# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Louise N. Dawe' 'Laurence K. Thompson' _publ_contact_author_name L.Thompson _publ_contact_author_address ; Department of Chemistry Memorial University St John's, Newfoundland A1B 3X7 CANADA ; _publ_contact_author_email LTHOMP@MUN.CA _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Complete and Incomplete [2x2] grids by self-assembly with a sterically hindered ditopic imidazole hydrazone ligand structural and magnetic studies ; data_shelxl_1 _database_code_depnum_ccdc_archive 'CCDC 674828' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H34.50 B2 Co2 F8 N12 O8.75 ' _chemical_formula_weight 898.56 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' Co Co 0.3494 0.9721 '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' 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.882(2) _cell_length_b 14.623(3) _cell_length_c 14.928(4) _cell_angle_alpha 107.465(3) _cell_angle_beta 107.784(3) _cell_angle_gamma 95.447(4) _cell_volume 1917.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6994 _cell_measurement_theta_min 2.4002 _cell_measurement_theta_max 30.6329 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 913 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.8491 _exptl_absorpt_correction_T_max 0.9356 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 18471 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 26.50 _reflns_number_total 7865 _reflns_number_gt 6636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.1591P)^2^+4.5988P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0021(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7865 _refine_ls_number_parameters 552 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1092 _refine_ls_R_factor_gt 0.0988 _refine_ls_wR_factor_ref 0.2902 _refine_ls_wR_factor_gt 0.2752 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.70618(7) 0.21433(5) 0.87768(5) 0.0353(2) Uani 1 1 d . . . Co2 Co 0.32833(9) 0.27361(7) 0.61266(7) 0.0526(3) Uani 1 1 d . . . F1 F 0.9323(12) 0.0114(6) 0.7506(8) 0.145(4) Uani 0.75 1 d P . . F2 F 1.1354(7) 0.0445(6) 0.7285(9) 0.149(4) Uani 0.75 1 d P . . F3 F 0.9797(10) 0.1316(6) 0.7019(6) 0.102(2) Uani 0.75 1 d P . . F4 F 0.9426(14) -0.0181(8) 0.6000(7) 0.157(4) Uani 0.75 1 d P . . F5 F 0.6662(6) 0.7039(6) 0.7644(6) 0.093(2) Uani 0.75 1 d P . . F6 F 0.8954(7) 0.6889(5) 0.8326(5) 0.0839(19) Uani 0.75 1 d P . . F7 F 0.8456(9) 0.8102(6) 0.7783(8) 0.126(4) Uani 0.75 1 d P . . F8 F 0.7935(13) 0.6651(9) 0.6682(7) 0.149(4) Uani 0.75 1 d P . . F9 F 0.7346(10) 0.3593(8) 0.5939(11) 0.104(4) Uani 0.50 1 d P . . F10 F 0.8928(17) 0.2959(11) 0.528(2) 0.198(11) Uani 0.50 1 d P . . F11 F 0.8303(14) 0.4362(11) 0.5127(8) 0.108(4) Uani 0.50 1 d P . . F12 F 0.9685(11) 0.4170(15) 0.6476(9) 0.141(7) Uani 0.50 1 d P . . O1 O 0.3508(5) 0.3252(4) 0.8660(4) 0.0712(15) Uani 1 1 d . . . O2 O 0.8298(5) -0.0361(4) 0.9925(4) 0.0593(12) Uani 1 1 d . . . O3 O 0.4833(6) 0.3965(4) 0.6361(5) 0.0727(14) Uani 1 1 d . . . O4 O 0.2445(6) 0.3692(4) 0.7075(4) 0.0704(14) Uani 1 1 d . . . O5 O 0.1589(7) 0.1602(5) 0.5820(5) 0.099(2) Uani 1 1 d . . . O6 O 0.1844(8) 0.3093(7) 0.4960(5) 0.112(3) Uani 1 1 d . . . O7 O 0.5921(10) 0.4283(6) 0.3504(8) 0.109(4) Uani 0.75 1 d P . . O8 O 0.807(3) 0.4468(18) 0.3561(13) 0.140(9) Uani 0.40 1 d P . . O9 O 0.9043(11) 0.3535(9) 0.3307(7) 0.087(3) Uani 0.60 1 d P . . O10 O 0.8467(6) 0.1469(5) 0.2109(6) 0.097(2) Uani 1 1 d . . . N1 N 0.6929(4) 0.2859(3) 1.0050(3) 0.0370(9) Uani 1 1 d . . . N2 N 0.6858(5) 0.3676(3) 1.1507(4) 0.0439(11) Uani 1 1 d . . . H2 H 0.7124 0.3947 1.2162 0.053 Uiso 1 1 calc R . . N3 N 0.5382(5) 0.2589(3) 0.8248(3) 0.0370(9) Uani 1 1 d . . . N4 N 0.4815(5) 0.2324(4) 0.7199(4) 0.0420(10) Uani 1 1 d . . . N5 N 0.6795(5) 0.1580(3) 0.7418(4) 0.0416(10) Uani 1 1 d . . . H6 H 0.7330 0.1283 0.7208 0.038 Uiso 1 1 d . . . N6 N 0.4210(6) 0.1815(4) 0.5222(4) 0.0509(12) Uani 1 1 d . . . N7 N 0.5897(5) 0.0975(3) 0.8708(3) 0.0349(9) Uani 1 1 d . . . N8 N 0.4103(5) -0.0191(4) 0.8389(4) 0.0439(11) Uani 1 1 d . . . H12 H 0.3208 -0.0527 0.8169 0.053 Uiso 1 1 calc R . . N9 N 0.9045(5) 0.0962(4) 0.9624(4) 0.0452(11) Uani 1 1 d . . . N10 N 0.8868(5) 0.1747(3) 0.9291(4) 0.0390(10) Uani 1 1 d . . . N11 N 1.1339(5) 0.2068(4) 0.9474(4) 0.0511(12) Uani 1 1 d . . . H16 H 1.1523 0.1557 0.9650 0.061 Uiso 1 1 calc R . . H17 H 1.2036 0.2458 0.9434 0.061 Uiso 1 1 calc R . . N12 N 0.8354(5) 0.3246(3) 0.8816(3) 0.0358(9) Uani 1 1 d . . . C1 C 0.7600(6) 0.3114(4) 1.1019(4) 0.0417(12) Uani 1 1 d . . . H1 H 0.8472 0.2932 1.1330 0.050 Uiso 1 1 calc R . . C2 C 0.5631(6) 0.3758(4) 1.0825(5) 0.0458(13) Uani 1 1 d . . . C3 C 0.4566(8) 0.4323(6) 1.1120(6) 0.0634(18) Uani 1 1 d . . . H3 H 0.3819 0.3890 1.1193 0.076 Uiso 1 1 calc R . . H4 H 0.4111 0.4594 1.0603 0.076 Uiso 1 1 calc R . . H5 H 0.5069 0.4859 1.1760 0.076 Uiso 1 1 calc R . . C4 C 0.5685(6) 0.3236(4) 0.9915(4) 0.0407(12) Uani 1 1 d . . . C5 C 0.4737(6) 0.3026(5) 0.8866(4) 0.0456(13) Uani 1 1 d . . . C6 C 0.5698(6) 0.1809(4) 0.6820(4) 0.0397(11) Uani 1 1 d . . . C7 C 0.5389(7) 0.1531(4) 0.5727(4) 0.0463(13) Uani 1 1 d . . . C8 C 0.6254(9) 0.1037(6) 0.5264(5) 0.0636(18) Uani 1 1 d . . . H7 H 0.7078 0.0855 0.5640 0.076 Uiso 1 1 calc R . . C9 C 0.5895(10) 0.0814(6) 0.4247(6) 0.073(2) Uani 1 1 d . . . H8 H 0.6485 0.0486 0.3914 0.088 Uiso 1 1 calc R . . C10 C 0.4682(11) 0.1067(6) 0.3712(6) 0.075(2) Uani 1 1 d . . . H9 H 0.4405 0.0900 0.3006 0.090 Uiso 1 1 calc R . . C11 C 0.3869(9) 0.1572(6) 0.4227(5) 0.0622(18) Uani 1 1 d . . . H10 H 0.3035 0.1752 0.3859 0.075 Uiso 1 1 calc R . . C12 C 0.4485(6) 0.0677(4) 0.8299(4) 0.0404(11) Uani 1 1 d . . . H11 H 0.3832 0.1020 0.7987 0.048 Uiso 1 1 calc R . . C13 C 0.5298(6) -0.0468(4) 0.8869(5) 0.0427(12) Uani 1 1 d . . . C14 C 0.5219(7) -0.1410(4) 0.9051(5) 0.0531(15) Uani 1 1 d . . . H13 H 0.4399 -0.1897 0.8511 0.064 Uiso 1 1 calc R . . H14 H 0.5083 -0.1316 0.9694 0.064 Uiso 1 1 calc R . . H15 H 0.6122 -0.1642 0.9070 0.064 Uiso 1 1 calc R . . C15 C 0.6449(6) 0.0267(4) 0.9072(4) 0.0397(11) Uani 1 1 d . . . C16 C 0.7965(6) 0.0285(4) 0.9563(5) 0.0434(12) Uani 1 1 d . . . C17 C 1.0010(6) 0.2249(4) 0.9268(4) 0.0426(12) Uani 1 1 d . . . C18 C 0.9747(6) 0.3148(4) 0.9027(4) 0.0413(12) Uani 1 1 d . . . C19 C 1.0789(6) 0.3832(5) 0.9017(5) 0.0484(13) Uani 1 1 d . . . H18 H 1.1768 0.3755 0.9175 0.058 Uiso 1 1 calc R . . C20 C 1.0401(7) 0.4633(5) 0.8777(5) 0.0529(15) Uani 1 1 d . . . H19 H 1.1105 0.5114 0.8765 0.063 Uiso 1 1 calc R . . C21 C 0.8960(6) 0.4720(4) 0.8551(5) 0.0480(14) Uani 1 1 d . . . H20 H 0.8667 0.5266 0.8384 0.058 Uiso 1 1 calc R . . C22 C 0.7964(6) 0.4018(4) 0.8571(4) 0.0433(12) Uani 1 1 d . . . H21 H 0.6977 0.4078 0.8409 0.052 Uiso 1 1 calc R . . B1 B 0.9971(10) 0.0376(8) 0.6945(8) 0.052(2) Uani 0.75 1 d P . . B2 B 0.8027(11) 0.7142(9) 0.7617(8) 0.058(3) Uani 0.75 1 d P . . B3 B 0.8520(17) 0.3781(16) 0.5727(13) 0.067(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0273(4) 0.0399(4) 0.0431(4) 0.0201(3) 0.0120(3) 0.0095(3) Co2 0.0409(5) 0.0719(6) 0.0474(5) 0.0274(4) 0.0100(4) 0.0181(4) F1 0.194(10) 0.090(5) 0.143(8) -0.006(5) 0.119(8) -0.044(6) F2 0.027(3) 0.112(6) 0.246(12) 0.025(7) -0.001(4) 0.021(3) F3 0.135(7) 0.106(5) 0.091(5) 0.050(4) 0.047(5) 0.068(5) F4 0.185(10) 0.133(8) 0.088(6) -0.032(5) 0.047(7) -0.026(7) F5 0.047(3) 0.116(5) 0.095(5) 0.013(4) 0.025(3) 0.000(3) F6 0.069(4) 0.087(4) 0.096(5) 0.058(4) 0.002(3) 0.021(3) F7 0.086(5) 0.103(6) 0.204(10) 0.107(7) 0.020(6) 0.015(4) F8 0.197(11) 0.222(12) 0.100(6) 0.085(7) 0.099(7) 0.115(9) F9 0.053(5) 0.100(8) 0.169(12) 0.041(7) 0.061(7) 0.010(5) F10 0.106(11) 0.091(9) 0.44(3) 0.086(15) 0.146(17) 0.052(8) F11 0.105(8) 0.162(11) 0.074(7) 0.062(7) 0.025(6) 0.058(8) F12 0.044(5) 0.32(2) 0.082(7) 0.107(11) 0.019(5) 0.046(9) O1 0.042(2) 0.119(4) 0.051(3) 0.022(3) 0.014(2) 0.043(3) O2 0.041(2) 0.067(3) 0.093(4) 0.055(3) 0.026(2) 0.021(2) O3 0.077(4) 0.062(3) 0.090(4) 0.033(3) 0.036(3) 0.016(3) O4 0.057(3) 0.092(4) 0.072(3) 0.032(3) 0.025(3) 0.038(3) O5 0.067(4) 0.119(5) 0.085(4) 0.021(4) 0.021(3) -0.030(4) O6 0.085(4) 0.204(8) 0.075(4) 0.081(5) 0.021(3) 0.073(5) O7 0.079(6) 0.071(5) 0.140(9) 0.045(5) -0.018(5) 0.011(4) O8 0.141(19) 0.17(2) 0.057(10) 0.001(11) 0.024(11) -0.019(16) O9 0.068(6) 0.122(9) 0.058(5) 0.025(5) 0.017(5) 0.001(6) O10 0.048(3) 0.115(5) 0.134(6) 0.080(5) 0.010(3) -0.001(3) N1 0.027(2) 0.042(2) 0.045(2) 0.0220(19) 0.0113(18) 0.0053(17) N2 0.042(2) 0.047(3) 0.040(2) 0.017(2) 0.010(2) 0.004(2) N3 0.032(2) 0.046(2) 0.035(2) 0.0180(19) 0.0101(18) 0.0084(18) N4 0.038(2) 0.049(3) 0.040(2) 0.018(2) 0.0107(19) 0.0141(19) N5 0.032(2) 0.047(3) 0.050(3) 0.020(2) 0.018(2) 0.0106(18) N6 0.052(3) 0.054(3) 0.042(3) 0.017(2) 0.011(2) 0.008(2) N7 0.032(2) 0.037(2) 0.042(2) 0.0202(18) 0.0161(18) 0.0077(17) N8 0.031(2) 0.048(3) 0.050(3) 0.020(2) 0.010(2) 0.0028(19) N9 0.034(2) 0.050(3) 0.065(3) 0.036(2) 0.018(2) 0.0159(19) N10 0.033(2) 0.040(2) 0.046(2) 0.021(2) 0.0104(19) 0.0097(17) N11 0.033(2) 0.050(3) 0.077(4) 0.032(3) 0.018(2) 0.011(2) N12 0.033(2) 0.039(2) 0.046(2) 0.0206(19) 0.0213(19) 0.0119(17) C1 0.037(3) 0.043(3) 0.044(3) 0.022(2) 0.008(2) 0.005(2) C2 0.039(3) 0.051(3) 0.047(3) 0.017(3) 0.014(2) 0.010(2) C3 0.056(4) 0.073(5) 0.056(4) 0.013(3) 0.019(3) 0.024(3) C4 0.030(2) 0.052(3) 0.041(3) 0.022(2) 0.009(2) 0.009(2) C5 0.030(2) 0.064(4) 0.043(3) 0.019(3) 0.010(2) 0.017(2) C6 0.036(3) 0.042(3) 0.046(3) 0.021(2) 0.015(2) 0.012(2) C7 0.048(3) 0.051(3) 0.043(3) 0.021(3) 0.015(3) 0.014(3) C8 0.073(5) 0.066(4) 0.054(4) 0.019(3) 0.024(4) 0.024(4) C9 0.092(6) 0.088(6) 0.047(4) 0.023(4) 0.033(4) 0.031(5) C10 0.103(7) 0.076(5) 0.048(4) 0.023(4) 0.031(4) 0.016(5) C11 0.068(4) 0.078(5) 0.040(3) 0.024(3) 0.015(3) 0.014(4) C12 0.028(2) 0.048(3) 0.046(3) 0.021(2) 0.011(2) 0.005(2) C13 0.037(3) 0.047(3) 0.051(3) 0.023(3) 0.019(2) 0.008(2) C14 0.043(3) 0.048(3) 0.074(4) 0.032(3) 0.020(3) 0.003(2) C15 0.032(2) 0.043(3) 0.047(3) 0.020(2) 0.013(2) 0.008(2) C16 0.035(3) 0.045(3) 0.056(3) 0.024(3) 0.017(2) 0.012(2) C17 0.033(3) 0.045(3) 0.051(3) 0.015(2) 0.015(2) 0.012(2) C18 0.034(3) 0.050(3) 0.042(3) 0.019(2) 0.015(2) 0.008(2) C19 0.034(3) 0.061(4) 0.059(4) 0.026(3) 0.023(3) 0.014(2) C20 0.049(3) 0.054(4) 0.070(4) 0.034(3) 0.028(3) 0.011(3) C21 0.046(3) 0.047(3) 0.064(4) 0.031(3) 0.024(3) 0.015(2) C22 0.045(3) 0.045(3) 0.050(3) 0.025(3) 0.021(3) 0.014(2) B1 0.038(4) 0.059(6) 0.055(5) 0.013(4) 0.019(4) 0.006(4) B2 0.049(5) 0.085(7) 0.060(6) 0.043(6) 0.025(5) 0.031(5) B3 0.041(7) 0.108(14) 0.060(9) 0.037(9) 0.012(7) 0.040(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N5 1.868(5) . ? Co1 N3 1.876(4) . ? Co1 N7 1.925(4) . ? Co1 N1 1.926(5) . ? Co1 N12 1.934(4) . ? Co1 N10 1.934(4) . ? Co2 O5 2.077(6) . ? Co2 N6 2.091(6) . ? Co2 O4 2.096(5) . ? Co2 O3 2.114(5) . ? Co2 N4 2.119(5) . ? Co2 O6 2.122(5) . ? F1 B1 1.316(12) . ? F2 B1 1.286(11) . ? F3 B1 1.377(12) . ? F4 B1 1.306(13) . ? F5 B2 1.357(11) . ? F6 B2 1.344(11) . ? F7 B2 1.351(14) . ? F8 B2 1.334(14) . ? F9 B3 1.318(19) . ? F10 B3 1.35(2) . ? F11 B3 1.39(2) . ? F12 B3 1.27(2) . ? O1 C5 1.260(7) . ? O2 C16 1.245(7) . ? O8 O9 1.76(3) . ? N1 C1 1.309(7) . ? N1 C4 1.379(7) . ? N2 C1 1.350(8) . ? N2 C2 1.367(7) . ? N3 C5 1.322(7) . ? N3 N4 1.405(6) . ? N4 C6 1.349(7) . ? N5 C6 1.320(7) . ? N6 C11 1.342(8) . ? N6 C7 1.356(8) . ? N7 C12 1.309(7) . ? N7 C15 1.389(6) . ? N8 C12 1.348(7) . ? N8 C13 1.349(7) . ? N9 C16 1.347(7) . ? N9 N10 1.387(6) . ? N10 C17 1.302(7) . ? N11 C17 1.325(7) . ? N12 C22 1.342(7) . ? N12 C18 1.347(7) . ? C2 C4 1.363(8) . ? C2 C3 1.488(9) . ? C4 C5 1.478(8) . ? C6 C7 1.482(8) . ? C7 C8 1.382(9) . ? C8 C9 1.375(10) . ? C9 C10 1.373(12) . ? C10 C11 1.390(11) . ? C13 C15 1.379(8) . ? C13 C14 1.482(8) . ? C15 C16 1.446(7) . ? C17 C18 1.489(8) . ? C18 C19 1.372(8) . ? C19 C20 1.378(9) . ? C20 C21 1.387(9) . ? C21 C22 1.367(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Co1 N3 81.84(19) . . ? N5 Co1 N7 90.0(2) . . ? N3 Co1 N7 90.54(19) . . ? N5 Co1 N1 165.76(19) . . ? N3 Co1 N1 83.96(19) . . ? N7 Co1 N1 91.02(18) . . ? N5 Co1 N12 87.6(2) . . ? N3 Co1 N12 93.65(19) . . ? N7 Co1 N12 174.86(17) . . ? N1 Co1 N12 92.38(18) . . ? N5 Co1 N10 96.7(2) . . ? N3 Co1 N10 175.85(18) . . ? N7 Co1 N10 93.34(18) . . ? N1 Co1 N10 97.45(19) . . ? N12 Co1 N10 82.40(18) . . ? O5 Co2 N6 92.2(3) . . ? O5 Co2 O4 89.8(3) . . ? N6 Co2 O4 177.5(2) . . ? O5 Co2 O3 173.7(3) . . ? N6 Co2 O3 90.6(2) . . ? O4 Co2 O3 87.5(2) . . ? O5 Co2 N4 95.0(3) . . ? N6 Co2 N4 78.8(2) . . ? O4 Co2 N4 99.6(2) . . ? O3 Co2 N4 91.1(2) . . ? O5 Co2 O6 86.3(3) . . ? N6 Co2 O6 96.1(3) . . ? O4 Co2 O6 85.4(3) . . ? O3 Co2 O6 87.8(3) . . ? N4 Co2 O6 174.8(2) . . ? C1 N1 C4 106.9(5) . . ? C1 N1 Co1 142.4(4) . . ? C4 N1 Co1 110.7(4) . . ? C1 N2 C2 109.5(5) . . ? C5 N3 N4 125.0(4) . . ? C5 N3 Co1 118.1(4) . . ? N4 N3 Co1 116.4(3) . . ? C6 N4 N3 107.9(4) . . ? C6 N4 Co2 113.1(4) . . ? N3 N4 Co2 137.5(4) . . ? C6 N5 Co1 113.5(4) . . ? C11 N6 C7 117.3(6) . . ? C11 N6 Co2 127.2(5) . . ? C7 N6 Co2 115.0(4) . . ? C12 N7 C15 107.4(4) . . ? C12 N7 Co1 128.1(4) . . ? C15 N7 Co1 124.5(3) . . ? C12 N8 C13 109.8(5) . . ? C16 N9 N10 125.6(4) . . ? C17 N10 N9 117.8(4) . . ? C17 N10 Co1 115.4(4) . . ? N9 N10 Co1 126.7(3) . . ? C22 N12 C18 119.5(5) . . ? C22 N12 Co1 126.3(4) . . ? C18 N12 Co1 113.9(4) . . ? N1 C1 N2 109.4(5) . . ? C4 C2 N2 104.5(5) . . ? C4 C2 C3 132.5(6) . . ? N2 C2 C3 122.9(6) . . ? C2 C4 N1 109.7(5) . . ? C2 C4 C5 133.9(5) . . ? N1 C4 C5 116.4(5) . . ? O1 C5 N3 128.8(6) . . ? O1 C5 C4 121.4(5) . . ? N3 C5 C4 109.8(5) . . ? N5 C6 N4 120.1(5) . . ? N5 C6 C7 122.5(5) . . ? N4 C6 C7 117.3(5) . . ? N6 C7 C8 122.8(6) . . ? N6 C7 C6 114.8(5) . . ? C8 C7 C6 122.4(6) . . ? C9 C8 C7 118.6(7) . . ? C10 C9 C8 119.8(8) . . ? C9 C10 C11 118.5(7) . . ? N6 C11 C10 122.9(7) . . ? N7 C12 N8 109.4(5) . . ? N8 C13 C15 105.5(5) . . ? N8 C13 C14 122.0(5) . . ? C15 C13 C14 132.4(5) . . ? C13 C15 N7 107.9(5) . . ? C13 C15 C16 125.8(5) . . ? N7 C15 C16 126.2(5) . . ? O2 C16 N9 118.1(5) . . ? O2 C16 C15 119.3(5) . . ? N9 C16 C15 122.6(5) . . ? N10 C17 N11 127.5(5) . . ? N10 C17 C18 113.6(5) . . ? N11 C17 C18 118.9(5) . . ? N12 C18 C19 121.5(5) . . ? N12 C18 C17 113.4(5) . . ? C19 C18 C17 125.1(5) . . ? C18 C19 C20 119.4(5) . . ? C19 C20 C21 118.6(6) . . ? C22 C21 C20 119.7(5) . . ? N12 C22 C21 121.3(5) . . ? F2 B1 F4 110.4(11) . . ? F2 B1 F1 112.6(12) . . ? F4 B1 F1 113.6(10) . . ? F2 B1 F3 104.7(9) . . ? F4 B1 F3 108.5(10) . . ? F1 B1 F3 106.5(9) . . ? F8 B2 F6 114.4(9) . . ? F8 B2 F7 106.9(10) . . ? F6 B2 F7 109.3(10) . . ? F8 B2 F5 107.6(10) . . ? F6 B2 F5 112.4(9) . . ? F7 B2 F5 105.8(9) . . ? F12 B3 F9 115.6(15) . . ? F12 B3 F10 98.0(15) . . ? F9 B3 F10 112.5(18) . . ? F12 B3 F11 109.5(18) . . ? F9 B3 F11 110.1(12) . . ? F10 B3 F11 110.6(18) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.330 _refine_diff_density_min -1.127 _refine_diff_density_rms 0.134 #===END data_shelxl_2 _database_code_depnum_ccdc_archive 'CCDC 674829' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H52 Mn3 N28 O19' _chemical_formula_weight 1441.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7348(13) _cell_length_b 13.6851(18) _cell_length_c 23.480(3) _cell_angle_alpha 88.283(5) _cell_angle_beta 80.327(5) _cell_angle_gamma 86.514(5) _cell_volume 3393.4(7) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 10390 _cell_measurement_theta_min 1.9810 _cell_measurement_theta_max 30.9427 _exptl_crystal_description Prism _exptl_crystal_colour Orange _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1478 _exptl_absorpt_coefficient_mu 0.634 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.8627 _exptl_absorpt_correction_T_max 0.9334 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 34286 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0527 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15289 _reflns_number_gt 11165 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 222.3 electrons per unit cell in one void (total volume 1001.4 A^3); that is 111.15 electrons per formula unit. Four disordered nitrates appeared to be present prior to the application of Squeeze, though a good point atom model could not be achieved for these. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the framework structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; 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 0.319 0.093 0.713 1001.4 222.3 _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^)+(0.1519P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0055(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15289 _refine_ls_number_parameters 705 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.2393 _refine_ls_wR_factor_gt 0.2209 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 Mn1 Mn 1.14180(5) 0.17936(4) 0.12541(2) 0.05621(16) Uani 1 1 d . . . Mn2 Mn 0.86744(4) 0.23080(3) 0.255366(19) 0.04732(15) Uani 1 1 d . . . Mn3 Mn 1.07195(4) 0.31659(3) 0.36644(2) 0.05209(16) Uani 1 1 d . . . O1 O 1.0022(2) 0.27312(15) 0.17976(9) 0.0533(5) Uani 1 1 d . . . O2 O 0.99252(19) 0.20476(14) 0.31951(9) 0.0474(4) Uani 1 1 d . . . O3 O 1.1912(2) 0.37375(17) 0.28981(10) 0.0619(6) Uani 1 1 d . . . O4 O 1.2347(2) 0.13683(18) 0.20019(10) 0.0625(6) Uani 1 1 d . . . O5 O 1.3085(3) 0.1139(2) 0.07130(13) 0.0844(8) Uani 1 1 d . . . O6 O 1.1615(2) 0.3952(2) 0.42652(13) 0.0728(7) Uani 1 1 d . . . O7 O 0.7570(3) 0.0492(2) 0.44818(13) 0.0847(8) Uani 1 1 d . . . N1 N 1.1534(3) 0.3234(2) 0.08229(12) 0.0680(8) Uani 1 1 d . . . N2 N 1.1747(5) 0.4594(3) 0.0331(2) 0.1129(15) Uani 1 1 d . . . H2 H 1.1900 0.5068 0.0000 0.049 Uiso 1 1 d . . . N3 N 0.8714(3) 0.4158(2) 0.17567(12) 0.0602(7) Uani 1 1 d . . . N4 N 0.8034(3) 0.37288(19) 0.22538(12) 0.0558(6) Uani 1 1 d . . . N5 N 0.6498(3) 0.5004(2) 0.22422(17) 0.0763(9) Uani 1 1 d . . . H6 H 0.6888 0.5256 0.1916 0.092 Uiso 1 1 calc R . . H7 H 0.5781 0.5283 0.2417 0.092 Uiso 1 1 calc R . . N6 N 0.6940(2) 0.29240(19) 0.31981(11) 0.0510(6) Uani 1 1 d . . . N7 N 1.1266(3) 0.1775(2) 0.40590(12) 0.0569(6) Uani 1 1 d . . . N8 N 1.1732(3) 0.0464(2) 0.45552(12) 0.0659(7) Uani 1 1 d . . . H13 H 1.2198 -0.0042 0.4825 0.049 Uiso 1 1 d . . . N9 N 0.9221(3) 0.04824(19) 0.33080(12) 0.0537(6) Uani 1 1 d . . . N10 N 0.8559(2) 0.08113(18) 0.28638(11) 0.0508(5) Uani 1 1 d . . . N11 N 0.7602(4) -0.0679(3) 0.29529(18) 0.0895(11) Uani 1 1 d . . . H17 H 0.8011 -0.0887 0.3232 0.107 Uiso 1 1 calc R . . H18 H 0.7068 -0.1056 0.2832 0.107 Uiso 1 1 calc R . . N12 N 0.7384(3) 0.1480(2) 0.20421(12) 0.0561(6) Uani 1 1 d . . . N13 N 1.1931(5) 0.5871(3) 0.1945(2) 0.1089(14) Uani 1 1 d . . . N14 N 1.3624(6) 0.5184(4) 0.13851(18) 0.1131(16) Uani 1 1 d . . . H24 H 1.4284 0.5132 0.1107 0.136 Uiso 1 1 calc R . . N15 N 1.0354(3) 0.4892(2) 0.28492(13) 0.0632(7) Uani 1 1 d . . . H28 H 0.9979 0.5462 0.2622 0.049 Uiso 1 1 d . . . N16 N 0.9717(3) 0.4453(2) 0.33414(12) 0.0572(6) Uani 1 1 d . . . N17 N 0.8020(4) 0.5629(2) 0.34435(18) 0.0827(10) Uani 1 1 d . . . H29 H 0.8316 0.5948 0.3123 0.099 Uiso 1 1 calc R . . H30 H 0.7301 0.5834 0.3655 0.099 Uiso 1 1 calc R . . N18 N 0.8787(3) 0.3468(2) 0.42609(11) 0.0546(6) Uani 1 1 d . . . N19 N 1.2783(4) -0.0863(3) 0.28056(15) 0.0790(9) Uani 1 1 d . . . N20 N 1.3940(3) -0.0136(3) 0.33372(14) 0.0757(9) Uani 1 1 d . . . H36 H 1.4396 -0.0135 0.3665 0.049 Uiso 1 1 d . . . N21 N 1.1386(3) -0.0053(2) 0.20075(14) 0.0650(7) Uani 1 1 d . . . H40 H 1.1370 -0.0793 0.2158 0.049 Uiso 1 1 d . . . N22 N 1.0818(3) 0.0351(2) 0.15711(12) 0.0590(6) Uani 1 1 d . . . N23 N 0.9677(3) -0.1047(2) 0.15127(16) 0.0767(9) Uani 1 1 d . . . H41 H 1.0009 -0.1364 0.1788 0.092 Uiso 1 1 calc R . . H42 H 0.9124 -0.1327 0.1342 0.092 Uiso 1 1 calc R . . N24 N 0.9916(3) 0.1281(2) 0.07414(12) 0.0607(7) Uani 1 1 d . . . C1 C 1.2168(5) 0.3689(4) 0.03833(19) 0.0870(12) Uani 1 1 d . . . H1 H 1.2862 0.3394 0.0129 0.104 Uiso 1 1 calc R . . C2 C 1.0700(5) 0.4768(3) 0.0754(2) 0.0912(14) Uani 1 1 d . . . C3 C 0.9983(8) 0.5736(4) 0.0832(3) 0.146(3) Uani 1 1 d . . . H3 H 1.0014 0.6072 0.0456 0.175 Uiso 1 1 calc R . . H4 H 1.0362 0.6134 0.1090 0.175 Uiso 1 1 calc R . . H5 H 0.9100 0.5636 0.1001 0.175 Uiso 1 1 calc R . . C4 C 1.0596(4) 0.3899(3) 0.10571(15) 0.0651(8) Uani 1 1 d . . . C5 C 0.9705(4) 0.3588(2) 0.15750(14) 0.0582(8) Uani 1 1 d . . . C6 C 0.7001(4) 0.4186(2) 0.24744(16) 0.0605(8) Uani 1 1 d . . . C7 C 0.6336(3) 0.3739(2) 0.30134(15) 0.0550(7) Uani 1 1 d . . . C8 C 0.5191(4) 0.4104(3) 0.33143(19) 0.0715(10) Uani 1 1 d . . . H8 H 0.4760 0.4660 0.3169 0.086 Uiso 1 1 calc R . . C9 C 0.4681(4) 0.3656(3) 0.3827(2) 0.0755(11) Uani 1 1 d . . . H9 H 0.3901 0.3903 0.4041 0.091 Uiso 1 1 calc R . . C10 C 0.5320(3) 0.2840(3) 0.40267(17) 0.0649(8) Uani 1 1 d . . . H10 H 0.5000 0.2525 0.4383 0.078 Uiso 1 1 calc R . . C11 C 0.6436(3) 0.2497(3) 0.36920(15) 0.0575(7) Uani 1 1 d . . . H11 H 0.6865 0.1928 0.3822 0.069 Uiso 1 1 calc R . . C12 C 1.1876(4) 0.1427(3) 0.44698(16) 0.0682(9) Uani 1 1 d . . . H12 H 1.2354 0.1806 0.4678 0.082 Uiso 1 1 calc R . . C13 C 1.0944(3) 0.0163(3) 0.41984(14) 0.0584(8) Uani 1 1 d . . . C14 C 1.0612(5) -0.0857(3) 0.41812(17) 0.0747(10) Uani 1 1 d . . . H14 H 1.1220 -0.1204 0.3887 0.090 Uiso 1 1 calc R . . H15 H 0.9759 -0.0876 0.4086 0.090 Uiso 1 1 calc R . . H16 H 1.0633 -0.1174 0.4560 0.090 Uiso 1 1 calc R . . C15 C 1.0668(3) 0.0994(2) 0.38864(13) 0.0520(7) Uani 1 1 d . . . C16 C 0.9902(3) 0.1173(2) 0.34317(12) 0.0484(6) Uani 1 1 d . . . C17 C 0.7792(3) 0.0210(2) 0.27121(15) 0.0582(7) Uani 1 1 d . . . C18 C 0.7127(3) 0.0567(3) 0.22387(15) 0.0586(7) Uani 1 1 d . . . C19 C 0.6296(4) 0.0019(3) 0.2008(2) 0.0763(11) Uani 1 1 d . . . H19 H 0.6140 -0.0628 0.2147 0.092 Uiso 1 1 calc R . . C20 C 0.5694(4) 0.0427(3) 0.15720(19) 0.0772(11) Uani 1 1 d . . . H20 H 0.5109 0.0068 0.1413 0.093 Uiso 1 1 calc R . . C21 C 0.5962(4) 0.1361(3) 0.13739(19) 0.0787(12) Uani 1 1 d . . . H21 H 0.5560 0.1661 0.1077 0.094 Uiso 1 1 calc R . . C22 C 0.6814(4) 0.1847(3) 0.16116(16) 0.0681(9) Uani 1 1 d . . . H22 H 0.7014 0.2482 0.1463 0.082 Uiso 1 1 calc R . . C23 C 1.2775(8) 0.5968(5) 0.1476(3) 0.129(2) Uani 1 1 d . . . H23 H 1.2792 0.6527 0.1225 0.155 Uiso 1 1 calc R . . C24 C 1.3266(5) 0.4497(3) 0.18035(17) 0.0795(12) Uani 1 1 d . . . C25 C 1.3963(5) 0.3542(4) 0.1826(2) 0.1000(16) Uani 1 1 d . . . H25 H 1.4856 0.3609 0.1661 0.120 Uiso 1 1 calc R . . H26 H 1.3603 0.3069 0.1603 0.120 Uiso 1 1 calc R . . H27 H 1.3895 0.3311 0.2228 0.120 Uiso 1 1 calc R . . C26 C 1.2236(4) 0.4922(3) 0.21455(18) 0.0751(10) Uani 1 1 d . . . C27 C 1.1504(4) 0.4471(3) 0.26485(16) 0.0645(9) Uani 1 1 d . . . C28 C 0.8667(3) 0.4824(2) 0.36099(17) 0.0609(8) Uani 1 1 d . . . C29 C 0.8147(3) 0.4294(3) 0.41567(15) 0.0592(8) Uani 1 1 d . . . C30 C 0.7102(4) 0.4639(3) 0.4527(2) 0.0731(10) Uani 1 1 d . . . H31 H 0.6666 0.5238 0.4446 0.088 Uiso 1 1 calc R . . C31 C 0.6691(4) 0.4095(3) 0.50257(19) 0.0758(10) Uani 1 1 d . . . H32 H 0.5976 0.4324 0.5294 0.091 Uiso 1 1 calc R . . C32 C 0.7314(4) 0.3244(3) 0.51244(17) 0.0725(10) Uani 1 1 d . . . H33 H 0.7032 0.2852 0.5456 0.087 Uiso 1 1 calc R . . C33 C 0.8381(3) 0.2944(3) 0.47322(14) 0.0606(8) Uani 1 1 d . . . H34 H 0.8831 0.2346 0.4804 0.073 Uiso 1 1 calc R . . C34 C 1.3472(5) -0.0985(4) 0.32207(18) 0.0860(13) Uani 1 1 d . . . H35 H 1.3618 -0.1592 0.3412 0.103 Uiso 1 1 calc R . . C35 C 1.3560(3) 0.0574(3) 0.29783(15) 0.0679(9) Uani 1 1 d . . . C36 C 1.3898(4) 0.1614(4) 0.29884(19) 0.0814(12) Uani 1 1 d . . . H37 H 1.4048 0.1765 0.3376 0.098 Uiso 1 1 calc R . . H38 H 1.3202 0.2047 0.2889 0.098 Uiso 1 1 calc R . . H39 H 1.4666 0.1714 0.2707 0.098 Uiso 1 1 calc R . . C37 C 1.2838(3) 0.0109(3) 0.26543(15) 0.0634(8) Uani 1 1 d . . . C38 C 1.2183(3) 0.0527(3) 0.22005(15) 0.0593(8) Uani 1 1 d . . . C39 C 1.0013(3) -0.0140(3) 0.13532(16) 0.0619(8) Uani 1 1 d . . . C40 C 0.9480(3) 0.0389(3) 0.08819(15) 0.0601(8) Uani 1 1 d . . . C41 C 0.8582(4) -0.0002(3) 0.05998(19) 0.0731(10) Uani 1 1 d . . . H43 H 0.8281 -0.0632 0.0705 0.088 Uiso 1 1 calc R . . C42 C 0.8144(4) 0.0548(4) 0.01664(19) 0.0808(12) Uani 1 1 d . . . H44 H 0.7546 0.0289 -0.0035 0.097 Uiso 1 1 calc R . . C43 C 0.8552(5) 0.1452(4) 0.00235(19) 0.0827(12) Uani 1 1 d . . . H45 H 0.8239 0.1839 -0.0270 0.099 Uiso 1 1 calc R . . C44 C 0.9456(4) 0.1799(3) 0.03246(17) 0.0715(10) Uani 1 1 d . . . H46 H 0.9754 0.2432 0.0227 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mn1 0.0578(3) 0.0610(3) 0.0529(3) -0.0073(2) -0.0137(2) -0.0115(2) Mn2 0.0496(3) 0.0471(2) 0.0482(3) 0.00240(17) -0.01670(19) -0.00367(18) Mn3 0.0509(3) 0.0546(3) 0.0534(3) 0.00159(19) -0.0149(2) -0.0082(2) O1 0.0638(13) 0.0487(10) 0.0496(11) -0.0003(8) -0.0158(9) -0.0048(9) O2 0.0502(10) 0.0466(10) 0.0494(10) 0.0049(8) -0.0191(9) -0.0070(8) O3 0.0637(14) 0.0626(13) 0.0587(13) -0.0010(10) -0.0037(11) -0.0158(11) O4 0.0647(14) 0.0655(14) 0.0624(13) -0.0129(11) -0.0240(11) -0.0035(11) O5 0.0703(16) 0.103(2) 0.0815(18) -0.0339(16) -0.0117(14) -0.0041(15) O6 0.0549(13) 0.0831(17) 0.0882(18) -0.0184(14) -0.0294(13) -0.0094(12) O7 0.0882(19) 0.092(2) 0.0780(18) 0.0259(15) -0.0279(15) -0.0136(16) N1 0.083(2) 0.0731(18) 0.0498(15) -0.0039(13) -0.0085(14) -0.0256(16) N2 0.143(4) 0.094(3) 0.094(3) 0.034(2) 0.007(3) -0.038(3) N3 0.0739(18) 0.0556(14) 0.0528(14) 0.0089(11) -0.0164(13) -0.0048(14) N4 0.0659(16) 0.0502(13) 0.0540(14) 0.0042(11) -0.0201(13) 0.0010(12) N5 0.0722(19) 0.0559(16) 0.101(2) 0.0163(15) -0.0228(18) 0.0093(14) N6 0.0469(12) 0.0523(13) 0.0571(14) -0.0043(11) -0.0188(11) -0.0005(10) N7 0.0536(14) 0.0670(16) 0.0538(14) 0.0106(12) -0.0195(12) -0.0099(12) N8 0.0737(18) 0.0726(18) 0.0542(15) 0.0132(13) -0.0243(14) 0.0038(15) N9 0.0523(13) 0.0534(13) 0.0584(14) 0.0075(11) -0.0172(12) -0.0087(11) N10 0.0486(13) 0.0497(12) 0.0571(14) 0.0048(10) -0.0171(11) -0.0076(10) N11 0.113(3) 0.0682(19) 0.098(3) 0.0147(17) -0.037(2) -0.0446(19) N12 0.0519(14) 0.0559(14) 0.0647(16) -0.0086(12) -0.0221(12) -0.0005(11) N13 0.129(4) 0.087(3) 0.108(3) 0.035(2) -0.012(3) -0.022(2) N14 0.147(4) 0.117(4) 0.072(2) 0.013(2) 0.006(3) -0.057(3) N15 0.0691(18) 0.0602(15) 0.0625(16) 0.0117(12) -0.0177(14) -0.0097(14) N16 0.0586(15) 0.0573(15) 0.0578(15) 0.0067(11) -0.0149(12) -0.0093(12) N17 0.073(2) 0.0623(18) 0.112(3) 0.0161(17) -0.019(2) 0.0014(16) N18 0.0515(14) 0.0637(15) 0.0534(14) -0.0004(11) -0.0199(11) -0.0113(12) N19 0.093(2) 0.079(2) 0.0672(19) -0.0062(16) -0.0252(18) 0.0163(19) N20 0.0702(19) 0.100(3) 0.0588(17) -0.0037(16) -0.0213(15) 0.0133(18) N21 0.0626(17) 0.0682(17) 0.0690(18) 0.0017(14) -0.0240(14) -0.0070(14) N22 0.0608(16) 0.0609(15) 0.0614(15) 0.0006(12) -0.0251(13) -0.0128(12) N23 0.078(2) 0.0627(17) 0.099(2) -0.0008(16) -0.0368(19) -0.0174(15) N24 0.0657(17) 0.0615(16) 0.0584(15) -0.0120(12) -0.0185(13) -0.0032(13) C1 0.097(3) 0.092(3) 0.068(2) 0.009(2) 0.002(2) -0.026(3) C2 0.110(4) 0.076(3) 0.081(3) 0.014(2) 0.002(3) -0.018(2) C3 0.197(7) 0.063(3) 0.164(6) 0.047(3) -0.003(6) -0.004(4) C4 0.079(2) 0.0599(18) 0.0568(18) 0.0053(14) -0.0105(17) -0.0140(17) C5 0.077(2) 0.0521(16) 0.0512(16) 0.0073(12) -0.0245(15) -0.0177(16) C6 0.066(2) 0.0483(15) 0.072(2) -0.0022(14) -0.0251(17) -0.0034(14) C7 0.0525(16) 0.0494(15) 0.0672(19) -0.0042(13) -0.0223(14) -0.0002(13) C8 0.059(2) 0.064(2) 0.092(3) -0.0068(19) -0.0199(19) 0.0106(17) C9 0.0545(19) 0.077(2) 0.096(3) -0.026(2) -0.0150(19) 0.0051(18) C10 0.0554(18) 0.077(2) 0.064(2) -0.0115(17) -0.0118(15) -0.0119(16) C11 0.0567(17) 0.0622(18) 0.0584(17) -0.0010(14) -0.0200(14) -0.0135(14) C12 0.069(2) 0.081(2) 0.0590(19) 0.0105(16) -0.0264(17) -0.0078(18) C13 0.0593(18) 0.0665(19) 0.0488(16) 0.0055(13) -0.0127(14) 0.0076(15) C14 0.096(3) 0.065(2) 0.065(2) 0.0092(16) -0.024(2) 0.011(2) C15 0.0574(17) 0.0526(15) 0.0460(14) 0.0060(12) -0.0104(13) -0.0018(13) C16 0.0473(14) 0.0521(15) 0.0451(14) 0.0044(11) -0.0072(11) -0.0019(12) C17 0.0584(17) 0.0515(16) 0.068(2) 0.0022(14) -0.0186(15) -0.0123(14) C18 0.0507(16) 0.0660(19) 0.0622(18) -0.0043(14) -0.0164(14) -0.0072(14) C19 0.061(2) 0.084(3) 0.091(3) -0.019(2) -0.025(2) -0.0150(19) C20 0.060(2) 0.097(3) 0.083(3) -0.027(2) -0.0296(19) -0.008(2) C21 0.073(2) 0.094(3) 0.078(2) -0.025(2) -0.038(2) 0.011(2) C22 0.075(2) 0.072(2) 0.066(2) -0.0129(16) -0.0359(18) 0.0042(18) C23 0.175(7) 0.121(5) 0.088(4) 0.044(3) -0.005(4) -0.050(5) C24 0.103(3) 0.087(3) 0.0520(19) -0.0016(17) -0.011(2) -0.042(2) C25 0.106(4) 0.122(4) 0.066(3) -0.016(3) 0.011(2) -0.024(3) C26 0.085(3) 0.073(2) 0.069(2) 0.0048(18) -0.014(2) -0.023(2) C27 0.077(2) 0.0623(19) 0.0594(19) 0.0071(15) -0.0213(17) -0.0261(17) C28 0.0574(18) 0.0532(16) 0.079(2) 0.0006(15) -0.0301(17) -0.0080(14) C29 0.0566(17) 0.0629(18) 0.0639(19) -0.0121(14) -0.0211(15) -0.0142(15) C30 0.0533(18) 0.074(2) 0.093(3) -0.013(2) -0.0150(18) -0.0048(17) C31 0.059(2) 0.095(3) 0.074(2) -0.017(2) -0.0065(18) -0.010(2) C32 0.062(2) 0.099(3) 0.059(2) -0.0058(19) -0.0136(16) -0.015(2) C33 0.0560(17) 0.078(2) 0.0526(17) 0.0052(15) -0.0178(14) -0.0179(16) C34 0.102(3) 0.090(3) 0.064(2) 0.000(2) -0.018(2) 0.019(3) C35 0.0551(18) 0.094(3) 0.0525(17) -0.0051(17) -0.0078(15) 0.0080(18) C36 0.075(2) 0.109(3) 0.067(2) -0.004(2) -0.028(2) -0.016(2) C37 0.0583(18) 0.082(2) 0.0521(17) -0.0095(15) -0.0169(14) 0.0057(17) C38 0.0508(16) 0.069(2) 0.0581(18) -0.0101(15) -0.0115(14) 0.0052(15) C39 0.0569(18) 0.068(2) 0.0628(19) -0.0024(15) -0.0142(15) -0.0104(15) C40 0.0570(18) 0.0631(18) 0.0633(19) -0.0176(15) -0.0163(15) -0.0025(15) C41 0.068(2) 0.073(2) 0.085(3) -0.0188(19) -0.025(2) -0.0119(18) C42 0.079(3) 0.094(3) 0.081(3) -0.029(2) -0.042(2) -0.005(2) C43 0.090(3) 0.096(3) 0.069(2) -0.012(2) -0.037(2) 0.009(2) C44 0.087(3) 0.066(2) 0.065(2) -0.0070(16) -0.0252(19) -0.0011(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O5 2.175(3) . ? Mn1 O1 2.178(2) . ? Mn1 N22 2.184(3) . ? Mn1 N1 2.189(3) . ? Mn1 O4 2.207(2) . ? Mn1 N24 2.320(3) . ? Mn2 N10 2.157(3) . ? Mn2 N4 2.160(3) . ? Mn2 O1 2.181(2) . ? Mn2 O2 2.1880(19) . ? Mn2 N6 2.325(3) . ? Mn2 N12 2.340(3) . ? Mn3 O6 2.178(2) . ? Mn3 O3 2.180(2) . ? Mn3 N7 2.183(3) . ? Mn3 N16 2.190(3) . ? Mn3 O2 2.204(2) . ? Mn3 N18 2.321(3) . ? O1 C5 1.319(4) . ? O2 C16 1.304(3) . ? O3 C27 1.241(4) . ? O4 C38 1.240(4) . ? N1 C1 1.302(5) . ? N1 C4 1.370(5) . ? N2 C1 1.302(7) . ? N2 C2 1.383(7) . ? N3 C5 1.300(5) . ? N3 N4 1.402(4) . ? N4 C6 1.278(5) . ? N5 C6 1.352(4) . ? N6 C11 1.329(4) . ? N6 C7 1.352(4) . ? N7 C12 1.317(4) . ? N7 C15 1.383(4) . ? N8 C12 1.341(5) . ? N8 C13 1.374(5) . ? N9 C16 1.298(4) . ? N9 N10 1.406(3) . ? N10 C17 1.296(4) . ? N11 C17 1.339(4) . ? N12 C22 1.338(4) . ? N12 C18 1.347(4) . ? N13 C23 1.313(8) . ? N13 C26 1.407(6) . ? N14 C23 1.362(9) . ? N14 C24 1.364(6) . ? N15 C27 1.346(5) . ? N15 N16 1.381(4) . ? N16 C28 1.280(5) . ? N17 C28 1.349(4) . ? N18 C29 1.325(5) . ? N18 C33 1.326(4) . ? N19 C34 1.320(5) . ? N19 C37 1.369(5) . ? N20 C34 1.346(6) . ? N20 C35 1.356(5) . ? N21 C38 1.343(5) . ? N21 N22 1.365(4) . ? N22 C39 1.304(4) . ? N23 C39 1.339(5) . ? N24 C44 1.335(5) . ? N24 C40 1.346(5) . ? C2 C4 1.367(5) . ? C2 C3 1.492(8) . ? C4 C5 1.484(5) . ? C6 C7 1.480(5) . ? C7 C8 1.384(5) . ? C8 C9 1.379(6) . ? C9 C10 1.386(6) . ? C10 C11 1.381(5) . ? C13 C15 1.378(4) . ? C13 C14 1.466(5) . ? C15 C16 1.460(4) . ? C17 C18 1.475(5) . ? C18 C19 1.386(5) . ? C19 C20 1.385(6) . ? C20 C21 1.378(7) . ? C21 C22 1.363(5) . ? C24 C26 1.363(7) . ? C24 C25 1.470(7) . ? C26 C27 1.448(5) . ? C28 C29 1.496(5) . ? C29 C30 1.368(5) . ? C30 C31 1.390(6) . ? C31 C32 1.341(6) . ? C32 C33 1.393(5) . ? C35 C37 1.369(5) . ? C35 C36 1.491(6) . ? C37 C38 1.457(5) . ? C39 C40 1.480(5) . ? C40 C41 1.398(5) . ? C41 C42 1.377(6) . ? C42 C43 1.351(7) . ? C43 C44 1.405(6) . ? 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 O5 Mn1 O1 166.84(11) . . ? O5 Mn1 N22 91.12(12) . . ? O1 Mn1 N22 100.42(10) . . ? O5 Mn1 N1 95.17(13) . . ? O1 Mn1 N1 75.44(10) . . ? N22 Mn1 N1 163.60(12) . . ? O5 Mn1 O4 87.04(11) . . ? O1 Mn1 O4 90.62(8) . . ? N22 Mn1 O4 71.44(10) . . ? N1 Mn1 O4 123.93(11) . . ? O5 Mn1 N24 97.69(10) . . ? O1 Mn1 N24 92.24(9) . . ? N22 Mn1 N24 70.01(10) . . ? N1 Mn1 N24 94.10(11) . . ? O4 Mn1 N24 141.22(11) . . ? N10 Mn2 N4 158.09(11) . . ? N10 Mn2 O1 122.20(9) . . ? N4 Mn2 O1 72.13(10) . . ? N10 Mn2 O2 71.09(8) . . ? N4 Mn2 O2 125.44(9) . . ? O1 Mn2 O2 101.00(8) . . ? N10 Mn2 N6 95.76(10) . . ? N4 Mn2 N6 70.03(10) . . ? O1 Mn2 N6 141.68(9) . . ? O2 Mn2 N6 95.88(8) . . ? N10 Mn2 N12 70.28(10) . . ? N4 Mn2 N12 93.00(10) . . ? O1 Mn2 N12 95.80(9) . . ? O2 Mn2 N12 141.14(9) . . ? N6 Mn2 N12 92.04(9) . . ? O6 Mn3 O3 94.21(10) . . ? O6 Mn3 N7 90.15(11) . . ? O3 Mn3 N7 119.99(10) . . ? O6 Mn3 N16 96.06(10) . . ? O3 Mn3 N16 71.69(10) . . ? N7 Mn3 N16 166.43(11) . . ? O6 Mn3 O2 165.41(9) . . ? O3 Mn3 O2 94.64(8) . . ? N7 Mn3 O2 75.37(9) . . ? N16 Mn3 O2 97.73(9) . . ? O6 Mn3 N18 88.70(10) . . ? O3 Mn3 N18 141.85(10) . . ? N7 Mn3 N18 98.00(10) . . ? N16 Mn3 N18 70.18(10) . . ? O2 Mn3 N18 91.48(9) . . ? C5 O1 Mn1 116.9(2) . . ? C5 O1 Mn2 112.7(2) . . ? Mn1 O1 Mn2 127.93(10) . . ? C16 O2 Mn2 114.68(17) . . ? C16 O2 Mn3 115.65(17) . . ? Mn2 O2 Mn3 126.77(9) . . ? C27 O3 Mn3 118.1(2) . . ? C38 O4 Mn1 116.2(2) . . ? C1 N1 C4 105.2(4) . . ? C1 N1 Mn1 141.4(3) . . ? C4 N1 Mn1 113.3(2) . . ? C1 N2 C2 108.5(4) . . ? C5 N3 N4 108.5(3) . . ? C6 N4 N3 116.2(3) . . ? C6 N4 Mn2 124.1(2) . . ? N3 N4 Mn2 119.5(2) . . ? C11 N6 C7 118.5(3) . . ? C11 N6 Mn2 125.9(2) . . ? C7 N6 Mn2 115.3(2) . . ? C12 N7 C15 105.9(3) . . ? C12 N7 Mn3 140.6(3) . . ? C15 N7 Mn3 112.83(19) . . ? C12 N8 C13 109.0(3) . . ? C16 N9 N10 109.4(2) . . ? C17 N10 N9 116.3(3) . . ? C17 N10 Mn2 123.6(2) . . ? N9 N10 Mn2 119.64(18) . . ? C22 N12 C18 117.9(3) . . ? C22 N12 Mn2 126.6(2) . . ? C18 N12 Mn2 115.3(2) . . ? C23 N13 C26 102.7(5) . . ? C23 N14 C24 107.6(5) . . ? C27 N15 N16 114.8(3) . . ? C28 N16 N15 121.7(3) . . ? C28 N16 Mn3 123.0(2) . . ? N15 N16 Mn3 115.0(2) . . ? C29 N18 C33 118.9(3) . . ? C29 N18 Mn3 116.2(2) . . ? C33 N18 Mn3 124.3(2) . . ? C34 N19 C37 104.7(4) . . ? C34 N20 C35 108.6(3) . . ? C38 N21 N22 114.4(3) . . ? C39 N22 N21 119.9(3) . . ? C39 N22 Mn1 124.1(2) . . ? N21 N22 Mn1 115.9(2) . . ? C44 N24 C40 118.2(3) . . ? C44 N24 Mn1 125.3(3) . . ? C40 N24 Mn1 116.5(2) . . ? N1 C1 N2 112.5(4) . . ? C4 C2 N2 103.7(4) . . ? C4 C2 C3 132.8(5) . . ? N2 C2 C3 123.5(5) . . ? C2 C4 N1 110.0(4) . . ? C2 C4 C5 132.1(4) . . ? N1 C4 C5 117.8(3) . . ? N3 C5 O1 127.1(3) . . ? N3 C5 C4 118.6(3) . . ? O1 C5 C4 114.3(3) . . ? N4 C6 N5 124.7(4) . . ? N4 C6 C7 114.8(3) . . ? N5 C6 C7 120.5(3) . . ? N6 C7 C8 121.4(3) . . ? N6 C7 C6 114.5(3) . . ? C8 C7 C6 124.1(3) . . ? C9 C8 C7 119.4(3) . . ? C8 C9 C10 119.2(4) . . ? C11 C10 C9 118.0(4) . . ? N6 C11 C10 123.4(3) . . ? N7 C12 N8 110.8(3) . . ? N8 C13 C15 104.4(3) . . ? N8 C13 C14 122.5(3) . . ? C15 C13 C14 133.0(3) . . ? C13 C15 N7 109.8(3) . . ? C13 C15 C16 132.4(3) . . ? N7 C15 C16 117.9(3) . . ? N9 C16 O2 125.0(3) . . ? N9 C16 C15 118.9(3) . . ? O2 C16 C15 116.1(3) . . ? N10 C17 N11 124.1(3) . . ? N10 C17 C18 115.1(3) . . ? N11 C17 C18 120.8(3) . . ? N12 C18 C19 121.6(3) . . ? N12 C18 C17 114.9(3) . . ? C19 C18 C17 123.5(3) . . ? C20 C19 C18 119.3(4) . . ? C21 C20 C19 118.7(4) . . ? C22 C21 C20 118.8(4) . . ? N12 C22 C21 123.7(4) . . ? N13 C23 N14 113.1(5) . . ? C26 C24 N14 104.9(5) . . ? C26 C24 C25 133.1(4) . . ? N14 C24 C25 122.0(5) . . ? C24 C26 N13 111.6(4) . . ? C24 C26 C27 125.8(4) . . ? N13 C26 C27 122.6(4) . . ? O3 C27 N15 120.3(3) . . ? O3 C27 C26 122.4(4) . . ? N15 C27 C26 117.3(3) . . ? N16 C28 N17 126.0(4) . . ? N16 C28 C29 114.9(3) . . ? N17 C28 C29 119.1(4) . . ? N18 C29 C30 122.2(4) . . ? N18 C29 C28 114.9(3) . . ? C30 C29 C28 122.9(3) . . ? C29 C30 C31 118.7(4) . . ? C32 C31 C30 119.3(4) . . ? C31 C32 C33 118.9(4) . . ? N18 C33 C32 122.0(4) . . ? N19 C34 N20 111.1(4) . . ? N20 C35 C37 104.5(4) . . ? N20 C35 C36 123.4(4) . . ? C37 C35 C36 132.1(4) . . ? C35 C37 N19 111.0(3) . . ? C35 C37 C38 128.0(4) . . ? N19 C37 C38 121.0(3) . . ? O4 C38 N21 121.6(3) . . ? O4 C38 C37 122.4(3) . . ? N21 C38 C37 116.0(3) . . ? N22 C39 N23 125.9(3) . . ? N22 C39 C40 113.8(3) . . ? N23 C39 C40 120.3(3) . . ? N24 C40 C41 121.8(4) . . ? N24 C40 C39 115.5(3) . . ? C41 C40 C39 122.7(4) . . ? C42 C41 C40 118.3(4) . . ? C43 C42 C41 121.0(4) . . ? C42 C43 C44 117.6(4) . . ? N24 C44 C43 123.1(4) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.945 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.082 #===END data_shelxl_3 _database_code_depnum_ccdc_archive 'CCDC 674830' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H56 Cu4 N32 O16' _chemical_formula_weight 1639.45 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' Cu Cu 0.3201 1.2651 '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 tetragonal _symmetry_space_group_name_H-M 'I 41/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x+1/2, -y, z+1/2' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1, -y+1/2, z+1' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x-1/2, y, -z-1/2' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x, y+1/2, -z' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 18.9374(11) _cell_length_b 18.9374(11) _cell_length_c 18.2748(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6553.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 12295 _cell_measurement_theta_min 2.1508 _cell_measurement_theta_max 30.8436 _exptl_crystal_description Prism _exptl_crystal_colour Green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 1.373 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.7720 _exptl_absorpt_correction_T_max 0.8541 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 29320 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3757 _reflns_number_gt 3694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _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^)+(0.0575P)^2^+10.6681P] 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 3757 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1070 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 Cu1 Cu -0.002074(13) 0.398738(13) 0.106242(13) 0.02285(11) Uani 1 1 d . . . O1 O -0.07693(8) 0.32795(8) 0.08369(8) 0.0252(3) Uani 1 1 d . . . O2 O 0.31976(10) 0.44761(9) 0.07727(10) 0.0402(4) Uani 1 1 d . . . O3 O 0.39621(12) 0.50182(13) 0.00971(13) 0.0595(6) Uani 1 1 d . . . O4 O 0.32069(11) 0.43198(11) -0.04009(10) 0.0507(5) Uani 1 1 d . . . N1 N -0.16545(9) 0.22482(9) 0.04091(9) 0.0242(3) Uani 1 1 d . . . N2 N -0.19289(10) 0.18343(10) -0.06687(10) 0.0295(4) Uani 1 1 d . . . H2 H -0.2136 0.1577 -0.1007 0.035 Uiso 1 1 calc R . . N3 N -0.03519(9) 0.34465(9) -0.03500(10) 0.0253(4) Uani 1 1 d . . . N4 N 0.00851(9) 0.39015(9) 0.00321(10) 0.0246(4) Uani 1 1 d . . . N5 N 0.06361(10) 0.42700(11) -0.10445(10) 0.0316(4) Uani 1 1 d . . . H6 H 0.0358 0.3985 -0.1283 0.038 Uiso 1 1 d . . . H7 H 0.1008 0.4400 -0.1242 0.038 Uiso 1 1 d . . . N6 N 0.07599(9) 0.47198(9) 0.08752(10) 0.0257(4) Uani 1 1 d . . . N7 N 0.34583(11) 0.46035(11) 0.01487(11) 0.0349(4) Uani 1 1 d . . . N8 N 0.37249(16) 0.74564(16) 0.00211(16) 0.0594(7) Uani 1 1 d . . . C1 C -0.20423(11) 0.17786(12) 0.00556(12) 0.0280(4) Uani 1 1 d . . . H1 H -0.2354 0.1451 0.0280 0.034 Uiso 1 1 calc R . . C2 C -0.14414(11) 0.23541(12) -0.07972(12) 0.0269(4) Uani 1 1 d . . . C3 C -0.11912(15) 0.25415(14) -0.15485(12) 0.0370(5) Uani 1 1 d . . . H3 H -0.1599 0.2610 -0.1871 0.044 Uiso 1 1 calc R . . H4 H -0.0896 0.2159 -0.1740 0.044 Uiso 1 1 calc R . . H5 H -0.0914 0.2978 -0.1527 0.044 Uiso 1 1 calc R . . C4 C -0.12718(11) 0.26136(11) -0.01190(11) 0.0235(4) Uani 1 1 d . . . C5 C -0.07689(10) 0.31456(11) 0.01321(11) 0.0235(4) Uani 1 1 d . . . C6 C 0.05634(11) 0.42625(11) -0.03149(11) 0.0250(4) Uani 1 1 d . . . C7 C 0.09923(11) 0.47145(11) 0.01756(12) 0.0253(4) Uani 1 1 d . . . C8 C 0.15748(12) 0.51035(12) -0.00422(13) 0.0318(5) Uani 1 1 d . . . H8 H 0.1731 0.5095 -0.0536 0.038 Uiso 1 1 calc R . . C9 C 0.19260(12) 0.55066(12) 0.04807(14) 0.0350(5) Uani 1 1 d . . . H9 H 0.2338 0.5764 0.0351 0.042 Uiso 1 1 calc R . . C10 C 0.16720(12) 0.55304(12) 0.11906(14) 0.0339(5) Uani 1 1 d . . . H10 H 0.1895 0.5817 0.1549 0.041 Uiso 1 1 calc R . . C11 C 0.10874(12) 0.51296(12) 0.13669(13) 0.0301(5) Uani 1 1 d . . . H11 H 0.0911 0.5145 0.1853 0.036 Uiso 1 1 calc R . . C12 C 0.35332(19) 0.7439(2) 0.14301(17) 0.0635(11) Uani 1 1 d . . . H12 H 0.3213 0.7054 0.1565 0.076 Uiso 1 1 calc R . . H13 H 0.3328 0.7891 0.1583 0.076 Uiso 1 1 calc R . . H14 H 0.3989 0.7372 0.1674 0.076 Uiso 1 1 calc R . . C13 C 0.36368(16) 0.74404(16) 0.06357(16) 0.0456(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02464(15) 0.02629(16) 0.01763(16) 0.00171(9) 0.00061(9) -0.00080(9) O1 0.0278(7) 0.0300(7) 0.0179(6) 0.0004(6) 0.0005(5) -0.0039(6) O2 0.0505(10) 0.0385(9) 0.0314(9) 0.0089(7) -0.0011(8) 0.0061(8) O3 0.0528(12) 0.0621(13) 0.0637(14) 0.0064(11) -0.0092(11) -0.0273(10) O4 0.0599(12) 0.0606(12) 0.0317(10) 0.0022(9) -0.0086(9) -0.0207(10) N1 0.0242(8) 0.0277(8) 0.0207(8) -0.0002(7) 0.0018(6) 0.0010(7) N2 0.0296(9) 0.0350(10) 0.0240(9) -0.0074(7) -0.0013(7) -0.0004(7) N3 0.0255(8) 0.0306(9) 0.0200(8) -0.0005(7) 0.0001(6) -0.0008(7) N4 0.0258(8) 0.0286(8) 0.0193(8) 0.0017(6) 0.0006(7) -0.0005(7) N5 0.0285(9) 0.0439(11) 0.0225(9) 0.0052(8) 0.0044(7) -0.0025(8) N6 0.0250(8) 0.0257(8) 0.0263(9) 0.0037(7) 0.0000(7) 0.0010(7) N7 0.0359(10) 0.0354(10) 0.0332(10) 0.0095(8) -0.0073(8) -0.0030(8) N8 0.0656(17) 0.0725(19) 0.0401(15) 0.0006(12) 0.0013(13) 0.0114(14) C1 0.0265(10) 0.0316(11) 0.0259(10) -0.0044(8) 0.0018(8) -0.0006(8) C2 0.0275(10) 0.0311(10) 0.0221(10) -0.0026(8) -0.0007(8) 0.0030(8) C3 0.0456(14) 0.0442(14) 0.0211(10) -0.0030(9) 0.0019(10) -0.0014(11) C4 0.0242(9) 0.0270(10) 0.0193(9) 0.0004(7) 0.0007(7) 0.0001(8) C5 0.0251(9) 0.0259(9) 0.0193(9) 0.0028(7) -0.0004(7) 0.0039(7) C6 0.0236(9) 0.0279(10) 0.0235(10) 0.0053(8) 0.0017(7) 0.0042(7) C7 0.0239(9) 0.0259(10) 0.0261(10) 0.0055(8) -0.0006(8) 0.0032(7) C8 0.0300(11) 0.0339(11) 0.0315(11) 0.0063(9) 0.0025(9) 0.0000(9) C9 0.0292(11) 0.0324(11) 0.0433(13) 0.0080(10) -0.0012(10) -0.0042(9) C10 0.0333(12) 0.0279(11) 0.0405(13) 0.0005(9) -0.0089(10) -0.0009(9) C11 0.0312(11) 0.0298(11) 0.0293(11) 0.0008(8) -0.0053(9) 0.0005(9) C12 0.061(2) 0.096(3) 0.0331(18) 0.0026(15) 0.0046(13) 0.0144(18) C13 0.0469(15) 0.0540(16) 0.0357(15) 0.0012(11) -0.0014(11) 0.0089(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 Cu1 N4 1.9005(19) . ? Cu1 N1 1.9556(17) 14 ? Cu1 O1 1.9940(14) . ? Cu1 N6 2.0557(18) . ? Cu1 O1 2.3132(14) 14 ? O1 C5 1.313(2) . ? O1 Cu1 2.3131(14) 12_666 ? O2 N7 1.266(3) . ? O3 N7 1.239(3) . ? O4 N7 1.235(3) . ? N1 C1 1.322(3) . ? N1 C4 1.391(3) . ? N1 Cu1 1.9556(17) 12_666 ? N2 C1 1.345(3) . ? N2 C2 1.370(3) . ? N3 C5 1.313(3) . ? N3 N4 1.384(2) . ? N4 C6 1.300(3) . ? N5 C6 1.340(3) . ? N6 C11 1.340(3) . ? N6 C7 1.352(3) . ? N8 C13 1.136(4) . ? C2 C4 1.371(3) . ? C2 C3 1.495(3) . ? C4 C5 1.460(3) . ? C6 C7 1.482(3) . ? C7 C8 1.385(3) . ? C8 C9 1.392(3) . ? C9 C10 1.384(4) . ? C10 C11 1.380(3) . ? C12 C13 1.465(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 N4 Cu1 N1 171.75(7) . 14 ? N4 Cu1 O1 79.21(7) . . ? N1 Cu1 O1 98.53(6) 14 . ? N4 Cu1 N6 79.46(7) . . ? N1 Cu1 N6 102.22(7) 14 . ? O1 Cu1 N6 158.49(7) . . ? N4 Cu1 O1 110.53(7) . 14 ? N1 Cu1 O1 77.62(6) 14 14 ? O1 Cu1 O1 99.71(8) . 14 ? N6 Cu1 O1 90.26(6) . 14 ? C5 O1 Cu1 109.41(12) . . ? C5 O1 Cu1 109.84(12) . 12_666 ? Cu1 O1 Cu1 139.49(7) . 12_666 ? C1 N1 C4 106.56(17) . . ? C1 N1 Cu1 135.25(15) . 12_666 ? C4 N1 Cu1 118.10(14) . 12_666 ? C1 N2 C2 109.43(18) . . ? C5 N3 N4 106.94(17) . . ? C6 N4 N3 119.87(18) . . ? C6 N4 Cu1 120.78(15) . . ? N3 N4 Cu1 119.35(13) . . ? C11 N6 C7 119.19(19) . . ? C11 N6 Cu1 127.75(15) . . ? C7 N6 Cu1 112.73(14) . . ? O4 N7 O3 120.7(2) . . ? O4 N7 O2 120.0(2) . . ? O3 N7 O2 119.3(2) . . ? N1 C1 N2 109.85(19) . . ? N2 C2 C4 105.09(19) . . ? N2 C2 C3 122.8(2) . . ? C4 C2 C3 132.1(2) . . ? C2 C4 N1 109.07(18) . . ? C2 C4 C5 133.15(19) . . ? N1 C4 C5 117.71(18) . . ? O1 C5 N3 125.08(19) . . ? O1 C5 C4 116.18(17) . . ? N3 C5 C4 118.74(18) . . ? N4 C6 N5 124.2(2) . . ? N4 C6 C7 112.99(18) . . ? N5 C6 C7 122.63(19) . . ? N6 C7 C8 121.8(2) . . ? N6 C7 C6 113.45(18) . . ? C8 C7 C6 124.7(2) . . ? C7 C8 C9 118.4(2) . . ? C10 C9 C8 119.7(2) . . ? C11 C10 C9 118.7(2) . . ? N6 C11 C10 122.2(2) . . ? N8 C13 C12 178.4(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.577 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.070 #===END data_shelxl_4 _database_code_depnum_ccdc_archive 'CCDC 674831' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H50 F15 N24 Ni4 O16 P S3' _chemical_formula_weight 1854.10 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 42.677(3) _cell_length_b 42.677(3) _cell_length_c 22.0593(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 34795(4) _cell_formula_units_Z 18 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 38262 _cell_measurement_theta_min 2.1502 _cell_measurement_theta_max 30.9129 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 16884 _exptl_absorpt_coefficient_mu 1.170 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.5944 _exptl_absorpt_correction_T_max 0.8270 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_reflns_number 130730 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -53 _diffrn_reflns_limit_h_max 53 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.50 _reflns_number_total 16011 _reflns_number_gt 14990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _computing_publication_material 'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)' _platon_squeeze_details ; The Platon Squeeze procedure was applied to recover 828.5 electrons per unit cell in three voids (total volume 6820.1 A^3); that is 46.03 electrons per formula unit. An area of disperse electron density appeared to be present prior to the application of Squeeze, which is presumed to be the 2/3-occupancy hexafluorophosphate anion, though a good point atom model could not be achieved for this. The application of Squeeze gave a good improvement in the data statistics and allowed for a full anisotropic refinement of the framework structure. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; 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 0.000 0.000 0.000 2273.3 276.4 2 0.333 0.667 0.667 2273.4 276.0 3 -0.333 0.333 0.333 2273.4 276.1 _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^)+(0.1504P)^2^+215.7550P] 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 16011 _refine_ls_number_parameters 959 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0883 _refine_ls_wR_factor_ref 0.2520 _refine_ls_wR_factor_gt 0.2460 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.002 _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 0.421193(19) 0.186163(19) 1.09830(3) 0.04771(19) Uani 1 1 d . . . Ni2 Ni 0.382076(18) 0.085169(18) 1.05095(3) 0.04613(19) Uani 1 1 d . . . Ni3 Ni 0.488147(17) 0.218272(16) 0.96309(3) 0.04016(17) Uani 1 1 d . . . Ni4 Ni 0.431978(15) 0.119714(15) 0.89609(3) 0.03519(16) Uani 1 1 d . . . S1 S 0.42298(13) 0.25978(10) 1.1428(2) 0.1435(13) Uani 1 1 d . . . S2 S 0.28898(3) 0.16029(3) 0.73158(6) 0.0420(3) Uani 1 1 d . . . S3 S 0.57457(11) 0.24138(10) 0.5389(2) 0.1379(12) Uani 1 1 d . . . P1 P 0.6667 0.3333 0.9694(2) 0.0814(9) Uani 1 3 d S . . F1 F 0.4166(6) 0.2891(5) 1.0496(9) 0.293(8) Uani 1 1 d . . . F2 F 0.4682(6) 0.3197(3) 1.0997(10) 0.344(13) Uani 1 1 d . . . F3 F 0.4246(6) 0.3205(5) 1.1322(8) 0.341(11) Uani 1 1 d . . . F4 F 0.27285(10) 0.18386(11) 0.82869(17) 0.0725(10) Uani 1 1 d . . . F5 F 0.23914(10) 0.12697(11) 0.81335(18) 0.0766(11) Uani 1 1 d . . . F6 F 0.23211(10) 0.16437(12) 0.75973(18) 0.0729(10) Uani 1 1 d . . . F7 F 0.5358(3) 0.1850(4) 0.4779(7) 0.252(7) Uani 1 1 d . . . F8 F 0.5098(3) 0.2159(4) 0.4941(6) 0.226(5) Uani 1 1 d . . . F9 F 0.5499(7) 0.2321(7) 0.4325(7) 0.350(14) Uani 1 1 d . . . F10 F 0.6462(4) 0.2987(3) 1.0124(8) 0.268(7) Uani 1 1 d . . . F11 F 0.6847(3) 0.3172(4) 0.9353(6) 0.261(7) Uani 1 1 d . . . O1 O 0.41813(9) 0.13629(10) 1.09096(16) 0.0459(8) Uani 1 1 d . . . O2 O 0.47420(8) 0.16448(8) 0.94464(15) 0.0381(7) Uani 1 1 d . . . O3 O 0.43879(9) 0.19915(10) 1.00989(15) 0.0457(8) Uani 1 1 d . . . O4 O 0.39170(9) 0.10596(9) 0.96311(14) 0.0418(7) Uani 1 1 d . . . O5 O 0.39738(13) 0.17573(15) 1.18439(19) 0.0714(12) Uani 1 1 d . . . O6 O 0.36284(12) 0.06451(11) 1.14041(18) 0.0615(10) Uani 1 1 d . . . O7 O 0.49953(12) 0.26720(10) 1.0099(2) 0.0581(10) Uani 1 1 d . . . O8 O 0.43756(13) 0.24320(12) 1.1038(3) 0.0752(13) Uani 1 1 d . . . O9 O 0.3876(4) 0.2393(3) 1.1542(7) 0.256(9) Uani 1 1 d . . . O10 O 0.4385(5) 0.2740(5) 1.1992(5) 0.269(9) Uani 1 1 d . . . O11 O 0.30786(11) 0.19739(10) 0.71318(19) 0.0574(9) Uani 1 1 d . . . O12 O 0.31015(11) 0.14895(13) 0.7651(2) 0.0654(11) Uani 1 1 d . . . O13 O 0.26698(9) 0.13585(9) 0.68437(16) 0.0436(7) Uani 1 1 d . . . O14 O 0.6039(3) 0.2398(3) 0.5146(6) 0.185(5) Uani 1 1 d . . . O15 O 0.5674(6) 0.2272(4) 0.6086(11) 0.230(14) Uani 0.50 1 d P . . O16 O 0.5752(2) 0.2736(2) 0.5359(4) 0.125(3) Uani 1 1 d . . . O17 O 0.5758(5) 0.2540(4) 0.4879(5) 0.108(5) Uani 0.50 1 d P . . N1 N 0.46936(13) 0.19872(13) 1.1355(2) 0.0543(11) Uani 1 1 d . . . N2 N 0.51846(14) 0.21365(16) 1.1872(2) 0.0653(13) Uani 1 1 d . . . H1 H 0.5382 0.2269 1.2085 0.078 Uiso 1 1 calc R . . N3 N 0.45501(13) 0.11058(14) 1.0979(2) 0.0537(11) Uani 1 1 d . . . N4 N 0.42604(13) 0.08245(13) 1.06802(19) 0.0504(10) Uani 1 1 d . . . N5 N 0.45191(19) 0.04621(18) 1.0823(3) 0.0784(17) Uani 1 1 d . . . H2 H 0.4706 0.0635 1.1017 0.094 Uiso 1 1 calc R . . H3 H 0.4504 0.0251 1.0767 0.094 Uiso 1 1 calc R . . N6 N 0.36732(15) 0.03237(13) 1.0189(2) 0.0575(12) Uani 1 1 d . . . N7 N 0.52591(11) 0.21454(10) 1.01314(19) 0.0410(8) Uani 1 1 d . . . N8 N 0.57196(11) 0.21721(11) 1.0610(2) 0.0463(9) Uani 1 1 d . . . H4 H 0.5916 0.2259 1.0834 0.056 Uiso 1 1 calc R . . N9 N 0.49524(9) 0.12380(9) 0.95823(16) 0.0329(7) Uani 1 1 d . . . N10 N 0.46410(9) 0.10163(10) 0.92445(17) 0.0344(7) Uani 1 1 d . . . N11 N 0.47630(10) 0.05414(10) 0.93186(19) 0.0418(9) Uani 1 1 d . . . H5 H 0.4963 0.0671 0.9526 0.050 Uiso 1 1 calc R . . H6 H 0.4693 0.0315 0.9229 0.050 Uiso 1 1 calc R . . N12 N 0.40548(10) 0.06530(10) 0.86349(17) 0.0377(8) Uani 1 1 d . . . N13 N 0.37379(12) 0.17424(13) 1.0589(2) 0.0518(10) Uani 1 1 d . . . N14 N 0.32329(16) 0.1682(2) 1.0238(3) 0.093(2) Uani 1 1 d . . . H7 H 0.3006 0.1632 1.0230 0.111 Uiso 1 1 calc R . . N15 N 0.42011(12) 0.21109(12) 0.9179(2) 0.0464(9) Uani 1 1 d . . . N16 N 0.45601(11) 0.22196(11) 0.90269(18) 0.0416(8) Uani 1 1 d . . . N17 N 0.44579(12) 0.23667(11) 0.80608(19) 0.0466(9) Uani 1 1 d . . . H8 H 0.4229 0.2292 0.8138 0.056 Uiso 1 1 calc R . . H9 H 0.4549 0.2455 0.7702 0.056 Uiso 1 1 calc R . . N18 N 0.52262(12) 0.24155(11) 0.8849(2) 0.0463(9) Uani 1 1 d . . . N19 N 0.33431(13) 0.08259(13) 1.0341(2) 0.0540(11) Uani 1 1 d . . . N20 N 0.27997(16) 0.0737(3) 1.0200(3) 0.101(3) Uani 1 1 d . . . H10 H 0.2575 0.0679 1.0279 0.121 Uiso 1 1 calc R . . N21 N 0.36462(11) 0.12146(12) 0.88534(19) 0.0451(9) Uani 1 1 d . . . N22 N 0.39785(10) 0.13229(11) 0.85800(18) 0.0382(8) Uani 1 1 d . . . N23 N 0.37927(11) 0.15027(11) 0.77189(18) 0.0417(8) Uani 1 1 d . . . H11 H 0.3581 0.1444 0.7877 0.050 Uiso 1 1 calc R . . H12 H 0.3847 0.1594 0.7351 0.050 Uiso 1 1 calc R . . N24 N 0.45765(11) 0.14312(11) 0.81441(19) 0.0425(9) Uani 1 1 d . . . C1 C 0.49572(17) 0.22445(18) 1.1660(3) 0.0602(14) Uani 1 1 d . . . H13 H 0.4986 0.2477 1.1726 0.072 Uiso 1 1 calc R . . C2 C 0.50554(16) 0.17851(17) 1.1698(3) 0.0568(13) Uani 1 1 d . . . C3 C 0.52345(19) 0.1579(2) 1.1884(3) 0.0714(17) Uani 1 1 d . . . H14 H 0.5418 0.1613 1.1583 0.086 Uiso 1 1 calc R . . H15 H 0.5054 0.1321 1.1912 0.086 Uiso 1 1 calc R . . H16 H 0.5350 0.1666 1.2280 0.086 Uiso 1 1 calc R . . C4 C 0.47485(15) 0.16960(15) 1.1368(2) 0.0486(11) Uani 1 1 d . . . C5 C 0.44766(15) 0.13651(15) 1.1065(2) 0.0495(12) Uani 1 1 d . . . C6 C 0.42538(18) 0.05205(17) 1.0612(3) 0.0571(14) Uani 1 1 d . . . C7 C 0.39335(19) 0.02361(16) 1.0318(3) 0.0590(14) Uani 1 1 d . . . C8 C 0.3874(2) -0.0106(2) 1.0174(3) 0.077(2) Uani 1 1 d . . . H17 H 0.4051 -0.0170 1.0277 0.092 Uiso 1 1 calc R . . C9 C 0.3566(3) -0.0351(2) 0.9886(4) 0.094(3) Uani 1 1 d . . . H18 H 0.3527 -0.0583 0.9781 0.113 Uiso 1 1 calc R . . C10 C 0.3312(3) -0.0254(2) 0.9750(4) 0.092(2) Uani 1 1 d . . . H19 H 0.3096 -0.0418 0.9544 0.110 Uiso 1 1 calc R . . C11 C 0.3374(2) 0.00807(18) 0.9917(3) 0.0686(16) Uani 1 1 d . . . H20 H 0.3193 0.0142 0.9832 0.082 Uiso 1 1 calc R . . C12 C 0.55391(14) 0.23458(13) 1.0472(2) 0.0469(11) Uani 1 1 d . . . H21 H 0.5606 0.2583 1.0605 0.056 Uiso 1 1 calc R . . C13 C 0.55456(12) 0.18357(12) 1.0345(2) 0.0393(9) Uani 1 1 d . . . C14 C 0.56643(15) 0.15670(15) 1.0433(3) 0.0492(11) Uani 1 1 d . . . H22 H 0.5840 0.1599 1.0118 0.059 Uiso 1 1 calc R . . H23 H 0.5455 0.1322 1.0405 0.059 Uiso 1 1 calc R . . H24 H 0.5777 0.1601 1.0833 0.059 Uiso 1 1 calc R . . C15 C 0.52603(12) 0.18241(12) 1.0041(2) 0.0380(9) Uani 1 1 d . . . C16 C 0.49704(11) 0.15525(11) 0.9669(2) 0.0332(8) Uani 1 1 d . . . C17 C 0.45641(11) 0.06894(12) 0.9139(2) 0.0353(9) Uani 1 1 d . . . C18 C 0.42317(11) 0.04763(12) 0.8774(2) 0.0359(9) Uani 1 1 d . . . C19 C 0.41104(14) 0.01230(14) 0.8585(3) 0.0484(11) Uani 1 1 d . . . H25 H 0.4242 0.0004 0.8682 0.058 Uiso 1 1 calc R . . C20 C 0.37923(15) -0.00521(15) 0.8250(3) 0.0534(13) Uani 1 1 d . . . H26 H 0.3703 -0.0293 0.8114 0.064 Uiso 1 1 calc R . . C21 C 0.36071(15) 0.01292(15) 0.8117(3) 0.0535(12) Uani 1 1 d . . . H27 H 0.3388 0.0013 0.7892 0.064 Uiso 1 1 calc R . . C22 C 0.37445(13) 0.04781(14) 0.8313(2) 0.0473(11) Uani 1 1 d . . . H28 H 0.3617 0.0602 0.8220 0.057 Uiso 1 1 calc R . . C23 C 0.33972(17) 0.1630(2) 1.0715(3) 0.0693(17) Uani 1 1 d . . . H29 H 0.3283 0.1528 1.1091 0.083 Uiso 1 1 calc R . . C24 C 0.3472(2) 0.1823(3) 0.9765(3) 0.086(3) Uani 1 1 d . . . C25 C 0.3384(3) 0.1917(4) 0.9174(4) 0.136(5) Uani 1 1 d . . . H30 H 0.3292 0.1708 0.8903 0.163 Uiso 1 1 calc R . . H31 H 0.3602 0.2120 0.8998 0.163 Uiso 1 1 calc R . . H32 H 0.3199 0.1987 0.9227 0.163 Uiso 1 1 calc R . . C26 C 0.37886(15) 0.18636(18) 0.9992(3) 0.0558(13) Uani 1 1 d . . . C27 C 0.41462(15) 0.19970(15) 0.9731(2) 0.0482(11) Uani 1 1 d . . . C28 C 0.46697(13) 0.23448(11) 0.8493(2) 0.0410(10) Uani 1 1 d . . . C29 C 0.50499(14) 0.24533(12) 0.8372(2) 0.0452(11) Uani 1 1 d . . . C30 C 0.52173(17) 0.25827(16) 0.7820(3) 0.0575(13) Uani 1 1 d . . . H33 H 0.5090 0.2613 0.7493 0.069 Uiso 1 1 calc R . . C31 C 0.55783(17) 0.26684(18) 0.7750(3) 0.0660(16) Uani 1 1 d . . . H34 H 0.5699 0.2754 0.7373 0.079 Uiso 1 1 calc R . . C32 C 0.57510(18) 0.26275(19) 0.8229(3) 0.0660(16) Uani 1 1 d . . . H35 H 0.5996 0.2684 0.8190 0.079 Uiso 1 1 calc R . . C33 C 0.55726(15) 0.25031(15) 0.8776(3) 0.0549(13) Uani 1 1 d . . . H36 H 0.5699 0.2479 0.9110 0.066 Uiso 1 1 calc R . . C34 C 0.30218(18) 0.0703(2) 1.0583(3) 0.0735(18) Uani 1 1 d . . . H37 H 0.2957 0.0604 1.0980 0.088 Uiso 1 1 calc R . . C35 C 0.29737(18) 0.0874(3) 0.9668(3) 0.090(3) Uani 1 1 d . . . C36 C 0.2798(2) 0.0942(4) 0.9135(4) 0.147(6) Uani 1 1 d . . . H38 H 0.2686 0.0727 0.8875 0.177 Uiso 1 1 calc R . . H39 H 0.2981 0.1149 0.8904 0.177 Uiso 1 1 calc R . . H40 H 0.2612 0.0995 0.9279 0.177 Uiso 1 1 calc R . . C37 C 0.33206(14) 0.09368(18) 0.9764(2) 0.0553(13) Uani 1 1 d . . . C38 C 0.36465(13) 0.10805(14) 0.9393(2) 0.0449(10) Uani 1 1 d . . . C39 C 0.40309(12) 0.14540(12) 0.80369(19) 0.0341(8) Uani 1 1 d . . . C40 C 0.43836(12) 0.15293(12) 0.7775(2) 0.0365(9) Uani 1 1 d . . . C41 C 0.45084(14) 0.16794(14) 0.7212(2) 0.0457(11) Uani 1 1 d . . . H41 H 0.4368 0.1742 0.6959 0.055 Uiso 1 1 calc R . . C42 C 0.48391(18) 0.1737(2) 0.7025(3) 0.0660(17) Uani 1 1 d . . . H42 H 0.4930 0.1838 0.6637 0.079 Uiso 1 1 calc R . . C43 C 0.5041(2) 0.1646(2) 0.7405(3) 0.079(2) Uani 1 1 d . . . H43 H 0.5272 0.1686 0.7284 0.095 Uiso 1 1 calc R . . C44 C 0.48986(16) 0.14967(19) 0.7962(3) 0.0618(16) Uani 1 1 d . . . H44 H 0.5038 0.1439 0.8226 0.074 Uiso 1 1 calc R . . C45 C 0.4341(6) 0.2978(4) 1.1111(9) 0.160(7) Uani 1 1 d . . . C46 C 0.25633(15) 0.15900(17) 0.7862(3) 0.0545(13) Uani 1 1 d . . . C47 C 0.5402(5) 0.2156(5) 0.4849(12) 0.186(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0516(4) 0.0554(4) 0.0435(4) 0.0007(3) 0.0033(3) 0.0323(3) Ni2 0.0510(4) 0.0487(4) 0.0402(3) 0.0075(3) 0.0068(3) 0.0261(3) Ni3 0.0449(3) 0.0380(3) 0.0451(3) 0.0038(2) 0.0010(2) 0.0264(3) Ni4 0.0328(3) 0.0411(3) 0.0376(3) 0.0041(2) 0.0004(2) 0.0229(2) S1 0.174(4) 0.119(2) 0.161(3) -0.018(2) 0.004(3) 0.091(3) S2 0.0352(5) 0.0439(6) 0.0492(6) -0.0101(5) -0.0096(5) 0.0215(5) S3 0.152(3) 0.133(3) 0.165(3) -0.030(2) -0.020(2) 0.098(2) P1 0.0707(12) 0.0707(12) 0.103(3) 0.000 0.000 0.0353(6) F1 0.36(2) 0.239(16) 0.33(2) 0.035(15) 0.022(18) 0.186(17) F2 0.41(2) 0.095(6) 0.47(3) 0.060(11) 0.24(2) 0.085(10) F3 0.57(3) 0.320(18) 0.324(18) 0.025(14) 0.124(19) 0.37(2) F4 0.063(2) 0.088(3) 0.061(2) -0.0291(19) -0.0079(16) 0.0331(19) F5 0.064(2) 0.077(2) 0.063(2) 0.0095(18) 0.0046(17) 0.0163(19) F6 0.060(2) 0.108(3) 0.069(2) -0.018(2) -0.0051(17) 0.056(2) F7 0.214(11) 0.219(11) 0.350(18) -0.151(12) -0.076(11) 0.128(10) F8 0.145(7) 0.294(14) 0.277(13) -0.094(10) -0.013(8) 0.140(9) F9 0.48(3) 0.56(4) 0.164(11) 0.110(17) 0.046(15) 0.38(3) F10 0.255(13) 0.146(8) 0.361(18) 0.104(10) 0.052(12) 0.068(9) F11 0.195(10) 0.301(15) 0.296(13) -0.158(12) 0.033(9) 0.129(10) O1 0.0486(19) 0.0517(19) 0.0438(18) 0.0087(15) 0.0048(14) 0.0299(16) O2 0.0354(15) 0.0372(16) 0.0487(18) 0.0014(13) -0.0025(13) 0.0234(13) O3 0.0488(19) 0.056(2) 0.0428(18) 0.0055(15) 0.0015(14) 0.0339(17) O4 0.0406(17) 0.0535(19) 0.0372(16) 0.0058(14) 0.0026(13) 0.0281(15) O5 0.070(3) 0.103(4) 0.051(2) 0.002(2) 0.013(2) 0.050(3) O6 0.069(3) 0.059(2) 0.045(2) 0.0152(17) 0.0148(18) 0.024(2) O7 0.073(3) 0.0413(19) 0.070(2) -0.0019(17) -0.006(2) 0.0365(19) O8 0.069(3) 0.057(2) 0.106(4) -0.007(2) -0.002(3) 0.036(2) O9 0.206(11) 0.136(8) 0.332(18) -0.027(9) 0.198(12) 0.016(8) O10 0.283(17) 0.34(2) 0.122(8) -0.105(11) -0.064(10) 0.105(15) O11 0.052(2) 0.050(2) 0.059(2) -0.0064(17) 0.0008(17) 0.0178(17) O12 0.057(2) 0.080(3) 0.074(3) -0.012(2) -0.021(2) 0.046(2) O13 0.0380(16) 0.0427(17) 0.0496(19) -0.0126(14) -0.0073(14) 0.0198(14) O14 0.196(10) 0.197(10) 0.244(12) 0.005(9) 0.034(9) 0.161(9) O15 0.30(2) 0.141(12) 0.35(3) 0.192(17) 0.28(2) 0.181(16) O16 0.169(7) 0.135(6) 0.134(6) -0.025(5) 0.011(5) 0.123(6) O17 0.207(15) 0.112(10) 0.046(5) 0.018(6) 0.005(7) 0.111(11) N1 0.055(3) 0.060(3) 0.049(2) 0.002(2) 0.004(2) 0.029(2) N2 0.057(3) 0.077(4) 0.057(3) -0.005(2) -0.010(2) 0.030(3) N3 0.056(3) 0.067(3) 0.045(2) 0.013(2) 0.0040(19) 0.036(2) N4 0.060(3) 0.056(3) 0.042(2) 0.0086(19) 0.0038(19) 0.035(2) N5 0.103(5) 0.081(4) 0.080(4) 0.003(3) -0.007(3) 0.067(4) N6 0.077(3) 0.052(3) 0.044(2) 0.010(2) 0.010(2) 0.032(2) N7 0.042(2) 0.0347(19) 0.049(2) -0.0036(16) -0.0040(17) 0.0210(17) N8 0.044(2) 0.042(2) 0.053(2) -0.0052(18) -0.0093(18) 0.0224(18) N9 0.0305(17) 0.0333(17) 0.0383(18) 0.0024(14) -0.0015(14) 0.0184(15) N10 0.0278(16) 0.0337(18) 0.0409(19) 0.0015(14) 0.0003(14) 0.0148(14) N11 0.0348(19) 0.0336(18) 0.058(2) -0.0030(16) -0.0143(17) 0.0178(16) N12 0.0346(18) 0.043(2) 0.0379(19) 0.0041(15) -0.0003(15) 0.0209(16) N13 0.050(2) 0.066(3) 0.048(2) -0.002(2) 0.0051(19) 0.036(2) N14 0.059(3) 0.183(7) 0.054(3) 0.000(4) 0.011(3) 0.074(4) N15 0.049(2) 0.057(2) 0.049(2) 0.0053(19) 0.0039(18) 0.037(2) N16 0.051(2) 0.045(2) 0.042(2) 0.0055(16) 0.0036(17) 0.0330(19) N17 0.056(2) 0.043(2) 0.044(2) 0.0015(17) -0.0055(18) 0.027(2) N18 0.053(2) 0.041(2) 0.049(2) 0.0042(17) 0.0014(18) 0.0265(19) N19 0.048(2) 0.060(3) 0.049(2) 0.004(2) 0.0091(19) 0.024(2) N20 0.048(3) 0.173(8) 0.075(4) 0.032(4) 0.018(3) 0.049(4) N21 0.0358(19) 0.061(3) 0.044(2) 0.0050(18) 0.0055(16) 0.0285(19) N22 0.0337(18) 0.045(2) 0.042(2) 0.0026(16) 0.0031(15) 0.0237(16) N23 0.042(2) 0.051(2) 0.040(2) 0.0056(16) -0.0003(16) 0.0288(18) N24 0.039(2) 0.051(2) 0.045(2) 0.0090(17) 0.0043(16) 0.0291(18) C1 0.061(3) 0.066(4) 0.056(3) -0.006(3) -0.007(3) 0.033(3) C2 0.055(3) 0.066(3) 0.049(3) 0.007(3) 0.000(2) 0.030(3) C3 0.064(4) 0.085(5) 0.068(4) 0.010(3) -0.012(3) 0.039(4) C4 0.056(3) 0.055(3) 0.040(2) 0.009(2) 0.004(2) 0.032(2) C5 0.055(3) 0.058(3) 0.040(2) 0.014(2) 0.007(2) 0.031(3) C6 0.079(4) 0.062(3) 0.049(3) 0.016(2) 0.017(3) 0.049(3) C7 0.082(4) 0.057(3) 0.046(3) 0.016(2) 0.019(3) 0.041(3) C8 0.114(6) 0.068(4) 0.063(4) 0.007(3) 0.019(4) 0.057(4) C9 0.117(7) 0.055(4) 0.096(6) -0.005(4) 0.013(5) 0.032(5) C10 0.109(7) 0.064(4) 0.092(6) -0.006(4) -0.008(5) 0.036(5) C11 0.075(4) 0.057(3) 0.061(4) 0.000(3) 0.000(3) 0.023(3) C12 0.052(3) 0.034(2) 0.055(3) -0.005(2) -0.005(2) 0.021(2) C13 0.036(2) 0.038(2) 0.045(2) 0.0005(18) -0.0025(18) 0.0196(19) C14 0.053(3) 0.053(3) 0.054(3) -0.003(2) -0.009(2) 0.036(2) C15 0.041(2) 0.035(2) 0.042(2) 0.0044(17) 0.0032(18) 0.0216(19) C16 0.0313(19) 0.0302(19) 0.039(2) 0.0024(16) 0.0030(16) 0.0161(16) C17 0.0279(19) 0.037(2) 0.040(2) 0.0037(17) -0.0025(16) 0.0154(17) C18 0.031(2) 0.037(2) 0.040(2) 0.0035(17) -0.0022(17) 0.0170(18) C19 0.044(3) 0.041(2) 0.061(3) 0.000(2) -0.009(2) 0.021(2) C20 0.049(3) 0.043(3) 0.062(3) -0.010(2) -0.018(2) 0.019(2) C21 0.044(3) 0.056(3) 0.057(3) -0.006(2) -0.015(2) 0.023(2) C22 0.040(2) 0.052(3) 0.052(3) -0.004(2) -0.014(2) 0.024(2) C23 0.056(3) 0.100(5) 0.055(3) 0.000(3) 0.009(3) 0.042(4) C24 0.077(5) 0.163(8) 0.053(4) 0.006(4) 0.007(3) 0.086(5) C25 0.112(7) 0.301(17) 0.069(5) 0.028(7) 0.013(5) 0.158(10) C26 0.051(3) 0.081(4) 0.049(3) 0.000(3) 0.005(2) 0.044(3) C27 0.055(3) 0.052(3) 0.052(3) 0.005(2) 0.005(2) 0.038(2) C28 0.049(3) 0.027(2) 0.051(3) 0.0022(18) -0.002(2) 0.0212(19) C29 0.053(3) 0.030(2) 0.052(3) 0.0029(19) 0.001(2) 0.021(2) C30 0.066(3) 0.050(3) 0.056(3) 0.009(2) 0.003(3) 0.028(3) C31 0.059(3) 0.070(4) 0.063(4) 0.019(3) 0.019(3) 0.028(3) C32 0.055(3) 0.071(4) 0.072(4) 0.014(3) 0.009(3) 0.032(3) C33 0.051(3) 0.054(3) 0.062(3) 0.009(2) 0.005(2) 0.028(3) C34 0.057(4) 0.098(5) 0.055(3) 0.009(3) 0.014(3) 0.031(4) C35 0.048(3) 0.160(8) 0.068(4) 0.026(5) 0.013(3) 0.057(5) C36 0.070(5) 0.299(18) 0.082(6) 0.059(8) 0.018(4) 0.099(8) C37 0.042(3) 0.080(4) 0.045(3) 0.006(3) 0.007(2) 0.031(3) C38 0.040(2) 0.054(3) 0.046(3) 0.002(2) 0.004(2) 0.028(2) C39 0.036(2) 0.038(2) 0.035(2) -0.0035(16) -0.0010(16) 0.0232(18) C40 0.039(2) 0.041(2) 0.038(2) 0.0014(17) 0.0003(17) 0.0267(19) C41 0.055(3) 0.052(3) 0.043(2) 0.005(2) 0.004(2) 0.036(2) C42 0.076(4) 0.091(5) 0.055(3) 0.028(3) 0.027(3) 0.061(4) C43 0.078(4) 0.121(6) 0.077(4) 0.047(4) 0.039(4) 0.079(5) C44 0.055(3) 0.092(4) 0.064(3) 0.022(3) 0.013(3) 0.056(3) C45 0.201(16) 0.081(7) 0.179(14) 0.003(8) 0.082(13) 0.057(9) C46 0.044(3) 0.068(3) 0.049(3) -0.014(3) -0.007(2) 0.026(3) C47 0.172(16) 0.126(12) 0.29(3) -0.078(14) -0.043(16) 0.096(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 N13 2.019(5) . ? Ni1 N1 2.021(5) . ? Ni1 O3 2.064(3) . ? Ni1 O1 2.072(4) . ? Ni1 O5 2.094(4) . ? Ni1 O8 2.174(4) . ? Ni2 N4 1.973(5) . ? Ni2 N19 2.020(5) . ? Ni2 O4 2.085(3) . ? Ni2 O1 2.133(4) . ? Ni2 N6 2.134(5) . ? Ni2 O6 2.150(4) . ? Ni3 N16 1.974(4) . ? Ni3 N7 2.025(4) . ? Ni3 O2 2.103(3) . ? Ni3 O3 2.109(4) . ? Ni3 O7 2.156(4) . ? Ni3 N18 2.160(4) . ? Ni4 N22 1.974(4) . ? Ni4 N10 1.981(4) . ? Ni4 N24 2.086(4) . ? Ni4 O4 2.116(3) . ? Ni4 N12 2.136(4) . ? Ni4 O2 2.145(3) . ? S1 O9 1.339(11) . ? S1 O10 1.398(11) . ? S1 O8 1.437(6) . ? S1 C45 1.604(16) . ? S2 O12 1.427(4) . ? S2 O11 1.430(4) . ? S2 O13 1.440(3) . ? S2 C46 1.823(6) . ? S3 O17 1.236(10) . ? S3 O16 1.362(7) . ? S3 O14 1.393(10) . ? S3 O15 1.62(2) . ? S3 C47 1.780(19) . ? P1 F11 1.470(8) . ? P1 F11 1.470(8) 3_665 ? P1 F11 1.470(8) 2_655 ? P1 F10 1.598(11) . ? P1 F10 1.598(11) 2_655 ? P1 F10 1.598(11) 3_665 ? F1 C45 1.50(2) . ? F2 C45 1.30(2) . ? F3 C45 1.307(16) . ? F4 C46 1.323(6) . ? F5 C46 1.327(7) . ? F6 C46 1.304(7) . ? F7 C47 1.234(17) . ? F8 C47 1.317(19) . ? F9 C47 1.31(3) . ? F9 O17 1.60(3) . ? O1 C5 1.301(6) . ? O2 C16 1.315(5) . ? O3 C27 1.322(6) . ? O4 C38 1.311(6) . ? O14 O17 1.696(16) . ? O16 O17 1.357(13) . ? O17 C47 1.59(2) . ? N1 C1 1.300(8) . ? N1 C4 1.375(7) . ? N2 C1 1.349(8) . ? N2 C2 1.369(8) . ? N3 C5 1.306(7) . ? N3 N4 1.386(7) . ? N4 C6 1.293(7) . ? N5 C6 1.358(8) . ? N6 C11 1.320(8) . ? N6 C7 1.367(8) . ? N7 C12 1.305(7) . ? N7 C15 1.388(6) . ? N8 C12 1.344(7) . ? N8 C13 1.375(6) . ? N9 C16 1.320(5) . ? N9 N10 1.400(5) . ? N10 C17 1.285(6) . ? N11 C17 1.347(6) . ? N12 C18 1.342(6) . ? N12 C22 1.351(6) . ? N13 C23 1.313(7) . ? N13 C26 1.391(7) . ? N14 C23 1.342(9) . ? N14 C24 1.370(9) . ? N15 C27 1.290(7) . ? N15 N16 1.401(6) . ? N16 C28 1.282(6) . ? N17 C28 1.349(6) . ? N18 C33 1.341(7) . ? N18 C29 1.350(7) . ? N19 C34 1.313(8) . ? N19 C37 1.377(7) . ? N20 C34 1.331(10) . ? N20 C35 1.355(9) . ? N21 C38 1.321(7) . ? N21 N22 1.390(5) . ? N22 C39 1.293(6) . ? N23 C39 1.334(6) . ? N24 C44 1.321(6) . ? N24 C40 1.364(6) . ? C2 C4 1.375(8) . ? C2 C3 1.484(9) . ? C4 C5 1.467(8) . ? C6 C7 1.450(10) . ? C7 C8 1.389(9) . ? C8 C9 1.360(12) . ? C9 C10 1.369(13) . ? C10 C11 1.367(10) . ? C13 C15 1.368(6) . ? C13 C14 1.480(6) . ? C15 C16 1.455(6) . ? C17 C18 1.483(6) . ? C18 C19 1.391(7) . ? C19 C20 1.390(7) . ? C20 C21 1.386(8) . ? C21 C22 1.370(8) . ? C24 C26 1.368(8) . ? C24 C25 1.467(11) . ? C26 C27 1.455(7) . ? C28 C29 1.472(7) . ? C29 C30 1.378(8) . ? C30 C31 1.403(9) . ? C31 C32 1.348(9) . ? C32 C33 1.384(9) . ? C35 C37 1.383(8) . ? C35 C36 1.499(11) . ? C37 C38 1.459(7) . ? C39 C40 1.490(6) . ? C40 C41 1.377(7) . ? C41 C42 1.370(8) . ? C42 C43 1.389(9) . ? C43 C44 1.377(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N13 Ni1 N1 178.4(2) . . ? N13 Ni1 O3 81.10(16) . . ? N1 Ni1 O3 97.31(16) . . ? N13 Ni1 O1 99.59(17) . . ? N1 Ni1 O1 80.66(17) . . ? O3 Ni1 O1 91.69(14) . . ? N13 Ni1 O5 91.04(18) . . ? N1 Ni1 O5 90.52(19) . . ? O3 Ni1 O5 170.74(16) . . ? O1 Ni1 O5 94.46(18) . . ? N13 Ni1 O8 91.54(19) . . ? N1 Ni1 O8 88.0(2) . . ? O3 Ni1 O8 83.25(18) . . ? O1 Ni1 O8 166.94(16) . . ? O5 Ni1 O8 92.1(2) . . ? N4 Ni2 N19 174.4(2) . . ? N4 Ni2 O4 102.21(15) . . ? N19 Ni2 O4 80.25(16) . . ? N4 Ni2 O1 76.14(17) . . ? N19 Ni2 O1 108.91(17) . . ? O4 Ni2 O1 93.52(13) . . ? N4 Ni2 N6 77.8(2) . . ? N19 Ni2 N6 97.1(2) . . ? O4 Ni2 N6 91.90(15) . . ? O1 Ni2 N6 153.92(18) . . ? N4 Ni2 O6 88.86(18) . . ? N19 Ni2 O6 88.78(18) . . ? O4 Ni2 O6 168.90(16) . . ? O1 Ni2 O6 88.40(15) . . ? N6 Ni2 O6 91.15(17) . . ? N16 Ni3 N7 170.58(17) . . ? N16 Ni3 O2 97.34(15) . . ? N7 Ni3 O2 79.72(13) . . ? N16 Ni3 O3 76.23(15) . . ? N7 Ni3 O3 112.51(15) . . ? O2 Ni3 O3 89.40(13) . . ? N16 Ni3 O7 94.30(16) . . ? N7 Ni3 O7 90.71(15) . . ? O2 Ni3 O7 162.48(15) . . ? O3 Ni3 O7 80.69(16) . . ? N16 Ni3 N18 76.40(17) . . ? N7 Ni3 N18 94.93(17) . . ? O2 Ni3 N18 95.93(14) . . ? O3 Ni3 N18 152.56(15) . . ? O7 Ni3 N18 99.51(16) . . ? N22 Ni4 N10 171.38(16) . . ? N22 Ni4 N24 77.55(15) . . ? N10 Ni4 N24 99.17(15) . . ? N22 Ni4 O4 76.43(14) . . ? N10 Ni4 O4 107.20(14) . . ? N24 Ni4 O4 153.63(14) . . ? N22 Ni4 N12 95.20(15) . . ? N10 Ni4 N12 77.07(14) . . ? N24 Ni4 N12 95.49(16) . . ? O4 Ni4 N12 91.06(14) . . ? N22 Ni4 O2 112.07(14) . . ? N10 Ni4 O2 75.67(13) . . ? N24 Ni4 O2 89.92(15) . . ? O4 Ni4 O2 95.88(13) . . ? N12 Ni4 O2 152.71(13) . . ? O9 S1 O10 104.5(10) . . ? O9 S1 O8 114.6(6) . . ? O10 S1 O8 121.2(9) . . ? O9 S1 C45 114.2(11) . . ? O10 S1 C45 96.5(12) . . ? O8 S1 C45 104.8(6) . . ? O12 S2 O11 114.9(3) . . ? O12 S2 O13 115.0(2) . . ? O11 S2 O13 113.5(2) . . ? O12 S2 C46 104.5(3) . . ? O11 S2 C46 102.7(3) . . ? O13 S2 C46 104.2(2) . . ? O17 S3 O16 62.7(7) . . ? O17 S3 O14 80.1(9) . . ? O16 S3 O14 117.7(7) . . ? O17 S3 O15 169.1(9) . . ? O16 S3 O15 108.9(6) . . ? O14 S3 O15 110.7(8) . . ? O17 S3 C47 60.3(12) . . ? O16 S3 C47 100.7(7) . . ? O14 S3 C47 101.4(9) . . ? O15 S3 C47 117.3(14) . . ? F11 P1 F11 96.2(9) . 3_665 ? F11 P1 F11 96.2(9) . 2_655 ? F11 P1 F11 96.2(9) 3_665 2_655 ? F11 P1 F10 92.5(9) . . ? F11 P1 F10 82.9(8) 3_665 . ? F11 P1 F10 171.3(8) 2_655 . ? F11 P1 F10 82.9(8) . 2_655 ? F11 P1 F10 171.3(8) 3_665 2_655 ? F11 P1 F10 92.6(9) 2_655 2_655 ? F10 P1 F10 88.4(9) . 2_655 ? F11 P1 F10 171.3(8) . 3_665 ? F11 P1 F10 92.5(9) 3_665 3_665 ? F11 P1 F10 82.9(8) 2_655 3_665 ? F10 P1 F10 88.4(9) . 3_665 ? F10 P1 F10 88.4(9) 2_655 3_665 ? C47 F9 O17 65.2(12) . . ? C5 O1 Ni1 114.1(3) . . ? C5 O1 Ni2 108.5(3) . . ? Ni1 O1 Ni2 136.53(17) . . ? C16 O2 Ni3 114.0(3) . . ? C16 O2 Ni4 109.7(3) . . ? Ni3 O2 Ni4 136.21(15) . . ? C27 O3 Ni1 113.7(3) . . ? C27 O3 Ni3 109.3(3) . . ? Ni1 O3 Ni3 136.50(17) . . ? C38 O4 Ni2 114.1(3) . . ? C38 O4 Ni4 108.8(3) . . ? Ni2 O4 Ni4 136.68(16) . . ? S1 O8 Ni1 127.5(4) . . ? S3 O14 O17 45.9(5) . . ? O17 O16 S3 54.1(5) . . ? S3 O17 O16 63.2(6) . . ? S3 O17 C47 77.1(13) . . ? O16 O17 C47 111.4(13) . . ? S3 O17 F9 125.0(14) . . ? O16 O17 F9 137.3(14) . . ? C47 O17 F9 48.5(11) . . ? S3 O17 O14 54.0(7) . . ? O16 O17 O14 100.5(9) . . ? C47 O17 O14 97.4(10) . . ? F9 O17 O14 117.6(11) . . ? C1 N1 C4 106.6(5) . . ? C1 N1 Ni1 140.4(4) . . ? C4 N1 Ni1 112.3(4) . . ? C1 N2 C2 108.2(5) . . ? C5 N3 N4 108.3(4) . . ? C6 N4 N3 119.2(5) . . ? C6 N4 Ni2 119.5(4) . . ? N3 N4 Ni2 120.2(3) . . ? C11 N6 C7 118.6(6) . . ? C11 N6 Ni2 129.7(5) . . ? C7 N6 Ni2 111.6(4) . . ? C12 N7 C15 106.0(4) . . ? C12 N7 Ni3 140.1(3) . . ? C15 N7 Ni3 113.3(3) . . ? C12 N8 C13 108.7(4) . . ? C16 N9 N10 108.5(3) . . ? C17 N10 N9 118.1(3) . . ? C17 N10 Ni4 121.0(3) . . ? N9 N10 Ni4 120.9(3) . . ? C18 N12 C22 118.7(4) . . ? C18 N12 Ni4 113.2(3) . . ? C22 N12 Ni4 128.1(3) . . ? C23 N13 C26 105.9(5) . . ? C23 N13 Ni1 142.0(4) . . ? C26 N13 Ni1 111.3(3) . . ? C23 N14 C24 109.5(5) . . ? C27 N15 N16 108.2(4) . . ? C28 N16 N15 117.9(4) . . ? C28 N16 Ni3 122.0(3) . . ? N15 N16 Ni3 120.0(3) . . ? C33 N18 C29 118.4(5) . . ? C33 N18 Ni3 128.8(4) . . ? C29 N18 Ni3 112.7(3) . . ? C34 N19 C37 106.0(5) . . ? C34 N19 Ni2 140.4(5) . . ? C37 N19 Ni2 113.2(3) . . ? C34 N20 C35 109.3(6) . . ? C38 N21 N22 108.2(4) . . ? C39 N22 N21 118.2(4) . . ? C39 N22 Ni4 121.3(3) . . ? N21 N22 Ni4 119.6(3) . . ? C44 N24 C40 118.5(4) . . ? C44 N24 Ni4 127.3(4) . . ? C40 N24 Ni4 114.2(3) . . ? N1 C1 N2 111.0(6) . . ? N2 C2 C4 104.9(5) . . ? N2 C2 C3 121.8(6) . . ? C4 C2 C3 133.2(6) . . ? C2 C4 N1 109.3(5) . . ? C2 C4 C5 133.9(5) . . ? N1 C4 C5 116.8(5) . . ? O1 C5 N3 126.7(5) . . ? O1 C5 C4 115.1(5) . . ? N3 C5 C4 118.2(5) . . ? N4 C6 N5 122.8(6) . . ? N4 C6 C7 115.5(5) . . ? N5 C6 C7 121.6(6) . . ? N6 C7 C8 119.6(7) . . ? N6 C7 C6 114.8(5) . . ? C8 C7 C6 125.6(6) . . ? C9 C8 C7 120.7(8) . . ? C8 C9 C10 118.6(8) . . ? C11 C10 C9 119.2(9) . . ? N6 C11 C10 123.3(8) . . ? N7 C12 N8 111.0(4) . . ? C15 C13 N8 104.6(4) . . ? C15 C13 C14 132.8(4) . . ? N8 C13 C14 122.5(4) . . ? C13 C15 N7 109.7(4) . . ? C13 C15 C16 133.8(4) . . ? N7 C15 C16 116.5(4) . . ? O2 C16 N9 125.2(4) . . ? O2 C16 C15 115.8(4) . . ? N9 C16 C15 119.0(4) . . ? N10 C17 N11 125.3(4) . . ? N10 C17 C18 114.3(4) . . ? N11 C17 C18 120.4(4) . . ? N12 C18 C19 122.1(4) . . ? N12 C18 C17 114.4(4) . . ? C19 C18 C17 123.4(4) . . ? C20 C19 C18 118.4(5) . . ? C21 C20 C19 119.3(5) . . ? C22 C21 C20 119.1(5) . . ? N12 C22 C21 122.4(5) . . ? N13 C23 N14 110.4(6) . . ? C26 C24 N14 104.4(6) . . ? C26 C24 C25 131.6(7) . . ? N14 C24 C25 124.0(6) . . ? C24 C26 N13 109.8(5) . . ? C24 C26 C27 132.9(6) . . ? N13 C26 C27 117.2(5) . . ? N15 C27 O3 126.2(5) . . ? N15 C27 C26 118.6(5) . . ? O3 C27 C26 115.2(5) . . ? N16 C28 N17 124.1(5) . . ? N16 C28 C29 114.4(4) . . ? N17 C28 C29 121.4(5) . . ? N18 C29 C30 121.9(5) . . ? N18 C29 C28 114.4(4) . . ? C30 C29 C28 123.7(5) . . ? C29 C30 C31 118.9(6) . . ? C32 C31 C30 118.7(6) . . ? C31 C32 C33 120.1(6) . . ? N18 C33 C32 122.0(6) . . ? N19 C34 N20 110.9(6) . . ? N20 C35 C37 104.7(6) . . ? N20 C35 C36 122.9(6) . . ? C37 C35 C36 132.4(7) . . ? N19 C37 C35 109.1(5) . . ? N19 C37 C38 116.6(5) . . ? C35 C37 C38 134.3(6) . . ? O4 C38 N21 125.6(4) . . ? O4 C38 C37 115.7(4) . . ? N21 C38 C37 118.7(4) . . ? N22 C39 N23 125.0(4) . . ? N22 C39 C40 113.0(4) . . ? N23 C39 C40 121.9(4) . . ? N24 C40 C41 121.9(4) . . ? N24 C40 C39 113.7(4) . . ? C41 C40 C39 124.4(4) . . ? C42 C41 C40 118.6(5) . . ? C41 C42 C43 119.7(5) . . ? C44 C43 C42 118.4(5) . . ? N24 C44 C43 122.8(5) . . ? F2 C45 F3 100.7(15) . . ? F2 C45 F1 104.0(16) . . ? F3 C45 F1 102(2) . . ? F2 C45 S1 118.0(18) . . ? F3 C45 S1 123.3(13) . . ? F1 C45 S1 106.4(12) . . ? F6 C46 F4 109.1(5) . . ? F6 C46 F5 107.7(5) . . ? F4 C46 F5 107.8(5) . . ? F6 C46 S2 111.0(4) . . ? F4 C46 S2 110.5(4) . . ? F5 C46 S2 110.5(4) . . ? F7 C47 F9 107(2) . . ? F7 C47 F8 113.5(18) . . ? F9 C47 F8 100.3(19) . . ? F7 C47 O17 131.2(16) . . ? F9 C47 O17 66.3(16) . . ? F8 C47 O17 115.2(13) . . ? F7 C47 S3 112.3(15) . . ? F9 C47 S3 108.5(18) . . ? F8 C47 S3 113.8(14) . . ? O17 C47 S3 42.6(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.620 _refine_diff_density_min -1.612 _refine_diff_density_rms 0.133 #===END