Variable dimensionality of the anion framework in four new borophosphates and fluoroborophosphates with short cutoff edges
Zhang, Ruonan; Guo, Siru; Wang, Xuping; Yang, Rong; Chen, Zhen; Zhang, Wenyao; Zhang, Fangfang; Guo, Zhiyong; Han, Shujuan; Yang, Zhihua; Dalton Transactions  (2022) –; doi:10.1039/D1DT04266A

data_7709397
_publ_section_title
;
 Variable dimensionality of the anion framework in four new borophosphates
 and fluoroborophosphates with short cutoff edges
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04266A
_journal_year                    2022
_chemical_formula_moiety         'B3 Li O16 P4, 2(H4 N)'
_chemical_formula_sum            'B3 H8 Li N2 O16 P4'
_chemical_formula_weight         455.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-12-17 deposited with the CCDC.	2022-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.951(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3237(4)
_cell_length_b                   25.6466(14)
_cell_length_c                   7.6796(4)
_cell_measurement_reflns_used    3040
_cell_measurement_temperature    300.0
_cell_measurement_theta_max      54.870
_cell_measurement_theta_min      6.325
_cell_volume                     1249.81(13)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      300.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'PHOTON III C28 detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            12631
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         3.163
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6537
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0758 before and 0.0626 after correction.
The Ratio of minimum to maximum transmission is 0.8769.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.420
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         2865
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0462P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2180
_reflns_number_total             2865
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt04266a2.cif
_cod_data_source_block           mo_gsr20201220004_0m
_cod_original_cell_volume        1249.81(12)
_cod_database_code               7709397
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H,H,H,H,H) groups
2. Restrained distances
 N2-H2A = N2-H2B = N2-H2C = N2-H2D
 0.98 with sigma of 0.02
 N1-H1A = N1-H1B = N1-H1C = N1-H1D
 0.98 with sigma of 0.02
 H1A-H1B \\sim H1A-H1C \\sim H1A-H1D \\sim H1B-H1C \\sim H1B-H1D \\sim H1C-H1D
 with sigma of 0.04
 H2A-H2B \\sim H2A-H2C \\sim H2A-H2D \\sim H2B-H2C \\sim H2B-H2D \\sim H2C-H2D
 with sigma of 0.04
;
_shelx_res_checksum              46790
_olex2_submission_special_instructions 'No special instructions were received'