Masking thiol reactivity with thioamide, thiourea, and thiocarbamate-based MBPs.
Seo, Hyeonglim; Kohlbrand, Alysia J.; Stokes, Ryjul W.; Chung, Jeewon; Cohen, Seth M.; Chemical communications (Cambridge, England) 59 (2023) 2283–2286; doi:10.1039/d2cc06596g

data_7131245
_publ_section_title
;
 Masking thiol reactivity with thioamide, thiourea, and
 thiocarbamate-based MBPs.
;
_journal_issue                   16
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2283
_journal_page_last               2286
_journal_paper_doi               10.1039/d2cc06596g
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C39 H34 B N7 S2 Zn, 0.5(C6 H6)'
_chemical_formula_sum            'C42 H37 B N7 S2 Zn'
_chemical_formula_weight         780.08
_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             2022-04-22
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-10-07 deposited with the CCDC.	2023-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.684(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.078(2)
_cell_length_b                   20.118(3)
_cell_length_c                   23.900(4)
_cell_measurement_reflns_used    9682
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.51
_cell_volume                     7642(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3439
_diffrn_reflns_av_unetI/netI     0.0969
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            176725
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.263
_diffrn_reflns_theta_min         2.480
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           50.0
_diffrn_source_power             2.5
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.793
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1422 before and 0.0867 after correction.
The Ratio of minimum to maximum transmission is 0.8121.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.686
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         13706
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.1546
_refine_ls_R_factor_gt           0.1325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+162.8532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3099
_refine_ls_wR_factor_ref         0.3223
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10828
_reflns_number_total             13706
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06596g2.cif
_cod_data_source_block           292
_cod_depositor_comments
'Adding full bibliography for 7131239--7131245.cif.'
_cod_database_code               7131245
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.925
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 B1(H1), B2(H2A)
1.b Aromatic/amide H refined with riding coordinates:
 C00O(H00O), C00U(H00U), C00V(H00V), C00X(H00X), C012(H012), C015(H015),
 C017(H017), C019(H019), C01B(H01B), C01D(H01R), C01H(H01H), C01J(H01V),
 C01K(H01W), C01L(H01L), C01M(H01Z), C01N(H01), C01P(H01P), C01Q(H01Q),
 C01T(H2), C01U(H3), C01X(H01X), C01Y(H01Y), C01Z(H4), C020(H020), C021(H021),
 C022(H022), C023(H023), C024(H024), C025(H025), C026(H026), C027(H027),
 C029(H029), C02A(H02A), C02B(H02E), C02D(H02J), C02E(H02K), C02F(H02F),
 C02G(H02G), C02H(H02H), C02I(H02I), C02J(H02L), C02L(H02M), C02M(H02T),
 C02N(H02N), C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R), C02S(H02S),
 C02T(H02U), C02U(H02W), C02V(H02V), C02X(H02X), C02Y(H02Y)
1.c Idealised Me refined as rotating group:
 C018(H01M,H01N,H01O), C01F(H01A,H01C,H01D), C01G(H01S,H01T,H01U), C01R(H01E,
 H01F,H01G), C01V(H01I,H01J,H01K), C028(H02B,H02C,H02D)
;
_shelx_res_checksum              37822
_shelx_hkl_checksum              22234
_olex2_submission_special_instructions 'No special instructions were received'