Double deboronation and homometalation of 1,1'-bis(ortho-carborane).
Thiripuranathar, Gobika; Chan, Antony P. Y.; Mandal, Dipendu; Man, Wing Y.; Argentari, Mario; Rosair, Georgina M.; Welch, Alan J.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1811–1821; doi:10.1039/c6dt04457c

data_7702121
_publ_section_title
;
 Double deboronation and homometalation of 1,1'-bis(ortho-carborane).
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1811
_journal_page_last               1821
_journal_paper_doi               10.1039/c6dt04457c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C14 H30 B18 Co2'
_chemical_formula_sum            'C14 H30 B18 Co2'
_chemical_formula_weight         510.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-11-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-11-11 deposited with the CCDC.
2016-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6943(5)
_cell_length_b                   13.8151(5)
_cell_length_c                   14.4745(6)
_cell_measurement_reflns_used    11042
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5380
_cell_measurement_theta_min      2.6430
_cell_volume                     2338.47(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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    -31.00  77.00   1.00    5.00    --  -13.00  72.00  90.00  108
  2  \w    -67.00  23.00   1.00    5.00    --  -13.00 -72.00 -30.00   90
  3  \w    -67.00  23.00   1.00    5.00    --  -13.00 -72.00 150.00   90
  4  \w    -78.00  -8.00   1.00    5.00    --  -13.00   0.00 150.00   70
  5  \w      3.00  23.00   1.00    5.00    --  -13.00 -72.00-180.00   20
  6  \w    -95.00  14.00   1.00    5.00    --  -13.00 -54.00 150.00  109
;
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ 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      -0.0153349500
_diffrn_orient_matrix_UB_12      -0.0496703500
_diffrn_orient_matrix_UB_13      -0.0000166000
_diffrn_orient_matrix_UB_21      0.0069610000
_diffrn_orient_matrix_UB_22      -0.0015715000
_diffrn_orient_matrix_UB_23      0.0486206000
_diffrn_orient_matrix_UB_31      -0.0583090000
_diffrn_orient_matrix_UB_32      0.0129241000
_diffrn_orient_matrix_UB_33      0.0058092000
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13750
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         2.681
_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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0224
_refine_ls_R_factor_gt           0.0216
_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^)+(0.0316P)^2^+3.0113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1360
_reflns_number_total             1399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04457c2.cif
_cod_data_source_block           2016ncs0723
_cod_original_cell_volume        2338.47(17)
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7702121
_chemical_oxdiff_formula         'C14 H30 B18 Co2'
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Shared sites
{C1, B1}
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(B1)
4. Others
 Fixed Sof: C1(0.5) B1(0.5)
5.a Ternary CH refined with riding coordinates:
 C23(H23), C24(H24), C25(H25)
;
_shelx_res_checksum              64970
_shelx_shelxl_version_number     2014/7
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.180
_oxdiff_exptl_absorpt_empirical_full_min 0.506