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_7702117
_publ_section_title
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 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, C2 H3 N'
_chemical_formula_sum            'C16 H33 B18 Co2 N'
_chemical_formula_weight         551.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9085(6)
_cell_length_b                   13.5333(10)
_cell_length_c                   20.8343(16)
_cell_measurement_reflns_used    874
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      15.70
_cell_measurement_theta_min      2.49
_cell_volume                     2511.8(3)
_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)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.998
_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  0.0860
_diffrn_reflns_av_unetI/netI     0.1176
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            26419
_diffrn_reflns_point_group_measured_fraction_full 0.554
_diffrn_reflns_point_group_measured_fraction_max 0.568
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.761
_diffrn_reflns_theta_min         2.467
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'TWINABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1202 before and 0.0853 after correction. The Ratio of minimum to maximum transmission is 0.7824. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
No quotients, so Flack parameter determined by classical intensity fit
;
_refine_ls_abs_structure_Flack   0.34(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         2873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0256P)^2^+3.0532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.1007
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    0.000
_reflns_Friedel_fraction_max     0.000
_reflns_number_gt                2163
_reflns_number_total             2873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04457c2.cif
_cod_data_source_block           4976o
_cod_database_code               7702117
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.618(3) 0.382(3)
2. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.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')
3.b Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              1436
_olex2_submission_special_instructions 'No special instructions were received'