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_7711359
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-06-23
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_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_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -74.00  10.00   0.50   20.00    --  -33.40  72.00-155.00  168
  2  \w    -74.00 -48.00   0.50   20.00    --  -33.40 -72.00  74.00   52
  3  \w     -3.00 116.00   0.50   20.00    --   33.40  72.00-155.00  238
  4  \w    -13.00  40.00   0.50   20.00    --   33.40 -72.00  74.00  106
  5  \w    -72.00 -47.00   0.50   62.00    --  -92.00  72.00-155.00   50
  6  \w   -144.00 -51.00   0.50   62.00    --  -92.00 -72.00  74.00  186
  7  \w     58.00 157.00   0.50   62.00    --   99.01  72.00-155.00  198
  8  \w     43.00  79.00   0.50   62.00    --   99.01 -72.00  74.00   72
  9  \w     43.00  96.00   0.50   20.00    --   33.40 178.00  60.00  106
 10  \w     42.00 122.00   0.50   20.00    --   33.40 178.00 -30.00  160
 11  \w      1.00 113.00   0.50   20.00    --   33.40  57.00-180.00  224
 12  \w     32.00 119.00   0.50   20.00    --   33.40  77.00 -90.00  174
 13  \w     29.00  55.00   0.50   20.00    --   33.40  77.00   0.00   52
 14  \w     45.00 112.00   0.50   20.00    --   33.40 178.00  90.00  134
 15  \w     42.00 116.00   0.50   20.00    --   33.40 178.00-180.00  148
 16  \w     -8.00  18.00   0.50   20.00    --   33.40  77.00   0.00   52
 17  \w      0.00 108.00   0.50   20.00    --   33.40  57.00  60.00  216
 18  \w      0.00  26.00   0.50   20.00    --   33.40  77.00 -90.00   52
 19  \w     -2.00 113.00   0.50   20.00    --   33.40  57.00 -30.00  230
 20  \w     -9.00 112.00   0.50   20.00    --   33.40  77.00  90.00  242
 21  \w     70.00  98.00   0.50   20.00    --   33.40  77.00   0.00   56
 22  \w   -162.00-136.00   0.50   62.00    --  -92.00 -76.00  94.53   52
 23  \w    -74.00 -49.00   0.50   62.00    --  -92.00 -76.00-162.48   50
 24  \w   -172.00-111.00   0.50   62.00    --  -92.00 -77.00 -57.99  122
 25  \w   -131.00-105.00   0.50   62.00    --  -92.00 -76.00-162.48   52
 26  \w    -74.00 -49.00   0.50   62.00    --  -92.00 -77.00-180.00   50
 27  \w    -74.00 -49.00   0.50   62.00    --  -92.00 -77.00 -57.99   50
 28  \w    -81.00 -49.00   0.50   62.00    --  -92.00 -75.00-122.31   64
 29  \w   -125.00 -49.00   0.50   62.00    --  -92.00 -77.00  60.00  152
 30  \w    -55.00 -24.00   0.50   62.00    --  -92.00 111.00-150.00   62
 31  \w   -177.00-136.00   0.50   62.00    --  -92.00 -76.00-162.48   82
 32  \w    -89.00 -49.00   0.50   62.00    --  -92.00 -75.00  32.93   80
 33  \w   -175.00 -49.00   0.50   62.00    --  -92.00 -77.00 -22.17  252
 34  \w   -176.00-150.00   0.50   62.00    --  -92.00 -77.00 108.35   52
 35  \w    -87.00 -49.00   0.50   62.00    --  -92.00 -77.00 -13.05   76
 36  \w    -74.00 -49.00   0.50   62.00    --  -92.00 -77.00 108.35   50
 37  \w   -107.00 -49.00   0.50   62.00    --  -92.00 -76.00  19.30  116
 38  \w   -177.00-107.00   0.50   62.00    --  -92.00 -75.00-147.94  140
 39  \w    -85.00 -49.00   0.50   62.00    --  -92.00 -77.00  -3.87   72
 40  \w   -108.00 -59.00   0.50   62.00    --  -92.00 111.00-150.00   98
 41  \w   -137.00-111.00   0.50   62.00    --  -92.00 -75.00  32.93   52
 42  \w   -177.00-132.00   0.50   62.00    --  -92.00 -77.00  -3.87   90
 43  \w    -75.00 -49.00   0.50   62.00    --  -92.00 -75.00 -42.65   52
 44  \w    -79.00 -49.00   0.50   62.00    --  -92.00 -75.00 -74.94   60
 45  \w   -144.00-118.00   0.50   62.00    --  -92.00 -75.00 -74.94   52
 46  \w   -111.00 -49.00   0.50   62.00    --  -92.00 -77.00 150.00  124
 47  \w    -76.00 -49.00   0.50   62.00    --  -92.00 -77.00  71.05   54
 48  \w    -74.00 -49.00   0.50   62.00    --  -92.00 -76.00  94.53   50
 49  \w   -176.00-135.00   0.50   62.00    --  -92.00 -77.00-180.00   82
 50  \w   -161.00-134.00   0.50   62.00    --  -92.00 -77.00   4.34   54
 51  \w   -117.00 -49.00   0.50   62.00    --  -92.00 -77.00   4.34  136
 52  \w    -74.00 -49.00   0.50   62.00    --  -92.00 -77.00 168.17   50
 53  \w   -105.00 -33.00   0.50   62.00    --  -92.00 111.00   0.00  144
 54  \w    -90.00 -49.00   0.50   62.00    --  -92.00 -77.00 124.58   82
 55  \w   -173.00-148.00   0.50   62.00    --  -92.00 -76.00-130.59   50
 56  \w    -81.00 -49.00   0.50   62.00    --  -92.00 -76.00-130.59   64
 57  \w   -170.00-145.00   0.50   62.00    --  -92.00 -77.00 150.00   50
 58  \w    -76.00 -49.00   0.50   62.00    --  -92.00 -77.00 -90.00   54
 59  \w   -176.00-150.00   0.50   62.00    --  -92.00 -77.00 138.05   52
 60  \w   -112.00 -49.00   0.50   62.00    --  -92.00 -77.00 138.05  126
 61  \w   -119.00 -93.00   0.50   62.00    --  -92.00 -76.00  94.53   52
 62  \w   -128.00 -96.00   0.50   62.00    --  -92.00 -77.00 -13.05   64
 63  \w   -145.00 -91.00   0.50   62.00    --  -92.00 -75.00 -42.65  108
 64  \w   -127.00-101.00   0.50   62.00    --  -92.00 -77.00 108.35   52
 65  \w   -139.00-113.00   0.50   62.00    --  -92.00 -75.00  44.69   52
 66  \w    -79.00 -49.00   0.50   62.00    --  -92.00 -75.00  44.69   60
 67  \w   -146.00-107.00   0.50   62.00    --  -92.00 -77.00 168.17   78
 68  \w   -150.00-124.00   0.50   62.00    --  -92.00 -76.00-108.54   52
 69  \w   -100.00 -49.00   0.50   62.00    --  -92.00 -76.00-108.54  102
 70  \w   -117.00 -82.00   0.50   62.00    --  -92.00 -77.00 -90.00   70
 71  \w   -145.00-119.00   0.50   62.00    --  -92.00 -77.00  71.05   52
 72  \w    -76.00 -49.00   0.50   62.00    --  -92.00 -75.00-147.94   54
 73  \w   -168.00-142.00   0.50   62.00    --  -92.00 -76.00 -83.50   52
 74  \w    -91.00 -49.00   0.50   62.00    --  -92.00 -76.00 -83.50   84
 75  \w     82.00 133.00   0.50   62.00    --   99.01 111.00 -30.00  102
 76  \w    118.00 157.00   0.50   62.00    --   99.01  77.00-180.00   78
 77  \w     56.00 114.00   0.50   62.00    --   99.01  77.00-180.00  116
 78  \w     56.00 157.00   0.50   62.00    --   99.01  77.00  30.00  202
 79  \w     56.00 156.00   0.50   62.00    --   99.01  77.00  90.00  200
 80  \w      9.00  53.00   0.50   62.00    --   99.01 -94.00-180.00   88
 81  \w    109.00 134.00   0.50   62.00    --   99.01 -88.00-114.84   50
 82  \w     66.00 156.00   0.50   62.00    --   99.01  77.00-120.00  180
 83  \w      9.00 102.00   0.50   62.00    --   99.01 -88.00-114.84  186
 84  \w    122.00 147.00   0.50   62.00    --   99.01 -87.00  26.11   50
 85  \w     68.00 117.00   0.50   62.00    --   99.01 -87.00  26.11   98
 86  \w    106.00 146.00   0.50   62.00    --   99.01 -85.00 -67.92   80
 87  \w      9.00  21.50   0.50   62.00    --   99.01 -87.00  26.11   25
;
_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         1.343
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Flack x determined using 6570 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         17621
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          14.346
_refine_ls_shift/su_mean         0.113
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0715P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1179
_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           Independent_Atom_Model
_cod_database_code               7711359
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         B4O11N2H16
_olex2_refinement_description
;
1. Restrained distances
 O10-H10A
 0.952 with sigma of 0.02
 O10-H10B
 0.952 with sigma of 0.02
 O11-H11A
 0.952 with sigma of 0.02
 O11-H11B
 0.952 with sigma of 0.02
 O7-H7
 0.952 with sigma of 0.02
 O6-H6
 0.952 with sigma of 0.02
 O8-H8
 0.952 with sigma of 0.02
 O9-H9
 0.952 with sigma of 0.02
 N2-H2D
 0.8 with sigma of 0.02
;
_shelx_res_checksum              14678
_shelx_hkl_checksum              67906
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_diffrn_reflns_filtered   3777
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.548
_oxdiff_exptl_absorpt_empirical_full_min 0.719