Regioselective B2–6 penta-iodination of the [CB11H12]– monocarborane cluster by palladium catalysis
Lin, Chuhao; Jin, Yujie; Sun, Jizeng; Ye, Zehua; Chen, Tao; Liu, Jiyong; Duttwyler, Simon; Dalton Transactions  (2023) –; doi:10.1039/D3DT02275G

data_7713632
_publ_section_title
;
 Regioselective B2--6 penta-iodination of the [CB11H12]-- monocarborane
 cluster by palladium catalysis
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02275G
_journal_year                    2023
_chemical_formula_moiety         'C7 H11 B11 I5, C8 H20 N'
_chemical_formula_sum            'C15 H31 B11 I5 N'
_chemical_formula_weight         978.82
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-09 deposited with the CCDC.	2023-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                100.782(2)
_cell_angle_beta                 98.898(2)
_cell_angle_gamma                94.691(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8044(5)
_cell_length_b                   11.8241(6)
_cell_length_c                   13.6777(7)
_cell_measurement_reflns_used    9768
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      2.39
_cell_volume                     1528.85(14)
_computing_cell_refinement       'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_data_collection       'Bruker Instrument Service vV6.2.14'
_computing_data_reduction        'SAINT V8.40B (Bruker Nano, Inc., 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'zju Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            53432
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.124
_diffrn_reflns_theta_min         2.093
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.093
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1014 before and 0.0520 after correction.
The Ratio of minimum to maximum transmission is 0.6681.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.126
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.406
_refine_diff_density_min         -1.641
_refine_diff_density_rms         0.100
_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     293
_refine_ls_number_reflns         6760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0205P)^2^+4.5972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0742
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6176
_reflns_number_total             6760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02275g2.cif
_cod_data_source_block           mo_221102_lch_12_ph_0m
_cod_database_code               7713632
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.557
_shelx_estimated_absorpt_t_min   0.224
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C12(H12A,H12B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7A), C5(H5), C4(H4), C6(H6A)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C)
2.d Boron cage BH refined with riding coordinates:
 C1(H1), B10(H10), B6(H6), B9(H9), B7(H7), B8(H8)
;
_shelx_res_checksum              32290
_olex2_submission_special_instructions 'No special instructions were received'