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_7702119
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-14
_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                 109.935(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6962(13)
_cell_length_b                   15.9743(17)
_cell_length_c                   12.9143(13)
_cell_measurement_reflns_used    4942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.672
_cell_measurement_theta_min      2.550
_cell_volume                     2268.3(4)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19160
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.991
_diffrn_reflns_theta_min         2.249
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.467
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1300 before and 0.0839 after correction.
The Ratio of minimum to maximum transmission is 0.5533.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLE
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.032
_refine_diff_density_min         -1.037
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4434
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0457
_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^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3399
_reflns_number_total             4434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04457c2.cif
_cod_data_source_block           x83132
_cod_database_code               7702119
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.394
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Rigid bond restraints
 C31, C32, C33, C34, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C32 \\sim C34 \\sim C35: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C32) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C21'(H21'), C22'(H22'),
 C23'(H23'), C24'(H24'), C25'(H25')
;
_shelx_res_checksum              70972
_olex2_submission_special_instructions 'No special instructions were received'