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_7125029
_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         'C20 H32 B10 O8'
_chemical_formula_sum            'C20 H32 B10 O8'
_chemical_formula_weight         508.55
_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   geom
_audit_creation_date             2016-01-06
_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                98.928(5)
_cell_angle_beta                 92.479(5)
_cell_angle_gamma                90.262(5)
_cell_formula_units_Z            4
_cell_length_a                   12.7205(9)
_cell_length_b                   13.3454(8)
_cell_length_c                   16.3950(11)
_cell_measurement_reflns_used    2144
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.7010
_cell_measurement_theta_min      3.4970
_cell_volume                     2746.7(3)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -13.00   25.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9916  -99.0000  120.0000 38

  2 omega  -13.00   14.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9916  -99.0000  -60.0000 27

  3 omega  -46.00   32.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  -38.0000  -90.0000 78

  4 omega  -30.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291    0.0000  -60.0000 122

  5 omega   38.00   83.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       20.4291  178.0000 -150.0000 45

  6 omega  -68.00  -23.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9916  125.0000    5.0000 45

  7 omega  -80.00  -38.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9916  146.0000  171.0000 42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
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_diffrn_orient_matrix_UB_11      0.0251149000
_diffrn_orient_matrix_UB_12      0.0266209000
_diffrn_orient_matrix_UB_13      0.0365165000
_diffrn_orient_matrix_UB_21      0.0382883000
_diffrn_orient_matrix_UB_22      0.0190358000
_diffrn_orient_matrix_UB_23      -0.0240037000
_diffrn_orient_matrix_UB_31      -0.0319172000
_diffrn_orient_matrix_UB_32      0.0427073000
_diffrn_orient_matrix_UB_33      -0.0034729000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.1597
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19409
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.993
_diffrn_reflns_theta_min         3.389
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96489
_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    1.230
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.670
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_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         10785
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.2397
_refine_ls_R_factor_gt           0.1084
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1472P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2601
_refine_ls_wR_factor_ref         0.3649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3809
_reflns_number_total             10785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc06200h2.cif
_cod_data_source_block           wj_533_4
_cod_original_cell_volume        2746.8(3)
_cod_database_code               7125029
_shelxl_version_number           2013-2
_reflns_odcompleteness_completeness 99.80
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O8') \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O6') \\sim Ueq, Uanis(O8)
\\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O12') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: O6(0.65) O8(0.8) O6'(0.35) O8'(0.2) O12(0.65) O12'(0.35)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C29(H29A,H29B), C30(H30A,H30B),
 C31(H31A,H31B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C24(H24), C25(H25), C26(H26),
 C27(H27), C28(H28)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C)
4.d Boron cage BH refined with riding coordinates:
 B3(H3), B4(H4A), B5(H5A), B6(H6A), B7(H7A), B11(H11), B13(H13), B14(H14),
 B15(H15), B16(H16), B17(H17), B21(H21)
;
_shelx_res_checksum              98047
_olex2_submission_special_instructions 'No special instructions were received'