# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Pablo Albores' _publ_contact_author_email ALBORES@UNI-MAINZ.DE _publ_section_title ; Ferromagnetic coupled mu-phenoxo-mu-carboxylato heterodinuclear complexes based on the Cr(salen) moiety: structural and magnetic characterization. ; loop_ _publ_author_name 'Pablo Albores' 'Eva Rentschler' 'Johanna Seeman' # Attachment 'albores_et.al_revised.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 720440' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H34 Cr N4 O3 P' _chemical_formula_weight 725.70 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.496(4) _cell_length_b 13.230(5) _cell_length_c 14.082(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.183(12) _cell_angle_gamma 90.00 _cell_volume 1767.9(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 754 _exptl_absorpt_coefficient_mu 0.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8115 _exptl_absorpt_correction_T_max 0.9878 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9740 _diffrn_reflns_av_R_equivalents 0.1327 _diffrn_reflns_av_sigmaI/netI 0.1489 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 20.31 _reflns_number_total 3413 _reflns_number_gt 2316 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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. ; _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^)+(0.0121P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.07(4) _refine_ls_number_reflns 3413 _refine_ls_number_parameters 460 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.0829 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _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 Cr1 Cr 0.57452(14) 0.33459(11) 0.92708(9) 0.0266(4) Uani 1 1 d . . . P1 P 0.1347(2) 0.25942(17) 0.49720(15) 0.0268(6) Uani 1 1 d . . . O1 O 0.7406(6) 0.4195(4) 0.9341(4) 0.0273(15) Uani 1 1 d . . . O2 O 0.4469(6) 0.4358(4) 0.8737(4) 0.0299(16) Uani 1 1 d . . . N1 N 0.6845(8) 0.2166(5) 0.9810(5) 0.027(2) Uani 1 1 d . . . N2 N 0.5159(8) 0.4056(6) 1.1446(5) 0.045(2) Uani 1 1 d . . . N3 N 0.4180(8) 0.2348(5) 0.9362(5) 0.030(2) Uani 1 1 d . . . N4 N 0.6481(8) 0.2424(7) 0.7185(5) 0.055(3) Uani 1 1 d . . . C5 C 0.3889(9) 0.5431(7) 0.5687(6) 0.034(2) Uani 1 1 d . . . H5 H 0.4448 0.6015 0.5811 0.041 Uiso 1 1 calc R . . C6 C 0.2206(9) 0.2000(6) 0.3990(5) 0.027(2) Uani 1 1 d . . . C8 C 1.0653(10) 0.4789(7) 1.0635(6) 0.044(3) Uani 1 1 d . . . H8 H 1.1244 0.5362 1.0734 0.052 Uiso 1 1 calc R . . C9 C 0.2064(8) 0.0966(6) 0.3868(6) 0.027(2) Uani 1 1 d . . . H9 H 0.1568 0.0575 0.4312 0.033 Uiso 1 1 calc R . . C10 C -0.1348(9) 0.3348(8) 0.5207(5) 0.034(2) Uani 1 1 d . . . H10 H -0.1020 0.3544 0.5825 0.041 Uiso 1 1 calc R . . C12 C 0.1389(9) 0.1725(6) 0.5949(6) 0.028(2) Uani 1 1 d . . . C13 C 0.8527(9) 0.4062(7) 0.9904(6) 0.025(2) Uani 1 1 d . . . C14 C 0.2650(8) 0.0509(7) 0.3094(6) 0.033(2) Uani 1 1 d . . . H14 H 0.2561 -0.0201 0.3009 0.040 Uiso 1 1 calc R . . C15 C 0.4580(8) 0.1399(7) 0.9881(6) 0.031(2) Uani 1 1 d . . . H15A H 0.3998 0.0827 0.9640 0.038 Uiso 1 1 calc R . . H15B H 0.4431 0.1479 1.0569 0.038 Uiso 1 1 calc R . . C16 C 0.8880(9) 0.3140(7) 1.0370(5) 0.024(2) Uani 1 1 d . . . C17 C 0.2353(9) 0.3345(9) 0.8571(5) 0.030(2) Uani 1 1 d . . . C18 C 0.2265(9) 0.3745(7) 0.5309(6) 0.029(3) Uani 1 1 d . . . C19 C 0.3352(9) 0.1065(7) 0.2457(6) 0.032(2) Uani 1 1 d . . . H19 H 0.3753 0.0741 0.1929 0.038 Uiso 1 1 calc R . . C21 C 1.1017(10) 0.3868(8) 1.1069(6) 0.040(3) Uani 1 1 d . . . H21 H 1.1867 0.3807 1.1443 0.048 Uiso 1 1 calc R . . C22 C 0.0184(9) 0.1460(6) 0.6422(6) 0.030(2) Uani 1 1 d . . . H22 H -0.0694 0.1758 0.6235 0.037 Uiso 1 1 calc R . . C23 C 0.2661(10) 0.1273(7) 0.6231(6) 0.035(3) Uani 1 1 d . . . H23 H 0.3494 0.1436 0.5911 0.042 Uiso 1 1 calc R . . C24 C 0.1521(12) 0.0341(7) 0.7444(6) 0.044(3) Uani 1 1 d . . . H24 H 0.1570 -0.0122 0.7961 0.053 Uiso 1 1 calc R . . C25 C 0.8039(11) 0.2226(6) 1.0252(6) 0.032(3) Uani 1 1 d . . . H25 H 0.8412 0.1623 1.0527 0.039 Uiso 1 1 calc R . . C26 C -0.0417(8) 0.2887(6) 0.4579(6) 0.023(2) Uani 1 1 d . . . C27 C 0.2939(8) 0.2561(7) 0.3339(6) 0.030(2) Uani 1 1 d . . . H27 H 0.3060 0.3268 0.3426 0.036 Uiso 1 1 calc R . . C28 C 0.3340(9) 0.3731(7) 0.6023(5) 0.034(3) Uani 1 1 d . . . H28 H 0.3520 0.3133 0.6381 0.040 Uiso 1 1 calc R . . C29 C -0.2290(10) 0.2885(7) 0.3371(7) 0.046(3) Uani 1 1 d . . . H29 H -0.2616 0.2731 0.2741 0.055 Uiso 1 1 calc R . . C30 C 0.2428(10) 0.5071(7) 0.8041(6) 0.031(2) Uani 1 1 d . . . H30 H 0.2938 0.5683 0.7977 0.037 Uiso 1 1 calc R . . C31 C 0.0937(9) 0.3331(9) 0.8240(5) 0.040(2) Uani 1 1 d . . . H31 H 0.0404 0.2730 0.8315 0.048 Uiso 1 1 calc R . . C33 C 0.2044(10) 0.4624(7) 0.4793(6) 0.043(3) Uani 1 1 d . . . H33 H 0.1330 0.4650 0.4302 0.051 Uiso 1 1 calc R . . C34 C 0.4129(9) 0.4585(7) 0.6202(6) 0.035(3) Uani 1 1 d . . . H34 H 0.4846 0.4580 0.6690 0.043 Uiso 1 1 calc R . . C35 C 0.1052(10) 0.5042(7) 0.7719(6) 0.042(3) Uani 1 1 d . . . H35 H 0.0620 0.5622 0.7435 0.050 Uiso 1 1 calc R . . C36 C 0.3122(10) 0.4241(8) 0.8462(6) 0.026(2) Uani 1 1 d . . . C37 C 1.0140(10) 0.3062(7) 1.0949(6) 0.039(3) Uani 1 1 d . . . H37 H 1.0369 0.2440 1.1255 0.046 Uiso 1 1 calc R . . C38 C 0.0297(10) 0.4147(9) 0.7814(6) 0.046(3) Uani 1 1 d . . . H38 H -0.0655 0.4105 0.7584 0.055 Uiso 1 1 calc R . . C39 C -0.3200(9) 0.3311(8) 0.4013(7) 0.043(2) Uani 1 1 d . . . H39 H -0.4145 0.3460 0.3818 0.052 Uiso 1 1 calc R . . C40 C 0.6114(8) 0.1204(6) 0.9715(5) 0.029(2) Uani 1 1 d . . . H40A H 0.6503 0.0714 1.0186 0.034 Uiso 1 1 calc R . . H40B H 0.6226 0.0922 0.9070 0.034 Uiso 1 1 calc R . . C41 C -0.0908(9) 0.2689(7) 0.3659(6) 0.035(2) Uani 1 1 d . . . H41 H -0.0282 0.2412 0.3217 0.042 Uiso 1 1 calc R . . C43 C 0.2911(10) 0.2446(7) 0.9037(5) 0.031(2) Uani 1 1 d . . . H43 H 0.2290 0.1890 0.9105 0.037 Uiso 1 1 calc R . . C44 C 0.2722(11) 0.0580(7) 0.6982(6) 0.047(3) Uani 1 1 d . . . H44 H 0.3594 0.0275 0.7172 0.056 Uiso 1 1 calc R . . C45 C 0.0246(11) 0.0764(7) 0.7167(6) 0.040(3) Uani 1 1 d . . . H45 H -0.0586 0.0583 0.7481 0.048 Uiso 1 1 calc R . . C46 C 0.5323(9) 0.3783(6) 1.0674(6) 0.030(3) Uani 1 1 d . . . C47 C 0.9450(10) 0.4873(7) 1.0066(6) 0.032(2) Uani 1 1 d . . . H47 H 0.9238 0.5504 0.9773 0.039 Uiso 1 1 calc R . . C48 C 0.6204(8) 0.2785(7) 0.7888(6) 0.031(3) Uani 1 1 d . . . C49 C 0.3488(9) 0.2086(7) 0.2567(6) 0.036(3) Uani 1 1 d . . . H49 H 0.3964 0.2470 0.2108 0.043 Uiso 1 1 calc R . . C50 C -0.2738(9) 0.3514(7) 0.4921(7) 0.049(3) Uani 1 1 d . . . H50 H -0.3378 0.3774 0.5363 0.059 Uiso 1 1 calc R . . C51 C 0.2858(10) 0.5456(7) 0.4992(6) 0.046(3) Uani 1 1 d . . . H51 H 0.2699 0.6061 0.4640 0.055 Uiso 1 1 calc R . . O1W O 0.3401(7) 0.5111(5) 0.2761(5) 0.071(2) 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 Cr1 0.0311(8) 0.0225(8) 0.0262(8) 0.0006(8) 0.0015(6) 0.0006(9) P1 0.0330(15) 0.0243(16) 0.0232(15) 0.0005(13) 0.0010(12) 0.0012(13) O1 0.031(4) 0.017(4) 0.034(4) 0.005(3) 0.001(3) -0.006(3) O2 0.031(4) 0.026(4) 0.033(4) 0.006(3) -0.002(3) -0.003(3) N1 0.035(5) 0.018(5) 0.028(5) 0.000(4) -0.008(4) -0.005(4) N2 0.058(6) 0.027(5) 0.050(6) -0.007(5) 0.000(5) -0.009(4) N3 0.028(5) 0.033(6) 0.028(5) -0.003(4) -0.001(4) -0.001(4) N4 0.075(6) 0.073(7) 0.018(5) 0.003(5) 0.005(5) 0.010(6) C5 0.032(7) 0.029(7) 0.041(7) 0.000(6) 0.000(5) -0.006(5) C6 0.038(6) 0.018(6) 0.023(6) -0.005(5) -0.008(5) 0.006(5) C8 0.039(7) 0.040(8) 0.052(7) -0.014(6) 0.001(6) -0.014(6) C9 0.015(6) 0.026(7) 0.041(6) 0.012(5) 0.009(5) 0.001(5) C10 0.032(6) 0.037(6) 0.033(5) -0.004(6) -0.009(5) -0.003(6) C12 0.021(6) 0.024(6) 0.039(6) -0.010(5) 0.006(5) 0.005(5) C13 0.024(6) 0.032(7) 0.020(6) 0.000(5) -0.003(5) 0.003(6) C14 0.024(6) 0.035(6) 0.041(7) -0.012(6) -0.003(5) -0.009(5) C15 0.041(7) 0.020(6) 0.033(6) 0.005(5) 0.004(5) -0.004(5) C16 0.035(6) 0.020(7) 0.017(5) -0.003(5) 0.000(4) -0.005(6) C17 0.023(6) 0.043(7) 0.025(5) -0.017(6) 0.006(4) -0.011(7) C18 0.025(6) 0.032(8) 0.030(6) -0.002(5) 0.006(5) 0.000(5) C19 0.031(7) 0.034(7) 0.031(6) -0.006(5) 0.004(5) 0.005(6) C21 0.045(7) 0.039(7) 0.035(7) -0.003(6) -0.003(6) 0.007(6) C22 0.031(7) 0.025(6) 0.034(6) 0.014(5) -0.015(5) -0.006(5) C23 0.043(7) 0.037(7) 0.026(6) 0.006(5) 0.005(5) 0.012(6) C24 0.078(8) 0.031(7) 0.024(6) 0.010(5) 0.015(7) -0.001(7) C25 0.057(8) 0.020(7) 0.021(6) 0.002(5) 0.004(6) 0.006(6) C26 0.025(5) 0.020(6) 0.024(6) -0.006(4) 0.006(5) 0.004(4) C27 0.028(6) 0.024(6) 0.037(6) 0.013(6) 0.005(5) -0.013(5) C28 0.042(6) 0.030(7) 0.029(6) -0.001(5) 0.000(5) 0.006(5) C29 0.041(7) 0.035(7) 0.059(8) -0.001(6) -0.023(6) 0.002(5) C30 0.031(7) 0.031(7) 0.031(6) -0.007(5) 0.002(5) 0.002(5) C31 0.042(7) 0.053(7) 0.025(6) -0.020(6) 0.005(5) -0.004(7) C33 0.049(7) 0.019(6) 0.057(8) 0.011(6) -0.029(6) -0.010(6) C34 0.036(7) 0.037(7) 0.033(6) -0.014(6) 0.002(5) -0.001(6) C35 0.049(8) 0.039(8) 0.037(7) 0.001(5) -0.002(6) 0.009(6) C36 0.022(6) 0.038(7) 0.018(6) -0.003(5) 0.007(5) 0.016(6) C37 0.055(7) 0.036(8) 0.025(6) 0.001(5) 0.004(6) 0.000(6) C38 0.040(7) 0.081(10) 0.015(6) -0.005(6) -0.010(5) 0.017(8) C39 0.030(6) 0.038(6) 0.062(7) 0.004(7) 0.002(6) -0.006(7) C40 0.041(7) 0.022(6) 0.023(6) 0.000(4) 0.002(5) -0.009(5) C41 0.041(7) 0.028(6) 0.035(7) 0.005(5) 0.002(5) 0.000(6) C43 0.057(8) 0.022(7) 0.014(6) -0.007(5) -0.002(5) -0.006(6) C44 0.054(8) 0.050(8) 0.034(7) 0.003(6) -0.010(6) 0.007(6) C45 0.044(7) 0.043(8) 0.032(7) -0.006(6) 0.006(5) -0.008(6) C46 0.038(6) 0.017(6) 0.036(6) -0.001(5) 0.000(5) -0.001(4) C47 0.037(6) 0.026(7) 0.034(6) -0.007(5) 0.013(5) -0.011(6) C48 0.030(6) 0.037(6) 0.026(6) -0.001(5) -0.004(5) 0.003(5) C49 0.048(7) 0.035(8) 0.026(6) 0.004(5) 0.012(5) 0.009(6) C50 0.042(7) 0.048(8) 0.057(7) 0.000(7) 0.007(5) 0.011(7) C51 0.062(7) 0.022(6) 0.053(7) -0.004(6) -0.014(6) 0.001(6) O1W 0.074(5) 0.064(5) 0.076(5) -0.001(4) 0.029(4) -0.005(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 Cr1 O1 1.936(5) . ? Cr1 O2 1.938(6) . ? Cr1 N3 1.996(7) . ? Cr1 N1 2.012(7) . ? Cr1 C46 2.112(9) . ? Cr1 C48 2.144(9) . ? P1 C26 1.787(8) . ? P1 C12 1.793(8) . ? P1 C18 1.809(8) . ? P1 C6 1.812(8) . ? O1 C13 1.314(9) . ? O2 C36 1.331(9) . ? N1 C25 1.274(10) . ? N1 C40 1.453(9) . ? N2 C46 1.162(9) . ? N3 C43 1.279(10) . ? N3 C15 1.495(10) . ? N4 C48 1.138(9) . ? C5 C34 1.348(10) . ? C5 C51 1.358(10) . ? C6 C9 1.384(10) . ? C6 C27 1.387(10) . ? C8 C47 1.374(11) . ? C8 C21 1.402(11) . ? C9 C14 1.381(10) . ? C10 C50 1.382(9) . ? C10 C26 1.412(10) . ? C12 C22 1.390(10) . ? C12 C23 1.392(10) . ? C13 C47 1.399(11) . ? C13 C16 1.419(11) . ? C14 C19 1.355(11) . ? C15 C40 1.506(9) . ? C16 C37 1.426(10) . ? C16 C25 1.455(11) . ? C17 C36 1.404(12) . ? C17 C31 1.407(10) . ? C17 C43 1.448(11) . ? C18 C33 1.383(10) . ? C18 C28 1.405(10) . ? C19 C49 1.365(10) . ? C21 C37 1.359(11) . ? C22 C45 1.396(11) . ? C23 C44 1.399(10) . ? C24 C44 1.371(11) . ? C24 C45 1.377(11) . ? C26 C41 1.386(9) . ? C27 C49 1.376(10) . ? C28 C34 1.374(10) . ? C29 C39 1.393(11) . ? C29 C41 1.384(11) . ? C30 C35 1.367(10) . ? C30 C36 1.400(11) . ? C31 C38 1.367(12) . ? C33 C51 1.368(11) . ? C35 C38 1.394(12) . ? C39 C50 1.362(10) . ? 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 O1 Cr1 O2 96.6(2) . . ? O1 Cr1 N3 171.1(3) . . ? O2 Cr1 N3 91.5(3) . . ? O1 Cr1 N1 91.2(3) . . ? O2 Cr1 N1 172.2(3) . . ? N3 Cr1 N1 80.8(3) . . ? O1 Cr1 C46 88.6(3) . . ? O2 Cr1 C46 92.0(3) . . ? N3 Cr1 C46 87.3(3) . . ? N1 Cr1 C46 88.5(3) . . ? O1 Cr1 C48 93.1(3) . . ? O2 Cr1 C48 91.8(3) . . ? N3 Cr1 C48 90.4(3) . . ? N1 Cr1 C48 87.3(3) . . ? C46 Cr1 C48 175.5(4) . . ? C26 P1 C12 111.7(4) . . ? C26 P1 C18 109.6(4) . . ? C12 P1 C18 110.0(4) . . ? C26 P1 C6 107.6(4) . . ? C12 P1 C6 108.0(4) . . ? C18 P1 C6 109.8(4) . . ? C13 O1 Cr1 126.4(6) . . ? C36 O2 Cr1 127.8(6) . . ? C25 N1 C40 120.9(7) . . ? C25 N1 Cr1 125.1(6) . . ? C40 N1 Cr1 113.9(5) . . ? C43 N3 C15 118.6(8) . . ? C43 N3 Cr1 127.1(7) . . ? C15 N3 Cr1 114.3(5) . . ? C34 C5 C51 120.7(9) . . ? C9 C6 C27 119.7(8) . . ? C9 C6 P1 118.6(7) . . ? C27 C6 P1 121.6(7) . . ? C47 C8 C21 120.7(9) . . ? C14 C9 C6 119.3(8) . . ? C50 C10 C26 120.0(7) . . ? C22 C12 C23 118.4(8) . . ? C22 C12 P1 122.3(7) . . ? C23 C12 P1 119.2(7) . . ? O1 C13 C47 118.9(9) . . ? O1 C13 C16 124.4(9) . . ? C47 C13 C16 116.6(8) . . ? C19 C14 C9 120.5(9) . . ? N3 C15 C40 107.3(7) . . ? C13 C16 C37 120.3(8) . . ? C13 C16 C25 122.8(8) . . ? C37 C16 C25 116.8(9) . . ? C36 C17 C31 118.0(10) . . ? C36 C17 C43 124.1(8) . . ? C31 C17 C43 117.9(10) . . ? C33 C18 C28 118.6(8) . . ? C33 C18 P1 120.5(7) . . ? C28 C18 P1 120.4(7) . . ? C14 C19 C49 120.6(9) . . ? C37 C21 C8 119.2(9) . . ? C12 C22 C45 121.0(8) . . ? C44 C23 C12 120.5(9) . . ? C44 C24 C45 120.7(8) . . ? N1 C25 C16 125.6(8) . . ? C41 C26 C10 118.1(7) . . ? C41 C26 P1 121.8(6) . . ? C10 C26 P1 120.1(6) . . ? C49 C27 C6 119.5(8) . . ? C34 C28 C18 119.7(8) . . ? C39 C29 C41 119.4(9) . . ? C35 C30 C36 123.2(9) . . ? C38 C31 C17 122.6(10) . . ? C51 C33 C18 119.7(8) . . ? C5 C34 C28 120.3(8) . . ? C30 C35 C38 118.7(9) . . ? O2 C36 C30 117.6(9) . . ? O2 C36 C17 124.3(9) . . ? C30 C36 C17 118.1(9) . . ? C21 C37 C16 120.8(9) . . ? C31 C38 C35 119.5(9) . . ? C50 C39 C29 120.3(8) . . ? N1 C40 C15 107.3(7) . . ? C26 C41 C29 121.3(9) . . ? N3 C43 C17 124.7(9) . . ? C24 C44 C23 119.9(8) . . ? C24 C45 C22 119.5(9) . . ? N2 C46 Cr1 176.2(8) . . ? C8 C47 C13 122.4(9) . . ? N4 C48 Cr1 175.0(8) . . ? C19 C49 C27 120.3(9) . . ? C39 C50 C10 120.7(8) . . ? C5 C51 C33 120.9(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 20.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.212 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.049 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 720441' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H45 Cr N2 Ni O10' _chemical_formula_weight 716.40 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.473(3) _cell_length_b 17.499(4) _cell_length_c 23.282(4) _cell_angle_alpha 90.000 _cell_angle_beta 90.000 _cell_angle_gamma 90.000 _cell_volume 7119(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3016 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7636 _exptl_absorpt_correction_T_max 0.9141 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 110567 _diffrn_reflns_av_R_equivalents 0.3133 _diffrn_reflns_av_sigmaI/netI 0.2382 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.56 _reflns_number_total 8784 _reflns_number_gt 3207 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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. ; _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^)+(0.0473P)^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 8784 _refine_ls_number_parameters 418 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1907 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1041 _refine_ls_goodness_of_fit_ref 0.799 _refine_ls_restrained_S_all 0.799 _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 Ni1 Ni 0.97304(3) 0.02871(3) 0.09931(2) 0.02504(16) Uani 1 1 d . . . Cr1 Cr 1.01798(4) 0.14708(4) 0.18762(3) 0.02627(19) Uani 1 1 d . . . O1 O 1.03933(17) 0.20281(17) 0.11543(13) 0.0295(8) Uani 1 1 d . . . O2 O 0.91869(16) 0.11770(17) 0.15795(13) 0.0264(8) Uani 1 1 d . . . O3 O 1.00389(16) 0.11833(17) 0.04808(13) 0.0272(8) Uani 1 1 d . . . O4 O 0.88512(17) 0.00585(17) 0.04319(13) 0.0303(8) Uani 1 1 d . . . O5 O 0.9393(2) -0.05591(19) 0.15175(14) 0.0299(8) Uani 1 1 d D . . O6 O 1.06342(17) 0.05494(16) 0.15746(13) 0.0264(8) Uani 1 1 d . . . O7 O 1.00056(18) 0.10488(18) 0.26374(13) 0.0339(9) Uani 1 1 d . . . O8 O 1.04073(18) -0.04304(19) 0.05258(14) 0.0300(8) Uani 1 1 d D . . O9 O 0.9540(2) -0.01400(19) 0.25870(14) 0.0441(10) Uani 1 1 d . . . O10 O 0.80613(18) -0.0612(2) 0.09993(15) 0.0421(9) Uani 1 1 d . . . C1 C 0.9608(4) 0.2966(3) 0.0266(3) 0.077(2) Uani 1 1 d . . . H1A H 0.9574 0.3148 0.0664 0.115 Uiso 1 1 calc R . . H1B H 0.9154 0.2661 0.0175 0.115 Uiso 1 1 calc R . . H1C H 0.9636 0.3405 0.0006 0.115 Uiso 1 1 calc R . . C2 C 0.8600(3) 0.1653(3) 0.1512(2) 0.0282(12) Uani 1 1 d . . . C3 C 0.8584(3) 0.2430(3) 0.1705(2) 0.0302(12) Uani 1 1 d . . . C4 C 1.1244(3) 0.0202(3) 0.1814(2) 0.0293(12) Uani 1 1 d . . . N1 N 0.9823(2) 0.2479(2) 0.21782(16) 0.0312(10) Uani 1 1 d . . . C5 C 1.0310(3) 0.2484(3) 0.0197(2) 0.0378(13) Uani 1 1 d . . . N2 N 1.1191(2) 0.1839(2) 0.21645(17) 0.0320(10) Uani 1 1 d . . . C6 C 0.6854(3) -0.0515(4) 0.0285(3) 0.093(3) Uani 1 1 d . . . H6A H 0.6706 -0.0120 0.0563 0.139 Uiso 1 1 calc R . . H6B H 0.6871 -0.1013 0.0477 0.139 Uiso 1 1 calc R . . H6C H 0.6478 -0.0531 -0.0027 0.139 Uiso 1 1 calc R . . C7 C 1.1793(3) 0.0603(3) 0.2142(2) 0.0313(12) Uani 1 1 d . . . C31 C 1.0456(4) 0.0734(4) 0.3747(2) 0.081(2) Uani 1 1 d . . . H31A H 1.0584 0.1216 0.3555 0.121 Uiso 1 1 calc R . . H31B H 1.0873 0.0367 0.3690 0.121 Uiso 1 1 calc R . . H31C H 1.0386 0.0826 0.4159 0.121 Uiso 1 1 calc R . . C8 C 1.1977(3) -0.0958(3) 0.1951(2) 0.0421(14) Uani 1 1 d . . . H8 H 1.2030 -0.1492 0.1890 0.050 Uiso 1 1 calc R . . C9 C 1.1350(3) -0.0580(3) 0.1729(2) 0.0339(13) Uani 1 1 d . . . H9 H 1.0982 -0.0858 0.1512 0.041 Uiso 1 1 calc R . . C10 C 0.7939(3) 0.2886(3) 0.1582(2) 0.0379(14) Uani 1 1 d . . . H10 H 0.7937 0.3404 0.1703 0.045 Uiso 1 1 calc R . . C11 C 0.7303(3) 0.1842(3) 0.1135(2) 0.0455(15) Uani 1 1 d . . . H11 H 0.6866 0.1636 0.0948 0.055 Uiso 1 1 calc R . . C12 C 0.7929(3) 0.1381(3) 0.1247(2) 0.0353(13) Uani 1 1 d . . . H12 H 0.7904 0.0857 0.1140 0.042 Uiso 1 1 calc R . . C13 C 1.1184(3) 0.2672(3) 0.2294(2) 0.0400(14) Uani 1 1 d . . . H13A H 1.1280 0.2969 0.1939 0.048 Uiso 1 1 calc R . . H13B H 1.1589 0.2797 0.2576 0.048 Uiso 1 1 calc R . . C14 C 0.8219(3) -0.0298(3) 0.0536(2) 0.0331(12) Uani 1 1 d . . . C15 C 1.0247(3) 0.1837(3) 0.0637(2) 0.0285(11) Uani 1 1 d . . . C16 C 0.7577(4) 0.0468(4) -0.0253(3) 0.078(2) Uani 1 1 d . . . H16A H 0.7397 0.0847 0.0026 0.118 Uiso 1 1 calc R . . H16B H 0.7216 0.0440 -0.0574 0.118 Uiso 1 1 calc R . . H16C H 0.8082 0.0619 -0.0397 0.118 Uiso 1 1 calc R . . C17 C 1.1766(3) 0.1412(3) 0.2265(2) 0.0366(13) Uani 1 1 d . . . H17 H 1.2207 0.1641 0.2431 0.044 Uiso 1 1 calc R . . C18 C 0.9187(3) 0.2788(3) 0.2037(2) 0.0368(14) Uani 1 1 d . . . H18 H 0.9102 0.3299 0.2160 0.044 Uiso 1 1 calc R . . C19 C 0.9758(3) 0.0426(3) 0.2849(2) 0.0314(12) Uani 1 1 d . . . C20 C 0.7635(3) -0.0329(3) 0.0043(2) 0.0431(14) Uani 1 1 d . . . C21 C 1.2435(3) 0.0202(3) 0.2355(2) 0.0459(15) Uani 1 1 d . . . H21 H 1.2812 0.0472 0.2567 0.055 Uiso 1 1 calc R . . C22 C 1.2528(3) -0.0569(3) 0.2262(2) 0.0492(16) Uani 1 1 d . . . H22 H 1.2963 -0.0829 0.2408 0.059 Uiso 1 1 calc R . . C23 C 1.0406(3) 0.2872(3) 0.2537(2) 0.0440(15) Uani 1 1 d . . . H23A H 1.0367 0.2698 0.2941 0.053 Uiso 1 1 calc R . . H23B H 1.0325 0.3432 0.2526 0.053 Uiso 1 1 calc R . . C24 C 0.7313(3) 0.2605(3) 0.1294(2) 0.0449(15) Uani 1 1 d . . . H24 H 0.6894 0.2930 0.1205 0.054 Uiso 1 1 calc R . . C25 C 1.0398(3) 0.2184(3) -0.0415(2) 0.0542(17) Uani 1 1 d . . . H25A H 1.0863 0.1872 -0.0441 0.081 Uiso 1 1 calc R . . H25B H 1.0436 0.2615 -0.0682 0.081 Uiso 1 1 calc R . . H25C H 0.9953 0.1870 -0.0514 0.081 Uiso 1 1 calc R . . C26 C 0.9735(4) 0.0420(3) 0.3499(2) 0.0537(16) Uani 1 1 d . . . C27 C 1.1028(4) 0.2985(3) 0.0333(3) 0.070(2) Uani 1 1 d . . . H27A H 1.1492 0.2676 0.0290 0.104 Uiso 1 1 calc R . . H27B H 1.0995 0.3175 0.0728 0.104 Uiso 1 1 calc R . . H27C H 1.1047 0.3419 0.0067 0.104 Uiso 1 1 calc R . . C28 C 0.9105(4) 0.1069(5) 0.3666(3) 0.112(3) Uani 1 1 d . . . H28A H 0.9282 0.1569 0.3531 0.168 Uiso 1 1 calc R . . H28B H 0.9038 0.1082 0.4084 0.168 Uiso 1 1 calc R . . H28C H 0.8615 0.0945 0.3483 0.168 Uiso 1 1 calc R . . C29 C 0.7912(3) -0.0895(4) -0.0392(3) 0.084(2) Uani 1 1 d . . . H29A H 0.7546 -0.0924 -0.0710 0.127 Uiso 1 1 calc R . . H29B H 0.7959 -0.1399 -0.0212 0.127 Uiso 1 1 calc R . . H29C H 0.8412 -0.0734 -0.0539 0.127 Uiso 1 1 calc R . . C30 C 0.9422(5) -0.0307(4) 0.3735(3) 0.119(3) Uani 1 1 d . . . H30A H 0.9408 -0.0279 0.4155 0.178 Uiso 1 1 calc R . . H30B H 0.9749 -0.0734 0.3617 0.178 Uiso 1 1 calc R . . H30C H 0.8903 -0.0387 0.3588 0.178 Uiso 1 1 calc R . . H2 H 0.938(4) -0.045(4) 0.1860(12) 0.142 Uiso 1 1 d D . . H1 H 0.897(2) -0.070(4) 0.138(3) 0.142 Uiso 1 1 d D . . H3 H 1.017(4) -0.072(4) 0.030(3) 0.142 Uiso 1 1 d D . . H4 H 1.073(3) -0.024(4) 0.030(3) 0.142 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0338(3) 0.0216(3) 0.0198(3) -0.0006(3) -0.0011(3) -0.0008(3) Cr1 0.0360(4) 0.0209(4) 0.0219(4) -0.0018(4) -0.0022(4) -0.0015(4) O1 0.045(2) 0.0236(18) 0.0198(19) -0.0001(15) 0.0007(16) -0.0038(15) O2 0.0287(18) 0.0224(18) 0.0281(19) -0.0004(16) -0.0008(15) 0.0045(15) O3 0.038(2) 0.0214(18) 0.0219(19) 0.0015(15) 0.0009(14) -0.0035(14) O4 0.034(2) 0.033(2) 0.0246(19) -0.0013(16) -0.0016(16) -0.0019(16) O5 0.045(2) 0.0204(18) 0.0239(19) 0.0012(17) -0.0013(18) -0.0060(16) O6 0.0285(18) 0.0239(18) 0.0269(19) -0.0002(16) -0.0037(15) 0.0026(14) O7 0.054(2) 0.0269(19) 0.0209(19) -0.0011(16) 0.0011(16) -0.0070(16) O8 0.037(2) 0.029(2) 0.024(2) -0.0025(16) 0.0006(15) 0.0015(15) O9 0.074(3) 0.035(2) 0.023(2) -0.0025(18) -0.0015(18) -0.0166(19) O10 0.045(2) 0.047(2) 0.034(2) 0.008(2) -0.0062(19) -0.0152(18) C1 0.104(6) 0.070(5) 0.057(5) 0.034(4) 0.022(4) 0.049(4) C2 0.037(3) 0.027(3) 0.021(3) 0.003(2) 0.008(2) 0.001(2) C3 0.033(3) 0.028(3) 0.030(3) 0.003(2) 0.004(2) 0.002(2) C4 0.033(3) 0.033(3) 0.022(3) 0.004(3) 0.000(2) 0.001(2) N1 0.040(2) 0.024(2) 0.030(2) -0.0048(19) -0.001(2) -0.002(2) C5 0.063(4) 0.025(3) 0.025(3) 0.008(2) 0.003(3) 0.002(3) N2 0.043(3) 0.027(2) 0.026(3) 0.001(2) -0.006(2) -0.005(2) C6 0.038(4) 0.183(9) 0.057(5) 0.002(5) -0.012(3) -0.023(4) C7 0.032(3) 0.034(3) 0.028(3) 0.004(3) -0.002(2) 0.000(2) C31 0.081(5) 0.129(7) 0.032(4) -0.002(4) -0.023(4) -0.010(5) C8 0.048(4) 0.033(3) 0.046(4) 0.003(3) 0.000(3) 0.010(3) C9 0.037(3) 0.028(3) 0.036(3) 0.000(3) -0.003(2) 0.003(2) C10 0.048(4) 0.030(3) 0.036(3) 0.002(3) 0.008(3) 0.011(3) C11 0.039(3) 0.050(4) 0.047(4) -0.007(3) -0.001(3) 0.008(3) C12 0.036(3) 0.035(3) 0.036(3) -0.007(3) 0.000(2) 0.001(3) C13 0.052(4) 0.033(3) 0.035(3) -0.002(3) -0.010(3) -0.011(3) C14 0.039(3) 0.031(3) 0.029(3) -0.011(3) -0.005(3) 0.006(3) C15 0.029(3) 0.030(3) 0.026(3) 0.004(2) 0.003(3) 0.005(3) C16 0.079(5) 0.082(5) 0.074(5) 0.004(4) -0.029(4) 0.023(4) C17 0.041(3) 0.040(3) 0.029(3) 0.004(3) -0.009(3) -0.012(3) C18 0.051(4) 0.025(3) 0.033(3) -0.006(3) 0.009(3) -0.002(3) C19 0.036(3) 0.035(3) 0.023(3) 0.001(2) 0.001(3) -0.004(3) C20 0.033(3) 0.062(4) 0.034(3) -0.009(3) -0.008(3) 0.002(3) C21 0.041(3) 0.046(4) 0.050(4) 0.003(3) -0.010(3) 0.004(3) C22 0.042(4) 0.056(4) 0.050(4) 0.006(3) -0.014(3) 0.009(3) C23 0.067(4) 0.029(3) 0.036(3) -0.014(3) -0.013(3) -0.002(3) C24 0.038(3) 0.054(4) 0.043(4) 0.001(3) -0.001(3) 0.015(3) C25 0.095(5) 0.039(3) 0.029(3) 0.006(3) 0.012(3) -0.015(3) C26 0.087(5) 0.057(4) 0.017(3) 0.000(3) 0.002(3) -0.029(4) C27 0.103(5) 0.053(4) 0.052(4) 0.005(4) 0.006(4) -0.027(4) C28 0.107(6) 0.170(9) 0.059(5) -0.047(6) 0.025(5) -0.007(6) C29 0.077(5) 0.107(6) 0.069(5) -0.059(5) -0.035(4) 0.025(4) C30 0.228(10) 0.100(6) 0.027(4) 0.022(4) 0.012(5) -0.055(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O5 2.008(3) . ? Ni1 O8 2.039(3) . ? Ni1 O3 2.043(3) . ? Ni1 O4 2.056(3) . ? Ni1 O6 2.130(3) . ? Ni1 O2 2.278(3) . ? Cr1 O6 1.930(3) . ? Cr1 O2 1.937(3) . ? Cr1 O7 1.944(3) . ? Cr1 O1 1.979(3) . ? Cr1 N2 1.997(4) . ? Cr1 N1 1.999(4) . ? O1 C15 1.277(5) . ? O2 C2 1.331(5) . ? O3 C15 1.254(5) . ? O4 C14 1.291(5) . ? O6 C4 1.347(5) . ? O7 C19 1.272(5) . ? O9 C19 1.224(5) . ? O10 C14 1.242(5) . ? C1 C5 1.498(7) . ? C2 C12 1.408(6) . ? C2 C3 1.433(6) . ? C3 C10 1.409(6) . ? C3 C18 1.449(6) . ? C4 C9 1.394(6) . ? C4 C7 1.413(6) . ? N1 C18 1.279(6) . ? N1 C23 1.486(6) . ? C5 C25 1.526(7) . ? C5 C15 1.530(6) . ? C5 C27 1.563(7) . ? N2 C17 1.274(6) . ? N2 C13 1.490(6) . ? C6 C20 1.512(7) . ? C7 C21 1.413(6) . ? C7 C17 1.445(7) . ? C31 C26 1.491(7) . ? C8 C9 1.381(6) . ? C8 C22 1.384(7) . ? C10 C24 1.373(7) . ? C11 C12 1.384(6) . ? C11 C24 1.386(7) . ? C13 C23 1.514(7) . ? C14 C20 1.537(6) . ? C16 C20 1.560(7) . ? C19 C26 1.515(6) . ? C20 C29 1.497(7) . ? C21 C22 1.376(7) . ? C26 C30 1.490(8) . ? C26 C28 1.629(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Ni1 O8 92.34(14) . . ? O5 Ni1 O3 177.19(14) . . ? O8 Ni1 O3 90.47(13) . . ? O5 Ni1 O4 91.33(13) . . ? O8 Ni1 O4 88.54(13) . . ? O3 Ni1 O4 88.60(12) . . ? O5 Ni1 O6 89.45(12) . . ? O8 Ni1 O6 92.39(12) . . ? O3 Ni1 O6 90.58(12) . . ? O4 Ni1 O6 178.75(12) . . ? O5 Ni1 O2 90.98(12) . . ? O8 Ni1 O2 169.18(12) . . ? O3 Ni1 O2 86.28(12) . . ? O4 Ni1 O2 101.67(11) . . ? O6 Ni1 O2 77.34(11) . . ? O6 Cr1 O2 90.97(13) . . ? O6 Cr1 O7 94.52(13) . . ? O2 Cr1 O7 94.82(13) . . ? O6 Cr1 O1 91.44(13) . . ? O2 Cr1 O1 89.81(13) . . ? O7 Cr1 O1 172.39(13) . . ? O6 Cr1 N2 91.59(15) . . ? O2 Cr1 N2 176.47(15) . . ? O7 Cr1 N2 87.41(15) . . ? O1 Cr1 N2 87.69(14) . . ? O6 Cr1 N1 173.65(15) . . ? O2 Cr1 N1 94.62(15) . . ? O7 Cr1 N1 88.04(15) . . ? O1 Cr1 N1 85.56(14) . . ? N2 Cr1 N1 82.71(17) . . ? C15 O1 Cr1 129.5(3) . . ? C2 O2 Cr1 124.5(3) . . ? C2 O2 Ni1 132.7(3) . . ? Cr1 O2 Ni1 91.25(12) . . ? C15 O3 Ni1 127.5(3) . . ? C14 O4 Ni1 127.9(3) . . ? C4 O6 Cr1 123.5(3) . . ? C4 O6 Ni1 138.7(3) . . ? Cr1 O6 Ni1 96.11(13) . . ? C19 O7 Cr1 137.0(3) . . ? O2 C2 C12 118.8(4) . . ? O2 C2 C3 124.9(4) . . ? C12 C2 C3 116.3(4) . . ? C10 C3 C2 119.3(5) . . ? C10 C3 C18 116.4(5) . . ? C2 C3 C18 124.3(5) . . ? O6 C4 C9 119.3(4) . . ? O6 C4 C7 122.4(4) . . ? C9 C4 C7 118.3(5) . . ? C18 N1 C23 123.0(4) . . ? C18 N1 Cr1 123.6(3) . . ? C23 N1 Cr1 113.1(3) . . ? C1 C5 C25 112.2(5) . . ? C1 C5 C15 106.6(4) . . ? C25 C5 C15 112.1(4) . . ? C1 C5 C27 108.6(5) . . ? C25 C5 C27 107.6(5) . . ? C15 C5 C27 109.7(4) . . ? C17 N2 C13 122.9(4) . . ? C17 N2 Cr1 124.8(4) . . ? C13 N2 Cr1 112.1(3) . . ? C4 C7 C21 118.8(5) . . ? C4 C7 C17 124.9(5) . . ? C21 C7 C17 116.3(5) . . ? C9 C8 C22 120.8(5) . . ? C8 C9 C4 121.5(5) . . ? C24 C10 C3 122.2(5) . . ? C12 C11 C24 120.1(5) . . ? C11 C12 C2 122.9(5) . . ? N2 C13 C23 108.0(4) . . ? O10 C14 O4 124.5(4) . . ? O10 C14 C20 119.1(5) . . ? O4 C14 C20 116.4(5) . . ? O3 C15 O1 124.7(4) . . ? O3 C15 C5 120.2(4) . . ? O1 C15 C5 115.1(4) . . ? N2 C17 C7 124.3(5) . . ? N1 C18 C3 125.9(5) . . ? O9 C19 O7 127.3(5) . . ? O9 C19 C26 119.0(4) . . ? O7 C19 C26 113.7(4) . . ? C29 C20 C6 113.7(5) . . ? C29 C20 C14 108.3(4) . . ? C6 C20 C14 109.2(4) . . ? C29 C20 C16 108.3(5) . . ? C6 C20 C16 107.4(5) . . ? C14 C20 C16 109.9(5) . . ? C22 C21 C7 121.7(5) . . ? C21 C22 C8 118.9(5) . . ? N1 C23 C13 107.4(4) . . ? C10 C24 C11 119.0(5) . . ? C30 C26 C31 118.9(6) . . ? C30 C26 C19 112.6(5) . . ? C31 C26 C19 111.2(5) . . ? C30 C26 C28 105.0(6) . . ? C31 C26 C28 102.9(5) . . ? C19 C26 C28 104.6(5) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 28.56 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.783 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.090 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 720442' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H45 Co Cr N2 O10' _chemical_formula_weight 716.62 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.4198(4) _cell_length_b 17.6220(4) _cell_length_c 23.3583(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7170.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3008 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7294 _exptl_absorpt_correction_T_max 0.9281 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 123131 _diffrn_reflns_av_R_equivalents 0.1317 _diffrn_reflns_av_sigmaI/netI 0.0796 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.65 _reflns_number_total 8897 _reflns_number_gt 4985 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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. ; _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^)+(0.1075P)^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 8897 _refine_ls_number_parameters 410 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1579 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.47381(3) 0.02735(3) 0.10003(2) 0.02434(15) Uani 1 1 d . . . Cr1 Cr 0.51994(4) 0.14616(3) 0.18889(2) 0.02475(16) Uani 1 1 d . . . O1 O 0.56566(15) 0.05442(14) 0.15928(10) 0.0267(6) Uani 1 1 d . . . O2 O 0.38367(15) 0.00168(15) 0.04331(11) 0.0298(6) Uani 1 1 d . . . O3 O 0.54082(15) 0.20161(14) 0.11628(11) 0.0296(6) Uani 1 1 d . . . O4 O 0.4551(2) -0.01332(17) 0.25986(12) 0.0433(8) Uani 1 1 d . . . O5 O 0.50408(15) 0.11828(14) 0.04908(11) 0.0277(6) Uani 1 1 d . . . O6 O 0.50376(16) 0.10444(15) 0.26506(11) 0.0331(7) Uani 1 1 d . . . C1 C 0.3614(2) 0.1662(2) 0.15231(15) 0.0272(8) Uani 1 1 d . . . O7 O 0.41975(14) 0.11797(14) 0.15970(11) 0.0264(6) Uani 1 1 d . . . O8 O 0.43724(17) -0.05527(15) 0.15340(11) 0.0309(6) Uani 1 1 d D . . O9 O 0.30507(17) -0.06188(17) 0.10087(12) 0.0415(7) Uani 1 1 d . . . C2 C 0.6270(2) 0.0208(2) 0.18232(15) 0.0259(8) Uani 1 1 d . . . O10 O 0.54237(17) -0.04457(16) 0.05122(12) 0.0299(6) Uani 1 1 d D . . N1 N 0.6222(2) 0.18396(18) 0.21714(13) 0.0315(8) Uani 1 1 d . . . N2 N 0.4840(2) 0.24701(18) 0.21909(14) 0.0331(8) Uani 1 1 d . . . C3 C 0.3204(2) -0.0334(2) 0.05377(17) 0.0319(9) Uani 1 1 d . B . C4 C 0.6829(2) 0.0611(2) 0.21445(17) 0.0321(9) Uani 1 1 d . . . C5 C 0.3604(2) 0.2424(2) 0.17205(17) 0.0320(9) Uani 1 1 d . . . C6 C 0.4791(2) 0.0424(2) 0.28615(16) 0.0314(9) Uani 1 1 d . A . C7 C 0.2954(2) 0.1394(2) 0.12431(18) 0.0363(10) Uani 1 1 d . . . H7 H 0.2936 0.0889 0.1128 0.044 Uiso 1 1 calc R . . C8 C 0.5320(3) 0.2468(2) 0.02074(18) 0.0402(11) Uani 1 1 d . . . C9 C 0.7472(3) 0.0215(3) 0.2355(2) 0.0436(11) Uani 1 1 d . . . H9 H 0.7842 0.0478 0.2562 0.052 Uiso 1 1 calc R . . C10 C 0.2613(2) -0.0370(3) 0.00507(19) 0.0413(11) Uani 1 1 d D . . C11 C 0.5261(2) 0.1830(2) 0.06492(16) 0.0268(8) Uani 1 1 d . . . C12 C 0.2960(3) 0.2881(2) 0.15943(18) 0.0398(10) Uani 1 1 d . . . H12 H 0.2960 0.3383 0.1716 0.048 Uiso 1 1 calc R . . C13 C 0.2334(3) 0.1854(3) 0.1134(2) 0.0443(11) Uani 1 1 d . . . H13 H 0.1906 0.1659 0.0947 0.053 Uiso 1 1 calc R . . C14 C 0.2345(3) 0.2618(3) 0.1305(2) 0.0462(11) Uani 1 1 d . . . H14 H 0.1935 0.2937 0.1219 0.055 Uiso 1 1 calc R . . C15 C 0.7570(3) -0.0546(3) 0.2262(2) 0.0489(12) Uani 1 1 d . . . H15 H 0.8003 -0.0798 0.2399 0.059 Uiso 1 1 calc R . . C16 C 0.6216(3) 0.2655(2) 0.22991(19) 0.0406(11) Uani 1 1 d . . . H16A H 0.6308 0.2945 0.1953 0.049 Uiso 1 1 calc R . . H16B H 0.6615 0.2776 0.2574 0.049 Uiso 1 1 calc R . . C17 C 0.6378(2) -0.0575(2) 0.17395(17) 0.0334(9) Uani 1 1 d . . . H17 H 0.6018 -0.0851 0.1532 0.040 Uiso 1 1 calc R . . C18 C 0.7007(3) -0.0933(3) 0.1960(2) 0.0450(11) Uani 1 1 d . . . H18 H 0.7060 -0.1454 0.1906 0.054 Uiso 1 1 calc R . . C19 C 0.4204(2) 0.2774(2) 0.20622(18) 0.0355(10) Uani 1 1 d . . . H19 H 0.4114 0.3262 0.2198 0.043 Uiso 1 1 calc R . . C22 C 0.5421(3) 0.2849(2) 0.2547(2) 0.0446(11) Uani 1 1 d . . . H22A H 0.5384 0.2674 0.2940 0.054 Uiso 1 1 calc R . . H22B H 0.5341 0.3394 0.2542 0.054 Uiso 1 1 calc R . . C24 C 0.6799(2) 0.1409(2) 0.22699(17) 0.0366(10) Uani 1 1 d . . . H24 H 0.7230 0.1629 0.2435 0.044 Uiso 1 1 calc R . . C25 C 0.4803(3) 0.0402(3) 0.3517(2) 0.0657(18) Uani 1 1 d D . . C26 C 0.6039(4) 0.2982(3) 0.0356(2) 0.0703(17) Uani 1 1 d . . . H26A H 0.6500 0.2690 0.0315 0.105 Uiso 1 1 calc R . . H26B H 0.5996 0.3161 0.0742 0.105 Uiso 1 1 calc R . . H26C H 0.6054 0.3408 0.0099 0.105 Uiso 1 1 calc R . . C27 C 0.5440(3) 0.2170(3) -0.03937(18) 0.0518(13) Uani 1 1 d . . . H27A H 0.5906 0.1880 -0.0408 0.078 Uiso 1 1 calc R . . H27B H 0.5474 0.2588 -0.0656 0.078 Uiso 1 1 calc R . . H27C H 0.5015 0.1852 -0.0499 0.078 Uiso 1 1 calc R . . C28 C 0.4616(4) 0.2929(4) 0.0265(3) 0.090(2) Uani 1 1 d . . . H28A H 0.4571 0.3106 0.0653 0.135 Uiso 1 1 calc R . . H28B H 0.4177 0.2625 0.0170 0.135 Uiso 1 1 calc R . . H28C H 0.4644 0.3356 0.0011 0.135 Uiso 1 1 calc R . . C20A C 0.4169(5) 0.1018(5) 0.3694(4) 0.075(2) Uiso 0.686(7) 1 d PD A 1 H20A H 0.3674 0.0855 0.3561 0.113 Uiso 0.686(7) 1 calc PR A 1 H20B H 0.4294 0.1498 0.3524 0.113 Uiso 0.686(7) 1 calc PR A 1 H20C H 0.4158 0.1068 0.4103 0.113 Uiso 0.686(7) 1 calc PR A 1 C23A C 0.4553(6) -0.0356(5) 0.3744(4) 0.069(2) Uiso 0.686(7) 1 d PD A 1 H23A H 0.4071 -0.0494 0.3574 0.103 Uiso 0.686(7) 1 calc PR A 1 H23B H 0.4495 -0.0326 0.4152 0.103 Uiso 0.686(7) 1 calc PR A 1 H23C H 0.4932 -0.0732 0.3651 0.103 Uiso 0.686(7) 1 calc PR A 1 C30A C 0.5548(5) 0.0707(5) 0.3744(4) 0.060(2) Uiso 0.686(7) 1 d PD A 1 H30A H 0.5651 0.1192 0.3572 0.089 Uiso 0.686(7) 1 calc PR A 1 H30B H 0.5956 0.0361 0.3653 0.089 Uiso 0.686(7) 1 calc PR A 1 H30C H 0.5513 0.0765 0.4152 0.089 Uiso 0.686(7) 1 calc PR A 1 C20B C 0.5352(11) -0.0345(9) 0.3580(9) 0.075(2) Uiso 0.314(7) 1 d PD A 2 H20D H 0.5087 -0.0782 0.3435 0.113 Uiso 0.314(7) 1 calc PR A 2 H20E H 0.5476 -0.0422 0.3976 0.113 Uiso 0.314(7) 1 calc PR A 2 H20F H 0.5816 -0.0269 0.3366 0.113 Uiso 0.314(7) 1 calc PR A 2 C23B C 0.4163(10) -0.0093(11) 0.3772(8) 0.069(2) Uiso 0.314(7) 1 d PD A 2 H23D H 0.3911 -0.0367 0.3470 0.103 Uiso 0.314(7) 1 calc PR A 2 H23E H 0.3797 0.0224 0.3964 0.103 Uiso 0.314(7) 1 calc PR A 2 H23F H 0.4380 -0.0446 0.4040 0.103 Uiso 0.314(7) 1 calc PR A 2 C30B C 0.5318(10) 0.0974(10) 0.3782(8) 0.060(2) Uiso 0.314(7) 1 d PD A 2 H30D H 0.5292 0.0929 0.4192 0.089 Uiso 0.314(7) 1 calc PR A 2 H30E H 0.5159 0.1473 0.3670 0.089 Uiso 0.314(7) 1 calc PR A 2 H30F H 0.5836 0.0887 0.3658 0.089 Uiso 0.314(7) 1 calc PR A 2 C21A C 0.1826(5) -0.0485(6) 0.0297(4) 0.065(2) Uiso 0.657(10) 1 d PD B 1 H21A H 0.1712 -0.0080 0.0559 0.097 Uiso 0.657(10) 1 calc PR B 1 H21B H 0.1808 -0.0961 0.0496 0.097 Uiso 0.657(10) 1 calc PR B 1 H21C H 0.1454 -0.0486 -0.0007 0.097 Uiso 0.657(10) 1 calc PR B 1 C29A C 0.2881(5) -0.0936(5) -0.0388(4) 0.0518(18) Uiso 0.657(10) 1 d PD B 1 H29A H 0.2513 -0.0964 -0.0693 0.078 Uiso 0.657(10) 1 calc PR B 1 H29B H 0.2932 -0.1426 -0.0212 0.078 Uiso 0.657(10) 1 calc PR B 1 H29C H 0.3368 -0.0779 -0.0539 0.078 Uiso 0.657(10) 1 calc PR B 1 C31A C 0.2595(6) 0.0426(5) -0.0267(4) 0.065(2) Uiso 0.657(10) 1 d PD B 1 H31A H 0.2430 0.0812 -0.0005 0.097 Uiso 0.657(10) 1 calc PR B 1 H31B H 0.2245 0.0402 -0.0584 0.097 Uiso 0.657(10) 1 calc PR B 1 H31C H 0.3100 0.0545 -0.0405 0.097 Uiso 0.657(10) 1 calc PR B 1 C21B C 0.1979(9) -0.0937(11) 0.0226(7) 0.065(2) Uiso 0.343(10) 1 d PD B 2 H21D H 0.1727 -0.0758 0.0565 0.097 Uiso 0.343(10) 1 calc PR B 2 H21E H 0.2206 -0.1424 0.0301 0.097 Uiso 0.343(10) 1 calc PR B 2 H21F H 0.1612 -0.0983 -0.0078 0.097 Uiso 0.343(10) 1 calc PR B 2 C29B C 0.2962(9) -0.0644(11) -0.0511(6) 0.0518(18) Uiso 0.343(10) 1 d PD B 2 H29D H 0.2572 -0.0659 -0.0801 0.078 Uiso 0.343(10) 1 calc PR B 2 H29E H 0.3172 -0.1143 -0.0459 0.078 Uiso 0.343(10) 1 calc PR B 2 H29F H 0.3363 -0.0303 -0.0627 0.078 Uiso 0.343(10) 1 calc PR B 2 C31B C 0.2354(12) 0.0401(8) -0.0103(9) 0.065(2) Uiso 0.343(10) 1 d PD B 2 H31D H 0.2132 0.0641 0.0227 0.097 Uiso 0.343(10) 1 calc PR B 2 H31E H 0.1977 0.0370 -0.0402 0.097 Uiso 0.343(10) 1 calc PR B 2 H31F H 0.2784 0.0693 -0.0234 0.097 Uiso 0.343(10) 1 calc PR B 2 H1W H 0.431(3) -0.043(3) 0.1876(10) 0.078 Uiso 1 1 d D . . H2W H 0.3913(14) -0.061(3) 0.142(2) 0.078 Uiso 1 1 d D . . H3W H 0.563(3) -0.017(3) 0.026(2) 0.09(2) Uiso 1 1 d D . . H4W H 0.513(3) -0.075(3) 0.033(2) 0.065(18) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0328(3) 0.0202(3) 0.0200(2) -0.00028(19) -0.0015(2) -0.0014(2) Cr1 0.0339(3) 0.0186(3) 0.0217(3) -0.0021(2) -0.0026(3) -0.0014(3) O1 0.0320(14) 0.0229(13) 0.0251(13) -0.0008(10) -0.0034(11) 0.0007(11) O2 0.0304(15) 0.0311(15) 0.0279(14) -0.0010(11) -0.0003(11) -0.0015(12) O3 0.0409(16) 0.0229(14) 0.0249(13) 0.0006(11) -0.0006(11) -0.0023(12) O4 0.066(2) 0.0352(17) 0.0281(15) -0.0025(13) 0.0008(14) -0.0165(15) O5 0.0370(15) 0.0224(14) 0.0237(13) -0.0003(11) 0.0001(11) -0.0018(12) O6 0.0493(17) 0.0272(15) 0.0227(13) -0.0012(11) 0.0002(12) -0.0064(13) C1 0.031(2) 0.026(2) 0.0249(18) 0.0008(15) 0.0041(16) 0.0033(16) O7 0.0306(14) 0.0187(13) 0.0298(13) -0.0022(10) -0.0003(11) 0.0022(11) O8 0.0448(17) 0.0243(14) 0.0234(13) -0.0005(11) -0.0015(13) -0.0045(13) O9 0.0461(18) 0.0441(18) 0.0344(16) 0.0066(14) -0.0036(14) -0.0157(15) C2 0.030(2) 0.027(2) 0.0208(17) 0.0052(15) 0.0012(15) 0.0017(16) O10 0.0362(16) 0.0288(16) 0.0248(14) -0.0014(12) -0.0001(12) 0.0007(12) N1 0.042(2) 0.0238(17) 0.0283(17) 0.0008(13) -0.0066(15) -0.0050(15) N2 0.047(2) 0.0200(16) 0.0326(18) -0.0063(13) -0.0024(16) -0.0039(16) C3 0.033(2) 0.027(2) 0.036(2) -0.0087(17) -0.0009(18) 0.0022(18) C4 0.033(2) 0.034(2) 0.029(2) 0.0034(17) -0.0027(17) -0.0015(18) C5 0.040(2) 0.023(2) 0.033(2) -0.0006(16) 0.0087(18) 0.0023(18) C6 0.038(2) 0.033(2) 0.0233(19) 0.0005(16) 0.0010(17) -0.0018(19) C7 0.039(2) 0.030(2) 0.040(2) -0.0067(18) -0.0011(19) 0.0059(19) C8 0.066(3) 0.024(2) 0.031(2) 0.0067(17) 0.007(2) 0.005(2) C9 0.035(2) 0.047(3) 0.049(3) 0.002(2) -0.012(2) 0.001(2) C10 0.029(2) 0.057(3) 0.038(2) -0.009(2) -0.0080(18) 0.001(2) C11 0.031(2) 0.024(2) 0.0251(18) 0.0004(15) 0.0014(16) 0.0017(17) C12 0.048(3) 0.029(2) 0.043(2) -0.0015(19) 0.006(2) 0.008(2) C13 0.039(2) 0.047(3) 0.047(3) -0.006(2) -0.005(2) 0.011(2) C14 0.048(3) 0.041(3) 0.050(3) 0.000(2) 0.002(2) 0.016(2) C15 0.042(3) 0.044(3) 0.061(3) 0.007(2) -0.013(2) 0.010(2) C16 0.051(3) 0.026(2) 0.045(3) -0.0022(18) -0.015(2) -0.010(2) C17 0.038(2) 0.027(2) 0.035(2) 0.0038(17) -0.0013(18) 0.0019(18) C18 0.047(3) 0.028(2) 0.060(3) 0.005(2) -0.002(2) 0.007(2) C19 0.044(3) 0.022(2) 0.041(2) -0.0083(17) 0.005(2) 0.0044(18) C22 0.062(3) 0.026(2) 0.046(3) -0.015(2) -0.013(2) 0.000(2) C24 0.038(2) 0.037(2) 0.035(2) 0.0047(18) -0.0100(18) -0.009(2) C25 0.099(5) 0.072(4) 0.025(2) 0.001(2) 0.002(3) -0.046(3) C26 0.097(5) 0.049(3) 0.065(4) 0.007(3) 0.002(3) -0.028(3) C27 0.089(4) 0.034(3) 0.032(2) 0.0062(19) 0.007(2) -0.006(3) C28 0.111(6) 0.085(5) 0.074(4) 0.047(4) 0.029(4) 0.058(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 Co1 O8 2.020(3) . ? Co1 O5 2.064(3) . ? Co1 O10 2.081(3) . ? Co1 O2 2.104(3) . ? Co1 O1 2.169(3) . ? Co1 O7 2.319(2) . ? Cr1 O1 1.930(3) . ? Cr1 O7 1.938(3) . ? Cr1 O6 1.946(3) . ? Cr1 O3 1.991(3) . ? Cr1 N2 2.012(3) . ? Cr1 N1 2.013(3) . ? O1 C2 1.335(4) . ? O2 C3 1.287(5) . ? O3 C11 1.270(4) . ? O4 C6 1.230(5) . ? O5 C11 1.259(5) . ? O6 C6 1.275(5) . ? C1 O7 1.336(4) . ? C1 C7 1.405(6) . ? C1 C5 1.420(5) . ? O9 C3 1.238(5) . ? C2 C17 1.406(5) . ? C2 C4 1.420(5) . ? N1 C24 1.279(5) . ? N1 C16 1.467(5) . ? N2 C19 1.266(5) . ? N2 C22 1.471(5) . ? C3 C10 1.536(6) . ? C4 C9 1.409(6) . ? C4 C24 1.438(6) . ? C5 C12 1.411(6) . ? C5 C19 1.453(6) . ? C6 C25 1.531(6) . ? C7 C13 1.374(6) . ? C8 C28 1.477(7) . ? C8 C27 1.514(6) . ? C8 C11 1.530(5) . ? C8 C26 1.583(7) . ? C9 C15 1.369(6) . ? C10 C31B 1.475(14) . ? C10 C21A 1.500(9) . ? C10 C29A 1.504(8) . ? C10 C29B 1.525(12) . ? C10 C21B 1.545(13) . ? C10 C31A 1.587(9) . ? C12 C14 1.349(6) . ? C13 C14 1.404(6) . ? C15 C18 1.387(7) . ? C16 C22 1.540(6) . ? C17 C18 1.366(6) . ? C25 C30B 1.485(13) . ? C25 C23A 1.502(8) . ? C25 C30A 1.502(8) . ? C25 C23B 1.536(13) . ? C25 C20A 1.604(9) . ? C25 C20B 1.634(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 O8 Co1 O5 174.78(11) . . ? O8 Co1 O10 94.59(12) . . ? O5 Co1 O10 90.59(11) . . ? O8 Co1 O2 89.90(11) . . ? O5 Co1 O2 89.69(10) . . ? O10 Co1 O2 87.27(11) . . ? O8 Co1 O1 89.85(10) . . ? O5 Co1 O1 90.49(10) . . ? O10 Co1 O1 93.45(10) . . ? O2 Co1 O1 179.26(10) . . ? O8 Co1 O7 89.85(10) . . ? O5 Co1 O7 85.17(9) . . ? O10 Co1 O7 168.91(11) . . ? O2 Co1 O7 102.92(10) . . ? O1 Co1 O7 76.38(9) . . ? O1 Cr1 O7 91.77(11) . . ? O1 Cr1 O6 94.07(11) . . ? O7 Cr1 O6 95.41(11) . . ? O1 Cr1 O3 91.74(11) . . ? O7 Cr1 O3 89.46(11) . . ? O6 Cr1 O3 172.29(11) . . ? O1 Cr1 N2 173.60(13) . . ? O7 Cr1 N2 93.99(12) . . ? O6 Cr1 N2 88.17(13) . . ? O3 Cr1 N2 85.53(12) . . ? O1 Cr1 N1 91.68(12) . . ? O7 Cr1 N1 175.43(12) . . ? O6 Cr1 N1 87.33(12) . . ? O3 Cr1 N1 87.43(12) . . ? N2 Cr1 N1 82.43(14) . . ? C2 O1 Cr1 123.9(2) . . ? C2 O1 Co1 138.6(2) . . ? Cr1 O1 Co1 96.23(11) . . ? C3 O2 Co1 128.5(3) . . ? C11 O3 Cr1 129.9(2) . . ? C11 O5 Co1 127.7(2) . . ? C6 O6 Cr1 136.6(3) . . ? O7 C1 C7 118.0(3) . . ? O7 C1 C5 124.7(4) . . ? C7 C1 C5 117.3(4) . . ? C1 O7 Cr1 124.6(2) . . ? C1 O7 Co1 132.0(2) . . ? Cr1 O7 Co1 91.28(10) . . ? O1 C2 C17 119.1(3) . . ? O1 C2 C4 122.7(3) . . ? C17 C2 C4 118.2(4) . . ? C24 N1 C16 123.3(4) . . ? C24 N1 Cr1 123.9(3) . . ? C16 N1 Cr1 112.6(3) . . ? C19 N2 C22 123.0(3) . . ? C19 N2 Cr1 124.2(3) . . ? C22 N2 Cr1 112.7(3) . . ? O9 C3 O2 123.2(4) . . ? O9 C3 C10 119.8(4) . . ? O2 C3 C10 116.9(4) . . ? C9 C4 C2 118.8(4) . . ? C9 C4 C24 116.3(4) . . ? C2 C4 C24 124.9(4) . . ? C12 C5 C1 118.8(4) . . ? C12 C5 C19 116.5(4) . . ? C1 C5 C19 124.8(4) . . ? O4 C6 O6 127.3(4) . . ? O4 C6 C25 118.9(4) . . ? O6 C6 C25 113.8(4) . . ? C13 C7 C1 122.1(4) . . ? C28 C8 C27 112.9(4) . . ? C28 C8 C11 106.7(4) . . ? C27 C8 C11 112.3(3) . . ? C28 C8 C26 108.7(5) . . ? C27 C8 C26 107.0(4) . . ? C11 C8 C26 109.1(4) . . ? C15 C9 C4 122.0(4) . . ? C31B C10 C21A 86.4(9) . . ? C31B C10 C29A 122.7(9) . . ? C21A C10 C29A 117.1(6) . . ? C31B C10 C29B 101.8(10) . . ? C21A C10 C29B 130.7(8) . . ? C29A C10 C29B 23.1(7) . . ? C31B C10 C3 110.4(8) . . ? C21A C10 C3 109.5(5) . . ? C29A C10 C3 108.9(5) . . ? C29B C10 C3 112.5(7) . . ? C31B C10 C21B 116.2(11) . . ? C21A C10 C21B 32.7(7) . . ? C29A C10 C21B 88.5(8) . . ? C29B C10 C21B 108.0(10) . . ? C3 C10 C21B 108.0(7) . . ? C31B C10 C31A 21.1(9) . . ? C21A C10 C31A 106.3(6) . . ? C29A C10 C31A 105.9(5) . . ? C29B C10 C31A 83.4(8) . . ? C3 C10 C31A 108.9(5) . . ? C21B C10 C31A 133.0(8) . . ? O5 C11 O3 125.0(3) . . ? O5 C11 C8 119.2(3) . . ? O3 C11 C8 115.7(3) . . ? C14 C12 C5 122.7(4) . . ? C7 C13 C14 120.2(4) . . ? C12 C14 C13 118.8(4) . . ? C9 C15 C18 118.3(4) . . ? N1 C16 C22 107.5(3) . . ? C18 C17 C2 120.6(4) . . ? C17 C18 C15 122.1(4) . . ? N2 C19 C5 125.5(4) . . ? N2 C22 C16 107.8(3) . . ? N1 C24 C4 124.9(4) . . ? C30B C25 C23A 129.1(10) . . ? C30B C25 C30A 24.1(8) . . ? C23A C25 C30A 116.4(6) . . ? C30B C25 C6 114.2(8) . . ? C23A C25 C6 111.8(5) . . ? C30A C25 C6 110.9(5) . . ? C30B C25 C23B 131.4(11) . . ? C23A C25 C23B 31.5(8) . . ? C30A C25 C23B 134.0(9) . . ? C6 C25 C23B 113.0(8) . . ? C30B C25 C20A 81.3(9) . . ? C23A C25 C20A 108.1(6) . . ? C30A C25 C20A 105.1(6) . . ? C6 C25 C20A 103.4(5) . . ? C23B C25 C20A 77.5(9) . . ? C30B C25 C20B 98.9(12) . . ? C23A C25 C20B 54.7(8) . . ? C30A C25 C20B 75.6(9) . . ? C6 C25 C20B 96.9(8) . . ? C23B C25 C20B 86.2(11) . . ? C20A C25 C20B 157.7(9) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 28.65 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.132 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.098