Regioselective B(3)-H bond activation based on an o-carboranyl dithiocarboxylate ligand and its derivatives.
Yuan, Run-Ze; Cui, Peng-Fei; Guo, Shu-Ting; Jin, Guo-Xin; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1060–1068; doi:10.1039/d0dt03832f

data_7705931
_publ_section_title
;
 Regioselective B(3)-H bond activation based on an o-carboranyl
 dithiocarboxylate ligand and its derivatives.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1060
_journal_page_last               1068
_journal_paper_doi               10.1039/d0dt03832f
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C3 H11 B10 S2, C24 H20 P'
_chemical_formula_sum            'C27 H31 B10 P S2'
_chemical_formula_weight         558.70
_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             2020-07-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2020-11-04 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.346(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5156(5)
_cell_length_b                   8.7984(4)
_cell_length_c                   28.8360(12)
_cell_measurement_reflns_used    8390
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      71.62
_cell_measurement_theta_min      3.12
_cell_volume                     3123.7(2)
_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      302.0
_diffrn_measured_fraction_theta_full 1.000
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0737
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            34916
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.533
_diffrn_reflns_theta_min         3.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.136
_exptl_absorpt_correction_T_max  0.8644
_exptl_absorpt_correction_T_min  0.6333
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1559 before and 0.0841 after correction.
The Ratio of minimum to maximum transmission is 0.7326.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6182
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0735P)^2^+0.6219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1547
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4476
_reflns_number_total             6182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03832f2.cif
_cod_data_source_block           cu_200617b_a
_cod_depositor_comments
;
Adding full bibliography for 7705931--7705941.cif.

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C54 H62 B20 P2 S4'
_cod_original_formula_weight         1117.41
_cod_original_formula_moiety         '2(C3 H11 B10 S2), 2(C24 H20 P)'
_cod_original_formula_units_Z            2
_cod_database_code               7705931
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.769
_shelx_estimated_absorpt_t_min   0.663
_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:
 C00B(H00B), C00C(H00C), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H),
 C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00U(H00U),
 C00Y(H00Y), C008(H008)
2.b Boron cage BH refined with riding coordinates:
 C00D(H00D), B00T(H00T), B00V(H00V), B00W(H00W), B00X(H00X), B00Z(H00Z),
 B010(H010), B011(H011), B012(H012), B013(H013), B014(H014)
;
_shelx_res_checksum              41015
_olex2_submission_special_instructions 'No special instructions were received'