Palladium catalyzed/silver tuned selective mono-/tetra-acetoxylation of o-carboranes via B-H activation.
Cao, Ke; Xu, Tao-Tao; Wu, Ji; Jiang, Linhai; Yang, Junxiao; Chemical communications (Cambridge, England) 52 (2016) 11446–11449; doi:10.1039/c6cc06200h

data_7125028
_publ_section_title
;
 Palladium catalyzed/silver tuned selective mono-/tetra-acetoxylation of
 o-carboranes via B-H activation.
;
_journal_issue                   76
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11446
_journal_page_last               11449
_journal_paper_doi               10.1039/c6cc06200h
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C12 H24 B10 O8'
_chemical_formula_sum            'C12 H24 B10 O8'
_chemical_formula_weight         404.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-03-17 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.058(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7899(6)
_cell_length_b                   13.5842(4)
_cell_length_c                   13.7280(7)
_cell_measurement_reflns_used    1483
_cell_measurement_temperature    294.96(10)
_cell_measurement_theta_max      23.2310
_cell_measurement_theta_min      3.8210
_cell_volume                     2132.78(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.96(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   -5.00   91.00   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   38.0000  150.0000 80

  2 omega  -13.00   17.00   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000    0.0000 25

  3 omega   -3.00   36.60   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000  -60.0000 33

  4 omega  -41.00   32.20   1.2000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000 -180.0000 61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0325756000
_diffrn_orient_matrix_UB_12      0.0007382000
_diffrn_orient_matrix_UB_13      -0.0371825000
_diffrn_orient_matrix_UB_21      -0.0527686000
_diffrn_orient_matrix_UB_22      0.0008034000
_diffrn_orient_matrix_UB_23      -0.0381098000
_diffrn_orient_matrix_UB_31      0.0003698000
_diffrn_orient_matrix_UB_32      0.0522065000
_diffrn_orient_matrix_UB_33      0.0011161000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8958
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         3.367
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4190
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0772
_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^)+(0.1082P)^2^+0.8532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1995
_refine_ls_wR_factor_ref         0.2483
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2285
_reflns_number_total             4190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06200h2.cif
_cod_data_source_block           wj_494_2
_cod_original_cell_volume        2132.79(18)
_cod_database_code               7125028
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq, Uanis(O8') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Fixed Sof: O8(0.5) O8'(0.5)
4.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C6(H6A,H6B,H6C)
4.b Boron cage BH refined with riding coordinates:
 B5(H5), B3(H3), B4(H4), B6(H6), B11(H11), B7(H7)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-12-07
_olex2_submission_special_instructions 'No special instructions were received'