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_7702123
_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         'C4 H20.52 B18, 2(C10 H16 N)'
_chemical_formula_sum            'C24 H54 B18 N2'
_chemical_formula_weight         565.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-12-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-12-15 deposited with the CCDC.
2016-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                116.225(6)
_cell_angle_beta                 101.483(7)
_cell_angle_gamma                104.113(5)
_cell_formula_units_Z            1
_cell_length_a                   8.8436(12)
_cell_length_b                   10.5897(11)
_cell_length_c                   11.103(2)
_cell_measurement_reflns_used    3097
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      2.54
_cell_volume                     846.5(2)
_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 0.983
_diffrn_measured_fraction_theta_max 0.968
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11069
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.333
_diffrn_reflns_theta_min         2.185
_exptl_absorpt_coefficient_mu    0.055
_exptl_absorpt_correction_T_max  0.9978
_exptl_absorpt_correction_T_min  0.9772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4082
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0592P)^2^+0.2382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2951
_reflns_number_total             4082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04457c2.cif
_cod_data_source_block           229a
_cod_database_code               7702123
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C8, B8}
{C11, B11}
{B12, C12}
3. Uiso/Uaniso restraints and constraints
Uanis(B12) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.004
Uanis(C8) = Uanis(B8)
Uanis(C11) = Uanis(B11)
Uanis(B12) = Uanis(C12)
4. Others
 Fixed Sof: H6(0.66) B8(0.15) C8(0.51) H8(0.66) H10A(0.6) B11(0.65) C11(0.29)
 H11(0.94) B12(0.2) H12(0.4) C12(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C103(H10K,H10L)
5.b Aromatic/amide H refined with riding coordinates:
 C105(H105), C106(H106), C107(H107), C108(H108), C109(H109)
5.c Idealised Me refined as rotating group:
 C100(H10B,H10C,H10D), C101(H10E,H10F,H10G), C102(H10H,H10I,H10J)
;
_shelx_shelxl_version_number     2014/7
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'