#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:03:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179465 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/62/4336253.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_4336253
loop_
_publ_author_name
'Lingyun Dong'
'Shilie Pan'
'Ying Wang'
'Hongwei Yu'
'Xiaoyu Dong'
'Shujuan Han'
'Min Zhang'
_publ_section_title
;
 Special ∞1[OPb2] Chains and ∞1[O2Pb3] Ribbons Based on OPb4
 Anion-Centered Tetrahedra in Pb2(O4Pb8)(BO3)3Br3 and Pb2(O8Pb12)(BO3)2Br6
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11377
_journal_page_last               11384
_journal_paper_doi               10.1021/ic401655h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'B3 Br3 O13 Pb10'
_chemical_formula_weight         2552.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 114.337(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.482(9)
_cell_length_b                   8.947(5)
_cell_length_c                   16.645(9)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.69
_cell_volume                     2236(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0577
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6670
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    80.384
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6235
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   Face-indexed
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    7.579
_exptl_crystal_description       block
_exptl_crystal_F_000             4176
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.066
_refine_diff_density_max         2.862
_refine_diff_density_min         -2.417
_refine_diff_density_rms         0.578
_refine_ls_extinction_coef       0.000098(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2544
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0395
_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)+(0.0218P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                1886
_reflns_number_total             2544
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401655h_si_003_1.cif
_cod_data_source_block           Pb2(O4Pb8)(BO3)3Br3
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4336253
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Pb1 Pb 0.27873(4) 1.04499(7) 0.39796(4) 0.01814(18) Uani 1 1 d .
Pb2 Pb 0.60739(4) 0.53838(7) 0.50069(5) 0.01813(18) Uani 1 1 d .
Pb3 Pb 0.47702(4) 0.84694(7) 0.56362(4) 0.01733(18) Uani 1 1 d .
Pb4 Pb 0.40792(4) 0.75591(7) 0.33379(4) 0.01767(18) Uani 1 1 d .
Pb5 Pb 0.15647(5) 0.67843(8) 0.29425(5) 0.0261(2) Uani 1 1 d .
B1 B 0.6959(13) 0.578(2) 0.6902(13) 0.020(4) Uani 1 1 d U
B2 B 0.2500 0.7500 0.5000 0.022(6) Uani 1 2 d SU
O1 O 0.4131(8) 0.9577(12) 0.4264(8) 0.022(3) Uani 1 1 d .
O2 O 0.4731(8) 0.6489(11) 0.4676(8) 0.021(3) Uani 1 1 d .
O3 O 0.6429(7) 0.6738(12) 0.6267(8) 0.019(3) Uani 1 1 d .
O4 O 0.2376(7) 0.8722(12) 0.2773(7) 0.022(3) Uani 1 1 d .
O5 O 0.2930(7) 0.5664(12) 0.3324(9) 0.026(3) Uani 1 1 d .
O6 O 0.1638(14) 0.724(2) 0.4224(15) 0.018(5) Uani 0.50 1 d PU
O7 O 0.3122(16) 0.843(2) 0.4896(16) 0.022(6) Uani 0.50 1 d PU
O8 O 0.2386(16) 0.816(2) 0.4244(17) 0.025(6) Uani 0.50 1 d P
Br1 Br 0.61742(14) 0.8534(2) 0.39229(14) 0.0325(5) Uani 1 1 d .
Br2 Br 0.5000 0.4573(3) 0.2500 0.0483(9) Uani 1 2 d S
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'
Br Br -0.2901 2.4595 '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 Pb1 O8 89.2(7) . .
O1 Pb1 O7 68.4(7) . .
O8 Pb1 O7 32.7(8) . .
O1 Pb1 O4 82.2(4) . .
O8 Pb1 O4 64.7(7) . .
O7 Pb1 O4 87.6(6) . .
O2 Pb2 O3 81.2(4) . .
O2 Pb2 O2 77.3(4) . 5_666
O3 Pb2 O2 97.3(4) . 5_666
O2 Pb2 O5 120.7(4) . 5_666
O3 Pb2 O5 55.3(4) . 5_666
O2 Pb2 O5 71.6(4) 5_666 5_666
O2 Pb2 Pb2 39.2(3) . 5_666
O3 Pb2 Pb2 89.2(3) . 5_666
O2 Pb2 Pb2 38.1(3) 5_666 5_666
O5 Pb2 Pb2 96.8(3) 5_666 5_666
O1 Pb3 O2 77.2(4) . .
O1 Pb3 O1 77.6(4) . 5_676
O2 Pb3 O1 112.9(4) . 5_676
O1 Pb3 O7 63.5(6) . .
O2 Pb3 O7 86.3(6) . .
O1 Pb3 O7 131.7(6) 5_676 .
O1 Pb3 O6 97.9(6) . 7_566
O2 Pb3 O6 96.0(6) . 7_566
O1 Pb3 O6 148.5(6) 5_676 7_566
O7 Pb3 O6 34.5(7) . 7_566
O2 Pb4 O1 78.7(4) . .
O2 Pb4 O5 77.0(4) . .
O1 Pb4 O5 110.1(4) . .
O6 Pb5 O4 100.7(7) . .
O6 Pb5 O5 99.3(7) . .
O4 Pb5 O5 79.0(4) . .
O6 Pb5 O8 37.7(8) . .
O4 Pb5 O8 64.8(7) . .
O5 Pb5 O8 81.3(7) . .
O3 B1 O5 119.5(16) . 5_666
O3 B1 O4 119.5(16) . 8_566
O5 B1 O4 121.0(16) 5_666 8_566
O8 B2 O8 180.000(5) 7_566 .
O8 B2 O7 124.2(13) 7_566 .
O8 B2 O7 55.8(13) . .
O8 B2 O7 55.8(13) 7_566 7_566
O8 B2 O7 124.2(13) . 7_566
O7 B2 O7 180(2) . 7_566
O8 B2 O6 62.5(13) 7_566 7_566
O8 B2 O6 117.5(13) . 7_566
O7 B2 O6 61.7(13) . 7_566
O7 B2 O6 118.3(13) 7_566 7_566
O8 B2 O6 117.5(13) 7_566 .
O8 B2 O6 62.5(13) . .
O7 B2 O6 118.3(13) . .
O7 B2 O6 61.7(13) 7_566 .
O6 B2 O6 180.000(5) 7_566 .
Pb1 O1 Pb3 111.9(5) . .
Pb1 O1 Pb4 111.6(5) . .
Pb3 O1 Pb4 101.4(4) . .
Pb1 O1 Pb3 114.0(4) . 5_676
Pb3 O1 Pb3 102.4(4) . 5_676
Pb4 O1 Pb3 114.5(5) . 5_676
Pb4 O2 Pb2 116.4(5) . .
Pb4 O2 Pb2 116.5(5) . 5_666
Pb2 O2 Pb2 102.7(4) . 5_666
Pb4 O2 Pb3 102.6(4) . .
Pb2 O2 Pb3 114.1(5) . .
Pb2 O2 Pb3 104.2(5) 5_666 .
B1 O3 Pb2 102.8(10) . .
B1 O4 Pb5 107.8(10) 8_465 .
B1 O4 Pb1 120.9(11) 8_465 .
Pb5 O4 Pb1 111.4(5) . .
B1 O5 Pb5 123.9(10) 5_666 .
B1 O5 Pb4 116.5(11) 5_666 .
Pb5 O5 Pb4 110.7(4) . .
B1 O5 Pb2 82.2(10) 5_666 5_666
Pb5 O5 Pb2 122.5(6) . 5_666
Pb4 O5 Pb2 94.9(3) . 5_666
O8 O6 O7 109.0(18) . 7_566
O8 O6 B2 53.4(12) . .
O7 O6 B2 55.7(12) 7_566 .
O8 O6 Pb5 80.2(14) . .
O7 O6 Pb5 142.9(16) 7_566 .
B2 O6 Pb5 122.5(14) . .
O8 O6 Pb3 159.7(16) . 7_566
O7 O6 Pb3 71.6(13) 7_566 7_566
B2 O6 Pb3 123.1(13) . 7_566
Pb5 O6 Pb3 111.9(9) . 7_566
O8 O7 B2 59.8(15) . .
O8 O7 O6 122(2) . 7_566
B2 O7 O6 62.6(13) . 7_566
O8 O7 Pb1 72.5(15) . .
B2 O7 Pb1 124.9(14) . .
O6 O7 Pb1 151.3(17) 7_566 .
O8 O7 Pb3 153(2) . .
B2 O7 Pb3 131.3(14) . .
O6 O7 Pb3 73.8(13) 7_566 .
Pb1 O7 Pb3 103.7(9) . .
O7 O8 B2 64.3(16) . .
O7 O8 O6 128(2) . .
B2 O8 O6 64.1(14) . .
O7 O8 Pb1 74.8(15) . .
B2 O8 Pb1 130.6(14) . .
O6 O8 Pb1 144.7(17) . .
O7 O8 Pb5 150(2) . .
B2 O8 Pb5 115.9(13) . .
O6 O8 Pb5 62.0(12) . .
Pb1 O8 Pb5 113.4(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 O1 2.208(11) .
Pb1 O8 2.25(2) .
Pb1 O7 2.28(2) .
Pb1 O4 2.401(11) .
Pb2 O2 2.275(11) .
Pb2 O3 2.280(12) .
Pb2 O2 2.329(11) 5_666
Pb2 O5 2.745(12) 5_666
Pb3 O1 2.308(12) .
Pb3 O2 2.369(11) .
Pb3 O1 2.473(12) 5_676
Pb3 O7 2.48(2) .
Pb3 O6 2.51(2) 7_566
Pb4 O2 2.249(12) .
Pb4 O1 2.353(11) .
Pb4 O5 2.535(11) .
Pb5 O6 2.13(2) .
Pb5 O4 2.277(12) .
Pb5 O5 2.300(11) .
Pb5 O8 2.37(2) .
B1 O3 1.36(2) .
B1 O5 1.38(2) 5_666
B1 O4 1.40(2) 8_566
B2 O8 1.33(3) 7_566
B2 O8 1.33(3) .
B2 O7 1.39(2) .
B2 O7 1.39(2) 7_566
B2 O6 1.49(2) 7_566
B2 O6 1.49(2) .
O1 Pb3 2.473(12) 5_676
O2 Pb2 2.329(11) 5_666
O4 B1 1.40(2) 8_465
O5 B1 1.38(2) 5_666
O5 Pb2 2.745(12) 5_666
O6 O8 1.47(3) .
O6 O7 1.48(3) 7_566
O6 Pb3 2.51(2) 7_566
O7 O8 1.27(3) .
O7 O6 1.48(3) 7_566
