Crystal structure of a carborane endo/exo-dianion and its use in the synthesis of ditopic ligands for supramolecular frameworks.
Zhang, Kang; Shen, Yunjun; Liu, Jiyong; Spingler, Bernhard; Duttwyler, Simon; Chemical communications (Cambridge, England) 54 (2018) 1698–1701; doi:10.1039/c7cc07724f

data_7121046
_publ_section_title
;
 Crystal structure of a carborane endo/exo-dianion and its use in the
 synthesis of ditopic ligands for supramolecular frameworks.
;
_journal_issue                   14
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1698
_journal_page_last               1701
_journal_paper_doi               10.1039/c7cc07724f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C10 H24 B22 N2, 2(C8 H20 N)'
_chemical_formula_sum            'C26 H64 B22 N4'
_chemical_formula_weight         670.63
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-05
_audit_creation_method
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Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
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_audit_update_record
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2017-12-11 deposited with the CCDC.
2017-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                91.607(7)
_cell_angle_beta                 96.421(7)
_cell_angle_gamma                92.598(6)
_cell_formula_units_Z            1
_cell_length_a                   8.5061(6)
_cell_length_b                   10.3155(9)
_cell_length_c                   12.1216(11)
_cell_measurement_reflns_used    1693
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3512
_cell_measurement_theta_min      3.1874
_cell_volume                     1055.26(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
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_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -61.00   34.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6871  -38.0000  -60.0000 95

  2 omega  -16.00   76.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6871   38.0000  120.0000 92

  3 omega  -77.00   21.00   1.0000   70.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.5621  -77.0000 -180.0000 98
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0120894000
_diffrn_orient_matrix_UB_12      0.0649491000
_diffrn_orient_matrix_UB_13      0.0165687000
_diffrn_orient_matrix_UB_21      0.0178044000
_diffrn_orient_matrix_UB_22      -0.0157782000
_diffrn_orient_matrix_UB_23      0.0564598000
_diffrn_orient_matrix_UB_31      0.0812106000
_diffrn_orient_matrix_UB_32      0.0166041000
_diffrn_orient_matrix_UB_33      -0.0030082000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6948
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         3.194
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_description       plate
_exptl_crystal_F_000             358
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.226
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3863
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0890P)^2^+0.0847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1885
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2502
_reflns_number_total             3863
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07724f2.cif
_cod_data_source_block           161110_2016_zk_dicn
_cod_depositor_comments
'Adding full bibliography for 7121042--7121048.cif.'
_cod_database_code               7121046
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'c10 h10 n2 o8 b1'
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.978
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C)
2.d Boron cage BH refined with riding coordinates:
 B2(H2), B3(H3A), B4(H4A), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9), B10(H10),
 B11(H11)
;
_shelx_res_checksum              46213
_olex2_submission_special_instructions 'No special instructions were received'