# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Santokh Tandon' _publ_contact_author_email STANDON@KENT.EDU _publ_section_title ; Self-assembly of mixed-valence cobalt (II, III) and nickel(II) clusters: azide-bridged one-dimensional single chain coordination polymers [Co2IICo2III]n comprised of tetranuclear units, tetranuclear cobalt [Co2IICo2III] complexes, ferromagnetically coupled azide-bridged tetranuclear, and hexanuclear nickel(II) complexes: synthesis, structural, and magnetic properties ; loop_ _publ_author_name 'Santokh Tandon' 'Scott Bunge' 'Robert Rakosi' 'Laurence K Thompson' 'Zhiqiang Xu' # Attachment 'tandon-CIF Files.Revised.cif' data_try2 _database_code_depnum_ccdc_archive 'CCDC 677376' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Co2IICo2III(HL)2(CH3O)2(N3)3) (1)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H52 Cl Co4 N13 O18' _chemical_formula_weight 1142.01 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6432(19) _cell_length_b 10.269(2) _cell_length_c 11.465(2) _cell_angle_alpha 105.953(3) _cell_angle_beta 95.676(3) _cell_angle_gamma 100.701(3) _cell_volume 1059.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4404 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 30.39 _exptl_crystal_description irregular _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 586 _exptl_absorpt_coefficient_mu 1.692 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7854 _exptl_absorpt_correction_T_max 0.9202 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_% ? _diffrn_reflns_number 7301 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3718 _reflns_number_gt 3090 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The solvent electron density was modeled using PLATON/SQUEEZE (ver. 01-11-99), which located a potential solvent volume of 315.6 \%A3 and an electron count of 35 electrons/cell, consistent with five water and one methanol molecules/cell. Five water molecules and one methanol molecule were added to the contents of the unit cell during the final refinement to properly calculate the crystal data. ; _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^)+(0.0888P)^2^+9.7950P] 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 3718 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0830 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 0.477 _refine_ls_restrained_S_all 0.477 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.64725(3) 0.49749(3) 0.05465(3) 0.01248(11) Uani 1 1 d . . . Co2 Co 0.39302(4) 0.26874(3) 0.06594(3) 0.01436(11) Uani 1 1 d . . . N1 N 0.8039(2) 0.6130(2) 0.1710(2) 0.0168(5) Uani 1 1 d . . . N2 N 0.3320(2) 0.2215(2) 0.2180(2) 0.0193(5) Uani 1 1 d . . . N3 N 0.7615(2) 0.3599(2) 0.0145(2) 0.0187(5) Uani 1 1 d . . . N4 N 0.8080(2) 0.3179(2) 0.0952(2) 0.0200(5) Uani 1 1 d . . . N5 N 0.8571(3) 0.2733(3) 0.1682(3) 0.0323(6) Uani 1 1 d . . . N6 N 0.5137(3) 0.1201(2) 0.0176(3) 0.0277(6) Uani 1 1 d . . . N7 N 0.5000 0.0000 0.0000 0.0216(7) Uani 1 2 d S . . O1 O 0.56253(19) 0.42031(18) 0.17343(16) 0.0158(4) Uani 1 1 d . . . O2 O 0.72333(18) 0.58841(18) -0.05530(16) 0.0148(4) Uani 1 1 d . . . O3 O 0.2062(2) 0.0904(2) -0.0135(2) 0.0230(4) Uani 1 1 d . . . O4 O 0.48156(18) 0.37460(18) -0.06321(16) 0.0138(4) Uani 1 1 d . . . O5 O 0.0012(14) 0.0925(17) 0.4454(10) 0.118(4) Uani 0.50 1 d P . . O6 O 0.1722(12) 0.0898(10) 0.5517(14) 0.173(6) Uani 0.50 1 d P . . O7 O -0.007(2) 0.0497(15) 0.6197(10) 0.153(6) Uani 0.50 1 d P . . O8 O -0.0756(17) 0.103(2) 0.538(3) 0.266(15) Uani 0.50 1 d P . . Cl1 Cl 0.0000 0.0000 0.5000 0.1516(16) Uani 1 2 d S . . H1A H 0.756(4) 0.510(4) 0.728(4) 0.051(12) Uiso 1 1 d . . . C1 C 0.8131(4) 0.4770(4) 0.6622(3) 0.0304(7) Uani 1 1 d . . . H1B H 0.9030 0.5427 0.6843 0.055(12) Uiso 1 1 d R . . H1C H 0.8288 0.3881 0.6645 0.055(12) Uiso 1 1 d R . . C2 C 0.7450(3) 0.4672(3) 0.5353(3) 0.0228(6) Uani 1 1 d . . . C3 C 0.6127(3) 0.3789(3) 0.4814(3) 0.0221(6) Uani 1 1 d . . . H3 H 0.5644 0.3271 0.5282 0.026 Uiso 1 1 calc R . . C4 C 0.5471(3) 0.3623(3) 0.3623(3) 0.0194(6) Uani 1 1 d . . . C5 C 0.6170(3) 0.4377(3) 0.2895(2) 0.0161(5) Uani 1 1 d . . . C6 C 0.7485(3) 0.5330(3) 0.3462(2) 0.0185(6) Uani 1 1 d . . . C7 C 0.8086(3) 0.5453(3) 0.4663(3) 0.0220(6) Uani 1 1 d . . . H7 H 0.8968 0.6100 0.5017 0.026 Uiso 1 1 calc R . . C8 C 0.8333(3) 0.6154(3) 0.2827(3) 0.0188(6) Uani 1 1 d . . . H8 H 0.9191 0.6772 0.3289 0.023 Uiso 1 1 calc R . . C9 C 0.4082(3) 0.2638(3) 0.3243(3) 0.0216(6) Uani 1 1 d . . . H9 H 0.3709 0.2274 0.3853 0.026 Uiso 1 1 calc R . . C10 C 0.9079(3) 0.6962(3) 0.1171(3) 0.0218(6) Uani 1 1 d . . . H10A H 1.0068 0.6949 0.1488 0.029(9) Uiso 1 1 d R . . H10B H 0.8979 0.7938 0.1386 0.029(9) Uiso 1 1 d R . . C11 C 0.1962(3) 0.1192(3) 0.1969(3) 0.0258(6) Uani 1 1 d . . . H11A H 0.1152 0.1660 0.1975 0.018(8) Uiso 1 1 d R . . H11B H 0.1939 0.0735 0.2625 0.026(8) Uiso 1 1 d R . . C12 C 0.8748(3) 0.6297(3) -0.0205(3) 0.0187(6) Uani 1 1 d . . . H12A H 0.9158 0.6967 -0.0625 0.022(8) Uiso 1 1 d R . . H12B H 0.9176 0.5476 -0.0440 0.022(8) Uiso 1 1 d R . . C13 C 0.1841(3) 0.0130(3) 0.0735(3) 0.0260(7) Uani 1 1 d . . . H13A H 0.2575 -0.0424 0.0758 0.026(8) Uiso 1 1 d R . . H13B H 0.0887 -0.0508 0.0511 0.037(10) Uiso 1 1 d R . . C14 C 0.5049(3) 0.2963(3) -0.1815(3) 0.0217(6) Uani 1 1 d . . . H14A H 0.4152 0.2423 -0.2302 0.058(13) Uiso 1 1 d R . . H14B H 0.5661 0.2353 -0.1717 0.039(10) Uiso 1 1 d R . . H14C H 0.5488 0.3583 -0.2235 0.048(11) Uiso 1 1 d R . . H15 H 0.211(4) 0.049(4) -0.080(4) 0.043(12) 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 Co1 0.01063(18) 0.01070(18) 0.01630(19) 0.00610(14) 0.00139(13) 0.00016(13) Co2 0.01248(19) 0.01139(19) 0.0195(2) 0.00697(14) 0.00170(14) 0.00020(13) N1 0.0139(11) 0.0132(11) 0.0230(12) 0.0083(9) 0.0011(9) -0.0008(9) N2 0.0156(11) 0.0182(12) 0.0254(13) 0.0109(10) 0.0031(10) 0.0003(9) N3 0.0163(11) 0.0180(12) 0.0240(12) 0.0093(10) 0.0021(9) 0.0050(9) N4 0.0136(11) 0.0181(12) 0.0297(13) 0.0092(11) 0.0058(10) 0.0025(9) N5 0.0282(14) 0.0357(15) 0.0431(17) 0.0249(14) 0.0075(12) 0.0111(12) N6 0.0210(13) 0.0107(14) 0.0534(18) 0.0124(11) 0.0089(12) 0.0025(9) N7 0.0117(16) 0.022(2) 0.033(2) 0.0110(15) 0.0053(14) 0.0021(13) O1 0.0146(9) 0.0158(9) 0.0170(9) 0.0083(8) 0.0002(7) -0.0002(7) O2 0.0119(9) 0.0137(9) 0.0192(9) 0.0074(7) 0.0025(7) 0.0003(7) O3 0.0228(11) 0.0191(10) 0.0257(12) 0.0087(9) 0.0026(9) -0.0011(8) O4 0.0133(9) 0.0120(9) 0.0164(9) 0.0048(7) 0.0037(7) 0.0014(7) O5 0.120(9) 0.133(11) 0.085(7) 0.044(8) 0.004(6) -0.024(8) O6 0.118(8) 0.068(6) 0.235(14) -0.069(7) 0.004(9) -0.029(6) O7 0.234(17) 0.103(9) 0.080(7) 0.014(7) 0.051(9) -0.064(10) O8 0.104(11) 0.131(14) 0.41(4) -0.113(19) -0.068(17) 0.001(10) Cl1 0.288(5) 0.0703(16) 0.0620(15) -0.0095(14) 0.010(2) 0.010(2) C1 0.0285(17) 0.0412(19) 0.0218(16) 0.0134(14) 0.0008(13) 0.0044(14) C2 0.0235(15) 0.0281(16) 0.0163(14) 0.0057(12) 0.0024(11) 0.0062(12) C3 0.0224(14) 0.0257(15) 0.0207(14) 0.0116(12) 0.0055(11) 0.0038(12) C4 0.0181(14) 0.0198(14) 0.0223(14) 0.0091(11) 0.0052(11) 0.0038(11) C5 0.0163(13) 0.0162(13) 0.0170(13) 0.0053(11) 0.0030(10) 0.0056(10) C6 0.0173(13) 0.0197(14) 0.0189(14) 0.0069(11) 0.0031(11) 0.0033(11) C7 0.0206(14) 0.0228(15) 0.0192(14) 0.0029(12) 0.0013(11) 0.0024(11) C8 0.0144(13) 0.0176(13) 0.0218(14) 0.0056(11) -0.0008(11) -0.0001(11) C9 0.0198(14) 0.0230(15) 0.0256(15) 0.0131(12) 0.0079(12) 0.0026(11) C10 0.0132(13) 0.0232(15) 0.0284(15) 0.0144(12) -0.0016(11) -0.0046(11) C11 0.0172(14) 0.0270(16) 0.0357(17) 0.0182(14) 0.0040(12) -0.0022(12) C12 0.0104(12) 0.0198(14) 0.0278(15) 0.0118(12) 0.0037(11) 0.0005(10) C13 0.0189(14) 0.0197(14) 0.0415(18) 0.0163(13) 0.0040(13) -0.0011(11) C14 0.0221(14) 0.0191(14) 0.0217(14) 0.0034(12) 0.0030(12) 0.0034(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 Co1 N1 1.880(2) . ? Co1 O2 1.8905(18) . ? Co1 O1 1.9296(18) . ? Co1 N3 1.935(2) . ? Co1 O4 1.9588(18) 2_665 ? Co1 O4 1.9642(18) . ? Co2 O2 2.0269(18) 2_665 ? Co2 N2 2.046(2) . ? Co2 O1 2.0532(18) . ? Co2 N6 2.077(2) . ? Co2 O4 2.2121(18) . ? Co2 O3 2.227(2) . ? N1 C8 1.276(4) . ? N1 C10 1.487(3) . ? N2 C9 1.275(4) . ? N2 C11 1.471(3) . ? N3 N4 1.204(3) . ? N4 N5 1.161(3) . ? N6 N7 1.174(2) . ? N7 N6 1.174(2) 2_655 ? O1 C5 1.332(3) . ? O2 C12 1.426(3) . ? O2 Co2 2.0269(18) 2_665 ? O3 C13 1.445(4) . ? O3 H15 0.77(4) . ? O4 C14 1.437(3) . ? O4 Co1 1.9588(18) 2_665 ? O5 Cl1 1.272(14) . ? O5 O8 1.35(3) . ? O5 O7 1.461(19) 2_556 ? O6 Cl1 1.702(10) . ? O7 Cl1 1.340(11) . ? O7 O8 1.38(3) . ? O7 O5 1.461(19) 2_556 ? O8 Cl1 1.393(18) . ? Cl1 O5 1.272(14) 2_556 ? Cl1 O7 1.340(11) 2_556 ? Cl1 O8 1.393(18) 2_556 ? Cl1 O6 1.702(10) 2_556 ? C1 C2 1.504(4) . ? C1 H1A 1.00(4) . ? C1 H1B 0.9574 . ? C1 H1C 0.9592 . ? C2 C7 1.381(4) . ? C2 C3 1.392(4) . ? C3 C4 1.398(4) . ? C3 H3 0.9500 . ? C4 C5 1.423(4) . ? C4 C9 1.465(4) . ? C5 C6 1.420(4) . ? C6 C7 1.403(4) . ? C6 C8 1.454(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C12 1.511(4) . ? C10 H10A 0.9898 . ? C10 H10B 0.9899 . ? C11 C13 1.509(4) . ? C11 H11A 0.9896 . ? C11 H11B 0.9898 . ? C12 H12A 0.9895 . ? C12 H12B 0.9895 . ? C13 H13A 0.9891 . ? C13 H13B 0.9892 . ? C14 H14A 0.9607 . ? C14 H14B 0.9580 . ? C14 H14C 0.9620 . ? 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 N1 Co1 O2 85.62(9) . . ? N1 Co1 O1 93.24(9) . . ? O2 Co1 O1 174.49(8) . . ? N1 Co1 N3 88.11(10) . . ? O2 Co1 N3 92.05(9) . . ? O1 Co1 N3 93.31(9) . . ? N1 Co1 O4 100.11(9) . 2_665 ? O2 Co1 O4 82.31(7) . 2_665 ? O1 Co1 O4 92.60(8) . 2_665 ? N3 Co1 O4 169.59(9) . 2_665 ? N1 Co1 O4 178.35(9) . . ? O2 Co1 O4 96.03(8) . . ? O1 Co1 O4 85.11(7) . . ? N3 Co1 O4 91.91(9) . . ? O4 Co1 O4 80.06(8) 2_665 . ? O2 Co2 N2 100.26(8) 2_665 . ? O2 Co2 O1 91.52(7) 2_665 . ? N2 Co2 O1 90.57(8) . . ? O2 Co2 N6 161.29(10) 2_665 . ? N2 Co2 N6 97.42(10) . . ? O1 Co2 N6 94.40(9) . . ? O2 Co2 O4 73.27(7) 2_665 . ? N2 Co2 O4 164.86(8) . . ? O1 Co2 O4 76.16(7) . . ? N6 Co2 O4 90.93(9) . . ? O2 Co2 O3 93.32(8) 2_665 . ? N2 Co2 O3 77.17(9) . . ? O1 Co2 O3 167.44(8) . . ? N6 Co2 O3 84.64(9) . . ? O4 Co2 O3 116.35(8) . . ? C8 N1 C10 119.8(2) . . ? C8 N1 Co1 126.88(19) . . ? C10 N1 Co1 112.97(17) . . ? C9 N2 C11 119.0(2) . . ? C9 N2 Co2 124.95(19) . . ? C11 N2 Co2 115.74(18) . . ? N4 N3 Co1 118.38(19) . . ? N5 N4 N3 176.1(3) . . ? N7 N6 Co2 138.03(17) . . ? N6 N7 N6 180.0(2) 2_655 . ? C5 O1 Co1 128.65(16) . . ? C5 O1 Co2 127.41(16) . . ? Co1 O1 Co2 102.37(8) . . ? C12 O2 Co1 108.41(15) . . ? C12 O2 Co2 120.33(15) . 2_665 ? Co1 O2 Co2 106.73(8) . 2_665 ? C13 O3 Co2 109.15(17) . . ? C13 O3 H15 117(3) . . ? Co2 O3 H15 112(3) . . ? C14 O4 Co1 119.03(16) . 2_665 ? C14 O4 Co1 118.56(15) . . ? Co1 O4 Co1 99.94(8) 2_665 . ? C14 O4 Co2 120.94(15) . . ? Co1 O4 Co2 97.69(7) 2_665 . ? Co1 O4 Co2 95.85(7) . . ? Cl1 O5 O8 64.2(13) . . ? Cl1 O5 O7 58.2(8) . 2_556 ? O8 O5 O7 114.3(16) . 2_556 ? Cl1 O7 O8 61.6(11) . . ? Cl1 O7 O5 53.8(6) . 2_556 ? O8 O7 O5 108.3(13) . 2_556 ? O5 O8 O7 105.2(16) . . ? O5 O8 Cl1 55.3(10) . . ? O7 O8 Cl1 57.7(10) . . ? O5 Cl1 O5 180.000(2) 2_556 . ? O5 Cl1 O7 67.9(8) 2_556 . ? O5 Cl1 O7 112.1(8) . . ? O5 Cl1 O7 112.1(8) 2_556 2_556 ? O5 Cl1 O7 67.9(8) . 2_556 ? O7 Cl1 O7 180.000(1) . 2_556 ? O5 Cl1 O8 119.5(15) 2_556 . ? O5 Cl1 O8 60.5(15) . . ? O7 Cl1 O8 60.7(13) . . ? O7 Cl1 O8 119.3(13) 2_556 . ? O5 Cl1 O8 60.5(15) 2_556 2_556 ? O5 Cl1 O8 119.5(15) . 2_556 ? O7 Cl1 O8 119.3(13) . 2_556 ? O7 Cl1 O8 60.7(13) 2_556 2_556 ? O8 Cl1 O8 180.000(4) . 2_556 ? O5 Cl1 O6 81.1(8) 2_556 2_556 ? O5 Cl1 O6 98.9(8) . 2_556 ? O7 Cl1 O6 99.4(8) . 2_556 ? O7 Cl1 O6 80.6(8) 2_556 2_556 ? O8 Cl1 O6 78.1(7) . 2_556 ? O8 Cl1 O6 101.9(7) 2_556 2_556 ? O5 Cl1 O6 98.9(8) 2_556 . ? O5 Cl1 O6 81.1(8) . . ? O7 Cl1 O6 80.6(8) . . ? O7 Cl1 O6 99.4(8) 2_556 . ? O8 Cl1 O6 101.9(7) . . ? O8 Cl1 O6 78.1(7) 2_556 . ? O6 Cl1 O6 180.000(1) 2_556 . ? C2 C1 H1A 114(2) . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 105.5 . . ? C2 C1 H1C 110.1 . . ? H1A C1 H1C 108.2 . . ? H1B C1 H1C 108.9 . . ? C7 C2 C3 116.3(3) . . ? C7 C2 C1 122.4(3) . . ? C3 C2 C1 121.3(3) . . ? C2 C3 C4 123.6(3) . . ? C2 C3 H3 118.2 . . ? C4 C3 H3 118.2 . . ? C3 C4 C5 119.7(3) . . ? C3 C4 C9 114.4(2) . . ? C5 C4 C9 125.9(3) . . ? O1 C5 C6 121.1(2) . . ? O1 C5 C4 122.0(2) . . ? C6 C5 C4 116.9(2) . . ? C7 C6 C5 120.7(3) . . ? C7 C6 C8 116.1(2) . . ? C5 C6 C8 123.1(2) . . ? C2 C7 C6 122.7(3) . . ? C2 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? N1 C8 C6 126.5(3) . . ? N1 C8 H8 116.7 . . ? C6 C8 H8 116.7 . . ? N2 C9 C4 127.0(3) . . ? N2 C9 H9 116.5 . . ? C4 C9 H9 116.5 . . ? N1 C10 C12 106.6(2) . . ? N1 C10 H10A 110.1 . . ? C12 C10 H10A 110.6 . . ? N1 C10 H10B 110.6 . . ? C12 C10 H10B 110.4 . . ? H10A C10 H10B 108.6 . . ? N2 C11 C13 108.0(2) . . ? N2 C11 H11A 110.0 . . ? C13 C11 H11A 110.0 . . ? N2 C11 H11B 110.2 . . ? C13 C11 H11B 110.2 . . ? H11A C11 H11B 108.4 . . ? O2 C12 C10 108.3(2) . . ? O2 C12 H12A 110.5 . . ? C10 C12 H12A 109.9 . . ? O2 C12 H12B 109.9 . . ? C10 C12 H12B 110.0 . . ? H12A C12 H12B 108.4 . . ? O3 C13 C11 106.2(2) . . ? O3 C13 H13A 110.5 . . ? C11 C13 H13A 110.3 . . ? O3 C13 H13B 110.8 . . ? C11 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? O4 C14 H14A 109.9 . . ? O4 C14 H14B 109.8 . . ? H14A C14 H14B 109.2 . . ? O4 C14 H14C 110.0 . . ? H14A C14 H14C 108.8 . . ? H14B C14 H14C 109.2 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.441 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.068 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 1 0.500 1.000 0.500 128.0 36.7 _platon_squeeze_details ; ; #===END data_st033_mono _database_code_depnum_ccdc_archive 'CCDC 677377' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Ni4(H2L)2(OCH3)2(CH3CO2)2(N3)2) (2)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H62 N10 Ni4 O16' _chemical_formula_weight 1125.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.753(5) _cell_length_b 14.687(3) _cell_length_c 14.904(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.030(3) _cell_angle_gamma 90.00 _cell_volume 4762.0(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7591 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 30.21 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.570 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.634 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.4781 _exptl_absorpt_correction_T_max 0.7800 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_% ? _diffrn_reflns_number 36312 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8385 _reflns_number_gt 7179 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The solvent electron density was modeled using PLATON/SQUEEZE (ver. 01-11-99), which located a potential solvent volume of 1356.6 \%A3 and an electron count of 284 electrons/cell, consistent with sixteen methanol molecules/cell. Sixteen methanol molecules were added to the contents of the unitcell during the final refinement to properly calculate the crystal data. ; _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^)+(0.1000P)^2^+0.0123P] 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 8385 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1022 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.2947 _refine_ls_wR_factor_gt 0.2920 _refine_ls_goodness_of_fit_ref 2.309 _refine_ls_restrained_S_all 2.309 _refine_ls_shift/su_max 0.007 _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 0.01277(4) 0.40970(6) 0.45057(6) 0.0182(3) Uani 1 1 d . . . Ni2 Ni 0.09101(4) 0.56978(6) 0.44767(7) 0.0210(3) Uani 1 1 d . . . Ni3 Ni 0.40821(4) 0.57437(6) 0.37099(7) 0.0213(3) Uani 1 1 d . . . Ni4 Ni 0.48320(4) 0.41046(6) 0.43868(6) 0.0183(3) Uani 1 1 d . . . N1 N 0.1828(3) 0.5877(5) 0.4918(5) 0.0341(17) Uani 1 1 d . . . N2 N 0.0810(3) 0.6144(5) 0.5781(4) 0.0261(15) Uani 1 1 d . . . N3 N 0.1226(4) 0.6325(7) 0.6442(6) 0.057(3) Uani 1 1 d . . . N4 N 0.1656(5) 0.6536(16) 0.7051(9) 0.165(9) Uani 1 1 d . . . N5 N 0.0388(3) 0.2746(4) 0.4809(4) 0.0243(14) Uani 1 1 d . . . N6 N 0.3174(3) 0.5964(5) 0.3334(5) 0.0340(17) Uani 1 1 d . . . N7 N 0.5763(3) 0.3801(4) 0.4892(4) 0.0223(14) Uani 1 1 d . . . N8 N 0.6105(3) 0.3781(6) 0.4415(6) 0.049(2) Uani 1 1 d . . . N9 N 0.6430(5) 0.3781(10) 0.3943(9) 0.098(5) Uani 1 1 d . . . N10 N 0.4550(3) 0.2768(4) 0.4437(4) 0.0222(13) Uani 1 1 d . . . O1 O -0.0005(2) 0.5508(4) 0.4244(3) 0.0213(11) Uani 1 1 d . . . O2 O 0.1025(2) 0.4434(3) 0.4980(4) 0.0226(11) Uani 1 1 d . . . O3 O 0.0857(2) 0.5138(3) 0.3152(4) 0.0255(12) Uani 1 1 d . . . O4 O 0.0232(2) 0.3966(3) 0.3207(4) 0.0231(12) Uani 1 1 d . . . O5 O -0.0331(3) 0.2378(4) 0.2804(4) 0.0373(14) Uani 1 1 d . . . H5 H -0.0122 0.2857 0.2939 0.056 Uiso 1 1 calc R . . O6 O 0.0934(3) 0.7018(4) 0.3941(4) 0.0308(13) Uani 1 1 d . . . H6A H 0.0690 0.7197 0.3432 0.046 Uiso 1 1 calc R . . O7 O 0.5000(2) 0.5499(3) 0.4249(3) 0.0205(11) Uani 1 1 d . . . O8 O 0.3942(2) 0.4491(4) 0.4120(4) 0.0243(12) Uani 1 1 d . . . O9 O 0.4087(2) 0.5161(4) 0.2409(4) 0.0290(12) Uani 1 1 d . . . O10 O 0.4082(3) 0.7055(4) 0.3146(4) 0.0340(14) Uani 1 1 d . . . H10A H 0.4300 0.7067 0.2780 0.051 Uiso 1 1 calc R . . O11 O 0.4706(2) 0.3968(3) 0.2982(4) 0.0230(12) Uani 1 1 d . . . O12 O 0.5300(3) 0.2364(4) 0.3100(4) 0.0323(13) Uani 1 1 d . . . H12 H 0.5206 0.2891 0.3229 0.048 Uiso 1 1 calc R . . C1 C -0.0434(3) 0.5794(5) 0.3422(5) 0.0202(16) Uani 1 1 d . . . H1C H -0.0408 0.6457 0.3364 0.030 Uiso 1 1 calc R . . H1D H -0.0847 0.5627 0.3438 0.030 Uiso 1 1 calc R . . H1E H -0.0348 0.5501 0.2883 0.030 Uiso 1 1 calc R . . C2 C 0.1524(3) 0.3971(6) 0.5348(5) 0.0274(18) Uani 1 1 d . . . C3 C 0.1497(4) 0.3030(6) 0.5504(6) 0.0324(19) Uani 1 1 d . . . C4 C 0.2046(4) 0.2521(7) 0.5933(6) 0.042(2) Uani 1 1 d . . . H4 H 0.2016 0.1893 0.6065 0.050 Uiso 1 1 calc R . . C5 C 0.2618(4) 0.2930(8) 0.6158(7) 0.050(3) Uani 1 1 d . . . C6 C 0.2643(4) 0.3826(10) 0.5967(7) 0.056(3) Uani 1 1 d . . . H6 H 0.3035 0.4107 0.6124 0.068 Uiso 1 1 calc R . . C7 C 0.2117(4) 0.4378(7) 0.5542(7) 0.041(2) Uani 1 1 d . . . C8 C 0.0937(4) 0.2479(6) 0.5226(5) 0.0297(19) Uani 1 1 d . . . H8 H 0.0985 0.1848 0.5372 0.036 Uiso 1 1 calc R . . C9 C 0.3196(5) 0.2394(10) 0.6577(8) 0.073(4) Uani 1 1 d . . . H9A H 0.3328 0.2110 0.6074 0.109 Uiso 1 1 calc R . . H9B H 0.3116 0.1920 0.6990 0.109 Uiso 1 1 calc R . . H9C H 0.3519 0.2802 0.6941 0.109 Uiso 1 1 calc R . . C10 C 0.2224(4) 0.5319(8) 0.5356(6) 0.041(2) Uani 1 1 d . . . H10 H 0.2635 0.5535 0.5589 0.050 Uiso 1 1 calc R . . C11 C 0.0571(3) 0.4441(5) 0.2802(5) 0.0211(16) Uani 1 1 d . . . C12 C 0.0585(4) 0.4154(6) 0.1833(6) 0.0314(19) Uani 1 1 d . . . H12A H 0.0895 0.4512 0.1651 0.047 Uiso 1 1 calc R . . H12B H 0.0181 0.4258 0.1381 0.047 Uiso 1 1 calc R . . H12C H 0.0689 0.3506 0.1840 0.047 Uiso 1 1 calc R . . C13 C -0.0065(5) 0.2012(6) 0.4493(6) 0.036(2) Uani 1 1 d . . . H13A H -0.0476 0.2230 0.4496 0.044 Uiso 1 1 calc R . . H13B H 0.0048 0.1489 0.4929 0.044 Uiso 1 1 calc R . . C14 C -0.0086(5) 0.1708(6) 0.3498(6) 0.042(2) Uani 1 1 d . . . H14A H 0.0336 0.1555 0.3489 0.050 Uiso 1 1 calc R . . H14B H -0.0338 0.1149 0.3339 0.050 Uiso 1 1 calc R . . C15 C 0.1987(4) 0.6813(7) 0.4796(8) 0.050(3) Uani 1 1 d . . . H15A H 0.2415 0.6847 0.4765 0.059 Uiso 1 1 calc R . . H15B H 0.1957 0.7182 0.5336 0.059 Uiso 1 1 calc R . . C16 C 0.1567(4) 0.7170(7) 0.3930(7) 0.048(2) Uani 1 1 d . . . H16A H 0.1639 0.6860 0.3383 0.058 Uiso 1 1 calc R . . H16B H 0.1640 0.7830 0.3878 0.058 Uiso 1 1 calc R . . C17 C 0.5415(4) 0.5784(5) 0.3774(5) 0.0227(16) Uani 1 1 d . . . H17A H 0.5412 0.6450 0.3736 0.034 Uiso 1 1 calc R . . H17B H 0.5295 0.5527 0.3140 0.034 Uiso 1 1 calc R . . H17C H 0.5830 0.5574 0.4115 0.034 Uiso 1 1 calc R . . C18 C 0.3430(3) 0.4016(5) 0.3921(5) 0.0210(16) Uani 1 1 d . . . C19 C 0.2830(3) 0.4430(5) 0.3549(5) 0.0241(16) Uani 1 1 d . . . C20 C 0.2300(4) 0.3904(6) 0.3401(6) 0.0330(19) Uani 1 1 d . . . H20 H 0.1912 0.4198 0.3188 0.040 Uiso 1 1 calc R . . C21 C 0.2313(4) 0.2988(6) 0.3549(6) 0.0325(19) Uani 1 1 d . . . C22 C 0.2882(4) 0.2570(6) 0.3867(6) 0.033(2) Uani 1 1 d . . . H22 H 0.2898 0.1930 0.3963 0.040 Uiso 1 1 calc R . . C23 C 0.3436(3) 0.3058(5) 0.4053(5) 0.0220(16) Uani 1 1 d . . . C24 C 0.2762(4) 0.5404(6) 0.3319(6) 0.035(2) Uani 1 1 d . . . H24 H 0.2354 0.5633 0.3136 0.042 Uiso 1 1 calc R . . C25 C 0.1719(4) 0.2450(7) 0.3334(8) 0.047(2) Uani 1 1 d . . . H25A H 0.1388 0.2846 0.3401 0.070 Uiso 1 1 calc R . . H25B H 0.1771 0.1938 0.3773 0.070 Uiso 1 1 calc R . . H25C H 0.1615 0.2217 0.2690 0.070 Uiso 1 1 calc R . . C26 C 0.3994(3) 0.2516(5) 0.4303(5) 0.0246(16) Uani 1 1 d . . . H26 H 0.3937 0.1883 0.4377 0.030 Uiso 1 1 calc R . . C27 C 0.3019(5) 0.6932(7) 0.3069(10) 0.062(3) Uani 1 1 d . . . H27A H 0.2596 0.6974 0.2638 0.074 Uiso 1 1 calc R . . H27B H 0.3040 0.7297 0.3636 0.074 Uiso 1 1 calc R . . C28 C 0.3443(5) 0.7269(8) 0.2624(12) 0.081(5) Uani 1 1 d . . . H28A H 0.3396 0.7938 0.2556 0.097 Uiso 1 1 calc R . . H28B H 0.3349 0.7004 0.1987 0.097 Uiso 1 1 calc R . . C29 C 0.4368(4) 0.4446(5) 0.2307(5) 0.0232(16) Uani 1 1 d . . . C30 C 0.4348(5) 0.4174(6) 0.1317(6) 0.043(2) Uani 1 1 d . . . H30A H 0.3976 0.4424 0.0872 0.064 Uiso 1 1 calc R . . H30B H 0.4343 0.3509 0.1266 0.064 Uiso 1 1 calc R . . H30C H 0.4712 0.4414 0.1171 0.064 Uiso 1 1 calc R . . C31 C 0.4999(4) 0.2018(5) 0.4530(6) 0.0282(17) Uani 1 1 d . . . H31A H 0.4873 0.1495 0.4850 0.034 Uiso 1 1 calc R . . H31B H 0.5408 0.2224 0.4919 0.034 Uiso 1 1 calc R . . C32 C 0.5037(4) 0.1721(5) 0.3567(6) 0.0326(19) Uani 1 1 d . . . H32A H 0.5281 0.1153 0.3643 0.039 Uiso 1 1 calc R . . H32B H 0.4617 0.1579 0.3165 0.039 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0205(5) 0.0184(5) 0.0162(5) -0.0012(3) 0.0062(4) 0.0008(4) Ni2 0.0207(5) 0.0225(5) 0.0206(5) -0.0011(4) 0.0075(4) -0.0017(4) Ni3 0.0214(6) 0.0220(5) 0.0213(6) 0.0012(4) 0.0076(4) 0.0009(4) Ni4 0.0203(5) 0.0193(5) 0.0174(5) -0.0015(3) 0.0086(4) -0.0012(4) N1 0.033(4) 0.040(4) 0.030(4) 0.001(3) 0.009(3) -0.009(3) N2 0.019(3) 0.044(4) 0.014(3) 0.010(3) 0.002(3) -0.010(3) N3 0.030(4) 0.107(8) 0.035(5) -0.034(5) 0.012(4) 0.005(5) N4 0.038(6) 0.35(3) 0.084(9) -0.143(14) -0.012(6) 0.011(10) N5 0.037(4) 0.019(3) 0.021(3) -0.001(3) 0.015(3) 0.003(3) N6 0.032(4) 0.030(4) 0.037(4) 0.011(3) 0.005(3) 0.008(3) N7 0.017(3) 0.025(3) 0.027(3) 0.008(3) 0.009(3) 0.004(3) N8 0.032(4) 0.069(6) 0.051(5) -0.040(4) 0.022(4) -0.016(4) N9 0.071(7) 0.148(11) 0.105(9) -0.082(9) 0.074(7) -0.066(8) N10 0.029(4) 0.021(3) 0.018(3) -0.005(3) 0.010(3) -0.002(3) O1 0.021(3) 0.026(3) 0.015(2) 0.003(2) 0.002(2) 0.003(2) O2 0.017(3) 0.024(3) 0.027(3) 0.003(2) 0.007(2) 0.007(2) O3 0.031(3) 0.023(3) 0.026(3) 0.000(2) 0.014(2) 0.001(2) O4 0.027(3) 0.015(3) 0.027(3) 0.010(2) 0.007(2) -0.002(2) O5 0.055(4) 0.030(3) 0.027(3) -0.005(2) 0.013(3) -0.007(3) O6 0.041(3) 0.024(3) 0.031(3) 0.002(2) 0.015(3) -0.005(3) O7 0.024(3) 0.019(3) 0.023(3) 0.005(2) 0.013(2) -0.002(2) O8 0.028(3) 0.024(3) 0.024(3) 0.001(2) 0.012(2) -0.001(2) O9 0.030(3) 0.034(3) 0.021(3) 0.003(2) 0.005(2) -0.003(2) O10 0.049(4) 0.024(3) 0.036(3) 0.002(2) 0.023(3) 0.004(3) O11 0.028(3) 0.019(3) 0.027(3) 0.005(2) 0.017(2) 0.002(2) O12 0.040(3) 0.026(3) 0.038(3) -0.007(3) 0.023(3) -0.004(3) C1 0.021(4) 0.030(4) 0.012(3) -0.005(3) 0.008(3) -0.006(3) C2 0.017(4) 0.046(5) 0.020(4) 0.006(3) 0.006(3) 0.007(3) C3 0.037(5) 0.037(5) 0.031(4) 0.007(4) 0.022(4) 0.014(4) C4 0.041(5) 0.058(6) 0.028(5) 0.017(4) 0.014(4) 0.022(5) C5 0.035(5) 0.075(8) 0.045(6) 0.030(5) 0.017(4) 0.031(5) C6 0.026(5) 0.108(10) 0.035(5) 0.013(6) 0.009(4) 0.012(6) C7 0.018(4) 0.067(7) 0.035(5) 0.018(4) 0.005(4) 0.008(4) C8 0.044(5) 0.027(4) 0.027(4) 0.008(3) 0.023(4) 0.014(4) C9 0.045(6) 0.115(11) 0.060(7) 0.056(7) 0.019(6) 0.048(7) C10 0.015(4) 0.076(7) 0.035(5) 0.002(5) 0.009(4) 0.003(4) C11 0.016(4) 0.023(4) 0.024(4) 0.007(3) 0.005(3) 0.005(3) C12 0.035(5) 0.033(5) 0.030(5) -0.003(3) 0.015(4) -0.001(3) C13 0.061(6) 0.021(4) 0.030(4) -0.001(3) 0.018(4) -0.001(4) C14 0.074(7) 0.025(4) 0.025(4) -0.008(4) 0.013(4) 0.001(4) C15 0.041(5) 0.047(6) 0.063(7) -0.003(5) 0.018(5) -0.014(5) C16 0.045(6) 0.047(6) 0.054(6) 0.006(5) 0.015(5) -0.015(5) C17 0.021(4) 0.024(4) 0.024(4) -0.002(3) 0.008(3) 0.003(3) C18 0.020(4) 0.027(4) 0.016(4) -0.001(3) 0.005(3) -0.004(3) C19 0.021(4) 0.027(4) 0.027(4) 0.001(3) 0.010(3) 0.001(3) C20 0.022(4) 0.040(5) 0.035(5) -0.012(4) 0.005(4) -0.001(4) C21 0.029(4) 0.039(5) 0.030(4) -0.001(4) 0.010(4) -0.003(4) C22 0.030(4) 0.036(5) 0.033(5) -0.006(4) 0.008(4) -0.022(4) C23 0.026(4) 0.024(4) 0.018(4) -0.003(3) 0.009(3) -0.005(3) C24 0.019(4) 0.044(5) 0.041(5) -0.001(4) 0.007(4) 0.005(4) C25 0.028(5) 0.056(6) 0.057(6) -0.004(5) 0.013(5) 0.002(4) C26 0.030(4) 0.023(4) 0.021(4) -0.003(3) 0.008(3) -0.007(3) C27 0.043(6) 0.036(6) 0.100(9) 0.015(6) 0.009(6) 0.016(5) C28 0.048(7) 0.054(7) 0.156(14) 0.061(8) 0.055(8) 0.027(6) C29 0.026(4) 0.022(4) 0.020(4) -0.002(3) 0.005(3) -0.009(3) C30 0.069(7) 0.036(5) 0.023(5) -0.008(4) 0.012(5) -0.013(4) C31 0.033(4) 0.017(4) 0.038(5) -0.002(3) 0.016(4) -0.004(3) C32 0.036(5) 0.023(4) 0.044(5) -0.005(4) 0.020(4) -0.003(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 O2 2.017(5) . ? Ni1 O4 2.027(5) . ? Ni1 O1 2.047(5) 3_566 ? Ni1 N2 2.079(6) 3_566 ? Ni1 N5 2.082(6) . ? Ni1 O1 2.114(5) . ? Ni2 O2 1.990(5) . ? Ni2 N1 2.014(8) . ? Ni2 O1 2.026(5) . ? Ni2 O3 2.110(5) . ? Ni2 N2 2.126(7) . ? Ni3 O8 1.993(5) . ? Ni3 N6 2.002(7) . ? Ni3 O7 2.038(5) . ? Ni3 N7 2.117(7) 3_666 ? Ni3 O9 2.122(5) . ? Ni4 O8 2.026(5) . ? Ni4 O11 2.038(5) . ? Ni4 O7 2.040(5) 3_666 ? Ni4 N10 2.074(6) . ? Ni4 N7 2.078(6) . ? Ni4 O7 2.105(5) . ? N1 C10 1.253(12) . ? N1 C15 1.446(12) . ? N2 N3 1.180(10) . ? N2 Ni1 2.079(6) 3_566 ? N3 N4 1.165(12) . ? N5 C8 1.283(10) . ? N5 C13 1.471(11) . ? N6 C24 1.242(11) . ? N6 C27 1.490(11) . ? N7 N8 1.198(9) . ? N7 Ni3 2.117(7) 3_666 ? N8 N9 1.160(11) . ? N10 C26 1.276(10) . ? N10 C31 1.480(10) . ? O1 C1 1.390(9) . ? O1 Ni1 2.047(5) 3_566 ? O2 C2 1.300(9) . ? O3 C11 1.242(9) . ? O4 C11 1.311(9) . ? O5 C14 1.418(11) . ? O5 H5 0.8400 . ? O6 C16 1.462(11) . ? O6 H6A 0.8400 . ? O7 C17 1.400(9) . ? O7 Ni4 2.040(5) 3_666 ? O8 C18 1.316(9) . ? O9 C29 1.262(9) . ? O10 C28 1.468(13) . ? O10 H10A 0.8400 . ? O11 C29 1.281(9) . ? O12 C32 1.406(10) . ? O12 H12 0.8400 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C2 C3 1.407(12) . ? C2 C7 1.424(12) . ? C3 C4 1.436(12) . ? C3 C8 1.463(12) . ? C4 C5 1.380(15) . ? C4 H4 0.9500 . ? C5 C6 1.351(17) . ? C5 C9 1.503(12) . ? C6 C7 1.431(13) . ? C6 H6 0.9500 . ? C7 C10 1.444(14) . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10 0.9500 . ? C11 C12 1.514(11) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.536(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.459(14) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.421(10) . ? C18 C19 1.449(11) . ? C19 C20 1.393(11) . ? C19 C24 1.468(12) . ? C20 C21 1.362(12) . ? C20 H20 0.9500 . ? C21 C22 1.384(12) . ? C21 C25 1.517(12) . ? C22 C23 1.404(10) . ? C22 H22 0.9500 . ? C23 C26 1.452(11) . ? C24 H24 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26 0.9500 . ? C27 C28 1.411(15) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.517(11) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.527(11) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? 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 O2 Ni1 O4 88.2(2) . . ? O2 Ni1 O1 90.3(2) . 3_566 ? O4 Ni1 O1 168.9(2) . 3_566 ? O2 Ni1 N2 170.4(2) . 3_566 ? O4 Ni1 N2 100.8(2) . 3_566 ? O1 Ni1 N2 80.2(2) 3_566 3_566 ? O2 Ni1 N5 87.9(2) . . ? O4 Ni1 N5 90.7(2) . . ? O1 Ni1 N5 100.3(2) 3_566 . ? N2 Ni1 N5 95.3(3) 3_566 . ? O2 Ni1 O1 84.2(2) . . ? O4 Ni1 O1 88.13(19) . . ? O1 Ni1 O1 80.8(2) 3_566 . ? N2 Ni1 O1 92.7(2) 3_566 . ? N5 Ni1 O1 172.0(2) . . ? O2 Ni2 N1 89.4(3) . . ? O2 Ni2 O1 87.2(2) . . ? N1 Ni2 O1 171.2(3) . . ? O2 Ni2 O3 87.4(2) . . ? N1 Ni2 O3 97.3(3) . . ? O1 Ni2 O3 90.7(2) . . ? O2 Ni2 N2 88.9(2) . . ? N1 Ni2 N2 92.3(3) . . ? O1 Ni2 N2 79.5(2) . . ? O3 Ni2 N2 169.7(2) . . ? O8 Ni3 N6 89.5(3) . . ? O8 Ni3 O7 87.3(2) . . ? N6 Ni3 O7 173.2(3) . . ? O8 Ni3 N7 89.1(2) . 3_666 ? N6 Ni3 N7 94.9(3) . 3_666 ? O7 Ni3 N7 79.1(2) . 3_666 ? O8 Ni3 O9 87.2(2) . . ? N6 Ni3 O9 95.2(3) . . ? O7 Ni3 O9 90.6(2) . . ? N7 Ni3 O9 169.2(2) 3_666 . ? O8 Ni4 O11 89.6(2) . . ? O8 Ni4 O7 90.0(2) . 3_666 ? O11 Ni4 O7 168.7(2) . 3_666 ? O8 Ni4 N10 88.3(2) . . ? O11 Ni4 N10 89.5(2) . . ? O7 Ni4 N10 101.8(2) 3_666 . ? O8 Ni4 N7 170.0(2) . . ? O11 Ni4 N7 100.0(2) . . ? O7 Ni4 N7 80.0(2) 3_666 . ? N10 Ni4 N7 94.5(2) . . ? O8 Ni4 O7 84.7(2) . . ? O11 Ni4 O7 88.3(2) . . ? O7 Ni4 O7 80.4(2) 3_666 . ? N10 Ni4 O7 172.7(2) . . ? N7 Ni4 O7 92.8(2) . . ? C10 N1 C15 121.3(8) . . ? C10 N1 Ni2 127.2(7) . . ? C15 N1 Ni2 110.9(6) . . ? N3 N2 Ni1 137.3(6) . 3_566 ? N3 N2 Ni2 123.9(6) . . ? Ni1 N2 Ni2 97.9(3) 3_566 . ? N4 N3 N2 175.1(15) . . ? C8 N5 C13 115.0(7) . . ? C8 N5 Ni1 124.9(6) . . ? C13 N5 Ni1 120.1(5) . . ? C24 N6 C27 120.5(8) . . ? C24 N6 Ni3 127.5(6) . . ? C27 N6 Ni3 111.9(6) . . ? N8 N7 Ni4 124.1(6) . . ? N8 N7 Ni3 130.0(6) . 3_666 ? Ni4 N7 Ni3 98.5(3) . 3_666 ? N9 N8 N7 178.3(14) . . ? C26 N10 C31 115.1(6) . . ? C26 N10 Ni4 124.9(5) . . ? C31 N10 Ni4 119.7(5) . . ? C1 O1 Ni2 122.0(4) . . ? C1 O1 Ni1 118.0(4) . 3_566 ? Ni2 O1 Ni1 102.3(2) . 3_566 ? C1 O1 Ni1 118.9(4) . . ? Ni2 O1 Ni1 91.1(2) . . ? Ni1 O1 Ni1 99.2(2) 3_566 . ? C2 O2 Ni2 130.5(5) . . ? C2 O2 Ni1 133.6(5) . . ? Ni2 O2 Ni1 95.1(2) . . ? C11 O3 Ni2 126.4(5) . . ? C11 O4 Ni1 129.7(5) . . ? C14 O5 H5 109.5 . . ? C16 O6 H6A 109.5 . . ? C17 O7 Ni3 120.9(4) . . ? C17 O7 Ni4 117.5(4) . 3_666 ? Ni3 O7 Ni4 102.4(2) . 3_666 ? C17 O7 Ni4 120.6(4) . . ? Ni3 O7 Ni4 90.9(2) . . ? Ni4 O7 Ni4 99.6(2) 3_666 . ? C18 O8 Ni3 129.1(5) . . ? C18 O8 Ni4 131.6(5) . . ? Ni3 O8 Ni4 94.5(2) . . ? C29 O9 Ni3 125.8(5) . . ? C28 O10 H10A 109.5 . . ? C29 O11 Ni4 128.7(5) . . ? C32 O12 H12 109.5 . . ? O1 C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? O1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? O2 C2 C3 120.5(8) . . ? O2 C2 C7 121.6(8) . . ? C3 C2 C7 117.7(8) . . ? C2 C3 C4 120.6(9) . . ? C2 C3 C8 125.1(7) . . ? C4 C3 C8 114.3(8) . . ? C5 C4 C3 121.2(9) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C6 C5 C4 117.8(9) . . ? C6 C5 C9 120.8(11) . . ? C4 C5 C9 121.4(11) . . ? C5 C6 C7 124.4(10) . . ? C5 C6 H6 117.8 . . ? C7 C6 H6 117.8 . . ? C2 C7 C6 118.1(9) . . ? C2 C7 C10 124.5(8) . . ? C6 C7 C10 117.4(9) . . ? N5 C8 C3 127.6(7) . . ? N5 C8 H8 116.2 . . ? C3 C8 H8 116.2 . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 C7 126.1(8) . . ? N1 C10 H10 117.0 . . ? C7 C10 H10 117.0 . . ? O3 C11 O4 123.4(7) . . ? O3 C11 C12 118.4(7) . . ? O4 C11 C12 118.1(7) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N5 C13 C14 110.0(7) . . ? N5 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? N5 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? O5 C14 C13 113.4(7) . . ? O5 C14 H14A 108.9 . . ? C13 C14 H14A 108.9 . . ? O5 C14 H14B 108.9 . . ? C13 C14 H14B 108.9 . . ? H14A C14 H14B 107.7 . . ? N1 C15 C16 109.3(8) . . ? N1 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? N1 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.3 . . ? C15 C16 O6 109.1(8) . . ? C15 C16 H16A 109.9 . . ? O6 C16 H16A 109.9 . . ? C15 C16 H16B 109.9 . . ? O6 C16 H16B 109.9 . . ? H16A C16 H16B 108.3 . . ? O7 C17 H17A 109.5 . . ? O7 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O7 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O8 C18 C23 121.5(7) . . ? O8 C18 C19 122.5(7) . . ? C23 C18 C19 116.0(7) . . ? C20 C19 C18 120.2(7) . . ? C20 C19 C24 118.5(7) . . ? C18 C19 C24 121.3(7) . . ? C21 C20 C19 123.1(8) . . ? C21 C20 H20 118.5 . . ? C19 C20 H20 118.5 . . ? C20 C21 C22 117.8(8) . . ? C20 C21 C25 120.3(8) . . ? C22 C21 C25 121.8(8) . . ? C21 C22 C23 122.4(8) . . ? C21 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C22 C23 C18 120.4(7) . . ? C22 C23 C26 116.0(7) . . ? C18 C23 C26 123.4(7) . . ? N6 C24 C19 127.9(8) . . ? N6 C24 H24 116.0 . . ? C19 C24 H24 116.0 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N10 C26 C23 129.3(7) . . ? N10 C26 H26 115.3 . . ? C23 C26 H26 115.3 . . ? C28 C27 N6 108.5(9) . . ? C28 C27 H27A 110.0 . . ? N6 C27 H27A 110.0 . . ? C28 C27 H27B 110.0 . . ? N6 C27 H27B 110.0 . . ? H27A C27 H27B 108.4 . . ? C27 C28 O10 112.5(10) . . ? C27 C28 H28A 109.1 . . ? O10 C28 H28A 109.1 . . ? C27 C28 H28B 109.1 . . ? O10 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? O9 C29 O11 124.7(7) . . ? O9 C29 C30 117.7(7) . . ? O11 C29 C30 117.4(7) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N10 C31 C32 110.6(7) . . ? N10 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N10 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? O12 C32 C31 115.0(6) . . ? O12 C32 H32A 108.5 . . ? C31 C32 H32A 108.5 . . ? O12 C32 H32B 108.5 . . ? C31 C32 H32B 108.5 . . ? H32A C32 H32B 107.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.929 _refine_diff_density_min -1.343 _refine_diff_density_rms 0.201 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 1 0.305 0.000 0.500 676.9 141.9 2 0.675 0.500 0.000 677.2 141.9 _platon_squeeze_details ; ; #===END #===END data_st072tri _database_code_depnum_ccdc_archive 'CCDC 720881' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((Co2IICo2III(HL)2(CH3O)2(N3)3)Cl?H2O)(2) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H42 Cl Co4 N13 O10' _chemical_formula_weight 991.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/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 19.644(8) _cell_length_b 21.213(8) _cell_length_c 10.010(4) _cell_angle_alpha 90.00 _cell_angle_beta 113.759(8) _cell_angle_gamma 90.00 _cell_volume 3818(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 3633 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 25.30 _exptl_crystal_description irregular _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_absorpt_coefficient_mu 1.849 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7087 _exptl_absorpt_correction_T_max 0.7320 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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_% ? _diffrn_reflns_number 14766 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3379 _reflns_number_gt 2582 _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^)+(0.1000P)^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 3379 _refine_ls_number_parameters 260 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.919 _refine_ls_shift/su_max 0.008 _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 0.24638(3) 0.22941(2) 0.85545(6) 0.01838(19) Uani 1 1 d . . . Co2 Co 0.15531(3) 0.15555(3) 0.99169(6) 0.0205(2) Uani 1 1 d . . . Cl1 Cl 0.5000 0.15340(10) 0.7500 0.0496(5) Uani 1 2 d S . . O3 O 0.18009(15) 0.25146(13) 0.9504(3) 0.0197(6) Uani 1 1 d . . . O2 O 0.23307(15) 0.14548(13) 0.9078(3) 0.0210(6) Uani 1 1 d . . . N5 N 0.0649(2) 0.15118(19) 0.7897(4) 0.0324(9) Uani 1 1 d . . . O1 O 0.07261(18) 0.14596(16) 1.0837(4) 0.0309(8) Uani 1 1 d . . . O4 O 0.26544(15) 0.31267(13) 0.8169(3) 0.0220(7) Uani 1 1 d . . . N2 N 0.1657(2) 0.22009(17) 0.6659(4) 0.0224(8) Uani 1 1 d . . . N1 N 0.31079(19) 0.20624(17) 0.7699(4) 0.0225(8) Uani 1 1 d . . . N3 N 0.15777(19) 0.17017(18) 0.6064(4) 0.0241(8) Uani 1 1 d . . . N7 N 0.16280(19) 0.06279(17) 1.0435(4) 0.0261(8) Uani 1 1 d . . . N4 N 0.1468(2) 0.1235(2) 0.5427(5) 0.0390(10) Uani 1 1 d . . . N6 N 0.0000 0.1514(2) 0.7500 0.0239(12) Uani 1 2 d S . . C4 C 0.2585(2) 0.0355(2) 0.9565(5) 0.0247(10) Uani 1 1 d . . . C9 C 0.3203(2) 0.0957(2) 0.8336(5) 0.0268(10) Uani 1 1 d . . . C12 C 0.3298(3) 0.2586(2) 0.6932(5) 0.0276(10) Uani 1 1 d . . . H12A H 0.3223 0.2455 0.5933 0.033 Uiso 1 1 calc R . . H12B H 0.3824 0.2711 0.7466 0.033 Uiso 1 1 calc R . . C3 C 0.2068(2) 0.0237(2) 1.0239(5) 0.0291(11) Uani 1 1 d . . . H3 H 0.2057 -0.0180 1.0572 0.035 Uiso 1 1 calc R . . C5 C 0.2693(2) 0.0938(2) 0.8985(5) 0.0233(10) Uani 1 1 d . . . C11 C 0.3348(2) 0.1513(2) 0.7650(5) 0.0249(10) Uani 1 1 d . . . H11 H 0.3650 0.1460 0.7117 0.030 Uiso 1 1 calc R . . C6 C 0.2993(3) -0.0168(2) 0.9465(5) 0.0333(11) Uani 1 1 d . . . H6 H 0.2910 -0.0559 0.9839 0.040 Uiso 1 1 calc R . . O5 O 0.9874(2) 0.24648(18) 0.0174(4) 0.0488(10) Uani 1 1 d . . . C13 C 0.2785(2) 0.3130(2) 0.6874(5) 0.0249(10) Uani 1 1 d . . . H13A H 0.3017 0.3534 0.6790 0.030 Uiso 1 1 calc R . . H13B H 0.2309 0.3086 0.6011 0.030 Uiso 1 1 calc R . . C8 C 0.3606(3) 0.0414(2) 0.8288(5) 0.0320(11) Uani 1 1 d . . . H8 H 0.3955 0.0439 0.7853 0.038 Uiso 1 1 calc R . . C14 C 0.1202(2) 0.2950(2) 0.8791(5) 0.0285(10) Uani 1 1 d . . . H14A H 0.0933 0.3026 0.9413 0.043 Uiso 1 1 calc R . . H14B H 0.0861 0.2772 0.7857 0.043 Uiso 1 1 calc R . . H14C H 0.1404 0.3349 0.8615 0.043 Uiso 1 1 calc R . . C7 C 0.3506(3) -0.0151(2) 0.8856(6) 0.0359(12) Uani 1 1 d . . . C2 C 0.1153(2) 0.0421(2) 1.1178(6) 0.0315(11) Uani 1 1 d . . . H2A H 0.1426 0.0464 1.2248 0.038 Uiso 1 1 calc R . . H2B H 0.1014 -0.0027 1.0951 0.038 Uiso 1 1 calc R . . C10 C 0.3941(4) -0.0724(3) 0.8798(7) 0.0566(17) Uani 1 1 d . . . H10A H 0.4313 -0.0819 0.9779 0.085 Uiso 1 1 calc R . . H10B H 0.4192 -0.0644 0.8143 0.085 Uiso 1 1 calc R . . H10C H 0.3603 -0.1084 0.8432 0.085 Uiso 1 1 calc R . . C1 C 0.0465(3) 0.0825(2) 1.0659(6) 0.0340(11) Uani 1 1 d . . . H1A H 0.0148 0.0737 0.9621 0.041 Uiso 1 1 calc R . . H1B H 0.0173 0.0745 1.1248 0.041 Uiso 1 1 calc R . . H1 H 0.035(4) 0.170(3) 1.040(7) 0.06(2) 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 Co1 0.0173(3) 0.0202(3) 0.0175(3) -0.0002(2) 0.0068(2) -0.0015(2) Co2 0.0181(3) 0.0221(3) 0.0214(4) 0.0000(2) 0.0080(2) -0.0028(2) Cl1 0.0325(9) 0.0659(14) 0.0549(13) 0.000 0.0225(9) 0.000 O3 0.0167(14) 0.0219(15) 0.0209(16) -0.0007(12) 0.0080(12) 0.0012(12) O2 0.0187(14) 0.0218(15) 0.0225(17) 0.0017(12) 0.0084(13) 0.0008(12) N5 0.019(2) 0.046(3) 0.031(2) 0.0007(18) 0.0091(17) -0.0049(18) O1 0.0232(16) 0.0349(19) 0.034(2) 0.0015(15) 0.0107(15) -0.0016(15) O4 0.0238(15) 0.0249(16) 0.0182(16) 0.0034(12) 0.0096(13) -0.0003(13) N2 0.0250(19) 0.023(2) 0.019(2) -0.0031(15) 0.0079(16) -0.0023(15) N1 0.0221(18) 0.028(2) 0.0185(19) 0.0005(15) 0.0093(15) -0.0040(16) N3 0.0207(18) 0.029(2) 0.022(2) 0.0018(18) 0.0081(15) -0.0028(16) N7 0.0252(19) 0.029(2) 0.024(2) 0.0022(16) 0.0104(16) -0.0085(17) N4 0.046(3) 0.034(2) 0.033(2) -0.007(2) 0.012(2) 0.002(2) N6 0.028(3) 0.029(3) 0.014(3) 0.000 0.008(2) 0.000 C4 0.028(2) 0.021(2) 0.021(2) -0.0032(17) 0.0059(19) 0.0004(19) C9 0.021(2) 0.031(3) 0.027(3) -0.0032(19) 0.0078(19) 0.0053(19) C12 0.031(2) 0.031(3) 0.025(3) -0.0022(19) 0.016(2) -0.006(2) C3 0.028(2) 0.019(2) 0.035(3) 0.0011(19) 0.008(2) -0.0044(19) C5 0.022(2) 0.024(2) 0.021(2) -0.0036(18) 0.0059(18) 0.0004(18) C11 0.017(2) 0.034(3) 0.026(3) -0.0014(19) 0.0113(19) -0.0010(19) C6 0.040(3) 0.020(2) 0.033(3) 0.001(2) 0.009(2) 0.005(2) O5 0.033(2) 0.046(2) 0.058(3) -0.0103(18) 0.0093(19) -0.0014(17) C13 0.029(2) 0.029(2) 0.019(2) 0.0005(18) 0.0120(19) -0.0037(19) C8 0.032(2) 0.029(3) 0.034(3) -0.001(2) 0.012(2) 0.010(2) C14 0.025(2) 0.031(3) 0.027(3) -0.001(2) 0.009(2) 0.005(2) C7 0.038(3) 0.030(3) 0.037(3) -0.007(2) 0.012(2) 0.009(2) C2 0.030(2) 0.031(3) 0.036(3) 0.005(2) 0.015(2) -0.007(2) C10 0.070(4) 0.041(3) 0.062(4) -0.003(3) 0.030(3) 0.025(3) C1 0.029(2) 0.033(3) 0.042(3) 0.001(2) 0.015(2) -0.012(2) _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 N1 1.857(4) . ? Co1 O4 1.878(3) . ? Co1 O2 1.904(3) . ? Co1 N2 1.931(4) . ? Co1 O3 1.941(3) 7_557 ? Co1 O3 1.953(3) . ? Co1 Co1 2.9712(16) 7_557 ? Co2 N7 2.025(4) . ? Co2 O2 2.029(3) . ? Co2 O4 2.036(3) 7_557 ? Co2 N5 2.087(4) . ? Co2 O3 2.170(3) . ? Co2 O1 2.176(3) . ? O3 C14 1.439(5) . ? O3 Co1 1.941(3) 7_557 ? O2 C5 1.330(5) . ? N5 N6 1.173(4) . ? O1 C1 1.426(5) . ? O1 H1 0.86(6) . ? O4 C13 1.420(5) . ? O4 Co2 2.036(3) 7_557 ? N2 N3 1.194(5) . ? N1 C11 1.266(5) . ? N1 C12 1.480(6) . ? N3 N4 1.150(5) . ? N7 C3 1.268(6) . ? N7 C2 1.475(6) . ? N6 N5 1.173(4) 2_556 ? C4 C6 1.396(6) . ? C4 C5 1.418(6) . ? C4 C3 1.451(6) . ? C9 C5 1.396(6) . ? C9 C8 1.410(6) . ? C9 C11 1.450(6) . ? C12 C13 1.517(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C3 H3 0.9500 . ? C11 H11 0.9500 . ? C6 C7 1.372(7) . ? C6 H6 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C8 C7 1.375(7) . ? C8 H8 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C7 C10 1.501(7) . ? C2 C1 1.505(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? 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 N1 Co1 O4 85.69(14) . . ? N1 Co1 O2 94.26(14) . . ? O4 Co1 O2 175.84(12) . . ? N1 Co1 N2 87.80(16) . . ? O4 Co1 N2 92.69(14) . . ? O2 Co1 N2 91.47(14) . . ? N1 Co1 O3 98.45(14) . 7_557 ? O4 Co1 O3 83.08(12) . 7_557 ? O2 Co1 O3 92.81(12) . 7_557 ? N2 Co1 O3 172.14(13) . 7_557 ? N1 Co1 O3 178.02(14) . . ? O4 Co1 O3 95.85(12) . . ? O2 Co1 O3 84.11(12) . . ? N2 Co1 O3 93.36(14) . . ? O3 Co1 O3 80.54(12) 7_557 . ? N1 Co1 Co1 138.84(11) . 7_557 ? O4 Co1 Co1 89.33(9) . 7_557 ? O2 Co1 Co1 87.97(9) . 7_557 ? N2 Co1 Co1 133.28(11) . 7_557 ? O3 Co1 Co1 40.42(8) 7_557 7_557 ? O3 Co1 Co1 40.11(8) . 7_557 ? N7 Co2 O2 90.83(13) . . ? N7 Co2 O4 97.57(13) . 7_557 ? O2 Co2 O4 90.38(12) . 7_557 ? N7 Co2 N5 98.66(15) . . ? O2 Co2 N5 94.74(14) . . ? O4 Co2 N5 162.90(13) 7_557 . ? N7 Co2 O3 163.95(13) . . ? O2 Co2 O3 75.86(10) . . ? O4 Co2 O3 73.96(11) 7_557 . ? N5 Co2 O3 91.46(13) . . ? N7 Co2 O1 77.90(14) . . ? O2 Co2 O1 168.58(12) . . ? O4 Co2 O1 92.90(12) 7_557 . ? N5 Co2 O1 85.26(15) . . ? O3 Co2 O1 115.55(12) . . ? C14 O3 Co1 119.5(3) . 7_557 ? C14 O3 Co1 119.0(3) . . ? Co1 O3 Co1 99.46(12) 7_557 . ? C14 O3 Co2 119.7(2) . . ? Co1 O3 Co2 97.98(12) 7_557 . ? Co1 O3 Co2 96.48(12) . . ? C5 O2 Co1 127.9(3) . . ? C5 O2 Co2 129.0(3) . . ? Co1 O2 Co2 103.03(12) . . ? N6 N5 Co2 135.4(3) . . ? C1 O1 Co2 109.1(3) . . ? C1 O1 H1 108(4) . . ? Co2 O1 H1 111(4) . . ? C13 O4 Co1 108.5(2) . . ? C13 O4 Co2 120.4(2) . 7_557 ? Co1 O4 Co2 104.96(13) . 7_557 ? N3 N2 Co1 118.1(3) . . ? C11 N1 C12 119.6(4) . . ? C11 N1 Co1 126.6(3) . . ? C12 N1 Co1 113.7(3) . . ? N4 N3 N2 176.1(5) . . ? C3 N7 C2 119.5(4) . . ? C3 N7 Co2 125.4(3) . . ? C2 N7 Co2 115.0(3) . . ? N5 N6 N5 179.5(6) . 2_556 ? C6 C4 C5 118.7(4) . . ? C6 C4 C3 115.2(4) . . ? C5 C4 C3 126.1(4) . . ? C5 C9 C8 120.7(4) . . ? C5 C9 C11 124.0(4) . . ? C8 C9 C11 115.3(4) . . ? N1 C12 C13 106.8(3) . . ? N1 C12 H12A 110.4 . . ? C13 C12 H12A 110.4 . . ? N1 C12 H12B 110.4 . . ? C13 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? N7 C3 C4 127.4(4) . . ? N7 C3 H3 116.3 . . ? C4 C3 H3 116.3 . . ? O2 C5 C9 120.9(4) . . ? O2 C5 C4 121.1(4) . . ? C9 C5 C4 118.0(4) . . ? N1 C11 C9 125.6(4) . . ? N1 C11 H11 117.2 . . ? C9 C11 H11 117.2 . . ? C7 C6 C4 123.8(4) . . ? C7 C6 H6 118.1 . . ? C4 C6 H6 118.1 . . ? O4 C13 C12 108.8(3) . . ? O4 C13 H13A 109.9 . . ? C12 C13 H13A 109.9 . . ? O4 C13 H13B 109.9 . . ? C12 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? C7 C8 C9 121.5(5) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C6 C7 C8 117.3(4) . . ? C6 C7 C10 121.9(5) . . ? C8 C7 C10 120.7(5) . . ? N7 C2 C1 108.6(4) . . ? N7 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N7 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C1 C2 105.5(4) . . ? O1 C1 H1A 110.7 . . ? C2 C1 H1A 110.7 . . ? O1 C1 H1B 110.7 . . ? C2 C1 H1B 110.7 . . ? H1A C1 H1B 108.8 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.673 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.115 #===END data_st064_0m _database_code_depnum_ccdc_archive 'CCDC 720882' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Co2IICo2III (HL)2(OMe)2(N3)4)(3)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H44 Co4 N16 O11' _chemical_formula_weight 1028.52 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6451(10) _cell_length_b 11.8912(11) _cell_length_c 15.6920(14) _cell_angle_alpha 83.769(2) _cell_angle_beta 86.914(2) _cell_angle_gamma 74.5820(10) _cell_volume 2081.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8098 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 30.40 _exptl_crystal_description irregular _exptl_crystal_colour purple _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 1.640 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.5390 _exptl_absorpt_correction_T_max 0.7041 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_% ? _diffrn_reflns_number 16728 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.05 _reflns_number_total 7354 _reflns_number_gt 5674 _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^)+(0.1000P)^2^+0.3131P] 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 7354 _refine_ls_number_parameters 547 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0937 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2729 _refine_ls_wR_factor_gt 0.2524 _refine_ls_goodness_of_fit_ref 2.004 _refine_ls_restrained_S_all 2.004 _refine_ls_shift/su_max 0.119 _refine_ls_shift/su_mean 0.005 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 0.17918(6) 0.34917(6) 0.30528(4) 0.0148(3) Uani 1 1 d . . . Co2 Co 0.31731(6) 0.16887(6) 0.19355(4) 0.0147(3) Uani 1 1 d . . . Co3 Co 0.03881(6) 0.21504(7) 0.21044(5) 0.0189(3) Uani 1 1 d . . . Co4 Co 0.45652(7) 0.30710(7) 0.28688(5) 0.0210(3) Uani 1 1 d . . . N1 N 0.0522(4) 0.4903(4) 0.2810(3) 0.0248(11) Uani 1 1 d . . . N2 N -0.0412(4) 0.4936(4) 0.3189(3) 0.0225(11) Uani 1 1 d . . . N3 N -0.1328(5) 0.5011(5) 0.3535(4) 0.0351(13) Uani 1 1 d . . . N4 N 0.4439(4) 0.0280(4) 0.2181(3) 0.0254(12) Uani 1 1 d . . . N5 N 0.5361(4) 0.0190(4) 0.1780(3) 0.0208(11) Uani 1 1 d . . . N6 N 0.6271(5) 0.0044(5) 0.1413(3) 0.0316(12) Uani 1 1 d . . . N7 N -0.0934(5) 0.3619(5) 0.1689(4) 0.0306(13) Uani 1 1 d . . . N8 N -0.1169(5) 0.4550(6) 0.1354(4) 0.0357(14) Uani 1 1 d . . . N9 N -0.1470(7) 0.5537(7) 0.1033(5) 0.073(2) Uani 1 1 d . . . N10 N 0.5908(5) 0.1599(6) 0.3219(4) 0.0395(15) Uani 1 1 d . . . N11 N 0.6167(5) 0.0770(7) 0.3659(4) 0.0424(16) Uani 1 1 d . . . N12 N 0.6480(8) -0.0111(9) 0.4077(7) 0.120(5) Uani 1 1 d . . . N13 N 0.1760(4) 0.3867(4) 0.4181(3) 0.0206(11) Uani 1 1 d . . . N14 N -0.0720(4) 0.1188(5) 0.2636(3) 0.0269(12) Uani 1 1 d . . . N15 N 0.3204(4) 0.1306(4) 0.0812(3) 0.0194(10) Uani 1 1 d . . . N16 N 0.5645(4) 0.4057(5) 0.2317(3) 0.0275(12) Uani 1 1 d . . . O1 O 0.0681(3) 0.2558(3) 0.3300(2) 0.0176(8) Uani 1 1 d . . . O2 O -0.0187(4) 0.1482(4) 0.0956(3) 0.0318(10) Uani 1 1 d . . . O3 O 0.2975(3) 0.4321(3) 0.2857(2) 0.0190(9) Uani 1 1 d . . . O4 O 0.4280(3) 0.2638(3) 0.1682(2) 0.0192(9) Uani 1 1 d . . . O5 O 0.1976(3) 0.0878(3) 0.2145(2) 0.0181(8) Uani 1 1 d . . . O6 O 0.5133(4) 0.3750(5) 0.3997(3) 0.0407(12) Uani 1 1 d . . . O7 O 0.3162(3) 0.2130(3) 0.3104(2) 0.0180(9) Uani 1 1 d . . . O8 O 0.1807(3) 0.3068(3) 0.1881(2) 0.0163(8) Uani 1 1 d . . . O9 O -0.0028(6) 0.2926(6) 0.9508(4) 0.0671(18) Uani 1 1 d . . . H9 H 0.0608 0.2873 0.9756 0.101 Uiso 1 1 calc R . . O10 O 0.5080(11) 0.2522(14) 0.5562(5) 0.216(7) Uani 1 1 d . . . O11 O 0.2986(15) 0.2307(9) 0.661(2) 0.523(18) Uani 1 1 d . . . C1 C 0.0181(5) 0.2286(5) 0.4052(3) 0.0174(12) Uani 1 1 d . . . C2 C 0.0436(5) 0.2715(5) 0.4814(4) 0.0207(12) Uani 1 1 d . . . C3 C -0.0099(5) 0.2426(5) 0.5603(4) 0.0248(13) Uani 1 1 d . . . H3 H 0.0080 0.2733 0.6099 0.030 Uiso 1 1 calc R . . C4 C -0.0865(6) 0.1723(5) 0.5689(4) 0.0292(15) Uani 1 1 d . . . C5 C -0.1118(5) 0.1302(5) 0.4946(4) 0.0247(13) Uani 1 1 d . . . H5 H -0.1651 0.0815 0.4987 0.030 Uiso 1 1 calc R . . C6 C -0.0618(5) 0.1566(5) 0.4139(3) 0.0183(12) Uani 1 1 d . . . C7 C -0.1460(7) 0.1450(6) 0.6544(4) 0.0411(18) Uani 1 1 d . . . H7A H -0.1012 0.1600 0.7012 0.062 Uiso 1 1 calc R . . H7B H -0.1473 0.0624 0.6609 0.062 Uiso 1 1 calc R . . H7C H -0.2278 0.1948 0.6564 0.062 Uiso 1 1 calc R . . C8 C 0.1181(5) 0.3505(5) 0.4823(4) 0.0248(13) Uani 1 1 d . . . H8 H 0.1250 0.3785 0.5358 0.030 Uiso 1 1 calc R . . C9 C -0.1013(5) 0.1052(5) 0.3432(4) 0.0226(13) Uani 1 1 d . . . H9A H -0.1539 0.0569 0.3582 0.027 Uiso 1 1 calc R . . C10 C -0.1222(6) 0.0589(6) 0.2039(4) 0.0374(17) Uani 1 1 d . . . H10A H -0.2016 0.0515 0.2253 0.045 Uiso 1 1 calc R . . H10B H -0.0697 -0.0208 0.1990 0.045 Uiso 1 1 calc R . . C11 C -0.1328(6) 0.1291(7) 0.1175(4) 0.0362(16) Uani 1 1 d . . . H11A H -0.1566 0.0856 0.0742 0.043 Uiso 1 1 calc R . . H11B H -0.1935 0.2049 0.1202 0.043 Uiso 1 1 calc R . . C13 C 0.2719(5) 0.5240(5) 0.3404(4) 0.0254(13) Uani 1 1 d . . . H13A H 0.2023 0.5873 0.3197 0.030 Uiso 1 1 calc R . . H13B H 0.3411 0.5574 0.3416 0.030 Uiso 1 1 calc R . . C14 C 0.4826(5) 0.2844(5) 0.0928(3) 0.0164(12) Uani 1 1 d . . . C15 C 0.5651(5) 0.3545(4) 0.0848(4) 0.0185(12) Uani 1 1 d . . . C16 C 0.6223(5) 0.3709(5) 0.0062(4) 0.0234(13) Uani 1 1 d . . . H16 H 0.6779 0.4171 0.0022 0.028 Uiso 1 1 calc R . . C17 C 0.6023(6) 0.3228(5) -0.0670(4) 0.0286(14) Uani 1 1 d . . . C18 C 0.5198(5) 0.2576(5) -0.0587(4) 0.0251(13) Uani 1 1 d . . . H18 H 0.5035 0.2248 -0.1078 0.030 Uiso 1 1 calc R . . C19 C 0.4597(5) 0.2377(5) 0.0177(3) 0.0204(12) Uani 1 1 d . . . C20 C 0.6686(7) 0.3402(6) -0.1511(4) 0.0404(18) Uani 1 1 d . . . H20A H 0.6409 0.3015 -0.1949 0.061 Uiso 1 1 calc R . . H20B H 0.7542 0.3062 -0.1435 0.061 Uiso 1 1 calc R . . H20C H 0.6535 0.4242 -0.1693 0.061 Uiso 1 1 calc R . . C21 C 0.5994(5) 0.4111(5) 0.1532(4) 0.0251(13) Uani 1 1 d . . . H21 H 0.6538 0.4573 0.1378 0.030 Uiso 1 1 calc R . . C22 C 0.3817(5) 0.1614(5) 0.0169(4) 0.0225(13) Uani 1 1 d . . . H22 H 0.3754 0.1315 -0.0359 0.027 Uiso 1 1 calc R . . C23 C 0.2488(6) 0.0458(5) 0.0703(4) 0.0264(14) Uani 1 1 d . . . H23A H 0.2947 -0.0175 0.0363 0.032 Uiso 1 1 calc R . . H23B H 0.1740 0.0862 0.0406 0.032 Uiso 1 1 calc R . . C24 C 0.2217(5) -0.0042(5) 0.1603(4) 0.0249(13) Uani 1 1 d . . . H24A H 0.1519 -0.0368 0.1599 0.030 Uiso 1 1 calc R . . H24B H 0.2908 -0.0679 0.1814 0.030 Uiso 1 1 calc R . . C25 C 0.6112(6) 0.4709(7) 0.2902(4) 0.0416(18) Uani 1 1 d . . . H25A H 0.5552 0.5489 0.2950 0.050 Uiso 1 1 calc R . . H25B H 0.6889 0.4823 0.2680 0.050 Uiso 1 1 calc R . . C26 C 0.6257(7) 0.4009(8) 0.3765(5) 0.050(2) Uani 1 1 d . . . H26A H 0.6897 0.3274 0.3736 0.060 Uiso 1 1 calc R . . H26B H 0.6468 0.4466 0.4196 0.060 Uiso 1 1 calc R . . C12 C 0.2454(6) 0.4710(6) 0.4295(4) 0.0273(14) Uani 1 1 d . . . H27A H 0.3205 0.4307 0.4589 0.033 Uiso 1 1 calc R . . H27B H 0.1990 0.5330 0.4644 0.033 Uiso 1 1 calc R . . C28 C 0.1755(5) 0.3961(5) 0.1182(4) 0.0224(13) Uani 1 1 d . . . H28A H 0.1051 0.4614 0.1258 0.034 Uiso 1 1 calc R . . H28B H 0.1706 0.3637 0.0641 0.034 Uiso 1 1 calc R . . H28C H 0.2474 0.4244 0.1169 0.034 Uiso 1 1 calc R . . C27 C 0.3234(6) 0.1232(5) 0.3805(4) 0.0273(14) Uani 1 1 d . . . H27C H 0.3229 0.1571 0.4348 0.041 Uiso 1 1 calc R . . H27D H 0.3973 0.0612 0.3746 0.041 Uiso 1 1 calc R . . H27E H 0.2550 0.0900 0.3799 0.041 Uiso 1 1 calc R . . C29 C 0.0233(14) 0.2245(11) 0.8766(8) 0.154(7) Uani 1 1 d . . . H29A H -0.0256 0.2677 0.8286 0.231 Uiso 1 1 calc R . . H29B H 0.0051 0.1488 0.8913 0.231 Uiso 1 1 calc R . . H29C H 0.1078 0.2115 0.8600 0.231 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0114(4) 0.0234(5) 0.0118(4) -0.0039(3) 0.0019(3) -0.0078(3) Co2 0.0112(4) 0.0219(4) 0.0124(4) -0.0029(3) 0.0023(3) -0.0069(3) Co3 0.0126(5) 0.0300(5) 0.0166(5) -0.0062(3) 0.0008(3) -0.0087(3) Co4 0.0127(5) 0.0363(5) 0.0168(5) -0.0059(3) -0.0002(3) -0.0101(3) N1 0.015(3) 0.030(3) 0.030(3) -0.006(2) 0.001(2) -0.006(2) N2 0.021(3) 0.027(3) 0.023(3) -0.013(2) -0.002(2) -0.006(2) N3 0.021(3) 0.048(3) 0.038(3) -0.020(3) 0.006(3) -0.007(2) N4 0.019(3) 0.028(3) 0.028(3) 0.001(2) 0.003(2) -0.005(2) N5 0.018(3) 0.021(2) 0.024(3) -0.006(2) -0.003(2) -0.005(2) N6 0.022(3) 0.044(3) 0.031(3) -0.015(2) 0.005(2) -0.007(2) N7 0.018(3) 0.030(3) 0.045(4) -0.010(3) -0.004(2) -0.006(2) N8 0.020(3) 0.061(4) 0.026(3) -0.006(3) -0.003(2) -0.011(3) N9 0.054(5) 0.071(5) 0.084(6) 0.044(4) -0.023(4) -0.015(4) N10 0.025(3) 0.056(4) 0.039(4) -0.009(3) -0.006(3) -0.011(3) N11 0.017(3) 0.080(5) 0.026(3) -0.003(3) 0.000(2) -0.007(3) N12 0.060(6) 0.128(9) 0.130(9) 0.090(7) -0.004(6) 0.008(6) N13 0.019(3) 0.033(3) 0.014(2) -0.007(2) 0.001(2) -0.014(2) N14 0.019(3) 0.037(3) 0.029(3) -0.013(2) -0.001(2) -0.011(2) N15 0.019(3) 0.026(3) 0.016(2) -0.0071(19) 0.001(2) -0.009(2) N16 0.018(3) 0.041(3) 0.029(3) -0.012(2) 0.002(2) -0.015(2) O1 0.015(2) 0.026(2) 0.015(2) -0.0044(16) 0.0034(16) -0.0117(16) O2 0.023(2) 0.048(3) 0.028(2) -0.013(2) -0.0028(19) -0.011(2) O3 0.016(2) 0.027(2) 0.017(2) -0.0077(16) 0.0039(16) -0.0111(17) O4 0.015(2) 0.030(2) 0.014(2) -0.0049(16) 0.0042(16) -0.0089(16) O5 0.019(2) 0.021(2) 0.017(2) -0.0019(16) 0.0023(16) -0.0101(16) O6 0.026(3) 0.079(4) 0.027(2) -0.017(2) -0.001(2) -0.025(2) O7 0.0111(19) 0.028(2) 0.0144(19) 0.0004(16) -0.0019(15) -0.0042(16) O8 0.015(2) 0.023(2) 0.0125(19) -0.0012(15) -0.0007(15) -0.0073(16) O9 0.098(5) 0.061(4) 0.046(4) 0.000(3) -0.005(3) -0.029(4) O10 0.197(12) 0.44(2) 0.061(6) 0.062(9) -0.017(6) -0.204(14) O11 0.237(16) 0.044(6) 1.28(5) 0.072(17) -0.31(3) -0.022(8) C1 0.011(3) 0.020(3) 0.019(3) -0.004(2) 0.005(2) -0.001(2) C2 0.019(3) 0.027(3) 0.017(3) -0.004(2) 0.004(2) -0.007(2) C3 0.030(3) 0.024(3) 0.019(3) -0.001(2) 0.006(3) -0.006(3) C4 0.039(4) 0.021(3) 0.025(3) -0.001(2) 0.013(3) -0.007(3) C5 0.026(3) 0.015(3) 0.030(3) -0.001(2) 0.008(3) -0.002(2) C6 0.012(3) 0.019(3) 0.021(3) -0.003(2) 0.005(2) -0.001(2) C7 0.069(5) 0.033(4) 0.025(4) -0.001(3) 0.021(3) -0.027(4) C8 0.026(3) 0.037(3) 0.014(3) -0.010(2) 0.004(2) -0.012(3) C9 0.017(3) 0.025(3) 0.028(3) -0.005(2) 0.005(2) -0.009(2) C10 0.027(4) 0.056(5) 0.040(4) -0.016(3) 0.002(3) -0.027(3) C11 0.026(4) 0.060(5) 0.029(4) -0.014(3) -0.007(3) -0.017(3) C13 0.026(3) 0.032(3) 0.024(3) -0.008(3) 0.003(3) -0.015(3) C14 0.012(3) 0.021(3) 0.015(3) -0.003(2) 0.006(2) -0.004(2) C15 0.013(3) 0.015(3) 0.025(3) 0.001(2) 0.000(2) -0.001(2) C16 0.024(3) 0.014(3) 0.030(3) 0.002(2) 0.010(3) -0.003(2) C17 0.035(4) 0.019(3) 0.027(3) 0.000(2) 0.010(3) -0.004(3) C18 0.031(3) 0.025(3) 0.018(3) -0.003(2) 0.008(3) -0.005(3) C19 0.021(3) 0.023(3) 0.015(3) -0.003(2) 0.005(2) -0.005(2) C20 0.061(5) 0.037(4) 0.028(4) -0.005(3) 0.024(3) -0.026(3) C21 0.014(3) 0.031(3) 0.031(3) -0.004(3) 0.003(2) -0.008(2) C22 0.024(3) 0.031(3) 0.015(3) -0.006(2) 0.004(2) -0.011(3) C23 0.025(3) 0.037(4) 0.023(3) -0.014(3) 0.007(3) -0.017(3) C24 0.025(3) 0.030(3) 0.026(3) -0.009(3) 0.002(3) -0.015(3) C25 0.032(4) 0.070(5) 0.037(4) -0.022(4) 0.003(3) -0.033(4) C26 0.032(4) 0.089(6) 0.043(4) -0.025(4) -0.006(3) -0.031(4) C12 0.026(3) 0.043(4) 0.023(3) -0.014(3) 0.006(3) -0.023(3) C28 0.021(3) 0.026(3) 0.021(3) 0.000(2) -0.001(2) -0.006(2) C27 0.027(3) 0.035(4) 0.017(3) 0.006(3) -0.002(3) -0.006(3) C29 0.202(16) 0.106(11) 0.137(12) -0.065(10) -0.062(12) 0.021(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 Co1 N13 1.868(4) . ? Co1 O3 1.891(4) . ? Co1 O1 1.917(4) . ? Co1 N1 1.937(5) . ? Co1 O7 1.946(4) . ? Co1 O8 1.957(4) . ? Co2 N15 1.865(4) . ? Co2 O5 1.891(4) . ? Co2 O4 1.927(4) . ? Co2 N4 1.933(5) . ? Co2 O8 1.956(4) . ? Co2 O7 1.960(4) . ? Co3 N14 2.033(5) . ? Co3 O5 2.054(4) . ? Co3 O1 2.055(4) . ? Co3 N7 2.068(6) . ? Co3 O8 2.203(4) . ? Co3 O2 2.248(4) . ? Co4 N16 2.038(5) . ? Co4 O3 2.043(4) . ? Co4 O4 2.052(4) . ? Co4 N10 2.059(6) . ? Co4 O7 2.208(4) . ? Co4 O6 2.224(4) . ? N1 N2 1.205(7) . ? N2 N3 1.156(7) . ? N4 N5 1.201(7) . ? N5 N6 1.159(7) . ? N7 N8 1.143(8) . ? N8 N9 1.194(9) . ? N10 N11 1.121(9) . ? N11 N12 1.155(10) . ? N13 C8 1.282(7) . ? N13 C12 1.476(7) . ? N14 C9 1.282(8) . ? N14 C10 1.468(8) . ? N15 C22 1.283(7) . ? N15 C23 1.497(7) . ? N16 C21 1.276(8) . ? N16 C25 1.474(8) . ? O1 C1 1.334(6) . ? O2 C11 1.425(8) . ? O3 C13 1.422(7) . ? O4 C14 1.343(6) . ? O5 C24 1.419(7) . ? O6 C26 1.441(8) . ? O7 C27 1.437(7) . ? O8 C28 1.433(7) . ? O9 C29 1.462(12) . ? O9 H9 0.8400 . ? C1 C6 1.415(8) . ? C1 C2 1.424(8) . ? C2 C3 1.406(8) . ? C2 C8 1.440(8) . ? C3 C4 1.368(9) . ? C3 H3 0.9500 . ? C4 C5 1.393(9) . ? C4 C7 1.520(8) . ? C5 C6 1.404(8) . ? C5 H5 0.9500 . ? C6 C9 1.471(8) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8 0.9500 . ? C9 H9A 0.9500 . ? C10 C11 1.505(10) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 C12 1.521(8) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.422(8) . ? C14 C19 1.422(8) . ? C15 C16 1.390(8) . ? C15 C21 1.452(8) . ? C16 C17 1.394(9) . ? C16 H16 0.9500 . ? C17 C18 1.378(9) . ? C17 C20 1.516(8) . ? C18 C19 1.386(8) . ? C18 H18 0.9500 . ? C19 C22 1.445(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.522(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.504(11) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C12 H27A 0.9900 . ? C12 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C27 H27C 0.9800 . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N13 Co1 O3 85.07(19) . . ? N13 Co1 O1 93.55(19) . . ? O3 Co1 O1 175.61(16) . . ? N13 Co1 N1 88.4(2) . . ? O3 Co1 N1 92.16(19) . . ? O1 Co1 N1 91.97(19) . . ? N13 Co1 O7 99.33(19) . . ? O3 Co1 O7 83.07(17) . . ? O1 Co1 O7 93.05(17) . . ? N1 Co1 O7 170.50(19) . . ? N13 Co1 O8 178.58(18) . . ? O3 Co1 O8 96.27(16) . . ? O1 Co1 O8 85.08(16) . . ? N1 Co1 O8 92.01(19) . . ? O7 Co1 O8 80.41(16) . . ? N15 Co2 O5 85.60(19) . . ? N15 Co2 O4 93.67(18) . . ? O5 Co2 O4 174.74(16) . . ? N15 Co2 N4 88.3(2) . . ? O5 Co2 N4 92.71(19) . . ? O4 Co2 N4 92.48(19) . . ? N15 Co2 O8 99.51(18) . . ? O5 Co2 O8 82.93(16) . . ? O4 Co2 O8 92.05(17) . . ? N4 Co2 O8 170.66(19) . . ? N15 Co2 O7 178.28(18) . . ? O5 Co2 O7 96.00(16) . . ? O4 Co2 O7 84.68(16) . . ? N4 Co2 O7 92.19(19) . . ? O8 Co2 O7 80.10(16) . . ? N14 Co3 O5 99.83(18) . . ? N14 Co3 O1 90.03(17) . . ? O5 Co3 O1 89.97(15) . . ? N14 Co3 N7 96.4(2) . . ? O5 Co3 N7 160.5(2) . . ? O1 Co3 N7 100.69(19) . . ? N14 Co3 O8 164.14(18) . . ? O5 Co3 O8 73.43(14) . . ? O1 Co3 O8 75.83(15) . . ? N7 Co3 O8 93.29(18) . . ? N14 Co3 O2 77.45(18) . . ? O5 Co3 O2 92.02(16) . . ? O1 Co3 O2 167.48(17) . . ? N7 Co3 O2 81.10(19) . . ? O8 Co3 O2 116.56(15) . . ? N16 Co4 O3 99.75(19) . . ? N16 Co4 O4 89.79(18) . . ? O3 Co4 O4 91.46(15) . . ? N16 Co4 N10 96.3(2) . . ? O3 Co4 N10 161.7(2) . . ? O4 Co4 N10 97.4(2) . . ? N16 Co4 O7 163.61(18) . . ? O3 Co4 O7 73.44(15) . . ? O4 Co4 O7 75.73(15) . . ? N10 Co4 O7 93.2(2) . . ? N16 Co4 O6 77.76(19) . . ? O3 Co4 O6 91.10(17) . . ? O4 Co4 O6 167.54(17) . . ? N10 Co4 O6 83.7(2) . . ? O7 Co4 O6 116.66(16) . . ? N2 N1 Co1 116.2(4) . . ? N3 N2 N1 177.3(6) . . ? N5 N4 Co2 117.8(4) . . ? N6 N5 N4 176.4(6) . . ? N8 N7 Co3 147.5(5) . . ? N7 N8 N9 176.3(8) . . ? N11 N10 Co4 145.5(6) . . ? N10 N11 N12 176.1(9) . . ? C8 N13 C12 119.5(5) . . ? C8 N13 Co1 127.0(4) . . ? C12 N13 Co1 113.5(4) . . ? C9 N14 C10 117.5(5) . . ? C9 N14 Co3 126.7(4) . . ? C10 N14 Co3 115.8(4) . . ? C22 N15 C23 118.8(5) . . ? C22 N15 Co2 127.8(4) . . ? C23 N15 Co2 113.2(4) . . ? C21 N16 C25 117.9(5) . . ? C21 N16 Co4 126.2(4) . . ? C25 N16 Co4 115.8(4) . . ? C1 O1 Co1 128.8(3) . . ? C1 O1 Co3 128.7(3) . . ? Co1 O1 Co3 102.45(17) . . ? C11 O2 Co3 106.4(4) . . ? C13 O3 Co1 108.4(3) . . ? C13 O3 Co4 122.3(4) . . ? Co1 O3 Co4 105.66(18) . . ? C14 O4 Co2 128.0(3) . . ? C14 O4 Co4 128.9(3) . . ? Co2 O4 Co4 102.73(17) . . ? C24 O5 Co2 108.2(3) . . ? C24 O5 Co3 121.4(3) . . ? Co2 O5 Co3 105.62(17) . . ? C26 O6 Co4 107.1(4) . . ? C27 O7 Co1 119.0(3) . . ? C27 O7 Co2 118.2(4) . . ? Co1 O7 Co2 99.86(17) . . ? C27 O7 Co4 121.0(3) . . ? Co1 O7 Co4 97.84(16) . . ? Co2 O7 Co4 96.32(16) . . ? C28 O8 Co2 118.7(3) . . ? C28 O8 Co1 118.7(3) . . ? Co2 O8 Co1 99.62(17) . . ? C28 O8 Co3 121.0(3) . . ? Co2 O8 Co3 98.01(16) . . ? Co1 O8 Co3 96.04(16) . . ? C29 O9 H9 109.5 . . ? O1 C1 C6 122.5(5) . . ? O1 C1 C2 120.8(5) . . ? C6 C1 C2 116.7(5) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 C8 116.2(5) . . ? C1 C2 C8 123.3(5) . . ? C4 C3 C2 123.1(6) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C3 C4 C5 116.8(5) . . ? C3 C4 C7 122.2(6) . . ? C5 C4 C7 121.0(6) . . ? C4 C5 C6 122.8(6) . . ? C4 C5 H5 118.6 . . ? C6 C5 H5 118.6 . . ? C5 C6 C1 120.3(5) . . ? C5 C6 C9 114.5(5) . . ? C1 C6 C9 125.2(5) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N13 C8 C2 126.3(5) . . ? N13 C8 H8 116.8 . . ? C2 C8 H8 116.8 . . ? N14 C9 C6 126.7(5) . . ? N14 C9 H9A 116.6 . . ? C6 C9 H9A 116.6 . . ? N14 C10 C11 108.7(6) . . ? N14 C10 H10A 109.9 . . ? C11 C10 H10A 109.9 . . ? N14 C10 H10B 109.9 . . ? C11 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? O2 C11 C10 106.8(5) . . ? O2 C11 H11A 110.4 . . ? C10 C11 H11A 110.4 . . ? O2 C11 H11B 110.4 . . ? C10 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? O3 C13 C12 107.1(5) . . ? O3 C13 H13A 110.3 . . ? C12 C13 H13A 110.3 . . ? O3 C13 H13B 110.3 . . ? C12 C13 H13B 110.3 . . ? H13A C13 H13B 108.6 . . ? O4 C14 C15 121.3(5) . . ? O4 C14 C19 121.3(5) . . ? C15 C14 C19 117.4(5) . . ? C16 C15 C14 119.4(5) . . ? C16 C15 C21 114.7(5) . . ? C14 C15 C21 125.9(5) . . ? C15 C16 C17 123.3(6) . . ? C15 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C18 C17 C16 116.5(5) . . ? C18 C17 C20 121.7(6) . . ? C16 C17 C20 121.8(6) . . ? C17 C18 C19 123.2(6) . . ? C17 C18 H18 118.4 . . ? C19 C18 H18 118.4 . . ? C18 C19 C14 120.1(5) . . ? C18 C19 C22 116.2(5) . . ? C14 C19 C22 123.5(5) . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N16 C21 C15 127.3(6) . . ? N16 C21 H21 116.4 . . ? C15 C21 H21 116.3 . . ? N15 C22 C19 125.7(5) . . ? N15 C22 H22 117.2 . . ? C19 C22 H22 117.2 . . ? N15 C23 C24 106.2(5) . . ? N15 C23 H23A 110.5 . . ? C24 C23 H23A 110.5 . . ? N15 C23 H23B 110.5 . . ? C24 C23 H23B 110.5 . . ? H23A C23 H23B 108.7 . . ? O5 C24 C23 108.0(5) . . ? O5 C24 H24A 110.1 . . ? C23 C24 H24A 110.1 . . ? O5 C24 H24B 110.1 . . ? C23 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? N16 C25 C26 108.0(6) . . ? N16 C25 H25A 110.1 . . ? C26 C25 H25A 110.1 . . ? N16 C25 H25B 110.1 . . ? C26 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? O6 C26 C25 107.0(6) . . ? O6 C26 H26A 110.3 . . ? C25 C26 H26A 110.3 . . ? O6 C26 H26B 110.3 . . ? C25 C26 H26B 110.3 . . ? H26A C26 H26B 108.6 . . ? N13 C12 C13 106.9(5) . . ? N13 C12 H27A 110.3 . . ? C13 C12 H27A 110.3 . . ? N13 C12 H27B 110.3 . . ? C13 C12 H27B 110.3 . . ? H27A C12 H27B 108.6 . . ? O8 C28 H28A 109.5 . . ? O8 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O8 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O7 C27 H27C 109.5 . . ? O7 C27 H27D 109.5 . . ? H27C C27 H27D 109.5 . . ? O7 C27 H27E 109.5 . . ? H27C C27 H27E 109.5 . . ? H27D C27 H27E 109.5 . . ? O9 C29 H29A 109.5 . . ? O9 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O9 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.903 _refine_diff_density_min -1.579 _refine_diff_density_rms 0.208 #===END data_st040z _database_code_depnum_ccdc_archive 'CCDC 720883' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co2IICo2III(HL)2(CH3O)2(N3)2(CH3CO2)2)(4) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H56 Co4 N10 O16' _chemical_formula_weight 1096.61 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 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 10.8017(16) _cell_length_b 21.477(3) _cell_length_c 9.6371(15) _cell_angle_alpha 90.00 _cell_angle_beta 106.372(3) _cell_angle_gamma 90.00 _cell_volume 2145.1(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5773 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 29.04 _exptl_crystal_description irregular _exptl_crystal_colour black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 1.602 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6902 _exptl_absorpt_correction_T_max 0.8068 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_% ? _diffrn_reflns_number 16945 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0333 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3796 _reflns_number_gt 3228 _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^)+(0.1000P)^2^+0.4997P] 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 3796 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 O7 O 0.9479(5) 0.3570(2) 0.8375(5) 0.0824(13) Uani 1 1 d . . . H7 H 0.9654 0.3262 0.8933 0.124 Uiso 1 1 calc R . . Co1 Co 0.49862(4) 0.47669(2) 0.64612(4) 0.01636(17) Uani 1 1 d . . . Co2 Co 0.31863(4) 0.41508(2) 0.37670(5) 0.01815(17) Uani 1 1 d . . . O4 O 0.4551(2) 0.39561(10) 0.5626(2) 0.0185(5) Uani 1 1 d . . . C4 C 0.4758(3) 0.28611(16) 0.5263(4) 0.0206(7) Uani 1 1 d . . . C11 C 0.6522(3) 0.38934(16) 0.8385(3) 0.0206(7) Uani 1 1 d . . . H11 H 0.7124 0.3807 0.9293 0.025 Uiso 1 1 calc R . . C8 C 0.6705(3) 0.27997(17) 0.7856(4) 0.0231(7) Uani 1 1 d . . . H8 H 0.7361 0.2783 0.8751 0.028 Uiso 1 1 calc R . . C10 C 0.5111(3) 0.34141(16) 0.6091(3) 0.0189(7) Uani 1 1 d . . . C9 C 0.6088(3) 0.33640(16) 0.7419(4) 0.0205(7) Uani 1 1 d . . . C5 C 0.5410(3) 0.23040(16) 0.5768(4) 0.0229(7) Uani 1 1 d . . . H5 H 0.5156 0.1937 0.5209 0.028 Uiso 1 1 calc R . . C3 C 0.3773(3) 0.28074(16) 0.3869(4) 0.0221(7) Uani 1 1 d . . . H3 H 0.3660 0.2404 0.3449 0.027 Uiso 1 1 calc R . . N2 N 0.6176(3) 0.44588(13) 0.8131(3) 0.0191(6) Uani 1 1 d . . . N1 N 0.3042(3) 0.32370(14) 0.3140(3) 0.0218(6) Uani 1 1 d . . . C12 C 0.6726(3) 0.49464(16) 0.9213(3) 0.0216(7) Uani 1 1 d . . . H12A H 0.7626 0.5039 0.9223 0.026 Uiso 1 1 calc R . . H12B H 0.6723 0.4807 1.0191 0.026 Uiso 1 1 calc R . . N3 N 0.3640(3) 0.47230(13) 0.7420(3) 0.0211(6) Uani 1 1 d . . . N4 N 0.3288(3) 0.42124(14) 0.7680(3) 0.0228(7) Uani 1 1 d . . . N5 N 0.2902(3) 0.37412(16) 0.7957(4) 0.0337(8) Uani 1 1 d . . . O3 O 0.6195(2) 0.49320(10) 0.5333(2) 0.0171(5) Uani 1 1 d . . . O6 O 0.1487(3) 0.42161(12) 0.4512(3) 0.0307(6) Uani 1 1 d . . . O2 O 0.5496(2) 0.55626(10) 0.7239(2) 0.0189(5) Uani 1 1 d . . . C13 C 0.5885(3) 0.55222(16) 0.8776(3) 0.0211(7) Uani 1 1 d . . . H13A H 0.5116 0.5491 0.9140 0.025 Uiso 1 1 calc R . . H13B H 0.6375 0.5899 0.9196 0.025 Uiso 1 1 calc R . . C15 C 0.0863(4) 0.44198(17) 0.3295(4) 0.0306(9) Uani 1 1 d . . . C16 C -0.0515(4) 0.4626(2) 0.3024(5) 0.0398(10) Uani 1 1 d . . . H16A H -0.1002 0.4304 0.3365 0.060 Uiso 1 1 calc R . . H16B H -0.0899 0.4693 0.1986 0.060 Uiso 1 1 calc R . . H16C H -0.0542 0.5015 0.3545 0.060 Uiso 1 1 calc R . . C6 C 0.6402(3) 0.22602(16) 0.7039(4) 0.0239(8) Uani 1 1 d . . . C7 C 0.7136(4) 0.16646(18) 0.7469(4) 0.0348(9) Uani 1 1 d . . . H7A H 0.6527 0.1318 0.7378 0.052 Uiso 1 1 calc R . . H7B H 0.7670 0.1696 0.8473 0.052 Uiso 1 1 calc R . . H7C H 0.7689 0.1591 0.6835 0.052 Uiso 1 1 calc R . . C2 C 0.2115(4) 0.30258(17) 0.1776(4) 0.0267(8) Uani 1 1 d . . . H2A H 0.2452 0.2648 0.1421 0.032 Uiso 1 1 calc R . . H2B H 0.2012 0.3354 0.1031 0.032 Uiso 1 1 calc R . . C1 C 0.0807(4) 0.28831(19) 0.2019(4) 0.0333(9) Uani 1 1 d . . . H1A H 0.0890 0.2524 0.2682 0.040 Uiso 1 1 calc R . . H1B H 0.0512 0.3246 0.2472 0.040 Uiso 1 1 calc R . . C14 C 0.7117(3) 0.44581(16) 0.5256(4) 0.0229(8) Uani 1 1 d . . . H14A H 0.6660 0.4079 0.4828 0.034 Uiso 1 1 calc R . . H14B H 0.7667 0.4366 0.6231 0.034 Uiso 1 1 calc R . . H14C H 0.7653 0.4606 0.4655 0.034 Uiso 1 1 calc R . . O1 O -0.0116(3) 0.27441(14) 0.0669(3) 0.0410(7) Uani 1 1 d . . . O5 O 0.1401(3) 0.44614(13) 0.2295(3) 0.0343(7) Uani 1 1 d . . . C17 C 0.9892(6) 0.4072(3) 0.9093(6) 0.0696(17) Uani 1 1 d . . . H17A H 0.9742 0.4047 1.0048 0.104 Uiso 1 1 calc R . . H17B H 0.9431 0.4432 0.8568 0.104 Uiso 1 1 calc R . . H17C H 1.0819 0.4118 0.9209 0.104 Uiso 1 1 calc R . . O8 O -0.0193(3) 0.15036(17) 0.0701(5) 0.0530(9) Uani 1 1 d . . . H8A H 0.047(6) 0.131(3) 0.053(6) 0.08(2) Uiso 1 1 d . . . H8B H -0.012(4) 0.1392(17) 0.166(5) 0.018(10) Uiso 1 1 d . . . H1 H -0.006(5) 0.229(3) 0.056(5) 0.059(15) 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 O7 0.070(3) 0.102(4) 0.072(3) 0.014(3) 0.014(2) -0.002(3) Co1 0.0150(3) 0.0229(3) 0.0096(3) -0.00111(16) 0.00075(18) -0.00084(17) Co2 0.0151(3) 0.0244(3) 0.0126(3) -0.00027(17) 0.00010(19) -0.00079(17) O4 0.0181(12) 0.0229(12) 0.0126(11) -0.0023(9) 0.0009(9) -0.0007(10) C4 0.0217(18) 0.0250(18) 0.0146(17) -0.0011(13) 0.0045(14) -0.0029(14) C11 0.0176(17) 0.032(2) 0.0111(16) 0.0005(13) 0.0016(13) -0.0027(14) C8 0.0194(18) 0.0319(19) 0.0157(17) 0.0061(14) 0.0010(14) -0.0008(15) C10 0.0159(17) 0.0258(18) 0.0143(16) 0.0028(13) 0.0032(13) 0.0019(13) C9 0.0204(18) 0.0264(18) 0.0143(16) 0.0012(13) 0.0043(14) -0.0040(14) C5 0.0252(19) 0.0235(18) 0.0193(18) -0.0010(13) 0.0050(15) -0.0029(14) C3 0.0222(18) 0.0245(17) 0.0185(18) -0.0030(14) 0.0035(14) -0.0023(14) N2 0.0181(14) 0.0269(16) 0.0114(13) -0.0034(11) 0.0027(11) -0.0047(12) N1 0.0198(15) 0.0274(15) 0.0163(15) -0.0025(12) 0.0018(12) -0.0035(12) C12 0.0222(19) 0.0285(18) 0.0120(16) -0.0052(14) 0.0012(14) -0.0067(14) N3 0.0187(15) 0.0286(17) 0.0163(15) -0.0025(11) 0.0053(12) -0.0022(12) N4 0.0200(16) 0.0334(19) 0.0134(14) -0.0020(12) 0.0024(12) -0.0021(13) N5 0.042(2) 0.0310(18) 0.0307(18) 0.0021(14) 0.0149(16) -0.0076(15) O3 0.0150(12) 0.0225(12) 0.0133(11) -0.0018(9) 0.0030(9) 0.0008(9) O6 0.0248(14) 0.0380(15) 0.0279(15) -0.0068(11) 0.0052(12) -0.0038(11) O2 0.0180(12) 0.0257(13) 0.0108(11) -0.0015(9) 0.0006(9) 0.0001(10) C13 0.0215(18) 0.0288(19) 0.0111(16) -0.0028(13) 0.0014(13) -0.0030(14) C15 0.022(2) 0.028(2) 0.041(2) -0.0068(17) 0.0073(18) -0.0038(15) C16 0.021(2) 0.051(3) 0.046(3) -0.008(2) 0.0074(19) 0.0005(18) C6 0.026(2) 0.0257(18) 0.0192(18) 0.0037(14) 0.0057(15) 0.0025(15) C7 0.040(2) 0.031(2) 0.027(2) 0.0020(16) -0.0020(18) 0.0069(18) C2 0.029(2) 0.0289(19) 0.0171(18) -0.0058(14) -0.0016(15) 0.0009(15) C1 0.027(2) 0.038(2) 0.029(2) -0.0062(16) -0.0032(16) -0.0095(17) C14 0.0215(18) 0.0273(19) 0.0199(18) 0.0008(14) 0.0057(14) 0.0018(14) O1 0.0317(16) 0.0412(17) 0.0371(17) -0.0045(13) -0.0117(13) -0.0069(13) O5 0.0233(14) 0.0375(16) 0.0428(17) 0.0107(12) 0.0102(13) 0.0040(11) C17 0.054(4) 0.101(5) 0.042(3) -0.006(3) -0.007(3) 0.025(3) O8 0.038(2) 0.051(2) 0.067(3) -0.0201(18) 0.0093(18) 0.0021(16) _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 O7 C17 1.290(7) . ? O7 H7 0.8400 . ? Co1 N2 1.874(3) . ? Co1 O2 1.885(2) . ? Co1 O4 1.920(2) . ? Co1 N3 1.933(3) . ? Co1 O3 1.947(2) 3_666 ? Co1 O3 1.952(2) . ? Co1 Co1 2.9971(9) 3_666 ? Co2 O4 2.017(2) . ? Co2 O2 2.030(2) 3_666 ? Co2 N1 2.047(3) . ? Co2 O5 2.152(3) . ? Co2 O6 2.156(3) . ? Co2 O3 2.180(2) 3_666 ? O4 C10 1.330(4) . ? C4 C5 1.404(5) . ? C4 C10 1.422(5) . ? C4 C3 1.464(5) . ? C11 N2 1.274(5) . ? C11 C9 1.461(5) . ? C11 H11 0.9500 . ? C8 C6 1.388(5) . ? C8 C9 1.390(5) . ? C8 H8 0.9500 . ? C10 C9 1.414(5) . ? C5 C6 1.385(5) . ? C5 H5 0.9500 . ? C3 N1 1.287(5) . ? C3 H3 0.9500 . ? N2 C12 1.479(4) . ? N1 C2 1.481(4) . ? C12 C13 1.522(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N3 N4 1.210(4) . ? N4 N5 1.154(4) . ? O3 C14 1.441(4) . ? O3 Co1 1.947(2) 3_666 ? O3 Co2 2.180(2) 3_666 ? O6 C15 1.255(5) . ? O2 C13 1.424(4) . ? O2 Co2 2.030(2) 3_666 ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 O5 1.261(5) . ? C15 C16 1.504(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C6 C7 1.500(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C2 C1 1.527(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C1 O1 1.430(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O1 H1 0.99(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O8 H1 1.70(6) . ? O8 H8A 0.88(7) . ? O8 H8B 0.93(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 C17 O7 H7 109.5 . . ? N2 Co1 O2 85.75(11) . . ? N2 Co1 O4 93.85(11) . . ? O2 Co1 O4 176.71(10) . . ? N2 Co1 N3 89.89(12) . . ? O2 Co1 N3 91.67(11) . . ? O4 Co1 N3 91.59(11) . . ? N2 Co1 O3 177.01(11) . 3_666 ? O2 Co1 O3 95.56(9) . 3_666 ? O4 Co1 O3 84.68(10) . 3_666 ? N3 Co1 O3 92.75(11) . 3_666 ? N2 Co1 O3 97.95(11) . . ? O2 Co1 O3 83.70(10) . . ? O4 Co1 O3 93.12(10) . . ? N3 Co1 O3 170.55(11) . . ? O3 Co1 O3 79.55(10) 3_666 . ? N2 Co1 Co1 137.64(9) . 3_666 ? O2 Co1 Co1 89.52(7) . 3_666 ? O4 Co1 Co1 88.58(7) . 3_666 ? N3 Co1 Co1 132.36(9) . 3_666 ? O3 Co1 Co1 39.84(7) 3_666 3_666 ? O3 Co1 Co1 39.71(7) . 3_666 ? O4 Co2 O2 92.98(9) . 3_666 ? O4 Co2 N1 92.25(10) . . ? O2 Co2 N1 98.91(10) 3_666 . ? O4 Co2 O5 160.76(10) . . ? O2 Co2 O5 102.10(10) 3_666 . ? N1 Co2 O5 97.08(11) . . ? O4 Co2 O6 101.27(10) . . ? O2 Co2 O6 156.43(10) 3_666 . ? N1 Co2 O6 99.19(11) . . ? O5 Co2 O6 60.69(11) . . ? O4 Co2 O3 76.62(9) . 3_666 ? O2 Co2 O3 74.83(9) 3_666 3_666 ? N1 Co2 O3 166.72(10) . 3_666 ? O5 Co2 O3 95.71(10) . 3_666 ? O6 Co2 O3 90.19(9) . 3_666 ? C10 O4 Co1 128.2(2) . . ? C10 O4 Co2 129.0(2) . . ? Co1 O4 Co2 102.45(10) . . ? C5 C4 C10 119.2(3) . . ? C5 C4 C3 114.5(3) . . ? C10 C4 C3 126.3(3) . . ? N2 C11 C9 126.5(3) . . ? N2 C11 H11 116.7 . . ? C9 C11 H11 116.7 . . ? C6 C8 C9 122.7(3) . . ? C6 C8 H8 118.7 . . ? C9 C8 H8 118.7 . . ? O4 C10 C9 121.6(3) . . ? O4 C10 C4 121.2(3) . . ? C9 C10 C4 117.3(3) . . ? C8 C9 C10 120.8(3) . . ? C8 C9 C11 116.4(3) . . ? C10 C9 C11 122.8(3) . . ? C6 C5 C4 123.5(3) . . ? C6 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N1 C3 C4 128.3(3) . . ? N1 C3 H3 115.9 . . ? C4 C3 H3 115.9 . . ? C11 N2 C12 120.1(3) . . ? C11 N2 Co1 126.5(2) . . ? C12 N2 Co1 113.4(2) . . ? C3 N1 C2 115.0(3) . . ? C3 N1 Co2 122.9(2) . . ? C2 N1 Co2 122.1(2) . . ? N2 C12 C13 106.9(3) . . ? N2 C12 H12A 110.4 . . ? C13 C12 H12A 110.4 . . ? N2 C12 H12B 110.4 . . ? C13 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? N4 N3 Co1 117.8(2) . . ? N5 N4 N3 176.2(4) . . ? C14 O3 Co1 118.57(19) . 3_666 ? C14 O3 Co1 118.8(2) . . ? Co1 O3 Co1 100.45(10) 3_666 . ? C14 O3 Co2 121.31(19) . 3_666 ? Co1 O3 Co2 95.97(9) 3_666 3_666 ? Co1 O3 Co2 96.94(9) . 3_666 ? C15 O6 Co2 89.7(2) . . ? C13 O2 Co1 109.01(19) . . ? C13 O2 Co2 118.3(2) . 3_666 ? Co1 O2 Co2 104.52(10) . 3_666 ? O2 C13 C12 108.4(3) . . ? O2 C13 H13A 110.0 . . ? C12 C13 H13A 110.0 . . ? O2 C13 H13B 110.0 . . ? C12 C13 H13B 110.0 . . ? H13A C13 H13B 108.4 . . ? O6 C15 O5 119.8(4) . . ? O6 C15 C16 120.6(4) . . ? O5 C15 C16 119.6(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C5 C6 C8 116.4(3) . . ? C5 C6 C7 121.3(3) . . ? C8 C6 C7 122.3(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C2 C1 110.4(3) . . ? N1 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? N1 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.1 . . ? O1 C1 C2 109.9(3) . . ? O1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C1 O1 H1 105(3) . . ? C15 O5 Co2 89.7(2) . . ? O7 C17 H17A 109.5 . . ? O7 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O7 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? H1 O8 H8A 111(4) . . ? H1 O8 H8B 110(3) . . ? H8A O8 H8B 102(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.782 _refine_diff_density_min -0.819 _refine_diff_density_rms 0.109 #===END data_st075_0m _database_code_depnum_ccdc_archive 'CCDC 720884' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Co2IICo2III(HL)2(CH3O)2(N3)2(CH3OH)2)(5) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H46 Co4 N12 O16' _chemical_formula_weight 1066.51 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 P2(1)/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 7.468(3) _cell_length_b 20.480(8) _cell_length_c 13.609(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.424(7) _cell_angle_gamma 90.00 _cell_volume 2079.6(13) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 1267 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 18.23 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.703 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1092 _exptl_absorpt_coefficient_mu 1.651 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8523 _exptl_absorpt_correction_T_max 0.8932 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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_% ? _diffrn_reflns_number 16516 _diffrn_reflns_av_R_equivalents 0.1177 _diffrn_reflns_av_sigmaI/netI 0.0959 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.05 _reflns_number_total 3680 _reflns_number_gt 2208 _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^)+(0.1000P)^2^+0.8783P] 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 3680 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1112 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1642 _refine_ls_wR_factor_gt 0.1233 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.142 _refine_ls_shift/su_mean 0.005 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 0.07963(12) 1.03825(4) 0.91752(6) 0.0271(3) Uani 1 1 d . . . Co2 Co 0.01244(12) 0.89120(4) 0.88916(6) 0.0306(3) Uani 1 1 d . . . O1 O 0.1796(6) 1.0971(2) 1.0109(3) 0.0310(10) Uani 1 1 d . . . O2 O -0.0458(6) 0.9801(2) 0.8279(3) 0.0306(10) Uani 1 1 d . . . O3 O 0.0744(8) 0.7922(2) 0.9216(4) 0.0447(13) Uani 1 1 d . . . O4 O 0.2556(6) 0.8988(2) 0.8187(4) 0.0462(13) Uani 1 1 d . . . O5 O 0.0377(9) 0.2184(3) 0.5826(4) 0.0729(19) Uani 1 1 d . . . O6 O 0.1598(8) 0.2575(3) 0.4564(4) 0.0607(16) Uani 1 1 d . . . O7 O -0.0896(8) 0.2039(3) 0.4384(4) 0.0620(16) Uani 1 1 d . . . O8 O -0.1258(6) 1.0410(2) 1.0024(3) 0.0297(10) Uani 1 1 d . . . N1 N 0.2986(7) 1.0236(3) 0.8510(4) 0.0317(13) Uani 1 1 d . . . N2 N 0.3608(8) 1.0626(3) 0.7908(5) 0.0484(16) Uani 1 1 d . . . N3 N 0.4306(11) 1.0980(4) 0.7372(6) 0.083(3) Uani 1 1 d . . . N4 N 0.0296(7) 1.1118(3) 0.8391(4) 0.0315(12) Uani 1 1 d . . . N5 N -0.1229(8) 0.8453(3) 0.7779(4) 0.0395(15) Uani 1 1 d . . . N6 N 0.0352(10) 0.2258(3) 0.4924(5) 0.0496(17) Uani 1 1 d . . . C1 C 0.2441(9) 1.1543(3) 0.9606(5) 0.0381(17) Uani 1 1 d . . . H1A H 0.3584 1.1443 0.9295 0.046 Uiso 1 1 calc R . . H1B H 0.2654 1.1904 1.0080 0.046 Uiso 1 1 calc R . . C2 C 0.1042(10) 1.1740(3) 0.8834(5) 0.0417(18) Uani 1 1 d . . . H2A H 0.1585 1.2011 0.8323 0.050 Uiso 1 1 calc R . . H2B H 0.0080 1.1995 0.9134 0.050 Uiso 1 1 calc R . . C3 C -0.0405(9) 1.1118(3) 0.7510(5) 0.0356(16) Uani 1 1 d . . . H3 H -0.0502 1.1528 0.7186 0.043 Uiso 1 1 calc R . . C4 C -0.1055(9) 1.0558(3) 0.6967(5) 0.0331(16) Uani 1 1 d . . . C5 C -0.1040(9) 0.9915(3) 0.7349(5) 0.0313(15) Uani 1 1 d . . . C6 C -0.1662(9) 0.9405(4) 0.6715(5) 0.0344(16) Uani 1 1 d . . . C7 C -0.2227(9) 0.9558(4) 0.5753(5) 0.0404(18) Uani 1 1 d . . . H7 H -0.2631 0.9212 0.5336 0.048 Uiso 1 1 calc R . . C8 C -0.2234(10) 1.0186(4) 0.5368(5) 0.0426(18) Uani 1 1 d . . . C9 C -0.1648(9) 1.0684(4) 0.5988(5) 0.0417(18) Uani 1 1 d . . . H9 H -0.1645 1.1120 0.5750 0.050 Uiso 1 1 calc R . . C10 C -0.2833(11) 1.0330(4) 0.4313(5) 0.058(2) Uani 1 1 d . . . H10A H -0.3226 1.0785 0.4257 0.087 Uiso 1 1 calc R . . H10B H -0.3830 1.0040 0.4115 0.087 Uiso 1 1 calc R . . H10C H -0.1832 1.0256 0.3883 0.087 Uiso 1 1 calc R . . C11 C -0.1761(9) 0.8717(4) 0.6971(5) 0.0380(17) Uani 1 1 d . . . H11 H -0.2277 0.8434 0.6484 0.046 Uiso 1 1 calc R . . C12 C -0.1390(12) 0.7741(4) 0.7908(6) 0.051(2) Uani 1 1 d . . . H12A H -0.1608 0.7527 0.7262 0.062 Uiso 1 1 calc R . . H12B H -0.2408 0.7640 0.8325 0.062 Uiso 1 1 calc R . . C13 C 0.0337(12) 0.7494(4) 0.8390(6) 0.059(2) Uani 1 1 d . . . H13A H 0.0194 0.7039 0.8617 0.071 Uiso 1 1 calc R . . H13B H 0.1313 0.7508 0.7920 0.071 Uiso 1 1 calc R . . C14 C 0.4001(14) 0.8580(5) 0.7954(8) 0.097(4) Uani 1 1 d . . . H14A H 0.3903 0.8163 0.8300 0.145 Uiso 1 1 calc R . . H14B H 0.5133 0.8793 0.8156 0.145 Uiso 1 1 calc R . . H14C H 0.3971 0.8502 0.7243 0.145 Uiso 1 1 calc R . . C15 C -0.3013(9) 1.0503(3) 0.9554(5) 0.0360(17) Uani 1 1 d . . . H15A H -0.3919 1.0508 1.0054 0.054 Uiso 1 1 calc R . . H15B H -0.3267 1.0145 0.9091 0.054 Uiso 1 1 calc R . . H15C H -0.3041 1.0919 0.9197 0.054 Uiso 1 1 calc R . . H1 H 0.317(7) 0.960(2) 0.820(4) 0.012(14) Uiso 1 1 d . . . H2 H 0.170(12) 0.774(4) 0.949(7) 0.09(4) 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 Co1 0.0310(5) 0.0264(5) 0.0243(5) -0.0008(4) 0.0045(4) 0.0018(4) Co2 0.0379(5) 0.0265(5) 0.0280(5) -0.0030(4) 0.0061(4) 0.0008(4) O1 0.038(3) 0.026(2) 0.029(2) -0.0005(19) 0.003(2) -0.005(2) O2 0.033(3) 0.032(3) 0.027(2) -0.0042(19) 0.004(2) 0.000(2) O3 0.062(4) 0.027(3) 0.046(3) -0.008(2) 0.007(3) 0.004(3) O4 0.043(3) 0.049(3) 0.048(3) -0.005(3) 0.018(2) 0.007(3) O5 0.109(5) 0.071(4) 0.039(3) 0.010(3) 0.011(3) -0.030(4) O6 0.073(4) 0.063(4) 0.047(3) -0.012(3) 0.013(3) -0.032(3) O7 0.053(4) 0.056(4) 0.077(4) -0.022(3) -0.001(3) -0.001(3) O8 0.030(2) 0.029(2) 0.031(2) 0.0026(19) 0.003(2) 0.0025(19) N1 0.039(3) 0.031(3) 0.025(3) 0.006(2) 0.008(3) -0.004(3) N2 0.045(4) 0.047(4) 0.054(4) -0.008(3) 0.010(3) 0.004(3) N3 0.086(6) 0.079(6) 0.087(6) 0.033(5) 0.037(5) -0.007(5) N4 0.034(3) 0.034(3) 0.027(3) 0.002(3) 0.005(2) 0.004(3) N5 0.047(4) 0.038(3) 0.034(4) -0.010(3) 0.006(3) -0.005(3) N6 0.062(5) 0.030(4) 0.057(5) -0.010(3) 0.010(4) 0.005(3) C1 0.040(4) 0.038(4) 0.037(4) -0.006(3) 0.009(3) -0.007(3) C2 0.060(5) 0.028(4) 0.038(4) 0.001(3) 0.014(4) -0.007(4) C3 0.036(4) 0.034(4) 0.038(4) 0.008(3) 0.013(3) 0.007(3) C4 0.032(4) 0.039(4) 0.028(4) 0.003(3) 0.004(3) 0.004(3) C5 0.028(4) 0.039(4) 0.028(4) 0.005(3) 0.005(3) 0.003(3) C6 0.034(4) 0.051(4) 0.019(3) -0.005(3) 0.006(3) 0.000(3) C7 0.031(4) 0.055(5) 0.036(4) -0.017(4) 0.007(3) -0.005(3) C8 0.036(4) 0.063(5) 0.029(4) 0.007(4) 0.007(3) 0.000(4) C9 0.040(4) 0.052(5) 0.034(4) 0.010(4) 0.006(3) 0.007(4) C10 0.053(5) 0.089(7) 0.031(4) -0.002(4) -0.003(4) -0.005(5) C11 0.032(4) 0.052(5) 0.030(4) -0.015(3) 0.007(3) -0.005(3) C12 0.076(6) 0.038(4) 0.040(5) -0.010(4) 0.005(4) -0.010(4) C13 0.086(7) 0.037(5) 0.055(5) -0.017(4) 0.009(5) 0.004(5) C14 0.101(8) 0.065(7) 0.129(10) 0.019(6) 0.073(8) 0.023(6) C15 0.031(4) 0.039(4) 0.039(4) -0.002(3) 0.003(3) 0.003(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 Co1 N4 1.875(5) . ? Co1 O1 1.883(4) . ? Co1 O2 1.920(4) . ? Co1 N1 1.926(6) . ? Co1 O8 1.960(4) . ? Co1 O8 1.976(4) 3_577 ? Co2 N5 2.017(6) . ? Co2 O1 2.032(4) 3_577 ? Co2 O2 2.041(4) . ? Co2 O4 2.095(5) . ? Co2 O3 2.123(5) . ? Co2 O8 2.172(4) 3_577 ? O1 C1 1.449(8) . ? O1 Co2 2.032(4) 3_577 ? O2 C5 1.342(7) . ? O3 C13 1.447(9) . ? O3 H2 0.88(9) . ? O4 C14 1.411(9) . ? O4 H1 1.33(5) . ? O5 N6 1.237(8) . ? O6 N6 1.252(8) . ? O7 N6 1.245(8) . ? O8 C15 1.447(8) . ? O8 Co1 1.976(4) 3_577 ? O8 Co2 2.172(4) 3_577 ? N1 N2 1.247(8) . ? N1 H1 1.38(5) . ? N2 N3 1.167(9) . ? N4 C3 1.288(8) . ? N4 C2 1.505(8) . ? N5 C11 1.273(9) . ? N5 C12 1.474(9) . ? C1 C2 1.505(10) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.437(9) . ? C3 H3 0.9500 . ? C4 C9 1.409(9) . ? C4 C5 1.415(9) . ? C5 C6 1.419(9) . ? C6 C7 1.394(9) . ? C6 C11 1.456(10) . ? C7 C8 1.389(10) . ? C7 H7 0.9500 . ? C8 C9 1.383(10) . ? C8 C10 1.515(10) . ? C9 H9 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 0.9500 . ? C12 C13 1.509(11) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Co1 O1 86.2(2) . . ? N4 Co1 O2 93.3(2) . . ? O1 Co1 O2 174.09(19) . . ? N4 Co1 N1 90.6(2) . . ? O1 Co1 N1 95.5(2) . . ? O2 Co1 N1 90.3(2) . . ? N4 Co1 O8 99.8(2) . . ? O1 Co1 O8 83.22(18) . . ? O2 Co1 O8 91.09(18) . . ? N1 Co1 O8 169.4(2) . . ? N4 Co1 O8 178.0(2) . 3_577 ? O1 Co1 O8 95.69(18) . 3_577 ? O2 Co1 O8 84.81(18) . 3_577 ? N1 Co1 O8 90.0(2) . 3_577 ? O8 Co1 O8 79.68(19) . 3_577 ? N5 Co2 O1 102.2(2) . 3_577 ? N5 Co2 O2 91.0(2) . . ? O1 Co2 O2 91.40(17) 3_577 . ? N5 Co2 O4 96.2(2) . . ? O1 Co2 O4 161.40(18) 3_577 . ? O2 Co2 O4 85.48(18) . . ? N5 Co2 O3 79.0(2) . . ? O1 Co2 O3 97.27(19) 3_577 . ? O2 Co2 O3 167.93(19) . . ? O4 Co2 O3 88.9(2) . . ? N5 Co2 O8 167.6(2) . 3_577 ? O1 Co2 O8 74.69(16) 3_577 3_577 ? O2 Co2 O8 77.12(16) . 3_577 ? O4 Co2 O8 86.75(18) . 3_577 ? O3 Co2 O8 113.2(2) . 3_577 ? C1 O1 Co1 109.2(4) . . ? C1 O1 Co2 118.6(4) . 3_577 ? Co1 O1 Co2 104.8(2) . 3_577 ? C5 O2 Co1 128.4(4) . . ? C5 O2 Co2 126.6(4) . . ? Co1 O2 Co2 101.8(2) . . ? C13 O3 Co2 112.3(5) . . ? C13 O3 H2 102(6) . . ? Co2 O3 H2 132(6) . . ? C14 O4 Co2 138.2(5) . . ? C14 O4 H1 107(2) . . ? Co2 O4 H1 111(2) . . ? C15 O8 Co1 117.4(4) . . ? C15 O8 Co1 119.1(4) . 3_577 ? Co1 O8 Co1 100.32(18) . 3_577 ? C15 O8 Co2 122.4(4) . 3_577 ? Co1 O8 Co2 97.26(18) . 3_577 ? Co1 O8 Co2 95.56(18) 3_577 3_577 ? N2 N1 Co1 123.8(5) . . ? N2 N1 H1 111(2) . . ? Co1 N1 H1 113(2) . . ? N3 N2 N1 175.3(8) . . ? C3 N4 C2 120.2(6) . . ? C3 N4 Co1 126.3(5) . . ? C2 N4 Co1 113.0(4) . . ? C11 N5 C12 119.9(6) . . ? C11 N5 Co2 125.3(5) . . ? C12 N5 Co2 114.4(5) . . ? O5 N6 O7 121.5(7) . . ? O5 N6 O6 118.1(7) . . ? O7 N6 O6 120.3(7) . . ? O1 C1 C2 108.1(5) . . ? O1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? O1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? C1 C2 N4 106.7(5) . . ? C1 C2 H2A 110.4 . . ? N4 C2 H2A 110.4 . . ? C1 C2 H2B 110.4 . . ? N4 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? N4 C3 C4 126.5(6) . . ? N4 C3 H3 116.7 . . ? C4 C3 H3 116.7 . . ? C9 C4 C5 121.0(7) . . ? C9 C4 C3 115.2(6) . . ? C5 C4 C3 123.8(6) . . ? O2 C5 C4 120.4(6) . . ? O2 C5 C6 122.0(6) . . ? C4 C5 C6 117.6(6) . . ? C7 C6 C5 118.9(7) . . ? C7 C6 C11 115.2(6) . . ? C5 C6 C11 125.8(6) . . ? C8 C7 C6 123.9(7) . . ? C8 C7 H7 118.0 . . ? C6 C7 H7 118.0 . . ? C7 C8 C9 117.2(7) . . ? C7 C8 C10 122.2(7) . . ? C9 C8 C10 120.6(7) . . ? C8 C9 C4 121.3(7) . . ? C8 C9 H9 119.3 . . ? C4 C9 H9 119.3 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N5 C11 C6 127.0(6) . . ? N5 C11 H11 116.5 . . ? C6 C11 H11 116.5 . . ? N5 C12 C13 108.1(6) . . ? N5 C12 H12A 110.1 . . ? C13 C12 H12A 110.1 . . ? N5 C12 H12B 110.1 . . ? C13 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? O3 C13 C12 106.5(6) . . ? O3 C13 H13A 110.4 . . ? C12 C13 H13A 110.4 . . ? O3 C13 H13B 110.4 . . ? C12 C13 H13B 110.4 . . ? H13A C13 H13B 108.6 . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O8 C15 H15A 109.5 . . ? O8 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O8 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.385 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.096 #===END data_three _database_code_depnum_ccdc_archive 'CCDC 720885' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ni6(H2L)2(HL-1)2(H2O)2(N3)6)(ClO4)(6) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H31 Cl N12 Ni3 O12' _chemical_formula_weight 903.20 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' Cl Cl 0.1484 0.1585 '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 16.471(6) _cell_length_b 15.791(5) _cell_length_c 14.370(5) _cell_angle_alpha 90.00 _cell_angle_beta 111.084(5) _cell_angle_gamma 90.00 _cell_volume 3487(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2190 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 22.26 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 1.757 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6207 _exptl_absorpt_correction_T_max 0.8439 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_% ? _diffrn_reflns_number 27127 _diffrn_reflns_av_R_equivalents 0.1653 _diffrn_reflns_av_sigmaI/netI 0.1522 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6168 _reflns_number_gt 2503 _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^)+(0.1485P)^2^+2.0359P] 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 6168 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2104 _refine_ls_R_factor_gt 0.0814 _refine_ls_wR_factor_ref 0.2927 _refine_ls_wR_factor_gt 0.2004 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.45367(10) 0.41153(9) 0.44930(11) 0.0445(5) Uani 1 1 d . . . Ni2 Ni 0.24663(11) 0.40711(11) 0.35094(12) 0.0599(6) Uani 1 1 d . . . Ni3 Ni 0.34187(10) 0.57420(10) 0.43449(12) 0.0484(5) Uani 1 1 d . . . N1 N 0.4415(6) 0.5091(6) 0.5452(7) 0.045(2) Uani 1 1 d . . . N2 N 0.4288(7) 0.4830(7) 0.6213(10) 0.058(3) Uani 1 1 d . . . N3 N 0.4178(9) 0.4556(8) 0.6878(11) 0.084(4) Uani 1 1 d . . . N4 N 0.5515(6) 0.3581(7) 0.5667(7) 0.051(3) Uani 1 1 d . . . N5 N 0.5563(6) 0.2889(7) 0.6030(8) 0.047(3) Uani 1 1 d . . . N6 N 0.5655(8) 0.2256(8) 0.6416(9) 0.070(3) Uani 1 1 d . . . N7 N 0.3483(7) 0.3495(7) 0.4602(8) 0.058(3) Uani 1 1 d . . . N8 N 0.3384(7) 0.3069(7) 0.5231(9) 0.065(3) Uani 1 1 d . . . N9 N 0.3259(9) 0.2674(10) 0.5814(11) 0.101(5) Uani 1 1 d . . . N10 N 0.2658(7) 0.6389(7) 0.3147(9) 0.057(3) Uani 1 1 d . . . N11 N 0.4609(6) 0.3350(6) 0.3413(8) 0.048(3) Uani 1 1 d . . . N12 N 0.1511(8) 0.3486(9) 0.3790(10) 0.084(4) Uani 1 1 d . . . O1 O 0.3574(5) 0.4785(5) 0.3419(6) 0.047(2) Uani 1 1 d . . . O2 O 0.2449(5) 0.4990(5) 0.4437(7) 0.058(2) Uani 1 1 d . . . O3 O 0.3238(6) 0.6503(6) 0.5351(7) 0.063(3) Uani 1 1 d . . . O4 O 0.0840(8) 0.6120(8) 0.2420(9) 0.104(4) Uani 1 1 d . . . H4 H 0.0690 0.6392 0.1882 0.156 Uiso 1 1 calc R . . O5 O 0.1628(6) 0.4676(7) 0.2298(7) 0.079(3) Uani 1 1 d . . . H5 H 0.1254 0.4935 0.2460 0.118 Uiso 1 1 calc R . . O6 O 0.2369(7) 0.3040(6) 0.2570(7) 0.077(3) Uani 1 1 d . . . O7 O 0.3562(6) 0.1814(6) 0.3007(7) 0.070(3) Uani 1 1 d . . . H7 H 0.3590 0.2072 0.2508 0.104 Uiso 1 1 calc R . . C25 C 0.161(2) 0.395(2) 0.016(3) 0.31(3) Uani 1 1 d . . . H25A H 0.2107 0.4220 0.0061 0.466 Uiso 1 1 calc R . . H25B H 0.1150 0.3847 -0.0490 0.466 Uiso 1 1 calc R . . H25C H 0.1789 0.3414 0.0513 0.466 Uiso 1 1 calc R . . O9 O 0.9966(8) 0.2484(11) 0.0660(10) 0.149(6) Uani 1 1 d . . . O10 O 0.9373(12) 0.2507(14) -0.0976(13) 0.190(8) Uani 1 1 d . . . O11 O 0.8495(7) 0.2692(10) -0.0168(11) 0.150(6) Uani 1 1 d . . . O12 O 0.9414(13) 0.3684(11) -0.008(2) 0.303(18) Uani 1 1 d . . . Cl1 Cl 0.9345(3) 0.2866(4) -0.0102(4) 0.0979(15) Uani 1 1 d . . . C1 C 0.3607(8) 0.4961(8) 0.2520(10) 0.048(3) Uani 1 1 d . . . C2 C 0.3219(7) 0.5691(7) 0.2003(9) 0.047(3) Uani 1 1 d . . . C3 C 0.3251(8) 0.5816(9) 0.1052(9) 0.055(3) Uani 1 1 d . . . H3 H 0.3004 0.6319 0.0703 0.066 Uiso 1 1 calc R . . C4 C 0.3615(9) 0.5260(9) 0.0607(10) 0.060(4) Uani 1 1 d . . . C5 C 0.3987(8) 0.4566(9) 0.1128(9) 0.057(3) Uani 1 1 d . . . H5A H 0.4261 0.4171 0.0838 0.068 Uiso 1 1 calc R . . C6 C 0.3982(8) 0.4407(8) 0.2069(9) 0.050(3) Uani 1 1 d . . . C7 C 0.2722(8) 0.6303(8) 0.2298(10) 0.055(3) Uani 1 1 d . . . H7A H 0.2399 0.6693 0.1798 0.066 Uiso 1 1 calc R . . C8 C 0.3593(10) 0.5432(9) -0.0433(10) 0.077(5) Uani 1 1 d . . . H8A H 0.3188 0.5897 -0.0727 0.116 Uiso 1 1 calc R . . H8B H 0.3399 0.4922 -0.0842 0.116 Uiso 1 1 calc R . . H8C H 0.4177 0.5588 -0.0406 0.116 Uiso 1 1 calc R . . C9 C 0.4399(8) 0.3591(8) 0.2520(10) 0.051(3) Uani 1 1 d . . . H9 H 0.4521 0.3206 0.2080 0.061 Uiso 1 1 calc R . . C10 C 0.2064(8) 0.5016(9) 0.5107(11) 0.056(3) Uani 1 1 d . . . C11 C 0.1447(9) 0.4390(10) 0.5124(11) 0.070(4) Uani 1 1 d . . . C12 C 0.1051(10) 0.4429(11) 0.5809(14) 0.080(5) Uani 1 1 d . . . H12 H 0.0636 0.4006 0.5793 0.096 Uiso 1 1 calc R . . C13 C 0.1225(12) 0.5048(13) 0.6518(17) 0.096(6) Uani 1 1 d . . . C14 C 0.1821(11) 0.5644(10) 0.6514(12) 0.082(5) Uani 1 1 d . . . H14 H 0.1957 0.6081 0.7002 0.099 Uiso 1 1 calc R . . C15 C 0.2240(9) 0.5642(9) 0.5824(11) 0.063(4) Uani 1 1 d . . . C16 C 0.2830(9) 0.6336(10) 0.5918(13) 0.077(5) Uani 1 1 d . . . H16 H 0.2921 0.6708 0.6466 0.092 Uiso 1 1 calc R . . C17 C 0.0757(13) 0.5060(14) 0.7237(17) 0.141(8) Uani 1 1 d . . . H17A H 0.0144 0.5200 0.6882 0.211 Uiso 1 1 calc R . . H17B H 0.1022 0.5486 0.7754 0.211 Uiso 1 1 calc R . . H17C H 0.0801 0.4501 0.7548 0.211 Uiso 1 1 calc R . . C18 C 0.1197(10) 0.3686(11) 0.4436(12) 0.080(5) Uani 1 1 d . . . H18 H 0.0743 0.3335 0.4478 0.096 Uiso 1 1 calc R . . C19 C 0.1192(19) 0.2763(17) 0.3129(18) 0.175(14) Uani 1 1 d . . . H19 H 0.0650 0.2500 0.3041 0.209 Uiso 1 1 calc R . . C20 C 0.1687(11) 0.2504(15) 0.268(2) 0.161(13) Uani 1 1 d . . . H20 H 0.1607 0.1949 0.2400 0.194 Uiso 1 1 calc R . . C21 C 0.4974(8) 0.2484(7) 0.3592(9) 0.048(3) Uani 1 1 d . . . H21A H 0.5529 0.2490 0.4171 0.058 Uiso 1 1 calc R . . H21B H 0.5100 0.2292 0.3002 0.058 Uiso 1 1 calc R . . C22 C 0.4358(9) 0.1875(8) 0.3790(10) 0.060(4) Uani 1 1 d . . . H22A H 0.4631 0.1308 0.3922 0.072 Uiso 1 1 calc R . . H22B H 0.4255 0.2058 0.4398 0.072 Uiso 1 1 calc R . . C23 C 0.2062(8) 0.7056(8) 0.3243(11) 0.065(4) Uani 1 1 d . . . H23A H 0.1941 0.7464 0.2687 0.078 Uiso 1 1 calc R . . H23B H 0.2342 0.7368 0.3876 0.078 Uiso 1 1 calc R . . C24 C 0.1226(11) 0.6679(12) 0.3230(13) 0.102(6) Uani 1 1 d . . . H24A H 0.1335 0.6368 0.3862 0.122 Uiso 1 1 calc R . . H24B H 0.0811 0.7142 0.3198 0.122 Uiso 1 1 calc R . . O8 O 0.128(3) 0.451(2) 0.074(3) 0.39(2) Uani 1 1 d . . . H8 H 0.1016 0.4917 0.0387 0.578 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0469(9) 0.0396(9) 0.0377(9) 0.0005(7) 0.0039(7) -0.0043(7) Ni2 0.0563(11) 0.0570(11) 0.0524(11) 0.0039(9) 0.0027(9) -0.0102(9) Ni3 0.0471(9) 0.0443(9) 0.0457(10) 0.0027(7) 0.0068(7) -0.0022(7) N1 0.053(6) 0.039(6) 0.035(6) 0.006(5) 0.007(5) -0.010(5) N2 0.059(7) 0.043(7) 0.060(8) 0.001(6) 0.008(7) -0.010(5) N3 0.091(10) 0.071(9) 0.086(10) 0.013(8) 0.028(9) -0.008(7) N4 0.057(6) 0.041(6) 0.052(7) -0.005(5) 0.015(5) -0.001(5) N5 0.047(6) 0.041(7) 0.052(7) 0.001(5) 0.016(5) 0.000(5) N6 0.077(8) 0.054(7) 0.070(8) 0.016(6) 0.016(7) 0.005(6) N7 0.070(7) 0.048(7) 0.038(6) -0.005(5) -0.004(6) -0.014(6) N8 0.056(7) 0.062(8) 0.061(8) 0.025(7) 0.002(6) 0.000(6) N9 0.083(9) 0.120(12) 0.092(11) 0.059(10) 0.024(8) -0.009(9) N10 0.049(6) 0.047(6) 0.064(8) 0.000(6) 0.007(6) -0.006(5) N11 0.052(6) 0.038(6) 0.048(7) -0.001(5) 0.010(5) -0.004(5) N12 0.076(9) 0.096(10) 0.063(9) 0.006(8) 0.003(7) -0.040(8) O1 0.056(5) 0.040(5) 0.037(5) -0.001(4) 0.006(4) -0.004(4) O2 0.054(5) 0.054(5) 0.059(6) 0.008(4) 0.011(5) 0.003(4) O3 0.057(6) 0.057(6) 0.073(7) -0.003(5) 0.020(5) -0.009(5) O4 0.067(7) 0.125(10) 0.095(9) 0.005(8) -0.001(7) -0.003(7) O5 0.065(7) 0.093(8) 0.061(6) 0.018(6) 0.002(5) -0.009(6) O6 0.095(7) 0.055(6) 0.065(6) -0.008(5) 0.010(6) -0.007(6) O7 0.075(6) 0.052(6) 0.074(7) -0.011(5) 0.017(6) -0.011(5) C25 0.16(3) 0.26(4) 0.46(7) -0.25(5) 0.05(4) -0.06(3) O9 0.087(9) 0.226(17) 0.099(10) 0.022(11) -0.008(8) 0.041(10) O10 0.191(17) 0.25(2) 0.119(14) 0.046(14) 0.041(13) 0.107(16) O11 0.062(8) 0.213(16) 0.156(13) 0.101(12) 0.015(8) 0.003(9) O12 0.21(2) 0.068(11) 0.47(4) 0.001(17) -0.07(2) -0.005(12) Cl1 0.068(3) 0.110(4) 0.095(4) 0.009(3) 0.006(3) 0.008(3) C1 0.047(7) 0.038(7) 0.052(8) -0.009(6) 0.009(7) 0.000(6) C2 0.041(7) 0.045(7) 0.041(7) 0.009(6) -0.001(6) 0.001(6) C3 0.047(7) 0.055(8) 0.049(8) 0.009(7) 0.001(6) -0.010(7) C4 0.061(9) 0.058(9) 0.051(9) 0.015(7) 0.010(7) 0.003(7) C5 0.057(8) 0.071(9) 0.040(8) -0.005(7) 0.014(7) -0.008(7) C6 0.046(7) 0.044(7) 0.048(8) 0.007(6) 0.003(6) -0.013(6) C7 0.042(7) 0.057(8) 0.051(9) 0.011(7) -0.001(7) -0.003(6) C8 0.104(12) 0.082(11) 0.046(9) 0.007(8) 0.028(9) -0.008(9) C9 0.053(8) 0.049(8) 0.051(8) -0.003(6) 0.017(7) 0.000(6) C10 0.045(8) 0.062(9) 0.053(9) 0.006(7) 0.008(7) 0.007(7) C11 0.059(9) 0.082(11) 0.059(10) 0.005(8) 0.007(8) -0.008(8) C12 0.069(11) 0.076(12) 0.100(14) 0.035(11) 0.035(11) 0.012(9) C13 0.085(13) 0.082(13) 0.129(18) 0.041(13) 0.049(13) 0.025(11) C14 0.101(13) 0.067(11) 0.075(11) 0.007(9) 0.027(10) 0.018(10) C15 0.069(9) 0.064(9) 0.065(10) 0.002(8) 0.034(8) 0.016(8) C16 0.054(9) 0.069(11) 0.090(12) 0.010(9) 0.003(9) 0.008(8) C17 0.140(18) 0.16(2) 0.17(2) 0.020(18) 0.113(18) 0.029(17) C18 0.077(11) 0.094(12) 0.054(10) 0.024(9) 0.006(9) -0.026(10) C19 0.21(3) 0.19(3) 0.15(2) -0.09(2) 0.10(2) -0.17(3) C20 0.054(11) 0.122(18) 0.31(4) -0.09(2) 0.061(17) -0.045(12) C21 0.053(7) 0.036(7) 0.040(7) -0.007(5) -0.003(6) 0.006(6) C22 0.077(10) 0.032(7) 0.059(9) -0.003(6) 0.010(8) 0.003(7) C23 0.046(8) 0.058(9) 0.085(11) 0.004(8) 0.016(8) 0.005(7) C24 0.097(14) 0.105(14) 0.083(13) 0.002(11) 0.007(11) 0.037(12) O8 0.43(5) 0.21(3) 0.50(6) -0.01(3) 0.15(5) 0.11(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 N11 2.005(10) . ? Ni1 N7 2.048(11) . ? Ni1 N4 2.049(10) . ? Ni1 O1 2.063(8) . ? Ni1 N1 2.113(9) 3_666 ? Ni1 N1 2.124(10) . ? Ni2 O2 1.977(9) . ? Ni2 N12 1.987(13) . ? Ni2 O5 2.029(9) . ? Ni2 N7 2.051(10) . ? Ni2 O6 2.084(9) . ? Ni2 O1 2.188(8) . ? Ni3 O3 1.983(10) . ? Ni3 N10 2.007(11) . ? Ni3 O2 2.032(9) . ? Ni3 N4 2.062(10) 3_666 ? Ni3 O1 2.089(8) . ? Ni3 N1 2.098(9) . ? N1 N2 1.255(15) . ? N1 Ni1 2.113(9) 3_666 ? N2 N3 1.122(15) . ? N4 N5 1.200(13) . ? N4 Ni3 2.062(10) 3_666 ? N5 N6 1.128(13) . ? N7 N8 1.184(14) . ? N8 N9 1.120(15) . ? N10 C7 1.269(15) . ? N10 C23 1.481(16) . ? N11 C9 1.261(14) . ? N11 C21 1.479(14) . ? N12 C18 1.254(19) . ? N12 C19 1.46(2) . ? O1 C1 1.341(14) . ? O2 C10 1.330(15) . ? O3 C16 1.256(17) . ? O4 C24 1.417(18) . ? O4 H4 0.8400 . ? O5 H5 0.8400 . ? O6 C20 1.46(2) . ? O7 C22 1.390(14) . ? O7 H7 0.8400 . ? C25 O8 1.45(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O9 Cl1 1.343(12) . ? O10 Cl1 1.394(18) . ? O11 Cl1 1.396(12) . ? O12 Cl1 1.295(17) . ? C1 C6 1.362(17) . ? C1 C2 1.395(16) . ? C2 C3 1.401(17) . ? C2 C7 1.425(18) . ? C3 C4 1.347(18) . ? C3 H3 0.9500 . ? C4 C5 1.344(17) . ? C4 C8 1.506(17) . ? C5 C6 1.378(17) . ? C5 H5A 0.9500 . ? C6 C9 1.494(17) . ? C7 H7A 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9 0.9500 . ? C10 C15 1.381(18) . ? C10 C11 1.425(18) . ? C11 C12 1.36(2) . ? C11 C18 1.45(2) . ? C12 C13 1.37(2) . ? C12 H12 0.9500 . ? C13 C14 1.36(2) . ? C13 C17 1.50(2) . ? C14 C15 1.40(2) . ? C14 H14 0.9500 . ? C15 C16 1.44(2) . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18 0.9500 . ? C19 C20 1.28(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.497(16) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.49(2) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? O8 H8 0.8400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Ni1 N7 93.4(4) . . ? N11 Ni1 N4 98.1(4) . . ? N7 Ni1 N4 100.2(4) . . ? N11 Ni1 O1 88.5(4) . . ? N7 Ni1 O1 81.8(4) . . ? N4 Ni1 O1 172.9(4) . . ? N11 Ni1 N1 96.4(4) . 3_666 ? N7 Ni1 N1 170.1(4) . 3_666 ? N4 Ni1 N1 79.8(4) . 3_666 ? O1 Ni1 N1 97.0(3) . 3_666 ? N11 Ni1 N1 170.2(4) . . ? N7 Ni1 N1 91.0(4) . . ? N4 Ni1 N1 89.7(4) . . ? O1 Ni1 N1 83.5(3) . . ? N1 Ni1 N1 79.2(4) 3_666 . ? O2 Ni2 N12 90.0(5) . . ? O2 Ni2 O5 93.6(4) . . ? N12 Ni2 O5 92.8(5) . . ? O2 Ni2 N7 90.8(4) . . ? N12 Ni2 N7 97.2(5) . . ? O5 Ni2 N7 169.0(4) . . ? O2 Ni2 O6 173.5(4) . . ? N12 Ni2 O6 83.5(5) . . ? O5 Ni2 O6 86.7(4) . . ? N7 Ni2 O6 90.1(4) . . ? O2 Ni2 O1 82.9(3) . . ? N12 Ni2 O1 171.8(5) . . ? O5 Ni2 O1 91.8(4) . . ? N7 Ni2 O1 78.8(4) . . ? O6 Ni2 O1 103.6(4) . . ? O3 Ni3 N10 96.1(4) . . ? O3 Ni3 O2 88.8(4) . . ? N10 Ni3 O2 95.2(4) . . ? O3 Ni3 N4 92.5(4) . 3_666 ? N10 Ni3 N4 90.0(4) . 3_666 ? O2 Ni3 N4 174.5(4) . 3_666 ? O3 Ni3 O1 170.9(4) . . ? N10 Ni3 O1 90.2(4) . . ? O2 Ni3 O1 84.1(3) . . ? N4 Ni3 O1 94.0(4) 3_666 . ? O3 Ni3 N1 91.5(4) . . ? N10 Ni3 N1 167.6(4) . . ? O2 Ni3 N1 94.7(3) . . ? N4 Ni3 N1 79.9(4) 3_666 . ? O1 Ni3 N1 83.5(3) . . ? N2 N1 Ni3 119.5(8) . . ? N2 N1 Ni1 123.5(8) . 3_666 ? Ni3 N1 Ni1 98.2(4) . 3_666 ? N2 N1 Ni1 114.3(7) . . ? Ni3 N1 Ni1 95.4(4) . . ? Ni1 N1 Ni1 100.8(4) 3_666 . ? N3 N2 N1 176.5(14) . . ? N5 N4 Ni1 129.9(8) . . ? N5 N4 Ni3 123.5(8) . 3_666 ? Ni1 N4 Ni3 101.5(5) . 3_666 ? N6 N5 N4 175.7(13) . . ? N8 N7 Ni1 133.1(9) . . ? N8 N7 Ni2 122.5(10) . . ? Ni1 N7 Ni2 102.1(5) . . ? N9 N8 N7 177.5(15) . . ? C7 N10 C23 117.0(12) . . ? C7 N10 Ni3 121.9(9) . . ? C23 N10 Ni3 120.8(9) . . ? C9 N11 C21 113.7(11) . . ? C9 N11 Ni1 122.3(9) . . ? C21 N11 Ni1 123.8(8) . . ? C18 N12 C19 122.1(16) . . ? C18 N12 Ni2 126.9(12) . . ? C19 N12 Ni2 111.0(13) . . ? C1 O1 Ni1 122.7(7) . . ? C1 O1 Ni3 121.3(7) . . ? Ni1 O1 Ni3 97.5(3) . . ? C1 O1 Ni2 119.2(7) . . ? Ni1 O1 Ni2 97.1(3) . . ? Ni3 O1 Ni2 92.2(3) . . ? C10 O2 Ni2 129.6(8) . . ? C10 O2 Ni3 128.3(8) . . ? Ni2 O2 Ni3 100.5(4) . . ? C16 O3 Ni3 127.0(10) . . ? C24 O4 H4 109.5 . . ? Ni2 O5 H5 109.5 . . ? C20 O6 Ni2 105.6(12) . . ? C22 O7 H7 109.5 . . ? O8 C25 H25A 109.5 . . ? O8 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O8 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O12 Cl1 O9 113.0(13) . . ? O12 Cl1 O10 113.5(17) . . ? O9 Cl1 O10 106.8(10) . . ? O12 Cl1 O11 105.9(13) . . ? O9 Cl1 O11 114.7(10) . . ? O10 Cl1 O11 102.5(12) . . ? O1 C1 C6 120.5(11) . . ? O1 C1 C2 121.0(11) . . ? C6 C1 C2 118.4(12) . . ? C1 C2 C3 117.7(12) . . ? C1 C2 C7 127.1(12) . . ? C3 C2 C7 115.0(11) . . ? C4 C3 C2 123.4(13) . . ? C4 C3 H3 118.3 . . ? C2 C3 H3 118.3 . . ? C5 C4 C3 117.3(13) . . ? C5 C4 C8 122.9(14) . . ? C3 C4 C8 119.8(13) . . ? C4 C5 C6 122.2(14) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C1 C6 C5 120.9(12) . . ? C1 C6 C9 124.3(12) . . ? C5 C6 C9 114.7(13) . . ? N10 C7 C2 127.9(12) . . ? N10 C7 H7A 116.1 . . ? C2 C7 H7A 116.1 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N11 C9 C6 128.1(12) . . ? N11 C9 H9 116.0 . . ? C6 C9 H9 116.0 . . ? O2 C10 C15 122.4(13) . . ? O2 C10 C11 121.3(13) . . ? C15 C10 C11 116.3(14) . . ? C12 C11 C10 120.7(15) . . ? C12 C11 C18 115.9(16) . . ? C10 C11 C18 123.4(15) . . ? C11 C12 C13 123.0(17) . . ? C11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C12 C13 C14 116.8(18) . . ? C12 C13 C17 120(2) . . ? C14 C13 C17 123(2) . . ? C13 C14 C15 122.8(17) . . ? C13 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C10 C15 C14 120.5(15) . . ? C10 C15 C16 124.6(14) . . ? C14 C15 C16 114.9(15) . . ? O3 C16 C15 126.8(16) . . ? O3 C16 H16 116.6 . . ? C15 C16 H16 116.6 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N12 C18 C11 127.5(16) . . ? N12 C18 H18 116.3 . . ? C11 C18 H18 116.3 . . ? C20 C19 N12 116(2) . . ? C20 C19 H19 122.1 . . ? N12 C19 H19 122.1 . . ? C19 C20 O6 122(2) . . ? C19 C20 H20 119.2 . . ? O6 C20 H20 119.2 . . ? N11 C21 C22 111.5(10) . . ? N11 C21 H21A 109.3 . . ? C22 C21 H21A 109.3 . . ? N11 C21 H21B 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? O7 C22 C21 113.3(10) . . ? O7 C22 H22A 108.9 . . ? C21 C22 H22A 108.9 . . ? O7 C22 H22B 108.9 . . ? C21 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? N10 C23 C24 110.8(12) . . ? N10 C23 H23A 109.5 . . ? C24 C23 H23A 109.5 . . ? N10 C23 H23B 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? O4 C24 C23 113.5(15) . . ? O4 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? O4 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C25 O8 H8 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.638 _refine_diff_density_min -1.104 _refine_diff_density_rms 0.148 #===END data_st061 _database_code_depnum_ccdc_archive 'CCDC 720886' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Ni6(H2L)2(HL-1)2(CH3OH)2(N3)6)(BF4)2 (7)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H66 B2 F8 N24 Ni6 O14' _chemical_formula_weight 1753.15 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' B B 0.0013 0.0007 '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' 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 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 16.476(3) _cell_length_b 16.049(3) _cell_length_c 14.198(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.149(3) _cell_angle_gamma 90.00 _cell_volume 3501.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2067 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 19.31 _exptl_crystal_description irregular _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 1.679 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.5911 _exptl_absorpt_correction_T_max 0.6694 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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_% ? _diffrn_reflns_number 27599 _diffrn_reflns_av_R_equivalents 0.1302 _diffrn_reflns_av_sigmaI/netI 0.1164 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6207 _reflns_number_gt 2918 _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^)+(0.1000P)^2^+0.4532P] 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 6207 _refine_ls_number_parameters 474 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1617 _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.2126 _refine_ls_wR_factor_gt 0.1521 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.45311(7) 0.41173(6) 0.44939(8) 0.0352(3) Uani 1 1 d . . . Ni2 Ni 0.24452(8) 0.40676(8) 0.34941(9) 0.0495(4) Uani 1 1 d . . . Ni3 Ni 0.34049(7) 0.57335(7) 0.43252(8) 0.0383(3) Uani 1 1 d . . . O1 O 0.2428(4) 0.5003(4) 0.4426(5) 0.0507(16) Uani 1 1 d . . . O2 O 0.3550(3) 0.4784(3) 0.3399(4) 0.0383(14) Uani 1 1 d . . . O3 O 0.3229(4) 0.6503(4) 0.5356(5) 0.0525(17) Uani 1 1 d . . . O4 O 0.3573(5) 0.1815(4) 0.3034(6) 0.067(2) Uani 1 1 d . . . H4 H 0.3325 0.2281 0.2912 0.100 Uiso 1 1 calc R . . O5 O 0.2345(4) 0.3017(4) 0.2572(5) 0.0625(19) Uani 1 1 d . . . O6 O 0.1610(4) 0.4685(4) 0.2265(5) 0.067(2) Uani 1 1 d . . . O7 O 0.0813(5) 0.6091(5) 0.2360(6) 0.078(2) Uani 1 1 d . . . H7 H 0.0637 0.6368 0.1822 0.117 Uiso 1 1 calc R . . N1 N 0.3462(5) 0.3515(4) 0.4608(6) 0.0451(19) Uani 1 1 d . . . N2 N 0.3370(5) 0.3078(5) 0.5256(7) 0.053(2) Uani 1 1 d . . . N3 N 0.3248(6) 0.2669(7) 0.5851(8) 0.093(4) Uani 1 1 d . . . N4 N 0.4410(4) 0.5091(4) 0.5488(5) 0.0323(16) Uani 1 1 d . . . N5 N 0.4291(5) 0.4825(4) 0.6240(6) 0.0427(19) Uani 1 1 d . . . N6 N 0.4175(6) 0.4567(6) 0.6914(7) 0.065(3) Uani 1 1 d . . . N7 N 0.5529(4) 0.3603(4) 0.5694(5) 0.0383(17) Uani 1 1 d . . . N8 N 0.5597(4) 0.2910(5) 0.6060(5) 0.0398(18) Uani 1 1 d . . . N9 N 0.5701(5) 0.2272(5) 0.6429(7) 0.062(2) Uani 1 1 d . . . N10 N 0.1495(6) 0.3496(5) 0.3782(7) 0.070(3) Uani 1 1 d . . . N11 N 0.4607(5) 0.3358(4) 0.3385(6) 0.0431(18) Uani 1 1 d . . . N12 N 0.2634(5) 0.6364(4) 0.3108(6) 0.0437(19) Uani 1 1 d . . . B1 B 0.9370(11) 0.2807(12) 0.9918(13) 0.085(5) Uani 1 1 d . . . F1 F 0.9383(8) 0.2451(9) 0.9020(9) 0.207(6) Uani 1 1 d . . . F2 F 0.8541(5) 0.2597(6) 0.9781(7) 0.146(4) Uani 1 1 d . . . F3 F 0.9965(5) 0.2384(5) 1.0644(5) 0.108(3) Uani 1 1 d . . . F4 F 0.9425(8) 0.3564(6) 0.9870(12) 0.288(11) Uani 1 1 d . . . C1 C 0.2059(6) 0.5030(6) 0.5119(8) 0.050(2) Uani 1 1 d . . . C2 C 0.1450(6) 0.4404(6) 0.5149(8) 0.058(3) Uani 1 1 d . . . C3 C 0.1043(7) 0.4449(7) 0.5858(9) 0.065(3) Uani 1 1 d . . . H3 H 0.0613 0.4047 0.5835 0.078 Uiso 1 1 calc R . . C4 C 0.1247(8) 0.5059(8) 0.6588(9) 0.074(3) Uani 1 1 d . . . C5 C 0.1835(7) 0.5645(6) 0.6567(8) 0.062(3) Uani 1 1 d . . . H5 H 0.1973 0.6077 0.7057 0.075 Uiso 1 1 calc R . . C6 C 0.2251(6) 0.5648(6) 0.5858(8) 0.055(3) Uani 1 1 d . . . C7 C 0.0815(9) 0.5085(9) 0.7364(11) 0.109(5) Uani 1 1 d . . . H7A H 0.0866 0.4538 0.7688 0.164 Uiso 1 1 calc R . . H7B H 0.0199 0.5227 0.7032 0.164 Uiso 1 1 calc R . . H7C H 0.1101 0.5506 0.7877 0.164 Uiso 1 1 calc R . . C8 C 0.1168(7) 0.3703(7) 0.4460(9) 0.072(3) Uani 1 1 d . . . H8 H 0.0709 0.3369 0.4507 0.086 Uiso 1 1 calc R . . C9 C 0.2820(7) 0.6333(6) 0.5928(8) 0.058(3) Uani 1 1 d . . . H9 H 0.2901 0.6707 0.6473 0.070 Uiso 1 1 calc R . . C10 C 0.1159(12) 0.2780(10) 0.3127(12) 0.130(7) Uani 1 1 d . . . H10A H 0.1020 0.2333 0.3525 0.156 Uiso 1 1 calc R . . H10B H 0.0610 0.2942 0.2582 0.156 Uiso 1 1 calc R . . C11 C 0.1710(10) 0.2472(9) 0.2704(17) 0.153(9) Uani 1 1 d . . . H11A H 0.1355 0.2246 0.2032 0.183 Uiso 1 1 calc R . . H11B H 0.2023 0.1996 0.3121 0.183 Uiso 1 1 calc R . . C12 C 0.3584(6) 0.4946(5) 0.2475(6) 0.040(2) Uani 1 1 d . . . C13 C 0.3971(6) 0.4384(5) 0.2020(7) 0.044(2) Uani 1 1 d . . . C14 C 0.3985(6) 0.4534(6) 0.1053(7) 0.048(2) Uani 1 1 d . . . H14 H 0.4263 0.4146 0.0765 0.058 Uiso 1 1 calc R . . C15 C 0.3602(7) 0.5233(6) 0.0512(7) 0.054(3) Uani 1 1 d . . . C16 C 0.3235(6) 0.5778(6) 0.0957(7) 0.052(3) Uani 1 1 d . . . H16 H 0.2982 0.6267 0.0593 0.062 Uiso 1 1 calc R . . C17 C 0.3199(5) 0.5671(5) 0.1935(6) 0.041(2) Uani 1 1 d . . . C18 C 0.3589(8) 0.5380(7) -0.0553(7) 0.074(3) Uani 1 1 d . . . H18A H 0.3001 0.5282 -0.1042 0.111 Uiso 1 1 calc R . . H18B H 0.3997 0.4997 -0.0690 0.111 Uiso 1 1 calc R . . H18C H 0.3761 0.5956 -0.0615 0.111 Uiso 1 1 calc R . . C19 C 0.4392(6) 0.3593(5) 0.2474(7) 0.042(2) Uani 1 1 d . . . H19 H 0.4518 0.3215 0.2030 0.051 Uiso 1 1 calc R . . C20 C 0.2698(6) 0.6278(5) 0.2250(7) 0.046(2) Uani 1 1 d . . . H20 H 0.2374 0.6663 0.1746 0.055 Uiso 1 1 calc R . . C21 C 0.4976(6) 0.2502(5) 0.3605(7) 0.045(2) Uani 1 1 d . . . H21A H 0.5110 0.2301 0.3018 0.054 Uiso 1 1 calc R . . H21B H 0.5529 0.2526 0.4192 0.054 Uiso 1 1 calc R . . C22 C 0.4387(6) 0.1898(5) 0.3822(7) 0.048(2) Uani 1 1 d . . . H22A H 0.4675 0.1346 0.3958 0.058 Uiso 1 1 calc R . . H22B H 0.4292 0.2075 0.4442 0.058 Uiso 1 1 calc R . . C23 C 0.2033(6) 0.7010(6) 0.3187(8) 0.059(3) Uani 1 1 d . . . H23A H 0.1906 0.7401 0.2612 0.070 Uiso 1 1 calc R . . H23B H 0.2310 0.7330 0.3818 0.070 Uiso 1 1 calc R . . C24 C 0.1195(7) 0.6633(7) 0.3185(9) 0.076(3) Uani 1 1 d . . . H24A H 0.1311 0.6320 0.3821 0.091 Uiso 1 1 calc R . . H24B H 0.0779 0.7085 0.3160 0.091 Uiso 1 1 calc R . . C25 C 0.1291(11) 0.4431(11) 0.1067(18) 0.191(11) Uani 1 1 d . . . H25A H 0.1350 0.4914 0.0674 0.287 Uiso 1 1 calc R . . H25B H 0.0680 0.4255 0.0830 0.287 Uiso 1 1 calc R . . H25C H 0.1651 0.3973 0.0981 0.287 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0362(6) 0.0348(6) 0.0282(6) 0.0009(5) 0.0038(5) -0.0035(5) Ni2 0.0447(7) 0.0510(8) 0.0431(8) 0.0003(6) 0.0044(6) -0.0085(6) Ni3 0.0355(6) 0.0383(6) 0.0354(6) 0.0021(5) 0.0061(5) -0.0014(5) O1 0.047(4) 0.056(4) 0.046(4) -0.004(3) 0.013(3) -0.013(3) O2 0.040(3) 0.034(3) 0.032(3) 0.000(3) 0.002(3) -0.004(3) O3 0.045(4) 0.053(4) 0.061(5) -0.004(3) 0.020(4) -0.008(3) O4 0.068(5) 0.051(4) 0.072(5) -0.010(4) 0.014(4) -0.006(4) O5 0.064(5) 0.053(4) 0.053(4) -0.009(3) 0.000(4) -0.010(4) O6 0.054(5) 0.081(5) 0.045(4) 0.000(4) -0.008(4) -0.008(4) O7 0.055(5) 0.091(6) 0.071(6) 0.016(5) 0.003(4) 0.001(4) N1 0.043(5) 0.040(4) 0.041(5) 0.002(4) 0.001(4) -0.006(4) N2 0.043(5) 0.058(5) 0.052(6) 0.013(5) 0.010(4) -0.001(4) N3 0.069(7) 0.119(9) 0.083(8) 0.057(7) 0.019(6) 0.000(6) N4 0.034(4) 0.032(4) 0.027(4) 0.007(3) 0.005(3) 0.001(3) N5 0.044(5) 0.037(4) 0.042(5) -0.001(4) 0.009(4) -0.003(4) N6 0.063(6) 0.084(7) 0.047(6) 0.012(5) 0.017(5) -0.017(5) N7 0.040(4) 0.039(4) 0.033(4) 0.003(3) 0.010(4) 0.005(3) N8 0.038(4) 0.043(5) 0.035(4) -0.003(4) 0.009(4) -0.004(4) N9 0.062(6) 0.044(5) 0.076(7) 0.019(5) 0.019(5) 0.001(4) N10 0.063(6) 0.067(6) 0.062(6) -0.003(5) 0.003(5) -0.032(5) N11 0.044(5) 0.039(4) 0.041(5) 0.002(3) 0.008(4) -0.002(3) N12 0.037(4) 0.039(4) 0.048(5) 0.003(4) 0.007(4) 0.001(3) B1 0.063(10) 0.116(14) 0.067(11) 0.027(10) 0.014(9) -0.008(10) F1 0.188(11) 0.301(16) 0.121(9) 0.070(10) 0.042(9) 0.120(11) F2 0.078(6) 0.175(9) 0.145(8) 0.070(7) -0.007(6) -0.006(6) F3 0.074(5) 0.167(7) 0.069(5) 0.028(5) 0.009(4) 0.034(5) F4 0.212(13) 0.079(7) 0.37(2) 0.046(10) -0.133(13) -0.043(7) C1 0.037(6) 0.056(6) 0.046(6) 0.004(5) 0.003(5) 0.003(5) C2 0.044(6) 0.058(6) 0.059(7) 0.003(5) 0.004(5) 0.003(5) C3 0.054(7) 0.085(8) 0.067(8) 0.016(7) 0.034(6) 0.003(6) C4 0.083(9) 0.074(8) 0.077(9) 0.014(7) 0.045(8) 0.002(7) C5 0.075(8) 0.054(6) 0.064(7) -0.002(5) 0.032(6) 0.001(6) C6 0.053(6) 0.060(6) 0.051(6) 0.010(5) 0.018(5) 0.006(5) C7 0.127(12) 0.114(11) 0.132(13) 0.005(10) 0.101(11) 0.010(10) C8 0.061(8) 0.091(9) 0.059(8) -0.005(7) 0.018(6) -0.022(6) C9 0.055(7) 0.051(6) 0.062(7) -0.005(5) 0.012(6) 0.008(5) C10 0.152(16) 0.140(14) 0.115(13) -0.070(11) 0.068(12) -0.107(13) C11 0.085(11) 0.096(11) 0.30(3) -0.099(14) 0.095(14) -0.045(9) C12 0.046(6) 0.042(5) 0.026(5) 0.004(4) 0.005(4) -0.005(4) C13 0.048(6) 0.036(5) 0.039(5) 0.003(4) 0.004(5) -0.005(4) C14 0.059(6) 0.050(6) 0.036(6) 0.002(4) 0.016(5) 0.000(5) C15 0.063(7) 0.057(6) 0.043(6) 0.004(5) 0.019(5) -0.004(5) C16 0.055(6) 0.051(6) 0.039(6) 0.013(5) 0.004(5) -0.006(5) C17 0.038(5) 0.042(5) 0.034(5) -0.004(4) 0.000(4) 0.001(4) C18 0.097(9) 0.084(8) 0.044(7) 0.009(6) 0.029(7) 0.008(7) C19 0.043(5) 0.042(5) 0.043(6) -0.001(4) 0.016(5) -0.003(4) C20 0.038(5) 0.041(5) 0.047(6) 0.010(4) 0.002(5) 0.004(4) C21 0.060(6) 0.033(5) 0.034(5) -0.002(4) 0.007(5) 0.007(4) C22 0.068(7) 0.028(5) 0.043(6) -0.002(4) 0.013(5) 0.002(5) C23 0.047(6) 0.051(6) 0.071(8) 0.006(5) 0.013(6) 0.008(5) C24 0.069(8) 0.076(8) 0.077(9) 0.021(7) 0.021(7) 0.008(6) C25 0.110(14) 0.124(15) 0.33(3) 0.085(19) 0.064(19) 0.014(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N11 2.030(7) . ? Ni1 N7 2.066(7) . ? Ni1 N1 2.066(8) . ? Ni1 O2 2.089(5) . ? Ni1 N4 2.150(7) 3_666 ? Ni1 N4 2.163(7) . ? Ni2 N10 1.980(9) . ? Ni2 O1 2.008(6) . ? Ni2 N1 2.045(7) . ? Ni2 O6 2.046(7) . ? Ni2 O5 2.104(6) . ? Ni2 O2 2.197(6) . ? Ni3 N12 2.010(7) . ? Ni3 O3 2.014(7) . ? Ni3 O1 2.037(6) . ? Ni3 N7 2.064(7) 3_666 ? Ni3 O2 2.081(5) . ? Ni3 N4 2.135(6) . ? O1 C1 1.331(11) . ? O2 C12 1.359(9) . ? O3 C9 1.259(12) . ? O4 C22 1.409(10) . ? O4 H4 0.8400 . ? O5 C11 1.426(15) . ? O6 C25 1.64(2) . ? O7 C24 1.410(13) . ? O7 H7 0.8400 . ? N1 N2 1.209(10) . ? N2 N3 1.143(11) . ? N4 N5 1.230(10) . ? N4 Ni1 2.150(7) 3_666 ? N5 N6 1.120(10) . ? N7 N8 1.215(9) . ? N7 Ni3 2.064(7) 3_666 ? N8 N9 1.135(10) . ? N10 C8 1.305(13) . ? N10 C10 1.457(14) . ? N11 C19 1.268(10) . ? N11 C21 1.489(10) . ? N12 C20 1.268(11) . ? N12 C23 1.465(11) . ? B1 F4 1.222(19) . ? B1 F3 1.325(16) . ? B1 F2 1.351(16) . ? B1 F1 1.40(2) . ? C1 C6 1.395(13) . ? C1 C2 1.432(13) . ? C2 C3 1.398(14) . ? C2 C8 1.452(14) . ? C3 C4 1.377(15) . ? C3 H3 0.9500 . ? C4 C5 1.358(14) . ? C4 C7 1.513(15) . ? C5 C6 1.407(13) . ? C5 H5 0.9500 . ? C6 C9 1.424(14) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.351(18) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.390(12) . ? C12 C17 1.411(12) . ? C13 C14 1.402(12) . ? C13 C19 1.478(12) . ? C14 C15 1.377(12) . ? C14 H14 0.9500 . ? C15 C16 1.344(13) . ? C15 C18 1.523(13) . ? C16 C17 1.422(12) . ? C16 H16 0.9500 . ? C17 C20 1.448(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.481(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.507(14) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Ni1 N7 98.4(3) . . ? N11 Ni1 N1 94.2(3) . . ? N7 Ni1 N1 101.3(3) . . ? N11 Ni1 O2 88.8(2) . . ? N7 Ni1 O2 172.2(2) . . ? N1 Ni1 O2 81.1(3) . . ? N11 Ni1 N4 95.0(3) . 3_666 ? N7 Ni1 N4 80.0(3) . 3_666 ? N1 Ni1 N4 170.5(3) . 3_666 ? O2 Ni1 N4 96.5(2) . 3_666 ? N11 Ni1 N4 170.4(3) . . ? N7 Ni1 N4 89.1(3) . . ? N1 Ni1 N4 90.3(3) . . ? O2 Ni1 N4 83.5(2) . . ? N4 Ni1 N4 80.3(3) 3_666 . ? N10 Ni2 O1 90.6(3) . . ? N10 Ni2 N1 97.3(3) . . ? O1 Ni2 N1 91.0(3) . . ? N10 Ni2 O6 93.5(3) . . ? O1 Ni2 O6 92.0(3) . . ? N1 Ni2 O6 168.7(3) . . ? N10 Ni2 O5 82.3(3) . . ? O1 Ni2 O5 172.9(3) . . ? N1 Ni2 O5 89.6(3) . . ? O6 Ni2 O5 88.8(3) . . ? N10 Ni2 O2 171.5(3) . . ? O1 Ni2 O2 81.8(2) . . ? N1 Ni2 O2 79.0(3) . . ? O6 Ni2 O2 90.7(2) . . ? O5 Ni2 O2 105.2(2) . . ? N12 Ni3 O3 96.0(3) . . ? N12 Ni3 O1 94.6(3) . . ? O3 Ni3 O1 88.7(3) . . ? N12 Ni3 N7 90.3(3) . 3_666 ? O3 Ni3 N7 92.3(3) . 3_666 ? O1 Ni3 N7 174.9(3) . 3_666 ? N12 Ni3 O2 90.4(3) . . ? O3 Ni3 O2 170.7(2) . . ? O1 Ni3 O2 84.1(2) . . ? N7 Ni3 O2 94.4(2) 3_666 . ? N12 Ni3 N4 168.9(3) . . ? O3 Ni3 N4 90.5(3) . . ? O1 Ni3 N4 94.6(3) . . ? N7 Ni3 N4 80.4(3) 3_666 . ? O2 Ni3 N4 84.4(2) . . ? C1 O1 Ni2 129.0(6) . . ? C1 O1 Ni3 128.0(6) . . ? Ni2 O1 Ni3 100.7(3) . . ? C12 O2 Ni3 121.6(5) . . ? C12 O2 Ni1 121.7(5) . . ? Ni3 O2 Ni1 98.0(2) . . ? C12 O2 Ni2 118.9(5) . . ? Ni3 O2 Ni2 93.3(2) . . ? Ni1 O2 Ni2 97.0(2) . . ? C9 O3 Ni3 126.0(6) . . ? C22 O4 H4 109.5 . . ? C11 O5 Ni2 107.9(8) . . ? C25 O6 Ni2 129.0(8) . . ? C24 O7 H7 109.5 . . ? N2 N1 Ni2 123.2(6) . . ? N2 N1 Ni1 132.4(6) . . ? Ni2 N1 Ni1 102.7(3) . . ? N3 N2 N1 177.2(10) . . ? N5 N4 Ni3 121.1(6) . . ? N5 N4 Ni1 125.3(5) . 3_666 ? Ni3 N4 Ni1 97.1(3) . 3_666 ? N5 N4 Ni1 113.4(5) . . ? Ni3 N4 Ni1 94.1(3) . . ? Ni1 N4 Ni1 99.7(3) 3_666 . ? N6 N5 N4 178.5(10) . . ? N8 N7 Ni3 122.0(6) . 3_666 ? N8 N7 Ni1 130.0(6) . . ? Ni3 N7 Ni1 102.1(3) 3_666 . ? N9 N8 N7 176.7(9) . . ? C8 N10 C10 120.6(10) . . ? C8 N10 Ni2 127.0(8) . . ? C10 N10 Ni2 112.4(9) . . ? C19 N11 C21 115.6(8) . . ? C19 N11 Ni1 122.6(6) . . ? C21 N11 Ni1 121.7(6) . . ? C20 N12 C23 116.3(8) . . ? C20 N12 Ni3 121.7(6) . . ? C23 N12 Ni3 121.7(7) . . ? F4 B1 F3 120.3(16) . . ? F4 B1 F2 109.4(16) . . ? F3 B1 F2 114.2(13) . . ? F4 B1 F1 109.2(16) . . ? F3 B1 F1 104.4(15) . . ? F2 B1 F1 96.5(14) . . ? O1 C1 C6 122.6(9) . . ? O1 C1 C2 120.8(9) . . ? C6 C1 C2 116.6(10) . . ? C3 C2 C1 120.6(10) . . ? C3 C2 C8 113.9(10) . . ? C1 C2 C8 125.5(10) . . ? C4 C3 C2 121.8(11) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? C5 C4 C3 117.3(11) . . ? C5 C4 C7 121.6(12) . . ? C3 C4 C7 121.0(11) . . ? C4 C5 C6 123.6(11) . . ? C4 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C1 C6 C5 119.9(10) . . ? C1 C6 C9 124.5(10) . . ? C5 C6 C9 115.5(10) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N10 C8 C2 125.3(11) . . ? N10 C8 H8 117.3 . . ? C2 C8 H8 117.3 . . ? O3 C9 C6 127.9(10) . . ? O3 C9 H9 116.1 . . ? C6 C9 H9 116.1 . . ? C11 C10 N10 114.3(13) . . ? C11 C10 H10A 108.7 . . ? N10 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? N10 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 O5 118.4(12) . . ? C10 C11 H11A 107.7 . . ? O5 C11 H11A 107.7 . . ? C10 C11 H11B 107.7 . . ? O5 C11 H11B 107.7 . . ? H11A C11 H11B 107.1 . . ? O2 C12 C13 120.7(8) . . ? O2 C12 C17 120.9(8) . . ? C13 C12 C17 118.3(8) . . ? C12 C13 C14 121.0(8) . . ? C12 C13 C19 125.2(8) . . ? C14 C13 C19 113.8(8) . . ? C15 C14 C13 121.4(9) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C16 C15 C14 117.4(9) . . ? C16 C15 C18 121.2(9) . . ? C14 C15 C18 121.4(10) . . ? C15 C16 C17 124.4(9) . . ? C15 C16 H16 117.8 . . ? C17 C16 H16 117.8 . . ? C12 C17 C16 117.4(8) . . ? C12 C17 C20 125.6(8) . . ? C16 C17 C20 116.7(8) . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N11 C19 C13 127.9(9) . . ? N11 C19 H19 116.0 . . ? C13 C19 H19 116.0 . . ? N12 C20 C17 128.6(8) . . ? N12 C20 H20 115.7 . . ? C17 C20 H20 115.7 . . ? C22 C21 N11 113.5(8) . . ? C22 C21 H21A 108.9 . . ? N11 C21 H21A 108.9 . . ? C22 C21 H21B 108.9 . . ? N11 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? O4 C22 C21 113.8(8) . . ? O4 C22 H22A 108.8 . . ? C21 C22 H22A 108.8 . . ? O4 C22 H22B 108.8 . . ? C21 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? N12 C23 C24 111.1(8) . . ? N12 C23 H23A 109.4 . . ? C24 C23 H23A 109.4 . . ? N12 C23 H23B 109.4 . . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? O7 C24 C23 112.5(10) . . ? O7 C24 H24A 109.1 . . ? C23 C24 H24A 109.1 . . ? O7 C24 H24B 109.1 . . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.8 . . ? O6 C25 H25A 109.5 . . ? O6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.837 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.141