Tetrahydroxidohexaoxidopentaborate(1-) Salts of C6-Linked Substituted Diimidazolium and Dipyrrolidinium Cations: Synthesis, Characterization and XRD Studies
Al-Dulayymi, Ahmad R.; Beckett, Michael A.; Braganca, Radek; Coles, Simon J.; Horton, Peter N.; Rixon, Thomas A.; Inorganics 12 (2024) 220–; doi:10.3390/inorganics12080220

data_1572523
_publ_section_title
;
 Tetrahydroxidohexaoxidopentaborate(1-) Salts of C6-Linked Substituted
 Diimidazolium and Dipyrrolidinium Cations: Synthesis, Characterization
 and XRD Studies
;
_journal_issue                   8
_journal_name_full               Inorganics
_journal_page_first              220
_journal_paper_doi               10.3390/inorganics12080220
_journal_volume                  12
_journal_year                    2024
_chemical_formula_moiety         'C18 H38 N2, 2(B5 H4 O10)'
_chemical_formula_sum            'C18 H46 B10 N2 O20'
_chemical_formula_weight         718.67
_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             2018-07-16
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.6290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.06420(10)
_cell_length_b                   11.55510(10)
_cell_length_c                   15.7004(2)
_cell_measurement_reflns_used    15705
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.2000
_cell_measurement_theta_min      4.5840
_cell_volume                     1740.10(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -83.00  69.00   0.50    1.00    --    0.00  20.00-120.00  304
  2  \w      3.00  79.00   0.50    1.00    --    5.00  50.00  90.00  152
  3  \w   -179.00 -12.00   0.50    4.00    --  -90.00  60.00  42.87  334
  4  \w   -179.00-129.00   0.50    4.00    --  -90.00  60.00  -7.73  100
  5  \w   -125.00 -99.00   0.50    4.00    --  -90.00  60.00  -7.73   52
  6  \w    -58.00 -29.00   0.50    4.00    --  -90.00  60.00  -7.73   58
  7  \w    -93.00 -67.00   0.50    4.00    --  -90.00  57.00  91.85   52
  8  \w    -83.00 -27.00   0.50    4.00    --  -90.00   0.00  30.00  112
  9  \w   -146.00-120.00   0.50    4.00    --  -90.00  60.00 179.62   52
 10  \w    -70.00 -43.00   0.50    4.00    --  -90.00  60.00 179.62   54
 11  \w   -121.00 -68.00   0.50    4.00    --  -90.00  60.00 -64.95  106
 12  \w    -44.00 -18.00   0.50    4.00    --  -90.00  60.00 -64.95   52
 13  \w   -179.00-143.00   0.50    4.00    --  -90.00  57.00  91.85   72
 14  \w   -140.00 -91.00   0.50    4.00    --  -90.00   0.00  30.00   98
 15  \w    -87.00  -1.00   0.50    4.00    --  -90.00  30.00 -60.00  172
 16  \w   -178.00 -20.00   0.50    4.00    --  -90.00  60.00 100.24  316
 17  \w   -107.00 -28.00   0.50    4.00    --  -90.00  60.00   6.25  158
 18  \w   -164.00-112.00   0.50    4.00    --  -90.00  60.00-159.34  104
 19  \w    -72.00 -21.00   0.50    4.00    --  -90.00  60.00-159.34  102
 20  \w   -179.00 -88.00   0.50    4.00    --  -90.00  60.00 139.10  182
 21  \w    -76.00 -18.00   0.50    4.00    --  -90.00  60.00 139.10  116
 22  \w   -179.00  -1.00   0.50    4.00    --  -90.00  60.00-111.76  356
 23  \w   -173.00-105.00   0.50    4.00    --  -90.00  60.00 -84.08  136
 24  \w   -178.00-130.00   0.50    4.00    --  -90.00  60.00  80.77   96
 25  \w   -104.00  -2.00   0.50    4.00    --  -90.00  60.00  80.77  204
 26  \w   -179.00-128.00   0.50    4.00    --  -90.00  30.00 -60.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details 'Rigaku, AFC11 quarter \c goniometer'
_diffrn_measurement_device_type
'Rigaku 007HF equipped with Varimax confocal mirrors and an AFC11 goniometer and HyPix 6000 detector'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0225110000
_diffrn_orient_matrix_UB_12      0.1250711000
_diffrn_orient_matrix_UB_13      0.0354477000
_diffrn_orient_matrix_UB_21      0.1584019000
_diffrn_orient_matrix_UB_22      -0.0216129000
_diffrn_orient_matrix_UB_23      0.0350382000
_diffrn_orient_matrix_UB_31      0.0146344000
_diffrn_orient_matrix_UB_32      0.0408858000
_diffrn_orient_matrix_UB_33      -0.0900835000
_diffrn_radiation_collimation    'Varimax focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0162
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25011
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.237
_diffrn_reflns_theta_min         4.610
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_recrystallization_method
'The material was recrystallised from water'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0735P)^2^+0.6048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1259
_refine_ls_wR_factor_ref         0.1290
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2928
_reflns_number_total             3183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MAB5.cif
_cod_data_source_block           MAB5
_cod_database_code               1572523
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C18H46N2B10O20
_chemical_oxdiff_usercomment     'MAB/TAR/AR104 B5'
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.867
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B)
2.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C)
;
_shelx_res_checksum              59832
_shelx_hkl_checksum              7176
_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/TAR/AR104 B5'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.727