# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'M. Laura Mercuri' _publ_contact_author_email MERCURI@UNICA.IT _publ_section_title ; Self-assembly supramolecular architectures of Chromium (III) complexes using croconate as building block ; loop_ _publ_author_name 'M. Laura Mercuri' 'Flavia Artizzu' 'G Concas' 'F Congiu' 'P Deplano' 'Luciano Marchio' ; L.Pilia ; 'Marco Salidu' 'Angela Serpe' # Attachment 'Compound 1.cif' data_crcro906 _database_code_depnum_ccdc_archive 'CCDC 689099' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H22 Cr2 O22' _chemical_formula_sum 'C10 H22 Cr2 O22' _chemical_formula_weight 598.28 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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Cmca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x, -y, -z' '-x+1/2, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x, y, z' 'x-1/2, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z-1/2' _cell_length_a 6.741(7) _cell_length_b 18.841(9) _cell_length_c 16.886(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2145(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3449 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 27.04 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.744 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart 1000 area detector' _diffrn_measurement_method 'theta & omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 12325 _diffrn_reflns_av_R_equivalents 0.0921 _diffrn_reflns_av_sigmaI/netI 0.0655 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 27.04 _reflns_number_total 1280 _reflns_number_gt 778 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for windows' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^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 1280 _refine_ls_number_parameters 159 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0722 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0625 _refine_ls_wR_factor_gt 0.0580 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.026(3) 0.1536(2) 0.4580(2) 0.024(3) Uani 0.50 1 d P A -1 C2 C 0.034(3) 0.1197(2) 0.3840(3) 0.031(5) Uani 0.50 1 d P A -1 O1 O -0.032(2) 0.12818(14) 0.52710(16) 0.024(3) Uani 0.50 1 d P A -1 O2 O 0.026(5) 0.05394(13) 0.36452(17) 0.026(5) Uani 0.50 1 d P . -1 C3 C 0.0803(9) 0.1737(2) 0.3225(3) 0.0381(18) Uani 0.50 1 d P A -1 C4 C 0.1024(8) 0.2422(3) 0.3646(3) 0.0388(15) Uani 0.50 1 d P A -1 C5 C 0.0530(8) 0.2296(2) 0.4488(3) 0.033(2) Uani 0.50 1 d P A -1 O3 O 0.0984(6) 0.16326(19) 0.2518(2) 0.0544(14) Uani 0.50 1 d P A -1 O4 O 0.1557(8) 0.2975(2) 0.3322(3) 0.0569(14) Uani 0.50 1 d P A -1 O5 O 0.0468(11) 0.27342(16) 0.5024(2) 0.043(2) Uani 0.50 1 d P A -1 O4W O -0.3131(9) 0.2868(2) 0.3480(3) 0.0601(15) Uani 0.50 1 d PD B -2 O1W O 0.2059(5) 0.07118(11) 0.64978(15) 0.0715(8) Uani 1 1 d D A . O2W O 0.5000 -0.01662(16) 0.6957(2) 0.0600(10) Uani 1 2 d SD . . O3W O -0.5000 0.08701(15) 0.45130(19) 0.0496(9) Uani 1 2 d SD . . O6 O -0.1910(4) 0.0000 0.5000 0.0325(7) Uani 1 2 d SD . . Cr Cr 0.0000 0.03558(3) 0.57629(4) 0.0325(2) Uani 1 2 d S . . H1W H 0.227(5) 0.1217(8) 0.654(2) 0.120(14) Uiso 1 1 d D . . H7W H -0.400(7) 0.271(3) 0.391(2) 0.08(3) Uiso 0.50 1 d PD . . H8W H -0.367(7) 0.265(3) 0.3029(19) 0.07(2) Uiso 0.50 1 d PD . . H2W H 0.322(4) 0.0464(15) 0.660(2) 0.093(14) Uiso 1 1 d D . . H4W H 0.5000 -0.033(2) 0.7486(13) 0.11(2) Uiso 1 2 d SD . . H3W H 0.5000 -0.0524(18) 0.6561(18) 0.087(19) Uiso 1 2 d SD . . H5W H -0.5000 0.1336(12) 0.473(2) 0.067(15) Uiso 1 2 d SD . . H6W H -0.599(6) 0.069(2) 0.486(3) 0.05(2) Uiso 0.50 1 d PD . . H6 H -0.294(5) 0.026(2) 0.479(2) 0.018(13) Uiso 0.50 1 d PD . . 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 C1 0.018(8) 0.0199(12) 0.0338(13) 0.0002(10) -0.0023(18) 0.0010(17) C2 0.037(14) 0.021(2) 0.036(3) -0.0014(19) 0.001(3) 0.000(3) O1 0.018(8) 0.0199(12) 0.0338(13) 0.0002(10) -0.0023(18) 0.0010(17) O2 0.030(14) 0.0176(14) 0.0309(16) 0.0008(11) 0.003(3) 0.002(2) C3 0.055(5) 0.019(3) 0.040(3) 0.001(2) 0.004(3) -0.003(2) C4 0.055(4) 0.021(3) 0.041(3) 0.004(3) -0.007(3) -0.007(3) C5 0.038(6) 0.018(2) 0.044(3) 0.001(2) -0.005(3) -0.003(2) O3 0.098(4) 0.0319(19) 0.033(2) 0.0002(18) 0.009(2) -0.011(2) O4 0.099(4) 0.027(2) 0.045(3) 0.011(2) -0.010(3) -0.021(3) O5 0.062(8) 0.0224(16) 0.0444(19) -0.0063(15) -0.002(2) -0.006(2) O4W 0.104(5) 0.035(3) 0.042(3) -0.009(2) 0.009(3) -0.002(3) O1W 0.120(2) 0.0251(12) 0.0690(16) 0.0021(12) -0.0520(16) -0.0156(15) O2W 0.094(3) 0.0411(19) 0.045(2) 0.0092(17) 0.000 0.000 O3W 0.060(2) 0.0242(16) 0.065(2) -0.0044(16) 0.000 0.000 O6 0.0311(19) 0.0271(15) 0.0394(17) 0.0059(13) 0.000 0.000 Cr 0.0534(4) 0.0158(3) 0.0283(3) -0.0011(3) 0.000 0.000 _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 C1 O1 1.321(11) . ? C1 C2 1.404(6) . ? C1 C5 1.452(6) . ? C2 O2 1.283(5) . ? C2 C3 1.488(8) . ? O1 Cr 1.944(3) . ? O2 Cr 1.968(4) 9_556 ? C3 O3 1.215(6) . ? C3 C4 1.481(7) . ? C4 O4 1.232(6) . ? C4 C5 1.479(7) . ? C5 O5 1.226(5) . ? O1W Cr 1.979(3) . ? O6 Cr 1.941(2) . ? O6 Cr 1.941(2) 9_556 ? Cr O6 1.941(2) 9_556 ? Cr O1 1.944(3) 11 ? Cr O2 1.968(4) 9_556 ? Cr O2 1.968(4) 3_556 ? Cr O1W 1.979(3) 11 ? Cr Cr 2.9045(18) 9_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 129.2(7) . . ? O1 C1 C5 119.3(5) . . ? C2 C1 C5 110.5(4) . . ? O2 C2 C1 131.8(5) . . ? O2 C2 C3 119.3(6) . . ? C1 C2 C3 108.5(5) . . ? C1 O1 Cr 132.1(8) . . ? C2 O2 Cr 134.5(3) . 9_556 ? O3 C3 C4 127.1(5) . . ? O3 C3 C2 126.6(4) . . ? C4 C3 C2 106.3(4) . . ? O4 C4 C5 128.9(5) . . ? O4 C4 C3 123.6(5) . . ? C5 C4 C3 107.5(4) . . ? O5 C5 C1 125.5(5) . . ? O5 C5 C4 127.6(4) . . ? C1 C5 C4 106.8(4) . . ? Cr O6 Cr 96.87(14) . 9_556 ? O6 Cr O6 83.13(14) . 9_556 ? O6 Cr O1 95.7(3) . 11 ? O6 Cr O1 87.3(3) 9_556 11 ? O6 Cr O1 87.3(3) . . ? O6 Cr O1 95.7(3) 9_556 . ? O1 Cr O1 12.6(8) 11 . ? O6 Cr O2 88.9(6) . 9_556 ? O6 Cr O2 95.8(6) 9_556 9_556 ? O1 Cr O2 174.7(3) 11 9_556 ? O1 Cr O2 167.4(9) . 9_556 ? O6 Cr O2 95.8(6) . 3_556 ? O6 Cr O2 88.9(6) 9_556 3_556 ? O1 Cr O2 167.4(9) 11 3_556 ? O1 Cr O2 174.7(3) . 3_556 ? O2 Cr O2 10.3(19) 9_556 3_556 ? O6 Cr O1W 176.96(12) . . ? O6 Cr O1W 93.90(13) 9_556 . ? O1 Cr O1W 83.5(3) 11 . ? O1 Cr O1W 92.3(3) . . ? O2 Cr O1W 92.0(7) 9_556 . ? O2 Cr O1W 84.8(7) 3_556 . ? O6 Cr O1W 93.90(13) . 11 ? O6 Cr O1W 176.96(12) 9_556 11 ? O1 Cr O1W 92.3(3) 11 11 ? O1 Cr O1W 83.5(3) . 11 ? O2 Cr O1W 84.8(7) 9_556 11 ? O2 Cr O1W 92.0(7) 3_556 11 ? O1W Cr O1W 89.1(2) . 11 ? O6 Cr Cr 41.57(7) . 9_556 ? O6 Cr Cr 41.57(7) 9_556 9_556 ? O1 Cr Cr 92.01(9) 11 9_556 ? O1 Cr Cr 92.01(9) . 9_556 ? O2 Cr Cr 93.15(9) 9_556 9_556 ? O2 Cr Cr 93.15(9) 3_556 9_556 ? O1W Cr Cr 135.46(10) . 9_556 ? O1W Cr Cr 135.46(10) 11 9_556 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.04 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.281 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.061 #END #BEGIN data_crc5o52 _database_code_depnum_ccdc_archive 'CCDC 689100' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H25 Cr2 K5 O38' _chemical_formula_sum 'C22.50 H24 Cr2 K5 O35.50' _chemical_formula_weight 1161.92 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.216(9) _cell_length_b 14.895(8) _cell_length_c 18.503(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.77(5) _cell_angle_gamma 90.00 _cell_volume 4164(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 5.40 _cell_measurement_theta_max 12.35 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2344 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Philips PW 1100 diffractometer' _diffrn_measurement_method Theta-2-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3380 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2052 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 24.04 _reflns_number_total 3380 _reflns_number_gt 1456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'local program' _computing_cell_refinement 'local program' _computing_data_reduction 'local program' _computing_structure_solution Sir97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for windows' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(16) _refine_ls_number_reflns 3380 _refine_ls_number_parameters 312 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.2067 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2243 _refine_ls_wR_factor_gt 0.1902 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.257 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.288(2) 0.877(3) 0.4327(19) 0.020(10) Uiso 1 1 d . . . C31 C 0.325(3) 1.030(3) 0.406(2) 0.024(10) Uiso 1 1 d . . . C41 C 0.279(2) 1.025(2) 0.4751(19) 0.016(9) Uiso 1 1 d . . . C51 C 0.255(2) 0.933(2) 0.486(2) 0.022(9) Uiso 1 1 d . . . C12 C 0.396(2) 0.564(2) 0.2624(19) 0.006(8) Uiso 1 1 d . . . C22 C 0.431(2) 0.623(2) 0.2191(17) 0.009(8) Uiso 1 1 d . . . C32 C 0.455(2) 0.576(2) 0.158(2) 0.023(9) Uiso 1 1 d . . . C42 C 0.436(2) 0.481(3) 0.172(2) 0.033(11) Uiso 1 1 d . . . C52 C 0.400(2) 0.479(2) 0.239(2) 0.015(9) Uiso 1 1 d . . . C13 C 0.215(2) 0.584(3) 0.147(2) 0.026(10) Uiso 1 1 d . . . C23 C 0.238(2) 0.527(2) 0.083(2) 0.021(10) Uiso 1 1 d . . . C33 C 0.228(2) 0.427(2) 0.1035(19) 0.015(8) Uiso 1 1 d . . . C43 C 0.172(3) 0.428(3) 0.163(3) 0.041(13) Uiso 1 1 d . . . C53 C 0.173(2) 0.521(3) 0.193(2) 0.020(10) Uiso 1 1 d . . . C15 C 0.507(2) 0.070(2) -0.006(2) 0.019(9) Uiso 1 1 d . . . C25 C 0.475(2) 0.023(2) 0.052(2) 0.021(10) Uiso 1 1 d . . . C35 C 0.506(3) -0.063(3) 0.047(2) 0.042(13) Uiso 1 1 d . . . C45 C 0.541(2) -0.073(2) -0.020(2) 0.018(9) Uiso 1 1 d . . . C55 C 0.548(2) 0.013(3) -0.051(2) 0.020(10) Uiso 1 1 d . . . O1 O 0.2888(15) 0.7545(18) 0.2797(14) 0.025(7) Uiso 1 1 d . . . O6W O -0.2202(15) 0.5228(16) 0.1837(12) 0.043(6) Uiso 1 1 d . . . O2W O 0.5271(16) 0.8598(17) 0.2822(13) 0.022(6) Uiso 1 1 d . . . O2 O 0.4341(15) 0.7402(17) 0.3654(13) 0.018(6) Uiso 1 1 d . . . O10W O 0.247(3) 0.255(3) 0.383(2) 0.154(16) Uiso 1 1 d . . . O8W O 0.599(2) 0.294(2) 0.1075(18) 0.021(9) Uiso 0.50 1 d P . . O7W O 0.336(2) 0.227(2) 0.2195(17) 0.087(10) Uiso 1 1 d . . . O9W O 0.426(2) 0.298(2) 0.4443(19) 0.107(12) Uiso 1 1 d . . . O3W O 0.3702(19) 0.872(2) 0.1822(16) 0.039(8) Uiso 1 1 d . . . O11 O 0.2896(14) 0.7844(16) 0.4330(12) 0.025(6) Uiso 1 1 d . . . O4W O 0.1998(19) 0.635(2) 0.3665(17) 0.045(9) Uiso 1 1 d . . . O12 O 0.3578(15) 0.5815(17) 0.3227(12) 0.022(6) Uiso 1 1 d . . . O12W O 0.470(3) 0.507(3) 0.473(2) 0.135(15) Uiso 1 1 d . . . O13 O 0.2267(18) 0.661(2) 0.1574(16) 0.043(9) Uiso 1 1 d . . . O5W O 0.3536(17) 0.627(2) 0.4648(15) 0.030(7) Uiso 1 1 d . . . O15 O 0.4915(16) 0.1575(18) -0.0132(14) 0.027(7) Uiso 1 1 d . . . O21 O 0.3776(14) 0.9154(16) 0.3297(11) 0.016(6) Uiso 1 1 d . . . O22 O 0.4509(13) 0.7055(14) 0.2207(11) 0.013(5) Uiso 1 1 d . . . O23 O 0.2900(14) 0.5512(14) 0.0387(12) 0.021(6) Uiso 1 1 d . . . O25 O 0.4535(17) 0.0601(18) 0.1109(15) 0.050(9) Uiso 1 1 d . . . O31 O 0.3486(17) 1.093(2) 0.3741(16) 0.037(8) Uiso 1 1 d . . . O32 O 0.5018(14) 0.5966(16) 0.1078(12) 0.023(6) Uiso 1 1 d . . . O33 O 0.2512(15) 0.3632(17) 0.0652(13) 0.023(6) Uiso 1 1 d . . . O35 O 0.486(2) -0.132(2) 0.0830(18) 0.060(10) Uiso 1 1 d . . . O41 O 0.2706(12) 1.0887(14) 0.5121(11) 0.014(5) Uiso 1 1 d . . . O42 O 0.432(2) 0.416(2) 0.1247(18) 0.074(10) Uiso 1 1 d . . . O43 O 0.1321(15) 0.3617(17) 0.1803(13) 0.037(7) Uiso 1 1 d . . . O45 O 0.5717(14) -0.1465(15) -0.0495(12) 0.027(6) Uiso 1 1 d . . . O51 O 0.2402(16) 0.8943(19) 0.5461(14) 0.043(8) Uiso 1 1 d . . . O52 O 0.3676(15) 0.4096(18) 0.2665(14) 0.022(7) Uiso 1 1 d . . . O53 O 0.1301(18) 0.5423(19) 0.2472(16) 0.050(8) Uiso 1 1 d . . . O55 O 0.5778(15) 0.0311(16) -0.1111(13) 0.027(6) Uiso 1 1 d . . . C21 C 0.330(3) 0.931(3) 0.379(2) 0.026(11) Uiso 1 1 d . . . K1 K 0.2735(7) 0.4285(7) 0.3855(6) 0.047(3) Uani 1 1 d . . . K2 K 0.3261(9) 0.7392(8) 0.0559(6) 0.067(4) Uani 1 1 d . . . K3 K -0.0487(7) 0.5722(8) 0.2552(6) 0.049(3) Uani 1 1 d . . . K4 K 0.1129(9) 0.2273(4) 0.0667(9) 0.056(2) Uani 1 1 d . . . K5 K 0.3974(8) 0.2422(7) 0.0887(6) 0.049(3) Uani 1 1 d . . . Cr2 Cr 0.4073(3) 0.8078(4) 0.2734(3) 0.0222(18) Uani 1 1 d . . . Cr1 Cr 0.3192(4) 0.6905(4) 0.3680(3) 0.0246(18) Uani 1 1 d . . . O11W O 0.099(2) 1.116(2) 0.3833(17) 0.090(9) Uiso 1 1 d . . . O54 O 0.079(2) 0.894(2) 0.3973(18) 0.022(9) Uiso 0.50 1 d P . 1 O34 O 0.150(2) 0.883(2) 0.1563(18) 0.019(8) Uiso 0.50 1 d P . 1 O44 O 0.156(2) 0.997(2) 0.2846(18) 0.016(8) Uiso 0.50 1 d P . 1 O24 O 0.036(2) 0.7159(19) 0.1774(16) 0.008(9) Uiso 0.50 1 d PD . 1 O14 O -0.002(2) 0.733(2) 0.3281(18) 0.014(8) Uiso 0.50 1 d P . 1 C14 C 0.050(2) 0.791(2) 0.2998(16) 0.012(11) Uiso 0.50 1 d PGD . 1 C24 C 0.074(2) 0.7908(19) 0.2312(15) 0.011(12) Uiso 0.50 1 d PGD . 1 C34 C 0.121(2) 0.868(2) 0.2222(16) 0.008(11) Uiso 0.50 1 d PGD . 1 C44 C 0.125(2) 0.916(2) 0.2853(17) 0.017(13) Uiso 0.50 1 d PG . 1 C54 C 0.081(2) 0.869(2) 0.3333(16) 0.014(12) Uiso 0.50 1 d PG . 1 O13W O 0.044(4) 0.742(4) 0.202(3) 0.056(15) Uiso 0.50 1 d P . 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 K1 0.075(8) 0.033(7) 0.036(7) 0.011(5) 0.020(6) 0.002(6) K2 0.110(10) 0.041(8) 0.053(8) -0.002(7) 0.026(7) -0.036(7) K3 0.060(7) 0.057(9) 0.037(7) -0.011(6) 0.032(6) -0.017(6) K4 0.053(4) 0.026(3) 0.094(6) 0.004(8) 0.032(4) 0.018(7) K5 0.081(8) 0.028(7) 0.040(7) -0.004(6) 0.018(6) 0.000(6) Cr2 0.039(4) 0.014(4) 0.017(4) -0.006(3) 0.020(3) -0.010(3) Cr1 0.044(5) 0.010(4) 0.024(4) 0.001(3) 0.024(4) -0.007(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 C11 O11 1.37(4) . ? C11 C51 1.43(5) . ? C11 C21 1.47(5) . ? C31 O31 1.20(5) . ? C31 C41 1.53(5) . ? C31 C21 1.56(5) . ? C41 O41 1.19(4) . ? C41 C51 1.44(5) . ? C51 O51 1.30(4) . ? C12 C22 1.34(5) . ? C12 C52 1.34(5) . ? C12 O12 1.34(4) . ? C22 O22 1.27(4) . ? C22 C32 1.41(5) . ? C32 O32 1.27(4) . ? C32 C42 1.48(5) . ? C32 K2 3.53(4) . ? C42 O42 1.29(5) . ? C42 C52 1.41(6) . ? C52 O52 1.28(4) . ? C13 O13 1.18(4) . ? C13 C53 1.47(5) . ? C13 C23 1.53(5) . ? C13 K2 3.42(4) . ? C23 O23 1.26(4) . ? C23 C33 1.56(5) . ? C23 K2 3.49(4) . ? C33 O33 1.26(4) . ? C33 C43 1.47(5) . ? C33 K4 3.47(3) . ? C43 O43 1.22(5) . ? C43 C53 1.50(6) . ? C43 K4 3.53(5) . ? C53 O53 1.29(4) . ? C15 O15 1.33(4) . ? C15 C55 1.39(5) . ? C15 C25 1.42(5) . ? C25 O25 1.29(4) . ? C25 C35 1.37(5) . ? C35 O35 1.29(5) . ? C35 C45 1.41(5) . ? C35 K4 3.52(4) 3_545 ? C45 O45 1.33(4) . ? C45 C55 1.42(5) . ? C45 K4 3.49(4) 3_545 ? C55 O55 1.27(4) . ? O1 Cr1 1.90(3) . ? O1 Cr2 1.99(2) . ? O6W K3 2.88(3) . ? O2W Cr2 1.97(2) . ? O2W K3 3.38(3) 3 ? O2 Cr1 1.90(2) . ? O2 Cr2 1.98(3) . ? O10W K1 2.61(5) . ? O10W K2 3.28(4) 2_565 ? O8W O34 1.74(5) 3_545 ? O8W K5 3.14(3) . ? O7W K5 2.70(3) . ? O7W K3 2.93(3) 3_545 ? O9W K2 2.77(4) 2_565 ? O9W K1 3.13(4) . ? O3W Cr2 1.97(3) . ? O3W K2 3.08(3) . ? O11 Cr1 1.93(2) . ? O11 K5 3.17(2) 2_565 ? O4W Cr1 1.99(3) . ? O4W K1 3.28(3) . ? O12 Cr1 1.95(3) . ? O12 K1 2.92(3) . ? O13 K2 2.80(3) . ? O5W Cr1 2.04(3) . ? O5W K5 3.02(3) 2_565 ? O15 K5 2.80(3) . ? O21 C21 1.26(5) . ? O21 Cr2 1.99(2) . ? O21 K3 3.00(3) 3 ? O22 Cr2 1.97(2) . ? O23 K1 2.83(2) 2_564 ? O23 K2 2.86(2) . ? O25 K3 2.68(3) 3_545 ? O25 K5 2.86(3) . ? O31 K3 2.86(3) 3 ? O32 K4 2.74(3) 3 ? O33 K5 2.86(3) . ? O33 K4 2.92(3) . ? O35 K4 2.88(3) 3_545 ? O35 K2 3.09(3) 1_545 ? O41 K2 2.79(2) 2_575 ? O42 K5 2.72(4) . ? O43 K4 2.89(3) . ? O45 K4 2.87(3) 3_545 ? O51 K4 2.71(3) 2_565 ? O51 K5 3.17(3) 2_565 ? O52 K1 2.78(3) . ? O53 K3 2.78(3) . ? O55 K1 3.05(2) 4_554 ? O55 K3 3.33(2) 4_554 ? K1 O23 2.83(2) 2_565 ? K1 O55 3.05(3) 4_455 ? K1 Cr1 3.983(13) . ? K1 K2 4.028(16) 2_565 ? K2 O9W 2.77(4) 2_564 ? K2 O41 2.79(2) 2_574 ? K2 O35 3.09(3) 1_565 ? K2 O10W 3.28(4) 2_564 ? K2 K1 4.028(16) 2_564 ? K2 K4 4.349(19) 3 ? K3 O25 2.68(3) 3_455 ? K3 O14 2.80(3) . ? K3 O31 2.86(3) 3_445 ? K3 O7W 2.93(3) 3_455 ? K3 O24 2.96(3) . ? K3 O21 3.00(3) 3_445 ? K3 O13W 3.11(5) . ? K3 O55 3.33(2) 4_455 ? K3 O2W 3.38(3) 3_445 ? K3 K5 3.998(17) 3_455 ? K4 O51 2.71(3) 2_564 ? K4 O32 2.74(3) 3_445 ? K4 O45 2.87(3) 3_455 ? K4 O35 2.88(3) 3_455 ? K4 C45 3.49(4) 3_455 ? K4 C35 3.52(4) 3_455 ? K4 K5 4.306(18) . ? K4 K2 4.349(19) 3_445 ? K5 O24 2.54(3) 3_545 ? K5 O13W 2.87(6) 3_545 ? K5 O5W 3.02(3) 2_564 ? K5 O11 3.17(2) 2_564 ? K5 O51 3.17(3) 2_564 ? K5 K3 3.998(17) 3_545 ? Cr2 Cr1 2.909(5) . ? O54 C54 1.25(4) . ? O34 C34 1.36(4) . ? O34 O8W 1.74(5) 3_455 ? O44 C44 1.29(4) . ? O24 C24 1.563(19) . ? O24 K5 2.54(3) 3_455 ? O14 C14 1.33(4) . ? C14 C54 1.37(2) . ? C14 C24 1.37(2) . ? C24 C34 1.37(2) . ? C34 C44 1.37(2) . ? C44 C54 1.37(2) . ? O13W K5 2.87(6) 3_455 ? 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 O11 C11 C51 126(3) . . ? O11 C11 C21 123(3) . . ? C51 C11 C21 111(3) . . ? O31 C31 C41 130(4) . . ? O31 C31 C21 125(4) . . ? C41 C31 C21 105(3) . . ? O41 C41 C51 129(3) . . ? O41 C41 C31 122(3) . . ? C51 C41 C31 108(3) . . ? O51 C51 C11 116(3) . . ? O51 C51 C41 128(3) . . ? C11 C51 C41 110(3) . . ? C22 C12 C52 113(3) . . ? C22 C12 O12 128(3) . . ? C52 C12 O12 120(3) . . ? O22 C22 C12 137(3) . . ? O22 C22 C32 114(3) . . ? C12 C22 C32 109(3) . . ? O32 C32 C22 134(3) . . ? O32 C32 C42 120(3) . . ? C22 C32 C42 105(3) . . ? O32 C32 K2 76.4(19) . . ? C22 C32 K2 85(2) . . ? C42 C32 K2 130(2) . . ? O42 C42 C52 126(4) . . ? O42 C42 C32 126(4) . . ? C52 C42 C32 106(3) . . ? O52 C52 C12 127(4) . . ? O52 C52 C42 125(4) . . ? C12 C52 C42 108(4) . . ? O13 C13 C53 126(4) . . ? O13 C13 C23 129(4) . . ? C53 C13 C23 105(3) . . ? O13 C13 K2 49(2) . . ? C53 C13 K2 174(3) . . ? C23 C13 K2 80(2) . . ? O23 C23 C13 125(3) . . ? O23 C23 C33 122(3) . . ? C13 C23 C33 108(3) . . ? O23 C23 K2 50.7(17) . . ? C13 C23 K2 75(2) . . ? C33 C23 K2 163(2) . . ? O33 C33 C43 131(3) . . ? O33 C33 C23 123(3) . . ? C43 C33 C23 105(3) . . ? O33 C33 K4 54.3(17) . . ? C43 C33 K4 80(2) . . ? C23 C33 K4 147(2) . . ? O43 C43 C33 123(4) . . ? O43 C43 C53 129(4) . . ? C33 C43 C53 108(4) . . ? O43 C43 K4 49(2) . . ? C33 C43 K4 76(2) . . ? C53 C43 K4 165(3) . . ? O53 C53 C13 126(4) . . ? O53 C53 C43 122(4) . . ? C13 C53 C43 111(4) . . ? O15 C15 C55 128(4) . . ? O15 C15 C25 119(3) . . ? C55 C15 C25 112(3) . . ? O25 C25 C35 126(4) . . ? O25 C25 C15 125(3) . . ? C35 C25 C15 104(4) . . ? O35 C35 C25 127(4) . . ? O35 C35 C45 120(4) . . ? C25 C35 C45 110(4) . . ? O35 C35 K4 51(2) . 3_545 ? C25 C35 K4 168(3) . 3_545 ? C45 C35 K4 77(2) . 3_545 ? O45 C45 C35 129(4) . . ? O45 C45 C55 122(3) . . ? C35 C45 C55 108(4) . . ? O45 C45 K4 51.9(17) . 3_545 ? C35 C45 K4 80(2) . 3_545 ? C55 C45 K4 158(2) . 3_545 ? O55 C55 C15 129(4) . . ? O55 C55 C45 127(4) . . ? C15 C55 C45 104(3) . . ? Cr1 O1 Cr2 96.9(10) . . ? Cr2 O2W K3 93.4(9) . 3 ? Cr1 O2 Cr2 97.0(10) . . ? K1 O10W K2 85.6(12) . 2_565 ? O34 O8W K5 128.1(18) 3_545 . ? K5 O7W K3 90.4(9) . 3_545 ? K2 O9W K1 85.9(9) 2_565 . ? Cr2 O3W K2 110.6(13) . . ? C11 O11 Cr1 136(2) . . ? C11 O11 K5 97.7(18) . 2_565 ? Cr1 O11 K5 110.0(9) . 2_565 ? Cr1 O4W K1 95.0(11) . . ? C12 O12 Cr1 135(2) . . ? C12 O12 K1 116(2) . . ? Cr1 O12 K1 108.0(10) . . ? C13 O13 K2 112(3) . . ? Cr1 O5W K5 112.3(12) . 2_565 ? C15 O15 K5 118(2) . . ? C21 O21 Cr2 136(3) . . ? C21 O21 K3 118(2) . 3 ? Cr2 O21 K3 105.4(9) . 3 ? C22 O22 Cr2 132(2) . . ? C23 O23 K1 134(2) . 2_564 ? C23 O23 K2 109(2) . . ? K1 O23 K2 90.0(7) 2_564 . ? C25 O25 K3 154(2) . 3_545 ? C25 O25 K5 113(2) . . ? K3 O25 K5 92.4(9) 3_545 . ? C31 O31 K3 121(3) . 3 ? C32 O32 K4 142(2) . 3 ? C33 O33 K5 131(2) . . ? C33 O33 K4 105(2) . . ? K5 O33 K4 96.3(8) . . ? C35 O35 K4 109(3) . 3_545 ? C35 O35 K2 130(3) . 1_545 ? K4 O35 K2 93.4(10) 3_545 1_545 ? C41 O41 K2 148(2) . 2_575 ? C42 O42 K5 150(3) . . ? C43 O43 K4 112(3) . . ? C45 O45 K4 107(2) . 3_545 ? C51 O51 K4 128(2) . 2_565 ? C51 O51 K5 107(2) . 2_565 ? K4 O51 K5 93.9(8) 2_565 2_565 ? C52 O52 K1 120(2) . . ? C53 O53 K3 132(2) . . ? C55 O55 K1 120(2) . 4_554 ? C55 O55 K3 109(2) . 4_554 ? K1 O55 K3 123.9(8) 4_554 4_554 ? O21 C21 C11 136(4) . . ? O21 C21 C31 117(4) . . ? C11 C21 C31 106(4) . . ? O10W K1 O52 89.0(11) . . ? O10W K1 O23 96.6(11) . 2_565 ? O52 K1 O23 144.2(8) . 2_565 ? O10W K1 O12 147.1(11) . . ? O52 K1 O12 58.2(7) . . ? O23 K1 O12 108.9(7) 2_565 . ? O10W K1 O55 92.5(11) . 4_455 ? O52 K1 O55 129.3(7) . 4_455 ? O23 K1 O55 86.0(7) 2_565 4_455 ? O12 K1 O55 109.3(7) . 4_455 ? O10W K1 O9W 59.9(11) . . ? O52 K1 O9W 77.3(8) . . ? O23 K1 O9W 75.2(8) 2_565 . ? O12 K1 O9W 106.3(8) . . ? O55 K1 O9W 143.5(8) 4_455 . ? O10W K1 O4W 151.0(11) . . ? O52 K1 O4W 102.2(8) . . ? O23 K1 O4W 89.8(8) 2_565 . ? O12 K1 O4W 52.1(7) . . ? O55 K1 O4W 59.6(7) 4_455 . ? O9W K1 O4W 148.4(9) . . ? O10W K1 Cr1 174.3(11) . . ? O52 K1 Cr1 85.6(6) . . ? O23 K1 Cr1 88.9(5) 2_565 . ? O12 K1 Cr1 27.7(5) . . ? O55 K1 Cr1 89.4(5) 4_455 . ? O9W K1 Cr1 120.6(7) . . ? O4W K1 Cr1 29.9(5) . . ? O10W K1 K2 54.2(10) . 2_565 ? O52 K1 K2 118.9(6) . 2_565 ? O23 K1 K2 45.3(5) 2_565 2_565 ? O12 K1 K2 137.6(6) . 2_565 ? O55 K1 K2 102.2(5) 4_455 2_565 ? O9W K1 K2 43.2(7) . 2_565 ? O4W K1 K2 134.4(7) . 2_565 ? Cr1 K1 K2 130.6(4) . 2_565 ? O9W K2 O41 98.1(9) 2_564 2_574 ? O9W K2 O13 144.0(11) 2_564 . ? O41 K2 O13 114.0(9) 2_574 . ? O9W K2 O23 80.7(9) 2_564 . ? O41 K2 O23 145.0(8) 2_574 . ? O13 K2 O23 63.7(8) . . ? O9W K2 O3W 127.2(10) 2_564 . ? O41 K2 O3W 70.1(8) 2_574 . ? O13 K2 O3W 81.0(9) . . ? O23 K2 O3W 137.4(8) . . ? O9W K2 O35 75.5(10) 2_564 1_565 ? O41 K2 O35 71.6(8) 2_574 1_565 ? O13 K2 O35 128.7(10) . 1_565 ? O23 K2 O35 139.4(9) . 1_565 ? O3W K2 O35 51.8(8) . 1_565 ? O9W K2 O10W 56.6(10) 2_564 2_564 ? O41 K2 O10W 68.3(9) 2_574 2_564 ? O13 K2 O10W 119.9(10) . 2_564 ? O23 K2 O10W 82.7(9) . 2_564 ? O3W K2 O10W 138.2(11) . 2_564 ? O35 K2 O10W 109.6(10) 1_565 2_564 ? O9W K2 C13 125.6(11) 2_564 . ? O41 K2 C13 127.8(9) 2_574 . ? O13 K2 C13 18.6(9) . . ? O23 K2 C13 45.2(8) . . ? O3W K2 C13 97.9(10) . . ? O35 K2 C13 139.8(10) 1_565 . ? O10W K2 C13 110.4(10) 2_564 . ? O9W K2 C23 100.6(10) 2_564 . ? O41 K2 C23 140.1(8) 2_574 . ? O13 K2 C23 44.0(9) . . ? O23 K2 C23 19.8(7) . . ? O3W K2 C23 121.7(9) . . ? O35 K2 C23 147.5(10) 1_565 . ? O10W K2 C23 93.5(10) 2_564 . ? C13 K2 C23 25.5(8) . . ? O9W K2 C32 86.7(10) 2_564 . ? O41 K2 C32 156.6(8) 2_574 . ? O13 K2 C32 70.5(9) . . ? O23 K2 C32 58.3(7) . . ? O3W K2 C32 88.7(9) . . ? O35 K2 C32 87.6(9) 1_565 . ? O10W K2 C32 131.0(10) 2_564 . ? C13 K2 C32 63.2(8) . . ? C23 K2 C32 59.9(8) . . ? O9W K2 K1 50.9(7) 2_564 2_564 ? O41 K2 K1 108.5(6) 2_574 2_564 ? O13 K2 K1 101.2(7) . 2_564 ? O23 K2 K1 44.7(5) . 2_564 ? O3W K2 K1 177.7(7) . 2_564 ? O35 K2 K1 126.2(7) 1_565 2_564 ? O10W K2 K1 40.3(8) 2_564 2_564 ? C13 K2 K1 84.4(7) . 2_564 ? C23 K2 K1 60.5(7) . 2_564 ? C32 K2 K1 92.3(7) . 2_564 ? O9W K2 K4 52.1(7) 2_564 3 ? O41 K2 K4 108.6(5) 2_574 3 ? O13 K2 K4 124.8(7) . 3 ? O23 K2 K4 98.2(6) . 3 ? O3W K2 K4 82.1(6) . 3 ? O35 K2 K4 41.4(6) 1_565 3 ? O10W K2 K4 107.4(8) 2_564 3 ? C13 K2 K4 120.1(7) . 3 ? C23 K2 K4 110.8(7) . 3 ? C32 K2 K4 56.9(6) . 3 ? K1 K2 K4 96.7(4) 2_564 3 ? O25 K3 O53 79.0(9) 3_455 . ? O25 K3 O14 120.3(10) 3_455 . ? O53 K3 O14 88.3(9) . . ? O25 K3 O31 147.7(9) 3_455 3_445 ? O53 K3 O31 133.3(9) . 3_445 ? O14 K3 O31 70.4(9) . 3_445 ? O25 K3 O6W 69.0(8) 3_455 . ? O53 K3 O6W 140.8(8) . . ? O14 K3 O6W 127.1(9) . . ? O31 K3 O6W 80.4(8) 3_445 . ? O25 K3 O7W 84.6(9) 3_455 3_455 ? O53 K3 O7W 132.7(9) . 3_455 ? O14 K3 O7W 62.8(9) . 3_455 ? O31 K3 O7W 73.7(9) 3_445 3_455 ? O6W K3 O7W 67.2(8) . 3_455 ? O25 K3 O24 60.4(8) 3_455 . ? O53 K3 O24 66.8(9) . . ? O14 K3 O24 61.0(9) . . ? O31 K3 O24 127.0(9) 3_445 . ? O6W K3 O24 112.6(9) . . ? O7W K3 O24 66.5(9) 3_455 . ? O25 K3 O21 117.1(8) 3_455 3_445 ? O53 K3 O21 108.8(8) . 3_445 ? O14 K3 O21 122.2(8) . 3_445 ? O31 K3 O21 57.6(8) 3_445 3_445 ? O6W K3 O21 69.1(6) . 3_445 ? O7W K3 O21 118.2(8) 3_455 3_445 ? O24 K3 O21 175.0(9) . 3_445 ? O25 K3 O13W 71.2(12) 3_455 . ? O53 K3 O13W 68.3(12) . . ? O14 K3 O13W 50.2(13) . . ? O31 K3 O13W 117.6(13) 3_445 . ? O6W K3 O13W 118.8(12) . . ? O7W K3 O13W 64.4(12) 3_455 . ? O24 K3 O13W 10.9(11) . . ? O21 K3 O13W 171.0(12) 3_445 . ? O25 K3 O55 129.5(8) 3_455 4_455 ? O53 K3 O55 58.7(6) . 4_455 ? O14 K3 O55 87.0(8) . 4_455 ? O31 K3 O55 78.5(8) 3_445 4_455 ? O6W K3 O55 129.6(7) . 4_455 ? O7W K3 O55 144.2(8) 3_455 4_455 ? O24 K3 O55 116.8(8) . 4_455 ? O21 K3 O55 60.8(6) 3_445 4_455 ? O13W K3 O55 111.6(11) . 4_455 ? O25 K3 O2W 92.3(8) 3_455 3_445 ? O53 K3 O2W 62.6(8) . 3_445 ? O14 K3 O2W 131.9(9) . 3_445 ? O31 K3 O2W 101.4(8) 3_445 3_445 ? O6W K3 O2W 95.9(7) . 3_445 ? O7W K3 O2W 162.8(8) 3_455 3_445 ? O24 K3 O2W 126.1(8) . 3_445 ? O21 K3 O2W 48.9(6) 3_445 3_445 ? O13W K3 O2W 130.3(11) . 3_445 ? O55 K3 O2W 45.6(6) 4_455 3_445 ? O25 K3 K5 45.6(6) 3_455 3_455 ? O53 K3 K5 100.0(7) . 3_455 ? O14 K3 K5 81.1(7) . 3_455 ? O31 K3 K5 116.2(7) 3_445 3_455 ? O6W K3 K5 73.4(5) . 3_455 ? O7W K3 K5 42.5(6) 3_455 3_455 ? O24 K3 K5 39.4(7) . 3_455 ? O21 K3 K5 142.6(5) 3_445 3_455 ? O13W K3 K5 45.6(10) . 3_455 ? O55 K3 K5 156.1(5) 4_455 3_455 ? O2W K3 K5 137.8(5) 3_445 3_455 ? O51 K4 O32 92.2(5) 2_564 3_445 ? O51 K4 O45 115.4(9) 2_564 3_455 ? O32 K4 O45 125.8(8) 3_445 3_455 ? O51 K4 O35 175.2(10) 2_564 3_455 ? O32 K4 O35 92.6(9) 3_445 3_455 ? O45 K4 O35 60.9(8) 3_455 3_455 ? O51 K4 O43 123.5(9) 2_564 . ? O32 K4 O43 107.6(9) 3_445 . ? O45 K4 O43 94.9(5) 3_455 . ? O35 K4 O43 55.5(8) 3_455 . ? O51 K4 O33 86.2(8) 2_564 . ? O32 K4 O33 164.1(9) 3_445 . ? O45 K4 O33 68.5(7) 3_455 . ? O35 K4 O33 89.4(5) 3_455 . ? O43 K4 O33 61.1(7) . . ? O51 K4 C33 104.3(9) 2_564 . ? O32 K4 C33 149.9(10) 3_445 . ? O45 K4 C33 69.4(7) 3_455 . ? O35 K4 C33 71.8(8) 3_455 . ? O43 K4 C33 42.3(8) . . ? O33 K4 C33 20.4(7) . . ? O51 K4 C45 134.0(10) 2_564 3_455 ? O32 K4 C45 124.2(9) 3_445 3_455 ? O45 K4 C45 21.4(8) 3_455 3_455 ? O35 K4 C45 41.7(9) 3_455 3_455 ? O43 K4 C45 75.1(8) . 3_455 ? O33 K4 C45 65.9(8) . 3_455 ? C33 K4 C45 59.0(8) . 3_455 ? O51 K4 C35 155.1(11) 2_564 3_455 ? O32 K4 C35 111.5(9) 3_445 3_455 ? O45 K4 C35 44.2(8) 3_455 3_455 ? O35 K4 C35 20.2(9) 3_455 3_455 ? O43 K4 C35 57.8(8) . 3_455 ? O33 K4 C35 73.1(8) . 3_455 ? C33 K4 C35 58.6(6) . 3_455 ? C45 K4 C35 23.2(9) 3_455 3_455 ? O51 K4 C43 119.5(10) 2_564 . ? O32 K4 C43 126.0(11) 3_445 . ? O45 K4 C43 81.0(9) 3_455 . ? O35 K4 C43 57.8(9) 3_455 . ? O43 K4 C43 18.6(9) . . ? O33 K4 C43 44.0(9) . . ? C33 K4 C43 24.2(9) . . ? C45 K4 C43 63.7(6) 3_455 . ? C35 K4 C43 52.4(9) 3_455 . ? O51 K4 K5 47.2(6) 2_564 . ? O32 K4 K5 131.0(6) 3_445 . ? O45 K4 K5 99.5(6) 3_455 . ? O35 K4 K5 129.0(7) 3_455 . ? O43 K4 K5 83.2(6) . . ? O33 K4 K5 41.2(5) . . ? C33 K4 K5 57.3(6) . . ? C45 K4 K5 104.8(7) 3_455 . ? C35 K4 K5 114.3(7) 3_455 . ? C43 K4 K5 73.6(8) . . ? O51 K4 K2 138.6(6) 2_564 3_445 ? O32 K4 K2 52.7(5) 3_445 3_445 ? O45 K4 K2 79.0(5) 3_455 3_445 ? O35 K4 K2 45.2(7) 3_455 3_445 ? O43 K4 K2 91.1(6) . 3_445 ? O33 K4 K2 133.7(6) . 3_445 ? C33 K4 K2 117.0(6) . 3_445 ? C45 K4 K2 71.7(7) 3_455 3_445 ? C35 K4 K2 60.7(7) 3_455 3_445 ? C43 K4 K2 100.5(8) . 3_445 ? K5 K4 K2 174.0(3) . 3_445 ? O24 K5 O7W 75.9(10) 3_545 . ? O24 K5 O42 82.3(9) 3_545 . ? O7W K5 O42 86.3(10) . . ? O24 K5 O15 85.2(9) 3_545 . ? O7W K5 O15 145.5(10) . . ? O42 K5 O15 119.7(10) . . ? O24 K5 O33 140.0(9) 3_545 . ? O7W K5 O33 81.0(9) . . ? O42 K5 O33 63.9(8) . . ? O15 K5 O33 129.3(8) . . ? O24 K5 O25 63.3(8) 3_545 . ? O7W K5 O25 85.5(9) . . ? O42 K5 O25 145.6(10) . . ? O15 K5 O25 60.1(8) . . ? O33 K5 O25 146.6(8) . . ? O24 K5 O13W 10.5(13) 3_545 3_545 ? O7W K5 O13W 70.6(12) . 3_545 ? O42 K5 O13W 73.2(13) . 3_545 ? O15 K5 O13W 94.3(12) . 3_545 ? O33 K5 O13W 129.5(13) . 3_545 ? O25 K5 O13W 72.6(13) . 3_545 ? O24 K5 O5W 132.9(9) 3_545 2_564 ? O7W K5 O5W 131.5(10) . 2_564 ? O42 K5 O5W 65.8(9) . 2_564 ? O15 K5 O5W 82.2(8) . 2_564 ? O33 K5 O5W 51.6(7) . 2_564 ? O25 K5 O5W 139.1(9) . 2_564 ? O13W K5 O5W 129.5(12) 3_545 2_564 ? O24 K5 O8W 40.8(9) 3_545 . ? O7W K5 O8W 110.9(10) . . ? O42 K5 O8W 65.1(9) . . ? O15 K5 O8W 67.3(8) . . ? O33 K5 O8W 126.5(8) . . ? O25 K5 O8W 86.9(8) . . ? O13W K5 O8W 41.9(12) 3_545 . ? O5W K5 O8W 92.9(9) 2_564 . ? O24 K5 O11 150.3(9) 3_545 2_564 ? O7W K5 O11 127.4(9) . 2_564 ? O42 K5 O11 114.0(9) . 2_564 ? O15 K5 O11 65.3(7) . 2_564 ? O33 K5 O11 68.3(7) . 2_564 ? O25 K5 O11 97.3(8) . 2_564 ? O13W K5 O11 159.5(12) 3_545 2_564 ? O5W K5 O11 49.2(7) 2_564 2_564 ? O8W K5 O11 121.7(8) . 2_564 ? O24 K5 O51 127.3(9) 3_545 2_564 ? O7W K5 O51 80.8(9) . 2_564 ? O42 K5 O51 142.5(9) . 2_564 ? O15 K5 O51 88.5(8) . 2_564 ? O33 K5 O51 79.4(7) . 2_564 ? O25 K5 O51 68.3(7) . 2_564 ? O13W K5 O51 132.8(12) 3_545 2_564 ? O5W K5 O51 97.6(8) 2_564 2_564 ? O8W K5 O51 152.1(9) . 2_564 ? O11 K5 O51 53.0(7) 2_564 2_564 ? O24 K5 K3 47.6(7) 3_545 3_545 ? O7W K5 K3 47.1(7) . 3_545 ? O42 K5 K3 113.6(8) . 3_545 ? O15 K5 K3 99.1(6) . 3_545 ? O33 K5 K3 127.1(6) . 3_545 ? O25 K5 K3 42.0(6) . 3_545 ? O13W K5 K3 50.7(11) 3_545 3_545 ? O5W K5 K3 178.7(7) 2_564 3_545 ? O8W K5 K3 87.8(7) . 3_545 ? O11 K5 K3 131.2(6) 2_564 3_545 ? O51 K5 K3 82.3(5) 2_564 3_545 ? O3W Cr2 O22 91.8(11) . . ? O3W Cr2 O2W 92.7(11) . . ? O22 Cr2 O2W 89.0(10) . . ? O3W Cr2 O2 175.2(11) . . ? O22 Cr2 O2 89.1(10) . . ? O2W Cr2 O2 92.0(10) . . ? O3W Cr2 O1 94.3(12) . . ? O22 Cr2 O1 94.6(10) . . ? O2W Cr2 O1 172.0(11) . . ? O2 Cr2 O1 80.9(10) . . ? O3W Cr2 O21 89.8(11) . . ? O22 Cr2 O21 173.4(9) . . ? O2W Cr2 O21 84.6(10) . . ? O2 Cr2 O21 89.8(10) . . ? O1 Cr2 O21 91.6(10) . . ? O3W Cr2 Cr1 134.7(9) . . ? O22 Cr2 Cr1 92.3(6) . . ? O2W Cr2 Cr1 132.4(7) . . ? O2 Cr2 Cr1 40.5(7) . . ? O1 Cr2 Cr1 40.4(7) . . ? O21 Cr2 Cr1 91.1(7) . . ? O1 Cr1 O2 85.1(11) . . ? O1 Cr1 O11 97.0(11) . . ? O2 Cr1 O11 90.9(11) . . ? O1 Cr1 O12 95.9(11) . . ? O2 Cr1 O12 89.3(11) . . ? O11 Cr1 O12 167.1(10) . . ? O1 Cr1 O4W 93.8(12) . . ? O2 Cr1 O4W 177.3(13) . . ? O11 Cr1 O4W 91.7(12) . . ? O12 Cr1 O4W 88.3(12) . . ? O1 Cr1 O5W 177.4(12) . . ? O2 Cr1 O5W 93.5(11) . . ? O11 Cr1 O5W 80.9(11) . . ? O12 Cr1 O5W 86.2(11) . . ? O4W Cr1 O5W 87.8(11) . . ? O1 Cr1 Cr2 42.6(7) . . ? O2 Cr1 Cr2 42.4(8) . . ? O11 Cr1 Cr2 95.6(7) . . ? O12 Cr1 Cr2 93.3(7) . . ? O4W Cr1 Cr2 136.4(9) . . ? O5W Cr1 Cr2 135.9(8) . . ? O1 Cr1 K1 122.3(9) . . ? O2 Cr1 K1 123.5(8) . . ? O11 Cr1 K1 127.1(8) . . ? O12 Cr1 K1 44.3(7) . . ? O4W Cr1 K1 55.2(9) . . ? O5W Cr1 K1 60.3(8) . . ? Cr2 Cr1 K1 137.3(2) . . ? C34 O34 O8W 100(2) . 3_455 ? C24 O24 K5 122(2) . 3_455 ? C24 O24 K3 111.1(16) . . ? K5 O24 K3 93.0(9) 3_455 . ? C14 O14 K3 120(2) . . ? O14 C14 C54 124(2) . . ? O14 C14 C24 127(2) . . ? C54 C14 C24 108.0 . . ? C14 C24 C34 108.0 . . ? C14 C24 O24 118.2(18) . . ? C34 C24 O24 133.1(18) . . ? O34 C34 C24 118(2) . . ? O34 C34 C44 134(2) . . ? C24 C34 C44 108.0 . . ? O44 C44 C54 134(3) . . ? O44 C44 C34 117(3) . . ? C54 C44 C34 108.0 . . ? O54 C54 C44 122(3) . . ? O54 C54 C14 130(3) . . ? C44 C54 C14 108.0 . . ? K5 O13W K3 83.7(15) 3_455 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.04 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.933 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.166 #END # Attachment 'polymer.cif' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # If this CIF has been generated directly or indirectly from an entry in the # Cambridge Structural Database, then it will include bibliographic, chemical, # crystal, experimental, refinement or atomic coordinate data resulting from # the CCDC's data processing and validation procedures. Files generated from # CSD entries are Copyright 2008 Cambridge Crystallographic Data Centre. They # may be used in bona fide research applications only, and may not be copied or # further disseminated in any form, whether machine-readable or not, except for # the purposes of generating routine backup copies on your local computer # system. # # Files arising from any other source may also contain material that is the # copyright of third parties, including the originator, and you should check # with the originator concerning the permitted uses of the information # contained in this CIF. # # For further information on the CCDC and the free tools enCIFer and Mercury # for validating and visualising CIF files, please visit www.ccdc.cam.ac.uk # ####################################################################### data_crc5o5 _database_code_depnum_ccdc_archive 'CCDC 689101' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C c' _symmetry_Int_Tables_number 9 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 x,-y,1/2+z 3 1/2+x,1/2+y,z 4 1/2+x,1/2-y,1/2+z _cell_length_a 15.216(9) _cell_length_b 14.895(8) _cell_length_c 18.503(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.77(5) _cell_angle_gamma 90.00 _cell_volume 4164.32 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z C11 C 0.7925(18) 0.378(2) 0.4308(15) C21 C 0.8321(16) 0.4281(17) 0.3806(15) C31 C 0.8263(18) 0.525(2) 0.4089(16) C41 C 0.777(2) 0.520(2) 0.4748(19) C51 C 0.7567(17) 0.429(2) 0.4865(17) C12 C 0.8986(16) 0.0607(17) 0.2636(15) C22 C 0.9357(18) 0.124(2) 0.2184(16) C32 C 0.9566(19) 0.072(2) 0.1578(18) C42 C 0.9354(15) -0.0249(17) 0.1720(13) C52 C 0.9002(18) -0.026(2) 0.2405(16) C13 C 0.7163(17) 0.0834(19) 0.1476(16) C23 C 0.7384(16) 0.0283(18) 0.0871(15) C33 C 0.7273(18) -0.0730(19) 0.1053(16) C43 C 0.677(2) -0.074(2) 0.1638(19) C53 C 0.6742(18) 0.022(2) 0.1953(16) O54 O 0.5746(15) 0.3887(16) 0.4033(13) O34 O 0.6504(14) 0.3875(15) 0.1554(12) O44 O 0.6567(14) 0.5018(17) 0.2859(12) O24 O 0.5380(11) 0.2231(12) 0.1861(9) O14 O 0.4954(15) 0.2306(15) 0.3318(13) C14 C 0.547(2) 0.283(2) 0.2995(18) C24 C 0.5643(18) 0.2817(19) 0.2270(15) C34 C 0.621(3) 0.359(3) 0.229(2) C44 C 0.623(2) 0.419(2) 0.2790(18) C54 C 0.586(2) 0.371(2) 0.333(2) C15 C 1.0079(18) -0.4302(19) -0.0063(16) C25 C 0.9717(17) -0.4796(19) 0.0537(16) C35 C 1.0005(19) -0.565(2) 0.0467(16) C45 C 1.043(2) -0.571(2) -0.0205(19) C55 C 1.0503(16) -0.4883(19) -0.0488(15) O1 O 0.7893(10) 0.2581(13) 0.2815(9) O6W O 0.2823(11) 0.0234(11) 0.1849(9) O2W O 1.0298(12) 0.3544(13) 0.2855(10) O1W O 0.9365(12) 0.2432(14) 0.3686(10) O10W O 0.7424(18) -0.246(2) 0.3885(16) O8W O 0.5993(16) 0.2932(15) 0.1082(12) O7W O 0.8314(14) -0.2729(14) 0.2186(11) O9W O 0.9280(16) -0.2008(17) 0.4478(13) O3W O 0.8642(12) 0.3705(14) 0.1806(10) O11 O 0.7860(11) 0.2874(12) 0.4309(9) O4W O 0.7008(11) 0.1326(11) 0.3682(9) O12 O 0.8603(10) 0.0809(11) 0.3235(8) O13 O 0.7250(13) 0.1598(16) 0.1581(12) O5W O 0.8482(12) 0.1250(14) 0.4641(11) O15 O 0.9915(12) -0.3407(14) -0.0122(11) O21 O 0.8799(10) 0.4148(11) 0.3306(8) O22 O 0.9503(12) 0.2071(12) 0.2202(10) O23 O 0.7867(11) 0.0534(12) 0.0387(9) O25 O 0.9509(13) -0.4432(15) 0.1107(12) O31 O 0.8490(13) 0.5911(16) 0.3771(12) O32 O 1.0031(11) 0.0954(12) 0.1086(10) O33 O 0.7409(11) -0.1323(13) 0.0595(10) O35 O 0.9716(13) -0.6382(14) 0.0744(11) O41 O 0.7743(11) 0.5866(13) 0.5162(10) O42 O 0.9418(16) -0.0874(18) 0.1319(14) O43 O 0.6352(10) -0.1378(12) 0.1827(9) O45 O 1.0700(12) -0.6490(13) -0.0490(10) O51 O 0.7375(11) 0.3945(12) 0.5455(9) O52 O 0.8679(11) -0.0936(13) 0.2687(10) O53 O 0.6297(13) 0.0410(13) 0.2470(11) O55 O 1.0770(11) -0.4699(12) -0.1114(10) K1 K 0.7727(5) -0.0711(6) 0.3865(4) K2 K 0.8241(6) 0.2393(6) 0.0559(4) K3 K 0.4507(5) 0.0732(6) 0.2566(4) K4 K 0.6132(7) -0.2729(3) 0.0688(7) K5 K 0.8962(6) -0.2577(6) 0.0890(4) Cr2 Cr 0.9059(3) 0.3087(3) 0.2736(2) Cr1 Cr 0.8177(3) 0.1915(3) 0.3682(2) O24 O 1.038 -0.2769 0.1861 O10W O 0.7424 0.246 -0.1115 O8W O 1.0993 -0.2068 0.1082 O7W O 0.3314 0.2271 0.2186 O9W O 0.928 0.2008 -0.0522 O11 O 0.786 -0.2874 -0.0691 O5W O 0.8482 -0.125 -0.0359 O21 O 0.3799 -0.0852 0.3306 O23 O 0.7867 -0.0534 0.5387 O25 O 0.4509 0.0568 0.1107 O31 O 0.349 0.0911 0.3771 O32 O 0.5031 -0.4046 0.1086 O35 O 0.9716 0.3618 0.0744 O35 O 0.4716 -0.1382 0.0744 O41 O 0.7743 0.4134 0.0162 O45 O 0.57 -0.149 -0.049 O51 O 0.7375 -0.3945 0.0455 O55 O 0.577 -0.0301 0.3886 K1 K 0.7727 0.0711 -0.1135 K1 K 1.2727 -0.4289 -0.1135 K2 K 0.8241 -0.7607 0.0559 K2 K 0.8241 -0.2393 0.5559 K2 K 0.8241 0.7607 0.5559 K3 K 0.9507 -0.4268 0.2566 K3 K 0.9507 0.5732 0.2566 K3 K 0.9507 -0.5732 -0.2434 K4 K 0.6132 0.2729 0.5688 K4 K 1.1132 -0.7729 0.0688 K4 K 1.1132 0.2271 0.0688 K5 K 0.8962 0.2577 0.589 K5 K 0.3962 0.2423 0.089 O12W O 0.9750(16) 0.0063(18) 0.4740(14) O11W O 0.596(2) 0.621(2) 0.3863(17) #END