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_7121043
_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         'C3 H12 B11 O4, C8 H20 N'
_chemical_formula_sum            'C11 H32 B11 N O4'
_chemical_formula_weight         361.28
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-11 deposited with the CCDC.
2017-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3385(9)
_cell_length_b                   12.3385(9)
_cell_length_c                   13.745(2)
_cell_measurement_reflns_used    1418
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6145
_cell_measurement_theta_min      3.2956
_cell_volume                     2092.5(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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
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      293.15
_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  -36.00   52.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.5621   38.0000  -90.0000 88

  2 omega  -80.00   13.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.5621  -77.0000    0.0000 93

  3 omega  -83.00   12.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.5621  -38.0000   90.0000 95
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0570372000
_diffrn_orient_matrix_UB_12      0.0038448000
_diffrn_orient_matrix_UB_13      -0.0052940000
_diffrn_orient_matrix_UB_21      -0.0031440000
_diffrn_orient_matrix_UB_22      0.0294593000
_diffrn_orient_matrix_UB_23      0.0442577000
_diffrn_orient_matrix_UB_31      0.0062728000
_diffrn_orient_matrix_UB_32      0.0492156000
_diffrn_orient_matrix_UB_33      -0.0260381000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6595
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.344
_diffrn_reflns_theta_max         25.344
_diffrn_reflns_theta_min         3.302
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82111
_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    1.147
_exptl_crystal_description       needle
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.032
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         994
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0723P)^2^+0.9610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1529
_reflns_Friedel_coverage         0.000
_reflns_number_gt                777
_reflns_number_total             994
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07724f2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7121042--7121048.cif.'
_cod_database_code               7121043
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'c10 h10 n2 o8 B1'
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.972
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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,H,H,H) groups
2. Shared sites
{C1, B1A}
3. Restrained distances
 O2-H2
 0.83 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(B1A)
5. Others
 Fixed Sof: C1(0.25) B1A(0.25) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5)
 H4B(0.5) H5AA(0.5) H5AB(0.5) H5AC(0.5) H5BD(0.5) H5BE(0.5) H5BF(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B)
6.b Me refined with riding coordinates:
 C5(H5AA,H5AB,H5AC), C5(H5BD,H5BE,H5BF)
;
_shelx_res_checksum              50096
_olex2_submission_special_instructions 'No special instructions were received'