Structural (XRD) Characterization and an Analysis of H-Bonding Motifs in Some Tetrahydroxidohexaoxidopentaborate(1-) Salts of <i>N</i>-Substituted Guanidinium Cations.
Beckett, Michael A.; Coles, Simon J.; Horton, Peter N.; Rixon, Thomas A.; Molecules (Basel, Switzerland) 28 (2023) 3273–; doi:10.3390/molecules28073273

data_1569077
_publ_section_title
;
 Structural (XRD) Characterization and an Analysis of H-Bonding Motifs in
 Some Tetrahydroxidohexaoxidopentaborate(1-) Salts of <i>N</i>-Substituted
 Guanidinium Cations.
;
_journal_issue                   7
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              3273
_journal_paper_doi               10.3390/molecules28073273
_journal_volume                  28
_journal_year                    2023
_chemical_formula_moiety         'B5 H4 O10, H2 O, C2 H8 N3'
_chemical_formula_sum            'C2 H14 B5 N3 O11'
_chemical_formula_weight         310.21
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-21
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.101(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9962(2)
_cell_length_b                   10.9047(2)
_cell_length_c                   11.7215(2)
_cell_measurement_reflns_used    14324
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.5450
_cell_measurement_theta_min      2.4940
_cell_volume                     1270.47(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      100(2)
_diffrn_detector                 'hybrid pixel detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_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    -84.00  36.00   0.50    0.50    --    5.00 -57.00-150.00  240
  2  \w    -39.00  82.00   0.50    0.50    --   -7.80  57.00  30.00  242
  3  \w    -40.00  82.00   0.50    0.50    --   -7.80  60.00  90.00  244
  4  \w    -84.00  -7.00   0.50    0.50    --    5.00 -38.00 -60.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0306273000
_diffrn_orient_matrix_UB_12      -0.0401169000
_diffrn_orient_matrix_UB_13      -0.0427545000
_diffrn_orient_matrix_UB_21      0.0640164000
_diffrn_orient_matrix_UB_22      -0.0133100000
_diffrn_orient_matrix_UB_23      -0.0179177000
_diffrn_orient_matrix_UB_31      0.0075552000
_diffrn_orient_matrix_UB_32      -0.0494661000
_diffrn_orient_matrix_UB_33      0.0393900000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0115
_diffrn_reflns_av_unetI/netI     0.0071
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17592
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.558
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_target            Mo
_diffrn_source_type              'Rigaku FRE+'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_recrystallization_method
'The material was recrystallised from water'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.246
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0414P)^2^+0.4187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0743
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2810
_reflns_number_total             2893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MAB1.cif
_cod_data_source_block           MAB1
_cod_database_code               1569077
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C8 H48 B20 N12 O40 '
_chemical_oxdiff_usercomment     'MAB/TR/MeGuanB5 (block)'
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.942
_reflns_odcompleteness_completeness 99.25
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C2(H2C,H2D,H2E)
;
_shelx_res_checksum              64136
_shelx_hkl_checksum              81946
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in perfluoroether oil'
_olex2_submission_original_sample_id MAB/TR/MeGaunB5
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.154
_oxdiff_exptl_absorpt_empirical_full_min 0.802