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_7128671
_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         'C16 H21 B10 I'
_chemical_formula_sum            'C16 H21 B10 I'
_chemical_formula_weight         448.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-02
_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                 99.1390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.4458(2)
_cell_length_b                   12.7974(2)
_cell_length_c                   14.4835(3)
_cell_measurement_reflns_used    9676
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.905
_cell_measurement_theta_min      3.01
_cell_volume                     2094.56(7)
_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      170.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23832
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.910
_diffrn_reflns_theta_min         3.989
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.008
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1159 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.7063. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.095
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3963
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0251P)^2^+4.2702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3808
_reflns_number_total             3963
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03449a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7128668--7128673.cif.'
_cod_database_code               7128671
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.567
_shelx_estimated_absorpt_t_min   0.380
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2.a 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)
2.b Boron cage BH refined with riding coordinates:
 C1(H1), C2(H2), B3(H3), B6(H6A), B7(H7A), B8(H8A), B9(H9A), B10(H10A),
 B11(H11), B12(H12A)
;
_shelx_res_checksum              70852
_olex2_submission_special_instructions 'No special instructions were received'