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_7128670
_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         'C30 H30 B10 I2'
_chemical_formula_sum            'C30 H30 B10 I2'
_chemical_formula_weight         752.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-23
_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                 133.6760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.0553(4)
_cell_length_b                   10.9373(2)
_cell_length_c                   17.0806(3)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      55.01
_cell_measurement_theta_min      3.20
_cell_volume                     3250.25(11)
_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      170.0
_diffrn_measured_fraction_theta_full 0.999
_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  0.0555
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16868
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.987
_diffrn_reflns_theta_min         4.154
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.273
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.3726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1508 before and 0.0782 after correction. The Ratio of minimum to maximum transmission is 0.4963. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.238
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+13.0924P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2697
_reflns_number_total             3099
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03449a2.cif
_cod_data_source_block           5c
_cod_depositor_comments
'Adding full bibliography for 7128668--7128673.cif.'
_cod_original_cell_volume        3250.24(11)
_cod_database_code               7128670
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.578
_shelx_estimated_absorpt_t_min   0.308
_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:
 C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15)
2.b Boron cage BH refined with riding coordinates:
 C1(H1), B3(H3A), B4(H4), B5(H5A)
;
_shelx_res_checksum              28262
_olex2_submission_special_instructions 'No special instructions were received'