Unexpected reaction patterns enable simultaneous differentiation of H2S, H2Sn and biothiols
Chen, Wenqiang; Fu, Li; Chen, Chunfei; Xiao, Jun-An; Li, Wenxiu; Zhang, Liangliang; Xiao, Qi; Huang, Chusheng; Sheng, Jiarong; Song, Xiangzhi; Chemical Communications  (2019) –; doi:10.1039/C9CC03054A

data_7123622
_publ_section_title
;
 Unexpected reaction patterns enable simultaneous differentiation of H2S,
 H2Sn and biothiols
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03054A
_journal_year                    2019
_chemical_formula_moiety         'C2 H6 O S, C20 H17 N5 O3'
_chemical_formula_sum            'C22 H23 N5 O4 S'
_chemical_formula_weight         453.51
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc21bb0r
_audit_creation_date             2018-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-21 deposited with the CCDC.    2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.6650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.2305(2)
_cell_length_b                   19.0645(8)
_cell_length_c                   21.8678(9)
_cell_measurement_reflns_used    6523
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.963
_cell_measurement_theta_min      2.995
_cell_volume                     2178.23(15)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            34498
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.546
_diffrn_reflns_theta_min         3.339
_exptl_absorpt_coefficient_mu    0.189
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0696 before and 0.0613 after correction.
The Ratio of minimum to maximum transmission is 0.9142.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.465
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.0784
_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^)+(0.0864P)^2^+1.7200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.2065
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2750
_reflns_number_total             5014
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03054a2.cif
_cod_data_source_block           111
_cod_database_code               7123622
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.953
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 H6-H2AA
 3 with sigma of 0.02
 H6-H2AB
 3.2 with sigma of 0.02
 H5_$1-H22C_$2
 2.5 with sigma of 0.02
 C1B-C2 \\sim C2-C1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1B) \\sim Ueq, Uanis(C1A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C1B) = Uanis(C1A)
4. Others
 Sof(H2BC)=Sof(H2BD)=Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(1)
5.a Rotating group:
 N3(H3A)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2BC,H2BD), C2(H2AA,H2AB)
5.c Aromatic/amide H refined with riding coordinates:
 N5(H5), C7(H7), C17(H17), C6(H6), C10(H10)
5.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C3(H3B,H3C,H3D), C1B(H1BA,H1BB,
 H1BC), C1A(H1AA,H1AB,H1AC)
5.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_shelx_res_checksum              76528
_olex2_submission_special_instructions 'No special instructions were received'