0.001(5) -0.023(6) -0.074(9) N21 0.067(3) 0.060(3) 0.032(2) 0.0075(19) -0.0032(19) -0.005(2) O21 0.114(3) 0.062(2) 0.064(2) 0.0040(19) -0.039(2) -0.028(2) O22 0.063(2) 0.056(2) 0.090(3) -0.017(2) -0.004(2) -0.0112(18) O23 0.081(3) 0.086(3) 0.092(3) 0.022(2) -0.024(3) 0.001(2) O61 0.0447(17) 0.0480(17) 0.0334(15) -0.0033(13) -0.0018(13) -0.0093(13) C61 0.055(3) 0.049(3) 0.045(3) -0.004(2) -0.002(2) -0.008(2) C62 0.112(5) 0.062(4) 0.062(4) 0.008(3) 0.014(3) -0.020(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 2.014(3) . ? Zn1 N3 2.048(4) . ? Zn1 N4 2.059(3) . ? Zn1 O1 2.065(3) . ? Zn1 O61 2.152(3) . ? Zn1 O11 2.344(8) . ? Zn1 O13' 2.906(13) . ? Zn1 O11' 2.938(16) . ? Zn2 O2 1.999(3) . ? Zn2 O11' 2.025(10) . ? Zn2 N1 2.065(3) . ? Zn2 N2 2.071(3) . ? Zn2 O12 2.104(7) . ? Zn2 O4 2.108(3) . ? O1 C1 1.367(5) . ? C1 C10 1.384(6) . ? C1 C2 1.404(5) . ? C2 C3 1.396(6) . ? C2 C52 1.461(6) . ? C3 C4 1.381(7) . ? C4 C9 1.393(6) . ? C4 C5 1.529(6) . ? C5 C7 1.509(8) . ? C5 C8 1.527(8) . ? C5 C6 1.541(7) . ? C9 C10 1.384(6) . ? C10 C11 1.509(5) . ? C11 C12 1.509(5) . ? C12 C13 1.393(5) . ? C12 C21 1.403(6) . ? C13 C14 1.398(6) . ? C14 C19 1.376(6) . ? C14 C15 1.536(5) . ? C15 C16 1.513(8) . ? C15 C18 1.519(6) . ? C15 C17 1.535(7) . ? C19 C20 1.412(5) . ? C20 C21 1.408(5) . ? C20 C22 1.448(6) . ? C21 O2 1.338(4) . ? C22 N1 1.277(5) . ? N1 C23 1.469(5) . ? C23 C24 1.519(6) . ? C24 O3 1.292(10) . ? C24 C25 1.515(6) . ? C25 N2 1.471(5) . ? N2 C26 1.278(5) . ? C26 C27 1.455(5) . ? C27 C28 1.398(5) . ? C27 C36 1.404(5) . ? C28 C29 1.382(6) . ? C29 C34 1.387(6) . ? C29 C30 1.532(5) . ? C30 C32 1.470(7) . ? C30 C31 1.507(6) . ? C30 C33 1.556(8) . ? C34 C35 1.398(5) . ? C35 C36 1.393(5) . ? C35 C37 1.521(5) . ? C36 O4 1.357(4) . ? C37 C38 1.514(6) . ? C38 C47 1.394(6) . ? C38 C39 1.401(6) . ? C39 C40 1.395(6) . ? C40 C45 1.396(7) . ? C40 C41 1.542(6) . ? C41 C44 1.517(7) . ? C41 C43 1.521(8) . ? C41 C42 1.533(7) . ? C45 C46 1.396(6) . ? C46 C47 1.416(6) . ? C46 C48 1.437(7) . ? C47 O5 1.346(5) . ? C48 N3 1.275(6) . ? N3 C49 1.472(6) . ? C49 C50 1.524(7) . ? C50 O6 1.430(6) . ? C50 C51 1.523(6) . ? C51 N4 1.478(5) . ? N4 C52 1.275(6) . ? N11 O13 1.168(18) . ? N11 O11 1.232(17) . ? N11 O12 1.283(19) . ? N11' O11' 1.06(3) . ? N11' O12' 1.26(3) . ? N11' O13' 1.33(3) . ? N21 O23 1.220(6) . ? N21 O21 1.230(5) . ? N21 O22 1.248(5) . ? O61 C61 1.438(5) . ? C61 C62 1.508(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zn1 N3 88.09(13) . . ? O5 Zn1 N4 174.35(13) . . ? N3 Zn1 N4 97.54(14) . . ? O5 Zn1 O1 88.44(11) . . ? N3 Zn1 O1 171.73(13) . . ? N4 Zn1 O1 85.92(12) . . ? O5 Zn1 O61 90.87(12) . . ? N3 Zn1 O61 94.84(14) . . ? N4 Zn1 O61 89.17(12) . . ? O1 Zn1 O61 92.72(11) . . ? O5 Zn1 O11 86.7(3) . . ? N3 Zn1 O11 100.6(2) . . ? N4 Zn1 O11 91.7(3) . . ? O1 Zn1 O11 71.66(19) . . ? O61 Zn1 O11 164.2(2) . . ? O5 Zn1 O13' 102.8(2) . . ? N3 Zn1 O13' 78.0(3) . . ? N4 Zn1 O13' 78.0(2) . . ? O1 Zn1 O13' 95.5(3) . . ? O61 Zn1 O13' 164.21(19) . . ? O11 Zn1 O13' 28.4(3) . . ? O5 Zn1 O11' 66.51(19) . . ? N3 Zn1 O11' 96.7(2) . . ? N4 Zn1 O11' 112.08(19) . . ? O1 Zn1 O11' 75.0(2) . . ? O61 Zn1 O11' 154.1(2) . . ? O11 Zn1 O11' 20.4(3) . . ? O13' Zn1 O11' 41.7(3) . . ? O2 Zn2 O11' 92.5(5) . . ? O2 Zn2 N1 88.71(12) . . ? O11' Zn2 N1 118.3(3) . . ? O2 Zn2 N2 145.05(12) . . ? O11' Zn2 N2 118.1(4) . . ? N1 Zn2 N2 90.78(13) . . ? O2 Zn2 O12 123.7(2) . . ? O11' Zn2 O12 37.6(4) . . ? N1 Zn2 O12 95.5(2) . . ? N2 Zn2 O12 91.2(2) . . ? O2 Zn2 O4 86.42(11) . . ? O11' Zn2 O4 77.5(3) . . ? N1 Zn2 O4 163.70(12) . . ? N2 Zn2 O4 84.40(11) . . ? O12 Zn2 O4 100.1(2) . . ? C1 O1 Zn1 120.9(2) . . ? O1 C1 C10 120.7(3) . . ? O1 C1 C2 118.9(4) . . ? C10 C1 C2 120.4(4) . . ? C3 C2 C1 118.3(4) . . ? C3 C2 C52 117.0(4) . . ? C1 C2 C52 124.7(4) . . ? C4 C3 C2 122.8(4) . . ? C3 C4 C9 116.7(4) . . ? C3 C4 C5 120.7(4) . . ? C9 C4 C5 122.6(4) . . ? C7 C5 C8 108.8(5) . . ? C7 C5 C4 108.6(4) . . ? C8 C5 C4 112.4(4) . . ? C7 C5 C6 110.9(4) . . ? C8 C5 C6 107.9(5) . . ? C4 C5 C6 108.2(4) . . ? C10 C9 C4 123.0(4) . . ? C9 C10 C1 118.9(4) . . ? C9 C10 C11 119.4(4) . . ? C1 C10 C11 121.5(3) . . ? C12 C11 C10 110.4(3) . . ? C13 C12 C21 119.6(4) . . ? C13 C12 C11 120.0(4) . . ? C21 C12 C11 120.3(3) . . ? C12 C13 C14 122.9(4) . . ? C19 C14 C13 116.9(4) . . ? C19 C14 C15 120.2(4) . . ? C13 C14 C15 122.9(4) . . ? C16 C15 C18 109.0(4) . . ? C16 C15 C17 110.8(5) . . ? C18 C15 C17 106.0(5) . . ? C16 C15 C14 112.6(4) . . ? C18 C15 C14 109.4(4) . . ? C17 C15 C14 108.8(4) . . ? C14 C19 C20 122.4(4) . . ? C21 C20 C19 119.6(4) . . ? C21 C20 C22 124.0(3) . . ? C19 C20 C22 116.3(4) . . ? O2 C21 C12 118.8(3) . . ? O2 C21 C20 122.6(4) . . ? C12 C21 C20 118.6(3) . . ? C21 O2 Zn2 128.5(2) . . ? N1 C22 C20 127.3(4) . . ? C22 N1 C23 117.3(3) . . ? C22 N1 Zn2 125.2(3) . . ? C23 N1 Zn2 117.2(3) . . ? N1 C23 C24 112.3(4) . . ? O3 C24 C25 109.0(5) . . ? O3 C24 C23 116.8(6) . . ? C25 C24 C23 114.5(4) . . ? N2 C25 C24 115.0(4) . . ? C26 N2 C25 116.4(3) . . ? C26 N2 Zn2 125.0(3) . . ? C25 N2 Zn2 118.6(3) . . ? N2 C26 C27 127.9(4) . . ? C28 C27 C36 119.0(3) . . ? C28 C27 C26 116.7(3) . . ? C36 C27 C26 124.4(3) . . ? C29 C28 C27 123.0(4) . . ? C28 C29 C34 116.3(4) . . ? C28 C29 C30 121.5(4) . . ? C34 C29 C30 122.2(4) . . ? C32 C30 C31 113.6(5) . . ? C32 C30 C29 109.9(4) . . ? C31 C30 C29 110.6(4) . . ? C32 C30 C33 109.4(6) . . ? C31 C30 C33 103.2(5) . . ? C29 C30 C33 109.8(4) . . ? C29 C34 C35 123.3(4) . . ? C36 C35 C34 118.8(3) . . ? C36 C35 C37 121.9(3) . . ? C34 C35 C37 119.3(4) . . ? O4 C36 C35 121.5(3) . . ? O4 C36 C27 118.9(3) . . ? C35 C36 C27 119.6(3) . . ? C36 O4 Zn2 126.4(2) . . ? C38 C37 C35 115.3(3) . . ? C47 C38 C39 119.7(4) . . ? C47 C38 C37 120.1(4) . . ? C39 C38 C37 120.2(4) . . ? C40 C39 C38 122.1(4) . . ? C39 C40 C45 117.0(4) . . ? C39 C40 C41 122.5(5) . . ? C45 C40 C41 120.5(4) . . ? C44 C41 C43 107.2(5) . . ? C44 C41 C42 112.7(5) . . ? C43 C41 C42 106.6(4) . . ? C44 C41 C40 109.3(4) . . ? C43 C41 C40 112.5(4) . . ? C42 C41 C40 108.6(4) . . ? C40 C45 C46 123.1(4) . . ? C45 C46 C47 118.3(4) . . ? C45 C46 C48 117.1(4) . . ? C47 C46 C48 124.7(4) . . ? O5 C47 C38 119.4(4) . . ? O5 C47 C46 120.8(4) . . ? C38 C47 C46 119.9(4) . . ? C47 O5 Zn1 121.2(2) . . ? N3 C48 C46 127.0(4) . . ? C48 N3 C49 117.6(4) . . ? C48 N3 Zn1 121.1(3) . . ? C49 N3 Zn1 119.7(3) . . ? N3 C49 C50 111.4(4) . . ? O6 C50 C51 112.3(4) . . ? O6 C50 C49 107.2(4) . . ? C51 C50 C49 115.5(4) . . ? N4 C51 C50 112.6(4) . . ? C52 N4 C51 117.0(4) . . ? C52 N4 Zn1 122.2(3) . . ? C51 N4 Zn1 120.0(3) . . ? N4 C52 C2 126.7(4) . . ? O13 N11 O11 121.6(17) . . ? O13 N11 O12 123.6(15) . . ? O11 N11 O12 113.1(13) . . ? N11 O11 Zn1 133.3(8) . . ? N11 O12 Zn2 117.6(8) . . ? O11' N11' O12' 127(3) . . ? O11' N11' O13' 121(2) . . ? O12' N11' O13' 112(3) . . ? N11' O11' Zn2 118.9(16) . . ? N11' O11' Zn1 98.2(15) . . ? Zn2 O11' Zn1 126.2(7) . . ? N11' O13' Zn1 93.2(15) . . ? O23 N21 O21 121.2(5) . . ? O23 N21 O22 119.5(5) . . ? O21 N21 O22 119.3(5) . . ? C61 O61 Zn1 129.1(2) . . ? O61 C61 C62 111.3(4) . . ? 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 O1 H1 O2 0.98 1.51 2.480(3) 173.3 . O4 H4 O5 1.09 1.34 2.426(4) 173.3 . O6 H6 O22 1.11 1.54 2.650(5) 178.6 . O6 H6 O21 1.11 2.53 3.282(6) 123.9 . O61 H61 O21 0.94 1.85 2.794(5) 176.1 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.941 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.080 data_Complex8a _database_code_depnum_ccdc_archive 'CCDC 249427' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62.70 H90.50 Cl2 Mn2 N6.50 O9.80 S' _chemical_formula_weight 1304.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8935(8) _cell_length_b 19.5914(13) _cell_length_c 32.009(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.6830(10) _cell_angle_gamma 90.00 _cell_volume 7329.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10567 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.82 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2762 _exptl_absorpt_coefficient_mu 0.499 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.881341 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 51860 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12907 _reflns_number_gt 9375 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. [Mn2(H2L)Cl2(dmf)(dmso)].1.5dmf.0.3Et2O (7.1.5dmf.0.3Et2O): In addition to the coordinated dmf and dmso molecules, the lattice contained a partial-occupancy ether molecule, refined isotropically with 30% occupancy, one disordered dmf molecule, modeled as 50% occupancy of each of two overlapping sites and a further 50% occupancy dmf molecule. One of the pendant alcohol groups of the macrocycle was disordered and refined with 50% occupancy of two related positions (O3 and O3') and one of the t-butyl groups was modeled with 60:40 occupancy of two positions. The hydrogen atoms of the pendant alcohols were not located or included in the model. ; _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^)+(0.1037P)^2^+13.4069P] 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 12907 _refine_ls_number_parameters 866 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0658 _refine_ls_wR_factor_ref 0.2055 _refine_ls_wR_factor_gt 0.1874 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.083 _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 Mn1 Mn -0.01663(6) 0.22443(3) 0.67412(2) 0.03040(19) Uani 1 1 d . . . Mn2 Mn 0.37516(5) 0.53528(3) 0.691896(19) 0.02441(17) Uani 1 1 d . . . O1 O 0.0396(3) 0.28896(15) 0.71633(9) 0.0333(7) Uani 1 1 d . . . C1 C -0.0159(4) 0.3152(2) 0.74487(14) 0.0305(10) Uani 1 1 d . . . C2 C -0.1008(4) 0.2782(2) 0.76114(15) 0.0347(10) Uani 1 1 d . B . C3 C -0.1504(4) 0.3057(2) 0.79401(15) 0.0372(11) Uani 1 1 d . . . H3 H -0.2047 0.2792 0.8053 0.045 Uiso 1 1 calc R . . C4 C -0.1229(4) 0.3697(2) 0.81043(16) 0.0388(11) Uani 1 1 d . . . C5 C -0.1741(5) 0.4010(3) 0.84655(18) 0.0466(13) Uani 1 1 d . . . C6 C -0.2466(7) 0.3491(4) 0.8653(2) 0.078(2) Uani 1 1 d . . . H6A H -0.3070 0.3317 0.8428 0.117 Uiso 1 1 calc R . . H6B H -0.2812 0.3711 0.8873 0.117 Uiso 1 1 calc R . . H6C H -0.1981 0.3112 0.8778 0.117 Uiso 1 1 calc R . . C7 C -0.2551(7) 0.4602(4) 0.8282(3) 0.085(2) Uani 1 1 d . . . H7A H -0.3166 0.4424 0.8063 0.128 Uiso 1 1 calc R . . H7B H -0.2116 0.4947 0.8157 0.128 Uiso 1 1 calc R . . H7C H -0.2880 0.4809 0.8511 0.128 Uiso 1 1 calc R . . C8 C -0.0802(6) 0.4275(5) 0.8805(2) 0.101(3) Uani 1 1 d . . . H8A H -0.0343 0.4608 0.8681 0.152 Uiso 1 1 calc R . . H8B H -0.0314 0.3896 0.8927 0.152 Uiso 1 1 calc R . . H8C H -0.1135 0.4496 0.9028 0.152 Uiso 1 1 calc R . . C9 C -0.0445(4) 0.4073(2) 0.79173(15) 0.0376(11) Uani 1 1 d . . . H9 H -0.0278 0.4528 0.8011 0.045 Uiso 1 1 calc R . . C10 C 0.0100(4) 0.3815(2) 0.76025(14) 0.0328(10) Uani 1 1 d . . . C11 C 0.0973(4) 0.4244(2) 0.74342(14) 0.0335(10) Uani 1 1 d . . . H11A H 0.0654 0.4707 0.7370 0.040 Uiso 1 1 calc R . . H11B H 0.1107 0.4042 0.7164 0.040 Uiso 1 1 calc R . . C12 C 0.2115(4) 0.4306(2) 0.77385(14) 0.0295(9) Uani 1 1 d . . . C13 C 0.2373(4) 0.3958(2) 0.81197(14) 0.0334(10) Uani 1 1 d . . . H13 H 0.1826 0.3643 0.8188 0.040 Uiso 1 1 calc R . . C14 C 0.3405(4) 0.4045(2) 0.84118(15) 0.0369(11) Uani 1 1 d . . . C15 C 0.3610(5) 0.3619(3) 0.88217(16) 0.0465(13) Uani 1 1 d . . . C16 C 0.3750(8) 0.2873(3) 0.8707(2) 0.082(2) Uani 1 1 d . . . H16A H 0.3879 0.2596 0.8967 0.123 Uiso 1 1 calc R . . H16B H 0.4406 0.2827 0.8564 0.123 Uiso 1 1 calc R . . H16C H 0.3055 0.2716 0.8517 0.123 Uiso 1 1 calc R . . C17 C 0.2587(6) 0.3694(4) 0.9045(2) 0.0710(19) Uani 1 1 d . . . H17A H 0.2718 0.3422 0.9307 0.106 Uiso 1 1 calc R . . H17B H 0.1893 0.3532 0.8857 0.106 Uiso 1 1 calc R . . H17C H 0.2494 0.4175 0.9115 0.106 Uiso 1 1 calc R . . C18 C 0.4667(6) 0.3858(4) 0.9125(2) 0.076(2) Uani 1 1 d . . . H18A H 0.4776 0.3580 0.9384 0.114 Uiso 1 1 calc R . . H18B H 0.4573 0.4338 0.9199 0.114 Uiso 1 1 calc R . . H18C H 0.5337 0.3813 0.8989 0.114 Uiso 1 1 calc R . . C19 C 0.4186(4) 0.4497(2) 0.83025(15) 0.0351(10) Uani 1 1 d . . . H19 H 0.4879 0.4580 0.8497 0.042 Uiso 1 1 calc R . . C20 C 0.3979(4) 0.4844(2) 0.79078(14) 0.0292(9) Uani 1 1 d . . . C21 C 0.2937(4) 0.4754(2) 0.76221(13) 0.0262(9) Uani 1 1 d . . . O2 O 0.2685(2) 0.50849(14) 0.72588(9) 0.0258(6) Uani 1 1 d . . . C22 C 0.4814(4) 0.5330(2) 0.78216(14) 0.0305(10) Uani 1 1 d . . . H22 H 0.5390 0.5463 0.8054 0.037 Uiso 1 1 calc R . . N1 N 0.4853(3) 0.56019(17) 0.74593(11) 0.0280(8) Uani 1 1 d . B . C23 C 0.5714(4) 0.6141(2) 0.74518(15) 0.0354(10) Uani 1 1 d . . . H23A H 0.6208 0.6171 0.7736 0.042 Uiso 1 1 calc R A 1 H23B H 0.5318 0.6584 0.7392 0.042 Uiso 1 1 calc R A 1 C24 C 0.6460(4) 0.6018(3) 0.71230(16) 0.0421(12) Uani 0.50 1 d P B 1 H24 H 0.6771 0.5545 0.7171 0.051 Uiso 0.50 1 calc PR B 1 O3 O 0.7388(6) 0.6446(4) 0.7146(2) 0.0478(18) Uani 0.50 1 d P B 1 C24' C 0.6460(4) 0.6018(3) 0.71230(16) 0.0421(12) Uani 0.50 1 d P B 2 H24' H 0.6986 0.6421 0.7151 0.051 Uiso 0.50 1 calc PR B 2 O3' O 0.7136(6) 0.5494(3) 0.7223(2) 0.0426(16) Uani 0.50 1 d P B 2 C25 C 0.5824(4) 0.6045(2) 0.66681(14) 0.0356(10) Uani 1 1 d . . . H25A H 0.5442 0.6495 0.6617 0.043 Uiso 1 1 calc R B 1 H25B H 0.6385 0.6009 0.6476 0.043 Uiso 1 1 calc R B 1 N2 N 0.4961(3) 0.55064(17) 0.65584(11) 0.0274(8) Uani 1 1 d . B . C26 C 0.4980(4) 0.5165(2) 0.62115(14) 0.0300(9) Uani 1 1 d . . . H26 H 0.5612 0.5246 0.6075 0.036 Uiso 1 1 calc R B . C27 C 0.4146(4) 0.4680(2) 0.60137(14) 0.0290(9) Uani 1 1 d . B . C28 C 0.4362(4) 0.4320(2) 0.56601(14) 0.0354(10) Uani 1 1 d . . . H28 H 0.5064 0.4394 0.5566 0.042 Uiso 1 1 calc R B . C29 C 0.3580(4) 0.3857(2) 0.54406(15) 0.0376(11) Uani 1 1 d . B . C30 C 0.3840(5) 0.3468(3) 0.50492(17) 0.0475(13) Uani 1 1 d . . . C31 C 0.4854(7) 0.2981(4) 0.5192(2) 0.083(2) Uani 1 1 d . B . H31A H 0.5022 0.2733 0.4945 0.125 Uiso 1 1 calc R . . H31B H 0.4658 0.2656 0.5400 0.125 Uiso 1 1 calc R . . H31C H 0.5527 0.3246 0.5323 0.125 Uiso 1 1 calc R . . C32 C 0.4183(6) 0.3960(4) 0.47334(19) 0.0693(18) Uani 1 1 d . B . H32A H 0.4347 0.3707 0.4488 0.104 Uiso 1 1 calc R . . H32B H 0.4868 0.4211 0.4868 0.104 Uiso 1 1 calc R . . H32C H 0.3557 0.4282 0.4640 0.104 Uiso 1 1 calc R . . C33 C 0.2824(6) 0.3058(4) 0.4836(2) 0.092(3) Uani 1 1 d . B . H33A H 0.3016 0.2817 0.4590 0.138 Uiso 1 1 calc R . . H33B H 0.2176 0.3365 0.4741 0.138 Uiso 1 1 calc R . . H33C H 0.2617 0.2726 0.5037 0.138 Uiso 1 1 calc R . . C34 C 0.2549(4) 0.3774(2) 0.55844(14) 0.0341(10) Uani 1 1 d . . . H34 H 0.2009 0.3455 0.5442 0.041 Uiso 1 1 calc R B . C35 C 0.2275(4) 0.4135(2) 0.59230(13) 0.0283(9) Uani 1 1 d . B . C36 C 0.3076(4) 0.4607(2) 0.61426(13) 0.0271(9) Uani 1 1 d . . . O4 O 0.2771(2) 0.49739(14) 0.64496(9) 0.0271(6) Uani 1 1 d . B . C37 C 0.1137(4) 0.4071(2) 0.60719(15) 0.0345(10) Uani 1 1 d . . . H37A H 0.1285 0.3909 0.6370 0.041 Uiso 1 1 calc R B . H37B H 0.0787 0.4530 0.6068 0.041 Uiso 1 1 calc R . . C38 C 0.0291(4) 0.3595(2) 0.58097(14) 0.0308(10) Uani 1 1 d . B . C39 C -0.0239(4) 0.3779(2) 0.54032(15) 0.0379(11) Uani 1 1 d . . . H39 H -0.0056 0.4212 0.5300 0.046 Uiso 1 1 calc R B . C40 C -0.1027(4) 0.3371(3) 0.51328(15) 0.0404(11) Uani 1 1 d . B . C41 C -0.1564(5) 0.3614(4) 0.46908(19) 0.0673(19) Uani 1 1 d . . . C42 C -0.105(3) 0.4231(11) 0.4497(10) 0.087(10) Uani 0.40 1 d P B 1 H42A H -0.0245 0.4283 0.4631 0.130 Uiso 0.40 1 calc PR B 1 H42B H -0.1473 0.4645 0.4545 0.130 Uiso 0.40 1 calc PR B 1 H42C H -0.1109 0.4160 0.4190 0.130 Uiso 0.40 1 calc PR B 1 C43 C -0.0979(19) 0.3022(9) 0.4354(4) 0.083(6) Uani 0.40 1 d P B 1 H43A H -0.0142 0.3045 0.4419 0.125 Uiso 0.40 1 calc PR B 1 H43B H -0.1251 0.3142 0.4055 0.125 Uiso 0.40 1 calc PR B 1 H43C H -0.1228 0.2558 0.4406 0.125 Uiso 0.40 1 calc PR B 1 C44 C -0.273(2) 0.356(3) 0.4540(13) 0.27(4) Uani 0.40 1 d P B 1 H44A H -0.2911 0.3763 0.4255 0.405 Uiso 0.40 1 calc PR B 1 H44B H -0.3142 0.3809 0.4731 0.405 Uiso 0.40 1 calc PR B 1 H44C H -0.2953 0.3081 0.4527 0.405 Uiso 0.40 1 calc PR B 1 C42' C -0.0766(16) 0.3890(9) 0.4463(5) 0.078(5) Uani 0.60 1 d PU B 2 H42D H -0.1163 0.4039 0.4182 0.117 Uiso 0.60 1 calc PR B 2 H42E H -0.0198 0.3541 0.4430 0.117 Uiso 0.60 1 calc PR B 2 H42F H -0.0381 0.4281 0.4619 0.117 Uiso 0.60 1 calc PR B 2 C43' C -0.2300(11) 0.4325(6) 0.4800(4) 0.079(4) Uani 0.60 1 d PU B 2 H43D H -0.2880 0.4193 0.4966 0.119 Uiso 0.60 1 calc PR B 2 H43E H -0.2674 0.4537 0.4533 0.119 Uiso 0.60 1 calc PR B 2 H43F H -0.1766 0.4650 0.4964 0.119 Uiso 0.60 1 calc PR B 2 C44' C -0.2475(13) 0.3155(8) 0.4481(4) 0.072(4) Uani 0.60 1 d PU B 2 H44D H -0.2947 0.3013 0.4686 0.108 Uiso 0.60 1 calc PR B 2 H44E H -0.2131 0.2752 0.4374 0.108 Uiso 0.60 1 calc PR B 2 H44F H -0.2952 0.3394 0.4244 0.108 Uiso 0.60 1 calc PR B 2 C45 C -0.1275(4) 0.2743(3) 0.52969(15) 0.0384(11) Uani 1 1 d . . . H45 H -0.1789 0.2443 0.5123 0.046 Uiso 1 1 calc R B . C46 C -0.0789(4) 0.2537(2) 0.57120(14) 0.0321(10) Uani 1 1 d . B . C47 C 0.0020(4) 0.2952(2) 0.59737(13) 0.0286(9) Uani 1 1 d . . . O5 O 0.0534(2) 0.27612(15) 0.63605(9) 0.0314(7) Uani 1 1 d . B . C48 C -0.1120(4) 0.1888(2) 0.58562(15) 0.0371(11) Uani 1 1 d . . . H48 H -0.1528 0.1592 0.5646 0.045 Uiso 1 1 calc R B . N3 N -0.0922(3) 0.16632(18) 0.62412(12) 0.0351(9) Uani 1 1 d . B . C49 C -0.1344(5) 0.0968(2) 0.63081(17) 0.0489(13) Uani 1 1 d . . . H49A H -0.0685 0.0664 0.6412 0.059 Uiso 1 1 calc R B . H49B H -0.1757 0.0784 0.6034 0.059 Uiso 1 1 calc R . . C50 C -0.2138(5) 0.0974(3) 0.66280(17) 0.0524(14) Uani 1 1 d . B . H50 H -0.2489 0.0510 0.6621 0.063 Uiso 1 1 calc R . . O6 O -0.3066(3) 0.1449(2) 0.65142(14) 0.0622(11) Uani 1 1 d . . . C51 C -0.1511(6) 0.1088(2) 0.70785(16) 0.0521(15) Uani 1 1 d . . . H51A H -0.2033 0.0990 0.7279 0.062 Uiso 1 1 calc R B . H51B H -0.0858 0.0767 0.7142 0.062 Uiso 1 1 calc R . . N4 N -0.1086(4) 0.17938(19) 0.71423(13) 0.0386(9) Uani 1 1 d . B . C52 C -0.1361(4) 0.2102(2) 0.74636(15) 0.0386(11) Uani 1 1 d . . . H52 H -0.1840 0.1861 0.7619 0.046 Uiso 1 1 calc R B . Cl1 Cl 0.13183(13) 0.13357(7) 0.69457(5) 0.0581(4) Uani 1 1 d . . . Cl2 Cl 0.31491(11) 0.65600(6) 0.68023(4) 0.0392(3) Uani 1 1 d . . . O61 O -0.1843(3) 0.28697(16) 0.65679(10) 0.0370(7) Uani 1 1 d . . . S61 S -0.18015(10) 0.36386(6) 0.65269(4) 0.0395(3) Uani 1 1 d . . . C61 C -0.2720(6) 0.3980(3) 0.6858(2) 0.0643(17) Uani 1 1 d . . . H61A H -0.2364 0.3920 0.7157 0.097 Uiso 1 1 calc R . . H61B H -0.3456 0.3741 0.6801 0.097 Uiso 1 1 calc R . . H61C H -0.2844 0.4468 0.6797 0.097 Uiso 1 1 calc R . . C62 C -0.2657(5) 0.3824(3) 0.60262(18) 0.0541(14) Uani 1 1 d . . . H62A H -0.2267 0.3666 0.5800 0.081 Uiso 1 1 calc R . . H62B H -0.2782 0.4318 0.6000 0.081 Uiso 1 1 calc R . . H62C H -0.3395 0.3591 0.6002 0.081 Uiso 1 1 calc R . . O71 O 0.4584(3) 0.42655(15) 0.70331(10) 0.0338(7) Uani 1 1 d . . . C71 C 0.3822(4) 0.3766(2) 0.70378(14) 0.0355(11) Uani 1 1 d . . . H71 H 0.3083 0.3801 0.6866 0.043 Uiso 1 1 calc R . . N71 N 0.4079(4) 0.3246(2) 0.72691(16) 0.0506(11) Uani 1 1 d . . . C72 C 0.3161(5) 0.2761(3) 0.7283(2) 0.0666(18) Uani 1 1 d . . . H72A H 0.2445 0.2938 0.7116 0.100 Uiso 1 1 calc R . . H72B H 0.3071 0.2696 0.7579 0.100 Uiso 1 1 calc R . . H72C H 0.3348 0.2324 0.7165 0.100 Uiso 1 1 calc R . . C73 C 0.5183(6) 0.3114(4) 0.7534(2) 0.077(2) Uani 1 1 d . . . H73A H 0.5542 0.2722 0.7420 0.115 Uiso 1 1 calc R . . H73B H 0.5081 0.3012 0.7824 0.115 Uiso 1 1 calc R . . H73C H 0.5673 0.3517 0.7536 0.115 Uiso 1 1 calc R . . O81 O -0.3790(10) 0.5491(7) 0.9042(5) 0.120(5) Uani 0.50 1 d PD . . C81 C -0.3901(16) 0.6127(9) 0.8924(5) 0.123(9) Uani 0.50 1 d PD . . H81 H -0.4635 0.6253 0.8772 0.050 Uiso 0.50 1 calc P . . N81 N -0.3227(10) 0.6562(8) 0.8980(5) 0.108(6) Uani 0.50 1 d PD . . C82 C -0.2075(10) 0.6481(8) 0.9196(4) 0.077(4) Uani 0.50 1 d PD . . H82A H -0.2069 0.6275 0.9476 0.050 Uiso 0.50 1 calc PR . . H82B H -0.1701 0.6929 0.9233 0.050 Uiso 0.50 1 calc PR . . H82C H -0.1662 0.6185 0.9030 0.050 Uiso 0.50 1 calc PR . . C83 C -0.3675(19) 0.7182(8) 0.8743(4) 0.159(12) Uani 0.50 1 d PD . . H83A H -0.4503 0.7213 0.8732 0.050 Uiso 0.50 1 calc PR . . H83B H -0.3520 0.7159 0.8453 0.050 Uiso 0.50 1 calc PR . . H83C H -0.3301 0.7586 0.8887 0.050 Uiso 0.50 1 calc PR . . O91 O -0.2010(18) 0.5348(11) 0.6166(9) 0.098(9) Uani 0.50 1 d PD C 1 C91 C -0.1532(14) 0.5936(6) 0.6178(4) 0.060(4) Uani 0.50 1 d PD C 1 H91 H -0.1836 0.6281 0.5981 0.050 Uiso 0.50 1 calc P D 1 N91 N -0.0716(4) 0.6043(3) 0.6436(2) 0.0697(16) Uani 0.50 1 d PD C 1 C92 C -0.018(2) 0.5595(9) 0.6751(6) 0.138(13) Uani 0.50 1 d PD C 1 H92A H -0.0428 0.5693 0.7019 0.050 Uiso 0.50 1 calc PR C 1 H92B H 0.0655 0.5654 0.6789 0.050 Uiso 0.50 1 calc PR C 1 H92C H -0.0376 0.5124 0.6665 0.050 Uiso 0.50 1 calc PR C 1 C93 C -0.0413(15) 0.6805(6) 0.6492(5) 0.076(4) Uani 0.50 1 d PD C 1 H93A H -0.0735 0.7052 0.6231 0.050 Uiso 0.50 1 calc PR C 1 H93B H 0.0421 0.6859 0.6551 0.050 Uiso 0.50 1 calc PR C 1 H93C H -0.0731 0.6990 0.6730 0.050 Uiso 0.50 1 calc PR C 1 O91' O -0.2227(13) 0.5501(11) 0.6093(6) 0.064(5) Uani 0.50 1 d PD E 2 C91' C -0.1169(14) 0.5571(9) 0.6261(5) 0.120(11) Uani 0.50 1 d PD E 2 H91' H -0.0695 0.5188 0.6239 0.050 Uiso 0.50 1 calc P F 2 N91' N -0.0716(4) 0.6043(3) 0.6436(2) 0.0697(16) Uani 0.50 1 d PD E 2 C92' C 0.0317(14) 0.5826(9) 0.6715(5) 0.083(6) Uani 0.50 1 d PD E 2 H92D H 0.0136 0.5685 0.6988 0.050 Uiso 0.50 1 calc PR E 2 H92E H 0.0864 0.6205 0.6760 0.050 Uiso 0.50 1 calc PR E 2 H92F H 0.0653 0.5441 0.6586 0.050 Uiso 0.50 1 calc PR E 2 C93' C -0.1250(13) 0.6690(7) 0.6451(7) 0.087(5) Uani 0.50 1 d PD E 2 H93D H -0.1885 0.6734 0.6209 0.050 Uiso 0.50 1 calc PR E 2 H93E H -0.0690 0.7053 0.6439 0.050 Uiso 0.50 1 calc PR E 2 H93F H -0.1544 0.6729 0.6717 0.050 Uiso 0.50 1 calc PR E 2 C101 C -0.4158(16) 0.1021(10) 0.5341(6) 0.053(5) Uiso 0.30 1 d PD . . H10A H -0.4923 0.0817 0.5304 0.050 Uiso 0.30 1 calc PR . . H10B H -0.4204 0.1467 0.5201 0.050 Uiso 0.30 1 calc PR . . H10C H -0.3852 0.1077 0.5645 0.050 Uiso 0.30 1 calc PR . . C102 C -0.3424(14) 0.0586(9) 0.5159(6) 0.051(4) Uiso 0.30 1 d PD . . H10D H -0.3411 0.0137 0.5302 0.050 Uiso 0.30 1 calc PR . . H10E H -0.3779 0.0515 0.4857 0.050 Uiso 0.30 1 calc PR . . O101 O -0.2465(9) 0.0756(6) 0.5170(4) 0.044(3) Uiso 0.30 1 d PD . . C103 C -0.1865(18) 0.0407(12) 0.4985(8) 0.076(6) Uiso 0.30 1 d PD . . H10F H -0.2199 0.0418 0.4678 0.050 Uiso 0.30 1 calc PR . . H10G H -0.1909 -0.0071 0.5081 0.050 Uiso 0.30 1 calc PR . . C104 C -0.069(2) 0.059(2) 0.5033(13) 0.150(15) Uiso 0.30 1 d PD . . H10H H -0.0304 0.0263 0.4873 0.050 Uiso 0.30 1 calc PR . . H10I H -0.0338 0.0568 0.5335 0.050 Uiso 0.30 1 calc PR . . H10J H -0.0625 0.1049 0.4924 0.050 Uiso 0.30 1 calc PR . . 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 0.0356(4) 0.0230(3) 0.0320(4) 0.0014(3) 0.0045(3) -0.0004(3) Mn2 0.0262(3) 0.0202(3) 0.0275(3) -0.0007(2) 0.0067(3) -0.0018(3) O1 0.0356(17) 0.0319(17) 0.0338(17) -0.0029(13) 0.0103(13) -0.0061(13) C1 0.031(2) 0.031(2) 0.030(2) 0.0050(18) 0.0052(18) -0.0019(19) C2 0.040(3) 0.028(2) 0.037(3) 0.0053(19) 0.010(2) -0.006(2) C3 0.036(3) 0.033(3) 0.044(3) 0.006(2) 0.013(2) -0.004(2) C4 0.038(3) 0.038(3) 0.044(3) 0.000(2) 0.016(2) -0.004(2) C5 0.049(3) 0.043(3) 0.055(3) -0.012(2) 0.027(3) -0.012(2) C6 0.109(6) 0.064(4) 0.081(5) -0.012(4) 0.065(4) -0.016(4) C7 0.097(6) 0.064(4) 0.109(6) 0.004(4) 0.058(5) 0.024(4) C8 0.069(5) 0.170(9) 0.073(5) -0.066(5) 0.038(4) -0.029(5) C9 0.039(3) 0.035(3) 0.041(3) -0.004(2) 0.013(2) -0.010(2) C10 0.034(2) 0.030(2) 0.036(2) 0.0009(19) 0.0103(19) -0.0103(19) C11 0.037(3) 0.032(2) 0.034(2) -0.0046(19) 0.013(2) -0.011(2) C12 0.033(2) 0.026(2) 0.032(2) -0.0049(18) 0.0118(18) -0.0019(18) C13 0.036(3) 0.029(2) 0.039(3) 0.004(2) 0.017(2) -0.0045(19) C14 0.040(3) 0.034(3) 0.039(3) 0.008(2) 0.014(2) 0.001(2) C15 0.049(3) 0.050(3) 0.042(3) 0.016(2) 0.012(2) 0.002(2) C16 0.130(7) 0.059(4) 0.065(4) 0.033(3) 0.038(4) 0.020(4) C17 0.069(4) 0.096(5) 0.055(4) 0.030(4) 0.029(3) 0.009(4) C18 0.067(4) 0.105(6) 0.051(4) 0.040(4) -0.001(3) -0.004(4) C19 0.036(3) 0.035(3) 0.035(2) 0.005(2) 0.009(2) 0.002(2) C20 0.034(2) 0.024(2) 0.032(2) -0.0006(18) 0.0093(18) 0.0000(18) C21 0.032(2) 0.019(2) 0.029(2) -0.0022(17) 0.0098(18) -0.0015(17) O2 0.0257(15) 0.0235(15) 0.0285(15) -0.0005(12) 0.0058(12) -0.0009(12) C22 0.029(2) 0.031(2) 0.031(2) 0.0013(19) 0.0027(18) -0.0011(19) N1 0.0311(19) 0.0220(18) 0.032(2) -0.0004(15) 0.0083(15) -0.0054(15) C23 0.041(3) 0.029(2) 0.035(2) -0.0002(19) 0.006(2) -0.015(2) C24 0.039(3) 0.046(3) 0.042(3) 0.001(2) 0.009(2) -0.014(2) O3 0.042(4) 0.054(4) 0.048(4) -0.001(3) 0.011(3) -0.031(3) C24' 0.039(3) 0.046(3) 0.042(3) 0.001(2) 0.009(2) -0.014(2) O3' 0.038(4) 0.037(4) 0.052(4) -0.001(3) 0.007(3) -0.003(3) C25 0.038(3) 0.035(3) 0.035(2) -0.001(2) 0.010(2) -0.013(2) N2 0.0289(19) 0.0216(18) 0.0316(19) 0.0025(15) 0.0056(15) -0.0025(14) C26 0.029(2) 0.030(2) 0.032(2) 0.0046(19) 0.0090(18) 0.0003(18) C27 0.029(2) 0.027(2) 0.032(2) -0.0001(18) 0.0073(18) 0.0000(18) C28 0.034(2) 0.040(3) 0.035(2) -0.002(2) 0.014(2) 0.001(2) C29 0.043(3) 0.037(3) 0.036(3) -0.009(2) 0.014(2) -0.003(2) C30 0.048(3) 0.054(3) 0.045(3) -0.019(3) 0.020(2) -0.006(3) C31 0.117(6) 0.067(4) 0.075(5) -0.010(4) 0.041(4) 0.030(4) C32 0.094(5) 0.077(5) 0.041(3) -0.010(3) 0.025(3) -0.005(4) C33 0.082(5) 0.118(6) 0.087(5) -0.070(5) 0.045(4) -0.040(5) C34 0.041(3) 0.030(2) 0.033(2) -0.0056(19) 0.010(2) -0.008(2) C35 0.034(2) 0.022(2) 0.030(2) 0.0014(17) 0.0091(18) -0.0032(18) C36 0.032(2) 0.021(2) 0.029(2) 0.0032(17) 0.0078(18) 0.0006(17) O4 0.0267(15) 0.0269(15) 0.0285(15) -0.0037(12) 0.0075(12) 0.0016(12) C37 0.033(2) 0.035(3) 0.037(3) -0.003(2) 0.009(2) -0.008(2) C38 0.027(2) 0.032(2) 0.034(2) 0.0003(19) 0.0086(18) -0.0017(18) C39 0.041(3) 0.032(2) 0.040(3) 0.006(2) 0.006(2) -0.005(2) C40 0.036(3) 0.047(3) 0.037(3) 0.012(2) 0.001(2) -0.003(2) C41 0.060(4) 0.080(5) 0.052(4) 0.033(3) -0.017(3) -0.025(3) C42 0.10(2) 0.066(15) 0.075(15) 0.025(14) -0.029(14) -0.031(14) C43 0.150(18) 0.077(12) 0.021(7) 0.001(7) 0.009(9) 0.028(12) C44 0.025(11) 0.56(10) 0.22(4) 0.30(6) 0.012(17) 0.03(3) C42' 0.077(9) 0.118(13) 0.036(6) 0.036(9) 0.000(5) -0.014(10) C43' 0.071(8) 0.068(7) 0.083(8) 0.026(6) -0.028(6) -0.001(6) C44' 0.073(10) 0.100(9) 0.030(5) 0.023(6) -0.026(5) -0.016(7) C45 0.035(3) 0.040(3) 0.038(3) -0.002(2) 0.000(2) -0.006(2) C46 0.036(2) 0.027(2) 0.033(2) -0.0005(19) 0.0049(19) -0.0019(19) C47 0.028(2) 0.028(2) 0.030(2) 0.0012(18) 0.0064(18) 0.0007(18) O5 0.0291(16) 0.0332(17) 0.0306(16) 0.0010(13) 0.0021(13) -0.0021(13) C48 0.043(3) 0.030(2) 0.037(3) -0.002(2) 0.004(2) -0.006(2) N3 0.045(2) 0.0223(19) 0.037(2) 0.0002(16) 0.0071(17) -0.0011(17) C49 0.074(4) 0.026(3) 0.044(3) -0.002(2) 0.004(3) -0.011(2) C50 0.076(4) 0.034(3) 0.048(3) 0.000(2) 0.014(3) -0.021(3) O6 0.054(2) 0.064(3) 0.067(3) 0.000(2) 0.010(2) -0.015(2) C51 0.089(4) 0.025(2) 0.041(3) 0.005(2) 0.010(3) -0.019(3) N4 0.052(2) 0.025(2) 0.038(2) 0.0005(17) 0.0049(19) -0.0081(18) C52 0.044(3) 0.035(3) 0.037(3) 0.007(2) 0.008(2) -0.007(2) Cl1 0.0561(8) 0.0415(7) 0.0695(9) 0.0002(7) -0.0072(7) 0.0172(6) Cl2 0.0535(7) 0.0237(5) 0.0427(6) 0.0018(5) 0.0145(5) 0.0084(5) O61 0.0343(17) 0.0300(17) 0.0467(19) 0.0018(14) 0.0076(14) -0.0014(14) S61 0.0355(6) 0.0284(6) 0.0534(8) 0.0008(5) 0.0057(5) 0.0047(5) C61 0.066(4) 0.064(4) 0.063(4) -0.008(3) 0.011(3) 0.032(3) C62 0.053(3) 0.050(3) 0.058(3) 0.013(3) 0.006(3) 0.017(3) O71 0.0343(17) 0.0287(17) 0.0393(18) 0.0057(14) 0.0093(14) 0.0055(14) C71 0.045(3) 0.039(3) 0.026(2) 0.016(2) 0.016(2) 0.030(2) N71 0.040(2) 0.038(2) 0.072(3) -0.006(2) 0.007(2) -0.001(2) C72 0.056(4) 0.039(3) 0.104(5) 0.014(3) 0.013(4) -0.005(3) C73 0.063(4) 0.061(4) 0.094(5) 0.035(4) -0.017(4) -0.005(3) O81 0.081(8) 0.145(13) 0.136(11) -0.039(10) 0.027(8) -0.019(8) C81 0.16(2) 0.15(2) 0.068(11) 0.023(13) 0.038(12) 0.099(19) N81 0.075(10) 0.126(14) 0.138(14) -0.035(11) 0.060(10) -0.045(9) C82 0.055(8) 0.104(11) 0.079(9) 0.002(8) 0.035(7) -0.027(8) C83 0.35(4) 0.097(13) 0.056(9) -0.029(9) 0.107(16) -0.118(18) O91 0.077(11) 0.068(12) 0.140(17) 0.031(9) -0.004(9) 0.009(9) C91 0.107(12) 0.037(7) 0.038(7) -0.002(5) 0.019(8) -0.010(8) N91 0.043(3) 0.087(5) 0.083(4) 0.026(4) 0.020(3) 0.006(3) C92 0.22(3) 0.129(19) 0.050(10) 0.022(11) -0.013(13) -0.107(19) C93 0.103(12) 0.052(8) 0.065(9) 0.000(7) -0.009(9) 0.028(8) O91' 0.064(8) 0.062(10) 0.071(8) -0.010(9) 0.025(7) -0.007(9) C91' 0.123(17) 0.18(2) 0.039(8) -0.046(11) -0.033(9) 0.139(18) N91' 0.043(3) 0.087(5) 0.083(4) 0.026(4) 0.020(3) 0.006(3) C92' 0.093(12) 0.076(11) 0.064(10) -0.001(9) -0.027(9) 0.052(11) C93' 0.057(9) 0.067(10) 0.138(16) -0.003(10) 0.021(10) 0.006(8) _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 O1 1.881(3) . ? Mn1 O5 1.892(3) . ? Mn1 N3 2.033(4) . ? Mn1 N4 2.036(4) . ? Mn1 O61 2.318(3) . ? Mn1 Cl1 2.5073(14) . ? Mn2 O4 1.876(3) . ? Mn2 O2 1.892(3) . ? Mn2 N1 2.026(4) . ? Mn2 N2 2.027(4) . ? Mn2 O71 2.349(3) . ? Mn2 Cl2 2.4792(12) . ? O1 C1 1.327(5) . ? C1 C10 1.403(6) . ? C1 C2 1.418(6) . ? C2 C3 1.405(7) . ? C2 C52 1.450(7) . ? C3 C4 1.375(7) . ? C4 C9 1.406(6) . ? C4 C5 1.531(7) . ? C5 C8 1.499(9) . ? C5 C6 1.525(8) . ? C5 C7 1.552(9) . ? C9 C10 1.390(6) . ? C10 C11 1.510(6) . ? C11 C12 1.523(6) . ? C12 C13 1.382(6) . ? C12 C21 1.414(6) . ? C13 C14 1.409(7) . ? C14 C19 1.376(6) . ? C14 C15 1.535(7) . ? C15 C18 1.514(8) . ? C15 C16 1.523(9) . ? C15 C17 1.529(8) . ? C19 C20 1.415(6) . ? C20 C21 1.409(6) . ? C20 C22 1.440(6) . ? C21 O2 1.317(5) . ? C22 N1 1.284(6) . ? N1 C23 1.474(5) . ? C23 C24 1.516(7) . ? C24 O3 1.376(8) . ? C24 C25 1.512(7) . ? C25 N2 1.469(5) . ? N2 C26 1.300(6) . ? C26 C27 1.435(6) . ? C27 C28 1.397(6) . ? C27 C36 1.416(6) . ? C28 C29 1.392(7) . ? C29 C34 1.397(6) . ? C29 C30 1.546(6) . ? C30 C33 1.505(8) . ? C30 C32 1.507(8) . ? C30 C31 1.538(9) . ? C34 C35 1.382(6) . ? C35 C36 1.417(6) . ? C35 C37 1.521(6) . ? C36 O4 1.322(5) . ? C37 C38 1.508(6) . ? C38 C39 1.385(6) . ? C38 C47 1.425(6) . ? C39 C40 1.401(7) . ? C40 C45 1.391(7) . ? C40 C41 1.517(7) . ? C41 C44 1.38(3) . ? C41 C42' 1.408(18) . ? C41 C44' 1.470(15) . ? C41 C42 1.54(3) . ? C41 C43' 1.715(15) . ? C41 C43 1.808(18) . ? C45 C46 1.406(6) . ? C46 C47 1.410(6) . ? C46 C48 1.432(6) . ? C47 O5 1.329(5) . ? C48 N3 1.289(6) . ? N3 C49 1.481(6) . ? C49 C50 1.516(8) . ? C50 O6 1.439(7) . ? C50 C51 1.512(8) . ? C51 N4 1.474(6) . ? N4 C52 1.286(6) . ? O61 S61 1.514(3) . ? S61 C62 1.770(5) . ? S61 C61 1.787(6) . ? O71 C71 1.336(6) . ? C71 N71 1.262(6) . ? N71 C73 1.448(7) . ? N71 C72 1.455(7) . ? O81 C81 1.301(16) . ? C81 N81 1.161(17) . ? N81 C82 1.425(14) . ? N81 C83 1.478(16) . ? O91 C91 1.282(17) . ? C91 N91 1.170(13) . ? N91 C92 1.400(14) . ? N91 C93 1.539(12) . ? O91' C91' 1.280(18) . ? C101 C102 1.42(2) . ? C102 O101 1.183(17) . ? O101 C103 1.219(18) . ? C103 C104 1.42(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 Mn1 O5 87.85(13) . . ? O1 Mn1 N3 171.38(15) . . ? O5 Mn1 N3 88.63(14) . . ? O1 Mn1 N4 89.97(14) . . ? O5 Mn1 N4 172.00(15) . . ? N3 Mn1 N4 92.45(16) . . ? O1 Mn1 O61 89.56(13) . . ? O5 Mn1 O61 91.43(12) . . ? N3 Mn1 O61 82.66(14) . . ? N4 Mn1 O61 80.86(14) . . ? O1 Mn1 Cl1 98.63(11) . . ? O5 Mn1 Cl1 100.10(10) . . ? N3 Mn1 Cl1 89.73(11) . . ? N4 Mn1 Cl1 87.84(12) . . ? O61 Mn1 Cl1 166.05(9) . . ? O4 Mn2 O2 88.12(12) . . ? O4 Mn2 N1 170.59(13) . . ? O2 Mn2 N1 88.41(13) . . ? O4 Mn2 N2 90.23(13) . . ? O2 Mn2 N2 172.28(13) . . ? N1 Mn2 N2 92.05(14) . . ? O4 Mn2 O71 86.97(12) . . ? O2 Mn2 O71 88.12(11) . . ? N1 Mn2 O71 84.18(13) . . ? N2 Mn2 O71 84.26(12) . . ? O4 Mn2 Cl2 97.90(9) . . ? O2 Mn2 Cl2 98.36(9) . . ? N1 Mn2 Cl2 91.25(10) . . ? N2 Mn2 Cl2 89.34(10) . . ? O71 Mn2 Cl2 171.98(9) . . ? C1 O1 Mn1 126.8(3) . . ? O1 C1 C10 119.7(4) . . ? O1 C1 C2 122.3(4) . . ? C10 C1 C2 118.0(4) . . ? C3 C2 C1 120.3(4) . . ? C3 C2 C52 117.4(4) . . ? C1 C2 C52 122.2(4) . . ? C4 C3 C2 122.2(4) . . ? C3 C4 C9 116.4(4) . . ? C3 C4 C5 123.6(4) . . ? C9 C4 C5 120.0(4) . . ? C8 C5 C6 110.2(6) . . ? C8 C5 C4 109.8(4) . . ? C6 C5 C4 111.3(4) . . ? C8 C5 C7 109.9(6) . . ? C6 C5 C7 106.9(5) . . ? C4 C5 C7 108.6(5) . . ? C10 C9 C4 123.6(4) . . ? C9 C10 C1 119.3(4) . . ? C9 C10 C11 120.0(4) . . ? C1 C10 C11 120.7(4) . . ? C10 C11 C12 114.0(4) . . ? C13 C12 C21 119.2(4) . . ? C13 C12 C11 123.4(4) . . ? C21 C12 C11 117.4(4) . . ? C12 C13 C14 123.4(4) . . ? C19 C14 C13 117.1(4) . . ? C19 C14 C15 124.0(5) . . ? C13 C14 C15 118.9(4) . . ? C18 C15 C16 109.7(6) . . ? C18 C15 C17 108.0(5) . . ? C16 C15 C17 109.6(5) . . ? C18 C15 C14 111.2(5) . . ? C16 C15 C14 108.8(5) . . ? C17 C15 C14 109.5(4) . . ? C14 C19 C20 121.5(4) . . ? C21 C20 C19 120.4(4) . . ? C21 C20 C22 120.9(4) . . ? C19 C20 C22 118.5(4) . . ? O2 C21 C20 122.7(4) . . ? O2 C21 C12 118.9(4) . . ? C20 C21 C12 118.4(4) . . ? C21 O2 Mn2 125.2(3) . . ? N1 C22 C20 126.1(4) . . ? C22 N1 C23 116.9(4) . . ? C22 N1 Mn2 123.1(3) . . ? C23 N1 Mn2 120.0(3) . . ? N1 C23 C24 113.3(4) . . ? O3 C24 C25 106.5(5) . . ? O3 C24 C23 115.7(5) . . ? C25 C24 C23 114.2(4) . . ? N2 C25 C24 114.1(4) . . ? C26 N2 C25 116.8(4) . . ? C26 N2 Mn2 122.5(3) . . ? C25 N2 Mn2 120.6(3) . . ? N2 C26 C27 126.7(4) . . ? C28 C27 C36 119.7(4) . . ? C28 C27 C26 118.4(4) . . ? C36 C27 C26 121.6(4) . . ? C29 C28 C27 122.1(4) . . ? C28 C29 C34 117.0(4) . . ? C28 C29 C30 121.0(4) . . ? C34 C29 C30 122.0(4) . . ? C33 C30 C32 109.3(6) . . ? C33 C30 C31 108.9(6) . . ? C32 C30 C31 107.5(5) . . ? C33 C30 C29 111.5(4) . . ? C32 C30 C29 110.3(5) . . ? C31 C30 C29 109.1(5) . . ? C35 C34 C29 123.2(4) . . ? C34 C35 C36 119.2(4) . . ? C34 C35 C37 123.8(4) . . ? C36 C35 C37 117.0(4) . . ? O4 C36 C27 123.1(4) . . ? O4 C36 C35 118.2(4) . . ? C27 C36 C35 118.6(4) . . ? C36 O4 Mn2 126.6(3) . . ? C38 C37 C35 114.7(4) . . ? C39 C38 C47 118.8(4) . . ? C39 C38 C37 120.2(4) . . ? C47 C38 C37 121.0(4) . . ? C38 C39 C40 124.6(4) . . ? C45 C40 C39 115.8(4) . . ? C45 C40 C41 123.2(5) . . ? C39 C40 C41 121.0(5) . . ? C44 C41 C42' 125.0(15) . . ? C44 C41 C44' 36(3) . . ? C42' C41 C44' 120.6(11) . . ? C44 C41 C40 121.7(13) . . ? C42' C41 C40 113.3(8) . . ? C44' C41 C40 112.4(7) . . ? C44 C41 C42 111(2) . . ? C42' C41 C42 29.8(13) . . ? C44' C41 C42 127.7(12) . . ? C40 C41 C42 119.6(11) . . ? C44 C41 C43' 67(3) . . ? C42' C41 C43' 102.3(10) . . ? C44' C41 C43' 103.3(8) . . ? C40 C41 C43' 101.9(6) . . ? C42 C41 C43' 72.5(13) . . ? C44 C41 C43 102(3) . . ? C42' C41 C43 64.3(10) . . ? C44' C41 C43 70.6(10) . . ? C40 C41 C43 102.3(7) . . ? C42 C41 C43 92.2(14) . . ? C43' C41 C43 155.5(7) . . ? C40 C45 C46 122.1(4) . . ? C45 C46 C47 120.7(4) . . ? C45 C46 C48 118.0(4) . . ? C47 C46 C48 121.2(4) . . ? O5 C47 C46 122.5(4) . . ? O5 C47 C38 119.7(4) . . ? C46 C47 C38 117.8(4) . . ? C47 O5 Mn1 124.7(3) . . ? N3 C48 C46 126.8(4) . . ? C48 N3 C49 116.5(4) . . ? C48 N3 Mn1 122.5(3) . . ? C49 N3 Mn1 120.9(3) . . ? N3 C49 C50 111.1(4) . . ? O6 C50 C51 111.5(5) . . ? O6 C50 C49 112.3(4) . . ? C51 C50 C49 112.7(5) . . ? N4 C51 C50 111.4(4) . . ? C52 N4 C51 114.8(4) . . ? C52 N4 Mn1 123.1(3) . . ? C51 N4 Mn1 122.0(3) . . ? N4 C52 C2 126.3(4) . . ? S61 O61 Mn1 120.42(18) . . ? O61 S61 C62 105.1(2) . . ? O61 S61 C61 106.7(3) . . ? C62 S61 C61 98.5(3) . . ? C71 O71 Mn2 113.5(2) . . ? N71 C71 O71 120.5(4) . . ? C71 N71 C73 125.6(5) . . ? C71 N71 C72 116.3(5) . . ? C73 N71 C72 118.0(5) . . ? N81 C81 O81 128.9(18) . . ? C81 N81 C82 124.6(16) . . ? C81 N81 C83 110.6(14) . . ? C82 N81 C83 124.3(13) . . ? N91 C91 O91 119.1(15) . . ? C91 N91 C92 127.3(11) . . ? C91 N91 C93 113.7(9) . . ? C92 N91 C93 117.2(11) . . ? O101 C102 C101 118.9(17) . . ? C102 O101 C103 118.5(18) . . ? O101 C103 C104 117(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.200 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.097