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_7710238
_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         'C41 H32 Cl2 Hg2 N4 P2 S2'
_chemical_formula_sum            'C41 H32 Cl2 Hg2 N4 P2 S2'
_chemical_formula_weight         1178.84
_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
_audit_creation_date             2021-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-20 deposited with the CCDC.	2022-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                72.695(4)
_cell_angle_beta                 83.393(4)
_cell_angle_gamma                65.524(4)
_cell_formula_units_Z            2
_cell_length_a                   12.4945(7)
_cell_length_b                   13.6153(7)
_cell_length_c                   13.7342(7)
_cell_measurement_reflns_used    14279
_cell_measurement_temperature    213
_cell_measurement_theta_max      29.45
_cell_measurement_theta_min      1.55
_cell_volume                     2030.1(2)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL2017/7 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT2014/7 (Sheldrick, 2015a)'
_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 0.987
_diffrn_measured_fraction_theta_max 0.986
_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  0.0609
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16999
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.553
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    7.902
_exptl_absorpt_correction_T_max  0.7170
_exptl_absorpt_correction_T_min  0.3829
_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    1.928
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.232
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         8731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0614P)^2^+8.3707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6461
_reflns_number_total             8731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00391k2.cif
_cod_data_source_block           ipds4373
_cod_database_code               7710238
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.743
_shelx_estimated_absorpt_t_min   0.264
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C10(H10), C11(H11), C13(H13), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38),
 C39(H39), C40(H40), C41(H41)
;
_shelx_res_checksum              40327
_olex2_submission_special_instructions 'No special instructions were received'