Two Lead Borate-nitrates with Anion-Centered [OPb4] Tetrahedra and Two Types of π-Conjugated Planar Units Showing Large Birefringence
Bai, Shuo; Yang, Daqing; Zhang, Bingbing; Li, Ling; Wang, Ying; Dalton Transactions  (2022) –; doi:10.1039/D2DT00183G

data_7709455
_publ_section_title
;
 Two Lead Borate-nitrates with Anion-Centered [OPb4] Tetrahedra and Two
 Types of \p-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(B4 F2 N2 O22 Pb12)'
_chemical_formula_sum            'B2 F N O11 Pb6'
_chemical_formula_weight         1473.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_audit_creation_date             2021-05-07
_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                 101.704(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.8025(7)
_cell_length_b                   11.5092(9)
_cell_length_c                   8.8989(9)
_cell_measurement_reflns_used    8596
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.53
_cell_volume                     682.22(11)
_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)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0663
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.337
_exptl_absorpt_coefficient_mu    73.830
_exptl_absorpt_correction_T_max  0.0481
_exptl_absorpt_correction_T_min  0.0007
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1015 before and 0.0698 after correction. The Ratio of minimum to maximum transmission is 0.0146. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    7.174
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.811
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.340
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1645
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0231
_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/[\s^2^(Fo^2^)+(0.0298P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1462
_reflns_number_total             1645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00183g2.cif
_cod_data_source_block           ww
_cod_database_code               7709455
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.156
_shelx_estimated_absorpt_t_min   0.022
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
;
_shelx_res_checksum              98258
_shelx_hkl_checksum              32319
_olex2_submission_special_instructions 'No special instructions were received'