# 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 ; 'Annie K. Powell' ; _publ_contact_author_email powell@aoc.uni-karlsruhe.de _publ_contact_author_phone '+49 721 608 2135' _publ_section_title ; Di-, tetra- and hexanuclear iron(III), manganese(II/III) and copper(II) complexes of Schiff-base ligands derived from 2,3-disubstituted benzaldehydes ; loop_ _publ_author_name _publ_author_address 'Yanhua Lan.' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Ghenadie Novitchi' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Rodolphe Clerac' ; Centre de Recherche Paul Pascal CNRS UPR 8641 115 Avenue Dr. A. Schweitzer 33600 Pessac France ; 'Jin-Kui Tang.' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'N.T. Madhu' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; ; I.J.Hewitt ; ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Christopher E. Anson' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; 'Sally Brooker' ; Department of Chemistry and The MacDiarmid Institute for Advanced Materials and Nanotechnology, University of Otago, PO Box 56, Dunedin, New Zealand ; 'Annie K. Powell' ; Institut f\"ur Anorganische Chemie Universit\"at Karlsruhe Engesserstr. Geb. 30.45 D-76128 Karlsruhe Germany ; _publ_contact_author_name 'Annie K. Powell' data_sc246 _database_code_depnum_ccdc_archive 'CCDC 700804' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H38 Fe2 N4 O10, 2(C H4 O)' _chemical_formula_sum 'C40 H46 Fe2 N4 O12' _chemical_formula_weight 886.51 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.0203(11) _cell_length_b 14.7485(8) _cell_length_c 24.089(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.134(7) _cell_angle_gamma 90.00 _cell_volume 3899.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 24513 _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 27.13 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.814 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.836 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details ; XPREP in SHELXTL 5.1 (Bruker AXS Inc., 1997) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26049 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.12 _reflns_number_total 8551 _reflns_number_gt 6981 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.05 (Stoe & Cie GmbH, 2000)' _computing_cell_refinement 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_data_reduction 'X-Area 1.09 (Stoe & Cie GmbH, 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The O-H bond lengths for the lattice methanols were restrained. ; _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^)+(0.0813P)^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 8551 _refine_ls_number_parameters 535 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0521 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Fe1 Fe 0.25008(2) 0.261867(18) 0.183758(11) 0.01753(9) Uani 1 1 d . . . Fe2 Fe 0.34719(2) 0.258851(18) 0.315714(11) 0.01683(9) Uani 1 1 d . . . O1 O 0.35930(12) 0.32764(9) 0.24231(5) 0.0190(3) Uani 1 1 d . . . C1 C 0.35460(18) 0.42386(13) 0.24224(8) 0.0212(4) Uani 1 1 d . . . H1 H 0.4076 0.4485 0.2142 0.025 Uiso 1 1 calc R . . C2 C 0.22279(18) 0.45468(13) 0.22793(8) 0.0238(4) Uani 1 1 d . . . H2A H 0.1801 0.4579 0.2623 0.029 Uiso 1 1 calc R . . H2B H 0.2218 0.5158 0.2110 0.029 Uiso 1 1 calc R . . N1 N 0.16042(14) 0.39020(11) 0.18879(6) 0.0206(3) Uani 1 1 d . . . C3 C 0.05828(18) 0.41472(14) 0.16302(8) 0.0235(4) Uani 1 1 d . . . H3 H 0.0361 0.4767 0.1656 0.028 Uiso 1 1 calc R . . C4 C -0.02527(18) 0.35597(14) 0.13058(8) 0.0225(4) Uani 1 1 d . . . C5 C -0.13125(19) 0.39422(16) 0.10288(9) 0.0278(4) Uani 1 1 d . . . H5 H -0.1423 0.4581 0.1032 0.033 Uiso 1 1 calc R . . C6 C -0.2188(2) 0.34004(17) 0.07538(9) 0.0319(5) Uani 1 1 d . . . H6 H -0.2883 0.3665 0.0555 0.038 Uiso 1 1 calc R . . C7 C -0.2048(2) 0.24614(16) 0.07700(9) 0.0301(5) Uani 1 1 d . . . H7 H -0.2666 0.2087 0.0590 0.036 Uiso 1 1 calc R . . C8 C -0.10292(18) 0.20664(15) 0.10424(8) 0.0252(4) Uani 1 1 d . . . C9 C -0.00668(18) 0.26077(14) 0.12947(8) 0.0217(4) Uani 1 1 d . . . O2 O 0.09413(13) 0.22162(10) 0.14995(6) 0.0235(3) Uani 1 1 d . . . O3 O -0.09360(14) 0.11371(11) 0.10191(7) 0.0312(3) Uani 1 1 d . . . C10 C -0.0490(3) 0.06680(19) 0.15131(12) 0.0473(7) Uani 1 1 d . . . H10A H 0.0397 0.0733 0.1570 0.071 Uiso 1 1 calc R . . H10B H -0.0701 0.0024 0.1476 0.071 Uiso 1 1 calc R . . H10C H -0.0861 0.0924 0.1833 0.071 Uiso 1 1 calc R . . N2 N 0.34083(14) 0.39909(11) 0.33978(7) 0.0199(3) Uani 1 1 d . . . C11 C 0.40178(18) 0.45534(13) 0.30069(8) 0.0222(4) Uani 1 1 d . . . H11A H 0.4912 0.4475 0.3066 0.027 Uiso 1 1 calc R . . H11B H 0.3823 0.5202 0.3059 0.027 Uiso 1 1 calc R . . C12 C 0.29491(17) 0.43580(14) 0.38131(8) 0.0213(4) Uani 1 1 d . . . H12 H 0.3054 0.4993 0.3863 0.026 Uiso 1 1 calc R . . C13 C 0.22850(17) 0.38808(14) 0.42111(8) 0.0218(4) Uani 1 1 d . . . C14 C 0.1835(2) 0.43819(16) 0.46520(8) 0.0286(4) Uani 1 1 d . . . H14 H 0.1981 0.5016 0.4681 0.034 Uiso 1 1 calc R . . C15 C 0.1187(2) 0.39515(17) 0.50365(9) 0.0319(5) Uani 1 1 d . . . H15 H 0.0874 0.4289 0.5328 0.038 Uiso 1 1 calc R . . C16 C 0.0991(2) 0.30189(17) 0.49983(8) 0.0294(4) Uani 1 1 d . . . H16 H 0.0559 0.2724 0.5271 0.035 Uiso 1 1 calc R . . C17 C 0.14105(18) 0.25157(14) 0.45724(8) 0.0224(4) Uani 1 1 d . . . C18 C 0.20780(17) 0.29388(14) 0.41608(8) 0.0209(4) Uani 1 1 d . . . O4 O 0.24666(14) 0.24331(9) 0.37670(6) 0.0234(3) Uani 1 1 d . . . O5 O 0.12432(14) 0.15999(11) 0.45039(6) 0.0285(3) Uani 1 1 d . . . C19 C 0.0885(2) 0.11228(17) 0.49801(9) 0.0340(5) Uani 1 1 d . . . H19A H 0.1438 0.1279 0.5308 0.051 Uiso 1 1 calc R . . H19B H 0.0922 0.0468 0.4913 0.051 Uiso 1 1 calc R . . H19C H 0.0051 0.1294 0.5046 0.051 Uiso 1 1 calc R . . O6 O 0.23258(12) 0.19719(9) 0.25699(5) 0.0185(3) Uani 1 1 d . . . C20 C 0.22268(17) 0.10109(13) 0.25608(8) 0.0214(4) Uani 1 1 d . . . H20 H 0.1360 0.0828 0.2465 0.026 Uiso 1 1 calc R . . C21 C 0.3033(2) 0.06255(14) 0.21300(8) 0.0268(4) Uani 1 1 d . . . H21A H 0.3827 0.0437 0.2319 0.032 Uiso 1 1 calc R . . H21B H 0.2638 0.0083 0.1952 0.032 Uiso 1 1 calc R . . N3 N 0.32318(15) 0.13050(11) 0.17014(7) 0.0211(3) Uani 1 1 d . . . C22 C 0.37770(17) 0.10398(14) 0.12787(8) 0.0223(4) Uani 1 1 d . . . H22 H 0.3962 0.0412 0.1259 0.027 Uiso 1 1 calc R . . C23 C 0.41309(17) 0.16046(14) 0.08346(8) 0.0231(4) Uani 1 1 d . . . C24 C 0.47355(19) 0.11792(16) 0.04096(9) 0.0284(4) Uani 1 1 d . . . H24 H 0.4902 0.0548 0.0432 0.034 Uiso 1 1 calc R . . C25 C 0.5084(2) 0.16681(17) -0.00348(9) 0.0316(5) Uani 1 1 d . . . H25 H 0.5502 0.1380 -0.0315 0.038 Uiso 1 1 calc R . . C26 C 0.4817(2) 0.25969(16) -0.00703(9) 0.0291(5) Uani 1 1 d . . . H26 H 0.5052 0.2938 -0.0378 0.035 Uiso 1 1 calc R . . C27 C 0.42165(18) 0.30227(15) 0.03360(8) 0.0244(4) Uani 1 1 d . . . C28 C 0.38716(18) 0.25425(14) 0.08115(8) 0.0213(4) Uani 1 1 d . . . O7 O 0.33197(13) 0.29834(10) 0.11924(6) 0.0239(3) Uani 1 1 d . . . O8 O 0.38999(15) 0.39217(11) 0.03184(6) 0.0302(3) Uani 1 1 d . . . C29 C 0.3841(2) 0.43443(18) -0.02179(9) 0.0352(5) Uani 1 1 d . . . H29A H 0.4667 0.4416 -0.0332 0.053 Uiso 1 1 calc R . . H29B H 0.3456 0.4941 -0.0199 0.053 Uiso 1 1 calc R . . H29C H 0.3361 0.3965 -0.0490 0.053 Uiso 1 1 calc R . . C30 C 0.26737(17) 0.06653(14) 0.31419(8) 0.0218(4) Uani 1 1 d . . . H30A H 0.2062 0.0787 0.3409 0.026 Uiso 1 1 calc R . . H30B H 0.2831 0.0005 0.3134 0.026 Uiso 1 1 calc R . . N4 N 0.37997(14) 0.11632(11) 0.32978(7) 0.0204(3) Uani 1 1 d . . . C31 C 0.47608(18) 0.07466(14) 0.34941(8) 0.0215(4) Uani 1 1 d . . . H31 H 0.4722 0.0106 0.3527 0.026 Uiso 1 1 calc R . . C32 C 0.59065(18) 0.11889(14) 0.36703(8) 0.0221(4) Uani 1 1 d . . . C33 C 0.68568(19) 0.06478(15) 0.39255(8) 0.0266(4) Uani 1 1 d . . . H33 H 0.6752 0.0011 0.3956 0.032 Uiso 1 1 calc R . . C34 C 0.7929(2) 0.10439(17) 0.41279(9) 0.0325(5) Uani 1 1 d . . . H34 H 0.8576 0.0678 0.4290 0.039 Uiso 1 1 calc R . . C35 C 0.80801(19) 0.19858(16) 0.40983(9) 0.0292(4) Uani 1 1 d . . . H35 H 0.8820 0.2254 0.4251 0.035 Uiso 1 1 calc R . . C36 C 0.71664(19) 0.25274(14) 0.38503(8) 0.0230(4) Uani 1 1 d . . . C37 C 0.60547(17) 0.21334(14) 0.36108(8) 0.0204(4) Uani 1 1 d . . . O9 O 0.52327(13) 0.26729(9) 0.33499(6) 0.0226(3) Uani 1 1 d . . . O10 O 0.72164(13) 0.34513(10) 0.38095(6) 0.0283(3) Uani 1 1 d . . . C38 C 0.8233(2) 0.38823(17) 0.41056(10) 0.0345(5) Uani 1 1 d . . . H38A H 0.8285 0.3696 0.4498 0.052 Uiso 1 1 calc R . . H38B H 0.8133 0.4542 0.4081 0.052 Uiso 1 1 calc R . . H38C H 0.8982 0.3706 0.3942 0.052 Uiso 1 1 calc R . . O41 O 0.65908(15) 0.34009(13) 0.24801(7) 0.0360(4) Uani 1 1 d D . . H41 H 0.614(3) 0.324(2) 0.2727(12) 0.054 Uiso 1 1 d D . . C41 C 0.6390(3) 0.2723(3) 0.20678(14) 0.0582(8) Uani 1 1 d . . . H41A H 0.7026 0.2759 0.1809 0.087 Uiso 1 1 calc R . . H41B H 0.5591 0.2815 0.1863 0.087 Uiso 1 1 calc R . . H41C H 0.6415 0.2125 0.2246 0.087 Uiso 1 1 calc R . . O42 O 0.90579(17) 0.38992(14) 0.27222(8) 0.0438(4) Uani 1 1 d D . . H42 H 0.833(2) 0.381(3) 0.2631(15) 0.066 Uiso 1 1 d D . . C42 C 0.9686(3) 0.3074(2) 0.28436(11) 0.0459(6) Uani 1 1 d . . . H42A H 1.0467 0.3201 0.3056 0.069 Uiso 1 1 calc R . . H42B H 0.9830 0.2767 0.2495 0.069 Uiso 1 1 calc R . . H42C H 0.9193 0.2683 0.3064 0.069 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 Fe1 0.01830(15) 0.01855(15) 0.01616(14) 0.00002(9) 0.00389(10) 0.00055(9) Fe2 0.01676(14) 0.01750(15) 0.01669(14) 0.00053(9) 0.00394(10) -0.00057(9) O1 0.0214(6) 0.0178(6) 0.0182(6) 0.0017(5) 0.0049(5) -0.0012(5) C1 0.0264(9) 0.0165(9) 0.0213(9) 0.0028(7) 0.0058(7) -0.0043(7) C2 0.0300(10) 0.0167(9) 0.0244(9) -0.0005(7) 0.0015(8) 0.0010(7) N1 0.0227(8) 0.0205(8) 0.0193(7) 0.0002(6) 0.0054(6) 0.0006(6) C3 0.0279(10) 0.0228(10) 0.0203(9) 0.0020(7) 0.0058(7) 0.0053(8) C4 0.0232(9) 0.0281(10) 0.0167(8) 0.0008(7) 0.0050(7) 0.0032(8) C5 0.0281(10) 0.0310(11) 0.0248(9) 0.0031(8) 0.0039(8) 0.0084(8) C6 0.0265(10) 0.0407(13) 0.0278(10) 0.0038(9) -0.0015(8) 0.0062(9) C7 0.0233(10) 0.0417(13) 0.0248(10) -0.0008(9) 0.0000(8) -0.0024(8) C8 0.0236(9) 0.0305(11) 0.0217(9) -0.0022(8) 0.0035(7) -0.0005(8) C9 0.0195(9) 0.0287(10) 0.0173(9) 0.0011(7) 0.0037(7) 0.0004(7) O2 0.0202(6) 0.0222(7) 0.0276(7) -0.0006(6) -0.0002(5) 0.0012(5) O3 0.0312(8) 0.0278(8) 0.0332(8) -0.0018(6) -0.0044(6) -0.0020(6) C10 0.0561(16) 0.0358(14) 0.0459(14) 0.0091(11) -0.0175(12) -0.0143(12) N2 0.0193(7) 0.0205(8) 0.0198(7) -0.0004(6) 0.0024(6) -0.0013(6) C11 0.0242(9) 0.0176(9) 0.0251(9) 0.0003(7) 0.0046(7) -0.0059(7) C12 0.0219(9) 0.0208(9) 0.0208(9) -0.0019(7) -0.0005(7) 0.0008(7) C13 0.0223(9) 0.0264(10) 0.0167(8) -0.0006(7) 0.0010(7) 0.0043(7) C14 0.0318(11) 0.0306(11) 0.0234(9) -0.0033(8) 0.0032(8) 0.0054(8) C15 0.0331(11) 0.0411(13) 0.0222(10) -0.0051(9) 0.0069(8) 0.0071(9) C16 0.0271(10) 0.0426(13) 0.0193(9) 0.0022(9) 0.0067(7) 0.0040(9) C17 0.0195(9) 0.0293(11) 0.0186(9) 0.0030(7) 0.0032(7) 0.0021(7) C18 0.0182(8) 0.0283(10) 0.0163(8) 0.0010(7) 0.0015(6) 0.0024(7) O4 0.0282(7) 0.0228(7) 0.0207(7) -0.0015(5) 0.0102(6) -0.0019(5) O5 0.0319(8) 0.0297(8) 0.0255(7) 0.0063(6) 0.0117(6) -0.0021(6) C19 0.0315(11) 0.0429(13) 0.0290(11) 0.0121(10) 0.0107(9) -0.0046(10) O6 0.0208(6) 0.0174(7) 0.0177(6) 0.0005(5) 0.0036(5) -0.0019(5) C20 0.0223(8) 0.0195(9) 0.0224(9) 0.0015(7) 0.0023(7) -0.0047(7) C21 0.0417(12) 0.0185(9) 0.0209(9) 0.0014(7) 0.0062(8) 0.0023(8) N3 0.0234(8) 0.0207(8) 0.0193(7) -0.0001(6) 0.0028(6) 0.0006(6) C22 0.0213(9) 0.0242(10) 0.0208(9) -0.0037(7) -0.0003(7) 0.0027(7) C23 0.0189(8) 0.0297(11) 0.0207(9) -0.0039(8) 0.0022(7) 0.0001(7) C24 0.0255(10) 0.0347(12) 0.0255(10) -0.0065(8) 0.0055(8) 0.0009(8) C25 0.0273(10) 0.0462(14) 0.0226(9) -0.0087(9) 0.0093(8) -0.0009(9) C26 0.0251(10) 0.0435(13) 0.0197(10) -0.0019(8) 0.0074(8) -0.0058(9) C27 0.0220(9) 0.0311(11) 0.0203(9) -0.0006(8) 0.0028(7) -0.0033(8) C28 0.0176(9) 0.0303(11) 0.0162(9) -0.0029(7) 0.0035(7) -0.0011(7) O7 0.0291(7) 0.0243(7) 0.0196(6) 0.0001(5) 0.0088(5) 0.0018(6) O8 0.0390(8) 0.0320(8) 0.0211(7) 0.0049(6) 0.0101(6) -0.0012(7) C29 0.0404(12) 0.0420(13) 0.0235(10) 0.0085(9) 0.0050(9) -0.0087(10) C30 0.0223(9) 0.0201(9) 0.0236(9) 0.0021(7) 0.0050(7) -0.0048(7) N4 0.0213(8) 0.0207(8) 0.0198(7) 0.0000(6) 0.0055(6) -0.0020(6) C31 0.0259(9) 0.0218(9) 0.0177(8) 0.0000(7) 0.0074(7) 0.0020(7) C32 0.0234(9) 0.0261(10) 0.0168(8) -0.0006(7) 0.0028(7) 0.0026(7) C33 0.0318(10) 0.0244(10) 0.0235(9) 0.0026(8) 0.0016(8) 0.0057(8) C34 0.0290(11) 0.0351(12) 0.0321(11) 0.0043(9) -0.0041(8) 0.0084(9) C35 0.0239(10) 0.0354(12) 0.0274(10) 0.0015(9) -0.0027(8) 0.0003(8) C36 0.0229(10) 0.0254(10) 0.0211(9) 0.0021(7) 0.0030(7) -0.0001(7) C37 0.0195(9) 0.0250(10) 0.0173(8) 0.0003(7) 0.0044(7) 0.0021(7) O9 0.0196(7) 0.0215(7) 0.0264(7) 0.0042(5) 0.0004(5) 0.0002(5) O10 0.0252(7) 0.0253(8) 0.0333(8) 0.0014(6) -0.0041(6) -0.0044(6) C38 0.0289(11) 0.0324(12) 0.0404(12) -0.0051(10) -0.0062(9) -0.0049(9) O41 0.0329(8) 0.0441(10) 0.0326(8) 0.0006(7) 0.0118(7) -0.0047(7) C41 0.0502(17) 0.078(2) 0.0488(17) -0.0270(16) 0.0174(14) -0.0113(15) O42 0.0328(9) 0.0430(11) 0.0559(11) -0.0038(9) 0.0060(8) 0.0017(8) C42 0.0419(14) 0.0571(17) 0.0401(14) 0.0090(12) 0.0122(11) 0.0117(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 Fe1 O2 1.9284(14) . ? Fe1 O7 1.9417(14) . ? Fe1 O1 2.0187(13) . ? Fe1 O6 2.0297(13) . ? Fe1 N3 2.1348(17) . ? Fe1 N1 2.1435(17) . ? Fe2 O4 1.9312(15) . ? Fe2 O9 1.9583(14) . ? Fe2 O6 2.0258(13) . ? Fe2 O1 2.0533(13) . ? Fe2 N2 2.1508(17) . ? Fe2 N4 2.1546(17) . ? O1 C1 1.420(2) . ? C1 C11 1.529(3) . ? C1 C2 1.532(3) . ? C1 H1 1.0000 . ? C2 N1 1.466(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N1 C3 1.288(3) . ? C3 C4 1.442(3) . ? C3 H3 0.9500 . ? C4 C5 1.410(3) . ? C4 C9 1.420(3) . ? C5 C6 1.377(3) . ? C5 H5 0.9500 . ? C6 C7 1.394(3) . ? C6 H6 0.9500 . ? C7 C8 1.378(3) . ? C7 H7 0.9500 . ? C8 O3 1.376(3) . ? C8 C9 1.420(3) . ? C9 O2 1.309(2) . ? O3 C10 1.425(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? N2 C12 1.281(2) . ? N2 C11 1.463(2) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.441(3) . ? C12 H12 0.9500 . ? C13 C18 1.411(3) . ? C13 C14 1.420(3) . ? C14 C15 1.374(3) . ? C14 H14 0.9500 . ? C15 C16 1.394(3) . ? C15 H15 0.9500 . ? C16 C17 1.379(3) . ? C16 H16 0.9500 . ? C17 O5 1.371(3) . ? C17 C18 1.430(3) . ? C18 O4 1.308(2) . ? O5 C19 1.431(2) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O6 C20 1.421(2) . ? C20 C30 1.529(3) . ? C20 C21 1.535(3) . ? C20 H20 1.0000 . ? C21 N3 1.469(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? N3 C22 1.289(3) . ? C22 C23 1.437(3) . ? C22 H22 0.9500 . ? C23 C28 1.413(3) . ? C23 C24 1.417(3) . ? C24 C25 1.374(3) . ? C24 H24 0.9500 . ? C25 C26 1.402(3) . ? C25 H25 0.9500 . ? C26 C27 1.381(3) . ? C26 H26 0.9500 . ? C27 O8 1.371(3) . ? C27 C28 1.427(3) . ? C28 O7 1.317(2) . ? O8 C29 1.431(2) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 N4 1.462(2) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? N4 C31 1.278(3) . ? C31 C32 1.450(3) . ? C31 H31 0.9500 . ? C32 C37 1.411(3) . ? C32 C33 1.413(3) . ? C33 C34 1.368(3) . ? C33 H33 0.9500 . ? C34 C35 1.402(3) . ? C34 H34 0.9500 . ? C35 C36 1.379(3) . ? C35 H35 0.9500 . ? C36 O10 1.368(3) . ? C36 C37 1.430(3) . ? C37 O9 1.322(2) . ? O10 C38 1.423(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O41 C41 1.413(3) . ? O41 H41 0.84(2) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? O42 C42 1.417(3) . ? O42 H42 0.83(2) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 O2 Fe1 O7 101.99(6) . . ? O2 Fe1 O1 153.65(6) . . ? O7 Fe1 O1 97.78(6) . . ? O2 Fe1 O6 94.13(6) . . ? O7 Fe1 O6 155.91(6) . . ? O1 Fe1 O6 73.48(5) . . ? O2 Fe1 N3 89.43(6) . . ? O7 Fe1 N3 85.39(6) . . ? O1 Fe1 N3 109.50(6) . . ? O6 Fe1 N3 76.91(6) . . ? O2 Fe1 N1 84.13(6) . . ? O7 Fe1 N1 92.88(6) . . ? O1 Fe1 N1 77.60(6) . . ? O6 Fe1 N1 106.60(6) . . ? N3 Fe1 N1 172.85(6) . . ? O4 Fe2 O9 116.80(6) . . ? O4 Fe2 O6 96.53(6) . . ? O9 Fe2 O6 137.46(6) . . ? O4 Fe2 O1 143.10(6) . . ? O9 Fe2 O1 91.92(6) . . ? O6 Fe2 O1 72.84(5) . . ? O4 Fe2 N2 82.78(6) . . ? O9 Fe2 N2 86.01(6) . . ? O6 Fe2 N2 125.91(6) . . ? O1 Fe2 N2 76.30(6) . . ? O4 Fe2 N4 82.19(6) . . ? O9 Fe2 N4 82.89(6) . . ? O6 Fe2 N4 75.94(6) . . ? O1 Fe2 N4 126.49(6) . . ? N2 Fe2 N4 154.81(6) . . ? C1 O1 Fe1 117.38(11) . . ? C1 O1 Fe2 119.32(11) . . ? Fe1 O1 Fe2 106.48(6) . . ? O1 C1 C11 107.04(15) . . ? O1 C1 C2 109.30(15) . . ? C11 C1 C2 110.78(16) . . ? O1 C1 H1 109.9 . . ? C11 C1 H1 109.9 . . ? C2 C1 H1 109.9 . . ? N1 C2 C1 109.44(16) . . ? N1 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? N1 C2 H2B 109.8 . . ? C1 C2 H2B 109.8 . . ? H2A C2 H2B 108.2 . . ? C3 N1 C2 117.84(17) . . ? C3 N1 Fe1 127.46(14) . . ? C2 N1 Fe1 114.66(12) . . ? N1 C3 C4 125.50(19) . . ? N1 C3 H3 117.3 . . ? C4 C3 H3 117.3 . . ? C5 C4 C9 120.11(19) . . ? C5 C4 C3 118.54(19) . . ? C9 C4 C3 121.20(18) . . ? C6 C5 C4 120.7(2) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 119.5(2) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C8 C7 C6 121.1(2) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? O3 C8 C7 117.54(19) . . ? O3 C8 C9 121.46(18) . . ? C7 C8 C9 120.8(2) . . ? O2 C9 C4 123.25(18) . . ? O2 C9 C8 119.31(18) . . ? C4 C9 C8 117.43(18) . . ? C9 O2 Fe1 135.87(13) . . ? C8 O3 C10 118.10(18) . . ? O3 C10 H10A 109.5 . . ? O3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 N2 C11 119.96(17) . . ? C12 N2 Fe2 129.91(14) . . ? C11 N2 Fe2 110.12(12) . . ? N2 C11 C1 106.42(15) . . ? N2 C11 H11A 110.4 . . ? C1 C11 H11A 110.4 . . ? N2 C11 H11B 110.4 . . ? C1 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? N2 C12 C13 124.96(19) . . ? N2 C12 H12 117.5 . . ? C13 C12 H12 117.5 . . ? C18 C13 C14 120.79(19) . . ? C18 C13 C12 120.78(17) . . ? C14 C13 C12 118.43(19) . . ? C15 C14 C13 120.1(2) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.9(2) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C17 C16 C15 121.3(2) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? O5 C17 C16 124.69(19) . . ? O5 C17 C18 114.74(17) . . ? C16 C17 C18 120.57(19) . . ? O4 C18 C13 124.22(18) . . ? O4 C18 C17 118.43(19) . . ? C13 C18 C17 117.35(18) . . ? C18 O4 Fe2 136.98(13) . . ? C17 O5 C19 115.57(17) . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C20 O6 Fe2 120.04(11) . . ? C20 O6 Fe1 117.93(11) . . ? Fe2 O6 Fe1 107.11(6) . . ? O6 C20 C30 107.47(15) . . ? O6 C20 C21 109.35(15) . . ? C30 C20 C21 109.70(16) . . ? O6 C20 H20 110.1 . . ? C30 C20 H20 110.1 . . ? C21 C20 H20 110.1 . . ? N3 C21 C20 110.75(16) . . ? N3 C21 H21A 109.5 . . ? C20 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C22 N3 C21 117.23(17) . . ? C22 N3 Fe1 127.30(14) . . ? C21 N3 Fe1 115.41(12) . . ? N3 C22 C23 126.09(19) . . ? N3 C22 H22 117.0 . . ? C23 C22 H22 117.0 . . ? C28 C23 C24 120.78(19) . . ? C28 C23 C22 121.97(18) . . ? C24 C23 C22 117.23(19) . . ? C25 C24 C23 120.9(2) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.2(2) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C27 C26 C25 120.8(2) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? O8 C27 C26 123.70(19) . . ? O8 C27 C28 114.81(17) . . ? C26 C27 C28 121.5(2) . . ? O7 C28 C23 124.09(18) . . ? O7 C28 C27 119.14(18) . . ? C23 C28 C27 116.75(18) . . ? C28 O7 Fe1 134.23(13) . . ? C27 O8 C29 116.11(17) . . ? O8 C29 H29A 109.5 . . ? O8 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? O8 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N4 C30 C20 105.33(15) . . ? N4 C30 H30A 110.7 . . ? C20 C30 H30A 110.7 . . ? N4 C30 H30B 110.7 . . ? C20 C30 H30B 110.7 . . ? H30A C30 H30B 108.8 . . ? C31 N4 C30 120.66(17) . . ? C31 N4 Fe2 130.46(14) . . ? C30 N4 Fe2 108.85(12) . . ? N4 C31 C32 124.26(18) . . ? N4 C31 H31 117.9 . . ? C32 C31 H31 117.9 . . ? C37 C32 C33 120.91(18) . . ? C37 C32 C31 121.32(17) . . ? C33 C32 C31 117.72(19) . . ? C34 C33 C32 119.8(2) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.5(2) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C36 C35 C34 120.7(2) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? O10 C36 C35 125.15(19) . . ? O10 C36 C37 114.48(18) . . ? C35 C36 C37 120.36(19) . . ? O9 C37 C32 124.19(17) . . ? O9 C37 C36 118.24(18) . . ? C32 C37 C36 117.57(17) . . ? C37 O9 Fe2 134.18(13) . . ? C36 O10 C38 116.36(17) . . ? O10 C38 H38A 109.5 . . ? O10 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O10 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41 O41 H41 104(2) . . ? O41 C41 H41A 109.5 . . ? O41 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O41 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C42 O42 H42 111(3) . . ? O42 C42 H42A 109.5 . . ? O42 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O42 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O41 H41 O9 0.84(2) 2.06(2) 2.889(2) 170(3) . O42 H42 O41 0.83(2) 2.01(3) 2.826(3) 170(4) . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.323 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.086 ######################################################################## data_sc639 _database_code_depnum_ccdc_archive 'CCDC 700805' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 Cl2 Fe4 N4 O12' _chemical_formula_weight 1008.97 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' Fe Fe 0.3463 0.8444 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 9.5718(19) _cell_length_b 20.987(4) _cell_length_c 10.219(2) _cell_angle_alpha 90.00 _cell_angle_beta 114.621(3) _cell_angle_gamma 90.00 _cell_volume 1866.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1376 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 22.48 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 1.738 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5971 _diffrn_reflns_av_R_equivalents 0.2030 _diffrn_reflns_av_sigmaI/netI 0.3626 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2416 _reflns_number_gt 873 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0158P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2416 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2233 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 0.790 _refine_ls_restrained_S_all 0.790 _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 Fe1 Fe 0.4172(2) 0.49763(10) 0.3263(2) 0.0229(5) Uani 1 1 d . . . Fe2 Fe 0.5726(2) 0.36705(9) 0.5049(2) 0.0224(6) Uani 1 1 d . . . O1 O 0.4234(8) 0.4499(3) 0.5187(8) 0.013(2) Uiso 1 1 d . . . C1 C 0.2834(13) 0.4362(6) 0.5300(14) 0.038(4) Uiso 1 1 d . . . H1A H 0.2338 0.4754 0.5347 0.057 Uiso 1 1 calc R . . H1B H 0.3045 0.4118 0.6155 0.057 Uiso 1 1 calc R . . H1C H 0.2172 0.4123 0.4473 0.057 Uiso 1 1 calc R . . Cl1 Cl 0.4398(4) 0.54146(16) 0.1333(3) 0.0272(10) Uani 1 1 d . . . O2 O 0.5018(8) 0.4134(4) 0.3141(9) 0.021(2) Uiso 1 1 d . . . C2 C 0.4000(13) 0.3791(6) 0.1849(13) 0.024(4) Uiso 1 1 d . . . H2A H 0.4104 0.3950 0.0993 0.029 Uiso 1 1 calc R . . C3 C 0.2335(13) 0.3870(6) 0.1702(14) 0.033(4) Uiso 1 1 d . . . H3A H 0.1619 0.3770 0.0725 0.039 Uiso 1 1 calc R . . H3B H 0.2153 0.3576 0.2347 0.039 Uiso 1 1 calc R . . N1 N 0.2072(10) 0.4532(5) 0.2054(10) 0.016(3) Uiso 1 1 d . . . C4 C 0.0757(14) 0.4739(5) 0.1684(13) 0.020(4) Uiso 1 1 d . . . H4A H -0.0041 0.4485 0.1066 0.025 Uiso 1 1 calc R . . C5 C 0.0327(14) 0.5343(6) 0.2118(13) 0.028(4) Uiso 1 1 d . . . C6 C -0.1212(12) 0.5522(6) 0.1666(12) 0.014(3) Uiso 1 1 d . . . H6A H -0.1972 0.5257 0.1032 0.016 Uiso 1 1 calc R . . C7 C -0.1641(14) 0.6070(6) 0.2120(12) 0.020(4) Uiso 1 1 d . . . H7A H -0.2675 0.6178 0.1777 0.025 Uiso 1 1 calc R . . C8 C -0.0508(12) 0.6472(6) 0.3115(13) 0.022(4) Uiso 1 1 d . . . H8A H -0.0798 0.6843 0.3434 0.026 Uiso 1 1 calc R . . C9 C 0.1028(13) 0.6314(6) 0.3611(12) 0.017(3) Uiso 1 1 d . . . O4 O 0.2236(9) 0.6649(4) 0.4547(9) 0.028(3) Uiso 1 1 d . . . C10 C 0.1432(14) 0.5745(6) 0.3118(14) 0.021(4) Uiso 1 1 d . . . O3 O 0.2943(8) 0.5634(3) 0.3643(8) 0.011(2) Uiso 1 1 d . . . C11 C 0.4478(14) 0.3100(6) 0.2131(13) 0.028(4) Uiso 1 1 d . . . H11A H 0.3710 0.2829 0.1425 0.034 Uiso 1 1 calc R . . H11B H 0.5450 0.3034 0.2064 0.034 Uiso 1 1 calc R . . N2 N 0.4634(10) 0.2939(5) 0.3609(11) 0.021(3) Uiso 1 1 d . . . C12 C 0.3967(13) 0.2439(6) 0.3807(14) 0.027(4) Uiso 1 1 d . . . H12A H 0.3459 0.2171 0.3027 0.032 Uiso 1 1 calc R . . C13 C 0.3967(14) 0.2271(7) 0.5193(15) 0.028(4) Uiso 1 1 d . . . C14 C 0.3272(14) 0.1689(6) 0.5284(14) 0.026(4) Uiso 1 1 d . . . H14A H 0.2896 0.1415 0.4496 0.031 Uiso 1 1 calc R . . C15 C 0.3151(13) 0.1525(6) 0.6546(14) 0.031(4) Uiso 1 1 d . . . H15A H 0.2723 0.1135 0.6615 0.037 Uiso 1 1 calc R . . C16 C 0.3683(13) 0.1952(6) 0.7743(14) 0.025(4) Uiso 1 1 d . . . H16A H 0.3576 0.1855 0.8585 0.030 Uiso 1 1 calc R . . C17 C 0.4354(14) 0.2509(6) 0.7609(14) 0.024(4) Uiso 1 1 d . . . O6 O 0.4783(10) 0.2918(4) 0.8759(9) 0.033(3) Uiso 1 1 d . . . H6 H 0.5411 0.3174 0.8721 0.050 Uiso 1 1 calc R . . C18 C 0.4549(14) 0.2682(6) 0.6393(15) 0.025(4) Uiso 1 1 d . . . O5 O 0.5175(8) 0.3239(4) 0.6406(8) 0.017(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 Fe1 0.0289(11) 0.0135(12) 0.0195(11) -0.0018(11) 0.0033(9) -0.0020(11) Fe2 0.0272(12) 0.0133(12) 0.0213(13) -0.0023(12) 0.0048(10) -0.0016(11) Cl1 0.043(2) 0.017(2) 0.014(2) 0.0016(19) 0.0048(19) -0.0045(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 Fe1 O3 1.955(7) . ? Fe1 O2 1.971(8) . ? Fe1 O1 2.009(7) 3_666 ? Fe1 N1 2.090(9) . ? Fe1 O1 2.186(8) . ? Fe1 Cl1 2.266(4) . ? Fe2 O5 1.906(8) . ? Fe2 O4 1.938(8) 3_666 ? Fe2 O2 2.026(8) . ? Fe2 O3 2.030(7) 3_666 ? Fe2 N2 2.081(10) . ? Fe2 O1 2.292(8) . ? O1 C1 1.421(12) . ? O1 Fe1 2.009(7) 3_666 ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? O2 C2 1.462(12) . ? C2 C11 1.513(15) . ? C2 C3 1.546(14) . ? C2 H2A 0.9800 . ? C3 N1 1.481(14) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N1 C4 1.233(12) . ? C4 C5 1.457(15) . ? C4 H4A 0.9300 . ? C5 C6 1.399(14) . ? C5 C10 1.405(15) . ? C6 C7 1.366(14) . ? C6 H6A 0.9300 . ? C7 C8 1.415(14) . ? C7 H7A 0.9300 . ? C8 C9 1.381(14) . ? C8 H8A 0.9300 . ? C9 O4 1.351(12) . ? C9 C10 1.412(15) . ? O4 Fe2 1.937(8) 3_666 ? C10 O3 1.337(12) . ? O3 Fe2 2.030(7) 3_666 ? C11 N2 1.494(14) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? N2 C12 1.288(13) . ? C12 C13 1.459(17) . ? C12 H12A 0.9300 . ? C13 C18 1.410(16) . ? C13 C14 1.413(16) . ? C14 C15 1.386(15) . ? C14 H14A 0.9300 . ? C15 C16 1.429(15) . ? C15 H15A 0.9300 . ? C16 C17 1.368(15) . ? C16 H16A 0.9300 . ? C17 O6 1.371(13) . ? C17 C18 1.379(16) . ? O6 H6 0.8200 . ? C18 O5 1.311(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Fe1 O2 160.6(3) . . ? O3 Fe1 O1 77.2(3) . 3_666 ? O2 Fe1 O1 110.2(3) . 3_666 ? O3 Fe1 N1 85.6(3) . . ? O2 Fe1 N1 83.2(4) . . ? O1 Fe1 N1 159.8(3) 3_666 . ? O3 Fe1 O1 86.4(3) . . ? O2 Fe1 O1 77.7(3) . . ? O1 Fe1 O1 79.3(3) 3_666 . ? N1 Fe1 O1 89.2(3) . . ? O3 Fe1 Cl1 99.8(3) . . ? O2 Fe1 Cl1 96.8(3) . . ? O1 Fe1 Cl1 98.5(2) 3_666 . ? N1 Fe1 Cl1 94.8(3) . . ? O1 Fe1 Cl1 172.8(3) . . ? O5 Fe2 O4 103.9(3) . 3_666 ? O5 Fe2 O2 147.7(3) . . ? O4 Fe2 O2 105.9(3) 3_666 . ? O5 Fe2 O3 98.7(3) . 3_666 ? O4 Fe2 O3 79.0(3) 3_666 3_666 ? O2 Fe2 O3 98.9(3) . 3_666 ? O5 Fe2 N2 87.4(4) . . ? O4 Fe2 N2 93.4(4) 3_666 . ? O2 Fe2 N2 78.8(4) . . ? O3 Fe2 N2 171.2(4) 3_666 . ? O5 Fe2 O1 87.0(3) . . ? O4 Fe2 O1 147.9(3) 3_666 . ? O2 Fe2 O1 74.2(3) . . ? O3 Fe2 O1 69.5(3) 3_666 . ? N2 Fe2 O1 117.4(3) . . ? C1 O1 Fe1 118.6(7) . 3_666 ? C1 O1 Fe1 119.5(7) . . ? Fe1 O1 Fe1 100.7(3) 3_666 . ? C1 O1 Fe2 119.0(7) . . ? Fe1 O1 Fe2 100.2(3) 3_666 . ? Fe1 O1 Fe2 94.4(3) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C2 O2 Fe1 111.2(6) . . ? C2 O2 Fe2 117.6(7) . . ? Fe1 O2 Fe2 110.6(4) . . ? O2 C2 C11 105.4(9) . . ? O2 C2 C3 107.9(10) . . ? C11 C2 C3 109.9(10) . . ? O2 C2 H2A 111.2 . . ? C11 C2 H2A 111.2 . . ? C3 C2 H2A 111.2 . . ? N1 C3 C2 110.5(10) . . ? N1 C3 H3A 109.6 . . ? C2 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C2 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? C4 N1 C3 120.8(10) . . ? C4 N1 Fe1 129.1(9) . . ? C3 N1 Fe1 110.1(7) . . ? N1 C4 C5 126.6(11) . . ? N1 C4 H4A 116.7 . . ? C5 C4 H4A 116.7 . . ? C6 C5 C10 116.7(12) . . ? C6 C5 C4 121.6(11) . . ? C10 C5 C4 121.3(11) . . ? C7 C6 C5 122.5(12) . . ? C7 C6 H6A 118.7 . . ? C5 C6 H6A 118.7 . . ? C6 C7 C8 119.8(11) . . ? C6 C7 H7A 120.1 . . ? C8 C7 H7A 120.1 . . ? C9 C8 C7 120.0(12) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? O4 C9 C8 127.0(12) . . ? O4 C9 C10 114.3(10) . . ? C8 C9 C10 118.7(11) . . ? C9 O4 Fe2 117.4(7) . 3_666 ? O3 C10 C5 123.3(12) . . ? O3 C10 C9 114.6(11) . . ? C5 C10 C9 122.1(11) . . ? C10 O3 Fe1 133.1(7) . . ? C10 O3 Fe2 114.6(7) . 3_666 ? Fe1 O3 Fe2 112.0(3) . 3_666 ? N2 C11 C2 107.6(11) . . ? N2 C11 H11A 110.2 . . ? C2 C11 H11A 110.2 . . ? N2 C11 H11B 110.2 . . ? C2 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C12 N2 C11 119.7(11) . . ? C12 N2 Fe2 128.8(10) . . ? C11 N2 Fe2 111.0(7) . . ? N2 C12 C13 123.3(13) . . ? N2 C12 H12A 118.4 . . ? C13 C12 H12A 118.4 . . ? C18 C13 C14 119.9(13) . . ? C18 C13 C12 122.5(13) . . ? C14 C13 C12 117.5(13) . . ? C15 C14 C13 120.0(13) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 120.1(12) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C17 C16 C15 117.8(13) . . ? C17 C16 H16A 121.1 . . ? C15 C16 H16A 121.1 . . ? C16 C17 O6 115.7(13) . . ? C16 C17 C18 124.0(13) . . ? O6 C17 C18 120.2(12) . . ? C17 O6 H6 109.5 . . ? O5 C18 C17 117.2(13) . . ? O5 C18 C13 124.6(13) . . ? C17 C18 C13 118.1(13) . . ? C18 O5 Fe2 132.8(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.574 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.142 ######################################################################## data_lyh14bx _database_code_depnum_ccdc_archive 'CCDC 700806' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H62 Mn4 N8 O16' _chemical_formula_weight 1226.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4306(9) _cell_length_b 10.7571(9) _cell_length_c 12.2161(10) _cell_angle_alpha 104.446(2) _cell_angle_beta 101.777(1) _cell_angle_gamma 92.127(2) _cell_volume 1293.79(19) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4370 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.99 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634 _exptl_absorpt_coefficient_mu 1.032 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.844 _exptl_absorpt_correction_T_max 0.863 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6454 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0697 _diffrn_reflns_limit_h_min -12 _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 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4484 _reflns_number_gt 3580 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The non-coordinated ligand hydroxyl group and the oxygen of the lattice DMF molecule were twofold disordered, and restraints were applied to the respective C-O bond lengths. ; _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^)+(0.0523P)^2^+3.9193P] 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 4484 _refine_ls_number_parameters 350 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1321 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 0.59338(7) 0.41401(7) 0.54565(6) 0.01383(19) Uani 1 1 d . . . Mn2 Mn 0.27435(7) 0.23281(7) 0.36605(7) 0.0176(2) Uani 1 1 d . B . O1 O 0.5625(3) 0.5029(3) 0.4236(3) 0.0135(7) Uani 1 1 d . . . C1 C 0.5770(5) 0.4491(5) 0.3088(4) 0.0224(11) Uani 1 1 d . . . H1A H 0.6616 0.4119 0.3110 0.034 Uiso 0.50 1 calc PR . . H1B H 0.5741 0.5167 0.2676 0.034 Uiso 0.50 1 calc PR . . H1C H 0.5054 0.3815 0.2684 0.034 Uiso 0.50 1 calc PR . . H1D H 0.4991 0.4615 0.2536 0.034 Uiso 0.50 1 calc PR . . H1E H 0.5866 0.3567 0.2970 0.034 Uiso 0.50 1 calc PR . . H1F H 0.6553 0.4919 0.2963 0.034 Uiso 0.50 1 calc PR . . C2 C 0.0718(5) -0.0500(5) 0.1946(4) 0.0242(12) Uani 1 1 d D . . H2C H -0.0021 -0.1194 0.1742 0.029 Uiso 0.85 1 calc PR A 1 H2D H 0.1241 -0.0688 0.1332 0.029 Uiso 0.15 1 calc PR A 2 O2A O 0.1468(4) -0.0849(4) 0.1082(4) 0.0255(10) Uani 0.85 1 d PD B 1 H2A H 0.1440 -0.0289 0.0707 0.038 Uiso 0.85 1 calc PR B 1 O2B O -0.0500(19) -0.131(2) 0.158(2) 0.030(6) Uiso 0.15 1 d PD B 2 H2B H -0.1132 -0.0857 0.1495 0.045 Uiso 0.15 1 calc PR B 2 C3 C 0.1556(5) -0.0566(5) 0.3106(4) 0.0224(11) Uani 1 1 d . B . H3A H 0.1054 -0.0292 0.3717 0.027 Uiso 1 1 calc R . . H3B H 0.1745 -0.1470 0.3064 0.027 Uiso 1 1 calc R . . N1 N 0.2799(4) 0.0251(4) 0.3424(4) 0.0195(9) Uani 1 1 d . . . C4 C 0.3837(5) -0.0361(5) 0.3457(4) 0.0206(11) Uani 1 1 d . B . H4A H 0.3705 -0.1273 0.3295 0.025 Uiso 1 1 calc R . . C5 C 0.5193(5) 0.0197(5) 0.3716(4) 0.0196(11) Uani 1 1 d . . . C6 C 0.5567(5) 0.1520(5) 0.4145(4) 0.0168(10) Uani 1 1 d . B . O3 O 0.4740(3) 0.2418(3) 0.4369(3) 0.0170(7) Uani 1 1 d . . . C7 C 0.6933(5) 0.1960(5) 0.4403(4) 0.0188(11) Uani 1 1 d . . . O4 O 0.7285(3) 0.3229(3) 0.4868(3) 0.0185(8) Uani 1 1 d . B . C8 C 0.7844(5) 0.1092(5) 0.4166(4) 0.0217(11) Uani 1 1 d . B . H8A H 0.8746 0.1390 0.4306 0.026 Uiso 1 1 calc R . . C9 C 0.7443(5) -0.0229(5) 0.3721(5) 0.0268(12) Uani 1 1 d . . . H9A H 0.8076 -0.0820 0.3554 0.032 Uiso 1 1 calc R B . C10 C 0.6149(5) -0.0673(5) 0.3524(5) 0.0247(12) Uani 1 1 d . B . H10A H 0.5894 -0.1573 0.3256 0.030 Uiso 1 1 calc R . . C11 C 0.0086(5) 0.0747(5) 0.1959(5) 0.0223(11) Uani 1 1 d . B . H11A H -0.0542 0.0643 0.1209 0.027 Uiso 1 1 calc R . . H11B H -0.0420 0.0915 0.2576 0.027 Uiso 1 1 calc R . . N2 N 0.1036(4) 0.1872(4) 0.2156(4) 0.0204(9) Uani 1 1 d . . . C12 C 0.0881(5) 0.2451(5) 0.1347(5) 0.0238(12) Uani 1 1 d . B . H12A H 0.0227 0.2059 0.0669 0.029 Uiso 1 1 calc R . . C13 C 0.1589(5) 0.3636(5) 0.1347(4) 0.0186(11) Uani 1 1 d . . . C14 C 0.2443(5) 0.4442(5) 0.2319(4) 0.0171(10) Uani 1 1 d . B . O5 O 0.2778(3) 0.4174(3) 0.3354(3) 0.0165(7) Uani 1 1 d . . . C15 C 0.2982(5) 0.5642(5) 0.2242(4) 0.0200(11) Uani 1 1 d . . . O6 O 0.3779(3) 0.6432(3) 0.3181(3) 0.0184(7) Uani 1 1 d . . . C16 C 0.2690(5) 0.5982(5) 0.1209(5) 0.0266(12) Uani 1 1 d . B . H16A H 0.3060 0.6782 0.1162 0.032 Uiso 1 1 calc R . . C17 C 0.1865(6) 0.5173(6) 0.0242(5) 0.0381(15) Uani 1 1 d . . . H17A H 0.1681 0.5411 -0.0469 0.046 Uiso 1 1 calc R B . C18 C 0.1313(6) 0.4030(6) 0.0311(5) 0.0315(13) Uani 1 1 d . B . H18A H 0.0732 0.3488 -0.0353 0.038 Uiso 1 1 calc R . . O7 O 0.1642(3) 0.2787(3) 0.4981(3) 0.0201(8) Uani 1 1 d . . . C19 C 0.1464(5) 0.3918(5) 0.5433(4) 0.0185(11) Uani 1 1 d . B . H19A H 0.1810 0.4575 0.5150 0.022 Uiso 1 1 calc R . . N3 N 0.0829(4) 0.4277(4) 0.6276(4) 0.0191(9) Uani 1 1 d . . . C20 C 0.0671(5) 0.5632(5) 0.6754(5) 0.0238(12) Uani 1 1 d . B . H20A H 0.1057 0.6156 0.6331 0.036 Uiso 1 1 calc R . . H20B H 0.1117 0.5899 0.7575 0.036 Uiso 1 1 calc R . . H20C H -0.0267 0.5751 0.6678 0.036 Uiso 1 1 calc R . . C21 C 0.0254(6) 0.3358(5) 0.6763(5) 0.0293(13) Uani 1 1 d . B . H21A H 0.0397 0.2483 0.6359 0.044 Uiso 1 1 calc R . . H21B H -0.0693 0.3438 0.6671 0.044 Uiso 1 1 calc R . . H21C H 0.0666 0.3529 0.7588 0.044 Uiso 1 1 calc R . . C32 C 0.6568(8) 0.1955(9) 0.0785(8) 0.069(2) Uani 1 1 d . . . H32A H 0.6966 0.1517 0.1366 0.104 Uiso 1 1 calc R . . H32B H 0.6887 0.2871 0.1047 0.104 Uiso 1 1 calc R . . H32C H 0.6810 0.1567 0.0048 0.104 Uiso 1 1 calc R . . C33 C 0.4409(8) 0.2494(9) -0.0138(8) 0.066(2) Uani 1 1 d . . . H33A H 0.3466 0.2306 -0.0204 0.099 Uiso 1 1 calc R . . H33B H 0.4613 0.2213 -0.0906 0.099 Uiso 1 1 calc R . . H33C H 0.4649 0.3424 0.0176 0.099 Uiso 1 1 calc R . . N31 N 0.5145(6) 0.1818(5) 0.0624(4) 0.0387(13) Uani 1 1 d . D . C31 C 0.4632(8) 0.1153(8) 0.1224(8) 0.061(2) Uani 1 1 d D . . H31A H 0.5155 0.0914 0.1859 0.074 Uiso 0.58 1 calc PR C 1 H31B H 0.5122 0.0503 0.1463 0.074 Uiso 0.42 1 calc PR C 2 O31A O 0.3402(10) 0.0848(12) 0.0908(11) 0.076(3) Uiso 0.58 1 d PD D 1 O31B O 0.3592(11) 0.1302(13) 0.1493(12) 0.051(3) Uiso 0.42 1 d PD D 2 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 0.0157(4) 0.0112(4) 0.0149(4) 0.0035(3) 0.0038(3) 0.0014(3) Mn2 0.0164(4) 0.0119(4) 0.0224(4) 0.0035(3) 0.0017(3) -0.0020(3) O1 0.0179(17) 0.0096(16) 0.0131(17) 0.0023(13) 0.0043(14) 0.0048(13) C1 0.019(3) 0.031(3) 0.016(3) 0.004(2) 0.002(2) 0.002(2) C2 0.026(3) 0.021(3) 0.020(3) -0.003(2) 0.008(2) -0.015(2) O2A 0.032(2) 0.026(2) 0.020(2) 0.0059(19) 0.0081(19) 0.001(2) C3 0.032(3) 0.015(3) 0.022(3) 0.002(2) 0.012(2) -0.006(2) N1 0.022(2) 0.016(2) 0.018(2) 0.0021(17) 0.0030(18) -0.0022(18) C4 0.035(3) 0.015(3) 0.013(2) 0.003(2) 0.007(2) 0.001(2) C5 0.031(3) 0.015(3) 0.014(3) 0.004(2) 0.007(2) 0.002(2) C6 0.023(3) 0.014(2) 0.015(2) 0.0034(19) 0.007(2) 0.003(2) O3 0.0136(17) 0.0123(17) 0.0219(19) 0.0008(14) 0.0009(14) 0.0012(13) C7 0.028(3) 0.015(3) 0.014(3) 0.004(2) 0.005(2) 0.004(2) O4 0.0172(17) 0.0119(17) 0.027(2) 0.0042(15) 0.0065(15) 0.0029(14) C8 0.024(3) 0.022(3) 0.022(3) 0.007(2) 0.009(2) 0.007(2) C9 0.031(3) 0.026(3) 0.026(3) 0.007(2) 0.010(2) 0.013(2) C10 0.037(3) 0.014(3) 0.021(3) -0.002(2) 0.008(2) 0.006(2) C11 0.014(2) 0.029(3) 0.024(3) 0.007(2) 0.006(2) -0.008(2) N2 0.021(2) 0.021(2) 0.017(2) 0.0005(18) 0.0057(18) -0.0031(18) C12 0.022(3) 0.026(3) 0.020(3) -0.001(2) 0.006(2) -0.001(2) C13 0.021(3) 0.021(3) 0.013(2) 0.005(2) 0.003(2) 0.001(2) C14 0.016(2) 0.021(3) 0.015(3) 0.004(2) 0.006(2) 0.003(2) O5 0.0188(17) 0.0159(18) 0.0150(17) 0.0039(14) 0.0044(14) -0.0005(14) C15 0.020(3) 0.022(3) 0.017(3) 0.003(2) 0.005(2) 0.003(2) O6 0.0240(18) 0.0161(18) 0.0164(18) 0.0080(14) 0.0030(15) -0.0014(15) C16 0.032(3) 0.026(3) 0.024(3) 0.013(2) 0.003(2) -0.002(2) C17 0.053(4) 0.042(4) 0.020(3) 0.017(3) 0.000(3) -0.005(3) C18 0.039(3) 0.033(3) 0.017(3) 0.005(2) -0.002(2) -0.007(3) O7 0.0229(19) 0.0163(19) 0.0221(19) 0.0036(15) 0.0088(15) 0.0015(15) C19 0.012(2) 0.026(3) 0.018(3) 0.008(2) 0.003(2) -0.001(2) N3 0.019(2) 0.019(2) 0.021(2) 0.0064(18) 0.0050(18) 0.0007(18) C20 0.026(3) 0.022(3) 0.023(3) 0.004(2) 0.008(2) 0.003(2) C21 0.035(3) 0.027(3) 0.031(3) 0.010(2) 0.016(3) -0.001(3) C32 0.060(5) 0.083(7) 0.069(6) 0.030(5) 0.015(5) 0.006(5) C33 0.057(5) 0.077(6) 0.077(6) 0.036(5) 0.025(4) 0.006(4) N31 0.058(3) 0.036(3) 0.031(3) 0.011(2) 0.027(3) 0.005(3) C31 0.065(5) 0.066(5) 0.076(6) 0.035(5) 0.047(5) 0.016(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O6 1.886(3) 2_666 ? Mn1 O4 1.905(3) . ? Mn1 O1 1.942(3) 2_666 ? Mn1 O1 1.944(3) . ? Mn1 O3 2.161(3) . ? Mn1 O5 2.216(3) 2_666 ? Mn1 Mn1 2.9785(14) 2_666 ? Mn2 O3 2.075(3) . ? Mn2 O5 2.110(3) . ? Mn2 O7 2.137(3) . ? Mn2 N1 2.185(4) . ? Mn2 N2 2.223(4) . ? O1 C1 1.419(6) . ? O1 Mn1 1.942(3) 2_666 ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C1 H1F 0.9800 . ? C2 O2A 1.425(6) . ? C2 O2B 1.439(17) . ? C2 C11 1.514(8) . ? C2 C3 1.525(7) . ? C2 H2C 1.0000 . ? C2 H2D 1.0000 . ? O2A H2A 0.8400 . ? O2B H2B 0.8400 . ? C3 N1 1.464(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N1 C4 1.286(6) . ? C4 C5 1.456(7) . ? C4 H4A 0.9500 . ? C5 C6 1.398(7) . ? C5 C10 1.407(7) . ? C6 O3 1.333(6) . ? C6 C7 1.430(7) . ? C7 O4 1.346(6) . ? C7 C8 1.379(7) . ? C8 C9 1.402(8) . ? C8 H8A 0.9500 . ? C9 C10 1.368(8) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 N2 1.473(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N2 C12 1.281(7) . ? C12 C13 1.449(7) . ? C12 H12A 0.9500 . ? C13 C14 1.397(7) . ? C13 C18 1.411(7) . ? C14 O5 1.348(6) . ? C14 C15 1.421(7) . ? O5 Mn1 2.216(3) 2_666 ? C15 O6 1.342(6) . ? C15 C16 1.378(7) . ? O6 Mn1 1.886(3) 2_666 ? C16 C17 1.382(8) . ? C16 H16A 0.9500 . ? C17 C18 1.367(8) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? O7 C19 1.242(6) . ? C19 N3 1.322(6) . ? C19 H19A 0.9500 . ? N3 C21 1.444(6) . ? N3 C20 1.457(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C32 N31 1.454(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 N31 1.440(9) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? N31 C31 1.315(8) . ? C31 O31B 1.201(12) . ? C31 O31A 1.268(11) . ? C31 H31A 0.9500 . ? C31 H31B 0.9500 . ? 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 O6 Mn1 O4 94.26(15) 2_666 . ? O6 Mn1 O1 93.79(14) 2_666 2_666 ? O4 Mn1 O1 169.50(14) . 2_666 ? O6 Mn1 O1 169.79(14) 2_666 . ? O4 Mn1 O1 92.99(14) . . ? O1 Mn1 O1 79.94(14) 2_666 . ? O6 Mn1 O3 95.40(14) 2_666 . ? O4 Mn1 O3 81.47(13) . . ? O1 Mn1 O3 91.06(13) 2_666 . ? O1 Mn1 O3 92.79(13) . . ? O6 Mn1 O5 81.20(13) 2_666 2_666 ? O4 Mn1 O5 97.01(13) . 2_666 ? O1 Mn1 O5 90.88(13) 2_666 2_666 ? O1 Mn1 O5 90.78(13) . 2_666 ? O3 Mn1 O5 176.19(13) . 2_666 ? O3 Mn2 O5 96.24(13) . . ? O3 Mn2 O7 111.30(14) . . ? O5 Mn2 O7 95.52(13) . . ? O3 Mn2 N1 84.57(14) . . ? O5 Mn2 N1 162.05(14) . . ? O7 Mn2 N1 100.91(14) . . ? O3 Mn2 N2 151.63(15) . . ? O5 Mn2 N2 83.61(14) . . ? O7 Mn2 N2 96.90(14) . . ? N1 Mn2 N2 87.24(16) . . ? C1 O1 Mn1 121.5(3) . 2_666 ? C1 O1 Mn1 124.2(3) . . ? Mn1 O1 Mn1 100.06(14) 2_666 . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C1 H1D 109.5 . . ? O1 C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? O1 C1 H1F 109.5 . . ? H1D C1 H1F 109.5 . . ? H1E C1 H1F 109.5 . . ? O2A C2 C11 113.9(4) . . ? O2B C2 C11 95.3(11) . . ? O2A C2 C3 108.7(4) . . ? O2B C2 C3 114.6(11) . . ? C11 C2 C3 115.1(4) . . ? O2A C2 H2C 106.1 . . ? C11 C2 H2C 106.1 . . ? C3 C2 H2C 106.1 . . ? O2B C2 H2D 110.3 . . ? C11 C2 H2D 110.3 . . ? C3 C2 H2D 110.3 . . ? H2C C2 H2D 108.4 . . ? C2 O2A H2A 109.5 . . ? C2 O2B H2B 109.5 . . ? N1 C3 C2 112.3(4) . . ? N1 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? N1 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C4 N1 C3 115.0(4) . . ? C4 N1 Mn2 126.0(3) . . ? C3 N1 Mn2 118.8(3) . . ? N1 C4 C5 126.8(5) . . ? N1 C4 H4A 116.6 . . ? C5 C4 H4A 116.6 . . ? C6 C5 C10 120.1(5) . . ? C6 C5 C4 123.4(5) . . ? C10 C5 C4 116.5(4) . . ? O3 C6 C5 124.7(4) . . ? O3 C6 C7 116.6(4) . . ? C5 C6 C7 118.7(4) . . ? C6 O3 Mn2 128.3(3) . . ? C6 O3 Mn1 106.4(3) . . ? Mn2 O3 Mn1 124.78(15) . . ? O4 C7 C8 122.0(5) . . ? O4 C7 C6 118.1(4) . . ? C8 C7 C6 119.9(4) . . ? C7 O4 Mn1 113.3(3) . . ? C7 C8 C9 120.3(5) . . ? C7 C8 H8A 119.9 . . ? C9 C8 H8A 119.9 . . ? C10 C9 C8 120.5(5) . . ? C10 C9 H9A 119.7 . . ? C8 C9 H9A 119.7 . . ? C9 C10 C5 120.3(5) . . ? C9 C10 H10A 119.8 . . ? C5 C10 H10A 119.8 . . ? N2 C11 C2 113.7(4) . . ? N2 C11 H11A 108.8 . . ? C2 C11 H11A 108.8 . . ? N2 C11 H11B 108.8 . . ? C2 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C12 N2 C11 115.4(4) . . ? C12 N2 Mn2 123.7(3) . . ? C11 N2 Mn2 120.4(3) . . ? N2 C12 C13 127.5(5) . . ? N2 C12 H12A 116.3 . . ? C13 C12 H12A 116.3 . . ? C14 C13 C18 118.7(5) . . ? C14 C13 C12 124.3(5) . . ? C18 C13 C12 116.8(5) . . ? O5 C14 C13 124.2(4) . . ? O5 C14 C15 116.6(4) . . ? C13 C14 C15 119.2(4) . . ? C14 O5 Mn2 126.6(3) . . ? C14 O5 Mn1 106.7(3) . 2_666 ? Mn2 O5 Mn1 122.99(15) . 2_666 ? O6 C15 C16 120.7(5) . . ? O6 C15 C14 119.3(4) . . ? C16 C15 C14 120.0(5) . . ? C15 O6 Mn1 116.2(3) . 2_666 ? C15 C16 C17 120.8(5) . . ? C15 C16 H16A 119.6 . . ? C17 C16 H16A 119.6 . . ? C18 C17 C16 119.8(5) . . ? C18 C17 H17A 120.1 . . ? C16 C17 H17A 120.1 . . ? C17 C18 C13 121.5(5) . . ? C17 C18 H18A 119.3 . . ? C13 C18 H18A 119.3 . . ? C19 O7 Mn2 121.6(3) . . ? O7 C19 N3 125.0(5) . . ? O7 C19 H19A 117.5 . . ? N3 C19 H19A 117.5 . . ? C19 N3 C21 122.1(4) . . ? C19 N3 C20 121.1(4) . . ? C21 N3 C20 116.8(4) . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N31 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N31 C33 H33A 109.5 . . ? N31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 N31 C33 125.0(7) . . ? C31 N31 C32 118.3(7) . . ? C33 N31 C32 116.6(6) . . ? O31B C31 N31 125.1(9) . . ? O31A C31 N31 116.3(9) . . ? O31A C31 H31A 121.9 . . ? N31 C31 H31A 121.9 . . ? O31B C31 H31B 117.5 . . ? N31 C31 H31B 117.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.385 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.093 ########################################################################### data_lyh7bx _database_code_depnum_ccdc_archive 'CCDC 700807' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C40 H46 Cu6 N4 O24 S3), 3.5(C2 H3 N), 3.5(C H4 O), H2 O' _chemical_formula_sum 'C50.50 H72.50 Cu6 N7.50 O28.50 S3' _chemical_formula_weight 1718.08 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 20.428(2) _cell_length_b 21.839(3) _cell_length_c 16.2244(18) _cell_angle_alpha 90.00 _cell_angle_beta 105.001(2) _cell_angle_gamma 90.00 _cell_volume 6991.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4028 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.07 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3512 _exptl_absorpt_coefficient_mu 1.967 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.782 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details 'SADABS (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13166 _diffrn_reflns_av_R_equivalents 0.0866 _diffrn_reflns_av_sigmaI/netI 0.1970 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.12 _reflns_number_total 6209 _reflns_number_gt 2787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2000)' _computing_data_reduction 'SAINT+ 6.0 (Bruker AXS Inc., 2000)' _computing_structure_solution 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_structure_refinement 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_molecular_graphics 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _computing_publication_material 'SHELXTL 5.1 (Bruker AXS Inc., 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The sulphate ligand containing S(1) lies across a crystal-twofold axis, and atoms S(1), O(11) and O(13) are disordered. The lattice solvent molecules are also disordered and were refined with partial atoms, using geometrical restraints, and in some cases similarity restraints on the temperature factors. No attempt was made to place H atoms on these lattice solvent molecules. ; _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^)+(0.0191P)^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 6209 _refine_ls_number_parameters 451 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1457 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1002 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 1.330 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.002 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 0.53596(6) 0.04872(6) 0.15194(8) 0.0335(4) Uani 1 1 d . . . Cu2 Cu 0.39160(6) 0.13373(6) 0.16772(8) 0.0329(4) Uani 1 1 d . . . Cu3 Cu 0.39823(6) 0.27657(6) 0.21491(8) 0.0344(4) Uani 1 1 d . . . S1 S 0.5003(9) 0.3879(3) 0.2716(5) 0.045(3) Uani 0.50 -1 d P . . O11 O 0.501(3) 0.4463(6) 0.229(3) 0.058(11) Uani 0.50 -1 d P . . O12 O 0.4413(4) 0.3529(4) 0.2569(5) 0.068(3) Uani 1 1 d . . . O13 O 0.5277(8) 0.3947(7) 0.3640(11) 0.058(5) Uani 0.50 -1 d P . . S2 S 0.52593(13) 0.18869(12) 0.13634(18) 0.0300(7) Uani 1 1 d . . . O21 O 0.5611(3) 0.1339(3) 0.1854(4) 0.0282(16) Uani 1 1 d . . . O22 O 0.4589(3) 0.1964(3) 0.1570(4) 0.0301(18) Uani 1 1 d . . . O23 O 0.5681(3) 0.2433(3) 0.1687(4) 0.0323(18) Uani 1 1 d . . . O24 O 0.5172(3) 0.1813(3) 0.0463(4) 0.0330(18) Uani 1 1 d . . . O1 O 0.4439(3) 0.0622(3) 0.1575(4) 0.0356(19) Uani 1 1 d . . . C1 C 0.4000(5) 0.0130(5) 0.1201(7) 0.044(3) Uani 1 1 d . . . H1A H 0.3874 0.0231 0.0579 0.053 Uiso 1 1 calc R . . C2 C 0.4370(5) -0.0449(5) 0.1242(7) 0.048(3) Uani 1 1 d . . . H2A H 0.4141 -0.0714 0.0758 0.058 Uiso 1 1 calc R . . H2B H 0.4372 -0.0666 0.1779 0.058 Uiso 1 1 calc R . . N1 N 0.5075(4) -0.0331(4) 0.1207(5) 0.035(2) Uani 1 1 d . . . C3 C 0.5432(5) -0.0757(5) 0.0976(6) 0.032(3) Uani 1 1 d . . . H3A H 0.5216 -0.1140 0.0810 0.038 Uiso 1 1 calc R . . C4 C 0.6123(5) -0.0699(5) 0.0952(6) 0.027(3) Uani 1 1 d . . . C5 C 0.6500(6) -0.0150(5) 0.1194(6) 0.034(3) Uani 1 1 d . . . O2 O 0.6253(3) 0.0357(3) 0.1442(4) 0.0366(19) Uani 1 1 d . . . C6 C 0.7189(5) -0.0165(5) 0.1152(6) 0.038(3) Uani 1 1 d . . . O3 O 0.7528(3) 0.0380(3) 0.1408(5) 0.047(2) Uani 1 1 d . . . C10 C 0.8205(5) 0.0405(5) 0.1333(8) 0.064(4) Uani 1 1 d . . . H10A H 0.8402 0.0805 0.1530 0.097 Uiso 1 1 calc R . . H10B H 0.8207 0.0346 0.0735 0.097 Uiso 1 1 calc R . . H10C H 0.8473 0.0081 0.1683 0.097 Uiso 1 1 calc R . . C7 C 0.7455(6) -0.0663(5) 0.0858(7) 0.043(3) Uani 1 1 d . . . H7A H 0.7911 -0.0649 0.0819 0.052 Uiso 1 1 calc R . . C8 C 0.7083(6) -0.1188(5) 0.0616(7) 0.047(3) Uani 1 1 d . . . H8A H 0.7280 -0.1534 0.0419 0.056 Uiso 1 1 calc R . . C9 C 0.6420(6) -0.1203(5) 0.0662(6) 0.037(3) Uani 1 1 d . . . H9A H 0.6160 -0.1564 0.0494 0.044 Uiso 1 1 calc R . . C11 C 0.3351(5) 0.0145(5) 0.1424(8) 0.052(3) Uani 1 1 d . . . H11A H 0.2995 -0.0042 0.0960 0.062 Uiso 1 1 calc R . . H11B H 0.3384 -0.0095 0.1951 0.062 Uiso 1 1 calc R . . N2 N 0.3166(4) 0.0778(4) 0.1557(5) 0.034(2) Uani 1 1 d . . . C12 C 0.2580(5) 0.0910(5) 0.1647(6) 0.038(3) Uani 1 1 d . . . H12A H 0.2263 0.0584 0.1575 0.045 Uiso 1 1 calc R . . C13 C 0.2350(5) 0.1500(5) 0.1846(7) 0.036(3) Uani 1 1 d . . . C14 C 0.2761(5) 0.2030(5) 0.1942(6) 0.032(3) Uani 1 1 d . . . O4 O 0.3379(3) 0.2048(3) 0.1783(4) 0.0314(18) Uani 1 1 d . . . C15 C 0.2512(5) 0.2578(5) 0.2237(6) 0.034(3) Uani 1 1 d . . . O5 O 0.2959(3) 0.3062(3) 0.2343(4) 0.0381(19) Uani 1 1 d . . . C19 C 0.2795(5) 0.3590(5) 0.2779(7) 0.058(4) Uani 1 1 d . . . H19A H 0.2311 0.3586 0.2754 0.086 Uiso 1 1 calc R . . H19B H 0.2904 0.3962 0.2505 0.086 Uiso 1 1 calc R . . H19C H 0.3059 0.3582 0.3377 0.086 Uiso 1 1 calc R . . C16 C 0.1882(6) 0.2591(6) 0.2378(7) 0.049(3) Uani 1 1 d . . . H16A H 0.1721 0.2961 0.2563 0.059 Uiso 1 1 calc R . . C17 C 0.1472(6) 0.2073(6) 0.2254(8) 0.054(4) Uani 1 1 d . . . H17A H 0.1031 0.2087 0.2345 0.065 Uiso 1 1 calc R . . C18 C 0.1720(5) 0.1539(6) 0.1994(7) 0.046(3) Uani 1 1 d . . . H18A H 0.1443 0.1183 0.1914 0.055 Uiso 1 1 calc R . . O6 O 0.3728(3) 0.3121(3) 0.0996(5) 0.0387(19) Uani 1 1 d D . . H6 H 0.395(4) 0.347(3) 0.104(6) 0.046 Uiso 1 1 d D . . C20 C 0.3617(5) 0.2801(5) 0.0211(7) 0.048(3) Uani 1 1 d . . . H20A H 0.3502 0.3094 -0.0263 0.072 Uiso 1 1 calc R . . H20B H 0.3243 0.2511 0.0160 0.072 Uiso 1 1 calc R . . H20C H 0.4029 0.2578 0.0192 0.072 Uiso 1 1 calc R . . O31A O 0.4074(7) 0.4236(7) 0.0680(10) 0.056(5) Uani 0.50 1 d P . 1 O41A O 0.5058(8) 0.5495(8) 0.3255(10) 0.071(5) Uiso 0.50 1 d PD A -1 C41A C 0.5038(19) 0.5968(8) 0.2669(18) 0.051(7) Uiso 0.50 1 d PD A -1 O51A O 0.5873(8) 0.4673(8) 0.5742(12) 0.117(6) Uiso 0.70 1 d PD B 1 C51A C 0.6225(11) 0.5217(9) 0.5895(18) 0.084(7) Uiso 0.70 1 d PD B 1 O51B O 0.6128(16) 0.5033(17) 0.637(2) 0.086(11) Uiso 0.30 1 d PD C 2 C51B C 0.614(5) 0.489(5) 0.549(3) 0.21(4) Uiso 0.30 1 d PD C 2 N61A N 0.3035(8) 0.1415(8) 0.5631(11) 0.056(5) Uiso 0.60 1 d PD D 1 C61A C 0.3039(12) 0.1591(11) 0.4969(13) 0.049(8) Uiso 0.60 1 d PD D 1 C62A C 0.3099(12) 0.1660(10) 0.4097(13) 0.029(8) Uiso 0.60 1 d PD D 1 N61B N 0.2699(14) 0.1168(13) 0.5391(19) 0.077(9) Uiso 0.40 1 d PD E 2 C61B C 0.2900(16) 0.1405(15) 0.4843(17) 0.034(10) Uiso 0.40 1 d PD E 2 C62B C 0.3026(18) 0.1818(16) 0.415(2) 0.033(12) Uiso 0.40 1 d PD E 2 O71A O 0.5134(13) 0.7442(12) 0.2964(16) 0.040(7) Uiso 0.25 1 d PDU . -1 C71A C 0.5000 0.8000(17) 0.2500 0.058(9) Uiso 0.50 2 d SPDU . -1 N71B N 0.5617(15) 0.6940(14) 0.4482(19) 0.109(10) Uiso 0.40 1 d PDU F 2 C71B C 0.5604(13) 0.6585(12) 0.5050(17) 0.049(8) Uiso 0.40 1 d PDU F 2 C72B C 0.5658(11) 0.6141(11) 0.5789(15) 0.034(7) Uiso 0.40 1 d PDU F 2 N71C N 0.5376(13) 0.7466(13) 0.3957(18) 0.062(8) Uiso 0.35 1 d PDU G -3 C71C C 0.5366(14) 0.7791(14) 0.349(2) 0.038(7) Uiso 0.35 1 d PDU G -3 C72C C 0.520(2) 0.8150(18) 0.270(3) 0.083(11) Uiso 0.35 1 d PDU G -3 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 0.0283(8) 0.0272(8) 0.0404(9) -0.0033(7) 0.0008(6) -0.0022(7) Cu2 0.0269(7) 0.0314(9) 0.0369(8) 0.0013(7) 0.0018(6) -0.0001(7) Cu3 0.0342(8) 0.0313(9) 0.0358(9) 0.0031(7) 0.0059(7) 0.0032(7) S1 0.057(4) 0.035(4) 0.044(10) -0.002(3) 0.012(9) 0.015(5) O11 0.074(10) 0.016(8) 0.10(4) -0.002(11) 0.05(3) 0.000(13) O12 0.089(6) 0.062(6) 0.064(6) -0.020(5) 0.036(5) -0.032(5) O13 0.070(12) 0.050(12) 0.067(14) -0.010(10) 0.038(11) 0.020(9) S2 0.0281(17) 0.0289(17) 0.0322(19) -0.0014(15) 0.0066(14) -0.0010(14) O21 0.021(3) 0.022(4) 0.038(4) -0.004(4) 0.002(3) 0.000(3) O22 0.026(4) 0.031(4) 0.031(5) 0.003(3) 0.003(3) 0.004(3) O23 0.037(4) 0.026(4) 0.033(4) 0.005(3) 0.008(3) -0.001(3) O24 0.033(4) 0.043(5) 0.023(5) -0.006(4) 0.007(3) -0.006(4) O1 0.028(4) 0.026(5) 0.048(5) -0.004(4) 0.002(4) 0.002(3) C1 0.038(7) 0.037(8) 0.062(9) 0.001(7) 0.021(7) -0.005(6) C2 0.030(7) 0.024(7) 0.085(10) -0.006(7) 0.006(6) -0.005(6) N1 0.026(5) 0.030(6) 0.047(6) -0.003(5) 0.007(4) -0.001(4) C3 0.044(7) 0.022(7) 0.023(7) 0.001(5) -0.001(6) -0.001(6) C4 0.031(7) 0.030(7) 0.017(6) 0.003(5) 0.000(5) 0.009(6) C5 0.042(7) 0.034(8) 0.021(7) -0.002(6) -0.002(5) 0.003(6) O2 0.036(4) 0.030(5) 0.039(5) -0.008(4) 0.002(4) 0.002(4) C6 0.031(7) 0.043(8) 0.033(7) -0.011(6) 0.000(6) 0.000(6) O3 0.027(4) 0.043(5) 0.068(6) -0.019(5) 0.007(4) -0.004(4) C10 0.044(8) 0.057(9) 0.099(11) -0.027(8) 0.031(8) -0.011(7) C7 0.036(7) 0.034(8) 0.057(9) -0.008(6) 0.007(6) -0.003(6) C8 0.040(7) 0.033(8) 0.066(9) -0.002(7) 0.012(7) 0.008(7) C9 0.055(8) 0.020(7) 0.029(7) -0.006(5) 0.001(6) -0.002(6) C11 0.025(7) 0.046(9) 0.083(10) -0.011(7) 0.011(7) 0.002(6) N2 0.022(5) 0.052(7) 0.024(6) 0.002(5) -0.004(4) -0.001(5) C12 0.031(7) 0.049(8) 0.028(7) -0.006(6) -0.001(6) -0.009(7) C13 0.019(6) 0.053(9) 0.036(7) 0.003(6) 0.007(5) -0.003(6) C14 0.035(7) 0.038(8) 0.022(7) 0.013(5) 0.008(6) 0.015(6) O4 0.022(4) 0.034(5) 0.037(5) 0.000(3) 0.003(4) 0.001(3) C15 0.026(7) 0.043(8) 0.036(7) 0.014(6) 0.013(6) 0.002(6) O5 0.043(5) 0.032(5) 0.041(5) 0.008(4) 0.015(4) 0.012(4) C19 0.063(8) 0.056(9) 0.057(9) -0.004(8) 0.022(7) 0.014(7) C16 0.040(8) 0.055(9) 0.059(9) 0.017(7) 0.024(7) 0.012(7) C17 0.031(7) 0.067(10) 0.070(10) 0.022(8) 0.022(7) 0.007(8) C18 0.030(7) 0.056(9) 0.053(9) 0.003(7) 0.014(6) 0.000(7) O6 0.046(5) 0.032(5) 0.040(5) -0.004(4) 0.015(4) 0.000(4) C20 0.047(7) 0.043(8) 0.049(9) 0.009(7) 0.004(6) 0.016(6) O31A 0.040(9) 0.047(11) 0.074(13) -0.002(9) 0.002(9) 0.012(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 Cu1 O2 1.883(6) . ? Cu1 N1 1.906(8) . ? Cu1 O1 1.929(6) . ? Cu1 O21 1.968(6) . ? Cu2 O1 1.923(6) . ? Cu2 N2 1.930(8) . ? Cu2 O4 1.934(6) . ? Cu2 O22 1.979(6) . ? Cu2 O21 2.328(6) 2_655 ? Cu3 O12 1.926(8) . ? Cu3 O6 1.967(7) . ? Cu3 O23 1.974(6) 2_655 ? Cu3 O4 1.987(6) . ? Cu3 O5 2.286(6) . ? Cu3 O22 2.468(6) . ? S1 O12 1.395(17) . ? S1 O11 1.455(19) . ? S1 O13 1.47(2) . ? S1 O12 1.583(16) 2_655 ? O12 S1 1.583(16) 2_655 ? S2 O24 1.434(6) . ? S2 O23 1.484(6) . ? S2 O22 1.501(6) . ? S2 O21 1.512(6) . ? O21 Cu2 2.328(6) 2_655 ? O23 Cu3 1.973(6) 2_655 ? O1 C1 1.431(11) . ? C1 C11 1.463(12) . ? C1 C2 1.466(13) . ? C1 H1A 1.0000 . ? C2 N1 1.478(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? N1 C3 1.297(11) . ? C3 C4 1.428(12) . ? C3 H3A 0.9500 . ? C4 C9 1.396(12) . ? C4 C5 1.425(13) . ? C5 O2 1.320(11) . ? C5 C6 1.428(13) . ? C6 C7 1.356(13) . ? C6 O3 1.386(11) . ? O3 C10 1.418(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C7 C8 1.376(13) . ? C7 H7A 0.9500 . ? C8 C9 1.374(12) . ? C8 H8A 0.9500 . ? C9 H9A 0.9500 . ? C11 N2 1.462(12) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? N2 C12 1.276(11) . ? C12 C13 1.437(13) . ? C12 H12A 0.9500 . ? C13 C18 1.370(13) . ? C13 C14 1.417(13) . ? C14 O4 1.353(11) . ? C14 C15 1.430(13) . ? C15 C16 1.363(13) . ? C15 O5 1.379(11) . ? O5 C19 1.437(11) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C16 C17 1.391(14) . ? C16 H16A 0.9500 . ? C17 C18 1.382(14) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? O6 C20 1.420(11) . ? O6 H6 0.89(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O41A C41A 1.396(19) . ? O51A C51A 1.378(19) . ? O51B C51B 1.47(3) . ? N61A C61A 1.144(18) . ? C61A C62A 1.46(2) . ? N61B C61B 1.19(2) . ? C61B C62B 1.51(2) . ? O71A C71A 1.42(2) . ? N71B C71B 1.21(2) . ? C71B C72B 1.52(2) . ? N71C C71C 1.04(2) . ? C71C C72C 1.47(5) . ? 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 Cu1 N1 94.3(3) . . ? O2 Cu1 O1 178.9(3) . . ? N1 Cu1 O1 85.5(3) . . ? O2 Cu1 O21 88.5(3) . . ? N1 Cu1 O21 177.2(3) . . ? O1 Cu1 O21 91.8(3) . . ? O1 Cu2 N2 85.5(3) . . ? O1 Cu2 O4 179.1(3) . . ? N2 Cu2 O4 93.7(3) . . ? O1 Cu2 O22 98.0(3) . . ? N2 Cu2 O22 168.7(3) . . ? O4 Cu2 O22 82.9(3) . . ? O1 Cu2 O21 89.8(2) . 2_655 ? N2 Cu2 O21 102.3(3) . 2_655 ? O4 Cu2 O21 90.2(2) . 2_655 ? O22 Cu2 O21 88.6(2) . 2_655 ? O12 Cu3 O6 88.8(3) . . ? O12 Cu3 O23 88.1(3) . 2_655 ? O6 Cu3 O23 175.0(3) . 2_655 ? O12 Cu3 O4 168.5(3) . . ? O6 Cu3 O4 92.1(3) . . ? O23 Cu3 O4 91.8(3) 2_655 . ? O12 Cu3 O5 93.2(3) . . ? O6 Cu3 O5 89.6(3) . . ? O23 Cu3 O5 94.4(2) 2_655 . ? O4 Cu3 O5 75.3(3) . . ? O12 Cu3 O22 121.4(3) . . ? O6 Cu3 O22 87.3(3) . . ? O23 Cu3 O22 91.0(2) 2_655 . ? O4 Cu3 O22 70.1(2) . . ? O5 Cu3 O22 145.1(2) . . ? O12 S1 O11 121(3) . . ? O12 S1 O13 108.3(9) . . ? O11 S1 O13 110.6(19) . . ? O12 S1 O12 111.7(7) . 2_655 ? O11 S1 O12 100.3(19) . 2_655 ? O13 S1 O12 103.4(11) . 2_655 ? S1 O12 Cu3 146.1(6) . . ? O24 S2 O23 111.0(4) . . ? O24 S2 O22 111.1(4) . . ? O23 S2 O22 108.1(4) . . ? O24 S2 O21 111.3(4) . . ? O23 S2 O21 107.2(3) . . ? O22 S2 O21 107.9(4) . . ? S2 O21 Cu1 123.2(4) . . ? S2 O21 Cu2 123.7(3) . 2_655 ? Cu1 O21 Cu2 106.9(3) . 2_655 ? S2 O22 Cu2 129.6(4) . . ? S2 O22 Cu3 137.9(4) . . ? Cu2 O22 Cu3 91.6(2) . . ? S2 O23 Cu3 131.4(4) . 2_655 ? C1 O1 Cu2 110.2(6) . . ? C1 O1 Cu1 112.1(6) . . ? Cu2 O1 Cu1 134.3(4) . . ? O1 C1 C11 112.7(9) . . ? O1 C1 C2 111.7(8) . . ? C11 C1 C2 119.9(10) . . ? O1 C1 H1A 103.4 . . ? C11 C1 H1A 103.4 . . ? C2 C1 H1A 103.4 . . ? C1 C2 N1 110.0(9) . . ? C1 C2 H2A 109.7 . . ? N1 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? N1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C3 N1 C2 120.8(9) . . ? C3 N1 Cu1 126.5(7) . . ? C2 N1 Cu1 112.8(6) . . ? N1 C3 C4 125.3(10) . . ? N1 C3 H3A 117.3 . . ? C4 C3 H3A 117.3 . . ? C9 C4 C5 120.3(10) . . ? C9 C4 C3 117.3(10) . . ? C5 C4 C3 122.3(10) . . ? O2 C5 C4 124.6(10) . . ? O2 C5 C6 119.5(10) . . ? C4 C5 C6 115.9(10) . . ? C5 O2 Cu1 126.9(7) . . ? C7 C6 O3 125.4(10) . . ? C7 C6 C5 121.7(11) . . ? O3 C6 C5 112.9(10) . . ? C6 O3 C10 115.5(8) . . ? O3 C10 H10A 109.5 . . ? O3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C7 C8 121.7(11) . . ? C6 C7 H7A 119.1 . . ? C8 C7 H7A 119.1 . . ? C9 C8 C7 119.0(11) . . ? C9 C8 H8A 120.5 . . ? C7 C8 H8A 120.5 . . ? C8 C9 C4 121.3(10) . . ? C8 C9 H9A 119.3 . . ? C4 C9 H9A 119.3 . . ? N2 C11 C1 110.1(9) . . ? N2 C11 H11A 109.6 . . ? C1 C11 H11A 109.6 . . ? N2 C11 H11B 109.6 . . ? C1 C11 H11B 109.6 . . ? H11A C11 H11B 108.2 . . ? C12 N2 C11 121.1(9) . . ? C12 N2 Cu2 126.1(8) . . ? C11 N2 Cu2 112.6(6) . . ? N2 C12 C13 126.9(10) . . ? N2 C12 H12A 116.6 . . ? C13 C12 H12A 116.6 . . ? C18 C13 C14 119.1(11) . . ? C18 C13 C12 118.1(11) . . ? C14 C13 C12 122.6(9) . . ? O4 C14 C13 124.0(10) . . ? O4 C14 C15 118.1(10) . . ? C13 C14 C15 117.9(10) . . ? C14 O4 Cu2 124.9(6) . . ? C14 O4 Cu3 120.2(6) . . ? Cu2 O4 Cu3 109.7(3) . . ? C16 C15 O5 125.9(11) . . ? C16 C15 C14 120.5(11) . . ? O5 C15 C14 113.6(9) . . ? C15 O5 C19 116.4(8) . . ? C15 O5 Cu3 111.5(6) . . ? C19 O5 Cu3 129.3(6) . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C16 C17 121.2(11) . . ? C15 C16 H16A 119.4 . . ? C17 C16 H16A 119.4 . . ? C18 C17 C16 118.4(10) . . ? C18 C17 H17A 120.8 . . ? C16 C17 H17A 120.8 . . ? C13 C18 C17 122.8(11) . . ? C13 C18 H18A 118.6 . . ? C17 C18 H18A 118.6 . . ? C20 O6 Cu3 126.9(6) . . ? C20 O6 H6 118(6) . . ? Cu3 O6 H6 105(6) . . ? O6 C20 H20A 109.5 . . ? O6 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O6 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N61A C61A C62A 166(3) . . ? N61B C61B C62B 166(3) . . ? N71B C71B C72B 175(3) . . ? N71C C71C C72C 165(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.737 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.101