# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2098 data_global _publ_contact_author_name 'Lee Brammer' _publ_contact_author_address ; Department of Chemistry University of Missouri-St.Louis 8001 Natural Bridge Road St. Louis, MO 63121-4499 USA ; _publ_contact_author_phone '+1-314-516-5345' _publ_contact_author_fax '+1-314-516-5342' _publ_contact_author_email 'lee.brammer@umsl.edu' #Data for compound 1 data_lee598sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H24 Cl2 N8 O4 Pt' _chemical_formula_weight 754.50 _chemical_melting_point ? _chemical_compound_source 'synthesis' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1500(1) _cell_length_b 8.7935(1) _cell_length_c 10.0075(1) _cell_angle_alpha 85.985(1) _cell_angle_beta 89.699(1) _cell_angle_gamma 70.680(1) _cell_volume 675.05(1) _cell_formula_units_Z 1 _cell_measurement_temperature 213(5) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 29.80 _exptl_crystal_description 'triangular prism' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.856 _exptl_crystal_density_method ? _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 5.442 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Absorption correction was based upon symmetry equivalentand repeated intensity measurements using the program SADABS (Sheldrick, 1995) which is based upon the method of Blessing (Blessing, 1995) ; _exptl_absorpt_correction_T_min 0.5092 _exptl_absorpt_correction_T_max 0.6947 _exptl_special_details ; Data were collected with a Siemens SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 10s duration at a crystal-to detector distance of 4.908 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14500 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 29.80 _reflns_number_total 3550 _reflns_number_observed 3342 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SMART (Siemens, 1994)' _computing_data_reduction 'SMART (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement 'SHELXTL (Siemens, 1994)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Arene hydrogens were placed in calculated positions and refined using a riding model. Amide hydrogens were located directly from the difference map and refined without positional constraints, but with a fixed isotropic displacement parameter. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^] 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 3550 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0455 _refine_ls_R_factor_obs 0.0390 _refine_ls_wR_factor_all 0.0833 _refine_ls_wR_factor_obs 0.0796 _refine_ls_goodness_of_fit_all 0.979 _refine_ls_goodness_of_fit_obs 0.965 _refine_ls_restrained_S_all 0.979 _refine_ls_restrained_S_obs 0.965 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.0000 0.0000 0.0000 0.02213(9) Uani 1 d S . Cl1 Cl 0.46431(14) -0.1989(2) 0.09957(13) 0.0344(3) Uani 1 d . . N1 N 0.0398(4) 0.0791(4) -0.1886(4) 0.0207(7) Uani 1 d . . C2 C -0.0955(5) 0.1265(5) -0.2752(4) 0.0231(9) Uani 1 d . . H2 H -0.2025(5) 0.1183(5) -0.2466(4) 0.028 Uiso 1 calc R . C3 C -0.0839(6) 0.1871(5) -0.4054(5) 0.0255(9) Uani 1 d . . C4 C 0.0772(6) 0.1926(6) -0.4477(5) 0.0322(10) Uani 1 d . . H4 H 0.0912(6) 0.2297(6) -0.5360(5) 0.039 Uiso 1 calc R . C5 C 0.2169(6) 0.1424(6) -0.3578(5) 0.0338(11) Uani 1 d . . H5 H 0.3261(6) 0.1465(6) -0.3845(5) 0.041 Uiso 1 calc R . C6 C 0.1947(6) 0.0863(5) -0.2288(5) 0.0265(9) Uani 1 d . . H6 H 0.2897(6) 0.0526(5) -0.1682(5) 0.032 Uiso 1 calc R . C7 C -0.2388(6) 0.2440(6) -0.4993(5) 0.0294(10) Uani 1 d . . O1 O -0.2168(5) 0.2519(5) -0.6205(4) 0.0435(9) Uani 1 d . . N2 N -0.3943(6) 0.2799(6) -0.4432(5) 0.0363(10) Uani 1 d . . H2N H -0.4767(85) 0.3121(74) -0.4951(65) 0.044 Uiso 1 d . . H1N H -0.4036(82) 0.2767(73) -0.3562(68) 0.044 Uiso 1 d . . N11 N 0.0110(4) 0.2063(4) 0.0705(4) 0.0197(7) Uani 1 d . . C12 C 0.1601(5) 0.2110(5) 0.1267(4) 0.0227(8) Uani 1 d . . H12 H 0.2633(5) 0.1233(5) 0.1204(4) 0.027 Uiso 1 calc R . C13 C 0.1626(5) 0.3428(5) 0.1932(4) 0.0223(8) Uani 1 d . . C14 C 0.0102(6) 0.4719(5) 0.2015(5) 0.0276(9) Uani 1 d . . H14 H 0.0086(6) 0.5604(5) 0.2496(5) 0.033 Uiso 1 calc R . C15 C -0.1399(6) 0.4699(5) 0.1385(5) 0.0268(9) Uani 1 d . . H15 H -0.2430(6) 0.5587(5) 0.1400(5) 0.032 Uiso 1 calc R . C16 C -0.1355(5) 0.3352(5) 0.0735(4) 0.0243(9) Uani 1 d . . H16 H -0.2370(5) 0.3333(5) 0.0305(4) 0.029 Uiso 1 calc R . C17 C 0.3231(6) 0.3421(5) 0.2679(5) 0.0259(9) Uani 1 d . . O11 O 0.3040(5) 0.3972(5) 0.3794(4) 0.0384(8) Uani 1 d . . N12 N 0.4745(6) 0.2806(6) 0.2108(5) 0.0371(10) Uani 1 d . . H3N H 0.4797(83) 0.2638(74) 0.1324(67) 0.045 Uiso 1 d . . H4N H 0.5669(85) 0.2830(72) 0.2515(63) 0.045 Uiso 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 Pt1 0.01778(12) 0.02784(14) 0.02200(15) -0.00151(9) -0.00212(9) -0.00922(9) Cl1 0.0206(5) 0.0445(6) 0.0347(7) -0.0068(5) 0.0019(5) -0.0054(5) N1 0.019(2) 0.026(2) 0.018(2) -0.0025(14) 0.0000(14) -0.0091(14) C2 0.016(2) 0.031(2) 0.024(2) -0.002(2) -0.004(2) -0.011(2) C3 0.026(2) 0.029(2) 0.024(2) -0.004(2) -0.003(2) -0.013(2) C4 0.032(2) 0.044(3) 0.026(3) 0.000(2) 0.004(2) -0.020(2) C5 0.025(2) 0.043(3) 0.035(3) 0.000(2) 0.004(2) -0.015(2) C6 0.018(2) 0.032(2) 0.031(3) -0.003(2) 0.001(2) -0.010(2) C7 0.033(2) 0.033(2) 0.028(3) 0.003(2) -0.008(2) -0.019(2) O1 0.041(2) 0.077(3) 0.019(2) 0.007(2) -0.008(2) -0.030(2) N2 0.027(2) 0.056(3) 0.024(2) 0.003(2) -0.009(2) -0.013(2) N11 0.019(2) 0.022(2) 0.018(2) -0.0011(13) -0.0005(14) -0.0075(13) C12 0.019(2) 0.028(2) 0.020(2) 0.002(2) -0.004(2) -0.007(2) C13 0.021(2) 0.026(2) 0.022(2) 0.001(2) -0.002(2) -0.010(2) C14 0.031(2) 0.022(2) 0.029(3) -0.003(2) -0.003(2) -0.007(2) C15 0.019(2) 0.028(2) 0.030(3) -0.002(2) 0.000(2) -0.003(2) C16 0.018(2) 0.033(2) 0.022(2) 0.002(2) -0.002(2) -0.010(2) C17 0.022(2) 0.028(2) 0.030(3) 0.000(2) -0.004(2) -0.011(2) O11 0.032(2) 0.051(2) 0.034(2) -0.014(2) -0.006(2) -0.013(2) N12 0.025(2) 0.061(3) 0.029(2) -0.012(2) -0.001(2) -0.017(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 Pt1 N11 2.021(3) . ? Pt1 N11 2.021(3) 2 ? Pt1 N1 2.027(4) 2 ? Pt1 N1 2.027(4) . ? N1 C6 1.343(5) . ? N1 C2 1.341(5) . ? C2 C3 1.387(6) . ? C3 C4 1.393(6) . ? C3 C7 1.502(6) . ? C4 C5 1.386(7) . ? C5 C6 1.382(7) . ? C7 O1 1.225(6) . ? C7 N2 1.332(7) . ? N11 C16 1.350(5) . ? N11 C12 1.356(5) . ? C12 C13 1.382(6) . ? C13 C14 1.384(6) . ? C13 C17 1.508(6) . ? C14 C15 1.385(6) . ? C15 C16 1.381(6) . ? C17 O11 1.235(6) . ? C17 N12 1.318(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Pt1 N11 180.0 . 2 ? N11 Pt1 N1 89.58(14) . 2 ? N11 Pt1 N1 90.42(14) 2 2 ? N11 Pt1 N1 90.42(14) . . ? N11 Pt1 N1 89.58(14) 2 . ? N1 Pt1 N1 180.0 2 . ? C6 N1 C2 119.4(4) . . ? C6 N1 Pt1 122.7(3) . . ? C2 N1 Pt1 117.9(3) . . ? N1 C2 C3 122.6(4) . . ? C2 C3 C4 117.9(4) . . ? C2 C3 C7 121.6(4) . . ? C4 C3 C7 120.4(4) . . ? C5 C4 C3 119.1(5) . . ? C4 C5 C6 119.7(4) . . ? N1 C6 C5 121.2(4) . . ? O1 C7 N2 123.9(5) . . ? O1 C7 C3 119.6(4) . . ? N2 C7 C3 116.4(4) . . ? C16 N11 C12 119.7(4) . . ? C16 N11 Pt1 119.5(3) . . ? C12 N11 Pt1 120.5(3) . . ? N11 C12 C13 121.0(4) . . ? C12 C13 C14 119.1(4) . . ? C12 C13 C17 121.3(4) . . ? C14 C13 C17 119.3(4) . . ? C15 C14 C13 119.7(4) . . ? C16 C15 C14 118.9(4) . . ? N11 C16 C15 121.5(4) . . ? O11 C17 N12 124.4(4) . . ? O11 C17 C13 117.8(4) . . ? N12 C17 C13 117.8(4) . . ? _refine_diff_density_max 1.449 _refine_diff_density_min -2.309 _refine_diff_density_rms 0.198 #END #Data for compound 2.H2O data_lee998sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H28 F12 N8 O6 P2 Pt' _chemical_formula_weight 1009.57 _chemical_melting_point ? _chemical_compound_source 'synthesis' 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' 'F' 'F' 0.0171 0.0103 '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.678(3) _cell_length_b 10.099(2) _cell_length_c 10.321(2) _cell_angle_alpha 69.03(2) _cell_angle_beta 65.396(15) _cell_angle_gamma 70.32(2) _cell_volume 835.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 213(5) _cell_measurement_reflns_used 3252 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 29.72 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method ? _exptl_crystal_F_000 492 _exptl_absorpt_coefficient_mu 4.416 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995) which is based upon the method of Blessing (Blessing, 1995) ; _exptl_absorpt_correction_T_min 0.4247 _exptl_absorpt_correction_T_max 0.5640 _exptl_special_details ; Data were collected with a Siemens SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 10s duration at a crystal-to detector distance of 4.900 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 213(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8747 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.1279 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 29.72 _reflns_number_total 4236 _reflns_number_observed 3182 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SMART (Siemens, 1994)' _computing_data_reduction 'SMART (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement 'SHELXTL (Siemens, 1994)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Arene and amide hydrogens were placed in calculated positions and refined using a riding model. Solvate water hydrogens were located directly from the difference map and refined without positional constraints, but with a fixed isotropic displacement parameter. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^] 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 4236 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1010 _refine_ls_R_factor_obs 0.0634 _refine_ls_wR_factor_all 0.1237 _refine_ls_wR_factor_obs 0.1039 _refine_ls_goodness_of_fit_all 1.016 _refine_ls_goodness_of_fit_obs 0.992 _refine_ls_restrained_S_all 1.016 _refine_ls_restrained_S_obs 0.992 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.0000 0.0000 0.0000 0.0300(2) Uani 1 d S . N1 N -0.0539(7) -0.1479(6) -0.0515(6) 0.0266(13) Uani 1 d . . C2 C 0.0611(8) -0.2503(7) -0.1136(7) 0.029(2) Uani 1 d . . H2 H 0.1648(8) -0.2521(7) -0.1304(7) 0.035 Uiso 1 calc R . C3 C 0.0325(8) -0.3519(7) -0.1532(7) 0.027(2) Uani 1 d . . C4 C -0.1215(10) -0.3458(9) -0.1290(8) 0.040(2) Uani 1 d . . H4 H -0.1454(10) -0.4128(9) -0.1561(8) 0.048 Uiso 1 calc R . C5 C -0.2394(9) -0.2421(9) -0.0654(8) 0.041(2) Uani 1 d . . H5 H -0.3440(9) -0.2383(9) -0.0474(8) 0.049 Uiso 1 calc R . C6 C -0.2012(9) -0.1433(8) -0.0285(8) 0.037(2) Uani 1 d . . H6 H -0.2810(9) -0.0714(8) 0.0139(8) 0.045 Uiso 1 calc R . C7 C 0.1574(10) -0.4668(8) -0.2203(8) 0.038(2) Uani 1 d . . N2 N 0.3029(8) -0.4706(7) -0.2387(7) 0.050(2) Uani 1 d . . H1N H 0.3794(8) -0.5352(7) -0.2785(7) 0.060 Uiso 1 calc R . H2N H 0.3215(8) -0.4085(7) -0.2109(7) 0.060 Uiso 1 calc R . O1 O 0.1244(7) -0.5509(6) -0.2570(6) 0.0438(14) Uani 1 d . . N11 N -0.0199(7) 0.1411(6) -0.1916(6) 0.0291(13) Uani 1 d . . C12 C -0.1370(8) 0.2595(7) -0.1919(7) 0.026(2) Uani 1 d . . H12 H -0.2102(8) 0.2766(7) -0.1015(7) 0.032 Uiso 1 calc R . C13 C -0.1527(8) 0.3570(7) -0.3217(7) 0.030(2) Uani 1 d . . C14 C -0.0459(9) 0.3292(8) -0.4532(8) 0.036(2) Uani 1 d . . H14 H -0.0543(9) 0.3937(8) -0.5429(8) 0.043 Uiso 1 calc R . C15 C 0.0737(9) 0.2062(8) -0.4530(8) 0.038(2) Uani 1 d . . H15 H 0.1463(9) 0.1856(8) -0.5421(8) 0.046 Uiso 1 calc R . C16 C 0.0845(8) 0.1154(8) -0.3218(7) 0.032(2) Uani 1 d . . H16 H 0.1666(8) 0.0326(8) -0.3214(7) 0.038 Uiso 1 calc R . C17 C -0.2842(8) 0.4885(8) -0.3076(8) 0.035(2) Uani 1 d . . O11 O -0.3593(7) 0.5111(6) -0.1855(6) 0.052(2) Uani 1 d . . N12 N -0.3131(8) 0.5752(7) -0.4301(7) 0.042(2) Uani 1 d . . H3N H -0.3886(8) 0.6523(7) -0.4256(7) 0.050 Uiso 1 calc R . H4N H -0.2565(8) 0.5546(7) -0.5144(7) 0.050 Uiso 1 calc R . P1 P 0.4168(2) 0.8759(2) 0.3604(2) 0.0415(5) Uani 1 d . . F1 F 0.3977(6) 1.0446(5) 0.3418(6) 0.071(2) Uani 1 d . . F2 F 0.4369(7) 0.7064(6) 0.3829(7) 0.084(2) Uani 1 d . . F3 F 0.4374(7) 0.9057(8) 0.1934(6) 0.097(2) Uani 1 d . . F4 F 0.5981(6) 0.8502(7) 0.3173(7) 0.078(2) Uani 1 d . . F5 F 0.4008(8) 0.8440(6) 0.5278(6) 0.087(2) Uani 1 d . . F6 F 0.2360(6) 0.9023(7) 0.4025(8) 0.094(2) Uani 1 d . . O1S O 0.4014(7) -0.2480(7) -0.1464(6) 0.049(2) Uani 1 d . . H1S H 0.4415(107) -0.1756(101) -0.2020(98) 0.059 Uiso 1 d . . H2S H 0.4836(106) -0.3200(97) -0.1579(93) 0.059 Uiso 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 Pt1 0.0323(3) 0.0255(2) 0.0308(2) -0.0104(2) -0.0119(2) 0.0003(2) N1 0.023(3) 0.030(3) 0.025(3) -0.004(2) -0.008(2) -0.006(3) C2 0.032(4) 0.029(4) 0.029(3) -0.006(3) -0.013(3) -0.007(3) C3 0.038(4) 0.023(4) 0.023(3) 0.001(3) -0.012(3) -0.015(3) C4 0.048(5) 0.042(5) 0.035(4) -0.008(3) -0.013(4) -0.017(4) C5 0.029(4) 0.047(5) 0.047(4) -0.015(4) -0.012(3) -0.007(4) C6 0.036(5) 0.039(5) 0.035(4) -0.014(3) -0.008(3) -0.006(4) C7 0.048(5) 0.035(4) 0.029(4) -0.009(3) -0.012(3) -0.008(4) N2 0.039(4) 0.044(4) 0.067(5) -0.032(4) -0.005(3) -0.007(3) O1 0.058(4) 0.036(3) 0.045(3) -0.017(3) -0.026(3) -0.001(3) N11 0.036(4) 0.024(3) 0.024(3) -0.005(2) -0.011(2) -0.004(3) C12 0.034(4) 0.018(3) 0.030(3) -0.006(3) -0.012(3) -0.007(3) C13 0.032(4) 0.023(4) 0.034(4) -0.009(3) -0.009(3) -0.005(3) C14 0.038(5) 0.037(4) 0.031(4) -0.006(3) -0.013(3) -0.008(4) C15 0.035(5) 0.040(5) 0.033(4) -0.015(3) -0.004(3) -0.004(4) C16 0.023(4) 0.032(4) 0.038(4) -0.015(3) -0.009(3) 0.002(3) C17 0.031(4) 0.034(4) 0.041(4) -0.012(3) -0.015(3) -0.003(3) O11 0.053(4) 0.048(4) 0.042(3) -0.021(3) -0.017(3) 0.016(3) N12 0.052(4) 0.030(4) 0.038(3) -0.006(3) -0.023(3) 0.005(3) P1 0.0359(13) 0.0396(13) 0.0455(12) -0.0148(10) -0.0128(10) -0.0012(10) F1 0.066(4) 0.045(3) 0.088(4) -0.013(3) -0.015(3) -0.014(3) F2 0.090(5) 0.049(3) 0.118(5) -0.045(3) -0.034(4) 0.001(3) F3 0.091(5) 0.133(6) 0.055(3) -0.032(4) -0.041(3) 0.019(4) F4 0.037(3) 0.097(5) 0.097(4) -0.034(4) -0.022(3) -0.001(3) F5 0.129(6) 0.071(4) 0.043(3) -0.012(3) -0.022(3) -0.013(4) F6 0.032(3) 0.085(4) 0.172(7) -0.071(5) -0.015(4) -0.004(3) O1S 0.031(3) 0.043(4) 0.053(4) -0.009(3) -0.003(3) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N11 2.023(5) . ? Pt1 N11 2.023(5) 2 ? Pt1 N1 2.027(6) . ? Pt1 N1 2.027(6) 2 ? N1 C6 1.331(9) . ? N1 C2 1.351(9) . ? C2 C3 1.371(9) . ? C3 C4 1.388(10) . ? C3 C7 1.490(10) . ? C4 C5 1.376(11) . ? C5 C6 1.384(10) . ? C7 O1 1.217(9) . ? C7 N2 1.329(10) . ? N11 C12 1.343(8) . ? N11 C16 1.355(8) . ? C12 C13 1.383(9) . ? C13 C14 1.377(9) . ? C13 C17 1.500(10) . ? C14 C15 1.384(10) . ? C15 C16 1.360(10) . ? C17 O11 1.225(8) . ? C17 N12 1.334(9) . ? P1 F6 1.568(6) . ? P1 F4 1.571(6) . ? P1 F3 1.576(6) . ? P1 F5 1.590(6) . ? P1 F2 1.597(6) . ? P1 F1 1.600(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Pt1 N11 180.0 . 2 ? N11 Pt1 N1 88.2(2) . . ? N11 Pt1 N1 91.8(2) 2 . ? N11 Pt1 N1 91.8(2) . 2 ? N11 Pt1 N1 88.2(2) 2 2 ? N1 Pt1 N1 180.0 . 2 ? C6 N1 C2 119.3(6) . . ? C6 N1 Pt1 120.9(5) . . ? C2 N1 Pt1 119.8(5) . . ? N1 C2 C3 122.6(7) . . ? C2 C3 C4 117.6(7) . . ? C2 C3 C7 123.5(7) . . ? C4 C3 C7 119.0(7) . . ? C5 C4 C3 120.2(7) . . ? C4 C5 C6 118.8(7) . . ? N1 C6 C5 121.5(7) . . ? O1 C7 N2 122.9(7) . . ? O1 C7 C3 120.1(8) . . ? N2 C7 C3 117.0(7) . . ? C12 N11 C16 119.2(6) . . ? C12 N11 Pt1 120.8(4) . . ? C16 N11 Pt1 120.0(5) . . ? N11 C12 C13 121.6(6) . . ? C14 C13 C12 118.4(6) . . ? C14 C13 C17 124.9(6) . . ? C12 C13 C17 116.7(6) . . ? C13 C14 C15 119.9(7) . . ? C16 C15 C14 118.9(7) . . ? N11 C16 C15 121.8(6) . . ? O11 C17 N12 123.3(7) . . ? O11 C17 C13 118.9(6) . . ? N12 C17 C13 117.8(6) . . ? F6 P1 F4 179.6(4) . . ? F6 P1 F3 90.1(4) . . ? F4 P1 F3 89.7(3) . . ? F6 P1 F5 91.4(4) . . ? F4 P1 F5 88.9(4) . . ? F3 P1 F5 178.5(4) . . ? F6 P1 F2 91.1(3) . . ? F4 P1 F2 89.1(3) . . ? F3 P1 F2 90.3(4) . . ? F5 P1 F2 89.3(3) . . ? F6 P1 F1 89.4(3) . . ? F4 P1 F1 90.4(3) . . ? F3 P1 F1 91.2(4) . . ? F5 P1 F1 89.2(3) . . ? F2 P1 F1 178.5(4) . . ? _refine_diff_density_max 0.997 _refine_diff_density_min -1.101 _refine_diff_density_rms 0.210 #END #Data for compound 3.7H2O data_lee5398sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H24 Cl2 N8 O11 Pt' _chemical_formula_weight 866.50 _chemical_melting_point ? _chemical_compound_source 'synthesis' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C2/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 12.6582(1) _cell_length_b 17.2961(2) _cell_length_c 7.8045(1) _cell_angle_alpha 90.00 _cell_angle_beta 94.430(1) _cell_angle_gamma 90.00 _cell_volume 1703.59(3) _cell_formula_units_Z 2 _cell_measurement_temperature 203(5) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 30.20 _exptl_crystal_description 'triangular prism' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.689 _exptl_crystal_density_method ? _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 4.339 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_process_details ; Absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995) which is based upon the method of Blessing (Blessing, 1995) ; _exptl_absorpt_correction_T_min 0.484019 _exptl_absorpt_correction_T_max 0.604297 _exptl_special_details ; Data were collected with a Siemens SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 10s duration at a crystal-to detector distance of 4.908 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment.No significant decay was noted. One of the solvate water molecule is disordered (50%). ; _diffrn_ambient_temperature 203(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13033 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 30.20 _reflns_number_total 2468 _reflns_number_observed 2379 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SMART (Siemens, 1994)' _computing_data_reduction 'SMART (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement 'SHELXTL (Siemens, 1994)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0500P)^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 2468 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_obs 0.0343 _refine_ls_wR_factor_all 0.0808 _refine_ls_wR_factor_obs 0.0777 _refine_ls_goodness_of_fit_all 1.078 _refine_ls_goodness_of_fit_obs 1.056 _refine_ls_restrained_S_all 1.078 _refine_ls_restrained_S_obs 1.056 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 1.0000 0.0000 1.0000 0.01763(10) Uani 1 d S . Cl1 Cl 1.18380(12) 0.0000 1.4158(2) 0.0411(4) Uani 1 d S . N1 N 1.0904(2) 0.0820(2) 0.8980(4) 0.0181(5) Uani 1 d . . C2 C 1.1876(3) 0.0990(2) 0.9726(5) 0.0235(7) Uani 1 d . . H2 H 1.2139(3) 0.0712(2) 1.0701(5) 0.028 Uiso 1 calc R . C3 C 1.2486(3) 0.1564(2) 0.9084(5) 0.0235(7) Uani 1 d . . H3 H 1.3171(3) 0.1660(2) 0.9592(5) 0.028 Uiso 1 calc R . C4 C 1.2090(3) 0.2002(2) 0.7682(4) 0.0196(7) Uani 1 d . . C5 C 1.1103(3) 0.1813(2) 0.6920(5) 0.0245(7) Uani 1 d . . H5 H 1.0818(3) 0.2093(2) 0.5960(5) 0.029 Uiso 1 calc R . C6 C 1.0532(3) 0.1211(2) 0.7568(5) 0.0229(7) Uani 1 d . . H6 H 0.9874(3) 0.1072(2) 0.7012(5) 0.027 Uiso 1 calc R . C7 C 1.2736(3) 0.2668(2) 0.7085(5) 0.0250(7) Uani 1 d . . O O 1.3718(2) 0.2635(2) 0.7211(4) 0.0344(7) Uani 1 d . . N2 N 1.2194(3) 0.3278(2) 0.6464(4) 0.0279(7) Uani 1 d . . H1N H 1.2529(3) 0.3682(2) 0.6121(4) 0.033 Uiso 1 calc R . H2N H 1.1505(3) 0.3273(2) 0.6401(4) 0.033 Uiso 1 calc R . O1A O 1.4091(8) 0.0000 1.6761(13) 0.043(2) Uiso 0.50 d SP . O1B O 1.4216(8) 0.0000 1.5479(13) 0.043(2) Uiso 0.50 d SP . O2 O 1.5061(3) 0.1364(3) 1.7415(7) 0.0801(15) Uani 1 d . . O3 O 1.5792(9) 0.0000 1.9689(14) 0.052(2) Uiso 0.50 d SP . 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 Pt1 0.02197(15) 0.01186(13) 0.01995(15) 0.000 0.00740(9) 0.000 Cl1 0.0356(7) 0.0193(6) 0.0695(11) 0.000 0.0118(7) 0.000 N1 0.0203(13) 0.0153(13) 0.0196(13) 0.0002(10) 0.0075(11) 0.0008(11) C2 0.027(2) 0.019(2) 0.025(2) 0.0012(13) -0.0013(14) -0.0005(14) C3 0.021(2) 0.024(2) 0.025(2) 0.0004(14) -0.0032(13) -0.0019(14) C4 0.020(2) 0.021(2) 0.019(2) 0.0019(12) 0.0054(12) -0.0019(13) C5 0.022(2) 0.024(2) 0.027(2) 0.0084(14) -0.0004(14) -0.0045(14) C6 0.018(2) 0.022(2) 0.029(2) 0.0072(14) 0.0018(13) -0.0033(13) C7 0.027(2) 0.027(2) 0.021(2) 0.0007(14) 0.0027(14) -0.0099(15) O 0.0209(13) 0.040(2) 0.042(2) 0.0052(13) 0.0044(12) -0.0098(12) N2 0.029(2) 0.025(2) 0.030(2) 0.0060(13) 0.0012(13) -0.0088(13) O2 0.041(2) 0.093(4) 0.107(4) -0.027(3) 0.010(2) 0.016(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 Pt1 N1 2.023(3) . ? Pt1 N1 2.023(3) 5_757 ? Pt1 N1 2.023(3) 2_757 ? Pt1 N1 2.023(3) 6 ? N1 C6 1.346(4) . ? N1 C2 1.352(5) . ? C2 C3 1.375(5) . ? C3 C4 1.392(5) . ? C4 C5 1.382(5) . ? C4 C7 1.506(5) . ? C5 C6 1.385(5) . ? C7 O 1.241(5) . ? C7 N2 1.329(5) . ? O1A O1B 1.025(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 N1 Pt1 N1 180.0 . 5_757 ? N1 Pt1 N1 91.0(2) . 2_757 ? N1 Pt1 N1 89.0(2) 5_757 2_757 ? N1 Pt1 N1 89.0(2) . 6 ? N1 Pt1 N1 91.0(2) 5_757 6 ? N1 Pt1 N1 180.0 2_757 6 ? C6 N1 C2 119.4(3) . . ? C6 N1 Pt1 120.1(2) . . ? C2 N1 Pt1 120.5(2) . . ? N1 C2 C3 121.2(3) . . ? C2 C3 C4 120.1(3) . . ? C5 C4 C3 117.9(3) . . ? C5 C4 C7 122.8(3) . . ? C3 C4 C7 119.3(3) . . ? C6 C5 C4 120.0(3) . . ? N1 C6 C5 121.2(3) . . ? O C7 N2 123.4(4) . . ? O C7 C4 120.3(3) . . ? N2 C7 C4 116.3(3) . . ? _refine_diff_density_max 0.927 _refine_diff_density_min -1.265 _refine_diff_density_rms 0.167 #END #Data for compound 4 data_l7298sad _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H24 F12 N8 O4 P2 Pt' _chemical_formula_weight 973.54 _chemical_melting_point ? _chemical_compound_source 'synthesis' 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' 'F' 'F' 0.0171 0.0103 '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' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.888(3) _cell_length_b 32.843(11) _cell_length_c 16.711(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.43(2) _cell_angle_gamma 90.00 _cell_volume 4825.6(24) _cell_formula_units_Z 6 _cell_measurement_temperature 203(5) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.24 _cell_measurement_theta_max 23.00 _exptl_crystal_description rectangular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method ? _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 4.578 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; Absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995) which is based upon the method of Blessing (Blessing, 1995) ; _exptl_absorpt_correction_T_min 0.3732 _exptl_absorpt_correction_T_max 0.4933 _exptl_special_details ; Data were collected with a Siemens SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 10s duration at a crystal-to detector distance of 4.908 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment.No significant decay was noted. ; _diffrn_ambient_temperature 203(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53008 _diffrn_reflns_av_R_equivalents 0.1969 _diffrn_reflns_av_sigmaI/netI 0.1009 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 45 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 23.00 _reflns_number_total 6724 _reflns_number_observed 4435 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SMART (Siemens, 1994)' _computing_data_reduction 'SMART (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement 'SHELXTL (Siemens, 1994)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 15 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6709 _refine_ls_number_parameters 655 _refine_ls_number_restraints 304 _refine_ls_R_factor_all 0.1345 _refine_ls_R_factor_obs 0.0829 _refine_ls_wR_factor_all 0.2071 _refine_ls_wR_factor_obs 0.1815 _refine_ls_goodness_of_fit_all 1.164 _refine_ls_goodness_of_fit_obs 1.288 _refine_ls_restrained_S_all 1.157 _refine_ls_restrained_S_obs 1.265 _refine_ls_shift/esd_max -0.097 _refine_ls_shift/esd_mean 0.006 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.94704(8) 0.16943(2) 0.49010(4) 0.0317(3) Uani 1 d . . Pt2 Pt 0.0000 0.0000 0.0000 0.0312(3) Uani 1 d S . N1 N 0.7566(18) 0.2034(4) 0.4687(8) 0.039(4) Uani 1 d . . C2 C 0.6194(20) 0.1842(7) 0.4473(11) 0.049(5) Uani 1 d . . H2 H 0.6127(20) 0.1559(7) 0.4394(11) 0.058 Uiso 1 calc R . C3 C 0.4901(20) 0.2090(6) 0.4377(10) 0.039(5) Uani 1 d . . H3 H 0.3945(20) 0.1966(6) 0.4237(10) 0.047 Uiso 1 calc R . C4 C 0.4959(22) 0.2503(6) 0.4479(11) 0.042(5) Uani 1 d . . C5 C 0.6362(20) 0.2678(6) 0.4639(11) 0.041(5) Uani 1 d . . H5 H 0.6446(20) 0.2963(6) 0.4671(11) 0.050 Uiso 1 calc R . C6 C 0.7646(18) 0.2446(6) 0.4752(10) 0.041(5) Uani 1 d . . H6 H 0.8600(18) 0.2572(6) 0.4877(10) 0.049 Uiso 1 calc R . C7 C 0.3487(23) 0.2726(6) 0.4418(11) 0.044(5) Uani 1 d . . O1 O 0.2392(15) 0.2587(4) 0.4685(9) 0.060(4) Uani 1 d . . N2 N 0.3463(19) 0.3100(6) 0.4053(10) 0.061(5) Uani 1 d . . H1N H 0.2643(19) 0.3248(6) 0.4005(10) 0.073 Uiso 1 calc R . H2N H 0.4268(19) 0.3189(6) 0.3869(10) 0.073 Uiso 1 calc R . N11 N 0.9648(14) 0.1715(4) 0.3718(8) 0.029(3) Uani 1 d . . C12 C 1.0579(20) 0.1997(6) 0.3447(13) 0.051(6) Uani 1 d . . H12 H 1.1112(20) 0.2177(6) 0.3822(13) 0.061 Uiso 1 calc R . C13 C 1.0775(22) 0.2029(6) 0.2652(11) 0.048(5) Uani 1 d . . H13 H 1.1450(22) 0.2223(6) 0.2495(11) 0.058 Uiso 1 calc R . C14 C 0.9994(20) 0.1780(6) 0.2093(11) 0.038(5) Uani 1 d . . C15 C 0.9046(22) 0.1483(6) 0.2390(12) 0.053(6) Uani 1 d . . H15 H 0.8516(22) 0.1297(6) 0.2024(12) 0.064 Uiso 1 calc R . C16 C 0.8886(24) 0.1459(6) 0.3165(11) 0.049(5) Uani 1 d . . H16 H 0.8232(24) 0.1262(6) 0.3333(11) 0.059 Uiso 1 calc R . C17 C 1.0042(26) 0.1816(6) 0.1196(12) 0.050(6) Uani 1 d . . O11 O 0.8882(15) 0.1743(4) 0.0718(8) 0.051(4) Uani 1 d . . N12 N 1.1287(18) 0.1984(5) 0.0990(10) 0.061(5) Uani 1 d . . H3N H 1.1319(18) 0.2051(5) 0.0489(10) 0.073 Uiso 1 calc R . H4N H 1.2071(18) 0.2029(5) 0.1357(10) 0.073 Uiso 1 calc R . N21 N 1.1350(13) 0.1347(4) 0.5117(7) 0.020(3) Uani 1 d U . C22 C 1.2668(17) 0.1467(5) 0.5550(9) 0.024(3) Uani 1 d U . H22 H 1.2767(17) 0.1742(5) 0.5703(9) 0.029 Uiso 1 calc R . C23 C 1.3838(18) 0.1222(5) 0.5777(10) 0.031(3) Uani 1 d U . H23 H 1.4751(18) 0.1328(5) 0.6054(10) 0.037 Uiso 1 calc R . C24 C 1.3707(17) 0.0800(5) 0.5599(10) 0.029(3) Uani 1 d U . C25 C 1.2404(17) 0.0666(5) 0.5142(9) 0.029(3) Uani 1 d U . H25 H 1.2279(17) 0.0392(5) 0.4990(9) 0.035 Uiso 1 calc R . C26 C 1.1216(18) 0.0963(5) 0.4901(10) 0.030(3) Uani 1 d U . H26 H 1.0317(18) 0.0877(5) 0.4577(10) 0.035 Uiso 1 calc R . C27 C 1.4950(19) 0.0509(6) 0.5887(10) 0.033(4) Uani 1 d . . O21 O 1.6292(14) 0.0636(4) 0.5966(8) 0.048(3) Uani 1 d . . N22 N 1.4597(16) 0.0125(5) 0.6022(9) 0.046(4) Uani 1 d . . H5N H 1.5313(16) -0.0051(5) 0.6174(9) 0.056 Uiso 1 calc R . H6N H 1.3649(16) 0.0049(5) 0.5960(9) 0.056 Uiso 1 calc R . N31 N 0.9271(14) 0.1670(4) 0.6097(8) 0.027(3) Uani 1 d . . C32 C 1.0207(22) 0.1882(6) 0.6648(11) 0.048(5) Uani 1 d . . H32 H 1.0928(22) 0.2058(6) 0.6472(11) 0.057 Uiso 1 calc R . C33 C 1.0141(21) 0.1850(6) 0.7450(11) 0.045(5) Uani 1 d . . H33 H 1.0767(21) 0.2016(6) 0.7817(11) 0.054 Uiso 1 calc R . C34 C 0.9169(18) 0.1577(5) 0.7734(11) 0.038(5) Uani 1 d . . C35 C 0.8182(18) 0.1378(5) 0.7170(10) 0.031(4) Uani 1 d . . H35 H 0.7412(18) 0.1214(5) 0.7332(10) 0.037 Uiso 1 calc R . C36 C 0.8308(19) 0.1416(6) 0.6366(10) 0.041(5) Uani 1 d . . H36 H 0.7682(19) 0.1254(6) 0.5990(10) 0.049 Uiso 1 calc R . C37 C 0.9197(21) 0.1509(6) 0.8641(12) 0.045(5) Uani 1 d . . O31 O 1.0366(16) 0.1610(4) 0.9096(8) 0.063(4) Uani 1 d . . N32 N 0.8069(16) 0.1348(5) 0.8897(9) 0.044(4) Uani 1 d . . H7N H 0.8094(16) 0.1303(5) 0.9411(9) 0.053 Uiso 1 calc R . H8N H 0.7268(16) 0.1281(5) 0.8558(9) 0.053 Uiso 1 calc R . N41 N -0.0059(15) -0.0032(4) 0.1192(9) 0.036(3) Uani 1 d U . C42 C 0.0879(20) -0.0270(5) 0.1683(10) 0.039(3) Uani 1 d U . H42 H 0.1532(20) -0.0443(5) 0.1448(10) 0.047 Uiso 1 calc R . C43 C 0.0953(19) -0.0277(5) 0.2499(10) 0.037(3) Uani 1 d U . H43A H 0.1682(19) -0.0436(5) 0.2825(10) 0.045 Uiso 1 calc R . C44 C -0.0046(17) -0.0051(5) 0.2821(10) 0.029(3) Uani 1 d U . C45 C -0.1039(19) 0.0202(5) 0.2379(10) 0.036(3) Uani 1 d U . H45 H -0.1707(19) 0.0368(5) 0.2620(10) 0.043 Uiso 1 calc R . C46 C -0.1021(20) 0.0204(6) 0.1525(11) 0.041(3) Uani 1 d U . H46 H -0.1696(20) 0.0375(6) 0.1194(11) 0.049 Uiso 1 calc R . C47 C -0.0105(17) -0.0041(5) 0.3752(10) 0.028(4) Uiso 1 d . . O41 O -0.1136(13) 0.0145(4) 0.4032(7) 0.042(3) Uani 1 d . . N42 N 0.0958(15) -0.0245(4) 0.4210(8) 0.036(4) Uani 1 d . . H11N H 0.0964(15) -0.0254(4) 0.4731(8) 0.044 Uiso 1 calc R . H12N H 0.1659(15) -0.0371(4) 0.3994(8) 0.044 Uiso 1 calc R . N51 N 0.1827(15) 0.0332(4) 0.0247(8) 0.035(3) Uani 1 d U . C52 C 0.1828(20) 0.0737(6) 0.0205(10) 0.039(3) Uani 1 d U . H52 H 0.0869(20) 0.0858(6) 0.0059(10) 0.046 Uiso 1 calc R . C53 C 0.3051(19) 0.1007(6) 0.0346(10) 0.038(3) Uani 1 d U . H53 H 0.2937(19) 0.1291(6) 0.0304(10) 0.046 Uiso 1 calc R . C54 C 0.4475(19) 0.0815(5) 0.0559(10) 0.035(3) Uani 1 d U . C55 C 0.4570(19) 0.0403(5) 0.0664(10) 0.037(3) Uani 1 d U . H55 H 0.5507(19) 0.0275(5) 0.0835(10) 0.044 Uiso 1 calc R . C56 C 0.3209(18) 0.0179(6) 0.0507(10) 0.036(3) Uani 1 d U . H56 H 0.3277(18) -0.0104(6) 0.0593(10) 0.043 Uiso 1 calc R . C57 C 0.5969(22) 0.1044(6) 0.0651(11) 0.044(5) Uani 1 d . . O51 O 0.7114(14) 0.0890(5) 0.0470(9) 0.068(5) Uani 1 d . . N52 N 0.5896(18) 0.1442(6) 0.0886(9) 0.060(5) Uani 1 d . . H13N H 0.6695(18) 0.1597(6) 0.0911(9) 0.072 Uiso 1 calc R . H14N H 0.5050(18) 0.1540(6) 0.1011(9) 0.072 Uiso 1 calc R . P1 P 0.5371(6) 0.24354(15) 0.7031(3) 0.0497(14) Uani 1 d D . F1 F 0.3805(13) 0.2454(5) 0.7346(9) 0.133(8) Uiso 0.779(15) d PD 1 F2 F 0.4779(18) 0.2091(3) 0.6425(7) 0.108(7) Uiso 0.779(15) d PD 1 F3 F 0.6940(12) 0.2422(4) 0.6721(8) 0.116(7) Uiso 0.779(15) d PD 1 F4 F 0.5998(19) 0.2780(3) 0.7637(7) 0.140(9) Uiso 0.779(15) d PD 1 F5 F 0.4803(12) 0.2762(3) 0.6370(7) 0.062(5) Uiso 0.779(15) d PD 1 F6 F 0.5925(12) 0.2105(3) 0.7685(6) 0.060(5) Uiso 0.779(15) d PD 1 F1' F 0.3751(17) 0.2227(6) 0.6880(13) 0.032(12) Uiso 0.221(15) d PD 2 F2' F 0.5892(30) 0.2153(5) 0.6359(7) 0.024(11) Uiso 0.221(15) d PD 2 F3' F 0.6979(17) 0.2641(6) 0.7174(13) 0.083(20) Uiso 0.221(15) d PD 2 F4' F 0.4783(34) 0.2739(10) 0.7642(22) 0.052(15) Uiso 0.221(15) d PD 2 P11 P 0.3777(9) 0.0915(2) 0.2965(4) 0.087(2) Uani 1 d D . F11 F 0.2798(19) 0.1213(5) 0.3422(9) 0.102(9) Uiso 0.65(2) d PD 1 F12 F 0.4544(21) 0.1286(6) 0.2568(10) 0.184(15) Uiso 0.65(2) d PD 1 F13 F 0.4831(18) 0.0621(4) 0.2536(9) 0.098(8) Uiso 0.65(2) d PD 1 F14 F 0.3136(16) 0.0527(4) 0.3364(8) 0.056(6) Uiso 0.65(2) d PD 1 F15 F 0.5160(19) 0.0942(5) 0.3703(11) 0.125(11) Uiso 0.65(2) d PD 1 F16 F 0.2544(20) 0.0890(5) 0.2199(10) 0.136(11) Uiso 0.65(2) d PD 1 F11' F 0.1984(25) 0.0918(9) 0.3040(15) 0.121(19) Uiso 0.35(2) d PD 2 F12' F 0.3226(29) 0.1227(7) 0.2232(13) 0.055(11) Uiso 0.35(2) d PD 2 F13' F 0.5544(25) 0.0911(9) 0.2879(16) 0.153(24) Uiso 0.35(2) d PD 2 F14' F 0.3843(37) 0.0603(7) 0.3707(14) 0.118(18) Uiso 0.35(2) d PD 2 F15' F 0.3843(31) 0.1240(7) 0.3684(14) 0.053(11) Uiso 0.35(2) d PD 2 F16' F 0.3306(40) 0.0503(8) 0.2463(22) 0.214(34) Uiso 0.35(2) d PD 2 P21 P 1.3918(5) 0.0835(2) 0.8065(3) 0.054(2) Uani 1 d D . F21 F 1.3351(29) 0.1263(4) 0.7679(10) 0.074(12) Uiso 0.42(3) d PD 1 F22 F 1.4820(11) 0.1066(3) 0.8818(6) 0.097(5) Uiso 1 d D 1 F23 F 1.4463(30) 0.0405(4) 0.8447(11) 0.124(16) Uiso 0.42(3) d PD 1 F24 F 1.2991(11) 0.0615(3) 0.7299(6) 0.085(4) Uiso 1 d D 1 F25 F 1.5329(17) 0.0856(8) 0.7589(11) 0.053(10) Uiso 0.42(3) d PD 1 F26 F 1.2425(17) 0.0815(9) 0.8484(12) 0.112(16) Uiso 0.42(3) d PD 1 F21' F 1.4284(38) 0.1215(6) 0.7513(10) 0.130(12) Uiso 0.58(3) d PD 2 F23' F 1.3747(21) 0.0453(4) 0.8631(9) 0.065(8) Uiso 0.58(3) d PD 2 F25' F 1.5491(16) 0.0643(7) 0.7890(12) 0.099(10) Uiso 0.58(3) d PD 2 F26' F 1.2376(15) 0.1011(7) 0.8326(10) 0.071(8) Uiso 0.58(3) d PD 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0315(4) 0.0399(5) 0.0233(4) 0.0027(3) 0.0030(3) 0.0021(3) Pt2 0.0339(6) 0.0448(7) 0.0154(6) 0.0023(4) 0.0048(4) 0.0000(5) N1 0.077(13) 0.016(9) 0.027(9) 0.009(7) 0.019(8) 0.010(8) C2 0.026(11) 0.076(15) 0.043(13) -0.007(11) -0.001(9) -0.004(11) C3 0.041(12) 0.049(14) 0.029(11) 0.010(9) 0.015(8) -0.001(9) C4 0.050(13) 0.042(13) 0.032(12) -0.007(9) 0.001(9) 0.017(10) C5 0.039(12) 0.044(12) 0.040(12) 0.003(10) 0.005(9) 0.015(10) C6 0.016(10) 0.067(15) 0.037(12) 0.016(10) -0.008(8) -0.005(9) C7 0.044(13) 0.054(14) 0.029(12) -0.012(10) -0.009(9) 0.020(11) O1 0.038(9) 0.069(10) 0.076(11) -0.004(8) 0.019(8) 0.002(7) N2 0.056(12) 0.064(13) 0.060(13) 0.010(10) -0.001(9) 0.018(9) N11 0.020(7) 0.038(9) 0.027(8) 0.011(7) -0.007(6) 0.009(7) C12 0.035(12) 0.055(14) 0.060(16) -0.010(11) -0.004(10) -0.022(10) C13 0.055(13) 0.068(15) 0.026(12) -0.009(11) 0.017(10) -0.014(11) C14 0.040(11) 0.051(13) 0.026(11) 0.019(9) 0.015(9) 0.005(9) C15 0.058(14) 0.066(15) 0.035(13) -0.006(11) 0.001(10) -0.023(11) C16 0.097(17) 0.038(12) 0.014(11) 0.011(9) 0.011(11) -0.006(11) C17 0.076(16) 0.045(13) 0.026(12) 0.019(10) 0.000(12) 0.007(11) O11 0.061(9) 0.059(10) 0.029(8) -0.007(6) -0.003(7) -0.010(7) N12 0.054(11) 0.096(15) 0.037(11) 0.011(10) 0.024(8) -0.021(10) N21 0.017(5) 0.018(6) 0.023(6) 0.003(5) -0.003(5) -0.001(5) C22 0.028(6) 0.015(6) 0.029(7) 0.002(6) 0.003(6) -0.001(5) C23 0.033(7) 0.028(7) 0.030(7) -0.005(6) -0.001(6) 0.007(6) C24 0.027(7) 0.030(7) 0.028(7) 0.002(6) -0.004(6) 0.004(6) C25 0.030(7) 0.027(7) 0.029(7) -0.005(6) -0.001(6) -0.001(6) C26 0.027(6) 0.029(7) 0.029(7) -0.003(6) -0.006(6) -0.002(6) C27 0.024(10) 0.048(13) 0.028(11) 0.002(9) 0.007(8) 0.004(9) O21 0.036(8) 0.051(9) 0.058(9) 0.002(7) 0.005(6) 0.006(6) N22 0.038(9) 0.041(11) 0.058(12) 0.009(8) -0.003(8) 0.002(7) N31 0.023(8) 0.022(8) 0.033(8) -0.006(7) 0.001(6) 0.007(6) C32 0.056(13) 0.057(14) 0.026(12) 0.010(10) -0.008(10) -0.011(10) C33 0.045(12) 0.051(13) 0.034(13) -0.007(10) -0.008(10) -0.010(10) C34 0.024(10) 0.045(12) 0.045(12) 0.010(10) 0.010(9) 0.001(8) C35 0.029(10) 0.045(12) 0.019(10) 0.000(8) 0.007(8) -0.013(8) C36 0.032(11) 0.066(14) 0.023(11) 0.008(10) 0.002(8) -0.031(10) C37 0.031(12) 0.059(14) 0.043(13) 0.000(11) -0.005(10) -0.004(10) O31 0.053(9) 0.097(12) 0.040(9) -0.002(8) 0.010(7) -0.028(8) N32 0.039(10) 0.069(12) 0.022(9) -0.003(8) -0.004(7) -0.015(8) N41 0.041(6) 0.042(7) 0.025(6) 0.001(6) 0.007(5) 0.008(5) C42 0.046(7) 0.045(7) 0.026(7) 0.000(6) 0.005(6) 0.013(6) C43 0.041(7) 0.046(7) 0.024(7) 0.004(6) 0.005(6) 0.012(6) C44 0.032(7) 0.040(7) 0.016(7) 0.002(6) 0.005(6) 0.007(6) C45 0.041(7) 0.044(7) 0.024(7) -0.008(6) 0.013(6) 0.013(6) C46 0.047(7) 0.048(8) 0.029(7) -0.002(7) 0.007(6) 0.013(6) O41 0.044(7) 0.049(8) 0.035(8) 0.006(6) 0.006(6) 0.012(6) N42 0.045(9) 0.051(10) 0.014(8) -0.003(7) 0.009(7) -0.001(7) N51 0.032(6) 0.054(7) 0.019(6) 0.009(6) 0.009(5) 0.026(6) C52 0.033(7) 0.053(8) 0.030(7) 0.002(7) 0.004(6) 0.015(6) C53 0.034(7) 0.047(8) 0.035(7) 0.002(6) 0.012(6) 0.007(6) C54 0.037(7) 0.041(7) 0.025(7) -0.004(6) 0.004(6) 0.001(6) C55 0.037(7) 0.045(7) 0.027(7) 0.001(6) -0.003(6) 0.005(6) C56 0.036(7) 0.049(7) 0.024(7) 0.008(6) 0.003(6) 0.002(6) C57 0.040(13) 0.053(14) 0.034(12) 0.007(10) -0.013(9) -0.017(10) O51 0.020(7) 0.099(12) 0.084(12) 0.020(9) 0.008(7) 0.012(8) N52 0.050(11) 0.070(14) 0.054(12) 0.003(10) -0.010(9) -0.004(9) P1 0.056(4) 0.060(4) 0.035(3) -0.006(3) 0.010(3) 0.001(3) P11 0.158(7) 0.059(4) 0.049(4) 0.010(3) 0.037(4) 0.027(4) P21 0.065(4) 0.064(4) 0.035(3) 0.005(3) 0.012(3) -0.019(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N11 2.007(14) . ? Pt1 N21 2.011(11) . ? Pt1 N1 2.015(14) . ? Pt1 N31 2.034(14) . ? Pt2 N51 1.949(15) . ? Pt2 N51 1.949(15) 3 ? Pt2 N41 2.002(14) 3 ? Pt2 N41 2.003(14) . ? N1 C6 1.36(2) . ? N1 C2 1.37(2) . ? C2 C3 1.40(2) . ? C3 C4 1.37(2) . ? C4 C5 1.36(2) . ? C4 C7 1.49(2) . ? C5 C6 1.36(2) . ? C7 O1 1.22(2) . ? C7 N2 1.37(2) . ? N11 C16 1.35(2) . ? N11 C12 1.36(2) . ? C12 C13 1.37(3) . ? C13 C14 1.35(2) . ? C14 C15 1.43(3) . ? C14 C17 1.51(3) . ? C15 C16 1.33(2) . ? C17 O11 1.23(2) . ? C17 N12 1.33(3) . ? N21 C26 1.31(2) . ? N21 C22 1.34(2) . ? C22 C23 1.32(2) . ? C23 C24 1.42(2) . ? C24 C25 1.36(2) . ? C24 C27 1.49(2) . ? C25 C26 1.45(2) . ? C27 O21 1.25(2) . ? C27 N22 1.33(2) . ? N31 C36 1.32(2) . ? N31 C32 1.34(2) . ? C32 C33 1.35(3) . ? C33 C34 1.38(2) . ? C34 C35 1.36(2) . ? C34 C37 1.53(3) . ? C35 C36 1.37(2) . ? C37 O31 1.24(2) . ? C37 N32 1.26(2) . ? N41 C42 1.33(2) . ? N41 C46 1.34(2) . ? C42 C43 1.36(2) . ? C43 C44 1.33(2) . ? C44 C45 1.35(2) . ? C44 C47 1.57(2) . ? C45 C46 1.43(2) . ? C47 O41 1.25(2) . ? C47 N42 1.31(2) . ? N51 C52 1.33(2) . ? N51 C56 1.34(2) . ? C52 C53 1.40(2) . ? C53 C54 1.41(2) . ? C54 C55 1.36(2) . ? C54 C57 1.51(2) . ? C55 C56 1.41(2) . ? C57 O51 1.21(2) . ? C57 N52 1.37(2) . ? P1 F2 1.557(9) . ? P1 F3 1.558(9) . ? P1 F1 1.560(10) . ? P1 F4 1.566(9) . ? P1 F3' 1.566(11) . ? P1 F6 1.568(8) . ? P1 F5 1.569(8) . ? P1 F4' 1.570(10) . ? P1 F2' 1.578(10) . ? P1 F1' 1.580(12) . ? P11 F16 1.561(13) . ? P11 F11 1.579(13) . ? P11 F14 1.582(12) . ? P11 F13 1.588(13) . ? P11 F12 1.588(13) . ? P11 F13' 1.60(2) . ? P11 F15' 1.60(2) . ? P11 F14' 1.60(2) . ? P11 F15 1.612(12) . ? P11 F16' 1.61(2) . ? P11 F12' 1.62(2) . ? P11 F11' 1.62(2) . ? P21 F25 1.582(10) . ? P21 F22 1.584(10) . ? P21 F26 1.590(11) . ? P21 F24 1.591(10) . ? P21 F23' 1.592(13) . ? P21 F23 1.596(12) . ? P21 F21 1.596(12) . ? P21 F25' 1.600(14) . ? P21 F26' 1.605(13) . ? P21 F21' 1.611(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Pt1 N21 90.7(5) . . ? N11 Pt1 N1 89.6(5) . . ? N21 Pt1 N1 179.1(5) . . ? N11 Pt1 N31 179.4(5) . . ? N21 Pt1 N31 89.5(5) . . ? N1 Pt1 N31 90.2(5) . . ? N51 Pt2 N51 179.998(2) . 3 ? N51 Pt2 N41 92.2(5) . 3 ? N51 Pt2 N41 87.8(5) 3 3 ? N51 Pt2 N41 87.8(5) . . ? N51 Pt2 N41 92.2(5) 3 . ? N41 Pt2 N41 180.0 3 . ? C6 N1 C2 120.8(16) . . ? C6 N1 Pt1 120.3(12) . . ? C2 N1 Pt1 118.9(12) . . ? N1 C2 C3 116.6(19) . . ? C4 C3 C2 123.2(18) . . ? C5 C4 C3 117.3(17) . . ? C5 C4 C7 125.1(18) . . ? C3 C4 C7 117.6(18) . . ? C6 C5 C4 120.9(19) . . ? N1 C6 C5 121.0(17) . . ? O1 C7 N2 122.6(17) . . ? O1 C7 C4 122.1(19) . . ? N2 C7 C4 115.3(19) . . ? C16 N11 C12 117.4(16) . . ? C16 N11 Pt1 123.3(12) . . ? C12 N11 Pt1 119.3(12) . . ? N11 C12 C13 123.0(17) . . ? C14 C13 C12 119.9(18) . . ? C13 C14 C15 116.2(17) . . ? C13 C14 C17 123.5(17) . . ? C15 C14 C17 120.3(18) . . ? C16 C15 C14 122.3(18) . . ? C15 C16 N11 121.1(18) . . ? O11 C17 N12 124.4(19) . . ? O11 C17 C14 119.0(19) . . ? N12 C17 C14 115.9(18) . . ? C26 N21 C22 117.8(13) . . ? C26 N21 Pt1 117.1(10) . . ? C22 N21 Pt1 124.6(10) . . ? C23 C22 N21 124.3(15) . . ? C22 C23 C24 119.7(15) . . ? C25 C24 C23 117.9(14) . . ? C25 C24 C27 120.3(15) . . ? C23 C24 C27 121.8(14) . . ? C24 C25 C26 117.7(15) . . ? N21 C26 C25 122.4(14) . . ? O21 C27 N22 122.9(16) . . ? O21 C27 C24 118.2(17) . . ? N22 C27 C24 118.9(15) . . ? C36 N31 C32 117.6(16) . . ? C36 N31 Pt1 120.9(11) . . ? C32 N31 Pt1 121.3(12) . . ? N31 C32 C33 121.6(18) . . ? C32 C33 C34 120.9(18) . . ? C35 C34 C33 116.6(17) . . ? C35 C34 C37 122.1(16) . . ? C33 C34 C37 121.2(17) . . ? C34 C35 C36 120.0(16) . . ? N31 C36 C35 122.7(15) . . ? O31 C37 N32 122.7(19) . . ? O31 C37 C34 117.4(17) . . ? N32 C37 C34 119.9(16) . . ? C42 N41 C46 117.6(16) . . ? C42 N41 Pt2 122.6(12) . . ? C46 N41 Pt2 119.8(12) . . ? N41 C42 C43 124.3(17) . . ? C44 C43 C42 117.3(16) . . ? C43 C44 C45 123.0(16) . . ? C43 C44 C47 122.4(14) . . ? C45 C44 C47 114.6(14) . . ? C44 C45 C46 116.5(15) . . ? N41 C46 C45 121.0(16) . . ? O41 C47 N42 122.6(16) . . ? O41 C47 C44 121.1(14) . . ? N42 C47 C44 116.4(14) . . ? C52 N51 C56 112.6(15) . . ? C52 N51 Pt2 123.6(11) . . ? C56 N51 Pt2 123.7(12) . . ? N51 C52 C53 129.2(16) . . ? C52 C53 C54 113.9(17) . . ? C55 C54 C53 120.8(16) . . ? C55 C54 C57 116.2(16) . . ? C53 C54 C57 123.0(17) . . ? C54 C55 C56 117.4(16) . . ? N51 C56 C55 125.8(18) . . ? O51 C57 N52 123.1(18) . . ? O51 C57 C54 121.6(19) . . ? N52 C57 C54 115.2(18) . . ? F2 P1 F3 89.7(4) . . ? F2 P1 F1 90.9(5) . . ? F3 P1 F1 179.3(5) . . ? F2 P1 F4 178.9(7) . . ? F3 P1 F4 89.1(5) . . ? F1 P1 F4 90.2(4) . . ? F2 P1 F6 89.6(4) . . ? F3 P1 F6 90.4(4) . . ? F1 P1 F6 89.8(4) . . ? F4 P1 F6 90.2(4) . . ? F2 P1 F5 89.7(4) . . ? F3 P1 F5 89.8(4) . . ? F1 P1 F5 90.0(4) . . ? F4 P1 F5 90.5(4) . . ? F6 P1 F5 179.3(5) . . ? F3' P1 F4' 90.6(5) . . ? F3' P1 F2' 90.3(5) . . ? F4' P1 F2' 175.3(18) . . ? F3' P1 F1' 179.5(5) . . ? F4' P1 F1' 89.8(5) . . ? F2' P1 F1' 89.3(5) . . ? F16 P11 F11 93.4(6) . . ? F16 P11 F14 92.9(6) . . ? F11 P11 F14 92.1(6) . . ? F16 P11 F13 89.3(6) . . ? F11 P11 F13 177.2(5) . . ? F14 P11 F13 88.5(6) . . ? F16 P11 F12 89.5(6) . . ? F11 P11 F12 91.5(6) . . ? F14 P11 F12 175.6(9) . . ? F13 P11 F12 87.8(6) . . ? F13' P11 F15' 98.3(7) . . ? F13' P11 F14' 98.0(8) . . ? F15' P11 F14' 81.5(10) . . ? F16 P11 F15 175.0(13) . . ? F11 P11 F15 90.5(6) . . ? F14 P11 F15 90.2(6) . . ? F13 P11 F15 86.8(6) . . ? F12 P11 F15 87.2(6) . . ? F13' P11 F16' 97.5(8) . . ? F15' P11 F16' 157.8(20) . . ? F14' P11 F16' 80.9(10) . . ? F13' P11 F12' 97.4(7) . . ? F15' P11 F12' 96.9(8) . . ? F14' P11 F12' 164.5(13) . . ? F16' P11 F12' 96.4(8) . . ? F13' P11 F11' 179.3(6) . . ? F15' P11 F11' 82.3(7) . . ? F14' P11 F11' 82.5(7) . . ? F16' P11 F11' 82.1(7) . . ? F12' P11 F11' 82.1(7) . . ? F25 P21 F22 91.9(5) . . ? F25 P21 F26 176.0(10) . . ? F22 P21 F26 91.6(5) . . ? F25 P21 F24 88.3(5) . . ? F22 P21 F24 178.4(4) . . ? F26 P21 F24 88.2(5) . . ? F25 P21 F23 91.3(4) . . ? F22 P21 F23 91.0(4) . . ? F26 P21 F23 90.7(4) . . ? F24 P21 F23 90.6(4) . . ? F25 P21 F21 89.2(4) . . ? F22 P21 F21 89.6(4) . . ? F26 P21 F21 88.9(4) . . ? F24 P21 F21 88.9(4) . . ? F23 P21 F21 179.3(5) . . ? F23' P21 F25' 87.6(6) . . ? F23' P21 F26' 87.8(6) . . ? F25' P21 F26' 174.5(10) . . ? F23' P21 F21' 173.9(11) . . ? F25' P21 F21' 86.9(6) . . ? F26' P21 F21' 97.5(15) . . ? _refine_diff_density_max 2.824 _refine_diff_density_min -1.216 _refine_diff_density_rms 0.237 #END # Data for compound 5 data_l5898 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H6 Cr O5' _chemical_formula_weight 258.15 _chemical_melting_point ? _chemical_compound_source 'synthesis' 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.0349(3) _cell_length_b 7.2332(3) _cell_length_c 11.1518(5) _cell_angle_alpha 88.7100(10) _cell_angle_beta 81.7330(10) _cell_angle_gamma 63.0120(10) _cell_volume 499.82(4) _cell_formula_units_Z 2 _cell_measurement_temperature 208(5) _cell_measurement_reflns_used 3326 _cell_measurement_theta_min 1.85 _cell_measurement_theta_max 29.30 _exptl_crystal_description plates _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method ? _exptl_crystal_F_000 260 _exptl_absorpt_coefficient_mu 1.145 _exptl_absorpt_correction_type 'empirical: (SADABS)' _exptl_absorpt_correction_T_min 0.610 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_process_details ; Absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995), which is based upon the method of Blessing (Blessing, 1995). ; _exptl_special_details ; Data were collected with a Siemens SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 25s duration at a crystal-to-detector distance of 4.908 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 208(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5785 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 29.31 _reflns_number_total 2437 _reflns_number_observed 1868 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement 'SHELXTL (Siemens, 1994)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.5303P] 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 ; Arene hydrogen atoms were included in the final cycles in their calculated positions; the carboxyl hydrogen was located directly from a difference map. All hydrogen atoms were refined using riding models. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2437 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_obs 0.0449 _refine_ls_wR_factor_all 0.1158 _refine_ls_wR_factor_obs 0.0981 _refine_ls_goodness_of_fit_all 1.058 _refine_ls_goodness_of_fit_obs 1.032 _refine_ls_restrained_S_all 1.058 _refine_ls_restrained_S_obs 1.032 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr Cr 0.18733(8) 0.13063(7) 0.21501(4) 0.0270(2) Uani 1 d . . O1 O -0.3657(3) 0.5841(3) 0.3815(2) 0.0407(6) Uani 1 d . . H1 H -0.5212(3) 0.6357(3) 0.4268(2) 0.049 Uiso 1 d R . O2 O -0.2465(4) 0.3219(4) 0.5058(2) 0.0403(6) Uani 1 d . . O10 O -0.0856(4) -0.0809(4) 0.2984(2) 0.0401(6) Uani 1 d . . C10 C 0.0231(5) -0.0032(4) 0.2652(3) 0.0286(6) Uani 1 d . . C1 C -0.2149(5) 0.4250(5) 0.4215(3) 0.0294(6) Uani 1 d . . C2 C 0.0096(5) 0.3665(4) 0.3618(3) 0.0277(6) Uani 1 d . . C9 C 0.4017(6) -0.1199(6) 0.1408(3) 0.0420(8) Uani 1 d . . O9 O 0.5298(5) -0.2772(4) 0.0967(3) 0.0676(9) Uani 1 d . . C3 C 0.1852(5) 0.1990(5) 0.4063(3) 0.0319(7) Uani 1 d . . H3 H 0.1600(5) 0.1332(5) 0.4760(3) 0.038 Uiso 1 calc R . O8 O -0.0039(6) 0.2264(5) -0.0154(3) 0.0695(9) Uani 1 d . . C6 C 0.2606(5) 0.3996(5) 0.1979(3) 0.0349(7) Uani 1 d . . H6 H 0.2866(5) 0.4679(5) 0.1295(3) 0.042 Uiso 1 calc R . C7 C 0.0475(5) 0.4652(5) 0.2575(3) 0.0304(7) Uani 1 d . . H7 H -0.0686(5) 0.5745(5) 0.2276(3) 0.036 Uiso 1 calc R . C8 C 0.0706(6) 0.1884(5) 0.0729(3) 0.0419(8) Uani 1 d . . C5 C 0.4325(5) 0.2334(5) 0.2403(3) 0.0378(8) Uani 1 d . . H5 H 0.5736(5) 0.1877(5) 0.1991(3) 0.045 Uiso 1 calc R . C4 C 0.3949(5) 0.1330(5) 0.3456(3) 0.0360(7) Uani 1 d . . H4 H 0.5113(5) 0.0223(5) 0.3745(3) 0.043 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0299(3) 0.0280(3) 0.0212(3) 0.0035(2) -0.0013(2) -0.0123(2) O1 0.0292(11) 0.0357(12) 0.0445(14) 0.0085(10) -0.0001(10) -0.0056(10) O2 0.0347(12) 0.0424(13) 0.0336(13) 0.0087(10) 0.0042(10) -0.0117(10) O10 0.0403(13) 0.0383(12) 0.0448(14) 0.0037(10) -0.0003(11) -0.0223(11) C10 0.0302(15) 0.0271(14) 0.0218(15) -0.0007(11) -0.0038(11) -0.0073(12) C1 0.0318(15) 0.0294(15) 0.0230(15) -0.0022(12) -0.0020(12) -0.0109(12) C2 0.0330(15) 0.0276(14) 0.0212(14) -0.0044(11) -0.0001(12) -0.0134(12) C9 0.044(2) 0.044(2) 0.033(2) 0.0024(15) 0.0062(15) -0.019(2) O9 0.064(2) 0.046(2) 0.062(2) -0.0145(14) 0.0245(15) -0.0076(14) C3 0.035(2) 0.040(2) 0.0209(15) 0.0018(12) -0.0042(12) -0.0168(14) O8 0.121(3) 0.065(2) 0.042(2) 0.0221(14) -0.046(2) -0.051(2) C6 0.042(2) 0.037(2) 0.032(2) 0.0045(13) -0.0022(14) -0.0240(15) C7 0.033(2) 0.0256(14) 0.033(2) 0.0014(12) -0.0033(13) -0.0141(12) C8 0.062(2) 0.034(2) 0.036(2) 0.0071(14) -0.012(2) -0.026(2) C5 0.032(2) 0.050(2) 0.036(2) 0.0050(15) -0.0021(13) -0.0230(15) C4 0.031(2) 0.046(2) 0.032(2) 0.0063(14) -0.0085(13) -0.0182(14) _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 Cr C10 1.841(3) . ? Cr C8 1.843(4) . ? Cr C9 1.863(4) . ? Cr C2 2.180(3) . ? Cr C7 2.192(3) . ? Cr C3 2.196(3) . ? Cr C4 2.212(3) . ? Cr C5 2.218(3) . ? Cr C6 2.225(3) . ? O1 C1 1.285(4) . ? O1 H1 1.03 . ? O2 C1 1.245(4) . ? O10 C10 1.156(4) . ? C1 C2 1.490(4) . ? C2 C7 1.407(4) . ? C2 C3 1.425(4) . ? C9 O9 1.148(4) . ? C3 C4 1.396(4) . ? C3 H3 0.94 . ? O8 C8 1.151(4) . ? C6 C5 1.397(5) . ? C6 C7 1.413(4) . ? C6 H6 0.94 . ? C7 H7 0.94 . ? C5 C4 1.423(5) . ? C5 H5 0.94 . ? C4 H4 0.94 . ? 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 C10 Cr C8 89.40(14) . . ? C10 Cr C9 88.50(14) . . ? C8 Cr C9 88.5(2) . . ? C10 Cr C2 90.32(12) . . ? C8 Cr C2 114.74(14) . . ? C9 Cr C2 156.70(14) . . ? C10 Cr C7 118.32(12) . . ? C8 Cr C7 89.07(13) . . ? C9 Cr C7 153.04(14) . . ? C2 Cr C7 37.53(11) . . ? C10 Cr C3 88.80(13) . . ? C8 Cr C3 152.65(14) . . ? C9 Cr C3 118.69(14) . . ? C2 Cr C3 38.00(11) . . ? C7 Cr C3 68.00(12) . . ? C10 Cr C4 114.60(13) . . ? C8 Cr C4 156.00(14) . . ? C9 Cr C4 91.97(15) . . ? C2 Cr C4 67.47(12) . . ? C7 Cr C4 79.71(12) . . ? C3 Cr C4 36.93(11) . . ? C10 Cr C5 152.02(13) . . ? C8 Cr C5 118.55(14) . . ? C9 Cr C5 90.82(15) . . ? C2 Cr C5 79.50(12) . . ? C7 Cr C5 67.00(12) . . ? C3 Cr C5 67.15(12) . . ? C4 Cr C5 37.46(12) . . ? C10 Cr C6 155.55(12) . . ? C8 Cr C6 91.40(14) . . ? C9 Cr C6 115.95(14) . . ? C2 Cr C6 67.23(12) . . ? C7 Cr C6 37.29(11) . . ? C3 Cr C6 79.41(12) . . ? C4 Cr C6 66.88(12) . . ? C5 Cr C6 36.65(12) . . ? C1 O1 H1 117.6(2) . . ? O10 C10 Cr 177.7(3) . . ? O2 C1 O1 124.0(3) . . ? O2 C1 C2 119.6(3) . . ? O1 C1 C2 116.4(3) . . ? C7 C2 C3 120.1(3) . . ? C7 C2 C1 120.5(3) . . ? C3 C2 C1 119.2(3) . . ? C7 C2 Cr 71.7(2) . . ? C3 C2 Cr 71.6(2) . . ? C1 C2 Cr 125.2(2) . . ? O9 C9 Cr 177.8(3) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 Cr 72.1(2) . . ? C2 C3 Cr 70.4(2) . . ? C4 C3 H3 120.2(2) . . ? C2 C3 H3 120.2(2) . . ? Cr C3 H3 129.74(8) . . ? C5 C6 C7 120.1(3) . . ? C5 C6 Cr 71.4(2) . . ? C7 C6 Cr 70.1(2) . . ? C5 C6 H6 120.0(2) . . ? C7 C6 H6 120.0(2) . . ? Cr C6 H6 131.35(9) . . ? C2 C7 C6 119.8(3) . . ? C2 C7 Cr 70.8(2) . . ? C6 C7 Cr 72.6(2) . . ? C2 C7 H7 120.1(2) . . ? C6 C7 H7 120.1(2) . . ? Cr C7 H7 128.76(8) . . ? O8 C8 Cr 179.3(3) . . ? C6 C5 C4 120.3(3) . . ? C6 C5 Cr 72.0(2) . . ? C4 C5 Cr 71.0(2) . . ? C6 C5 H5 119.9(2) . . ? C4 C5 H5 119.9(2) . . ? Cr C5 H5 129.61(9) . . ? C3 C4 C5 120.0(3) . . ? C3 C4 Cr 70.9(2) . . ? C5 C4 Cr 71.5(2) . . ? C3 C4 H4 120.0(2) . . ? C5 C4 H4 120.0(2) . . ? Cr C4 H4 130.06(9) . . ? _refine_diff_density_max 0.591 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.088 #END # Data for compound 7.2DMSO data_lee3398 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C11 H6 O7 Cr, 2(C2 H6 S O2)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C15 H18 Cr O9 S2' _chemical_formula_weight 458.41 _chemical_melting_point ? _chemical_compound_source 'synthesis' 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' 'S' 'S' 0.1246 0.1234 '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 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 8.0183(2) _cell_length_b 21.3486(3) _cell_length_c 11.8935(1) _cell_angle_alpha 90.00 _cell_angle_beta 93.521(1) _cell_angle_gamma 90.00 _cell_volume 2032.08(6) _cell_formula_units_Z 4 _cell_measurement_temperature 208(5) _cell_measurement_reflns_used 3081 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 29.255 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method ? _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.811 _exptl_absorpt_correction_type 'empirical: SADABS' _exptl_absorpt_correction_T_min 0.5653 _exptl_absorpt_correction_T_max 0.9119 _exptl_absorpt_process_details ; Absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995), which is based upon the method of Blessing (Blessing, 1995). ; _exptl_special_details ; Data were collected with a Siemens SMART CCD-based diffractometer using \w-scans of width 0.3 deg. and 15s duration at a crystal-to-detector distance of 4.700 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 208(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17215 _diffrn_reflns_av_R_equivalents 0.1621 _diffrn_reflns_av_sigmaI/netI 0.1371 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3580 _reflns_number_gt 1659 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement 'SHELXTL (Bruker, 1999)' _computing_molecular_graphics 'SHELXTL (Bruker, 1999)' _computing_publication_material 'SHELXTL (Bruker, 1999)' _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^)+(0.0800P)^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 3580 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1830 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1909 _refine_ls_wR_factor_gt 0.1384 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.76077(14) -0.05840(5) 0.25772(9) 0.0412(4) Uani 1 1 d . . . C1 C 0.6187(8) 0.0009(3) 0.1357(5) 0.0374(17) Uani 1 1 d . . . O1 O 0.5391(6) 0.1046(2) 0.1805(4) 0.0545(14) Uani 1 1 d . . . O2 O 0.3410(6) 0.0307(2) 0.1550(4) 0.0494(13) Uani 1 1 d . . . H2A H 0.2506 0.0689 0.1586 0.059 Uiso 1 1 d R . . C2 C 0.5694(9) -0.0617(3) 0.1170(5) 0.0379(17) Uani 1 1 d . . . H2 H 0.4556 -0.0724 0.1162 0.045 Uiso 1 1 calc R . . C3 C 0.6877(8) -0.1083(3) 0.0995(5) 0.0386(17) Uani 1 1 d . . . H3 H 0.6531 -0.1500 0.0869 0.046 Uiso 1 1 calc R . . C4 C 0.8608(9) -0.0927(3) 0.1006(6) 0.0401(18) Uani 1 1 d . . . C5 C 0.9099(9) -0.0291(3) 0.1157(5) 0.0389(17) Uani 1 1 d . . . H5 H 1.0231 -0.0178 0.1142 0.047 Uiso 1 1 calc R . . C6 C 0.7895(8) 0.0165(3) 0.1329(5) 0.0384(17) Uani 1 1 d . . . H6 H 0.8227 0.0585 0.1427 0.046 Uiso 1 1 calc R . . C7 C 0.4963(9) 0.0512(3) 0.1607(6) 0.0416(18) Uani 1 1 d . . . C8 C 0.9873(10) -0.1441(4) 0.0930(6) 0.0450(19) Uani 1 1 d . . . O3 O 0.9474(6) -0.1986(2) 0.0834(4) 0.0520(14) Uani 1 1 d . . . O4 O 1.1415(6) -0.1237(2) 0.1006(4) 0.0546(14) Uani 1 1 d . . . H4A H 1.2504 -0.1623 0.0960 0.066 Uiso 1 1 d R . . C9 C 0.6001(12) -0.0900(5) 0.3446(8) 0.098(4) Uani 1 1 d . . . O9 O 0.5003(10) -0.1107(5) 0.3983(7) 0.184(5) Uani 1 1 d . . . C10 C 0.9069(10) -0.1113(4) 0.3323(6) 0.054(2) Uani 1 1 d . . . O10 O 1.0009(8) -0.1456(3) 0.3793(5) 0.093(2) Uani 1 1 d . . . C11 C 0.8164(13) -0.0005(4) 0.3649(7) 0.079(3) Uani 1 1 d . . . O11 O 0.8528(13) 0.0372(3) 0.4327(6) 0.155(4) Uani 1 1 d . . . S11 S 0.1044(2) 0.17088(9) 0.24191(17) 0.0515(6) Uani 1 1 d . . . O12 O 0.1076(5) 0.1134(2) 0.1679(4) 0.0498(13) Uani 1 1 d . . . C13 C 0.2542(10) 0.2230(3) 0.1940(7) 0.062(2) Uani 1 1 d . . . H13A H 0.2700 0.2574 0.2469 0.093 Uiso 1 1 calc R . . H13B H 0.2160 0.2393 0.1207 0.093 Uiso 1 1 calc R . . H13C H 0.3593 0.2012 0.1879 0.093 Uiso 1 1 calc R . . C14 C 0.2080(10) 0.1505(4) 0.3719(6) 0.069(2) Uani 1 1 d . . . H14A H 0.3149 0.1315 0.3586 0.104 Uiso 1 1 calc R . . H14B H 0.1401 0.1209 0.4110 0.104 Uiso 1 1 calc R . . H14C H 0.2258 0.1878 0.4176 0.104 Uiso 1 1 calc R . . S21 S 1.4019(2) -0.25715(9) 0.03108(17) 0.0498(6) Uani 1 1 d . . . O22 O 1.3815(6) -0.2030(2) 0.1103(5) 0.0581(15) Uani 1 1 d . . . C23 C 1.2790(10) -0.2393(4) -0.0931(6) 0.063(2) Uani 1 1 d . . . H23A H 1.2710 -0.2759 -0.1413 0.094 Uiso 1 1 d R . . H23B H 1.1680 -0.2268 -0.0739 0.094 Uiso 1 1 d R . . H23C H 1.3307 -0.2053 -0.1323 0.094 Uiso 1 1 d R . . C24 C 1.2794(9) -0.3183(3) 0.0814(6) 0.052(2) Uani 1 1 d . . . H24A H 1.1681 -0.3029 0.0936 0.078 Uiso 1 1 d R . . H24B H 1.2720 -0.3518 0.0261 0.078 Uiso 1 1 d R . . H24C H 1.3307 -0.3341 0.1517 0.078 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 Cr1 0.0442(7) 0.0404(7) 0.0387(7) 0.0033(6) 0.0004(5) 0.0005(6) C1 0.032(4) 0.038(4) 0.042(4) -0.003(3) -0.005(3) -0.004(3) O1 0.051(3) 0.034(3) 0.078(4) -0.007(3) -0.001(3) 0.002(2) O2 0.037(3) 0.044(3) 0.066(3) -0.006(3) 0.000(3) 0.000(2) C2 0.038(4) 0.036(4) 0.040(4) -0.006(4) -0.001(3) -0.007(4) C3 0.044(5) 0.035(4) 0.035(4) -0.003(3) -0.007(3) -0.011(4) C4 0.047(5) 0.034(4) 0.040(4) -0.006(3) 0.009(4) -0.006(4) C5 0.035(4) 0.047(4) 0.035(4) 0.010(4) 0.002(3) -0.003(4) C6 0.037(4) 0.033(4) 0.045(4) 0.006(3) -0.003(3) -0.004(3) C7 0.043(5) 0.042(5) 0.038(4) 0.010(4) -0.007(4) -0.004(4) C8 0.054(5) 0.040(5) 0.041(5) -0.002(4) 0.006(4) -0.004(4) O3 0.048(3) 0.037(3) 0.070(4) -0.001(3) 0.002(3) 0.000(2) O4 0.038(3) 0.040(3) 0.085(4) -0.004(3) 0.002(3) 0.000(2) C9 0.058(6) 0.166(10) 0.070(7) 0.049(7) 0.001(5) -0.019(7) O9 0.084(6) 0.341(14) 0.129(7) 0.121(8) 0.026(5) -0.037(7) C10 0.069(6) 0.049(5) 0.042(5) -0.011(4) -0.013(4) 0.009(4) O10 0.110(6) 0.092(5) 0.073(4) -0.002(4) -0.025(4) 0.049(4) C11 0.132(9) 0.052(5) 0.050(6) -0.002(5) -0.014(6) 0.024(6) O11 0.301(12) 0.076(5) 0.080(5) -0.034(4) -0.066(6) 0.045(6) S11 0.0400(12) 0.0592(13) 0.0550(13) -0.0096(11) 0.0002(10) 0.0046(10) O12 0.033(3) 0.054(3) 0.061(3) -0.014(3) -0.006(2) 0.002(2) C13 0.059(5) 0.053(5) 0.073(6) 0.001(5) 0.002(5) -0.002(4) C14 0.078(6) 0.082(6) 0.047(5) -0.005(5) -0.002(5) -0.008(5) S21 0.0358(11) 0.0488(12) 0.0647(14) 0.0002(11) 0.0024(10) -0.0016(9) O22 0.042(3) 0.050(3) 0.081(4) -0.013(3) -0.011(3) 0.000(3) C23 0.073(6) 0.058(5) 0.057(5) 0.005(4) 0.003(5) -0.005(4) C24 0.052(5) 0.054(5) 0.049(5) 0.007(4) 0.001(4) -0.015(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 C11 1.811(10) . ? Cr1 C10 1.819(8) . ? Cr1 C9 1.829(10) . ? Cr1 C1 2.192(7) . ? Cr1 C2 2.202(7) . ? Cr1 C4 2.204(7) . ? Cr1 C6 2.204(6) . ? Cr1 C5 2.218(6) . ? Cr1 C3 2.211(6) . ? C1 C6 1.412(9) . ? C1 C2 1.408(8) . ? C1 C7 1.497(9) . ? O1 C7 1.209(7) . ? O2 C7 1.317(8) . ? O2 O12 2.584(6) . ? C2 C3 1.399(8) . ? C3 C4 1.426(9) . ? C4 C5 1.423(9) . ? C4 C8 1.500(9) . ? C5 C6 1.395(9) . ? C8 O3 1.210(8) . ? C8 O4 1.309(8) . ? O4 O22 2.561(6) . ? C9 O9 1.143(9) . ? C10 O10 1.168(8) . ? C11 O11 1.164(9) . ? S11 O12 1.511(5) . ? S11 C13 1.759(7) . ? S11 C14 1.764(8) . ? S21 O22 1.507(5) . ? S21 C24 1.760(6) . ? S21 C23 1.766(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Cr1 C10 87.6(3) . . ? C11 Cr1 C9 90.4(5) . . ? C10 Cr1 C9 87.1(4) . . ? C11 Cr1 C1 99.6(3) . . ? C10 Cr1 C1 167.1(3) . . ? C9 Cr1 C1 103.4(3) . . ? C11 Cr1 C2 133.4(3) . . ? C10 Cr1 C2 138.5(3) . . ? C9 Cr1 C2 86.3(3) . . ? C1 Cr1 C2 37.4(2) . . ? C11 Cr1 C4 137.5(4) . . ? C10 Cr1 C4 87.1(3) . . ? C9 Cr1 C4 131.4(4) . . ? C1 Cr1 C4 80.3(3) . . ? C2 Cr1 C4 67.5(3) . . ? C11 Cr1 C6 87.0(3) . . ? C10 Cr1 C6 133.5(3) . . ? C9 Cr1 C6 139.0(4) . . ? C1 Cr1 C6 37.5(2) . . ? C2 Cr1 C6 66.9(2) . . ? C4 Cr1 C6 67.1(2) . . ? C11 Cr1 C5 102.8(3) . . ? C10 Cr1 C5 100.7(3) . . ? C9 Cr1 C5 164.8(4) . . ? C1 Cr1 C5 67.4(2) . . ? C2 Cr1 C5 79.2(2) . . ? C4 Cr1 C5 37.5(2) . . ? C6 Cr1 C5 36.8(2) . . ? C11 Cr1 C3 165.7(3) . . ? C10 Cr1 C3 104.1(3) . . ? C9 Cr1 C3 98.3(4) . . ? C1 Cr1 C3 67.4(2) . . ? C2 Cr1 C3 37.0(2) . . ? C4 Cr1 C3 37.7(2) . . ? C6 Cr1 C3 79.0(2) . . ? C5 Cr1 C3 67.3(2) . . ? C6 C1 C2 118.9(6) . . ? C6 C1 C7 119.0(6) . . ? C2 C1 C7 122.1(6) . . ? C6 C1 Cr1 71.7(4) . . ? C2 C1 Cr1 71.7(4) . . ? C7 C1 Cr1 127.1(4) . . ? C7 O2 O12 117.1(4) . . ? C3 C2 C1 120.8(6) . . ? C3 C2 Cr1 71.9(4) . . ? C1 C2 Cr1 70.9(4) . . ? C2 C3 C4 120.0(6) . . ? C2 C3 Cr1 71.1(4) . . ? C4 C3 Cr1 70.9(4) . . ? C5 C4 C3 119.1(6) . . ? C5 C4 C8 121.5(6) . . ? C3 C4 C8 119.3(6) . . ? C5 C4 Cr1 71.8(4) . . ? C3 C4 Cr1 71.4(4) . . ? C8 C4 Cr1 125.2(5) . . ? C6 C5 C4 119.7(6) . . ? C6 C5 Cr1 71.0(4) . . ? C4 C5 Cr1 70.7(4) . . ? C5 C6 C1 121.4(6) . . ? C5 C6 Cr1 72.2(4) . . ? C1 C6 Cr1 70.8(4) . . ? O1 C7 O2 125.4(7) . . ? O1 C7 C1 122.2(6) . . ? O2 C7 C1 112.4(6) . . ? O3 C8 O4 124.8(7) . . ? O3 C8 C4 122.1(7) . . ? O4 C8 C4 113.1(6) . . ? C8 O4 O22 119.1(4) . . ? O9 C9 Cr1 179.0(12) . . ? O10 C10 Cr1 179.4(7) . . ? O11 C11 Cr1 179.2(9) . . ? O12 S11 C13 106.8(3) . . ? O12 S11 C14 106.6(3) . . ? C13 S11 C14 98.4(4) . . ? S11 O12 O2 128.9(3) . . ? O22 S21 C24 105.8(3) . . ? O22 S21 C23 106.3(3) . . ? C24 S21 C23 98.6(4) . . ? S21 O22 O4 126.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.506 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.094 #END # Data for compound 9.2DMF data_lee9998 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C11 H6 O7 Cr1 2(C3 H7 N2 O1)' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C17 H20 Cr N2 O9' _chemical_formula_weight 448.35 _chemical_melting_point ? _chemical_compound_source synthesis 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.5676(1) _cell_length_b 10.6471(1) _cell_length_c 15.3866(2) _cell_angle_alpha 79.540(1) _cell_angle_beta 77.794(1) _cell_angle_gamma 82.222(1) _cell_volume 1028.85(2) _cell_formula_units_Z 2 _cell_measurement_temperature 208(5) _cell_measurement_reflns_used 4864 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 30.20 _exptl_crystal_description needles _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 464 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7164 _exptl_absorpt_correction_T_max 0.9011 _exptl_absorpt_process_details ; Absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995), which is based upon the method of Blessing (Blessing, 1995). ; _exptl_special_details ; Data were collected with a Siemens SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 30s duration at a crystal-to-detector distance of 4.706 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 208(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART' _diffrn_measurement_method '\w-scans' _diffrn_standards_number 'see experimental' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12220 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4701 _reflns_number_gt 2980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement 'SHELXTL (Bruker, 1999)' _computing_molecular_graphics 'SHELXTL (Bruker, 1999)' _computing_publication_material 'SHELXTL (Bruker, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4701 _refine_ls_number_parameters 269 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1120 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1527 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 -0.43568(9) 0.49261(5) 0.24492(4) 0.0370(2) Uani 1 1 d . . . C1 C -0.2305(6) 0.3164(3) 0.2152(2) 0.0383(8) Uani 1 1 d . . . C2 C -0.1320(5) 0.4268(3) 0.1680(2) 0.0347(8) Uani 1 1 d . . . H2 H 0.0025 0.4369 0.1760 0.042 Uiso 1 1 calc R . . C3 C -0.2309(5) 0.5214(3) 0.1097(2) 0.0373(8) Uani 1 1 d . . . C4 C -0.4376(6) 0.5070(4) 0.1004(2) 0.0419(9) Uani 1 1 d . . . H4 H -0.5097 0.5713 0.0645 0.050 Uiso 1 1 calc R . . C5 C -0.5329(6) 0.3969(4) 0.1447(3) 0.0471(10) Uani 1 1 d . . . H5 H -0.6647 0.3847 0.1347 0.057 Uiso 1 1 calc R . . C6 C -0.4342(6) 0.3043(4) 0.2040(3) 0.0450(9) Uani 1 1 d . . . H6 H -0.5044 0.2339 0.2363 0.054 Uiso 1 1 calc R . . C7 C -0.1241(6) 0.2165(4) 0.2765(3) 0.0451(9) Uani 1 1 d . . . O1 O -0.2190(4) 0.1245(3) 0.3214(2) 0.0553(7) Uani 1 1 d . . . O2 O 0.0668(4) 0.2327(3) 0.2781(2) 0.0542(7) Uani 1 1 d . . . H2A H 0.1130 0.1749 0.3150 0.065 Uiso 1 1 calc R . . C8 C -0.1153(6) 0.6342(4) 0.0608(2) 0.0400(8) Uani 1 1 d . . . O3 O 0.0666(4) 0.6402(3) 0.06595(17) 0.0481(7) Uani 1 1 d . . . O4 O -0.2259(4) 0.7201(3) 0.01295(18) 0.0502(7) Uani 1 1 d . . . H4A H -0.1529 0.7783 -0.0141 0.060 Uiso 1 1 calc R . . C9 C -0.2806(7) 0.5547(4) 0.3136(3) 0.0518(10) Uani 1 1 d . . . O9 O -0.1815(6) 0.5939(4) 0.3542(2) 0.0813(11) Uani 1 1 d . . . C10 C -0.6150(7) 0.4314(4) 0.3503(3) 0.0522(10) Uani 1 1 d . . . O10 O -0.7267(6) 0.3956(3) 0.4164(2) 0.0781(10) Uani 1 1 d . . . C11 C -0.6099(6) 0.6452(4) 0.2416(3) 0.0467(9) Uani 1 1 d . . . O11 O -0.7202(5) 0.7401(3) 0.2411(2) 0.0682(9) Uani 1 1 d . . . N21 N 0.2755(6) -0.1511(3) 0.4435(2) 0.0524(9) Uani 1 1 d . . . C21 C 0.1712(7) -0.0506(4) 0.4039(3) 0.0534(10) Uani 1 1 d D . . O21A O 0.2529(7) 0.0534(4) 0.3728(3) 0.0621(12) Uani 0.70 1 d PD . . O21B O -0.0155(15) -0.0559(9) 0.4036(6) 0.054(2) Uiso 0.30 1 d PD . . C22 C 0.1802(10) -0.2705(5) 0.4797(4) 0.0813(16) Uani 1 1 d . . . H22A H 0.2640 -0.3401 0.4518 0.122 Uiso 1 1 calc R . . H22B H 0.0399 -0.2617 0.4671 0.122 Uiso 1 1 calc R . . H22C H 0.1733 -0.2890 0.5443 0.122 Uiso 1 1 calc R . . C23 C 0.4935(8) -0.1469(5) 0.4540(3) 0.0688(13) Uani 1 1 d . . . H23A H 0.4996 -0.1616 0.5175 0.103 Uiso 1 1 calc R . . H23B H 0.5391 -0.0634 0.4265 0.103 Uiso 1 1 calc R . . H23C H 0.5845 -0.2130 0.4249 0.103 Uiso 1 1 calc R . . N31 N 0.2819(5) 0.9928(3) -0.1257(2) 0.0443(8) Uani 1 1 d . . . C31 C 0.1621(6) 0.9077(4) -0.0742(2) 0.0436(9) Uani 1 1 d . . . H31 H 0.2215 0.8444 -0.0332 0.052 Uiso 1 1 calc R . . O31 O -0.0270(5) 0.9067(3) -0.0772(2) 0.0603(8) Uani 1 1 d . . . C32 C 0.5043(7) 0.9872(5) -0.1222(3) 0.0628(12) Uani 1 1 d . . . H32A H 0.5886 0.9664 -0.1786 0.094 Uiso 1 1 calc R . . H33B H 0.5366 0.9216 -0.0731 0.094 Uiso 1 1 calc R . . H32C H 0.5347 1.0698 -0.1128 0.094 Uiso 1 1 calc R . . C33 C 0.1971(8) 1.0974(4) -0.1888(3) 0.0622(12) Uani 1 1 d . . . H33A H 0.2167 1.1793 -0.1743 0.093 Uiso 0.73(5) 1 calc PR A 1 H32B H 0.0489 1.0915 -0.1839 0.093 Uiso 0.73(5) 1 calc PR A 1 H33C H 0.2698 1.0903 -0.2498 0.093 Uiso 0.73(5) 1 calc PR A 1 H33D H 0.3075 1.1503 -0.2203 0.093 Uiso 0.27(5) 1 d PR A 2 H33E H 0.0848 1.1494 -0.1559 0.093 Uiso 0.27(5) 1 d PR A 2 H33F H 0.1435 1.0613 -0.2320 0.093 Uiso 0.27(5) 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0348(3) 0.0367(3) 0.0364(3) -0.0061(2) -0.0020(2) 0.0004(2) C1 0.038(2) 0.0320(18) 0.044(2) -0.0088(15) -0.0036(16) -0.0017(15) C2 0.0273(17) 0.0392(19) 0.0363(18) -0.0096(15) -0.0036(14) 0.0026(14) C3 0.0339(19) 0.046(2) 0.0305(18) -0.0091(15) -0.0032(14) -0.0001(16) C4 0.035(2) 0.055(2) 0.0369(19) -0.0144(17) -0.0078(15) 0.0012(17) C5 0.0294(19) 0.063(3) 0.055(2) -0.021(2) -0.0115(17) -0.0053(18) C6 0.037(2) 0.041(2) 0.058(2) -0.0159(18) -0.0028(18) -0.0081(16) C7 0.051(2) 0.036(2) 0.046(2) -0.0109(17) -0.0004(18) -0.0028(18) O1 0.0519(17) 0.0411(15) 0.0666(19) 0.0022(14) -0.0028(14) -0.0106(13) O2 0.0442(16) 0.0471(16) 0.0652(19) 0.0146(13) -0.0155(14) -0.0075(13) C8 0.042(2) 0.046(2) 0.0283(18) -0.0061(16) -0.0050(15) 0.0044(17) O3 0.0358(15) 0.0518(16) 0.0510(16) 0.0051(12) -0.0078(12) -0.0027(12) O4 0.0449(16) 0.0530(17) 0.0470(16) 0.0097(13) -0.0127(13) -0.0028(13) C9 0.055(3) 0.050(2) 0.049(2) -0.0133(19) -0.007(2) 0.003(2) O9 0.087(3) 0.095(3) 0.080(2) -0.042(2) -0.036(2) -0.001(2) C10 0.055(3) 0.038(2) 0.053(3) -0.0008(18) 0.002(2) 0.0011(19) O10 0.086(2) 0.065(2) 0.059(2) 0.0062(16) 0.0216(18) -0.0039(18) C11 0.046(2) 0.049(2) 0.039(2) -0.0030(18) -0.0013(17) -0.0002(19) O11 0.068(2) 0.0487(18) 0.075(2) -0.0018(16) -0.0070(17) 0.0174(16) N21 0.069(2) 0.0401(18) 0.0425(19) -0.0018(15) -0.0020(17) -0.0054(17) C21 0.062(3) 0.049(2) 0.045(2) 0.0010(19) -0.011(2) -0.002(2) O21A 0.055(3) 0.047(2) 0.078(3) 0.018(2) -0.020(2) -0.008(2) C22 0.119(5) 0.047(3) 0.069(3) 0.008(2) -0.006(3) -0.021(3) C23 0.071(3) 0.059(3) 0.067(3) -0.004(2) -0.013(2) 0.016(2) N31 0.050(2) 0.0367(17) 0.0424(18) -0.0025(14) -0.0061(15) -0.0013(15) C31 0.045(2) 0.040(2) 0.041(2) -0.0066(17) -0.0029(17) 0.0050(17) O31 0.0541(19) 0.0563(18) 0.0637(19) 0.0043(15) -0.0110(15) -0.0009(15) C32 0.050(3) 0.059(3) 0.075(3) -0.006(2) -0.003(2) -0.010(2) C33 0.087(3) 0.040(2) 0.055(3) 0.0057(19) -0.016(2) -0.006(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 Cr1 C11 1.855(4) . ? Cr1 C10 1.860(4) . ? Cr1 C9 1.866(5) . ? Cr1 C2 2.189(3) . ? Cr1 C4 2.204(4) . ? Cr1 C6 2.206(4) . ? Cr1 C1 2.217(3) . ? Cr1 C3 2.220(3) . ? Cr1 C5 2.234(4) . ? C1 C6 1.410(5) . ? C1 C2 1.423(5) . ? C1 C7 1.491(5) . ? C2 C3 1.409(5) . ? C2 H2 0.9400 . ? C3 C4 1.426(5) . ? C3 C8 1.503(5) . ? C4 C5 1.400(5) . ? C4 H4 0.9400 . ? C5 C6 1.405(6) . ? C5 H5 0.9400 . ? C6 H6 0.9400 . ? C7 O1 1.250(4) . ? C7 O2 1.295(5) . ? O2 H2A 0.8300 . ? C8 O3 1.225(4) . ? C8 O4 1.307(4) . ? O4 H4A 0.8300 . ? C9 O9 1.153(5) . ? C10 O10 1.156(5) . ? C11 O11 1.161(5) . ? N21 C21 1.314(5) . ? N21 C22 1.459(6) . ? N21 C23 1.482(6) . ? C21 O21B 1.236(9) . ? C21 O21A 1.266(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 H22C 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 H23C 0.9700 . ? N31 C31 1.318(5) . ? N31 C32 1.466(5) . ? N31 C33 1.470(5) . ? C31 O31 1.254(5) . ? C31 H31 0.9400 . ? C32 H32A 0.9700 . ? C32 H33B 0.9700 . ? C32 H32C 0.9700 . ? C33 H33A 0.9700 . ? C33 H32B 0.9700 . ? C33 H33C 0.9700 . ? C33 H33D 0.9700 . ? C33 H33E 0.9700 . ? C33 H33F 0.9700 . ? 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 C11 Cr1 C10 87.47(17) . . ? C11 Cr1 C9 89.76(18) . . ? C10 Cr1 C9 89.29(19) . . ? C11 Cr1 C2 135.37(15) . . ? C10 Cr1 C2 136.68(15) . . ? C9 Cr1 C2 85.58(16) . . ? C11 Cr1 C4 86.77(15) . . ? C10 Cr1 C4 134.20(18) . . ? C9 Cr1 C4 136.04(17) . . ? C2 Cr1 C4 67.36(13) . . ? C11 Cr1 C6 135.87(16) . . ? C10 Cr1 C6 86.69(17) . . ? C9 Cr1 C6 133.82(16) . . ? C2 Cr1 C6 67.21(14) . . ? C4 Cr1 C6 67.16(15) . . ? C11 Cr1 C1 166.65(15) . . ? C10 Cr1 C1 101.87(15) . . ? C9 Cr1 C1 99.76(16) . . ? C2 Cr1 C1 37.67(13) . . ? C4 Cr1 C1 79.88(14) . . ? C6 Cr1 C1 37.18(13) . . ? C11 Cr1 C3 101.39(15) . . ? C10 Cr1 C3 166.23(16) . . ? C9 Cr1 C3 101.15(16) . . ? C2 Cr1 C3 37.25(12) . . ? C4 Cr1 C3 37.60(13) . . ? C6 Cr1 C3 79.61(14) . . ? C1 Cr1 C3 67.74(13) . . ? C11 Cr1 C5 102.47(16) . . ? C10 Cr1 C5 101.36(18) . . ? C9 Cr1 C5 164.02(16) . . ? C2 Cr1 C5 78.49(13) . . ? C4 Cr1 C5 36.77(14) . . ? C6 Cr1 C5 36.89(15) . . ? C1 Cr1 C5 66.59(14) . . ? C3 Cr1 C5 66.63(14) . . ? C6 C1 C2 118.4(3) . . ? C6 C1 C7 120.3(3) . . ? C2 C1 C7 121.3(3) . . ? C6 C1 Cr1 71.0(2) . . ? C2 C1 Cr1 70.12(19) . . ? C7 C1 Cr1 129.5(3) . . ? C3 C2 C1 121.7(3) . . ? C3 C2 Cr1 72.57(19) . . ? C1 C2 Cr1 72.2(2) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? Cr1 C2 H2 128.4 . . ? C2 C3 C4 118.5(3) . . ? C2 C3 C8 118.7(3) . . ? C4 C3 C8 122.8(3) . . ? C2 C3 Cr1 70.18(19) . . ? C4 C3 Cr1 70.6(2) . . ? C8 C3 Cr1 130.3(2) . . ? C5 C4 C3 119.9(3) . . ? C5 C4 Cr1 72.8(2) . . ? C3 C4 Cr1 71.81(19) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? Cr1 C4 H4 127.4 . . ? C4 C5 C6 120.9(3) . . ? C4 C5 Cr1 70.5(2) . . ? C6 C5 Cr1 70.5(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? Cr1 C5 H5 132.6 . . ? C5 C6 C1 120.4(3) . . ? C5 C6 Cr1 72.6(2) . . ? C1 C6 Cr1 71.8(2) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? Cr1 C6 H6 128.0 . . ? O1 C7 O2 124.5(4) . . ? O1 C7 C1 120.0(4) . . ? O2 C7 C1 115.5(3) . . ? C7 O2 H2A 109.5 . . ? O3 C8 O4 125.0(3) . . ? O3 C8 C3 121.3(3) . . ? O4 C8 C3 113.7(3) . . ? C8 O4 H4A 109.5 . . ? O9 C9 Cr1 178.4(4) . . ? O10 C10 Cr1 178.7(4) . . ? O11 C11 Cr1 178.8(4) . . ? C21 N21 C22 121.3(4) . . ? C21 N21 C23 121.2(4) . . ? C22 N21 C23 117.5(4) . . ? O21B C21 O21A 119.8(6) . . ? O21B C21 N21 118.5(6) . . ? O21A C21 N21 121.5(4) . . ? N21 C22 H22A 109.5 . . ? N21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N21 C23 H23A 109.5 . . ? N21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C31 N31 C32 121.4(3) . . ? C31 N31 C33 121.2(3) . . ? C32 N31 C33 117.4(3) . . ? O31 C31 N31 123.4(4) . . ? O31 C31 H31 118.3 . . ? N31 C31 H31 118.3 . . ? N31 C32 H32A 109.5 . . ? N31 C32 H33B 109.5 . . ? H32A C32 H33B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H33B C32 H32C 109.5 . . ? N31 C33 H33A 109.5 . . ? N31 C33 H32B 109.5 . . ? H33A C33 H32B 109.5 . . ? N31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H32B C33 H33C 109.5 . . ? N31 C33 H33D 109.4 . . ? H33A C33 H33D 55.0 . . ? H32B C33 H33D 141.1 . . ? H33C C33 H33D 57.5 . . ? N31 C33 H33E 109.7 . . ? H33A C33 H33E 57.5 . . ? H32B C33 H33E 54.9 . . ? H33C C33 H33E 140.9 . . ? H33D C33 H33E 109.5 . . ? N31 C33 H33F 109.4 . . ? H33A C33 H33F 141.1 . . ? H32B C33 H33F 57.6 . . ? H33C C33 H33F 54.9 . . ? H33D C33 H33F 109.5 . . ? H33E C33 H33F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.649 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.069 #END # Data for compound 10.n-Bu2O data_l15198 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H24 Cr O10' _chemical_formula_weight 476.39 _chemical_melting_point ? _chemical_compound_source 'synthesis' 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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6029(3) _cell_length_b 13.0537(2) _cell_length_c 15.2638(2) _cell_angle_alpha 87.472(1) _cell_angle_beta 75.734(1) _cell_angle_gamma 86.752(1) _cell_volume 2235.89(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5704 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 29.66 _exptl_crystal_description Irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method ? _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type 'empirical: SADABS' _exptl_absorpt_correction_T_min 0.473 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details ; Absorption correction was based upon symmetry equivalent and repeated intensity measurements using the program SADABS (Sheldrick, 1995), which is based upon the method of Blessing (Blessing, 1995). ; _exptl_special_details ; Data were collected with a Siemens SMART CCD-based diffractometer using /w-scans of width 0.3 deg. and 50s duration at a crystal-to-detector distance of 4.942 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted. ; _diffrn_ambient_temperature 173(5) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18389 _diffrn_reflns_av_R_equivalents 0.1250 _diffrn_reflns_av_sigmaI/netI 0.1370 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5833 _reflns_number_observed 3651 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1994)' _computing_data_reduction 'SAINT (Siemens, 1994)' _computing_structure_solution 'SHELXTL (Siemens, 1994)' _computing_structure_refinement 'SHELXTL (Siemens, 1994)' _computing_molecular_graphics 'SHELXTL (Siemens, 1994)' _computing_publication_material 'SHELXTL (Siemens, 1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 326 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1281P)^2^+10.8240P] 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 ; Arene hydrogen atoms were included in calculated positions, whereas carboxyl hydrogen atoms were located directly from the difference map. Both types were then refined by using riding models. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5507 _refine_ls_number_parameters 559 _refine_ls_number_restraints 108 _refine_ls_R_factor_all 0.1643 _refine_ls_R_factor_obs 0.1101 _refine_ls_wR_factor_all 0.3001 _refine_ls_wR_factor_obs 0.2674 _refine_ls_goodness_of_fit_all 1.145 _refine_ls_goodness_of_fit_obs 1.328 _refine_ls_restrained_S_all 1.151 _refine_ls_restrained_S_obs 1.307 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cr1 Cr 1.1149(2) 0.55811(13) -0.29278(11) 0.0230(5) Uani 1 d . . C10 C 1.2706(11) 0.5051(10) -0.3403(8) 0.035(3) Uani 1 d U . C11 C 1.1810(11) 0.6772(12) -0.2648(8) 0.041(3) Uani 1 d U . C12 C 1.1225(11) 0.5004(10) -0.1798(8) 0.038(3) Uani 1 d U . O10 O 1.3659(8) 0.4737(7) -0.3657(6) 0.050(3) Uani 1 d U . O11 O 1.2194(8) 0.7509(7) -0.2493(7) 0.056(3) Uani 1 d U . O12 O 1.1261(10) 0.4627(9) -0.1108(7) 0.071(3) Uani 1 d U . C13 C 1.0614(9) 0.6104(8) -0.4155(6) 0.019(2) Uani 1 d U . C14 C 0.9923(9) 0.6641(8) -0.3409(6) 0.021(2) Uani 1 d U . H14 H 0.9893(9) 0.7370(8) -0.3423(6) 0.025 Uiso 1 calc R . C15 C 0.9271(9) 0.6094(8) -0.2637(7) 0.021(2) Uani 1 d U . C16 C 0.9351(9) 0.5033(8) -0.2634(7) 0.021(2) Uani 1 d U . H16 H 0.8922(9) 0.4672(8) -0.2112(7) 0.025 Uiso 1 calc R . C17 C 1.0041(9) 0.4446(8) -0.3369(7) 0.021(2) Uani 1 d U . C18 C 1.0703(9) 0.5037(8) -0.4124(7) 0.021(2) Uani 1 d U . H18 H 1.1217(9) 0.4689(8) -0.4615(7) 0.025 Uiso 1 calc R . C131 C 1.1402(9) 0.6662(8) -0.4963(7) 0.021(3) Uani 1 d . . O132 O 1.1340(6) 0.7658(5) -0.4905(4) 0.026(2) Uani 1 d . . H132 H 1.1871(6) 0.8142(5) -0.5465(4) 0.031 Uiso 1 d R . O133 O 1.1976(7) 0.6181(6) -0.5606(5) 0.031(2) Uani 1 d . . C151 C 0.8576(10) 0.6657(9) -0.1834(7) 0.023(3) Uani 1 d . . O152 O 0.8579(7) 0.7629(6) -0.1922(5) 0.035(2) Uani 1 d . . H152 H 0.8207(7) 0.8043(6) -0.1377(5) 0.042 Uiso 1 d R . O153 O 0.8050(7) 0.6170(6) -0.1168(5) 0.033(2) Uani 1 d . . C171 C 1.0157(10) 0.3334(8) -0.3383(7) 0.025(3) Uani 1 d . . O172 O 0.9534(7) 0.2894(6) -0.2624(5) 0.037(2) Uani 1 d . . H172 H 0.9668(7) 0.2142(6) -0.2544(5) 0.044 Uiso 1 d R . O173 O 1.0694(7) 0.2865(6) -0.4031(5) 0.038(2) Uani 1 d . . C101 C 0.9867(16) 0.2583(14) 0.0072(11) 0.084(6) Uani 1 d . . H10A H 1.0663(16) 0.2700(14) 0.0150(11) 0.127 Uiso 1 calc R . H10B H 0.9350(16) 0.2375(14) 0.0655(11) 0.127 Uiso 1 calc R . H10C H 0.9534(16) 0.3218(14) -0.0155(11) 0.127 Uiso 1 calc R . C102 C 0.9952(14) 0.1763(12) -0.0583(9) 0.059(4) Uani 1 d . . H10D H 1.0311(14) 0.1132(12) -0.0355(9) 0.070 Uiso 1 calc R . H10E H 1.0494(14) 0.1974(12) -0.1163(9) 0.070 Uiso 1 calc R . C103 C 0.8770(13) 0.1510(11) -0.0761(8) 0.051(4) Uani 1 d . . H10F H 0.8207(13) 0.1359(11) -0.0174(8) 0.061 Uiso 1 calc R . H10G H 0.8444(13) 0.2127(11) -0.1035(8) 0.061 Uiso 1 calc R . C104 C 0.8813(12) 0.0635(11) -0.1358(9) 0.052(4) Uani 1 d . . H10H H 0.9183(12) 0.0022(11) -0.1112(9) 0.063 Uiso 1 calc R . H10I H 0.7992(12) 0.0476(11) -0.1367(9) 0.063 Uiso 1 calc R . O105 O 0.9484(7) 0.0857(6) -0.2270(5) 0.038(2) Uani 1 d . . C106 C 0.9593(12) 0.0002(9) -0.2832(9) 0.041(3) Uani 1 d . . H10J H 0.8790(12) -0.0217(9) -0.2830(9) 0.049 Uiso 1 calc R . H10K H 1.0018(12) -0.0577(9) -0.2584(9) 0.049 Uiso 1 calc R . C107 C 1.0258(12) 0.0249(10) -0.3787(9) 0.045(4) Uani 1 d . . H10L H 0.9887(12) 0.0884(10) -0.3998(9) 0.054 Uiso 1 calc R . H10M H 1.0155(12) -0.0312(10) -0.4174(9) 0.054 Uiso 1 calc R . C108 C 1.1572(12) 0.0395(11) -0.3931(10) 0.052(4) Uani 1 d . . H10N H 1.1960(12) -0.0244(11) -0.3743(10) 0.062 Uiso 1 calc R . H10O H 1.1688(12) 0.0952(11) -0.3546(10) 0.062 Uiso 1 calc R . C109 C 1.2161(13) 0.0663(11) -0.4917(9) 0.056(4) Uani 1 d . . H10P H 1.3012(13) 0.0751(11) -0.4982(9) 0.085 Uiso 1 calc R . H10Q H 1.1790(13) 0.1302(11) -0.5102(9) 0.085 Uiso 1 calc R . H10R H 1.2061(13) 0.0107(11) -0.5299(9) 0.085 Uiso 1 calc R . Cr2 Cr 0.5886(2) 0.91291(13) 0.21254(11) 0.0238(5) Uani 1 d . . C20 C 0.7301(11) 0.9842(9) 0.1790(8) 0.031(3) Uani 1 d U . C21 C 0.6777(12) 0.7994(10) 0.2457(8) 0.039(3) Uani 1 d U . C22 C 0.5634(11) 0.9636(10) 0.3293(8) 0.040(3) Uani 1 d U . O20 O 0.8138(9) 1.0305(7) 0.1600(6) 0.056(3) Uani 1 d U . O22 O 0.5450(9) 0.9966(9) 0.3998(6) 0.070(3) Uani 1 d U . O21 O 0.7345(9) 0.7308(8) 0.2651(7) 0.064(3) Uani 1 d U . C23 C 0.5669(10) 0.8610(8) 0.0837(7) 0.025(2) Uani 1 d U . C24 C 0.4925(9) 0.8049(8) 0.1558(7) 0.024(2) Uani 1 d U . H24 H 0.4990(9) 0.7320(8) 0.1581(7) 0.029 Uiso 1 calc R . C25 C 0.4088(9) 0.8581(8) 0.2241(7) 0.021(2) Uani 1 d U . C26 C 0.4035(9) 0.9664(8) 0.2238(7) 0.023(2) Uani 1 d U . H26 H 0.3509(9) 1.0016(8) 0.2719(7) 0.028 Uiso 1 calc R . C27 C 0.4767(9) 1.0226(8) 0.1514(6) 0.021(2) Uani 1 d U . C28 C 0.5582(10) 0.9674(8) 0.0831(7) 0.025(2) Uani 1 d U . H28 H 0.6087(10) 1.0045(8) 0.0352(7) 0.030 Uiso 1 calc R . C231 C 0.6577(10) 0.8035(9) 0.0126(7) 0.021(3) Uani 1 d . . O232 O 0.6639(7) 0.7071(6) 0.0227(5) 0.034(2) Uani 1 d . . H232 H 0.6991(7) 0.6611(6) -0.0190(5) 0.041 Uiso 1 d R . O233 O 0.7217(7) 0.8548(5) -0.0520(5) 0.035(2) Uani 1 d . . C251 C 0.3328(9) 0.8015(9) 0.3022(7) 0.027(3) Uani 1 d . . O252 O 0.3453(7) 0.7026(6) 0.3000(5) 0.035(2) Uani 1 d . . H252 H 0.2931(7) 0.6555(6) 0.3543(5) 0.042 Uiso 1 d R . O253 O 0.2646(7) 0.8492(6) 0.3627(5) 0.037(2) Uani 1 d . . C271 C 0.4770(10) 1.1356(9) 0.1518(7) 0.027(3) Uani 1 d . . O272 O 0.4047(7) 1.1740(6) 0.2266(5) 0.039(2) Uani 1 d . . H272 H 0.4017(7) 1.2501(6) 0.2343(5) 0.046 Uiso 1 d R . O273 O 0.5339(8) 1.1873(6) 0.0895(5) 0.041(2) Uani 1 d . . C201 C 0.5530(14) 1.2689(13) 0.4900(11) 0.078(5) Uani 1 d . . H20A H 0.6192(14) 1.2177(13) 0.4742(11) 0.117 Uiso 1 calc R . H20B H 0.5015(14) 1.2504(13) 0.5491(11) 0.117 Uiso 1 calc R . H20C H 0.5845(14) 1.3365(13) 0.4927(11) 0.117 Uiso 1 calc R . C202 C 0.4812(12) 1.2725(12) 0.4185(10) 0.058(4) Uani 1 d . . H20D H 0.5343(12) 1.2896(12) 0.3588(10) 0.070 Uiso 1 calc R . H20E H 0.4514(12) 1.2036(12) 0.4152(10) 0.070 Uiso 1 calc R . C203 C 0.3776(11) 1.3494(11) 0.4375(9) 0.044(3) Uani 1 d . . H20F H 0.3291(11) 1.3361(11) 0.4997(9) 0.053 Uiso 1 calc R . H20G H 0.4085(11) 1.4189(11) 0.4354(9) 0.053 Uiso 1 calc R . C204 C 0.2991(11) 1.3485(11) 0.3737(8) 0.044(4) Uani 1 d . . H20H H 0.2586(11) 1.2827(11) 0.3822(8) 0.053 Uiso 1 calc R . H20I H 0.2369(11) 1.4045(11) 0.3888(8) 0.053 Uiso 1 calc R . O205 O 0.3632(8) 1.3612(6) 0.2777(5) 0.041(2) Uani 1 d . . C206 C 0.3890(12) 1.4660(10) 0.2510(9) 0.045(4) Uani 1 d . . H20J H 0.4338(12) 1.4951(10) 0.2907(9) 0.054 Uiso 1 calc R . H20K H 0.3144(12) 1.5082(10) 0.2548(9) 0.054 Uiso 1 calc R . C207 C 0.4638(13) 1.4642(10) 0.1533(10) 0.053(4) Uani 1 d . . H20L H 0.4253(13) 1.4215(10) 0.1178(10) 0.064 Uiso 1 calc R . H20M H 0.4658(13) 1.5349(10) 0.1268(10) 0.064 Uiso 1 calc R . C208 C 0.5890(12) 1.4229(12) 0.1455(8) 0.052(4) Uani 1 d . . H20N H 0.5876(12) 1.3537(12) 0.1748(8) 0.062 Uiso 1 calc R . H20O H 0.6297(12) 1.4680(12) 0.1776(8) 0.062 Uiso 1 calc R . C209 C 0.6599(14) 1.4164(12) 0.0449(10) 0.066(5) Uani 1 d . . H20P H 0.7411(14) 1.3892(12) 0.0421(10) 0.099 Uiso 1 calc R . H20Q H 0.6626(14) 1.4851(12) 0.0160(10) 0.099 Uiso 1 calc R . H20R H 0.6205(14) 1.3709(12) 0.0133(10) 0.099 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0201(10) 0.0291(11) 0.0156(10) 0.0000(8) 0.0048(8) -0.0069(8) C10 0.020(8) 0.054(9) 0.031(7) 0.005(6) -0.004(6) -0.004(7) C11 0.029(8) 0.065(10) 0.021(7) -0.006(7) 0.009(6) 0.009(7) C12 0.042(8) 0.048(8) 0.026(7) 0.019(6) -0.011(6) -0.015(7) O10 0.028(6) 0.060(6) 0.064(6) -0.022(5) -0.013(5) 0.010(5) O11 0.049(6) 0.041(6) 0.081(7) -0.014(5) -0.016(5) -0.020(5) O12 0.073(8) 0.097(9) 0.048(7) 0.033(6) -0.023(6) -0.033(6) C13 0.015(5) 0.027(5) 0.013(5) -0.001(4) 0.003(4) -0.008(4) C14 0.018(5) 0.028(5) 0.014(5) 0.001(4) 0.002(4) -0.002(4) C15 0.016(5) 0.030(5) 0.012(4) -0.001(4) 0.010(4) -0.010(4) C16 0.014(5) 0.032(5) 0.011(4) 0.002(4) 0.011(4) -0.006(4) C17 0.013(5) 0.035(5) 0.013(4) 0.000(4) 0.001(4) -0.005(4) C18 0.014(5) 0.032(5) 0.015(5) -0.005(4) 0.003(4) -0.009(4) C131 0.019(6) 0.027(7) 0.013(6) 0.003(5) 0.003(5) 0.001(5) O132 0.027(5) 0.023(5) 0.017(4) 0.008(3) 0.016(3) -0.003(3) O133 0.034(5) 0.030(5) 0.015(4) 0.000(4) 0.021(4) -0.011(4) C151 0.017(6) 0.028(7) 0.024(7) 0.000(5) -0.003(5) -0.004(5) O152 0.037(5) 0.030(5) 0.027(5) 0.000(4) 0.018(4) -0.008(4) O153 0.036(5) 0.037(5) 0.016(4) 0.000(4) 0.012(4) -0.011(4) C171 0.026(7) 0.026(7) 0.017(6) 0.002(5) 0.011(5) -0.008(5) O172 0.047(5) 0.023(4) 0.027(5) 0.002(4) 0.017(4) -0.007(4) O173 0.046(5) 0.026(5) 0.036(5) -0.003(4) 0.005(4) -0.003(4) C101 0.074(13) 0.113(16) 0.059(11) 0.001(11) 0.001(9) -0.019(11) C102 0.060(11) 0.084(12) 0.030(8) -0.002(8) -0.004(7) -0.020(9) C103 0.052(10) 0.066(10) 0.025(7) 0.011(7) 0.009(7) -0.011(8) C104 0.037(8) 0.068(10) 0.045(9) 0.010(8) 0.005(7) -0.021(7) O105 0.046(6) 0.036(5) 0.024(5) 0.003(4) 0.010(4) -0.016(4) C106 0.038(8) 0.023(7) 0.065(10) 0.012(7) -0.016(7) -0.010(6) C107 0.049(9) 0.044(8) 0.045(8) -0.003(7) -0.018(7) -0.003(7) C108 0.046(9) 0.044(9) 0.061(10) -0.011(7) -0.001(8) -0.012(7) C109 0.059(10) 0.057(10) 0.050(9) -0.012(7) -0.007(8) 0.002(8) Cr2 0.0223(11) 0.0287(11) 0.0140(10) 0.0025(8) 0.0077(8) -0.0031(8) C20 0.026(7) 0.036(7) 0.029(7) 0.005(6) -0.007(6) -0.001(6) C21 0.035(8) 0.039(8) 0.034(8) 0.000(6) 0.011(6) -0.014(7) C22 0.036(8) 0.062(9) 0.021(7) -0.008(7) -0.004(6) 0.004(7) O20 0.044(6) 0.060(6) 0.060(6) 0.012(5) 0.001(5) -0.034(5) O22 0.056(7) 0.121(9) 0.035(6) -0.034(6) -0.015(5) 0.018(6) O21 0.054(7) 0.043(6) 0.087(8) 0.018(6) -0.013(6) 0.017(5) C23 0.024(5) 0.026(5) 0.017(5) 0.000(4) 0.009(4) -0.007(4) C24 0.023(5) 0.024(5) 0.019(5) 0.004(4) 0.005(4) -0.003(4) C25 0.018(5) 0.022(5) 0.015(5) 0.000(4) 0.009(4) -0.004(4) C26 0.021(5) 0.031(5) 0.010(4) -0.006(4) 0.012(4) 0.003(4) C27 0.024(5) 0.029(5) 0.006(4) 0.002(4) 0.005(4) -0.001(4) C28 0.028(5) 0.031(5) 0.010(5) 0.004(4) 0.008(4) -0.008(4) C231 0.026(7) 0.024(7) 0.012(6) -0.011(5) -0.003(5) 0.004(5) O232 0.050(6) 0.020(5) 0.017(4) -0.006(3) 0.024(4) 0.002(4) O233 0.045(5) 0.024(4) 0.020(4) 0.005(4) 0.026(4) -0.009(4) C251 0.014(6) 0.033(8) 0.025(7) 0.001(6) 0.012(5) -0.001(5) O252 0.035(5) 0.024(5) 0.028(5) 0.001(4) 0.026(4) -0.010(4) O253 0.035(5) 0.037(5) 0.024(5) 0.001(4) 0.020(4) -0.004(4) C271 0.029(7) 0.033(7) 0.016(6) 0.002(6) 0.000(6) -0.001(6) O272 0.048(6) 0.026(5) 0.035(5) -0.005(4) 0.003(4) 0.001(4) O273 0.055(6) 0.031(5) 0.028(5) 0.006(4) 0.008(4) -0.011(4) C201 0.051(11) 0.095(13) 0.088(13) 0.030(10) -0.019(10) -0.013(10) C202 0.034(9) 0.081(11) 0.060(10) 0.000(8) -0.014(8) -0.003(8) C203 0.033(8) 0.063(9) 0.039(8) -0.016(7) -0.011(6) -0.003(7) C204 0.025(7) 0.056(9) 0.048(9) -0.020(7) -0.002(7) 0.005(6) O205 0.047(6) 0.032(5) 0.042(5) -0.006(4) -0.006(4) -0.002(4) C206 0.038(8) 0.037(8) 0.059(9) -0.012(7) -0.004(7) -0.013(6) C207 0.053(10) 0.037(8) 0.083(12) 0.013(8) -0.038(9) -0.021(7) C208 0.045(9) 0.072(10) 0.036(8) 0.014(7) -0.004(7) -0.021(8) C209 0.066(11) 0.067(11) 0.055(10) 0.013(8) 0.004(8) -0.021(9) _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 C12 1.871(12) . ? Cr1 C10 1.878(13) . ? Cr1 C11 1.88(2) . ? Cr1 C14 2.163(11) . ? Cr1 C18 2.173(10) . ? Cr1 C16 2.178(10) . ? Cr1 C13 2.184(10) . ? Cr1 C15 2.185(11) . ? Cr1 C17 2.244(10) . ? C10 O10 1.136(14) . ? C11 O11 1.141(15) . ? C12 O12 1.153(13) . ? C13 C18 1.390(14) . ? C13 C14 1.410(14) . ? C13 C131 1.526(14) . ? C14 C15 1.421(14) . ? C15 C16 1.382(14) . ? C15 C151 1.490(15) . ? C16 C17 1.433(14) . ? C17 C18 1.437(14) . ? C17 C171 1.451(15) . ? C131 O133 1.220(12) . ? C131 O132 1.304(12) . ? C151 O153 1.221(12) . ? C151 O152 1.270(13) . ? C171 O173 1.202(12) . ? C171 O172 1.331(12) . ? C101 C102 1.48(2) . ? C102 C103 1.52(2) . ? C103 C104 1.48(2) . ? C104 O105 1.443(14) . ? O105 C106 1.418(14) . ? C106 C107 1.50(2) . ? C107 C108 1.51(2) . ? C108 C109 1.53(2) . ? Cr2 C22 1.877(13) . ? Cr2 C21 1.88(2) . ? Cr2 C20 1.882(13) . ? Cr2 C28 2.174(11) . ? Cr2 C24 2.178(11) . ? Cr2 C23 2.184(11) . ? Cr2 C26 2.189(11) . ? Cr2 C25 2.207(10) . ? Cr2 C27 2.208(11) . ? C20 O20 1.142(13) . ? C21 O21 1.153(14) . ? C22 O22 1.144(13) . ? C23 C28 1.386(15) . ? C23 C24 1.423(14) . ? C23 C231 1.507(14) . ? C24 C25 1.414(14) . ? C25 C26 1.410(14) . ? C25 C251 1.491(14) . ? C26 C27 1.420(14) . ? C27 C28 1.415(14) . ? C27 C271 1.48(2) . ? C231 O232 1.261(12) . ? C231 O233 1.268(12) . ? C251 O253 1.226(12) . ? C251 O252 1.292(13) . ? C271 O273 1.217(13) . ? C271 O272 1.337(13) . ? C201 C202 1.53(2) . ? C202 C203 1.50(2) . ? C203 C204 1.49(2) . ? C204 O205 1.478(14) . ? O205 C206 1.437(14) . ? C206 C207 1.53(2) . ? C207 C208 1.50(2) . ? C208 C209 1.56(2) . ? 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 C12 Cr1 C10 88.8(5) . . ? C12 Cr1 C11 89.2(5) . . ? C10 Cr1 C11 88.0(5) . . ? C12 Cr1 C14 134.9(5) . . ? C10 Cr1 C14 135.4(5) . . ? C11 Cr1 C14 84.8(5) . . ? C12 Cr1 C18 135.4(5) . . ? C10 Cr1 C18 87.4(5) . . ? C11 Cr1 C18 135.1(5) . . ? C14 Cr1 C18 68.1(4) . . ? C12 Cr1 C16 86.2(5) . . ? C10 Cr1 C16 137.4(5) . . ? C11 Cr1 C16 134.1(4) . . ? C14 Cr1 C16 67.4(4) . . ? C18 Cr1 C16 67.7(4) . . ? C12 Cr1 C13 165.6(5) . . ? C10 Cr1 C13 101.6(4) . . ? C11 Cr1 C13 100.9(5) . . ? C14 Cr1 C13 37.8(4) . . ? C18 Cr1 C13 37.2(4) . . ? C16 Cr1 C13 79.4(4) . . ? C12 Cr1 C15 100.1(5) . . ? C10 Cr1 C15 168.1(4) . . ? C11 Cr1 C15 99.9(5) . . ? C14 Cr1 C15 38.1(4) . . ? C18 Cr1 C15 80.7(4) . . ? C16 Cr1 C15 36.9(4) . . ? C13 Cr1 C15 68.3(4) . . ? C12 Cr1 C17 100.5(5) . . ? C10 Cr1 C17 102.5(5) . . ? C11 Cr1 C17 165.7(5) . . ? C14 Cr1 C17 80.9(4) . . ? C18 Cr1 C17 37.9(4) . . ? C16 Cr1 C17 37.8(4) . . ? C13 Cr1 C17 67.8(4) . . ? C15 Cr1 C17 68.2(4) . . ? O10 C10 Cr1 177.2(11) . . ? O11 C11 Cr1 178.0(12) . . ? O12 C12 Cr1 178.2(12) . . ? C18 C13 C14 120.2(9) . . ? C18 C13 C131 117.9(9) . . ? C14 C13 C131 121.5(9) . . ? C18 C13 Cr1 71.0(6) . . ? C14 C13 Cr1 70.3(6) . . ? C131 C13 Cr1 125.2(7) . . ? C13 C14 C15 120.1(10) . . ? C13 C14 Cr1 71.9(6) . . ? C15 C14 Cr1 71.8(6) . . ? C16 C15 C14 118.4(9) . . ? C16 C15 C151 121.2(9) . . ? C14 C15 C151 120.3(10) . . ? C16 C15 Cr1 71.3(6) . . ? C14 C15 Cr1 70.1(6) . . ? C151 C15 Cr1 127.3(7) . . ? C15 C16 C17 124.0(9) . . ? C15 C16 Cr1 71.8(6) . . ? C17 C16 Cr1 73.6(6) . . ? C16 C17 C18 115.3(10) . . ? C16 C17 C171 125.4(9) . . ? C18 C17 C171 119.3(9) . . ? C16 C17 Cr1 68.6(6) . . ? C18 C17 Cr1 68.4(6) . . ? C171 C17 Cr1 130.6(8) . . ? C13 C18 C17 121.9(9) . . ? C13 C18 Cr1 71.8(6) . . ? C17 C18 Cr1 73.7(6) . . ? O133 C131 O132 125.6(9) . . ? O133 C131 C13 120.2(10) . . ? O132 C131 C13 114.1(9) . . ? O153 C151 O152 125.8(10) . . ? O153 C151 C15 119.2(10) . . ? O152 C151 C15 115.0(10) . . ? O173 C171 O172 123.9(10) . . ? O173 C171 C17 123.6(9) . . ? O172 C171 C17 112.4(9) . . ? C101 C102 C103 114.5(13) . . ? C104 C103 C102 115.6(12) . . ? O105 C104 C103 111.8(10) . . ? C106 O105 C104 112.2(9) . . ? O105 C106 C107 111.8(9) . . ? C106 C107 C108 115.8(11) . . ? C107 C108 C109 111.9(12) . . ? C22 Cr2 C21 90.0(5) . . ? C22 Cr2 C20 88.6(5) . . ? C21 Cr2 C20 88.3(5) . . ? C22 Cr2 C28 137.0(5) . . ? C21 Cr2 C28 132.3(5) . . ? C20 Cr2 C28 85.9(5) . . ? C22 Cr2 C24 131.9(5) . . ? C21 Cr2 C24 87.6(5) . . ? C20 Cr2 C24 139.2(4) . . ? C28 Cr2 C24 67.7(4) . . ? C22 Cr2 C23 164.8(5) . . ? C21 Cr2 C23 99.7(5) . . ? C20 Cr2 C23 103.3(4) . . ? C28 Cr2 C23 37.1(4) . . ? C24 Cr2 C23 38.1(4) . . ? C22 Cr2 C26 84.3(5) . . ? C21 Cr2 C26 140.3(5) . . ? C20 Cr2 C26 130.6(5) . . ? C28 Cr2 C26 67.9(4) . . ? C24 Cr2 C26 68.3(4) . . ? C23 Cr2 C26 80.7(4) . . ? C22 Cr2 C25 98.2(5) . . ? C21 Cr2 C25 105.6(5) . . ? C20 Cr2 C25 164.4(4) . . ? C28 Cr2 C25 79.4(4) . . ? C24 Cr2 C25 37.6(4) . . ? C23 Cr2 C25 67.9(4) . . ? C26 Cr2 C25 37.4(4) . . ? C22 Cr2 C27 101.5(5) . . ? C21 Cr2 C27 167.2(5) . . ? C20 Cr2 C27 97.5(4) . . ? C28 Cr2 C27 37.7(4) . . ? C24 Cr2 C27 80.6(4) . . ? C23 Cr2 C27 67.9(4) . . ? C26 Cr2 C27 37.7(4) . . ? C25 Cr2 C27 67.5(4) . . ? O20 C20 Cr2 177.6(11) . . ? O21 C21 Cr2 178.5(11) . . ? O22 C22 Cr2 177.7(11) . . ? C28 C23 C24 119.2(9) . . ? C28 C23 C231 121.5(9) . . ? C24 C23 C231 119.2(10) . . ? C28 C23 Cr2 71.1(6) . . ? C24 C23 Cr2 70.7(6) . . ? C231 C23 Cr2 127.5(8) . . ? C25 C24 C23 119.7(10) . . ? C25 C24 Cr2 72.3(6) . . ? C23 C24 Cr2 71.2(6) . . ? C26 C25 C24 120.3(9) . . ? C26 C25 C251 118.6(9) . . ? C24 C25 C251 120.8(9) . . ? C26 C25 Cr2 70.6(6) . . ? C24 C25 Cr2 70.1(6) . . ? C251 C25 Cr2 127.6(8) . . ? C25 C26 C27 120.0(9) . . ? C25 C26 Cr2 72.0(6) . . ? C27 C26 Cr2 71.9(6) . . ? C28 C27 C26 118.4(10) . . ? C28 C27 C271 120.3(9) . . ? C26 C27 C271 121.0(9) . . ? C28 C27 Cr2 69.9(6) . . ? C26 C27 Cr2 70.4(6) . . ? C271 C27 Cr2 126.3(7) . . ? C23 C28 C27 122.2(10) . . ? C23 C28 Cr2 71.8(6) . . ? C27 C28 Cr2 72.5(6) . . ? O232 C231 O233 125.2(9) . . ? O232 C231 C23 116.6(9) . . ? O233 C231 C23 118.2(10) . . ? O253 C251 O252 124.6(10) . . ? O253 C251 C25 119.9(10) . . ? O252 C251 C25 115.4(9) . . ? O273 C271 O272 124.4(11) . . ? O273 C271 C27 123.3(10) . . ? O272 C271 C27 112.3(9) . . ? C203 C202 C201 113.0(13) . . ? C204 C203 C202 114.5(11) . . ? O205 C204 C203 113.7(10) . . ? C206 O205 C204 113.1(9) . . ? O205 C206 C207 106.3(10) . . ? C208 C207 C206 113.1(11) . . ? C207 C208 C209 111.5(12) . . ? _refine_diff_density_max 1.461 _refine_diff_density_min -0.760 _refine_diff_density_rms 0.137 #END