Charge density studies of single and transient (single to double) boron–oxygen bonds in (NH4)2B4O5(OH)4·2H2O
Gajda, Roman; Piekara, Anna; Tchoń, Daniel; Woźniak, Krzysztof; Sławiński, Wojciech A.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02442J

data_7711360
_publ_section_title
;
 Charge density studies of single and transient (single to double)
 boron--oxygen bonds in (NH4)2B4O5(OH)4&#x00B7;2H2O
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02442J
_journal_year                    2022
_chemical_formula_moiety         'B4 H4 O9, 2(H4 N), 2(H2 O)'
_chemical_formula_sum            'B4 H16 N2 O11'
_chemical_formula_weight         263.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_audit_update_record
;
2022-06-23 deposited with the CCDC.	2022-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.6290(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.16499(7)
_cell_length_b                   10.59066(11)
_cell_length_c                   7.24742(6)
_cell_measurement_reflns_used    51795
_cell_measurement_temperature    90.1(6)
_cell_measurement_theta_max      65.9010
_cell_measurement_theta_min      3.4460
_cell_volume                     543.723(9)
_computing_cell_refinement       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.36a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      90.1(6)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0680994000
_diffrn_orient_matrix_UB_12      -0.0409611000
_diffrn_orient_matrix_UB_13      0.0496646000
_diffrn_orient_matrix_UB_21      -0.0036795000
_diffrn_orient_matrix_UB_22      0.0349905000
_diffrn_orient_matrix_UB_23      0.0828323000
_diffrn_orient_matrix_UB_31      -0.0733158000
_diffrn_orient_matrix_UB_32      -0.0397881000
_diffrn_orient_matrix_UB_33      0.0217033000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0555
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            94540
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         62.671
_diffrn_reflns_theta_min         3.433
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.159
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.36a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       irregular
_exptl_crystal_F_000             276
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         13460
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.038
_refine_ls_R_factor_gt           0.031
_refine_ls_R_Fsqd_factor         0.039
_refine_ls_shift/su_max          0.01514
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w2 = 1/[s^2^(Fo^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.071
_reflns_Friedel_coverage         0.934
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                15709
_reflns_number_total             17621
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02442j2.cif
_cod_data_source_block           Multipole_Model_Refinement
_cod_database_code               7711360
_chemical_oxdiff_formula         B4O11N2H16