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_7710236
_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         'C10.944 H13.832 Hg N2 O3 S'
_chemical_formula_sum            'C10.95 H13.83 Hg N2 O3 S'
_chemical_formula_weight         454.06
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-04-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-04-21 deposited with the CCDC.	2022-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.388(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.161(4)
_cell_length_b                   8.363(3)
_cell_length_c                   13.481(5)
_cell_measurement_reflns_used    2927
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.5
_cell_measurement_theta_min      1.8
_cell_volume                     1257.2(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10017
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.480
_diffrn_reflns_theta_min         1.826
_exptl_absorpt_coefficient_mu    12.410
_exptl_absorpt_correction_T_max  0.5758
_exptl_absorpt_correction_T_min  0.3700
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             854
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.422
_refine_diff_density_min         -2.368
_refine_diff_density_rms         0.410
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2927
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0626P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1954
_reflns_number_total             2927
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00391k2.cif
_cod_data_source_block           str0936
_cod_database_code               7710236
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.576
_shelx_estimated_absorpt_t_min   0.370
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(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
 O1-H1
 0.87 with sigma of 0.01
 Hg1-H1
 3.062906 with sigma of 0.02
 C8-H1
 1.89686 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(N1)
4. Others
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C6(H6), C5(H5), C4(H4)
5.c Fitted hexagon refined as free rotating group:
 C3(C2,C7,C6,C5,C4)
5.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              22529
_olex2_submission_original_sample_id Complex3
_olex2_submission_special_instructions 'No special instructions were received'