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_4126079
_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 H15 B10 N O2'
_chemical_formula_sum            'C10 H15 B10 N O2'
_chemical_formula_weight         289.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.5400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.08280(10)
_cell_length_b                   7.54140(10)
_cell_length_c                   27.6234(5)
_cell_measurement_reflns_used    2806
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.08
_cell_measurement_theta_min      3.22
_cell_volume                     1465.88(4)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0964
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            4703
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.043
_diffrn_reflns_theta_min         3.221
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.1776
_exptl_absorpt_correction_T_min  0.1453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         2596
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0580
_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^)+(0.1075P)^2^+0.4351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1585
_refine_ls_wR_factor_ref         0.1657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2220
_reflns_number_total             2596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04080_si_002.cif
_cod_data_source_block           spok37_a
_cod_database_code               4126079
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.879
_olex2_refinement_description
;
1. Restrained distances
 C2-H2
 0.9 with sigma of 0.001
;
_shelx_res_checksum              39605
_shelx_hkl_checksum              75529
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'