# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chen, Xiao-Ming' _publ_contact_author_email cxm@mail.sysu.edu.cn loop_ _publ_author_name 'Xiao-Ming Chen' 'Qing Chen' 'Wei Xue' 'Rui-Biao Lin' 'Hua Zeng' data_1 _database_code_depnum_ccdc_archive 'CCDC 850281' #TrackingRef '- M4_120104.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H50 Co4 N6 O23' _chemical_formula_weight 1170.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0975(6) _cell_length_b 18.1635(9) _cell_length_c 21.5542(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.2380(10) _cell_angle_gamma 90.00 _cell_volume 5011.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 1.385 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6695 _exptl_absorpt_correction_T_max 0.7722 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 ? _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 22483 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9725 _reflns_number_gt 7478 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0612P)^2^+17.5000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9725 _refine_ls_number_parameters 502 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.006 _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 0.97164(5) 0.21664(3) 0.21797(3) 0.01698(14) Uani 1 1 d . . . C1 C 1.2951(4) 0.5021(2) 0.2413(2) 0.0231(9) Uani 1 1 d . . . N1 N 1.4355(3) 0.61857(19) 0.27415(17) 0.0228(8) Uani 1 1 d . . . O11 O 1.1438(2) 0.43892(16) 0.25260(14) 0.0249(7) Uani 1 1 d . . . Co3 Co 0.77503(5) 0.29236(3) 0.13423(3) 0.01901(15) Uani 1 1 d . . . C2 C 1.3735(4) 0.5147(3) 0.2090(2) 0.0273(10) Uani 1 1 d . . . H2A H 1.3807 0.4834 0.1749 0.033 Uiso 1 1 calc R . . N2 N 0.8688(5) 0.0122(3) -0.0322(3) 0.0675(17) Uani 1 1 d . . . O12 O 1.2194(2) 0.40582(16) 0.17261(14) 0.0238(7) Uani 1 1 d . . . Co2 Co 1.00993(4) 0.37753(3) 0.23405(3) 0.01774(14) Uani 1 1 d . . . C3 C 1.4421(4) 0.5728(3) 0.2263(2) 0.0286(10) Uani 1 1 d . . . H3A H 1.4957 0.5806 0.2034 0.034 Uiso 1 1 calc R . . N3 N 0.5738(3) -0.03022(19) 0.24378(17) 0.0212(8) Uani 1 1 d . . . O5 O 0.9036(2) 0.22003(16) 0.11822(13) 0.0215(6) Uani 1 1 d . . . Co4 Co 1.10941(5) 0.33385(3) 0.11846(3) 0.01939(15) Uani 1 1 d . . . C4 C 1.3619(4) 0.6043(3) 0.3071(2) 0.0279(10) Uani 1 1 d . . . H4A H 1.3583 0.6350 0.3423 0.033 Uiso 1 1 calc R . . N4 N 0.8811(3) 0.6040(2) -0.03411(18) 0.0240(8) Uani 1 1 d . . . O6 O 1.0132(3) 0.25871(17) 0.05783(14) 0.0263(7) Uani 1 1 d . . . C5 C 1.2913(4) 0.5477(3) 0.2927(2) 0.0294(11) Uani 1 1 d . . . H5A H 1.2405 0.5397 0.3175 0.035 Uiso 1 1 calc R . . N5 N 0.6838(3) 0.2648(2) 0.04383(17) 0.0258(8) Uani 1 1 d . . . O7 O 0.8513(2) 0.15014(17) 0.22988(15) 0.0260(7) Uani 1 1 d . . . C6 C 1.2132(3) 0.4434(2) 0.2205(2) 0.0223(9) Uani 1 1 d . . . N6 N 0.5389(15) 0.3578(11) 0.2940(10) 0.69(4) Uiso 1 1 d D . . O8 O 0.7098(2) 0.20277(16) 0.16899(14) 0.0245(7) Uani 1 1 d . . . C7 C 0.9263(4) 0.1433(3) 0.0350(2) 0.0316(11) Uani 1 1 d . . . O3 O 0.9870(2) 0.41158(16) 0.13389(13) 0.0212(6) Uani 1 1 d . . . C8 C 0.8928(5) 0.0812(3) 0.0643(3) 0.0416(13) Uani 1 1 d . . . H8A H 0.8885 0.0829 0.1078 0.050 Uiso 1 1 calc R . . O4 O 0.8201(3) 0.38557(17) 0.09134(15) 0.0290(7) Uani 1 1 d . . . C9 C 0.8662(6) 0.0176(3) 0.0291(4) 0.0587(18) Uani 1 1 d . . . H9A H 0.8450 -0.0242 0.0496 0.070 Uiso 1 1 calc R . . O9 O 0.5187(3) 0.27574(16) -0.18463(13) 0.0248(7) Uani 1 1 d . . . C10 C 0.9027(6) 0.0715(4) -0.0590(3) 0.0613(19) Uani 1 1 d . . . H10A H 0.9052 0.0683 -0.1027 0.074 Uiso 1 1 calc R . . O10 O 0.5472(2) 0.15419(17) -0.17036(14) 0.0247(7) Uani 1 1 d . . . C11 C 0.9345(5) 0.1375(3) -0.0278(3) 0.0468(15) Uani 1 1 d . . . H11A H 0.9607 0.1770 -0.0487 0.056 Uiso 1 1 calc R . . O1 O 0.8794(2) 0.31170(15) 0.21646(13) 0.0185(6) Uani 1 1 d . . . H1A H 0.8440 0.3122 0.2533 0.022 Uiso 1 1 calc R . . C12 C 0.9509(4) 0.2135(2) 0.0728(2) 0.0232(10) Uani 1 1 d . . . O2 O 1.0852(2) 0.28712(15) 0.20048(13) 0.0183(6) Uani 1 1 d . . . H2B H 1.1535 0.2766 0.2300 0.022 Uiso 1 1 calc R . . C13 C 0.6905(4) 0.0896(2) 0.2180(2) 0.0228(9) Uani 1 1 d . . . C14 C 0.5870(5) 0.0840(3) 0.1922(4) 0.059(2) Uani 1 1 d . . . H14A H 0.5529 0.1215 0.1647 0.070 Uiso 1 1 calc R . . O14 O 0.6518(3) 0.35476(18) 0.15747(16) 0.0311(8) Uani 1 1 d . . . C15 C 0.5311(4) 0.0236(3) 0.2060(4) 0.059(2) Uani 1 1 d . . . H15A H 0.4586 0.0209 0.1874 0.071 Uiso 1 1 calc R . . O15 O 0.4537(14) 0.3602(10) 0.3063(9) 0.311(8) Uiso 1 1 d D . . C16 C 0.6742(4) -0.0237(3) 0.2679(4) 0.060(2) Uani 1 1 d . . . H16A H 0.7070 -0.0616 0.2955 0.072 Uiso 1 1 calc R . . O16 O 0.6008(12) 0.4055(8) 0.3118(7) 0.258(6) Uiso 1 1 d D . . C17 C 0.7347(5) 0.0338(3) 0.2562(4) 0.067(2) Uani 1 1 d . . . H17A H 0.8072 0.0346 0.2748 0.080 Uiso 1 1 calc R . . O17 O 0.5499(10) 0.3158(7) 0.2534(6) 0.211(5) Uiso 1 1 d D . . C18 C 0.7562(4) 0.1528(2) 0.20457(19) 0.0208(9) Uani 1 1 d . . . C19 C 0.8910(4) 0.4911(2) 0.0548(2) 0.0228(9) Uani 1 1 d . . . C20 C 0.8048(4) 0.4992(3) 0.0051(2) 0.0334(12) Uani 1 1 d . . . H20A H 0.7472 0.4664 0.0007 0.040 Uiso 1 1 calc R . . C21 C 0.8043(4) 0.5555(3) -0.0379(2) 0.0343(12) Uani 1 1 d . . . H21A H 0.7455 0.5598 -0.0721 0.041 Uiso 1 1 calc R . . C22 C 0.9606(4) 0.6000(2) 0.0167(2) 0.0247(10) Uani 1 1 d . . . H22A H 1.0136 0.6366 0.0221 0.030 Uiso 1 1 calc R . . C24 C 0.9682(4) 0.5443(2) 0.0616(2) 0.0240(10) Uani 1 1 d . . . H24A H 1.0260 0.5427 0.0967 0.029 Uiso 1 1 calc R . . C25 C 0.8992(3) 0.4239(2) 0.09740(19) 0.0202(9) Uani 1 1 d . . . C26 C 0.5912(4) 0.2338(3) -0.0818(2) 0.0250(10) Uani 1 1 d . . . C27 C 0.5913(4) 0.3050(3) -0.0578(2) 0.0327(12) Uani 1 1 d . . . H27A H 0.5597 0.3441 -0.0844 0.039 Uiso 1 1 calc R . . C28 C 0.6372(4) 0.3186(3) 0.0047(2) 0.0313(11) Uani 1 1 d . . . H28A H 0.6361 0.3672 0.0207 0.038 Uiso 1 1 calc R . . C29 C 0.6773(4) 0.1964(3) 0.0218(2) 0.0282(10) Uani 1 1 d . . . H29A H 0.7050 0.1579 0.0502 0.034 Uiso 1 1 calc R . . C30 C 0.6320(4) 0.1781(3) -0.0405(2) 0.0278(10) Uani 1 1 d . . . H30A H 0.6293 0.1284 -0.0543 0.033 Uiso 1 1 calc R . . C31 C 0.5477(3) 0.2198(2) -0.1516(2) 0.0228(9) Uani 1 1 d . . . O13 O 1.2338(3) 0.26439(19) 0.11187(18) 0.0363(8) Uani 1 1 d U . . C32 C 1.3345(13) 0.2644(8) 0.1354(7) 0.152(5) Uiso 1 1 d U . . C33 C 1.4081(16) 0.2647(11) 0.0855(10) 0.209(8) Uiso 1 1 d U . . 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 0.0201(3) 0.0149(3) 0.0145(3) 0.0008(2) 0.0003(2) -0.0001(2) C1 0.025(2) 0.019(2) 0.023(2) 0.0003(17) -0.0002(18) -0.0030(18) N1 0.026(2) 0.0164(18) 0.0236(19) -0.0017(15) -0.0012(16) -0.0026(15) O11 0.0271(17) 0.0228(16) 0.0246(16) -0.0037(13) 0.0049(14) -0.0061(13) Co3 0.0222(3) 0.0174(3) 0.0149(3) 0.0030(2) -0.0015(2) -0.0025(2) C2 0.028(3) 0.023(2) 0.029(2) -0.0097(19) 0.004(2) -0.0039(19) N2 0.074(4) 0.049(3) 0.082(4) -0.029(3) 0.022(3) -0.012(3) O12 0.0251(17) 0.0200(15) 0.0256(16) -0.0037(13) 0.0039(13) -0.0027(13) Co2 0.0201(3) 0.0149(3) 0.0168(3) -0.0010(2) 0.0008(2) 0.0003(2) C3 0.026(2) 0.028(2) 0.032(3) -0.003(2) 0.008(2) -0.004(2) N3 0.0221(19) 0.0178(18) 0.0226(18) 0.0042(15) 0.0020(15) -0.0031(15) O5 0.0244(16) 0.0232(16) 0.0157(14) -0.0003(12) 0.0017(12) 0.0003(13) Co4 0.0237(3) 0.0161(3) 0.0177(3) 0.0019(2) 0.0028(2) -0.0006(2) C4 0.036(3) 0.026(2) 0.022(2) -0.0061(18) 0.008(2) -0.009(2) N4 0.026(2) 0.0199(19) 0.027(2) 0.0042(15) 0.0076(16) 0.0025(16) O6 0.0322(18) 0.0275(17) 0.0189(15) 0.0020(13) 0.0052(14) -0.0077(14) C5 0.033(3) 0.032(3) 0.024(2) -0.004(2) 0.008(2) -0.010(2) N5 0.030(2) 0.024(2) 0.0196(18) 0.0039(16) -0.0043(16) 0.0000(17) O7 0.0219(17) 0.0239(16) 0.0291(17) 0.0088(13) -0.0014(14) -0.0050(13) C6 0.022(2) 0.018(2) 0.024(2) 0.0008(17) -0.0007(19) 0.0006(17) O8 0.0271(17) 0.0210(16) 0.0223(15) 0.0074(13) -0.0017(13) -0.0028(13) C7 0.034(3) 0.031(3) 0.028(2) -0.012(2) 0.005(2) -0.004(2) O3 0.0229(16) 0.0195(15) 0.0191(15) 0.0023(12) -0.0003(13) 0.0020(12) C8 0.048(3) 0.026(3) 0.052(3) -0.008(2) 0.012(3) -0.006(2) O4 0.0262(18) 0.0291(17) 0.0278(17) 0.0117(14) -0.0031(14) -0.0068(14) C9 0.072(5) 0.036(3) 0.073(5) -0.015(3) 0.025(4) -0.009(3) O9 0.0328(18) 0.0229(16) 0.0146(14) 0.0011(12) -0.0040(13) 0.0007(13) C10 0.081(5) 0.062(4) 0.041(3) -0.026(3) 0.014(3) -0.001(4) O10 0.0300(18) 0.0247(17) 0.0167(14) 0.0005(12) -0.0008(13) -0.0019(13) C11 0.053(4) 0.053(4) 0.036(3) -0.017(3) 0.012(3) -0.010(3) O1 0.0220(16) 0.0170(14) 0.0159(14) -0.0018(11) 0.0025(12) 0.0008(12) C12 0.028(2) 0.022(2) 0.017(2) -0.0021(17) -0.0013(19) 0.0019(19) O2 0.0202(15) 0.0157(14) 0.0171(14) 0.0013(11) -0.0003(12) 0.0000(12) C13 0.025(2) 0.021(2) 0.021(2) 0.0022(17) 0.0020(18) -0.0029(18) C14 0.030(3) 0.040(3) 0.098(5) 0.042(3) -0.006(3) -0.007(3) O14 0.0262(18) 0.0293(18) 0.0365(19) 0.0015(15) 0.0035(15) 0.0038(14) C15 0.025(3) 0.045(3) 0.099(5) 0.042(4) -0.005(3) -0.002(3) C16 0.030(3) 0.038(3) 0.102(5) 0.043(3) -0.008(3) -0.007(3) C17 0.025(3) 0.050(4) 0.114(6) 0.047(4) -0.012(3) -0.010(3) C18 0.027(2) 0.020(2) 0.0147(19) 0.0008(16) 0.0032(18) 0.0012(18) C19 0.025(2) 0.021(2) 0.024(2) 0.0037(18) 0.0087(19) 0.0028(18) C20 0.023(2) 0.040(3) 0.033(3) 0.016(2) -0.001(2) -0.006(2) C21 0.023(3) 0.042(3) 0.036(3) 0.016(2) 0.001(2) -0.001(2) C22 0.032(3) 0.018(2) 0.025(2) 0.0019(18) 0.007(2) 0.0012(19) C24 0.031(3) 0.020(2) 0.020(2) 0.0031(17) 0.0031(19) 0.0024(19) C25 0.025(2) 0.020(2) 0.016(2) 0.0016(17) 0.0050(18) 0.0023(18) C26 0.029(2) 0.026(2) 0.017(2) 0.0004(18) -0.0024(18) -0.0025(19) C27 0.043(3) 0.025(2) 0.024(2) 0.0054(19) -0.007(2) -0.001(2) C28 0.040(3) 0.024(2) 0.025(2) 0.0020(19) -0.004(2) -0.003(2) C29 0.033(3) 0.025(2) 0.024(2) 0.0055(19) -0.001(2) -0.003(2) C30 0.035(3) 0.026(2) 0.020(2) 0.0020(18) 0.000(2) -0.002(2) C31 0.021(2) 0.029(2) 0.017(2) -0.0012(18) 0.0006(18) -0.0033(19) O13 0.0258(18) 0.0285(18) 0.056(2) -0.0003(17) 0.0107(17) 0.0052(15) _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 O7 2.045(3) . ? Co1 O2 2.057(3) . ? Co1 O9 2.063(3) 4_666 ? Co1 O1 2.104(3) . ? Co1 N1 2.143(4) 2_745 ? Co1 O5 2.147(3) . ? Co1 Co2 2.9728(8) . ? C1 C2 1.375(7) . ? C1 C5 1.393(6) . ? C1 C6 1.512(6) . ? N1 C4 1.338(6) . ? N1 C3 1.341(6) . ? N1 Co1 2.143(4) 2_755 ? O11 C6 1.256(6) . ? O11 Co2 2.044(3) . ? Co3 O1 2.026(3) . ? Co3 O8 2.052(3) . ? Co3 O4 2.074(3) . ? Co3 O14 2.117(3) . ? Co3 N5 2.119(4) . ? Co3 O5 2.220(3) . ? C2 C3 1.385(6) . ? C2 H2A 0.9500 . ? N2 C9 1.333(9) . ? N2 C10 1.342(9) . ? O12 C6 1.255(5) . ? O12 Co4 2.106(3) . ? Co2 O1 2.055(3) . ? Co2 O10 2.095(3) 4_666 ? Co2 N3 2.112(4) 2_655 ? Co2 O2 2.120(3) . ? Co2 O3 2.204(3) . ? C3 H3A 0.9500 . ? N3 C16 1.313(7) . ? N3 C15 1.319(6) . ? N3 Co2 2.112(4) 2_645 ? O5 C12 1.271(5) . ? Co4 O2 2.045(3) . ? Co4 O13 2.089(3) . ? Co4 O6 2.112(3) . ? Co4 N4 2.166(4) 3_765 ? Co4 O3 2.214(3) . ? C4 C5 1.374(6) . ? C4 H4A 0.9500 . ? N4 C21 1.328(6) . ? N4 C22 1.343(6) . ? N4 Co4 2.166(4) 3_765 ? O6 C12 1.247(5) . ? C5 H5A 0.9500 . ? N5 C29 1.326(6) . ? N5 C28 1.349(6) . ? O7 C18 1.250(5) . ? N6 O16 1.192(10) . ? N6 O17 1.193(10) . ? N6 O15 1.202(10) . ? O8 C18 1.259(5) . ? C7 C11 1.382(7) . ? C7 C8 1.408(7) . ? C7 C12 1.512(6) . ? O3 C25 1.267(5) . ? C8 C9 1.386(8) . ? C8 H8A 0.9500 . ? O4 C25 1.232(5) . ? C9 H9A 0.9500 . ? O9 C31 1.253(5) . ? O9 Co1 2.063(3) 4_565 ? C10 C11 1.395(8) . ? C10 H10A 0.9500 . ? O10 C31 1.258(5) . ? O10 Co2 2.095(3) 4_565 ? C11 H11A 0.9500 . ? O1 H1A 1.0000 . ? O2 H2B 1.0000 . ? C13 C14 1.355(7) . ? C13 C17 1.356(7) . ? C13 C18 1.500(6) . ? C14 C15 1.386(8) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.366(8) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C19 C24 1.383(6) . ? C19 C20 1.391(6) . ? C19 C25 1.517(6) . ? C20 C21 1.378(7) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C24 1.389(6) . ? C22 H22A 0.9500 . ? C24 H24A 0.9500 . ? C26 C30 1.379(6) . ? C26 C27 1.394(7) . ? C26 C31 1.512(6) . ? C27 C28 1.375(7) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.389(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? O13 C32 1.309(16) . ? C32 C33 1.59(2) . ? 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 Co1 O2 175.77(12) . . ? O7 Co1 O9 89.08(13) . 4_666 ? O2 Co1 O9 94.19(12) . 4_666 ? O7 Co1 O1 91.78(12) . . ? O2 Co1 O1 85.51(11) . . ? O9 Co1 O1 90.43(12) 4_666 . ? O7 Co1 N1 86.48(14) . 2_745 ? O2 Co1 N1 96.41(13) . 2_745 ? O9 Co1 N1 86.16(13) 4_666 2_745 ? O1 Co1 N1 176.19(13) . 2_745 ? O7 Co1 O5 88.57(12) . . ? O2 Co1 O5 87.79(11) . . ? O9 Co1 O5 171.15(12) 4_666 . ? O1 Co1 O5 81.12(11) . . ? N1 Co1 O5 102.20(13) 2_745 . ? O7 Co1 Co2 132.96(10) . . ? O2 Co1 Co2 45.49(8) . . ? O9 Co1 Co2 78.98(9) 4_666 . ? O1 Co1 Co2 43.71(8) . . ? N1 Co1 Co2 136.80(10) 2_745 . ? O5 Co1 Co2 96.46(8) . . ? C2 C1 C5 117.4(4) . . ? C2 C1 C6 121.8(4) . . ? C5 C1 C6 120.8(4) . . ? C4 N1 C3 117.3(4) . . ? C4 N1 Co1 125.4(3) . 2_755 ? C3 N1 Co1 116.6(3) . 2_755 ? C6 O11 Co2 128.2(3) . . ? O1 Co3 O8 94.24(12) . . ? O1 Co3 O4 92.60(12) . . ? O8 Co3 O4 171.93(13) . . ? O1 Co3 O14 96.14(12) . . ? O8 Co3 O14 86.61(13) . . ? O4 Co3 O14 88.39(13) . . ? O1 Co3 N5 171.83(14) . . ? O8 Co3 N5 87.21(13) . . ? O4 Co3 N5 86.63(14) . . ? O14 Co3 N5 91.97(14) . . ? O1 Co3 O5 81.10(11) . . ? O8 Co3 O5 88.60(12) . . ? O4 Co3 O5 96.70(12) . . ? O14 Co3 O5 174.29(12) . . ? N5 Co3 O5 90.91(13) . . ? C1 C2 C3 120.1(4) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C9 N2 C10 116.7(6) . . ? C6 O12 Co4 129.6(3) . . ? O11 Co2 O1 177.45(12) . . ? O11 Co2 O10 86.93(12) . 4_666 ? O1 Co2 O10 91.87(12) . 4_666 ? O11 Co2 N3 89.31(13) . 2_655 ? O1 Co2 N3 92.96(13) . 2_655 ? O10 Co2 N3 91.11(13) 4_666 2_655 ? O11 Co2 O2 92.72(12) . . ? O1 Co2 O2 85.15(11) . . ? O10 Co2 O2 95.42(11) 4_666 . ? N3 Co2 O2 173.25(12) 2_655 . ? O11 Co2 O3 88.38(12) . . ? O1 Co2 O3 92.70(11) . . ? O10 Co2 O3 174.51(12) 4_666 . ? N3 Co2 O3 91.69(13) 2_655 . ? O2 Co2 O3 81.94(11) . . ? O11 Co2 Co1 132.49(9) . . ? O1 Co2 Co1 45.03(8) . . ? O10 Co2 Co1 80.95(9) 4_666 . ? N3 Co2 Co1 136.33(10) 2_655 . ? O2 Co2 Co1 43.79(8) . . ? O3 Co2 Co1 100.20(8) . . ? N1 C3 C2 122.4(4) . . ? N1 C3 H3A 118.8 . . ? C2 C3 H3A 118.8 . . ? C16 N3 C15 115.9(4) . . ? C16 N3 Co2 120.4(3) . 2_645 ? C15 N3 Co2 123.7(3) . 2_645 ? C12 O5 Co1 127.0(3) . . ? C12 O5 Co3 133.2(3) . . ? Co1 O5 Co3 91.66(11) . . ? O2 Co4 O13 94.24(13) . . ? O2 Co4 O12 89.52(12) . . ? O13 Co4 O12 87.75(13) . . ? O2 Co4 O6 94.90(11) . . ? O13 Co4 O6 86.51(14) . . ? O12 Co4 O6 173.00(12) . . ? O2 Co4 N4 171.40(13) . 3_765 ? O13 Co4 N4 94.22(14) . 3_765 ? O12 Co4 N4 89.28(13) . 3_765 ? O6 Co4 N4 87.15(13) . 3_765 ? O2 Co4 O3 83.40(11) . . ? O13 Co4 O3 174.55(13) . . ? O12 Co4 O3 87.32(11) . . ? O6 Co4 O3 98.57(12) . . ? N4 Co4 O3 88.03(12) 3_765 . ? N1 C4 C5 123.4(4) . . ? N1 C4 H4A 118.3 . . ? C5 C4 H4A 118.3 . . ? C21 N4 C22 117.4(4) . . ? C21 N4 Co4 118.2(3) . 3_765 ? C22 N4 Co4 122.7(3) . 3_765 ? C12 O6 Co4 127.1(3) . . ? C4 C5 C1 119.3(4) . . ? C4 C5 H5A 120.4 . . ? C1 C5 H5A 120.4 . . ? C29 N5 C28 117.9(4) . . ? C29 N5 Co3 122.1(3) . . ? C28 N5 Co3 119.8(3) . . ? C18 O7 Co1 130.2(3) . . ? O12 C6 O11 126.8(4) . . ? O12 C6 C1 117.4(4) . . ? O11 C6 C1 115.7(4) . . ? O16 N6 O17 121.4(18) . . ? O16 N6 O15 120.2(17) . . ? O17 N6 O15 116.5(17) . . ? C18 O8 Co3 127.6(3) . . ? C11 C7 C8 118.4(5) . . ? C11 C7 C12 122.6(5) . . ? C8 C7 C12 119.0(4) . . ? C25 O3 Co2 125.1(3) . . ? C25 O3 Co4 127.6(3) . . ? Co2 O3 Co4 90.88(10) . . ? C9 C8 C7 119.2(6) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C25 O4 Co3 136.6(3) . . ? N2 C9 C8 123.2(6) . . ? N2 C9 H9A 118.4 . . ? C8 C9 H9A 118.4 . . ? C31 O9 Co1 128.5(3) . 4_565 ? N2 C10 C11 125.0(6) . . ? N2 C10 H10A 117.5 . . ? C11 C10 H10A 117.5 . . ? C31 O10 Co2 124.1(3) . 4_565 ? C7 C11 C10 117.4(6) . . ? C7 C11 H11A 121.3 . . ? C10 C11 H11A 121.3 . . ? Co3 O1 Co2 130.01(15) . . ? Co3 O1 Co1 98.63(12) . . ? Co2 O1 Co1 91.26(12) . . ? Co3 O1 H1A 110.8 . . ? Co2 O1 H1A 110.8 . . ? Co1 O1 H1A 110.8 . . ? O6 C12 O5 126.2(4) . . ? O6 C12 C7 119.5(4) . . ? O5 C12 C7 114.3(4) . . ? Co4 O2 Co1 131.84(14) . . ? Co4 O2 Co2 98.17(11) . . ? Co1 O2 Co2 90.72(12) . . ? Co4 O2 H2B 110.4 . . ? Co1 O2 H2B 110.4 . . ? Co2 O2 H2B 110.4 . . ? C14 C13 C17 117.0(5) . . ? C14 C13 C18 122.9(4) . . ? C17 C13 C18 120.1(4) . . ? C13 C14 C15 120.0(5) . . ? C13 C14 H14A 120.0 . . ? C15 C14 H14A 120.0 . . ? N3 C15 C14 123.0(5) . . ? N3 C15 H15A 118.5 . . ? C14 C15 H15A 118.5 . . ? N3 C16 C17 124.5(5) . . ? N3 C16 H16A 117.7 . . ? C17 C16 H16A 117.7 . . ? C13 C17 C16 119.6(5) . . ? C13 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? O7 C18 O8 127.0(4) . . ? O7 C18 C13 116.5(4) . . ? O8 C18 C13 116.5(4) . . ? C24 C19 C20 117.6(4) . . ? C24 C19 C25 122.8(4) . . ? C20 C19 C25 119.5(4) . . ? C21 C20 C19 118.9(5) . . ? C21 C20 H20A 120.5 . . ? C19 C20 H20A 120.5 . . ? N4 C21 C20 123.8(5) . . ? N4 C21 H21A 118.1 . . ? C20 C21 H21A 118.1 . . ? N4 C22 C24 122.4(4) . . ? N4 C22 H22A 118.8 . . ? C24 C22 H22A 118.8 . . ? C19 C24 C22 119.5(4) . . ? C19 C24 H24A 120.3 . . ? C22 C24 H24A 120.3 . . ? O4 C25 O3 126.7(4) . . ? O4 C25 C19 116.1(4) . . ? O3 C25 C19 117.2(4) . . ? C30 C26 C27 118.1(4) . . ? C30 C26 C31 122.1(4) . . ? C27 C26 C31 119.8(4) . . ? C28 C27 C26 119.7(4) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? N5 C28 C27 121.9(4) . . ? N5 C28 H28A 119.0 . . ? C27 C28 H28A 119.0 . . ? N5 C29 C30 123.5(4) . . ? N5 C29 H29A 118.3 . . ? C30 C29 H29A 118.3 . . ? C26 C30 C29 118.5(4) . . ? C26 C30 H30A 120.7 . . ? C29 C30 H30A 120.7 . . ? O9 C31 O10 127.2(4) . . ? O9 C31 C26 115.7(4) . . ? O10 C31 C26 117.0(4) . . ? C32 O13 Co4 135.2(7) . . ? O13 C32 C33 116.4(13) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.152 _refine_diff_density_min -0.936 _refine_diff_density_rms 0.125 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.026 0.500 775 146 ' ' 2 0.500 0.308 1.000 775 147 ' ' _platon_squeeze_details ; The contribution of any disordered solvent removed by the SQUEEZE process have be included in the overall formula, formula weight, density, F(000), etc. ; data_2 _database_code_depnum_ccdc_archive 'CCDC 850282' #TrackingRef '- M4_120104.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H55 N5 Ni4 O20' _chemical_formula_weight 1172.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0989(7) _cell_length_b 18.4444(9) _cell_length_c 22.0504(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.2020(10) _cell_angle_gamma 90.00 _cell_volume 5186.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2 _cell_measurement_theta_max 26 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 1.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7267 _exptl_absorpt_correction_T_max 0.8082 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 ? _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 26635 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10175 _reflns_number_gt 7654 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0657P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10175 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Ni3 Ni 0.28413(4) 0.21726(2) 0.12489(2) 0.02069(13) Uani 1 1 d . . . Ni4 Ni 0.61261(4) 0.14078(3) 0.12878(2) 0.02189(13) Uani 1 1 d . . . Ni1 Ni 0.48533(4) 0.26846(2) 0.21574(2) 0.01720(12) Uani 1 1 d . . . Ni2 Ni 0.48916(4) 0.11058(2) 0.23287(2) 0.01743(12) Uani 1 1 d . . . N1 N 0.3904(2) 0.03222(16) 0.25551(14) 0.0230(7) Uani 1 1 d . . . N2 N 0.5961(2) 0.35211(16) 0.22309(14) 0.0234(7) Uani 1 1 d . . . N3 N 0.3730(3) -0.08567(17) -0.04635(14) 0.0251(7) Uani 1 1 d . . . N4 N 0.2075(3) 0.24840(17) 0.03323(14) 0.0257(7) Uani 1 1 d . A . O2 O 0.5854(2) 0.18647(13) 0.20696(13) 0.0201(6) Uani 1 1 d . . . O1 O 0.3754(2) 0.18823(15) 0.20905(14) 0.0194(6) Uani 1 1 d . . . O9 O 0.1211(2) -0.15420(13) 0.27180(12) 0.0240(6) Uani 1 1 d . . . O10 O 0.2606(2) -0.18525(13) 0.34677(11) 0.0257(6) Uani 1 1 d . . . O11 O 0.8151(2) 0.55442(14) 0.32421(12) 0.0284(6) Uani 1 1 d . . . O12 O 0.8922(2) 0.53304(14) 0.24525(12) 0.0267(6) Uani 1 1 d . . . O7 O 0.0316(2) 0.23855(13) -0.18950(11) 0.0253(6) Uani 1 1 d . . . O8 O 0.0318(2) 0.35881(14) -0.17391(11) 0.0262(6) Uani 1 1 d . . . O3 O 0.46850(19) 0.07986(13) 0.13701(11) 0.0233(6) Uani 1 1 d . . . O4 O 0.3080(2) 0.11845(14) 0.08716(12) 0.0314(7) Uani 1 1 d . . . O6 O 0.5448(3) 0.22162(15) 0.07138(13) 0.0405(8) Uani 1 1 d . . . O5 O 0.4275(2) 0.27056(14) 0.11809(11) 0.0251(6) Uani 1 1 d . B . C1 C 0.4286(3) -0.0109(2) 0.30380(19) 0.0358(11) Uani 1 1 d . . . H1A H 0.4970 -0.0012 0.3280 0.043 Uiso 1 1 calc R . . C2 C 0.3750(3) -0.0686(2) 0.32053(19) 0.0361(11) Uani 1 1 d . . . H2A H 0.4066 -0.0984 0.3548 0.043 Uiso 1 1 calc R . . C3 C 0.2743(3) -0.0828(2) 0.28676(17) 0.0252(9) Uani 1 1 d . . . C4 C 0.2331(3) -0.0358(2) 0.23805(19) 0.0343(10) Uani 1 1 d . . . H4A H 0.1631 -0.0421 0.2147 0.041 Uiso 1 1 calc R . . C5 C 0.2934(3) 0.0199(2) 0.2236(2) 0.0329(10) Uani 1 1 d . . . H5A H 0.2643 0.0506 0.1894 0.039 Uiso 1 1 calc R . . C6 C 0.2130(3) -0.1461(2) 0.30290(17) 0.0232(8) Uani 1 1 d . . . C7 C 0.6801(3) 0.3554(2) 0.19834(19) 0.0312(10) Uani 1 1 d . . . H7A H 0.6886 0.3187 0.1696 0.037 Uiso 1 1 calc R . . C8 C 0.7554(3) 0.4091(2) 0.21217(19) 0.0344(10) Uani 1 1 d . . . H8A H 0.8130 0.4097 0.1927 0.041 Uiso 1 1 calc R . . C9 C 0.7454(3) 0.4623(2) 0.25512(17) 0.0254(9) Uani 1 1 d . . . C10 C 0.6577(4) 0.4599(2) 0.2797(2) 0.0374(11) Uani 1 1 d . . . H10A H 0.6472 0.4964 0.3082 0.045 Uiso 1 1 calc R . . C11 C 0.5854(3) 0.4052(2) 0.2635(2) 0.0344(10) Uani 1 1 d . . . H11A H 0.5257 0.4047 0.2812 0.041 Uiso 1 1 calc R . . C12 C 0.8258(3) 0.5218(2) 0.27620(18) 0.0236(8) Uani 1 1 d . . . C13 C 0.4445(3) -0.0887(2) 0.00744(17) 0.0253(9) Uani 1 1 d . . . H13A H 0.4953 -0.1264 0.0128 0.030 Uiso 1 1 calc R . . C14 C 0.4491(3) -0.0399(2) 0.05616(18) 0.0270(9) Uani 1 1 d . . . H14A H 0.5013 -0.0443 0.0937 0.032 Uiso 1 1 calc R . . C15 C 0.3751(3) 0.0157(2) 0.04847(16) 0.0219(8) Uani 1 1 d . . . C16 C 0.2953(3) 0.0153(2) -0.00437(17) 0.0296(9) Uani 1 1 d . . . H16A H 0.2396 0.0494 -0.0093 0.036 Uiso 1 1 calc R . . C17 C 0.2974(3) -0.0355(2) -0.05020(18) 0.0310(10) Uani 1 1 d . . . H17A H 0.2422 -0.0348 -0.0866 0.037 Uiso 1 1 calc R . . C18 C 0.3839(3) 0.0760(2) 0.09486(16) 0.0238(8) Uani 1 1 d . . . C19 C 0.1340(7) 0.2994(4) 0.0208(3) 0.039(2) Uani 0.671(8) 1 d P A 1 H19A H 0.1138 0.3233 0.0544 0.047 Uiso 0.671(8) 1 calc PR A 1 C20 C 0.0858(7) 0.3188(4) -0.0399(3) 0.038(2) Uani 0.671(8) 1 d P A 1 H20A H 0.0394 0.3591 -0.0469 0.046 Uiso 0.671(8) 1 calc PR A 1 C22 C 0.1838(6) 0.2289(3) -0.0766(3) 0.040(2) Uani 0.671(8) 1 d P A 1 H22A H 0.2028 0.2031 -0.1096 0.047 Uiso 0.671(8) 1 calc PR A 1 C23 C 0.2353(6) 0.2149(3) -0.0156(3) 0.0326(18) Uani 0.671(8) 1 d P A 1 H23A H 0.2914 0.1811 -0.0076 0.039 Uiso 0.671(8) 1 calc PR A 1 C19A C 0.1988(15) 0.3161(7) 0.0104(6) 0.035(4) Uani 0.329(8) 1 d P A 2 H19B H 0.2272 0.3544 0.0378 0.042 Uiso 0.329(8) 1 calc PR A 2 C20A C 0.1512(13) 0.3337(7) -0.0505(6) 0.031(3) Uani 0.329(8) 1 d P A 2 H20B H 0.1517 0.3823 -0.0646 0.037 Uiso 0.329(8) 1 calc PR A 2 C22A C 0.0978(12) 0.2134(7) -0.0649(6) 0.036(4) Uani 0.329(8) 1 d P A 2 H22B H 0.0595 0.1763 -0.0901 0.043 Uiso 0.329(8) 1 calc PR A 2 C23A C 0.1469(12) 0.1985(7) -0.0038(5) 0.035(4) Uani 0.329(8) 1 d P A 2 H23B H 0.1380 0.1520 0.0129 0.042 Uiso 0.329(8) 1 calc PR A 2 C21 C 0.1038(3) 0.2811(2) -0.08971(17) 0.0264(9) Uani 1 1 d . . . C24 C 0.0506(3) 0.2946(2) -0.15691(17) 0.0226(8) Uani 1 1 d . A . C31 C 0.4824(3) 0.2702(2) 0.07751(18) 0.0273(9) Uani 1 1 d . B . C32 C 0.4685(5) 0.3336(3) 0.0321(3) 0.0614(16) Uani 1 1 d . . . C33 C 0.4266(9) 0.4006(6) 0.0551(5) 0.099(3) Uiso 0.70 1 d P B 1 C33A C 0.568(2) 0.3561(15) 0.0197(13) 0.105(8) Uiso 0.30 1 d P B 2 N5 N 0.145(2) 0.1824(13) 0.1452(9) 0.0318(18) Uani 0.508(6) 1 d P . 1 C25 C 0.1180(12) 0.2005(7) 0.1991(7) 0.0318(18) Uani 0.508(6) 1 d P . 1 H25A H 0.1743 0.2156 0.2319 0.038 Uiso 0.508(6) 1 calc PR . 1 C26 C 0.0180(8) 0.2001(6) 0.2134(5) 0.046(3) Uani 0.508(6) 1 d P . 1 H26A H 0.0100 0.2120 0.2540 0.055 Uiso 0.508(6) 1 calc PR . 1 C27 C -0.0662(9) 0.1822(5) 0.1672(4) 0.027(2) Uani 0.508(6) 1 d P . 1 C28 C -0.0470(8) 0.1621(7) 0.1108(5) 0.037(3) Uani 0.508(6) 1 d P . 1 H28A H -0.1038 0.1495 0.0774 0.045 Uiso 0.508(6) 1 calc PR . 1 C29 C 0.0556(6) 0.1603(5) 0.1022(4) 0.0318(18) Uani 0.508(6) 1 d P . 1 H29A H 0.0651 0.1422 0.0635 0.038 Uiso 0.508(6) 1 calc PR . 1 C30 C -0.1770(9) 0.1878(5) 0.1772(6) 0.0288(18) Uani 0.508(6) 1 d P . 1 O13 O -0.1887(4) 0.1922(4) 0.2307(3) 0.0375(18) Uani 0.508(6) 1 d P . 1 O14 O -0.2483(7) 0.1863(5) 0.1288(4) 0.0288(18) Uani 0.508(6) 1 d P . 1 N5A N -0.2256(11) 0.1781(8) 0.1459(6) 0.0340(16) Uani 0.492(6) 1 d P . 2 C25A C -0.1776(7) 0.2000(5) 0.1014(4) 0.0340(16) Uani 0.492(6) 1 d P . 2 H25B H -0.2192 0.2139 0.0626 0.041 Uiso 0.492(6) 1 d PR . 2 C26A C -0.0714(9) 0.2040(6) 0.1096(5) 0.037(3) Uani 0.492(6) 1 d P . 2 H26B H -0.0411 0.2176 0.0761 0.044 Uiso 0.492(6) 1 calc PR . 2 C27A C -0.0064(10) 0.1876(5) 0.1692(5) 0.030(2) Uani 0.492(6) 1 d P . 2 C28A C -0.0559(7) 0.1696(5) 0.2155(5) 0.035(2) Uani 0.492(6) 1 d P . 2 H28B H -0.0163 0.1599 0.2564 0.042 Uiso 0.492(6) 1 calc PR . 2 C29A C -0.1642(8) 0.1656(6) 0.2018(6) 0.0340(16) Uani 0.492(6) 1 d P . 2 H29B H -0.1963 0.1540 0.2346 0.041 Uiso 0.492(6) 1 d PR . 2 C30A C 0.1149(9) 0.1841(6) 0.1751(7) 0.035(4) Uani 0.492(6) 1 d P . 2 O14' O 0.1647(5) 0.1938(4) 0.2324(3) 0.045(2) Uani 0.492(6) 1 d P . 2 O13' O 0.1436(15) 0.1772(10) 0.1302(5) 0.035(3) Uani 0.492(6) 1 d P . 2 H2Z H 0.636(5) 0.191(3) 0.234(3) 0.07(2) Uiso 1 1 d . . . H1Z H 0.349(4) 0.190(2) 0.229(2) 0.026(16) 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 Ni3 0.0186(3) 0.0191(3) 0.0215(3) -0.00371(19) -0.0013(2) 0.0036(2) Ni4 0.0240(3) 0.0173(3) 0.0265(3) -0.0006(2) 0.0102(2) 0.0026(2) Ni1 0.0164(3) 0.0144(2) 0.0198(2) -0.00166(18) 0.00212(19) -0.00050(18) Ni2 0.0175(3) 0.0144(2) 0.0196(2) 0.00047(18) 0.00258(19) -0.00048(18) N1 0.0236(18) 0.0158(16) 0.0281(17) 0.0032(13) 0.0025(14) -0.0021(13) N2 0.0219(18) 0.0184(17) 0.0298(18) -0.0028(13) 0.0057(14) -0.0046(13) N3 0.0247(18) 0.0221(18) 0.0287(18) -0.0046(14) 0.0065(14) 0.0016(14) N4 0.029(2) 0.0240(18) 0.0204(17) -0.0024(13) -0.0022(14) 0.0023(15) O2 0.0185(15) 0.0157(14) 0.0265(15) -0.0020(11) 0.0060(12) 0.0006(11) O1 0.0161(15) 0.0209(15) 0.0219(15) -0.0025(11) 0.0058(13) -0.0015(11) O9 0.0189(15) 0.0207(14) 0.0302(14) 0.0082(11) 0.0009(12) -0.0021(11) O10 0.0269(16) 0.0236(14) 0.0241(14) 0.0094(11) 0.0003(12) -0.0087(12) O11 0.0306(16) 0.0259(15) 0.0294(15) -0.0054(12) 0.0085(12) -0.0116(12) O12 0.0267(16) 0.0216(14) 0.0317(15) -0.0030(11) 0.0062(12) -0.0059(12) O7 0.0339(17) 0.0207(14) 0.0175(13) -0.0004(11) -0.0020(11) -0.0004(12) O8 0.0366(17) 0.0219(15) 0.0178(13) 0.0011(11) 0.0013(12) 0.0023(12) O3 0.0179(14) 0.0262(15) 0.0233(14) -0.0030(11) -0.0003(11) 0.0001(11) O4 0.0320(17) 0.0271(16) 0.0268(15) -0.0106(12) -0.0106(12) 0.0133(13) O6 0.063(2) 0.0289(17) 0.0373(17) 0.0105(13) 0.0266(16) 0.0202(15) O5 0.0247(15) 0.0301(15) 0.0201(13) -0.0007(11) 0.0038(11) 0.0013(12) C1 0.028(2) 0.035(2) 0.040(3) 0.013(2) -0.0014(19) -0.011(2) C2 0.032(3) 0.038(3) 0.033(2) 0.0167(19) -0.0031(19) -0.006(2) C3 0.026(2) 0.022(2) 0.027(2) 0.0033(16) 0.0055(17) -0.0040(17) C4 0.023(2) 0.035(2) 0.040(2) 0.0133(19) -0.0032(19) -0.0071(19) C5 0.028(2) 0.031(2) 0.038(2) 0.0129(19) 0.0041(19) 0.0010(19) C6 0.027(2) 0.023(2) 0.0212(19) 0.0041(16) 0.0082(17) 0.0009(17) C7 0.028(2) 0.034(2) 0.032(2) -0.0108(18) 0.0079(18) -0.0071(19) C8 0.036(3) 0.035(2) 0.035(2) -0.0063(19) 0.014(2) -0.010(2) C9 0.023(2) 0.023(2) 0.027(2) -0.0010(16) 0.0004(17) -0.0069(17) C10 0.042(3) 0.024(2) 0.048(3) -0.019(2) 0.015(2) -0.010(2) C11 0.026(2) 0.028(2) 0.053(3) -0.015(2) 0.017(2) -0.0091(18) C12 0.022(2) 0.018(2) 0.028(2) 0.0036(16) 0.0007(17) -0.0043(16) C13 0.027(2) 0.021(2) 0.028(2) -0.0011(16) 0.0080(17) 0.0040(17) C14 0.029(2) 0.026(2) 0.025(2) -0.0009(16) 0.0037(17) 0.0031(17) C15 0.022(2) 0.022(2) 0.0213(19) -0.0034(15) 0.0031(16) 0.0005(16) C16 0.028(2) 0.032(2) 0.027(2) -0.0060(17) 0.0015(18) 0.0088(18) C17 0.027(2) 0.034(2) 0.029(2) -0.0129(18) -0.0002(18) 0.0018(19) C18 0.032(2) 0.022(2) 0.0175(19) -0.0019(15) 0.0060(17) -0.0023(17) C19 0.042(5) 0.046(5) 0.023(4) -0.004(3) -0.006(3) 0.019(4) C20 0.043(5) 0.040(4) 0.027(4) -0.002(3) -0.002(3) 0.027(4) C22 0.058(6) 0.033(4) 0.021(3) -0.005(3) -0.005(3) 0.015(3) C23 0.037(4) 0.027(4) 0.029(3) 0.001(3) -0.002(3) 0.017(3) C19A 0.063(12) 0.016(7) 0.016(7) -0.004(5) -0.009(7) 0.018(7) C20A 0.037(9) 0.033(8) 0.024(7) 0.001(5) 0.012(6) 0.015(7) C22A 0.039(9) 0.034(8) 0.030(7) -0.012(6) -0.004(6) -0.002(6) C23A 0.055(11) 0.021(7) 0.020(6) 0.000(5) -0.009(6) 0.006(6) C21 0.035(2) 0.018(2) 0.023(2) 0.0012(16) 0.0011(17) 0.0022(17) C24 0.019(2) 0.025(2) 0.0217(19) 0.0015(16) 0.0024(16) 0.0014(16) C31 0.038(3) 0.021(2) 0.023(2) 0.0040(16) 0.0070(18) 0.0037(18) C32 0.086(5) 0.044(3) 0.065(4) 0.036(3) 0.038(3) 0.025(3) N5 0.024(4) 0.045(4) 0.028(4) -0.009(3) 0.009(3) -0.011(3) C25 0.024(4) 0.045(4) 0.028(4) -0.009(3) 0.009(3) -0.011(3) C26 0.031(6) 0.086(8) 0.022(5) -0.012(5) 0.010(4) 0.002(5) C27 0.018(5) 0.035(5) 0.027(6) -0.006(4) 0.005(4) -0.003(4) C28 0.014(5) 0.059(8) 0.037(5) -0.019(6) 0.002(4) -0.017(5) C29 0.024(4) 0.045(4) 0.028(4) -0.009(3) 0.009(3) -0.011(3) C30 0.026(4) 0.025(3) 0.038(4) 0.001(3) 0.012(3) -0.004(3) O13 0.013(3) 0.070(5) 0.029(3) -0.004(3) 0.005(2) 0.000(3) O14 0.026(4) 0.025(3) 0.038(4) 0.001(3) 0.012(3) -0.004(3) N5A 0.029(4) 0.039(4) 0.037(4) 0.000(3) 0.015(3) -0.002(3) C25A 0.029(4) 0.039(4) 0.037(4) 0.000(3) 0.015(3) -0.002(3) C26A 0.035(6) 0.042(7) 0.037(6) 0.004(5) 0.016(5) -0.004(5) C27A 0.021(6) 0.035(5) 0.037(7) -0.003(4) 0.014(5) 0.000(5) C28A 0.013(5) 0.058(6) 0.032(6) 0.002(4) -0.001(4) -0.002(4) C29A 0.029(4) 0.039(4) 0.037(4) 0.000(3) 0.015(3) -0.002(3) C30A 0.012(5) 0.022(6) 0.060(11) -0.014(6) -0.012(6) -0.001(4) O14' 0.023(4) 0.084(6) 0.027(4) -0.005(3) 0.006(3) -0.006(3) O13' 0.030(5) 0.041(5) 0.027(7) -0.011(5) -0.009(5) -0.002(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 Ni3 O13' 2.01(2) . ? Ni3 O10 2.033(2) 2 ? Ni3 O1 2.036(3) . ? Ni3 O4 2.057(3) . ? Ni3 N5 2.08(2) . ? Ni3 N4 2.120(3) . ? Ni3 O5 2.155(3) . ? Ni4 O14 2.006(9) 1_655 ? Ni4 O11 2.015(3) 2_645 ? Ni4 O2 2.022(3) . ? Ni4 O6 2.025(3) . ? Ni4 N3 2.128(3) 3_655 ? Ni4 N5A 2.178(15) 1_655 ? Ni4 O3 2.240(3) . ? Ni1 O2 2.039(3) . ? Ni1 O7 2.042(2) 4_666 ? Ni1 O1 2.046(3) . ? Ni1 O9 2.057(2) 2 ? Ni1 N2 2.099(3) . ? Ni1 O5 2.113(2) . ? Ni1 Ni2 2.9353(6) . ? Ni2 O1 2.047(3) . ? Ni2 O2 2.050(3) . ? Ni2 N1 2.075(3) . ? Ni2 O8 2.081(2) 4_666 ? Ni2 O12 2.086(3) 2_645 ? Ni2 O3 2.145(2) . ? N1 C5 1.324(5) . ? N1 C1 1.332(5) . ? N2 C7 1.337(5) . ? N2 C11 1.353(5) . ? N3 C13 1.335(5) . ? N3 C17 1.344(5) . ? N3 Ni4 2.128(3) 3_655 ? N4 C19 1.329(8) . ? N4 C19A 1.341(14) . ? N4 C23A 1.359(13) . ? N4 C23 1.360(7) . ? O9 C6 1.250(4) . ? O9 Ni1 2.057(2) 2_545 ? O10 C6 1.253(4) . ? O10 Ni3 2.033(2) 2_545 ? O11 C12 1.253(4) . ? O11 Ni4 2.015(3) 2_655 ? O12 C12 1.239(4) . ? O12 Ni2 2.086(3) 2_655 ? O7 C24 1.251(4) . ? O7 Ni1 2.042(2) 4_565 ? O8 C24 1.250(4) . ? O8 Ni2 2.081(2) 4_565 ? O3 C18 1.276(4) . ? O4 C18 1.246(5) . ? O6 C31 1.240(5) . ? O5 C31 1.270(5) . ? C1 C2 1.370(5) . ? C2 C3 1.384(6) . ? C3 C4 1.390(5) . ? C3 C6 1.506(5) . ? C4 C5 1.377(5) . ? C7 C8 1.382(6) . ? C8 C9 1.391(5) . ? C9 C10 1.378(6) . ? C9 C12 1.519(5) . ? C10 C11 1.374(5) . ? C13 C14 1.393(5) . ? C14 C15 1.394(5) . ? C15 C16 1.376(5) . ? C15 C18 1.497(5) . ? C16 C17 1.383(5) . ? C19 C20 1.389(9) . ? C20 C21 1.366(8) . ? C22 C23 1.384(8) . ? C22 C21 1.403(8) . ? C19A C20A 1.383(17) . ? C20A C21 1.353(15) . ? C22A C21 1.371(14) . ? C22A C23A 1.382(17) . ? C21 C24 1.508(5) . ? C31 C32 1.524(6) . ? C32 C33A 1.45(3) . ? C32 C33 1.489(12) . ? N5 C25 1.35(2) . ? N5 C29 1.39(2) . ? C25 C26 1.416(17) . ? C26 C27 1.360(14) . ? C27 C28 1.375(14) . ? C27 C30 1.520(15) . ? C28 C29 1.400(12) . ? C30 O13 1.225(12) . ? C30 O14 1.247(13) . ? O14 Ni4 2.006(9) 1_455 ? N5A C29A 1.328(13) . ? N5A C25A 1.343(15) . ? N5A Ni4 2.178(15) 1_455 ? C25A C26A 1.362(14) . ? C26A C27A 1.425(16) . ? C27A C28A 1.368(14) . ? C27A C30A 1.566(17) . ? C28A C29A 1.384(13) . ? C30A O13' 1.14(2) . ? C30A O14' 1.295(14) . ? 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 O13' Ni3 O10 88.6(4) . 2 ? O13' Ni3 O1 101.8(4) . . ? O10 Ni3 O1 95.91(11) 2 . ? O13' Ni3 O4 85.6(4) . . ? O10 Ni3 O4 171.52(11) 2 . ? O1 Ni3 O4 91.36(11) . . ? O13' Ni3 N5 9.4(6) . . ? O10 Ni3 N5 83.0(7) 2 . ? O1 Ni3 N5 94.8(6) . . ? O4 Ni3 N5 92.0(6) . . ? O13' Ni3 N4 85.1(4) . . ? O10 Ni3 N4 86.93(11) 2 . ? O1 Ni3 N4 172.53(13) . . ? O4 Ni3 N4 86.39(11) . . ? N5 Ni3 N4 92.4(6) . . ? O13' Ni3 O5 174.3(5) . . ? O10 Ni3 O5 86.25(11) 2 . ? O1 Ni3 O5 81.00(11) . . ? O4 Ni3 O5 99.24(11) . . ? N5 Ni3 O5 168.0(5) . . ? N4 Ni3 O5 92.31(11) . . ? O14 Ni4 O11 90.6(2) 1_655 2_645 ? O14 Ni4 O2 99.4(3) 1_655 . ? O11 Ni4 O2 92.56(11) 2_645 . ? O14 Ni4 O6 87.8(2) 1_655 . ? O11 Ni4 O6 172.36(11) 2_645 . ? O2 Ni4 O6 95.07(11) . . ? O14 Ni4 N3 86.7(3) 1_655 3_655 ? O11 Ni4 N3 86.49(11) 2_645 3_655 ? O2 Ni4 N3 173.90(12) . 3_655 ? O6 Ni4 N3 85.97(12) . 3_655 ? O14 Ni4 N5A 11.4(4) 1_655 1_655 ? O11 Ni4 N5A 80.6(3) 2_645 1_655 ? O2 Ni4 N5A 94.3(4) . 1_655 ? O6 Ni4 N5A 98.4(3) . 1_655 ? N3 Ni4 N5A 91.5(4) 3_655 1_655 ? O14 Ni4 O3 172.9(2) 1_655 . ? O11 Ni4 O3 82.40(10) 2_645 . ? O2 Ni4 O3 79.86(10) . . ? O6 Ni4 O3 99.36(12) . . ? N3 Ni4 O3 94.04(11) 3_655 . ? N5A Ni4 O3 161.7(3) 1_655 . ? O2 Ni1 O7 90.18(11) . 4_666 ? O2 Ni1 O1 85.04(11) . . ? O7 Ni1 O1 93.89(11) 4_666 . ? O2 Ni1 O9 175.68(10) . 2 ? O7 Ni1 O9 87.66(10) 4_666 2 ? O1 Ni1 O9 91.37(11) . 2 ? O2 Ni1 N2 96.00(12) . . ? O7 Ni1 N2 85.92(11) 4_666 . ? O1 Ni1 N2 178.94(12) . . ? O9 Ni1 N2 87.58(11) 2 . ? O2 Ni1 O5 90.32(11) . . ? O7 Ni1 O5 175.58(11) 4_666 . ? O1 Ni1 O5 81.78(11) . . ? O9 Ni1 O5 91.55(10) 2 . ? N2 Ni1 O5 98.39(11) . . ? O2 Ni1 Ni2 44.27(7) . . ? O7 Ni1 Ni2 79.24(7) 4_666 . ? O1 Ni1 Ni2 44.18(8) . . ? O9 Ni1 Ni2 131.53(8) 2 . ? N2 Ni1 Ni2 136.73(9) . . ? O5 Ni1 Ni2 98.10(7) . . ? O1 Ni2 O2 84.74(11) . . ? O1 Ni2 N1 95.27(12) . . ? O2 Ni2 N1 177.74(11) . . ? O1 Ni2 O8 94.54(11) . 4_666 ? O2 Ni2 O8 92.67(11) . 4_666 ? N1 Ni2 O8 89.58(11) . 4_666 ? O1 Ni2 O12 177.90(12) . 2_645 ? O2 Ni2 O12 93.41(11) . 2_645 ? N1 Ni2 O12 86.53(11) . 2_645 ? O8 Ni2 O12 86.55(10) 4_666 2_645 ? O1 Ni2 O3 90.65(11) . . ? O2 Ni2 O3 81.55(10) . . ? N1 Ni2 O3 96.19(11) . . ? O8 Ni2 O3 171.86(11) 4_666 . ? O12 Ni2 O3 88.08(10) 2_645 . ? O1 Ni2 Ni1 44.17(8) . . ? O2 Ni2 Ni1 43.97(7) . . ? N1 Ni2 Ni1 136.76(9) . . ? O8 Ni2 Ni1 81.42(7) 4_666 . ? O12 Ni2 Ni1 134.41(8) 2_645 . ? O3 Ni2 Ni1 98.09(7) . . ? C5 N1 C1 117.5(3) . . ? C5 N1 Ni2 124.6(3) . . ? C1 N1 Ni2 117.8(3) . . ? C7 N2 C11 117.1(3) . . ? C7 N2 Ni1 128.4(3) . . ? C11 N2 Ni1 114.1(3) . . ? C13 N3 C17 116.3(3) . . ? C13 N3 Ni4 123.9(3) . 3_655 ? C17 N3 Ni4 118.9(3) . 3_655 ? C19 N4 C19A 43.0(7) . . ? C19 N4 C23A 93.4(7) . . ? C19A N4 C23A 114.6(8) . . ? C19 N4 C23 118.0(5) . . ? C19A N4 C23 98.1(7) . . ? C23A N4 C23 56.1(7) . . ? C19 N4 Ni3 123.5(4) . . ? C19A N4 Ni3 126.3(6) . . ? C23A N4 Ni3 118.3(5) . . ? C23 N4 Ni3 118.5(3) . . ? Ni4 O2 Ni1 129.22(14) . . ? Ni4 O2 Ni2 101.09(11) . . ? Ni1 O2 Ni2 91.76(11) . . ? Ni3 O1 Ni1 97.63(12) . . ? Ni3 O1 Ni2 131.26(15) . . ? Ni1 O1 Ni2 91.65(12) . . ? C6 O9 Ni1 127.3(2) . 2_545 ? C6 O10 Ni3 128.2(2) . 2_545 ? C12 O11 Ni4 133.1(2) . 2_655 ? C12 O12 Ni2 124.5(2) . 2_655 ? C24 O7 Ni1 127.8(2) . 4_565 ? C24 O8 Ni2 122.9(2) . 4_565 ? C18 O3 Ni2 128.7(2) . . ? C18 O3 Ni4 125.3(2) . . ? Ni2 O3 Ni4 91.62(9) . . ? C18 O4 Ni3 133.8(2) . . ? C31 O6 Ni4 132.0(3) . . ? C31 O5 Ni1 126.1(3) . . ? C31 O5 Ni3 133.6(3) . . ? Ni1 O5 Ni3 92.07(10) . . ? N1 C1 C2 123.8(4) . . ? C1 C2 C3 119.1(4) . . ? C2 C3 C4 116.9(4) . . ? C2 C3 C6 120.9(3) . . ? C4 C3 C6 122.2(4) . . ? C5 C4 C3 120.1(4) . . ? N1 C5 C4 122.5(4) . . ? O9 C6 O10 127.0(3) . . ? O9 C6 C3 117.4(3) . . ? O10 C6 C3 115.5(3) . . ? N2 C7 C8 123.7(4) . . ? C7 C8 C9 118.9(4) . . ? C10 C9 C8 117.5(4) . . ? C10 C9 C12 119.0(4) . . ? C8 C9 C12 123.5(4) . . ? C11 C10 C9 120.5(4) . . ? N2 C11 C10 122.3(4) . . ? O12 C12 O11 127.9(3) . . ? O12 C12 C9 118.5(3) . . ? O11 C12 C9 113.6(3) . . ? N3 C13 C14 123.8(4) . . ? C13 C14 C15 118.4(4) . . ? C16 C15 C14 118.1(3) . . ? C16 C15 C18 120.5(3) . . ? C14 C15 C18 121.3(3) . . ? C15 C16 C17 119.0(4) . . ? N3 C17 C16 123.9(4) . . ? O4 C18 O3 126.6(3) . . ? O4 C18 C15 116.1(3) . . ? O3 C18 C15 117.2(3) . . ? N4 C19 C20 122.0(6) . . ? C21 C20 C19 121.3(6) . . ? C23 C22 C21 120.2(6) . . ? N4 C23 C22 121.7(6) . . ? N4 C19A C20A 124.4(12) . . ? C21 C20A C19A 119.4(12) . . ? C21 C22A C23A 120.9(11) . . ? N4 C23A C22A 121.9(11) . . ? C20A C21 C20 42.1(6) . . ? C20A C21 C22A 117.2(8) . . ? C20 C21 C22A 96.1(7) . . ? C20A C21 C22 98.5(7) . . ? C20 C21 C22 116.2(5) . . ? C22A C21 C22 53.3(7) . . ? C20A C21 C24 123.4(6) . . ? C20 C21 C24 125.4(4) . . ? C22A C21 C24 119.1(6) . . ? C22 C21 C24 118.2(4) . . ? O8 C24 O7 127.7(3) . . ? O8 C24 C21 117.8(3) . . ? O7 C24 C21 114.5(3) . . ? O6 C31 O5 125.1(3) . . ? O6 C31 C32 117.7(4) . . ? O5 C31 C32 117.2(4) . . ? C33A C32 C33 104.0(13) . . ? C33A C32 C31 111.5(12) . . ? C33 C32 C31 114.2(6) . . ? C25 N5 C29 109.1(18) . . ? C25 N5 Ni3 121.9(13) . . ? C29 N5 Ni3 125.9(12) . . ? N5 C25 C26 129.2(15) . . ? C27 C26 C25 117.8(11) . . ? C26 C27 C28 117.2(11) . . ? C26 C27 C30 120.9(10) . . ? C28 C27 C30 121.9(9) . . ? C27 C28 C29 120.6(9) . . ? N5 C29 C28 125.8(11) . . ? O13 C30 O14 126.3(9) . . ? O13 C30 C27 118.5(10) . . ? O14 C30 C27 115.3(9) . . ? C30 O14 Ni4 120.8(7) . 1_455 ? C29A N5A C25A 116.4(12) . . ? C29A N5A Ni4 117.7(9) . 1_455 ? C25A N5A Ni4 124.6(10) . 1_455 ? N5A C25A C26A 123.6(10) . . ? C25A C26A C27A 119.2(10) . . ? C28A C27A C26A 117.0(11) . . ? C28A C27A C30A 124.9(11) . . ? C26A C27A C30A 117.9(10) . . ? C27A C28A C29A 119.1(11) . . ? N5A C29A C28A 124.5(12) . . ? O13' C30A O14' 132.0(13) . . ? O13' C30A C27A 117.4(11) . . ? O14' C30A C27A 110.6(13) . . ? C30A O13' Ni3 119.7(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.623 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.106 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.007 0.010 0.000 943 128 ' ' 2 0.057 0.049 0.500 943 129 ' ' _platon_squeeze_details ; The contribution of any disordered solvent removed by the SQUEEZE process have be included in the overall formula, formula weight, density, F(000), etc. ;