# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 915043' #TrackingRef 'Paper1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H21 Cd2 N O12' _chemical_formula_sum 'C21 H21 Cd2 N O12' _chemical_formula_weight 704.19 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' Cd Cd -0.8075 1.2024 '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' N N 0.0061 0.0033 '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' 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 14.3175(3) _cell_length_b 14.4020(3) _cell_length_c 22.6162(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.4977(10) _cell_angle_gamma 90.00 _cell_volume 4585.42(16) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9525 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 27.85 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.020 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7613 _exptl_absorpt_correction_T_max 0.8309 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34856 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.85 _reflns_number_total 10854 _reflns_number_gt 6168 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 structure contains also severely disordered dimethyl acetamide solvent which could not be precisely modeled by discrete atoms. Its contribution to the diffraction pattern was subtracted by the SQUEEZE procedure, using the PLATON software (Spek, 2009). ; _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^)+(0.0909P)^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 10854 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0869 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1481 _refine_ls_wR_factor_gt 0.1380 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.011 _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 Cd1 Cd -0.24472(2) -0.25293(2) 0.241120(13) 0.03042(11) Uani 1 1 d . . . Cd2 Cd 0.31474(3) 0.12532(3) 0.139335(14) 0.04302(12) Uani 1 1 d . . . O3 O -0.1955(2) -0.1803(2) 0.16262(13) 0.0427(8) Uani 1 1 d . . . O4 O -0.1206(2) -0.1377(2) 0.25330(13) 0.0438(8) Uani 1 1 d . . . C5 C -0.1322(3) -0.1337(3) 0.1964(2) 0.0386(10) Uani 1 1 d . . . C6 C -0.0691(3) -0.0721(4) 0.16728(19) 0.0399(11) Uani 1 1 d . . . C7 C -0.0034(3) -0.0146(3) 0.2013(2) 0.0433(11) Uani 1 1 d . . . H7 H 0.0017 -0.0122 0.2437 0.052 Uiso 1 1 calc R . . C8 C 0.0547(3) 0.0396(3) 0.1731(2) 0.0423(11) Uani 1 1 d . . . C9 C 0.0479(4) 0.0355(4) 0.1112(2) 0.0516(14) Uani 1 1 d . . . H9 H 0.0886 0.0728 0.0922 0.062 Uiso 1 1 calc R . . C10 C -0.0174(4) -0.0222(4) 0.0771(2) 0.0570(15) Uani 1 1 d . . . C11 C -0.0769(4) -0.0747(4) 0.1050(2) 0.0494(13) Uani 1 1 d . . . H11 H -0.1237 -0.1130 0.0816 0.059 Uiso 1 1 calc R . . C12 C -0.0162(8) -0.0497(8) 0.0122(4) 0.039(3) Uiso 0.50 1 d P . 1 H12A H -0.0797 -0.0693 -0.0092 0.047 Uiso 0.50 1 calc PR . 1 H12B H 0.0307 -0.0994 0.0095 0.047 Uiso 0.50 1 calc PR . 1 C13 C 0.1238(3) 0.1075(3) 0.2089(2) 0.0436(12) Uani 1 1 d . . . O14 O 0.1233(2) 0.1214(2) 0.26277(14) 0.0478(8) Uani 1 1 d . . . O15 O 0.1805(2) 0.1510(2) 0.18093(14) 0.0422(8) Uani 1 1 d . . . O16 O 0.3946(3) 0.0940(3) 0.23150(14) 0.0585(10) Uani 1 1 d . . . O17 O 0.3517(2) 0.1560(2) 0.31312(15) 0.0491(8) Uani 1 1 d . . . C18 C 0.3964(3) 0.1001(3) 0.2869(2) 0.0418(11) Uani 1 1 d . . . C19 C 0.4629(3) 0.0340(3) 0.32689(19) 0.0373(10) Uani 1 1 d . . . C20 C 0.4661(4) 0.0333(4) 0.3883(2) 0.0458(12) Uani 1 1 d . . . H20 H 0.4277 0.0756 0.4055 0.055 Uiso 1 1 calc R . . C21 C 0.5239(4) -0.0278(4) 0.4250(2) 0.0557(15) Uani 1 1 d . . . C22 C 0.5780(4) -0.0897(4) 0.4001(2) 0.0551(14) Uani 1 1 d . . . H22 H 0.6163 -0.1332 0.4253 0.066 Uiso 1 1 calc R . . C23 C 0.5779(3) -0.0902(3) 0.3386(2) 0.0441(11) Uani 1 1 d . . . C24 C 0.5185(3) -0.0278(3) 0.3016(2) 0.0424(11) Uani 1 1 d . . . H24 H 0.5164 -0.0280 0.2594 0.051 Uiso 1 1 calc R . . C25 C 0.5367(8) -0.0120(9) 0.4890(5) 0.036(3) Uiso 0.50 1 d P . 1 H25A H 0.5627 -0.0696 0.5096 0.044 Uiso 0.50 1 calc PR . 1 H25B H 0.5855 0.0369 0.4995 0.044 Uiso 0.50 1 calc PR . 1 C26 C 0.6372(4) -0.1582(4) 0.3115(3) 0.0605(17) Uani 1 1 d . . . O27 O 0.6442(3) -0.1481(3) 0.2578(2) 0.0726(13) Uani 1 1 d . . . O28 O 0.6803(3) -0.2187(3) 0.3456(2) 0.0794(14) Uani 1 1 d . . . O29 O 0.2411(3) 0.1571(3) 0.04544(16) 0.0706(12) Uani 1 1 d . . . C30 C 0.2111(5) 0.2318(5) 0.0214(3) 0.0701(19) Uani 1 1 d . . . C31 C 0.1275(5) 0.2760(6) 0.0424(4) 0.100(3) Uani 1 1 d . . . H31A H 0.0697 0.2646 0.0127 0.151 Uiso 1 1 calc R . . H31B H 0.1381 0.3430 0.0471 0.151 Uiso 1 1 calc R . . H31C H 0.1203 0.2491 0.0811 0.151 Uiso 1 1 calc R . . N32 N 0.2468(4) 0.2692(4) -0.0215(2) 0.0753(16) Uani 1 1 d . . . C33 C 0.2076(6) 0.3521(5) -0.0563(3) 0.091(2) Uani 1 1 d . . . H33A H 0.1499 0.3726 -0.0425 0.136 Uiso 1 1 calc R . . H33B H 0.1921 0.3364 -0.0992 0.136 Uiso 1 1 calc R . . H33C H 0.2547 0.4022 -0.0503 0.136 Uiso 1 1 calc R . . C34 C 0.3318(5) 0.2259(5) -0.0390(3) 0.0774(19) Uani 1 1 d . . . H34A H 0.3786 0.2120 -0.0028 0.116 Uiso 1 1 calc R . . H34B H 0.3595 0.2687 -0.0646 0.116 Uiso 1 1 calc R . . H34C H 0.3133 0.1682 -0.0610 0.116 Uiso 1 1 calc R . . O35 O 0.2939(5) -0.0266(3) 0.1227(3) 0.142(3) Uani 1 1 d . . . H35A H 0.2709 -0.0370 0.0797 0.213 Uiso 1 1 d R . . H35B H 0.2470 -0.0499 0.1456 0.213 Uiso 1 1 d R . . O36 O 0.4566(5) 0.1134(5) 0.1066(3) 0.153(3) Uani 1 1 d . . . H36A H 0.5066 0.0981 0.1409 0.184 Uiso 1 1 d R . . H36B H 0.4521 0.0639 0.0764 0.184 Uiso 1 1 d R . . O12' O -0.0361(5) -0.0171(6) 0.0148(3) 0.0443(19) Uiso 0.50 1 d P . 21 O25' O 0.5233(7) -0.0421(7) 0.4881(4) 0.064(3) Uiso 0.50 1 d P . 21 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 Cd1 0.03136(18) 0.03076(18) 0.03030(17) 0.00013(13) 0.00870(12) -0.00250(13) Cd2 0.0495(2) 0.0483(2) 0.03100(18) 0.00071(15) 0.00662(14) 0.01055(17) O3 0.0428(19) 0.053(2) 0.0332(15) 0.0018(15) 0.0076(14) -0.0200(16) O4 0.0435(18) 0.053(2) 0.0346(16) 0.0002(15) 0.0073(14) -0.0147(16) C5 0.033(2) 0.045(3) 0.038(2) 0.009(2) 0.0087(19) -0.003(2) C6 0.036(2) 0.054(3) 0.028(2) 0.002(2) 0.0009(18) -0.010(2) C7 0.047(3) 0.050(3) 0.032(2) 0.008(2) 0.004(2) -0.012(2) C8 0.035(2) 0.049(3) 0.041(2) 0.006(2) 0.000(2) -0.016(2) C9 0.053(3) 0.060(3) 0.041(3) 0.011(2) 0.007(2) -0.029(3) C10 0.058(3) 0.082(4) 0.030(2) 0.007(3) 0.005(2) -0.026(3) C11 0.051(3) 0.064(3) 0.030(2) 0.009(2) -0.002(2) -0.029(3) C13 0.036(3) 0.042(3) 0.050(3) 0.010(2) 0.000(2) -0.003(2) O14 0.049(2) 0.054(2) 0.0411(18) -0.0047(16) 0.0097(15) -0.0179(17) O15 0.0326(17) 0.049(2) 0.0449(18) 0.0034(15) 0.0064(14) -0.0141(15) O16 0.061(2) 0.077(3) 0.0343(18) 0.0139(18) -0.0005(16) 0.022(2) O17 0.049(2) 0.047(2) 0.0490(19) 0.0014(16) 0.0046(16) 0.0200(17) C18 0.040(3) 0.043(3) 0.042(3) -0.002(2) 0.006(2) 0.004(2) C19 0.041(3) 0.038(3) 0.032(2) 0.0000(19) 0.0014(19) 0.011(2) C20 0.050(3) 0.054(3) 0.033(2) -0.002(2) 0.007(2) 0.024(2) C21 0.056(3) 0.076(4) 0.036(2) 0.010(3) 0.013(2) 0.020(3) C22 0.058(3) 0.054(3) 0.049(3) 0.016(3) -0.001(2) 0.018(3) C23 0.042(3) 0.038(3) 0.054(3) -0.001(2) 0.012(2) 0.008(2) C24 0.041(3) 0.047(3) 0.038(2) -0.002(2) 0.004(2) 0.006(2) C26 0.029(3) 0.040(3) 0.113(5) -0.039(3) 0.014(3) -0.003(2) O27 0.052(2) 0.073(3) 0.099(3) -0.035(3) 0.030(2) 0.010(2) O28 0.050(2) 0.042(2) 0.133(4) -0.017(2) -0.017(2) 0.0264(19) O29 0.095(3) 0.069(3) 0.040(2) -0.001(2) -0.007(2) -0.005(2) C30 0.091(5) 0.066(4) 0.043(3) 0.013(3) -0.015(3) -0.026(4) C31 0.072(5) 0.139(7) 0.092(5) 0.041(5) 0.021(4) 0.014(5) N32 0.094(4) 0.063(3) 0.062(3) 0.004(3) -0.004(3) -0.010(3) C33 0.134(7) 0.071(5) 0.070(4) 0.030(4) 0.027(4) 0.025(4) C34 0.061(4) 0.085(5) 0.086(5) -0.013(4) 0.011(3) 0.005(4) O35 0.264(9) 0.049(3) 0.107(4) -0.013(3) 0.015(5) -0.005(4) O36 0.169(6) 0.229(8) 0.081(4) 0.042(4) 0.076(4) 0.068(6) _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 Cd1 O17 2.211(3) 2_545 ? Cd1 O27 2.273(4) 1_455 ? Cd1 O3 2.280(3) . ? Cd1 O15 2.297(3) 2_545 ? Cd1 O4 2.411(3) . ? Cd1 O14 2.523(3) 2_545 ? Cd1 C5 2.676(4) . ? Cd1 C13 2.757(5) 2_545 ? Cd2 O35 2.230(5) . ? Cd2 O16 2.233(3) . ? Cd2 O29 2.239(4) . ? Cd2 O28 2.272(4) 2_655 ? Cd2 O36 2.291(6) . ? Cd2 O15 2.319(3) . ? O3 C5 1.266(5) . ? O4 C5 1.268(5) . ? C5 C6 1.501(6) . ? C6 C7 1.378(6) . ? C6 C11 1.393(6) . ? C7 C8 1.379(6) . ? C7 H7 0.9500 . ? C8 C9 1.387(6) . ? C8 C13 1.516(6) . ? C9 C10 1.377(7) . ? C9 H9 0.9500 . ? C10 C11 1.375(7) . ? C10 O12' 1.388(8) . ? C10 C12 1.523(11) . ? C11 H11 0.9500 . ? C12 C12 1.63(2) 3 ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 O14 1.235(6) . ? C13 O15 1.281(6) . ? C13 Cd1 2.757(5) 2 ? O14 Cd1 2.523(3) 2 ? O15 Cd1 2.297(3) 2 ? O16 C18 1.252(5) . ? O17 C18 1.244(6) . ? O17 Cd1 2.211(3) 2 ? C18 C19 1.522(6) . ? C19 C20 1.382(6) . ? C19 C24 1.385(6) . ? C20 C21 1.378(7) . ? C20 H20 0.9500 . ? C21 C22 1.367(7) . ? C21 O25' 1.444(11) . ? C21 C25 1.445(12) . ? C22 C23 1.392(7) . ? C22 H22 0.9500 . ? C23 C24 1.403(7) . ? C23 C26 1.498(7) . ? C24 H24 0.9500 . ? C25 C25 1.29(2) 3_656 ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 O27 1.247(8) . ? C26 O28 1.248(8) . ? O27 Cd1 2.273(4) 1_655 ? O28 Cd2 2.272(4) 2_645 ? O29 C30 1.247(7) . ? C30 N32 1.294(9) . ? C30 C31 1.507(10) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? N32 C34 1.483(8) . ? N32 C33 1.483(8) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O35 H35A 0.9800 . ? O35 H35B 0.9800 . ? O36 H36A 0.9800 . ? O36 H36B 0.9800 . ? O12' O12' 1.420(14) 3 ? O25' O25' 1.53(2) 3_656 ? 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 O17 Cd1 O27 92.94(14) 2_545 1_455 ? O17 Cd1 O3 96.97(11) 2_545 . ? O27 Cd1 O3 98.55(16) 1_455 . ? O17 Cd1 O15 102.04(12) 2_545 2_545 ? O27 Cd1 O15 117.86(15) 1_455 2_545 ? O3 Cd1 O15 137.44(11) . 2_545 ? O17 Cd1 O4 153.36(11) 2_545 . ? O27 Cd1 O4 92.70(14) 1_455 . ? O3 Cd1 O4 56.43(10) . . ? O15 Cd1 O4 98.23(11) 2_545 . ? O17 Cd1 O14 88.12(13) 2_545 2_545 ? O27 Cd1 O14 171.80(15) 1_455 2_545 ? O3 Cd1 O14 89.39(12) . 2_545 ? O15 Cd1 O14 54.02(10) 2_545 2_545 ? O4 Cd1 O14 89.96(12) . 2_545 ? O17 Cd1 C5 125.11(13) 2_545 . ? O27 Cd1 C5 97.11(16) 1_455 . ? O15 Cd1 C5 119.46(12) 2_545 . ? O14 Cd1 C5 88.90(13) 2_545 . ? O17 Cd1 C13 96.59(13) 2_545 2_545 ? O27 Cd1 C13 145.34(17) 1_455 2_545 ? O3 Cd1 C13 113.16(14) . 2_545 ? O4 Cd1 C13 93.44(13) . 2_545 ? C5 Cd1 C13 104.24(14) . 2_545 ? O35 Cd2 O16 89.38(19) . . ? O35 Cd2 O29 90.87(19) . . ? O16 Cd2 O29 177.35(15) . . ? O35 Cd2 O28 174.2(2) . 2_655 ? O16 Cd2 O28 93.62(15) . 2_655 ? O29 Cd2 O28 86.37(16) . 2_655 ? O35 Cd2 O36 88.3(3) . . ? O16 Cd2 O36 87.34(18) . . ? O29 Cd2 O36 90.03(19) . . ? O28 Cd2 O36 96.7(2) 2_655 . ? O35 Cd2 O15 97.5(2) . . ? O16 Cd2 O15 88.56(12) . . ? O29 Cd2 O15 94.02(14) . . ? O28 Cd2 O15 77.69(14) 2_655 . ? O36 Cd2 O15 172.9(2) . . ? C5 O3 Cd1 93.5(3) . . ? C5 O4 Cd1 87.6(3) . . ? O3 C5 O4 122.4(4) . . ? O3 C5 C6 118.0(4) . . ? O4 C5 C6 119.6(4) . . ? O3 C5 Cd1 58.3(2) . . ? O4 C5 Cd1 64.2(2) . . ? C6 C5 Cd1 175.4(3) . . ? C7 C6 C11 120.1(4) . . ? C7 C6 C5 120.9(4) . . ? C11 C6 C5 119.0(4) . . ? C6 C7 C8 119.3(4) . . ? C6 C7 H7 120.3 . . ? C8 C7 H7 120.3 . . ? C7 C8 C9 120.4(4) . . ? C7 C8 C13 120.5(4) . . ? C9 C8 C13 119.1(4) . . ? C10 C9 C8 120.4(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 119.3(4) . . ? C11 C10 O12' 118.2(5) . . ? C9 C10 O12' 121.5(5) . . ? C11 C10 C12 114.5(6) . . ? C9 C10 C12 124.8(6) . . ? C10 C11 C6 120.4(4) . . ? C10 C11 H11 119.8 . . ? C6 C11 H11 119.8 . . ? C10 C12 C12 98.7(9) . 3 ? C10 C12 H12A 112.0 . . ? C12 C12 H12A 112.0 3 . ? C10 C12 H12B 112.0 . . ? C12 C12 H12B 112.0 3 . ? H12A C12 H12B 109.7 . . ? O14 C13 O15 121.8(4) . . ? O14 C13 C8 120.7(4) . . ? O15 C13 C8 117.5(4) . . ? O14 C13 Cd1 66.1(2) . 2 ? O15 C13 Cd1 55.8(2) . 2 ? C8 C13 Cd1 171.5(3) . 2 ? C13 O14 Cd1 87.4(3) . 2 ? C13 O15 Cd1 96.7(3) . 2 ? C13 O15 Cd2 140.3(3) . . ? Cd1 O15 Cd2 99.32(11) 2 . ? C18 O16 Cd2 146.5(3) . . ? C18 O17 Cd1 119.0(3) . 2 ? O17 C18 O16 127.2(4) . . ? O17 C18 C19 116.2(4) . . ? O16 C18 C19 116.6(4) . . ? C20 C19 C24 119.6(4) . . ? C20 C19 C18 120.3(4) . . ? C24 C19 C18 120.1(4) . . ? C21 C20 C19 121.0(4) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 119.5(5) . . ? C22 C21 O25' 114.8(6) . . ? C20 C21 O25' 125.1(6) . . ? C22 C21 C25 122.5(6) . . ? C20 C21 C25 117.1(6) . . ? C21 C22 C23 121.1(4) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C24 118.8(4) . . ? C22 C23 C26 120.9(5) . . ? C24 C23 C26 120.2(5) . . ? C19 C24 C23 119.9(4) . . ? C19 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C25 C25 C21 117.7(12) 3_656 . ? C25 C25 H25A 107.9 3_656 . ? C21 C25 H25A 107.9 . . ? C25 C25 H25B 107.9 3_656 . ? C21 C25 H25B 107.9 . . ? H25A C25 H25B 107.2 . . ? O27 C26 O28 124.4(5) . . ? O27 C26 C23 118.3(6) . . ? O28 C26 C23 117.2(6) . . ? C26 O27 Cd1 105.5(4) . 1_655 ? C26 O28 Cd2 141.3(4) . 2_645 ? C30 O29 Cd2 131.0(4) . . ? O29 C30 N32 122.3(8) . . ? O29 C30 C31 117.2(6) . . ? N32 C30 C31 120.5(6) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 N32 C34 118.7(6) . . ? C30 N32 C33 124.7(7) . . ? C34 N32 C33 116.6(6) . . ? N32 C33 H33A 109.5 . . ? N32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N32 C34 H34A 109.5 . . ? N32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Cd2 O35 H35A 109.1 . . ? Cd2 O35 H35B 109.3 . . ? H35A O35 H35B 109.5 . . ? Cd2 O36 H36A 108.9 . . ? Cd2 O36 H36B 109.3 . . ? H36A O36 H36B 109.5 . . ? C10 O12' O12' 118.3(8) . 3 ? C21 O25' O25' 108.5(9) . 3_656 ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.035 0.003 0.367 2512 816 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.985 _refine_diff_density_min -1.290 _refine_diff_density_rms 0.128 data_2 _database_code_depnum_ccdc_archive 'CCDC 915044' #TrackingRef 'Paper1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C207 H102 Cu24 O129' _chemical_formula_sum 'C207 H102 Cu24 O129' _chemical_formula_weight 6177.95 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' O O 0.0106 0.0060 '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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 22.8595(6) _cell_length_b 18.7420(6) _cell_length_c 29.6690(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.8580(10) _cell_angle_gamma 90.00 _cell_volume 12286.2(7) _cell_formula_units_Z 1 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 21694 _cell_measurement_theta_min 1.30 _cell_measurement_theta_max 25.05 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3072 _exptl_absorpt_coefficient_mu 1.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7306 _exptl_absorpt_correction_T_max 0.8872 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa Apex2' _diffrn_measurement_method '0.5 deg. \f and \w scans' _diffrn_detector_area_resol_mean 1.75 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48544 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 25.05 _reflns_number_total 21694 _reflns_number_gt 13936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2, Bruker-AXS' _computing_cell_refinement 'Saint, Bruker-AXS' _computing_data_reduction 'Saint, Bruker-AXS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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. This framework solid contains a large amount of severely disordered solvent, which could not be resolved reliably by discrete atoms. Correspondingly, its contribution to the diffraction pattern was subtracted by the SQUEEZE procedure, using the PLATON software (Spek, 2009). The carboxylate residues also reveal partial disorder. Two of the ligand species in the asymmetric unit are located on inversion, with twofold disorder about the latter of the central CH2-O bond. The hydrogen atoms of the Cu-coordinated water species could not be located. ; _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^)+(0.0735P)^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 21694 _refine_ls_number_parameters 802 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1222 _refine_ls_wR_factor_gt 0.1175 _refine_ls_goodness_of_fit_ref 0.911 _refine_ls_restrained_S_all 0.911 _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 Cu1 Cu 0.778881(16) 0.197545(19) 0.470210(12) 0.03360(10) Uani 1 1 d . . . Cu2 Cu 0.681874(16) 0.266666(19) 0.484860(12) 0.03375(11) Uani 1 1 d . . . Cu3 Cu 0.697899(16) -0.307490(19) 0.498842(12) 0.03351(10) Uani 1 1 d . . . Cu4 Cu 0.794047(15) -0.240172(19) 0.485037(12) 0.03264(10) Uani 1 1 d . . . Cu5 Cu 0.507409(14) 0.497369(19) 0.805266(11) 0.02953(10) Uani 1 1 d . . . Cu6 Cu 0.536103(14) 0.499665(19) 0.724046(11) 0.02735(10) Uani 1 1 d . . . O7 O 0.75705(9) -0.26754(12) 0.42021(7) 0.0507(6) Uani 1 1 d . . . O8 O 0.67137(9) -0.31695(12) 0.43148(7) 0.0470(6) Uani 1 1 d . . . C9 C 0.70651(15) -0.29880(17) 0.40602(11) 0.0419(8) Uani 1 1 d . . . C10 C 0.68636(14) -0.31530(18) 0.35562(11) 0.0455(9) Uani 1 1 d . . . C11 C 0.63426(13) -0.35318(17) 0.33755(10) 0.0378(8) Uani 1 1 d . . . H11 H 0.6095 -0.3675 0.3572 0.045 Uiso 1 1 calc R . . C12 C 0.61764(14) -0.37066(19) 0.29031(11) 0.0475(9) Uani 1 1 d . . . C13 C 0.56387(13) -0.41630(18) 0.26982(11) 0.0391(8) Uani 1 1 d . . . O14 O 0.53154(9) -0.43343(12) 0.29700(7) 0.0441(6) Uani 1 1 d . . . O15 O 0.55547(10) -0.43327(15) 0.22805(7) 0.0623(7) Uani 1 1 d . . . C16 C 0.65430(18) -0.3500(2) 0.26142(12) 0.0789(14) Uani 1 1 d . . . H16 H 0.6444 -0.3632 0.2294 0.095 Uiso 1 1 calc R . . C17 C 0.70545(19) -0.3097(3) 0.28080(13) 0.0870(16) Uani 1 1 d . . . C18 C 0.72146(18) -0.2923(2) 0.32667(13) 0.0745(13) Uani 1 1 d . . . H18 H 0.7566 -0.2644 0.3389 0.089 Uiso 1 1 calc R . . O19 O 0.73964(18) -0.2903(3) 0.24848(13) 0.173(2) Uani 1 1 d . . . C20 C 0.28986(19) 0.7500(2) 0.76585(13) 0.0826(15) Uani 1 1 d . . . H20A H 0.2779 0.7074 0.7811 0.099 Uiso 1 1 calc R . . H20B H 0.3183 0.7780 0.7903 0.099 Uiso 1 1 calc R . . C21 C 0.32039(19) 0.7273(2) 0.73344(14) 0.0776(14) Uani 1 1 d . . . C22 C 0.30461(17) 0.7477(2) 0.68849(13) 0.0710(13) Uani 1 1 d . . . H22 H 0.2722 0.7803 0.6778 0.085 Uiso 1 1 calc R . . C23 C 0.33622(14) 0.72070(19) 0.65764(11) 0.0481(9) Uani 1 1 d . . . C24 C 0.31354(15) 0.73997(17) 0.60694(11) 0.0425(8) Uani 1 1 d . . . O25 O 0.34748(10) 0.71949(12) 0.58094(7) 0.0491(6) Uani 1 1 d . . . O26 O 0.26537(9) 0.77319(12) 0.59442(7) 0.0469(6) Uani 1 1 d . . . C27 C 0.38424(13) 0.67380(16) 0.67311(10) 0.0371(7) Uani 1 1 d . . . H27 H 0.4056 0.6563 0.6518 0.045 Uiso 1 1 calc R . . C28 C 0.40124(13) 0.65225(17) 0.71955(10) 0.0393(8) Uani 1 1 d . . . C29 C 0.36970(17) 0.6792(2) 0.75057(12) 0.0729(13) Uani 1 1 d . . . H29 H 0.3809 0.6657 0.7825 0.088 Uiso 1 1 calc R . . C30 C 0.44773(13) 0.59765(18) 0.73619(10) 0.0391(8) Uani 1 1 d . . . O31 O 0.47769(9) 0.57751(12) 0.70780(7) 0.0444(6) Uani 1 1 d . . . O32 O 0.45564(10) 0.57625(14) 0.77712(7) 0.0606(7) Uani 1 1 d . . . O33 O 0.58836(9) 0.41935(11) 0.75174(7) 0.0419(5) Uani 1 1 d . . . O34 O 0.56411(10) 0.41790(12) 0.82016(7) 0.0495(6) Uani 1 1 d . . . C35 C 0.59382(13) 0.39667(17) 0.79215(10) 0.0384(8) Uani 1 1 d . . . C36 C 0.63887(14) 0.33883(17) 0.80912(11) 0.0431(8) Uani 1 1 d . . . C37 C 0.65266(14) 0.31749(17) 0.85522(10) 0.0422(8) Uani 1 1 d . . . H37 H 0.6305 0.3363 0.8756 0.051 Uiso 1 1 calc R . . C38 C 0.69848(15) 0.26904(18) 0.87174(11) 0.0465(9) Uani 1 1 d . . . C39 C 0.71635(15) 0.25026(17) 0.92228(10) 0.0419(8) Uani 1 1 d . . . O40 O 0.68593(10) 0.27641(12) 0.94734(7) 0.0458(6) Uani 1 1 d . . . O41 O 0.76220(10) 0.20964(12) 0.93525(7) 0.0543(7) Uani 1 1 d . . . C42 C 0.72697(17) 0.2368(2) 0.84127(12) 0.0600(11) Uani 1 1 d . . . H42 H 0.7571 0.2016 0.8523 0.072 Uiso 1 1 calc R . . C43 C 0.71146(18) 0.2560(2) 0.79438(13) 0.0675(12) Uani 1 1 d . . . C44 C 0.66786(17) 0.30717(19) 0.77818(12) 0.0604(11) Uani 1 1 d . . . H44 H 0.6577 0.3208 0.7463 0.073 Uiso 1 1 calc R . . O45 O 0.74449(18) 0.2226(2) 0.76572(11) 0.0981(14) Uani 1 1 d . . . C46 C 0.73062(16) 0.2407(2) 0.71984(11) 0.0594(11) Uani 1 1 d . . . H46A H 0.7350 0.2931 0.7178 0.071 Uiso 1 1 calc R . . H46B H 0.6874 0.2293 0.7063 0.071 Uiso 1 1 calc R . . C47 C 0.76422(17) 0.2089(2) 0.69146(13) 0.0654(11) Uani 1 1 d . . . C48 C 0.81121(16) 0.1649(2) 0.70933(11) 0.0566(10) Uani 1 1 d . . . H48 H 0.8220 0.1540 0.7417 0.068 Uiso 1 1 calc R . . C49 C 0.84373(14) 0.13564(17) 0.68019(11) 0.0421(8) Uani 1 1 d . . . C50 C 0.89493(13) 0.08400(17) 0.70064(11) 0.0372(8) Uani 1 1 d . . . O51 O 0.90283(9) 0.06760(12) 0.74248(7) 0.0453(6) Uani 1 1 d . . . O52 O 0.92560(10) 0.06321(13) 0.67354(7) 0.0501(6) Uani 1 1 d . . . C53 C 0.82955(13) 0.15125(16) 0.63317(10) 0.0402(8) Uani 1 1 d . . . H53 H 0.8521 0.1309 0.6136 0.048 Uiso 1 1 calc R . . C54 C 0.78238(14) 0.19669(16) 0.61537(10) 0.0408(8) Uani 1 1 d . . . C55 C 0.74919(16) 0.2258(2) 0.64403(12) 0.0602(11) Uani 1 1 d . . . H55 H 0.7164 0.2571 0.6314 0.072 Uiso 1 1 calc R . . C56 C 0.76311(15) 0.21278(17) 0.56423(11) 0.0405(8) Uani 1 1 d . . . O57 O 0.71736(10) 0.25037(12) 0.54996(8) 0.0553(7) Uani 1 1 d . . . O58 O 0.79572(10) 0.18599(13) 0.53957(7) 0.0497(6) Uani 1 1 d . . . O59 O 0.65329(10) 0.16441(11) 0.47858(9) 0.0576(7) Uani 1 1 d . . . O60 O 0.73419(10) 0.11033(11) 0.46353(8) 0.0466(6) Uani 1 1 d . . . C61 C 0.68225(14) 0.11095(18) 0.47227(11) 0.0423(8) Uani 1 1 d . . . C62 C 0.65356(15) 0.04085(17) 0.47561(14) 0.0524(10) Uani 1 1 d . . . C63 C 0.68566(14) -0.02320(17) 0.47434(12) 0.0439(8) Uani 1 1 d . . . H63 H 0.7246 -0.0224 0.4685 0.053 Uiso 1 1 calc R . . C64 C 0.65912(15) -0.08782(18) 0.48179(13) 0.0521(9) Uani 1 1 d . . . C65 C 0.69242(15) -0.15591(17) 0.48367(11) 0.0416(8) Uani 1 1 d . . . O66 O 0.74453(10) -0.15377(11) 0.47650(8) 0.0459(6) Uani 1 1 d . . . O67 O 0.66683(10) -0.21028(11) 0.49464(9) 0.0521(6) Uani 1 1 d . . . C68 C 0.60204(17) -0.0891(2) 0.48838(18) 0.0892(16) Uani 1 1 d . . . H68 H 0.5826 -0.1329 0.4917 0.107 Uiso 1 1 calc R . . C69 C 0.57304(19) -0.0232(2) 0.4900(3) 0.123(3) Uani 1 1 d . . . C70 C 0.59753(17) 0.0387(2) 0.48336(19) 0.0906(16) Uani 1 1 d . . . H70 H 0.5758 0.0818 0.4840 0.109 Uiso 1 1 calc R . . C71 C 0.5157(2) -0.0298(3) 0.49775(19) 0.1058(18) Uiso 1 1 d . . . H71A H 0.4906 -0.0574 0.4713 0.127 Uiso 1 1 d R . . H71B H 0.5196 -0.0587 0.5263 0.127 Uiso 1 1 d R . . O72 O 0.81914(10) 0.28844(12) 0.48003(8) 0.0541(6) Uani 1 1 d . . . O73 O 0.73719(10) 0.34928(11) 0.48734(8) 0.0500(6) Uani 1 1 d . . . C74 C 0.79136(16) 0.34297(18) 0.48543(11) 0.0467(9) Uani 1 1 d . . . C75 C 0.88817(16) 0.4120(2) 0.49182(14) 0.0643(11) Uani 1 1 d . . . H75 H 0.9072 0.3678 0.4889 0.077 Uiso 1 1 calc R . . C76 C 0.82758(14) 0.41281(18) 0.49111(12) 0.0481(9) Uani 1 1 d . . . C77 C 0.79977(15) 0.47662(16) 0.49408(12) 0.0428(8) Uani 1 1 d . . . H77 H 0.7581 0.4779 0.4937 0.051 Uiso 1 1 calc R . . C78 C 0.83251(15) 0.53932(18) 0.49760(12) 0.0495(9) Uani 1 1 d . . . C79 C 0.80084(14) 0.60996(17) 0.49788(11) 0.0399(8) Uani 1 1 d . . . O80 O 0.74654(10) 0.60716(11) 0.50022(8) 0.0489(6) Uani 1 1 d . . . O81 O 0.83101(10) 0.66497(11) 0.49586(8) 0.0539(6) Uani 1 1 d . . . C82 C 0.89277(16) 0.5389(2) 0.49875(14) 0.0619(11) Uani 1 1 d . . . H82 H 0.9150 0.5822 0.5010 0.074 Uiso 1 1 calc R . . C83 C 0.92083(16) 0.47263(19) 0.49656(16) 0.0639(11) Uani 1 1 d . . . C84 C 0.98217(16) 0.4710(2) 0.49862(15) 0.063(5) Uiso 0.75 1 d P . . H84A H 1.0019 0.4395 0.5249 0.076 Uiso 0.75 1 d PR . . H84B H 0.9851 0.4467 0.4696 0.076 Uiso 0.75 1 d PR . . O84' O 0.98407(16) 0.4658(2) 0.49587(15) 0.089(13) Uiso 0.25 1 d PR . . O85 O 0.61627(10) -0.35770(13) 0.51421(9) 0.0638(7) Uani 1 1 d . . . O86 O 0.87530(10) -0.19211(13) 0.47042(8) 0.0606(7) Uani 1 1 d . . . O87 O 0.85745(11) 0.14754(14) 0.45549(10) 0.0756(8) Uani 1 1 d . . . O88 O 0.60379(11) 0.31867(15) 0.49946(9) 0.0790(9) Uani 1 1 d . . . O89 O 0.56770(11) 0.49986(12) 0.66045(8) 0.0572(7) Uani 1 1 d . . . O90 O 0.47570(12) 0.49623(13) 0.86953(9) 0.0668(7) 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 0.0421(2) 0.0210(2) 0.0331(2) 0.00456(17) 0.00131(16) 0.00707(17) Cu2 0.0433(2) 0.0226(2) 0.0305(2) 0.00638(17) 0.00068(16) 0.01063(17) Cu3 0.0450(2) 0.0214(2) 0.0311(2) -0.00797(17) 0.00432(16) -0.01329(17) Cu4 0.0409(2) 0.0222(2) 0.0316(2) -0.00761(17) 0.00328(16) -0.01029(17) Cu5 0.03240(18) 0.0344(2) 0.01580(18) 0.00101(16) -0.00481(14) 0.00221(17) Cu6 0.03172(18) 0.0291(2) 0.01582(17) 0.00030(16) -0.00372(14) 0.00185(16) O7 0.0567(13) 0.0567(16) 0.0359(13) -0.0196(12) 0.0068(11) -0.0296(13) O8 0.0480(12) 0.0581(16) 0.0308(12) -0.0071(11) 0.0028(10) -0.0188(12) C9 0.054(2) 0.034(2) 0.0302(18) -0.0091(16) -0.0022(16) -0.0104(17) C10 0.0523(19) 0.050(2) 0.0311(18) -0.0071(17) 0.0060(15) -0.0113(18) C11 0.0425(17) 0.043(2) 0.0261(17) -0.0053(15) 0.0062(14) -0.0114(16) C12 0.057(2) 0.051(2) 0.0322(19) -0.0047(17) 0.0060(16) -0.0243(18) C13 0.0354(16) 0.046(2) 0.0272(18) -0.0004(16) -0.0073(14) -0.0069(16) O14 0.0437(12) 0.0496(15) 0.0352(13) -0.0112(11) 0.0030(10) -0.0172(11) O15 0.0611(14) 0.090(2) 0.0303(13) -0.0143(14) 0.0019(11) -0.0324(15) C16 0.099(3) 0.102(4) 0.030(2) -0.017(2) 0.007(2) -0.061(3) C17 0.096(3) 0.136(4) 0.034(2) -0.014(3) 0.027(2) -0.069(3) C18 0.080(3) 0.090(3) 0.052(2) -0.016(2) 0.016(2) -0.062(3) O19 0.157(4) 0.269(6) 0.103(3) -0.026(3) 0.049(3) -0.138(4) C20 0.093(3) 0.107(4) 0.058(3) 0.026(3) 0.038(2) 0.081(3) C21 0.095(3) 0.092(3) 0.047(2) 0.010(2) 0.021(2) 0.062(3) C22 0.081(3) 0.090(3) 0.043(2) 0.015(2) 0.017(2) 0.058(3) C23 0.0512(19) 0.053(2) 0.0359(19) 0.0088(18) 0.0036(16) 0.0234(18) C24 0.060(2) 0.0284(19) 0.0345(19) 0.0073(16) 0.0048(17) 0.0027(17) O25 0.0575(14) 0.0562(16) 0.0283(12) 0.0138(12) 0.0013(11) 0.0180(12) O26 0.0518(13) 0.0477(15) 0.0338(13) 0.0165(11) -0.0023(10) 0.0258(12) C27 0.0477(17) 0.0307(18) 0.0287(17) 0.0018(14) 0.0022(14) 0.0092(15) C28 0.0401(16) 0.045(2) 0.0277(17) 0.0038(16) 0.0002(14) 0.0180(16) C29 0.085(3) 0.108(4) 0.030(2) 0.011(2) 0.0201(19) 0.048(3) C30 0.0360(16) 0.051(2) 0.0212(17) -0.0007(16) -0.0092(14) 0.0074(16) O31 0.0542(13) 0.0418(14) 0.0326(12) 0.0079(11) 0.0030(10) 0.0182(11) O32 0.0694(15) 0.082(2) 0.0290(13) 0.0131(13) 0.0093(11) 0.0394(14) O33 0.0527(12) 0.0409(14) 0.0284(12) 0.0118(11) 0.0037(10) 0.0195(11) O34 0.0646(14) 0.0486(15) 0.0346(13) 0.0150(11) 0.0116(11) 0.0274(12) C35 0.0414(17) 0.043(2) 0.0251(17) -0.0020(16) -0.0024(14) 0.0102(16) C36 0.0527(19) 0.041(2) 0.0323(18) 0.0023(16) 0.0055(15) 0.0205(17) C37 0.0525(19) 0.042(2) 0.0276(17) 0.0027(16) 0.0026(15) 0.0128(17) C38 0.055(2) 0.041(2) 0.038(2) 0.0106(17) 0.0018(16) 0.0100(18) C39 0.061(2) 0.036(2) 0.0230(17) 0.0051(15) 0.0017(16) 0.0143(18) O40 0.0613(14) 0.0432(14) 0.0270(12) 0.0037(11) 0.0004(11) 0.0227(12) O41 0.0723(15) 0.0514(16) 0.0326(13) 0.0083(12) 0.0015(11) 0.0367(13) C42 0.078(2) 0.052(2) 0.045(2) 0.0055(19) 0.0060(19) 0.040(2) C43 0.089(3) 0.078(3) 0.038(2) -0.005(2) 0.021(2) 0.044(2) C44 0.094(3) 0.055(3) 0.0310(19) 0.0107(18) 0.0134(19) 0.034(2) O45 0.123(4) 0.103(3) 0.066(2) 0.009(2) 0.020(2) 0.041(3) C46 0.073(2) 0.090(3) 0.0179(17) 0.0043(18) 0.0170(16) 0.038(2) C47 0.077(3) 0.071(3) 0.045(2) 0.003(2) 0.009(2) 0.035(2) C48 0.070(2) 0.069(3) 0.0283(19) 0.0081(19) 0.0072(17) 0.027(2) C49 0.0531(19) 0.035(2) 0.0307(18) 0.0034(16) -0.0031(15) 0.0092(16) C50 0.0353(16) 0.037(2) 0.0309(18) 0.0004(16) -0.0063(14) 0.0029(15) O51 0.0498(12) 0.0555(16) 0.0251(12) 0.0120(11) -0.0005(10) 0.0194(12) O52 0.0591(14) 0.0577(16) 0.0293(12) 0.0097(12) 0.0037(11) 0.0285(13) C53 0.0488(18) 0.0325(19) 0.0320(18) 0.0048(15) -0.0028(14) 0.0077(16) C54 0.060(2) 0.0282(18) 0.0296(17) -0.0043(15) 0.0024(15) 0.0199(16) C55 0.071(2) 0.063(3) 0.040(2) 0.013(2) 0.0026(18) 0.034(2) C56 0.057(2) 0.0226(18) 0.0338(19) 0.0078(15) -0.0027(16) 0.0044(16) O57 0.0692(15) 0.0527(16) 0.0367(14) 0.0122(12) 0.0007(11) 0.0310(13) O58 0.0563(14) 0.0570(16) 0.0297(12) 0.0086(12) -0.0001(11) 0.0157(12) O59 0.0649(15) 0.0191(13) 0.088(2) 0.0067(13) 0.0171(14) 0.0093(12) O60 0.0587(14) 0.0196(12) 0.0606(15) 0.0032(11) 0.0137(12) -0.0043(11) C61 0.0438(19) 0.033(2) 0.047(2) 0.0096(17) 0.0057(16) -0.0004(17) C62 0.049(2) 0.0237(19) 0.086(3) 0.0098(19) 0.0195(19) 0.0068(17) C63 0.0458(18) 0.033(2) 0.050(2) -0.0058(16) 0.0072(16) -0.0016(16) C64 0.054(2) 0.028(2) 0.076(3) -0.0001(19) 0.0206(19) -0.0055(17) C65 0.057(2) 0.0196(18) 0.045(2) -0.0042(15) 0.0085(17) 0.0007(17) O66 0.0584(14) 0.0254(13) 0.0566(15) 0.0018(11) 0.0194(12) -0.0001(11) O67 0.0620(14) 0.0226(13) 0.0802(18) -0.0061(12) 0.0338(13) -0.0037(12) C68 0.063(3) 0.039(3) 0.184(5) 0.009(3) 0.065(3) -0.001(2) C69 0.048(2) 0.055(3) 0.291(8) 0.042(4) 0.088(4) 0.006(2) C70 0.055(2) 0.047(3) 0.179(5) 0.001(3) 0.047(3) 0.010(2) O72 0.0548(14) 0.0261(13) 0.0725(18) -0.0006(12) 0.0001(12) 0.0109(12) O73 0.0515(14) 0.0257(13) 0.0694(17) -0.0023(12) 0.0092(12) -0.0016(11) C74 0.062(2) 0.027(2) 0.043(2) 0.0121(17) -0.0003(17) 0.0041(19) C75 0.064(2) 0.033(2) 0.091(3) 0.005(2) 0.012(2) 0.012(2) C76 0.050(2) 0.032(2) 0.056(2) -0.0010(17) 0.0008(17) 0.0039(17) C77 0.0507(19) 0.0216(18) 0.051(2) -0.0010(16) 0.0038(16) -0.0041(16) C78 0.048(2) 0.035(2) 0.059(2) -0.0038(18) 0.0022(17) -0.0061(17) C79 0.0430(18) 0.0250(19) 0.046(2) -0.0132(16) 0.0000(15) -0.0045(16) O80 0.0530(14) 0.0204(12) 0.0704(17) -0.0001(11) 0.0105(12) 0.0001(11) O81 0.0563(14) 0.0196(13) 0.0807(18) -0.0099(12) 0.0081(12) -0.0091(11) C82 0.054(2) 0.034(2) 0.091(3) -0.007(2) 0.005(2) -0.0020(19) C83 0.053(2) 0.032(2) 0.106(4) -0.007(2) 0.019(2) -0.0036(18) O85 0.0577(14) 0.0521(16) 0.0777(19) -0.0059(14) 0.0100(13) -0.0176(13) O86 0.0661(15) 0.0533(17) 0.0658(17) 0.0015(14) 0.0234(13) -0.0093(13) O87 0.0767(17) 0.0561(18) 0.095(2) -0.0103(16) 0.0248(15) 0.0141(15) O88 0.0673(16) 0.094(2) 0.0740(19) -0.0008(17) 0.0143(14) 0.0336(16) O89 0.0654(15) 0.0602(17) 0.0443(15) 0.0057(13) 0.0111(12) 0.0057(13) O90 0.0869(18) 0.0709(19) 0.0427(15) 0.0034(14) 0.0169(13) -0.0018(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O60 1.911(2) . ? Cu1 O72 1.923(2) . ? Cu1 O26 2.0017(19) 3_666 ? Cu1 O58 2.006(2) . ? Cu1 O87 2.167(2) . ? Cu1 Cu2 2.6979(5) . ? Cu2 O25 1.912(2) 3_666 ? Cu2 O57 1.918(2) . ? Cu2 O73 1.989(2) . ? Cu2 O59 2.018(2) . ? Cu2 O88 2.172(2) . ? Cu3 O8 1.942(2) . ? Cu3 O80 1.942(2) 1_545 ? Cu3 O67 1.948(2) . ? Cu3 O41 1.960(2) 2_646 ? Cu3 O85 2.239(2) . ? Cu3 Cu4 2.6556(5) . ? Cu4 O66 1.955(2) . ? Cu4 O81 1.959(2) 1_545 ? Cu4 O7 1.960(2) . ? Cu4 O40 1.965(2) 2_646 ? Cu4 O86 2.205(2) . ? Cu5 O15 1.938(2) 3_656 ? Cu5 O52 1.942(2) 2_656 ? Cu5 O32 1.943(2) . ? Cu5 O34 1.949(2) . ? Cu5 O90 2.207(2) . ? Cu5 Cu6 2.6551(5) . ? Cu6 O31 1.953(2) . ? Cu6 O14 1.956(2) 3_656 ? Cu6 O51 1.9609(19) 2_656 ? Cu6 O33 1.9659(19) . ? Cu6 O89 2.186(2) . ? O7 C9 1.267(3) . ? O8 C9 1.282(4) . ? C9 C10 1.480(4) . ? C10 C11 1.372(4) . ? C10 C18 1.386(4) . ? C11 C12 1.394(4) . ? C12 C16 1.398(5) . ? C12 C13 1.493(4) . ? C13 O15 1.246(3) . ? C13 O14 1.267(3) . ? O14 Cu6 1.956(2) 3_656 ? O15 Cu5 1.938(2) 3_656 ? C16 C17 1.387(5) . ? C17 C18 1.356(5) . ? C17 O19 1.431(5) . ? O19 C20 1.360(5) 4_665 ? C20 O19 1.360(5) 4_566 ? C20 C21 1.392(5) . ? C21 C22 1.345(5) . ? C21 C29 1.431(5) . ? C22 C23 1.398(4) . ? C23 C27 1.389(4) . ? C23 C24 1.504(4) . ? C24 O26 1.236(4) . ? C24 O25 1.285(4) . ? O25 Cu2 1.912(2) 3_666 ? O26 Cu1 2.0016(19) 3_666 ? C27 C28 1.392(4) . ? C28 C29 1.401(4) . ? C28 C30 1.467(4) . ? C30 O32 1.247(3) . ? C30 O31 1.272(3) . ? O33 C35 1.248(3) . ? O34 C35 1.265(3) . ? C35 C36 1.491(4) . ? C36 C37 1.381(4) . ? C36 C44 1.395(4) . ? C37 C38 1.378(4) . ? C38 C42 1.381(4) . ? C38 C39 1.492(4) . ? C39 O40 1.242(4) . ? C39 O41 1.272(4) . ? O40 Cu4 1.965(2) 2_656 ? O41 Cu3 1.961(2) 2_656 ? C42 C43 1.392(5) . ? C43 C44 1.378(5) . ? C43 O45 1.419(4) . ? O45 C46 1.359(4) . ? C46 C47 1.409(4) . ? C47 C48 1.350(4) . ? C47 C55 1.397(5) . ? C48 C49 1.389(4) . ? C49 C53 1.380(4) . ? C49 C50 1.520(4) . ? C50 O51 1.246(3) . ? C50 O52 1.257(3) . ? O51 Cu6 1.9609(19) 2_646 ? O52 Cu5 1.942(2) 2_646 ? C53 C54 1.369(4) . ? C54 C55 1.388(4) . ? C54 C56 1.498(4) . ? C56 O57 1.242(4) . ? C56 O58 1.274(4) . ? O59 C61 1.241(4) . ? O60 C61 1.279(3) . ? C61 C62 1.483(4) . ? C62 C70 1.359(5) . ? C62 C63 1.412(4) . ? C63 C64 1.397(4) . ? C64 C68 1.368(4) . ? C64 C65 1.480(4) . ? C65 O67 1.259(4) . ? C65 O66 1.263(4) . ? C68 C69 1.409(5) . ? C69 C70 1.325(5) . ? C69 C71 1.393(6) . ? C71 C71 1.354(9) 3_656 ? O72 C74 1.235(4) . ? O73 C74 1.260(4) . ? C74 C76 1.535(5) . ? C75 C83 1.347(5) . ? C75 C76 1.380(4) . ? C76 C77 1.368(4) . ? C77 C78 1.383(4) . ? C78 C82 1.369(4) . ? C78 C79 1.510(4) . ? C79 O81 1.250(4) . ? C79 O80 1.262(3) . ? O80 Cu3 1.942(2) 1_565 ? O81 Cu4 1.959(2) 1_565 ? C82 C83 1.408(5) . ? C83 C84 1.388(5) . ? C83 O84' 1.457(5) . ? C84 C84 1.350(7) 3_766 ? C84 O84' 1.401(7) 3_766 ? 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 O60 Cu1 O72 174.96(10) . . ? O60 Cu1 O26 90.55(9) . 3_666 ? O72 Cu1 O26 90.41(10) . 3_666 ? O60 Cu1 O58 88.33(9) . . ? O72 Cu1 O58 88.96(10) . . ? O26 Cu1 O58 158.33(9) 3_666 . ? O60 Cu1 O87 93.32(10) . . ? O72 Cu1 O87 91.40(10) . . ? O26 Cu1 O87 99.61(10) 3_666 . ? O58 Cu1 O87 102.06(10) . . ? O60 Cu1 Cu2 89.30(7) . . ? O72 Cu1 Cu2 86.07(7) . . ? O26 Cu1 Cu2 77.78(6) 3_666 . ? O58 Cu1 Cu2 80.56(6) . . ? O87 Cu1 Cu2 176.33(8) . . ? O25 Cu2 O57 175.40(10) 3_666 . ? O25 Cu2 O73 89.17(10) 3_666 . ? O57 Cu2 O73 89.20(10) . . ? O25 Cu2 O59 90.81(10) 3_666 . ? O57 Cu2 O59 89.14(10) . . ? O73 Cu2 O59 158.54(9) . . ? O25 Cu2 O88 92.95(10) 3_666 . ? O57 Cu2 O88 91.58(10) . . ? O73 Cu2 O88 100.98(10) . . ? O59 Cu2 O88 100.45(10) . . ? O25 Cu2 Cu1 89.34(7) 3_666 . ? O57 Cu2 Cu1 86.15(7) . . ? O73 Cu2 Cu1 80.72(7) . . ? O59 Cu2 Cu1 77.83(7) . . ? O88 Cu2 Cu1 177.16(8) . . ? O8 Cu3 O80 88.42(10) . 1_545 ? O8 Cu3 O67 90.40(10) . . ? O80 Cu3 O67 165.69(9) 1_545 . ? O8 Cu3 O41 169.71(9) . 2_646 ? O80 Cu3 O41 89.80(10) 1_545 2_646 ? O67 Cu3 O41 88.82(10) . 2_646 ? O8 Cu3 O85 96.58(9) . . ? O80 Cu3 O85 98.74(9) 1_545 . ? O67 Cu3 O85 95.56(9) . . ? O41 Cu3 O85 93.71(9) 2_646 . ? O8 Cu3 Cu4 86.39(6) . . ? O80 Cu3 Cu4 84.41(6) 1_545 . ? O67 Cu3 Cu4 81.28(6) . . ? O41 Cu3 Cu4 83.35(6) 2_646 . ? O85 Cu3 Cu4 175.70(7) . . ? O66 Cu4 O81 169.76(9) . 1_545 ? O66 Cu4 O7 89.99(10) . . ? O81 Cu4 O7 89.01(10) 1_545 . ? O66 Cu4 O40 88.68(9) . 2_646 ? O81 Cu4 O40 89.91(10) 1_545 2_646 ? O7 Cu4 O40 166.44(9) . 2_646 ? O66 Cu4 O86 97.19(9) . . ? O81 Cu4 O86 93.05(9) 1_545 . ? O7 Cu4 O86 95.00(9) . . ? O40 Cu4 O86 98.56(9) 2_646 . ? O66 Cu4 Cu3 86.50(6) . . ? O81 Cu4 Cu3 83.27(7) 1_545 . ? O7 Cu4 Cu3 82.02(6) . . ? O40 Cu4 Cu3 84.43(6) 2_646 . ? O86 Cu4 Cu3 175.28(7) . . ? O15 Cu5 O52 168.29(9) 3_656 2_656 ? O15 Cu5 O32 87.83(12) 3_656 . ? O52 Cu5 O32 89.91(11) 2_656 . ? O15 Cu5 O34 90.29(11) 3_656 . ? O52 Cu5 O34 89.36(10) 2_656 . ? O32 Cu5 O34 167.14(9) . . ? O15 Cu5 O90 93.99(10) 3_656 . ? O52 Cu5 O90 97.64(9) 2_656 . ? O32 Cu5 O90 94.58(9) . . ? O34 Cu5 O90 98.24(9) . . ? O15 Cu5 Cu6 82.57(7) 3_656 . ? O52 Cu5 Cu6 85.74(6) 2_656 . ? O32 Cu5 Cu6 82.10(6) . . ? O34 Cu5 Cu6 85.04(6) . . ? O90 Cu5 Cu6 175.29(7) . . ? O31 Cu6 O14 87.75(10) . 3_656 ? O31 Cu6 O51 89.59(9) . 2_656 ? O14 Cu6 O51 167.29(9) 3_656 2_656 ? O31 Cu6 O33 168.23(9) . . ? O14 Cu6 O33 89.62(9) 3_656 . ? O51 Cu6 O33 90.46(9) 2_656 . ? O31 Cu6 O89 98.16(9) . . ? O14 Cu6 O89 97.73(9) 3_656 . ? O51 Cu6 O89 94.95(9) 2_656 . ? O33 Cu6 O89 93.56(8) . . ? O31 Cu6 Cu5 85.63(6) . . ? O14 Cu6 Cu5 85.44(6) 3_656 . ? O51 Cu6 Cu5 81.97(6) 2_656 . ? O33 Cu6 Cu5 82.73(6) . . ? O89 Cu6 Cu5 175.13(6) . . ? C9 O7 Cu4 125.0(2) . . ? C9 O8 Cu3 120.31(18) . . ? O7 C9 O8 125.6(3) . . ? O7 C9 C10 117.0(3) . . ? O8 C9 C10 117.4(3) . . ? C11 C10 C18 120.1(3) . . ? C11 C10 C9 121.1(3) . . ? C18 C10 C9 118.8(3) . . ? C10 C11 C12 120.0(3) . . ? C11 C12 C16 120.0(3) . . ? C11 C12 C13 121.8(3) . . ? C16 C12 C13 118.0(3) . . ? O15 C13 O14 127.0(3) . . ? O15 C13 C12 116.9(3) . . ? O14 C13 C12 116.1(3) . . ? C13 O14 Cu6 119.99(19) . 3_656 ? C13 O15 Cu5 124.8(2) . 3_656 ? C17 C16 C12 118.1(3) . . ? C18 C17 C16 122.0(3) . . ? C18 C17 O19 123.9(4) . . ? C16 C17 O19 114.1(3) . . ? C17 C18 C10 119.8(3) . . ? C20 O19 C17 116.1(4) 4_665 . ? O19 C20 C21 115.6(4) 4_566 . ? C22 C21 C20 122.9(3) . . ? C22 C21 C29 121.2(3) . . ? C20 C21 C29 115.9(3) . . ? C21 C22 C23 119.6(3) . . ? C27 C23 C22 120.7(3) . . ? C27 C23 C24 121.5(3) . . ? C22 C23 C24 117.7(3) . . ? O26 C24 O25 126.8(3) . . ? O26 C24 C23 118.3(3) . . ? O25 C24 C23 115.0(3) . . ? C24 O25 Cu2 117.67(19) . 3_666 ? C24 O26 Cu1 128.2(2) . 3_666 ? C23 C27 C28 120.5(3) . . ? C27 C28 C29 119.1(3) . . ? C27 C28 C30 122.0(3) . . ? C29 C28 C30 118.8(3) . . ? C28 C29 C21 119.0(3) . . ? O32 C30 O31 125.5(3) . . ? O32 C30 C28 117.6(3) . . ? O31 C30 C28 116.8(3) . . ? C30 O31 Cu6 120.57(19) . . ? C30 O32 Cu5 125.7(2) . . ? C35 O33 Cu6 124.2(2) . . ? C35 O34 Cu5 122.0(2) . . ? O33 C35 O34 125.9(3) . . ? O33 C35 C36 117.5(3) . . ? O34 C35 C36 116.6(3) . . ? C37 C36 C44 120.1(3) . . ? C37 C36 C35 120.5(3) . . ? C44 C36 C35 119.4(3) . . ? C38 C37 C36 120.2(3) . . ? C37 C38 C42 119.9(3) . . ? C37 C38 C39 120.0(3) . . ? C42 C38 C39 120.1(3) . . ? O40 C39 O41 126.8(3) . . ? O40 C39 C38 117.2(3) . . ? O41 C39 C38 115.9(3) . . ? C39 O40 Cu4 121.96(19) . 2_656 ? C39 O41 Cu3 122.4(2) . 2_656 ? C38 C42 C43 120.0(3) . . ? C44 C43 C42 120.3(3) . . ? C44 C43 O45 123.1(3) . . ? C42 C43 O45 116.6(3) . . ? C43 C44 C36 119.3(3) . . ? C46 O45 C43 117.9(3) . . ? O45 C46 C47 118.0(3) . . ? C48 C47 C55 120.0(3) . . ? C48 C47 C46 121.6(3) . . ? C55 C47 C46 118.3(3) . . ? C47 C48 C49 119.7(3) . . ? C53 C49 C48 121.4(3) . . ? C53 C49 C50 119.7(3) . . ? C48 C49 C50 118.9(3) . . ? O51 C50 O52 126.8(3) . . ? O51 C50 C49 117.1(3) . . ? O52 C50 C49 116.2(3) . . ? C50 O51 Cu6 124.6(2) . 2_646 ? C50 O52 Cu5 120.87(19) . 2_646 ? C54 C53 C49 118.6(3) . . ? C53 C54 C55 120.5(3) . . ? C53 C54 C56 120.9(3) . . ? C55 C54 C56 118.4(3) . . ? C54 C55 C47 119.7(3) . . ? O57 C56 O58 126.4(3) . . ? O57 C56 C54 117.6(3) . . ? O58 C56 C54 116.0(3) . . ? C56 O57 Cu2 122.4(2) . . ? C56 O58 Cu1 124.05(19) . . ? C61 O59 Cu2 127.4(2) . . ? C61 O60 Cu1 118.1(2) . . ? O59 C61 O60 126.6(3) . . ? O59 C61 C62 116.3(3) . . ? O60 C61 C62 117.1(3) . . ? C70 C62 C63 119.9(3) . . ? C70 C62 C61 119.3(3) . . ? C63 C62 C61 120.6(3) . . ? C64 C63 C62 118.9(3) . . ? C68 C64 C63 120.4(3) . . ? C68 C64 C65 118.7(3) . . ? C63 C64 C65 120.9(3) . . ? O67 C65 O66 126.2(3) . . ? O67 C65 C64 116.1(3) . . ? O66 C65 C64 117.7(3) . . ? C65 O66 Cu4 119.4(2) . . ? C65 O67 Cu3 126.0(2) . . ? C64 C68 C69 117.6(3) . . ? C70 C69 C71 123.7(4) . . ? C70 C69 C68 122.8(4) . . ? C71 C69 C68 113.5(4) . . ? C69 C70 C62 120.3(4) . . ? C71 C71 C69 119.2(6) 3_656 . ? C74 O72 Cu1 120.7(2) . . ? C74 O73 Cu2 123.3(2) . . ? O72 C74 O73 128.9(3) . . ? O72 C74 C76 116.0(3) . . ? O73 C74 C76 115.1(3) . . ? C83 C75 C76 121.3(3) . . ? C77 C76 C75 119.3(3) . . ? C77 C76 C74 120.4(3) . . ? C75 C76 C74 120.2(3) . . ? C76 C77 C78 119.8(3) . . ? C82 C78 C77 121.3(3) . . ? C82 C78 C79 119.0(3) . . ? C77 C78 C79 119.6(3) . . ? O81 C79 O80 126.8(3) . . ? O81 C79 C78 116.8(3) . . ? O80 C79 C78 116.3(3) . . ? C79 O80 Cu3 122.0(2) . 1_565 ? C79 O81 Cu4 122.4(2) . 1_565 ? C78 C82 C83 118.1(3) . . ? C75 C83 C84 120.8(4) . . ? C75 C83 C82 120.2(3) . . ? C84 C83 C82 119.0(4) . . ? C84 C84 C83 124.9(6) 3_766 . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.002 -0.017 -0.001 8092 4218 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.721 _refine_diff_density_min -0.691 _refine_diff_density_rms 0.087 data_3 _database_code_depnum_ccdc_archive 'CCDC 915045' #TrackingRef 'Paper1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H18 Co2 O14' _chemical_formula_sum 'C17 H18 Co2 O14' _chemical_formula_weight 564.17 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.8167(3) _cell_length_b 14.2636(3) _cell_length_c 12.0070(3) _cell_angle_alpha 90.00 _cell_angle_beta 118.4686(9) _cell_angle_gamma 90.00 _cell_volume 2531.81(9) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 2701 _cell_measurement_theta_min 3.19 _cell_measurement_theta_max 27.84 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 1.372 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6099 _exptl_absorpt_correction_T_max 0.7710 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9395 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.84 _reflns_number_total 3001 _reflns_number_gt 2042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 structure contains also severely disordered dimethyl acetamide solvent which could not be precicely modeled by discrete atoms. Its contribution to the diffraction pattern was subtracted by the SQUEEZE procedure, using the PLATON software (Spek, 2009). ; _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^)+(0.1010P)^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 3001 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0733 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1511 _refine_ls_wR_factor_gt 0.1387 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.40322(2) -0.17301(3) 0.59902(4) 0.02972(19) Uani 1 1 d . . . O2 O 0.29843(16) -0.09397(18) 0.5858(3) 0.0519(7) Uani 1 1 d . . . O3 O 0.36117(16) 0.00405(19) 0.7501(2) 0.0518(7) Uani 1 1 d . . . C4 C 0.2957(2) -0.0256(2) 0.6503(3) 0.0375(8) Uani 1 1 d . . . C5 C 0.2056(2) 0.0240(2) 0.5984(3) 0.0358(7) Uani 1 1 d . . . C6 C 0.1883(2) 0.0898(2) 0.6688(3) 0.0370(8) Uani 1 1 d . . . H6 H 0.2325 0.1030 0.7535 0.044 Uiso 1 1 calc R . . C7 C 0.1047(2) 0.1369(2) 0.6142(3) 0.0367(8) Uani 1 1 d . . . C8 C 0.0792(2) 0.2103(2) 0.6824(3) 0.0377(8) Uani 1 1 d . . . O9 O 0.12989(17) 0.22675(17) 0.7970(2) 0.0457(6) Uani 1 1 d . . . O10 O 0.00576(18) 0.2477(2) 0.6147(3) 0.0756(11) Uani 1 1 d . . . C11 C 0.0412(2) 0.1168(3) 0.4894(3) 0.0453(9) Uani 1 1 d . . . H11 H -0.0150 0.1490 0.4513 0.054 Uiso 1 1 calc R . . C12 C 0.0591(2) 0.0509(3) 0.4207(3) 0.0533(11) Uani 1 1 d . . . C13 C 0.1412(2) 0.0042(3) 0.4742(3) 0.0457(9) Uani 1 1 d . . . H13 H 0.1535 -0.0411 0.4264 0.055 Uiso 1 1 calc R . . O14 O -0.0042(3) 0.0650(4) 0.2893(4) 0.0371(12) Uani 0.50 1 d P . . C15 C 0.0145(5) 0.0111(6) 0.2056(6) 0.0291(14) Uani 0.50 1 d P . . H15A H 0.0067 -0.0556 0.2131 0.035 Uiso 0.50 1 d PR . . H15B H 0.0748 0.0230 0.2173 0.035 Uiso 0.50 1 d PR . . O16 O 0.5000 -0.0860(2) 0.7500 0.0348(7) Uani 1 2 d S . . H16A H 0.5359 -0.0383 0.7528 0.042 Uiso 0.50 1 d PR . . H16B H 0.4808 -0.0669 0.8046 0.042 Uiso 0.50 1 d PR . . O17 O 0.31630(14) -0.24962(17) 0.4370(2) 0.0376(5) Uani 1 1 d . . . H17A H 0.2601 -0.2257 0.3956 0.045 Uiso 1 1 d R . . H17B H 0.3083 -0.2995 0.4765 0.045 Uiso 1 1 d R . . O18 O 0.4250(3) -0.0804(3) 0.4794(3) 0.1013(15) Uani 1 1 d . . . H18A H 0.4029 -0.0542 0.4016 0.122 Uiso 1 1 d R . . H18B H 0.4660 -0.0356 0.5215 0.122 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0215(3) 0.0359(3) 0.0231(3) 0.00052(17) 0.00353(18) 0.00220(16) O2 0.0314(12) 0.0414(14) 0.0591(17) -0.0173(12) 0.0021(12) 0.0064(11) O3 0.0306(12) 0.0599(16) 0.0394(14) -0.0174(12) -0.0041(11) 0.0100(12) C4 0.0274(16) 0.0342(16) 0.0355(19) -0.0015(14) 0.0024(14) 0.0038(14) C5 0.0262(15) 0.0415(18) 0.0292(17) -0.0034(14) 0.0046(13) -0.0008(14) C6 0.0255(15) 0.0431(18) 0.0286(16) -0.0011(14) 0.0017(13) 0.0023(14) C7 0.0303(16) 0.0448(18) 0.0241(16) -0.0046(14) 0.0041(13) 0.0051(14) C8 0.0278(15) 0.0453(18) 0.0317(18) -0.0026(15) 0.0075(14) 0.0063(14) O9 0.0443(13) 0.0490(14) 0.0277(12) -0.0076(11) 0.0042(11) 0.0107(11) O10 0.0395(15) 0.117(3) 0.0425(16) -0.0237(17) -0.0032(13) 0.0387(17) C11 0.0262(16) 0.074(3) 0.0248(17) -0.0049(17) 0.0036(14) 0.0151(17) C12 0.0261(16) 0.101(3) 0.0221(17) -0.0130(19) 0.0024(14) 0.0104(19) C13 0.0250(16) 0.068(2) 0.0320(19) -0.0155(17) 0.0040(14) 0.0017(16) O14 0.028(2) 0.042(3) 0.030(3) -0.001(2) 0.005(2) 0.005(3) C15 0.023(3) 0.040(4) 0.017(3) -0.003(3) 0.004(2) 0.002(3) O16 0.0223(14) 0.0405(17) 0.0294(16) 0.000 0.0023(12) 0.000 O17 0.0285(11) 0.0460(13) 0.0284(12) -0.0044(10) 0.0056(9) 0.0025(10) O18 0.109(3) 0.119(3) 0.0324(16) 0.0179(18) -0.0019(17) -0.075(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O10 1.995(3) 3_545 ? Co1 O2 2.033(2) . ? Co1 O17 2.098(2) . ? Co1 O18 2.108(3) . ? Co1 O9 2.139(2) 4_546 ? Co1 O16 2.1589(19) . ? O2 C4 1.260(4) . ? O3 C4 1.253(4) . ? C4 C5 1.513(4) . ? C5 C6 1.383(5) . ? C5 C13 1.391(4) . ? C6 C7 1.406(4) . ? C6 H6 0.9500 . ? C7 C11 1.394(4) . ? C7 C8 1.511(5) . ? C8 O10 1.230(4) . ? C8 O9 1.247(4) . ? O9 Co1 2.139(2) 4_556 ? O10 Co1 1.995(3) 3_455 ? C11 C12 1.376(5) . ? C11 H11 0.9500 . ? C12 C13 1.384(5) . ? C12 O14 1.436(6) . ? C12 C15 1.538(7) 2 ? C13 H13 0.9500 . ? O14 C15 0.796(7) 2 ? O14 O14 1.019(9) 2 ? O14 C15 1.415(7) . ? C15 O14 0.796(7) 2 ? C15 C15 1.367(13) 2 ? C15 C12 1.538(7) 2 ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? O16 Co1 2.1589(18) 2_656 ? O16 H16A 0.8999 . ? O16 H16B 0.9000 . ? O17 H17A 0.8999 . ? O17 H17B 0.9001 . ? O18 H18A 0.9046 . ? O18 H18B 0.8990 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Co1 O2 178.77(14) 3_545 . ? O10 Co1 O17 88.92(10) 3_545 . ? O2 Co1 O17 91.22(9) . . ? O10 Co1 O18 89.81(17) 3_545 . ? O2 Co1 O18 91.42(16) . . ? O17 Co1 O18 88.00(11) . . ? O10 Co1 O9 91.12(13) 3_545 4_546 ? O2 Co1 O9 87.67(12) . 4_546 ? O17 Co1 O9 86.15(9) . 4_546 ? O18 Co1 O9 174.05(10) . 4_546 ? O10 Co1 O16 88.55(10) 3_545 . ? O2 Co1 O16 91.46(8) . . ? O17 Co1 O16 172.20(7) . . ? O18 Co1 O16 84.61(10) . . ? O9 Co1 O16 101.28(8) 4_546 . ? C4 O2 Co1 131.7(2) . . ? O3 C4 O2 125.2(3) . . ? O3 C4 C5 119.2(3) . . ? O2 C4 C5 115.6(3) . . ? C6 C5 C13 120.6(3) . . ? C6 C5 C4 121.8(3) . . ? C13 C5 C4 117.5(3) . . ? C5 C6 C7 119.6(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C11 C7 C6 119.0(3) . . ? C11 C7 C8 117.1(3) . . ? C6 C7 C8 123.9(3) . . ? O10 C8 O9 126.2(3) . . ? O10 C8 C7 113.4(3) . . ? O9 C8 C7 120.4(3) . . ? C8 O9 Co1 122.6(2) . 4_556 ? C8 O10 Co1 149.2(3) . 3_455 ? C12 C11 C7 120.7(3) . . ? C12 C11 H11 119.6 . . ? C7 C11 H11 119.6 . . ? C11 C12 C13 120.4(3) . . ? C11 C12 O14 107.7(4) . . ? C13 C12 O14 129.1(4) . . ? C11 C12 C15 122.7(4) . 2 ? C13 C12 C15 115.8(4) . 2 ? O14 C12 C15 30.8(3) . 2 ? C12 C13 C5 119.6(3) . . ? C12 C13 H13 120.2 . . ? C5 C13 H13 120.2 . . ? C15 O14 O14 101.6(7) 2 2 ? C15 O14 C12 81.7(7) 2 . ? O14 O14 C12 131.3(7) 2 . ? C15 O14 C12 113.9(4) . . ? C15 C15 C12 110.5(7) 2 2 ? O14 C15 C12 98.8(5) . 2 ? O14 C15 H15A 153.5 2 . ? C15 C15 H15A 79.2 2 . ? O14 C15 H15A 112.4 . . ? C12 C15 H15A 111.9 2 . ? O14 C15 H15B 94.1 2 . ? C15 C15 H15B 128.6 2 . ? O14 C15 H15B 111.9 . . ? C12 C15 H15B 111.9 2 . ? H15A C15 H15B 109.6 . . ? Co1 O16 Co1 109.86(14) . 2_656 ? Co1 O16 H16A 133.7 . . ? Co1 O16 H16A 100.3 2_656 . ? Co1 O16 H16B 113.4 . . ? Co1 O16 H16B 87.2 2_656 . ? H16A O16 H16B 102.1 . . ? Co1 O17 H17A 113.6 . . ? Co1 O17 H17B 97.8 . . ? H17A O17 H17B 102.1 . . ? Co1 O18 H18A 147.5 . . ? Co1 O18 H18B 113.4 . . ? H18A O18 H18B 96.6 . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.599 0.250 -0.151 368 187 ' ' 2 0.099 0.750 -0.151 368 187 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_PLAT417_3 ; PROBLEM: Short Inter D-H..H-D .. H18B...H18B 1.79 Ang. RESPONSE: Atom O18 is disordered, and the positions of its H-atoms are uncertain. ; _vrf_PLAT416_3 ; PROBLEM: Short Inter D-H..H-D .. H16B...H18B 1.89 Ang. RESPONSE: Atom O18 is disordered, and the positions of its H-atoms are uncertain. ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.84 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.795 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.105 data_4 _database_code_depnum_ccdc_archive 'CCDC 915046' #TrackingRef 'Paper1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H18 Mn2 O14' _chemical_formula_sum 'C17 H18 Mn2 O14' _chemical_formula_weight 556.19 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 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.8383(5) _cell_length_b 14.7317(4) _cell_length_c 11.9247(4) _cell_angle_alpha 90.00 _cell_angle_beta 117.3793(12) _cell_angle_gamma 90.00 _cell_volume 2626.65(14) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3013 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 27.93 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 1.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6856 _exptl_absorpt_correction_T_max 0.8219 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11591 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.93 _reflns_number_total 3124 _reflns_number_gt 2205 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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 structure contains also severely disordered dimethyl acetamide solvent which could not be precicely modeled by discrete atoms. Its contribution to the diffraction pattern was subtracted by the SQUEEZE procedure, using the PLATON software (Spek, 2009). ; _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^)+(0.1040P)^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 3124 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1551 _refine_ls_wR_factor_gt 0.1448 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.40242(2) -0.17630(3) 0.59732(4) 0.02481(19) Uani 1 1 d . . . O2 O 0.29414(14) -0.09786(16) 0.5905(2) 0.0446(6) Uani 1 1 d . . . O3 O 0.35702(14) 0.00462(18) 0.7426(2) 0.0453(7) Uani 1 1 d . . . C4 C 0.29135(19) -0.0271(2) 0.6479(3) 0.0331(7) Uani 1 1 d . . . C5 C 0.20321(18) 0.0215(2) 0.5959(3) 0.0291(6) Uani 1 1 d . . . C6 C 0.18707(18) 0.0873(2) 0.6666(3) 0.0302(7) Uani 1 1 d . . . H6 H 0.2309 0.1001 0.7506 0.036 Uiso 1 1 calc R . . C7 C 0.10555(18) 0.1346(2) 0.6130(3) 0.0321(7) Uani 1 1 d . . . C8 C 0.08358(19) 0.2065(2) 0.6835(3) 0.0333(7) Uani 1 1 d . . . O9 O 0.13456(14) 0.21846(16) 0.7992(2) 0.0397(6) Uani 1 1 d . . . O10 O 0.01406(15) 0.25016(18) 0.6213(2) 0.0518(7) Uani 1 1 d . . . C11 C 0.04309(19) 0.1150(3) 0.4893(3) 0.0389(8) Uani 1 1 d . . . H11 H -0.0117 0.1476 0.4520 0.047 Uiso 1 1 calc R . . C12 C 0.0589(2) 0.0497(3) 0.4205(3) 0.0469(10) Uani 1 1 d . . . C13 C 0.13872(19) 0.0023(2) 0.4729(3) 0.0379(8) Uani 1 1 d . . . H13 H 0.1496 -0.0433 0.4253 0.045 Uiso 1 1 calc R . . O14 O -0.0051(3) 0.0630(4) 0.2938(4) 0.0324(11) Uani 0.50 1 d P . . C15 C 0.0126(4) 0.0109(5) 0.2059(5) 0.0257(13) Uani 0.50 1 d P . . H15A H 0.0048 -0.0558 0.2135 0.031 Uiso 0.50 1 d PR . . H15B H 0.0730 0.0228 0.2177 0.031 Uiso 0.50 1 d PR . . O16 O 0.5000 -0.08200(19) 0.7500 0.0267(6) Uani 1 2 d S . . H16A H 0.5359 -0.0342 0.7528 0.032 Uiso 0.50 1 d PR . . H16B H 0.4808 -0.0629 0.8046 0.032 Uiso 0.50 1 d PR . . O17 O 0.31506(13) -0.25280(16) 0.42767(19) 0.0364(5) Uani 1 1 d . . . H17A H 0.2588 -0.2289 0.3862 0.044 Uiso 1 1 d R . . H17B H 0.3071 -0.3027 0.4672 0.044 Uiso 1 1 d R . . O18 O 0.4200(2) -0.0816(2) 0.4708(2) 0.0824(12) Uani 1 1 d . . . H18A H 0.3979 -0.0554 0.3931 0.099 Uiso 1 1 d R . . H18B H 0.4610 -0.0368 0.5130 0.099 Uiso 1 1 d 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 0.0191(3) 0.0261(3) 0.0237(3) 0.00021(17) 0.00521(19) 0.00206(15) O2 0.0280(11) 0.0359(13) 0.0607(15) -0.0224(12) 0.0124(11) 0.0014(9) O3 0.0287(11) 0.0543(16) 0.0346(12) -0.0177(11) -0.0011(10) 0.0117(10) C4 0.0257(14) 0.0338(17) 0.0328(15) -0.0022(13) 0.0075(13) 0.0043(12) C5 0.0238(14) 0.0317(16) 0.0273(14) -0.0028(12) 0.0078(12) 0.0031(12) C6 0.0227(13) 0.0360(17) 0.0230(14) -0.0043(12) 0.0029(11) 0.0038(12) C7 0.0245(14) 0.0359(18) 0.0279(14) -0.0021(13) 0.0052(12) 0.0048(12) C8 0.0240(15) 0.0362(17) 0.0351(16) -0.0033(14) 0.0097(13) 0.0053(13) O9 0.0307(11) 0.0425(14) 0.0374(12) -0.0099(10) 0.0084(10) 0.0074(10) O10 0.0351(12) 0.0641(18) 0.0454(13) -0.0025(13) 0.0092(11) 0.0259(12) C11 0.0215(14) 0.058(2) 0.0301(15) 0.0024(15) 0.0056(12) 0.0100(14) C12 0.0243(15) 0.087(3) 0.0226(15) -0.0109(16) 0.0047(13) 0.0028(16) C13 0.0258(15) 0.054(2) 0.0284(15) -0.0134(15) 0.0075(13) -0.0014(14) O14 0.024(2) 0.034(3) 0.030(2) -0.003(2) 0.0047(19) 0.004(2) C15 0.020(3) 0.033(4) 0.015(2) -0.003(3) 0.001(2) 0.003(3) O16 0.0204(13) 0.0271(15) 0.0249(13) 0.000 0.0039(11) 0.000 O17 0.0283(11) 0.0438(13) 0.0289(10) -0.0041(10) 0.0061(9) -0.0010(9) O18 0.108(2) 0.082(2) 0.0271(12) 0.0124(13) 0.0054(14) -0.048(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mn1 O10 2.072(2) 3_545 ? Mn1 O2 2.128(2) . ? Mn1 O18 2.172(3) . ? Mn1 O17 2.188(2) . ? Mn1 O9 2.241(2) 4_546 ? Mn1 O16 2.2789(17) . ? O2 C4 1.259(4) . ? O3 C4 1.253(4) . ? C4 C5 1.501(4) . ? C5 C6 1.391(4) . ? C5 C13 1.395(4) . ? C6 C7 1.404(4) . ? C6 H6 0.9500 . ? C7 C11 1.392(4) . ? C7 C8 1.500(4) . ? C8 O10 1.240(4) . ? C8 O9 1.258(4) . ? O9 Mn1 2.241(2) 4_556 ? O10 Mn1 2.072(2) 3_455 ? C11 C12 1.368(5) . ? C11 H11 0.9500 . ? C12 C13 1.383(5) . ? C12 O14 1.409(5) . ? C12 C15 1.543(6) 2 ? C13 H13 0.9500 . ? O14 C15 0.778(7) 2 ? O14 O14 1.134(9) 2 ? O14 C15 1.437(6) . ? C15 O14 0.778(7) 2 ? C15 C15 1.303(12) 2 ? C15 C12 1.543(6) 2 ? C15 H15A 1.0003 . ? C15 H15B 0.9750 . ? O16 Mn1 2.2788(17) 2_656 ? O16 H16A 0.9179 . ? O16 H16B 0.8951 . ? O17 H17A 0.9137 . ? O17 H17B 0.9157 . ? O18 H18A 0.9107 . ? O18 H18B 0.9201 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Mn1 O2 174.77(9) 3_545 . ? O10 Mn1 O18 91.56(13) 3_545 . ? O2 Mn1 O18 90.71(13) . . ? O10 Mn1 O17 92.29(9) 3_545 . ? O2 Mn1 O17 92.55(8) . . ? O18 Mn1 O17 86.39(10) . . ? O10 Mn1 O9 91.52(10) 3_545 4_546 ? O2 Mn1 O9 86.93(10) . 4_546 ? O18 Mn1 O9 171.02(9) . 4_546 ? O17 Mn1 O9 85.06(8) . 4_546 ? O10 Mn1 O16 86.18(8) 3_545 . ? O2 Mn1 O16 89.41(7) . . ? O18 Mn1 O16 83.39(8) . . ? O17 Mn1 O16 169.62(7) . . ? O9 Mn1 O16 105.23(7) 4_546 . ? C4 O2 Mn1 132.37(19) . . ? O3 C4 O2 124.1(3) . . ? O3 C4 C5 119.3(3) . . ? O2 C4 C5 116.6(3) . . ? C6 C5 C13 120.3(3) . . ? C6 C5 C4 120.9(2) . . ? C13 C5 C4 118.8(3) . . ? C5 C6 C7 119.5(2) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C11 C7 C6 118.9(3) . . ? C11 C7 C8 118.6(3) . . ? C6 C7 C8 122.4(3) . . ? O10 C8 O9 124.3(3) . . ? O10 C8 C7 116.1(3) . . ? O9 C8 C7 119.6(3) . . ? C8 O9 Mn1 118.62(19) . 4_556 ? C8 O10 Mn1 154.3(2) . 3_455 ? C12 C11 C7 121.4(3) . . ? C12 C11 H11 119.3 . . ? C7 C11 H11 119.3 . . ? C11 C12 C13 120.1(3) . . ? C11 C12 O14 106.3(3) . . ? C13 C12 O14 131.4(3) . . ? C11 C12 C15 124.5(4) . 2 ? C13 C12 C15 114.5(4) . 2 ? C12 C13 C5 119.9(3) . . ? C12 C13 H13 120.1 . . ? C5 C13 H13 120.1 . . ? C12 O14 C15 113.2(3) . . ? C15 C15 C12 112.9(6) 2 2 ? O14 C15 C12 100.6(4) . 2 ? O14 C15 H15A 160.0 2 . ? O14 C15 H15A 112.3 . . ? C12 C15 H15A 112.0 2 . ? O14 C15 H15B 89.1 2 . ? C15 C15 H15B 126.1 2 . ? O14 C15 H15B 110.6 . . ? C12 C15 H15B 111.6 2 . ? H15A C15 H15B 109.5 . . ? Mn1 O16 Mn1 104.87(11) 2_656 . ? Mn1 O16 H16A 102.5 2_656 . ? Mn1 O16 H16A 135.8 . . ? Mn1 O16 H16B 88.8 2_656 . ? Mn1 O16 H16B 113.8 . . ? H16A O16 H16B 100.6 . . ? Mn1 O17 H17A 113.0 . . ? Mn1 O17 H17B 97.7 . . ? H17A O17 H17B 103.1 . . ? Mn1 O18 H18A 149.0 . . ? Mn1 O18 H18B 112.9 . . ? H18A O18 H18B 96.0 . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.608 0.250 -0.142 391 182 ' ' 2 0.108 0.750 -0.142 391 182 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.93 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.679 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.102 #=================================END============================