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_7125031
_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         'C6 H18 B10 O2'
_chemical_formula_sum            'C6 H18 B10 O2'
_chemical_formula_weight         230.30
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-06-24 deposited with the CCDC.
2016-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.885(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7915(4)
_cell_length_b                   21.7000(13)
_cell_length_c                   8.0127(4)
_cell_measurement_reflns_used    1087
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      26.7790
_cell_measurement_theta_min      3.9560
_cell_volume                     1349.83(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -30.00   51.00   1.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.3571   57.0000  -30.0000 54

  2 omega    2.00   41.00   1.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946  -57.0000    0.0000 26

  3 omega   -9.00   90.00   1.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7946   77.0000 -120.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0696892000
_diffrn_orient_matrix_UB_12      -0.0185932000
_diffrn_orient_matrix_UB_13      0.0329348000
_diffrn_orient_matrix_UB_21      0.0518412000
_diffrn_orient_matrix_UB_22      0.0267131000
_diffrn_orient_matrix_UB_23      0.0133722000
_diffrn_orient_matrix_UB_31      -0.0282559000
_diffrn_orient_matrix_UB_32      0.0031293000
_diffrn_orient_matrix_UB_33      0.0814217000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0706
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5287
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.50
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2654
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0695
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+1.1514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1743
_refine_ls_wR_factor_ref         0.2008
_reflns_number_gt                1813
_reflns_number_total             2654
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc06200h2.cif
_cod_data_source_block           ck_256_2
_cod_database_code               7125031
_reflns_odcompleteness_completeness 99.65
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O2'-C5
 1.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq, Uanis(O2') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C5') \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: H6AA(0.78) H6AB(0.78) H6AC(0.78) H6BD(0.22) H6BE(0.22) H6BF(0.22)
 O2(0.78) C5(0.78) O2'(0.22) C5'(0.22)
5.a Me refined with riding coordinates:
 C6(H6AA,H6AB,H6AC), C6(H6BD,H6BE,H6BF)
5.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
5.c Boron cage BH refined with riding coordinates:
 B3(H3), B4(H4), B5(H5), B6(H6), B8(H8), B9(H9), B10(H10), B11(H11), B12(H12)
;
_olex2_date_sample_data_collection 2015-01-27
_olex2_submission_special_instructions 'No special instructions were received'