Pyridyl-Directed Cp*Rh(III)-Catalyzed B(3)-H Acyloxylation of o-Carborane.
Li, Chun-Xiao; Zhang, Hao-Yun; Wong, Tsz-Yung; Cao, Hou-Ji; Yan, Hong; Lu, Chang-Sheng; Organic letters 19 (2017) 5178–5181; doi:10.1021/acs.orglett.7b02450

data_1547264
_publ_section_title
;
 Pyridyl-Directed Cp*Rh(III)-Catalyzed B(3)-H Acyloxylation of
 o-Carborane.
;
_journal_issue                   19
_journal_name_full               'Organic letters'
_journal_page_first              5178
_journal_page_last               5181
_journal_paper_doi               10.1021/acs.orglett.7b02450
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C18 H29 B10 N O4'
_chemical_formula_weight         431.52
_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
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                84.083(7)
_cell_angle_beta                 81.585(7)
_cell_angle_gamma                75.119(7)
_cell_formula_units_Z            4
_cell_length_a                   10.435(5)
_cell_length_b                   10.813(5)
_cell_length_c                   21.420(9)
_cell_measurement_reflns_used    4001
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.68
_cell_measurement_theta_min      2.36
_cell_volume                     2305.3(18)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0810
_diffrn_reflns_av_unetI/netI     0.1277
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16811
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         0.963
_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             904.0
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         8023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0900
_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^)+(0.1803P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2534
_refine_ls_wR_factor_ref         0.2982
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5203
_reflns_number_total             8023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02450_si_002.cif
_cod_data_source_block           222_a
_cod_depositor_comments
'Adding full bibliography for 1547262--1547264.cif.'
_cod_original_cell_volume        2305.1(17)
_cod_database_code               1547264
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.968
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              91626
_shelx_hkl_checksum              19025