K5[B3O3F4(OH)]2(NO3): the first hydroxyfluorooxoborate-nitrate with short ultraviolet cutoff edge and large birefringence
Zhang, Luyong; Wang, Shibin; Zhang, Fangfang; Yang, Zhihua; Hou, Xueling; Dalton Transactions  (2023) –; doi:10.1039/D3DT02529B

data_7713950
_publ_section_title
;
 K5[B3O3F4(OH)]2(NO3): the first hydroxyfluorooxoborate-nitrate with short
 ultraviolet cutoff edge and large birefringence
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02529B
_journal_year                    2023
_chemical_formula_moiety         'B6 F8 H2 K5 N O11'
_chemical_formula_sum            'B6 F8 H2 K5 N O11'
_chemical_formula_weight         604.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-08-28
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2023-08-30 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.508(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1792(9)
_cell_length_b                   13.4126(8)
_cell_length_c                   8.1449(6)
_cell_measurement_reflns_used    312
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      20.30
_cell_measurement_theta_min      4.45
_cell_volume                     1737.84(19)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection
'Bruker BIS V6.2.15/2021-03-15 && APEX3 2019.11-0'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            9125
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.535
_diffrn_reflns_theta_min         1.986
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5425
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1039 before and 0.0755 after correction.
The Ratio of minimum to maximum transmission is 0.7276.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.310
_exptl_crystal_description       block
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.075
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.5425
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2008
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0218P)^2^+1.6781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1556
_reflns_number_total             2008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02529b2.cif
_cod_data_source_block           k5[b3o3f4(oh)]2(no3)
_cod_database_code               7713950
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.819
_olex2_refinement_description
;
1. Restrained distances
 O1-H1
 0.95 with sigma of 0.01
2. Others
 Fixed Sof: O5(0.5) O6(0.5) O7(0.5)
;
_shelx_res_checksum              87815
_olex2_submission_special_instructions 'No special instructions were received'