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_1572527
_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 H34 N2, 2(B5 H4 O10)'
_chemical_formula_sum            'C16 H42 B10 N2 O20'
_chemical_formula_weight         690.61
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                94.1950(10)
_cell_angle_beta                 104.1560(10)
_cell_angle_gamma                94.8550(10)
_cell_formula_units_Z            2
_cell_length_a                   9.05340(10)
_cell_length_b                   11.9367(2)
_cell_length_c                   14.5824(2)
_cell_measurement_reflns_used    42854
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.9880
_cell_measurement_theta_min      1.7300
_cell_volume                     1515.35(4)
_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_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -97.00  28.00   0.50    0.50    --   -8.00 -70.00-150.00  250
  2  \w    -45.00  81.00   0.50    0.50    --   -8.00  38.00-150.00  252
  3  \w    -45.00  81.00   0.50    0.50    --   -8.00  38.00  60.00  252
  4  \w    -97.00  28.00   0.50    0.50    --   -8.00 -70.00   0.00  250
  5  \w    -97.00  29.00   0.50    0.50    --   -8.00 -38.00  60.00  252
  6  \w    -44.00  81.00   0.50    0.50    --   -8.00  70.00  90.00  250
  7  \w    -45.00  81.00   0.50    0.50    --   -8.00  39.00 -27.08  252
  8  \w    -44.00  81.00   0.50    0.50    --   -8.00  70.00 150.00  250
  9  \w    -44.00  81.00   0.50    0.50    --   -8.00  70.00-120.00  250
 10  \w    -44.00  81.00   0.50    0.50    --   -8.00  70.00 -30.00  250
 11  \w    -75.00 -48.00   0.50    0.50    --   -8.00  19.00 120.00   54
 12  \w    -44.00  81.00   0.50    0.50    --   -8.00  70.00-150.00  250
;
_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      0.0708040000
_diffrn_orient_matrix_UB_12      0.0272108000
_diffrn_orient_matrix_UB_13      0.0283944000
_diffrn_orient_matrix_UB_21      0.0388606000
_diffrn_orient_matrix_UB_22      -0.0255425000
_diffrn_orient_matrix_UB_23      -0.0314115000
_diffrn_orient_matrix_UB_31      -0.0089128000
_diffrn_orient_matrix_UB_32      0.0468771000
_diffrn_orient_matrix_UB_33      -0.0273399000
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            69149
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.720
_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    0.127
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75663
_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    1.514
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_recrystallization_method
'The material was recrystallised from water'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0531P)^2^+0.4175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6407
_reflns_number_total             6954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MAB4a.cif
_cod_data_source_block           MAB4a
_cod_database_code               1572527
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16H42 N2 B10 O20'
_chemical_oxdiff_usercomment     MAB/TR/AR101B5
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.973
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(HB,HC), C2(HR,HS), C3(H1AA,H2AA), C4(H,HA), C5(HV,HW), C6(HP,HQ), C7(HD,
 HE), C8(HF,HG), C9(HX,HY), C10(HT,HU), C11(H0AA,HZ), C12(H5AA,H6AA), C13(H3AA,
 H4AA), C14(HN,HO)
2.b Idealised Me refined as rotating group:
 C15(HK,HL,HM), C16(HH,HI,HJ)
2.c Idealised tetrahedral OH refined as rotating group:
 O7(H7), O8(H8), O9(H9), O10(H10), O17(H17), O18(H18), O19(H19), O20(H20)
;
_shelx_res_checksum              55375
_shelx_hkl_checksum              50501
_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/AR101 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 1.329
_oxdiff_exptl_absorpt_empirical_full_min 0.641