#------------------------------------------------------------------------------
#$Date: 2019-11-23 02:32:22 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231892 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/66/4346637.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_4346637
loop_
_publ_author_name
'Lin, Yuan'
'Hu, Chun-Li'
'Mao, Jiang-Gao'
_publ_section_title
;
 K2Pb3(CO3)3F2 and KCdCO3F: Novel Fluoride Carbonates with Layered and 3D
 Framework Structures.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10407
_journal_page_last               10414
_journal_paper_doi               10.1021/acs.inorgchem.5b01848
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C3 F2 K2 O9 Pb3'
_chemical_formula_weight         917.80
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_cell_setting           hexagonal
_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
_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                   5.2989(3)
_cell_length_b                   5.2989(3)
_cell_length_c                   23.2326(18)
_cell_measurement_reflns_used    2300
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6370
_cell_measurement_theta_min      2.6248
_cell_volume                     564.94(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            4271
_diffrn_reflns_theta_full        26.69
_diffrn_reflns_theta_max         26.69
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    45.396
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51307
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    5.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocklike
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.0777
_exptl_crystal_size_mid          0.0632
_exptl_crystal_size_min          0.0469
_refine_diff_density_max         1.946
_refine_diff_density_min         -1.603
_refine_diff_density_rms         0.227
_refine_ls_extinction_coef       0.0072(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     28
_refine_ls_number_reflns         279
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0219
_refine_ls_R_factor_gt           0.0216
_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)+(0.0351P)²+5.0621P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0603
_reflns_number_gt                276
_reflns_number_total             279
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01848_si_002.cif
_cod_data_source_block           K2Pb3(CO3)3F2
_cod_original_sg_symbol_H-M      P63/mmc
_cod_database_code               4346637
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, x-y, z'
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 0.15307(12) 0.0156(9) Uani 1 6 d S
Pb1 Pb 0.3333 0.6667 0.2500 0.0113(3) Uani 1 12 d S
Pb2 Pb 0.3333 0.6667 0.04840(2) 0.0141(3) Uani 1 6 d S
F1 F 0.3333 0.6667 0.1452(3) 0.031(3) Uani 1 6 d S
O1 O -0.1400(6) 0.1400(6) 0.0648(3) 0.0188(12) Uani 1 2 d S
O2 O -0.1389(8) 0.1389(8) 0.2500 0.0212(19) Uani 1 4 d S
C1 C 0.0000 0.0000 0.0661(6) 0.012(2) Uani 1 6 d S
C2 C 0.0000 0.0000 0.2500 0.016(4) Uani 1 12 d S
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'
F F 0.0171 0.0103 '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'
Pb Pb -3.3944 10.1111 '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 69.0(2) 5 1_655
O1 K1 O1 69.0(2) 5 3_665
O1 K1 O1 69.0(2) 1_655 3_665
O1 K1 O2 142.73(8) 5 1_655
O1 K1 O2 100.73(19) 1_655 1_655
O1 K1 O2 142.73(8) 3_665 1_655
O1 K1 O2 142.73(8) 5 3_665
O1 K1 O2 142.73(8) 1_655 3_665
O1 K1 O2 100.7(2) 3_665 3_665
O2 K1 O2 65.1(2) 1_655 3_665
O1 K1 O2 100.7(2) 5 14_556
O1 K1 O2 142.73(8) 1_655 14_556
O1 K1 O2 142.73(8) 3_665 14_556
O2 K1 O2 65.1(2) 1_655 14_556
O2 K1 O2 65.1(2) 3_665 14_556
O1 K1 F1 68.16(13) 5 1_545
O1 K1 F1 68.16(13) 1_655 1_545
O1 K1 F1 127.4(2) 3_665 1_545
O2 K1 F1 74.75(13) 1_655 1_545
O2 K1 F1 131.8(2) 3_665 1_545
O2 K1 F1 74.75(13) 14_556 1_545
O1 K1 F1 127.4(2) 5 1_655
O1 K1 F1 68.16(13) 1_655 1_655
O1 K1 F1 68.16(13) 3_665 1_655
O2 K1 F1 74.75(13) 1_655 1_655
O2 K1 F1 74.75(13) 3_665 1_655
O2 K1 F1 131.8(2) 14_556 1_655
F1 K1 F1 119.64(3) 1_545 1_655
O1 K1 F1 68.16(13) 5 .
O1 K1 F1 127.4(2) 1_655 .
O1 K1 F1 68.16(13) 3_665 .
O2 K1 F1 131.8(2) 1_655 .
O2 K1 F1 74.75(13) 3_665 .
O2 K1 F1 74.75(13) 14_556 .
F1 K1 F1 119.64(3) 1_545 .
F1 K1 F1 119.64(3) 1_655 .
O1 K1 Pb1 167.23(14) 5 1_655
O1 K1 Pb1 100.64(9) 1_655 1_655
O1 K1 Pb1 100.64(9) 3_665 1_655
O2 K1 Pb1 44.38(3) 1_655 1_655
O2 K1 Pb1 44.38(3) 3_665 1_655
O2 K1 Pb1 92.04(14) 14_556 1_655
F1 K1 Pb1 115.94(10) 1_545 1_655
F1 K1 Pb1 39.79(14) 1_655 1_655
F1 K1 Pb1 115.94(10) . 1_655
O1 K1 Pb1 100.64(9) 5 1_545
O1 K1 Pb1 100.64(9) 1_655 1_545
O1 K1 Pb1 167.23(14) 3_665 1_545
O2 K1 Pb1 44.38(3) 1_655 1_545
O2 K1 Pb1 92.04(14) 3_665 1_545
O2 K1 Pb1 44.38(3) 14_556 1_545
F1 K1 Pb1 39.79(14) 1_545 1_545
F1 K1 Pb1 115.94(10) 1_655 1_545
F1 K1 Pb1 115.94(10) . 1_545
Pb1 K1 Pb1 88.45(5) 1_655 1_545
O1 K1 Pb1 100.64(9) 5 .
O1 K1 Pb1 167.23(14) 1_655 .
O1 K1 Pb1 100.64(9) 3_665 .
O2 K1 Pb1 92.04(14) 1_655 .
O2 K1 Pb1 44.38(3) 3_665 .
O2 K1 Pb1 44.38(3) 14_556 .
F1 K1 Pb1 115.94(10) 1_545 .
F1 K1 Pb1 115.94(10) 1_655 .
F1 K1 Pb1 39.79(14) . .
Pb1 K1 Pb1 88.45(5) 1_655 .
Pb1 K1 Pb1 88.45(5) 1_545 .
F1 Pb1 F1 180.000(1) . 14_566
F1 Pb1 O2 90.000(2) . 3_565
F1 Pb1 O2 90.000(2) 14_566 3_565
F1 Pb1 O2 90.000(1) . 14_566
F1 Pb1 O2 90.000(1) 14_566 14_566
O2 Pb1 O2 49.0(3) 3_565 14_566
F1 Pb1 O2 90.0 . .
F1 Pb1 O2 90.0 14_566 .
O2 Pb1 O2 71.0(3) 3_565 .
O2 Pb1 O2 120.000(1) 14_566 .
F1 Pb1 O2 90.0 . 1_665
F1 Pb1 O2 90.0 14_566 1_665
O2 Pb1 O2 120.000(1) 3_565 1_665
O2 Pb1 O2 71.0(3) 14_566 1_665
O2 Pb1 O2 169.0(3) . 1_665
F1 Pb1 O2 90.000(2) . 3_665
F1 Pb1 O2 90.000(2) 14_566 3_665
O2 Pb1 O2 169.0(3) 3_565 3_665
O2 Pb1 O2 120.000(1) 14_566 3_665
O2 Pb1 O2 120.0 . 3_665
O2 Pb1 O2 49.0(3) 1_665 3_665
F1 Pb1 O2 90.000(1) . 14_556
F1 Pb1 O2 90.000(2) 14_566 14_556
O2 Pb1 O2 120.000(1) 3_565 14_556
O2 Pb1 O2 169.0(3) 14_566 14_556
O2 Pb1 O2 49.0(3) . 14_556
O2 Pb1 O2 120.0 1_665 14_556
O2 Pb1 O2 71.0(3) 3_665 14_556
F1 Pb1 K1 126.36(4) . 14_676
F1 Pb1 K1 53.64(3) 14_566 14_676
O2 Pb1 K1 85.58(14) 3_565 14_676
O2 Pb1 K1 49.03(11) 14_566 14_676
O2 Pb1 K1 137.12(9) . 14_676
O2 Pb1 K1 49.03(11) 1_665 14_676
O2 Pb1 K1 85.58(13) 3_665 14_676
O2 Pb1 K1 137.12(9) 14_556 14_676
F1 Pb1 K1 53.64(3) . 1_455
F1 Pb1 K1 126.36(4) 14_566 1_455
O2 Pb1 K1 49.03(11) 3_565 1_455
O2 Pb1 K1 85.58(14) 14_566 1_455
O2 Pb1 K1 49.03(11) . 1_455
O2 Pb1 K1 137.12(9) 1_665 1_455
O2 Pb1 K1 137.12(9) 3_665 1_455
O2 Pb1 K1 85.58(13) 14_556 1_455
K1 Pb1 K1 132.51(2) 14_676 1_455
F1 Pb1 K1 53.64(3) . 1_565
F1 Pb1 K1 126.36(4) 14_566 1_565
O2 Pb1 K1 85.58(14) 3_565 1_565
O2 Pb1 K1 49.03(11) 14_566 1_565
O2 Pb1 K1 137.12(9) . 1_565
O2 Pb1 K1 49.03(10) 1_665 1_565
O2 Pb1 K1 85.58(13) 3_665 1_565
O2 Pb1 K1 137.12(9) 14_556 1_565
K1 Pb1 K1 72.71(7) 14_676 1_565
K1 Pb1 K1 88.45(5) 1_455 1_565
F1 Pb1 K1 126.36(3) . 14_666
F1 Pb1 K1 53.64(3) 14_566 14_666
O2 Pb1 K1 137.12(9) 3_565 14_666
O2 Pb1 K1 137.12(9) 14_566 14_666
O2 Pb1 K1 85.58(13) . 14_666
O2 Pb1 K1 85.58(13) 1_665 14_666
O2 Pb1 K1 49.03(11) 3_665 14_666
O2 Pb1 K1 49.03(11) 14_556 14_666
K1 Pb1 K1 88.45(5) 14_676 14_666
K1 Pb1 K1 132.51(2) 1_455 14_666
K1 Pb1 K1 132.51(2) 1_565 14_666
F1 Pb2 O1 81.83(13) . 3_565
F1 Pb2 O1 81.83(13) . 5_565
O1 Pb2 O1 48.9(2) 3_565 5_565
F1 Pb2 O1 81.83(13) . 1_665
O1 Pb2 O1 118.02(6) 3_565 1_665
O1 Pb2 O1 69.7(2) 5_565 1_665
F1 Pb2 O1 81.83(13) . .
O1 Pb2 O1 69.7(2) 3_565 .
O1 Pb2 O1 118.02(6) 5_565 .
O1 Pb2 O1 160.6(3) 1_665 .
F1 Pb2 O1 81.83(13) . 5
O1 Pb2 O1 118.02(6) 3_565 5
O1 Pb2 O1 160.6(3) 5_565 5
O1 Pb2 O1 118.02(6) 1_665 5
O1 Pb2 O1 48.9(2) . 5
F1 Pb2 O1 81.83(13) . 3_665
O1 Pb2 O1 160.6(3) 3_565 3_665
O1 Pb2 O1 118.02(6) 5_565 3_665
O1 Pb2 O1 48.9(2) 1_665 3_665
O1 Pb2 O1 118.02(6) . 3_665
O1 Pb2 O1 69.7(2) 5 3_665
F1 Pb2 K1 51.52(4) . 1_565
O1 Pb2 K1 80.81(12) 3_565 1_565
O1 Pb2 K1 43.86(12) 5_565 1_565
O1 Pb2 K1 43.86(12) 1_665 1_565
O1 Pb2 K1 127.99(13) . 1_565
O1 Pb2 K1 127.99(13) 5 1_565
O1 Pb2 K1 80.81(12) 3_665 1_565
F1 Pb2 K1 51.52(4) . 1_455
O1 Pb2 K1 43.86(12) 3_565 1_455
O1 Pb2 K1 80.81(12) 5_565 1_455
O1 Pb2 K1 127.99(13) 1_665 1_455
O1 Pb2 K1 43.86(12) . 1_455
O1 Pb2 K1 80.81(12) 5 1_455
O1 Pb2 K1 127.99(13) 3_665 1_455
K1 Pb2 K1 85.37(5) 1_565 1_455
F1 Pb2 K1 51.52(4) . .
O1 Pb2 K1 127.99(13) 3_565 .
O1 Pb2 K1 127.99(13) 5_565 .
O1 Pb2 K1 80.81(12) 1_665 .
O1 Pb2 K1 80.81(12) . .
O1 Pb2 K1 43.86(12) 5 .
O1 Pb2 K1 43.86(12) 3_665 .
K1 Pb2 K1 85.37(5) 1_565 .
K1 Pb2 K1 85.37(5) 1_455 .
Pb2 F1 Pb1 180.0 . .
Pb2 F1 K1 93.44(15) . 1_565
Pb1 F1 K1 86.56(15) . 1_565
Pb2 F1 K1 93.44(15) . 1_455
Pb1 F1 K1 86.56(15) . 1_455
K1 F1 K1 119.64(3) 1_565 1_455
Pb2 F1 K1 93.44(15) . .
Pb1 F1 K1 86.56(15) . .
K1 F1 K1 119.64(3) 1_565 .
K1 F1 K1 119.64(3) 1_455 .
C1 O1 Pb2 95.40(14) . 1_445
C1 O1 Pb2 95.40(14) . .
Pb2 O1 Pb2 160.6(3) 1_445 .
C1 O1 K1 129.6(7) . 1_455
Pb2 O1 K1 92.74(12) 1_445 1_455
Pb2 O1 K1 92.74(12) . 1_455
C2 O2 Pb1 95.50(17) . 1_445
C2 O2 Pb1 95.50(17) . .
Pb1 O2 Pb1 169.0(3) 1_445 .
C2 O2 K1 128.40(13) . 1_455
Pb1 O2 K1 86.59(11) 1_445 1_455
Pb1 O2 K1 86.59(11) . 1_455
C2 O2 K1 128.40(13) . 14_566
Pb1 O2 K1 86.59(11) 1_445 14_566
Pb1 O2 K1 86.59(11) . 14_566
K1 O2 K1 103.2(3) 1_455 14_566
O1 C1 O1 119.95(5) 3 5
O1 C1 O1 119.95(5) 3 .
O1 C1 O1 119.95(5) 5 .
O2 C2 O2 120.000(1) 3 14_556
O2 C2 O2 120.0 3 .
O2 C2 O2 120.000(1) 14_556 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O1 2.711(6) 5
K1 O1 2.711(6) 1_655
K1 O1 2.711(6) 3_665
K1 O2 2.873(5) 1_655
K1 O2 2.873(5) 3_665
K1 O2 2.873(5) 14_556
K1 F1 3.0648(5) 1_545
K1 F1 3.0648(5) 1_655
K1 F1 3.0648(5) .
K1 Pb1 3.7987(17) 1_655
K1 Pb1 3.7987(17) 1_545
K1 Pb1 3.7987(17) .
Pb1 F1 2.436(8) .
Pb1 F1 2.436(8) 14_566
Pb1 O2 2.6617(8) 3_565
Pb1 O2 2.6617(8) 14_566
Pb1 O2 2.6617(8) .
Pb1 O2 2.6617(8) 1_665
Pb1 O2 2.6617(7) 3_665
Pb1 O2 2.6617(7) 14_556
Pb1 K1 3.7987(17) 14_676
Pb1 K1 3.7987(17) 1_455
Pb1 K1 3.7987(17) 1_565
Pb1 K1 3.7987(17) 14_666
Pb2 F1 2.248(8) .
Pb2 O1 2.6880(10) 3_565
Pb2 O1 2.6880(10) 5_565
Pb2 O1 2.6880(10) 1_665
Pb2 O1 2.6880(10) .
Pb2 O1 2.6880(10) 5
Pb2 O1 2.6880(10) 3_665
Pb2 K1 3.9081(19) 1_565
Pb2 K1 3.9081(19) 1_455
F1 K1 3.0648(5) 1_565
F1 K1 3.0648(5) 1_455
O1 C1 1.285(5) .
O1 Pb2 2.6880(10) 1_445
O1 K1 2.711(6) 1_455
O2 C2 1.275(8) .
O2 Pb1 2.6617(8) 1_445
O2 K1 2.873(5) 1_455
O2 K1 2.873(5) 14_566
C1 O1 1.285(5) 3
C1 O1 1.285(5) 5
C2 O2 1.275(8) 3
C2 O2 1.275(8) 14_556
