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_7121047
_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         'C26 H58 B11 Li2 N O6'
_chemical_formula_sum            'C26 H58 B11 Li2 N O6'
_chemical_formula_weight         613.52
_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             2017-03-20
_audit_creation_method
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Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-07-01 deposited with the CCDC.
2017-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                87.873(9)
_cell_angle_beta                 74.958(10)
_cell_angle_gamma                64.502(12)
_cell_formula_units_Z            2
_cell_length_a                   10.4350(11)
_cell_length_b                   10.8304(13)
_cell_length_c                   18.597(2)
_cell_measurement_reflns_used    2152
_cell_measurement_temperature    170
_cell_measurement_theta_max      29.3168
_cell_measurement_theta_min      3.3998
_cell_volume                     1825.3(4)
_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)
;
_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)
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -66.00   42.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8433  -77.0000  150.0000 108

  2 omega  -65.00   35.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8433  -38.0000   30.0000 100

  3 omega  -47.00  -16.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       10.8433  140.0000   52.0000 31

  4 omega  -72.00    0.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.5621  129.0000 -119.0000 72
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0309558000
_diffrn_orient_matrix_UB_12      -0.0345311000
_diffrn_orient_matrix_UB_13      -0.0363720000
_diffrn_orient_matrix_UB_21      -0.0255374000
_diffrn_orient_matrix_UB_22      0.0640350000
_diffrn_orient_matrix_UB_23      -0.0156704000
_diffrn_orient_matrix_UB_31      0.0671336000
_diffrn_orient_matrix_UB_32      0.0032818000
_diffrn_orient_matrix_UB_33      -0.0016595000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0878
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11790
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.416
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90600
_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_colour_primary    colourless
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       plate
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         11790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1590
_refine_ls_R_factor_gt           0.0844
_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^)+(0.1376P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2120
_refine_ls_wR_factor_ref         0.2479
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5996
_reflns_number_total             11790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07724f2.cif
_cod_data_source_block           t2_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7121042--7121048.cif.'
_cod_database_code               7121047
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'c10 h10 n2 o8 b1 Li1'
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.972
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.4096(17)
 0.5904(17)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C6) = Uanis(C6A)
4. Others
 Sof(H5BC)=Sof(H5BD)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=1-FVAR(1)
 Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H5AA)=Sof(H5AB)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C5(H5AA,H5AB), C5(H5BC,H5BD), C4(H4A,H4B), C3(H3A,H3B), C7(H7A,
 H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
  C13(H13A,H13B), C14(H14A,H14B), C18(H18A,H18B), C17(H17A,H17B), C16(H16A,
 H16B), C15(H15A,H15B), C22(H22A,H22B), C21(H21A,H21B), C20(H20A,H20B),
 C19(H19A,H19B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
  C6A(H6AA,H6AB)
5.b Boron cage BH refined with riding coordinates:
 B1(H1), B2(H2), B3(H3), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8), B9(H9),
 B10(H10)
;
_shelx_res_checksum              55118
_olex2_submission_special_instructions 'No special instructions were received'