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_7116992
_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         'C12 H22 B10'
_chemical_formula_sum            'C12 H22 B10'
_chemical_formula_weight         274.39
_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'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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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_audit_update_record
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2015-01-15 deposited with the CCDC.
2015-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_formula_units_Z            4
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_cell_measurement_reflns_used    895
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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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_diffrn_ambient_temperature      294.12(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.995
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_diffrn_measurement_details
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  1 omega  -13.00   92.00   1.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946   19.0000  -90.0000 70

  2 omega   10.00   43.00   1.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  -77.0000  -90.0000 22
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
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_diffrn_orient_matrix_UB_13      0.0149296000
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_diffrn_orient_matrix_UB_23      0.0445673000
_diffrn_orient_matrix_UB_31      0.0737928000
_diffrn_orient_matrix_UB_32      -0.0032393000
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_diffrn_reflns_number            4243
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_diffrn_reflns_theta_full        25.500
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_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_T_max  1.00000
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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    1.105
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_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.114
_refine_diff_density_min         -0.127
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details
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 Flack x determined using 418 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
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_refine_ls_abs_structure_Flack   -2.1(10)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0736
_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^)+(0.0739P)^2^+0.3401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
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_reflns_Friedel_coverage         0.566
_reflns_Friedel_fraction_full    0.780
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_reflns_number_gt                1644
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc01331c2.cif
_cod_data_source_block           ck_209
_cod_database_code               7116992
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12)
2.c Boron cage BH refined with riding coordinates:
 B3(H3), B4(H4), B5(H5), B6(H6), B7(H7), B8(H8A), B10(H10A), B11(H11A),
 B12(H12A)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 1410857876.23
_olex2_submission_special_instructions 'No special instructions were received'