#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/55/7015522.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7015522 loop_ _publ_author_name 'Duan, Zhiming' 'Wang, Zheming' 'Gao, Song' _publ_section_title ; Irreversible transformation of chiral to achiral polymorph of K[Co(HCOO)3]: synthesis, structures, and magnetic properties. ; _journal_issue 17 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 4465 _journal_page_last 4473 _journal_volume 40 _journal_year 2011 _chemical_formula_sum 'C3 H3 Co K O6' _chemical_formula_weight 233.08 _chemical_name_systematic ; ? ; _space_group_IT_number 182 _symmetry_cell_setting hexagonal _symmetry_space_group_name_Hall 'P 6c 2c' _symmetry_space_group_name_H-M 'P 63 2 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_formula_units_Z 2 _cell_length_a 6.9930(13) _cell_length_b 6.9930(13) _cell_length_c 8.4439(15) _cell_measurement_reflns_used 2886 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 27.4835 _cell_measurement_theta_min 3.3617 _cell_volume 357.60(11) _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_molecular_graphics 'Bruker SHELXTL V5.1 (Sheldrick, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 180(2) _diffrn_detector_area_resol_mean 15 _diffrn_measured_fraction_theta_full 0.970 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measurement_device_type 'Rigaku Mercury CCD (AFC7)' _diffrn_measurement_method CCD _diffrn_radiation_detector CCD _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0145 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 5906 _diffrn_reflns_theta_full 27.43 _diffrn_reflns_theta_max 27.43 _diffrn_reflns_theta_min 3.36 _diffrn_source_current 100.0000 _diffrn_source_power '5.4 kW' _diffrn_source_voltage 50.0000 _diffrn_standards_decay_% none _exptl_absorpt_coefficient_mu 2.959 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8289 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private Communication' _exptl_crystal_colour pink _exptl_crystal_density_diffrn 2.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'hexagonal bipyramid' _exptl_crystal_F_000 230 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.173 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.053 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(4) _refine_ls_extinction_coef 0.027(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_hydrogen_treatment constr. _refine_ls_matrix_type full _refine_ls_number_parameters 20 _refine_ls_number_reflns 275 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.178 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0189 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.0264P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.0465 _reflns_number_gt 248 _reflns_number_total 275 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0dt01701a.txt _[local]_cod_data_source_block 1-at-180K _[local]_cod_cif_authors_sg_H-M 'P 6(3)22' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius ; _cod_database_code 7015522 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z' 'x-y, -y, -z' '-x, -x+y, -z' '-y, -x, -z+1/2' '-x+y, y, -z+1/2' 'x, x-y, -z+1/2' 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 0.6667 0.3333 0.2500 0.0120(2) Uani 1 6 d S . . K1 K 0.0000 0.0000 0.2500 0.0202(3) Uani 1 6 d S . . O1 O 0.4045(2) 0.1009(2) 0.10966(14) 0.0195(3) Uani 1 1 d . . . C1 C 0.4346(4) 0.0000 0.0000 0.0256(7) Uani 1 2 d S . . H1 H 0.5704 0.0000 0.0000 0.031 Uiso 1 2 calc SR . . 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 0.0138(2) 0.0138(2) 0.0083(3) 0.000 0.000 0.00690(11) K1 0.0184(3) 0.0184(3) 0.0238(5) 0.000 0.000 0.00918(16) O1 0.0190(6) 0.0217(6) 0.0167(5) -0.0068(6) -0.0014(5) 0.0093(5) C1 0.0198(10) 0.0329(18) 0.0285(13) -0.0154(12) -0.0077(6) 0.0164(9) 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' K K 0.2009 0.2494 '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' 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 Co1 O1 96.02(6) 11_655 . ? O1 Co1 O1 91.38(5) 11_655 10_665 ? O1 Co1 O1 170.19(6) . 10_665 ? O1 Co1 O1 82.03(6) 11_655 2_655 ? O1 Co1 O1 91.38(5) . 2_655 ? O1 Co1 O1 96.02(6) 10_665 2_655 ? O1 Co1 O1 91.38(5) 11_655 12 ? O1 Co1 O1 82.03(6) . 12 ? O1 Co1 O1 91.38(5) 10_665 12 ? O1 Co1 O1 170.19(6) 2_655 12 ? O1 Co1 O1 170.19(6) 11_655 3_665 ? O1 Co1 O1 91.38(5) . 3_665 ? O1 Co1 O1 82.03(6) 10_665 3_665 ? O1 Co1 O1 91.38(5) 2_655 3_665 ? O1 Co1 O1 96.02(6) 12 3_665 ? O1 K1 O1 154.90(5) 12 3 ? O1 K1 O1 58.81(5) 12 . ? O1 K1 O1 103.51(3) 3 . ? O1 K1 O1 98.34(5) 12 2 ? O1 K1 O1 103.51(3) 3 2 ? O1 K1 O1 103.51(3) . 2 ? O1 K1 O1 103.51(3) 12 10 ? O1 K1 O1 58.81(5) 3 10 ? O1 K1 O1 98.34(5) . 10 ? O1 K1 O1 154.90(5) 2 10 ? O1 K1 O1 103.51(3) 12 11 ? O1 K1 O1 98.34(5) 3 11 ? O1 K1 O1 154.90(5) . 11 ? O1 K1 O1 58.81(5) 2 11 ? O1 K1 O1 103.51(3) 10 11 ? O1 K1 K1 65.08(2) 12 4 ? O1 K1 K1 114.92(2) 3 4 ? O1 K1 K1 114.92(2) . 4 ? O1 K1 K1 114.92(2) 2 4 ? O1 K1 K1 65.08(2) 10 4 ? O1 K1 K1 65.08(2) 11 4 ? O1 K1 K1 114.92(2) 12 4_554 ? O1 K1 K1 65.08(2) 3 4_554 ? O1 K1 K1 65.08(2) . 4_554 ? O1 K1 K1 65.08(2) 2 4_554 ? O1 K1 K1 114.92(2) 10 4_554 ? O1 K1 K1 114.92(2) 11 4_554 ? K1 K1 K1 180.0 4 4_554 ? C1 O1 Co1 121.90(13) . . ? C1 O1 K1 127.25(12) . . ? Co1 O1 K1 109.58(5) . . ? O1 C1 O1 126.2(3) 8 . ? O1 C1 H1 116.9 8 . ? O1 C1 H1 116.9 . . ? 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 O1 2.1040(13) 11_655 ? Co1 O1 2.1040(13) . ? Co1 O1 2.1040(13) 10_665 ? Co1 O1 2.1040(13) 2_655 ? Co1 O1 2.1040(13) 12 ? Co1 O1 2.1040(13) 3_665 ? K1 O1 2.8122(13) 12 ? K1 O1 2.8122(13) 3 ? K1 O1 2.8122(13) . ? K1 O1 2.8122(13) 2 ? K1 O1 2.8122(13) 10 ? K1 O1 2.8122(13) 11 ? K1 K1 4.2219(7) 4 ? K1 K1 4.2219(7) 4_554 ? O1 C1 1.2441(17) . ? C1 O1 1.2441(17) 8 ? C1 H1 0.9500 . ? _journal_paper_doi 10.1039/c0dt01701a