Palladium catalyzed selective mono-arylation of o-carboranes via B-H activation
Ke Cao; Yawen Huang; Junxiao Yang; Ji Wu; Chem.Commun. 51 (2015) 7257–; doi:10.1039/C5cc01331C

data_7116995
_publ_section_title
;
 Palladium catalyzed selective mono-arylation of o-carboranes via B-H
 activation
;
_journal_name_full               Chem.Commun.
_journal_page_first              7257
_journal_paper_doi               10.1039/C5cc01331C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C10 H20 B10'
_chemical_formula_sum            'C10 H20 B10'
_chemical_formula_weight         248.36
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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Olex2 1.2
(compiled 2015.01.12 svn.r3133 for OlexSys, GUI svn.r4987)
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2015-01-15 deposited with the CCDC.
2015-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      294.17(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
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  1 omega   72.00   97.20   1.2000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.9508 -178.0000  120.0000 21

  2 omega  -14.00   36.40   1.2000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.9508  -99.0000   90.0000 42

  3 omega  -49.00   33.80   1.2000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       19.9508  -19.0000  120.0000 69
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
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_diffrn_orient_matrix_UB_12      -0.0583454000
_diffrn_orient_matrix_UB_13      -0.0026349000
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_diffrn_orient_matrix_UB_23      0.0432273000
_diffrn_orient_matrix_UB_31      -0.0182613000
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_diffrn_orient_matrix_UB_33      0.0160114000
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_diffrn_reflns_av_R_equivalents  0.0974
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_diffrn_reflns_Laue_measured_fraction_full 0.993
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_diffrn_reflns_point_group_measured_fraction_full 0.993
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_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         26.020
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_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.050
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71458
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.32
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_refine_diff_density_min         -0.168
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_refine_ls_extinction_coef       0.0019(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.2706
_refine_ls_R_factor_gt           0.1195
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                900
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_cod_data_source_file            c5cc01331c2.cif
_cod_data_source_block           ck_194
_cod_original_cell_volume        3091.4(9)
_cod_database_code               7116995
_reflns_odcompleteness_completeness 99.36
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_olex2_refinement_description
;
1. 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
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
2.c Boron cage BH refined with riding coordinates:
 B3(H3), B4(H4), B5(H5), B6(H6A), B7(H7A), B8(H8A), B10(H10A), B11(H11),
 B12(H12)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 1410860405.72
_olex2_submission_special_instructions 'No special instructions were received'