Synthesis, X-ray characterization, DFT calculations and Hirshfeld surface analysis of thiosemicarbazone complexes of Mn+ions (n = 2, 3; M = Ni, Cd, Mn, Co and Cu)
Mahmoudi, Ghodrat; Castiñeiras, Alfonso; Garczarek, Piotr; Bauzá, Antonio; Rheingold, Arnold L.; Kinzhybalo, Vasyl; Frontera, Antonio; CrystEngComm 18 (2016) 1009–; doi:10.1039/C5CE02371H

data_7223734
_publ_section_title
;
 Synthesis, X-ray characterization, DFT calculations and Hirshfeld surface
 analysis of thiosemicarbazone complexes of Mn+ions (n = 2, 3; M = Ni, Cd,
 Mn, Co and Cu)
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1009
_journal_paper_doi               10.1039/C5CE02371H
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C26 H20 Cl8 Hg4 N6'
_chemical_formula_sum            'C26 H20 Cl8 Hg4 N6'
_chemical_formula_weight         1502.44
_chemical_name_common            1
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-03-19 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                104.8910(10)
_cell_angle_beta                 101.344(2)
_cell_angle_gamma                99.190(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6970(3)
_cell_length_b                   15.9190(5)
_cell_length_c                   16.0270(7)
_cell_measurement_reflns_used    443
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     1814.35(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1547
_diffrn_reflns_av_unetI/netI     0.1717
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12858
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.489
_exptl_absorpt_correction_T_max  0.2737
_exptl_absorpt_correction_T_min  0.0773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2008
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.75
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.695
_refine_diff_density_min         -3.586
_refine_diff_density_rms         0.366
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         8150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1081P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1929
_refine_ls_wR_factor_ref         0.2325
_reflns_number_gt                4352
_reflns_number_total             8150
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5ce02371h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7223734--7223741.cif.'
_cod_original_cell_volume        1814.35(12)
_cod_database_code               7223734
_audit_block_doi                 10.5517/cc143g7y