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_4126075
_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     dual
_audit_creation_date             2016-12-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                105.498(4)
_cell_angle_beta                 99.460(4)
_cell_angle_gamma                110.281(6)
_cell_formula_units_Z            8
_cell_length_a                   11.895(2)
_cell_length_b                   15.005(3)
_cell_length_c                   20.362(3)
_cell_measurement_reflns_used    6348
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.319
_cell_measurement_theta_min      2.203
_cell_volume                     3149.5(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_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            43355
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.311
_diffrn_reflns_theta_min         1.082
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  0.4901
_exptl_absorpt_correction_T_min  0.4611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0732 before and 0.0608 after correction.
The Ratio of minimum to maximum transmission is 0.9408.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         11320
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0657P)^2^+1.3944P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1682
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7581
_reflns_number_total             11320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04080_si_002.cif
_cod_data_source_block           p-1_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4126075
_olex2_refinement_description
;
1. 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
2.a Aromatic/amide H refined with riding coordinates:
 C5B(H5B), C1D(H1D), C5D(H5D), C1C(H1C), C5C(H5C), C1B(H1B), C3B(H3B),
 C1A(H1A), C5A(H5A), C3C(H3C), C3A(H3A), C3D(H3D)
2.b Idealised Me refined as rotating group:
 C8B(H8BA,H8BB,H8BC), C8C(H8CA,H8CB,H8CC), C8A(H8AA,H8AB,H8AC), C7D(H7DA,H7DB,
 H7DC), C7C(H7CA,H7CB,H7CC), C7B(H7BA,H7BB,H7BC), C8D(H8DA,H8DB,H8DC), C7A(H7AA,
 H7AB,H7AC)
2.c Boron cage BH refined with riding coordinates:
 C9D(H9D), C9B(H9B), C9A(H9A), C10D(H10D), C10B(H10G), C9C(H9C), C10C(H10E),
 C10A(H10B), B5D(H5DA), B2A(H2A), B7C(H7C), B10C(H10F), B3B(H3BA), B3C(H3CA),
 B3A(H3AA), B5B(H5BA), B5C(H5CA), B2C(H2C), B3D(H3DA), B4D(H4D), B4A(H4A),
 B9A(H9AA), B4C(H4C), B9D(H9DA), B2D(H2D), B2B(H2B), B4B(H4B), B5A(H5AA),
 B10A(H10C), B8C(H8C), B7D(H7D), B8D(H8D), B10D(H10A), B9C(H9CA), B8B(H8B),
 B7A(H7A), B9B(H9BA), B8A(H8A), B10B(H10H), B7B(H7B), B6B(H6B), B6C(H6C),
 B6D(H6D), B6A(H6A)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'