Cage-walking: Vertex Differentiation by Palladium-Catalyzed Isomerization of B(9)-Bromo-meta-Carborane.
Dziedzic, Rafal Miroslaw; Martin, Joshua L.; Axtell, Jonathan C.; Saleh, Liban M. A.; Ong, Ta-Chung; Yang, Yun-Fang; Messina, Marco S.; Rheingold, Arnold L.; Houk, Kendall N.; Spokoyny, Alexander M.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b04080

data_4126073
_publ_section_title
;
 Cage-walking: Vertex Differentiation by Palladium-Catalyzed Isomerization
 of B(9)-Bromo-meta-Carborane.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b04080
_journal_year                    2017
_chemical_formula_moiety         'C10 H20 B10 O'
_chemical_formula_sum            'C10 H20 B10 O'
_chemical_formula_weight         264.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                104.277(3)
_cell_angle_beta                 99.855(3)
_cell_angle_gamma                110.189(2)
_cell_formula_units_Z            8
_cell_length_a                   11.7531(8)
_cell_length_b                   14.5081(9)
_cell_length_c                   20.6459(17)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.86
_cell_volume                     3072.4(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            52993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.061
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  0.2602
_exptl_absorpt_correction_T_min  0.2262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0800 before and 0.0542 after correction.
The Ratio of minimum to maximum transmission is 0.8693.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         10781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+2.0308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1660
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8445
_reflns_number_total             10781
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04080_si_002.cif
_cod_data_source_block           spok64_a
_cod_database_code               4126073
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.2091(13)
 0.7909(13)
2. 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
3.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C4A(H4A), C6A(H6A), C2C(H2C), C4C(H4C), C6C(H6C), C2B(H2B),
 C4B(H4B), C6B(H6B), C2D(H2D), C4D(H4D), C6D(H6D)
3.b Idealised Me refined as rotating group:
 C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C7C(H7CA,H7CB,H7CC), C8C(H8CA,H8CB,
 H8CC), C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC), C7D(H7DA,H7DB,H7DC), C8D(H8DA,
 H8DB,H8DC)
3.c Boron cage BH refined with riding coordinates:
 C9A(H9A), C10A(H10A), B2A(H2AA), B3A(H3A), B4A(H4AA), B5A(H5A), B6A(H6AA),
 B7A(H7A), B8A(H8A), B9A(H9AA), B10A(H10B), C9C(H9C), C10C(H10C), B2C(H2CA),
 B3C(H3C), B4C(H4CA), B5C(H5C), B6C(H6CA), B7C(H7C), B8C(H8C), B9C(H9CA),
 B10C(H10D), C9B(H9B), C10B(H10E), B2B(H2BA), B3B(H3B), B4B(H4BA), B5B(H5B),
 B6B(H6BA), B7B(H7B), B8B(H8B), B9B(H9BA), B10B(H10F), C9D(H9D), C10D(H10G),
 B1D(H1D), B3D(H3D), B4D(H4DA), B5D(H5D), B6D(H6DA), B7D(H7D), B8D(H8D),
 B9D(H9DA), B10D(H10H)
;
_olex2_submission_special_instructions 'No special instructions were received'