Synthesis, structure and reactivity with phosphines of Hg(ii) ortho-cyano-aminothiophenolate complexes formed via C–S bond cleavage and dehydrogenation of 2-aminobenzothiazoles
Al-Jibori, Subhi A.; Irzoqi, Ahmed A.; Al-Janabi, Ahmed S. M.; Al-Nassiry, Amenah I. A.; Basak-Modi, Sucharita; Ghosh, Shishir; Wagner, Christoph; Hogarth, Graeme; Dalton Transactions  (2022) –; doi:10.1039/D2DT00391K

data_7710237
_publ_section_title
;
 Synthesis, structure and reactivity with phosphines of Hg(ii)
 ortho-cyano-aminothiophenolate complexes formed via C--S bond cleavage
 and dehydrogenation of 2-aminobenzothiazoles
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00391K
_journal_year                    2022
_chemical_formula_moiety         'C21 H18 Hg N2 P S, C3 H7 N O'
_chemical_formula_sum            'C24 H25 Hg N3 O P S'
_chemical_formula_weight         635.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-04-05
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-22 deposited with the CCDC.	2022-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                76.019(4)
_cell_angle_beta                 71.357(4)
_cell_angle_gamma                72.842(4)
_cell_formula_units_Z            2
_cell_length_a                   10.1886(6)
_cell_length_b                   10.8397(6)
_cell_length_c                   12.3566(6)
_cell_measurement_reflns_used    11556
_cell_measurement_temperature    213
_cell_measurement_theta_max      29.65
_cell_measurement_theta_min      1.76
_cell_volume                     1219.06(12)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction        'STOE X-Area 1.77'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      213
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9597
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.763
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    6.484
_exptl_absorpt_correction_T_max  0.6199
_exptl_absorpt_correction_T_min  0.3363
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(IPDS Software; Stoe & Cie, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             618
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.319
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4766
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4230
_reflns_number_total             4766
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00391k2.cif
_cod_data_source_block           ipds4359
_cod_database_code               7710237
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.625
_shelx_estimated_absorpt_t_min   0.343
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C22-N3
 1.36 with sigma of 0.02
 N3-C24
 1.46 with sigma of 0.02
 N3-C23
 1.45 with sigma of 0.02
 C22-O1
 1.22 with sigma of 0.02
 N3-C24A
 1.46 with sigma of 0.02
 N3-C23A
 1.45 with sigma of 0.02
 C22-C24
 2.45 with sigma of 0.04
 C22-C23
 2.46 with sigma of 0.04
 C22-C24A
 2.45 with sigma of 0.04
 C22-C23A
 2.46 with sigma of 0.04
 N3-C23 \\sim N3-C24
 with sigma of 0.02
 N3-C23A \\sim N3-C24A
 with sigma of 0.02
3. Restrained planarity
 C22, N3, O1, C23, C24
 with sigma of 0.1
 C22, N3, O1, C23A, C24A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C22 \\sim N3 \\sim O1 \\sim C23 \\sim C24: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C22 \\sim N3 \\sim O1 \\sim C23A \\sim C24A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C22, N3, O1, C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22, C23A, C24A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=
 Sof(H24F)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B)
7.b Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C23A(H23D,H23E,H23F), C24A(H24D,
 H24E,H24F)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C)
;
_shelx_res_checksum              19695
_olex2_submission_special_instructions 'No special instructions were received'