Hydroxyfluorooxoborate (NH<sub>4</sub>)[C(NH<sub>2</sub>)<sub>3</sub>][B<sub>3</sub>O<sub>3</sub>F<sub>4</sub>(OH)] for exploring the effects of cation substitution on structure and optical properties.
Chen, Ziqi; Li, Fuming; Yang, Zhihua; Pan, Shilie; Mutailipu, Miriding; Chemical communications (Cambridge, England) 59 (2023) 12435–12438; doi:10.1039/d3cc04346k

data_7132298
_publ_section_title
;
 Hydroxyfluorooxoborate
 (NH<sub>4</sub>)[C(NH<sub>2</sub>)<sub>3</sub>][B<sub>3</sub>O<sub>3</sub>F<sub>4</sub>(OH)]
 for exploring the effects of cation substitution on structure and optical
 properties.
;
_journal_issue                   83
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12435
_journal_page_last               12438
_journal_paper_doi               10.1039/d3cc04346k
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'B3 F4 H O4, C H6 N3, H4 N'
_chemical_formula_sum            'C H11 B3 F4 N4 O4'
_chemical_formula_weight         251.57
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-09-02 deposited with the CCDC.	2023-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.748(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.280(2)
_cell_length_b                   8.7593(11)
_cell_length_c                   14.8039(18)
_cell_measurement_reflns_used    4985
_cell_measurement_temperature    156.0
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      2.69
_cell_volume                     1958.3(4)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      156.0
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.996
_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  0.0949
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31760
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_min         2.688
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.185
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6013
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1561 before and 0.0752 after correction.
The Ratio of minimum to maximum transmission is 0.8065.
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    1.706
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2254
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0407
_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/[\s^2^(Fo^2^)+(0.0319P)^2^+2.5029P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1702
_reflns_number_total             2254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04346k2.cif
_cod_data_source_block           111
_cod_original_cell_volume        1958.4(5)
_cod_database_code               7132298
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Restrained distances
 N4-H1 = N4-H2 = N4-H3 = N4-H11
 0.85 with sigma of 0.02
 N4-H1 \\sim N4-H2 \\sim N4-H3 \\sim N4-H11
 with sigma of 0.02
 H1-H2 \\sim H2-H3 \\sim H3-H11 \\sim H11-H1 \\sim H2-H11 \\sim H1-H3
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
N4 \\sim H1 \\sim H2 \\sim H3 \\sim H11: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 N4, H1, H2, H3, H11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a X=CH2 refined with riding coordinates:
 N3(H5,H4), N2(H8,H9), N1(H6,H7)
;
_shelx_res_checksum              26519
_shelx_hkl_checksum              35411
_olex2_submission_special_instructions 'No special instructions were received'