Pd-catalyzed selective tetrafunctionalization of diiodo-<i>o</i>-carboranes.
Ge, Yixiu; Qiu, Zaozao; Xie, Zuowei; Chemical communications (Cambridge, England) 57 (2021) 8071–8074; doi:10.1039/d1cc03449a

data_7128673
_publ_section_title
;
 Pd-catalyzed selective tetrafunctionalization of
 diiodo-<i>o</i>-carboranes.
;
_journal_issue                   65
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8071
_journal_page_last               8074
_journal_paper_doi               10.1039/d1cc03449a
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C36 H40 B10'
_chemical_formula_sum            'C36 H40 B10'
_chemical_formula_weight         580.78
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-21 deposited with the CCDC.	2021-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.1510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5313(3)
_cell_length_b                   21.5989(3)
_cell_length_c                   17.6102(3)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.93
_cell_measurement_theta_min      2.83
_cell_volume                     6668.48(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_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      170.04
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            72533
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.961
_diffrn_reflns_theta_min         2.824
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1293 before and 0.0741 after correction. The Ratio of minimum to maximum transmission is 0.7115. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         12640
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0595
_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^)+(0.0596P)^2^+4.0232P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1561
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9142
_reflns_number_total             12640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03449a2.cif
_cod_data_source_block           8g
_cod_depositor_comments
'Adding full bibliography for 7128668--7128673.cif.'
_cod_database_code               7128673
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.958
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 C17, B4, C34, B7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3.a Ternary CH refined with riding coordinates:
 C17(H17), C34(H34), C17A(H17A), C34A(H34A)
3.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B), C35(H35A,H35B), C36(H36A,H36B), C18A(H18C,
 H18D), C19A(H19C,H19D), C35A(H35C,H35D), C36A(H36C,H36D)
3.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C14(H14), C15(H15), C16(H16), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C4A(H4A),
 C6A(H6A), C7A(H7A), C8A(H8AA), C9A(H9AA), C10A(H10B), C12A(H12B), C13A(H13A),
 C14A(H14A), C15A(H15A), C16A(H16A), C21A(H21A), C23A(H23A), C24A(H24A),
 C25A(H25A), C26A(H26A), C27A(H27A), C29A(H29A), C30A(H30A), C31A(H31A),
 C32A(H32A), C33A(H33A)
3.d Boron cage BH refined with riding coordinates:
 C1(H1), C2(H2), B5(H5), B8(H8A), B9(H9A), B10(H10A), B11(H11), B12(H12A),
 C1A(H1A), C2A(H2A), B5A(H5A), B8A(H8AB), B9A(H9AB), B10A(H10C), B11A(H11A),
 B12A(H12C)
;
_shelx_res_checksum              58166
_olex2_submission_special_instructions 'No special instructions were received'