#------------------------------------------------------------------------------
#$Date: 2021-03-19 10:55:25 +0200 (Fri, 19 Mar 2021) $
#$Revision: 263170 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/11/1561146.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_1561146
loop_
_publ_author_name
'Ruan, Ting-Ting'
'Wang, Wen-Wen'
'Hu, Chun-Li'
'Xu, Xiang'
'Mao, Jiang-Gao'
_publ_section_title
;
 Pb4(BO3)2(SO4) and Pb2[(BO2)(OH)](SO4): New lead(II) borate-sulfate
 mixed-anion compounds with two types of 3D network structures
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              39
_journal_page_last               45
_journal_paper_doi               10.1016/j.jssc.2018.01.013
_journal_volume                  260
_journal_year                    2018
_chemical_formula_sum            'B2 O10 Pb4 S'
_chemical_formula_weight         1042.44
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 110.770(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9363(4)
_cell_length_b                   15.8784(8)
_cell_length_c                   9.6053(5)
_cell_measurement_reflns_used    4303
_cell_measurement_temperature    294.1(3)
_cell_measurement_theta_max      29.8460
_cell_measurement_theta_min      4.0400
_cell_volume                     989.15(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.1(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7908
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.39
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    68.127
_exptl_absorpt_correction_T_max  0.066
_exptl_absorpt_correction_T_min  0.023
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    7.000
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       granular
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.975
_refine_diff_density_min         -1.444
_refine_diff_density_rms         0.319
_refine_ls_extinction_coef       0.00098(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0225
_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)+(0.0171P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0474
_refine_ls_wR_factor_ref         0.0487
_reflns_number_gt                2003
_reflns_number_total             2173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            JSSC-2018-260-39.cif
_cod_data_source_block           Pb4SB2O10
_cod_original_cell_volume        989.15(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1561146
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.50653(5) 0.322099(18) 0.92495(3) 0.01911(10) Uani 1 1 d . . .
Pb2 Pb 0.06214(5) 0.324445(19) 0.09466(3) 0.02296(10) Uani 1 1 d . . .
Pb3 Pb 0.15028(4) 0.571353(17) 0.29525(3) 0.01696(9) Uani 1 1 d . . .
Pb4 Pb 0.35528(4) 0.560258(17) 0.70360(3) 0.01701(9) Uani 1 1 d . . .
S1 S 0.2153(3) 0.36618(12) 0.4880(2) 0.0187(4) Uani 1 1 d . . .
B1 B 0.2370(12) 0.4961(6) 0.0011(8) 0.0133(17) Uani 1 1 d . . .
B2 B 0.7041(13) 0.2479(5) 1.2257(9) 0.0159(18) Uani 1 1 d . . .
O1 O 0.4147(8) 0.4014(4) 0.5034(7) 0.0354(15) Uani 1 1 d . . .
O2 O 0.0511(9) 0.4110(4) 0.3716(7) 0.0407(16) Uani 1 1 d . . .
O3 O 0.1823(10) 0.3690(5) 0.6310(7) 0.0473(18) Uani 1 1 d . . .
O4 O 0.2044(10) 0.2768(4) 0.4404(8) 0.0415(16) Uani 1 1 d . . .
O5 O 0.3209(8) 0.4934(3) 0.1562(6) 0.0217(12) Uani 1 1 d . . .
O6 O 0.1156(8) 0.4299(3) -0.0724(6) 0.0216(12) Uani 1 1 d . . .
O7 O 0.2691(9) 0.5648(3) -0.0754(6) 0.0227(12) Uani 1 1 d . . .
O8 O 0.7607(8) 0.2471(3) 1.1042(6) 0.0208(12) Uani 1 1 d . . .
O9 O 0.5576(8) 0.3027(3) 1.2388(6) 0.0222(12) Uani 1 1 d . . .
O10 O 0.7796(8) 0.1848(3) 1.3329(6) 0.0187(11) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
S S 0.1246 0.1234 '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
O8 Pb1 O10 75.72(17) . 4_565
O8 Pb1 O7 77.50(18) . 3_666
O10 Pb1 O7 80.25(17) 4_565 3_666
O8 Pb1 O4 93.55(19) . 4_566
O10 Pb1 O4 138.15(18) 4_565 4_566
O7 Pb1 O4 137.60(19) 3_666 4_566
O8 Pb1 Pb2 42.20(13) . 1_656
O10 Pb1 Pb2 45.58(13) 4_565 1_656
O7 Pb1 Pb2 51.72(13) 3_666 1_656
O4 Pb1 Pb2 135.65(15) 4_566 1_656
O6 Pb2 O8 134.34(18) . 1_454
O6 Pb2 O10 68.83(16) . 4_464
O8 Pb2 O10 69.25(16) 1_454 4_464
O6 Pb2 O4 82.70(18) . 4_565
O8 Pb2 O4 102.23(18) 1_454 4_565
O10 Pb2 O4 73.81(19) 4_464 4_565
O6 Pb2 Pb1 95.57(13) . 1_454
O8 Pb2 Pb1 39.21(12) 1_454 1_454
O10 Pb2 Pb1 40.67(11) 4_464 1_454
O4 Pb2 Pb1 107.18(15) 4_565 1_454
O6 Pb3 O10 76.19(18) 3_565 2_656
O6 Pb3 O5 82.41(18) 3_565 .
O10 Pb3 O5 82.47(18) 2_656 .
O6 Pb3 Pb4 151.84(13) 3_565 .
O10 Pb3 Pb4 121.83(12) 2_656 .
O5 Pb3 Pb4 119.08(12) . .
O9 Pb4 O5 95.21(19) 3_667 3_666
O9 Pb4 O7 83.34(17) 3_667 1_556
O5 Pb4 O7 89.50(18) 3_666 1_556
O9 Pb4 O2 93.76(19) 3_667 3_566
O5 Pb4 O2 156.96(18) 3_666 3_566
O7 Pb4 O2 70.5(2) 1_556 3_566
O9 Pb4 Pb3 100.54(14) 3_667 .
O5 Pb4 Pb3 124.28(12) 3_666 .
O7 Pb4 Pb3 145.00(14) 1_556 .
O2 Pb4 Pb3 74.51(14) 3_566 .
O1 S1 O2 110.2(4) . .
O1 S1 O3 110.5(4) . .
O2 S1 O3 111.2(4) . .
O1 S1 O4 110.1(4) . .
O2 S1 O4 106.7(4) . .
O3 S1 O4 108.0(4) . .
O6 B1 O7 121.1(6) . .
O6 B1 O5 118.2(7) . .
O7 B1 O5 120.6(7) . .
O8 B2 O9 122.1(7) . .
O8 B2 O10 118.7(6) . .
O9 B2 O10 118.8(7) . .
S1 O2 Pb4 138.1(4) . 3_566
S1 O4 Pb2 113.8(3) . 4_566
S1 O4 Pb1 128.7(4) . 4_565
Pb2 O4 Pb1 97.6(2) 4_566 4_565
B1 O5 Pb4 125.4(4) . 3_666
B1 O5 Pb3 118.3(4) . .
Pb4 O5 Pb3 115.3(2) 3_666 .
B1 O6 Pb3 129.3(5) . 3_565
B1 O6 Pb2 113.3(4) . .
Pb3 O6 Pb2 110.6(2) 3_565 .
B1 O7 Pb4 125.9(4) . 1_554
B1 O7 Pb1 116.7(4) . 3_666
Pb4 O7 Pb1 103.62(19) 1_554 3_666
B2 O8 Pb1 105.0(4) . .
B2 O8 Pb2 122.5(5) . 1_656
Pb1 O8 Pb2 98.58(18) . 1_656
B2 O9 Pb4 119.1(5) . 3_667
B2 O10 Pb3 105.0(4) . 2_646
B2 O10 Pb1 99.7(4) . 4_566
Pb3 O10 Pb1 120.5(2) 2_646 4_566
B2 O10 Pb2 135.5(5) . 4_667
Pb3 O10 Pb2 103.97(18) 2_646 4_667
Pb1 O10 Pb2 93.75(17) 4_566 4_667
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O8 2.310(5) .
Pb1 O10 2.360(5) 4_565
Pb1 O7 2.478(5) 3_666
Pb1 O4 2.665(6) 4_566
Pb1 Pb2 3.6132(5) 1_656
Pb2 O6 2.437(5) .
Pb2 O8 2.455(5) 1_454
Pb2 O10 2.586(5) 4_464
Pb2 O4 2.606(6) 4_565
Pb2 Pb1 3.6132(5) 1_454
Pb3 O6 2.277(5) 3_565
Pb3 O10 2.329(5) 2_656
Pb3 O5 2.416(5) .
Pb3 Pb4 3.6718(5) .
Pb4 O9 2.274(5) 3_667
Pb4 O5 2.332(5) 3_666
Pb4 O7 2.402(5) 1_556
Pb4 O2 2.689(6) 3_566
S1 O1 1.450(6) .
S1 O2 1.466(6) .
S1 O3 1.471(6) .
S1 O4 1.484(6) .
B1 O6 1.375(10) .
B1 O7 1.377(10) .
B1 O5 1.394(9) .
B2 O8 1.357(9) .
B2 O9 1.377(9) .
B2 O10 1.398(9) .
O2 Pb4 2.689(6) 3_566
O4 Pb2 2.606(6) 4_566
O4 Pb1 2.665(6) 4_565
O5 Pb4 2.332(5) 3_666
O6 Pb3 2.277(5) 3_565
O7 Pb4 2.402(5) 1_554
O7 Pb1 2.478(5) 3_666
O8 Pb2 2.455(5) 1_656
O9 Pb4 2.274(5) 3_667
O10 Pb3 2.329(5) 2_646
O10 Pb1 2.360(5) 4_566
O10 Pb2 2.586(5) 4_667
