# 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 'Partha Mukherjee' _publ_contact_author_email PSM@IPC.IISC.ERNET.IN _publ_section_title ; Formamide-formate hybrid metal (CoII/CrIII) complexes: synthesis, structures and single crystal-to-single crystal transformation ; loop_ _publ_author_name 'Partha Mukherjee' 'Oindrila Sengupta' 'You Song.' # Attachment 'revised_cif.cif' data_1a_m _database_code_depnum_ccdc_archive 'CCDC 744583' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H7 Co N2 O6' _chemical_formula_sum 'C4 H7 Co N2 O6' _chemical_formula_weight 238.05 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 8.6935(2) _cell_length_b 11.6497(3) _cell_length_c 8.3121(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 841.82(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2046 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 30.51 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour pink _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.878 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 2.041 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6624 _exptl_absorpt_correction_T_max 0.7102 _exptl_absorpt_process_details SADABS _exptl_special_details ; 'none' ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3040 _diffrn_reflns_av_R_equivalents 0.0135 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 958 _reflns_number_gt 846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1999)' _computing_publication_material WinGX _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^)+(0.0680P)^2^+2.3070P] 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 958 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1380 _refine_ls_wR_factor_gt 0.1345 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.76352(7) 0.2500 0.2500 0.0170(3) Uani 1 2 d S . . O1 O 0.7620(3) 0.4054(2) 0.1180(3) 0.0278(6) Uani 1 1 d . . . O2 O 0.9169(4) 0.1777(2) 0.0886(4) 0.0416(8) Uani 1 1 d . . . C1 C 1.0308(4) 0.2196(3) 0.0221(4) 0.0274(7) Uani 1 1 d . . . H3 H 1.0776 0.2822 0.0713 0.033 Uiso 1 1 calc R . . N1 N 0.5872(3) 0.1841(2) 0.1055(3) 0.0235(6) Uani 1 1 d . . . H1A H 0.6171 0.1119 0.0833 0.028 Uiso 1 1 calc R . . H1B H 0.5064 0.1773 0.1725 0.028 Uiso 1 1 calc R . . C2 C 0.7500 0.5000 0.1862(6) 0.0245(10) Uani 1 2 d S . . H4 H 0.7500 0.5000 0.2981 0.029 Uiso 1 2 calc SR . . O3 O 0.8502(5) 0.4356(4) -0.2207(5) 0.0644(11) Uani 1 1 d . . . C3 C 0.7500 0.5000 -0.2950(8) 0.0458(17) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0180(4) 0.0176(4) 0.0153(4) 0.0000(2) 0.000 0.000 O1 0.0440(16) 0.0194(13) 0.0199(11) 0.0005(9) 0.0005(10) -0.0013(10) O2 0.0441(18) 0.0348(15) 0.0460(17) -0.0053(13) 0.0265(14) -0.0029(13) C1 0.0277(17) 0.0272(17) 0.0272(17) -0.0013(14) 0.0050(15) -0.0024(15) N1 0.0235(14) 0.0250(14) 0.0221(13) 0.0071(11) -0.0117(11) -0.0077(11) C2 0.032(3) 0.022(2) 0.019(2) 0.000 0.000 -0.0012(18) O3 0.068(3) 0.067(3) 0.058(2) -0.0028(19) 0.008(2) 0.018(2) C3 0.063(5) 0.047(4) 0.027(3) 0.000 0.000 -0.001(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 Co1 O2 2.071(3) 4 ? Co1 O2 2.071(3) . ? Co1 N1 2.093(3) . ? Co1 N1 2.093(3) 4 ? Co1 O1 2.117(3) 4 ? Co1 O1 2.117(3) . ? O1 C2 1.243(3) . ? O2 C1 1.234(5) . ? C1 N1 1.240(4) 6_655 ? N1 C1 1.240(4) 6 ? C2 O1 1.243(3) 2_665 ? O3 C3 1.305(5) . ? C3 O3 1.305(5) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O2 99.84(19) 4 . ? O2 Co1 N1 172.99(13) 4 . ? O2 Co1 N1 87.17(13) . . ? O2 Co1 N1 87.17(13) 4 4 ? O2 Co1 N1 172.99(13) . 4 ? N1 Co1 N1 85.84(18) . 4 ? O2 Co1 O1 90.92(11) 4 4 ? O2 Co1 O1 89.54(11) . 4 ? N1 Co1 O1 88.81(10) . 4 ? N1 Co1 O1 90.67(10) 4 4 ? O2 Co1 O1 89.54(11) 4 . ? O2 Co1 O1 90.92(11) . . ? N1 Co1 O1 90.67(10) . . ? N1 Co1 O1 88.81(10) 4 . ? O1 Co1 O1 179.30(15) 4 . ? C2 O1 Co1 121.5(3) . . ? C1 O2 Co1 130.2(3) . . ? O2 C1 N1 124.7(4) . 6_655 ? C1 N1 Co1 131.2(3) 6 . ? O1 C2 O1 125.7(5) . 2_665 ? O3 C3 O3 123.5(7) 2_665 . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.862 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.122 #===END data_1b_ _database_code_depnum_ccdc_archive 'CCDC 744584' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C3 H3 Co N3 O6' _chemical_formula_sum 'C3 H3 Co N3 O6' _chemical_formula_weight 236.01 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Imma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 8.658(4) _cell_length_b 11.709(3) _cell_length_c 8.307(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 842.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1336 _cell_measurement_theta_min 3.39 _cell_measurement_theta_max 25.32 _exptl_crystal_description 'rectangular block' _exptl_crystal_colour brown _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 2.042 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6621 _exptl_absorpt_correction_T_max 0.7100 _exptl_absorpt_process_details SADABS _exptl_special_details ; 'none' ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3900 _diffrn_reflns_av_R_equivalents 0.2042 _diffrn_reflns_av_sigmaI/netI 0.0774 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 420 _reflns_number_gt 322 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1999)' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.1709P)^2^+0.1970P] 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 420 _refine_ls_number_parameters 42 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0967 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2453 _refine_ls_wR_factor_gt 0.2243 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.5000 0.0000 0.0316(9) Uani 1 4 d S . . O1 O 0.0000 0.3438(6) 0.1326(9) 0.046(2) Uani 1 2 d S . . O2 O 0.1643(6) 0.5706(5) 0.1523(6) 0.0529(17) Uani 1 1 d . . . C1 C 0.0000 0.2500 0.0629(17) 0.041(4) Uani 1 4 d S . . H1 H 0.0000 0.2500 -0.0490 0.049 Uiso 1 4 calc SR . . C2 C 0.2500 0.5312(12) 0.2500 0.083(6) Uani 1 2 d S . . H2 H 0.2500 0.4518 0.2500 0.100 Uiso 1 2 calc SR . . N1 N 0.5000 0.7500 0.040(2) 0.071(5) Uani 1 4 d S . . N2 N 0.401(2) 0.686(2) -0.0269(17) 0.066(5) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0511(14) 0.0302(14) 0.0135(12) 0.0001(7) 0.000 0.000 O1 0.075(5) 0.031(4) 0.033(4) 0.000(4) 0.000 0.000 O2 0.057(3) 0.057(4) 0.045(3) 0.005(3) -0.016(3) -0.008(3) C1 0.052(8) 0.050(10) 0.020(7) 0.000 0.000 0.000 C2 0.138(16) 0.040(6) 0.072(11) 0.000 -0.069(12) 0.000 N1 0.081(12) 0.094(15) 0.039(8) 0.000 0.000 0.000 N2 0.069(11) 0.086(12) 0.044(8) 0.011(8) 0.005(7) -0.021(10) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 2.076(5) . ? Co1 O2 2.076(5) 9_565 ? Co1 O2 2.076(5) 12 ? Co1 O2 2.076(5) 4_565 ? Co1 O1 2.135(7) . ? Co1 O1 2.135(7) 9_565 ? O1 C1 1.242(10) . ? O2 C2 1.192(8) . ? C1 O1 1.242(10) 2 ? C2 O2 1.192(8) 7_545 ? N1 N2 1.27(2) . ? N1 N2 1.27(2) 11_575 ? N1 N2 1.27(2) 2_665 ? N1 N2 1.27(2) 12_655 ? N2 N2 1.50(5) 11_575 ? N2 N2 1.72(4) 12_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 O2 180.0 . 9_565 ? O2 Co1 O2 86.5(3) . 12 ? O2 Co1 O2 93.5(3) 9_565 12 ? O2 Co1 O2 93.5(3) . 4_565 ? O2 Co1 O2 86.5(3) 9_565 4_565 ? O2 Co1 O2 180.0 12 4_565 ? O2 Co1 O1 91.5(2) . . ? O2 Co1 O1 88.5(2) 9_565 . ? O2 Co1 O1 91.5(2) 12 . ? O2 Co1 O1 88.5(2) 4_565 . ? O2 Co1 O1 88.5(2) . 9_565 ? O2 Co1 O1 91.5(2) 9_565 9_565 ? O2 Co1 O1 88.5(2) 12 9_565 ? O2 Co1 O1 91.5(2) 4_565 9_565 ? O1 Co1 O1 180.0(4) . 9_565 ? C1 O1 Co1 121.1(7) . . ? C2 O2 Co1 133.4(8) . . ? O1 C1 O1 124.4(13) . 2 ? O2 C2 O2 134.5(14) 7_545 . ? N2 N1 N2 72(2) . 11_575 ? N2 N1 N2 128(2) . 2_665 ? N2 N1 N2 85(2) 11_575 2_665 ? N2 N1 N2 85(2) . 12_655 ? N2 N1 N2 128(2) 11_575 12_655 ? N2 N1 N2 72(2) 2_665 12_655 ? N1 N2 N2 53.9(11) . 11_575 ? N1 N2 N2 47.4(10) . 12_655 ? N2 N2 N2 90.000(4) 11_575 12_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.778 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.219 #===END data_2a_ _database_code_depnum_ccdc_archive 'CCDC 744585' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C6 H6 Cr N0 Na O14' _chemical_formula_sum 'C6 H6 Cr N0 Na O14' _chemical_formula_weight 377.10 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 7.9370(6) _cell_length_b 7.9370(6) _cell_length_c 21.449(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1170.16(17) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2207 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 27.66 _exptl_crystal_description 'prism shaped' _exptl_crystal_colour violet _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 567 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8391 _exptl_absorpt_correction_T_max 0.8791 _exptl_absorpt_process_details SADABS _exptl_special_details ; 'none' ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4203 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0134 _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 -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 26.32 _reflns_number_total 542 _reflns_number_gt 518 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1999)' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.0587P)^2^+2.2135P] 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 542 _refine_ls_number_parameters 35 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.1025 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 0.0000 0.0000 0.5000 0.0218(3) Uani 1 6 d S . . O1 O 0.2199(2) 0.1729(2) 0.55437(7) 0.0312(4) Uani 1 1 d . . . O2 O 0.3950(3) 0.4490(3) 0.60575(8) 0.0415(5) Uani 1 1 d . . . O3 O 0.0000 0.0000 0.68990(17) 0.0581(10) Uani 1 3 d S . . C1 C 0.2642(4) 0.3434(3) 0.57004(11) 0.0361(6) Uani 1 1 d . . . H1 H 0.1907 0.3934 0.5529 0.043 Uiso 1 1 calc R . . Na1 Na 0.3333 0.6667 0.6667 0.0282(5) Uani 1 6 d S . . 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 0.0199(3) 0.0199(3) 0.0255(4) 0.000 0.000 0.00997(16) O1 0.0290(8) 0.0261(8) 0.0381(8) -0.0062(6) -0.0079(6) 0.0135(6) O2 0.0357(9) 0.0356(10) 0.0529(11) -0.0174(8) -0.0114(8) 0.0177(8) O3 0.0583(14) 0.0583(14) 0.058(2) 0.000 0.000 0.0292(7) C1 0.0362(13) 0.0304(11) 0.0444(13) -0.0074(10) -0.0092(10) 0.0186(10) Na1 0.0265(7) 0.0265(7) 0.0316(10) 0.000 0.000 0.0132(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.9734(15) 10_556 ? Cr1 O1 1.9734(15) . ? Cr1 O1 1.9734(15) 2 ? Cr1 O1 1.9734(15) 11_556 ? Cr1 O1 1.9734(15) 12_556 ? Cr1 O1 1.9734(15) 3 ? O1 C1 1.262(3) . ? O2 C1 1.223(3) . ? O2 Na1 2.4034(17) . ? C1 Na1 3.126(2) . ? Na1 O2 2.4034(17) 3_565 ? Na1 O2 2.4034(17) 2_665 ? Na1 O2 2.4034(17) 15_556 ? Na1 O2 2.4035(17) 14_456 ? Na1 O2 2.4035(17) 13_566 ? Na1 C1 3.126(2) 3_565 ? Na1 C1 3.126(2) 2_665 ? Na1 C1 3.126(2) 15_556 ? Na1 C1 3.126(2) 14_456 ? Na1 C1 3.126(2) 13_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cr1 O1 180.0 10_556 . ? O1 Cr1 O1 91.37(7) 10_556 2 ? O1 Cr1 O1 88.63(7) . 2 ? O1 Cr1 O1 88.63(7) 10_556 11_556 ? O1 Cr1 O1 91.37(7) . 11_556 ? O1 Cr1 O1 180.00(7) 2 11_556 ? O1 Cr1 O1 88.63(7) 10_556 12_556 ? O1 Cr1 O1 91.37(7) . 12_556 ? O1 Cr1 O1 91.37(7) 2 12_556 ? O1 Cr1 O1 88.63(7) 11_556 12_556 ? O1 Cr1 O1 91.37(7) 10_556 3 ? O1 Cr1 O1 88.63(7) . 3 ? O1 Cr1 O1 88.63(7) 2 3 ? O1 Cr1 O1 91.37(7) 11_556 3 ? O1 Cr1 O1 180.0 12_556 3 ? C1 O1 Cr1 125.33(15) . . ? C1 O2 Na1 115.15(16) . . ? O2 C1 O1 126.0(2) . . ? O2 C1 Na1 44.10(12) . . ? O1 C1 Na1 153.80(17) . . ? O2 Na1 O2 93.25(6) 3_565 2_665 ? O2 Na1 O2 179.998(1) 3_565 15_556 ? O2 Na1 O2 86.75(6) 2_665 15_556 ? O2 Na1 O2 93.25(6) 3_565 . ? O2 Na1 O2 93.25(6) 2_665 . ? O2 Na1 O2 86.75(6) 15_556 . ? O2 Na1 O2 86.75(6) 3_565 14_456 ? O2 Na1 O2 180.0 2_665 14_456 ? O2 Na1 O2 93.25(6) 15_556 14_456 ? O2 Na1 O2 86.75(6) . 14_456 ? O2 Na1 O2 86.75(6) 3_565 13_566 ? O2 Na1 O2 86.75(6) 2_665 13_566 ? O2 Na1 O2 93.25(6) 15_556 13_566 ? O2 Na1 O2 179.999(1) . 13_566 ? O2 Na1 O2 93.25(6) 14_456 13_566 ? O2 Na1 C1 20.75(6) 3_565 3_565 ? O2 Na1 C1 72.96(7) 2_665 3_565 ? O2 Na1 C1 159.25(6) 15_556 3_565 ? O2 Na1 C1 98.45(7) . 3_565 ? O2 Na1 C1 107.04(7) 14_456 3_565 ? O2 Na1 C1 81.55(7) 13_566 3_565 ? O2 Na1 C1 98.45(7) 3_565 2_665 ? O2 Na1 C1 20.75(6) 2_665 2_665 ? O2 Na1 C1 81.55(7) 15_556 2_665 ? O2 Na1 C1 72.96(7) . 2_665 ? O2 Na1 C1 159.25(6) 14_456 2_665 ? O2 Na1 C1 107.04(7) 13_566 2_665 ? C1 Na1 C1 80.83(7) 3_565 2_665 ? O2 Na1 C1 72.96(7) 3_565 . ? O2 Na1 C1 98.45(7) 2_665 . ? O2 Na1 C1 107.04(7) 15_556 . ? O2 Na1 C1 20.75(6) . . ? O2 Na1 C1 81.55(7) 14_456 . ? O2 Na1 C1 159.25(6) 13_566 . ? C1 Na1 C1 80.83(7) 3_565 . ? C1 Na1 C1 80.83(7) 2_665 . ? O2 Na1 C1 159.25(6) 3_565 15_556 ? O2 Na1 C1 107.04(7) 2_665 15_556 ? O2 Na1 C1 20.75(6) 15_556 15_556 ? O2 Na1 C1 81.55(7) . 15_556 ? O2 Na1 C1 72.96(7) 14_456 15_556 ? O2 Na1 C1 98.45(7) 13_566 15_556 ? C1 Na1 C1 179.999(1) 3_565 15_556 ? C1 Na1 C1 99.17(7) 2_665 15_556 ? C1 Na1 C1 99.17(7) . 15_556 ? O2 Na1 C1 81.55(7) 3_565 14_456 ? O2 Na1 C1 159.25(6) 2_665 14_456 ? O2 Na1 C1 98.45(7) 15_556 14_456 ? O2 Na1 C1 107.04(7) . 14_456 ? O2 Na1 C1 20.75(6) 14_456 14_456 ? O2 Na1 C1 72.96(7) 13_566 14_456 ? C1 Na1 C1 99.17(7) 3_565 14_456 ? C1 Na1 C1 180.00(8) 2_665 14_456 ? C1 Na1 C1 99.17(7) . 14_456 ? C1 Na1 C1 80.83(7) 15_556 14_456 ? O2 Na1 C1 107.04(7) 3_565 13_566 ? O2 Na1 C1 81.55(7) 2_665 13_566 ? O2 Na1 C1 72.96(7) 15_556 13_566 ? O2 Na1 C1 159.25(6) . 13_566 ? O2 Na1 C1 98.45(7) 14_456 13_566 ? O2 Na1 C1 20.75(6) 13_566 13_566 ? C1 Na1 C1 99.17(7) 3_565 13_566 ? C1 Na1 C1 99.17(7) 2_665 13_566 ? C1 Na1 C1 180.00(12) . 13_566 ? C1 Na1 C1 80.83(7) 15_556 13_566 ? C1 Na1 C1 80.83(7) 14_456 13_566 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.32 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.589 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.065 #===END data_2b_ _database_code_depnum_ccdc_archive 'CCDC 744586' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _chemical_name_common ;Department of Chemistry University of Anywhere Sometown Somewhere, UK ; _chemical_melting_point ? _chemical_formula_moiety 'C6 H12 Cr N3 O12' _chemical_formula_sum 'C6 H12 Cr N3 O12' _chemical_formula_weight 370.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 trigonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 7.94120(10) _cell_length_b 7.94120(10) _cell_length_c 21.5191(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1175.24(3) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3370 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 30.43 _exptl_crystal_description 'prism shaped' _exptl_crystal_colour violet _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 567 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8325 _exptl_absorpt_correction_T_max 0.8705 _exptl_absorpt_process_details SADABS _exptl_special_details ; 'none' ; _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4689 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_max 30.51 _reflns_number_total 1112 _reflns_number_gt 1056 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1999)' _computing_publication_material WinGX _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^ > 2\s(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^)+(0.1450P)^2^+5.0031P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 10(10) _refine_ls_number_reflns 1112 _refine_ls_number_parameters 67 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0730 _refine_ls_wR_factor_ref 0.2226 _refine_ls_wR_factor_gt 0.2175 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.164 _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 0.3333 0.6667 0.10873(7) 0.0243(4) Uani 1 3 d S . . C2 C 0.5986(13) 0.5844(12) 0.1794(5) 0.050(2) Uani 1 1 d . . . H2 H 0.5277 0.4600 0.1627 0.060 Uiso 1 1 calc R . . C1 C 0.2559(12) 0.3264(10) 0.0394(4) 0.0333(14) Uani 1 1 d . . . H1 H 0.1326 0.2803 0.0562 0.040 Uiso 1 1 calc R . . O1 O 0.3776(7) 0.4898(7) 0.0536(2) 0.0305(10) Uani 1 1 d . . . O2 O 0.5501(9) 0.7156(7) 0.1613(3) 0.0364(12) Uani 1 1 d . . . O3 O 0.7293(8) 0.6142(8) 0.2162(3) 0.0401(14) Uani 1 1 d . . . N1 N 0.2763(9) 0.2154(10) 0.0056(3) 0.0366(15) Uani 1 1 d . . . H1A H 0.3875 0.2510 -0.0112 0.044 Uiso 1 1 calc R . . H1B H 0.1796 0.1013 -0.0016 0.044 Uiso 1 1 calc R . . O1W O 0.0000 0.0000 -0.0573(3) 0.0051(6) Uani 1 3 d S . . O2W O 0.0000 0.0000 0.2487(6) 0.048(3) Uani 1 3 d S . . O3W O 0.6667 0.3333 -0.0388(6) 0.060(3) Uani 1 3 d S . . 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 0.0229(4) 0.0229(4) 0.0271(6) 0.000 0.000 0.0114(2) C2 0.057(5) 0.022(3) 0.077(6) 0.006(3) 0.001(4) 0.025(4) C1 0.042(4) 0.035(3) 0.031(3) -0.009(3) 0.004(3) 0.025(3) O1 0.029(2) 0.026(2) 0.040(3) -0.0125(19) 0.0021(19) 0.0170(19) O2 0.048(3) 0.030(2) 0.038(3) 0.000(2) 0.002(2) 0.024(2) O3 0.041(3) 0.032(3) 0.047(3) 0.006(2) -0.008(2) 0.018(2) N1 0.034(3) 0.029(3) 0.053(4) -0.023(3) -0.004(3) 0.020(3) O1W 0.0030(7) 0.0030(7) 0.0092(14) 0.000 0.000 0.0015(4) O2W 0.043(3) 0.043(3) 0.059(6) 0.000 0.000 0.0216(17) O3W 0.068(5) 0.068(5) 0.044(6) 0.000 0.000 0.034(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O2 1.930(6) 2_665 ? Cr1 O2 1.930(6) . ? Cr1 O2 1.930(6) 3_565 ? Cr1 O1 2.000(5) 3_565 ? Cr1 O1 2.000(5) 2_665 ? Cr1 O1 2.000(5) . ? C2 O3 1.232(12) . ? C2 O2 1.337(9) . ? C1 O1 1.208(9) . ? C1 N1 1.214(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 O2 Cr1 O2 89.1(3) 2_665 . ? O2 Cr1 O2 89.1(3) 2_665 3_565 ? O2 Cr1 O2 89.1(3) . 3_565 ? O2 Cr1 O1 90.4(2) 2_665 3_565 ? O2 Cr1 O1 178.7(3) . 3_565 ? O2 Cr1 O1 92.1(2) 3_565 3_565 ? O2 Cr1 O1 92.1(2) 2_665 2_665 ? O2 Cr1 O1 90.4(2) . 2_665 ? O2 Cr1 O1 178.7(3) 3_565 2_665 ? O1 Cr1 O1 88.4(2) 3_565 2_665 ? O2 Cr1 O1 178.7(3) 2_665 . ? O2 Cr1 O1 92.1(2) . . ? O2 Cr1 O1 90.4(2) 3_565 . ? O1 Cr1 O1 88.4(2) 3_565 . ? O1 Cr1 O1 88.4(2) 2_665 . ? O3 C2 O2 125.5(8) . . ? O1 C1 N1 127.3(8) . . ? C1 O1 Cr1 125.3(4) . . ? C2 O2 Cr1 126.1(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 2.759 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.144 #===END