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_1572524
_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   mixed
_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                84.415(3)
_cell_angle_beta                 84.541(3)
_cell_angle_gamma                75.872(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6641(4)
_cell_length_b                   12.7484(4)
_cell_length_c                   13.0913(4)
_cell_measurement_reflns_used    11779
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0670
_cell_measurement_theta_min      1.6440
_cell_volume                     1552.40(10)
_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 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    -34.00  84.00   0.50    2.50    --   -4.50  65.00-121.00  236
  2  \w    -93.00  25.00   0.50    2.50    --   -4.50 -65.00 102.00  236
  3  \w    -93.00  27.00   0.50    2.50    --   -4.50 -70.00-150.00  240
  4  \w    -84.00  31.00   0.50    2.50    --    4.50 -38.00  60.00  230
  5  \w     -3.00  46.00   0.50    2.50    --    4.50  38.00  90.00   98
  6  \w    -14.00  92.00   0.50    2.50    --    4.50  38.00   0.00  212
;
_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      -0.0101146000
_diffrn_orient_matrix_UB_12      0.0421219000
_diffrn_orient_matrix_UB_13      -0.0401276000
_diffrn_orient_matrix_UB_21      0.0681054000
_diffrn_orient_matrix_UB_22      0.0089475000
_diffrn_orient_matrix_UB_23      0.0066096000
_diffrn_orient_matrix_UB_31      0.0319217000
_diffrn_orient_matrix_UB_32      -0.0381703000
_diffrn_orient_matrix_UB_33      -0.0364152000
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0292
_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       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35495
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         1.652
_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    0.124
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67343
_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    1.477
_exptl_crystal_description       plate
_exptl_crystal_F_000             724
_exptl_crystal_recrystallization_method
'The material was recrystallised from water'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     484
_refine_ls_number_reflns         7118
_refine_ls_number_restraints     94
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0466P)^2^+0.5145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6044
_reflns_number_total             7118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            MAB4b.cif
_cod_data_source_block           MAB4b
_cod_database_code               1572524
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16H42 N2 B10 O20'
_chemical_oxdiff_usercomment     'MAB/TR/AR101B5 plate'
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.968
_reflns_odcompleteness_completeness 99.99
_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. Restrained distances
 N2-C11A \\sim N2-C11 \\sim N2-C14A \\sim N2-C14
 with sigma of 0.02
 C14-C13 \\sim C14A-C13A \\sim C13A-C12A \\sim C13-C12 \\sim C12A-C11A \\sim
C12-C11
 with sigma of 0.02
 C11A-C13A \\sim C11-C13 \\sim C12A-C14A \\sim C12-C14
 with sigma of 0.04
 C13-N2 \\sim N2-C13A
 with sigma of 0.04
 C12A-N2 \\sim N2-C12
 with sigma of 0.04
 C14A-C11A \\sim C14-C11
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C11A)
Uanis(C14A) = Uanis(C14)
4. Rigid body (RIGU) restrains
 N2, C11, C12, C13, C14, C11A, C12A, C13A, C14A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=
 Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=1-FVAR(1)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(C13)=Sof(H13A)=
 Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=FVAR(1)
6.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), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C11A(H11C,H11D), C12A(H12C,
 H12D), C13A(H13C,H13D), C14A(H14C,H14D)
6.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              21260
_shelx_hkl_checksum              75712
_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 (plate)'
_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 1.715
_oxdiff_exptl_absorpt_empirical_full_min 0.754