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_1564521
_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         'C14 H19 B10 F1 S'
_chemical_formula_sum            'C14 H19 B10 F S'
_chemical_formula_weight         346.614
_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'
_symmetry_Int_Tables_number      14
_audit_creation_date             2020-12-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2020-12-10 deposited with the CCDC.	2021-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.877(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5577(11)
_cell_length_b                   27.779(5)
_cell_length_c                   10.1198(10)
_cell_measurement_reflns_used    9317
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.520
_cell_measurement_theta_min      2.519
_cell_volume                     1810.4(5)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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 0.9997
_diffrn_measured_fraction_theta_max 0.9983
_diffrn_measurement_device_type  'Bruker D8 Venture AgMo 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  0.0240
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            63225
_diffrn_reflns_point_group_measured_fraction_full 0.9997
_diffrn_reflns_point_group_measured_fraction_max 0.9983
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         31.53
_diffrn_reflns_theta_min         2.18
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.7679
_exptl_absorpt_correction_T_min  0.7489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0792 before and 0.0395 after correction.
The Ratio of minimum to maximum transmission is 0.9753.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             712.711
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.268
_exptl_crystal_size_min          0.263
_refine_diff_density_max         0.4257
_refine_diff_density_min         -0.2445
_refine_diff_density_rms         0.0481
_refine_ls_d_res_high            0.6795
_refine_ls_d_res_low             9.3572
_refine_ls_goodness_of_fit_ref   1.0881
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    31
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0881
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.1331
_refine_ls_shift/su_mean         0.0048
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.5238P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0806
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              40
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                5512
_reflns_number_total             6029
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1sc02905c2.cif
_cod_data_source_block           mo_1222_CG_0m
_cod_original_cell_volume        1810.3(5)
_cod_database_code               1564521
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
2. Others
 Sof(H2)=Sof(F1B)=1-FVAR(1)
 Sof(F1A)=Sof(H6)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'