Electrooxidative o-Carborane Chalcogenations Without Directing Groups: Cage Activation by Copper Catalysis at Room Temperature
Yang, Long; Jei, Becky Bongsuiru; Scheremetjew, Alexej; Yuan, Binbin; Stückl, A Claudia; Ackermann, Lutz; Chemical Science  (2021) –; doi:10.1039/D1SC02905C

data_1564522
_publ_section_title
;
 Electrooxidative o-Carborane Chalcogenations Without Directing Groups:
 Cage Activation by Copper Catalysis at Room Temperature
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02905C
_journal_year                    2021
_chemical_formula_moiety         'C26 H27 B10 N S'
_chemical_formula_sum            'C26 H27 B10 N S'
_chemical_formula_weight         493.819
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2021-02-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-02-19 deposited with the CCDC.	2021-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.765(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2524(16)
_cell_length_b                   12.5432(12)
_cell_length_c                   14.6594(17)
_cell_measurement_reflns_used    9925
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.598
_cell_measurement_theta_min      2.501
_cell_volume                     2607.4(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9943
_diffrn_measurement_device_type  'Bruker D8 Venture CuMo Dual Source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.9989
_diffrn_reflns_Laue_measured_fraction_max 0.9943
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            64187
_diffrn_reflns_point_group_measured_fraction_full 0.9989
_diffrn_reflns_point_group_measured_fraction_max 0.9943
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         29.62
_diffrn_reflns_theta_min         2.10
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8662
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1270 before and 0.0495 after correction.
The Ratio of minimum to maximum transmission is 0.8662.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             1024.773
_exptl_crystal_size_max          0.563
_exptl_crystal_size_mid          0.352
_exptl_crystal_size_min          0.202
_refine_diff_density_max         0.5241
_refine_diff_density_min         -0.3481
_refine_diff_density_rms         0.0570
_refine_ls_d_res_high            0.7189
_refine_ls_d_res_low             9.6922
_refine_ls_goodness_of_fit_ref   1.0666
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    44
_refine_ls_number_parameters     373
_refine_ls_number_reflns         7308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0666
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.0741
_refine_ls_shift/su_mean         0.0022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0544P)^2^+1.4256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -19
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -12
_reflns_number_gt                6824
_reflns_number_total             7308
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1sc02905c2.cif
_cod_data_source_block           mo_1274_CG_0m
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               1564522
_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), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24), C25(H25),
  C26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'