#------------------------------------------------------------------------------
#$Date: 2022-02-11 01:47:28 +0200 (Fri, 11 Feb 2022) $
#$Revision: 272904 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/94/7709454.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_7709454
loop_
_publ_author_name
'Bai, Shuo'
'Yang, Daqing'
'Zhang, Bingbing'
'Li, Ling'
'Wang, Ying'
_publ_section_title
;
 Two Lead Borate-nitrates with Anion-Centered [OPb4] Tetrahedra and Two
 Types of π-Conjugated Planar Units Showing Large Birefringence
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00183G
_journal_year                    2022
_chemical_formula_moiety         '0.5(B2 O14 Pb12), 2(N0.5 O1.5)'
_chemical_formula_sum            'B N O10 Pb6'
_chemical_formula_weight         1427.96
_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'
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-11 deposited with the CCDC.	2022-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.7481(5)
_cell_length_b                   9.4582(9)
_cell_length_c                   11.2770(12)
_cell_measurement_reflns_used    2775
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.81
_cell_volume                     613.09(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6656
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_min         2.811
_exptl_absorpt_coefficient_mu    82.125
_exptl_absorpt_correction_T_max  0.0206
_exptl_absorpt_correction_T_min  0.0040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1705 before and 0.0827 after correction. The Ratio of minimum to maximum transmission is 0.1942. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    7.735
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.077
_refine_diff_density_max         1.926
_refine_diff_density_min         -1.843
_refine_diff_density_rms         0.440
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0561P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                696
_reflns_number_total             823
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00183g2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               7709454
_shelx_shelxl_version_number     2018/3
_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_max   0.061
_shelx_estimated_absorpt_t_min   0.023
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, 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_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 0.750000 0.55607(7) 0.82033(7) 0.0357(2) Uani 1 2 d S T P . .
Pb2 Pb 0.250000 0.250000 0.86576(10) 0.0363(3) Uani 1 4 d S T P . .
Pb3 Pb 0.750000 0.250000 0.64357(10) 0.0347(3) Uani 1 4 d S T P . .
Pb4 Pb 0.250000 0.01269(8) 0.61924(6) 0.0359(2) Uani 1 2 d S T P . .
N1 N 0.250000 0.750000 0.914(3) 0.054(7) Uani 1 4 d S T P . .
B1 B 0.750000 0.750000 0.569(3) 0.039(7) Uani 1 4 d S T P . .
O1 O 0.250000 0.639(2) 0.963(2) 0.100(7) Uani 1 2 d S T P . .
O2 O 0.250000 0.750000 0.800(2) 0.080(9) Uani 1 4 d S T P . .
O3 O 1.0015(14) 0.3972(8) 0.7542(7) 0.0325(19) Uani 1 1 d . . . . .
O4 O 0.750000 0.6199(15) 0.6294(14) 0.053(4) Uani 1 2 d S T P . .
O5 O 0.250000 0.250000 0.5512(17) 0.037(4) Uani 1 4 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'
N N 0.0061 0.0033 '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
O3 Pb1 Pb1 132.7(2) . 2_665 ?
O3 Pb1 Pb1 132.7(2) 8_755 2_665 ?
O3 Pb1 O3 81.5(4) . 8_755 ?
O3 Pb1 O4 81.9(3) . . ?
O3 Pb1 O4 81.9(4) 8_755 . ?
O4 Pb1 Pb1 74.3(4) . 2_665 ?
Pb4 Pb2 Pb4 77.83(3) . 2 ?
O3 Pb2 Pb4 87.45(19) 8_755 . ?
O3 Pb2 Pb4 38.19(19) 1_455 2 ?
O3 Pb2 Pb4 38.19(19) 8_755 2 ?
O3 Pb2 Pb4 87.45(19) 1_455 . ?
O3 Pb2 Pb4 87.45(19) 2_655 2 ?
O3 Pb2 Pb4 38.19(19) 2_655 . ?
O3 Pb2 Pb4 38.19(19) 7_465 . ?
O3 Pb2 Pb4 87.45(19) 7_465 2 ?
O3 Pb2 O3 74.6(4) 7_465 2_655 ?
O3 Pb2 O3 74.6(4) 8_755 1_455 ?
O3 Pb2 O3 115.5(4) 7_465 8_755 ?
O3 Pb2 O3 72.3(4) 8_755 2_655 ?
O3 Pb2 O3 115.5(4) 1_455 2_655 ?
O3 Pb2 O3 72.3(4) 7_465 1_455 ?
Pb1 Pb3 Pb4 123.23(2) 2_655 2 ?
Pb1 Pb3 Pb4 62.422(13) 2_655 . ?
Pb1 Pb3 Pb4 123.23(2) 2_655 2_655 ?
Pb1 Pb3 Pb4 62.421(13) 2_655 1_655 ?
Pb4 Pb3 Pb4 171.39(4) . 2_655 ?
Pb4 Pb3 Pb4 75.72(2) 2_655 1_655 ?
Pb4 Pb3 Pb4 103.611(19) . 1_655 ?
Pb4 Pb3 Pb4 75.724(19) . 2 ?
Pb4 Pb3 Pb4 103.61(2) 2_655 2 ?
Pb4 Pb3 Pb4 171.39(4) 1_655 2 ?
O3 Pb3 Pb1 38.32(19) 2_655 2_655 ?
O3 Pb3 Pb1 100.71(19) 8_755 2_655 ?
O3 Pb3 Pb1 38.32(19) 7_565 2_655 ?
O3 Pb3 Pb1 100.71(19) . 2_655 ?
O3 Pb3 Pb4 151.89(19) 2_655 2_655 ?
O3 Pb3 Pb4 36.60(19) 2_655 . ?
O3 Pb3 Pb4 85.43(19) 7_565 2_655 ?
O3 Pb3 Pb4 36.60(19) . 2_655 ?
O3 Pb3 Pb4 85.43(19) 2_655 2 ?
O3 Pb3 Pb4 36.60(19) 8_755 2 ?
O3 Pb3 Pb4 99.14(19) . 2 ?
O3 Pb3 Pb4 99.15(19) 7_565 . ?
O3 Pb3 Pb4 151.89(19) 7_565 2 ?
O3 Pb3 Pb4 36.60(19) 7_565 1_655 ?
O3 Pb3 Pb4 85.43(19) . 1_655 ?
O3 Pb3 Pb4 151.89(19) 8_755 1_655 ?
O3 Pb3 Pb4 85.43(19) 8_755 . ?
O3 Pb3 Pb4 99.14(19) 2_655 1_655 ?
O3 Pb3 Pb4 151.89(19) . . ?
O3 Pb3 Pb4 99.14(19) 8_755 2_655 ?
O3 Pb3 O3 75.5(4) 2_655 7_565 ?
O3 Pb3 O3 72.2(4) . 7_565 ?
O3 Pb3 O3 116.3(4) . 2_655 ?
O3 Pb3 O3 75.5(4) . 8_755 ?
O3 Pb3 O3 72.2(4) 2_655 8_755 ?
O3 Pb3 O3 116.3(4) 7_565 8_755 ?
Pb2 Pb4 Pb3 63.645(19) . 1_455 ?
Pb2 Pb4 Pb3 63.645(19) . . ?
Pb3 Pb4 Pb3 103.61(2) . 1_455 ?
O3 Pb4 Pb2 40.3(2) 7_465 . ?
O3 Pb4 Pb2 40.3(2) 2_655 . ?
O3 Pb4 Pb3 38.67(19) 7_465 1_455 ?
O3 Pb4 Pb3 102.4(2) 2_655 1_455 ?
O3 Pb4 Pb3 38.67(19) 2_655 . ?
O3 Pb4 Pb3 102.4(2) 7_465 . ?
O3 Pb4 O3 78.6(4) 2_655 7_465 ?
O3 Pb4 O5 82.0(4) 7_465 . ?
O3 Pb4 O5 82.0(4) 2_655 . ?
O5 Pb4 Pb2 70.0(4) . . ?
O5 Pb4 Pb3 56.19(14) . . ?
O5 Pb4 Pb3 56.19(14) . 1_455 ?
O1 N1 O1 124(4) . 2_565 ?
O1 N1 O2 118.1(19) 2_565 . ?
O1 N1 O2 118.1(19) . . ?
O4 B1 O4 122(3) 2_665 . ?
O5 B1 O4 119.1(13) 5_666 2_665 ?
O5 B1 O4 119.1(13) 5_666 . ?
Pb1 O3 Pb2 128.0(3) . 1_655 ?
Pb1 O3 Pb3 100.3(3) . . ?
Pb1 O3 Pb4 112.6(3) . 2_655 ?
Pb2 O3 Pb3 107.7(3) 1_655 . ?
Pb4 O3 Pb2 101.5(3) 2_655 1_655 ?
Pb4 O3 Pb3 104.7(3) 2_655 . ?
B1 O4 Pb1 134.8(16) . . ?
Pb4 O5 Pb4 142.2(9) . 2 ?
B1 O5 Pb4 108.9(4) 5_666 2 ?
B1 O5 Pb4 108.9(4) 5_666 . ?
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 Pb1 3.6684(14) 2_665 ?
Pb1 O3 2.215(8) . ?
Pb1 O3 2.215(8) 8_755 ?
Pb1 O4 2.236(15) . ?
Pb2 Pb4 3.5730(11) 2 ?
Pb2 Pb4 3.5730(11) . ?
Pb2 O3 2.358(8) 1_455 ?
Pb2 O3 2.358(8) 8_755 ?
Pb2 O3 2.358(8) 2_655 ?
Pb2 O3 2.358(8) 7_465 ?
Pb3 Pb4 3.6570(5) 2_655 ?
Pb3 Pb4 3.6569(5) . ?
Pb3 Pb4 3.6570(5) 2 ?
Pb3 Pb4 3.6570(5) 1_655 ?
Pb3 O3 2.363(8) 7_565 ?
Pb3 O3 2.363(8) . ?
Pb3 O3 2.363(8) 2_655 ?
Pb3 O3 2.363(8) 8_755 ?
Pb4 O3 2.254(8) 2_655 ?
Pb4 O3 2.254(8) 7_465 ?
Pb4 O5 2.372(6) . ?
N1 O1 1.19(3) . ?
N1 O1 1.19(3) 2_565 ?
N1 O2 1.28(4) . ?
B1 O4 1.41(2) 2_665 ?
B1 O4 1.41(2) . ?
B1 O5 1.35(4) 5_666 ?
