#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/30/02/2300246.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2300246 loop_ _publ_author_name 'Kimura, Tsunehisa' 'Chang, Chengkang' 'Kimura, Fumiko' 'Maeyama, Masataka' _publ_section_title ; The pseudo-single-crystal method: a third approach to crystal structure determination ; _journal_issue 3 _journal_name_full 'Journal of Applied Crystallography' _journal_page_first 535 _journal_page_last 537 _journal_paper_doi 10.1107/S0021889809013430 _journal_volume 42 _journal_year 2009 _chemical_formula_moiety 'Co Li O4 P ' _chemical_formula_sum 'Co Li O4 P' _chemical_formula_weight 160.85 _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_formula_units_Z 4 _cell_length_a 10.202(6) _cell_length_b 5.918(3) _cell_length_c 4.709(2) _cell_measurement_reflns_used 1278 _cell_measurement_temperature 243.1 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 4.0 _cell_volume 284.3(3) _computing_cell_refinement PROCESS-AUTO _computing_data_collection PROCESS-AUTO _computing_data_reduction CrystalStructure _computing_publication_material 'CrystalStructure 3.8' _computing_structure_refinement SHELXL _computing_structure_solution SIR97 _diffrn_detector_area_resol_mean 10.00 _diffrn_measured_fraction_theta_full 0.956 _diffrn_measured_fraction_theta_max 0.958 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.133 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_number 4825 _diffrn_reflns_theta_full 27.50 _diffrn_reflns_theta_max 27.48 _exptl_absorpt_coefficient_mu 6.407 _exptl_absorpt_correction_T_max 0.146 _exptl_absorpt_correction_T_min 0.030 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _exptl_crystal_colour violet _exptl_crystal_density_diffrn 3.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 308.00 _exptl_crystal_size_max 3.00 _exptl_crystal_size_mid 3.00 _exptl_crystal_size_min 0.30 _refine_diff_density_max 1.44 _refine_diff_density_min -1.13 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_number_parameters 41 _refine_ls_number_reflns 345 _refine_ls_R_factor_gt 0.0659 _refine_ls_shift/su_max 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0479P)^2^+4.9483P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.1680 _reflns_number_gt 278 _reflns_number_total 345 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file db5060.cif _cod_data_source_block toritsu_3T_2nd _cod_original_formula_sum 'Co Li O4 P ' _cod_database_code 2300246 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2+Z 3 +X,1/2-Y,+Z 4 1/2-X,-Y,1/2+Z 5 -X,-Y,-Z 6 1/2+X,1/2-Y,1/2-Z 7 -X,1/2+Y,-Z 8 1/2+X,+Y,1/2-Z loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co Co(1) 0.72170(16) 0.2500 0.5213(4) 0.0334(6) Uani d S 1.00 . . P P(1) 0.5940(3) 0.7500 0.5816(8) 0.0334(8) Uani d S 1.00 . . O O(1) 0.6655(5) 0.5435(10) 0.7200(13) 0.0364(14) Uani d . 1.00 . . O O(2) 0.4522(8) 0.7500 0.704(2) 0.0356(19) Uani d S 1.00 . . O O(3) 0.5982(8) 0.7500 0.257(2) 0.0336(19) Uani d S 1.00 . . Li Li(1) 0.5000 0.5000 1.0000 0.032(4) Uani d S 1.00 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co(1) 0.0324(9) 0.0229(9) 0.0448(12) 0.0000 0.0004(6) 0.0000 P(1) 0.0305(15) 0.0234(15) 0.046(2) 0.0000 0.0012(13) 0.0000 O(1) 0.039(3) 0.027(3) 0.044(3) 0.004(2) -0.007(2) 0.000(2) O(2) 0.033(4) 0.029(4) 0.045(5) 0.0000 0.002(3) 0.0000 O(3) 0.035(4) 0.016(3) 0.050(5) 0.0000 0.004(3) 0.0000 Li(1) 0.023(8) 0.020(8) 0.052(12) -0.011(7) 0.006(7) -0.002(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Li Li 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Co Co 0.349 0.972 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; P P 0.102 0.094 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Co1 O1 . 3 115.4(4) ? O1 Co1 O2 . 5_666 89.6(2) ? O1 Co1 O2 3 5_666 89.6(2) ? O1 Co1 O3 . 2_645 90.2(2) ? O1 Co1 O3 3 2_645 90.2(2) ? O2 Co1 O3 5_666 2_645 179.7(4) ? O1 Co1 O1 . 2_644 155.5(3) ? O1 Co1 O1 3 2_644 88.29(15) ? O2 Co1 O1 5_666 2_644 96.8(3) ? O3 Co1 O1 2_645 2_644 83.5(3) ? O1 Co1 O1 . 4_664 88.28(15) ? O1 Co1 O1 3 4_664 155.5(3) ? O2 Co1 O1 5_666 4_664 96.8(3) ? O3 Co1 O1 2_645 4_664 83.5(3) ? O1 Co1 O1 2_644 4_664 67.6(3) ? O1 Co1 P1 . 2_644 121.66(19) ? O1 Co1 P1 3 2_644 121.66(19) ? O2 Co1 P1 5_666 2_644 101.4(3) ? O3 Co1 P1 2_645 2_644 78.9(3) ? O1 Co1 P1 2_644 2_644 33.92(16) ? O1 Co1 P1 4_664 2_644 33.92(16) ? O1 Co1 Li1 . 4_664 82.60(18) ? O1 Co1 Li1 3 4_664 130.71(18) ? O2 Co1 Li1 5_666 4_664 138.15(19) ? O3 Co1 Li1 2_645 4_664 42.08(18) ? O1 Co1 Li1 2_644 4_664 76.85(16) ? O1 Co1 Li1 4_664 4_664 42.16(17) ? P1 Co1 Li1 2_644 4_664 51.76(7) ? O1 Co1 Li1 . 2_644 130.71(18) ? O1 Co1 Li1 3 2_644 82.61(18) ? O2 Co1 Li1 5_666 2_644 138.15(19) ? O3 Co1 Li1 2_645 2_644 42.08(18) ? O1 Co1 Li1 2_644 2_644 42.16(17) ? O1 Co1 Li1 4_664 2_644 76.85(16) ? P1 Co1 Li1 2_644 2_644 51.76(7) ? Li1 Co1 Li1 4_664 2_644 55.02(4) ? O3 P1 O2 . . 113.3(5) ? O3 P1 O1 . . 113.8(3) ? O2 P1 O1 . . 106.2(4) ? O3 P1 O1 . 3_565 113.8(3) ? O2 P1 O1 . 3_565 106.2(4) ? O1 P1 O1 . 3_565 102.7(5) ? O3 P1 Li1 . 3_565 139.0(2) ? O2 P1 Li1 . 3_565 52.2(3) ? O1 P1 Li1 . 3_565 107.2(3) ? O1 P1 Li1 3_565 3_565 54.7(3) ? O3 P1 Li1 . . 139.0(2) ? O2 P1 Li1 . . 52.2(3) ? O1 P1 Li1 . . 54.7(3) ? O1 P1 Li1 3_565 . 107.2(3) ? Li1 P1 Li1 3_565 . 68.06(9) ? O3 P1 Co1 . 2_655 136.2(4) ? O2 P1 Co1 . 2_655 110.6(4) ? O1 P1 Co1 . 2_655 51.6(2) ? O1 P1 Co1 3_565 2_655 51.6(2) ? Li1 P1 Co1 3_565 2_655 72.08(10) ? Li1 P1 Co1 . 2_655 72.08(10) ? P1 O1 Co1 . . 126.9(4) ? P1 O1 Li1 . . 89.0(3) ? Co1 O1 Li1 . . 113.3(3) ? P1 O1 Co1 . 2_655 94.5(3) ? Co1 O1 Co1 . 2_655 128.2(3) ? Li1 O1 Co1 . 2_655 94.7(3) ? P1 O2 Co1 . 5_666 127.5(6) ? P1 O2 Li1 . 3_565 91.7(3) ? Co1 O2 Li1 5_666 3_565 122.8(3) ? P1 O2 Li1 . . 91.7(3) ? Co1 O2 Li1 5_666 . 122.8(3) ? Li1 O2 Li1 3_565 . 90.1(4) ? P1 O3 Co1 . 2_654 122.8(5) ? P1 O3 Li1 . 1_554 123.2(3) ? Co1 O3 Li1 2_654 1_554 96.1(3) ? P1 O3 Li1 . 3_564 123.2(3) ? Co1 O3 Li1 2_654 3_564 96.1(3) ? Li1 O3 Li1 1_554 3_564 86.5(3) ? O2 Li1 O2 5_667 . 179.9990(10) ? O2 Li1 O1 5_667 5_667 72.0(3) ? O2 Li1 O1 . 5_667 108.0(3) ? O2 Li1 O1 5_667 . 108.0(3) ? O2 Li1 O1 . . 72.0(3) ? O1 Li1 O1 5_667 . 179.9990(10) ? O2 Li1 O3 5_667 1_556 90.1(2) ? O2 Li1 O3 . 1_556 89.9(2) ? O1 Li1 O3 5_667 1_556 95.8(3) ? O1 Li1 O3 . 1_556 84.2(3) ? O2 Li1 O3 5_667 5_666 89.9(2) ? O2 Li1 O3 . 5_666 90.1(2) ? O1 Li1 O3 5_667 5_666 84.2(3) ? O1 Li1 O3 . 5_666 95.8(3) ? O3 Li1 O3 1_556 5_666 179.9990(10) ? O2 Li1 P1 5_667 . 143.9(2) ? O2 Li1 P1 . . 36.1(2) ? O1 Li1 P1 5_667 . 143.71(17) ? O1 Li1 P1 . . 36.29(17) ? O3 Li1 P1 1_556 . 82.3(2) ? O3 Li1 P1 5_666 . 97.7(2) ? O2 Li1 P1 5_667 5_667 36.1(2) ? O2 Li1 P1 . 5_667 143.9(2) ? O1 Li1 P1 5_667 5_667 36.29(17) ? O1 Li1 P1 . 5_667 143.71(17) ? O3 Li1 P1 1_556 5_667 97.7(2) ? O3 Li1 P1 5_666 5_667 82.3(2) ? P1 Li1 P1 . 5_667 180.0 ? O2 Li1 Li1 5_667 3_565 135.03(19) ? O2 Li1 Li1 . 3_565 44.97(19) ? O1 Li1 Li1 5_667 3_565 96.85(16) ? O1 Li1 Li1 . 3_565 83.15(16) ? O3 Li1 Li1 1_556 3_565 46.74(17) ? O3 Li1 Li1 5_666 3_565 133.26(17) ? P1 Li1 Li1 . 3_565 55.97(5) ? P1 Li1 Li1 5_667 3_565 124.03(5) ? O2 Li1 Li1 5_667 3 44.97(19) ? O2 Li1 Li1 . 3 135.03(19) ? O1 Li1 Li1 5_667 3 83.15(16) ? O1 Li1 Li1 . 3 96.85(16) ? O3 Li1 Li1 1_556 3 133.26(17) ? O3 Li1 Li1 5_666 3 46.74(17) ? P1 Li1 Li1 . 3 124.03(5) ? P1 Li1 Li1 5_667 3 55.97(5) ? Li1 Li1 Li1 3_565 3 180.0 ? O2 Li1 Co1 5_667 2_655 95.7(2) ? O2 Li1 Co1 . 2_655 84.3(2) ? O1 Li1 Co1 5_667 2_655 136.85(17) ? O1 Li1 Co1 . 2_655 43.15(17) ? O3 Li1 Co1 1_556 2_655 41.8(2) ? O3 Li1 Co1 5_666 2_655 138.2(2) ? P1 Li1 Co1 . 2_655 56.16(8) ? P1 Li1 Co1 5_667 2_655 123.84(8) ? Li1 Li1 Co1 3_565 2_655 62.49(2) ? Li1 Li1 Co1 3 2_655 117.51(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 O1 . 2.055(6) ? Co1 O1 3 2.055(6) ? Co1 O2 5_666 2.066(9) ? Co1 O3 2_645 2.147(9) ? Co1 O1 2_644 2.198(6) ? Co1 O1 4_664 2.198(6) ? Co1 P1 2_644 2.796(4) ? Co1 Li1 4_664 3.203(2) ? Co1 Li1 2_644 3.203(2) ? P1 O3 . 1.528(10) ? P1 O2 . 1.557(9) ? P1 O1 . 1.565(6) ? P1 O1 3_565 1.565(6) ? P1 Li1 3_565 2.644(3) ? P1 Li1 . 2.644(3) ? P1 Co1 2_655 2.796(4) ? O1 Li1 . 2.157(6) ? O1 Co1 2_655 2.198(6) ? O2 Co1 5_666 2.066(9) ? O2 Li1 3_565 2.091(7) ? O2 Li1 . 2.091(7) ? O3 Co1 2_654 2.147(9) ? O3 Li1 1_554 2.159(7) ? O3 Li1 3_564 2.159(7) ? Li1 O2 5_667 2.091(7) ? Li1 O1 5_667 2.157(6) ? Li1 O3 1_556 2.159(7) ? Li1 O3 5_666 2.159(7) ? Li1 P1 5_667 2.644(3) ? Li1 Li1 3_565 2.9592(15) ? Li1 Li1 3 2.9592(15) ? Li1 Co1 2_655 3.203(2) ?