New Fluoride Carbonates: Centrosymmetric KPb2(CO3)2F and Noncentrosymmetric K2.70Pb5.15(CO3)5F3
T. Thao Tran; P. Shiv Halasyamani; Inorganic Chemistry 52 (2013) 2466–2473; doi:10.1021/ic302357h

data_4333992
_publ_contact_author_address
;
Department of Chemistry
University of Houston
Houston, Texas
77204-5003
USA
;
_publ_contact_author_email       psh@uh.edu
_publ_contact_author_fax         1-713-743-0796
_publ_contact_author_name        'P. Shiv Halasyamani'
_publ_contact_author_phone       1-832-775-8696
_publ_section_title
;
 New Fluoride Carbonates: Centrosymmetric KPb2(CO3)2F and
 Noncentrosymmetric K2.70Pb5.15(CO3)5F3
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2466
_journal_page_last               2473
_journal_paper_doi               10.1021/ic302357h
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration unk
_chemical_formula_sum            'C5 F3 K2.7 O15 Pb5.15'
_chemical_formula_weight         1529.65
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           187
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6 2'
_symmetry_space_group_name_H-M   'P -6 m 2'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   5.3052(2)
_cell_length_b                   5.3052(2)
_cell_length_c                   18.5904(10)
_cell_measurement_reflns_used    1974
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.19
_cell_volume                     453.13(3)
_computing_cell_refinement       'SAINT v7.12A (Bruker-Nonius, 2004)'
_computing_data_collection       'APEX2 v1.0-27 (Bruker-Nonius, 2005)'
_computing_data_reduction        'SAINT v7.12A (Bruker-Nonius, 2004)'
_computing_structure_refinement  'SHELXL v6.12 (G.M. Sheldrick, 2001)'
_computing_structure_solution    'SHELXS v6.12 (G.M. Sheldrick, 2001)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 4K
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            376
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    48.401
_exptl_absorpt_correction_T_max  0.9959
_exptl_absorpt_correction_T_min  0.5705
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SAINT v7.12A'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.606
_exptl_crystal_description       column
_exptl_crystal_F_000             651
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.016
_refine_diff_density_min         -1.562
_refine_diff_density_rms         0.184
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       0.0055(4)
_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   1.186
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0169
_refine_ls_R_factor_gt           0.0169
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+1.3912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0478
_reflns_number_gt                376
_reflns_number_total             376
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302357h_si_003_3.cif
_cod_data_source_block           K2.70Pb5.15(CO3)5F3_2
_cod_original_formula_sum        'C5 F3 K2.70 O15 Pb5.15'
_cod_database_code               4333992