# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global #TrackingRef '- Compound 1-3.cif' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Chen, Zilu' _publ_contact_author_email chenziluczl@yahoo.co.uk _publ_section_title ; Structure, adsorption and magnetic properties of four chiral flexible Metal-Organic Frameworks bearing linear trinuclear secondary building blocks ; loop_ _publ_author_name 'Zilu Chen.' 'Xianlin Liu.' 'Chuanbing Zhang.' 'Zhong Zhang.' 'Fupei Liang.' # Attachment '1.cif' data_b _database_code_depnum_ccdc_archive 'CCDC 794252' #TrackingRef '- Compound 1-3.cif' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H68 Co3 N14 O18, 28(H2 O)' _chemical_formula_sum 'C76 H124 Co3 N14 O46' _chemical_formula_weight 2146.68 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' 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 P21212 _symmetry_space_group_name_Hall 'P 2 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 18.657(4) _cell_length_b 24.380(5) _cell_length_c 11.400(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5185.4(18) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 13649 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2254 _exptl_absorpt_coefficient_mu 0.569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8044 _exptl_absorpt_correction_T_max 0.9453 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15524 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.1091 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8497 _reflns_number_gt 6640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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. ; _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^)+(0.0729P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0048(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 8497 _refine_ls_number_parameters 633 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.1725 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.083 _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 0.5000 0.5000 0.45986(10) 0.0228(3) Uani 1 2 d S . . Co2 Co 0.69972(4) 0.48131(3) 0.46481(7) 0.0266(2) Uani 1 1 d . . . C1 C 0.6175(3) 0.3985(2) 0.4622(6) 0.0263(12) Uani 1 1 d . . . C2 C 0.5706(3) 0.3473(2) 0.4666(6) 0.0296(13) Uani 1 1 d . . . H2 H 0.5254 0.3550 0.4244 0.036 Uiso 1 1 calc R . . C3 C 0.5525(4) 0.3320(3) 0.5935(6) 0.0385(17) Uani 1 1 d . . . H3A H 0.5954 0.3191 0.6329 0.058 Uiso 1 1 calc R . . H3B H 0.5166 0.3032 0.5939 0.058 Uiso 1 1 calc R . . H3C H 0.5339 0.3639 0.6340 0.058 Uiso 1 1 calc R . . C4 C 0.6146(3) 0.2983(3) 0.2942(6) 0.0354(16) Uani 1 1 d . . . C5 C 0.6612(4) 0.2530(3) 0.2479(6) 0.0338(15) Uani 1 1 d . . . C6 C 0.6502(4) 0.2314(3) 0.1376(6) 0.0390(16) Uani 1 1 d . . . H6 H 0.6112 0.2436 0.0924 0.047 Uiso 1 1 calc R . . C7 C 0.6952(4) 0.1924(3) 0.0930(6) 0.0415(17) Uani 1 1 d . . . C8 C 0.7524(4) 0.1728(3) 0.1595(6) 0.0395(17) Uani 1 1 d . . . H8 H 0.7842 0.1468 0.1276 0.047 Uiso 1 1 calc R . . C9 C 0.7622(4) 0.1921(3) 0.2744(6) 0.0392(16) Uani 1 1 d . . . C10 C 0.7171(4) 0.2341(2) 0.3171(6) 0.0332(15) Uani 1 1 d . . . H10 H 0.7250 0.2491 0.3919 0.040 Uiso 1 1 calc R . . C11 C 0.6835(4) 0.1691(3) -0.0264(7) 0.0472(18) Uani 1 1 d . . . C12 C 0.5523(5) 0.1873(5) -0.2429(8) 0.078(3) Uani 1 1 d . . . H12A H 0.5355 0.2240 -0.2255 0.117 Uiso 1 1 calc R . . H12B H 0.5291 0.1613 -0.1908 0.117 Uiso 1 1 calc R . . H12C H 0.5409 0.1782 -0.3236 0.117 Uiso 1 1 calc R . . C13 C 0.6325(4) 0.1847(3) -0.2254(6) 0.0454(19) Uani 1 1 d . . . H13 H 0.6476 0.1461 -0.2364 0.054 Uiso 1 1 calc R . . C14 C 0.6721(4) 0.2193(4) -0.3149(7) 0.053(2) Uani 1 1 d . . . C15 C 0.8208(4) 0.1689(3) 0.3478(6) 0.0355(16) Uani 1 1 d . . . C16 C 0.8527(4) 0.1711(3) 0.6669(6) 0.0465(19) Uani 1 1 d . . . H16A H 0.8064 0.1570 0.6912 0.070 Uiso 1 1 calc R . . H16B H 0.8520 0.2109 0.6701 0.070 Uiso 1 1 calc R . . H16C H 0.8896 0.1573 0.7189 0.070 Uiso 1 1 calc R . . C17 C 0.8684(3) 0.1525(2) 0.5410(6) 0.0319(14) Uani 1 1 d . . . H17 H 0.9144 0.1687 0.5150 0.038 Uiso 1 1 calc R . . C18 C 0.8741(3) 0.0898(2) 0.5367(5) 0.0252(12) Uani 1 1 d . . . C19 C 0.7368(4) 0.5218(3) 0.8346(5) 0.0373(15) Uani 1 1 d . . . H19 H 0.7593 0.5514 0.8725 0.045 Uiso 1 1 calc R . . C20 C 0.7340(3) 0.5198(3) 0.7141(5) 0.0365(15) Uani 1 1 d . . . H20 H 0.7550 0.5487 0.6718 0.044 Uiso 1 1 calc R . . C21 C 0.6755(4) 0.4382(3) 0.7181(6) 0.0378(16) Uani 1 1 d . . . H21 H 0.6539 0.4087 0.6786 0.045 Uiso 1 1 calc R . . C22 C 0.6768(4) 0.4364(3) 0.8384(6) 0.0394(17) Uani 1 1 d . . . H22 H 0.6579 0.4060 0.8785 0.047 Uiso 1 1 calc R . . C23 C 0.7061(3) 0.4797(3) 0.9000(5) 0.0334(14) Uani 1 1 d . . . C24 C 0.7063(3) 0.4793(3) 1.0300(6) 0.0320(13) Uani 1 1 d . . . C25 C 0.7218(4) 0.4329(3) 1.0946(6) 0.0475(19) Uani 1 1 d . . . H25 H 0.7342 0.4002 1.0561 0.057 Uiso 1 1 calc R . . C26 C 0.7190(4) 0.4344(3) 1.2164(6) 0.0435(18) Uani 1 1 d . . . H26 H 0.7310 0.4026 1.2589 0.052 Uiso 1 1 calc R . . C27 C 0.6856(4) 0.5242(3) 1.2116(6) 0.0395(16) Uani 1 1 d . . . H27 H 0.6725 0.5563 1.2519 0.047 Uiso 1 1 calc R . . C28 C 0.6885(4) 0.5265(3) 1.0924(6) 0.0393(16) Uani 1 1 d . . . H28 H 0.6787 0.5595 1.0527 0.047 Uiso 1 1 calc R . . C29 C 0.8544(4) 0.4472(3) 0.4812(11) 0.076(3) Uani 1 1 d . . . H29 H 0.8329 0.4136 0.5012 0.091 Uiso 1 1 calc R . . C30 C 0.9275(4) 0.4491(3) 0.4773(11) 0.075(3) Uani 1 1 d . . . H30 H 0.9548 0.4176 0.4938 0.090 Uiso 1 1 calc R . . C31 C 0.9604(3) 0.4976(3) 0.4491(7) 0.0447(17) Uani 1 1 d . . . C32 C 0.9164(4) 0.5419(3) 0.4278(10) 0.073(3) Uani 1 1 d . . . H32 H 0.9362 0.5763 0.4097 0.088 Uiso 1 1 calc R . . C33 C 0.8435(4) 0.5354(3) 0.4333(9) 0.066(3) Uani 1 1 d . . . H33 H 0.8146 0.5662 0.4175 0.079 Uiso 1 1 calc R . . C34 C 0.5103(3) 0.4537(2) 0.2100(5) 0.0299(14) Uani 1 1 d . . . H34 H 0.5180 0.4208 0.2509 0.036 Uiso 1 1 calc R . . C35 C 0.5100(4) 0.4525(3) 0.0910(5) 0.0335(15) Uani 1 1 d . . . H35 H 0.5168 0.4189 0.0522 0.040 Uiso 1 1 calc R . . C36 C 0.5000 0.5000 0.0252(8) 0.0246(17) Uani 1 2 d S . . C37 C 0.5000 0.5000 -0.1036(8) 0.0274(19) Uani 1 2 d S . . C38 C 0.4656(4) 0.4592(2) -0.1672(6) 0.0318(15) Uani 1 1 d . . . H38 H 0.4415 0.4306 -0.1283 0.038 Uiso 1 1 calc R . . C39 C 0.4671(3) 0.4611(3) -0.2880(5) 0.0302(14) Uani 1 1 d . . . H39 H 0.4433 0.4330 -0.3291 0.036 Uiso 1 1 calc R . . N1 N 0.6064(3) 0.3017(2) 0.4090(4) 0.0306(12) Uani 1 1 d . . . H1 H 0.6232 0.2753 0.4524 0.037 Uiso 1 1 calc R . . N2 N 0.6507(4) 0.2007(3) -0.1045(5) 0.0495(16) Uani 1 1 d . . . H2A H 0.6390 0.2337 -0.0824 0.059 Uiso 1 1 calc R . . N3 N 0.8115(3) 0.17191(19) 0.4654(5) 0.0321(11) Uani 1 1 d . . . H3 H 0.7721 0.1852 0.4949 0.039 Uiso 1 1 calc R . . N4 N 0.7028(3) 0.4789(2) 0.6527(4) 0.0301(12) Uani 1 1 d . . . N5 N 0.7000(3) 0.4797(2) 1.2750(4) 0.0319(12) Uani 1 1 d . . . N6 N 0.8114(2) 0.48904(19) 0.4591(5) 0.0294(11) Uani 1 1 d . . . N7 N 0.5000 0.5000 0.2719(6) 0.0298(16) Uani 1 2 d S . . N8 N 0.5000 0.5000 -0.3511(6) 0.0249(16) Uani 1 2 d S . . O1 O 0.59072(19) 0.44628(15) 0.4644(4) 0.0262(8) Uani 1 1 d . . . O2 O 0.6857(2) 0.39360(15) 0.4617(4) 0.0281(9) Uani 1 1 d . . . O3 O 0.5869(3) 0.3324(2) 0.2264(4) 0.0466(13) Uani 1 1 d . . . O4 O 0.7063(3) 0.2602(2) -0.2801(5) 0.0623(15) Uani 1 1 d . . . O5 O 0.6655(3) 0.2054(3) -0.4213(4) 0.0621(16) Uani 1 1 d . . . O6 O 0.7011(4) 0.1211(2) -0.0509(5) 0.084(2) Uani 1 1 d . . . O7 O 0.8168(2) 0.06276(16) 0.5287(4) 0.0293(9) Uani 1 1 d . . . O8 O 0.9363(2) 0.06982(15) 0.5471(4) 0.0282(9) Uani 1 1 d . . . O9 O 0.8739(2) 0.1483(2) 0.3042(4) 0.0447(12) Uani 1 1 d . . . O10 O 0.5866(3) 0.3269(2) 0.9676(6) 0.0766(18) Uani 1 1 d . . . H101 H 0.5837 0.3323 1.0416 0.115 Uiso 1 1 d R . . H102 H 0.6310 0.3234 0.9527 0.115 Uiso 1 1 d R . . O11 O 0.7846(3) 0.3208(2) 0.5723(5) 0.0730(18) Uani 1 1 d . . . H111 H 0.7549 0.3427 0.5404 0.110 Uiso 1 1 d R . . H112 H 0.7622 0.2932 0.5998 0.110 Uiso 1 1 d R . . O12 O 0.5449(4) 0.1663(3) 0.4524(7) 0.100(2) Uani 1 1 d . . . H121 H 0.5836 0.1848 0.4520 0.150 Uiso 1 1 d R . . H122 H 0.5057 0.1782 0.4807 0.150 Uiso 1 1 d R . . O13 O 0.9116(4) 0.2932(3) 0.4526(8) 0.108(3) Uani 1 1 d . . . H131 H 0.8748 0.3083 0.4832 0.161 Uiso 1 1 d R . . H132 H 0.9251 0.3105 0.3916 0.161 Uiso 1 1 d R . . O14 O 0.9423(5) 0.1781(3) 0.0944(7) 0.120(3) Uani 1 1 d . . . H141 H 0.9862 0.1768 0.0743 0.180 Uiso 1 1 d R . . H142 H 0.9378 0.1922 0.1624 0.180 Uiso 1 1 d R . . O15 O 0.7562(6) 0.3150(3) 0.9111(7) 0.141(4) Uani 1 1 d . . . H151 H 0.7391 0.2897 0.8679 0.212 Uiso 1 1 d R . . H152 H 0.7924 0.3036 0.9492 0.212 Uiso 1 1 d R . . O16 O 0.8766(5) 0.2792(4) 0.0371(10) 0.146(4) Uani 1 1 d . . . H161 H 0.8749 0.2441 0.0372 0.219 Uiso 1 1 d R . . H162 H 0.9170 0.2897 0.0104 0.219 Uiso 1 1 d R . . O17 O 0.8677(4) 0.3444(4) 0.2377(9) 0.121(3) Uani 1 1 d . . . H171 H 0.8487 0.3440 0.3056 0.181 Uiso 1 1 d R . . H172 H 0.8814 0.3121 0.2196 0.181 Uiso 1 1 d R . . O18 O 0.5972(5) 0.0350(4) 0.9381(11) 0.163(4) Uani 1 1 d . . . H181 H 0.6281 0.0606 0.9428 0.245 Uiso 1 1 d R . . H182 H 0.5776 0.0356 0.8705 0.245 Uiso 1 1 d R . . O19 O 0.8523(6) 0.3847(5) 0.7683(10) 0.166(4) Uani 1 1 d . . . H191 H 0.8330 0.3665 0.7130 0.250 Uiso 1 1 d R . . H192 H 0.8368 0.3774 0.8341 0.250 Uiso 1 1 d R . . O20 O 0.9514(6) 0.4307(4) 0.1255(11) 0.172(5) Uani 1 1 d . . . H201 H 0.9556 0.4548 0.0715 0.257 Uiso 1 1 d R . . H202 H 0.9081 0.4297 0.1492 0.257 Uiso 1 1 d R . . O21 O 0.5797(6) 0.9961(6) 0.1807(11) 0.191(5) Uani 1 1 d . . . H211 H 0.5744 0.9836 0.1113 0.286 Uiso 1 1 d R . . H212 H 0.5791 0.9696 0.2297 0.286 Uiso 1 1 d R . . O22 O 0.5745(9) 0.1044(6) 0.2551(13) 0.239(7) Uani 1 1 d . . . H221 H 0.5464 0.1155 0.2015 0.359 Uiso 1 1 d R . . H222 H 0.5683 0.1235 0.3169 0.359 Uiso 1 1 d R . . O23 O 0.9751(10) 0.3590(7) 0.9234(14) 0.276(9) Uani 1 1 d . . . H231 H 0.9687 0.3801 0.9820 0.413 Uiso 1 1 d R . . H232 H 0.9402 0.3669 0.8785 0.413 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0239(6) 0.0249(5) 0.0196(5) 0.000 0.000 0.0004(4) Co2 0.0249(4) 0.0330(4) 0.0218(4) 0.0004(4) -0.0007(4) -0.0003(4) C1 0.027(3) 0.034(3) 0.018(3) -0.002(3) -0.001(3) 0.003(3) C2 0.025(3) 0.029(3) 0.035(3) -0.003(3) -0.001(3) 0.002(2) C3 0.041(4) 0.039(4) 0.036(4) 0.002(3) 0.014(3) -0.003(3) C4 0.033(4) 0.030(3) 0.043(4) -0.005(3) 0.001(3) -0.002(3) C5 0.041(4) 0.034(3) 0.026(3) 0.005(3) 0.000(3) 0.009(3) C6 0.037(4) 0.048(4) 0.032(4) 0.002(3) -0.007(3) 0.015(3) C7 0.053(4) 0.042(4) 0.030(4) -0.008(3) -0.002(3) 0.014(4) C8 0.056(5) 0.036(3) 0.026(3) -0.006(3) -0.001(3) 0.017(3) C9 0.054(4) 0.035(3) 0.029(4) 0.003(3) -0.003(3) 0.011(3) C10 0.049(4) 0.027(3) 0.024(3) -0.003(3) -0.002(3) 0.007(3) C11 0.060(5) 0.046(4) 0.035(4) -0.013(4) -0.006(4) 0.027(3) C12 0.059(6) 0.124(9) 0.050(6) -0.001(6) -0.004(4) -0.018(6) C13 0.054(5) 0.062(5) 0.020(3) -0.003(3) -0.002(3) -0.005(4) C14 0.053(5) 0.073(6) 0.032(4) -0.002(4) 0.001(4) 0.011(4) C15 0.037(4) 0.027(3) 0.042(4) 0.002(3) 0.004(3) 0.008(3) C16 0.063(5) 0.044(4) 0.032(4) -0.007(3) -0.008(4) 0.015(4) C17 0.028(3) 0.034(3) 0.033(3) -0.002(3) -0.005(3) 0.002(3) C18 0.031(3) 0.036(3) 0.008(2) 0.004(3) 0.003(3) -0.002(3) C19 0.045(4) 0.044(4) 0.023(3) -0.003(3) 0.001(3) -0.008(3) C20 0.039(4) 0.049(4) 0.022(3) 0.004(3) -0.001(3) -0.005(3) C21 0.046(4) 0.043(4) 0.024(3) -0.001(3) -0.004(3) -0.015(3) C22 0.052(5) 0.042(4) 0.024(3) 0.002(3) 0.005(3) -0.015(3) C23 0.037(4) 0.040(3) 0.024(3) 0.001(3) -0.002(3) 0.000(3) C24 0.033(3) 0.044(3) 0.019(3) 0.002(3) 0.002(3) 0.000(3) C25 0.068(5) 0.051(4) 0.024(3) -0.007(3) 0.001(3) 0.017(4) C26 0.054(5) 0.046(4) 0.031(4) -0.002(3) 0.007(3) 0.017(4) C27 0.057(5) 0.036(4) 0.026(3) -0.011(3) 0.003(3) 0.000(3) C28 0.051(4) 0.037(4) 0.030(3) 0.003(3) -0.006(3) -0.007(3) C29 0.035(4) 0.046(4) 0.146(10) 0.022(5) 0.012(5) -0.003(3) C30 0.029(4) 0.048(5) 0.149(10) 0.019(6) -0.005(5) 0.000(3) C31 0.028(3) 0.050(4) 0.056(5) -0.002(4) -0.001(3) -0.005(3) C32 0.024(4) 0.045(4) 0.150(11) 0.039(5) -0.001(5) -0.002(3) C33 0.032(4) 0.046(4) 0.121(9) 0.015(5) -0.007(5) 0.002(3) C34 0.043(4) 0.018(3) 0.029(3) 0.004(3) -0.001(3) 0.003(3) C35 0.048(4) 0.030(3) 0.022(3) -0.007(3) 0.000(3) 0.003(3) C36 0.031(4) 0.025(4) 0.018(4) 0.000 0.000 -0.001(4) C37 0.023(4) 0.034(5) 0.025(4) 0.000 0.000 0.005(4) C38 0.040(4) 0.025(3) 0.030(3) 0.001(3) 0.005(3) -0.008(3) C39 0.034(4) 0.032(3) 0.025(3) -0.007(3) 0.000(3) -0.004(3) N1 0.038(3) 0.025(3) 0.029(3) -0.001(2) -0.002(2) 0.007(2) N2 0.067(4) 0.055(4) 0.026(3) 0.001(3) 0.002(3) 0.010(3) N3 0.037(3) 0.032(2) 0.027(3) 0.006(3) 0.000(3) 0.008(2) N4 0.027(3) 0.036(3) 0.027(3) 0.000(2) 0.000(2) -0.002(3) N5 0.028(3) 0.042(3) 0.026(3) 0.006(3) -0.001(2) 0.001(3) N6 0.024(2) 0.034(3) 0.030(3) 0.004(3) 0.002(2) -0.003(2) N7 0.032(4) 0.030(4) 0.028(4) 0.000 0.000 0.003(4) N8 0.032(4) 0.022(3) 0.020(4) 0.000 0.000 -0.002(3) O1 0.026(2) 0.026(2) 0.027(2) -0.004(2) -0.003(2) 0.0018(16) O2 0.026(2) 0.031(2) 0.028(2) 0.001(2) 0.000(2) 0.0040(16) O3 0.061(3) 0.041(3) 0.037(3) 0.002(2) -0.007(2) 0.023(2) O4 0.072(4) 0.069(4) 0.047(3) 0.004(3) 0.002(3) -0.008(3) O5 0.060(4) 0.092(4) 0.034(3) -0.006(3) 0.006(3) -0.002(3) O6 0.130(5) 0.069(4) 0.052(4) -0.021(3) -0.024(4) 0.049(4) O7 0.031(2) 0.032(2) 0.025(2) -0.003(2) 0.000(2) 0.0031(18) O8 0.026(2) 0.027(2) 0.032(2) -0.002(2) -0.004(2) 0.0033(17) O9 0.046(3) 0.048(3) 0.041(3) -0.005(2) -0.002(2) 0.018(2) O10 0.100(5) 0.066(4) 0.064(4) 0.014(4) 0.003(4) 0.015(3) O11 0.060(4) 0.073(4) 0.086(5) 0.030(3) 0.003(3) 0.018(3) O12 0.096(5) 0.100(5) 0.105(6) 0.002(5) -0.019(5) -0.025(4) O13 0.100(6) 0.107(6) 0.116(7) -0.005(5) 0.032(5) -0.004(4) O14 0.152(7) 0.094(5) 0.114(7) 0.025(5) 0.072(6) 0.031(5) O15 0.269(12) 0.080(5) 0.075(6) -0.012(4) -0.023(7) 0.014(7) O16 0.185(10) 0.106(6) 0.147(9) 0.026(7) -0.026(8) -0.007(6) O17 0.094(6) 0.128(7) 0.140(8) 0.006(6) 0.005(5) 0.027(5) O18 0.123(7) 0.133(8) 0.234(14) -0.038(8) -0.026(9) -0.023(6) O19 0.152(9) 0.217(12) 0.131(9) 0.029(8) -0.024(7) 0.043(8) O20 0.171(10) 0.112(8) 0.232(14) 0.006(8) 0.035(9) -0.001(7) O21 0.142(9) 0.257(15) 0.172(11) -0.024(11) -0.002(7) -0.079(10) O22 0.315(19) 0.274(17) 0.129(11) -0.018(11) 0.011(12) -0.044(15) O23 0.33(2) 0.30(2) 0.201(18) 0.009(15) 0.047(14) 0.069(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O8 2.078(4) 4_456 ? Co1 O8 2.078(4) 3_656 ? Co1 O1 2.141(4) . ? Co1 O1 2.141(4) 2_665 ? Co1 N7 2.143(7) . ? Co1 N8 2.155(7) 1_556 ? Co2 O7 2.011(4) 3_656 ? Co2 N6 2.094(4) . ? Co2 N4 2.143(5) . ? Co2 O2 2.154(4) . ? Co2 N5 2.164(5) 1_554 ? Co2 O1 2.206(4) . ? C1 O1 1.269(6) . ? C1 O2 1.277(6) . ? C1 C2 1.525(8) . ? C2 N1 1.454(7) . ? C2 C3 1.531(9) . ? C2 H2 0.9900 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 O3 1.249(8) . ? C4 N1 1.320(8) . ? C4 C5 1.500(9) . ? C5 C6 1.379(9) . ? C5 C10 1.388(9) . ? C6 C7 1.365(9) . ? C6 H6 0.9400 . ? C7 C8 1.394(9) . ? C7 C11 1.492(9) . ? C8 C9 1.404(9) . ? C8 H8 0.9400 . ? C9 C10 1.411(9) . ? C9 C15 1.489(9) . ? C10 H10 0.9400 . ? C11 O6 1.246(8) . ? C11 N2 1.327(9) . ? C12 C13 1.511(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 N2 1.472(9) . ? C13 C14 1.516(10) . ? C13 H13 0.9900 . ? C14 O4 1.247(10) . ? C14 O5 1.265(9) . ? C15 O9 1.217(7) . ? C15 N3 1.353(8) . ? C16 C17 1.534(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 N3 1.447(8) . ? C17 C18 1.533(8) . ? C17 H17 0.9900 . ? C18 O7 1.259(7) . ? C18 O8 1.264(6) . ? C19 C20 1.376(8) . ? C19 C23 1.392(9) . ? C19 H19 0.9400 . ? C20 N4 1.350(8) . ? C20 H20 0.9400 . ? C21 N4 1.342(8) . ? C21 C22 1.372(9) . ? C21 H21 0.9400 . ? C22 C23 1.381(9) . ? C22 H22 0.9400 . ? C23 C24 1.482(7) . ? C24 C25 1.379(9) . ? C24 C28 1.394(9) . ? C25 C26 1.390(9) . ? C25 H25 0.9400 . ? C26 N5 1.338(8) . ? C26 H26 0.9400 . ? C27 N5 1.332(8) . ? C27 C28 1.361(9) . ? C27 H27 0.9400 . ? C28 H28 0.9400 . ? C29 N6 1.321(9) . ? C29 C30 1.366(10) . ? C29 H29 0.9400 . ? C30 C31 1.370(10) . ? C30 H30 0.9400 . ? C31 C32 1.379(10) . ? C31 C31 1.483(12) 2_765 ? C32 C33 1.371(10) . ? C32 H32 0.9400 . ? C33 N6 1.313(9) . ? C33 H33 0.9400 . ? C34 N7 1.345(7) . ? C34 C35 1.356(9) . ? C34 H34 0.9400 . ? C35 C36 1.392(8) . ? C35 H35 0.9400 . ? C36 C35 1.392(8) 2_665 ? C36 C37 1.469(10) . ? C37 C38 1.388(7) . ? C37 C38 1.388(8) 2_665 ? C38 C39 1.379(9) . ? C38 H38 0.9400 . ? C39 N8 1.340(7) . ? C39 H39 0.9400 . ? N1 H1 0.8700 . ? N2 H2A 0.8700 . ? N3 H3 0.8700 . ? N5 Co2 2.164(5) 1_556 ? N7 C34 1.345(7) 2_665 ? N8 C39 1.340(7) 2_665 ? N8 Co1 2.155(7) 1_554 ? O7 Co2 2.011(4) 3_646 ? O8 Co1 2.078(4) 3_646 ? O10 H101 0.8546 . ? O10 H102 0.8498 . ? O11 H111 0.8504 . ? O11 H112 0.8530 . ? O12 H121 0.8507 . ? O12 H122 0.8501 . ? O13 H131 0.8533 . ? O13 H132 0.8524 . ? O14 H141 0.8501 . ? O14 H142 0.8528 . ? O15 H151 0.8530 . ? O15 H152 0.8499 . ? O16 H161 0.8566 . ? O16 H162 0.8520 . ? O17 H171 0.8510 . ? O17 H172 0.8530 . ? O18 H181 0.8521 . ? O18 H182 0.8530 . ? O19 H191 0.8509 . ? O19 H192 0.8229 . ? O20 H201 0.8541 . ? O20 H202 0.8528 . ? O21 H211 0.8543 . ? O21 H212 0.8540 . ? O22 H221 0.8498 . ? O22 H222 0.8514 . ? O23 H231 0.8514 . ? O23 H232 0.8494 . ? 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 O8 Co1 O8 175.6(3) 4_456 3_656 ? O8 Co1 O1 87.26(15) 4_456 . ? O8 Co1 O1 92.84(15) 3_656 . ? O8 Co1 O1 92.84(15) 4_456 2_665 ? O8 Co1 O1 87.26(15) 3_656 2_665 ? O1 Co1 O1 177.2(2) . 2_665 ? O8 Co1 N7 87.80(13) 4_456 . ? O8 Co1 N7 87.80(13) 3_656 . ? O1 Co1 N7 91.40(12) . . ? O1 Co1 N7 91.40(12) 2_665 . ? O8 Co1 N8 92.20(13) 4_456 1_556 ? O8 Co1 N8 92.20(13) 3_656 1_556 ? O1 Co1 N8 88.60(12) . 1_556 ? O1 Co1 N8 88.60(12) 2_665 1_556 ? N7 Co1 N8 180.000(2) . 1_556 ? O7 Co2 N6 93.72(17) 3_656 . ? O7 Co2 N4 89.7(2) 3_656 . ? N6 Co2 N4 90.4(2) . . ? O7 Co2 O2 164.18(15) 3_656 . ? N6 Co2 O2 102.09(16) . . ? N4 Co2 O2 89.57(19) . . ? O7 Co2 N5 93.17(19) 3_656 1_554 ? N6 Co2 N5 88.17(19) . 1_554 ? N4 Co2 N5 176.88(19) . 1_554 ? O2 Co2 N5 88.02(19) . 1_554 ? O7 Co2 O1 103.95(15) 3_656 . ? N6 Co2 O1 162.28(16) . . ? N4 Co2 O1 90.91(18) . . ? O2 Co2 O1 60.26(14) . . ? N5 Co2 O1 89.61(18) 1_554 . ? O1 C1 O2 118.6(5) . . ? O1 C1 C2 121.7(5) . . ? O2 C1 C2 119.7(5) . . ? N1 C2 C1 110.3(5) . . ? N1 C2 C3 110.0(5) . . ? C1 C2 C3 111.0(6) . . ? N1 C2 H2 108.5 . . ? C1 C2 H2 108.5 . . ? C3 C2 H2 108.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O3 C4 N1 121.5(6) . . ? O3 C4 C5 120.9(6) . . ? N1 C4 C5 117.5(6) . . ? C6 C5 C10 120.3(6) . . ? C6 C5 C4 121.1(6) . . ? C10 C5 C4 118.7(6) . . ? C7 C6 C5 120.9(6) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C8 120.5(6) . . ? C6 C7 C11 121.0(6) . . ? C8 C7 C11 118.5(6) . . ? C7 C8 C9 119.4(6) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C8 C9 C10 119.3(6) . . ? C8 C9 C15 119.5(6) . . ? C10 C9 C15 121.2(6) . . ? C5 C10 C9 119.5(6) . . ? C5 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? O6 C11 N2 121.1(7) . . ? O6 C11 C7 121.6(7) . . ? N2 C11 C7 117.3(6) . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C12 109.9(6) . . ? N2 C13 C14 111.7(6) . . ? C12 C13 C14 111.7(7) . . ? N2 C13 H13 107.8 . . ? C12 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? O4 C14 O5 124.6(8) . . ? O4 C14 C13 118.7(7) . . ? O5 C14 C13 116.7(8) . . ? O9 C15 N3 122.1(6) . . ? O9 C15 C9 121.7(6) . . ? N3 C15 C9 116.2(6) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 110.9(5) . . ? N3 C17 C16 108.6(5) . . ? C18 C17 C16 109.7(6) . . ? N3 C17 H17 109.2 . . ? C18 C17 H17 109.2 . . ? C16 C17 H17 109.2 . . ? O7 C18 O8 125.7(5) . . ? O7 C18 C17 117.8(5) . . ? O8 C18 C17 116.4(5) . . ? C20 C19 C23 119.5(6) . . ? C20 C19 H19 120.3 . . ? C23 C19 H19 120.3 . . ? N4 C20 C19 124.1(6) . . ? N4 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? N4 C21 C22 125.0(6) . . ? N4 C21 H21 117.5 . . ? C22 C21 H21 117.5 . . ? C21 C22 C23 119.4(6) . . ? C21 C22 H22 120.3 . . ? C23 C22 H22 120.3 . . ? C22 C23 C19 117.1(6) . . ? C22 C23 C24 120.2(6) . . ? C19 C23 C24 122.7(6) . . ? C25 C24 C28 117.0(6) . . ? C25 C24 C23 122.8(6) . . ? C28 C24 C23 120.2(6) . . ? C24 C25 C26 120.3(6) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? N5 C26 C25 122.0(6) . . ? N5 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? N5 C27 C28 124.6(6) . . ? N5 C27 H27 117.7 . . ? C28 C27 H27 117.7 . . ? C27 C28 C24 119.0(6) . . ? C27 C28 H28 120.5 . . ? C24 C28 H28 120.5 . . ? N6 C29 C30 125.0(7) . . ? N6 C29 H29 117.5 . . ? C30 C29 H29 117.5 . . ? C29 C30 C31 119.0(7) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C30 C31 C32 116.8(6) . . ? C30 C31 C31 121.0(8) . 2_765 ? C32 C31 C31 122.0(8) . 2_765 ? C33 C32 C31 119.5(7) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? N6 C33 C32 124.1(7) . . ? N6 C33 H33 117.9 . . ? C32 C33 H33 117.9 . . ? N7 C34 C35 122.8(6) . . ? N7 C34 H34 118.6 . . ? C35 C34 H34 118.6 . . ? C34 C35 C36 121.4(6) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C35 C36 C35 114.8(8) . 2_665 ? C35 C36 C37 122.6(4) . . ? C35 C36 C37 122.6(4) 2_665 . ? C38 C37 C38 117.1(8) . 2_665 ? C38 C37 C36 121.5(4) . . ? C38 C37 C36 121.5(4) 2_665 . ? C39 C38 C37 119.2(6) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? N8 C39 C38 124.7(6) . . ? N8 C39 H39 117.7 . . ? C38 C39 H39 117.7 . . ? C4 N1 C2 123.3(6) . . ? C4 N1 H1 118.3 . . ? C2 N1 H1 118.3 . . ? C11 N2 C13 125.4(6) . . ? C11 N2 H2A 117.3 . . ? C13 N2 H2A 117.3 . . ? C15 N3 C17 118.5(5) . . ? C15 N3 H3 120.7 . . ? C17 N3 H3 120.7 . . ? C21 N4 C20 114.9(5) . . ? C21 N4 Co2 124.5(4) . . ? C20 N4 Co2 120.6(4) . . ? C27 N5 C26 117.0(6) . . ? C27 N5 Co2 121.8(4) . 1_556 ? C26 N5 Co2 121.0(4) . 1_556 ? C33 N6 C29 115.6(6) . . ? C33 N6 Co2 122.5(4) . . ? C29 N6 Co2 121.9(4) . . ? C34 N7 C34 116.7(7) . 2_665 ? C34 N7 Co1 121.7(4) . . ? C34 N7 Co1 121.7(4) 2_665 . ? C39 N8 C39 115.1(7) 2_665 . ? C39 N8 Co1 122.5(4) 2_665 1_554 ? C39 N8 Co1 122.5(4) . 1_554 ? C1 O1 Co1 150.9(4) . . ? C1 O1 Co2 89.5(3) . . ? Co1 O1 Co2 119.47(17) . . ? C1 O2 Co2 91.6(3) . . ? C18 O7 Co2 130.1(4) . 3_646 ? C18 O8 Co1 146.9(4) . 3_646 ? H101 O10 H102 105.9 . . ? H111 O11 H112 109.5 . . ? H121 O12 H122 123.5 . . ? H131 O13 H132 110.9 . . ? H141 O14 H142 110.8 . . ? H151 O15 H152 110.8 . . ? H161 O16 H162 109.5 . . ? H171 O17 H172 109.5 . . ? H181 O18 H182 109.5 . . ? H191 O19 H192 114.5 . . ? H201 O20 H202 109.6 . . ? H211 O21 H212 109.5 . . ? H221 O22 H222 109.7 . . ? H231 O23 H232 103.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 152.9(6) . . . . ? O2 C1 C2 N1 -30.5(8) . . . . ? O1 C1 C2 C3 -84.9(7) . . . . ? O2 C1 C2 C3 91.7(7) . . . . ? O3 C4 C5 C6 -30.1(10) . . . . ? N1 C4 C5 C6 152.3(7) . . . . ? O3 C4 C5 C10 148.1(6) . . . . ? N1 C4 C5 C10 -29.5(9) . . . . ? C10 C5 C6 C7 -2.0(11) . . . . ? C4 C5 C6 C7 176.1(6) . . . . ? C5 C6 C7 C8 1.4(12) . . . . ? C5 C6 C7 C11 -179.8(7) . . . . ? C6 C7 C8 C9 2.1(11) . . . . ? C11 C7 C8 C9 -176.7(7) . . . . ? C7 C8 C9 C10 -4.9(11) . . . . ? C7 C8 C9 C15 176.6(6) . . . . ? C6 C5 C10 C9 -0.8(10) . . . . ? C4 C5 C10 C9 -179.0(6) . . . . ? C8 C9 C10 C5 4.2(10) . . . . ? C15 C9 C10 C5 -177.2(6) . . . . ? C6 C7 C11 O6 -149.3(8) . . . . ? C8 C7 C11 O6 29.4(12) . . . . ? C6 C7 C11 N2 27.8(11) . . . . ? C8 C7 C11 N2 -153.4(7) . . . . ? N2 C13 C14 O4 -9.2(10) . . . . ? C12 C13 C14 O4 114.4(9) . . . . ? N2 C13 C14 O5 173.5(7) . . . . ? C12 C13 C14 O5 -62.9(10) . . . . ? C8 C9 C15 O9 24.7(10) . . . . ? C10 C9 C15 O9 -153.8(7) . . . . ? C8 C9 C15 N3 -155.1(6) . . . . ? C10 C9 C15 N3 26.4(9) . . . . ? N3 C17 C18 O7 -36.8(8) . . . . ? C16 C17 C18 O7 83.2(7) . . . . ? N3 C17 C18 O8 146.5(6) . . . . ? C16 C17 C18 O8 -93.5(7) . . . . ? C23 C19 C20 N4 -0.1(10) . . . . ? N4 C21 C22 C23 2.0(11) . . . . ? C21 C22 C23 C19 -3.7(10) . . . . ? C21 C22 C23 C24 178.4(6) . . . . ? C20 C19 C23 C22 2.8(10) . . . . ? C20 C19 C23 C24 -179.4(6) . . . . ? C22 C23 C24 C25 41.5(10) . . . . ? C19 C23 C24 C25 -136.3(7) . . . . ? C22 C23 C24 C28 -136.8(7) . . . . ? C19 C23 C24 C28 45.5(9) . . . . ? C28 C24 C25 C26 0.3(10) . . . . ? C23 C24 C25 C26 -178.0(7) . . . . ? C24 C25 C26 N5 1.6(11) . . . . ? N5 C27 C28 C24 1.4(11) . . . . ? C25 C24 C28 C27 -1.6(10) . . . . ? C23 C24 C28 C27 176.7(6) . . . . ? N6 C29 C30 C31 0.3(19) . . . . ? C29 C30 C31 C32 0.8(16) . . . . ? C29 C30 C31 C31 177.1(8) . . . 2_765 ? C30 C31 C32 C33 -1.3(15) . . . . ? C31 C31 C32 C33 -177.6(7) 2_765 . . . ? C31 C32 C33 N6 0.7(17) . . . . ? N7 C34 C35 C36 1.0(10) . . . . ? C34 C35 C36 C35 -0.5(5) . . . 2_665 ? C34 C35 C36 C37 179.5(5) . . . . ? C35 C36 C37 C38 42.0(4) . . . . ? C35 C36 C37 C38 -138.0(4) 2_665 . . . ? C35 C36 C37 C38 -138.0(4) . . . 2_665 ? C35 C36 C37 C38 42.0(4) 2_665 . . 2_665 ? C38 C37 C38 C39 0.0(4) 2_665 . . . ? C36 C37 C38 C39 180.0(4) . . . . ? C37 C38 C39 N8 0.1(9) . . . . ? O3 C4 N1 C2 -5.8(10) . . . . ? C5 C4 N1 C2 171.8(5) . . . . ? C1 C2 N1 C4 -72.2(8) . . . . ? C3 C2 N1 C4 165.0(6) . . . . ? O6 C11 N2 C13 -1.0(13) . . . . ? C7 C11 N2 C13 -178.2(7) . . . . ? C12 C13 N2 C11 119.1(9) . . . . ? C14 C13 N2 C11 -116.3(8) . . . . ? O9 C15 N3 C17 3.3(9) . . . . ? C9 C15 N3 C17 -176.9(5) . . . . ? C18 C17 N3 C15 -71.2(7) . . . . ? C16 C17 N3 C15 168.1(6) . . . . ? C22 C21 N4 C20 0.8(10) . . . . ? C22 C21 N4 Co2 -179.6(5) . . . . ? C19 C20 N4 C21 -1.8(9) . . . . ? C19 C20 N4 Co2 178.6(5) . . . . ? O7 Co2 N4 C21 142.6(5) 3_656 . . . ? N6 Co2 N4 C21 -123.7(5) . . . . ? O2 Co2 N4 C21 -21.6(5) . . . . ? N5 Co2 N4 C21 -61(4) 1_554 . . . ? O1 Co2 N4 C21 38.6(5) . . . . ? O7 Co2 N4 C20 -37.8(5) 3_656 . . . ? N6 Co2 N4 C20 55.9(5) . . . . ? O2 Co2 N4 C20 158.0(5) . . . . ? N5 Co2 N4 C20 119(3) 1_554 . . . ? O1 Co2 N4 C20 -141.8(5) . . . . ? C28 C27 N5 C26 0.5(10) . . . . ? C28 C27 N5 Co2 176.5(5) . . . 1_556 ? C25 C26 N5 C27 -1.9(10) . . . . ? C25 C26 N5 Co2 -178.0(6) . . . 1_556 ? C32 C33 N6 C29 0.4(14) . . . . ? C32 C33 N6 Co2 -179.5(8) . . . . ? C30 C29 N6 C33 -1.0(16) . . . . ? C30 C29 N6 Co2 178.9(9) . . . . ? O7 Co2 N6 C33 -16.2(7) 3_656 . . . ? N4 Co2 N6 C33 -106.0(7) . . . . ? O2 Co2 N6 C33 164.4(7) . . . . ? N5 Co2 N6 C33 76.8(7) 1_554 . . . ? O1 Co2 N6 C33 159.8(7) . . . . ? O7 Co2 N6 C29 163.9(7) 3_656 . . . ? N4 Co2 N6 C29 74.1(7) . . . . ? O2 Co2 N6 C29 -15.5(7) . . . . ? N5 Co2 N6 C29 -103.1(7) 1_554 . . . ? O1 Co2 N6 C29 -20.1(11) . . . . ? C35 C34 N7 C34 -0.5(5) . . . 2_665 ? C35 C34 N7 Co1 179.5(5) . . . . ? O8 Co1 N7 C34 -44.6(3) 4_456 . . . ? O8 Co1 N7 C34 135.4(3) 3_656 . . . ? O1 Co1 N7 C34 42.6(3) . . . . ? O1 Co1 N7 C34 -137.4(3) 2_665 . . . ? N8 Co1 N7 C34 -163(100) 1_556 . . . ? O8 Co1 N7 C34 135.4(3) 4_456 . . 2_665 ? O8 Co1 N7 C34 -44.6(3) 3_656 . . 2_665 ? O1 Co1 N7 C34 -137.4(3) . . . 2_665 ? O1 Co1 N7 C34 42.6(3) 2_665 . . 2_665 ? N8 Co1 N7 C34 17(100) 1_556 . . 2_665 ? C38 C39 N8 C39 0.0(5) . . . 2_665 ? C38 C39 N8 Co1 180.0(5) . . . 1_554 ? O2 C1 O1 Co1 175.4(5) . . . . ? C2 C1 O1 Co1 -7.9(12) . . . . ? O2 C1 O1 Co2 0.2(6) . . . . ? C2 C1 O1 Co2 176.9(6) . . . . ? O8 Co1 O1 C1 2.6(8) 4_456 . . . ? O8 Co1 O1 C1 -173.0(9) 3_656 . . . ? O1 Co1 O1 C1 94.9(8) 2_665 . . . ? N7 Co1 O1 C1 -85.1(8) . . . . ? N8 Co1 O1 C1 94.9(8) 1_556 . . . ? O8 Co1 O1 Co2 177.1(2) 4_456 . . . ? O8 Co1 O1 Co2 1.5(2) 3_656 . . . ? O1 Co1 O1 Co2 -90.7(2) 2_665 . . . ? N7 Co1 O1 Co2 89.3(2) . . . . ? N8 Co1 O1 Co2 -90.7(2) 1_556 . . . ? O7 Co2 O1 C1 -179.0(4) 3_656 . . . ? N6 Co2 O1 C1 5.0(8) . . . . ? N4 Co2 O1 C1 -89.1(4) . . . . ? O2 Co2 O1 C1 -0.1(4) . . . . ? N5 Co2 O1 C1 87.8(4) 1_554 . . . ? O7 Co2 O1 Co1 3.7(3) 3_656 . . . ? N6 Co2 O1 Co1 -172.2(5) . . . . ? N4 Co2 O1 Co1 93.6(2) . . . . ? O2 Co2 O1 Co1 -177.4(3) . . . . ? N5 Co2 O1 Co1 -89.5(2) 1_554 . . . ? O1 C1 O2 Co2 -0.2(6) . . . . ? C2 C1 O2 Co2 -177.0(5) . . . . ? O7 Co2 O2 C1 4.1(8) 3_656 . . . ? N6 Co2 O2 C1 -178.2(4) . . . . ? N4 Co2 O2 C1 91.4(4) . . . . ? N5 Co2 O2 C1 -90.6(4) 1_554 . . . ? O1 Co2 O2 C1 0.1(3) . . . . ? O8 C18 O7 Co2 2.6(10) . . . 3_646 ? C17 C18 O7 Co2 -173.9(4) . . . 3_646 ? O7 C18 O8 Co1 11.3(13) . . . 3_646 ? C17 C18 O8 Co1 -172.3(6) . . . 3_646 ? 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 N1 H1 O5 0.87 2.37 3.235(8) 177.0 1_556 N2 H2A O10 0.87 2.54 3.402(9) 171.4 1_554 N3 H3 O5 0.87 2.26 3.122(7) 170.7 1_556 O10 H101 O3 0.85 2.11 2.954(8) 169.9 1_556 O10 H102 O15 0.85 2.39 3.243(13) 179.2 . O11 H111 O2 0.85 2.00 2.853(7) 178.7 . O11 H112 O4 0.85 1.90 2.674(8) 150.3 1_556 O12 H121 O5 0.85 2.16 2.836(9) 136.1 1_556 O12 H122 O13 0.85 2.04 2.887(12) 179.5 4_456 O13 H131 O11 0.85 1.99 2.816(9) 162.7 . O13 H132 O17 0.85 2.22 2.869(13) 133.5 . O14 H141 O10 0.85 1.94 2.785(11) 178.6 4_556 O14 H142 O9 0.85 2.28 2.808(9) 120.5 . O15 H151 O4 0.85 1.93 2.722(10) 153.2 1_556 O15 H152 O16 0.85 1.96 2.805(14) 178.5 1_556 O16 H161 O14 0.86 2.14 2.829(11) 136.8 . O16 H162 O23 0.85 2.24 2.97(2) 144.4 1_554 O17 H171 O13 0.85 2.39 2.869(13) 116.1 . O17 H172 O16 0.85 2.23 2.791(14) 123.0 . O18 H181 O6 0.85 2.01 2.862(12) 178.4 1_556 O18 H182 O20 0.85 2.49 2.937(16) 113.2 4_456 O19 H191 O11 0.85 2.15 3.002(14) 179.6 . O19 H192 O15 0.82 2.31 2.956(16) 135.8 . O20 H201 O18 0.85 2.19 2.795(13) 127.4 3_656 O20 H202 O17 0.85 2.43 2.916(14) 116.7 . O21 H211 O18 0.85 2.38 2.942(18) 124.0 1_564 O21 H212 O19 0.85 2.44 3.055(19) 129.9 3_656 O22 H221 O23 0.85 2.05 2.90(2) 177.4 4_456 O22 H222 O12 0.85 1.92 2.764(16) 174.6 . O23 H231 O20 0.85 2.07 2.926(19) 178.9 1_556 O23 H232 O19 0.85 2.11 2.96(2) 178.4 . _chemical_absolute_configuration rmad _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.534 _refine_diff_density_min -0.426 _refine_diff_density_rms 0.083 # Attachment '2.CIF' data_cc _database_code_depnum_ccdc_archive 'CCDC 794253' #TrackingRef '- Compound 1-3.cif' #TrackingRef '2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H68 Co3 N14 O18, 28(H2 O)' _chemical_formula_sum 'C76 H124 Co3 N14 O46' _chemical_formula_weight 2146.68 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' 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 P21212 _symmetry_space_group_name_Hall 'P 2 2ab ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 18.663(4) _cell_length_b 24.329(5) _cell_length_c 11.395(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5174.0(18) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 14612 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2254 _exptl_absorpt_coefficient_mu 0.570 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8040 _exptl_absorpt_correction_T_max 0.9193 _exptl_absorpt_process_details 'SADABS (Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17138 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.1148 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8960 _reflns_number_gt 6893 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _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. ; _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^)+(0.0718P)^2^+0.1247P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(2) _refine_ls_number_reflns 8960 _refine_ls_number_parameters 633 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 Co1 Co 0.5000 0.5000 0.53936(9) 0.0221(3) Uani 1 2 d S . . Co2 Co 0.30007(4) 0.51926(4) 0.53456(6) 0.0267(2) Uani 1 1 d . . . C1 C 0.3825(3) 0.6023(3) 0.5364(5) 0.0260(13) Uani 1 1 d . . . C2 C 0.4301(3) 0.6526(3) 0.5337(6) 0.0300(13) Uani 1 1 d . . . H2 H 0.4751 0.6445 0.5763 0.036 Uiso 1 1 calc R . . C3 C 0.4482(3) 0.6678(3) 0.4057(5) 0.0366(17) Uani 1 1 d . . . H3A H 0.4053 0.6808 0.3665 0.055 Uiso 1 1 calc R . . H3B H 0.4664 0.6356 0.3652 0.055 Uiso 1 1 calc R . . H3C H 0.4842 0.6965 0.4049 0.055 Uiso 1 1 calc R . . C4 C 0.3872(3) 0.7022(3) 0.7074(5) 0.0352(16) Uani 1 1 d . . . C5 C 0.3400(3) 0.7476(3) 0.7515(5) 0.0360(16) Uani 1 1 d . . . C6 C 0.3516(4) 0.7691(3) 0.8621(5) 0.0410(18) Uani 1 1 d . . . H6 H 0.3910 0.7570 0.9068 0.049 Uiso 1 1 calc R . . C7 C 0.3062(4) 0.8079(3) 0.9068(6) 0.0476(19) Uani 1 1 d . . . C8 C 0.2497(4) 0.8278(3) 0.8396(5) 0.0426(18) Uani 1 1 d . . . H8 H 0.2191 0.8549 0.8702 0.051 Uiso 1 1 calc R . . C9 C 0.2383(4) 0.8072(3) 0.7255(5) 0.0370(16) Uani 1 1 d . . . C10 C 0.2830(3) 0.7667(3) 0.6831(5) 0.0317(15) Uani 1 1 d . . . H10 H 0.2752 0.7520 0.6079 0.038 Uiso 1 1 calc R . . C11 C 0.3175(4) 0.8330(3) 1.0276(6) 0.0494(19) Uani 1 1 d . . . C12 C 0.4486(5) 0.8129(5) 1.2432(8) 0.087(4) Uani 1 1 d . . . H12A H 0.4645 0.7751 1.2358 0.130 Uiso 1 1 calc R . . H12B H 0.4603 0.8266 1.3208 0.130 Uiso 1 1 calc R . . H12C H 0.4723 0.8353 1.1845 0.130 Uiso 1 1 calc R . . C13 C 0.3679(4) 0.8156(4) 1.2249(6) 0.054(2) Uani 1 1 d . . . H13 H 0.3527 0.8543 1.2359 0.065 Uiso 1 1 calc R . . C14 C 0.3280(4) 0.7804(4) 1.3156(6) 0.054(2) Uani 1 1 d . . . C15 C 0.1794(3) 0.8309(3) 0.6539(5) 0.0368(16) Uani 1 1 d . . . C16 C 0.1470(4) 0.8297(4) 0.3331(6) 0.053(2) Uani 1 1 d . . . H16A H 0.1933 0.8434 0.3076 0.080 Uiso 1 1 calc R . . H16B H 0.1099 0.8441 0.2820 0.080 Uiso 1 1 calc R . . H16C H 0.1468 0.7899 0.3297 0.080 Uiso 1 1 calc R . . C17 C 0.1329(3) 0.8484(3) 0.4591(5) 0.0321(14) Uani 1 1 d . . . H17 H 0.0869 0.8322 0.4852 0.039 Uiso 1 1 calc R . . C18 C 0.1261(3) 0.9099(2) 0.4637(5) 0.0249(12) Uani 1 1 d . . . C19 C 0.2633(4) 0.4792(3) 0.1636(5) 0.0404(16) Uani 1 1 d . . . H19 H 0.2412 0.4496 0.1252 0.049 Uiso 1 1 calc R . . C20 C 0.2663(3) 0.4808(4) 0.2846(5) 0.0430(18) Uani 1 1 d . . . H20 H 0.2458 0.4515 0.3265 0.052 Uiso 1 1 calc R . . C21 C 0.3242(4) 0.5627(3) 0.2807(5) 0.0417(18) Uani 1 1 d . . . H21 H 0.3462 0.5918 0.3211 0.050 Uiso 1 1 calc R . . C22 C 0.3229(4) 0.5654(3) 0.1598(5) 0.0423(18) Uani 1 1 d . . . H22 H 0.3416 0.5959 0.1196 0.051 Uiso 1 1 calc R . . C23 C 0.2929(3) 0.5215(3) 0.0997(5) 0.0337(15) Uani 1 1 d . . . C24 C 0.2930(3) 0.5216(3) -0.0299(5) 0.0323(14) Uani 1 1 d . . . C25 C 0.2791(4) 0.5677(4) -0.0942(5) 0.054(2) Uani 1 1 d . . . H25 H 0.2680 0.6009 -0.0560 0.064 Uiso 1 1 calc R . . C26 C 0.2813(4) 0.5658(3) -0.2176(5) 0.0427(18) Uani 1 1 d . . . H26 H 0.2693 0.5976 -0.2601 0.051 Uiso 1 1 calc R . . C27 C 0.3138(4) 0.4766(3) -0.2115(5) 0.0426(17) Uani 1 1 d . . . H27 H 0.3274 0.4444 -0.2513 0.051 Uiso 1 1 calc R . . C28 C 0.3101(4) 0.4741(3) -0.0921(5) 0.0410(17) Uani 1 1 d . . . H28 H 0.3190 0.4409 -0.0525 0.049 Uiso 1 1 calc R . . C29 C 0.1464(4) 0.5533(4) 0.5178(9) 0.070(3) Uani 1 1 d . . . H29 H 0.1678 0.5870 0.4978 0.083 Uiso 1 1 calc R . . C30 C 0.0727(4) 0.5509(4) 0.5218(11) 0.078(3) Uani 1 1 d . . . H30 H 0.0453 0.5825 0.5064 0.094 Uiso 1 1 calc R . . C31 C 0.0396(3) 0.5024(3) 0.5485(6) 0.0448(17) Uani 1 1 d . . . C32 C 0.0831(3) 0.4587(4) 0.5722(9) 0.072(3) Uani 1 1 d . . . H32 H 0.0628 0.4247 0.5928 0.086 Uiso 1 1 calc R . . C33 C 0.1573(4) 0.4642(4) 0.5662(8) 0.064(3) Uani 1 1 d . . . H33 H 0.1860 0.4332 0.5813 0.076 Uiso 1 1 calc R . . C34 C 0.4902(3) 0.5468(3) 0.7882(5) 0.0284(14) Uani 1 1 d . . . H34 H 0.4830 0.5797 0.7467 0.034 Uiso 1 1 calc R . . C35 C 0.4902(3) 0.5477(3) 0.9083(5) 0.0311(15) Uani 1 1 d . . . H35 H 0.4836 0.5813 0.9476 0.037 Uiso 1 1 calc R . . C36 C 0.5000 0.5000 0.9729(7) 0.0252(17) Uani 1 2 d S . . C37 C 0.5000 0.5000 1.1030(6) 0.027(2) Uani 1 2 d S . . C38 C 0.5352(3) 0.5412(3) 1.1674(5) 0.0311(15) Uani 1 1 d . . . H38 H 0.5593 0.5698 1.1285 0.037 Uiso 1 1 calc R . . C39 C 0.5339(3) 0.5393(3) 1.2878(5) 0.0288(14) Uani 1 1 d . . . H39 H 0.5581 0.5669 1.3295 0.035 Uiso 1 1 calc R . . N1 N 0.3944(3) 0.6993(2) 0.5900(4) 0.0329(13) Uani 1 1 d . . . H1 H 0.3774 0.7258 0.5467 0.039 Uiso 1 1 calc R . . N2 N 0.3494(4) 0.7994(3) 1.1047(5) 0.0553(18) Uani 1 1 d . . . H2A H 0.3598 0.7661 1.0823 0.066 Uiso 1 1 calc R . . N3 N 0.1890(2) 0.8282(2) 0.5353(4) 0.0323(11) Uani 1 1 d . . . H3 H 0.2282 0.8146 0.5061 0.039 Uiso 1 1 calc R . . N4 N 0.2964(3) 0.5215(2) 0.3456(4) 0.0310(12) Uani 1 1 d . . . N5 N 0.2997(2) 0.5208(2) -0.2764(4) 0.0304(12) Uani 1 1 d . . . N6 N 0.1889(2) 0.5110(2) 0.5403(4) 0.0314(12) Uani 1 1 d . . . N7 N 0.5000 0.5000 0.7283(5) 0.0259(16) Uani 1 2 d S . . N8 N 0.5000 0.5000 1.3492(5) 0.0233(16) Uani 1 2 d S . . O1 O 0.40925(19) 0.55445(17) 0.5349(3) 0.0273(9) Uani 1 1 d . . . O2 O 0.31475(19) 0.60730(18) 0.5372(4) 0.0313(10) Uani 1 1 d . . . O3 O 0.4146(3) 0.6675(2) 0.7740(4) 0.0490(14) Uani 1 1 d . . . O4 O 0.2931(3) 0.7395(3) 1.2809(4) 0.0662(16) Uani 1 1 d . . . O5 O 0.3353(3) 0.7952(3) 1.4219(4) 0.0654(18) Uani 1 1 d . . . O6 O 0.2983(4) 0.8785(3) 1.0514(5) 0.091(2) Uani 1 1 d . . . O7 O 0.18287(19) 0.93738(17) 0.4732(3) 0.0273(9) Uani 1 1 d . . . O8 O 0.06432(19) 0.93024(17) 0.4536(4) 0.0264(9) Uani 1 1 d . . . O9 O 0.1263(2) 0.8520(2) 0.6967(4) 0.0467(13) Uani 1 1 d . . . O10 O 0.4131(3) 0.6732(3) 0.0322(5) 0.0827(19) Uani 1 1 d . . . H101 H 0.4160 0.6679 -0.0418 0.124 Uiso 1 1 d R . . H102 H 0.3687 0.6767 0.0471 0.124 Uiso 1 1 d R . . O11 O 0.2154(3) 0.6804(3) 0.4298(5) 0.079(2) Uani 1 1 d . . . H111 H 0.2451 0.6586 0.4617 0.119 Uiso 1 1 d R . . H112 H 0.2377 0.7081 0.4022 0.119 Uiso 1 1 d R . . O12 O 0.4554(4) 0.8343(3) 0.5509(7) 0.111(3) Uani 1 1 d . . . H121 H 0.4167 0.8159 0.5512 0.167 Uiso 1 1 d R . . H122 H 0.4946 0.8225 0.5225 0.167 Uiso 1 1 d R . . O13 O 0.0883(4) 0.7068(4) 0.5470(8) 0.126(3) Uani 1 1 d . . . H131 H 0.1251 0.6916 0.5164 0.189 Uiso 1 1 d R . . H132 H 0.0748 0.6894 0.6081 0.189 Uiso 1 1 d R . . O14 O 0.0581(5) 0.8204(4) 0.9059(7) 0.136(4) Uani 1 1 d . . . H141 H 0.0142 0.8217 0.9260 0.203 Uiso 1 1 d R . . H142 H 0.0626 0.8063 0.8379 0.203 Uiso 1 1 d R . . O15 O 0.2423(7) 0.6862(4) 0.0895(7) 0.159(4) Uani 1 1 d . . . H151 H 0.2594 0.7116 0.1327 0.239 Uiso 1 1 d R . . H152 H 0.2061 0.6977 0.0514 0.239 Uiso 1 1 d R . . O16 O 0.1226(6) 0.7210(5) 0.9665(10) 0.182(5) Uani 1 1 d . . . H161 H 0.1243 0.7561 0.9664 0.274 Uiso 1 1 d R . . H162 H 0.0822 0.7105 0.9931 0.274 Uiso 1 1 d R . . O17 O 0.1325(5) 0.6552(4) 0.7621(9) 0.140(4) Uani 1 1 d . . . H171 H 0.1514 0.6556 0.6942 0.210 Uiso 1 1 d R . . H172 H 0.1188 0.6875 0.7801 0.210 Uiso 1 1 d R . . O18 O 0.4031(6) 0.9635(5) 0.0655(12) 0.191(5) Uani 1 1 d . . . H181 H 0.3722 0.9379 0.0608 0.286 Uiso 1 1 d R . . H182 H 0.4227 0.9628 0.1331 0.286 Uiso 1 1 d R . . O19 O 0.1459(7) 0.6145(6) 0.2297(11) 0.206(6) Uani 1 1 d . . . H191 H 0.1652 0.6327 0.2850 0.308 Uiso 1 1 d R . . H192 H 0.1614 0.6218 0.1639 0.308 Uiso 1 1 d R . . O20 O 0.0499(6) 0.5697(5) 0.8743(11) 0.185(5) Uani 1 1 d . . . H201 H 0.0457 0.5456 0.9282 0.277 Uiso 1 1 d R . . H202 H 0.0933 0.5707 0.8506 0.277 Uiso 1 1 d R . . O21 O 0.4224(7) -0.0003(8) 0.8203(11) 0.231(8) Uani 1 1 d . . . H211 H 0.4277 0.0123 0.8897 0.347 Uiso 1 1 d R . . H212 H 0.4230 0.0262 0.7713 0.347 Uiso 1 1 d R . . O22 O 0.4329(11) 0.8962(9) 0.7475(12) 0.326(12) Uani 1 1 d . . . H221 H 0.4610 0.8851 0.8011 0.489 Uiso 1 1 d R . . H222 H 0.4391 0.8771 0.6857 0.489 Uiso 1 1 d R . . O23 O 0.0259(10) 0.6423(9) 0.0748(15) 0.298(9) Uani 1 1 d . . . H231 H 0.0323 0.6211 0.0163 0.447 Uiso 1 1 d R . . H232 H 0.0607 0.6343 0.1197 0.447 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0234(5) 0.0251(7) 0.0178(4) 0.000 0.000 -0.0003(5) Co2 0.0249(4) 0.0360(5) 0.0190(3) -0.0002(4) -0.0002(3) -0.0002(4) C1 0.027(3) 0.035(4) 0.016(2) -0.005(3) 0.002(3) 0.010(3) C2 0.024(3) 0.029(4) 0.037(3) -0.003(3) 0.005(3) 0.003(3) C3 0.035(3) 0.042(5) 0.032(3) 0.005(3) 0.010(3) -0.004(3) C4 0.040(4) 0.030(4) 0.035(3) -0.008(3) -0.003(3) 0.002(3) C5 0.043(4) 0.034(4) 0.031(3) -0.003(3) 0.001(3) 0.009(3) C6 0.061(4) 0.037(5) 0.025(3) -0.001(3) -0.007(3) 0.023(4) C7 0.056(4) 0.053(5) 0.034(3) -0.007(3) -0.010(3) 0.020(4) C8 0.059(4) 0.041(5) 0.027(3) -0.002(3) 0.003(3) 0.025(4) C9 0.053(4) 0.031(4) 0.027(3) 0.003(3) 0.004(3) 0.013(3) C10 0.049(4) 0.019(4) 0.028(3) -0.001(3) -0.002(3) 0.005(3) C11 0.062(4) 0.047(5) 0.039(4) -0.013(4) -0.003(4) 0.029(4) C12 0.067(6) 0.144(12) 0.050(5) 0.010(6) 0.003(4) -0.022(7) C13 0.069(5) 0.064(6) 0.028(3) 0.001(4) 0.000(4) 0.004(4) C14 0.051(5) 0.077(7) 0.033(4) -0.001(4) 0.001(3) 0.010(5) C15 0.039(4) 0.033(4) 0.039(4) 0.004(3) 0.000(3) 0.005(3) C16 0.067(5) 0.056(6) 0.036(4) -0.019(4) -0.019(4) 0.017(4) C17 0.030(3) 0.040(4) 0.027(3) -0.008(3) -0.006(3) 0.007(3) C18 0.032(3) 0.031(4) 0.012(2) 0.004(3) -0.001(3) 0.005(3) C19 0.051(4) 0.042(5) 0.028(3) -0.009(3) -0.001(3) -0.002(4) C20 0.044(4) 0.063(5) 0.022(3) 0.001(3) -0.009(3) -0.014(4) C21 0.051(4) 0.053(5) 0.022(3) -0.002(3) -0.004(3) -0.016(4) C22 0.057(4) 0.047(5) 0.023(3) 0.002(3) -0.001(3) -0.010(4) C23 0.036(3) 0.042(4) 0.023(3) 0.004(3) -0.002(3) -0.003(4) C24 0.032(3) 0.042(4) 0.022(3) -0.004(3) -0.003(3) 0.001(3) C25 0.077(5) 0.063(6) 0.021(3) -0.007(3) 0.002(3) 0.016(4) C26 0.059(5) 0.041(5) 0.028(3) -0.001(3) -0.001(3) 0.016(4) C27 0.055(4) 0.039(5) 0.033(3) -0.007(3) 0.005(3) 0.003(4) C28 0.060(4) 0.037(5) 0.026(3) 0.005(3) -0.003(3) -0.006(4) C29 0.039(4) 0.040(5) 0.130(8) 0.019(5) 0.008(5) -0.012(4) C30 0.032(4) 0.035(5) 0.168(10) 0.022(6) -0.002(5) -0.001(3) C31 0.026(3) 0.050(5) 0.059(4) 0.010(4) -0.009(3) -0.005(3) C32 0.018(3) 0.055(6) 0.142(9) 0.033(6) -0.003(4) -0.011(3) C33 0.026(3) 0.051(6) 0.114(8) 0.023(5) -0.004(4) 0.007(3) C34 0.041(4) 0.019(4) 0.025(3) 0.000(3) -0.004(3) 0.003(3) C35 0.046(4) 0.026(4) 0.022(3) -0.004(3) 0.003(3) 0.003(3) C36 0.028(4) 0.031(5) 0.017(3) 0.000 0.000 0.002(4) C37 0.029(4) 0.041(6) 0.012(3) 0.000 0.000 0.002(4) C38 0.034(3) 0.034(4) 0.025(3) 0.002(3) 0.007(3) -0.001(3) C39 0.036(3) 0.022(4) 0.028(3) -0.007(3) 0.001(3) 0.000(3) N1 0.042(3) 0.034(4) 0.023(2) 0.003(2) -0.006(2) 0.002(3) N2 0.079(4) 0.061(5) 0.026(3) 0.000(3) 0.002(3) 0.015(4) N3 0.035(3) 0.033(3) 0.028(2) 0.003(3) -0.003(3) 0.008(2) N4 0.028(3) 0.034(3) 0.031(2) 0.002(2) 0.004(2) 0.000(3) N5 0.026(2) 0.042(4) 0.023(2) 0.002(2) 0.004(2) 0.000(3) N6 0.031(2) 0.038(4) 0.025(2) -0.001(3) 0.002(2) -0.001(2) N7 0.029(3) 0.029(5) 0.019(3) 0.000 0.000 0.001(4) N8 0.028(3) 0.021(4) 0.022(3) 0.000 0.000 -0.003(4) O1 0.028(2) 0.028(3) 0.0251(17) 0.000(2) 0.002(2) 0.0034(17) O2 0.025(2) 0.042(3) 0.0267(19) -0.003(2) -0.004(2) 0.0046(17) O3 0.065(3) 0.048(4) 0.034(2) -0.001(2) -0.005(2) 0.027(3) O4 0.079(4) 0.070(5) 0.050(3) -0.002(3) 0.004(3) -0.003(4) O5 0.058(3) 0.110(6) 0.028(2) -0.002(3) 0.001(2) 0.003(3) O6 0.142(6) 0.081(5) 0.051(3) -0.030(3) -0.037(4) 0.064(5) O7 0.032(2) 0.023(2) 0.0262(19) 0.0021(19) -0.0046(19) -0.0049(17) O8 0.027(2) 0.027(2) 0.0254(19) 0.000(2) -0.0038(19) 0.0057(17) O9 0.047(3) 0.053(4) 0.040(2) -0.005(2) 0.001(2) 0.022(3) O10 0.107(5) 0.074(5) 0.067(3) 0.009(4) 0.013(4) 0.018(4) O11 0.066(4) 0.078(5) 0.094(4) 0.038(4) 0.005(3) 0.012(3) O12 0.108(5) 0.107(7) 0.118(6) 0.011(6) -0.011(5) -0.022(5) O13 0.111(6) 0.114(7) 0.152(7) -0.008(6) 0.045(6) -0.002(5) O14 0.159(8) 0.122(8) 0.125(6) 0.045(6) 0.087(6) 0.042(6) O15 0.272(13) 0.120(9) 0.087(5) -0.008(5) -0.043(7) 0.012(9) O16 0.194(11) 0.169(12) 0.184(10) 0.059(9) -0.036(9) -0.006(9) O17 0.127(7) 0.145(10) 0.149(8) 0.015(7) 0.010(6) 0.016(7) O18 0.141(8) 0.151(12) 0.280(15) -0.043(10) -0.044(10) -0.012(7) O19 0.197(11) 0.266(18) 0.154(9) 0.035(10) -0.019(9) 0.061(12) O20 0.174(10) 0.142(12) 0.238(13) 0.005(10) 0.038(9) -0.026(9) O21 0.179(11) 0.34(2) 0.178(11) -0.028(13) 0.003(9) -0.054(14) O22 0.44(3) 0.41(3) 0.129(10) 0.017(14) 0.005(14) -0.13(2) O23 0.32(2) 0.27(2) 0.30(2) -0.018(18) 0.060(17) -0.033(18) _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 O8 2.080(4) 3_546 ? Co1 O8 2.080(4) 4_566 ? Co1 O1 2.151(4) . ? Co1 O1 2.151(4) 2_665 ? Co1 N7 2.153(6) . ? Co1 N8 2.167(6) 1_554 ? Co2 O7 2.019(4) 3_546 ? Co2 N6 2.085(5) . ? Co2 N5 2.154(4) 1_556 ? Co2 N4 2.156(5) . ? Co2 O2 2.160(4) . ? Co2 O1 2.210(4) . ? C1 O1 1.267(7) . ? C1 O2 1.271(6) . ? C1 C2 1.512(8) . ? C2 N1 1.466(8) . ? C2 C3 1.542(8) . ? C2 H2 0.9900 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 O3 1.246(8) . ? C4 N1 1.345(8) . ? C4 C5 1.500(9) . ? C5 C6 1.382(9) . ? C5 C10 1.398(9) . ? C6 C7 1.367(10) . ? C6 H6 0.9400 . ? C7 C8 1.390(9) . ? C7 C11 1.521(9) . ? C8 C9 1.409(9) . ? C8 H8 0.9400 . ? C9 C10 1.378(9) . ? C9 C15 1.486(9) . ? C10 H10 0.9400 . ? C11 O6 1.195(9) . ? C11 N2 1.340(9) . ? C12 C13 1.521(11) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 N2 1.466(9) . ? C13 C14 1.536(11) . ? C13 H13 0.9900 . ? C14 O4 1.253(10) . ? C14 O5 1.271(9) . ? C15 O9 1.219(7) . ? C15 N3 1.365(8) . ? C16 C17 1.529(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 N3 1.446(7) . ? C17 C18 1.502(9) . ? C17 H17 0.9900 . ? C18 O7 1.258(7) . ? C18 O8 1.261(6) . ? C19 C23 1.376(10) . ? C19 C20 1.380(8) . ? C19 H19 0.9400 . ? C20 N4 1.333(9) . ? C20 H20 0.9400 . ? C21 N4 1.349(9) . ? C21 C22 1.379(8) . ? C21 H21 0.9400 . ? C22 C23 1.386(10) . ? C22 H22 0.9400 . ? C23 C24 1.476(7) . ? C24 C25 1.365(10) . ? C24 C28 1.393(10) . ? C25 C26 1.408(8) . ? C25 H25 0.9400 . ? C26 N5 1.328(9) . ? C26 H26 0.9400 . ? C27 N5 1.331(9) . ? C27 C28 1.363(8) . ? C27 H27 0.9400 . ? C28 H28 0.9400 . ? C29 N6 1.324(10) . ? C29 C30 1.378(10) . ? C29 H29 0.9400 . ? C30 C31 1.366(10) . ? C30 H30 0.9400 . ? C31 C32 1.363(11) . ? C31 C31 1.484(11) 2_565 ? C32 C33 1.394(10) . ? C32 H32 0.9400 . ? C33 N6 1.316(9) . ? C33 H33 0.9400 . ? C34 N7 1.340(7) . ? C34 C35 1.368(8) . ? C34 H34 0.9400 . ? C35 C36 1.387(7) . ? C35 H35 0.9400 . ? C36 C35 1.387(7) 2_665 ? C36 C37 1.483(9) . ? C37 C38 1.405(7) . ? C37 C38 1.405(7) 2_665 ? C38 C39 1.372(8) . ? C38 H38 0.9400 . ? C39 N8 1.343(7) . ? C39 H39 0.9400 . ? N1 H1 0.8700 . ? N2 H2A 0.8700 . ? N3 H3 0.8700 . ? N5 Co2 2.154(4) 1_554 ? N7 C34 1.340(7) 2_665 ? N8 C39 1.343(7) 2_665 ? N8 Co1 2.167(6) 1_556 ? O7 Co2 2.019(4) 3_556 ? O8 Co1 2.080(4) 3_556 ? O10 H101 0.8543 . ? O10 H102 0.8500 . ? O11 H111 0.8497 . ? O11 H112 0.8519 . ? O12 H121 0.8504 . ? O12 H122 0.8501 . ? O13 H131 0.8530 . ? O13 H132 0.8518 . ? O14 H141 0.8503 . ? O14 H142 0.8522 . ? O15 H151 0.8520 . ? O15 H152 0.8498 . ? O16 H161 0.8548 . ? O16 H162 0.8520 . ? O17 H171 0.8508 . ? O17 H172 0.8515 . ? O18 H181 0.8513 . ? O18 H182 0.8528 . ? O19 H191 0.8503 . ? O19 H192 0.8226 . ? O20 H201 0.8531 . ? O20 H202 0.8530 . ? O21 H211 0.8537 . ? O21 H212 0.8528 . ? O22 H221 0.8496 . ? O22 H222 0.8506 . ? O23 H231 0.8506 . ? O23 H232 0.8493 . ? 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 O8 Co1 O8 175.6(2) 3_546 4_566 ? O8 Co1 O1 92.81(15) 3_546 . ? O8 Co1 O1 87.30(15) 4_566 . ? O8 Co1 O1 87.30(15) 3_546 2_665 ? O8 Co1 O1 92.81(15) 4_566 2_665 ? O1 Co1 O1 177.3(2) . 2_665 ? O8 Co1 N7 87.78(12) 3_546 . ? O8 Co1 N7 87.78(12) 4_566 . ? O1 Co1 N7 91.37(11) . . ? O1 Co1 N7 91.37(11) 2_665 . ? O8 Co1 N8 92.22(12) 3_546 1_554 ? O8 Co1 N8 92.22(12) 4_566 1_554 ? O1 Co1 N8 88.63(11) . 1_554 ? O1 Co1 N8 88.63(11) 2_665 1_554 ? N7 Co1 N8 180.000(2) . 1_554 ? O7 Co2 N6 93.65(18) 3_546 . ? O7 Co2 N5 93.5(2) 3_546 1_556 ? N6 Co2 N5 88.12(18) . 1_556 ? O7 Co2 N4 89.2(2) 3_546 . ? N6 Co2 N4 90.12(18) . . ? N5 Co2 N4 176.9(2) 1_556 . ? O7 Co2 O2 163.55(14) 3_546 . ? N6 Co2 O2 102.77(18) . . ? N5 Co2 O2 88.24(19) 1_556 . ? N4 Co2 O2 89.6(2) . . ? O7 Co2 O1 103.70(15) 3_546 . ? N6 Co2 O1 162.62(18) . . ? N5 Co2 O1 89.68(17) 1_556 . ? N4 Co2 O1 91.22(17) . . ? O2 Co2 O1 59.92(14) . . ? O1 C1 O2 118.7(5) . . ? O1 C1 C2 120.8(5) . . ? O2 C1 C2 120.5(5) . . ? N1 C2 C1 110.6(5) . . ? N1 C2 C3 109.1(5) . . ? C1 C2 C3 110.0(5) . . ? N1 C2 H2 109.0 . . ? C1 C2 H2 109.0 . . ? C3 C2 H2 109.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O3 C4 N1 122.0(6) . . ? O3 C4 C5 122.4(5) . . ? N1 C4 C5 115.5(6) . . ? C6 C5 C10 120.2(6) . . ? C6 C5 C4 119.5(6) . . ? C10 C5 C4 120.3(5) . . ? C7 C6 C5 120.2(6) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.4(6) . . ? C6 C7 C11 121.9(6) . . ? C8 C7 C11 117.6(6) . . ? C7 C8 C9 119.9(6) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 119.1(6) . . ? C10 C9 C15 122.2(5) . . ? C8 C9 C15 118.7(6) . . ? C9 C10 C5 120.1(6) . . ? C9 C10 H10 119.9 . . ? C5 C10 H10 119.9 . . ? O6 C11 N2 123.4(7) . . ? O6 C11 C7 122.4(7) . . ? N2 C11 C7 114.2(6) . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C12 110.4(7) . . ? N2 C13 C14 111.3(7) . . ? C12 C13 C14 111.3(7) . . ? N2 C13 H13 107.9 . . ? C12 C13 H13 107.9 . . ? C14 C13 H13 107.9 . . ? O4 C14 O5 125.5(8) . . ? O4 C14 C13 118.9(6) . . ? O5 C14 C13 115.5(8) . . ? O9 C15 N3 121.5(6) . . ? O9 C15 C9 123.2(6) . . ? N3 C15 C9 115.3(5) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C18 112.2(5) . . ? N3 C17 C16 109.8(5) . . ? C18 C17 C16 110.0(6) . . ? N3 C17 H17 108.2 . . ? C18 C17 H17 108.2 . . ? C16 C17 H17 108.2 . . ? O7 C18 O8 124.7(6) . . ? O7 C18 C17 117.5(5) . . ? O8 C18 C17 117.8(5) . . ? C23 C19 C20 119.5(7) . . ? C23 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? N4 C20 C19 123.9(7) . . ? N4 C20 H20 118.0 . . ? C19 C20 H20 118.0 . . ? N4 C21 C22 125.1(7) . . ? N4 C21 H21 117.4 . . ? C22 C21 H21 117.4 . . ? C21 C22 C23 117.7(7) . . ? C21 C22 H22 121.2 . . ? C23 C22 H22 121.2 . . ? C19 C23 C22 118.4(5) . . ? C19 C23 C24 122.1(7) . . ? C22 C23 C24 119.5(6) . . ? C25 C24 C28 116.8(5) . . ? C25 C24 C23 122.6(7) . . ? C28 C24 C23 120.5(7) . . ? C24 C25 C26 120.2(7) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? N5 C26 C25 122.6(7) . . ? N5 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? N5 C27 C28 125.5(7) . . ? N5 C27 H27 117.2 . . ? C28 C27 H27 117.2 . . ? C27 C28 C24 118.8(7) . . ? C27 C28 H28 120.6 . . ? C24 C28 H28 120.6 . . ? N6 C29 C30 123.9(8) . . ? N6 C29 H29 118.1 . . ? C30 C29 H29 118.1 . . ? C31 C30 C29 119.8(8) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C30 116.6(6) . . ? C32 C31 C31 122.2(8) . 2_565 ? C30 C31 C31 121.2(9) . 2_565 ? C31 C32 C33 120.5(8) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? N6 C33 C32 122.6(7) . . ? N6 C33 H33 118.7 . . ? C32 C33 H33 118.7 . . ? N7 C34 C35 121.6(6) . . ? N7 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C34 C35 C36 121.1(6) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C35 C36 C35 115.8(7) . 2_665 ? C35 C36 C37 122.1(3) . . ? C35 C36 C37 122.1(3) 2_665 . ? C38 C37 C38 117.0(7) . 2_665 ? C38 C37 C36 121.5(3) . . ? C38 C37 C36 121.5(3) 2_665 . ? C39 C38 C37 119.3(6) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? N8 C39 C38 123.6(6) . . ? N8 C39 H39 118.2 . . ? C38 C39 H39 118.2 . . ? C4 N1 C2 121.4(6) . . ? C4 N1 H1 119.3 . . ? C2 N1 H1 119.3 . . ? C11 N2 C13 123.5(7) . . ? C11 N2 H2A 118.2 . . ? C13 N2 H2A 118.2 . . ? C15 N3 C17 118.9(5) . . ? C15 N3 H3 120.6 . . ? C17 N3 H3 120.6 . . ? C20 N4 C21 115.3(5) . . ? C20 N4 Co2 121.1(4) . . ? C21 N4 Co2 123.6(4) . . ? C26 N5 C27 115.8(5) . . ? C26 N5 Co2 121.3(4) . 1_554 ? C27 N5 Co2 122.8(4) . 1_554 ? C33 N6 C29 116.6(6) . . ? C33 N6 Co2 122.4(4) . . ? C29 N6 Co2 121.0(5) . . ? C34 N7 C34 118.7(6) . 2_665 ? C34 N7 Co1 120.6(3) . . ? C34 N7 Co1 120.6(3) 2_665 . ? C39 N8 C39 117.2(7) . 2_665 ? C39 N8 Co1 121.4(3) . 1_556 ? C39 N8 Co1 121.4(3) 2_665 1_556 ? C1 O1 Co1 151.1(4) . . ? C1 O1 Co2 89.6(3) . . ? Co1 O1 Co2 119.17(19) . . ? C1 O2 Co2 91.8(4) . . ? C18 O7 Co2 130.9(4) . 3_556 ? C18 O8 Co1 147.7(4) . 3_556 ? H101 O10 H102 105.9 . . ? H111 O11 H112 109.4 . . ? H121 O12 H122 123.6 . . ? H131 O13 H132 111.0 . . ? H141 O14 H142 110.8 . . ? H151 O15 H152 110.9 . . ? H161 O16 H162 109.4 . . ? H171 O17 H172 109.5 . . ? H181 O18 H182 109.5 . . ? H191 O19 H192 114.5 . . ? H201 O20 H202 109.6 . . ? H211 O21 H212 109.5 . . ? H221 O22 H222 109.7 . . ? H231 O23 H232 103.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 -153.2(5) . . . . ? O2 C1 C2 N1 28.6(8) . . . . ? O1 C1 C2 C3 86.2(7) . . . . ? O2 C1 C2 C3 -92.0(7) . . . . ? O3 C4 C5 C6 31.4(11) . . . . ? N1 C4 C5 C6 -152.8(7) . . . . ? O3 C4 C5 C10 -146.4(7) . . . . ? N1 C4 C5 C10 29.5(9) . . . . ? C10 C5 C6 C7 2.2(12) . . . . ? C4 C5 C6 C7 -175.6(7) . . . . ? C5 C6 C7 C8 -2.8(13) . . . . ? C5 C6 C7 C11 -179.4(7) . . . . ? C6 C7 C8 C9 1.2(12) . . . . ? C11 C7 C8 C9 177.9(7) . . . . ? C7 C8 C9 C10 1.1(11) . . . . ? C7 C8 C9 C15 -177.5(7) . . . . ? C8 C9 C10 C5 -1.7(10) . . . . ? C15 C9 C10 C5 176.8(6) . . . . ? C6 C5 C10 C9 0.1(11) . . . . ? C4 C5 C10 C9 177.9(6) . . . . ? C6 C7 C11 O6 150.9(9) . . . . ? C8 C7 C11 O6 -25.7(13) . . . . ? C6 C7 C11 N2 -30.1(12) . . . . ? C8 C7 C11 N2 153.2(7) . . . . ? N2 C13 C14 O4 8.5(11) . . . . ? C12 C13 C14 O4 -115.2(9) . . . . ? N2 C13 C14 O5 -173.3(7) . . . . ? C12 C13 C14 O5 63.1(11) . . . . ? C10 C9 C15 O9 155.1(7) . . . . ? C8 C9 C15 O9 -26.4(11) . . . . ? C10 C9 C15 N3 -25.7(10) . . . . ? C8 C9 C15 N3 152.9(7) . . . . ? N3 C17 C18 O7 37.0(7) . . . . ? C16 C17 C18 O7 -85.6(7) . . . . ? N3 C17 C18 O8 -145.4(5) . . . . ? C16 C17 C18 O8 92.0(7) . . . . ? C23 C19 C20 N4 0.2(11) . . . . ? N4 C21 C22 C23 -2.4(11) . . . . ? C20 C19 C23 C22 -2.1(10) . . . . ? C20 C19 C23 C24 178.5(6) . . . . ? C21 C22 C23 C19 3.1(10) . . . . ? C21 C22 C23 C24 -177.5(6) . . . . ? C19 C23 C24 C25 138.6(8) . . . . ? C22 C23 C24 C25 -40.7(10) . . . . ? C19 C23 C24 C28 -43.7(9) . . . . ? C22 C23 C24 C28 136.9(7) . . . . ? C28 C24 C25 C26 0.9(10) . . . . ? C23 C24 C25 C26 178.7(7) . . . . ? C24 C25 C26 N5 -3.0(12) . . . . ? N5 C27 C28 C24 -2.6(11) . . . . ? C25 C24 C28 C27 1.6(10) . . . . ? C23 C24 C28 C27 -176.2(6) . . . . ? N6 C29 C30 C31 -1.2(18) . . . . ? C29 C30 C31 C32 1.4(16) . . . . ? C29 C30 C31 C31 -177.3(8) . . . 2_565 ? C30 C31 C32 C33 -1.5(15) . . . . ? C31 C31 C32 C33 177.1(7) 2_565 . . . ? C31 C32 C33 N6 1.5(16) . . . . ? N7 C34 C35 C36 -0.5(9) . . . . ? C34 C35 C36 C35 0.2(4) . . . 2_665 ? C34 C35 C36 C37 -179.8(4) . . . . ? C35 C36 C37 C38 -42.2(4) . . . . ? C35 C36 C37 C38 137.8(4) 2_665 . . . ? C35 C36 C37 C38 137.8(4) . . . 2_665 ? C35 C36 C37 C38 -42.2(4) 2_665 . . 2_665 ? C38 C37 C38 C39 0.3(4) 2_665 . . . ? C36 C37 C38 C39 -179.7(4) . . . . ? C37 C38 C39 N8 -0.6(9) . . . . ? O3 C4 N1 C2 4.9(10) . . . . ? C5 C4 N1 C2 -171.0(5) . . . . ? C1 C2 N1 C4 74.1(7) . . . . ? C3 C2 N1 C4 -164.8(6) . . . . ? O6 C11 N2 C13 -3.3(13) . . . . ? C7 C11 N2 C13 177.7(7) . . . . ? C12 C13 N2 C11 -117.8(10) . . . . ? C14 C13 N2 C11 118.0(9) . . . . ? O9 C15 N3 C17 -3.2(10) . . . . ? C9 C15 N3 C17 177.5(6) . . . . ? C18 C17 N3 C15 70.1(7) . . . . ? C16 C17 N3 C15 -167.2(6) . . . . ? C19 C20 N4 C21 0.6(10) . . . . ? C19 C20 N4 Co2 -178.8(5) . . . . ? C22 C21 N4 C20 0.5(11) . . . . ? C22 C21 N4 Co2 179.9(6) . . . . ? O7 Co2 N4 C20 37.4(5) 3_546 . . . ? N6 Co2 N4 C20 -56.3(5) . . . . ? N5 Co2 N4 C20 -112(4) 1_556 . . . ? O2 Co2 N4 C20 -159.0(5) . . . . ? O1 Co2 N4 C20 141.0(5) . . . . ? O7 Co2 N4 C21 -142.0(5) 3_546 . . . ? N6 Co2 N4 C21 124.4(5) . . . . ? N5 Co2 N4 C21 68(4) 1_556 . . . ? O2 Co2 N4 C21 21.6(5) . . . . ? O1 Co2 N4 C21 -38.3(5) . . . . ? C25 C26 N5 C27 2.2(10) . . . . ? C25 C26 N5 Co2 178.6(6) . . . 1_554 ? C28 C27 N5 C26 0.6(10) . . . . ? C28 C27 N5 Co2 -175.8(5) . . . 1_554 ? C32 C33 N6 C29 -1.2(13) . . . . ? C32 C33 N6 Co2 178.8(7) . . . . ? C30 C29 N6 C33 1.0(15) . . . . ? C30 C29 N6 Co2 -179.0(9) . . . . ? O7 Co2 N6 C33 16.6(6) 3_546 . . . ? N5 Co2 N6 C33 -76.8(6) 1_556 . . . ? N4 Co2 N6 C33 105.8(6) . . . . ? O2 Co2 N6 C33 -164.6(6) . . . . ? O1 Co2 N6 C33 -159.7(6) . . . . ? O7 Co2 N6 C29 -163.4(6) 3_546 . . . ? N5 Co2 N6 C29 103.2(7) 1_556 . . . ? N4 Co2 N6 C29 -74.2(7) . . . . ? O2 Co2 N6 C29 15.4(7) . . . . ? O1 Co2 N6 C29 20.3(10) . . . . ? C35 C34 N7 C34 0.3(5) . . . 2_665 ? C35 C34 N7 Co1 -179.7(5) . . . . ? O8 Co1 N7 C34 -135.6(3) 3_546 . . . ? O8 Co1 N7 C34 44.4(3) 4_566 . . . ? O1 Co1 N7 C34 -42.8(3) . . . . ? O1 Co1 N7 C34 137.2(3) 2_665 . . . ? N8 Co1 N7 C34 126(100) 1_554 . . . ? O8 Co1 N7 C34 44.4(3) 3_546 . . 2_665 ? O8 Co1 N7 C34 -135.6(3) 4_566 . . 2_665 ? O1 Co1 N7 C34 137.2(3) . . . 2_665 ? O1 Co1 N7 C34 -42.8(3) 2_665 . . 2_665 ? N8 Co1 N7 C34 -54(100) 1_554 . . 2_665 ? C38 C39 N8 C39 0.3(5) . . . 2_665 ? C38 C39 N8 Co1 -179.7(5) . . . 1_556 ? O2 C1 O1 Co1 -175.7(5) . . . . ? C2 C1 O1 Co1 6.1(11) . . . . ? O2 C1 O1 Co2 0.1(5) . . . . ? C2 C1 O1 Co2 -178.1(5) . . . . ? O8 Co1 O1 C1 173.7(8) 3_546 . . . ? O8 Co1 O1 C1 -1.8(8) 4_566 . . . ? O1 Co1 O1 C1 -94.1(8) 2_665 . . . ? N7 Co1 O1 C1 85.9(8) . . . . ? N8 Co1 O1 C1 -94.1(8) 1_554 . . . ? O8 Co1 O1 Co2 -1.5(2) 3_546 . . . ? O8 Co1 O1 Co2 -177.1(2) 4_566 . . . ? O1 Co1 O1 Co2 90.66(19) 2_665 . . . ? N7 Co1 O1 Co2 -89.34(18) . . . . ? N8 Co1 O1 Co2 90.66(18) 1_554 . . . ? O7 Co2 O1 C1 178.2(3) 3_546 . . . ? N6 Co2 O1 C1 -5.5(7) . . . . ? N5 Co2 O1 C1 -88.2(3) 1_556 . . . ? N4 Co2 O1 C1 88.8(4) . . . . ? O2 Co2 O1 C1 -0.1(3) . . . . ? O7 Co2 O1 Co1 -4.1(2) 3_546 . . . ? N6 Co2 O1 Co1 172.2(5) . . . . ? N5 Co2 O1 Co1 89.5(2) 1_556 . . . ? N4 Co2 O1 Co1 -93.5(2) . . . . ? O2 Co2 O1 Co1 177.6(3) . . . . ? O1 C1 O2 Co2 -0.1(6) . . . . ? C2 C1 O2 Co2 178.1(5) . . . . ? O7 Co2 O2 C1 -5.9(7) 3_546 . . . ? N6 Co2 O2 C1 178.4(3) . . . . ? N5 Co2 O2 C1 90.7(4) 1_556 . . . ? N4 Co2 O2 C1 -91.6(4) . . . . ? O1 Co2 O2 C1 0.1(3) . . . . ? O8 C18 O7 Co2 -4.8(9) . . . 3_556 ? C17 C18 O7 Co2 172.7(4) . . . 3_556 ? O7 C18 O8 Co1 -10.1(12) . . . 3_556 ? C17 C18 O8 Co1 172.4(5) . . . 3_556 ? 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 N1 H1 O5 0.87 2.34 3.214(8) 177.1 1_554 N2 H2A O10 0.87 2.54 3.394(10) 169.3 1_556 N3 H3 O5 0.87 2.27 3.126(7) 169.5 1_554 O10 H101 O3 0.85 2.10 2.945(8) 170.5 1_554 O10 H102 O15 0.85 2.42 3.269(14) 179.8 . O11 H111 O2 0.85 2.00 2.847(7) 179.8 . O11 H112 O4 0.85 1.89 2.654(8) 149.0 1_554 O12 H121 O5 0.85 2.17 2.844(9) 135.4 1_554 O12 H122 O13 0.85 2.05 2.899(12) 179.3 4_566 O13 H131 O11 0.85 1.97 2.796(10) 162.1 . O13 H132 O17 0.85 2.22 2.874(14) 133.4 . O14 H141 O10 0.85 1.95 2.800(11) 177.9 4_466 O14 H142 O9 0.85 2.29 2.810(8) 119.7 . O15 H151 O4 0.85 1.93 2.708(10) 152.2 1_554 O15 H152 O16 0.85 1.92 2.769(15) 177.9 1_554 O16 H161 O14 0.85 2.11 2.789(14) 136.1 . O16 H162 O23 0.85 2.17 2.91(2) 144.1 1_556 O17 H171 O13 0.85 2.40 2.874(14) 116.0 . O17 H172 O16 0.85 2.28 2.832(16) 123.1 . O18 H181 O6 0.85 2.00 2.851(14) 178.9 1_554 O18 H182 O20 0.85 2.51 2.938(16) 112.4 4_566 O19 H191 O11 0.85 2.22 3.074(16) 179.8 . O19 H192 O15 0.82 2.34 2.973(18) 134.6 . O20 H201 O18 0.85 2.22 2.814(17) 127.1 3_546 O20 H202 O17 0.85 2.40 2.886(15) 116.5 . O21 H211 O18 0.85 2.37 2.953(19) 125.5 1_546 O21 H212 O19 0.85 2.50 3.12(2) 130.1 3_546 O22 H221 O23 0.85 1.98 2.83(2) 179.0 4_566 O22 H222 O12 0.85 1.88 2.73(2) 178.3 . O23 H231 O20 0.85 2.07 2.92(2) 178.9 1_554 O23 H232 O19 0.85 2.08 2.93(2) 179.8 . _chemical_absolute_configuration rmad _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.547 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.083 # Attachment '3.CIF' data_r91103e1 _database_code_depnum_ccdc_archive 'CCDC 794254' #TrackingRef '- Compound 1-3.cif' #TrackingRef '3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H68 N14 Ni3 O18, 2(C2 H6 O), 14(H2 O)' _chemical_formula_sum 'C80 H108 N14 Ni3 O34' _chemical_formula_weight 1985.93 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 18.495(4) _cell_length_b 24.215(5) _cell_length_c 11.297(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5059.2(18) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 14793 _cell_measurement_theta_min 2.011 _cell_measurement_theta_max 27.866 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2084 _exptl_absorpt_coefficient_mu 0.636 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8834 _exptl_absorpt_correction_T_max 0.9629 _exptl_absorpt_process_details crystalclear _exptl_special_details ; Two disordered water molecules at (0.000,0.500, -0.005) and (0.500, 0.000, 0.004) were removed by the SQUEEZE routine in PLATON ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34659 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8930 _reflns_number_gt 8164 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _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. ; _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^)+(0.0685P)^2^+1.3691P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00152(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.028(12) _refine_ls_number_reflns 8930 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1173 _refine_ls_wR_factor_gt 0.1145 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.5000 0.5000 0.46507(3) 0.00893(7) Uani 1 2 d S . . Ni2 Ni 0.698972(12) 0.477910(10) 0.46707(2) 0.01159(5) Uani 1 1 d . . . C1 C 0.61559(10) 0.39729(7) 0.46439(16) 0.0103(4) Uani 1 1 d . . . C2 C 0.56642(10) 0.34650(7) 0.46789(17) 0.0134(4) Uani 1 1 d . . . H2 H 0.5210 0.3550 0.4252 0.016 Uiso 1 1 calc R . . C3 C 0.54830(11) 0.33165(9) 0.59573(17) 0.0182(5) Uani 1 1 d . . . H3A H 0.5914 0.3180 0.6351 0.027 Uiso 1 1 calc R . . H3B H 0.5113 0.3033 0.5968 0.027 Uiso 1 1 calc R . . H3C H 0.5307 0.3642 0.6367 0.027 Uiso 1 1 calc R . . C4 C 0.60854(11) 0.29824(9) 0.29145(17) 0.0180(5) Uani 1 1 d . . . C5 C 0.65669(12) 0.25330(8) 0.24644(17) 0.0183(5) Uani 1 1 d . . . C6 C 0.64456(13) 0.23233(9) 0.13251(17) 0.0239(6) Uani 1 1 d . . . H6 H 0.6058 0.2457 0.0870 0.029 Uiso 1 1 calc R . . C7 C 0.68972(13) 0.19183(9) 0.08689(17) 0.0242(6) Uani 1 1 d . . . C8 C 0.74619(12) 0.17185(9) 0.15580(17) 0.0224(6) Uani 1 1 d . . . H8 H 0.7770 0.1446 0.1249 0.027 Uiso 1 1 calc R . . C9 C 0.75780(11) 0.19165(9) 0.27023(17) 0.0181(5) Uani 1 1 d . . . C10 C 0.71370(11) 0.23399(8) 0.31372(17) 0.0163(5) Uani 1 1 d . . . H10 H 0.7229 0.2493 0.3887 0.020 Uiso 1 1 calc R . . C11 C 0.67871(13) 0.16795(10) -0.0355(2) 0.0316(6) Uani 1 1 d . . . C12 C 0.54209(14) 0.18524(12) -0.2523(2) 0.0398(8) Uani 1 1 d . . . H12A H 0.5269 0.2234 -0.2444 0.060 Uiso 1 1 calc R . . H12B H 0.5169 0.1628 -0.1944 0.060 Uiso 1 1 calc R . . H12C H 0.5307 0.1721 -0.3313 0.060 Uiso 1 1 calc R . . C13 C 0.62428(13) 0.18106(11) -0.23142(18) 0.0308(7) Uani 1 1 d . . . H13 H 0.6388 0.1419 -0.2404 0.037 Uiso 1 1 calc R . . C14 C 0.66595(13) 0.21554(11) -0.3226(2) 0.0308(7) Uani 1 1 d . . . C15 C 0.81679(11) 0.16823(8) 0.34314(17) 0.0174(5) Uani 1 1 d . . . C16 C 0.84976(13) 0.16836(9) 0.66588(18) 0.0259(6) Uani 1 1 d . . . H16A H 0.8043 0.1525 0.6920 0.039 Uiso 1 1 calc R . . H16B H 0.8469 0.2083 0.6698 0.039 Uiso 1 1 calc R . . H16C H 0.8885 0.1555 0.7167 0.039 Uiso 1 1 calc R . . C17 C 0.86480(10) 0.15069(8) 0.53862(17) 0.0157(5) Uani 1 1 d . . . H17 H 0.9109 0.1675 0.5127 0.019 Uiso 1 1 calc R . . C18 C 0.87220(10) 0.08770(8) 0.53369(16) 0.0111(4) Uani 1 1 d . . . C19 C 0.73522(12) 0.51916(9) 0.83725(17) 0.0206(5) Uani 1 1 d . . . H19 H 0.7567 0.5493 0.8762 0.025 Uiso 1 1 calc R . . C20 C 0.73184(11) 0.51742(9) 0.71517(17) 0.0189(5) Uani 1 1 d . . . H20 H 0.7506 0.5476 0.6728 0.023 Uiso 1 1 calc R . . C21 C 0.67784(12) 0.43261(9) 0.71780(17) 0.0231(6) Uani 1 1 d . . . H21 H 0.6588 0.4020 0.6772 0.028 Uiso 1 1 calc R . . C22 C 0.67790(13) 0.43129(9) 0.83801(16) 0.0219(6) Uani 1 1 d . . . H22 H 0.6588 0.4006 0.8782 0.026 Uiso 1 1 calc R . . C23 C 0.70634(11) 0.47551(9) 0.90138(16) 0.0177(5) Uani 1 1 d . . . C24 C 0.70457(10) 0.47590(8) 1.03238(16) 0.0156(5) Uani 1 1 d . . . C25 C 0.71564(12) 0.42799(9) 1.09809(17) 0.0212(6) Uani 1 1 d . . . H25 H 0.7249 0.3943 1.0596 0.025 Uiso 1 1 calc R . . C26 C 0.71295(12) 0.43035(9) 1.22047(17) 0.0214(6) Uani 1 1 d . . . H26 H 0.7219 0.3979 1.2637 0.026 Uiso 1 1 calc R . . C27 C 0.68656(12) 0.52252(9) 1.21562(17) 0.0214(5) Uani 1 1 d . . . H27 H 0.6756 0.5554 1.2561 0.026 Uiso 1 1 calc R . . C28 C 0.68974(11) 0.52425(9) 1.09401(16) 0.0190(5) Uani 1 1 d . . . H28 H 0.6820 0.5576 1.0533 0.023 Uiso 1 1 calc R . . C29 C 0.85354(11) 0.44388(9) 0.4833(2) 0.0269(6) Uani 1 1 d . . . H29 H 0.8327 0.4101 0.5059 0.032 Uiso 1 1 calc R . . C30 C 0.92832(12) 0.44732(10) 0.4770(2) 0.0295(6) Uani 1 1 d . . . H30 H 0.9571 0.4163 0.4939 0.035 Uiso 1 1 calc R . . C31 C 0.95966(11) 0.49649(9) 0.44597(18) 0.0221(5) Uani 1 1 d . . . C32 C 0.91509(12) 0.54028(10) 0.4182(2) 0.0309(6) Uani 1 1 d . . . H32 H 0.9350 0.5743 0.3945 0.037 Uiso 1 1 calc R . . C33 C 0.84057(12) 0.53378(9) 0.4256(2) 0.0273(6) Uani 1 1 d . . . H33 H 0.8107 0.5639 0.4068 0.033 Uiso 1 1 calc R . . C34 C 0.50867(11) 0.45335(8) 0.21802(16) 0.0139(5) Uani 1 1 d . . . H34 H 0.5152 0.4202 0.2598 0.017 Uiso 1 1 calc R . . C35 C 0.50848(11) 0.45130(8) 0.09652(16) 0.0148(5) Uani 1 1 d . . . H35 H 0.5140 0.4174 0.0571 0.018 Uiso 1 1 calc R . . C36 C 0.5000 0.5000 0.0320(2) 0.0132(6) Uani 1 2 d S . . C37 C 0.5000 0.5000 -0.0984(2) 0.0124(6) Uani 1 2 d S . . C38 C 0.46430(11) 0.45937(9) -0.16374(17) 0.0164(5) Uani 1 1 d . . . H38 H 0.4396 0.4309 -0.1244 0.020 Uiso 1 1 calc R . . C39 C 0.46522(11) 0.46094(8) -0.28614(16) 0.0142(5) Uani 1 1 d . . . H39 H 0.4402 0.4333 -0.3278 0.017 Uiso 1 1 calc R . . N1 N 0.60135(9) 0.30034(7) 0.41096(14) 0.0154(4) Uani 1 1 d . . . H1 H 0.6181 0.2734 0.4539 0.018 Uiso 1 1 calc R . . N2 N 0.64068(12) 0.19848(9) -0.11039(15) 0.0339(6) Uani 1 1 d . . . H2A H 0.6247 0.2304 -0.0864 0.041 Uiso 1 1 calc R . . N3 N 0.80721(9) 0.16995(6) 0.46115(14) 0.0156(4) Uani 1 1 d . . . H3 H 0.7670 0.1825 0.4908 0.019 Uiso 1 1 calc R . . N4 N 0.70346(9) 0.47528(7) 0.65288(13) 0.0166(4) Uani 1 1 d . . . N5 N 0.69816(8) 0.47685(7) 1.28009(13) 0.0131(4) Uani 1 1 d . . . N6 N 0.80981(8) 0.48607(7) 0.45869(13) 0.0166(4) Uani 1 1 d . . . N7 N 0.5000 0.5000 0.28035(18) 0.0123(5) Uani 1 2 d S . . N8 N 0.5000 0.5000 -0.34850(18) 0.0095(5) Uani 1 2 d S . . O1 O 0.59029(7) 0.44598(5) 0.46916(11) 0.0129(3) Uani 1 1 d . . . O2 O 0.68306(7) 0.39100(5) 0.46238(11) 0.0141(3) Uani 1 1 d . . . O3 O 0.57967(8) 0.33259(6) 0.22548(12) 0.0243(4) Uani 1 1 d . . . O4 O 0.70197(12) 0.25580(9) -0.28785(16) 0.0541(6) Uani 1 1 d . . . O5 O 0.65991(9) 0.20123(8) -0.42936(13) 0.0366(5) Uani 1 1 d . . . O6 O 0.70525(12) 0.12305(8) -0.06073(15) 0.0631(6) Uani 1 1 d . . . O7 O 0.81518(7) 0.05976(5) 0.52548(11) 0.0135(3) Uani 1 1 d . . . O8 O 0.93579(7) 0.06884(5) 0.54200(11) 0.0132(3) Uani 1 1 d . . . O9 O 0.87165(8) 0.14796(7) 0.29726(12) 0.0234(4) Uani 1 1 d . . . O10 O 0.78349(9) 0.31184(7) 0.55379(16) 0.0411(5) Uani 1 1 d . . . H101 H 0.7579 0.2942 0.6036 0.062 Uiso 1 1 d R . . H102 H 0.7566 0.3339 0.5149 0.062 Uiso 1 1 d R . . O11 O 0.58205(14) 0.32492(8) -0.03652(17) 0.0669(7) Uani 1 1 d . . . H111 H 0.5816 0.3271 0.0386 0.100 Uiso 1 1 d R . . H112 H 0.5368 0.3246 -0.0495 0.100 Uiso 1 1 d R . . O12 O 1.04536(13) 0.34315(10) 0.5582(2) 0.0735(8) Uani 1 1 d . . . H12 H 1.0806 0.3255 0.5328 0.110 Uiso 1 1 calc R . . C40 C 1.0650(3) 0.3707(2) 0.6653(3) 0.139(2) Uani 1 1 d . . . H40A H 1.0712 0.4103 0.6510 0.166 Uiso 1 1 calc R . . H40B H 1.1105 0.3558 0.6960 0.166 Uiso 1 1 calc R . . C41 C 1.0039(4) 0.3609(4) 0.7540(5) 0.340(4) Uani 1 1 d . . . H41A H 1.0167 0.3773 0.8295 0.510 Uiso 1 1 calc R . . H41B H 0.9965 0.3215 0.7640 0.510 Uiso 1 1 calc R . . H41C H 0.9598 0.3777 0.7248 0.510 Uiso 1 1 calc R . . O13 O 0.43502(15) 0.32460(10) -0.0795(2) 0.1099(9) Uani 1 1 d . . . H131 H 0.4167 0.2937 -0.0600 0.165 Uiso 1 1 d R . . H132 H 0.4239 0.3211 -0.1518 0.165 Uiso 1 1 d R . . O14 O 0.92213(17) 0.27958(13) 0.4823(4) 0.1903(17) Uani 1 1 d . . . H141 H 0.9313 0.3043 0.5344 0.286 Uiso 1 1 d R . . H142 H 0.8818 0.2642 0.4981 0.286 Uiso 1 1 d R . . O15 O 0.3805(4) 0.2328(5) -0.0203(7) 0.460(6) Uani 1 1 d . . . H151 H 0.3441 0.2265 0.0242 0.691 Uiso 1 1 d R . . H152 H 0.3776 0.2129 -0.0822 0.691 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.00911(14) 0.00974(15) 0.00795(14) 0.000 0.000 -0.00024(13) Ni2 0.00932(10) 0.01498(11) 0.01048(10) 0.00038(10) -0.00032(10) 0.00003(10) C1 0.0117(9) 0.0136(9) 0.0055(8) -0.0039(8) 0.0038(8) 0.0037(7) C2 0.0114(8) 0.0139(9) 0.0151(8) -0.0008(9) 0.0004(8) 0.0003(8) C3 0.0161(10) 0.0188(11) 0.0197(10) 0.0040(9) 0.0053(8) -0.0018(9) C4 0.0141(10) 0.0197(11) 0.0200(9) -0.0019(9) -0.0036(8) 0.0048(9) C5 0.0234(11) 0.0145(10) 0.0170(9) -0.0010(8) 0.0014(9) 0.0052(9) C6 0.0365(12) 0.0210(11) 0.0144(9) -0.0025(9) -0.0053(10) 0.0154(10) C7 0.0319(12) 0.0247(11) 0.0159(9) -0.0030(9) -0.0033(9) 0.0042(10) C8 0.0249(11) 0.0225(11) 0.0198(10) -0.0040(9) -0.0005(9) 0.0073(10) C9 0.0196(10) 0.0196(10) 0.0149(9) 0.0018(8) 0.0017(8) 0.0064(9) C10 0.0202(11) 0.0138(10) 0.0148(9) -0.0001(8) -0.0009(8) 0.0014(9) C11 0.0389(13) 0.0346(12) 0.0214(10) -0.0035(11) -0.0057(11) 0.0189(11) C12 0.0367(14) 0.0493(17) 0.0335(13) -0.0003(13) 0.0059(11) -0.0031(13) C13 0.0420(14) 0.0341(14) 0.0162(10) -0.0043(10) -0.0024(10) 0.0051(12) C14 0.0197(12) 0.0440(14) 0.0285(11) -0.0037(11) -0.0009(10) 0.0071(11) C15 0.0210(11) 0.0131(10) 0.0181(9) 0.0033(8) 0.0002(8) 0.0031(9) C16 0.0337(13) 0.0211(11) 0.0229(10) -0.0060(9) -0.0080(10) 0.0108(10) C17 0.0153(9) 0.0149(9) 0.0169(9) 0.0002(9) -0.0038(9) 0.0046(8) C18 0.0150(9) 0.0159(9) 0.0023(7) 0.0019(8) -0.0012(8) 0.0021(8) C19 0.0229(11) 0.0207(10) 0.0181(9) -0.0046(9) -0.0025(8) -0.0028(10) C20 0.0168(10) 0.0230(11) 0.0171(9) 0.0019(9) -0.0023(8) -0.0032(9) C21 0.0307(12) 0.0213(11) 0.0173(10) 0.0005(9) -0.0045(9) -0.0033(10) C22 0.0319(12) 0.0216(11) 0.0121(9) 0.0036(9) -0.0010(9) -0.0054(10) C23 0.0165(10) 0.0243(10) 0.0122(9) 0.0005(9) -0.0004(8) 0.0022(10) C24 0.0149(9) 0.0191(9) 0.0129(8) -0.0026(9) -0.0029(9) -0.0022(9) C25 0.0344(13) 0.0171(10) 0.0122(9) -0.0016(8) 0.0027(9) 0.0050(10) C26 0.0290(12) 0.0207(11) 0.0145(9) 0.0036(9) 0.0025(9) 0.0054(10) C27 0.0296(12) 0.0170(10) 0.0177(9) -0.0045(9) 0.0038(9) -0.0034(10) C28 0.0272(11) 0.0153(10) 0.0145(9) 0.0042(8) -0.0002(9) 0.0002(10) C29 0.0116(10) 0.0209(11) 0.0483(13) 0.0073(11) -0.0018(10) -0.0008(9) C30 0.0177(10) 0.0284(12) 0.0425(12) 0.0070(12) 0.0001(11) 0.0024(10) C31 0.0114(10) 0.0238(11) 0.0309(11) -0.0007(10) 0.0015(9) -0.0007(9) C32 0.0138(11) 0.0254(12) 0.0536(14) 0.0145(11) -0.0007(10) 0.0008(10) C33 0.0140(10) 0.0201(12) 0.0477(13) 0.0109(10) -0.0040(10) 0.0019(9) C34 0.0152(10) 0.0138(10) 0.0126(8) 0.0018(8) -0.0031(8) -0.0002(9) C35 0.0185(10) 0.0126(10) 0.0132(8) -0.0028(8) 0.0039(8) -0.0001(9) C36 0.0081(11) 0.0148(12) 0.0165(12) 0.000 0.000 0.0000(11) C37 0.0098(12) 0.0182(14) 0.0093(12) 0.000 0.000 0.0042(12) C38 0.0170(10) 0.0160(10) 0.0162(9) 0.0017(8) 0.0033(8) -0.0037(9) C39 0.0154(10) 0.0126(10) 0.0145(9) -0.0023(8) 0.0003(8) -0.0029(8) N1 0.0162(8) 0.0141(9) 0.0159(7) 0.0010(7) -0.0024(7) 0.0025(7) N2 0.0487(12) 0.0352(11) 0.0179(9) -0.0030(9) -0.0041(9) 0.0175(10) N3 0.0113(7) 0.0192(8) 0.0162(7) 0.0008(7) 0.0007(7) 0.0073(7) N4 0.0142(8) 0.0194(8) 0.0161(7) -0.0009(7) -0.0017(7) -0.0034(8) N5 0.0097(7) 0.0182(8) 0.0113(7) 0.0003(7) 0.0030(6) 0.0015(8) N6 0.0125(7) 0.0246(9) 0.0127(7) 0.0019(7) 0.0010(7) 0.0003(7) N7 0.0128(11) 0.0134(11) 0.0106(10) 0.000 0.000 0.0001(10) N8 0.0059(10) 0.0100(11) 0.0128(10) 0.000 0.000 0.0014(10) O1 0.0128(6) 0.0151(7) 0.0108(6) -0.0006(6) -0.0014(6) 0.0016(5) O2 0.0111(6) 0.0186(7) 0.0126(6) 0.0021(6) 0.0016(6) 0.0027(5) O3 0.0323(8) 0.0213(8) 0.0195(7) 0.0012(6) -0.0041(6) 0.0149(7) O4 0.0608(13) 0.0639(13) 0.0375(10) -0.0118(9) 0.0145(10) -0.0173(12) O5 0.0301(9) 0.0618(12) 0.0178(7) -0.0026(8) 0.0029(7) 0.0008(9) O6 0.0953(13) 0.0551(11) 0.0390(9) -0.0282(8) -0.0356(9) 0.0552(10) O7 0.0095(6) 0.0190(7) 0.0119(6) 0.0022(6) -0.0030(6) -0.0019(5) O8 0.0102(6) 0.0161(7) 0.0132(6) -0.0015(6) 0.0002(6) 0.0014(5) O9 0.0221(8) 0.0297(8) 0.0185(7) -0.0006(7) 0.0029(6) 0.0108(7) O10 0.0286(9) 0.0390(10) 0.0558(11) 0.0142(9) -0.0028(8) 0.0041(8) O11 0.1124(18) 0.0445(11) 0.0438(10) 0.0113(11) -0.0073(13) 0.0197(12) O12 0.0744(14) 0.0732(15) 0.0728(14) 0.0107(12) 0.0266(12) 0.0340(13) C40 0.218(5) 0.153(4) 0.044(2) 0.012(2) 0.011(3) 0.112(4) C41 0.302(6) 0.599(10) 0.119(3) 0.159(5) 0.120(4) 0.333(6) O13 0.1456(19) 0.0658(15) 0.1183(16) 0.0462(13) -0.1011(14) -0.0498(15) O14 0.105(2) 0.107(2) 0.359(5) -0.109(3) 0.128(2) -0.0422(19) O15 0.227(6) 0.898(18) 0.256(7) 0.165(9) 0.027(6) 0.239(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 Ni1 O8 2.0481(13) 4_456 ? Ni1 O8 2.0482(13) 3_656 ? Ni1 N7 2.087(2) . ? Ni1 N8 2.106(2) 1_556 ? Ni1 O1 2.1217(13) . ? Ni1 O1 2.1217(13) 2_665 ? Ni2 O7 2.0011(14) 3_656 ? Ni2 N6 2.0616(16) . ? Ni2 N4 2.1018(16) . ? Ni2 N5 2.1124(15) 1_554 ? Ni2 O2 2.1256(14) . ? Ni2 O1 2.1538(13) . ? Ni2 C1 2.4881(18) . ? C1 O2 1.257(2) . ? C1 O1 1.270(2) . ? C1 C2 1.530(3) . ? C2 N1 1.442(2) . ? C2 C3 1.526(3) . ? C2 H2 0.9900 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 H3C 0.9700 . ? C4 O3 1.238(2) . ? C4 N1 1.358(3) . ? C4 C5 1.495(3) . ? C5 C10 1.381(3) . ? C5 C6 1.402(3) . ? C6 C7 1.387(3) . ? C6 H6 0.9400 . ? C7 C8 1.390(3) . ? C7 C11 1.512(3) . ? C8 C9 1.395(3) . ? C8 H8 0.9400 . ? C9 C10 1.399(3) . ? C9 C15 1.480(3) . ? C10 H10 0.9400 . ? C11 O6 1.227(3) . ? C11 N2 1.326(3) . ? C12 C13 1.542(4) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 N2 1.463(3) . ? C13 C14 1.534(3) . ? C13 H13 0.9900 . ? C14 O4 1.244(3) . ? C14 O5 1.260(3) . ? C15 O9 1.241(2) . ? C15 N3 1.346(2) . ? C16 C17 1.526(3) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 N3 1.455(2) . ? C17 C18 1.532(3) . ? C17 H17 0.9900 . ? C18 O7 1.256(2) . ? C18 O8 1.265(2) . ? C19 C20 1.381(3) . ? C19 C23 1.388(3) . ? C19 H19 0.9400 . ? C20 N4 1.346(3) . ? C20 H20 0.9400 . ? C21 N4 1.353(3) . ? C21 C22 1.358(3) . ? C21 H21 0.9400 . ? C22 C23 1.391(3) . ? C22 H22 0.9400 . ? C23 C24 1.480(3) . ? C24 C28 1.389(3) . ? C24 C25 1.393(3) . ? C25 C26 1.385(3) . ? C25 H25 0.9400 . ? C26 N5 1.340(3) . ? C26 H26 0.9400 . ? C27 N5 1.342(3) . ? C27 C28 1.376(3) . ? C27 H27 0.9400 . ? C28 H28 0.9400 . ? C29 N6 1.332(3) . ? C29 C30 1.387(3) . ? C29 H29 0.9400 . ? C30 C31 1.370(3) . ? C30 H30 0.9400 . ? C31 C32 1.379(3) . ? C31 C31 1.502(4) 2_765 ? C32 C33 1.390(3) . ? C32 H32 0.9400 . ? C33 N6 1.341(3) . ? C33 H33 0.9400 . ? C34 N7 1.341(2) . ? C34 C35 1.374(3) . ? C34 H34 0.9400 . ? C35 C36 1.395(2) . ? C35 H35 0.9400 . ? C36 C35 1.395(2) 2_665 ? C36 C37 1.473(4) . ? C37 C38 1.396(2) . ? C37 C38 1.396(2) 2_665 ? C38 C39 1.383(3) . ? C38 H38 0.9400 . ? C39 N8 1.343(2) . ? C39 H39 0.9400 . ? N1 H1 0.8700 . ? N2 H2A 0.8700 . ? N3 H3 0.8700 . ? N5 Ni2 2.1124(15) 1_556 ? N7 C34 1.341(2) 2_665 ? N8 C39 1.343(2) 2_665 ? N8 Ni1 2.106(2) 1_554 ? O7 Ni2 2.0010(14) 3_646 ? O8 Ni1 2.0481(13) 3_646 ? O10 H101 0.8502 . ? O10 H102 0.8514 . ? O11 H111 0.8500 . ? O11 H112 0.8502 . ? O12 C40 1.429(5) . ? O12 H12 0.8300 . ? C40 C41 1.528(8) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? O13 H131 0.8510 . ? O13 H132 0.8462 . ? O14 H141 0.8569 . ? O14 H142 0.8528 . ? O15 H151 0.8540 . ? O15 H152 0.8510 . ? 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 O8 Ni1 O8 175.53(7) 4_456 3_656 ? O8 Ni1 N7 87.76(4) 4_456 . ? O8 Ni1 N7 87.76(4) 3_656 . ? O8 Ni1 N8 92.24(4) 4_456 1_556 ? O8 Ni1 N8 92.24(4) 3_656 1_556 ? N7 Ni1 N8 180.000(1) . 1_556 ? O8 Ni1 O1 87.44(5) 4_456 . ? O8 Ni1 O1 92.65(5) 3_656 . ? N7 Ni1 O1 91.25(3) . . ? N8 Ni1 O1 88.75(3) 1_556 . ? O8 Ni1 O1 92.65(5) 4_456 2_665 ? O8 Ni1 O1 87.44(5) 3_656 2_665 ? N7 Ni1 O1 91.25(3) . 2_665 ? N8 Ni1 O1 88.75(3) 1_556 2_665 ? O1 Ni1 O1 177.51(7) . 2_665 ? O7 Ni2 N6 92.12(6) 3_656 . ? O7 Ni2 N4 89.61(6) 3_656 . ? N6 Ni2 N4 90.54(6) . . ? O7 Ni2 N5 93.05(6) 3_656 1_554 ? N6 Ni2 N5 87.84(6) . 1_554 ? N4 Ni2 N5 176.94(6) . 1_554 ? O7 Ni2 O2 164.50(5) 3_656 . ? N6 Ni2 O2 103.38(6) . . ? N4 Ni2 O2 90.02(6) . . ? N5 Ni2 O2 87.83(6) 1_554 . ? O7 Ni2 O1 103.48(5) 3_656 . ? N6 Ni2 O1 164.34(6) . . ? N4 Ni2 O1 90.86(6) . . ? N5 Ni2 O1 90.00(5) 1_554 . ? O2 Ni2 O1 61.03(5) . . ? O7 Ni2 C1 134.16(6) 3_656 . ? N6 Ni2 C1 133.70(6) . . ? N4 Ni2 C1 90.74(6) . . ? N5 Ni2 C1 88.50(6) 1_554 . ? O2 Ni2 C1 30.35(5) . . ? O1 Ni2 C1 30.68(5) . . ? O2 C1 O1 118.62(16) . . ? O2 C1 C2 119.54(16) . . ? O1 C1 C2 121.76(16) . . ? O2 C1 Ni2 58.67(9) . . ? O1 C1 Ni2 59.95(9) . . ? C2 C1 Ni2 177.15(13) . . ? N1 C2 C3 109.76(16) . . ? N1 C2 C1 110.19(15) . . ? C3 C2 C1 110.15(15) . . ? N1 C2 H2 108.9 . . ? C3 C2 H2 108.9 . . ? C1 C2 H2 108.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O3 C4 N1 122.09(19) . . ? O3 C4 C5 122.77(17) . . ? N1 C4 C5 115.07(17) . . ? C10 C5 C6 120.32(19) . . ? C10 C5 C4 120.91(17) . . ? C6 C5 C4 118.72(18) . . ? C7 C6 C5 120.1(2) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C8 119.38(19) . . ? C6 C7 C11 121.9(2) . . ? C8 C7 C11 118.7(2) . . ? C7 C8 C9 121.0(2) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C8 C9 C10 119.17(19) . . ? C8 C9 C15 119.82(19) . . ? C10 C9 C15 121.01(17) . . ? C5 C10 C9 119.98(18) . . ? C5 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? O6 C11 N2 123.9(2) . . ? O6 C11 C7 119.8(2) . . ? N2 C11 C7 116.2(2) . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 111.5(2) . . ? N2 C13 C12 109.20(19) . . ? C14 C13 C12 110.90(19) . . ? N2 C13 H13 108.4 . . ? C14 C13 H13 108.4 . . ? C12 C13 H13 108.4 . . ? O4 C14 O5 124.4(2) . . ? O4 C14 C13 118.9(2) . . ? O5 C14 C13 116.7(2) . . ? O9 C15 N3 122.27(18) . . ? O9 C15 C9 121.47(17) . . ? N3 C15 C9 116.26(18) . . ? C17 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C17 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 C16 110.09(16) . . ? N3 C17 C18 111.26(15) . . ? C16 C17 C18 109.26(16) . . ? N3 C17 H17 108.7 . . ? C16 C17 H17 108.7 . . ? C18 C17 H17 108.7 . . ? O7 C18 O8 126.26(17) . . ? O7 C18 C17 117.62(16) . . ? O8 C18 C17 116.08(16) . . ? C20 C19 C23 118.72(19) . . ? C20 C19 H19 120.6 . . ? C23 C19 H19 120.6 . . ? N4 C20 C19 124.25(19) . . ? N4 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? N4 C21 C22 124.0(2) . . ? N4 C21 H21 118.0 . . ? C22 C21 H21 118.0 . . ? C21 C22 C23 119.8(2) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C19 C23 C22 117.57(17) . . ? C19 C23 C24 121.69(18) . . ? C22 C23 C24 120.73(18) . . ? C28 C24 C25 117.64(17) . . ? C28 C24 C23 120.71(18) . . ? C25 C24 C23 121.62(18) . . ? C26 C25 C24 119.51(19) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? N5 C26 C25 122.95(19) . . ? N5 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? N5 C27 C28 124.09(19) . . ? N5 C27 H27 118.0 . . ? C28 C27 H27 118.0 . . ? C27 C28 C24 118.89(19) . . ? C27 C28 H28 120.6 . . ? C24 C28 H28 120.6 . . ? N6 C29 C30 123.3(2) . . ? N6 C29 H29 118.4 . . ? C30 C29 H29 118.4 . . ? C31 C30 C29 119.1(2) . . ? C31 C30 H30 120.4 . . ? C29 C30 H30 120.4 . . ? C30 C31 C32 118.3(2) . . ? C30 C31 C31 121.2(2) . 2_765 ? C32 C31 C31 120.5(2) . 2_765 ? C31 C32 C33 119.5(2) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? N6 C33 C32 122.4(2) . . ? N6 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? N7 C34 C35 123.71(18) . . ? N7 C34 H34 118.1 . . ? C35 C34 H34 118.1 . . ? C34 C35 C36 119.45(19) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C35 C36 C35 117.0(2) . 2_665 ? C35 C36 C37 121.48(12) . . ? C35 C36 C37 121.48(12) 2_665 . ? C38 C37 C38 116.1(2) . 2_665 ? C38 C37 C36 121.93(12) . . ? C38 C37 C36 121.93(12) 2_665 . ? C39 C38 C37 120.24(19) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? N8 C39 C38 123.32(18) . . ? N8 C39 H39 118.3 . . ? C38 C39 H39 118.3 . . ? C4 N1 C2 121.09(17) . . ? C4 N1 H1 119.5 . . ? C2 N1 H1 119.5 . . ? C11 N2 C13 123.1(2) . . ? C11 N2 H2A 118.5 . . ? C13 N2 H2A 118.5 . . ? C15 N3 C17 119.31(16) . . ? C15 N3 H3 120.3 . . ? C17 N3 H3 120.3 . . ? C20 N4 C21 115.61(16) . . ? C20 N4 Ni2 120.97(13) . . ? C21 N4 Ni2 123.42(13) . . ? C26 N5 C27 116.89(16) . . ? C26 N5 Ni2 120.75(13) . 1_556 ? C27 N5 Ni2 122.28(13) . 1_556 ? C29 N6 C33 117.46(18) . . ? C29 N6 Ni2 121.37(14) . . ? C33 N6 Ni2 121.15(14) . . ? C34 N7 C34 116.6(2) . 2_665 ? C34 N7 Ni1 121.68(11) . . ? C34 N7 Ni1 121.68(11) 2_665 . ? C39 N8 C39 116.7(2) . 2_665 ? C39 N8 Ni1 121.63(11) . 1_554 ? C39 N8 Ni1 121.63(11) 2_665 1_554 ? C1 O1 Ni1 149.50(12) . . ? C1 O1 Ni2 89.37(10) . . ? Ni1 O1 Ni2 120.86(6) . . ? C1 O2 Ni2 90.98(11) . . ? C18 O7 Ni2 129.79(12) . 3_646 ? C18 O8 Ni1 146.08(12) . 3_646 ? H101 O10 H102 109.4 . . ? H111 O11 H112 99.3 . . ? C40 O12 H12 109.5 . . ? O12 C40 C41 107.2(5) . . ? O12 C40 H40A 110.3 . . ? C41 C40 H40A 110.3 . . ? O12 C40 H40B 110.3 . . ? C41 C40 H40B 110.3 . . ? H40A C40 H40B 108.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? H131 O13 H132 93.7 . . ? H141 O14 H142 109.5 . . ? H151 O15 H152 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Ni2 C1 O2 -178.95(9) 3_656 . . . ? N6 Ni2 C1 O2 2.67(14) . . . . ? N4 Ni2 C1 O2 -88.78(11) . . . . ? N5 Ni2 C1 O2 88.26(11) 1_554 . . . ? O1 Ni2 C1 O2 -179.23(17) . . . . ? O7 Ni2 C1 O1 0.28(14) 3_656 . . . ? N6 Ni2 C1 O1 -178.10(9) . . . . ? N4 Ni2 C1 O1 90.45(11) . . . . ? N5 Ni2 C1 O1 -92.52(10) 1_554 . . . ? O2 Ni2 C1 O1 179.23(17) . . . . ? O7 Ni2 C1 C2 -127(3) 3_656 . . . ? N6 Ni2 C1 C2 54(3) . . . . ? N4 Ni2 C1 C2 -37(3) . . . . ? N5 Ni2 C1 C2 140(3) 1_554 . . . ? O2 Ni2 C1 C2 52(3) . . . . ? O1 Ni2 C1 C2 -128(3) . . . . ? O2 C1 C2 N1 -28.7(2) . . . . ? O1 C1 C2 N1 154.78(16) . . . . ? Ni2 C1 C2 N1 -79(3) . . . . ? O2 C1 C2 C3 92.6(2) . . . . ? O1 C1 C2 C3 -84.0(2) . . . . ? Ni2 C1 C2 C3 42(3) . . . . ? O3 C4 C5 C10 147.7(2) . . . . ? N1 C4 C5 C10 -29.3(3) . . . . ? O3 C4 C5 C6 -30.0(3) . . . . ? N1 C4 C5 C6 153.0(2) . . . . ? C10 C5 C6 C7 0.3(3) . . . . ? C4 C5 C6 C7 178.0(2) . . . . ? C5 C6 C7 C8 0.9(3) . . . . ? C5 C6 C7 C11 180.0(2) . . . . ? C6 C7 C8 C9 0.4(3) . . . . ? C11 C7 C8 C9 -178.7(2) . . . . ? C7 C8 C9 C10 -2.8(3) . . . . ? C7 C8 C9 C15 177.9(2) . . . . ? C6 C5 C10 C9 -2.7(3) . . . . ? C4 C5 C10 C9 179.58(19) . . . . ? C8 C9 C10 C5 4.0(3) . . . . ? C15 C9 C10 C5 -176.73(19) . . . . ? C6 C7 C11 O6 -159.8(2) . . . . ? C8 C7 C11 O6 19.3(3) . . . . ? C6 C7 C11 N2 21.2(3) . . . . ? C8 C7 C11 N2 -159.8(2) . . . . ? N2 C13 C14 O4 -6.4(3) . . . . ? C12 C13 C14 O4 115.5(3) . . . . ? N2 C13 C14 O5 174.9(2) . . . . ? C12 C13 C14 O5 -63.2(3) . . . . ? C8 C9 C15 O9 27.4(3) . . . . ? C10 C9 C15 O9 -151.8(2) . . . . ? C8 C9 C15 N3 -152.2(2) . . . . ? C10 C9 C15 N3 28.5(3) . . . . ? N3 C17 C18 O7 -37.6(2) . . . . ? C16 C17 C18 O7 84.2(2) . . . . ? N3 C17 C18 O8 144.47(16) . . . . ? C16 C17 C18 O8 -93.8(2) . . . . ? C23 C19 C20 N4 -1.4(3) . . . . ? N4 C21 C22 C23 -0.7(4) . . . . ? C20 C19 C23 C22 2.4(3) . . . . ? C20 C19 C23 C24 -176.74(19) . . . . ? C21 C22 C23 C19 -1.4(3) . . . . ? C21 C22 C23 C24 177.8(2) . . . . ? C19 C23 C24 C28 38.5(3) . . . . ? C22 C23 C24 C28 -140.6(2) . . . . ? C19 C23 C24 C25 -143.2(2) . . . . ? C22 C23 C24 C25 37.7(3) . . . . ? C28 C24 C25 C26 -1.3(3) . . . . ? C23 C24 C25 C26 -179.5(2) . . . . ? C24 C25 C26 N5 1.8(3) . . . . ? N5 C27 C28 C24 1.2(3) . . . . ? C25 C24 C28 C27 -0.1(3) . . . . ? C23 C24 C28 C27 178.16(19) . . . . ? N6 C29 C30 C31 1.0(4) . . . . ? C29 C30 C31 C32 -2.1(3) . . . . ? C29 C30 C31 C31 175.79(17) . . . 2_765 ? C30 C31 C32 C33 1.7(3) . . . . ? C31 C31 C32 C33 -176.18(17) 2_765 . . . ? C31 C32 C33 N6 -0.2(4) . . . . ? N7 C34 C35 C36 1.0(3) . . . . ? C34 C35 C36 C35 -0.48(13) . . . 2_665 ? C34 C35 C36 C37 179.52(13) . . . . ? C35 C36 C37 C38 41.44(14) . . . . ? C35 C36 C37 C38 -138.56(14) 2_665 . . . ? C35 C36 C37 C38 -138.56(14) . . . 2_665 ? C35 C36 C37 C38 41.44(14) 2_665 . . 2_665 ? C38 C37 C38 C39 -0.34(14) 2_665 . . . ? C36 C37 C38 C39 179.66(14) . . . . ? C37 C38 C39 N8 0.7(3) . . . . ? O3 C4 N1 C2 -7.2(3) . . . . ? C5 C4 N1 C2 169.87(17) . . . . ? C3 C2 N1 C4 165.31(18) . . . . ? C1 C2 N1 C4 -73.2(2) . . . . ? O6 C11 N2 C13 1.9(4) . . . . ? C7 C11 N2 C13 -179.1(2) . . . . ? C14 C13 N2 C11 -109.9(3) . . . . ? C12 C13 N2 C11 127.2(3) . . . . ? O9 C15 N3 C17 4.0(3) . . . . ? C9 C15 N3 C17 -176.37(17) . . . . ? C16 C17 N3 C15 167.11(18) . . . . ? C18 C17 N3 C15 -71.6(2) . . . . ? C19 C20 N4 C21 -0.6(3) . . . . ? C19 C20 N4 Ni2 178.55(16) . . . . ? C22 C21 N4 C20 1.7(3) . . . . ? C22 C21 N4 Ni2 -177.40(18) . . . . ? O7 Ni2 N4 C20 -33.09(16) 3_656 . . . ? N6 Ni2 N4 C20 59.03(16) . . . . ? N5 Ni2 N4 C20 117.1(12) 1_554 . . . ? O2 Ni2 N4 C20 162.40(16) . . . . ? O1 Ni2 N4 C20 -136.57(16) . . . . ? C1 Ni2 N4 C20 -167.25(16) . . . . ? O7 Ni2 N4 C21 145.98(17) 3_656 . . . ? N6 Ni2 N4 C21 -121.91(17) . . . . ? N5 Ni2 N4 C21 -63.8(13) 1_554 . . . ? O2 Ni2 N4 C21 -18.53(17) . . . . ? O1 Ni2 N4 C21 42.50(17) . . . . ? C1 Ni2 N4 C21 11.82(17) . . . . ? C25 C26 N5 C27 -0.8(3) . . . . ? C25 C26 N5 Ni2 -177.63(17) . . . 1_556 ? C28 C27 N5 C26 -0.7(3) . . . . ? C28 C27 N5 Ni2 176.07(16) . . . 1_556 ? C30 C29 N6 C33 0.5(3) . . . . ? C30 C29 N6 Ni2 179.02(18) . . . . ? C32 C33 N6 C29 -0.9(3) . . . . ? C32 C33 N6 Ni2 -179.42(18) . . . . ? O7 Ni2 N6 C29 161.88(16) 3_656 . . . ? N4 Ni2 N6 C29 72.26(16) . . . . ? N5 Ni2 N6 C29 -105.14(16) 1_554 . . . ? O2 Ni2 N6 C29 -17.89(17) . . . . ? O1 Ni2 N6 C29 -22.9(3) . . . . ? C1 Ni2 N6 C29 -19.28(19) . . . . ? O7 Ni2 N6 C33 -19.65(16) 3_656 . . . ? N4 Ni2 N6 C33 -109.28(16) . . . . ? N5 Ni2 N6 C33 73.32(16) 1_554 . . . ? O2 Ni2 N6 C33 160.57(15) . . . . ? O1 Ni2 N6 C33 155.59(19) . . . . ? C1 Ni2 N6 C33 159.18(14) . . . . ? C35 C34 N7 C34 -0.53(14) . . . 2_665 ? C35 C34 N7 Ni1 179.47(15) . . . . ? O8 Ni1 N7 C34 -43.54(11) 4_456 . . . ? O8 Ni1 N7 C34 136.46(11) 3_656 . . . ? N8 Ni1 N7 C34 -174(100) 1_556 . . . ? O1 Ni1 N7 C34 43.85(11) . . . . ? O1 Ni1 N7 C34 -136.15(11) 2_665 . . . ? O8 Ni1 N7 C34 136.46(11) 4_456 . . 2_665 ? O8 Ni1 N7 C34 -43.54(11) 3_656 . . 2_665 ? N8 Ni1 N7 C34 6(63) 1_556 . . 2_665 ? O1 Ni1 N7 C34 -136.15(11) . . . 2_665 ? O1 Ni1 N7 C34 43.85(11) 2_665 . . 2_665 ? C38 C39 N8 C39 -0.36(15) . . . 2_665 ? C38 C39 N8 Ni1 179.64(15) . . . 1_554 ? O2 C1 O1 Ni1 173.55(15) . . . . ? C2 C1 O1 Ni1 -9.9(3) . . . . ? Ni2 C1 O1 Ni1 172.8(2) . . . . ? O2 C1 O1 Ni2 0.75(16) . . . . ? C2 C1 O1 Ni2 177.35(15) . . . . ? O8 Ni1 O1 C1 4.6(2) 4_456 . . . ? O8 Ni1 O1 C1 -170.9(2) 3_656 . . . ? N7 Ni1 O1 C1 -83.1(2) . . . . ? N8 Ni1 O1 C1 96.9(2) 1_556 . . . ? O1 Ni1 O1 C1 96.9(2) 2_665 . . . ? O8 Ni1 O1 Ni2 176.23(7) 4_456 . . . ? O8 Ni1 O1 Ni2 0.70(7) 3_656 . . . ? N7 Ni1 O1 Ni2 88.52(6) . . . . ? N8 Ni1 O1 Ni2 -91.48(6) 1_556 . . . ? O1 Ni1 O1 Ni2 -91.48(6) 2_665 . . . ? O7 Ni2 O1 C1 -179.79(10) 3_656 . . . ? N6 Ni2 O1 C1 5.1(3) . . . . ? N4 Ni2 O1 C1 -89.99(11) . . . . ? N5 Ni2 O1 C1 87.07(11) 1_554 . . . ? O2 Ni2 O1 C1 -0.45(10) . . . . ? O7 Ni2 O1 Ni1 4.46(8) 3_656 . . . ? N6 Ni2 O1 Ni1 -170.65(17) . . . . ? N4 Ni2 O1 Ni1 94.26(8) . . . . ? N5 Ni2 O1 Ni1 -88.68(7) 1_554 . . . ? O2 Ni2 O1 Ni1 -176.19(9) . . . . ? C1 Ni2 O1 Ni1 -175.75(14) . . . . ? O1 C1 O2 Ni2 -0.76(17) . . . . ? C2 C1 O2 Ni2 -177.43(14) . . . . ? O7 Ni2 O2 C1 2.8(2) 3_656 . . . ? N6 Ni2 O2 C1 -178.01(10) . . . . ? N4 Ni2 O2 C1 91.43(11) . . . . ? N5 Ni2 O2 C1 -90.75(11) 1_554 . . . ? O1 Ni2 O2 C1 0.45(10) . . . . ? O8 C18 O7 Ni2 4.5(3) . . . 3_646 ? C17 C18 O7 Ni2 -173.17(12) . . . 3_646 ? O7 C18 O8 Ni1 8.3(4) . . . 3_646 ? C17 C18 O8 Ni1 -174.00(15) . . . 3_646 ? 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 N1 H1 O5 0.87 2.32 3.192(2) 178.6 1_556 N2 H2A O11 0.87 2.49 3.354(3) 174.7 . N3 H3 O5 0.87 2.22 3.086(2) 171.4 1_556 O10 H101 O4 0.85 1.85 2.705(3) 179.8 1_556 O10 H102 O2 0.85 2.03 2.862(2) 165.9 . O11 H111 O3 0.85 2.12 2.966(2) 179.7 . O11 H112 O13 0.85 1.91 2.762(4) 179.4 . O12 H12 O5 0.83 1.98 2.786(3) 162.1 4 O13 H131 O15 0.85 1.68 2.530(11) 179.6 . O13 H132 O9 0.85 2.05 2.805(3) 148.4 4_455 O14 H141 O12 0.86 2.33 2.881(4) 122.8 . O14 H142 O10 0.85 2.24 2.800(4) 123.0 . O14 H142 N3 0.85 2.70 3.409(4) 141.5 . _chemical_absolute_configuration rmad _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.321 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.073 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 -0.005 401 34 ' ' 2 0.500 0.000 0.004 402 34 ' ' 3 0.459 0.271 0.165 11 1 ' ' 4 0.541 0.729 0.165 10 1 ' ' 5 0.041 0.771 0.835 10 1 ' ' 6 0.959 0.229 0.835 10 1 ' ' _platon_squeeze_details ; ;