#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:10:05 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179442 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/39/4333990.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_4333990
loop_
_publ_author_name
'T. Thao Tran'
'P. Shiv Halasyamani'
_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            'C2 F K O6 Pb2'
_chemical_formula_weight         592.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           194
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_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            2
_cell_length_a                   5.3000(2)
_cell_length_b                   5.3000(2)
_cell_length_c                   13.9302(8)
_cell_measurement_reflns_used    1811
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.24
_cell_measurement_theta_min      2.92
_cell_volume                     338.88(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 v5.10 (G.M. Sheldrick, 1997)'
_computing_structure_solution    'SHELXS v5.10 (G.M. Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 4K
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0471
_diffrn_reflns_av_sigmaI/netI    0.0060
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2074
_diffrn_reflns_theta_full        29.24
_diffrn_reflns_theta_max         29.24
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    50.237
_exptl_absorpt_correction_T_max  0.6817
_exptl_absorpt_correction_T_min  0.0561
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SAINT v7.12A'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    5.807
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.251
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.340
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.340
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0187
_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/[σ²(Fo²)+(0.0370P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0513
_reflns_number_gt                208
_reflns_number_total             208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302357h_si_003_1.cif
_cod_data_source_block           KPb2(CO3)2F
_cod_database_code               4333990
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'
'-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
K1 K 0.6667 0.3333 0.2500 0.0170(7) Uani 1 12 d S
Pb1 Pb 0.3333 0.6667 0.41745(2) 0.01677(19) Uani 1 6 d S
F1 F 0.3333 0.6667 0.2500 0.025(2) Uani 1 12 d S
O1 O 0.2782(7) 0.1391(4) 0.3935(3) 0.0216(7) Uani 1 2 d S
C1 C 0.0000 0.0000 0.3926(5) 0.0167(13) Uani 1 6 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
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
O1 K1 O1 96.54(16) 17_656 2_655
O1 K1 O1 70.40(13) 17_656 16_556
O1 K1 O1 141.12(6) 2_655 16_556
O1 K1 O1 141.12(6) 17_656 3_665
O1 K1 O1 70.40(13) 2_655 3_665
O1 K1 O1 141.12(6) 16_556 3_665
O1 K1 O1 141.12(6) 17_656 .
O1 K1 O1 70.40(13) 2_655 .
O1 K1 O1 96.54(16) 16_556 .
O1 K1 O1 70.40(13) 3_665 .
O1 K1 O1 70.40(13) 17_656 18_666
O1 K1 O1 141.12(6) 2_655 18_666
O1 K1 O1 70.40(13) 16_556 18_666
O1 K1 O1 96.54(16) 3_665 18_666
O1 K1 O1 141.12(6) . 18_666
O1 K1 F1 70.56(3) 17_656 1_655
O1 K1 F1 70.56(3) 2_655 1_655
O1 K1 F1 131.73(8) 16_556 1_655
O1 K1 F1 70.56(3) 3_665 1_655
O1 K1 F1 131.73(8) . 1_655
O1 K1 F1 70.56(3) 18_666 1_655
O1 K1 F1 70.56(3) 17_656 1_545
O1 K1 F1 70.56(3) 2_655 1_545
O1 K1 F1 70.56(3) 16_556 1_545
O1 K1 F1 131.73(8) 3_665 1_545
O1 K1 F1 70.56(3) . 1_545
O1 K1 F1 131.73(8) 18_666 1_545
F1 K1 F1 120.0 1_655 1_545
O1 K1 F1 131.73(8) 17_656 .
O1 K1 F1 131.73(8) 2_655 .
O1 K1 F1 70.56(3) 16_556 .
O1 K1 F1 70.56(3) 3_665 .
O1 K1 F1 70.56(3) . .
O1 K1 F1 70.56(3) 18_666 .
F1 K1 F1 120.0 1_655 .
F1 K1 F1 120.0 1_545 .
O1 K1 Pb1 44.183(13) 17_656 16_546
O1 K1 Pb1 100.82(6) 2_655 16_546
O1 K1 Pb1 44.183(13) 16_556 16_546
O1 K1 Pb1 169.05(8) 3_665 16_546
O1 K1 Pb1 100.82(6) . 16_546
O1 K1 Pb1 94.41(8) 18_666 16_546
F1 K1 Pb1 113.430(1) 1_655 16_546
F1 K1 Pb1 37.319(4) 1_545 16_546
F1 K1 Pb1 113.430(1) . 16_546
O1 K1 Pb1 100.82(6) 17_656 1_655
O1 K1 Pb1 44.183(13) 2_655 1_655
O1 K1 Pb1 169.05(8) 16_556 1_655
O1 K1 Pb1 44.183(13) 3_665 1_655
O1 K1 Pb1 94.41(8) . 1_655
O1 K1 Pb1 100.82(6) 18_666 1_655
F1 K1 Pb1 37.319(4) 1_655 1_655
F1 K1 Pb1 113.430(1) 1_545 1_655
F1 K1 Pb1 113.430(1) . 1_655
Pb1 K1 Pb1 133.139(3) 16_546 1_655
O1 K1 Pb1 44.183(13) 17_656 16_656
O1 K1 Pb1 100.82(6) 2_655 16_656
O1 K1 Pb1 94.41(8) 16_556 16_656
O1 K1 Pb1 100.82(6) 3_665 16_656
O1 K1 Pb1 169.05(8) . 16_656
O1 K1 Pb1 44.183(13) 18_666 16_656
F1 K1 Pb1 37.319(4) 1_655 16_656
F1 K1 Pb1 113.430(1) 1_545 16_656
F1 K1 Pb1 113.430(1) . 16_656
Pb1 K1 Pb1 87.058(6) 16_546 16_656
Pb1 K1 Pb1 74.638(8) 1_655 16_656
F1 Pb1 O1 82.86(9) . 3_565
F1 Pb1 O1 82.86(8) . 1_565
O1 Pb1 O1 48.68(15) 3_565 1_565
F1 Pb1 O1 82.86(9) . 2
O1 Pb1 O1 70.28(15) 3_565 2
O1 Pb1 O1 118.48(4) 1_565 2
F1 Pb1 O1 82.86(9) . 2_665
O1 Pb1 O1 118.48(4) 3_565 2_665
O1 Pb1 O1 70.28(15) 1_565 2_665
O1 Pb1 O1 162.04(16) 2 2_665
F1 Pb1 O1 82.86(9) . .
O1 Pb1 O1 118.48(4) 3_565 .
O1 Pb1 O1 162.04(16) 1_565 .
O1 Pb1 O1 48.68(14) 2 .
O1 Pb1 O1 118.48(4) 2_665 .
F1 Pb1 O1 82.86(9) . 3_665
O1 Pb1 O1 162.04(16) 3_565 3_665
O1 Pb1 O1 118.48(4) 1_565 3_665
O1 Pb1 O1 118.48(4) 2 3_665
O1 Pb1 O1 48.68(14) 2_665 3_665
O1 Pb1 O1 70.28(14) . 3_665
F1 Pb1 K1 52.681(4) . 1_455
O1 Pb1 K1 44.10(8) 3_565 1_455
O1 Pb1 K1 81.35(8) 1_565 1_455
O1 Pb1 K1 44.10(8) 2 1_455
O1 Pb1 K1 129.97(8) 2_665 1_455
O1 Pb1 K1 81.35(8) . 1_455
O1 Pb1 K1 129.97(8) 3_665 1_455
F1 Pb1 K1 52.681(4) . 1_565
O1 Pb1 K1 81.35(8) 3_565 1_565
O1 Pb1 K1 44.10(8) 1_565 1_565
O1 Pb1 K1 129.97(8) 2 1_565
O1 Pb1 K1 44.10(8) 2_665 1_565
O1 Pb1 K1 129.97(8) . 1_565
O1 Pb1 K1 81.35(8) 3_665 1_565
K1 Pb1 K1 87.058(6) 1_455 1_565
F1 Pb1 K1 52.681(4) . .
O1 Pb1 K1 129.97(8) 3_565 .
O1 Pb1 K1 129.97(8) 1_565 .
O1 Pb1 K1 81.35(8) 2 .
O1 Pb1 K1 81.35(8) 2_665 .
O1 Pb1 K1 44.10(8) . .
O1 Pb1 K1 44.10(8) 3_665 .
K1 Pb1 K1 87.058(6) 1_455 .
K1 Pb1 K1 87.058(6) 1_565 .
Pb1 F1 Pb1 180.0 16_556 .
Pb1 F1 K1 90.0 16_556 1_565
Pb1 F1 K1 90.0 . 1_565
Pb1 F1 K1 90.0 16_556 1_455
Pb1 F1 K1 90.0 . 1_455
K1 F1 K1 120.0 1_565 1_455
Pb1 F1 K1 90.0 16_556 .
Pb1 F1 K1 90.0 . .
K1 F1 K1 120.0 1_565 .
K1 F1 K1 120.0 1_455 .
C1 O1 K1 131.2(4) . .
C1 O1 Pb1 95.48(9) . 1_545
K1 O1 Pb1 91.72(8) . 1_545
C1 O1 Pb1 95.48(9) . .
K1 O1 Pb1 91.72(8) . .
Pb1 O1 Pb1 162.04(16) 1_545 .
O1 C1 O1 119.991(15) 3 .
O1 C1 O1 119.991(15) 3 2
O1 C1 O1 119.991(15) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O1 2.679(4) 17_656
K1 O1 2.679(4) 2_655
K1 O1 2.679(4) 16_556
K1 O1 2.679(4) 3_665
K1 O1 2.679(4) .
K1 O1 2.679(4) 18_666
K1 F1 3.05996(11) 1_655
K1 F1 3.05996(11) 1_545
K1 F1 3.05996(11) .
K1 Pb1 3.8477(2) 16_546
K1 Pb1 3.8477(2) 1_655
K1 Pb1 3.8477(2) 16_656
Pb1 F1 2.3327(3) .
Pb1 O1 2.6829(6) 3_565
Pb1 O1 2.6829(6) 1_565
Pb1 O1 2.6829(6) 2
Pb1 O1 2.6829(6) 2_665
Pb1 O1 2.6829(6) .
Pb1 O1 2.6829(6) 3_665
Pb1 K1 3.8477(2) 1_455
Pb1 K1 3.8477(2) 1_565
F1 Pb1 2.3327(3) 16_556
F1 K1 3.05996(12) 1_565
F1 K1 3.05996(11) 1_455
O1 C1 1.277(3) .
O1 Pb1 2.6829(6) 1_545
C1 O1 1.277(3) 3
C1 O1 1.277(3) 2
