Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Laurence Thompson' _publ_contact_author_address ; Department of Chemistry Memorial University Elizabeth Ave. St. John's Newfoundland A1B 3X7 CANADA ; _publ_contact_author_email LTHOMP@MUN.CA _publ_section_title ; Self-Assembled Polynuclear Clusters Derived from some Flexible Polydentate Dihydrazide Ligands. ; loop_ _publ_author_name 'Laurence Thompson' 'Rosemary G. Harvey' 'Sarah Heath' 'Judith A. K. Howard' 'Michael Leech' 'David O. Miller' ; V.A.Milway ; 'Virginie Niel' 'Claire Wilson' 'Zhiqiang Xu' 'Liang Zhao' data_shelxl_(1) _database_code_depnum_ccdc_archive 'CCDC 228041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H50 N22 Ni2 O22' _chemical_formula_weight 1308.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0804(5) _cell_length_b 11.3912(7) _cell_length_c 14.2513(8) _cell_angle_alpha 104.2220(10) _cell_angle_beta 92.6490(10) _cell_angle_gamma 90.3550(10) _cell_volume 1427.17(14) _cell_formula_units_Z 1 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 676 _exptl_absorpt_coefficient_mu 0.755 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7132 _exptl_absorpt_correction_T_max 0.8575 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8638 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.39 _reflns_number_total 5751 _reflns_number_gt 5009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+1.8412P] 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 5751 _refine_ls_number_parameters 403 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0617 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1553 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.48947(4) 0.22149(3) 0.81742(3) 0.02164(15) Uani 1 1 d . . . O1 O 0.6443(3) 0.0886(2) 0.75087(16) 0.0281(5) Uani 1 1 d . . . O2 O 0.9075(3) -0.1911(2) 0.29677(17) 0.0374(6) Uani 1 1 d . . . O3 O 0.6629(3) 0.3391(2) 0.87410(17) 0.0334(5) Uani 1 1 d . . . O4 O 0.0795(3) 0.2170(2) 0.18007(18) 0.0380(6) Uani 1 1 d . . . O5 O -0.0213(3) 0.1565(3) 0.03591(19) 0.0457(7) Uani 1 1 d . . . O6 O 0.1332(3) 0.3067(2) 0.0678(2) 0.0443(6) Uani 1 1 d . . . O7 O 0.2726(3) 0.7536(3) 0.6716(2) 0.0461(7) Uani 1 1 d . . . O8 O 0.2957(7) 0.6941(8) 0.5204(4) 0.200(5) Uani 1 1 d . . . O9 O 0.4370(4) 0.8267(3) 0.5936(3) 0.0592(9) Uani 1 1 d . . . O10 O 0.1616(6) 0.4811(5) 0.4952(4) 0.0390(12) Uani 0.50 1 d P . . O11 O 0.0678(4) 0.7457(4) 0.1294(2) 0.0731(12) Uani 1 1 d . . . O12 O 0.3189(5) 0.4636(4) 0.2017(3) 0.0580(11) Uani 0.75 1 d P . . N1 N 0.3487(3) 0.3651(2) 0.82128(19) 0.0243(5) Uani 1 1 d . . . N2 N 0.3963(5) 0.3382(4) 0.5655(3) 0.0601(12) Uani 1 1 d . . . N3 N 0.4997(3) 0.2456(2) 0.68254(18) 0.0234(5) Uani 1 1 d . . . N4 N 0.5860(3) 0.1636(2) 0.62087(18) 0.0269(6) Uani 1 1 d . . . N5 N 0.7541(3) -0.0122(2) 0.50876(18) 0.0229(5) Uani 1 1 d . . . N6 N 0.7346(3) -0.0445(2) 0.31325(18) 0.0257(5) Uani 1 1 d . . . N7 N 0.6712(3) -0.0897(2) 0.21853(18) 0.0241(5) Uani 1 1 d . . . N8 N 0.8362(3) 0.0322(3) 0.1611(2) 0.0344(6) Uani 1 1 d . . . N9 N 0.5460(3) -0.1831(2) 0.05115(18) 0.0235(5) Uani 1 1 d . . . N10 N 0.0642(3) 0.2269(3) 0.0957(2) 0.0319(6) Uani 1 1 d . . . N11 N 0.3380(4) 0.7548(3) 0.5995(2) 0.0439(8) Uani 1 1 d . . . C1 C 0.2722(4) 0.4242(3) 0.8961(2) 0.0309(7) Uani 1 1 d . . . C2 C 0.1789(4) 0.5184(3) 0.8899(3) 0.0404(8) Uani 1 1 d . . . C3 C 0.1673(5) 0.5540(4) 0.8043(3) 0.0475(10) Uani 1 1 d . . . C4 C 0.2454(5) 0.4927(3) 0.7263(3) 0.0385(8) Uani 1 1 d . . . C5 C 0.3332(3) 0.3988(3) 0.7365(2) 0.0265(6) Uani 1 1 d . . . C6 C 0.4167(4) 0.3237(3) 0.6553(2) 0.0304(7) Uani 1 1 d . . . C7 C 0.6580(3) 0.0871(3) 0.6642(2) 0.0242(6) Uani 1 1 d . . . C8 C 0.7577(3) -0.0022(3) 0.6046(2) 0.0239(6) Uani 1 1 d . . . C9 C 0.8473(4) -0.0715(3) 0.6511(2) 0.0288(7) Uani 1 1 d . . . C10 C 0.9395(4) -0.1547(3) 0.5960(2) 0.0315(7) Uani 1 1 d . . . C11 C 0.9391(3) -0.1649(3) 0.4971(2) 0.0282(7) Uani 1 1 d . . . C12 C 0.8440(3) -0.0933(3) 0.4569(2) 0.0237(6) Uani 1 1 d . . . C13 C 0.8331(3) -0.1133(3) 0.3480(2) 0.0256(6) Uani 1 1 d . . . C14 C 0.7259(3) -0.0481(3) 0.1499(2) 0.0235(6) Uani 1 1 d . . . C15 C 0.6506(3) -0.0980(3) 0.0528(2) 0.0227(6) Uani 1 1 d . . . C16 C 0.6809(4) -0.0583(3) -0.0294(2) 0.0273(6) Uani 1 1 d . . . C17 C 0.6018(4) -0.1092(3) -0.1157(2) 0.0313(7) Uani 1 1 d . . . C18 C 0.4969(4) -0.1983(3) -0.1179(2) 0.0332(7) Uani 1 1 d . . . C19 C 0.4720(4) -0.2321(3) -0.0326(2) 0.0295(7) Uani 1 1 d . . . C20 C 0.2836(18) 0.4687(13) 0.2911(7) 0.176(8) Uani 0.75 1 d P . . C21 C 0.0000 0.5000 0.5000 0.083(5) Uani 0.50 2 d SP . . H1 H 0.4487 0.3005 0.5204 0.076 Uiso 1 1 d . . . H2 H 0.3430 0.3640 0.5525 0.076 Uiso 1 1 d . . . H3 H 0.8730 0.0555 0.2149 0.076 Uiso 1 1 d . . . H4 H 0.8677 0.0480 0.1209 0.076 Uiso 1 1 d . . . H5 H 0.2816 0.4003 0.9552 0.037 Uiso 1 1 d . . . H6 H 0.1239 0.5575 0.9438 0.048 Uiso 1 1 d . . . H7 H 0.1060 0.6192 0.7985 0.056 Uiso 1 1 d . . . H8 H 0.2389 0.5158 0.6666 0.046 Uiso 1 1 d . . . H9 H 0.8451 -0.0623 0.7192 0.034 Uiso 1 1 d . . . H10 H 1.0014 -0.2040 0.6252 0.038 Uiso 1 1 d . . . H11 H 1.0029 -0.2198 0.4576 0.033 Uiso 1 1 d . . . H12 H 0.7545 0.0027 -0.0259 0.032 Uiso 1 1 d . . . H13 H 0.6201 -0.0831 -0.1727 0.037 Uiso 1 1 d . . . H14 H 0.4424 -0.2357 -0.1764 0.039 Uiso 1 1 d . . . H15 H 0.3989 -0.2930 -0.0340 0.035 Uiso 1 1 d . . . H16 H 0.6805 -0.0016 0.3570 0.076 Uiso 1 1 d . . . H17 H 0.5932 0.1678 0.5645 0.076 Uiso 1 1 d . . . H18 H 0.7485 0.3112 0.8684 0.076 Uiso 1 1 d . . . H19 H 0.6949 0.4237 0.8467 0.076 Uiso 1 1 d . . . H20 H 0.2514 0.4031 0.1521 0.076 Uiso 0.75 1 d P . . H21 H 0.3727 0.4627 0.3315 0.325 Uiso 0.75 1 d P . . H22 H 0.2337 0.5374 0.3199 0.325 Uiso 0.75 1 d P . . H23 H 0.2239 0.3970 0.2925 0.325 Uiso 0.75 1 d P . . H24 H -0.0274 0.5102 0.5650 0.176 Uiso 0.25 1 d P . . H25 H -0.0253 0.5701 0.4783 0.176 Uiso 0.25 1 d P . . H26 H -0.0506 0.4313 0.4598 0.176 Uiso 0.25 1 d P . . H27 H 0.2278 0.5355 0.5393 0.076 Uiso 0.50 1 d P . . H28 H 0.0296 0.7729 0.0874 0.076 Uiso 1 1 d . . . H29 H 0.0110 0.7770 0.1776 0.076 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0259(2) 0.0231(2) 0.0170(2) 0.00643(14) 0.00317(14) 0.00193(14) O1 0.0339(12) 0.0328(11) 0.0197(11) 0.0096(9) 0.0051(9) 0.0078(9) O2 0.0406(14) 0.0430(14) 0.0261(12) 0.0025(10) 0.0060(10) 0.0158(11) O3 0.0287(12) 0.0401(13) 0.0305(12) 0.0071(10) 0.0006(9) -0.0041(10) O4 0.0426(14) 0.0443(14) 0.0298(13) 0.0145(11) 0.0012(11) 0.0042(11) O5 0.0503(16) 0.0546(16) 0.0337(14) 0.0148(12) -0.0013(12) -0.0162(13) O6 0.0480(16) 0.0377(14) 0.0529(17) 0.0208(12) 0.0110(13) -0.0040(12) O7 0.0563(17) 0.0510(16) 0.0372(15) 0.0208(12) 0.0119(13) 0.0085(13) O8 0.133(5) 0.292(9) 0.098(4) -0.109(5) 0.076(4) -0.136(6) O9 0.064(2) 0.0425(16) 0.074(2) 0.0141(15) 0.0365(17) 0.0049(14) O10 0.049(3) 0.038(3) 0.030(3) 0.013(2) -0.012(2) 0.005(2) O11 0.0441(18) 0.140(4) 0.0435(18) 0.036(2) 0.0125(14) 0.040(2) O12 0.063(3) 0.038(2) 0.075(3) 0.021(2) -0.013(2) -0.0199(18) N1 0.0274(13) 0.0235(12) 0.0230(13) 0.0070(10) 0.0040(10) 0.0012(10) N2 0.066(2) 0.092(3) 0.0359(18) 0.0364(19) 0.0220(17) 0.052(2) N3 0.0290(13) 0.0240(12) 0.0190(12) 0.0078(9) 0.0056(10) 0.0043(10) N4 0.0295(14) 0.0342(14) 0.0188(12) 0.0087(10) 0.0076(10) 0.0089(11) N5 0.0232(12) 0.0254(12) 0.0202(12) 0.0059(10) 0.0019(9) 0.0012(9) N6 0.0308(14) 0.0265(13) 0.0188(12) 0.0035(10) 0.0024(10) 0.0018(10) N7 0.0306(14) 0.0253(12) 0.0169(12) 0.0064(9) 0.0004(10) -0.0007(10) N8 0.0367(16) 0.0413(16) 0.0261(14) 0.0098(12) 0.0040(12) -0.0097(12) N9 0.0266(13) 0.0251(12) 0.0197(12) 0.0067(10) 0.0034(10) 0.0054(10) N10 0.0307(15) 0.0305(14) 0.0359(16) 0.0092(12) 0.0083(12) 0.0064(11) N11 0.0364(17) 0.057(2) 0.0340(17) 0.0015(15) 0.0074(13) 0.0080(15) C1 0.0371(18) 0.0308(16) 0.0244(16) 0.0048(13) 0.0076(13) 0.0045(13) C2 0.047(2) 0.041(2) 0.0316(18) 0.0049(15) 0.0094(16) 0.0175(16) C3 0.059(3) 0.043(2) 0.042(2) 0.0116(17) 0.0070(18) 0.0263(18) C4 0.050(2) 0.0390(19) 0.0304(18) 0.0154(15) 0.0049(15) 0.0138(16) C5 0.0270(15) 0.0278(15) 0.0261(15) 0.0083(12) 0.0045(12) 0.0029(12) C6 0.0331(17) 0.0370(17) 0.0247(16) 0.0137(13) 0.0069(13) 0.0081(13) C7 0.0249(15) 0.0279(15) 0.0202(14) 0.0070(11) 0.0012(11) 0.0007(11) C8 0.0240(15) 0.0255(14) 0.0225(15) 0.0067(11) 0.0016(11) 0.0005(11) C9 0.0296(16) 0.0358(17) 0.0222(15) 0.0094(13) 0.0000(12) 0.0045(13) C10 0.0304(17) 0.0364(17) 0.0294(17) 0.0121(13) -0.0026(13) 0.0096(13) C11 0.0254(15) 0.0311(16) 0.0264(16) 0.0037(12) 0.0006(12) 0.0049(12) C12 0.0242(15) 0.0250(14) 0.0216(14) 0.0053(11) 0.0014(11) -0.0004(11) C13 0.0272(15) 0.0271(15) 0.0227(15) 0.0057(12) 0.0044(12) 0.0000(12) C14 0.0238(14) 0.0231(14) 0.0244(15) 0.0065(11) 0.0060(11) 0.0051(11) C15 0.0246(14) 0.0242(14) 0.0209(14) 0.0077(11) 0.0062(11) 0.0082(11) C16 0.0306(16) 0.0294(15) 0.0254(15) 0.0119(12) 0.0093(12) 0.0089(12) C17 0.0401(18) 0.0348(17) 0.0233(16) 0.0137(13) 0.0088(13) 0.0121(14) C18 0.0384(19) 0.0397(18) 0.0212(16) 0.0069(13) -0.0008(13) 0.0072(14) C19 0.0342(17) 0.0323(16) 0.0215(15) 0.0058(12) -0.0002(12) 0.0012(13) C20 0.269(17) 0.192(13) 0.047(5) -0.007(6) 0.008(7) -0.183(13) C21 0.077(11) 0.060(9) 0.115(15) 0.035(9) -0.019(10) -0.030(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 2.014(2) . ? Ni1 N7 2.042(3) 2_656 ? Ni1 O3 2.062(2) . ? Ni1 N9 2.064(3) 2_656 ? Ni1 N1 2.074(3) . ? Ni1 O1 2.148(2) . ? O1 C7 1.243(4) . ? O2 C13 1.228(4) . ? O4 N10 1.236(4) . ? O5 N10 1.252(4) . ? O6 N10 1.254(4) . ? O7 N11 1.214(4) . ? O8 N11 1.212(6) . ? O9 N11 1.231(5) . ? O10 C21 1.487(5) . ? O12 C20 1.315(10) . ? N1 C1 1.339(4) . ? N1 C5 1.356(4) . ? N2 C6 1.334(5) . ? N3 C6 1.289(4) . ? N3 N4 1.389(4) . ? N4 C7 1.343(4) . ? N5 C12 1.340(4) . ? N5 C8 1.341(4) . ? N6 C13 1.349(4) . ? N6 N7 1.415(3) . ? N7 C14 1.303(4) . ? N7 Ni1 2.042(3) 2_656 ? N8 C14 1.330(4) . ? N9 C19 1.335(4) . ? N9 C15 1.349(4) . ? N9 Ni1 2.064(3) 2_656 ? C1 C2 1.389(5) . ? C2 C3 1.377(6) . ? C3 C4 1.388(5) . ? C4 C5 1.371(5) . ? C5 C6 1.500(4) . ? C7 C8 1.494(4) . ? C8 C9 1.393(4) . ? C9 C10 1.386(5) . ? C10 C11 1.386(5) . ? C11 C12 1.389(4) . ? C12 C13 1.511(4) . ? C14 C15 1.492(4) . ? C15 C16 1.393(4) . ? C16 C17 1.388(5) . ? C17 C18 1.381(5) . ? C18 C19 1.390(5) . ? C21 O10 1.487(5) 2_566 ? 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 N3 Ni1 N7 95.06(10) . 2_656 ? N3 Ni1 O3 94.50(10) . . ? N7 Ni1 O3 169.29(10) 2_656 . ? N3 Ni1 N9 172.39(10) . 2_656 ? N7 Ni1 N9 77.47(10) 2_656 2_656 ? O3 Ni1 N9 93.06(10) . 2_656 ? N3 Ni1 N1 77.81(10) . . ? N7 Ni1 N1 95.66(10) 2_656 . ? O3 Ni1 N1 91.06(10) . . ? N9 Ni1 N1 101.26(10) 2_656 . ? N3 Ni1 O1 76.44(9) . . ? N7 Ni1 O1 88.22(10) 2_656 . ? O3 Ni1 O1 89.34(9) . . ? N9 Ni1 O1 104.48(9) 2_656 . ? N1 Ni1 O1 154.20(9) . . ? C7 O1 Ni1 111.9(2) . . ? C1 N1 C5 118.4(3) . . ? C1 N1 Ni1 127.4(2) . . ? C5 N1 Ni1 114.2(2) . . ? C6 N3 N4 124.1(3) . . ? C6 N3 Ni1 120.1(2) . . ? N4 N3 Ni1 115.32(19) . . ? C7 N4 N3 113.7(2) . . ? C12 N5 C8 116.7(3) . . ? C13 N6 N7 118.4(2) . . ? C14 N7 N6 116.9(2) . . ? C14 N7 Ni1 118.8(2) . 2_656 ? N6 N7 Ni1 124.26(19) . 2_656 ? C19 N9 C15 118.5(3) . . ? C19 N9 Ni1 125.7(2) . 2_656 ? C15 N9 Ni1 115.7(2) . 2_656 ? O4 N10 O5 120.3(3) . . ? O4 N10 O6 121.3(3) . . ? O5 N10 O6 118.4(3) . . ? O8 N11 O7 121.3(4) . . ? O8 N11 O9 111.8(4) . . ? O7 N11 O9 126.0(4) . . ? N1 C1 C2 122.4(3) . . ? C3 C2 C1 118.6(3) . . ? C2 C3 C4 119.2(3) . . ? C5 C4 C3 119.1(3) . . ? N1 C5 C4 122.1(3) . . ? N1 C5 C6 114.8(3) . . ? C4 C5 C6 123.1(3) . . ? N3 C6 N2 126.9(3) . . ? N3 C6 C5 112.7(3) . . ? N2 C6 C5 120.4(3) . . ? O1 C7 N4 122.4(3) . . ? O1 C7 C8 119.8(3) . . ? N4 C7 C8 117.8(3) . . ? N5 C8 C9 123.6(3) . . ? N5 C8 C7 117.9(3) . . ? C9 C8 C7 118.4(3) . . ? C10 C9 C8 118.6(3) . . ? C11 C10 C9 118.5(3) . . ? C10 C11 C12 118.7(3) . . ? N5 C12 C11 123.8(3) . . ? N5 C12 C13 117.6(3) . . ? C11 C12 C13 118.5(3) . . ? O2 C13 N6 124.0(3) . . ? O2 C13 C12 120.3(3) . . ? N6 C13 C12 115.7(3) . . ? N7 C14 N8 125.7(3) . . ? N7 C14 C15 113.5(3) . . ? N8 C14 C15 120.8(3) . . ? N9 C15 C16 122.0(3) . . ? N9 C15 C14 114.4(3) . . ? C16 C15 C14 123.6(3) . . ? C17 C16 C15 118.7(3) . . ? C18 C17 C16 119.3(3) . . ? C17 C18 C19 118.6(3) . . ? N9 C19 C18 122.9(3) . . ? O10 C21 O10 179.998(2) 2_566 . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.959 _refine_diff_density_min -1.887 _refine_diff_density_rms 0.095 #===END data_ihs5_(2) _database_code_depnum_ccdc_archive 'CCDC 228042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H32 Mn2 N12 O20' _chemical_formula_weight 834.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 7.4206(5) _cell_length_b 13.0519(9) _cell_length_c 16.7285(12) _cell_angle_alpha 90.00 _cell_angle_beta 93.7540(10) _cell_angle_gamma 90.00 _cell_volume 1616.73(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5420 _cell_measurement_theta_min 1.56 _cell_measurement_theta_max 28.29 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.883 _exptl_absorpt_correction_type Semi-empirical _exptl_absorpt_correction_T_min 0.7358 _exptl_absorpt_correction_T_max 0.9169 _exptl_absorpt_process_details 'repeated and equivalent reflections' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10404 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 28.29 _reflns_number_total 5362 _reflns_number_gt 4841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0723P)^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 0.636(18) _refine_ls_number_reflns 5362 _refine_ls_number_parameters 483 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.005 _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 0.58909(7) 1.01935(4) 0.35160(3) 0.02219(13) Uani 1 1 d . . . N1 N 0.5645(4) 0.8659(2) 0.42067(18) 0.0232(6) Uani 1 1 d . . . C1 C 0.4917(5) 0.7797(3) 0.3891(2) 0.0251(7) Uani 1 1 d . . . H1 H 0.4410 0.7818 0.3368 0.030 Uiso 1 1 calc R . . C2 C 0.4879(5) 0.6883(3) 0.4300(2) 0.0270(8) Uani 1 1 d . . . H2 H 0.4375 0.6299 0.4059 0.032 Uiso 1 1 calc R . . C3 C 0.5621(5) 0.6859(3) 0.5091(3) 0.0305(8) Uani 1 1 d . . . H3 H 0.5614 0.6257 0.5388 0.037 Uiso 1 1 calc R . . C4 C 0.6365(5) 0.7745(3) 0.5424(2) 0.0288(8) Uani 1 1 d . . . H4 H 0.6854 0.7747 0.5950 0.035 Uiso 1 1 calc R . . C5 C 0.6378(5) 0.8627(3) 0.4970(2) 0.0217(7) Uani 1 1 d . . . C6 C 0.7254(5) 0.9595(3) 0.5261(2) 0.0219(7) Uani 1 1 d . . . N2 N 0.8011(5) 0.9657(2) 0.6005(2) 0.0318(8) Uani 1 1 d . . . H2A H 0.8544 1.0212 0.6166 0.038 Uiso 1 1 calc R . . H2B H 0.7968 0.9141 0.6323 0.038 Uiso 1 1 calc R . . N3 N 0.7235(5) 1.0322(2) 0.4728(2) 0.0233(7) Uani 1 1 d . . . N4 N 0.7994(4) 1.1261(2) 0.49445(18) 0.0230(6) Uani 1 1 d . . . H4A H 0.8506 1.1374 0.5412 0.028 Uiso 1 1 calc R . . O1 O 0.7210(4) 1.18291(19) 0.36895(16) 0.0302(6) Uani 1 1 d . . . O3 O 0.3956(4) 0.9403(2) 0.25570(17) 0.0311(6) Uani 1 1 d . . . O4 O 0.5049(4) 1.0893(2) 0.22901(17) 0.0328(6) Uani 1 1 d . . . N9 N 0.4087(5) 1.0128(2) 0.2063(2) 0.0271(7) Uani 1 1 d . . . O5 O 0.3299(4) 1.0103(2) 0.13902(18) 0.0374(7) Uani 1 1 d . . . O6 O 0.8123(4) 0.9469(2) 0.29527(16) 0.0299(6) Uani 1 1 d D . . H6A H 0.894(5) 0.995(2) 0.283(3) 0.045 Uiso 1 1 d D . . H6B H 0.805(6) 0.894(2) 0.260(2) 0.045 Uiso 1 1 d D . . O7 O 0.3414(5) 1.0815(3) 0.39383(19) 0.0538(10) Uani 1 1 d . . . H7 H 0.2548 1.0944 0.3523 0.065 Uiso 1 1 calc R . . C15 C 0.2822(7) 1.1066(4) 0.4681(3) 0.0441(11) Uani 1 1 d . . . H15A H 0.3822 1.1048 0.5075 0.066 Uiso 1 1 calc R . . H15B H 0.1922 1.0583 0.4823 0.066 Uiso 1 1 calc R . . H15C H 0.2310 1.1742 0.4661 0.066 Uiso 1 1 calc R . . C7 C 0.7873(5) 1.1975(3) 0.4374(2) 0.0225(7) Uani 1 1 d . . . C8 C 0.8608(5) 1.2999(3) 0.4673(2) 0.0223(7) Uani 1 1 d . . . O2 O 0.9144(4) 1.31149(19) 0.53862(16) 0.0304(6) Uani 1 1 d . . . Mn2 Mn 1.04175(7) 1.46365(4) 0.57059(3) 0.02296(13) Uani 1 1 d . . . N5 N 0.8584(4) 1.3748(2) 0.41372(19) 0.0238(6) Uani 1 1 d . . . H5 H 0.8126 1.3678 0.3655 0.029 Uiso 1 1 calc R . . N6 N 0.9363(5) 1.4658(2) 0.4422(2) 0.0224(7) Uani 1 1 d . . . C9 C 0.9093(5) 1.5491(3) 0.4007(2) 0.0201(7) Uani 1 1 d . . . N7 N 0.8198(5) 1.5581(2) 0.32954(19) 0.0272(7) Uani 1 1 d . . . H7A H 0.7724 1.5049 0.3063 0.033 Uiso 1 1 calc R . . H7B H 0.8093 1.6171 0.3068 0.033 Uiso 1 1 calc R . . C10 C 0.9922(5) 1.6421(3) 0.4410(2) 0.0219(7) Uani 1 1 d . . . C11 C 1.0019(5) 1.7361(3) 0.4032(2) 0.0263(7) Uani 1 1 d . . . H11 H 0.9609 1.7434 0.3498 0.032 Uiso 1 1 calc R . . C12 C 1.0737(6) 1.8191(3) 0.4460(2) 0.0309(8) Uani 1 1 d . . . H12 H 1.0816 1.8829 0.4217 0.037 Uiso 1 1 calc R . . C13 C 1.1340(5) 1.8056(3) 0.5263(2) 0.0294(8) Uani 1 1 d . . . H13 H 1.1807 1.8601 0.5569 0.035 Uiso 1 1 calc R . . C14 C 1.1220(5) 1.7088(3) 0.5586(2) 0.0282(8) Uani 1 1 d . . . H14 H 1.1634 1.6995 0.6118 0.034 Uiso 1 1 calc R . . N8 N 1.0551(4) 1.6280(2) 0.51855(19) 0.0230(6) Uani 1 1 d . . . O8 O 1.1106(4) 1.3629(2) 0.68618(18) 0.0350(6) Uani 1 1 d . . . O9 O 1.1773(5) 1.5233(2) 0.6855(2) 0.0406(8) Uani 1 1 d . . . N10 N 1.1799(5) 1.4383(3) 0.7239(2) 0.0341(8) Uani 1 1 d . . . O10 O 1.2439(5) 1.4329(3) 0.79251(18) 0.0467(8) Uani 1 1 d . . . O11 O 0.7835(3) 1.5006(2) 0.61926(16) 0.0291(6) Uani 1 1 d D . . H11A H 0.758(7) 1.528(3) 0.5706(10) 0.044 Uiso 1 1 d D . . H11B H 0.778(7) 1.546(2) 0.6593(15) 0.044 Uiso 1 1 d D . . O12 O 1.3073(4) 1.4085(3) 0.5398(2) 0.0458(8) Uani 1 1 d . . . H12A H 1.3817 1.3869 0.5835 0.055 Uiso 1 1 calc R . . C16 C 1.3869(7) 1.3998(4) 0.4641(3) 0.0477(11) Uani 1 1 d . . . H16A H 1.3042 1.4255 0.4224 0.072 Uiso 1 1 calc R . . H16B H 1.4131 1.3292 0.4539 0.072 Uiso 1 1 calc R . . H16C H 1.4967 1.4389 0.4656 0.072 Uiso 1 1 calc R . . N11 N 1.0259(4) 0.8186(3) 0.76201(19) 0.0286(7) Uani 1 1 d . . . O13 O 0.9040(4) 0.7991(2) 0.70826(17) 0.0364(7) Uani 1 1 d . . . O14 O 1.0768(4) 0.9099(2) 0.77206(18) 0.0369(7) Uani 1 1 d . . . O15 O 1.0935(4) 0.7499(2) 0.80474(19) 0.0417(7) Uani 1 1 d . . . N12 N 0.6212(4) 1.7367(2) 0.17407(19) 0.0280(7) Uani 1 1 d . . . O16 O 0.5548(4) 1.6481(2) 0.16178(19) 0.0395(7) Uani 1 1 d . . . O17 O 0.5827(5) 1.8073(3) 0.12840(19) 0.0469(8) Uani 1 1 d . . . O18 O 0.7278(4) 1.7496(2) 0.23478(17) 0.0343(6) Uani 1 1 d . . . C17 C 0.5181(10) 1.3457(5) 0.2464(4) 0.0720(18) Uani 1 1 d . . . H17A H 0.4951 1.3065 0.2933 0.108 Uiso 1 1 calc R . . H17B H 0.4810 1.3071 0.1993 0.108 Uiso 1 1 calc R . . H17C H 0.4513 1.4087 0.2467 0.108 Uiso 1 1 calc R . . O19 O 0.7231(4) 1.3696(2) 0.24636(18) 0.0356(6) Uani 1 1 d . . . H19 H 0.7782 1.3171 0.2365 0.053 Uiso 1 1 calc R . . O20 O 1.0332(4) 1.1351(2) 0.64880(19) 0.0364(7) Uani 1 1 d D . . H20B H 1.134(3) 1.097(2) 0.654(3) 0.055 Uiso 1 1 d D . . H20A H 1.049(5) 1.1989(15) 0.669(3) 0.055 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0251(3) 0.0231(2) 0.0181(2) 0.0004(2) -0.0013(2) 0.0005(2) N1 0.0272(16) 0.0224(15) 0.0198(14) 0.0013(11) -0.0004(12) -0.0003(11) C1 0.0245(17) 0.0269(17) 0.0236(17) -0.0030(14) -0.0012(14) -0.0042(13) C2 0.0288(19) 0.0241(17) 0.0274(18) -0.0042(14) -0.0024(15) -0.0026(13) C3 0.031(2) 0.0217(17) 0.037(2) 0.0066(15) -0.0068(16) -0.0020(14) C4 0.034(2) 0.0246(17) 0.0275(18) 0.0039(15) -0.0027(15) -0.0043(14) C5 0.0210(17) 0.0247(16) 0.0190(16) 0.0020(13) -0.0009(13) 0.0002(12) C6 0.0225(18) 0.0233(16) 0.0201(18) 0.0039(13) 0.0034(14) 0.0019(13) N2 0.053(2) 0.0218(15) 0.0190(15) 0.0029(11) -0.0062(15) -0.0091(13) N3 0.0271(17) 0.0201(14) 0.0224(16) -0.0002(11) -0.0016(13) -0.0024(11) N4 0.0304(16) 0.0181(13) 0.0195(14) 0.0003(11) -0.0045(12) -0.0046(11) O1 0.0470(17) 0.0208(12) 0.0222(13) 0.0022(10) -0.0034(11) -0.0024(11) O3 0.0363(15) 0.0261(13) 0.0299(14) 0.0015(11) -0.0043(12) 0.0001(11) O4 0.0434(17) 0.0269(14) 0.0274(14) 0.0001(11) -0.0021(12) -0.0017(12) N9 0.0325(18) 0.0253(15) 0.0227(16) 0.0003(12) -0.0038(14) 0.0052(12) O5 0.0464(18) 0.0391(16) 0.0246(14) -0.0028(12) -0.0144(13) 0.0070(13) O6 0.0361(15) 0.0267(13) 0.0272(14) -0.0023(11) 0.0054(11) 0.0021(11) O7 0.0384(18) 0.098(3) 0.0246(15) -0.0089(17) -0.0019(13) 0.0300(18) C15 0.040(2) 0.057(3) 0.035(2) -0.007(2) 0.0059(19) 0.003(2) C7 0.0227(17) 0.0200(15) 0.0251(17) -0.0011(13) 0.0041(13) -0.0002(12) C8 0.0268(18) 0.0186(15) 0.0213(16) 0.0003(13) -0.0008(13) 0.0016(13) O2 0.0448(16) 0.0248(13) 0.0209(12) 0.0028(10) -0.0028(11) -0.0047(11) Mn2 0.0259(3) 0.0240(2) 0.0185(3) 0.0002(2) -0.0022(2) -0.0001(2) N5 0.0324(16) 0.0180(13) 0.0204(14) -0.0001(11) -0.0018(12) -0.0035(12) N6 0.0328(18) 0.0159(14) 0.0182(15) -0.0021(11) 0.0003(13) -0.0045(11) C9 0.0232(18) 0.0177(15) 0.0192(17) -0.0014(13) -0.0007(14) -0.0001(13) N7 0.0355(18) 0.0200(14) 0.0252(16) 0.0021(13) -0.0058(13) -0.0040(12) C10 0.0242(18) 0.0193(15) 0.0221(16) -0.0005(13) 0.0014(13) 0.0024(12) C11 0.0282(19) 0.0215(16) 0.0286(19) 0.0003(14) -0.0015(14) 0.0002(13) C12 0.033(2) 0.0229(17) 0.036(2) 0.0015(15) -0.0014(16) -0.0038(14) C13 0.029(2) 0.0215(16) 0.038(2) -0.0097(15) -0.0011(16) -0.0025(14) C14 0.0296(19) 0.0288(18) 0.0258(18) -0.0027(14) -0.0021(15) -0.0006(14) N8 0.0220(15) 0.0228(14) 0.0240(15) -0.0002(11) 0.0001(12) -0.0003(11) O8 0.0399(16) 0.0336(15) 0.0309(14) 0.0031(12) -0.0023(12) -0.0013(12) O9 0.053(2) 0.0386(17) 0.0287(16) 0.0015(12) -0.0094(14) -0.0081(14) N10 0.0309(18) 0.042(2) 0.0293(18) 0.0058(16) 0.0001(14) -0.0008(15) O10 0.0471(19) 0.069(2) 0.0228(14) 0.0063(15) -0.0094(13) -0.0052(16) O11 0.0311(15) 0.0297(13) 0.0270(14) -0.0010(11) 0.0046(11) 0.0008(11) O12 0.0363(17) 0.068(2) 0.0341(16) 0.0110(15) 0.0062(13) 0.0207(15) C16 0.046(3) 0.053(3) 0.046(3) 0.003(2) 0.015(2) 0.002(2) N11 0.0292(17) 0.0276(16) 0.0293(17) 0.0002(13) 0.0030(13) 0.0036(12) O13 0.0436(17) 0.0367(15) 0.0273(14) 0.0074(12) -0.0086(12) -0.0079(12) O14 0.0333(15) 0.0317(15) 0.0452(17) 0.0005(13) -0.0016(13) -0.0060(12) O15 0.0419(17) 0.0408(16) 0.0411(17) 0.0137(14) -0.0068(14) 0.0095(13) N12 0.0314(16) 0.0292(16) 0.0239(15) -0.0015(12) 0.0052(13) 0.0057(13) O16 0.0330(16) 0.0414(16) 0.0435(17) -0.0097(14) -0.0021(13) -0.0020(13) O17 0.0529(19) 0.0486(19) 0.0391(17) 0.0153(15) 0.0021(15) 0.0164(15) O18 0.0397(15) 0.0288(14) 0.0334(15) 0.0012(12) -0.0061(12) -0.0018(11) C17 0.094(5) 0.061(4) 0.061(4) 0.008(3) 0.002(3) 0.032(3) O19 0.0445(17) 0.0274(14) 0.0338(14) -0.0014(12) -0.0062(13) 0.0072(12) O20 0.0386(16) 0.0286(14) 0.0409(16) 0.0025(12) -0.0051(13) 0.0013(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O7 2.169(3) . ? Mn1 O6 2.175(3) . ? Mn1 N3 2.207(3) . ? Mn1 O4 2.293(3) . ? Mn1 O3 2.323(3) . ? Mn1 N1 2.326(3) . ? Mn1 O1 2.358(3) . ? N1 C1 1.341(5) . ? N1 C5 1.355(4) . ? C1 C2 1.377(5) . ? C2 C3 1.399(5) . ? C3 C4 1.383(5) . ? C4 C5 1.379(5) . ? C5 C6 1.489(5) . ? C6 N3 1.301(5) . ? C6 N2 1.333(5) . ? N3 N4 1.386(4) . ? N4 C7 1.332(5) . ? O1 C7 1.232(4) . ? O3 N9 1.264(4) . ? O4 N9 1.271(4) . ? N9 O5 1.234(4) . ? O7 C15 1.385(6) . ? C7 C8 1.516(4) . ? C8 O2 1.241(4) . ? C8 N5 1.327(5) . ? O2 Mn2 2.249(3) . ? Mn2 O11 2.184(3) . ? Mn2 O12 2.191(3) . ? Mn2 N6 2.237(3) . ? Mn2 O9 2.249(3) . ? Mn2 N8 2.320(3) . ? Mn2 O8 2.366(3) . ? N5 N6 1.391(4) . ? N6 C9 1.300(5) . ? C9 N7 1.330(5) . ? C9 C10 1.501(5) . ? C10 N8 1.362(5) . ? C10 C11 1.384(5) . ? C11 C12 1.386(5) . ? C12 C13 1.399(6) . ? C13 C14 1.380(5) . ? C14 N8 1.327(5) . ? O8 N10 1.260(5) . ? O9 N10 1.281(5) . ? N10 O10 1.216(5) . ? O12 C16 1.436(6) . ? N11 O15 1.233(4) . ? N11 O14 1.258(4) . ? N11 O13 1.259(4) . ? N12 O17 1.219(4) . ? N12 O18 1.257(4) . ? N12 O16 1.267(4) . ? C17 O19 1.554(8) . ? 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 O7 Mn1 O6 171.61(12) . . ? O7 Mn1 N3 90.79(12) . . ? O6 Mn1 N3 96.90(12) . . ? O7 Mn1 O4 87.44(12) . . ? O6 Mn1 O4 87.49(11) . . ? N3 Mn1 O4 150.65(11) . . ? O7 Mn1 O3 83.83(12) . . ? O6 Mn1 O3 87.79(11) . . ? N3 Mn1 O3 152.87(11) . . ? O4 Mn1 O3 55.90(10) . . ? O7 Mn1 N1 93.72(14) . . ? O6 Mn1 N1 85.83(11) . . ? N3 Mn1 N1 69.77(11) . . ? O4 Mn1 N1 139.58(10) . . ? O3 Mn1 N1 84.02(10) . . ? O7 Mn1 O1 88.57(14) . . ? O6 Mn1 O1 97.20(11) . . ? N3 Mn1 O1 70.07(10) . . ? O4 Mn1 O1 80.59(9) . . ? O3 Mn1 O1 136.02(9) . . ? N1 Mn1 O1 139.80(10) . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Mn1 124.7(2) . . ? C5 N1 Mn1 117.1(2) . . ? N1 C1 C2 123.5(3) . . ? C1 C2 C3 118.0(3) . . ? C4 C3 C2 118.9(3) . . ? C5 C4 C3 119.6(4) . . ? N1 C5 C4 121.8(3) . . ? N1 C5 C6 115.0(3) . . ? C4 C5 C6 123.1(3) . . ? N3 C6 N2 125.5(3) . . ? N3 C6 C5 114.2(3) . . ? N2 C6 C5 120.3(3) . . ? C6 N3 N4 118.6(3) . . ? C6 N3 Mn1 123.9(2) . . ? N4 N3 Mn1 117.3(2) . . ? C7 N4 N3 115.1(3) . . ? C7 O1 Mn1 113.0(2) . . ? N9 O3 Mn1 92.8(2) . . ? N9 O4 Mn1 94.0(2) . . ? O5 N9 O3 121.6(3) . . ? O5 N9 O4 121.2(3) . . ? O3 N9 O4 117.2(3) . . ? C15 O7 Mn1 134.9(3) . . ? O1 C7 N4 124.2(3) . . ? O1 C7 C8 123.8(3) . . ? N4 C7 C8 112.0(3) . . ? O2 C8 N5 123.3(3) . . ? O2 C8 C7 120.7(3) . . ? N5 C8 C7 116.0(3) . . ? C8 O2 Mn2 116.1(2) . . ? O11 Mn2 O12 169.96(12) . . ? O11 Mn2 N6 95.43(12) . . ? O12 Mn2 N6 92.40(13) . . ? O11 Mn2 O2 85.32(11) . . ? O12 Mn2 O2 91.40(13) . . ? N6 Mn2 O2 70.57(10) . . ? O11 Mn2 O9 87.67(12) . . ? O12 Mn2 O9 87.47(14) . . ? N6 Mn2 O9 157.63(11) . . ? O2 Mn2 O9 131.80(11) . . ? O11 Mn2 N8 89.76(11) . . ? O12 Mn2 N8 98.88(13) . . ? N6 Mn2 N8 69.47(10) . . ? O2 Mn2 N8 139.04(10) . . ? O9 Mn2 N8 88.43(11) . . ? O11 Mn2 O8 88.04(11) . . ? O12 Mn2 O8 81.96(12) . . ? N6 Mn2 O8 146.56(10) . . ? O2 Mn2 O8 76.61(10) . . ? O9 Mn2 O8 55.51(11) . . ? N8 Mn2 O8 143.93(11) . . ? C8 N5 N6 114.2(3) . . ? C9 N6 N5 119.0(3) . . ? C9 N6 Mn2 123.7(2) . . ? N5 N6 Mn2 115.5(2) . . ? N6 C9 N7 127.1(3) . . ? N6 C9 C10 113.1(3) . . ? N7 C9 C10 119.8(3) . . ? N8 C10 C11 122.0(3) . . ? N8 C10 C9 115.1(3) . . ? C11 C10 C9 122.9(3) . . ? C10 C11 C12 119.1(3) . . ? C11 C12 C13 119.1(4) . . ? C14 C13 C12 117.8(3) . . ? N8 C14 C13 124.2(3) . . ? C14 N8 C10 117.8(3) . . ? C14 N8 Mn2 124.7(2) . . ? C10 N8 Mn2 117.5(2) . . ? N10 O8 Mn2 91.9(2) . . ? N10 O9 Mn2 96.9(2) . . ? O10 N10 O8 123.2(4) . . ? O10 N10 O9 121.1(4) . . ? O8 N10 O9 115.7(3) . . ? C16 O12 Mn2 131.4(3) . . ? O15 N11 O14 120.3(3) . . ? O15 N11 O13 120.9(3) . . ? O14 N11 O13 118.8(3) . . ? O17 N12 O18 120.9(3) . . ? O17 N12 O16 121.0(3) . . ? O18 N12 O16 118.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O7 Mn1 N1 C1 95.4(3) . . . . ? O6 Mn1 N1 C1 -76.2(3) . . . . ? N3 Mn1 N1 C1 -175.2(3) . . . . ? O4 Mn1 N1 C1 4.9(4) . . . . ? O3 Mn1 N1 C1 12.0(3) . . . . ? O1 Mn1 N1 C1 -172.5(3) . . . . ? O7 Mn1 N1 C5 -88.1(3) . . . . ? O6 Mn1 N1 C5 100.3(3) . . . . ? N3 Mn1 N1 C5 1.3(3) . . . . ? O4 Mn1 N1 C5 -178.6(2) . . . . ? O3 Mn1 N1 C5 -171.5(3) . . . . ? O1 Mn1 N1 C5 4.0(3) . . . . ? C5 N1 C1 C2 -0.2(6) . . . . ? Mn1 N1 C1 C2 176.3(3) . . . . ? N1 C1 C2 C3 0.9(6) . . . . ? C1 C2 C3 C4 -0.4(6) . . . . ? C2 C3 C4 C5 -0.6(6) . . . . ? C1 N1 C5 C4 -0.9(5) . . . . ? Mn1 N1 C5 C4 -177.7(3) . . . . ? C1 N1 C5 C6 176.6(3) . . . . ? Mn1 N1 C5 C6 -0.2(4) . . . . ? C3 C4 C5 N1 1.3(6) . . . . ? C3 C4 C5 C6 -175.9(4) . . . . ? N1 C5 C6 N3 -2.0(5) . . . . ? C4 C5 C6 N3 175.5(4) . . . . ? N1 C5 C6 N2 179.6(4) . . . . ? C4 C5 C6 N2 -3.0(6) . . . . ? N2 C6 N3 N4 -2.7(6) . . . . ? C5 C6 N3 N4 179.0(3) . . . . ? N2 C6 N3 Mn1 -178.2(3) . . . . ? C5 C6 N3 Mn1 3.5(5) . . . . ? O7 Mn1 N3 C6 90.9(3) . . . . ? O6 Mn1 N3 C6 -85.7(3) . . . . ? O4 Mn1 N3 C6 177.1(3) . . . . ? O3 Mn1 N3 C6 13.0(5) . . . . ? N1 Mn1 N3 C6 -2.7(3) . . . . ? O1 Mn1 N3 C6 179.1(4) . . . . ? O7 Mn1 N3 N4 -84.6(3) . . . . ? O6 Mn1 N3 N4 98.7(3) . . . . ? O4 Mn1 N3 N4 1.6(4) . . . . ? O3 Mn1 N3 N4 -162.6(2) . . . . ? N1 Mn1 N3 N4 -178.3(3) . . . . ? O1 Mn1 N3 N4 3.6(3) . . . . ? C6 N3 N4 C7 -178.0(3) . . . . ? Mn1 N3 N4 C7 -2.2(4) . . . . ? O7 Mn1 O1 C7 86.5(3) . . . . ? O6 Mn1 O1 C7 -99.6(3) . . . . ? N3 Mn1 O1 C7 -4.8(3) . . . . ? O4 Mn1 O1 C7 174.2(3) . . . . ? O3 Mn1 O1 C7 166.1(2) . . . . ? N1 Mn1 O1 C7 -7.5(4) . . . . ? O7 Mn1 O3 N9 92.4(2) . . . . ? O6 Mn1 O3 N9 -87.2(2) . . . . ? N3 Mn1 O3 N9 172.0(3) . . . . ? O4 Mn1 O3 N9 1.3(2) . . . . ? N1 Mn1 O3 N9 -173.2(2) . . . . ? O1 Mn1 O3 N9 10.9(3) . . . . ? O7 Mn1 O4 N9 -85.6(2) . . . . ? O6 Mn1 O4 N9 87.7(2) . . . . ? N3 Mn1 O4 N9 -172.6(2) . . . . ? O3 Mn1 O4 N9 -1.3(2) . . . . ? N1 Mn1 O4 N9 7.2(3) . . . . ? O1 Mn1 O4 N9 -174.5(2) . . . . ? Mn1 O3 N9 O5 178.6(3) . . . . ? Mn1 O3 N9 O4 -2.2(3) . . . . ? Mn1 O4 N9 O5 -178.6(3) . . . . ? Mn1 O4 N9 O3 2.2(3) . . . . ? O6 Mn1 O7 C15 149.0(8) . . . . ? N3 Mn1 O7 C15 -7.5(5) . . . . ? O4 Mn1 O7 C15 -158.1(5) . . . . ? O3 Mn1 O7 C15 145.9(5) . . . . ? N1 Mn1 O7 C15 62.3(5) . . . . ? O1 Mn1 O7 C15 -77.5(5) . . . . ? Mn1 O1 C7 N4 5.9(5) . . . . ? Mn1 O1 C7 C8 -172.6(3) . . . . ? N3 N4 C7 O1 -2.8(6) . . . . ? N3 N4 C7 C8 175.8(3) . . . . ? O1 C7 C8 O2 174.9(4) . . . . ? N4 C7 C8 O2 -3.7(5) . . . . ? O1 C7 C8 N5 -3.1(5) . . . . ? N4 C7 C8 N5 178.3(4) . . . . ? N5 C8 O2 Mn2 -7.4(5) . . . . ? C7 C8 O2 Mn2 174.8(2) . . . . ? C8 O2 Mn2 O11 102.1(3) . . . . ? C8 O2 Mn2 O12 -87.4(3) . . . . ? C8 O2 Mn2 N6 4.6(3) . . . . ? C8 O2 Mn2 O9 -175.3(3) . . . . ? C8 O2 Mn2 N8 17.9(4) . . . . ? C8 O2 Mn2 O8 -168.8(3) . . . . ? O2 C8 N5 N6 5.5(6) . . . . ? C7 C8 N5 N6 -176.5(3) . . . . ? C8 N5 N6 C9 -166.3(4) . . . . ? C8 N5 N6 Mn2 -0.8(4) . . . . ? O11 Mn2 N6 C9 79.8(3) . . . . ? O12 Mn2 N6 C9 -106.5(3) . . . . ? O2 Mn2 N6 C9 162.9(4) . . . . ? O9 Mn2 N6 C9 -17.3(6) . . . . ? N8 Mn2 N6 C9 -7.9(3) . . . . ? O8 Mn2 N6 C9 174.5(3) . . . . ? O11 Mn2 N6 N5 -84.9(3) . . . . ? O12 Mn2 N6 N5 88.8(3) . . . . ? O2 Mn2 N6 N5 -1.9(2) . . . . ? O9 Mn2 N6 N5 178.0(3) . . . . ? N8 Mn2 N6 N5 -172.6(3) . . . . ? O8 Mn2 N6 N5 9.8(4) . . . . ? N5 N6 C9 N7 -3.5(6) . . . . ? Mn2 N6 C9 N7 -167.8(3) . . . . ? N5 N6 C9 C10 176.6(3) . . . . ? Mn2 N6 C9 C10 12.4(5) . . . . ? N6 C9 C10 N8 -10.2(5) . . . . ? N7 C9 C10 N8 169.9(3) . . . . ? N6 C9 C10 C11 170.8(4) . . . . ? N7 C9 C10 C11 -9.0(6) . . . . ? N8 C10 C11 C12 -1.7(6) . . . . ? C9 C10 C11 C12 177.2(4) . . . . ? C10 C11 C12 C13 -0.1(6) . . . . ? C11 C12 C13 C14 1.3(6) . . . . ? C12 C13 C14 N8 -0.8(6) . . . . ? C13 C14 N8 C10 -0.9(6) . . . . ? C13 C14 N8 Mn2 178.1(3) . . . . ? C11 C10 N8 C14 2.2(5) . . . . ? C9 C10 N8 C14 -176.8(3) . . . . ? C11 C10 N8 Mn2 -176.9(3) . . . . ? C9 C10 N8 Mn2 4.1(4) . . . . ? O11 Mn2 N8 C14 86.3(3) . . . . ? O12 Mn2 N8 C14 -88.6(3) . . . . ? N6 Mn2 N8 C14 -177.8(3) . . . . ? O2 Mn2 N8 C14 168.9(3) . . . . ? O9 Mn2 N8 C14 -1.4(3) . . . . ? O8 Mn2 N8 C14 0.0(4) . . . . ? O11 Mn2 N8 C10 -94.7(3) . . . . ? O12 Mn2 N8 C10 90.5(3) . . . . ? N6 Mn2 N8 C10 1.2(3) . . . . ? O2 Mn2 N8 C10 -12.1(3) . . . . ? O9 Mn2 N8 C10 177.6(3) . . . . ? O8 Mn2 N8 C10 179.0(2) . . . . ? O11 Mn2 O8 N10 -88.9(2) . . . . ? O12 Mn2 O8 N10 92.0(3) . . . . ? N6 Mn2 O8 N10 174.2(3) . . . . ? O2 Mn2 O8 N10 -174.6(3) . . . . ? O9 Mn2 O8 N10 -0.4(2) . . . . ? N8 Mn2 O8 N10 -2.0(3) . . . . ? O11 Mn2 O9 N10 89.6(3) . . . . ? O12 Mn2 O9 N10 -81.6(3) . . . . ? N6 Mn2 O9 N10 -171.7(3) . . . . ? O2 Mn2 O9 N10 8.0(3) . . . . ? N8 Mn2 O9 N10 179.5(3) . . . . ? O8 Mn2 O9 N10 0.4(2) . . . . ? Mn2 O8 N10 O10 179.9(4) . . . . ? Mn2 O8 N10 O9 0.7(4) . . . . ? Mn2 O9 N10 O10 -179.9(4) . . . . ? Mn2 O9 N10 O8 -0.7(4) . . . . ? O11 Mn2 O12 C16 152.7(6) . . . . ? N6 Mn2 O12 C16 11.3(4) . . . . ? O2 Mn2 O12 C16 82.0(4) . . . . ? O9 Mn2 O12 C16 -146.3(4) . . . . ? N8 Mn2 O12 C16 -58.2(5) . . . . ? O8 Mn2 O12 C16 158.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.809 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.080 #===END data_shelxl_(3) _database_code_depnum_ccdc_archive 'CCDC 228043' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.75 H48.50 Mn2 N25 O20.75' _chemical_formula_weight 1234.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2151(12) _cell_length_b 19.8918(19) _cell_length_c 22.877(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.009(2) _cell_angle_gamma 90.00 _cell_volume 5780.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7429 _exptl_absorpt_correction_T_max 0.8580 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27849 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.39 _reflns_number_total 11825 _reflns_number_gt 8959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1212P)^2^+56.4038P] 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 11825 _refine_ls_number_parameters 757 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1467 _refine_ls_R_factor_gt 0.1266 _refine_ls_wR_factor_ref 0.3598 _refine_ls_wR_factor_gt 0.3497 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _refine_ls_shift/su_max 0.003 _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 0.72264(9) 0.07916(7) 0.80852(5) 0.0382(3) Uani 1 1 d . . . Mn2 Mn 0.79082(10) 0.35589(7) 0.71801(6) 0.0406(3) Uani 1 1 d . . . O1 O 0.6822(5) 0.1837(3) 0.8160(3) 0.0496(15) Uani 1 1 d . . . O2 O 0.8817(5) 0.2739(4) 0.7670(3) 0.0591(17) Uani 1 1 d . . . O3 O 0.5923(5) 0.0633(3) 0.8492(3) 0.0598(18) Uani 1 1 d . . . O4 O 0.4837(6) -0.0059(4) 0.7928(3) 0.071(2) Uani 1 1 d . . . O5 O 0.5446(9) -0.0263(5) 0.8877(4) 0.090(3) Uani 1 1 d . . . O6 O 0.9405(6) 0.4082(4) 0.7243(3) 0.066(2) Uani 1 1 d . . . O7 O 0.9479(7) 0.3741(4) 0.6356(3) 0.074(2) Uani 1 1 d . . . O8 O 1.0294(7) 0.4634(5) 0.6741(4) 0.081(2) Uani 1 1 d . . . O9 O 0.3635(10) 0.2838(14) 0.5118(6) 0.248(13) Uani 1 1 d . . . O10 O 0.2675(17) 0.3614(15) 0.5280(11) 0.244(14) Uani 1 1 d . . . O11 O 0.2263(7) 0.3089(7) 0.4441(4) 0.107(4) Uani 1 1 d . . . O12 O 0.3597(13) 0.6330(8) -0.0134(11) 0.217(11) Uani 1 1 d . . . O13 O 0.4860(12) 0.6184(8) 0.0663(5) 0.148(5) Uani 1 1 d . . . O14 O 0.499(2) 0.6008(16) -0.0206(8) 0.286(15) Uani 1 1 d . . . O15 O 1.2479(5) 0.1824(4) 0.6955(3) 0.0615(18) Uani 1 1 d . . . O16 O 1.1094(5) 0.1618(5) 0.7247(4) 0.075(2) Uani 1 1 d . . . O17 O 1.2602(6) 0.1353(6) 0.7818(4) 0.096(3) Uani 1 1 d . . . O18 O 0.0920(7) 0.1860(5) 0.5892(4) 0.088(3) Uani 1 1 d . . . O19 O 0.1183(11) 0.0550(10) 0.4059(6) 0.106(5) Uani 0.75 1 d P . . O20 O 0.5427(15) 0.3249(10) 0.4125(6) 0.106(8) Uani 0.50 1 d P . . O21 O 0.8354(12) 0.2595(8) 0.8922(7) 0.069(4) Uani 0.50 1 d P . . O22 O 1.0368(16) 0.3055(10) 0.8686(10) 0.098(6) Uani 0.50 1 d P . . O23 O 0.3025(16) 0.1093(15) 0.4686(13) 0.136(9) Uani 0.50 1 d P . . N1 N 0.7132(5) -0.0323(4) 0.7816(3) 0.0447(16) Uani 1 1 d . . . N2 N 0.6080(8) 0.0086(5) 0.6219(4) 0.064(2) Uani 1 1 d . . . N3 N 0.6425(5) 0.0731(4) 0.7114(3) 0.0388(15) Uani 1 1 d . . . N4 N 0.6019(5) 0.1292(3) 0.6728(3) 0.0378(15) Uani 1 1 d . . . N5 N 0.4567(5) 0.1228(4) 0.7121(4) 0.0478(18) Uani 1 1 d . . . N6 N 0.4884(6) 0.3341(4) 0.6400(4) 0.054(2) Uani 1 1 d . . . N7 N 0.5876(5) 0.2734(3) 0.7254(3) 0.0407(15) Uani 1 1 d . . . N8 N 0.6432(5) 0.3351(3) 0.7437(3) 0.0403(15) Uani 1 1 d . . . N9 N 0.5633(7) 0.3397(5) 0.8211(4) 0.070(3) Uani 1 1 d . . . N10 N 0.7818(6) 0.4290(4) 0.7941(3) 0.0492(18) Uani 1 1 d . . . N11 N 0.7190(6) 0.4219(4) 0.6389(3) 0.0472(17) Uani 1 1 d . . . N12 N 0.6353(7) 0.2836(4) 0.5352(4) 0.063(2) Uani 1 1 d . . . N13 N 0.7379(5) 0.2917(3) 0.6358(3) 0.0390(15) Uani 1 1 d . . . N14 N 0.7482(5) 0.2197(3) 0.6335(3) 0.0358(14) Uani 1 1 d . . . N15 N 0.9151(6) 0.2351(4) 0.6242(4) 0.058(2) Uani 1 1 d . . . N16 N 0.8914(6) 0.0289(4) 0.7036(3) 0.0488(18) Uani 1 1 d . . . N17 N 0.8814(5) 0.1368(4) 0.7416(3) 0.0389(15) Uani 1 1 d . . . N18 N 0.8763(5) 0.1064(3) 0.7966(3) 0.0380(15) Uani 1 1 d . . . N19 N 1.0512(5) 0.1356(4) 0.8411(3) 0.0490(18) Uani 1 1 d . . . N20 N 0.8423(5) 0.0715(4) 0.9002(3) 0.0405(15) Uani 1 1 d . . . N21 N 0.5398(6) 0.0094(4) 0.8434(4) 0.0470(17) Uani 1 1 d . . . N22 N 0.9708(5) 0.4153(3) 0.6803(3) 0.0375(15) Uani 1 1 d . . . N23 N 0.2880(11) 0.3214(12) 0.4940(8) 0.141(10) Uani 1 1 d . . . N24 N 0.4362(15) 0.6149(7) 0.0146(5) 0.114(5) Uani 1 1 d . . . N25 N 1.2051(6) 0.1594(4) 0.7344(4) 0.0480(18) Uani 1 1 d . . . C1 C 0.7471(8) -0.0825(6) 0.8188(5) 0.060(3) Uani 1 1 d . . . C2 C 0.7519(10) -0.1482(6) 0.7991(6) 0.074(3) Uani 1 1 d . . . C3 C 0.7230(11) -0.1602(6) 0.7377(6) 0.083(4) Uani 1 1 d . . . C4 C 0.6875(9) -0.1059(5) 0.6974(5) 0.061(3) Uani 1 1 d . . . C5 C 0.6831(6) -0.0425(5) 0.7214(4) 0.045(2) Uani 1 1 d . . . C6 C 0.6419(6) 0.0170(4) 0.6830(4) 0.0402(18) Uani 1 1 d . . . C7 C 0.5122(6) 0.1521(4) 0.6779(4) 0.0406(18) Uani 1 1 d . . . C8 C 0.4678(6) 0.2139(4) 0.6423(4) 0.046(2) Uani 1 1 d . . . C9 C 0.5187(6) 0.2781(4) 0.6730(4) 0.0386(18) Uani 1 1 d . . . C10 C 0.6313(7) 0.3617(5) 0.7926(4) 0.048(2) Uani 1 1 d . . . C11 C 0.6989(7) 0.4209(5) 0.8161(4) 0.049(2) Uani 1 1 d . . . C12 C 0.6766(9) 0.4652(6) 0.8574(5) 0.065(3) Uani 1 1 d . . . C13 C 0.7430(10) 0.5187(6) 0.8783(5) 0.071(3) Uani 1 1 d . . . C14 C 0.8289(9) 0.5272(5) 0.8559(5) 0.064(3) Uani 1 1 d . . . C15 C 0.8450(8) 0.4824(5) 0.8138(5) 0.054(2) Uani 1 1 d . . . C16 C 0.7200(8) 0.4906(5) 0.6412(4) 0.053(2) Uani 1 1 d . . . C17 C 0.6812(9) 0.5297(5) 0.5917(5) 0.061(3) Uani 1 1 d . . . C18 C 0.6354(8) 0.5000(5) 0.5360(5) 0.059(3) Uani 1 1 d . . . C19 C 0.6318(7) 0.4303(5) 0.5323(4) 0.049(2) Uani 1 1 d . . . C20 C 0.6746(6) 0.3931(4) 0.5850(4) 0.0397(18) Uani 1 1 d . . . C21 C 0.6821(6) 0.3173(5) 0.5853(4) 0.0401(18) Uani 1 1 d . . . C22 C 0.8402(7) 0.1965(5) 0.6310(4) 0.0429(19) Uani 1 1 d . . . C23 C 0.8566(7) 0.1218(4) 0.6334(4) 0.0428(19) Uani 1 1 d . . . C24 C 0.8790(6) 0.0959(4) 0.6981(4) 0.0392(18) Uani 1 1 d . . . C25 C 0.9574(6) 0.1130(4) 0.8437(4) 0.0376(17) Uani 1 1 d . . . C26 C 0.9398(6) 0.0943(4) 0.9031(4) 0.0400(18) Uani 1 1 d . . . C27 C 1.0161(7) 0.1021(6) 0.9583(4) 0.055(2) Uani 1 1 d . . . C28 C 0.9901(8) 0.0854(6) 1.0109(4) 0.063(3) Uani 1 1 d . . . C29 C 0.8914(9) 0.0609(6) 1.0077(4) 0.065(3) Uani 1 1 d . . . C30 C 0.8199(7) 0.0538(5) 0.9511(4) 0.053(2) Uani 1 1 d . . . C31 C 0.088(4) 0.038(2) 0.4474(18) 0.28(3) Uani 0.75 1 d P . . C32 C 0.1212(13) 0.2263(11) 0.5488(7) 0.115(6) Uani 1 1 d . . . C33 C 0.825(2) 0.277(2) 0.9462(12) 0.107(11) Uani 0.50 1 d P . . C34 C 0.4555(12) 0.2950(9) 0.3844(8) 0.044(4) Uani 0.50 1 d P . . H1 H 0.6409 0.2362 0.5341 0.076 Uiso 1 1 d . . . H2 H 0.5949 0.3071 0.5000 0.076 Uiso 1 1 d . . . H3 H 1.1074 0.1394 0.8771 0.059 Uiso 1 1 d . . . H4 H 1.0610 0.1487 0.8030 0.059 Uiso 1 1 d . . . H5 H 0.5578 0.3614 0.8575 0.082 Uiso 1 1 d . . . H6 H 0.5197 0.3021 0.8060 0.082 Uiso 1 1 d . . . H7 H 0.4824 0.0832 0.7343 0.058 Uiso 1 1 d . . . H8 H 0.3920 0.1420 0.7141 0.058 Uiso 1 1 d . . . H9 H 0.9032 0.0086 0.7425 0.059 Uiso 1 1 d . . . H10 H 0.8884 0.0024 0.6689 0.059 Uiso 1 1 d . . . H11 H 0.9052 0.2829 0.6212 0.070 Uiso 1 1 d . . . H12 H 0.9809 0.2169 0.6229 0.070 Uiso 1 1 d . . . H13 H 0.5187 0.3759 0.6549 0.064 Uiso 1 1 d . . . H14 H 0.4365 0.3314 0.6019 0.064 Uiso 1 1 d . . . H15 H 0.6094 -0.0346 0.6046 0.076 Uiso 1 1 d . . . H16 H 0.5810 0.0460 0.5963 0.076 Uiso 1 1 d . . . H17 H 0.7699 -0.0741 0.8612 0.072 Uiso 1 1 d . . . H18 H 0.7736 -0.1838 0.8269 0.089 Uiso 1 1 d . . . H19 H 0.7289 -0.2042 0.7227 0.099 Uiso 1 1 d . . . H20 H 0.6669 -0.1127 0.6546 0.075 Uiso 1 1 d . . . H21 H 0.6157 0.4577 0.8713 0.079 Uiso 1 1 d . . . H22 H 0.7299 0.5493 0.9071 0.086 Uiso 1 1 d . . . H23 H 0.8773 0.5632 0.8699 0.077 Uiso 1 1 d . . . H24 H 0.9026 0.4896 0.7972 0.065 Uiso 1 1 d . . . H25 H 0.7496 0.5116 0.6791 0.063 Uiso 1 1 d . . . H26 H 0.6842 0.5771 0.5948 0.076 Uiso 1 1 d . . . H27 H 0.6072 0.5267 0.5007 0.070 Uiso 1 1 d . . . H28 H 0.6003 0.4090 0.4946 0.059 Uiso 1 1 d . . . H29 H 1.0848 0.1184 0.9597 0.067 Uiso 1 1 d . . . H30 H 1.0394 0.0916 1.0495 0.078 Uiso 1 1 d . . . H31 H 0.8724 0.0488 1.0437 0.078 Uiso 1 1 d . . . H32 H 0.7526 0.0355 0.9486 0.063 Uiso 1 1 d . . . H33 H 0.1215 0.0576 0.4871 0.196 Uiso 0.75 1 d P . . H34 H 0.0106 0.0505 0.4416 0.196 Uiso 0.75 1 d P . . H35 H 0.0870 -0.0104 0.4544 0.196 Uiso 0.75 1 d P . . H36 H 0.1516 0.2662 0.5680 0.138 Uiso 1 1 d . . . H37 H 0.1709 0.2030 0.5329 0.138 Uiso 1 1 d . . . H38 H 0.0608 0.2368 0.5161 0.138 Uiso 1 1 d . . . H39 H 0.8474 0.2395 0.9731 0.124 Uiso 0.50 1 d P . . H40 H 0.8630 0.3149 0.9606 0.124 Uiso 0.50 1 d P . . H41 H 0.7510 0.2838 0.9421 0.124 Uiso 0.50 1 d P . . H42 H 0.4213 0.2814 0.4180 0.057 Uiso 0.50 1 d P . . H43 H 0.4093 0.3207 0.3579 0.057 Uiso 0.50 1 d P . . H44 H 0.4706 0.2533 0.3688 0.057 Uiso 0.50 1 d P . . H45 H 0.6262 0.1956 0.8327 0.061 Uiso 1 1 d . . . H46 H 0.7207 0.2183 0.8027 0.061 Uiso 1 1 d . . . H47 H 0.8475 0.2349 0.7765 0.071 Uiso 1 1 d . . . H48 H 0.9566 0.2763 0.7796 0.071 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0322(6) 0.0454(7) 0.0345(6) 0.0043(5) 0.0052(5) -0.0021(5) Mn2 0.0373(6) 0.0439(7) 0.0386(7) -0.0017(5) 0.0070(5) 0.0012(5) O1 0.072(4) 0.027(3) 0.051(3) 0.004(2) 0.019(3) -0.007(3) O2 0.050(4) 0.059(4) 0.057(4) 0.009(3) -0.003(3) 0.007(3) O3 0.058(4) 0.056(4) 0.077(5) -0.020(3) 0.037(4) -0.020(3) O4 0.062(4) 0.081(5) 0.065(5) -0.019(4) 0.007(4) -0.022(4) O5 0.139(8) 0.073(6) 0.065(5) 0.016(4) 0.043(5) -0.008(5) O6 0.053(4) 0.079(5) 0.064(5) -0.004(4) 0.010(3) -0.021(4) O7 0.095(6) 0.065(5) 0.062(5) -0.005(4) 0.023(4) -0.026(4) O8 0.088(6) 0.084(6) 0.078(5) -0.017(4) 0.033(5) -0.042(5) O9 0.090(8) 0.53(4) 0.119(10) 0.132(17) 0.020(8) 0.130(16) O10 0.132(17) 0.33(4) 0.22(2) 0.01(2) -0.030(16) -0.082(19) O11 0.059(5) 0.182(11) 0.078(6) 0.059(7) 0.014(5) 0.034(6) O12 0.146(13) 0.112(11) 0.30(2) 0.054(13) -0.105(15) 0.003(9) O13 0.195(14) 0.192(14) 0.056(6) -0.020(7) 0.029(7) -0.040(11) O14 0.34(3) 0.42(4) 0.096(11) -0.103(18) 0.068(16) -0.11(3) O15 0.048(4) 0.063(4) 0.079(5) 0.014(4) 0.027(3) -0.003(3) O16 0.035(3) 0.120(7) 0.072(5) 0.017(5) 0.020(3) 0.004(4) O17 0.053(4) 0.152(10) 0.073(5) 0.030(6) 0.002(4) -0.001(5) O18 0.073(5) 0.103(7) 0.094(6) 0.031(5) 0.032(5) 0.009(5) O19 0.094(9) 0.164(16) 0.062(8) -0.015(9) 0.025(7) 0.006(9) O20 0.121(14) 0.127(15) 0.035(7) 0.054(9) -0.038(8) -0.080(12) O21 0.063(9) 0.073(10) 0.069(10) -0.007(8) 0.014(7) -0.023(8) O22 0.095(13) 0.075(12) 0.117(15) -0.021(11) 0.015(11) -0.010(10) O23 0.067(12) 0.17(2) 0.17(2) -0.03(2) 0.027(14) -0.029(14) N1 0.040(4) 0.049(4) 0.042(4) 0.002(3) 0.006(3) -0.007(3) N2 0.082(6) 0.060(5) 0.040(4) -0.001(4) 0.000(4) -0.004(5) N3 0.030(3) 0.047(4) 0.037(3) 0.000(3) 0.004(3) -0.003(3) N4 0.031(3) 0.043(4) 0.036(3) 0.008(3) 0.004(3) -0.003(3) N5 0.028(3) 0.056(5) 0.062(5) 0.010(4) 0.016(3) 0.000(3) N6 0.039(4) 0.049(4) 0.071(5) 0.022(4) 0.013(4) 0.008(3) N7 0.034(3) 0.039(4) 0.048(4) 0.004(3) 0.010(3) 0.001(3) N8 0.036(3) 0.037(4) 0.048(4) 0.001(3) 0.010(3) 0.004(3) N9 0.064(5) 0.084(7) 0.075(6) -0.026(5) 0.040(5) -0.016(5) N10 0.047(4) 0.053(5) 0.044(4) -0.001(3) 0.007(3) 0.007(3) N11 0.052(4) 0.049(4) 0.042(4) 0.001(3) 0.016(3) -0.003(3) N12 0.083(6) 0.037(4) 0.051(5) 0.003(3) -0.010(4) 0.002(4) N13 0.037(3) 0.034(3) 0.042(4) 0.005(3) 0.005(3) 0.004(3) N14 0.032(3) 0.032(3) 0.041(3) 0.000(3) 0.006(3) 0.005(3) N15 0.046(4) 0.054(5) 0.083(6) 0.016(4) 0.035(4) 0.006(4) N16 0.046(4) 0.055(5) 0.046(4) 0.007(3) 0.014(3) 0.001(3) N17 0.029(3) 0.048(4) 0.038(3) 0.010(3) 0.008(3) -0.001(3) N18 0.032(3) 0.042(4) 0.038(3) 0.008(3) 0.006(3) 0.002(3) N19 0.030(3) 0.068(5) 0.047(4) 0.000(4) 0.007(3) -0.002(3) N20 0.039(3) 0.045(4) 0.037(3) 0.004(3) 0.008(3) 0.001(3) N21 0.045(4) 0.049(4) 0.053(4) 0.000(4) 0.023(4) -0.011(3) N22 0.033(3) 0.028(3) 0.046(4) 0.001(3) 0.001(3) -0.010(3) N23 0.055(7) 0.26(3) 0.108(12) 0.124(16) 0.017(8) 0.018(11) N24 0.191(16) 0.091(9) 0.043(6) 0.001(6) 0.000(8) 0.005(10) N25 0.040(4) 0.044(4) 0.062(5) 0.000(4) 0.018(4) -0.004(3) C1 0.059(6) 0.059(6) 0.054(6) 0.010(5) 0.005(5) -0.006(5) C2 0.075(7) 0.055(6) 0.079(8) 0.016(6) -0.002(6) 0.004(6) C3 0.100(10) 0.050(6) 0.082(8) -0.010(6) -0.004(7) -0.001(6) C4 0.066(6) 0.053(6) 0.058(6) -0.007(5) 0.006(5) -0.012(5) C5 0.035(4) 0.051(5) 0.046(5) 0.002(4) 0.007(4) -0.013(4) C6 0.028(4) 0.051(5) 0.038(4) 0.003(4) 0.004(3) -0.003(3) C7 0.032(4) 0.042(4) 0.041(4) 0.004(3) 0.000(3) -0.009(3) C8 0.031(4) 0.043(5) 0.053(5) 0.011(4) -0.004(3) -0.001(3) C9 0.029(4) 0.037(4) 0.052(5) 0.012(4) 0.015(3) 0.004(3) C10 0.041(4) 0.051(5) 0.052(5) 0.004(4) 0.014(4) 0.016(4) C11 0.045(5) 0.050(5) 0.046(5) 0.005(4) 0.003(4) 0.017(4) C12 0.060(6) 0.074(7) 0.060(6) -0.011(5) 0.015(5) 0.022(5) C13 0.074(7) 0.062(7) 0.069(7) -0.031(6) 0.005(6) 0.008(6) C14 0.074(7) 0.041(5) 0.065(6) -0.009(5) -0.001(5) 0.001(5) C15 0.052(5) 0.049(5) 0.056(6) -0.009(4) 0.005(4) -0.008(4) C16 0.063(6) 0.045(5) 0.049(5) 0.005(4) 0.013(4) -0.004(4) C17 0.081(7) 0.043(5) 0.066(6) 0.001(5) 0.032(6) 0.003(5) C18 0.059(6) 0.058(6) 0.063(6) 0.019(5) 0.024(5) 0.005(5) C19 0.050(5) 0.053(5) 0.042(5) 0.010(4) 0.009(4) 0.000(4) C20 0.037(4) 0.042(4) 0.041(4) 0.004(3) 0.011(3) -0.001(3) C21 0.032(4) 0.052(5) 0.036(4) -0.002(4) 0.007(3) -0.006(3) C22 0.043(4) 0.053(5) 0.035(4) 0.004(4) 0.015(3) -0.004(4) C23 0.046(5) 0.041(4) 0.044(4) 0.007(4) 0.017(4) 0.007(4) C24 0.022(3) 0.048(5) 0.048(5) 0.012(4) 0.011(3) 0.007(3) C25 0.033(4) 0.040(4) 0.038(4) 0.001(3) 0.007(3) 0.002(3) C26 0.042(4) 0.038(4) 0.036(4) 0.007(3) 0.004(3) -0.005(3) C27 0.042(5) 0.073(7) 0.044(5) 0.002(5) 0.001(4) -0.004(4) C28 0.056(6) 0.082(8) 0.039(5) 0.007(5) -0.006(4) -0.005(5) C29 0.065(6) 0.086(8) 0.039(5) 0.011(5) 0.008(4) -0.004(6) C30 0.046(5) 0.064(6) 0.046(5) 0.009(4) 0.008(4) -0.004(4) C31 0.37(7) 0.20(4) 0.15(3) 0.03(3) -0.12(4) -0.17(4) C32 0.098(11) 0.164(17) 0.087(10) 0.026(11) 0.033(9) -0.021(11) C33 0.069(16) 0.19(4) 0.054(14) -0.020(18) 0.000(12) 0.009(19) C34 0.032(8) 0.051(10) 0.050(9) -0.013(8) 0.014(7) 0.007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O1 2.165(6) . ? Mn1 N3 2.186(7) . ? Mn1 N18 2.190(7) . ? Mn1 O3 2.195(6) . ? Mn1 N20 2.257(7) . ? Mn1 N1 2.295(8) . ? Mn2 O2 2.148(7) . ? Mn2 O6 2.205(7) . ? Mn2 N13 2.220(7) . ? Mn2 N8 2.225(7) . ? Mn2 N11 2.226(8) . ? Mn2 N10 2.297(8) . ? O3 N21 1.263(9) . ? O4 N21 1.229(10) . ? O5 N21 1.225(10) . ? O6 N22 1.189(10) . ? O7 N22 1.280(10) . ? O8 N22 1.263(10) . ? O9 N23 1.22(2) . ? O10 N23 1.19(3) . ? O11 N23 1.23(2) . ? O12 N24 1.098(18) . ? O13 N24 1.186(15) . ? O14 N24 1.34(3) . ? O15 N25 1.265(10) . ? O16 N25 1.223(9) . ? O17 N25 1.225(11) . ? O18 C32 1.359(17) . ? O19 C31 1.18(5) . ? O20 C34 1.30(2) . ? O21 C33 1.33(3) . ? N1 C1 1.310(12) . ? N1 C5 1.339(11) . ? N2 C6 1.354(11) . ? N3 C6 1.289(11) . ? N3 N4 1.432(9) . ? N4 C7 1.304(11) . ? N5 C7 1.344(11) . ? N6 C9 1.345(10) . ? N7 C9 1.292(11) . ? N7 N8 1.432(10) . ? N8 C10 1.287(11) . ? N9 C10 1.322(12) . ? N10 C11 1.335(12) . ? N10 C15 1.349(12) . ? N11 C20 1.340(11) . ? N11 C16 1.366(12) . ? N12 C21 1.326(11) . ? N13 C21 1.292(10) . ? N13 N14 1.440(9) . ? N14 C22 1.317(11) . ? N15 C22 1.296(11) . ? N16 C24 1.345(11) . ? N17 C24 1.277(11) . ? N17 N18 1.416(9) . ? N18 C25 1.299(10) . ? N19 C25 1.335(10) . ? N20 C30 1.327(11) . ? N20 C26 1.349(10) . ? C1 C2 1.389(16) . ? C2 C3 1.370(18) . ? C3 C4 1.414(16) . ? C4 C5 1.383(14) . ? C5 C6 1.486(12) . ? C7 C8 1.502(11) . ? C8 C9 1.522(12) . ? C10 C11 1.485(14) . ? C11 C12 1.382(14) . ? C12 C13 1.379(17) . ? C13 C14 1.379(17) . ? C14 C15 1.372(14) . ? C16 C17 1.355(14) . ? C17 C18 1.383(15) . ? C18 C19 1.388(14) . ? C19 C20 1.395(12) . ? C20 C21 1.510(12) . ? C22 C23 1.500(12) . ? C23 C24 1.518(11) . ? C25 C26 1.489(11) . ? C26 C27 1.391(12) . ? C27 C28 1.380(14) . ? C28 C29 1.374(15) . ? C29 C30 1.384(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 N3 94.2(3) . . ? O1 Mn1 N18 91.7(3) . . ? N3 Mn1 N18 95.4(2) . . ? O1 Mn1 O3 82.3(3) . . ? N3 Mn1 O3 101.9(3) . . ? N18 Mn1 O3 162.1(3) . . ? O1 Mn1 N20 96.7(3) . . ? N3 Mn1 N20 163.7(3) . . ? N18 Mn1 N20 72.3(2) . . ? O3 Mn1 N20 91.5(3) . . ? O1 Mn1 N1 162.3(3) . . ? N3 Mn1 N1 72.5(3) . . ? N18 Mn1 N1 100.9(3) . . ? O3 Mn1 N1 89.1(3) . . ? N20 Mn1 N1 99.0(3) . . ? O2 Mn2 O6 87.8(3) . . ? O2 Mn2 N13 90.3(3) . . ? O6 Mn2 N13 113.2(3) . . ? O2 Mn2 N8 97.2(3) . . ? O6 Mn2 N8 155.1(3) . . ? N13 Mn2 N8 91.3(3) . . ? O2 Mn2 N11 157.5(3) . . ? O6 Mn2 N11 87.0(3) . . ? N13 Mn2 N11 71.8(3) . . ? N8 Mn2 N11 96.7(3) . . ? O2 Mn2 N10 102.9(3) . . ? O6 Mn2 N10 83.4(3) . . ? N13 Mn2 N10 159.4(3) . . ? N8 Mn2 N10 71.6(3) . . ? N11 Mn2 N10 98.2(3) . . ? N21 O3 Mn1 123.4(5) . . ? N22 O6 Mn2 120.4(5) . . ? C1 N1 C5 120.3(9) . . ? C1 N1 Mn1 125.4(7) . . ? C5 N1 Mn1 113.7(6) . . ? C6 N3 N4 114.5(6) . . ? C6 N3 Mn1 119.6(6) . . ? N4 N3 Mn1 125.3(5) . . ? C7 N4 N3 114.3(6) . . ? C9 N7 N8 112.5(7) . . ? C10 N8 N7 115.6(7) . . ? C10 N8 Mn2 118.6(6) . . ? N7 N8 Mn2 119.9(5) . . ? C11 N10 C15 117.8(8) . . ? C11 N10 Mn2 115.4(6) . . ? C15 N10 Mn2 126.4(7) . . ? C20 N11 C16 117.5(8) . . ? C20 N11 Mn2 118.4(6) . . ? C16 N11 Mn2 124.1(6) . . ? C21 N13 N14 113.2(7) . . ? C21 N13 Mn2 119.9(6) . . ? N14 N13 Mn2 126.4(5) . . ? C22 N14 N13 116.6(7) . . ? C24 N17 N18 115.1(7) . . ? C25 N18 N17 117.6(7) . . ? C25 N18 Mn1 120.2(5) . . ? N17 N18 Mn1 119.3(4) . . ? C30 N20 C26 119.2(7) . . ? C30 N20 Mn1 124.4(6) . . ? C26 N20 Mn1 116.0(5) . . ? O5 N21 O4 121.0(9) . . ? O5 N21 O3 120.3(9) . . ? O4 N21 O3 118.7(8) . . ? O6 N22 O8 123.0(8) . . ? O6 N22 O7 122.6(7) . . ? O8 N22 O7 114.4(8) . . ? O10 N23 O9 120(2) . . ? O10 N23 O11 121.8(19) . . ? O9 N23 O11 117(2) . . ? O12 N24 O13 137(2) . . ? O12 N24 O14 110.1(19) . . ? O13 N24 O14 110(2) . . ? O16 N25 O17 120.7(8) . . ? O16 N25 O15 119.8(8) . . ? O17 N25 O15 119.5(8) . . ? N1 C1 C2 123.0(10) . . ? C3 C2 C1 118.2(10) . . ? C2 C3 C4 119.0(11) . . ? C5 C4 C3 118.7(10) . . ? N1 C5 C4 120.9(9) . . ? N1 C5 C6 116.3(8) . . ? C4 C5 C6 122.7(8) . . ? N3 C6 N2 125.5(8) . . ? N3 C6 C5 116.2(7) . . ? N2 C6 C5 118.3(8) . . ? N4 C7 N5 123.8(8) . . ? N4 C7 C8 117.8(7) . . ? N5 C7 C8 118.4(7) . . ? C7 C8 C9 112.3(7) . . ? N7 C9 N6 127.3(8) . . ? N7 C9 C8 118.4(7) . . ? N6 C9 C8 114.3(7) . . ? N8 C10 N9 123.8(9) . . ? N8 C10 C11 115.8(8) . . ? N9 C10 C11 120.4(9) . . ? N10 C11 C12 122.1(10) . . ? N10 C11 C10 115.7(8) . . ? C12 C11 C10 122.2(9) . . ? C13 C12 C11 119.6(11) . . ? C14 C13 C12 118.4(10) . . ? C15 C14 C13 119.0(10) . . ? N10 C15 C14 122.9(10) . . ? C17 C16 N11 123.0(9) . . ? C16 C17 C18 119.6(10) . . ? C17 C18 C19 118.8(9) . . ? C18 C19 C20 118.6(9) . . ? N11 C20 C19 122.6(8) . . ? N11 C20 C21 114.3(7) . . ? C19 C20 C21 123.0(8) . . ? N13 C21 N12 126.1(8) . . ? N13 C21 C20 114.7(7) . . ? N12 C21 C20 119.1(7) . . ? N15 C22 N14 122.8(9) . . ? N15 C22 C23 119.0(8) . . ? N14 C22 C23 118.2(7) . . ? C22 C23 C24 111.0(7) . . ? N17 C24 N16 125.6(8) . . ? N17 C24 C23 120.0(7) . . ? N16 C24 C23 114.4(8) . . ? N18 C25 N19 124.1(8) . . ? N18 C25 C26 115.5(7) . . ? N19 C25 C26 120.4(7) . . ? N20 C26 C27 121.7(8) . . ? N20 C26 C25 115.2(7) . . ? C27 C26 C25 123.0(8) . . ? C28 C27 C26 118.1(9) . . ? C29 C28 C27 120.0(9) . . ? C28 C29 C30 118.6(9) . . ? N20 C30 C29 122.3(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.153 _refine_diff_density_min -1.122 _refine_diff_density_rms 0.143 #===END data_sqz_(4) _database_code_depnum_ccdc_archive 'CCDC 228044' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H60 Br6 Co4 N32 O12' _chemical_formula_weight 2088.54 _refine_special_details ; Both anions (Br) and solvent show considerable disorder with both occurring in many partially occupied sites. The asymmetric unit contains 6 Br in total over 10 sites, 2 fully occupied, 2 sites are adjacent to one another and were refined to give an occupancy summing to 1 (Br3 and Br3'). One water molecule is included explicitly in the model and a number of partially occupied sites were also present. however these could not be satisfactorily modelled and SQUEEZE (Platon) was used to account for this density. A total of 240 electrons per unit cell was calculated in the voids in the structure, corresponding to 3 molecules of H20 per Co tetramer. There is also disorder present in part of one ligand which was modelled over 2 sites with occupancies 0.70 and 0.30. All non-H atoms were refined with anisotropic adps except for the partially occupied atom sites in the disordered ligand. ; 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' Br Br -0.2901 2.4595 '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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.664(2) _cell_length_b 17.8963(12) _cell_length_c 35.999(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.953(1) _cell_angle_gamma 90.00 _cell_volume 18758(2) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8027 _cell_measurement_theta_min 3.35 _cell_measurement_theta_max 24.7 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8272 _exptl_absorpt_coefficient_mu 3.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.460 _exptl_absorpt_correction_T_max 0.588 _exptl_absorpt_process_details 'XPREP, SHELXTL v6.12' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART 1K CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41461 _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_sigmaI/netI 0.0884 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16359 _reflns_number_gt 9140 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_data_reduction 'Bruker SAINT version 6.36a (Bruker, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement ; SHELXL-97 (Sheldrick, 1997); SQUEEZE - Sluis, P. v.d.; Spek, A. L. Acta Crystallogr., Sect A 1990, 46, 194-201.; PLATON (Spek, 2002) ; _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1032P)^2] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed, H2O not located' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16359 _refine_ls_number_parameters 992 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1770 _refine_ls_wR_factor_gt 0.1622 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _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 0.06431(3) 0.21752(4) 0.22151(3) 0.0310(2) Uani 1 1 d . . . Co2 Co -0.08032(3) -0.10963(4) 0.18282(3) 0.0308(2) Uani 1 1 d . . . Co3 Co 0.10958(3) 0.18296(5) 0.42343(3) 0.0330(2) Uani 1 1 d . . . Co4 Co -0.05891(3) -0.07567(4) 0.37613(3) 0.0323(2) Uani 1 1 d . . . O1 O 0.00131(13) 0.1509(2) 0.20117(12) 0.0296(9) Uani 1 1 d . . . O2 O -0.01782(13) -0.0446(2) 0.19626(12) 0.0303(9) Uani 1 1 d . . . O3 O 0.04607(14) 0.1468(2) 0.40672(12) 0.0334(10) Uani 1 1 d . A . O4 O 0.00230(14) -0.0380(2) 0.39473(13) 0.0332(10) Uani 1 1 d . A . O5 O 0.08321(14) 0.1970(2) 0.28661(12) 0.0317(10) Uani 1 1 d . A . O6 O 0.10033(13) 0.1811(2) 0.36540(12) 0.0321(10) Uani 1 1 d . A . O7 O -0.07773(14) -0.0896(2) 0.24312(12) 0.0335(10) Uani 1 1 d . . . O8 O -0.07006(14) -0.0728(2) 0.31892(12) 0.0320(10) Uani 1 1 d . . . N1 N 0.13383(18) 0.2262(3) 0.23144(16) 0.0384(13) Uani 1 1 d . . . N2 N 0.14603(18) 0.0262(3) 0.24121(18) 0.0463(15) Uani 1 1 d . . . H2B H 0.1288 -0.0135 0.2378 0.056 Uiso 1 1 calc R . . H2C H 0.1759 0.0214 0.2508 0.056 Uiso 1 1 calc R . . N3 N 0.08375(16) 0.1110(2) 0.21753(15) 0.0290(11) Uani 1 1 d . . . N4 N 0.05144(16) 0.0561(3) 0.21199(15) 0.0292(12) Uani 1 1 d . . . N5 N -0.06846(16) 0.0510(2) 0.17977(15) 0.0284(11) Uani 1 1 d . . . H5A H -0.0740 0.0991 0.1794 0.034 Uiso 1 1 calc R . . N6 N -0.10276(18) -0.0029(3) 0.16671(16) 0.0344(12) Uani 1 1 d . . . N7 N -0.16069(19) 0.0840(3) 0.15750(19) 0.0489(15) Uani 1 1 d . . . H7A H -0.1418 0.1223 0.1651 0.059 Uiso 1 1 calc R . . H7B H -0.1900 0.0908 0.1503 0.059 Uiso 1 1 calc R . . N8 N -0.15391(18) -0.1161(3) 0.15072(17) 0.0406(14) Uani 1 1 d . . . N9 N 0.1731(3) 0.1900(5) 0.4391(3) 0.039(3) Uiso 0.70 1 d P A 1 N10 N 0.1759(4) -0.0130(6) 0.4506(3) 0.057(3) Uiso 0.70 1 d P A 1 H10A H 0.1552 -0.0476 0.4470 0.069 Uiso 0.70 1 calc PR A 1 H10B H 0.2045 -0.0259 0.4578 0.069 Uiso 0.70 1 calc PR A 1 N11 N 0.12096(18) 0.0796(3) 0.43455(17) 0.0428(14) Uani 1 1 d . A . N12 N 0.08286(19) 0.0331(3) 0.42386(17) 0.0437(14) Uani 1 1 d . . . H12B H 0.0835 -0.0159 0.4262 0.052 Uiso 1 1 calc R A . N13 N -0.03511(17) 0.0754(3) 0.38890(15) 0.0318(12) Uani 1 1 d . A . N14 N -0.07157(18) 0.0245(3) 0.37829(15) 0.0325(12) Uani 1 1 d . . . N15 N -0.1275(2) 0.1167(3) 0.36382(19) 0.0520(16) Uani 1 1 d . . . H15C H -0.1074 0.1532 0.3704 0.062 Uiso 1 1 calc R . . H15D H -0.1568 0.1268 0.3555 0.062 Uiso 1 1 calc R . . N16 N -0.12404(18) -0.0854(3) 0.35809(16) 0.0375(13) Uani 1 1 d . . . N17 N 0.03999(18) 0.2912(3) 0.16916(17) 0.0386(13) Uani 1 1 d . . . N18 N 0.0406(2) 0.4467(3) 0.23358(18) 0.0523(16) Uani 1 1 d . . . H18C H 0.0449 0.4546 0.2592 0.063 Uiso 1 1 calc R . . H18D H 0.0337 0.4842 0.2160 0.063 Uiso 1 1 calc R . . N19 N 0.05459(18) 0.3176(3) 0.24378(16) 0.0369(13) Uani 1 1 d . . . N20 N 0.06323(18) 0.3196(3) 0.28532(16) 0.0358(13) Uani 1 1 d . A . H20A H 0.0594 0.3597 0.2976 0.043 Uiso 1 1 calc R . . N21 N 0.08335(19) 0.3069(3) 0.36822(16) 0.0394(13) Uani 1 1 d . . . N22 N 0.09350(18) 0.2846(3) 0.40879(17) 0.0394(13) Uani 1 1 d . A . N23 N 0.0895(2) 0.4069(4) 0.4303(2) 0.074(2) Uani 1 1 d . A . H23A H 0.0824 0.4256 0.4055 0.089 Uiso 1 1 calc R . . H23B H 0.0921 0.4366 0.4507 0.089 Uiso 1 1 calc R . . N24 N 0.1181(2) 0.2221(4) 0.47731(18) 0.0548(17) Uani 1 1 d . A . N25 N -0.07341(18) -0.1837(3) 0.14006(16) 0.0361(13) Uani 1 1 d . . . N26 N -0.0568(2) -0.3396(3) 0.20929(18) 0.0597(19) Uani 1 1 d . . . H26B H -0.0531 -0.3470 0.2348 0.072 Uiso 1 1 calc R . . H26C H -0.0567 -0.3779 0.1940 0.072 Uiso 1 1 calc R . . N27 N -0.06327(18) -0.2106(3) 0.21333(15) 0.0323(12) Uani 1 1 d . . . N28 N -0.05818(17) -0.2112(3) 0.25355(16) 0.0333(12) Uani 1 1 d . . . H28B H -0.0501 -0.2513 0.2694 0.040 Uiso 1 1 calc R . . N29 N -0.04770(19) -0.1970(3) 0.33374(16) 0.0364(13) Uani 1 1 d . . . N30 N -0.04486(17) -0.1742(3) 0.37177(15) 0.0323(12) Uani 1 1 d . . . N31 N -0.0258(2) -0.2922(3) 0.40219(19) 0.0606(19) Uani 1 1 d . . . H31B H -0.0273 -0.3126 0.3794 0.073 Uiso 1 1 calc R . . H31C H -0.0187 -0.3197 0.4245 0.073 Uiso 1 1 calc R . . N32 N -0.04465(18) -0.1069(3) 0.43175(16) 0.0360(13) Uani 1 1 d . . . C1 C 0.1573(3) 0.2892(4) 0.2338(2) 0.0501(19) Uani 1 1 d . . . H1A H 0.1416 0.3356 0.2297 0.060 Uiso 1 1 calc R . . C2 C 0.2037(3) 0.2903(5) 0.2419(2) 0.059(2) Uani 1 1 d . . . H2A H 0.2191 0.3359 0.2431 0.071 Uiso 1 1 calc R . . C3 C 0.2257(3) 0.2230(5) 0.2480(2) 0.056(2) Uani 1 1 d . . . H3A H 0.2572 0.2213 0.2542 0.068 Uiso 1 1 calc R . . C4 C 0.2023(2) 0.1583(4) 0.2453(2) 0.0509(19) Uani 1 1 d . . . H4A H 0.2173 0.1114 0.2490 0.061 Uiso 1 1 calc R . . C5 C 0.1568(2) 0.1617(3) 0.23703(19) 0.0351(15) Uani 1 1 d . . . C6 C 0.1269(2) 0.0935(4) 0.23192(19) 0.0359(16) Uani 1 1 d . . . C7 C 0.0105(2) 0.0832(3) 0.20292(17) 0.0239(13) Uani 1 1 d . . . C8 C -0.0268(2) 0.0234(3) 0.19278(17) 0.0249(13) Uani 1 1 d . . . C9 C -0.1451(2) 0.0163(3) 0.1569(2) 0.0348(15) Uani 1 1 d . . . C10 C -0.1758(2) -0.0500(4) 0.1446(2) 0.0424(17) Uani 1 1 d . . . C11 C -0.2226(3) -0.0432(5) 0.1277(3) 0.068(2) Uani 1 1 d . . . H11A H -0.2364 0.0046 0.1248 0.081 Uiso 1 1 calc R . . C12 C -0.2498(3) -0.1082(5) 0.1148(4) 0.098(4) Uani 1 1 d . . . H12A H -0.2823 -0.1057 0.1029 0.118 Uiso 1 1 calc R . . C13 C -0.2271(3) -0.1764(5) 0.1201(3) 0.084(3) Uani 1 1 d . . . H13A H -0.2442 -0.2215 0.1116 0.100 Uiso 1 1 calc R . . C14 C -0.1800(3) -0.1779(4) 0.1378(3) 0.064(2) Uani 1 1 d . . . H14A H -0.1652 -0.2248 0.1411 0.077 Uiso 1 1 calc R . . C15 C 0.1983(4) 0.2495(6) 0.4396(3) 0.045(3) Uiso 0.70 1 d P A 1 H15A H 0.1834 0.2966 0.4321 0.054 Uiso 0.70 1 calc PR A 1 C16 C 0.2444(4) 0.2463(8) 0.4505(4) 0.060(3) Uiso 0.70 1 d P A 1 H16A H 0.2613 0.2900 0.4512 0.072 Uiso 0.70 1 calc PR A 1 C17 C 0.2657(4) 0.1744(9) 0.4605(3) 0.045(3) Uiso 0.70 1 d P A 1 H17A H 0.2973 0.1697 0.4672 0.054 Uiso 0.70 1 calc PR A 1 C18 C 0.2414(4) 0.1121(7) 0.4605(4) 0.055(3) Uiso 0.70 1 d P A 1 H18A H 0.2558 0.0646 0.4674 0.066 Uiso 0.70 1 calc PR A 1 C19 C 0.1949(4) 0.1200(9) 0.4501(3) 0.038(3) Uiso 0.70 1 d P A 1 C20 C 0.1638(4) 0.0590(7) 0.4453(4) 0.041(3) Uiso 0.70 1 d P A 1 C21 C 0.0463(2) 0.0750(3) 0.40973(19) 0.0336(15) Uani 1 1 d . A . C22 C 0.0016(2) 0.0351(3) 0.39706(18) 0.0324(15) Uani 1 1 d . . . C23 C -0.1139(2) 0.0465(4) 0.3664(2) 0.0376(16) Uani 1 1 d . . . C24 C -0.1449(2) -0.0178(4) 0.3549(2) 0.0415(17) Uani 1 1 d . . . C25 C -0.1920(3) -0.0136(5) 0.3417(2) 0.059(2) Uani 1 1 d . . . H25A H -0.2067 0.0334 0.3389 0.070 Uiso 1 1 calc R . . C26 C -0.2174(3) -0.0803(5) 0.3326(3) 0.065(2) Uani 1 1 d . . . H26A H -0.2496 -0.0789 0.3236 0.078 Uiso 1 1 calc R . . C27 C -0.1959(3) -0.1465(5) 0.3366(2) 0.056(2) Uani 1 1 d . . . H27A H -0.2129 -0.1918 0.3310 0.068 Uiso 1 1 calc R . . C28 C -0.1487(3) -0.1480(4) 0.3491(2) 0.0472(18) Uani 1 1 d . . . H28A H -0.1340 -0.1947 0.3511 0.057 Uiso 1 1 calc R . . C29 C 0.0341(2) 0.2727(4) 0.1307(2) 0.0450(18) Uani 1 1 d . . . H29A H 0.0360 0.2215 0.1245 0.054 Uiso 1 1 calc R . . C30 C 0.0252(3) 0.3258(4) 0.0996(2) 0.055(2) Uani 1 1 d . . . H30A H 0.0224 0.3117 0.0731 0.066 Uiso 1 1 calc R . . C31 C 0.0207(3) 0.3992(4) 0.1085(2) 0.064(2) Uani 1 1 d . . . H31A H 0.0133 0.4364 0.0876 0.077 Uiso 1 1 calc R . . C32 C 0.0272(3) 0.4191(4) 0.1487(2) 0.057(2) Uani 1 1 d . . . H32A H 0.0249 0.4697 0.1555 0.068 Uiso 1 1 calc R . . C33 C 0.0370(2) 0.3629(3) 0.1779(2) 0.0341(15) Uani 1 1 d . . . C34 C 0.0447(2) 0.3770(3) 0.2213(2) 0.0363(16) Uani 1 1 d . . . C35 C 0.0780(2) 0.2538(3) 0.3048(2) 0.0339(15) Uani 1 1 d . . . C36 C 0.0875(2) 0.2471(3) 0.34881(19) 0.0333(15) Uani 1 1 d . A . C37 C 0.0964(3) 0.3335(4) 0.4369(2) 0.052(2) Uani 1 1 d . . . C38 C 0.1084(3) 0.2972(5) 0.4772(2) 0.062(2) Uani 1 1 d . A . C39 C 0.1104(3) 0.3325(6) 0.5122(3) 0.084(3) Uani 1 1 d . . . H39A H 0.1026 0.3837 0.5120 0.101 Uiso 1 1 calc R A . C40 C 0.1254(4) 0.2861(8) 0.5497(3) 0.099(4) Uani 1 1 d . A . H40A H 0.1276 0.3073 0.5747 0.118 Uiso 1 1 calc R . . C41 C 0.1361(4) 0.2137(9) 0.5490(3) 0.104(4) Uani 1 1 d . . . H41A H 0.1471 0.1848 0.5738 0.125 Uiso 1 1 calc R A . C42 C 0.1312(3) 0.1811(6) 0.5123(3) 0.080(3) Uani 1 1 d . A . H42A H 0.1372 0.1293 0.5118 0.096 Uiso 1 1 calc R . . C43 C -0.0790(3) -0.1661(4) 0.1020(2) 0.0518(19) Uani 1 1 d . . . H43A H -0.0811 -0.1148 0.0945 0.062 Uiso 1 1 calc R . . C44 C -0.0820(3) -0.2195(4) 0.0729(2) 0.055(2) Uani 1 1 d . . . H44A H -0.0860 -0.2053 0.0460 0.067 Uiso 1 1 calc R . . C45 C -0.0790(3) -0.2931(4) 0.0841(2) 0.062(2) Uani 1 1 d . . . H45A H -0.0818 -0.3308 0.0644 0.074 Uiso 1 1 calc R . . C46 C -0.0719(3) -0.3133(4) 0.1236(2) 0.0482(19) Uani 1 1 d . . . H46A H -0.0689 -0.3644 0.1317 0.058 Uiso 1 1 calc R . . C47 C -0.0694(2) -0.2577(3) 0.1509(2) 0.0358(15) Uani 1 1 d . . . C48 C -0.0624(2) -0.2717(3) 0.1942(2) 0.0367(16) Uani 1 1 d . . . C49 C -0.0665(2) -0.1454(3) 0.26617(19) 0.0298(14) Uani 1 1 d . . . C50 C -0.0608(2) -0.1395(3) 0.3096(2) 0.0322(15) Uani 1 1 d . . . C51 C -0.0341(2) -0.2205(4) 0.4029(2) 0.0434(17) Uani 1 1 d . . . C52 C -0.0324(2) -0.1805(4) 0.4396(2) 0.0438(17) Uani 1 1 d . . . C53 C -0.0180(3) -0.2118(4) 0.4788(2) 0.0513(19) Uani 1 1 d . . . H53A H -0.0085 -0.2625 0.4842 0.062 Uiso 1 1 calc R . . C54 C -0.0180(3) -0.1642(4) 0.5106(2) 0.055(2) Uani 1 1 d . . . H54A H -0.0079 -0.1830 0.5380 0.066 Uiso 1 1 calc R . . C55 C -0.0324(2) -0.0913(4) 0.5019(2) 0.0494(19) Uani 1 1 d . . . H55A H -0.0336 -0.0598 0.5226 0.059 Uiso 1 1 calc R . . C56 C -0.0452(2) -0.0652(4) 0.4618(2) 0.0418(17) Uani 1 1 d . . . H56A H -0.0549 -0.0147 0.4557 0.050 Uiso 1 1 calc R . . N9' N 0.1831(6) 0.1624(13) 0.4473(5) 0.017(4) Uiso 0.30 1 d P A 2 N10' N 0.1669(8) -0.0277(13) 0.4621(7) 0.057(7) Uiso 0.30 1 d P A 2 H10C H 0.1437 -0.0583 0.4564 0.068 Uiso 0.30 1 calc PR A 2 H10D H 0.1953 -0.0447 0.4744 0.068 Uiso 0.30 1 calc PR A 2 C15' C 0.2122(8) 0.2142(13) 0.4471(7) 0.033(5) Uiso 0.30 1 d P A 2 H15B H 0.2001 0.2632 0.4393 0.040 Uiso 0.30 1 calc PR A 2 C16' C 0.2580(7) 0.2054(16) 0.4568(6) 0.020(5) Uiso 0.30 1 d P A 2 H16B H 0.2780 0.2447 0.4578 0.024 Uiso 0.30 1 calc PR A 2 C17' C 0.2716(10) 0.1248(17) 0.4656(8) 0.051(7) Uiso 0.30 1 d P A 2 H17B H 0.3013 0.1097 0.4698 0.062 Uiso 0.30 1 calc PR A 2 C18' C 0.2410(9) 0.0706(16) 0.4677(8) 0.050(6) Uiso 0.30 1 d P A 2 H18B H 0.2512 0.0210 0.4763 0.060 Uiso 0.30 1 calc PR A 2 C19' C 0.1964(9) 0.0908(17) 0.4572(8) 0.041(7) Uiso 0.30 1 d P A 2 C20' C 0.1597(10) 0.0390(17) 0.4530(9) 0.043(8) Uiso 0.30 1 d P A 2 Br3 Br 0.15946(6) -0.00688(9) 0.55056(5) 0.0748(4) Uani 0.60 1 d P B 1 Br3' Br 0.09035(13) -0.08683(13) 0.50385(10) 0.1093(11) Uani 0.40 1 d P C 2 Br1 Br 0.04550(3) 0.61719(4) 0.19445(2) 0.0527(2) Uani 1 1 d . . . Br2 Br -0.08230(3) -0.50985(4) 0.16245(2) 0.0579(2) Uani 1 1 d . . . Br4 Br -0.17681(5) -0.17670(10) 0.24129(4) 0.0984(5) Uani 0.75 1 d P . . Br5 Br -0.19615(7) 0.29167(12) 0.15453(6) 0.0788(6) Uani 0.50 1 d P . . Br6 Br -0.26272(8) 0.15091(12) 0.13923(7) 0.0915(6) Uani 0.50 1 d P . . Br7 Br 0.13856(12) 0.53705(14) 0.50928(8) 0.1195(10) Uani 0.45 1 d P . . Br8 Br -0.01345(11) -0.41951(14) 0.47520(9) 0.1089(9) Uani 0.45 1 d P . . Br9 Br -0.25048(18) -0.0291(2) 0.22362(14) 0.1441(16) Uani 0.35 1 d P . . O1W O -0.2128(2) 0.1747(4) 0.3558(2) 0.103(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0407(5) 0.0177(4) 0.0383(5) -0.0003(4) 0.0211(4) -0.0052(4) Co2 0.0412(5) 0.0175(4) 0.0391(5) -0.0016(4) 0.0229(4) -0.0036(4) Co3 0.0368(5) 0.0305(5) 0.0347(5) -0.0049(4) 0.0190(4) -0.0079(4) Co4 0.0435(5) 0.0243(4) 0.0353(5) -0.0043(4) 0.0234(4) -0.0056(4) O1 0.041(3) 0.015(2) 0.035(2) 0.0020(17) 0.019(2) 0.0007(18) O2 0.036(2) 0.015(2) 0.044(3) 0.0024(18) 0.021(2) -0.0003(17) O3 0.042(3) 0.023(2) 0.039(3) -0.0008(19) 0.021(2) -0.0035(19) O4 0.039(3) 0.023(2) 0.044(3) -0.0044(19) 0.024(2) -0.0047(18) O5 0.042(3) 0.019(2) 0.037(2) 0.0003(18) 0.020(2) -0.0032(18) O6 0.038(3) 0.025(2) 0.033(2) -0.0033(19) 0.015(2) -0.0021(18) O7 0.045(3) 0.023(2) 0.038(2) -0.0036(19) 0.023(2) -0.0047(19) O8 0.043(3) 0.021(2) 0.038(2) -0.0058(19) 0.023(2) -0.0025(19) N1 0.045(3) 0.038(3) 0.035(3) -0.004(3) 0.021(3) -0.015(3) N2 0.035(3) 0.023(3) 0.072(4) -0.003(3) 0.017(3) 0.003(2) N3 0.030(3) 0.021(3) 0.041(3) 0.000(2) 0.020(2) -0.001(2) N4 0.032(3) 0.026(3) 0.035(3) -0.001(2) 0.020(2) -0.008(2) N5 0.030(3) 0.014(2) 0.044(3) 0.002(2) 0.019(2) -0.002(2) N6 0.038(3) 0.020(3) 0.051(3) -0.004(2) 0.026(3) -0.007(2) N7 0.036(3) 0.028(3) 0.086(5) 0.000(3) 0.031(3) -0.001(3) N8 0.043(3) 0.029(3) 0.054(4) -0.010(3) 0.025(3) -0.013(3) N11 0.035(3) 0.037(3) 0.053(4) -0.003(3) 0.017(3) -0.001(3) N12 0.044(4) 0.027(3) 0.053(4) 0.000(3) 0.016(3) -0.004(3) N13 0.042(3) 0.025(3) 0.030(3) -0.006(2) 0.018(2) -0.005(2) N14 0.040(3) 0.029(3) 0.034(3) -0.002(2) 0.022(3) 0.000(2) N15 0.048(4) 0.043(4) 0.072(4) -0.006(3) 0.034(3) 0.005(3) N16 0.046(3) 0.042(3) 0.035(3) -0.001(3) 0.028(3) -0.006(3) N17 0.047(3) 0.028(3) 0.042(3) 0.001(3) 0.021(3) -0.006(2) N18 0.088(5) 0.024(3) 0.050(4) 0.003(3) 0.036(4) 0.004(3) N19 0.049(3) 0.021(3) 0.043(3) 0.002(2) 0.023(3) -0.004(2) N20 0.055(4) 0.018(3) 0.045(3) -0.002(2) 0.031(3) -0.001(2) N21 0.054(4) 0.026(3) 0.040(3) -0.007(3) 0.023(3) -0.004(3) N22 0.047(3) 0.033(3) 0.044(3) -0.014(3) 0.025(3) -0.010(3) N23 0.106(6) 0.048(4) 0.075(5) -0.024(4) 0.047(4) 0.004(4) N24 0.042(4) 0.085(5) 0.039(4) 0.002(4) 0.019(3) -0.001(3) N25 0.050(3) 0.028(3) 0.040(3) 0.001(2) 0.028(3) -0.003(2) N26 0.130(6) 0.021(3) 0.048(4) 0.003(3) 0.058(4) 0.011(3) N27 0.049(3) 0.018(3) 0.038(3) 0.001(2) 0.026(3) -0.002(2) N28 0.050(3) 0.016(3) 0.043(3) 0.002(2) 0.029(3) -0.004(2) N29 0.054(4) 0.029(3) 0.035(3) -0.003(2) 0.027(3) -0.006(3) N30 0.045(3) 0.020(3) 0.036(3) -0.003(2) 0.022(3) -0.005(2) N31 0.112(6) 0.028(3) 0.052(4) 0.005(3) 0.047(4) -0.002(3) N32 0.045(3) 0.030(3) 0.039(3) -0.006(3) 0.024(3) -0.009(2) C1 0.056(5) 0.045(4) 0.045(4) -0.006(3) 0.019(4) -0.024(4) C2 0.047(5) 0.067(6) 0.059(5) -0.009(4) 0.019(4) -0.035(4) C3 0.043(5) 0.067(6) 0.063(5) -0.011(4) 0.027(4) -0.024(4) C4 0.039(4) 0.067(5) 0.048(5) -0.006(4) 0.021(4) -0.002(4) C5 0.038(4) 0.030(4) 0.038(4) -0.004(3) 0.017(3) -0.008(3) C6 0.039(4) 0.042(4) 0.036(4) -0.004(3) 0.025(3) -0.011(3) C7 0.034(4) 0.016(3) 0.027(3) 0.003(2) 0.019(3) 0.001(3) C8 0.032(4) 0.025(3) 0.021(3) 0.000(2) 0.015(3) 0.003(3) C9 0.031(4) 0.031(4) 0.046(4) 0.006(3) 0.019(3) 0.000(3) C10 0.028(4) 0.036(4) 0.062(5) -0.011(3) 0.020(3) -0.009(3) C11 0.043(5) 0.054(5) 0.100(7) -0.003(5) 0.027(5) -0.007(4) C12 0.054(6) 0.062(6) 0.156(10) -0.025(6) 0.029(6) -0.024(5) C13 0.048(5) 0.051(6) 0.133(9) -0.025(5) 0.025(5) -0.029(4) C14 0.066(6) 0.034(4) 0.099(7) -0.009(4) 0.044(5) -0.013(4) C21 0.045(4) 0.025(3) 0.030(4) -0.001(3) 0.016(3) -0.003(3) C22 0.044(4) 0.023(3) 0.031(4) -0.004(3) 0.018(3) -0.003(3) C23 0.040(4) 0.043(4) 0.035(4) -0.004(3) 0.022(3) 0.001(3) C24 0.044(4) 0.051(4) 0.039(4) -0.003(3) 0.026(3) -0.004(3) C25 0.052(5) 0.070(6) 0.062(5) -0.005(4) 0.034(4) -0.002(4) C26 0.050(5) 0.077(6) 0.070(6) -0.011(5) 0.029(4) -0.013(5) C27 0.060(5) 0.064(5) 0.052(5) -0.015(4) 0.030(4) -0.030(4) C28 0.062(5) 0.050(5) 0.042(4) -0.011(3) 0.035(4) -0.020(4) C29 0.060(5) 0.028(4) 0.047(4) -0.006(3) 0.024(4) -0.012(3) C30 0.085(6) 0.032(4) 0.045(4) 0.002(3) 0.027(4) -0.014(4) C31 0.107(7) 0.032(4) 0.050(5) 0.012(4) 0.031(5) -0.008(4) C32 0.090(6) 0.028(4) 0.056(5) -0.005(4) 0.036(5) -0.010(4) C33 0.050(4) 0.012(3) 0.043(4) 0.000(3) 0.023(3) -0.001(3) C34 0.048(4) 0.021(3) 0.040(4) 0.005(3) 0.020(3) -0.002(3) C35 0.032(4) 0.028(4) 0.044(4) -0.002(3) 0.019(3) -0.007(3) C36 0.036(4) 0.028(4) 0.036(4) -0.001(3) 0.016(3) -0.009(3) C37 0.050(5) 0.052(5) 0.055(5) -0.021(4) 0.023(4) -0.010(4) C38 0.042(5) 0.101(7) 0.046(5) -0.036(5) 0.022(4) -0.020(5) C39 0.065(6) 0.130(9) 0.077(7) -0.063(7) 0.049(5) -0.045(6) C40 0.083(8) 0.175(12) 0.065(7) -0.070(8) 0.057(6) -0.070(8) C41 0.076(7) 0.191(14) 0.060(7) -0.015(8) 0.044(6) -0.025(8) C42 0.047(5) 0.137(9) 0.060(6) 0.020(6) 0.028(5) -0.007(5) C43 0.074(6) 0.040(4) 0.055(5) 0.002(4) 0.041(4) -0.003(4) C44 0.095(6) 0.043(4) 0.044(4) 0.000(4) 0.045(4) -0.003(4) C45 0.107(7) 0.038(4) 0.059(5) -0.014(4) 0.054(5) -0.011(4) C46 0.086(6) 0.020(3) 0.050(4) -0.001(3) 0.040(4) -0.002(3) C47 0.050(4) 0.018(3) 0.046(4) -0.003(3) 0.027(3) -0.001(3) C48 0.051(4) 0.024(4) 0.044(4) 0.002(3) 0.029(3) 0.003(3) C49 0.039(4) 0.021(3) 0.036(4) -0.002(3) 0.023(3) -0.002(3) C50 0.034(4) 0.023(3) 0.046(4) -0.004(3) 0.024(3) -0.008(3) C51 0.061(5) 0.031(4) 0.046(4) -0.003(3) 0.031(4) -0.005(3) C52 0.058(5) 0.040(4) 0.039(4) 0.000(3) 0.027(4) -0.012(3) C53 0.076(6) 0.036(4) 0.039(4) 0.007(3) 0.023(4) -0.001(4) C54 0.083(6) 0.043(5) 0.036(4) 0.008(4) 0.024(4) 0.001(4) C55 0.064(5) 0.051(5) 0.033(4) -0.009(3) 0.021(4) -0.014(4) C56 0.054(5) 0.033(4) 0.043(4) -0.008(3) 0.027(4) -0.006(3) Br3 0.0797(11) 0.0791(11) 0.0653(10) 0.0007(8) 0.0327(8) 0.0035(8) Br3' 0.208(3) 0.0487(14) 0.147(3) 0.0019(15) 0.148(3) 0.0073(17) Br1 0.0953(6) 0.0220(4) 0.0534(5) -0.0002(3) 0.0446(4) -0.0023(4) Br2 0.0891(6) 0.0229(4) 0.0627(5) 0.0027(3) 0.0352(5) -0.0022(4) Br4 0.0833(9) 0.1518(14) 0.0792(9) -0.0326(9) 0.0535(8) -0.0691(9) Br5 0.0869(14) 0.0878(14) 0.0732(13) 0.0020(10) 0.0465(11) 0.0072(11) Br6 0.0966(16) 0.0869(15) 0.0799(14) 0.0055(11) 0.0302(12) 0.0154(12) Br7 0.189(3) 0.0784(17) 0.0791(16) -0.0332(13) 0.0499(18) -0.0406(18) Br8 0.153(3) 0.0736(16) 0.1068(19) 0.0302(14) 0.0643(18) 0.0316(16) Br9 0.194(4) 0.106(3) 0.130(3) 0.004(3) 0.072(3) -0.034(3) O1W 0.092(5) 0.099(5) 0.146(6) 0.004(5) 0.078(5) 0.034(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.035(5) . ? Co1 N19 2.045(5) . ? Co1 N17 2.136(5) . ? Co1 N1 2.138(5) . ? Co1 O5 2.167(4) . ? Co1 O1 2.197(4) . ? Co2 N6 2.033(5) . ? Co2 N27 2.056(5) . ? Co2 N25 2.119(5) . ? Co2 N8 2.147(5) . ? Co2 O7 2.164(4) . ? Co2 O2 2.205(4) . ? Co3 N9 1.893(9) . ? Co3 N11 1.894(5) . ? Co3 N22 1.901(5) . ? Co3 N24 1.959(6) . ? Co3 O6 1.971(4) . ? Co3 O3 1.988(4) . ? Co3 N9' 2.184(19) . ? Co4 N30 1.847(5) . ? Co4 N14 1.849(5) . ? Co4 O4 1.920(4) . ? Co4 N32 1.922(5) . ? Co4 O8 1.923(4) . ? Co4 N16 1.930(5) . ? O1 C7 1.243(6) . ? O2 C8 1.245(6) . ? O3 C21 1.289(7) . ? O4 C22 1.312(7) . ? O5 C35 1.261(7) . ? O6 C36 1.305(7) . ? O7 C49 1.243(7) . ? O8 C50 1.311(7) . ? N1 C5 1.340(8) . ? N1 C1 1.345(8) . ? N2 C6 1.326(8) . ? N3 C6 1.301(8) . ? N3 N4 1.388(6) . ? N4 C7 1.318(7) . ? N5 C8 1.316(7) . ? N5 N6 1.389(6) . ? N6 C9 1.310(7) . ? N7 C9 1.317(8) . ? N8 C14 1.345(8) . ? N8 C10 1.346(8) . ? N9 C15 1.339(13) . ? N9 C19 1.406(16) . ? N10 C20 1.336(16) . ? N11 C20 1.325(13) . ? N11 C20' 1.34(3) . ? N11 N12 1.398(7) . ? N12 C21 1.303(8) . ? N13 C22 1.314(8) . ? N13 N14 1.408(7) . ? N14 C23 1.308(8) . ? N15 C23 1.322(8) . ? N16 C28 1.332(8) . ? N16 C24 1.369(8) . ? N17 C33 1.336(7) . ? N17 C29 1.351(8) . ? N18 C34 1.350(8) . ? N19 C34 1.286(7) . ? N19 N20 1.391(7) . ? N20 C35 1.343(8) . ? N21 C36 1.319(8) . ? N21 N22 1.401(7) . ? N22 C37 1.309(8) . ? N23 C37 1.336(9) . ? N24 C42 1.349(10) . ? N24 C38 1.382(10) . ? N25 C43 1.336(8) . ? N25 C47 1.371(7) . ? N26 C48 1.311(8) . ? N27 C48 1.300(7) . ? N27 N28 1.381(6) . ? N28 C49 1.334(7) . ? N29 C50 1.287(7) . ? N29 N30 1.391(7) . ? N30 C51 1.306(8) . ? N31 C51 1.314(8) . ? N32 C56 1.322(8) . ? N32 C52 1.369(8) . ? C1 C2 1.409(10) . ? C2 C3 1.368(11) . ? C3 C4 1.366(10) . ? C4 C5 1.380(9) . ? C5 C6 1.522(8) . ? C7 C8 1.536(8) . ? C9 C10 1.486(8) . ? C10 C11 1.370(10) . ? C11 C12 1.410(11) . ? C12 C13 1.393(12) . ? C13 C14 1.373(11) . ? C15 C16 1.376(15) . ? C16 C17 1.430(17) . ? C17 C18 1.369(17) . ? C18 C19 1.397(16) . ? C19 C20 1.447(17) . ? C21 C22 1.498(8) . ? C23 C24 1.464(9) . ? C24 C25 1.391(9) . ? C25 C26 1.405(11) . ? C26 C27 1.350(11) . ? C27 C28 1.397(10) . ? C29 C30 1.394(9) . ? C30 C31 1.375(10) . ? C31 C32 1.410(10) . ? C32 C33 1.385(9) . ? C33 C34 1.485(9) . ? C35 C36 1.476(9) . ? C37 C38 1.471(11) . ? C38 C39 1.383(10) . ? C39 C40 1.466(15) . ? C40 C41 1.344(16) . ? C41 C42 1.385(13) . ? C43 C44 1.389(9) . ? C44 C45 1.369(10) . ? C45 C46 1.383(9) . ? C46 C47 1.374(8) . ? C47 C48 1.490(9) . ? C49 C50 1.493(8) . ? C51 C52 1.482(9) . ? C52 C53 1.386(9) . ? C53 C54 1.429(10) . ? C54 C55 1.374(10) . ? C55 C56 1.388(9) . ? N9' C15' 1.33(3) . ? N9' C19' 1.35(3) . ? N10' C20' 1.23(4) . ? C15' C16' 1.38(3) . ? C16' C17' 1.50(3) . ? C17' C18' 1.42(4) . ? C18' C19' 1.38(3) . ? C19' C20' 1.47(4) . ? 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 N3 Co1 N19 163.1(2) . . ? N3 Co1 N17 121.3(2) . . ? N19 Co1 N17 75.2(2) . . ? N3 Co1 N1 74.8(2) . . ? N19 Co1 N1 102.3(2) . . ? N17 Co1 N1 92.6(2) . . ? N3 Co1 O5 88.42(17) . . ? N19 Co1 O5 75.12(18) . . ? N17 Co1 O5 150.27(18) . . ? N1 Co1 O5 94.07(17) . . ? N3 Co1 O1 75.12(16) . . ? N19 Co1 O1 108.52(18) . . ? N17 Co1 O1 97.07(17) . . ? N1 Co1 O1 149.12(18) . . ? O5 Co1 O1 91.91(14) . . ? N6 Co2 N27 162.4(2) . . ? N6 Co2 N25 121.6(2) . . ? N27 Co2 N25 75.30(19) . . ? N6 Co2 N8 74.1(2) . . ? N27 Co2 N8 101.9(2) . . ? N25 Co2 N8 92.1(2) . . ? N6 Co2 O7 88.60(18) . . ? N27 Co2 O7 74.45(17) . . ? N25 Co2 O7 149.74(17) . . ? N8 Co2 O7 94.24(18) . . ? N6 Co2 O2 75.21(17) . . ? N27 Co2 O2 110.33(17) . . ? N25 Co2 O2 95.56(17) . . ? N8 Co2 O2 147.76(18) . . ? O7 Co2 O2 94.64(15) . . ? N9 Co3 N11 85.3(3) . . ? N9 Co3 N22 98.4(3) . . ? N11 Co3 N22 175.4(2) . . ? N9 Co3 N24 92.1(3) . . ? N11 Co3 N24 102.3(3) . . ? N22 Co3 N24 80.2(3) . . ? N9 Co3 O6 86.4(3) . . ? N11 Co3 O6 97.4(2) . . ? N22 Co3 O6 80.3(2) . . ? N24 Co3 O6 160.1(2) . . ? N9 Co3 O3 164.8(3) . . ? N11 Co3 O3 79.9(2) . . ? N22 Co3 O3 96.2(2) . . ? N24 Co3 O3 94.4(2) . . ? O6 Co3 O3 92.07(16) . . ? N9 Co3 N9' 14.6(5) . . ? N11 Co3 N9' 71.1(6) . . ? N22 Co3 N9' 112.8(6) . . ? N24 Co3 N9' 91.9(5) . . ? O6 Co3 N9' 91.5(4) . . ? O3 Co3 N9' 151.0(6) . . ? N30 Co4 N14 176.6(2) . . ? N30 Co4 O4 96.0(2) . . ? N14 Co4 O4 82.1(2) . . ? N30 Co4 N32 81.9(2) . . ? N14 Co4 N32 101.0(2) . . ? O4 Co4 N32 90.94(19) . . ? N30 Co4 O8 82.43(19) . . ? N14 Co4 O8 94.70(19) . . ? O4 Co4 O8 91.49(17) . . ? N32 Co4 O8 164.29(19) . . ? N30 Co4 N16 99.4(2) . . ? N14 Co4 N16 82.4(2) . . ? O4 Co4 N16 164.5(2) . . ? N32 Co4 N16 91.9(2) . . ? O8 Co4 N16 89.84(19) . . ? C7 O1 Co1 110.2(4) . . ? C8 O2 Co2 109.9(4) . . ? C21 O3 Co3 109.5(4) . . ? C22 O4 Co4 109.1(4) . . ? C35 O5 Co1 112.6(4) . . ? C36 O6 Co3 109.5(4) . . ? C49 O7 Co2 113.7(4) . . ? C50 O8 Co4 107.2(4) . . ? C5 N1 C1 116.7(6) . . ? C5 N1 Co1 116.3(4) . . ? C1 N1 Co1 127.1(5) . . ? C6 N3 N4 120.2(5) . . ? C6 N3 Co1 120.9(4) . . ? N4 N3 Co1 115.6(3) . . ? C7 N4 N3 113.3(5) . . ? C8 N5 N6 113.9(5) . . ? C9 N6 N5 120.0(5) . . ? C9 N6 Co2 121.6(4) . . ? N5 N6 Co2 115.1(4) . . ? C14 N8 C10 117.3(6) . . ? C14 N8 Co2 127.6(5) . . ? C10 N8 Co2 115.0(4) . . ? C15 N9 C19 118.4(9) . . ? C15 N9 Co3 129.8(8) . . ? C19 N9 Co3 111.8(7) . . ? C20 N11 C20' 21.9(13) . . ? C20 N11 N12 127.3(7) . . ? C20' N11 N12 109.6(14) . . ? C20 N11 Co3 114.4(7) . . ? C20' N11 Co3 133.1(14) . . ? N12 N11 Co3 117.3(4) . . ? C21 N12 N11 108.0(5) . . ? C22 N13 N14 106.2(5) . . ? C23 N14 N13 122.1(5) . . ? C23 N14 Co4 120.1(4) . . ? N13 N14 Co4 117.5(4) . . ? C28 N16 C24 120.0(6) . . ? C28 N16 Co4 127.7(5) . . ? C24 N16 Co4 112.3(4) . . ? C33 N17 C29 119.1(5) . . ? C33 N17 Co1 115.0(4) . . ? C29 N17 Co1 125.2(4) . . ? C34 N19 N20 121.8(5) . . ? C34 N19 Co1 121.1(4) . . ? N20 N19 Co1 116.9(4) . . ? C35 N20 N19 112.8(5) . . ? C36 N21 N22 106.8(5) . . ? C37 N22 N21 121.1(6) . . ? C37 N22 Co3 120.7(5) . . ? N21 N22 Co3 117.8(4) . . ? C42 N24 C38 120.4(8) . . ? C42 N24 Co3 125.0(7) . . ? C38 N24 Co3 114.6(5) . . ? C43 N25 C47 118.1(5) . . ? C43 N25 Co2 126.0(4) . . ? C47 N25 Co2 115.2(4) . . ? C48 N27 N28 121.9(5) . . ? C48 N27 Co2 121.4(4) . . ? N28 N27 Co2 116.2(3) . . ? C49 N28 N27 113.9(5) . . ? C50 N29 N30 106.4(5) . . ? C51 N30 N29 122.0(5) . . ? C51 N30 Co4 120.9(4) . . ? N29 N30 Co4 117.1(4) . . ? C56 N32 C52 119.0(6) . . ? C56 N32 Co4 127.1(5) . . ? C52 N32 Co4 113.9(4) . . ? N1 C1 C2 123.6(7) . . ? C3 C2 C1 117.3(7) . . ? C4 C3 C2 119.9(7) . . ? C3 C4 C5 119.4(7) . . ? N1 C5 C4 123.1(6) . . ? N1 C5 C6 112.9(6) . . ? C4 C5 C6 124.1(6) . . ? N3 C6 N2 128.3(6) . . ? N3 C6 C5 112.0(6) . . ? N2 C6 C5 119.7(6) . . ? O1 C7 N4 124.4(5) . . ? O1 C7 C8 121.3(5) . . ? N4 C7 C8 114.2(5) . . ? O2 C8 N5 124.1(5) . . ? O2 C8 C7 122.1(5) . . ? N5 C8 C7 113.8(5) . . ? N6 C9 N7 127.3(6) . . ? N6 C9 C10 110.9(5) . . ? N7 C9 C10 121.8(6) . . ? N8 C10 C11 123.6(6) . . ? N8 C10 C9 114.6(5) . . ? C11 C10 C9 121.7(6) . . ? C10 C11 C12 118.8(8) . . ? C13 C12 C11 117.5(8) . . ? C14 C13 C12 119.6(7) . . ? N8 C14 C13 123.1(7) . . ? N9 C15 C16 123.9(11) . . ? C15 C16 C17 117.0(11) . . ? C18 C17 C16 121.1(12) . . ? C17 C18 C19 118.6(13) . . ? C18 C19 N9 121.0(11) . . ? C18 C19 C20 125.1(14) . . ? N9 C19 C20 113.7(10) . . ? N11 C20 N10 120.9(12) . . ? N11 C20 C19 114.6(10) . . ? N10 C20 C19 124.5(13) . . ? O3 C21 N12 125.2(6) . . ? O3 C21 C22 118.9(6) . . ? N12 C21 C22 116.0(5) . . ? O4 C22 N13 125.0(6) . . ? O4 C22 C21 116.9(5) . . ? N13 C22 C21 118.0(5) . . ? N14 C23 N15 125.6(6) . . ? N14 C23 C24 110.5(6) . . ? N15 C23 C24 123.9(6) . . ? N16 C24 C25 120.6(7) . . ? N16 C24 C23 114.6(6) . . ? C25 C24 C23 124.8(7) . . ? C24 C25 C26 118.5(8) . . ? C27 C26 C25 119.9(8) . . ? C26 C27 C28 119.7(7) . . ? N16 C28 C27 121.3(7) . . ? N17 C29 C30 122.4(6) . . ? C31 C30 C29 118.0(7) . . ? C30 C31 C32 119.9(7) . . ? C33 C32 C31 118.1(6) . . ? N17 C33 C32 122.4(6) . . ? N17 C33 C34 114.6(5) . . ? C32 C33 C34 123.1(5) . . ? N19 C34 N18 126.2(6) . . ? N19 C34 C33 113.3(5) . . ? N18 C34 C33 120.5(5) . . ? O5 C35 N20 122.5(6) . . ? O5 C35 C36 118.7(6) . . ? N20 C35 C36 118.8(6) . . ? O6 C36 N21 125.5(6) . . ? O6 C36 C35 115.6(5) . . ? N21 C36 C35 118.8(6) . . ? N22 C37 N23 124.9(7) . . ? N22 C37 C38 111.2(7) . . ? N23 C37 C38 123.9(7) . . ? N24 C38 C39 121.7(9) . . ? N24 C38 C37 112.9(6) . . ? C39 C38 C37 125.3(9) . . ? C38 C39 C40 115.9(10) . . ? C41 C40 C39 120.7(9) . . ? C40 C41 C42 120.3(12) . . ? N24 C42 C41 120.8(11) . . ? N25 C43 C44 122.8(7) . . ? C45 C44 C43 118.0(7) . . ? C44 C45 C46 120.7(7) . . ? C47 C46 C45 118.3(6) . . ? N25 C47 C46 122.0(6) . . ? N25 C47 C48 114.2(5) . . ? C46 C47 C48 123.8(6) . . ? N27 C48 N26 126.3(6) . . ? N27 C48 C47 112.6(5) . . ? N26 C48 C47 121.1(5) . . ? O7 C49 N28 121.7(5) . . ? O7 C49 C50 120.1(5) . . ? N28 C49 C50 118.2(5) . . ? N29 C50 O8 126.9(6) . . ? N29 C50 C49 119.7(5) . . ? O8 C50 C49 113.4(5) . . ? N30 C51 N31 125.5(6) . . ? N30 C51 C52 110.2(6) . . ? N31 C51 C52 124.3(6) . . ? N32 C52 C53 122.2(6) . . ? N32 C52 C51 113.0(6) . . ? C53 C52 C51 124.8(6) . . ? C52 C53 C54 116.8(6) . . ? C55 C54 C53 120.6(6) . . ? C54 C55 C56 117.7(7) . . ? N32 C56 C55 123.6(6) . . ? C15' N9' C19' 121(2) . . ? C15' N9' Co3 122.8(18) . . ? C19' N9' Co3 115.4(14) . . ? N9' C15' C16' 128(2) . . ? C15' C16' C17' 110(2) . . ? C18' C17' C16' 121(2) . . ? C19' C18' C17' 119(3) . . ? N9' C19' C18' 120(3) . . ? N9' C19' C20' 115(2) . . ? C18' C19' C20' 125(3) . . ? N10' C20' N11 133(3) . . ? N10' C20' C19' 122(3) . . ? N11 C20' C19' 105(2) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.837 _refine_diff_density_min -1.503 _refine_diff_density_rms 0.106 #===END data_shelxl_(7) _database_code_depnum_ccdc_archive 'CCDC 228045' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H115 B6 F24 N48 Ni4 O27.50' _chemical_formula_weight 2992.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3c _symmetry_Int_Tables_number 167 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z+1/2' 'x, x-y, z+1/2' '-x+y, y, z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+2/3, -x+1/3, z+5/6' 'x+2/3, x-y+1/3, z+5/6' '-x+y+2/3, y+1/3, z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-y+1/3, -x+2/3, z+7/6' 'x+1/3, x-y+2/3, z+7/6' '-x+y+1/3, y+2/3, z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, -z-1/2' '-x, -x+y, -z-1/2' 'x-y, -y, -z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' 'y+2/3, x+1/3, -z-1/6' '-x+2/3, -x+y+1/3, -z-1/6' 'x-y+2/3, -y+1/3, -z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 'y+1/3, x+2/3, -z+1/6' '-x+1/3, -x+y+2/3, -z+1/6' 'x-y+1/3, -y+2/3, -z+1/6' _cell_length_a 24.5027(8) _cell_length_b 24.5027(8) _cell_length_c 84.524(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 43948(3) _cell_formula_units_Z 12 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 18396 _exptl_absorpt_coefficient_mu 0.612 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7659 _exptl_absorpt_correction_T_max 0.8669 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 71552 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -61 _diffrn_reflns_limit_l_max 105 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.41 _reflns_number_total 10009 _reflns_number_gt 7874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SMART (Bruker, 1997)' _computing_data_reduction 'Bruker SHELXTL (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1840P)^2^+322.9337P] 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 10009 _refine_ls_number_parameters 585 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1063 _refine_ls_R_factor_gt 0.0887 _refine_ls_wR_factor_ref 0.2914 _refine_ls_wR_factor_gt 0.2703 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 0.18028(3) 0.21357(3) 0.138701(7) 0.0343(2) Uani 1 1 d . . . Ni2 Ni 0.0000 0.0000 0.047640(11) 0.0311(3) Uani 1 3 d S . . F1 F 0.2140(4) 0.9516(4) 0.00914(7) 0.129(3) Uani 1 1 d . . . F2 F 0.2289(2) 0.9845(2) 0.03445(5) 0.0754(11) Uani 1 1 d . . . F3 F 0.1594(2) 0.99428(19) 0.01916(5) 0.0690(10) Uani 1 1 d . . . F4 F 0.1412(3) 0.8980(3) 0.02691(11) 0.149(3) Uani 1 1 d . . . F5 F 0.3576(14) 0.2286(14) 0.0513(3) 0.123(8) Uiso 0.25 1 d P . . F6 F 0.4100(5) 0.3339(5) 0.05095(14) 0.101(3) Uiso 0.50 1 d P . . F7 F 0.3575(8) 0.2751(8) 0.0319(2) 0.152(5) Uiso 0.50 1 d P . . F8 F 0.4366(7) 0.2947(7) 0.02971(18) 0.129(4) Uiso 0.50 1 d P . . F9 F 0.4079(11) 0.2374(11) 0.0509(3) 0.098(6) Uiso 0.25 1 d P . . F10 F 0.3800 0.9512 0.0695 0.0463(13) Uiso 0.50 1 d P . . F11 F 0.2776 0.9443 0.0715 0.0683(19) Uiso 0.50 1 d P . . F12 F 0.3246 0.9343 0.0956 0.103(3) Uiso 0.50 1 d P . . F13 F 0.2834 0.8511 0.0776 0.0350(11) Uiso 0.50 1 d P . . O1 O 0.16572(15) 0.16202(16) 0.08732(4) 0.0388(8) Uani 1 1 d . . . O2 O 0.00207(15) 0.07998(16) 0.09366(4) 0.0354(7) Uani 1 1 d . . . O3 O -0.07092(19) 0.13188(18) 0.15806(5) 0.0559(11) Uani 1 1 d . . . O4 O 0.02237(14) 0.09241(14) 0.13474(4) 0.0321(7) Uani 1 1 d . . . O5 O 0.5110(3) 0.1589(4) 0.05037(7) 0.109(2) Uani 1 1 d . . . O6 O 0.7695(4) 0.4454(4) 0.01772(10) 0.112(2) Uani 1 1 d . . . O7 O 0.1002(3) 0.3850(3) 0.00175(7) 0.096(2) Uani 1 1 d . . . O8 O 0.7933(5) 0.6862(3) 0.06385(12) 0.073(3) Uani 0.50 1 d P . . O9 O 0.6619(5) 0.6091(5) 0.05193(12) 0.076(3) Uani 0.50 1 d P . . O10 O 0.0157(7) 0.3882(10) 0.02312(15) 0.132(7) Uani 0.50 1 d P . . O11 O 0.5367(10) 0.9635(5) 0.0810(2) 0.149(8) Uani 0.50 1 d P . . O12 O 0.6667 0.3333 0.0365(8) 0.21(2) Uani 0.50 3 d SP . . N1 N 0.2623(2) 0.2078(2) 0.13858(5) 0.0456(10) Uani 1 1 d . . . N2 N 0.1970(2) 0.0856(2) 0.10894(6) 0.0461(10) Uani 1 1 d . . . N3 N 0.16481(17) 0.15218(19) 0.12036(5) 0.0340(8) Uani 1 1 d . . . N4 N 0.11173(16) 0.12523(17) 0.11045(4) 0.0297(8) Uani 1 1 d . . . N5 N 0.05999(17) 0.11160(18) 0.07099(4) 0.0302(8) Uani 1 1 d . . . N6 N 0.01089(18) 0.07661(17) 0.06023(4) 0.0313(8) Uani 1 1 d . . . N7 N -0.0229(2) 0.1501(2) 0.06355(6) 0.0523(12) Uani 1 1 d . . . N8 N 0.0848(2) 0.0612(2) 0.03606(5) 0.0410(10) Uani 1 1 d . . . N9 N 0.1999(2) 0.2652(2) 0.15972(5) 0.0440(10) Uani 1 1 d . . . N10 N 0.1480(2) 0.1245(2) 0.18287(5) 0.0437(10) Uani 1 1 d . . . N11 N 0.14255(19) 0.14401(18) 0.15583(5) 0.0349(8) Uani 1 1 d . . . N12 N 0.11681(18) 0.08044(18) 0.15253(5) 0.0341(8) Uani 1 1 d . . . N13 N 0.04344(19) 0.18965(18) 0.14326(5) 0.0363(9) Uani 1 1 d . . . N14 N 0.10072(19) 0.22114(18) 0.13516(5) 0.0354(8) Uani 1 1 d . . . N15 N 0.0665(3) 0.2895(3) 0.12583(7) 0.0630(14) Uani 1 1 d . . . N16 N 0.2127(2) 0.2899(2) 0.12335(5) 0.0439(10) Uani 1 1 d . . . C1 C 0.3110(3) 0.2374(3) 0.14840(8) 0.0619(17) Uani 1 1 d . . . C2 C 0.3610(3) 0.2258(5) 0.14849(10) 0.086(3) Uani 1 1 d . . . C3 C 0.3610(4) 0.1841(6) 0.13801(14) 0.111(4) Uani 1 1 d . . . C4 C 0.3109(4) 0.1526(5) 0.12786(10) 0.083(2) Uani 1 1 d . . . C5 C 0.2624(2) 0.1653(3) 0.12836(6) 0.0474(12) Uani 1 1 d . . . C6 C 0.2045(2) 0.1327(2) 0.11834(6) 0.0376(10) Uani 1 1 d . . . C7 C 0.1163(2) 0.1348(2) 0.09502(5) 0.0285(9) Uani 1 1 d . . . C8 C 0.0524(2) 0.10498(19) 0.08667(5) 0.0279(8) Uani 1 1 d . . . C9 C -0.0248(2) 0.1003(2) 0.05669(6) 0.0364(10) Uani 1 1 d . . . C10 C 0.1370(2) 0.0712(2) 0.04407(6) 0.0392(11) Uani 1 1 d . . . C11 C 0.1969(3) 0.1210(3) 0.04052(8) 0.0568(15) Uani 1 1 d . . . C12 C 0.2023(3) 0.1588(4) 0.02762(10) 0.072(2) Uani 1 1 d . . . C13 C 0.1498(4) 0.1471(4) 0.01930(9) 0.072(2) Uani 1 1 d . . . C14 C 0.0920(3) 0.0990(3) 0.02393(7) 0.0546(14) Uani 1 1 d . . . C15 C 0.2215(3) 0.3270(3) 0.16091(7) 0.0567(15) Uani 1 1 d . . . C16 C 0.2284(4) 0.3571(3) 0.17499(9) 0.075(2) Uani 1 1 d . . . C17 C 0.2106(5) 0.3223(4) 0.18853(9) 0.089(3) Uani 1 1 d . . . C18 C 0.1871(4) 0.2578(3) 0.18759(8) 0.070(2) Uani 1 1 d . . . C19 C 0.1825(3) 0.2307(2) 0.17308(6) 0.0427(11) Uani 1 1 d . . . C20 C 0.1565(2) 0.1619(2) 0.17053(6) 0.0361(10) Uani 1 1 d . . . C21 C -0.0512(2) 0.0996(2) 0.15232(6) 0.0368(10) Uani 1 1 d . . . C22 C 0.0097(2) 0.1265(2) 0.14269(5) 0.0324(9) Uani 1 1 d . . . C23 C 0.1083(3) 0.2704(2) 0.12723(6) 0.0426(11) Uani 1 1 d . . . C24 C 0.1701(3) 0.3058(2) 0.11912(6) 0.0447(12) Uani 1 1 d . . . C25 C 0.1830(4) 0.3521(3) 0.10797(9) 0.0659(17) Uani 1 1 d . . . C26 C 0.2415(4) 0.3828(3) 0.10092(9) 0.072(2) Uani 1 1 d . . . C27 C 0.2857(3) 0.3671(3) 0.10529(9) 0.0698(19) Uani 1 1 d . . . C28 C 0.2692(3) 0.3196(3) 0.11667(8) 0.0594(15) Uani 1 1 d . . . B1 B 0.1846(4) 0.9573(4) 0.02275(11) 0.066(2) Uani 1 1 d . . . B2 B 0.3986(9) 0.2814(9) 0.0431(2) 0.074(4) Uiso 0.50 1 d P . . B3 B 0.3289 0.9316 0.0797 0.087(5) Uiso 0.50 1 d P . . H1 H 0.2288 0.0746 0.1083 0.054 Uiso 1 1 d . . . H2 H 0.1592 0.0631 0.1030 0.054 Uiso 1 1 d . . . H3 H 0.0059 0.1719 0.0719 0.060 Uiso 1 1 d . . . H4 H -0.0515 0.1640 0.0603 0.060 Uiso 1 1 d . . . H5 H 0.1593 0.1426 0.1932 0.051 Uiso 1 1 d . . . H6 H 0.1308 0.0807 0.1815 0.051 Uiso 1 1 d . . . H7 H 0.0271 0.2673 0.1315 0.071 Uiso 1 1 d . . . H8 H 0.0753 0.3254 0.1199 0.071 Uiso 1 1 d . . . H9 H 0.3114 0.2678 0.1556 0.070 Uiso 1 1 d . . . H10 H 0.3945 0.2446 0.1559 0.099 Uiso 1 1 d . . . H11 H 0.3954 0.1764 0.1376 0.130 Uiso 1 1 d . . . H12 H 0.3104 0.1224 0.1206 0.105 Uiso 1 1 d . . . H13 H 0.2331 0.1297 0.0467 0.068 Uiso 1 1 d . . . H14 H 0.2425 0.1919 0.0244 0.085 Uiso 1 1 d . . . H15 H 0.1536 0.1742 0.0109 0.082 Uiso 1 1 d . . . H16 H 0.0553 0.0913 0.0182 0.063 Uiso 1 1 d . . . H17 H 0.2344 0.3516 0.1515 0.064 Uiso 1 1 d . . . H18 H 0.2432 0.4012 0.1753 0.088 Uiso 1 1 d . . . H19 H 0.2145 0.3413 0.1986 0.101 Uiso 1 1 d . . . H20 H 0.1731 0.2322 0.1970 0.083 Uiso 1 1 d . . . H21 H 0.1520 0.3631 0.1050 0.078 Uiso 1 1 d . . . H22 H 0.2511 0.4145 0.0933 0.085 Uiso 1 1 d . . . H23 H 0.3271 0.3871 0.1007 0.081 Uiso 1 1 d . . . H24 H 0.3003 0.3095 0.1200 0.068 Uiso 1 1 d . . . H25 H 0.0726 0.1098 0.1158 0.035 Uiso 1 1 d . . . H26 H 0.0977 0.1266 0.0674 0.035 Uiso 1 1 d . . . H27 H 0.0842 0.0668 0.1468 0.035 Uiso 1 1 d . . . H28 H 0.0344 0.2098 0.1496 0.035 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0322(3) 0.0303(3) 0.0319(4) -0.0018(2) -0.0052(2) 0.0092(2) Ni2 0.0354(4) 0.0354(4) 0.0225(5) 0.000 0.000 0.01772(18) F1 0.200(7) 0.204(7) 0.081(3) -0.034(4) -0.024(4) 0.175(7) F2 0.085(3) 0.076(3) 0.073(3) -0.015(2) -0.018(2) 0.046(2) F3 0.075(2) 0.075(2) 0.079(3) 0.005(2) 0.008(2) 0.053(2) F4 0.124(5) 0.067(3) 0.235(8) 0.016(4) -0.069(5) 0.032(3) O1 0.0272(16) 0.0443(19) 0.0369(18) 0.0066(14) 0.0030(13) 0.0118(14) O2 0.0301(16) 0.0415(18) 0.0319(16) 0.0004(13) -0.0003(13) 0.0157(14) O3 0.051(2) 0.044(2) 0.070(3) -0.0140(19) 0.0188(19) 0.0218(18) O4 0.0306(15) 0.0296(15) 0.0340(16) -0.0028(12) 0.0022(12) 0.0134(13) O5 0.105(5) 0.165(7) 0.054(3) 0.019(4) 0.004(3) 0.064(5) O6 0.119(5) 0.120(5) 0.140(6) -0.011(5) 0.009(5) 0.091(5) O7 0.119(5) 0.061(3) 0.087(4) -0.019(3) -0.038(4) 0.028(3) O8 0.091(7) 0.021(3) 0.072(6) 0.009(4) -0.008(5) 0.002(4) O9 0.058(5) 0.082(7) 0.074(6) -0.031(5) 0.012(5) 0.026(5) O10 0.122(11) 0.28(2) 0.072(7) -0.006(10) -0.012(7) 0.160(15) O11 0.208(18) 0.040(6) 0.187(16) -0.037(8) -0.120(14) 0.052(8) O12 0.101(14) 0.101(14) 0.43(8) 0.000 0.000 0.051(7) N1 0.033(2) 0.052(3) 0.042(2) 0.001(2) -0.0091(18) 0.0139(19) N2 0.041(2) 0.058(3) 0.051(3) -0.008(2) -0.0086(19) 0.034(2) N3 0.0247(17) 0.040(2) 0.0319(19) -0.0018(16) -0.0060(15) 0.0123(16) N4 0.0238(17) 0.0334(18) 0.0287(18) -0.0031(14) -0.0027(14) 0.0119(15) N5 0.0291(18) 0.0336(19) 0.0256(17) -0.0003(14) -0.0002(14) 0.0140(15) N6 0.0346(19) 0.0320(19) 0.0264(18) -0.0023(14) -0.0054(15) 0.0160(16) N7 0.064(3) 0.046(2) 0.061(3) -0.014(2) -0.024(2) 0.038(2) N8 0.052(2) 0.048(2) 0.030(2) 0.0097(17) 0.0132(18) 0.030(2) N9 0.048(2) 0.032(2) 0.041(2) -0.0052(17) -0.0116(19) 0.0115(18) N10 0.057(3) 0.039(2) 0.032(2) -0.0010(17) -0.0066(19) 0.022(2) N11 0.038(2) 0.0276(18) 0.035(2) -0.0040(15) -0.0059(16) 0.0135(16) N12 0.0349(19) 0.0301(19) 0.035(2) -0.0039(15) -0.0099(16) 0.0148(16) N13 0.040(2) 0.0290(19) 0.038(2) -0.0023(16) 0.0069(16) 0.0153(17) N14 0.037(2) 0.0287(18) 0.0339(19) -0.0008(15) 0.0016(16) 0.0118(16) N15 0.063(3) 0.049(3) 0.081(4) 0.024(3) 0.012(3) 0.032(3) N16 0.040(2) 0.035(2) 0.041(2) 0.0031(17) -0.0022(18) 0.0067(18) C1 0.046(3) 0.069(4) 0.054(4) -0.010(3) -0.023(3) 0.016(3) C2 0.048(4) 0.125(7) 0.077(5) -0.024(5) -0.037(4) 0.038(4) C3 0.062(5) 0.170(10) 0.126(8) -0.051(8) -0.045(5) 0.077(6) C4 0.063(4) 0.126(7) 0.082(5) -0.034(5) -0.031(4) 0.063(5) C5 0.035(3) 0.063(3) 0.043(3) -0.005(2) -0.008(2) 0.024(2) C6 0.032(2) 0.048(3) 0.032(2) 0.000(2) -0.0036(18) 0.019(2) C7 0.027(2) 0.028(2) 0.030(2) -0.0009(16) -0.0015(16) 0.0138(17) C8 0.028(2) 0.0251(19) 0.031(2) 0.0003(16) -0.0024(17) 0.0138(17) C9 0.041(2) 0.031(2) 0.038(2) 0.0032(18) -0.0058(19) 0.019(2) C10 0.040(2) 0.045(3) 0.036(2) 0.008(2) 0.013(2) 0.024(2) C11 0.045(3) 0.058(3) 0.069(4) 0.023(3) 0.024(3) 0.027(3) C12 0.060(4) 0.068(4) 0.092(5) 0.047(4) 0.042(4) 0.036(3) C13 0.086(5) 0.080(5) 0.062(4) 0.042(4) 0.037(4) 0.052(4) C14 0.069(4) 0.068(4) 0.040(3) 0.019(3) 0.014(3) 0.043(3) C15 0.071(4) 0.032(3) 0.052(3) -0.006(2) -0.018(3) 0.014(3) C16 0.113(6) 0.037(3) 0.062(4) -0.015(3) -0.020(4) 0.028(4) C17 0.152(8) 0.056(4) 0.052(4) -0.024(3) -0.026(5) 0.047(5) C18 0.115(6) 0.048(3) 0.042(3) -0.011(3) -0.014(3) 0.037(4) C19 0.050(3) 0.033(2) 0.039(3) -0.009(2) -0.013(2) 0.017(2) C20 0.037(2) 0.035(2) 0.032(2) -0.0040(18) -0.0069(18) 0.0146(19) C21 0.035(2) 0.036(2) 0.034(2) -0.0070(19) 0.0042(19) 0.014(2) C22 0.030(2) 0.035(2) 0.030(2) -0.0030(18) -0.0026(17) 0.0155(19) C23 0.046(3) 0.033(2) 0.044(3) 0.000(2) 0.000(2) 0.017(2) C24 0.050(3) 0.032(2) 0.041(3) 0.002(2) 0.000(2) 0.013(2) C25 0.074(4) 0.048(3) 0.068(4) 0.020(3) 0.011(3) 0.025(3) C26 0.082(5) 0.051(4) 0.067(4) 0.025(3) 0.018(4) 0.020(3) C27 0.061(4) 0.060(4) 0.064(4) 0.015(3) 0.017(3) 0.011(3) C28 0.044(3) 0.054(3) 0.061(4) 0.011(3) 0.006(3) 0.010(3) B1 0.073(5) 0.057(4) 0.081(6) -0.012(4) -0.018(4) 0.040(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N3 2.059(4) . ? Ni1 N11 2.069(4) . ? Ni1 N14 2.070(4) . ? Ni1 N16 2.081(4) . ? Ni1 N1 2.085(5) . ? Ni1 N9 2.093(4) . ? Ni2 N6 2.056(4) 3 ? Ni2 N6 2.056(4) 2 ? Ni2 N6 2.056(4) . ? Ni2 N8 2.099(4) . ? Ni2 N8 2.099(4) 2 ? Ni2 N8 2.099(4) 3 ? F1 B1 1.402(11) . ? F2 B1 1.371(9) . ? F3 B1 1.359(9) . ? F4 B1 1.350(11) . ? F5 F9 1.14(3) . ? F5 B2 1.37(3) . ? F6 B2 1.35(2) . ? F7 B2 1.34(2) . ? F7 F8 1.76(2) . ? F8 B2 1.40(2) . ? F9 B2 1.38(3) . ? F10 B3 1.3960 . ? F11 F12 1.2935 34_455 ? F11 B3 1.5943 . ? F11 B3 1.9386 34_455 ? F12 F11 1.2933 34_455 ? F12 B3 1.3522 . ? F13 B3 1.7223 . ? O1 C7 1.235(5) . ? O2 C8 1.220(5) . ? O3 C21 1.216(6) . ? O4 C22 1.227(6) . ? N1 C1 1.330(7) . ? N1 C5 1.355(8) . ? N2 C6 1.337(7) . ? N3 C6 1.292(6) . ? N3 N4 1.404(5) . ? N4 C7 1.320(6) . ? N5 C8 1.337(6) . ? N5 N6 1.407(5) . ? N6 C9 1.303(6) . ? N7 C9 1.332(7) . ? N8 C14 1.333(7) . ? N8 C10 1.358(7) . ? N9 C15 1.335(7) . ? N9 C19 1.345(7) . ? N10 C20 1.334(7) . ? N11 C20 1.305(6) . ? N11 N12 1.385(5) . ? N12 C21 1.343(6) 3 ? N13 C22 1.342(6) . ? N13 N14 1.397(6) . ? N14 C23 1.310(7) . ? N15 C23 1.327(8) . ? N16 C28 1.327(8) . ? N16 C24 1.330(7) . ? C1 C2 1.387(11) . ? C2 C3 1.354(14) . ? C3 C4 1.374(11) . ? C4 C5 1.371(9) . ? C5 C6 1.495(7) . ? C7 C8 1.531(6) . ? C9 C10 1.478(7) 2 ? C10 C11 1.393(8) . ? C10 C9 1.478(7) 3 ? C11 C12 1.393(9) . ? C12 C13 1.364(11) . ? C13 C14 1.370(10) . ? C15 C16 1.365(9) . ? C16 C17 1.361(11) . ? C17 C18 1.389(10) . ? C18 C19 1.373(8) . ? C19 C20 1.490(7) . ? C21 N12 1.343(6) 2 ? C21 C22 1.529(6) . ? C23 C24 1.485(8) . ? C24 C25 1.386(8) . ? C25 C26 1.378(10) . ? C26 C27 1.369(12) . ? C27 C28 1.404(10) . ? B3 F11 1.9389 34_455 ? 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 N3 Ni1 N11 94.69(16) . . ? N3 Ni1 N14 96.84(15) . . ? N11 Ni1 N14 97.00(16) . . ? N3 Ni1 N16 92.03(17) . . ? N11 Ni1 N16 171.75(18) . . ? N14 Ni1 N16 77.43(17) . . ? N3 Ni1 N1 77.21(16) . . ? N11 Ni1 N1 89.79(17) . . ? N14 Ni1 N1 171.35(17) . . ? N16 Ni1 N1 96.35(18) . . ? N3 Ni1 N9 169.60(17) . . ? N11 Ni1 N9 77.12(16) . . ? N14 Ni1 N9 90.58(17) . . ? N16 Ni1 N9 96.70(17) . . ? N1 Ni1 N9 96.16(18) . . ? N6 Ni2 N6 95.63(14) 3 2 ? N6 Ni2 N6 95.63(14) 3 . ? N6 Ni2 N6 95.64(14) 2 . ? N6 Ni2 N8 76.98(16) 3 . ? N6 Ni2 N8 172.22(16) 2 . ? N6 Ni2 N8 87.62(16) . . ? N6 Ni2 N8 172.22(16) 3 2 ? N6 Ni2 N8 87.62(16) 2 2 ? N6 Ni2 N8 76.98(16) . 2 ? N8 Ni2 N8 100.01(15) . 2 ? N6 Ni2 N8 87.62(16) 3 3 ? N6 Ni2 N8 76.98(16) 2 3 ? N6 Ni2 N8 172.22(16) . 3 ? N8 Ni2 N8 100.01(15) . 3 ? N8 Ni2 N8 100.01(15) 2 3 ? F9 F5 B2 66(2) . . ? B2 F7 F8 51.6(11) . . ? B2 F8 F7 48.6(11) . . ? F5 F9 B2 65(2) . . ? F12 F11 B3 135.002(1) 34_455 . ? F12 F11 B3 44.074(2) 34_455 34_455 ? B3 F11 B3 103.472(4) . 34_455 ? F11 F12 B3 94.2 34_455 . ? C1 N1 C5 118.1(5) . . ? C1 N1 Ni1 126.3(5) . . ? C5 N1 Ni1 115.3(3) . . ? C6 N3 N4 116.1(4) . . ? C6 N3 Ni1 118.1(3) . . ? N4 N3 Ni1 125.6(3) . . ? C7 N4 N3 121.9(4) . . ? C8 N5 N6 122.8(4) . . ? C9 N6 N5 115.9(4) . . ? C9 N6 Ni2 118.6(3) . . ? N5 N6 Ni2 124.9(3) . . ? C14 N8 C10 118.2(5) . . ? C14 N8 Ni2 126.6(4) . . ? C10 N8 Ni2 113.8(3) . . ? C15 N9 C19 118.1(5) . . ? C15 N9 Ni1 126.2(4) . . ? C19 N9 Ni1 115.3(3) . . ? C20 N11 N12 117.7(4) . . ? C20 N11 Ni1 117.1(3) . . ? N12 N11 Ni1 123.4(3) . . ? C21 N12 N11 123.2(4) 3 . ? C22 N13 N14 119.3(4) . . ? C23 N14 N13 113.6(4) . . ? C23 N14 Ni1 116.8(3) . . ? N13 N14 Ni1 127.7(3) . . ? C28 N16 C24 118.8(5) . . ? C28 N16 Ni1 125.6(4) . . ? C24 N16 Ni1 115.3(3) . . ? N1 C1 C2 122.3(7) . . ? C3 C2 C1 118.9(6) . . ? C2 C3 C4 119.7(7) . . ? C5 C4 C3 119.0(8) . . ? N1 C5 C4 121.9(5) . . ? N1 C5 C6 113.9(5) . . ? C4 C5 C6 124.1(6) . . ? N3 C6 N2 126.4(4) . . ? N3 C6 C5 114.7(4) . . ? N2 C6 C5 118.8(4) . . ? O1 C7 N4 126.2(4) . . ? O1 C7 C8 120.5(4) . . ? N4 C7 C8 113.2(4) . . ? O2 C8 N5 125.9(4) . . ? O2 C8 C7 123.5(4) . . ? N5 C8 C7 110.6(4) . . ? N6 C9 N7 125.8(4) . . ? N6 C9 C10 114.0(4) . 2 ? N7 C9 C10 120.2(4) . 2 ? N8 C10 C11 122.4(5) . . ? N8 C10 C9 114.6(4) . 3 ? C11 C10 C9 123.1(5) . 3 ? C12 C11 C10 117.4(6) . . ? C13 C12 C11 119.8(6) . . ? C12 C13 C14 119.6(6) . . ? N8 C14 C13 122.6(6) . . ? N9 C15 C16 123.3(6) . . ? C17 C16 C15 118.7(6) . . ? C16 C17 C18 119.0(6) . . ? C19 C18 C17 119.2(6) . . ? N9 C19 C18 121.5(5) . . ? N9 C19 C20 114.3(4) . . ? C18 C19 C20 124.1(5) . . ? N11 C20 N10 126.1(4) . . ? N11 C20 C19 114.2(4) . . ? N10 C20 C19 119.7(4) . . ? O3 C21 N12 126.1(4) . 2 ? O3 C21 C22 123.5(4) . . ? N12 C21 C22 110.4(4) 2 . ? O4 C22 N13 125.7(4) . . ? O4 C22 C21 121.5(4) . . ? N13 C22 C21 112.6(4) . . ? N14 C23 N15 126.3(5) . . ? N14 C23 C24 114.0(5) . . ? N15 C23 C24 119.7(5) . . ? N16 C24 C25 122.1(6) . . ? N16 C24 C23 115.2(5) . . ? C25 C24 C23 122.7(6) . . ? C26 C25 C24 119.3(7) . . ? C27 C26 C25 118.9(6) . . ? C26 C27 C28 118.6(6) . . ? N16 C28 C27 122.3(6) . . ? F4 B1 F3 113.6(7) . . ? F4 B1 F2 109.9(7) . . ? F3 B1 F2 110.6(6) . . ? F4 B1 F1 105.9(8) . . ? F3 B1 F1 108.0(7) . . ? F2 B1 F1 108.6(7) . . ? F7 B2 F6 104.1(16) . . ? F7 B2 F5 95.5(19) . . ? F6 B2 F5 111.1(19) . . ? F7 B2 F9 131(2) . . ? F6 B2 F9 118.6(18) . . ? F5 B2 F9 49.2(15) . . ? F7 B2 F8 79.8(15) . . ? F6 B2 F8 112.3(16) . . ? F5 B2 F8 136(2) . . ? F9 B2 F8 102.7(17) . . ? F12 B3 F10 132.670(1) . . ? F12 B3 F11 109.513(2) . . ? F10 B3 F11 108.807(3) . . ? F12 B3 F13 97.949(1) . . ? F10 B3 F13 106.583(1) . . ? F11 B3 F13 93.194(1) . . ? F12 B3 F11 41.700(2) . 34_455 ? F10 B3 F11 154.558(1) . 34_455 ? F11 B3 F11 67.835(4) . 34_455 ? F13 B3 F11 98.8 . 34_455 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.770 _refine_diff_density_min -1.186 _refine_diff_density_rms 0.145 #===END data_shelxl_(10) _database_code_depnum_ccdc_archive 'CCDC 228046' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H38 N10 Ni4 O18' _chemical_formula_weight 1061.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5023(6) _cell_length_b 25.4503(18) _cell_length_c 18.7049(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.8050(10) _cell_angle_gamma 90.00 _cell_volume 3988.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4823 _cell_measurement_theta_min 2.351 _cell_measurement_theta_max 26.354 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 1.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6019 _exptl_absorpt_correction_T_max 0.8441 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22448 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 26.40 _reflns_number_total 8135 _reflns_number_gt 6446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'teXsan for Windows (MSC, 1997)' _computing_publication_material 'teXsan for Windows (MSC, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+13.2343P] 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 8135 _refine_ls_number_parameters 553 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.012 _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 0.38414(7) 0.10006(2) 0.45730(3) 0.02185(15) Uani 1 1 d . . . Ni2 Ni 0.58175(7) 0.22603(2) 0.34549(3) 0.01668(14) Uani 1 1 d . . . Ni3 Ni 0.63569(7) 0.40943(2) 0.37547(3) 0.01889(15) Uani 1 1 d . . . Ni4 Ni 0.35152(7) 0.28402(2) 0.44801(3) 0.01646(14) Uani 1 1 d . . . O1 O 0.5852(4) 0.05579(13) 0.49496(19) 0.0279(8) Uani 1 1 d . . . O2 O 0.7854(4) 0.01984(14) 0.4484(2) 0.0427(10) Uani 1 1 d . . . O3 O 0.3129(5) 0.10844(14) 0.2510(2) 0.0360(9) Uani 1 1 d . . . O4 O 0.5387(4) 0.37308(12) 0.28037(17) 0.0228(7) Uani 1 1 d . . . O5 O 0.7318(4) 0.21220(12) 0.42511(17) 0.0229(7) Uani 1 1 d . . . O6 O 0.9552(4) 0.23173(14) 0.4989(2) 0.0348(9) Uani 1 1 d . . . O7 O 0.7147(4) 0.44791(12) 0.46865(18) 0.0241(7) Uani 1 1 d . . . O8 O 0.6387(4) 0.47682(14) 0.56961(19) 0.0300(8) Uani 1 1 d . . . O9 O 0.2039(4) 0.40775(13) 0.3234(2) 0.0309(8) Uani 1 1 d . . . O10 O 0.1922(4) 0.14044(12) 0.40428(18) 0.0230(7) Uani 1 1 d . . . O11 O 0.5165(4) 0.29146(12) 0.52374(17) 0.0232(7) Uani 1 1 d . . . O12 O 0.6585(5) 0.26350(15) 0.6262(2) 0.0419(10) Uani 1 1 d . . . O13 O 0.3129(4) 0.02824(13) 0.40994(19) 0.0278(8) Uani 1 1 d . . . O14 O 0.2698(4) 0.08236(14) 0.5435(2) 0.0321(8) Uani 1 1 d . . . O15 O 0.8437(4) 0.42639(14) 0.33993(18) 0.0287(8) Uani 1 1 d . . . O16 O 0.5345(4) 0.48027(13) 0.33690(18) 0.0276(8) Uani 1 1 d . . . O17 O 1.0393(10) 0.4861(3) 0.4303(5) 0.123(3) Uiso 1 1 d . . . O18 O -0.073(3) 0.1021(8) 0.1851(13) 0.196(8) Uiso 0.60 1 d P . . O19 O 0.058(2) 0.0821(8) 0.1461(11) 0.108(6) Uiso 0.40 1 d P . . N1 N 0.5225(5) 0.11670(14) 0.3802(2) 0.0213(8) Uani 1 1 d . . . N2 N 0.4975(4) 0.15756(14) 0.3290(2) 0.0203(8) Uani 1 1 d . . . N3 N 0.4418(4) 0.23933(14) 0.26271(19) 0.0182(7) Uani 1 1 d . . . N4 N 0.6225(4) 0.29690(14) 0.34350(19) 0.0180(7) Uani 1 1 d . . . N5 N 0.7161(4) 0.32785(14) 0.39495(19) 0.0178(7) Uani 1 1 d . . . N6 N 0.4554(4) 0.39256(14) 0.4348(2) 0.0195(8) Uani 1 1 d . . . N7 N 0.3353(4) 0.35502(14) 0.4169(2) 0.0191(8) Uani 1 1 d . . . N8 N 0.1825(4) 0.27623(14) 0.37497(19) 0.0165(7) Uani 1 1 d . . . N9 N 0.3316(4) 0.21229(14) 0.4581(2) 0.0182(8) Uani 1 1 d . . . N10 N 0.4334(4) 0.17746(15) 0.4999(2) 0.0206(8) Uani 1 1 d . . . C1 C 0.6796(6) 0.05268(18) 0.4484(3) 0.0274(11) Uani 1 1 d . . . C2 C 0.6572(6) 0.09295(18) 0.3885(3) 0.0241(10) Uani 1 1 d . . . C3 C 0.7848(6) 0.1001(2) 0.3449(3) 0.0342(12) Uani 1 1 d . . . C4 C 0.3845(6) 0.14912(18) 0.2703(3) 0.0239(10) Uani 1 1 d . . . C5 C 0.3559(5) 0.20039(18) 0.2286(2) 0.0213(9) Uani 1 1 d . . . C6 C 0.2498(6) 0.21001(19) 0.1656(3) 0.0244(10) Uani 1 1 d . . . C7 C 0.2352(6) 0.2614(2) 0.1387(3) 0.0271(10) Uani 1 1 d . . . C8 C 0.3272(6) 0.30165(18) 0.1755(2) 0.0224(9) Uani 1 1 d . . . C9 C 0.4314(5) 0.28918(17) 0.2383(2) 0.0191(9) Uani 1 1 d . . . C10 C 0.5368(5) 0.32454(17) 0.2888(2) 0.0174(9) Uani 1 1 d . . . C11 C 0.8129(5) 0.30487(18) 0.4456(2) 0.0195(9) Uani 1 1 d . . . C12 C 0.9167(6) 0.3379(2) 0.5002(3) 0.0310(11) Uani 1 1 d . . . C13 C 0.8362(5) 0.24549(18) 0.4570(2) 0.0213(9) Uani 1 1 d . . . C14 C 0.6199(5) 0.44901(17) 0.5137(2) 0.0210(9) Uani 1 1 d . . . C15 C 0.4747(5) 0.41335(17) 0.4982(3) 0.0226(10) Uani 1 1 d . . . C16 C 0.3716(7) 0.4058(2) 0.5539(3) 0.0355(12) Uani 1 1 d . . . C17 C 0.2250(5) 0.36646(18) 0.3575(2) 0.0218(9) Uani 1 1 d . . . C18 C 0.1268(5) 0.31817(17) 0.3356(2) 0.0189(9) Uani 1 1 d . . . C19 C 0.0005(5) 0.31223(18) 0.2785(3) 0.0230(10) Uani 1 1 d . . . C20 C -0.0632(6) 0.26240(19) 0.2633(3) 0.0248(10) Uani 1 1 d . . . C21 C 0.0002(6) 0.21916(18) 0.3044(3) 0.0235(10) Uani 1 1 d . . . C22 C 0.1234(5) 0.22769(17) 0.3613(2) 0.0188(9) Uani 1 1 d . . . C23 C 0.2161(5) 0.18851(17) 0.4103(2) 0.0200(9) Uani 1 1 d . . . C24 C 0.5438(5) 0.19655(18) 0.5489(3) 0.0224(9) Uani 1 1 d . . . C25 C 0.6563(6) 0.1590(2) 0.5926(3) 0.0319(11) Uani 1 1 d . . . C26 C 0.5748(5) 0.25448(19) 0.5682(3) 0.0239(10) Uani 1 1 d . . . C27 C 0.1490(7) 0.0195(2) 0.3798(3) 0.0370(13) Uani 1 1 d . . . C28 C 0.1147(7) 0.1034(2) 0.5509(3) 0.0391(13) Uani 1 1 d . . . C29 C 0.8436(7) 0.4508(3) 0.2721(4) 0.0481(16) Uani 1 1 d . . . C30 C 0.4452(7) 0.4903(2) 0.2659(3) 0.0390(13) Uani 1 1 d . . . H1 H 0.8844 0.1049 0.3763 0.041 Uiso 1 1 d . . . H2 H 0.7913 0.0697 0.3157 0.041 Uiso 1 1 d . . . H3 H 0.7625 0.1299 0.3145 0.041 Uiso 1 1 d . . . H4 H 0.1877 0.1824 0.1411 0.029 Uiso 1 1 d . . . H5 H 0.1628 0.2687 0.0952 0.032 Uiso 1 1 d . . . H6 H 0.3181 0.3368 0.1579 0.027 Uiso 1 1 d . . . H7 H 0.8952 0.3304 0.5473 0.036 Uiso 1 1 d . . . H8 H 1.0253 0.3309 0.4984 0.036 Uiso 1 1 d . . . H9 H 0.8947 0.3741 0.4895 0.036 Uiso 1 1 d . . . H10 H 0.4333 0.4108 0.6007 0.042 Uiso 1 1 d . . . H11 H 0.2868 0.4304 0.5461 0.042 Uiso 1 1 d . . . H12 H 0.3295 0.3711 0.5503 0.042 Uiso 1 1 d . . . H13 H -0.0414 0.3420 0.2507 0.027 Uiso 1 1 d . . . H14 H -0.1500 0.2575 0.2244 0.030 Uiso 1 1 d . . . H15 H -0.0412 0.1851 0.2935 0.028 Uiso 1 1 d . . . H16 H 0.6454 0.1614 0.6424 0.038 Uiso 1 1 d . . . H17 H 0.6312 0.1240 0.5762 0.038 Uiso 1 1 d . . . H18 H 0.7624 0.1670 0.5876 0.038 Uiso 1 1 d . . . H19 H 0.0886 0.0167 0.4184 0.044 Uiso 1 1 d . . . H20 H 0.1101 0.0478 0.3494 0.044 Uiso 1 1 d . . . H21 H 0.1391 -0.0124 0.3530 0.044 Uiso 1 1 d . . . H22 H 0.1056 0.1052 0.6008 0.046 Uiso 1 1 d . . . H23 H 0.1030 0.1376 0.5304 0.046 Uiso 1 1 d . . . H24 H 0.0320 0.0813 0.5263 0.046 Uiso 1 1 d . . . H25 H 0.8443 0.4881 0.2781 0.056 Uiso 1 1 d . . . H26 H 0.9355 0.4405 0.2532 0.056 Uiso 1 1 d . . . H27 H 0.7504 0.4409 0.2395 0.056 Uiso 1 1 d . . . H28 H 0.3416 0.5027 0.2700 0.047 Uiso 1 1 d . . . H29 H 0.4985 0.5162 0.2422 0.047 Uiso 1 1 d . . . H30 H 0.4359 0.4588 0.2382 0.047 Uiso 1 1 d . . . H31 H 0.3612 0.0005 0.4405 0.076 Uiso 1 1 d . . . H32 H 0.2626 0.0451 0.5441 0.076 Uiso 1 1 d . . . H33 H 0.9073 0.4426 0.3755 0.076 Uiso 1 1 d . . . H34 H 1.0271 0.5088 0.3879 0.076 Uiso 1 1 d . . . H35 H 1.0942 0.4554 0.4133 0.076 Uiso 1 1 d . . . H36 H -0.0361 0.0852 0.1323 0.076 Uiso 1 1 d . . . H37 H -0.0103 0.1124 0.2056 0.076 Uiso 0.60 1 d P . . H38 H 0.0236 0.0470 0.1394 0.076 Uiso 0.40 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0216(3) 0.0179(3) 0.0250(3) 0.0044(2) 0.0012(2) 0.0001(2) Ni2 0.0175(3) 0.0177(3) 0.0134(3) 0.0007(2) -0.0013(2) -0.0007(2) Ni3 0.0220(3) 0.0183(3) 0.0159(3) -0.0007(2) 0.0019(2) -0.0027(2) Ni4 0.0175(3) 0.0171(3) 0.0137(3) 0.0007(2) -0.0007(2) -0.0017(2) O1 0.0252(17) 0.0265(18) 0.0309(19) 0.0088(14) 0.0016(15) 0.0018(14) O2 0.031(2) 0.029(2) 0.070(3) 0.0202(19) 0.016(2) 0.0096(16) O3 0.046(2) 0.0245(18) 0.034(2) -0.0051(15) -0.0052(17) -0.0087(16) O4 0.0300(18) 0.0215(16) 0.0157(16) 0.0015(12) 0.0005(13) -0.0006(13) O5 0.0242(17) 0.0224(16) 0.0196(17) 0.0022(12) -0.0033(13) 0.0009(13) O6 0.0300(19) 0.035(2) 0.032(2) 0.0008(16) -0.0148(16) 0.0043(15) O7 0.0255(17) 0.0256(17) 0.0213(17) -0.0063(13) 0.0039(14) -0.0063(13) O8 0.0295(18) 0.0345(19) 0.0252(18) -0.0150(15) 0.0022(15) -0.0070(15) O9 0.0314(19) 0.0232(17) 0.035(2) 0.0097(15) -0.0046(15) -0.0009(14) O10 0.0216(16) 0.0192(16) 0.0270(18) 0.0025(13) 0.0007(13) -0.0012(12) O11 0.0259(17) 0.0223(16) 0.0182(16) -0.0001(12) -0.0052(13) -0.0033(13) O12 0.051(2) 0.035(2) 0.030(2) 0.0012(16) -0.0215(18) -0.0026(18) O13 0.0272(18) 0.0236(17) 0.0318(19) 0.0020(14) 0.0024(15) -0.0014(14) O14 0.035(2) 0.0267(18) 0.036(2) 0.0087(15) 0.0096(16) 0.0002(15) O15 0.0286(18) 0.0351(19) 0.0234(18) 0.0004(14) 0.0078(14) -0.0060(15) O16 0.0360(19) 0.0218(17) 0.0248(18) 0.0050(13) 0.0045(15) 0.0025(14) N1 0.025(2) 0.0138(18) 0.023(2) 0.0015(15) -0.0027(16) -0.0035(15) N2 0.0230(19) 0.0180(19) 0.0192(19) 0.0027(14) 0.0017(15) -0.0022(15) N3 0.0176(18) 0.0227(19) 0.0134(18) -0.0021(14) 0.0004(14) 0.0008(14) N4 0.0208(19) 0.0200(18) 0.0119(18) -0.0018(14) -0.0006(14) -0.0005(15) N5 0.0187(18) 0.0185(18) 0.0152(18) -0.0018(14) 0.0005(14) -0.0028(14) N6 0.0224(19) 0.0155(18) 0.020(2) 0.0013(14) 0.0014(15) -0.0024(14) N7 0.0194(18) 0.0174(18) 0.0202(19) -0.0009(14) 0.0020(15) -0.0023(14) N8 0.0140(17) 0.0207(18) 0.0148(18) 0.0003(14) 0.0021(14) -0.0006(14) N9 0.0186(18) 0.0184(18) 0.0168(19) 0.0030(14) 0.0008(15) -0.0001(14) N10 0.0207(19) 0.0226(19) 0.0192(19) 0.0030(15) 0.0050(15) -0.0006(15) C1 0.020(2) 0.021(2) 0.040(3) 0.004(2) 0.001(2) -0.0014(19) C2 0.022(2) 0.018(2) 0.032(3) 0.0001(18) 0.0003(19) -0.0018(18) C3 0.026(3) 0.031(3) 0.045(3) 0.009(2) 0.008(2) 0.001(2) C4 0.027(2) 0.025(2) 0.019(2) -0.0037(18) 0.0021(19) -0.0028(19) C5 0.022(2) 0.026(2) 0.017(2) -0.0032(18) 0.0052(18) -0.0017(18) C6 0.024(2) 0.032(3) 0.016(2) -0.0060(18) 0.0000(18) -0.0039(19) C7 0.024(2) 0.038(3) 0.017(2) 0.0005(19) -0.0029(19) 0.000(2) C8 0.024(2) 0.026(2) 0.016(2) 0.0012(18) -0.0008(18) 0.0018(18) C9 0.022(2) 0.021(2) 0.014(2) -0.0001(16) 0.0033(17) 0.0009(17) C10 0.018(2) 0.019(2) 0.015(2) 0.0006(16) 0.0034(16) -0.0006(16) C11 0.016(2) 0.027(2) 0.016(2) -0.0022(17) 0.0024(17) -0.0042(17) C12 0.031(3) 0.031(3) 0.026(3) -0.005(2) -0.009(2) -0.002(2) C13 0.020(2) 0.026(2) 0.017(2) 0.0007(17) 0.0022(18) 0.0023(18) C14 0.024(2) 0.019(2) 0.019(2) -0.0011(17) 0.0010(18) 0.0002(18) C15 0.024(2) 0.019(2) 0.024(2) 0.0013(18) 0.0031(19) -0.0008(18) C16 0.041(3) 0.039(3) 0.030(3) -0.012(2) 0.015(2) -0.015(2) C17 0.018(2) 0.026(2) 0.021(2) 0.0011(18) 0.0013(18) 0.0012(18) C18 0.018(2) 0.023(2) 0.016(2) 0.0011(17) 0.0032(17) 0.0012(17) C19 0.021(2) 0.027(2) 0.021(2) 0.0040(18) 0.0008(18) 0.0037(18) C20 0.022(2) 0.032(3) 0.018(2) -0.0005(19) -0.0011(18) -0.0012(19) C21 0.022(2) 0.023(2) 0.024(2) -0.0031(18) 0.0020(19) -0.0049(18) C22 0.015(2) 0.023(2) 0.018(2) -0.0008(17) 0.0032(17) -0.0020(17) C23 0.020(2) 0.022(2) 0.018(2) 0.0011(17) 0.0037(17) -0.0009(17) C24 0.021(2) 0.028(2) 0.018(2) 0.0028(18) 0.0026(18) 0.0014(18) C25 0.036(3) 0.032(3) 0.024(3) 0.001(2) -0.005(2) 0.007(2) C26 0.021(2) 0.030(3) 0.020(2) 0.0024(19) 0.0015(19) -0.0022(19) C27 0.033(3) 0.034(3) 0.041(3) -0.004(2) -0.003(2) -0.001(2) C28 0.040(3) 0.036(3) 0.042(3) -0.003(2) 0.010(3) 0.000(2) C29 0.038(3) 0.063(4) 0.045(4) 0.024(3) 0.015(3) 0.006(3) C30 0.046(3) 0.037(3) 0.032(3) 0.006(2) 0.001(3) 0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O10 2.038(3) . ? Ni1 N1 2.055(4) . ? Ni1 O1 2.068(3) . ? Ni1 O14 2.069(4) . ? Ni1 O13 2.076(3) . ? Ni1 N10 2.139(4) . ? Ni2 N3 1.817(4) . ? Ni2 O5 1.823(3) . ? Ni2 N4 1.838(4) . ? Ni2 N2 1.890(4) . ? Ni3 O7 2.012(3) . ? Ni3 O15 2.039(3) . ? Ni3 O4 2.049(3) . ? Ni3 O16 2.074(3) . ? Ni3 N6 2.084(4) . ? Ni3 N5 2.197(4) . ? Ni4 N8 1.817(4) . ? Ni4 O11 1.826(3) . ? Ni4 N9 1.846(4) . ? Ni4 N7 1.896(4) . ? O1 C1 1.284(6) . ? O2 C1 1.228(6) . ? O3 C4 1.224(6) . ? O4 C10 1.246(5) . ? O5 C13 1.297(6) . ? O6 C13 1.221(6) . ? O7 C14 1.262(6) . ? O8 C14 1.251(6) . ? O9 C17 1.226(6) . ? O10 C23 1.242(5) . ? O11 C26 1.298(6) . ? O12 C26 1.213(6) . ? O13 C27 1.429(6) . ? O14 C28 1.452(7) . ? O15 C29 1.412(7) . ? O16 C30 1.436(6) . ? O18 O19 1.52(3) . ? N1 C2 1.280(6) . ? N1 N2 1.405(5) . ? N2 C4 1.346(6) . ? N3 C5 1.328(6) . ? N3 C9 1.346(6) . ? N4 C10 1.348(6) . ? N4 N5 1.386(5) . ? N5 C11 1.285(6) . ? N6 C15 1.283(6) . ? N6 N7 1.397(5) . ? N7 C17 1.359(6) . ? N8 C18 1.337(6) . ? N8 C22 1.342(6) . ? N9 C23 1.353(6) . ? N9 N10 1.384(5) . ? N10 C24 1.290(6) . ? C1 C2 1.506(7) . ? C2 C3 1.476(7) . ? C4 C5 1.519(7) . ? C5 C6 1.378(6) . ? C6 C7 1.400(7) . ? C7 C8 1.396(7) . ? C8 C9 1.383(6) . ? C9 C10 1.489(6) . ? C11 C12 1.491(6) . ? C11 C13 1.534(6) . ? C14 C15 1.520(6) . ? C15 C16 1.484(7) . ? C17 C18 1.503(6) . ? C18 C19 1.387(6) . ? C19 C20 1.389(7) . ? C20 C21 1.398(7) . ? C21 C22 1.377(6) . ? C22 C23 1.486(6) . ? C24 C25 1.494(6) . ? C24 C26 1.530(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Ni1 N1 93.51(14) . . ? O10 Ni1 O1 170.94(14) . . ? N1 Ni1 O1 79.20(14) . . ? O10 Ni1 O14 92.60(14) . . ? N1 Ni1 O14 173.23(15) . . ? O1 Ni1 O14 94.98(14) . . ? O10 Ni1 O13 94.88(13) . . ? N1 Ni1 O13 92.42(14) . . ? O1 Ni1 O13 80.20(13) . . ? O14 Ni1 O13 89.95(14) . . ? O10 Ni1 N10 78.85(13) . . ? N1 Ni1 N10 88.43(14) . . ? O1 Ni1 N10 106.07(14) . . ? O14 Ni1 N10 89.91(14) . . ? O13 Ni1 N10 173.72(14) . . ? N3 Ni2 O5 176.44(16) . . ? N3 Ni2 N4 84.15(16) . . ? O5 Ni2 N4 95.61(15) . . ? N3 Ni2 N2 81.80(16) . . ? O5 Ni2 N2 98.56(15) . . ? N4 Ni2 N2 165.72(16) . . ? O7 Ni3 O15 89.95(14) . . ? O7 Ni3 O4 175.60(13) . . ? O15 Ni3 O4 93.19(14) . . ? O7 Ni3 O16 86.31(14) . . ? O15 Ni3 O16 91.95(14) . . ? O4 Ni3 O16 90.50(13) . . ? O7 Ni3 N6 78.83(14) . . ? O15 Ni3 N6 167.05(14) . . ? O4 Ni3 N6 98.38(14) . . ? O16 Ni3 N6 93.74(14) . . ? O7 Ni3 N5 105.53(13) . . ? O15 Ni3 N5 89.50(14) . . ? O4 Ni3 N5 77.60(13) . . ? O16 Ni3 N5 168.08(13) . . ? N6 Ni3 N5 87.33(14) . . ? N8 Ni4 O11 177.94(16) . . ? N8 Ni4 N9 83.93(16) . . ? O11 Ni4 N9 95.46(15) . . ? N8 Ni4 N7 82.34(16) . . ? O11 Ni4 N7 98.34(15) . . ? N9 Ni4 N7 166.09(16) . . ? C1 O1 Ni1 112.2(3) . . ? C10 O4 Ni3 110.4(3) . . ? C13 O5 Ni2 125.4(3) . . ? C14 O7 Ni3 115.6(3) . . ? C23 O10 Ni1 110.3(3) . . ? C26 O11 Ni4 125.6(3) . . ? C27 O13 Ni1 119.9(3) . . ? C28 O14 Ni1 123.3(3) . . ? C29 O15 Ni3 121.2(3) . . ? C30 O16 Ni3 126.8(3) . . ? C2 N1 N2 117.5(4) . . ? C2 N1 Ni1 115.1(3) . . ? N2 N1 Ni1 126.3(3) . . ? C4 N2 N1 116.2(4) . . ? C4 N2 Ni2 118.6(3) . . ? N1 N2 Ni2 124.2(3) . . ? C5 N3 C9 122.8(4) . . ? C5 N3 Ni2 119.8(3) . . ? C9 N3 Ni2 117.4(3) . . ? C10 N4 N5 113.7(3) . . ? C10 N4 Ni2 116.6(3) . . ? N5 N4 Ni2 129.2(3) . . ? C11 N5 N4 118.2(4) . . ? C11 N5 Ni3 134.0(3) . . ? N4 N5 Ni3 107.2(2) . . ? C15 N6 N7 118.4(4) . . ? C15 N6 Ni3 114.7(3) . . ? N7 N6 Ni3 126.0(3) . . ? C17 N7 N6 115.1(4) . . ? C17 N7 Ni4 117.3(3) . . ? N6 N7 Ni4 124.5(3) . . ? C18 N8 C22 122.9(4) . . ? C18 N8 Ni4 119.2(3) . . ? C22 N8 Ni4 117.8(3) . . ? C23 N9 N10 113.6(3) . . ? C23 N9 Ni4 116.3(3) . . ? N10 N9 Ni4 129.2(3) . . ? C24 N10 N9 118.0(4) . . ? C24 N10 Ni1 133.2(3) . . ? N9 N10 Ni1 108.4(3) . . ? O2 C1 O1 125.7(5) . . ? O2 C1 C2 117.6(5) . . ? O1 C1 C2 116.6(4) . . ? N1 C2 C3 127.0(5) . . ? N1 C2 C1 114.1(4) . . ? C3 C2 C1 118.9(4) . . ? O3 C4 N2 128.7(5) . . ? O3 C4 C5 123.2(4) . . ? N2 C4 C5 108.1(4) . . ? N3 C5 C6 120.3(4) . . ? N3 C5 C4 111.6(4) . . ? C6 C5 C4 128.0(4) . . ? C5 C6 C7 118.6(4) . . ? C8 C7 C6 120.0(4) . . ? C9 C8 C7 118.3(4) . . ? N3 C9 C8 120.0(4) . . ? N3 C9 C10 110.9(4) . . ? C8 C9 C10 129.0(4) . . ? O4 C10 N4 126.6(4) . . ? O4 C10 C9 122.6(4) . . ? N4 C10 C9 110.8(4) . . ? N5 C11 C12 118.6(4) . . ? N5 C11 C13 127.1(4) . . ? C12 C11 C13 114.3(4) . . ? O6 C13 O5 122.4(4) . . ? O6 C13 C11 116.4(4) . . ? O5 C13 C11 121.2(4) . . ? O8 C14 O7 124.5(4) . . ? O8 C14 C15 118.8(4) . . ? O7 C14 C15 116.8(4) . . ? N6 C15 C16 126.7(4) . . ? N6 C15 C14 113.2(4) . . ? C16 C15 C14 120.1(4) . . ? O9 C17 N7 128.9(4) . . ? O9 C17 C18 122.3(4) . . ? N7 C17 C18 108.8(4) . . ? N8 C18 C19 119.5(4) . . ? N8 C18 C17 112.0(4) . . ? C19 C18 C17 128.3(4) . . ? C18 C19 C20 118.8(4) . . ? C19 C20 C21 120.3(4) . . ? C22 C21 C20 118.2(4) . . ? N8 C22 C21 120.3(4) . . ? N8 C22 C23 110.9(4) . . ? C21 C22 C23 128.6(4) . . ? O10 C23 N9 126.1(4) . . ? O10 C23 C22 122.9(4) . . ? N9 C23 C22 110.9(4) . . ? N10 C24 C25 118.0(4) . . ? N10 C24 C26 127.3(4) . . ? C25 C24 C26 114.7(4) . . ? O12 C26 O11 122.5(5) . . ? O12 C26 C24 116.4(4) . . ? O11 C26 C24 121.0(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.365 _refine_diff_density_min -1.128 _refine_diff_density_rms 0.140