# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wei-Yin Sun' _publ_contact_author_email sunwy@nju.edu.cn _publ_author_name 'Wei-Yin Sun' data_1 _database_code_depnum_ccdc_archive 'CCDC 897815' #TrackingRef 'CE-ART-08-2012-026338.cif' _audit_creation_date 2012-09-17 _audit_creation_method SHELXL-97 _publ_section_comment ; The crystal was not a single crystal and reflections were found close to or overlapped with the undesired spots. Trials to select a single crystal and separation of spots in the data processing were unsuccessful. The partially overlapped spots resulted in incorrect intensities of the reflections and large R factors. The intense residual peaks were found in the same plane to the planar ligands and close to the ligands, like linear and parallel arrays along c-axis, showing pseudo-symmetry, which were probably caused by another crystal. ; _publ_section_references ; Rigaku Americas and Rigaku Corporation. (2007). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku Americas, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. SHELX97 ; _chemical_name_systematic ; [Mn4(H2O)6(L2)(B1)2]-DMF-5(H2O) ; _chemical_name_common (Mn4(H2O)6(L2)(B1)2)-DMF-5(H2O) _chemical_melting_point ? _chemical_formula_moiety 'C52 H61 Mn4 N11 O28' _chemical_formula_sum 'C52 H61 Mn4 N11 O28' _chemical_formula_weight 1507.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.9016(15) _cell_length_b 22.154(3) _cell_length_c 13.0426(19) _cell_angle_alpha 90.00 _cell_angle_beta 103.073(6) _cell_angle_gamma 90.00 _cell_volume 3068.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 200 _cell_measurement_reflns_used 23851 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1548 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8995 _exptl_absorpt_correction_T_max 0.9563 _exptl_absorpt_process_details ? _exptl_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 23108 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_sigmaI/netI 0.1530 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10728 _reflns_number_gt 8918 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.1896P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.11(3) _refine_ls_number_reflns 10728 _refine_ls_number_parameters 649 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1053 _refine_ls_R_factor_gt 0.0916 _refine_ls_wR_factor_ref 0.2605 _refine_ls_wR_factor_gt 0.2463 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.85920(11) 0.65077(5) 1.14997(9) 0.0247(3) Uani 1 1 d . . . Mn2 Mn 0.85819(12) 0.80011(5) 0.29613(9) 0.0251(3) Uani 1 1 d . . . Mn3 Mn 0.15000(13) 0.49276(5) 0.57820(10) 0.0285(3) Uani 1 1 d . . . Mn4 Mn 0.15385(12) 0.95778(5) 0.98618(9) 0.0260(3) Uani 1 1 d . . . O1 O 0.8697(6) 0.5635(2) 1.0386(5) 0.0341(14) Uani 1 1 d . . . O2 O 0.8364(6) 0.5301(2) 0.8731(5) 0.0324(14) Uani 1 1 d . . . O3 O 0.8595(5) 0.7547(2) 1.1350(4) 0.0259(13) Uani 1 1 d . . . O4 O 0.8747(8) 0.8335(3) 1.0300(5) 0.0452(18) Uani 1 1 d . . . O5 O 0.8605(5) 0.6942(3) 0.3118(4) 0.0268(13) Uani 1 1 d . . . O6 O 0.8654(6) 0.6171(3) 0.4229(5) 0.0360(15) Uani 1 1 d . . . O7 O 0.8736(6) 0.8890(2) 0.4128(5) 0.0284(13) Uani 1 1 d . . . O8 O 0.8381(6) 0.9205(3) 0.5652(5) 0.0390(16) Uani 1 1 d . . . O9 O 0.1190(7) 0.4847(3) 0.7441(6) 0.0511(18) Uani 1 1 d U . . O10 O 0.1412(6) 0.5286(3) 0.9020(5) 0.0338(14) Uani 1 1 d . . . H40 H 0.137(9) 0.494(5) 0.954(8) 0.041 Uiso 1 1 d . . . O11 O 0.1684(6) 0.5699(2) 0.4604(5) 0.030 Uani 1 1 d . . . O12 O 0.1636(6) 0.6687(3) 0.4292(4) 0.031 Uani 1 1 d . . . O13 O 0.1820(6) 0.8833(3) 1.1096(5) 0.032 Uani 1 1 d . . . O14 O 0.1686(6) 0.7832(3) 1.1349(5) 0.034 Uani 1 1 d . . . O15 O 0.1092(6) 0.9675(2) 0.7994(5) 0.030 Uani 1 1 d . . . O16 O 0.1383(6) 0.9232(3) 0.6527(4) 0.033 Uani 1 1 d . . . H41 H 0.168(9) 0.956(5) 0.614(8) 0.039 Uiso 1 1 d . . . O17 O 1.0594(6) 0.6431(3) 1.2118(5) 0.037 Uani 1 1 d . . . O18 O 0.7958(6) 0.5751(2) 1.2304(4) 0.029 Uani 1 1 d . . . H46 H 0.825(9) 0.535(4) 1.237(8) 0.035 Uiso 1 1 d . . . O19 O 0.6485(6) 0.6566(4) 1.0891(6) 0.056 Uani 1 1 d . . . O20 O 0.8032(8) 0.8781(3) 0.1923(6) 0.056 Uani 1 1 d . . . O21 O -0.0499(6) 0.5011(3) 0.5042(5) 0.039 Uani 1 1 d . . . O22 O -0.0467(5) 0.9469(2) 0.9815(5) 0.031 Uani 1 1 d . . . O23 O 0.1330(7) 0.5290(3) 0.2561(6) 0.045 Uani 1 1 d D . . H42 H 0.147(10) 0.498(5) 0.189(9) 0.054 Uiso 1 1 d . . . H43 H 0.128(9) 0.493(4) 0.325(6) 0.054 Uiso 1 1 d D . . O24 O 0.2029(8) 0.4014(3) 0.2162(7) 0.059 Uani 1 1 d . . . O25 O 0.8365(10) 0.4196(5) 0.6872(8) 0.084 Uani 1 1 d D . . H44 H 0.842(13) 0.462(4) 0.630(9) 0.100 Uiso 1 1 d D . . H45 H 0.841(13) 0.456(5) 0.756(8) 0.100 Uiso 1 1 d D . . O26 O 1.0634(7) 0.8003(6) 0.3094(6) 0.087 Uani 1 1 d U . . O27 O 0.5271(14) 0.6651(9) 0.8913(13) 0.162 Uani 1 1 d DU . . O28 O 0.2299(13) 0.8255(8) 0.5187(10) 0.137 Uani 1 1 d . . . N11 N 0.8646(6) 0.6764(3) 0.9847(5) 0.024 Uani 1 1 d . . . N21 N 0.8718(6) 0.7734(3) 0.4659(5) 0.021 Uani 1 1 d U . . N31 N 0.1601(6) 0.5849(3) 0.6542(5) 0.023 Uani 1 1 d . . . N41 N 0.1578(7) 0.8677(3) 0.9051(6) 0.027 Uani 1 1 d . . . N111 N 0.4713(7) 0.7497(4) 0.2945(7) 0.040 Uani 1 1 d . . . N112 N 0.6519(7) 0.7914(3) 0.2817(6) 0.038 Uani 1 1 d . . . N131 N 0.5344(7) 0.5116(3) 0.5626(6) 0.036 Uani 1 1 d . . . N132 N 0.3588(7) 0.4910(3) 0.6131(6) 0.037 Uani 1 1 d . . . N151 N 0.4659(7) 0.4832(3) 0.0548(6) 0.034 Uani 1 1 d . . . N152 N 0.6421(7) 0.4662(3) 0.0048(6) 0.035 Uani 1 1 d . . . N201 N 0.5119(14) 0.7543(7) 0.8026(13) 0.106 Uani 1 1 d D . . C1 C 0.8564(7) 0.5718(3) 0.9416(6) 0.024 Uani 1 1 d . . . C2 C 0.8673(7) 0.7810(4) 1.0504(6) 0.025 Uani 1 1 d . . . C3 C 0.8670(7) 0.6692(3) 0.3994(6) 0.019 Uani 1 1 d . . . C4 C 0.8588(8) 0.8801(3) 0.5048(7) 0.028 Uani 1 1 d . . . C5 C 0.1354(9) 0.5295(4) 0.8061(6) 0.032 Uani 1 1 d . . . C6 C 0.1688(8) 0.6249(3) 0.4859(6) 0.024 Uani 1 1 d . . . C7 C 0.1752(8) 0.8276(3) 1.0792(6) 0.024 Uani 1 1 d . . . C8 C 0.1307(8) 0.9236(4) 0.7466(7) 0.031 Uani 1 1 d . . . C12 C 0.8589(6) 0.6393(3) 0.9041(5) 0.014 Uani 1 1 d U . . C13 C 0.8541(6) 0.6529(4) 0.7962(6) 0.023 Uani 1 1 d . . . H1 H 0.8493 0.6229 0.7434 0.027 Uiso 1 1 calc R . . C14 C 0.8572(7) 0.7147(4) 0.7761(7) 0.0279(19) Uani 1 1 d . . . C15 C 0.8622(7) 0.7566(4) 0.8572(6) 0.0237(16) Uani 1 1 d . . . H2 H 0.8625 0.7987 0.8435 0.028 Uiso 1 1 calc R . . C16 C 0.8669(7) 0.7350(4) 0.9603(6) 0.0246(17) Uani 1 1 d . . . C22 C 0.8709(7) 0.7147(3) 0.4904(6) 0.0225(16) Uani 1 1 d . . . C23 C 0.8650(7) 0.6943(3) 0.5898(6) 0.0225(16) Uani 1 1 d . . . H3 H 0.8660 0.6523 0.6041 0.027 Uiso 1 1 calc R . . C24 C 0.8574(7) 0.7360(4) 0.6689(6) 0.0219(16) Uani 1 1 d . . . C25 C 0.8555(6) 0.7967(3) 0.6484(6) 0.0200(16) Uani 1 1 d . . . H4 H 0.8512 0.8264 0.7000 0.024 Uiso 1 1 calc R . . C26 C 0.8605(6) 0.8117(3) 0.5417(5) 0.0156(14) Uani 1 1 d . . . C32 C 0.1552(8) 0.5879(3) 0.7595(6) 0.0244(17) Uani 1 1 d . . . C33 C 0.1659(7) 0.6435(4) 0.8123(6) 0.0221(16) Uani 1 1 d . . . H5 H 0.1661 0.6449 0.8851 0.027 Uiso 1 1 calc R . . C34 C 0.1760(7) 0.6955(3) 0.7591(6) 0.0195(15) Uani 1 1 d . . . C35 C 0.1809(7) 0.6920(3) 0.6498(6) 0.0200(15) Uani 1 1 d . . . H6 H 0.1904 0.7275 0.6114 0.024 Uiso 1 1 calc R . . C36 C 0.1715(7) 0.6354(3) 0.6011(7) 0.0239(16) Uani 1 1 d . . . C42 C 0.1732(8) 0.8174(3) 0.9615(6) 0.0224(16) Uani 1 1 d . . . C43 C 0.1846(7) 0.7612(3) 0.9200(7) 0.0253(17) Uani 1 1 d . . . H7 H 0.1971 0.7264 0.9638 0.030 Uiso 1 1 calc R . . C44 C 0.1775(8) 0.7564(4) 0.8124(6) 0.0254(17) Uani 1 1 d . . . C45 C 0.1632(8) 0.8098(3) 0.7537(6) 0.0252(17) Uani 1 1 d . . . H8 H 0.1622 0.8089 0.6807 0.030 Uiso 1 1 calc R . . C46 C 0.1505(8) 0.8642(4) 0.8031(7) 0.0277(19) Uani 1 1 d . . . C101 C 0.4268(8) 0.6387(4) 0.2968(8) 0.037(2) Uani 1 1 d . . . C102 C 0.4982(9) 0.6151(5) 0.3897(8) 0.037(2) Uani 1 1 d . . . C103 C 0.5372(8) 0.5525(5) 0.3891(8) 0.039(2) Uani 1 1 d . . . C104 C 0.5018(9) 0.5167(5) 0.3001(8) 0.040(2) Uani 1 1 d . . . C105 C 0.4284(8) 0.5434(5) 0.2068(8) 0.042(2) Uani 1 1 d . . . C106 C 0.3997(8) 0.6057(4) 0.2049(7) 0.034(2) Uani 1 1 d . . . C111 C 0.3769(9) 0.7019(4) 0.2960(9) 0.044(2) Uani 1 1 d . . . H9 H 0.3068 0.7069 0.2334 0.053 Uiso 1 1 calc R . . H10 H 0.3420 0.7076 0.3592 0.053 Uiso 1 1 calc R . . C112 C 0.5883(9) 0.7402(4) 0.2774(9) 0.045(2) Uani 1 1 d . . . H11 H 0.6203 0.7018 0.2641 0.054 Uiso 1 1 calc R . . C113 C 0.5689(11) 0.8363(5) 0.3015(11) 0.059(3) Uani 1 1 d . . . H12 H 0.5850 0.8785 0.3053 0.070 Uiso 1 1 calc R . . C114 C 0.4608(11) 0.8088(6) 0.3145(13) 0.068(4) Uani 1 1 d . . . H13 H 0.3914 0.8279 0.3340 0.082 Uiso 1 1 calc R . . C121 C 0.5276(9) 0.6502(6) 0.4896(9) 0.051(3) Uani 1 1 d . . . H14 H 0.5326 0.6933 0.4735 0.061 Uiso 1 1 calc R . . H15 H 0.6084 0.6368 0.5330 0.061 Uiso 1 1 calc R . . H16 H 0.4610 0.6438 0.5279 0.061 Uiso 1 1 calc R . . C131 C 0.6157(9) 0.5246(5) 0.4905(8) 0.044(2) Uani 1 1 d . . . H17 H 0.6559 0.4869 0.4738 0.053 Uiso 1 1 calc R . . H18 H 0.6830 0.5530 0.5241 0.053 Uiso 1 1 calc R . . C132 C 0.4112(9) 0.4965(4) 0.5321(8) 0.041(2) Uani 1 1 d . . . H19 H 0.3679 0.4906 0.4610 0.049 Uiso 1 1 calc R . . C133 C 0.4539(11) 0.5020(5) 0.7004(8) 0.048(3) Uani 1 1 d . . . H20 H 0.4445 0.5003 0.7710 0.058 Uiso 1 1 calc R . . C134 C 0.5579(10) 0.5148(5) 0.6733(9) 0.049(3) Uani 1 1 d . . . H21 H 0.6359 0.5247 0.7195 0.058 Uiso 1 1 calc R . . C141 C 0.5310(11) 0.4498(5) 0.3021(11) 0.062(3) Uani 1 1 d . . . H22 H 0.4935 0.4320 0.2333 0.074 Uiso 1 1 calc R . . H23 H 0.4960 0.4301 0.3564 0.074 Uiso 1 1 calc R . . H24 H 0.6225 0.4439 0.3179 0.074 Uiso 1 1 calc R . . C151 C 0.3738(8) 0.5047(5) 0.1138(8) 0.043(2) Uani 1 1 d . . . H25 H 0.3332 0.4692 0.1384 0.052 Uiso 1 1 calc R . . H26 H 0.3073 0.5278 0.0654 0.052 Uiso 1 1 calc R . . C152 C 0.5831(10) 0.4969(5) 0.0683(9) 0.053(3) Uani 1 1 d . . . H27 H 0.6240 0.5258 0.1182 0.064 Uiso 1 1 calc R . . C153 C 0.5512(9) 0.4294(5) -0.0554(9) 0.047(3) Uani 1 1 d . . . H28 H 0.5617 0.4021 -0.1090 0.056 Uiso 1 1 calc R . . C154 C 0.4417(11) 0.4406(5) -0.0218(8) 0.053(3) Uani 1 1 d . . . H29 H 0.3627 0.4216 -0.0480 0.063 Uiso 1 1 calc R . . C161 C 0.3302(10) 0.6351(6) 0.1014(9) 0.054(3) Uani 1 1 d . . . H30 H 0.2400 0.6261 0.0893 0.065 Uiso 1 1 calc R . . H31 H 0.3633 0.6191 0.0430 0.065 Uiso 1 1 calc R . . H32 H 0.3428 0.6789 0.1059 0.065 Uiso 1 1 calc R . . C201 C 0.5159(17) 0.6922(10) 0.8106(14) 0.113(7) Uani 1 1 d D . . H33 H 0.5093 0.6696 0.7477 0.136 Uiso 1 1 calc R . . C202 C 0.5301(17) 0.7942(10) 0.8911(13) 0.105(6) Uani 1 1 d DU . . H34 H 0.5351 0.7706 0.9556 0.126 Uiso 1 1 calc R . . H35 H 0.4593 0.8224 0.8820 0.126 Uiso 1 1 calc R . . H36 H 0.6086 0.8168 0.8965 0.126 Uiso 1 1 calc R . . C203 C 0.500(2) 0.7834(15) 0.698(3) 0.215(17) Uani 1 1 d DU . . H37 H 0.4685 0.7539 0.6424 0.258 Uiso 1 1 calc R . . H38 H 0.5827 0.7982 0.6916 0.258 Uiso 1 1 calc R . . H39 H 0.4412 0.8174 0.6914 0.258 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0379(6) 0.0216(6) 0.0163(6) -0.0007(5) 0.0097(5) -0.0034(5) Mn2 0.0427(7) 0.0195(6) 0.0151(6) 0.0014(5) 0.0110(5) -0.0011(5) Mn3 0.0527(7) 0.0150(6) 0.0184(6) -0.0023(5) 0.0090(5) -0.0035(5) Mn4 0.0451(7) 0.0145(6) 0.0192(6) -0.0008(5) 0.0089(5) 0.0030(5) O1 0.064(4) 0.013(3) 0.029(3) 0.005(2) 0.018(3) -0.003(3) O2 0.058(4) 0.018(3) 0.023(3) -0.002(2) 0.014(3) 0.000(3) O3 0.055(3) 0.009(2) 0.014(3) -0.003(2) 0.006(2) 0.004(2) O4 0.094(5) 0.017(3) 0.023(3) 0.000(3) 0.012(3) 0.002(3) O5 0.044(3) 0.025(3) 0.013(3) -0.001(2) 0.009(2) 0.003(2) O6 0.067(4) 0.024(3) 0.018(3) -0.007(2) 0.013(3) 0.002(3) O7 0.052(3) 0.015(3) 0.020(3) 0.003(2) 0.013(3) 0.001(2) O8 0.065(4) 0.026(3) 0.025(3) 0.000(3) 0.007(3) 0.012(3) O9 0.068(3) 0.038(3) 0.046(3) -0.006(2) 0.011(2) -0.003(2) O10 0.055(4) 0.020(3) 0.028(3) 0.001(3) 0.014(3) -0.007(3) O11 0.051 0.018 0.022 -0.008 0.009 -0.001 O12 0.046 0.029 0.017 -0.005 0.004 0.002 O13 0.056 0.022 0.019 0.001 0.011 0.006 O14 0.056 0.025 0.026 0.004 0.018 0.007 O15 0.056 0.009 0.028 -0.004 0.016 0.007 O16 0.064 0.021 0.015 -0.004 0.013 0.010 O17 0.039 0.042 0.033 -0.003 0.013 0.000 O18 0.054 0.011 0.026 -0.004 0.018 -0.002 O19 0.046 0.067 0.054 -0.022 0.008 -0.008 O20 0.083 0.045 0.039 0.006 0.011 0.003 O21 0.054 0.031 0.029 -0.002 0.004 0.001 O22 0.044 0.022 0.034 -0.004 0.021 0.002 O23 0.067 0.029 0.038 -0.004 0.009 -0.004 O24 0.080 0.039 0.058 0.018 0.014 -0.010 O25 0.108 0.091 0.066 0.011 0.050 0.021 O26 0.056 0.173 0.037 -0.042 0.023 -0.036 O27 0.112 0.225 0.131 0.058 -0.012 0.026 O28 0.118 0.211 0.066 -0.015 -0.010 0.048 N11 0.026 0.025 0.022 -0.016 0.007 -0.001 N21 0.023 0.022 0.020 -0.013 0.009 0.002 N31 0.043 0.013 0.012 -0.004 0.009 -0.004 N41 0.040 0.018 0.024 0.001 0.008 0.004 N111 0.038 0.038 0.048 -0.001 0.019 0.001 N112 0.045 0.030 0.038 0.003 0.006 0.000 N131 0.036 0.036 0.032 0.007 0.001 0.007 N132 0.053 0.028 0.028 0.006 0.005 0.006 N151 0.044 0.032 0.026 0.004 0.008 -0.008 N152 0.050 0.030 0.027 0.003 0.011 -0.006 N201 0.097 0.086 0.126 0.017 0.009 0.006 C1 0.037 0.014 0.020 0.003 0.007 -0.011 C2 0.026 0.036 0.014 0.003 0.006 -0.001 C3 0.026 0.026 0.008 0.000 0.007 0.005 C4 0.049 0.012 0.026 0.002 0.012 0.004 C5 0.060 0.023 0.014 -0.002 0.009 -0.019 C6 0.035 0.012 0.025 -0.001 0.003 -0.002 C7 0.039 0.017 0.016 0.004 0.006 0.006 C8 0.037 0.030 0.021 0.001 -0.007 0.003 C12 0.018 0.020 0.003 0.000 0.002 0.001 C13 0.016 0.018 0.031 0.003 -0.001 -0.003 C14 0.027(4) 0.023(4) 0.030(5) -0.007(4) -0.003(3) 0.000(3) C15 0.032(4) 0.019(4) 0.020(4) 0.004(3) 0.007(3) 0.007(3) C16 0.034(4) 0.024(4) 0.017(4) -0.001(3) 0.008(3) -0.004(3) C22 0.036(4) 0.014(4) 0.017(4) 0.003(3) 0.004(3) 0.002(3) C23 0.031(4) 0.016(4) 0.020(4) -0.003(3) 0.007(3) 0.000(3) C24 0.026(4) 0.021(4) 0.021(4) 0.002(3) 0.009(3) 0.002(3) C25 0.020(3) 0.007(3) 0.035(4) -0.007(3) 0.010(3) -0.004(3) C26 0.023(3) 0.020(4) 0.005(3) -0.003(3) 0.004(3) -0.001(3) C32 0.041(4) 0.013(4) 0.018(4) 0.003(3) 0.004(3) -0.008(3) C33 0.033(4) 0.021(4) 0.015(3) -0.010(3) 0.010(3) -0.010(3) C34 0.032(4) 0.015(3) 0.013(3) -0.004(3) 0.008(3) 0.002(3) C35 0.031(4) 0.008(3) 0.023(4) -0.003(3) 0.012(3) 0.000(3) C36 0.030(4) 0.021(4) 0.025(4) -0.011(3) 0.014(3) -0.005(3) C42 0.032(4) 0.019(4) 0.018(4) 0.001(3) 0.010(3) 0.005(3) C43 0.035(4) 0.017(4) 0.024(4) 0.004(3) 0.008(3) 0.001(3) C44 0.037(4) 0.017(4) 0.018(4) -0.005(3) -0.001(3) 0.004(3) C45 0.046(5) 0.015(4) 0.012(3) 0.000(3) 0.002(3) 0.007(3) C46 0.031(4) 0.020(4) 0.028(4) -0.008(3) -0.003(3) 0.008(3) C101 0.034(4) 0.042(5) 0.038(5) 0.012(4) 0.017(4) 0.001(4) C102 0.039(5) 0.042(5) 0.033(5) -0.003(4) 0.013(4) -0.009(4) C103 0.031(4) 0.048(5) 0.037(5) -0.004(4) 0.005(4) -0.001(4) C104 0.040(5) 0.053(6) 0.032(5) -0.002(4) 0.018(4) 0.013(4) C105 0.030(4) 0.051(6) 0.048(6) -0.006(5) 0.016(4) -0.007(4) C106 0.028(4) 0.035(5) 0.041(5) 0.007(4) 0.012(4) -0.002(4) C111 0.039(5) 0.038(5) 0.059(6) 0.012(5) 0.019(5) 0.004(4) C112 0.049(5) 0.029(5) 0.061(7) 0.006(5) 0.024(5) 0.010(4) C113 0.059(6) 0.036(6) 0.084(9) 0.004(6) 0.022(6) 0.012(5) C114 0.043(6) 0.050(7) 0.112(11) -0.018(7) 0.019(6) 0.012(5) C121 0.044(5) 0.052(6) 0.056(7) -0.006(6) 0.008(5) -0.006(5) C131 0.044(5) 0.056(6) 0.036(5) 0.009(5) 0.014(4) 0.010(5) C132 0.056(5) 0.019(4) 0.046(6) -0.001(4) 0.006(4) -0.010(4) C133 0.067(7) 0.042(6) 0.031(5) 0.004(5) -0.001(5) 0.007(5) C134 0.049(6) 0.047(6) 0.041(6) -0.003(5) -0.010(5) -0.005(5) C141 0.060(7) 0.051(7) 0.074(8) 0.016(7) 0.016(6) 0.006(5) C151 0.031(4) 0.061(6) 0.041(5) -0.001(5) 0.015(4) -0.018(4) C152 0.058(6) 0.056(6) 0.041(6) -0.010(5) 0.001(5) -0.024(5) C153 0.045(5) 0.047(6) 0.041(6) -0.004(5) -0.005(5) -0.005(5) C154 0.063(7) 0.055(7) 0.036(5) -0.014(5) 0.002(5) -0.013(5) C161 0.045(5) 0.070(7) 0.049(6) 0.013(6) 0.012(5) 0.003(5) C201 0.090(11) 0.144(19) 0.105(15) -0.012(14) 0.018(11) -0.010(12) C202 0.093(11) 0.142(17) 0.076(11) -0.002(12) 0.008(9) 0.021(12) C203 0.112(17) 0.23(3) 0.31(4) 0.16(3) 0.07(2) 0.050(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O17 2.156(6) . ? Mn1 O18 2.171(6) . ? Mn1 N11 2.243(7) . ? Mn1 O19 2.258(7) . ? Mn1 O3 2.311(5) . ? Mn1 O5 2.317(6) 1_556 ? Mn1 O1 2.436(6) . ? Mn2 O20 2.193(8) . ? Mn2 O26 2.204(8) . ? Mn2 N112 2.222(8) . ? Mn2 N21 2.265(7) . ? Mn2 O3 2.333(5) 1_554 ? Mn2 O5 2.354(6) . ? Mn2 O7 2.470(6) . ? Mn3 O21 2.182(6) . ? Mn3 N132 2.218(8) . ? Mn3 N31 2.262(6) . ? Mn3 O9 2.271(8) . ? Mn3 O7 2.320(5) 2_646 ? Mn3 O11 2.337(6) . ? Mn3 O8 2.487(6) 2_646 ? Mn4 O22 2.187(6) . ? Mn4 N152 2.209(8) 2_656 ? Mn4 N41 2.264(7) . ? Mn4 O13 2.277(6) . ? Mn4 O1 2.371(6) 2_657 ? Mn4 O15 2.383(6) . ? Mn4 O2 2.421(6) 2_657 ? O1 C1 1.253(10) . ? O1 Mn4 2.371(6) 2_647 ? O2 C1 1.270(10) . ? O2 Mn4 2.421(6) 2_647 ? O3 C2 1.267(10) . ? O3 Mn2 2.333(5) 1_556 ? O4 C2 1.201(11) . ? O5 C3 1.257(9) . ? O5 Mn1 2.317(6) 1_554 ? O6 C3 1.194(10) . ? O7 C4 1.263(11) . ? O7 Mn3 2.320(5) 2_656 ? O8 C4 1.247(10) . ? O8 Mn3 2.487(6) 2_656 ? O9 C5 1.268(11) . ? O10 C5 1.238(11) . ? O10 H40 1.04(11) . ? O11 C6 1.262(10) . ? O12 C6 1.215(10) . ? O13 C7 1.294(10) . ? O14 C7 1.234(10) . ? O15 C8 1.244(11) . ? O16 C8 1.246(11) . ? O16 H41 0.98(11) . ? O18 H46 0.93(9) . ? O23 H42 1.15(12) . ? O23 H43 1.21(2) . ? O25 H44 1.20(2) . ? O25 H45 1.21(2) . ? O27 C201 1.194(10) . ? N11 C12 1.325(9) . ? N11 C16 1.337(11) . ? N21 C26 1.330(9) . ? N21 C22 1.340(10) . ? N31 C36 1.335(10) . ? N31 C32 1.388(11) . ? N41 C46 1.317(12) . ? N41 C42 1.326(10) . ? N111 C114 1.345(14) . ? N111 C112 1.360(12) . ? N111 C111 1.480(12) . ? N112 C112 1.324(13) . ? N112 C113 1.408(13) . ? N131 C132 1.353(12) . ? N131 C134 1.410(14) . ? N131 C131 1.460(13) . ? N132 C132 1.316(14) . ? N132 C133 1.377(13) . ? N151 C152 1.286(13) . ? N151 C154 1.356(13) . ? N151 C151 1.476(13) . ? N152 C152 1.343(14) . ? N152 C153 1.382(12) . ? N152 Mn4 2.209(8) 2_646 ? N201 C201 1.38(2) . ? N201 C202 1.431(19) . ? N201 C203 1.49(2) . ? C1 C12 1.576(10) . ? C2 C16 1.555(12) . ? C3 C22 1.551(11) . ? C4 C26 1.588(10) . ? C5 C32 1.466(11) . ? C6 C36 1.514(11) . ? C7 C42 1.547(11) . ? C8 C46 1.499(12) . ? C12 C13 1.429(10) . ? C13 C14 1.395(12) . ? C13 H1 0.9500 . ? C14 C15 1.400(12) . ? C14 C24 1.477(11) . ? C15 C16 1.417(11) . ? C15 H2 0.9500 . ? C22 C23 1.387(11) . ? C23 C24 1.401(11) . ? C23 H3 0.9500 . ? C24 C25 1.371(11) . ? C25 C26 1.443(10) . ? C25 H4 0.9500 . ? C32 C33 1.404(11) . ? C33 C34 1.362(11) . ? C33 H5 0.9500 . ? C34 C35 1.441(11) . ? C34 C44 1.515(10) . ? C35 C36 1.399(10) . ? C35 H6 0.9500 . ? C42 C43 1.374(11) . ? C43 C44 1.392(12) . ? C43 H7 0.9500 . ? C44 C45 1.400(11) . ? C45 C46 1.387(11) . ? C45 H8 0.9500 . ? C101 C106 1.379(14) . ? C101 C102 1.386(14) . ? C101 C111 1.501(14) . ? C102 C103 1.450(14) . ? C102 C121 1.489(15) . ? C103 C104 1.388(14) . ? C103 C131 1.533(13) . ? C104 C105 1.425(14) . ? C104 C141 1.515(15) . ? C105 C106 1.413(13) . ? C105 C151 1.496(14) . ? C106 C161 1.535(14) . ? C111 H9 0.9900 . ? C111 H10 0.9900 . ? C112 H11 0.9500 . ? C113 C114 1.371(18) . ? C113 H12 0.9500 . ? C114 H13 0.9500 . ? C121 H14 0.9800 . ? C121 H15 0.9800 . ? C121 H16 0.9800 . ? C131 H17 0.9900 . ? C131 H18 0.9900 . ? C132 H19 0.9500 . ? C133 C134 1.293(17) . ? C133 H20 0.9500 . ? C134 H21 0.9500 . ? C141 H22 0.9800 . ? C141 H23 0.9800 . ? C141 H24 0.9800 . ? C151 H25 0.9900 . ? C151 H26 0.9900 . ? C152 H27 0.9500 . ? C153 C154 1.384(16) . ? C153 H28 0.9500 . ? C154 H29 0.9500 . ? C161 H30 0.9800 . ? C161 H31 0.9800 . ? C161 H32 0.9800 . ? C201 H33 0.9500 . ? C202 H34 0.9800 . ? C202 H35 0.9800 . ? C202 H36 0.9800 . ? C203 H37 0.9800 . ? C203 H38 0.9800 . ? C203 H39 0.9800 . ? 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 O17 Mn1 O18 99.5(2) . . ? O17 Mn1 N11 97.8(2) . . ? O18 Mn1 N11 137.8(2) . . ? O17 Mn1 O19 178.2(3) . . ? O18 Mn1 O19 78.7(3) . . ? N11 Mn1 O19 83.9(3) . . ? O17 Mn1 O3 95.2(2) . . ? O18 Mn1 O3 144.7(2) . . ? N11 Mn1 O3 70.4(2) . . ? O19 Mn1 O3 86.2(3) . . ? O17 Mn1 O5 84.0(2) . 1_556 ? O18 Mn1 O5 79.5(2) . 1_556 ? N11 Mn1 O5 140.7(2) . 1_556 ? O19 Mn1 O5 95.3(2) . 1_556 ? O3 Mn1 O5 70.32(19) . 1_556 ? O17 Mn1 O1 88.9(2) . . ? O18 Mn1 O1 74.9(2) . . ? N11 Mn1 O1 67.2(2) . . ? O19 Mn1 O1 91.0(3) . . ? O3 Mn1 O1 137.62(19) . . ? O5 Mn1 O1 151.8(2) 1_556 . ? O20 Mn2 O26 100.2(4) . . ? O20 Mn2 N112 83.4(3) . . ? O26 Mn2 N112 175.1(4) . . ? O20 Mn2 N21 139.3(3) . . ? O26 Mn2 N21 94.7(3) . . ? N112 Mn2 N21 84.4(3) . . ? O20 Mn2 O3 80.8(3) . 1_554 ? O26 Mn2 O3 81.9(3) . 1_554 ? N112 Mn2 O3 95.7(3) . 1_554 ? N21 Mn2 O3 139.1(2) . 1_554 ? O20 Mn2 O5 146.6(3) . . ? O26 Mn2 O5 90.3(4) . . ? N112 Mn2 O5 84.9(2) . . ? N21 Mn2 O5 70.0(2) . . ? O3 Mn2 O5 69.31(18) 1_554 . ? O20 Mn2 O7 73.9(2) . . ? O26 Mn2 O7 91.3(3) . . ? N112 Mn2 O7 92.7(2) . . ? N21 Mn2 O7 68.0(2) . . ? O3 Mn2 O7 152.2(2) 1_554 . ? O5 Mn2 O7 137.96(19) . . ? O21 Mn3 N132 165.4(3) . . ? O21 Mn3 N31 93.6(2) . . ? N132 Mn3 N31 88.9(3) . . ? O21 Mn3 O9 94.6(3) . . ? N132 Mn3 O9 99.8(3) . . ? N31 Mn3 O9 69.9(2) . . ? O21 Mn3 O7 89.7(2) . 2_646 ? N132 Mn3 O7 95.3(2) . 2_646 ? N31 Mn3 O7 150.2(2) . 2_646 ? O9 Mn3 O7 80.3(2) . 2_646 ? O21 Mn3 O11 82.7(2) . . ? N132 Mn3 O11 84.9(2) . . ? N31 Mn3 O11 68.0(2) . . ? O9 Mn3 O11 137.5(2) . . ? O7 Mn3 O11 141.7(2) 2_646 . ? O21 Mn3 O8 86.5(2) . 2_646 ? N132 Mn3 O8 85.3(3) . 2_646 ? N31 Mn3 O8 154.8(2) . 2_646 ? O9 Mn3 O8 135.2(2) . 2_646 ? O7 Mn3 O8 54.9(2) 2_646 2_646 ? O11 Mn3 O8 87.1(2) . 2_646 ? O22 Mn4 N152 177.9(3) . 2_656 ? O22 Mn4 N41 90.8(2) . . ? N152 Mn4 N41 88.5(3) 2_656 . ? O22 Mn4 O13 85.0(2) . . ? N152 Mn4 O13 92.9(3) 2_656 . ? N41 Mn4 O13 71.2(2) . . ? O22 Mn4 O1 91.6(2) . 2_657 ? N152 Mn4 O1 90.1(3) 2_656 2_657 ? N41 Mn4 O1 145.1(2) . 2_657 ? O13 Mn4 O1 143.6(2) . 2_657 ? O22 Mn4 O15 90.6(2) . . ? N152 Mn4 O15 91.0(2) 2_656 . ? N41 Mn4 O15 67.8(2) . . ? O13 Mn4 O15 138.7(2) . . ? O1 Mn4 O15 77.4(2) 2_657 . ? O22 Mn4 O2 88.1(2) . 2_657 ? N152 Mn4 O2 91.9(2) 2_656 2_657 ? N41 Mn4 O2 159.3(2) . 2_657 ? O13 Mn4 O2 88.14(19) . 2_657 ? O1 Mn4 O2 55.5(2) 2_657 2_657 ? O15 Mn4 O2 132.78(19) . 2_657 ? C1 O1 Mn4 91.3(5) . 2_647 ? C1 O1 Mn1 118.4(5) . . ? Mn4 O1 Mn1 147.9(3) 2_647 . ? C1 O2 Mn4 88.6(5) . 2_647 ? C2 O3 Mn1 122.2(5) . . ? C2 O3 Mn2 127.0(5) . 1_556 ? Mn1 O3 Mn2 110.7(2) . 1_556 ? C3 O5 Mn1 129.1(5) . 1_554 ? C3 O5 Mn2 121.1(5) . . ? Mn1 O5 Mn2 109.7(2) 1_554 . ? C4 O7 Mn3 93.8(5) . 2_656 ? C4 O7 Mn2 117.1(5) . . ? Mn3 O7 Mn2 145.9(3) 2_656 . ? C4 O8 Mn3 86.6(5) . 2_656 ? C5 O9 Mn3 121.1(6) . . ? C5 O10 H40 132(6) . . ? C6 O11 Mn3 121.8(5) . . ? C7 O13 Mn4 119.0(5) . . ? C8 O15 Mn4 118.3(5) . . ? C8 O16 H41 127(6) . . ? Mn1 O18 H46 129(6) . . ? H42 O23 H43 102(8) . . ? H44 O25 H45 87(9) . . ? C12 N11 C16 114.5(7) . . ? C12 N11 Mn1 126.7(5) . . ? C16 N11 Mn1 118.7(5) . . ? C26 N21 C22 115.8(7) . . ? C26 N21 Mn2 124.3(5) . . ? C22 N21 Mn2 119.0(5) . . ? C36 N31 C32 120.2(6) . . ? C36 N31 Mn3 121.9(5) . . ? C32 N31 Mn3 117.8(5) . . ? C46 N41 C42 118.8(7) . . ? C46 N41 Mn4 121.4(5) . . ? C42 N41 Mn4 119.7(5) . . ? C114 N111 C112 107.9(9) . . ? C114 N111 C111 127.1(9) . . ? C112 N111 C111 124.9(8) . . ? C112 N112 C113 105.2(8) . . ? C112 N112 Mn2 126.0(6) . . ? C113 N112 Mn2 127.1(7) . . ? C132 N131 C134 104.6(9) . . ? C132 N131 C131 124.5(8) . . ? C134 N131 C131 130.8(8) . . ? C132 N132 C133 105.4(9) . . ? C132 N132 Mn3 116.4(6) . . ? C133 N132 Mn3 135.4(7) . . ? C152 N151 C154 106.7(9) . . ? C152 N151 C151 128.7(8) . . ? C154 N151 C151 124.5(8) . . ? C152 N152 C153 105.5(8) . . ? C152 N152 Mn4 128.8(6) . 2_646 ? C153 N152 Mn4 124.4(7) . 2_646 ? C201 N201 C202 124.0(17) . . ? C201 N201 C203 119.7(19) . . ? C202 N201 C203 116(2) . . ? O1 C1 O2 124.5(7) . . ? O1 C1 C12 116.5(7) . . ? O2 C1 C12 118.9(7) . . ? O4 C2 O3 131.2(8) . . ? O4 C2 C16 117.2(7) . . ? O3 C2 C16 111.6(7) . . ? O6 C3 O5 131.2(7) . . ? O6 C3 C22 115.5(7) . . ? O5 C3 C22 113.2(7) . . ? O8 C4 O7 124.7(7) . . ? O8 C4 C26 119.0(7) . . ? O7 C4 C26 116.2(7) . . ? O10 C5 O9 126.8(8) . . ? O10 C5 C32 117.1(7) . . ? O9 C5 C32 116.1(8) . . ? O12 C6 O11 127.9(8) . . ? O12 C6 C36 117.9(7) . . ? O11 C6 C36 114.1(7) . . ? O14 C7 O13 125.9(7) . . ? O14 C7 C42 118.5(7) . . ? O13 C7 C42 115.5(7) . . ? O15 C8 O16 127.7(8) . . ? O15 C8 C46 116.0(8) . . ? O16 C8 C46 116.3(8) . . ? N11 C12 C13 129.4(7) . . ? N11 C12 C1 110.1(6) . . ? C13 C12 C1 120.4(7) . . ? C14 C13 C12 113.2(8) . . ? C14 C13 H1 123.4 . . ? C12 C13 H1 123.4 . . ? C13 C14 C15 120.5(8) . . ? C13 C14 C24 119.8(7) . . ? C15 C14 C24 119.7(7) . . ? C14 C15 C16 118.6(8) . . ? C14 C15 H2 120.7 . . ? C16 C15 H2 120.7 . . ? N11 C16 C15 123.7(8) . . ? N11 C16 C2 116.9(7) . . ? C15 C16 C2 119.2(7) . . ? N21 C22 C23 122.8(7) . . ? N21 C22 C3 116.7(7) . . ? C23 C22 C3 120.3(7) . . ? C22 C23 C24 119.8(7) . . ? C22 C23 H3 120.1 . . ? C24 C23 H3 120.1 . . ? C25 C24 C23 120.3(8) . . ? C25 C24 C14 119.7(7) . . ? C23 C24 C14 120.0(7) . . ? C24 C25 C26 114.3(7) . . ? C24 C25 H4 122.9 . . ? C26 C25 H4 122.9 . . ? N21 C26 C25 126.9(7) . . ? N21 C26 C4 112.4(6) . . ? C25 C26 C4 120.7(6) . . ? N31 C32 C33 120.6(7) . . ? N31 C32 C5 114.3(7) . . ? C33 C32 C5 125.2(8) . . ? C34 C33 C32 120.1(7) . . ? C34 C33 H5 120.0 . . ? C32 C33 H5 120.0 . . ? C33 C34 C35 118.9(6) . . ? C33 C34 C44 120.8(7) . . ? C35 C34 C44 120.2(6) . . ? C36 C35 C34 118.8(7) . . ? C36 C35 H6 120.6 . . ? C34 C35 H6 120.6 . . ? N31 C36 C35 121.4(7) . . ? N31 C36 C6 113.8(6) . . ? C35 C36 C6 124.8(7) . . ? N41 C42 C43 123.7(7) . . ? N41 C42 C7 113.6(6) . . ? C43 C42 C7 122.8(7) . . ? C42 C43 C44 118.5(7) . . ? C42 C43 H7 120.8 . . ? C44 C43 H7 120.8 . . ? C43 C44 C45 117.4(7) . . ? C43 C44 C34 121.5(7) . . ? C45 C44 C34 120.9(7) . . ? C46 C45 C44 119.4(7) . . ? C46 C45 H8 120.3 . . ? C44 C45 H8 120.3 . . ? N41 C46 C45 122.1(8) . . ? N41 C46 C8 114.4(7) . . ? C45 C46 C8 123.5(8) . . ? C106 C101 C102 121.8(9) . . ? C106 C101 C111 118.9(9) . . ? C102 C101 C111 119.3(10) . . ? C101 C102 C103 117.7(9) . . ? C101 C102 C121 122.3(10) . . ? C103 C102 C121 119.9(9) . . ? C104 C103 C102 121.7(9) . . ? C104 C103 C131 119.1(9) . . ? C102 C103 C131 119.2(9) . . ? C103 C104 C105 118.2(9) . . ? C103 C104 C141 121.8(10) . . ? C105 C104 C141 119.9(10) . . ? C106 C105 C104 120.1(9) . . ? C106 C105 C151 120.0(9) . . ? C104 C105 C151 119.8(9) . . ? C101 C106 C105 120.0(9) . . ? C101 C106 C161 120.3(9) . . ? C105 C106 C161 119.6(10) . . ? N111 C111 C101 114.5(7) . . ? N111 C111 H9 108.6 . . ? C101 C111 H9 108.6 . . ? N111 C111 H10 108.6 . . ? C101 C111 H10 108.6 . . ? H9 C111 H10 107.6 . . ? N112 C112 N111 111.2(8) . . ? N112 C112 H11 124.4 . . ? N111 C112 H11 124.4 . . ? C114 C113 N112 108.3(10) . . ? C114 C113 H12 125.8 . . ? N112 C113 H12 125.8 . . ? N111 C114 C113 107.2(10) . . ? N111 C114 H13 126.4 . . ? C113 C114 H13 126.4 . . ? C102 C121 H14 109.5 . . ? C102 C121 H15 109.5 . . ? H14 C121 H15 109.5 . . ? C102 C121 H16 109.5 . . ? H14 C121 H16 109.5 . . ? H15 C121 H16 109.5 . . ? N131 C131 C103 109.5(8) . . ? N131 C131 H17 109.8 . . ? C103 C131 H17 109.8 . . ? N131 C131 H18 109.8 . . ? C103 C131 H18 109.8 . . ? H17 C131 H18 108.2 . . ? N132 C132 N131 111.7(9) . . ? N132 C132 H19 124.2 . . ? N131 C132 H19 124.2 . . ? C134 C133 N132 110.8(10) . . ? C134 C133 H20 124.6 . . ? N132 C133 H20 124.6 . . ? C133 C134 N131 107.6(9) . . ? C133 C134 H21 126.2 . . ? N131 C134 H21 126.2 . . ? C104 C141 H22 109.5 . . ? C104 C141 H23 109.5 . . ? H22 C141 H23 109.5 . . ? C104 C141 H24 109.5 . . ? H22 C141 H24 109.5 . . ? H23 C141 H24 109.5 . . ? N151 C151 C105 114.5(7) . . ? N151 C151 H25 108.6 . . ? C105 C151 H25 108.6 . . ? N151 C151 H26 108.6 . . ? C105 C151 H26 108.6 . . ? H25 C151 H26 107.6 . . ? N151 C152 N152 113.3(9) . . ? N151 C152 H27 123.3 . . ? N152 C152 H27 123.3 . . ? N152 C153 C154 105.9(9) . . ? N152 C153 H28 127.1 . . ? C154 C153 H28 127.1 . . ? N151 C154 C153 108.6(9) . . ? N151 C154 H29 125.7 . . ? C153 C154 H29 125.7 . . ? C106 C161 H30 109.5 . . ? C106 C161 H31 109.5 . . ? H30 C161 H31 109.5 . . ? C106 C161 H32 109.5 . . ? H30 C161 H32 109.5 . . ? H31 C161 H32 109.5 . . ? O27 C201 N201 124(2) . . ? O27 C201 H33 117.9 . . ? N201 C201 H33 117.9 . . ? N201 C202 H34 109.5 . . ? N201 C202 H35 109.5 . . ? H34 C202 H35 109.5 . . ? N201 C202 H36 109.5 . . ? H34 C202 H36 109.5 . . ? H35 C202 H36 109.5 . . ? N201 C203 H37 109.5 . . ? N201 C203 H38 109.5 . . ? H37 C203 H38 109.5 . . ? N201 C203 H39 109.5 . . ? H37 C203 H39 109.5 . . ? H38 C203 H39 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 O17 Mn1 O1 C1 -108.2(6) . . . . ? O18 Mn1 O1 C1 151.7(7) . . . . ? N11 Mn1 O1 C1 -9.3(6) . . . . ? O19 Mn1 O1 C1 73.6(6) . . . . ? O3 Mn1 O1 C1 -11.8(8) . . . . ? O5 Mn1 O1 C1 176.8(5) 1_556 . . . ? O17 Mn1 O1 Mn4 96.4(6) . . . 2_647 ? O18 Mn1 O1 Mn4 -3.7(5) . . . 2_647 ? N11 Mn1 O1 Mn4 -164.7(6) . . . 2_647 ? O19 Mn1 O1 Mn4 -81.8(6) . . . 2_647 ? O3 Mn1 O1 Mn4 -167.2(4) . . . 2_647 ? O5 Mn1 O1 Mn4 21.4(9) 1_556 . . 2_647 ? O17 Mn1 O3 C2 93.5(6) . . . . ? O18 Mn1 O3 C2 -152.0(5) . . . . ? N11 Mn1 O3 C2 -2.9(6) . . . . ? O19 Mn1 O3 C2 -87.7(6) . . . . ? O5 Mn1 O3 C2 175.3(6) 1_556 . . . ? O1 Mn1 O3 C2 -0.4(7) . . . . ? O17 Mn1 O3 Mn2 -82.4(3) . . . 1_556 ? O18 Mn1 O3 Mn2 32.0(5) . . . 1_556 ? N11 Mn1 O3 Mn2 -178.9(3) . . . 1_556 ? O19 Mn1 O3 Mn2 96.3(3) . . . 1_556 ? O5 Mn1 O3 Mn2 -0.7(2) 1_556 . . 1_556 ? O1 Mn1 O3 Mn2 -176.4(2) . . . 1_556 ? O20 Mn2 O5 C3 -155.5(6) . . . . ? O26 Mn2 O5 C3 95.3(6) . . . . ? N112 Mn2 O5 C3 -85.5(6) . . . . ? N21 Mn2 O5 C3 0.3(5) . . . . ? O3 Mn2 O5 C3 176.5(6) 1_554 . . . ? O7 Mn2 O5 C3 3.0(7) . . . . ? O20 Mn2 O5 Mn1 27.3(6) . . . 1_554 ? O26 Mn2 O5 Mn1 -81.9(3) . . . 1_554 ? N112 Mn2 O5 Mn1 97.3(3) . . . 1_554 ? N21 Mn2 O5 Mn1 -176.9(3) . . . 1_554 ? O3 Mn2 O5 Mn1 -0.7(2) 1_554 . . 1_554 ? O7 Mn2 O5 Mn1 -174.2(2) . . . 1_554 ? O20 Mn2 O7 C4 152.7(7) . . . . ? O26 Mn2 O7 C4 -107.1(7) . . . . ? N112 Mn2 O7 C4 70.3(6) . . . . ? N21 Mn2 O7 C4 -12.5(6) . . . . ? O3 Mn2 O7 C4 177.9(6) 1_554 . . . ? O5 Mn2 O7 C4 -15.2(8) . . . . ? O20 Mn2 O7 Mn3 -0.3(5) . . . 2_656 ? O26 Mn2 O7 Mn3 100.0(6) . . . 2_656 ? N112 Mn2 O7 Mn3 -82.7(5) . . . 2_656 ? N21 Mn2 O7 Mn3 -165.4(6) . . . 2_656 ? O3 Mn2 O7 Mn3 25.0(8) 1_554 . . 2_656 ? O5 Mn2 O7 Mn3 -168.1(4) . . . 2_656 ? O21 Mn3 O9 C5 -100.6(8) . . . . ? N132 Mn3 O9 C5 76.7(8) . . . . ? N31 Mn3 O9 C5 -8.5(7) . . . . ? O7 Mn3 O9 C5 170.5(8) 2_646 . . . ? O11 Mn3 O9 C5 -16.4(9) . . . . ? O8 Mn3 O9 C5 169.8(7) 2_646 . . . ? O21 Mn3 O11 C6 93.1(6) . . . . ? N132 Mn3 O11 C6 -94.6(7) . . . . ? N31 Mn3 O11 C6 -3.8(6) . . . . ? O9 Mn3 O11 C6 4.3(8) . . . . ? O7 Mn3 O11 C6 173.3(6) 2_646 . . . ? O8 Mn3 O11 C6 179.9(6) 2_646 . . . ? O22 Mn4 O13 C7 86.1(6) . . . . ? N152 Mn4 O13 C7 -93.9(6) 2_656 . . . ? N41 Mn4 O13 C7 -6.5(6) . . . . ? O1 Mn4 O13 C7 172.1(6) 2_657 . . . ? O15 Mn4 O13 C7 0.9(8) . . . . ? O2 Mn4 O13 C7 174.3(6) 2_657 . . . ? O22 Mn4 O15 C8 -103.5(6) . . . . ? N152 Mn4 O15 C8 75.1(7) 2_656 . . . ? N41 Mn4 O15 C8 -12.9(6) . . . . ? O13 Mn4 O15 C8 -20.4(8) . . . . ? O1 Mn4 O15 C8 164.9(7) 2_657 . . . ? O2 Mn4 O15 C8 168.6(6) 2_657 . . . ? O17 Mn1 N11 C12 92.1(6) . . . . ? O18 Mn1 N11 C12 -21.3(8) . . . . ? O19 Mn1 N11 C12 -87.1(6) . . . . ? O3 Mn1 N11 C12 -175.2(6) . . . . ? O5 Mn1 N11 C12 -178.0(5) 1_556 . . . ? O1 Mn1 N11 C12 6.6(5) . . . . ? O17 Mn1 N11 C16 -91.9(6) . . . . ? O18 Mn1 N11 C16 154.7(5) . . . . ? O19 Mn1 N11 C16 89.0(6) . . . . ? O3 Mn1 N11 C16 0.9(5) . . . . ? O5 Mn1 N11 C16 -1.9(8) 1_556 . . . ? O1 Mn1 N11 C16 -177.3(6) . . . . ? O20 Mn2 N21 C26 -10.7(8) . . . . ? O26 Mn2 N21 C26 101.0(6) . . . . ? N112 Mn2 N21 C26 -83.8(6) . . . . ? O3 Mn2 N21 C26 -175.9(5) 1_554 . . . ? O5 Mn2 N21 C26 -170.5(6) . . . . ? O7 Mn2 N21 C26 11.4(5) . . . . ? O20 Mn2 N21 C22 157.9(6) . . . . ? O26 Mn2 N21 C22 -90.4(6) . . . . ? N112 Mn2 N21 C22 84.8(6) . . . . ? O3 Mn2 N21 C22 -7.3(7) 1_554 . . . ? O5 Mn2 N21 C22 -1.8(5) . . . . ? O7 Mn2 N21 C22 -179.9(6) . . . . ? O21 Mn3 N31 C36 -81.0(6) . . . . ? N132 Mn3 N31 C36 84.6(6) . . . . ? O9 Mn3 N31 C36 -174.6(7) . . . . ? O7 Mn3 N31 C36 -176.7(5) 2_646 . . . ? O11 Mn3 N31 C36 -0.4(6) . . . . ? O8 Mn3 N31 C36 8.3(10) 2_646 . . . ? O21 Mn3 N31 C32 99.6(6) . . . . ? N132 Mn3 N31 C32 -94.8(6) . . . . ? O9 Mn3 N31 C32 6.0(6) . . . . ? O7 Mn3 N31 C32 3.9(9) 2_646 . . . ? O11 Mn3 N31 C32 -179.8(6) . . . . ? O8 Mn3 N31 C32 -171.2(5) 2_646 . . . ? O22 Mn4 N41 C46 98.5(7) . . . . ? N152 Mn4 N41 C46 -83.4(7) 2_656 . . . ? O13 Mn4 N41 C46 -177.0(7) . . . . ? O1 Mn4 N41 C46 4.5(9) 2_657 . . . ? O15 Mn4 N41 C46 8.2(6) . . . . ? O2 Mn4 N41 C46 -174.8(6) 2_657 . . . ? O22 Mn4 N41 C42 -84.4(6) . . . . ? N152 Mn4 N41 C42 93.6(7) 2_656 . . . ? O13 Mn4 N41 C42 0.0(6) . . . . ? O1 Mn4 N41 C42 -178.4(5) 2_657 . . . ? O15 Mn4 N41 C42 -174.7(7) . . . . ? O2 Mn4 N41 C42 2.2(11) 2_657 . . . ? O20 Mn2 N112 C112 143.8(9) . . . . ? O26 Mn2 N112 C112 4(4) . . . . ? N21 Mn2 N112 C112 -75.1(9) . . . . ? O3 Mn2 N112 C112 63.8(9) 1_554 . . . ? O5 Mn2 N112 C112 -4.8(8) . . . . ? O7 Mn2 N112 C112 -142.7(8) . . . . ? O20 Mn2 N112 C113 -53.5(9) . . . . ? O26 Mn2 N112 C113 167(3) . . . . ? N21 Mn2 N112 C113 87.6(9) . . . . ? O3 Mn2 N112 C113 -133.5(9) 1_554 . . . ? O5 Mn2 N112 C113 157.9(9) . . . . ? O7 Mn2 N112 C113 20.0(9) . . . . ? O21 Mn3 N132 C132 -9.1(15) . . . . ? N31 Mn3 N132 C132 -108.9(7) . . . . ? O9 Mn3 N132 C132 -178.3(6) . . . . ? O7 Mn3 N132 C132 100.7(7) 2_646 . . . ? O11 Mn3 N132 C132 -40.9(6) . . . . ? O8 Mn3 N132 C132 46.6(6) 2_646 . . . ? O21 Mn3 N132 C133 148.8(10) . . . . ? N31 Mn3 N132 C133 49.0(9) . . . . ? O9 Mn3 N132 C133 -20.4(9) . . . . ? O7 Mn3 N132 C133 -101.4(9) 2_646 . . . ? O11 Mn3 N132 C133 117.0(9) . . . . ? O8 Mn3 N132 C133 -155.5(9) 2_646 . . . ? Mn4 O1 C1 O2 1.0(9) 2_647 . . . ? Mn1 O1 C1 O2 -166.2(6) . . . . ? Mn4 O1 C1 C12 178.1(6) 2_647 . . . ? Mn1 O1 C1 C12 10.9(9) . . . . ? Mn4 O2 C1 O1 -1.0(9) 2_647 . . . ? Mn4 O2 C1 C12 -178.0(6) 2_647 . . . ? Mn1 O3 C2 O4 -176.0(8) . . . . ? Mn2 O3 C2 O4 -0.7(13) 1_556 . . . ? Mn1 O3 C2 C16 3.9(8) . . . . ? Mn2 O3 C2 C16 179.2(4) 1_556 . . . ? Mn1 O5 C3 O6 -6.0(13) 1_554 . . . ? Mn2 O5 C3 O6 177.3(7) . . . . ? Mn1 O5 C3 C22 177.6(5) 1_554 . . . ? Mn2 O5 C3 C22 0.9(8) . . . . ? Mn3 O8 C4 O7 -0.6(9) 2_656 . . . ? Mn3 O8 C4 C26 -177.4(7) 2_656 . . . ? Mn3 O7 C4 O8 0.6(10) 2_656 . . . ? Mn2 O7 C4 O8 -164.6(7) . . . . ? Mn3 O7 C4 C26 177.6(6) 2_656 . . . ? Mn2 O7 C4 C26 12.3(9) . . . . ? Mn3 O9 C5 O10 -167.6(8) . . . . ? Mn3 O9 C5 C32 9.3(12) . . . . ? Mn3 O11 C6 O12 -171.0(7) . . . . ? Mn3 O11 C6 C36 6.6(9) . . . . ? Mn4 O13 C7 O14 -167.8(7) . . . . ? Mn4 O13 C7 C42 11.1(9) . . . . ? Mn4 O15 C8 O16 -164.1(7) . . . . ? Mn4 O15 C8 C46 15.4(10) . . . . ? C16 N11 C12 C13 -0.4(11) . . . . ? Mn1 N11 C12 C13 175.8(5) . . . . ? C16 N11 C12 C1 -179.9(6) . . . . ? Mn1 N11 C12 C1 -3.7(8) . . . . ? O1 C1 C12 N11 -5.3(10) . . . . ? O2 C1 C12 N11 172.0(7) . . . . ? O1 C1 C12 C13 175.2(7) . . . . ? O2 C1 C12 C13 -7.6(11) . . . . ? N11 C12 C13 C14 0.6(10) . . . . ? C1 C12 C13 C14 -179.9(6) . . . . ? C12 C13 C14 C15 -1.0(10) . . . . ? C12 C13 C14 C24 177.9(6) . . . . ? C13 C14 C15 C16 1.4(11) . . . . ? C24 C14 C15 C16 -177.5(7) . . . . ? C12 N11 C16 C15 0.7(11) . . . . ? Mn1 N11 C16 C15 -175.8(6) . . . . ? C12 N11 C16 C2 177.2(6) . . . . ? Mn1 N11 C16 C2 0.7(9) . . . . ? C14 C15 C16 N11 -1.2(12) . . . . ? C14 C15 C16 C2 -177.7(7) . . . . ? O4 C2 C16 N11 177.0(8) . . . . ? O3 C2 C16 N11 -3.0(10) . . . . ? O4 C2 C16 C15 -6.4(11) . . . . ? O3 C2 C16 C15 173.7(7) . . . . ? C26 N21 C22 C23 -3.1(11) . . . . ? Mn2 N21 C22 C23 -172.8(6) . . . . ? C26 N21 C22 C3 172.6(6) . . . . ? Mn2 N21 C22 C3 2.9(9) . . . . ? O6 C3 C22 N21 -179.5(7) . . . . ? O5 C3 C22 N21 -2.5(10) . . . . ? O6 C3 C22 C23 -3.7(11) . . . . ? O5 C3 C22 C23 173.3(7) . . . . ? N21 C22 C23 C24 1.1(12) . . . . ? C3 C22 C23 C24 -174.4(7) . . . . ? C22 C23 C24 C25 0.2(11) . . . . ? C22 C23 C24 C14 -177.1(7) . . . . ? C13 C14 C24 C25 177.5(7) . . . . ? C15 C14 C24 C25 -3.6(11) . . . . ? C13 C14 C24 C23 -5.2(11) . . . . ? C15 C14 C24 C23 173.7(7) . . . . ? C23 C24 C25 C26 0.6(10) . . . . ? C14 C24 C25 C26 177.9(6) . . . . ? C22 N21 C26 C25 4.2(11) . . . . ? Mn2 N21 C26 C25 173.2(5) . . . . ? C22 N21 C26 C4 -178.4(6) . . . . ? Mn2 N21 C26 C4 -9.4(8) . . . . ? C24 C25 C26 N21 -3.0(11) . . . . ? C24 C25 C26 C4 179.9(7) . . . . ? O8 C4 C26 N21 174.1(7) . . . . ? O7 C4 C26 N21 -3.0(10) . . . . ? O8 C4 C26 C25 -8.3(12) . . . . ? O7 C4 C26 C25 174.5(7) . . . . ? C36 N31 C32 C33 -1.9(12) . . . . ? Mn3 N31 C32 C33 177.5(6) . . . . ? C36 N31 C32 C5 176.7(8) . . . . ? Mn3 N31 C32 C5 -3.9(9) . . . . ? O10 C5 C32 N31 173.9(8) . . . . ? O9 C5 C32 N31 -3.4(12) . . . . ? O10 C5 C32 C33 -7.6(14) . . . . ? O9 C5 C32 C33 175.1(8) . . . . ? N31 C32 C33 C34 2.7(12) . . . . ? C5 C32 C33 C34 -175.7(8) . . . . ? C32 C33 C34 C35 -2.7(11) . . . . ? C32 C33 C34 C44 175.2(7) . . . . ? C33 C34 C35 C36 1.8(11) . . . . ? C44 C34 C35 C36 -176.1(7) . . . . ? C32 N31 C36 C35 1.1(12) . . . . ? Mn3 N31 C36 C35 -178.3(6) . . . . ? C32 N31 C36 C6 -177.0(7) . . . . ? Mn3 N31 C36 C6 3.5(9) . . . . ? C34 C35 C36 N31 -1.0(11) . . . . ? C34 C35 C36 C6 176.9(7) . . . . ? O12 C6 C36 N31 171.4(7) . . . . ? O11 C6 C36 N31 -6.5(10) . . . . ? O12 C6 C36 C35 -6.6(12) . . . . ? O11 C6 C36 C35 175.5(8) . . . . ? C46 N41 C42 C43 1.3(13) . . . . ? Mn4 N41 C42 C43 -175.8(6) . . . . ? C46 N41 C42 C7 -177.8(7) . . . . ? Mn4 N41 C42 C7 5.1(9) . . . . ? O14 C7 C42 N41 168.4(8) . . . . ? O13 C7 C42 N41 -10.6(10) . . . . ? O14 C7 C42 C43 -10.7(12) . . . . ? O13 C7 C42 C43 170.3(8) . . . . ? N41 C42 C43 C44 -1.2(13) . . . . ? C7 C42 C43 C44 177.9(7) . . . . ? C42 C43 C44 C45 2.1(12) . . . . ? C42 C43 C44 C34 -173.7(8) . . . . ? C33 C34 C44 C43 8.2(12) . . . . ? C35 C34 C44 C43 -173.9(7) . . . . ? C33 C34 C44 C45 -167.5(8) . . . . ? C35 C34 C44 C45 10.4(12) . . . . ? C43 C44 C45 C46 -3.2(12) . . . . ? C34 C44 C45 C46 172.6(8) . . . . ? C42 N41 C46 C45 -2.5(13) . . . . ? Mn4 N41 C46 C45 174.6(6) . . . . ? C42 N41 C46 C8 178.9(8) . . . . ? Mn4 N41 C46 C8 -4.0(10) . . . . ? C44 C45 C46 N41 3.5(13) . . . . ? C44 C45 C46 C8 -178.1(8) . . . . ? O15 C8 C46 N41 -8.0(12) . . . . ? O16 C8 C46 N41 171.7(8) . . . . ? O15 C8 C46 C45 173.5(8) . . . . ? O16 C8 C46 C45 -6.9(13) . . . . ? C106 C101 C102 C103 -3.9(13) . . . . ? C111 C101 C102 C103 175.8(8) . . . . ? C106 C101 C102 C121 -179.7(9) . . . . ? C111 C101 C102 C121 -0.1(14) . . . . ? C101 C102 C103 C104 -1.9(14) . . . . ? C121 C102 C103 C104 174.0(9) . . . . ? C101 C102 C103 C131 -179.7(9) . . . . ? C121 C102 C103 C131 -3.8(14) . . . . ? C102 C103 C104 C105 1.9(14) . . . . ? C131 C103 C104 C105 179.7(9) . . . . ? C102 C103 C104 C141 -173.7(10) . . . . ? C131 C103 C104 C141 4.1(15) . . . . ? C103 C104 C105 C106 3.6(14) . . . . ? C141 C104 C105 C106 179.3(9) . . . . ? C103 C104 C105 C151 -171.8(9) . . . . ? C141 C104 C105 C151 3.9(14) . . . . ? C102 C101 C106 C105 9.5(14) . . . . ? C111 C101 C106 C105 -170.2(8) . . . . ? C102 C101 C106 C161 -174.7(9) . . . . ? C111 C101 C106 C161 5.6(13) . . . . ? C104 C105 C106 C101 -9.3(13) . . . . ? C151 C105 C106 C101 166.1(8) . . . . ? C104 C105 C106 C161 174.9(9) . . . . ? C151 C105 C106 C161 -9.8(13) . . . . ? C114 N111 C111 C101 -165.6(12) . . . . ? C112 N111 C111 C101 10.8(15) . . . . ? C106 C101 C111 N111 -103.1(10) . . . . ? C102 C101 C111 N111 77.2(12) . . . . ? C113 N112 C112 N111 -0.8(12) . . . . ? Mn2 N112 C112 N111 165.0(6) . . . . ? C114 N111 C112 N112 -2.4(14) . . . . ? C111 N111 C112 N112 -179.4(9) . . . . ? C112 N112 C113 C114 3.6(14) . . . . ? Mn2 N112 C113 C114 -162.0(9) . . . . ? C112 N111 C114 C113 4.6(16) . . . . ? C111 N111 C114 C113 -178.5(11) . . . . ? N112 C113 C114 N111 -5.1(16) . . . . ? C132 N131 C131 C103 31.0(13) . . . . ? C134 N131 C131 C103 -144.5(10) . . . . ? C104 C103 C131 N131 -101.9(11) . . . . ? C102 C103 C131 N131 76.0(11) . . . . ? C133 N132 C132 N131 -1.2(10) . . . . ? Mn3 N132 C132 N131 162.9(6) . . . . ? C134 N131 C132 N132 0.6(10) . . . . ? C131 N131 C132 N132 -176.0(8) . . . . ? C132 N132 C133 C134 1.4(11) . . . . ? Mn3 N132 C133 C134 -158.1(8) . . . . ? N132 C133 C134 N131 -1.1(12) . . . . ? C132 N131 C134 C133 0.3(11) . . . . ? C131 N131 C134 C133 176.6(9) . . . . ? C152 N151 C151 C105 -5.4(15) . . . . ? C154 N151 C151 C105 169.6(9) . . . . ? C106 C105 C151 N151 110.2(10) . . . . ? C104 C105 C151 N151 -74.5(12) . . . . ? C154 N151 C152 N152 0.2(13) . . . . ? C151 N151 C152 N152 176.0(9) . . . . ? C153 N152 C152 N151 0.3(12) . . . . ? Mn4 N152 C152 N151 -166.9(6) 2_646 . . . ? C152 N152 C153 C154 -0.7(11) . . . . ? Mn4 N152 C153 C154 167.3(7) 2_646 . . . ? C152 N151 C154 C153 -0.7(12) . . . . ? C151 N151 C154 C153 -176.7(9) . . . . ? N152 C153 C154 N151 0.9(12) . . . . ? C202 N201 C201 O27 5(3) . . . . ? C203 N201 C201 O27 178.9(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.047 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.201 #====END data_2 _database_code_depnum_ccdc_archive 'CCDC 897816' #TrackingRef 'CE-ART-08-2012-026338.cif' _audit_creation_date 2012-09-17 _audit_creation_method SHELXL-97 _publ_section_references ; Rigaku Americas and Rigaku Corporation. (2007). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku Americas, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (2008).Acta Cryst. A64, 112-122. SHELX97 ; _chemical_name_systematic ; [Ni2(B1)(L2)2]-13(H2O) ; _chemical_name_common (Ni2(B1)(L2)2)-13(H2O) _chemical_melting_point ? _chemical_formula_moiety 'C56 H78 N14 Ni2 O21' _chemical_formula_sum 'C56 H78 N14 Ni2 O21' _chemical_formula_weight 1400.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4995(19) _cell_length_b 12.4212(14) _cell_length_c 40.153(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.438(6) _cell_angle_gamma 90.00 _cell_volume 6387.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 33460 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description platelet _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 39912 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0379 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11102 _reflns_number_gt 8660 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0699P)^2^+6.2640P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11102 _refine_ls_number_parameters 966 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1406 _refine_ls_wR_factor_gt 0.1295 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.67903(3) 0.38792(3) 0.307516(10) 0.03060(12) Uani 1 1 d . . . Ni2 Ni 0.87118(3) 0.40527(4) 0.077570(10) 0.03643(13) Uani 1 1 d . . . O1 O 0.7799(2) 0.2361(2) 0.57835(6) 0.0517(7) Uani 1 1 d . . . O2 O 0.6778(3) 0.3548(3) 0.54228(8) 0.1011(14) Uani 1 1 d . . . O3 O 0.93874(17) -0.02921(18) 0.55275(5) 0.0371(5) Uani 1 1 d . . . O4 O 0.91953(19) -0.09130(19) 0.49866(6) 0.0416(6) Uani 1 1 d . . . O5 O 0.73725(16) 0.23072(17) 0.30377(5) 0.0323(5) Uani 1 1 d . . . O6 O 0.79589(17) 0.08310(18) 0.33615(5) 0.0370(5) Uani 1 1 d . . . O7 O 0.63273(18) 0.52211(18) 0.33543(6) 0.0413(6) Uani 1 1 d . . . O8 O 0.5937(2) 0.5531(2) 0.38476(7) 0.0602(7) Uani 1 1 d . . . O9 O 0.3413(3) 0.5875(2) 0.25338(8) 0.0611(8) Uani 1 1 d D . . H53 H 0.311(3) 0.632(3) 0.2384(9) 0.073 Uiso 1 1 d D . . H54 H 0.367(4) 0.619(3) 0.2725(8) 0.073 Uiso 1 1 d D . . O10 O 0.2505(3) 0.6475(4) 0.36457(9) 0.105 Uani 1 1 d D . . H55 H 0.248(5) 0.679(4) 0.3833(10) 0.126 Uiso 1 1 d D . . H56 H 0.276(5) 0.584(2) 0.3697(16) 0.126 Uiso 1 1 d D . . O11 O 0.9923(3) 0.7607(3) 0.58228(11) 0.1017(13) Uani 1 1 d . . . O12 O 0.8418(5) 0.6022(5) 0.57880(17) 0.174(3) Uani 1 1 d . . . O13 O 0.4117(6) 0.6612(6) 0.32782(16) 0.090(3) Uani 0.594(11) 1 d P . . O13B O 0.4677(8) 0.6723(7) 0.3087(3) 0.095(5) Uani 0.406(11) 1 d P . . O14 O 1.0011(10) 0.6785(11) 0.5113(3) 0.122(4) Uani 0.499(8) 1 d P . . O14B O 0.9672(8) 0.6964(8) 0.4929(3) 0.087(3) Uani 0.501(8) 1 d P . . O15 O 0.9115(7) 0.4452(7) 0.5391(2) 0.109(3) Uani 0.499(8) 1 d P . . O15B O 0.8611(15) 0.5091(16) 0.5012(5) 0.239(9) Uani 0.501(8) 1 d PU . . O16 O 0.6172(9) 0.5369(10) 0.6241(3) 0.144(4) Uani 0.592(11) 1 d P . . O16B O 0.6837(15) 0.5635(12) 0.6126(4) 0.143(6) Uani 0.408(11) 1 d P . . O17 O 0.6311(10) 0.5516(7) 0.4594(3) 0.120(5) Uani 0.496(15) 1 d P . . O17B O 0.503(2) 0.545(3) 0.4359(6) 0.319(17) Uani 0.504(15) 1 d PU . . O18 O 0.5195(11) 0.6489(11) 0.4991(5) 0.177(6) Uani 0.592(11) 1 d P . . O18B O 0.4996(15) 0.6263(15) 0.5218(6) 0.138(6) Uani 0.408(11) 1 d P . . O19 O 0.729(2) 0.531(2) 0.5928(7) 0.127(9) Uani 0.210(14) 1 d PU . . O19B O 0.6438(9) 0.5626(9) 0.5609(3) 0.112(5) Uani 0.408(11) 1 d PU . . O20 O 0.515(4) 0.613(3) 0.5501(12) 0.12(2) Uani 0.12(2) 1 d P . . O20B O 0.524(2) 0.598(2) 0.5806(11) 0.18(2) Uani 0.29(3) 1 d P . . O21 O 0.490(2) 0.687(3) 0.4312(8) 0.18(2) Uani 0.227(17) 1 d P . . O21B O 0.6812(15) 0.5567(15) 0.5043(6) 0.248(11) Uani 0.504(15) 1 d P . . O22 O 0.8227(8) 0.5376(6) 0.4748(2) 0.097(3) Uani 0.499(8) 1 d P . . O22B O 0.9368(7) 0.4079(7) 0.4446(2) 0.111(4) Uani 0.501(8) 1 d P . . O23 O 0.4125(12) 0.7530(13) 0.3649(4) 0.175(8) Uani 0.406(11) 1 d P . . N11 N 0.9440(2) 0.5837(2) 0.32250(7) 0.0399(7) Uani 1 1 d . . . N12 N 0.8260(2) 0.4579(2) 0.31954(7) 0.0370(6) Uani 1 1 d . . . N31 N 0.6436(2) 0.8334(2) 0.21220(8) 0.0421(7) Uani 1 1 d . . . N32 N 0.4748(2) 0.8337(2) 0.20446(6) 0.0323(6) Uani 1 1 d . . . N51 N 0.9665(2) 0.5550(2) 0.17419(7) 0.0400(7) Uani 1 1 d . . . N52 N 0.9101(2) 0.4485(2) 0.12872(6) 0.0380(6) Uani 1 1 d . . . N71 N 0.8235(2) 0.1384(2) 0.52767(6) 0.0370(6) Uani 1 1 d . . . N81 N 0.70724(19) 0.3326(2) 0.35609(6) 0.0312(6) Uani 1 1 d . . . N111 N 0.5382(2) 0.4779(2) 0.20318(6) 0.0361(6) Uani 1 1 d . . . N112 N 0.6407(2) 0.4349(2) 0.25587(7) 0.0351(6) Uani 1 1 d . . . N131 N 0.1666(2) 0.2659(2) 0.08674(8) 0.0461(7) Uani 1 1 d . . . N132 N 0.0088(2) 0.3166(2) 0.08586(6) 0.0378(6) Uani 1 1 d . . . N151 N 0.5816(2) 0.5718(3) 0.06042(7) 0.0471(7) Uani 1 1 d . . . N152 N 0.7382(2) 0.5049(3) 0.06829(7) 0.0427(7) Uani 1 1 d . . . C1 C 0.9552(2) 0.7158(2) 0.27806(8) 0.0337(7) Uani 1 1 d . . . C2 C 0.8741(3) 0.7890(3) 0.26454(9) 0.0382(8) Uani 1 1 d . . . C3 C 0.8352(3) 0.8058(3) 0.22821(9) 0.0390(8) Uani 1 1 d . . . C4 C 0.8813(3) 0.7555(3) 0.20573(9) 0.0381(8) Uani 1 1 d . . . C5 C 0.9676(3) 0.6895(3) 0.22000(9) 0.0377(8) Uani 1 1 d . . . C6 C 1.0028(2) 0.6655(3) 0.25565(8) 0.0345(7) Uani 1 1 d . . . C7 C 0.7384(3) 0.2778(4) 0.54875(9) 0.0576(11) Uani 1 1 d . . . C8 C 0.9090(2) -0.0227(3) 0.51934(8) 0.0341(7) Uani 1 1 d . . . C9 C 0.7620(2) 0.1755(3) 0.33215(8) 0.0310(7) Uani 1 1 d . . . C10 C 0.6332(3) 0.4986(3) 0.36600(9) 0.0424(8) Uani 1 1 d . . . C11 C 0.9907(3) 0.6865(3) 0.31623(9) 0.0469(9) Uani 1 1 d . . . H1 H 1.0678 0.6802 0.3247 0.056 Uiso 1 1 calc R . . H2 H 0.9708 0.7446 0.3298 0.056 Uiso 1 1 calc R . . C12 C 0.8450(3) 0.5509(3) 0.30733(8) 0.0439(9) Uani 1 1 d . . . H3 H 0.7944 0.5907 0.2898 0.053 Uiso 1 1 calc R . . C13 C 0.9180(3) 0.4301(3) 0.34444(9) 0.0412(8) Uani 1 1 d . . . H4 H 0.9290 0.3665 0.3583 0.049 Uiso 1 1 calc R . . C14 C 0.9912(3) 0.5070(3) 0.34641(9) 0.0443(8) Uani 1 1 d . . . H5 H 1.0614 0.5071 0.3615 0.053 Uiso 1 1 calc R . . C21 C 0.8271(3) 0.8479(3) 0.28907(12) 0.0611(12) Uani 1 1 d . . . H6 H 0.8009 0.7954 0.3025 0.073 Uiso 1 1 calc R . . H7 H 0.7693 0.8934 0.2753 0.073 Uiso 1 1 calc R . . H8 H 0.8806 0.8929 0.3053 0.073 Uiso 1 1 calc R . . C31 C 0.7438(3) 0.8816(3) 0.21297(13) 0.0567(11) Uani 1 1 d . . . H9 H 0.7552 0.9483 0.2272 0.068 Uiso 1 1 calc R . . H10 H 0.7406 0.9016 0.1888 0.068 Uiso 1 1 calc R . . C32 C 0.5524(3) 0.8831(3) 0.19756(8) 0.0358(7) Uani 1 1 d . . . H11 H 0.5444 0.9466 0.1838 0.043 Uiso 1 1 calc R . . C33 C 0.5190(3) 0.7485(3) 0.22530(9) 0.0418(8) Uani 1 1 d . . . H12 H 0.4827 0.6985 0.2351 0.050 Uiso 1 1 calc R . . C34 C 0.6226(3) 0.7464(3) 0.22990(11) 0.0525(10) Uani 1 1 d . . . H13 H 0.6714 0.6946 0.2429 0.063 Uiso 1 1 calc R . . C41 C 0.8375(3) 0.7719(4) 0.16624(10) 0.0627(11) Uani 1 1 d . . . H14 H 0.7612 0.7664 0.1588 0.075 Uiso 1 1 calc R . . H15 H 0.8656 0.7167 0.1543 0.075 Uiso 1 1 calc R . . H16 H 0.8575 0.8434 0.1602 0.075 Uiso 1 1 calc R . . C51 C 1.0250(3) 0.6436(3) 0.19614(10) 0.0512(10) Uani 1 1 d . . . H17 H 1.0363 0.7015 0.1808 0.061 Uiso 1 1 calc R . . H18 H 1.0943 0.6168 0.2107 0.061 Uiso 1 1 calc R . . C52 C 0.9724(3) 0.5287(3) 0.14276(8) 0.0410(8) Uani 1 1 d . . . H19 H 1.0165 0.5638 0.1318 0.049 Uiso 1 1 calc R . . C53 C 0.8620(3) 0.4210(3) 0.15304(9) 0.0435(8) Uani 1 1 d . . . H20 H 0.8121 0.3651 0.1504 0.052 Uiso 1 1 calc R . . C54 C 0.8970(3) 0.4860(3) 0.18117(9) 0.0465(9) Uani 1 1 d . . . H21 H 0.8772 0.4842 0.2019 0.056 Uiso 1 1 calc R . . C61 C 1.0887(3) 0.5848(3) 0.27029(12) 0.0577(10) Uani 1 1 d . . . H22 H 1.1565 0.6194 0.2738 0.069 Uiso 1 1 calc R . . H23 H 1.0803 0.5247 0.2538 0.069 Uiso 1 1 calc R . . H24 H 1.0853 0.5578 0.2928 0.069 Uiso 1 1 calc R . . C72 C 0.7660(3) 0.2265(3) 0.51837(8) 0.0462(9) Uani 1 1 d . . . C73 C 0.7368(3) 0.2644(3) 0.48439(9) 0.0473(9) Uani 1 1 d . . . H25 H 0.6956 0.3277 0.4781 0.057 Uiso 1 1 calc R . . C74 C 0.7685(3) 0.2088(3) 0.45931(8) 0.0392(8) Uani 1 1 d . . . C75 C 0.8256(3) 0.1142(3) 0.46973(8) 0.0362(7) Uani 1 1 d . . . H26 H 0.8466 0.0731 0.4532 0.043 Uiso 1 1 calc R . . C76 C 0.8516(2) 0.0804(3) 0.50426(8) 0.0345(7) Uani 1 1 d . . . C82 C 0.6835(3) 0.3913(3) 0.38028(8) 0.0366(7) Uani 1 1 d . . . C83 C 0.7015(3) 0.3528(3) 0.41381(8) 0.0432(8) Uani 1 1 d . . . H27 H 0.6851 0.3960 0.4309 0.052 Uiso 1 1 calc R . . C84 C 0.7438(3) 0.2505(3) 0.42274(8) 0.0380(8) Uani 1 1 d . . . C85 C 0.7636(2) 0.1887(3) 0.39637(8) 0.0349(7) Uani 1 1 d . . . H28 H 0.7895 0.1173 0.4011 0.042 Uiso 1 1 calc R . . C86 C 0.7450(2) 0.2332(2) 0.36337(8) 0.0320(7) Uani 1 1 d . . . C101 C 0.4255(2) 0.4837(3) 0.13974(8) 0.0376(8) Uani 1 1 d . . . C102 C 0.3647(3) 0.3919(3) 0.12823(9) 0.0410(8) Uani 1 1 d . . . C103 C 0.3357(3) 0.3618(3) 0.09286(9) 0.0422(8) Uani 1 1 d . . . C104 C 0.3745(3) 0.4203(3) 0.06947(9) 0.0420(8) Uani 1 1 d . . . C105 C 0.4352(2) 0.5116(3) 0.08154(8) 0.0407(8) Uani 1 1 d . . . C106 C 0.4620(3) 0.5445(3) 0.11668(8) 0.0393(8) Uani 1 1 d . . . C111 C 0.4444(3) 0.5230(3) 0.17673(8) 0.0434(8) Uani 1 1 d . . . H29 H 0.4508 0.6024 0.1769 0.052 Uiso 1 1 calc R . . H30 H 0.3825 0.5052 0.1838 0.052 Uiso 1 1 calc R . . C112 C 0.5485(3) 0.4723(3) 0.23733(8) 0.0359(7) Uani 1 1 d . . . H31 H 0.4956 0.4928 0.2471 0.043 Uiso 1 1 calc R . . C113 C 0.6926(3) 0.4156(3) 0.23183(9) 0.0460(9) Uani 1 1 d . . . H32 H 0.7615 0.3881 0.2372 0.055 Uiso 1 1 calc R . . C114 C 0.6292(3) 0.4422(3) 0.19922(9) 0.0491(9) Uani 1 1 d . . . H33 H 0.6452 0.4370 0.1779 0.059 Uiso 1 1 calc R . . C121 C 0.3288(3) 0.3254(4) 0.15392(10) 0.0588(11) Uani 1 1 d . . . H34 H 0.2615 0.3527 0.1548 0.071 Uiso 1 1 calc R . . H35 H 0.3806 0.3304 0.1773 0.071 Uiso 1 1 calc R . . H36 H 0.3211 0.2500 0.1463 0.071 Uiso 1 1 calc R . . C131 C 0.2675(3) 0.2642(3) 0.08005(12) 0.0566(10) Uani 1 1 d . . . H37 H 0.2541 0.2570 0.0545 0.068 Uiso 1 1 calc R . . H38 H 0.3065 0.1995 0.0914 0.068 Uiso 1 1 calc R . . C132 C 0.0962(3) 0.3454(3) 0.08000(8) 0.0381(7) Uani 1 1 d . . . H39 H 0.1077 0.4147 0.0719 0.046 Uiso 1 1 calc R . . C133 C 0.0247(3) 0.2134(3) 0.09718(11) 0.0588(11) Uani 1 1 d . . . H40 H -0.0246 0.1704 0.1035 0.071 Uiso 1 1 calc R . . C134 C 0.1214(4) 0.1806(4) 0.09811(14) 0.0733(13) Uani 1 1 d . . . H41 H 0.1518 0.1119 0.1052 0.088 Uiso 1 1 calc R . . C141 C 0.3535(3) 0.3808(4) 0.03220(10) 0.0606(11) Uani 1 1 d . . . H42 H 0.2794 0.3906 0.0190 0.073 Uiso 1 1 calc R . . H43 H 0.3715 0.3043 0.0325 0.073 Uiso 1 1 calc R . . H44 H 0.3961 0.4220 0.0209 0.073 Uiso 1 1 calc R . . C151 C 0.4699(3) 0.5823(4) 0.05649(10) 0.0537(10) Uani 1 1 d . . . H45 H 0.4286 0.5635 0.0321 0.064 Uiso 1 1 calc R . . H46 H 0.4549 0.6584 0.0605 0.064 Uiso 1 1 calc R . . C152 C 0.6409(3) 0.4834(3) 0.06639(9) 0.0456(9) Uani 1 1 d . . . H47 H 0.6160 0.4134 0.0690 0.055 Uiso 1 1 calc R . . C153 C 0.7402(3) 0.6141(3) 0.06346(11) 0.0566(10) Uani 1 1 d . . . H48 H 0.8002 0.6542 0.0636 0.068 Uiso 1 1 calc R . . C154 C 0.6446(3) 0.6562(4) 0.05848(11) 0.0599(11) Uani 1 1 d . . . H49 H 0.6249 0.7297 0.0544 0.072 Uiso 1 1 calc R . . C161 C 0.5286(3) 0.6426(3) 0.12952(10) 0.0540(10) Uani 1 1 d . . . H50 H 0.5828 0.6465 0.1181 0.065 Uiso 1 1 calc R . . H51 H 0.5615 0.6378 0.1550 0.065 Uiso 1 1 calc R . . H52 H 0.4849 0.7073 0.1238 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0290(2) 0.0343(2) 0.0270(2) 0.00528(15) 0.00660(16) -0.00387(17) Ni2 0.0346(2) 0.0527(3) 0.0225(2) -0.00252(17) 0.00979(17) -0.00399(19) O1 0.0597(16) 0.0694(17) 0.0273(12) 0.0014(11) 0.0154(11) 0.0219(14) O2 0.156(4) 0.102(3) 0.0455(17) 0.0072(17) 0.032(2) 0.078(3) O3 0.0358(12) 0.0499(14) 0.0274(11) 0.0052(9) 0.0127(9) 0.0001(10) O4 0.0479(14) 0.0453(14) 0.0345(12) -0.0004(10) 0.0172(11) 0.0010(11) O5 0.0320(12) 0.0396(12) 0.0252(10) 0.0048(9) 0.0090(9) -0.0003(9) O6 0.0364(13) 0.0410(13) 0.0337(12) 0.0052(9) 0.0113(10) 0.0033(10) O7 0.0449(14) 0.0350(12) 0.0413(13) 0.0055(10) 0.0097(11) -0.0053(11) O8 0.082(2) 0.0448(15) 0.0576(16) -0.0042(13) 0.0273(15) 0.0101(14) O9 0.069(2) 0.0581(18) 0.0635(19) 0.0235(14) 0.0316(17) 0.0144(15) O10 0.099 0.145 0.059 -0.026 0.007 0.043 O11 0.073(2) 0.092(3) 0.127(3) 0.033(2) 0.013(2) 0.002(2) O12 0.171(6) 0.144(5) 0.172(6) 0.028(4) 0.005(4) -0.027(4) O13 0.082(5) 0.121(5) 0.061(4) -0.001(3) 0.013(3) 0.032(4) O13B 0.070(7) 0.055(5) 0.121(10) -0.015(5) -0.024(6) 0.010(4) O14 0.110(9) 0.127(9) 0.108(9) 0.014(7) 0.003(7) -0.031(7) O14B 0.098(7) 0.074(5) 0.075(6) -0.012(5) 0.008(5) 0.015(5) O15 0.096(6) 0.117(7) 0.107(7) 0.011(5) 0.021(5) -0.005(5) O15B 0.26(2) 0.28(2) 0.167(16) -0.028(15) 0.053(15) -0.143(16) O16 0.124(8) 0.174(10) 0.138(8) -0.060(7) 0.048(7) -0.002(7) O16B 0.157(14) 0.145(11) 0.147(12) -0.024(9) 0.077(11) -0.047(10) O17 0.159(11) 0.098(7) 0.127(10) -0.010(6) 0.078(8) -0.003(6) O17B 0.36(3) 0.44(4) 0.23(2) 0.16(2) 0.19(2) 0.23(3) O18 0.169(11) 0.138(10) 0.224(17) -0.051(11) 0.061(11) -0.016(8) O18B 0.142(13) 0.140(12) 0.132(16) 0.015(11) 0.043(11) 0.037(10) O19 0.118(15) 0.140(15) 0.135(16) -0.034(13) 0.059(12) 0.039(12) O19B 0.104(9) 0.099(8) 0.140(10) -0.032(7) 0.049(7) -0.004(6) O20 0.18(5) 0.10(3) 0.06(3) 0.05(2) 0.04(3) 0.04(3) O20B 0.20(3) 0.14(2) 0.25(5) -0.02(2) 0.13(3) 0.056(16) O21 0.19(3) 0.17(3) 0.22(3) -0.09(2) 0.09(2) -0.13(2) O21B 0.251(19) 0.237(18) 0.29(3) 0.012(15) 0.130(17) 0.052(15) O22 0.145(8) 0.074(5) 0.078(5) -0.017(4) 0.042(5) -0.034(5) O22B 0.122(7) 0.095(6) 0.108(7) -0.005(5) 0.024(5) 0.014(5) O23 0.169(14) 0.196(16) 0.162(14) 0.021(11) 0.055(10) -0.070(12) N11 0.0427(17) 0.0452(16) 0.0327(14) -0.0037(12) 0.0133(13) -0.0175(13) N12 0.0344(15) 0.0414(16) 0.0340(14) 0.0047(12) 0.0091(12) -0.0088(13) N31 0.0313(15) 0.0336(15) 0.0628(19) 0.0056(13) 0.0168(13) 0.0007(12) N32 0.0314(14) 0.0347(14) 0.0309(13) -0.0039(11) 0.0097(11) 0.0004(12) N51 0.0387(16) 0.0528(17) 0.0353(14) -0.0107(13) 0.0212(13) -0.0050(14) N52 0.0338(15) 0.0546(18) 0.0271(13) -0.0026(12) 0.0116(11) 0.0008(14) N71 0.0379(15) 0.0477(16) 0.0255(13) 0.0010(12) 0.0104(11) 0.0044(13) N81 0.0299(14) 0.0324(14) 0.0302(13) 0.0023(11) 0.0077(11) -0.0056(11) N111 0.0343(15) 0.0462(16) 0.0277(13) 0.0045(11) 0.0099(11) 0.0099(13) N112 0.0345(15) 0.0372(15) 0.0331(14) 0.0060(11) 0.0098(12) -0.0022(12) N131 0.0433(17) 0.0420(17) 0.0566(18) 0.0024(14) 0.0209(14) 0.0029(14) N132 0.0418(16) 0.0453(16) 0.0278(13) 0.0000(12) 0.0133(12) -0.0028(13) N151 0.0353(16) 0.071(2) 0.0383(15) 0.0130(14) 0.0166(13) 0.0064(16) N152 0.0348(16) 0.065(2) 0.0308(14) -0.0002(13) 0.0138(12) -0.0007(14) C1 0.0358(18) 0.0328(17) 0.0361(16) -0.0088(13) 0.0163(14) -0.0123(14) C2 0.0354(18) 0.0330(17) 0.056(2) -0.0114(15) 0.0283(16) -0.0077(15) C3 0.0306(17) 0.0292(17) 0.059(2) 0.0040(15) 0.0170(16) -0.0038(14) C4 0.0345(18) 0.0382(18) 0.0420(18) 0.0011(14) 0.0128(15) -0.0080(15) C5 0.0352(18) 0.0397(18) 0.0451(19) -0.0092(15) 0.0227(15) -0.0072(15) C6 0.0274(16) 0.0378(17) 0.0406(18) -0.0039(14) 0.0139(14) -0.0020(14) C7 0.071(3) 0.068(3) 0.0337(19) 0.0019(18) 0.0158(18) 0.030(2) C8 0.0288(17) 0.0454(19) 0.0298(16) 0.0033(14) 0.0116(13) -0.0043(14) C9 0.0237(15) 0.0370(18) 0.0307(16) 0.0017(13) 0.0064(12) -0.0012(14) C10 0.046(2) 0.0370(18) 0.0399(19) -0.0020(15) 0.0081(16) -0.0070(16) C11 0.056(2) 0.047(2) 0.0400(19) -0.0068(15) 0.0176(17) -0.0241(18) C12 0.042(2) 0.048(2) 0.0348(17) 0.0083(15) 0.0035(15) -0.0132(17) C13 0.0334(18) 0.0402(19) 0.0476(19) 0.0037(15) 0.0096(15) -0.0011(15) C14 0.0355(19) 0.048(2) 0.047(2) -0.0021(16) 0.0101(16) -0.0036(16) C21 0.064(3) 0.048(2) 0.090(3) -0.026(2) 0.051(2) -0.011(2) C31 0.0297(19) 0.040(2) 0.102(3) 0.016(2) 0.023(2) -0.0006(16) C32 0.0328(18) 0.0347(17) 0.0385(17) 0.0006(14) 0.0092(14) 0.0026(14) C33 0.0343(19) 0.0368(19) 0.054(2) 0.0063(15) 0.0135(16) -0.0036(15) C34 0.0314(19) 0.041(2) 0.081(3) 0.0192(19) 0.0122(18) 0.0027(16) C41 0.065(3) 0.071(3) 0.047(2) 0.012(2) 0.010(2) -0.013(2) C51 0.047(2) 0.068(3) 0.051(2) -0.0269(19) 0.0312(18) -0.0165(19) C52 0.0357(18) 0.062(2) 0.0292(16) -0.0060(15) 0.0157(14) -0.0074(17) C53 0.053(2) 0.047(2) 0.0361(18) -0.0041(15) 0.0211(16) -0.0053(17) C54 0.055(2) 0.056(2) 0.0386(19) -0.0085(16) 0.0295(17) -0.0084(19) C61 0.040(2) 0.064(3) 0.071(3) 0.006(2) 0.020(2) 0.0168(19) C72 0.053(2) 0.055(2) 0.0297(17) -0.0012(15) 0.0117(15) 0.0110(19) C73 0.057(2) 0.050(2) 0.0321(17) 0.0035(15) 0.0099(16) 0.0139(18) C74 0.0429(19) 0.045(2) 0.0277(16) 0.0010(14) 0.0092(14) -0.0003(16) C75 0.0385(18) 0.0434(19) 0.0272(16) -0.0013(13) 0.0110(14) -0.0028(15) C76 0.0304(17) 0.0479(19) 0.0257(15) -0.0004(13) 0.0098(13) -0.0036(14) C82 0.0412(19) 0.0338(17) 0.0315(16) -0.0004(13) 0.0065(14) -0.0059(15) C83 0.055(2) 0.0414(19) 0.0321(17) -0.0039(14) 0.0126(16) -0.0005(17) C84 0.0418(19) 0.0421(19) 0.0271(16) 0.0014(14) 0.0068(14) -0.0051(15) C85 0.0364(18) 0.0382(18) 0.0270(15) 0.0044(13) 0.0057(13) -0.0005(14) C86 0.0271(16) 0.0360(17) 0.0294(15) 0.0018(13) 0.0041(12) -0.0059(14) C101 0.0323(17) 0.051(2) 0.0305(16) 0.0068(14) 0.0106(14) 0.0152(16) C102 0.0365(19) 0.049(2) 0.0408(19) 0.0098(15) 0.0166(15) 0.0104(16) C103 0.0331(18) 0.049(2) 0.0455(19) 0.0012(16) 0.0145(15) 0.0103(16) C104 0.0330(18) 0.058(2) 0.0352(17) 0.0032(15) 0.0118(15) 0.0137(17) C105 0.0293(17) 0.062(2) 0.0334(17) 0.0121(16) 0.0138(14) 0.0110(17) C106 0.0316(18) 0.049(2) 0.0374(18) 0.0088(15) 0.0119(14) 0.0103(15) C111 0.0399(19) 0.059(2) 0.0297(16) 0.0066(15) 0.0086(14) 0.0199(17) C112 0.0354(18) 0.0417(19) 0.0313(16) 0.0047(14) 0.0115(14) 0.0039(15) C113 0.0334(19) 0.070(3) 0.0373(18) 0.0097(17) 0.0150(15) 0.0093(17) C114 0.044(2) 0.073(3) 0.0332(18) 0.0072(17) 0.0175(16) 0.0161(19) C121 0.060(3) 0.069(3) 0.053(2) 0.019(2) 0.025(2) 0.003(2) C131 0.050(2) 0.051(2) 0.073(3) -0.006(2) 0.026(2) 0.0048(19) C132 0.0369(19) 0.0414(19) 0.0359(17) -0.0009(14) 0.0114(14) -0.0035(16) C133 0.060(3) 0.053(2) 0.069(3) 0.018(2) 0.029(2) -0.002(2) C134 0.066(3) 0.050(3) 0.108(4) 0.023(2) 0.034(3) 0.005(2) C141 0.054(3) 0.089(3) 0.038(2) -0.005(2) 0.0139(18) 0.004(2) C151 0.035(2) 0.084(3) 0.043(2) 0.0202(19) 0.0144(16) 0.0076(19) C152 0.039(2) 0.062(2) 0.0377(18) 0.0099(16) 0.0140(15) 0.0011(18) C153 0.043(2) 0.066(3) 0.070(3) -0.002(2) 0.030(2) -0.007(2) C154 0.055(3) 0.061(3) 0.074(3) 0.011(2) 0.035(2) 0.006(2) C161 0.048(2) 0.062(2) 0.051(2) 0.0062(19) 0.0150(18) -0.001(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N81 1.988(2) . ? Ni1 N112 2.057(3) . ? Ni1 N12 2.078(3) . ? Ni1 N32 2.090(3) 2_645 ? Ni1 O5 2.128(2) . ? Ni1 O7 2.206(2) . ? Ni2 N71 1.977(3) 4_565 ? Ni2 N52 2.025(3) . ? Ni2 N132 2.093(3) 1_655 ? Ni2 N152 2.114(3) . ? Ni2 O1 2.151(3) 4_565 ? Ni2 O3 2.184(2) 4_565 ? O1 C7 1.255(4) . ? O1 Ni2 2.151(3) 4_566 ? O2 C7 1.232(5) . ? O3 C8 1.275(4) . ? O3 Ni2 2.184(2) 4_566 ? O4 C8 1.230(4) . ? O5 C9 1.281(4) . ? O6 C9 1.227(4) . ? O7 C10 1.260(4) . ? O8 C10 1.251(4) . ? O9 H53 0.826(19) . ? O9 H54 0.834(19) . ? O10 H55 0.86(2) . ? O10 H56 0.86(2) . ? O13 O13B 1.243(13) . ? O14 O14B 0.769(10) . ? O15 O15B 1.66(2) . ? O15B O22 1.084(17) . ? O16 O16B 1.177(15) . ? O16B O19 1.22(2) . ? O17 O17B 1.69(3) . ? O17 O21B 1.71(2) . ? O17B O21 1.78(4) . ? O18 O18B 1.065(18) . ? O18B O20 1.10(5) . ? O19 O19B 1.48(3) . ? O19B O20 1.77(5) . ? O20 O20B 1.21(5) . ? N11 C12 1.345(4) . ? N11 C14 1.360(4) . ? N11 C11 1.481(4) . ? N12 C12 1.312(4) . ? N12 C13 1.370(4) . ? N31 C32 1.337(4) . ? N31 C34 1.371(4) . ? N31 C31 1.470(4) . ? N32 C32 1.316(4) . ? N32 C33 1.363(4) . ? N32 Ni1 2.090(3) 2_655 ? N51 C52 1.330(4) . ? N51 C54 1.363(4) . ? N51 C51 1.473(4) . ? N52 C52 1.311(4) . ? N52 C53 1.376(4) . ? N71 C72 1.325(4) . ? N71 C76 1.332(4) . ? N71 Ni2 1.977(3) 4_566 ? N81 C86 1.332(4) . ? N81 C82 1.332(4) . ? N111 C112 1.336(4) . ? N111 C114 1.361(4) . ? N111 C111 1.482(4) . ? N112 C112 1.317(4) . ? N112 C113 1.381(4) . ? N131 C132 1.337(4) . ? N131 C134 1.371(5) . ? N131 C131 1.469(5) . ? N132 C132 1.324(4) . ? N132 C133 1.354(5) . ? N132 Ni2 2.093(3) 1_455 ? N151 C152 1.335(5) . ? N151 C154 1.367(5) . ? N151 C151 1.472(4) . ? N152 C152 1.318(4) . ? N152 C153 1.371(5) . ? C1 C2 1.394(5) . ? C1 C6 1.406(4) . ? C1 C11 1.499(5) . ? C2 C3 1.401(5) . ? C2 C21 1.519(5) . ? C3 C4 1.395(5) . ? C3 C31 1.518(5) . ? C4 C5 1.392(5) . ? C4 C41 1.520(5) . ? C5 C6 1.391(5) . ? C5 C51 1.521(4) . ? C6 C61 1.505(5) . ? C7 C72 1.523(5) . ? C8 C76 1.519(5) . ? C9 C86 1.524(4) . ? C10 C82 1.523(5) . ? C11 H1 0.9900 . ? C11 H2 0.9900 . ? C12 H3 0.9500 . ? C13 C14 1.358(5) . ? C13 H4 0.9500 . ? C14 H5 0.9500 . ? C21 H6 0.9800 . ? C21 H7 0.9800 . ? C21 H8 0.9800 . ? C31 H9 0.9900 . ? C31 H10 0.9900 . ? C32 H11 0.9500 . ? C33 C34 1.352(5) . ? C33 H12 0.9500 . ? C34 H13 0.9500 . ? C41 H14 0.9800 . ? C41 H15 0.9800 . ? C41 H16 0.9800 . ? C51 H17 0.9900 . ? C51 H18 0.9900 . ? C52 H19 0.9500 . ? C53 C54 1.346(5) . ? C53 H20 0.9500 . ? C54 H21 0.9500 . ? C61 H22 0.9800 . ? C61 H23 0.9800 . ? C61 H24 0.9800 . ? C72 C73 1.378(5) . ? C73 C74 1.396(5) . ? C73 H25 0.9500 . ? C74 C75 1.395(5) . ? C74 C84 1.492(4) . ? C75 C76 1.383(4) . ? C75 H26 0.9500 . ? C82 C83 1.376(5) . ? C83 C84 1.393(5) . ? C83 H27 0.9500 . ? C84 C85 1.401(5) . ? C85 C86 1.383(4) . ? C85 H28 0.9500 . ? C101 C102 1.395(5) . ? C101 C106 1.400(5) . ? C101 C111 1.507(4) . ? C102 C103 1.400(5) . ? C102 C121 1.516(5) . ? C103 C104 1.412(5) . ? C103 C131 1.511(5) . ? C104 C105 1.393(5) . ? C104 C141 1.514(5) . ? C105 C106 1.402(5) . ? C105 C151 1.518(5) . ? C106 C161 1.505(5) . ? C111 H29 0.9900 . ? C111 H30 0.9900 . ? C112 H31 0.9500 . ? C113 C114 1.359(5) . ? C113 H32 0.9500 . ? C114 H33 0.9500 . ? C121 H34 0.9800 . ? C121 H35 0.9800 . ? C121 H36 0.9800 . ? C131 H37 0.9900 . ? C131 H38 0.9900 . ? C132 H39 0.9500 . ? C133 C134 1.357(6) . ? C133 H40 0.9500 . ? C134 H41 0.9500 . ? C141 H42 0.9800 . ? C141 H43 0.9800 . ? C141 H44 0.9800 . ? C151 H45 0.9900 . ? C151 H46 0.9900 . ? C152 H47 0.9500 . ? C153 C154 1.348(6) . ? C153 H48 0.9500 . ? C154 H49 0.9500 . ? C161 H50 0.9800 . ? C161 H51 0.9800 . ? C161 H52 0.9800 . ? 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 N81 Ni1 N112 175.16(10) . . ? N81 Ni1 N12 92.52(10) . . ? N112 Ni1 N12 91.88(10) . . ? N81 Ni1 N32 88.99(10) . 2_645 ? N112 Ni1 N32 86.83(10) . 2_645 ? N12 Ni1 N32 174.06(11) . 2_645 ? N81 Ni1 O5 77.98(9) . . ? N112 Ni1 O5 99.77(9) . . ? N12 Ni1 O5 93.05(10) . . ? N32 Ni1 O5 92.89(9) 2_645 . ? N81 Ni1 O7 76.11(9) . . ? N112 Ni1 O7 106.05(10) . . ? N12 Ni1 O7 88.23(10) . . ? N32 Ni1 O7 86.55(9) 2_645 . ? O5 Ni1 O7 154.09(8) . . ? N71 Ni2 N52 176.14(11) 4_565 . ? N71 Ni2 N132 90.29(11) 4_565 1_655 ? N52 Ni2 N132 92.63(10) . 1_655 ? N71 Ni2 N152 89.77(11) 4_565 . ? N52 Ni2 N152 87.52(11) . . ? N132 Ni2 N152 175.67(11) 1_655 . ? N71 Ni2 O1 77.66(10) 4_565 4_565 ? N52 Ni2 O1 99.65(10) . 4_565 ? N132 Ni2 O1 92.99(11) 1_655 4_565 ? N152 Ni2 O1 91.25(12) . 4_565 ? N71 Ni2 O3 77.30(10) 4_565 4_565 ? N52 Ni2 O3 105.32(10) . 4_565 ? N132 Ni2 O3 88.04(9) 1_655 4_565 ? N152 Ni2 O3 87.75(10) . 4_565 ? O1 Ni2 O3 154.94(8) 4_565 4_565 ? C7 O1 Ni2 114.2(2) . 4_566 ? C8 O3 Ni2 113.4(2) . 4_566 ? C9 O5 Ni1 115.27(19) . . ? C10 O7 Ni1 113.9(2) . . ? H53 O9 H54 108(5) . . ? H55 O10 H56 109(5) . . ? O22 O15B O15 170.3(16) . . ? O16 O16B O19 140(2) . . ? O17B O17 O21B 125.7(10) . . ? O17 O17B O21 93(2) . . ? O18 O18B O20 155(4) . . ? O16B O19 O19B 93.6(17) . . ? O19 O19B O20 138(2) . . ? O18B O20 O20B 175(6) . . ? O18B O20 O19B 99(4) . . ? O20B O20 O19B 85(3) . . ? C12 N11 C14 106.5(3) . . ? C12 N11 C11 126.8(3) . . ? C14 N11 C11 126.5(3) . . ? C12 N12 C13 104.8(3) . . ? C12 N12 Ni1 124.5(2) . . ? C13 N12 Ni1 130.0(2) . . ? C32 N31 C34 106.2(3) . . ? C32 N31 C31 122.3(3) . . ? C34 N31 C31 130.5(3) . . ? C32 N32 C33 105.6(3) . . ? C32 N32 Ni1 126.8(2) . 2_655 ? C33 N32 Ni1 127.0(2) . 2_655 ? C52 N51 C54 107.0(3) . . ? C52 N51 C51 124.7(3) . . ? C54 N51 C51 128.3(3) . . ? C52 N52 C53 105.4(3) . . ? C52 N52 Ni2 124.3(2) . . ? C53 N52 Ni2 128.7(2) . . ? C72 N71 C76 121.4(3) . . ? C72 N71 Ni2 119.1(2) . 4_566 ? C76 N71 Ni2 119.5(2) . 4_566 ? C86 N81 C82 120.7(3) . . ? C86 N81 Ni1 118.5(2) . . ? C82 N81 Ni1 120.7(2) . . ? C112 N111 C114 107.4(3) . . ? C112 N111 C111 122.9(3) . . ? C114 N111 C111 129.6(3) . . ? C112 N112 C113 105.3(3) . . ? C112 N112 Ni1 124.1(2) . . ? C113 N112 Ni1 129.4(2) . . ? C132 N131 C134 106.0(3) . . ? C132 N131 C131 127.9(3) . . ? C134 N131 C131 125.8(3) . . ? C132 N132 C133 105.0(3) . . ? C132 N132 Ni2 128.7(2) . 1_455 ? C133 N132 Ni2 126.2(3) . 1_455 ? C152 N151 C154 107.0(3) . . ? C152 N151 C151 128.9(3) . . ? C154 N151 C151 124.1(3) . . ? C152 N152 C153 104.8(3) . . ? C152 N152 Ni2 131.8(3) . . ? C153 N152 Ni2 123.4(2) . . ? C2 C1 C6 120.1(3) . . ? C2 C1 C11 121.0(3) . . ? C6 C1 C11 118.9(3) . . ? C1 C2 C3 119.5(3) . . ? C1 C2 C21 120.0(3) . . ? C3 C2 C21 120.5(3) . . ? C4 C3 C2 120.6(3) . . ? C4 C3 C31 119.3(3) . . ? C2 C3 C31 120.1(3) . . ? C5 C4 C3 119.0(3) . . ? C5 C4 C41 120.4(3) . . ? C3 C4 C41 120.6(3) . . ? C6 C5 C4 121.2(3) . . ? C6 C5 C51 119.5(3) . . ? C4 C5 C51 119.3(3) . . ? C5 C6 C1 119.2(3) . . ? C5 C6 C61 120.9(3) . . ? C1 C6 C61 119.8(3) . . ? O2 C7 O1 126.0(4) . . ? O2 C7 C72 118.0(3) . . ? O1 C7 C72 115.9(3) . . ? O4 C8 O3 126.9(3) . . ? O4 C8 C76 117.9(3) . . ? O3 C8 C76 115.1(3) . . ? O6 C9 O5 126.8(3) . . ? O6 C9 C86 118.7(3) . . ? O5 C9 C86 114.5(3) . . ? O8 C10 O7 126.1(3) . . ? O8 C10 C82 118.1(3) . . ? O7 C10 C82 115.7(3) . . ? N11 C11 C1 111.6(3) . . ? N11 C11 H1 109.3 . . ? C1 C11 H1 109.3 . . ? N11 C11 H2 109.3 . . ? C1 C11 H2 109.3 . . ? H1 C11 H2 108.0 . . ? N12 C12 N11 112.4(3) . . ? N12 C12 H3 123.8 . . ? N11 C12 H3 123.8 . . ? C14 C13 N12 109.9(3) . . ? C14 C13 H4 125.1 . . ? N12 C13 H4 125.1 . . ? C13 C14 N11 106.4(3) . . ? C13 C14 H5 126.8 . . ? N11 C14 H5 126.8 . . ? C2 C21 H6 109.5 . . ? C2 C21 H7 109.5 . . ? H6 C21 H7 109.5 . . ? C2 C21 H8 109.5 . . ? H6 C21 H8 109.5 . . ? H7 C21 H8 109.5 . . ? N31 C31 C3 112.4(3) . . ? N31 C31 H9 109.1 . . ? C3 C31 H9 109.1 . . ? N31 C31 H10 109.1 . . ? C3 C31 H10 109.1 . . ? H9 C31 H10 107.9 . . ? N32 C32 N31 112.1(3) . . ? N32 C32 H11 124.0 . . ? N31 C32 H11 124.0 . . ? C34 C33 N32 109.4(3) . . ? C34 C33 H12 125.3 . . ? N32 C33 H12 125.3 . . ? C33 C34 N31 106.8(3) . . ? C33 C34 H13 126.6 . . ? N31 C34 H13 126.6 . . ? C4 C41 H14 109.5 . . ? C4 C41 H15 109.5 . . ? H14 C41 H15 109.5 . . ? C4 C41 H16 109.5 . . ? H14 C41 H16 109.5 . . ? H15 C41 H16 109.5 . . ? N51 C51 C5 111.9(3) . . ? N51 C51 H17 109.2 . . ? C5 C51 H17 109.2 . . ? N51 C51 H18 109.2 . . ? C5 C51 H18 109.2 . . ? H17 C51 H18 107.9 . . ? N52 C52 N51 111.8(3) . . ? N52 C52 H19 124.1 . . ? N51 C52 H19 124.1 . . ? C54 C53 N52 109.1(3) . . ? C54 C53 H20 125.4 . . ? N52 C53 H20 125.4 . . ? C53 C54 N51 106.6(3) . . ? C53 C54 H21 126.7 . . ? N51 C54 H21 126.7 . . ? C6 C61 H22 109.5 . . ? C6 C61 H23 109.5 . . ? H22 C61 H23 109.5 . . ? C6 C61 H24 109.5 . . ? H22 C61 H24 109.5 . . ? H23 C61 H24 109.5 . . ? N71 C72 C73 121.3(3) . . ? N71 C72 C7 112.9(3) . . ? C73 C72 C7 125.8(3) . . ? C72 C73 C74 119.2(3) . . ? C72 C73 H25 120.4 . . ? C74 C73 H25 120.4 . . ? C75 C74 C73 117.9(3) . . ? C75 C74 C84 121.2(3) . . ? C73 C74 C84 121.0(3) . . ? C76 C75 C74 119.8(3) . . ? C76 C75 H26 120.1 . . ? C74 C75 H26 120.1 . . ? N71 C76 C75 120.3(3) . . ? N71 C76 C8 113.4(3) . . ? C75 C76 C8 126.2(3) . . ? N81 C82 C83 120.9(3) . . ? N81 C82 C10 112.7(3) . . ? C83 C82 C10 126.3(3) . . ? C82 C83 C84 120.0(3) . . ? C82 C83 H27 120.0 . . ? C84 C83 H27 120.0 . . ? C83 C84 C85 117.8(3) . . ? C83 C84 C74 121.1(3) . . ? C85 C84 C74 121.2(3) . . ? C86 C85 C84 119.0(3) . . ? C86 C85 H28 120.5 . . ? C84 C85 H28 120.5 . . ? N81 C86 C85 121.5(3) . . ? N81 C86 C9 113.7(3) . . ? C85 C86 C9 124.8(3) . . ? C102 C101 C106 121.0(3) . . ? C102 C101 C111 119.3(3) . . ? C106 C101 C111 119.5(3) . . ? C101 C102 C103 120.0(3) . . ? C101 C102 C121 120.1(3) . . ? C103 C102 C121 119.9(3) . . ? C102 C103 C104 119.6(3) . . ? C102 C103 C131 120.3(3) . . ? C104 C103 C131 120.1(3) . . ? C105 C104 C103 119.2(3) . . ? C105 C104 C141 120.9(3) . . ? C103 C104 C141 119.9(4) . . ? C104 C105 C106 121.6(3) . . ? C104 C105 C151 120.8(3) . . ? C106 C105 C151 117.5(3) . . ? C101 C106 C105 118.4(3) . . ? C101 C106 C161 120.5(3) . . ? C105 C106 C161 121.1(3) . . ? N111 C111 C101 115.1(3) . . ? N111 C111 H29 108.5 . . ? C101 C111 H29 108.5 . . ? N111 C111 H30 108.5 . . ? C101 C111 H30 108.5 . . ? H29 C111 H30 107.5 . . ? N112 C112 N111 111.8(3) . . ? N112 C112 H31 124.1 . . ? N111 C112 H31 124.1 . . ? C114 C113 N112 109.1(3) . . ? C114 C113 H32 125.5 . . ? N112 C113 H32 125.5 . . ? C113 C114 N111 106.5(3) . . ? C113 C114 H33 126.8 . . ? N111 C114 H33 126.8 . . ? C102 C121 H34 109.5 . . ? C102 C121 H35 109.5 . . ? H34 C121 H35 109.5 . . ? C102 C121 H36 109.5 . . ? H34 C121 H36 109.5 . . ? H35 C121 H36 109.5 . . ? N131 C131 C103 115.3(3) . . ? N131 C131 H37 108.5 . . ? C103 C131 H37 108.5 . . ? N131 C131 H38 108.5 . . ? C103 C131 H38 108.5 . . ? H37 C131 H38 107.5 . . ? N132 C132 N131 112.4(3) . . ? N132 C132 H39 123.8 . . ? N131 C132 H39 123.8 . . ? N132 C133 C134 110.1(4) . . ? N132 C133 H40 125.0 . . ? C134 C133 H40 125.0 . . ? C133 C134 N131 106.5(4) . . ? C133 C134 H41 126.8 . . ? N131 C134 H41 126.8 . . ? C104 C141 H42 109.5 . . ? C104 C141 H43 109.5 . . ? H42 C141 H43 109.5 . . ? C104 C141 H44 109.5 . . ? H42 C141 H44 109.5 . . ? H43 C141 H44 109.5 . . ? N151 C151 C105 113.5(3) . . ? N151 C151 H45 108.9 . . ? C105 C151 H45 108.9 . . ? N151 C151 H46 108.9 . . ? C105 C151 H46 108.9 . . ? H45 C151 H46 107.7 . . ? N152 C152 N151 111.9(3) . . ? N152 C152 H47 124.0 . . ? N151 C152 H47 124.0 . . ? C154 C153 N152 110.2(4) . . ? C154 C153 H48 124.9 . . ? N152 C153 H48 124.9 . . ? C153 C154 N151 106.1(4) . . ? C153 C154 H49 127.0 . . ? N151 C154 H49 127.0 . . ? C106 C161 H50 109.5 . . ? C106 C161 H51 109.5 . . ? H50 C161 H51 109.5 . . ? C106 C161 H52 109.5 . . ? H50 C161 H52 109.5 . . ? H51 C161 H52 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 N81 Ni1 O5 C9 0.2(2) . . . . ? N112 Ni1 O5 C9 -175.5(2) . . . . ? N12 Ni1 O5 C9 92.1(2) . . . . ? N32 Ni1 O5 C9 -88.2(2) 2_645 . . . ? O7 Ni1 O5 C9 -0.1(3) . . . . ? N81 Ni1 O7 C10 -7.9(2) . . . . ? N112 Ni1 O7 C10 167.7(2) . . . . ? N12 Ni1 O7 C10 -100.9(2) . . . . ? N32 Ni1 O7 C10 82.0(2) 2_645 . . . ? O5 Ni1 O7 C10 -7.5(3) . . . . ? O21B O17 O17B O21 92.4(16) . . . . ? O16 O16B O19 O19B 79(3) . . . . ? O16B O19 O19B O20 -7(4) . . . . ? O18 O18B O20 O20B 174(47) . . . . ? O18 O18B O20 O19B -38(8) . . . . ? O19 O19B O20 O18B 175(2) . . . . ? O19 O19B O20 O20B -8(4) . . . . ? N81 Ni1 N12 C12 -141.8(3) . . . . ? N112 Ni1 N12 C12 40.2(3) . . . . ? N32 Ni1 N12 C12 -37.1(11) 2_645 . . . ? O5 Ni1 N12 C12 140.1(3) . . . . ? O7 Ni1 N12 C12 -65.8(3) . . . . ? N81 Ni1 N12 C13 27.3(3) . . . . ? N112 Ni1 N12 C13 -150.7(3) . . . . ? N32 Ni1 N12 C13 132.0(9) 2_645 . . . ? O5 Ni1 N12 C13 -50.8(3) . . . . ? O7 Ni1 N12 C13 103.3(3) . . . . ? N71 Ni2 N52 C52 -138.8(17) 4_565 . . . ? N132 Ni2 N52 C52 82.3(3) 1_655 . . . ? N152 Ni2 N52 C52 -93.4(3) . . . . ? O1 Ni2 N52 C52 175.7(3) 4_565 . . . ? O3 Ni2 N52 C52 -6.4(3) 4_565 . . . ? N71 Ni2 N52 C53 24.5(19) 4_565 . . . ? N132 Ni2 N52 C53 -114.4(3) 1_655 . . . ? N152 Ni2 N52 C53 69.9(3) . . . . ? O1 Ni2 N52 C53 -20.9(3) 4_565 . . . ? O3 Ni2 N52 C53 156.9(3) 4_565 . . . ? N112 Ni1 N81 C86 62.4(14) . . . . ? N12 Ni1 N81 C86 -92.9(2) . . . . ? N32 Ni1 N81 C86 92.8(2) 2_645 . . . ? O5 Ni1 N81 C86 -0.3(2) . . . . ? O7 Ni1 N81 C86 179.5(2) . . . . ? N112 Ni1 N81 C82 -113.9(13) . . . . ? N12 Ni1 N81 C82 90.8(2) . . . . ? N32 Ni1 N81 C82 -83.5(2) 2_645 . . . ? O5 Ni1 N81 C82 -176.7(3) . . . . ? O7 Ni1 N81 C82 3.2(2) . . . . ? N81 Ni1 N112 C112 65.3(14) . . . . ? N12 Ni1 N112 C112 -139.4(3) . . . . ? N32 Ni1 N112 C112 34.8(3) 2_645 . . . ? O5 Ni1 N112 C112 127.2(3) . . . . ? O7 Ni1 N112 C112 -50.7(3) . . . . ? N81 Ni1 N112 C113 -100.4(13) . . . . ? N12 Ni1 N112 C113 55.0(3) . . . . ? N32 Ni1 N112 C113 -130.8(3) 2_645 . . . ? O5 Ni1 N112 C113 -38.4(3) . . . . ? O7 Ni1 N112 C113 143.7(3) . . . . ? N71 Ni2 N152 C152 81.5(3) 4_565 . . . ? N52 Ni2 N152 C152 -95.8(3) . . . . ? N132 Ni2 N152 C152 172.2(12) 1_655 . . . ? O1 Ni2 N152 C152 3.8(3) 4_565 . . . ? O3 Ni2 N152 C152 158.8(3) 4_565 . . . ? N71 Ni2 N152 C153 -100.0(3) 4_565 . . . ? N52 Ni2 N152 C153 82.7(3) . . . . ? N132 Ni2 N152 C153 -9.3(15) 1_655 . . . ? O1 Ni2 N152 C153 -177.7(3) 4_565 . . . ? O3 Ni2 N152 C153 -22.7(3) 4_565 . . . ? C6 C1 C2 C3 4.9(5) . . . . ? C11 C1 C2 C3 -173.1(3) . . . . ? C6 C1 C2 C21 -176.5(3) . . . . ? C11 C1 C2 C21 5.5(5) . . . . ? C1 C2 C3 C4 -4.3(5) . . . . ? C21 C2 C3 C4 177.1(3) . . . . ? C1 C2 C3 C31 177.3(3) . . . . ? C21 C2 C3 C31 -1.3(5) . . . . ? C2 C3 C4 C5 -0.9(5) . . . . ? C31 C3 C4 C5 177.5(3) . . . . ? C2 C3 C4 C41 178.7(3) . . . . ? C31 C3 C4 C41 -2.9(5) . . . . ? C3 C4 C5 C6 5.6(5) . . . . ? C41 C4 C5 C6 -174.0(3) . . . . ? C3 C4 C5 C51 -173.8(3) . . . . ? C41 C4 C5 C51 6.6(5) . . . . ? C4 C5 C6 C1 -5.0(5) . . . . ? C51 C5 C6 C1 174.4(3) . . . . ? C4 C5 C6 C61 173.4(3) . . . . ? C51 C5 C6 C61 -7.2(5) . . . . ? C2 C1 C6 C5 -0.3(5) . . . . ? C11 C1 C6 C5 177.7(3) . . . . ? C2 C1 C6 C61 -178.7(3) . . . . ? C11 C1 C6 C61 -0.7(5) . . . . ? Ni2 O1 C7 O2 175.3(4) 4_566 . . . ? Ni2 O1 C7 C72 -4.2(5) 4_566 . . . ? Ni2 O3 C8 O4 -166.3(3) 4_566 . . . ? Ni2 O3 C8 C76 11.6(3) 4_566 . . . ? Ni1 O5 C9 O6 179.1(2) . . . . ? Ni1 O5 C9 C86 0.0(3) . . . . ? Ni1 O7 C10 O8 -166.9(3) . . . . ? Ni1 O7 C10 C82 10.6(4) . . . . ? C12 N11 C11 C1 -41.2(5) . . . . ? C14 N11 C11 C1 143.4(3) . . . . ? C2 C1 C11 N11 98.4(4) . . . . ? C6 C1 C11 N11 -79.6(4) . . . . ? C13 N12 C12 N11 1.0(4) . . . . ? Ni1 N12 C12 N11 172.4(2) . . . . ? C14 N11 C12 N12 -0.9(4) . . . . ? C11 N11 C12 N12 -177.1(3) . . . . ? C12 N12 C13 C14 -0.7(4) . . . . ? Ni1 N12 C13 C14 -171.4(2) . . . . ? N12 C13 C14 N11 0.2(4) . . . . ? C12 N11 C14 C13 0.4(4) . . . . ? C11 N11 C14 C13 176.6(3) . . . . ? C32 N31 C31 C3 -175.1(3) . . . . ? C34 N31 C31 C3 17.7(6) . . . . ? C4 C3 C31 N31 105.3(4) . . . . ? C2 C3 C31 N31 -76.3(4) . . . . ? C33 N32 C32 N31 1.2(4) . . . . ? Ni1 N32 C32 N31 172.7(2) 2_655 . . . ? C34 N31 C32 N32 -0.4(4) . . . . ? C31 N31 C32 N32 -170.3(3) . . . . ? C32 N32 C33 C34 -1.6(4) . . . . ? Ni1 N32 C33 C34 -173.1(3) 2_655 . . . ? N32 C33 C34 N31 1.4(4) . . . . ? C32 N31 C34 C33 -0.6(4) . . . . ? C31 N31 C34 C33 168.1(4) . . . . ? C52 N51 C51 C5 151.8(3) . . . . ? C54 N51 C51 C5 -27.4(6) . . . . ? C6 C5 C51 N51 105.5(4) . . . . ? C4 C5 C51 N51 -75.0(4) . . . . ? C53 N52 C52 N51 -0.7(4) . . . . ? Ni2 N52 C52 N51 165.9(2) . . . . ? C54 N51 C52 N52 1.0(4) . . . . ? C51 N51 C52 N52 -178.4(3) . . . . ? C52 N52 C53 C54 0.0(4) . . . . ? Ni2 N52 C53 C54 -165.7(3) . . . . ? N52 C53 C54 N51 0.6(4) . . . . ? C52 N51 C54 C53 -1.0(4) . . . . ? C51 N51 C54 C53 178.4(4) . . . . ? C76 N71 C72 C73 -3.0(6) . . . . ? Ni2 N71 C72 C73 175.5(3) 4_566 . . . ? C76 N71 C72 C7 177.3(3) . . . . ? Ni2 N71 C72 C7 -4.2(4) 4_566 . . . ? O2 C7 C72 N71 -173.9(4) . . . . ? O1 C7 C72 N71 5.5(6) . . . . ? O2 C7 C72 C73 6.4(7) . . . . ? O1 C7 C72 C73 -174.1(4) . . . . ? N71 C72 C73 C74 0.0(6) . . . . ? C7 C72 C73 C74 179.7(4) . . . . ? C72 C73 C74 C75 2.4(6) . . . . ? C72 C73 C74 C84 -176.5(3) . . . . ? C73 C74 C75 C76 -2.0(5) . . . . ? C84 C74 C75 C76 176.9(3) . . . . ? C72 N71 C76 C75 3.4(5) . . . . ? Ni2 N71 C76 C75 -175.1(2) 4_566 . . . ? C72 N71 C76 C8 -174.9(3) . . . . ? Ni2 N71 C76 C8 6.7(4) 4_566 . . . ? C74 C75 C76 N71 -0.9(5) . . . . ? C74 C75 C76 C8 177.2(3) . . . . ? O4 C8 C76 N71 165.8(3) . . . . ? O3 C8 C76 N71 -12.4(4) . . . . ? O4 C8 C76 C75 -12.3(5) . . . . ? O3 C8 C76 C75 169.5(3) . . . . ? C86 N81 C82 C83 2.8(5) . . . . ? Ni1 N81 C82 C83 179.1(3) . . . . ? C86 N81 C82 C10 -175.2(3) . . . . ? Ni1 N81 C82 C10 1.0(4) . . . . ? O8 C10 C82 N81 169.6(3) . . . . ? O7 C10 C82 N81 -8.2(4) . . . . ? O8 C10 C82 C83 -8.4(5) . . . . ? O7 C10 C82 C83 173.9(3) . . . . ? N81 C82 C83 C84 -0.9(5) . . . . ? C10 C82 C83 C84 176.9(3) . . . . ? C82 C83 C84 C85 -1.9(5) . . . . ? C82 C83 C84 C74 177.2(3) . . . . ? C75 C74 C84 C83 -169.8(3) . . . . ? C73 C74 C84 C83 9.1(5) . . . . ? C75 C74 C84 C85 9.3(5) . . . . ? C73 C74 C84 C85 -171.9(3) . . . . ? C83 C84 C85 C86 2.8(5) . . . . ? C74 C84 C85 C86 -176.3(3) . . . . ? C82 N81 C86 C85 -1.9(4) . . . . ? Ni1 N81 C86 C85 -178.2(2) . . . . ? C82 N81 C86 C9 176.7(3) . . . . ? Ni1 N81 C86 C9 0.4(3) . . . . ? C84 C85 C86 N81 -1.0(5) . . . . ? C84 C85 C86 C9 -179.5(3) . . . . ? O6 C9 C86 N81 -179.5(3) . . . . ? O5 C9 C86 N81 -0.3(4) . . . . ? O6 C9 C86 C85 -0.9(5) . . . . ? O5 C9 C86 C85 178.3(3) . . . . ? C106 C101 C102 C103 -2.5(5) . . . . ? C111 C101 C102 C103 172.2(3) . . . . ? C106 C101 C102 C121 178.1(3) . . . . ? C111 C101 C102 C121 -7.2(5) . . . . ? C101 C102 C103 C104 4.5(5) . . . . ? C121 C102 C103 C104 -176.2(3) . . . . ? C101 C102 C103 C131 -178.4(3) . . . . ? C121 C102 C103 C131 1.0(5) . . . . ? C102 C103 C104 C105 -4.4(5) . . . . ? C131 C103 C104 C105 178.4(3) . . . . ? C102 C103 C104 C141 173.1(3) . . . . ? C131 C103 C104 C141 -4.0(5) . . . . ? C103 C104 C105 C106 2.5(5) . . . . ? C141 C104 C105 C106 -175.1(3) . . . . ? C103 C104 C105 C151 -174.3(3) . . . . ? C141 C104 C105 C151 8.1(5) . . . . ? C102 C101 C106 C105 0.5(5) . . . . ? C111 C101 C106 C105 -174.2(3) . . . . ? C102 C101 C106 C161 -179.3(3) . . . . ? C111 C101 C106 C161 6.0(5) . . . . ? C104 C105 C106 C101 -0.5(5) . . . . ? C151 C105 C106 C101 176.4(3) . . . . ? C104 C105 C106 C161 179.3(3) . . . . ? C151 C105 C106 C161 -3.8(5) . . . . ? C112 N111 C111 C101 -156.1(3) . . . . ? C114 N111 C111 C101 28.4(5) . . . . ? C102 C101 C111 N111 90.1(4) . . . . ? C106 C101 C111 N111 -95.1(4) . . . . ? C113 N112 C112 N111 0.1(4) . . . . ? Ni1 N112 C112 N111 -168.5(2) . . . . ? C114 N111 C112 N112 -0.1(4) . . . . ? C111 N111 C112 N112 -176.5(3) . . . . ? C112 N112 C113 C114 0.0(4) . . . . ? Ni1 N112 C113 C114 167.7(3) . . . . ? N112 C113 C114 N111 0.0(4) . . . . ? C112 N111 C114 C113 0.1(4) . . . . ? C111 N111 C114 C113 176.1(3) . . . . ? C132 N131 C131 C103 49.0(5) . . . . ? C134 N131 C131 C103 -138.0(4) . . . . ? C102 C103 C131 N131 56.8(5) . . . . ? C104 C103 C131 N131 -126.0(4) . . . . ? C133 N132 C132 N131 0.4(4) . . . . ? Ni2 N132 C132 N131 -176.8(2) 1_455 . . . ? C134 N131 C132 N132 -0.7(4) . . . . ? C131 N131 C132 N132 173.4(3) . . . . ? C132 N132 C133 C134 0.0(5) . . . . ? Ni2 N132 C133 C134 177.4(3) 1_455 . . . ? N132 C133 C134 N131 -0.5(5) . . . . ? C132 N131 C134 C133 0.7(5) . . . . ? C131 N131 C134 C133 -173.6(4) . . . . ? C152 N151 C151 C105 39.3(5) . . . . ? C154 N151 C151 C105 -140.6(4) . . . . ? C104 C105 C151 N151 -107.0(4) . . . . ? C106 C105 C151 N151 76.1(4) . . . . ? C153 N152 C152 N151 0.5(4) . . . . ? Ni2 N152 C152 N151 179.2(2) . . . . ? C154 N151 C152 N152 -0.3(4) . . . . ? C151 N151 C152 N152 179.9(3) . . . . ? C152 N152 C153 C154 -0.5(4) . . . . ? Ni2 N152 C153 C154 -179.4(3) . . . . ? N152 C153 C154 N151 0.3(5) . . . . ? C152 N151 C154 C153 0.0(4) . . . . ? C151 N151 C154 C153 179.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.599 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.076 #====END data_3 _database_code_depnum_ccdc_archive 'CCDC 897817' #TrackingRef 'CE-ART-08-2012-026338.cif' _audit_creation_date 2012-09-17 _audit_creation_method SHELXL-97 _publ_section_references ; Rigaku Americas and Rigaku Corporation. (2007). CrystalStructure (Version 3.8). Single Crystal Structure Analysis Software. Rigaku Americas, 9009 TX, USA 77381-5209. Rigaku, Tokyo 196-8666, Japan. Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M., Polidori, G., and Camalli, M. (1994) J. Appl. Cryst., 27, 435. SIR92 Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. SHELX97 ; _chemical_name_systematic ; [Co2(B1)(L2)2]-13(H2O) ; _chemical_name_common (Co2(B1)(L2)2)-13(H2O) _chemical_melting_point ? _chemical_formula_moiety 'C56 H78 Co2 N14 O21' _chemical_formula_sum 'C56 H78 Co2 N14 O21' _chemical_formula_weight 1401.18 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' Co Co 0.3494 0.9721 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.543(2) _cell_length_b 12.338(3) _cell_length_c 40.267(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.395(7) _cell_angle_gamma 90.00 _cell_volume 6385(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200 _cell_measurement_reflns_used 33097 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2936 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9308 _exptl_special_details ; ? ; _diffrn_ambient_temperature 200 _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; MicroMax-007HF microfocus rotating anode X-ray generator ; _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 42950 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11223 _reflns_number_gt 8357 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0872P)^2^+8.8322P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11223 _refine_ls_number_parameters 932 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1751 _refine_ls_wR_factor_gt 0.1592 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 0.32068(4) 0.38794(4) 0.193177(12) 0.03629(16) Uani 1 1 d . . . Co2 Co 0.12711(4) 0.40886(5) 0.420643(13) 0.04635(18) Uani 1 1 d . . . O1 O 0.0606(2) 0.5331(2) 0.44687(6) 0.0456(7) Uani 1 1 d . . . O2 O 0.0793(2) 0.5954(2) 0.50098(7) 0.0494(7) Uani 1 1 d . . . O3 O 0.2232(3) 0.2663(3) 0.42180(7) 0.0666(9) Uani 1 1 d . . . O4 O 0.3278(4) 0.1494(4) 0.45861(10) 0.1125(18) Uani 1 1 d . . . O5 O 0.26125(19) 0.2723(2) 0.69500(6) 0.0393(6) Uani 1 1 d . . . O6 O 0.2028(2) 0.4212(2) 0.66280(7) 0.0424(6) Uani 1 1 d . . . O7 O 0.3650(2) -0.0206(2) 0.66371(7) 0.0464(7) Uani 1 1 d . . . O8 O 0.4022(3) -0.0527(3) 0.61430(8) 0.0625(8) Uani 1 1 d . . . O9 O 0.3445(3) 0.0902(3) 0.25338(9) 0.0645(9) Uani 1 1 d . . . O10 O 0.0070(3) 0.7483(4) 0.41998(13) 0.1036(14) Uani 1 1 d . . . O11 O 0.2559(3) 0.1530(5) 0.36510(10) 0.1152(18) Uani 1 1 d . . . O12 O -0.0012(5) 0.1779(5) 0.50964(17) 0.140(2) Uani 1 1 d . . . O13 O 0.4163(6) 0.1597(6) 0.32753(18) 0.095(3) Uani 0.649(13) 1 d P . . O13B O 0.4715(10) 0.1730(9) 0.3082(4) 0.090(6) Uani 0.351(13) 1 d P . . O14 O 0.1570(6) 0.9087(6) 0.4234(2) 0.192(3) Uani 1 1 d . . . O15 O 0.8652(13) 0.0025(15) 0.5054(10) 0.161(9) Uani 0.57(5) 1 d PU . . O15B O 0.8486(18) 0.0216(17) 0.4807(11) 0.152(10) Uani 0.43(5) 1 d PU . . O16 O 0.5059(14) 0.1274(14) 0.5178(8) 0.204(9) Uani 0.64(4) 1 d PU . . O16B O 0.532(3) 0.139(3) 0.4944(14) 0.215(13) Uani 0.36(4) 1 d PU . . O17 O 0.5125(17) 0.4119(15) 0.0776(6) 0.194(10) Uani 0.426(15) 1 d P . . O17B O 0.4963(15) 0.538(2) 0.0635(4) 0.220(10) Uani 0.574(15) 1 d P . . O18 O 0.6839(16) 0.4342(14) 0.1141(4) 0.176(6) Uani 0.512(14) 1 d PU . . O18B O 0.6127(15) 0.4681(15) 0.1237(5) 0.184(7) Uani 0.488(14) 1 d PU . . O19 O 0.6455(18) 0.4448(18) 0.0627(6) 0.228(9) Uani 0.512(14) 1 d PU . . O19B O 0.717(2) 0.487(2) 0.0947(7) 0.241(9) Uani 0.488(14) 1 d PU . . O20 O 0.6450(12) 0.0478(10) 0.4626(4) 0.126(6) Uani 0.426(15) 1 d P . . O20B O 0.6789(14) 0.0461(13) 0.5037(6) 0.222(9) Uani 0.574(15) 1 d P . . O21 O 0.4157(17) 0.2462(19) 0.3663(5) 0.183(11) Uani 0.351(13) 1 d P . . O22 O 0.449(5) 0.625(6) 0.0494(18) 0.09(2) Uani 0.078(17) 1 d PU . . O22B O 0.511(4) 0.697(4) 0.0678(12) 0.121(19) Uani 0.118(14) 1 d PU . . N11 N 0.2904(2) 0.1696(2) 0.64310(8) 0.0371(7) Uani 1 1 d . . . N21 N 0.1772(3) 0.3651(3) 0.47180(8) 0.0471(8) Uani 1 1 d . . . N111 N 0.6451(2) 0.3346(3) 0.21176(10) 0.0479(9) Uani 1 1 d . . . N112 N 0.4775(2) 0.3323(3) 0.20443(8) 0.0368(7) Uani 1 1 d . . . N131 N 0.9456(3) 0.0892(3) 0.32286(9) 0.0467(8) Uani 1 1 d . . . N132 N 0.8286(3) -0.0404(3) 0.31871(8) 0.0454(8) Uani 1 1 d . . . N151 N 0.9688(3) 0.0582(3) 0.17630(9) 0.0509(9) Uani 1 1 d . . . N152 N 0.9107(3) -0.0504(3) 0.13126(8) 0.0464(8) Uani 1 1 d . . . N211 N 0.4653(3) 0.4735(3) 0.29849(8) 0.0424(8) Uani 1 1 d . . . N212 N 0.3606(2) 0.4328(3) 0.24585(8) 0.0405(7) Uani 1 1 d . . . N231 N 0.4189(3) 0.5775(4) 0.43914(9) 0.0572(10) Uani 1 1 d . . . N232 N 0.2615(3) 0.5119(4) 0.43004(9) 0.0534(9) Uani 1 1 d . . . N251 N 0.8345(3) 0.2646(3) 0.41583(9) 0.0530(9) Uani 1 1 d . . . N252 N 0.9886(3) 0.3169(3) 0.41373(8) 0.0474(8) Uani 1 1 d . . . C1 C 0.0899(3) 0.5265(3) 0.48015(10) 0.0407(9) Uani 1 1 d . . . C2 C 0.2647(5) 0.2262(5) 0.45137(12) 0.0721(15) Uani 1 1 d . . . C3 C 0.2359(3) 0.3282(3) 0.66673(9) 0.0357(8) Uani 1 1 d . . . C4 C 0.3634(3) 0.0023(3) 0.63319(11) 0.0480(10) Uani 1 1 d . . . C12 C 0.1472(3) 0.4231(3) 0.49501(10) 0.0418(9) Uani 1 1 d . . . C13 C 0.1718(3) 0.3888(3) 0.52948(9) 0.0425(9) Uani 1 1 d . . . H1 H 0.1499 0.4299 0.5458 0.051 Uiso 1 1 calc R . . C14 C 0.2284(3) 0.2940(4) 0.53993(10) 0.0464(10) Uani 1 1 d . . . C15 C 0.2630(4) 0.2383(4) 0.51510(10) 0.0530(11) Uani 1 1 d . . . H2 H 0.3055 0.1757 0.5216 0.064 Uiso 1 1 calc R . . C16 C 0.2340(4) 0.2764(4) 0.48128(10) 0.0561(12) Uani 1 1 d . . . C22 C 0.2532(3) 0.2700(3) 0.63569(9) 0.0364(8) Uani 1 1 d . . . C23 C 0.2337(3) 0.3143(3) 0.60278(9) 0.0405(9) Uani 1 1 d . . . H3 H 0.2082 0.3863 0.5981 0.049 Uiso 1 1 calc R . . C24 C 0.2525(3) 0.2507(3) 0.57631(9) 0.0446(10) Uani 1 1 d . . . C25 C 0.2940(3) 0.1477(3) 0.58515(10) 0.0462(10) Uani 1 1 d . . . H4 H 0.3093 0.1035 0.5681 0.055 Uiso 1 1 calc R . . C26 C 0.3129(3) 0.1098(3) 0.61875(10) 0.0407(9) Uani 1 1 d . . . C101 C 0.8369(3) 0.3106(3) 0.22868(12) 0.0453(10) Uani 1 1 d . . . C102 C 0.8739(3) 0.2953(3) 0.26478(11) 0.0430(10) Uani 1 1 d . . . C103 C 0.9564(3) 0.2228(3) 0.27886(10) 0.0396(9) Uani 1 1 d . . . C104 C 1.0059(3) 0.1726(3) 0.25710(10) 0.0390(9) Uani 1 1 d . . . C105 C 0.9714(3) 0.1949(3) 0.22150(11) 0.0445(10) Uani 1 1 d . . . C106 C 0.8850(3) 0.2601(3) 0.20670(11) 0.0460(10) Uani 1 1 d . . . C111 C 0.7460(3) 0.3849(4) 0.21285(17) 0.0696(15) Uani 1 1 d . . . H5 H 0.7559 0.4526 0.2267 0.083 Uiso 1 1 calc R . . H6 H 0.7438 0.4041 0.1888 0.083 Uiso 1 1 calc R . . C112 C 0.5542(3) 0.3841(3) 0.19781(10) 0.0407(9) Uani 1 1 d . . . H7 H 0.5456 0.4492 0.1846 0.049 Uiso 1 1 calc R . . C113 C 0.5226(3) 0.2453(3) 0.22445(11) 0.0477(10) Uani 1 1 d . . . H8 H 0.4870 0.1933 0.2338 0.057 Uiso 1 1 calc R . . C114 C 0.6262(3) 0.2447(4) 0.22887(14) 0.0591(13) Uani 1 1 d . . . H9 H 0.6757 0.1926 0.2413 0.071 Uiso 1 1 calc R . . C121 C 0.8241(4) 0.3522(4) 0.28854(15) 0.0714(15) Uani 1 1 d . . . H10 H 0.7692 0.4007 0.2747 0.086 Uiso 1 1 calc R . . H11 H 0.8768 0.3945 0.3060 0.086 Uiso 1 1 calc R . . H12 H 0.7939 0.2984 0.3004 0.086 Uiso 1 1 calc R . . C131 C 0.9905(4) 0.1938(4) 0.31748(11) 0.0552(11) Uani 1 1 d . . . H13 H 1.0674 0.1895 0.3265 0.066 Uiso 1 1 calc R . . H14 H 0.9677 0.2511 0.3306 0.066 Uiso 1 1 calc R . . C132 C 0.8484(3) 0.0544(4) 0.30684(11) 0.0530(11) Uani 1 1 d . . . H15 H 0.7989 0.0937 0.2889 0.064 Uiso 1 1 calc R . . C133 C 0.9197(3) -0.0662(4) 0.34453(11) 0.0495(10) Uani 1 1 d . . . H16 H 0.9303 -0.1295 0.3586 0.059 Uiso 1 1 calc R . . C134 C 0.9923(3) 0.0119(4) 0.34696(11) 0.0510(10) Uani 1 1 d . . . H17 H 1.0618 0.0127 0.3624 0.061 Uiso 1 1 calc R . . C141 C 1.0931(4) 0.0943(4) 0.27243(14) 0.0660(13) Uani 1 1 d . . . H18 H 1.1597 0.1327 0.2785 0.079 Uiso 1 1 calc R . . H19 H 1.0916 0.0374 0.2553 0.079 Uiso 1 1 calc R . . H20 H 1.0848 0.0614 0.2935 0.079 Uiso 1 1 calc R . . C151 C 1.0285(4) 0.1470(4) 0.19804(13) 0.0632(14) Uani 1 1 d . . . H21 H 1.0410 0.2045 0.1827 0.076 Uiso 1 1 calc R . . H22 H 1.0970 0.1191 0.2127 0.076 Uiso 1 1 calc R . . C152 C 0.9738(3) 0.0293(4) 0.14487(10) 0.0524(11) Uani 1 1 d . . . H23 H 1.0181 0.0629 0.1337 0.063 Uiso 1 1 calc R . . C153 C 0.8620(4) -0.0748(4) 0.15552(11) 0.0508(10) Uani 1 1 d . . . H24 H 0.8107 -0.1295 0.1530 0.061 Uiso 1 1 calc R . . C154 C 0.8983(4) -0.0090(4) 0.18336(11) 0.0531(11) Uani 1 1 d . . . H25 H 0.8785 -0.0094 0.2040 0.064 Uiso 1 1 calc R . . C161 C 0.8420(5) 0.2747(5) 0.16692(13) 0.0759(15) Uani 1 1 d . . . H26 H 0.8905 0.2429 0.1560 0.091 Uiso 1 1 calc R . . H27 H 0.8335 0.3521 0.1613 0.091 Uiso 1 1 calc R . . H28 H 0.7744 0.2384 0.1580 0.091 Uiso 1 1 calc R . . C201 C 0.5773(3) 0.4808(4) 0.36134(10) 0.0451(10) Uani 1 1 d . . . C202 C 0.5404(3) 0.5444(4) 0.38414(10) 0.0464(10) Uani 1 1 d . . . C203 C 0.5657(3) 0.5135(4) 0.41922(10) 0.0497(11) Uani 1 1 d . . . C204 C 0.6256(3) 0.4212(4) 0.43180(11) 0.0520(11) Uani 1 1 d . . . C205 C 0.6663(3) 0.3609(4) 0.40932(11) 0.0492(10) Uani 1 1 d . . . C206 C 0.6379(3) 0.3885(4) 0.37377(11) 0.0473(10) Uani 1 1 d . . . C211 C 0.5600(3) 0.5179(4) 0.32448(10) 0.0482(10) Uani 1 1 d . . . H29 H 0.5555 0.5980 0.3239 0.058 Uiso 1 1 calc R . . H30 H 0.6212 0.4970 0.3175 0.058 Uiso 1 1 calc R . . C212 C 0.4543(3) 0.4672(3) 0.26423(10) 0.0431(9) Uani 1 1 d . . . H31 H 0.5074 0.4853 0.2544 0.052 Uiso 1 1 calc R . . C213 C 0.3097(3) 0.4177(4) 0.27000(11) 0.0501(11) Uani 1 1 d . . . H32 H 0.2399 0.3932 0.2647 0.060 Uiso 1 1 calc R . . C214 C 0.3727(3) 0.4424(4) 0.30235(11) 0.0539(11) Uani 1 1 d . . . H33 H 0.3562 0.4389 0.3236 0.065 Uiso 1 1 calc R . . C221 C 0.4753(4) 0.6443(4) 0.37072(13) 0.0625(12) Uani 1 1 d . . . H34 H 0.4180 0.6474 0.3806 0.075 Uiso 1 1 calc R . . H35 H 0.4471 0.6411 0.3451 0.075 Uiso 1 1 calc R . . H36 H 0.5188 0.7091 0.3777 0.075 Uiso 1 1 calc R . . C231 C 0.5309(3) 0.5871(5) 0.44357(12) 0.0627(13) Uani 1 1 d . . . H37 H 0.5712 0.5693 0.4681 0.075 Uiso 1 1 calc R . . H38 H 0.5466 0.6632 0.4392 0.075 Uiso 1 1 calc R . . C232 C 0.3594(3) 0.4890(4) 0.43249(10) 0.0548(11) Uani 1 1 d . . . H39 H 0.3839 0.4184 0.4298 0.066 Uiso 1 1 calc R . . C233 C 0.2609(4) 0.6210(5) 0.43547(13) 0.0653(13) Uani 1 1 d . . . H40 H 0.2012 0.6617 0.4353 0.078 Uiso 1 1 calc R . . C234 C 0.3564(4) 0.6631(5) 0.44111(14) 0.0667(13) Uani 1 1 d . . . H41 H 0.3764 0.7368 0.4455 0.080 Uiso 1 1 calc R . . C241 C 0.6436(4) 0.3834(5) 0.46917(12) 0.0692(14) Uani 1 1 d . . . H42 H 0.5932 0.4185 0.4786 0.083 Uiso 1 1 calc R . . H43 H 0.7143 0.4028 0.4836 0.083 Uiso 1 1 calc R . . H44 H 0.6350 0.3046 0.4695 0.083 Uiso 1 1 calc R . . C251 C 0.7344(4) 0.2640(4) 0.42301(13) 0.0608(12) Uani 1 1 d . . . H45 H 0.7485 0.2598 0.4486 0.073 Uiso 1 1 calc R . . H46 H 0.6957 0.1978 0.4126 0.073 Uiso 1 1 calc R . . C252 C 0.9012(3) 0.3462(4) 0.41947(10) 0.0470(10) Uani 1 1 d . . . H47 H 0.8877 0.4178 0.4255 0.056 Uiso 1 1 calc R . . C253 C 0.9772(5) 0.2089(5) 0.40628(16) 0.0776(16) Uani 1 1 d . . . H48 H 1.0272 0.1642 0.4009 0.093 Uiso 1 1 calc R . . C254 C 0.8828(5) 0.1751(5) 0.40769(19) 0.093(2) Uani 1 1 d . . . H49 H 0.8556 0.1035 0.4038 0.112 Uiso 1 1 calc R . . C261 C 0.6737(4) 0.3203(4) 0.34863(12) 0.0647(13) Uani 1 1 d . . . H50 H 0.7403 0.3480 0.3475 0.078 Uiso 1 1 calc R . . H51 H 0.6218 0.3235 0.3253 0.078 Uiso 1 1 calc R . . H52 H 0.6823 0.2450 0.3568 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0323(3) 0.0412(3) 0.0316(3) -0.0057(2) 0.0047(2) 0.0041(2) Co2 0.0421(3) 0.0695(4) 0.0262(3) 0.0043(2) 0.0089(2) 0.0054(3) O1 0.0429(16) 0.0640(18) 0.0285(13) 0.0072(12) 0.0091(12) 0.0022(14) O2 0.0538(18) 0.0556(18) 0.0380(15) -0.0007(13) 0.0133(13) 0.0002(14) O3 0.073(2) 0.093(3) 0.0305(15) 0.0044(15) 0.0117(15) 0.0296(19) O4 0.168(5) 0.116(3) 0.052(2) 0.012(2) 0.032(3) 0.083(4) O5 0.0382(14) 0.0481(15) 0.0303(13) 0.0055(11) 0.0087(11) 0.0009(12) O6 0.0399(15) 0.0460(16) 0.0393(14) 0.0026(12) 0.0097(12) 0.0042(13) O7 0.0516(17) 0.0404(15) 0.0428(16) 0.0037(12) 0.0085(13) -0.0051(13) O8 0.079(2) 0.0513(19) 0.0588(19) -0.0030(15) 0.0233(18) 0.0080(17) O9 0.063(2) 0.066(2) 0.071(2) 0.0190(17) 0.0301(17) 0.0100(16) O10 0.077(3) 0.102(3) 0.122(4) 0.034(3) 0.018(3) 0.001(2) O11 0.091(3) 0.181(5) 0.061(2) -0.029(3) 0.005(2) 0.037(3) O12 0.146(5) 0.111(4) 0.173(6) -0.017(4) 0.063(4) -0.027(4) O13 0.089(5) 0.113(5) 0.070(4) -0.004(4) 0.008(4) 0.030(4) O13B 0.073(8) 0.063(7) 0.108(11) -0.016(6) -0.008(7) 0.005(6) O14 0.180(7) 0.162(6) 0.185(7) 0.046(5) -0.010(5) -0.054(5) O15 0.137(10) 0.146(10) 0.20(2) -0.027(11) 0.055(11) -0.028(8) O15B 0.172(13) 0.122(11) 0.157(19) -0.025(11) 0.046(12) -0.070(9) O16 0.187(12) 0.181(11) 0.228(17) -0.012(11) 0.043(10) 0.017(9) O16B 0.206(18) 0.207(17) 0.22(2) -0.003(15) 0.055(14) -0.023(14) O17 0.24(2) 0.127(14) 0.27(2) -0.030(14) 0.16(2) -0.075(13) O17B 0.200(17) 0.30(3) 0.177(14) -0.040(17) 0.081(13) -0.056(18) O18 0.220(16) 0.155(11) 0.183(12) 0.048(10) 0.106(12) 0.066(11) O18B 0.181(15) 0.190(13) 0.204(14) 0.057(11) 0.094(11) 0.043(11) O19 0.23(2) 0.213(17) 0.24(2) 0.028(15) 0.067(16) -0.020(15) O19B 0.25(2) 0.250(19) 0.24(2) 0.046(17) 0.090(17) -0.062(16) O20 0.157(14) 0.106(9) 0.135(13) 0.005(8) 0.077(11) 0.004(9) O20B 0.241(18) 0.187(14) 0.29(3) -0.006(13) 0.152(17) 0.051(12) O21 0.21(2) 0.20(2) 0.137(16) 0.004(14) 0.047(15) -0.078(17) O22 0.09(2) 0.09(2) 0.10(2) 0.005(10) 0.033(11) 0.006(10) O22B 0.12(2) 0.12(2) 0.12(2) 0.003(9) 0.029(10) 0.007(10) N11 0.0337(17) 0.0387(18) 0.0343(16) 0.0004(13) 0.0041(13) -0.0066(14) N21 0.049(2) 0.061(2) 0.0283(16) 0.0012(15) 0.0092(15) 0.0063(18) N111 0.0293(17) 0.0385(18) 0.073(2) 0.0084(17) 0.0124(16) 0.0000(14) N112 0.0319(16) 0.0404(18) 0.0372(16) -0.0033(13) 0.0096(13) 0.0006(14) N131 0.048(2) 0.053(2) 0.0381(18) -0.0061(15) 0.0120(16) -0.0201(17) N132 0.0385(18) 0.051(2) 0.0415(18) 0.0030(15) 0.0056(15) -0.0112(16) N151 0.045(2) 0.073(2) 0.0414(19) -0.0111(17) 0.0232(16) -0.0055(18) N152 0.0373(18) 0.071(2) 0.0304(16) -0.0068(16) 0.0095(14) 0.0003(17) N211 0.0418(18) 0.053(2) 0.0311(16) -0.0074(14) 0.0099(14) -0.0103(16) N212 0.0372(18) 0.0473(19) 0.0342(16) -0.0071(14) 0.0073(14) -0.0003(15) N231 0.040(2) 0.090(3) 0.042(2) -0.0129(19) 0.0142(16) -0.004(2) N232 0.041(2) 0.081(3) 0.0367(18) 0.0013(18) 0.0100(15) 0.0027(19) N251 0.058(2) 0.050(2) 0.053(2) -0.0011(17) 0.0207(18) -0.0012(18) N252 0.055(2) 0.056(2) 0.0312(17) -0.0004(15) 0.0144(15) 0.0008(17) C1 0.035(2) 0.056(2) 0.0317(19) 0.0041(18) 0.0104(16) -0.0034(18) C2 0.091(4) 0.082(4) 0.041(3) 0.001(2) 0.017(3) 0.029(3) C3 0.0264(18) 0.045(2) 0.0320(19) 0.0044(16) 0.0036(15) -0.0037(16) C4 0.050(3) 0.041(2) 0.048(2) -0.0052(19) 0.008(2) -0.0114(19) C12 0.040(2) 0.053(2) 0.0292(19) 0.0012(17) 0.0062(16) -0.0038(18) C13 0.044(2) 0.053(2) 0.0271(18) 0.0020(17) 0.0063(16) -0.0011(19) C14 0.049(2) 0.057(3) 0.0281(19) -0.0004(18) 0.0049(17) -0.003(2) C15 0.064(3) 0.057(3) 0.035(2) 0.0003(19) 0.011(2) 0.010(2) C16 0.066(3) 0.067(3) 0.030(2) -0.001(2) 0.009(2) 0.016(2) C22 0.0302(19) 0.045(2) 0.0294(18) 0.0012(16) 0.0027(15) -0.0033(16) C23 0.041(2) 0.044(2) 0.0319(19) 0.0033(16) 0.0048(16) 0.0004(17) C24 0.048(2) 0.053(3) 0.0266(19) 0.0008(17) 0.0023(17) -0.0031(19) C25 0.051(2) 0.049(2) 0.033(2) -0.0058(17) 0.0053(18) -0.002(2) C26 0.041(2) 0.038(2) 0.037(2) -0.0043(16) 0.0043(17) -0.0084(17) C101 0.031(2) 0.035(2) 0.071(3) 0.0046(19) 0.0161(19) -0.0039(16) C102 0.036(2) 0.037(2) 0.065(3) -0.0153(19) 0.030(2) -0.0098(17) C103 0.037(2) 0.042(2) 0.042(2) -0.0090(17) 0.0152(17) -0.0124(17) C104 0.0310(19) 0.039(2) 0.047(2) -0.0070(17) 0.0136(17) -0.0015(16) C105 0.035(2) 0.052(2) 0.052(2) -0.0117(19) 0.0209(18) -0.0093(18) C106 0.041(2) 0.050(2) 0.048(2) 0.0016(19) 0.0148(19) -0.0126(19) C111 0.031(2) 0.049(3) 0.125(5) 0.018(3) 0.020(3) 0.001(2) C112 0.038(2) 0.042(2) 0.041(2) 0.0002(17) 0.0092(17) 0.0013(18) C113 0.038(2) 0.043(2) 0.058(3) 0.0068(19) 0.0097(19) -0.0035(18) C114 0.036(2) 0.043(2) 0.092(4) 0.024(2) 0.012(2) 0.0024(19) C121 0.069(3) 0.058(3) 0.106(4) -0.030(3) 0.055(3) -0.012(3) C131 0.060(3) 0.060(3) 0.043(2) -0.007(2) 0.013(2) -0.026(2) C132 0.050(3) 0.058(3) 0.043(2) 0.009(2) 0.004(2) -0.019(2) C133 0.039(2) 0.051(2) 0.054(3) 0.003(2) 0.0085(19) -0.002(2) C134 0.039(2) 0.055(3) 0.054(3) -0.003(2) 0.009(2) -0.001(2) C141 0.047(3) 0.072(3) 0.078(3) 0.005(3) 0.018(2) 0.019(2) C151 0.054(3) 0.088(4) 0.059(3) -0.033(3) 0.034(2) -0.022(3) C152 0.043(2) 0.081(3) 0.035(2) -0.006(2) 0.0149(18) -0.005(2) C153 0.055(3) 0.058(3) 0.043(2) -0.002(2) 0.020(2) -0.003(2) C154 0.064(3) 0.064(3) 0.040(2) -0.008(2) 0.028(2) -0.006(2) C161 0.086(4) 0.084(4) 0.053(3) 0.014(3) 0.014(3) -0.014(3) C201 0.039(2) 0.061(3) 0.034(2) -0.0105(18) 0.0097(17) -0.020(2) C202 0.032(2) 0.065(3) 0.040(2) -0.0103(19) 0.0081(17) -0.0105(19) C203 0.031(2) 0.078(3) 0.039(2) -0.015(2) 0.0104(17) -0.012(2) C204 0.035(2) 0.079(3) 0.039(2) -0.007(2) 0.0079(18) -0.017(2) C205 0.040(2) 0.061(3) 0.046(2) -0.005(2) 0.0133(19) -0.016(2) C206 0.045(2) 0.056(3) 0.043(2) -0.0132(19) 0.0159(19) -0.017(2) C211 0.042(2) 0.064(3) 0.035(2) -0.0082(19) 0.0072(17) -0.019(2) C212 0.045(2) 0.051(2) 0.0329(19) -0.0048(17) 0.0109(17) -0.0066(19) C213 0.036(2) 0.071(3) 0.041(2) -0.011(2) 0.0100(18) -0.014(2) C214 0.044(2) 0.081(3) 0.038(2) -0.007(2) 0.0150(19) -0.015(2) C221 0.053(3) 0.074(3) 0.056(3) -0.011(2) 0.010(2) -0.002(2) C231 0.043(2) 0.096(4) 0.049(3) -0.021(2) 0.015(2) -0.007(2) C232 0.042(2) 0.083(3) 0.039(2) -0.012(2) 0.0124(19) -0.004(2) C233 0.049(3) 0.084(4) 0.068(3) 0.003(3) 0.026(2) 0.005(3) C234 0.056(3) 0.076(3) 0.077(3) -0.007(3) 0.033(3) -0.003(3) C241 0.062(3) 0.105(4) 0.039(2) 0.002(3) 0.013(2) -0.002(3) C251 0.059(3) 0.065(3) 0.062(3) 0.004(2) 0.024(2) -0.009(2) C252 0.050(2) 0.049(2) 0.041(2) -0.0009(18) 0.0143(19) -0.001(2) C253 0.079(4) 0.068(4) 0.097(4) -0.027(3) 0.043(3) 0.001(3) C254 0.092(5) 0.058(3) 0.144(6) -0.035(4) 0.058(4) -0.013(3) C261 0.072(3) 0.071(3) 0.052(3) -0.018(2) 0.022(2) -0.006(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N11 2.053(3) 4_565 ? Co1 N212 2.091(3) . ? Co1 N132 2.118(3) 2_655 ? Co1 N112 2.140(3) . ? Co1 O5 2.144(3) 4_565 ? Co1 O7 2.213(3) 4_565 ? Co2 N21 2.028(3) . ? Co2 N152 2.051(3) 2_655 ? Co2 N252 2.134(4) 1_455 ? Co2 N232 2.154(4) . ? Co2 O3 2.180(3) . ? Co2 O1 2.208(3) . ? O1 C1 1.275(4) . ? O2 C1 1.233(5) . ? O3 C2 1.247(6) . ? O4 C2 1.247(6) . ? O5 C3 1.282(4) . ? O5 Co1 2.144(3) 4_566 ? O6 C3 1.224(5) . ? O7 C4 1.254(5) . ? O7 Co1 2.213(3) 4_566 ? O8 C4 1.252(5) . ? O13 O13B 1.250(16) . ? O15 O15B 0.978(19) . ? O16 O16B 1.12(3) . ? O17 O17B 1.65(3) . ? O17B O22 1.29(6) . ? O18 O19B 1.21(2) . ? O18 O18B 1.220(18) . ? O19 O19B 1.44(3) . ? O20 O22 1.54(7) 2_645 ? O20 O20B 1.57(2) . ? O22 O22B 1.28(8) . ? O22 O20 1.54(7) 2_655 ? N11 C22 1.335(5) . ? N11 C26 1.337(5) . ? N11 Co1 2.053(3) 4_566 ? N21 C16 1.323(6) . ? N21 C12 1.337(5) . ? N111 C112 1.329(5) . ? N111 C114 1.372(5) . ? N111 C111 1.488(5) . ? N112 C112 1.317(5) . ? N112 C113 1.365(5) . ? N131 C132 1.341(5) . ? N131 C134 1.365(6) . ? N131 C131 1.472(5) . ? N132 C132 1.322(5) . ? N132 C133 1.377(5) . ? N132 Co1 2.118(3) 2_645 ? N151 C152 1.337(5) . ? N151 C154 1.361(6) . ? N151 C151 1.474(6) . ? N152 C152 1.304(6) . ? N152 C153 1.374(5) . ? N152 Co2 2.051(3) 2_645 ? N211 C212 1.342(5) . ? N211 C214 1.366(5) . ? N211 C211 1.480(5) . ? N212 C212 1.322(5) . ? N212 C213 1.371(5) . ? N231 C232 1.333(6) . ? N231 C234 1.371(6) . ? N231 C231 1.476(6) . ? N232 C232 1.328(5) . ? N232 C233 1.364(7) . ? N251 C252 1.330(5) . ? N251 C254 1.375(7) . ? N251 C251 1.472(6) . ? N252 C252 1.326(5) . ? N252 C253 1.363(6) . ? N252 Co2 2.134(4) 1_655 ? C1 C12 1.516(6) . ? C2 C16 1.524(6) . ? C3 C22 1.522(5) . ? C4 C26 1.520(6) . ? C12 C13 1.388(5) . ? C13 C14 1.388(6) . ? C13 H1 0.9500 . ? C14 C15 1.410(6) . ? C14 C24 1.495(5) . ? C15 C16 1.376(6) . ? C15 H2 0.9500 . ? C22 C23 1.380(5) . ? C23 C24 1.410(6) . ? C23 H3 0.9500 . ? C24 C25 1.390(6) . ? C25 C26 1.377(5) . ? C25 H4 0.9500 . ? C101 C102 1.393(6) . ? C101 C106 1.400(6) . ? C101 C111 1.506(6) . ? C102 C103 1.404(6) . ? C102 C121 1.507(6) . ? C103 C104 1.404(5) . ? C103 C131 1.518(6) . ? C104 C105 1.388(6) . ? C104 C141 1.500(6) . ? C105 C106 1.389(6) . ? C105 C151 1.518(5) . ? C106 C161 1.532(6) . ? C111 H5 0.9900 . ? C111 H6 0.9900 . ? C112 H7 0.9500 . ? C113 C114 1.358(6) . ? C113 H8 0.9500 . ? C114 H9 0.9500 . ? C121 H10 0.9800 . ? C121 H11 0.9800 . ? C121 H12 0.9800 . ? C131 H13 0.9900 . ? C131 H14 0.9900 . ? C132 H15 0.9500 . ? C133 C134 1.358(6) . ? C133 H16 0.9500 . ? C134 H17 0.9500 . ? C141 H18 0.9800 . ? C141 H19 0.9800 . ? C141 H20 0.9800 . ? C151 H21 0.9900 . ? C151 H22 0.9900 . ? C152 H23 0.9500 . ? C153 C154 1.346(6) . ? C153 H24 0.9500 . ? C154 H25 0.9500 . ? C161 H26 0.9800 . ? C161 H27 0.9800 . ? C161 H28 0.9800 . ? C201 C206 1.401(6) . ? C201 C202 1.414(6) . ? C201 C211 1.499(5) . ? C202 C203 1.397(6) . ? C202 C221 1.511(7) . ? C203 C204 1.397(7) . ? C203 C231 1.517(6) . ? C204 C205 1.412(6) . ? C204 C241 1.520(6) . ? C205 C206 1.402(6) . ? C205 C251 1.504(7) . ? C206 C261 1.509(6) . ? C211 H29 0.9900 . ? C211 H30 0.9900 . ? C212 H31 0.9500 . ? C213 C214 1.348(6) . ? C213 H32 0.9500 . ? C214 H33 0.9500 . ? C221 H34 0.9800 . ? C221 H35 0.9800 . ? C221 H36 0.9800 . ? C231 H37 0.9900 . ? C231 H38 0.9900 . ? C232 H39 0.9500 . ? C233 C234 1.344(7) . ? C233 H40 0.9500 . ? C234 H41 0.9500 . ? C241 H42 0.9800 . ? C241 H43 0.9800 . ? C241 H44 0.9800 . ? C251 H45 0.9900 . ? C251 H46 0.9900 . ? C252 H47 0.9500 . ? C253 C254 1.363(8) . ? C253 H48 0.9500 . ? C254 H49 0.9500 . ? C261 H50 0.9800 . ? C261 H51 0.9800 . ? C261 H52 0.9800 . ? 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 N11 Co1 N212 174.32(12) 4_565 . ? N11 Co1 N132 92.38(12) 4_565 2_655 ? N212 Co1 N132 92.37(12) . 2_655 ? N11 Co1 N112 88.55(12) 4_565 . ? N212 Co1 N112 87.06(12) . . ? N132 Co1 N112 173.89(13) 2_655 . ? N11 Co1 O5 75.76(11) 4_565 4_565 ? N212 Co1 O5 100.89(11) . 4_565 ? N132 Co1 O5 92.91(12) 2_655 4_565 ? N112 Co1 O5 93.17(11) . 4_565 ? N11 Co1 O7 74.52(11) 4_565 4_565 ? N212 Co1 O7 108.73(12) . 4_565 ? N132 Co1 O7 88.35(12) 2_655 4_565 ? N112 Co1 O7 86.07(11) . 4_565 ? O5 Co1 O7 150.28(10) 4_565 4_565 ? N21 Co2 N152 174.93(14) . 2_655 ? N21 Co2 N252 89.40(14) . 1_455 ? N152 Co2 N252 94.07(13) 2_655 1_455 ? N21 Co2 N232 89.15(14) . . ? N152 Co2 N232 87.68(13) 2_655 . ? N252 Co2 N232 175.01(14) 1_455 . ? N21 Co2 O3 75.96(12) . . ? N152 Co2 O3 100.08(13) 2_655 . ? N252 Co2 O3 93.89(14) 1_455 . ? N232 Co2 O3 90.39(15) . . ? N21 Co2 O1 75.82(12) . . ? N152 Co2 O1 107.98(12) 2_655 . ? N252 Co2 O1 87.53(12) 1_455 . ? N232 Co2 O1 87.49(13) . . ? O3 Co2 O1 151.73(10) . . ? C1 O1 Co2 114.9(3) . . ? C2 O3 Co2 115.2(3) . . ? C3 O5 Co1 117.6(2) . 4_566 ? C4 O7 Co1 115.8(3) . 4_566 ? O22 O17B O17 159(4) . . ? O19B O18 O18B 121(2) . . ? O18 O19B O19 96(2) . . ? O22 O20 O20B 106(3) 2_645 . ? O22B O22 O17B 100(5) . . ? O22B O22 O20 159(6) . 2_655 ? O17B O22 O20 83(4) . 2_655 ? C22 N11 C26 120.4(3) . . ? C22 N11 Co1 119.0(2) . 4_566 ? C26 N11 Co1 120.5(3) . 4_566 ? C16 N21 C12 121.2(3) . . ? C16 N21 Co2 119.4(3) . . ? C12 N21 Co2 119.3(3) . . ? C112 N111 C114 106.8(3) . . ? C112 N111 C111 122.7(3) . . ? C114 N111 C111 129.6(4) . . ? C112 N112 C113 105.5(3) . . ? C112 N112 Co1 126.5(3) . . ? C113 N112 Co1 127.3(3) . . ? C132 N131 C134 106.4(3) . . ? C132 N131 C131 126.8(4) . . ? C134 N131 C131 126.6(4) . . ? C132 N132 C133 104.0(3) . . ? C132 N132 Co1 125.1(3) . 2_645 ? C133 N132 Co1 129.7(3) . 2_645 ? C152 N151 C154 106.5(4) . . ? C152 N151 C151 125.3(4) . . ? C154 N151 C151 128.2(3) . . ? C152 N152 C153 105.4(3) . . ? C152 N152 Co2 122.2(3) . 2_645 ? C153 N152 Co2 130.5(3) . 2_645 ? C212 N211 C214 107.0(3) . . ? C212 N211 C211 122.6(3) . . ? C214 N211 C211 130.1(3) . . ? C212 N212 C213 104.8(3) . . ? C212 N212 Co1 123.2(3) . . ? C213 N212 Co1 131.0(3) . . ? C232 N231 C234 107.3(4) . . ? C232 N231 C231 128.5(4) . . ? C234 N231 C231 124.1(4) . . ? C232 N232 C233 104.8(4) . . ? C232 N232 Co2 131.0(4) . . ? C233 N232 Co2 124.3(3) . . ? C252 N251 C254 106.0(4) . . ? C252 N251 C251 128.1(4) . . ? C254 N251 C251 125.4(4) . . ? C252 N252 C253 105.0(4) . . ? C252 N252 Co2 129.0(3) . 1_655 ? C253 N252 Co2 125.6(3) . 1_655 ? O2 C1 O1 127.4(4) . . ? O2 C1 C12 117.8(3) . . ? O1 C1 C12 114.8(3) . . ? O3 C2 O4 126.4(5) . . ? O3 C2 C16 116.1(4) . . ? O4 C2 C16 117.5(4) . . ? O6 C3 O5 127.1(4) . . ? O6 C3 C22 118.8(3) . . ? O5 C3 C22 114.1(3) . . ? O8 C4 O7 126.3(4) . . ? O8 C4 C26 117.7(4) . . ? O7 C4 C26 116.0(4) . . ? N21 C12 C13 120.4(4) . . ? N21 C12 C1 113.9(3) . . ? C13 C12 C1 125.6(4) . . ? C12 C13 C14 119.7(4) . . ? C12 C13 H1 120.2 . . ? C14 C13 H1 120.2 . . ? C13 C14 C15 118.1(4) . . ? C13 C14 C24 121.8(4) . . ? C15 C14 C24 120.1(4) . . ? C16 C15 C14 118.8(4) . . ? C16 C15 H2 120.6 . . ? C14 C15 H2 120.6 . . ? N21 C16 C15 121.8(4) . . ? N21 C16 C2 112.8(4) . . ? C15 C16 C2 125.5(4) . . ? N11 C22 C23 121.8(3) . . ? N11 C22 C3 113.5(3) . . ? C23 C22 C3 124.7(4) . . ? C22 C23 C24 118.7(4) . . ? C22 C23 H3 120.7 . . ? C24 C23 H3 120.7 . . ? C25 C24 C23 118.0(4) . . ? C25 C24 C14 121.6(4) . . ? C23 C24 C14 120.4(4) . . ? C26 C25 C24 119.8(4) . . ? C26 C25 H4 120.1 . . ? C24 C25 H4 120.1 . . ? N11 C26 C25 121.2(4) . . ? N11 C26 C4 112.3(3) . . ? C25 C26 C4 126.4(4) . . ? C102 C101 C106 120.9(4) . . ? C102 C101 C111 120.0(4) . . ? C106 C101 C111 119.0(4) . . ? C101 C102 C103 119.1(3) . . ? C101 C102 C121 120.9(4) . . ? C103 C102 C121 119.9(4) . . ? C104 C103 C102 120.3(4) . . ? C104 C103 C131 119.0(4) . . ? C102 C103 C131 120.6(4) . . ? C105 C104 C103 119.1(4) . . ? C105 C104 C141 121.2(4) . . ? C103 C104 C141 119.7(4) . . ? C104 C105 C106 121.4(4) . . ? C104 C105 C151 119.6(4) . . ? C106 C105 C151 119.0(4) . . ? C105 C106 C101 118.9(4) . . ? C105 C106 C161 120.5(4) . . ? C101 C106 C161 120.6(4) . . ? N111 C111 C101 112.3(4) . . ? N111 C111 H5 109.1 . . ? C101 C111 H5 109.1 . . ? N111 C111 H6 109.1 . . ? C101 C111 H6 109.1 . . ? H5 C111 H6 107.9 . . ? N112 C112 N111 112.1(3) . . ? N112 C112 H7 124.0 . . ? N111 C112 H7 124.0 . . ? C114 C113 N112 109.4(4) . . ? C114 C113 H8 125.3 . . ? N112 C113 H8 125.3 . . ? C113 C114 N111 106.2(4) . . ? C113 C114 H9 126.9 . . ? N111 C114 H9 126.9 . . ? C102 C121 H10 109.5 . . ? C102 C121 H11 109.5 . . ? H10 C121 H11 109.5 . . ? C102 C121 H12 109.5 . . ? H10 C121 H12 109.5 . . ? H11 C121 H12 109.5 . . ? N131 C131 C103 110.5(3) . . ? N131 C131 H13 109.5 . . ? C103 C131 H13 109.5 . . ? N131 C131 H14 109.5 . . ? C103 C131 H14 109.5 . . ? H13 C131 H14 108.1 . . ? N132 C132 N131 112.9(4) . . ? N132 C132 H15 123.6 . . ? N131 C132 H15 123.6 . . ? C134 C133 N132 110.3(4) . . ? C134 C133 H16 124.9 . . ? N132 C133 H16 124.9 . . ? C133 C134 N131 106.4(4) . . ? C133 C134 H17 126.8 . . ? N131 C134 H17 126.8 . . ? C104 C141 H18 109.5 . . ? C104 C141 H19 109.5 . . ? H18 C141 H19 109.5 . . ? C104 C141 H20 109.5 . . ? H18 C141 H20 109.5 . . ? H19 C141 H20 109.5 . . ? N151 C151 C105 111.5(3) . . ? N151 C151 H21 109.3 . . ? C105 C151 H21 109.3 . . ? N151 C151 H22 109.3 . . ? C105 C151 H22 109.3 . . ? H21 C151 H22 108.0 . . ? N152 C152 N151 112.1(4) . . ? N152 C152 H23 123.9 . . ? N151 C152 H23 123.9 . . ? C154 C153 N152 109.2(4) . . ? C154 C153 H24 125.4 . . ? N152 C153 H24 125.4 . . ? C153 C154 N151 106.9(4) . . ? C153 C154 H25 126.6 . . ? N151 C154 H25 126.6 . . ? C106 C161 H26 109.5 . . ? C106 C161 H27 109.5 . . ? H26 C161 H27 109.5 . . ? C106 C161 H28 109.5 . . ? H26 C161 H28 109.5 . . ? H27 C161 H28 109.5 . . ? C206 C201 C202 120.5(4) . . ? C206 C201 C211 119.5(4) . . ? C202 C201 C211 119.8(4) . . ? C203 C202 C201 118.7(4) . . ? C203 C202 C221 120.9(4) . . ? C201 C202 C221 120.4(4) . . ? C204 C203 C202 121.2(4) . . ? C204 C203 C231 121.1(4) . . ? C202 C203 C231 117.5(4) . . ? C203 C204 C205 119.8(4) . . ? C203 C204 C241 120.2(4) . . ? C205 C204 C241 120.0(5) . . ? C206 C205 C204 119.3(4) . . ? C206 C205 C251 120.4(4) . . ? C204 C205 C251 120.2(4) . . ? C201 C206 C205 120.2(4) . . ? C201 C206 C261 119.3(4) . . ? C205 C206 C261 120.4(4) . . ? N211 C211 C201 114.7(3) . . ? N211 C211 H29 108.6 . . ? C201 C211 H29 108.6 . . ? N211 C211 H30 108.6 . . ? C201 C211 H30 108.6 . . ? H29 C211 H30 107.6 . . ? N212 C212 N211 111.7(3) . . ? N212 C212 H31 124.2 . . ? N211 C212 H31 124.2 . . ? C214 C213 N212 110.3(4) . . ? C214 C213 H32 124.8 . . ? N212 C213 H32 124.8 . . ? C213 C214 N211 106.1(4) . . ? C213 C214 H33 126.9 . . ? N211 C214 H33 126.9 . . ? C202 C221 H34 109.5 . . ? C202 C221 H35 109.5 . . ? H34 C221 H35 109.5 . . ? C202 C221 H36 109.5 . . ? H34 C221 H36 109.5 . . ? H35 C221 H36 109.5 . . ? N231 C231 C203 113.0(4) . . ? N231 C231 H37 109.0 . . ? C203 C231 H37 109.0 . . ? N231 C231 H38 109.0 . . ? C203 C231 H38 109.0 . . ? H37 C231 H38 107.8 . . ? N232 C232 N231 111.4(5) . . ? N232 C232 H39 124.3 . . ? N231 C232 H39 124.3 . . ? C234 C233 N232 110.7(5) . . ? C234 C233 H40 124.6 . . ? N232 C233 H40 124.6 . . ? C233 C234 N231 105.7(5) . . ? C233 C234 H41 127.1 . . ? N231 C234 H41 127.1 . . ? C204 C241 H42 109.5 . . ? C204 C241 H43 109.5 . . ? H42 C241 H43 109.5 . . ? C204 C241 H44 109.5 . . ? H42 C241 H44 109.5 . . ? H43 C241 H44 109.5 . . ? N251 C251 C205 114.9(4) . . ? N251 C251 H45 108.5 . . ? C205 C251 H45 108.5 . . ? N251 C251 H46 108.5 . . ? C205 C251 H46 108.5 . . ? H45 C251 H46 107.5 . . ? N252 C252 N251 112.8(4) . . ? N252 C252 H47 123.6 . . ? N251 C252 H47 123.6 . . ? C254 C253 N252 109.5(5) . . ? C254 C253 H48 125.2 . . ? N252 C253 H48 125.2 . . ? C253 C254 N251 106.6(5) . . ? C253 C254 H49 126.7 . . ? N251 C254 H49 126.7 . . ? C206 C261 H50 109.5 . . ? C206 C261 H51 109.5 . . ? H50 C261 H51 109.5 . . ? C206 C261 H52 109.5 . . ? H50 C261 H52 109.5 . . ? H51 C261 H52 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 N21 Co2 O1 C1 5.7(3) . . . . ? N152 Co2 O1 C1 -170.8(3) 2_655 . . . ? N252 Co2 O1 C1 95.7(3) 1_455 . . . ? N232 Co2 O1 C1 -84.0(3) . . . . ? O3 Co2 O1 C1 2.1(4) . . . . ? N21 Co2 O3 C2 -1.4(4) . . . . ? N152 Co2 O3 C2 175.3(4) 2_655 . . . ? N252 Co2 O3 C2 -89.8(4) 1_455 . . . ? N232 Co2 O3 C2 87.6(4) . . . . ? O1 Co2 O3 C2 2.2(6) . . . . ? O18B O18 O19B O19 -89(3) . . . . ? O17 O17B O22 O22B 147(7) . . . . ? O17 O17B O22 O20 -12(11) . . . 2_655 ? N152 Co2 N21 C16 -42.7(19) 2_655 . . . ? N252 Co2 N21 C16 90.6(4) 1_455 . . . ? N232 Co2 N21 C16 -94.2(4) . . . . ? O3 Co2 N21 C16 -3.5(4) . . . . ? O1 Co2 N21 C16 178.2(4) . . . . ? N152 Co2 N21 C12 141.1(16) 2_655 . . . ? N252 Co2 N21 C12 -85.6(3) 1_455 . . . ? N232 Co2 N21 C12 89.7(3) . . . . ? O3 Co2 N21 C12 -179.7(3) . . . . ? O1 Co2 N21 C12 2.0(3) . . . . ? N11 Co1 N112 C112 83.6(3) 4_565 . . . ? N212 Co1 N112 C112 -100.0(3) . . . . ? N132 Co1 N112 C112 -15.3(13) 2_655 . . . ? O5 Co1 N112 C112 159.2(3) 4_565 . . . ? O7 Co1 N112 C112 9.0(3) 4_565 . . . ? N11 Co1 N112 C113 -107.3(3) 4_565 . . . ? N212 Co1 N112 C113 69.1(3) . . . . ? N132 Co1 N112 C113 153.8(10) 2_655 . . . ? O5 Co1 N112 C113 -31.7(3) 4_565 . . . ? O7 Co1 N112 C113 178.1(3) 4_565 . . . ? N11 Co1 N212 C212 72.3(14) 4_565 . . . ? N132 Co1 N212 C212 -141.0(3) 2_655 . . . ? N112 Co1 N212 C212 32.9(3) . . . . ? O5 Co1 N212 C212 125.6(3) 4_565 . . . ? O7 Co1 N212 C212 -51.9(3) 4_565 . . . ? N11 Co1 N212 C213 -95.1(13) 4_565 . . . ? N132 Co1 N212 C213 51.6(4) 2_655 . . . ? N112 Co1 N212 C213 -134.5(4) . . . . ? O5 Co1 N212 C213 -41.8(4) 4_565 . . . ? O7 Co1 N212 C213 140.7(4) 4_565 . . . ? N21 Co2 N232 C232 80.2(4) . . . . ? N152 Co2 N232 C232 -95.8(4) 2_655 . . . ? N252 Co2 N232 C232 153.4(14) 1_455 . . . ? O3 Co2 N232 C232 4.2(4) . . . . ? O1 Co2 N232 C232 156.0(4) . . . . ? N21 Co2 N232 C233 -98.7(4) . . . . ? N152 Co2 N232 C233 85.3(4) 2_655 . . . ? N252 Co2 N232 C233 -25.5(17) 1_455 . . . ? O3 Co2 N232 C233 -174.7(4) . . . . ? O1 Co2 N232 C233 -22.9(4) . . . . ? Co2 O1 C1 O2 166.2(3) . . . . ? Co2 O1 C1 C12 -11.4(4) . . . . ? Co2 O3 C2 O4 -175.0(6) . . . . ? Co2 O3 C2 C16 5.4(7) . . . . ? Co1 O5 C3 O6 -178.4(3) 4_566 . . . ? Co1 O5 C3 C22 -0.3(4) 4_566 . . . ? Co1 O7 C4 O8 166.7(3) 4_566 . . . ? Co1 O7 C4 C26 -10.7(4) 4_566 . . . ? C16 N21 C12 C13 -2.6(6) . . . . ? Co2 N21 C12 C13 173.5(3) . . . . ? C16 N21 C12 C1 175.6(4) . . . . ? Co2 N21 C12 C1 -8.3(5) . . . . ? O2 C1 C12 N21 -164.7(4) . . . . ? O1 C1 C12 N21 13.1(5) . . . . ? O2 C1 C12 C13 13.3(6) . . . . ? O1 C1 C12 C13 -168.8(4) . . . . ? N21 C12 C13 C14 0.5(6) . . . . ? C1 C12 C13 C14 -177.5(4) . . . . ? C12 C13 C14 C15 2.7(6) . . . . ? C12 C13 C14 C24 -177.1(4) . . . . ? C13 C14 C15 C16 -3.8(7) . . . . ? C24 C14 C15 C16 175.9(4) . . . . ? C12 N21 C16 C15 1.4(7) . . . . ? Co2 N21 C16 C15 -174.7(4) . . . . ? C12 N21 C16 C2 -176.8(4) . . . . ? Co2 N21 C16 C2 7.1(6) . . . . ? C14 C15 C16 N21 1.9(7) . . . . ? C14 C15 C16 C2 179.8(5) . . . . ? O3 C2 C16 N21 -8.2(7) . . . . ? O4 C2 C16 N21 172.1(6) . . . . ? O3 C2 C16 C15 173.7(5) . . . . ? O4 C2 C16 C15 -5.9(9) . . . . ? C26 N11 C22 C23 2.1(5) . . . . ? Co1 N11 C22 C23 178.4(3) 4_566 . . . ? C26 N11 C22 C3 -177.7(3) . . . . ? Co1 N11 C22 C3 -1.4(4) 4_566 . . . ? O6 C3 C22 N11 179.4(3) . . . . ? O5 C3 C22 N11 1.1(4) . . . . ? O6 C3 C22 C23 -0.4(5) . . . . ? O5 C3 C22 C23 -178.7(3) . . . . ? N11 C22 C23 C24 0.8(6) . . . . ? C3 C22 C23 C24 -179.5(3) . . . . ? C22 C23 C24 C25 -2.6(6) . . . . ? C22 C23 C24 C14 177.5(3) . . . . ? C13 C14 C24 C25 169.3(4) . . . . ? C15 C14 C24 C25 -10.4(6) . . . . ? C13 C14 C24 C23 -10.8(6) . . . . ? C15 C14 C24 C23 169.4(4) . . . . ? C23 C24 C25 C26 1.6(6) . . . . ? C14 C24 C25 C26 -178.5(4) . . . . ? C22 N11 C26 C25 -3.1(6) . . . . ? Co1 N11 C26 C25 -179.3(3) 4_566 . . . ? C22 N11 C26 C4 174.7(3) . . . . ? Co1 N11 C26 C4 -1.5(4) 4_566 . . . ? C24 C25 C26 N11 1.2(6) . . . . ? C24 C25 C26 C4 -176.3(4) . . . . ? O8 C4 C26 N11 -169.3(4) . . . . ? O7 C4 C26 N11 8.3(5) . . . . ? O8 C4 C26 C25 8.4(6) . . . . ? O7 C4 C26 C25 -174.0(4) . . . . ? C106 C101 C102 C103 -4.0(6) . . . . ? C111 C101 C102 C103 177.8(3) . . . . ? C106 C101 C102 C121 178.2(4) . . . . ? C111 C101 C102 C121 0.1(6) . . . . ? C101 C102 C103 C104 4.7(5) . . . . ? C121 C102 C103 C104 -177.5(4) . . . . ? C101 C102 C103 C131 -172.8(3) . . . . ? C121 C102 C103 C131 5.0(5) . . . . ? C102 C103 C104 C105 -0.7(5) . . . . ? C131 C103 C104 C105 176.8(3) . . . . ? C102 C103 C104 C141 -179.2(4) . . . . ? C131 C103 C104 C141 -1.7(6) . . . . ? C103 C104 C105 C106 -4.1(6) . . . . ? C141 C104 C105 C106 174.4(4) . . . . ? C103 C104 C105 C151 176.1(4) . . . . ? C141 C104 C105 C151 -5.4(6) . . . . ? C104 C105 C106 C101 4.8(6) . . . . ? C151 C105 C106 C101 -175.4(4) . . . . ? C104 C105 C106 C161 -174.1(4) . . . . ? C151 C105 C106 C161 5.7(6) . . . . ? C102 C101 C106 C105 -0.6(6) . . . . ? C111 C101 C106 C105 177.5(4) . . . . ? C102 C101 C106 C161 178.2(4) . . . . ? C111 C101 C106 C161 -3.6(6) . . . . ? C112 N111 C111 C101 -177.7(4) . . . . ? C114 N111 C111 C101 14.9(8) . . . . ? C102 C101 C111 N111 -76.2(6) . . . . ? C106 C101 C111 N111 105.6(5) . . . . ? C113 N112 C112 N111 1.2(5) . . . . ? Co1 N112 C112 N111 172.2(3) . . . . ? C114 N111 C112 N112 -0.5(5) . . . . ? C111 N111 C112 N112 -170.3(4) . . . . ? C112 N112 C113 C114 -1.5(5) . . . . ? Co1 N112 C113 C114 -172.4(3) . . . . ? N112 C113 C114 N111 1.2(5) . . . . ? C112 N111 C114 C113 -0.5(5) . . . . ? C111 N111 C114 C113 168.5(5) . . . . ? C132 N131 C131 C103 -41.4(6) . . . . ? C134 N131 C131 C103 143.8(4) . . . . ? C104 C103 C131 N131 -78.5(5) . . . . ? C102 C103 C131 N131 99.0(4) . . . . ? C133 N132 C132 N131 1.1(5) . . . . ? Co1 N132 C132 N131 169.4(3) 2_645 . . . ? C134 N131 C132 N132 -0.3(5) . . . . ? C131 N131 C132 N132 -175.9(4) . . . . ? C132 N132 C133 C134 -1.4(5) . . . . ? Co1 N132 C133 C134 -169.0(3) 2_645 . . . ? N132 C133 C134 N131 1.3(5) . . . . ? C132 N131 C134 C133 -0.6(5) . . . . ? C131 N131 C134 C133 175.0(4) . . . . ? C152 N151 C151 C105 151.8(4) . . . . ? C154 N151 C151 C105 -27.4(7) . . . . ? C104 C105 C151 N151 106.4(5) . . . . ? C106 C105 C151 N151 -73.4(6) . . . . ? C153 N152 C152 N151 -0.2(5) . . . . ? Co2 N152 C152 N151 165.3(3) 2_645 . . . ? C154 N151 C152 N152 0.8(5) . . . . ? C151 N151 C152 N152 -178.5(4) . . . . ? C152 N152 C153 C154 -0.5(5) . . . . ? Co2 N152 C153 C154 -164.4(3) 2_645 . . . ? N152 C153 C154 N151 1.0(5) . . . . ? C152 N151 C154 C153 -1.1(5) . . . . ? C151 N151 C154 C153 178.2(5) . . . . ? C206 C201 C202 C203 0.2(6) . . . . ? C211 C201 C202 C203 -174.2(3) . . . . ? C206 C201 C202 C221 179.8(4) . . . . ? C211 C201 C202 C221 5.4(6) . . . . ? C201 C202 C203 C204 -0.6(6) . . . . ? C221 C202 C203 C204 179.8(4) . . . . ? C201 C202 C203 C231 176.2(4) . . . . ? C221 C202 C203 C231 -3.4(6) . . . . ? C202 C203 C204 C205 3.6(6) . . . . ? C231 C203 C204 C205 -173.1(4) . . . . ? C202 C203 C204 C241 -174.3(4) . . . . ? C231 C203 C204 C241 9.1(6) . . . . ? C203 C204 C205 C206 -6.1(6) . . . . ? C241 C204 C205 C206 171.7(4) . . . . ? C203 C204 C205 C251 177.5(4) . . . . ? C241 C204 C205 C251 -4.7(6) . . . . ? C202 C201 C206 C205 -2.8(6) . . . . ? C211 C201 C206 C205 171.6(3) . . . . ? C202 C201 C206 C261 178.3(4) . . . . ? C211 C201 C206 C261 -7.3(6) . . . . ? C204 C205 C206 C201 5.7(6) . . . . ? C251 C205 C206 C201 -177.8(4) . . . . ? C204 C205 C206 C261 -175.4(4) . . . . ? C251 C205 C206 C261 1.0(6) . . . . ? C212 N211 C211 C201 -157.4(4) . . . . ? C214 N211 C211 C201 29.5(7) . . . . ? C206 C201 C211 N211 91.8(5) . . . . ? C202 C201 C211 N211 -93.8(5) . . . . ? C213 N212 C212 N211 0.6(5) . . . . ? Co1 N212 C212 N211 -169.6(3) . . . . ? C214 N211 C212 N212 -0.7(5) . . . . ? C211 N211 C212 N212 -175.2(4) . . . . ? C212 N212 C213 C214 -0.3(5) . . . . ? Co1 N212 C213 C214 168.8(3) . . . . ? N212 C213 C214 N211 -0.1(6) . . . . ? C212 N211 C214 C213 0.5(5) . . . . ? C211 N211 C214 C213 174.4(4) . . . . ? C232 N231 C231 C203 37.2(7) . . . . ? C234 N231 C231 C203 -142.3(5) . . . . ? C204 C203 C231 N231 -107.2(5) . . . . ? C202 C203 C231 N231 76.1(5) . . . . ? C233 N232 C232 N231 0.1(5) . . . . ? Co2 N232 C232 N231 -179.0(3) . . . . ? C234 N231 C232 N232 -0.1(5) . . . . ? C231 N231 C232 N232 -179.6(4) . . . . ? C232 N232 C233 C234 -0.1(5) . . . . ? Co2 N232 C233 C234 179.1(3) . . . . ? N232 C233 C234 N231 0.0(6) . . . . ? C232 N231 C234 C233 0.0(5) . . . . ? C231 N231 C234 C233 179.6(4) . . . . ? C252 N251 C251 C205 45.1(6) . . . . ? C254 N251 C251 C205 -142.9(5) . . . . ? C206 C205 C251 N251 55.7(6) . . . . ? C204 C205 C251 N251 -127.9(4) . . . . ? C253 N252 C252 N251 -0.7(5) . . . . ? Co2 N252 C252 N251 -173.4(3) 1_655 . . . ? C254 N251 C252 N252 1.1(6) . . . . ? C251 N251 C252 N252 174.3(4) . . . . ? C252 N252 C253 C254 0.0(6) . . . . ? Co2 N252 C253 C254 173.1(4) 1_655 . . . ? N252 C253 C254 N251 0.6(7) . . . . ? C252 N251 C254 C253 -1.0(7) . . . . ? C251 N251 C254 C253 -174.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.769 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.073 #====END