Polar Materials with Isolated V4+ S = 1/2 Triangles: NaSr2V3O3(Ge4O13)Cl and KSr2V3O3(Ge4O13)Cl
Sanjeewa, Liurukara D.; McGuire, Michael A.; McMillen, Colin D.; Garlea, Vasile O.; Kolis, Joseph W.; Chemistry of Materials 29 (2017) 1404–; doi:10.1021/acs.chemmater.6b05320

data_4002703
_publ_section_title
;
 Polar Materials with Isolated V4+ S = 1/2 Triangles: NaSr2V3O3(Ge4O13)Cl
 and KSr2V3O3(Ge4O13)Cl
;
_journal_issue                   3
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1404
_journal_paper_doi               10.1021/acs.chemmater.6b05320
_journal_volume                  29
_journal_year                    2017
_chemical_formula_sum            'Cl Ge4 K O16 Sr2 V3'
_chemical_formula_weight         948.97
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.4679(7)
_cell_length_b                   10.4679(7)
_cell_length_c                   7.2427(5)
_cell_measurement_reflns_used    6229
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.88
_cell_measurement_theta_min      2.80
_cell_volume                     687.31(8)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku AFC8S, Mercury CCD'
_diffrn_measurement_method       'w\ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1365
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5913
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.057
_diffrn_reflns_theta_min         3.601
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    18.847
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB, CrystalClear'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.585
_exptl_crystal_description       block
_exptl_crystal_F_000             874
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details
;
 Flack x determined using 210 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.07(2)
_refine_ls_extinction_coef       0.0020(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         513
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0379
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+23.8938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.787
_reflns_Friedel_fraction_full    0.938
_reflns_Friedel_fraction_max     0.930
_reflns_number_gt                512
_reflns_number_total             513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm6b05320_si_001.cif
_cod_data_source_block           cd1251a
_cod_depositor_comments
'Adding full bibliography for 4002702--4002703.cif.'
_cod_original_cell_volume        687.31(10)
_cod_database_code               4002703
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.104
_shelx_estimated_absorpt_t_max   0.211
_shelx_res_checksum              12349
_shelx_hkl_checksum              79591