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_7121044
_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         'C12 H31 B22 N2, 2(C4 H10 N0.5)'
_chemical_formula_sum            'C20 H51 B22 N3'
_chemical_formula_weight         571.45
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-05
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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                73.928(9)
_cell_angle_beta                 86.356(8)
_cell_angle_gamma                88.275(9)
_cell_formula_units_Z            2
_cell_length_a                   10.2902(11)
_cell_length_b                   10.7001(12)
_cell_length_c                   16.1214(14)
_cell_measurement_reflns_used    1376
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      29.4258
_cell_measurement_theta_min      2.7796
_cell_volume                     1702.1(3)
_computing_cell_refinement
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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)
;
_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)
;
_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      170
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -28.00   61.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183   38.0000  -60.0000 89

  2 omega  -79.00   14.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183  -38.0000  -30.0000 93

  3 omega  -91.00   21.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -12.7183  -77.0000  150.0000 112
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0014977000
_diffrn_orient_matrix_UB_12      -0.0210926000
_diffrn_orient_matrix_UB_13      0.0458121000
_diffrn_orient_matrix_UB_21      -0.0429040000
_diffrn_orient_matrix_UB_22      0.0523053000
_diffrn_orient_matrix_UB_23      0.0021186000
_diffrn_orient_matrix_UB_31      -0.0541144000
_diffrn_orient_matrix_UB_32      -0.0397381000
_diffrn_orient_matrix_UB_33      0.0004185000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.1176
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11101
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.785
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.055
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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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)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       plate
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         6154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.1636
_refine_ls_R_factor_gt           0.0845
_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^)+(0.1315P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2202
_refine_ls_wR_factor_ref         0.2915
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2731
_reflns_number_total             6154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07724f2.cif
_cod_data_source_block           170111_zk_2_2nd
_cod_depositor_comments
'Adding full bibliography for 7121042--7121048.cif.'
_cod_database_code               7121044
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'c10 h10 n2 o8 b1'
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.974
_reflns_odcompleteness_completeness 98.71
_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,H,H,H) groups
2. Others
 Fixed Sof: C13(0.5) H13A(0.5) H13B(0.5) C16(0.5) H16A(0.5) H16B(0.5) C15(0.5)
 H15A(0.5) H15B(0.5) C18(0.5) H18A(0.5) H18B(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 H14D(0.5) H14E(0.5) H14F(0.5) H17A(0.5) H17B(0.5) H17C(0.5) H17D(0.5)
 H17E(0.5) H17F(0.5) C19(0.5) H19A(0.5) H19B(0.5) C22(0.5) H22A(0.5) H22B(0.5)
 C21(0.5) H21A(0.5) H21B(0.5) C23(0.5) H23A(0.5) H23B(0.5) H20A(0.5) H20B(0.5)
 H20C(0.5) H20D(0.5) H20E(0.5) H20F(0.5) H24A(0.5) H24B(0.5) H24C(0.5)
 H24D(0.5) H24E(0.5) H24F(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C16(H16A,H16B), C15(H15A,H15B), C18(H18A,H18B), C19(H19A,
 H19B), C22(H22A,H22B), C21(H21A,H21B), C23(H23A,H23B)
3.b Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C14(H14D,H14E,H14F), C17(H17A,H17B,H17C), C17(H17D,H17E,
 H17F), C20(H20A,H20B,H20C), C20(H20D,H20E,H20F), C24(H24A,H24B,H24C), C24(H24D,
 H24E,H24F)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9A), C10(H10A), C11(H11A), C12(H12)
3.d Boron cage BH refined with riding coordinates:
 B1(H1A), B2(H2), B3(H3A), B4(H4A), B5(H5A), B6(H6A), B7(H7), B8(H8), B9(H9),
 B10(H10), B11(H11), B12(H12A), B13(H13), B14(H14), B15(H15), B16(H16),
 B17(H17), B18(H18), B19(H19), B20(H20), B21(H21), B22(H22)
;
_shelx_res_checksum              67393
_olex2_submission_special_instructions 'No special instructions were received'