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_1572525
_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         'C16 H28 N4, 2(B5 H4 O10), 3(H2 O)'
_chemical_formula_sum            'C16 H42 B10 N4 O23'
_chemical_formula_weight         766.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-13
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.01.22 svn.r3481 for OlexSys, GUI svn.r5457)
;
_cell_angle_alpha                86.483(3)
_cell_angle_beta                 81.244(3)
_cell_angle_gamma                75.624(3)
_cell_formula_units_Z            2
_cell_length_a                   9.4616(4)
_cell_length_b                   9.4780(3)
_cell_length_c                   19.8856(8)
_cell_measurement_reflns_used    11311
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3210
_cell_measurement_theta_min      2.0540
_cell_volume                     1706.79(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_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_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  29.00   1.00   10.00    --    5.00 -38.00  60.00  113
  2  \w    -99.00  24.00   1.00   10.00    --   -9.70 -72.00  90.00  123
  3  \w    -99.00  15.00   1.00   10.00    --   -9.70 -38.00-180.00  114
  4  \w    -99.00  20.00   1.00   10.00    --   -9.70 -57.00 -60.00  119
  5  \w    -34.00  80.00   1.00   10.00    --   -9.70  38.00   0.00  114
  6  \w    -39.00  80.00   1.00   10.00    --   -9.70  57.00-150.00  119
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_details 'Rigaku, AFC12 \k goniometer'
_diffrn_measurement_device_type
'Rigaku FRE+ equipped with HF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ 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      -0.0663513000
_diffrn_orient_matrix_UB_12      0.0250603000
_diffrn_orient_matrix_UB_13      -0.0142780000
_diffrn_orient_matrix_UB_21      0.0400567000
_diffrn_orient_matrix_UB_22      -0.0133817000
_diffrn_orient_matrix_UB_23      -0.0330881000
_diffrn_orient_matrix_UB_31      -0.0102340000
_diffrn_orient_matrix_UB_32      -0.0718675000
_diffrn_orient_matrix_UB_33      0.0021370000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38202
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.073
_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    0.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
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    1.492
_exptl_crystal_description       plate
_exptl_crystal_F_000             800
_exptl_crystal_recrystallization_method
'The material was recrystallised from water'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         7820
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0457
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5988
_reflns_number_total             7820
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MAB2.cif
_cod_data_source_block           MAB2
_cod_database_code               1572525
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C16H28N4 (B5O6(OH)4)2'
_chemical_oxdiff_usercomment     MAB/TR/AR87/B5
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.965
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O8-H8 = O10-H10 = O9-H9 = O7-H7 = O17-H17 = O18-H18 = O19-H19 = O20-H20
 0.87 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O23 \\sim O23A: within 2A with sigma of 0.0025 and sigma for terminal atoms of
0.005
O22 \\sim O22A: within 2A with sigma of 0.0025 and sigma for terminal atoms of
0.005
4. Rigid body (RIGU) restrains
 O22, O22A, O23, O23A, O21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O22(0.5) H22A(0.5) H22B(0.5) O23(0.5) H23A(0.5) H23B(0.5)
 O22A(0.5) H22C(0.5) H22D(0.5) O23A(0.5) H23C(0.5) H23D(0.5)
6.a Free rotating group:
 O22(H22A,H22B), O21(H21A,H21B), O23(H23A,H23B), O22A(H22C,H22D), O23A(H23C,
 H23D)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C15(H15A,H15B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              15989
_shelx_hkl_checksum              70255
_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/AR87/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 1.371
_oxdiff_exptl_absorpt_empirical_full_min 0.568