#------------------------------------------------------------------------------
#$Date: 2020-08-06 17:02:27 +0300 (Thu, 06 Aug 2020) $
#$Revision: 254986 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/46/7704649.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_7704649
loop_
_publ_author_name
'Li, Kuan'
'Yalikun, Alimujiang'
'Su, Zhi'
_publ_section_title
;
 [O₂Pb₃]₂(BO₃)I: a new lead
 borate iodide with [O₂Pb₃] double chains.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8985
_journal_page_last               8990
_journal_paper_doi               10.1039/d0dt01722a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_sum            'B I O7 Pb6'
_chemical_formula_weight         1492.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n :2'
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2020-03-28 deposited with the CCDC.	2020-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.780(12)
_cell_length_b                   9.72(2)
_cell_length_c                   10.63(2)
_cell_measurement_reflns_used    434
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.84
_cell_volume                     597(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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1764
_diffrn_reflns_av_unetI/netI     0.1214
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3651
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.684
_diffrn_reflns_theta_min         1.916
_exptl_absorpt_coefficient_mu    86.859
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5243
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    8.302
_exptl_crystal_density_meas      8.302
_exptl_crystal_description       flake
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.110
_refine_diff_density_max         5.772
_refine_diff_density_min         -4.881
_refine_diff_density_rms         1.013
_refine_ls_extinction_coef       0.00108(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[σ²(Fo²)+(0.0476P)²] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1192
_refine_ls_wR_factor_ref         0.1322
_reflns_Friedel_coverage         0.000
_reflns_number_gt                548
_reflns_number_total             808
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0dt01722a2.cif
_cod_data_source_block           Yyy
_cod_depositor_comments          'Adding full bibliography for 7704649.cif.'
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               7704649
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.024
_shelx_estimated_absorpt_t_max   0.038
_shelxl_version_number           2013-2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.7500 0.52056(12) 0.38227(13) 0.0196(4) Uani 1 2 d S T P . .
Pb2 Pb 0.2500 0.45489(11) 0.16510(15) 0.0193(4) Uani 1 2 d S T P . .
Pb3 Pb 0.7500 0.7500 0.12874(19) 0.0178(5) Uani 1 4 d S T P . .
Pb4 Pb 0.2500 0.7500 0.3582(2) 0.0173(5) Uani 1 4 d S T P . .
B1 B 0.2500 0.2500 0.407(7) 0.032(16) Uani 1 4 d S T P . .
I1 I 0.7500 0.2500 0.1166(4) 0.0401(12) Uani 1 4 d S T P . .
O1 O 0.001(2) 0.6068(12) 0.2459(14) 0.013(3) Uani 1 1 d . . . . .
O2 O 0.2500 0.2500 0.547(3) 0.025(8) Uani 1 4 d S T P . .
O3 O 0.2500 0.377(2) 0.358(2) 0.025(6) Uani 1 2 d S T P . .
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'
I I -0.4742 1.8119 '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'
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
_geom_angle_publ_flag
O1 Pb1 O1 81.8(7) 7_655 1_655 ?
O1 Pb1 O2 81.5(7) 7_655 5_666 ?
O1 Pb1 O2 81.5(7) 1_655 5_666 ?
O1 Pb1 Pb3 41.8(4) 7_655 . ?
O1 Pb1 Pb3 41.8(4) 1_655 . ?
O2 Pb1 Pb3 69.1(8) 5_666 . ?
O1 Pb1 Pb4 37.5(4) 7_655 . ?
O1 Pb1 Pb4 104.0(3) 1_655 . ?
O2 Pb1 Pb4 56.3(3) 5_666 . ?
Pb3 Pb1 Pb4 63.74(8) . . ?
O1 Pb1 Pb4 104.0(3) 7_655 1_655 ?
O1 Pb1 Pb4 37.5(4) 1_655 1_655 ?
O2 Pb1 Pb4 56.3(3) 5_666 1_655 ?
Pb3 Pb1 Pb4 63.74(8) . 1_655 ?
Pb4 Pb1 Pb4 104.32(16) . 1_655 ?
O3 Pb2 O1 82.5(6) . 7_655 ?
O3 Pb2 O1 82.5(6) . . ?
O1 Pb2 O1 80.2(7) 7_655 . ?
O3 Pb2 Pb4 74.8(6) . . ?
O1 Pb2 Pb4 40.4(4) 7_655 . ?
O1 Pb2 Pb4 40.4(4) . . ?
O1 Pb3 O1 116.5(7) 8_675 7_655 ?
O1 Pb3 O1 75.7(7) 8_675 2_565 ?
O1 Pb3 O1 72.1(6) 7_655 2_565 ?
O1 Pb3 O1 72.1(6) 8_675 1_655 ?
O1 Pb3 O1 75.7(7) 7_655 1_655 ?
O1 Pb3 O1 116.5(7) 2_565 1_655 ?
O1 Pb3 Pb1 88.3(3) 8_675 . ?
O1 Pb3 Pb1 38.7(4) 7_655 . ?
O1 Pb3 Pb1 88.3(3) 2_565 . ?
O1 Pb3 Pb1 38.7(4) 1_655 . ?
O1 Pb3 Pb1 38.7(4) 8_675 2_665 ?
O1 Pb3 Pb1 88.3(3) 7_655 2_665 ?
O1 Pb3 Pb1 38.7(4) 2_565 2_665 ?
O1 Pb3 Pb1 88.3(3) 1_655 2_665 ?
Pb1 Pb3 Pb1 79.22(17) . 2_665 ?
O1 Pb4 O1 76.2(7) 2_565 8_575 ?
O1 Pb4 O1 73.4(6) 2_565 7_655 ?
O1 Pb4 O1 118.4(7) 8_575 7_655 ?
O1 Pb4 O1 118.4(7) 2_565 . ?
O1 Pb4 O1 73.4(6) 8_575 . ?
O1 Pb4 O1 76.2(7) 7_655 . ?
O1 Pb4 Pb2 38.4(3) 2_565 2_565 ?
O1 Pb4 Pb2 38.4(3) 8_575 2_565 ?
O1 Pb4 Pb2 100.8(4) 7_655 2_565 ?
O1 Pb4 Pb2 100.8(4) . 2_565 ?
O1 Pb4 Pb2 100.8(4) 2_565 . ?
O1 Pb4 Pb2 100.8(4) 8_575 . ?
O1 Pb4 Pb2 38.4(3) 7_655 . ?
O1 Pb4 Pb2 38.4(3) . . ?
Pb2 Pb4 Pb2 108.83(17) 2_565 . ?
O1 Pb4 Pb1 85.0(3) 2_565 . ?
O1 Pb4 Pb1 152.5(4) 8_575 . ?
O1 Pb4 Pb1 35.4(4) 7_655 . ?
O1 Pb4 Pb1 99.2(3) . . ?
Pb2 Pb4 Pb1 122.43(9) 2_565 . ?
Pb2 Pb4 Pb1 62.94(9) . . ?
O1 Pb4 Pb1 35.4(4) 2_565 2_665 ?
O1 Pb4 Pb1 99.2(3) 8_575 2_665 ?
O1 Pb4 Pb1 85.0(3) 7_655 2_665 ?
O1 Pb4 Pb1 152.5(4) . 2_665 ?
Pb2 Pb4 Pb1 62.94(9) 2_565 2_665 ?
Pb2 Pb4 Pb1 122.43(9) . 2_665 ?
Pb1 Pb4 Pb1 75.10(16) . 2_665 ?
O1 Pb4 Pb1 152.5(4) 2_565 1_455 ?
O1 Pb4 Pb1 85.0(3) 8_575 1_455 ?
O1 Pb4 Pb1 99.2(3) 7_655 1_455 ?
O1 Pb4 Pb1 35.4(4) . 1_455 ?
Pb2 Pb4 Pb1 122.43(9) 2_565 1_455 ?
Pb2 Pb4 Pb1 62.94(9) . 1_455 ?
Pb1 Pb4 Pb1 104.32(16) . 1_455 ?
Pb1 Pb4 Pb1 171.98(8) 2_665 1_455 ?
O1 Pb4 Pb1 99.2(3) 2_565 2_565 ?
O1 Pb4 Pb1 35.4(4) 8_575 2_565 ?
O1 Pb4 Pb1 152.5(4) 7_655 2_565 ?
O1 Pb4 Pb1 85.0(3) . 2_565 ?
Pb2 Pb4 Pb1 62.94(9) 2_565 2_565 ?
Pb2 Pb4 Pb1 122.43(9) . 2_565 ?
Pb1 Pb4 Pb1 171.98(8) . 2_565 ?
Pb1 Pb4 Pb1 104.32(16) 2_665 2_565 ?
Pb1 Pb4 Pb1 75.10(16) 1_455 2_565 ?
O3 B1 O3 134(6) 2 . ?
O3 B1 O2 113(3) 2 . ?
O3 B1 O2 113(3) . . ?
Pb1 O1 Pb2 115.1(5) 1_455 . ?
Pb1 O1 Pb4 107.1(6) 1_455 . ?
Pb2 O1 Pb4 101.2(6) . . ?
Pb1 O1 Pb3 99.5(5) 1_455 1_455 ?
Pb2 O1 Pb3 125.6(7) . 1_455 ?
Pb4 O1 Pb3 107.3(5) . 1_455 ?
B1 O2 Pb1 108.7(8) . 5_666 ?
B1 O2 Pb1 108.7(8) . 6_556 ?
Pb1 O2 Pb1 142.5(16) 5_666 6_556 ?
B1 O3 Pb2 133(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.216(15) 7_655 ?
Pb1 O1 2.216(15) 1_655 ?
Pb1 O2 2.355(12) 5_666 ?
Pb1 Pb3 3.498(5) . ?
Pb1 Pb4 3.659(6) . ?
Pb1 Pb4 3.659(6) 1_655 ?
Pb2 O3 2.19(3) . ?
Pb2 O1 2.233(13) 7_655 ?
Pb2 O1 2.233(13) . ?
Pb2 Pb4 3.527(6) . ?
Pb3 O1 2.365(14) 8_675 ?
Pb3 O1 2.365(14) 7_655 ?
Pb3 O1 2.365(14) 2_565 ?
Pb3 O1 2.365(14) 1_655 ?
Pb3 Pb1 3.498(5) 2_665 ?
Pb4 O1 2.331(14) 2_565 ?
Pb4 O1 2.331(14) 8_575 ?
Pb4 O1 2.331(14) 7_655 ?
Pb4 O1 2.331(14) . ?
Pb4 Pb2 3.527(6) 2_565 ?
Pb4 Pb1 3.659(6) 2_665 ?
Pb4 Pb1 3.659(6) 1_455 ?
Pb4 Pb1 3.659(6) 2_565 ?
B1 O3 1.33(3) 2 ?
B1 O3 1.33(3) . ?
B1 O2 1.48(7) . ?
O1 Pb1 2.216(15) 1_455 ?
O1 Pb3 2.365(14) 1_455 ?
O2 Pb1 2.355(12) 5_666 ?
O2 Pb1 2.355(12) 6_556 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 B1 O2 Pb1 180.000(5) 2 . . 5_666 ?
O3 B1 O2 Pb1 0.000(8) . . . 5_666 ?
O3 B1 O2 Pb1 0.000(5) 2 . . 6_556 ?
O3 B1 O2 Pb1 180.000(7) . . . 6_556 ?
O3 B1 O3 Pb2 0.000(10) 2 . . . ?
O2 B1 O3 Pb2 180.000(8) . . . . ?
