Synthesis, characterization and anti-cancer studies of Mn(II), Cu(II), Zn(II) and Pt(II) dithiocarbamate complexes - crystal structures of the Cu(II) and Pt(II) complexes
Ajibade, Peter A.; Fatokun, Amos A.; Andrew, Fartisincha P.; Inorganica Chimica Acta 504 (2020) 119431–; doi:10.1016/j.ica.2020.119431

data_1565244
_publ_section_title
;
 Synthesis, characterization and anti-cancer studies of Mn(II), Cu(II),
 Zn(II) and Pt(II) dithiocarbamate complexes - crystal structures of the
 Cu(II) and Pt(II) complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119431
_journal_paper_doi               10.1016/j.ica.2020.119431
_journal_volume                  504
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C30 H28 N2 O2 Pt S4'
_chemical_formula_sum            'C30 H28 N2 O2 Pt S4'
_chemical_formula_weight         771.87
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.219(6)
_cell_length_b                   17.750(4)
_cell_length_c                   7.6800(16)
_cell_measurement_reflns_used    8334
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.75
_cell_volume                     3846.8(14)
_computing_cell_refinement       'COSMO (Bruker, V1.61, 2009)'
_computing_data_collection       'COSMO (Bruker, V1.61, 2009)'
_computing_data_reduction        'SAINT (Bruker)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.2
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_av_unetI/netI     0.0804
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            13956
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         2.749
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.888
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_meas      .
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1520
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of DMSO and methanol  by slow evaporation'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         3.376
_refine_diff_density_min         -1.758
_refine_diff_density_rms         0.211
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.483(16)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         7216
_refine_ls_number_restraints     229
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0653P)^2^+45.7505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1514
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                6642
_reflns_number_total             7216
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-504-119431.cif
_cod_data_source_block           2
_cod_database_code               1565244
_shelx_estimated_absorpt_t_max   0.541
_shelx_estimated_absorpt_t_min   0.327
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.517(16)
 0.483(16)
2. 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, All O(H) groups
3. Restrained distances
 S3-H2
 2.681 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(N2) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C17) \\sim Ueq,
Uanis(C18) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(S1) \\sim Ueq, Uanis(S2) \\sim Ueq, Uanis(S3) \\sim Ueq, Uanis(S4) \\sim
Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5), C6(H6), C14(H14), C13(H13), C12(H12), C11(H11),
 C18(H18), C19(H19), C21(H21), C22(H22), C29(H29), C28(H28), C27(H27), C26(H26)
5.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C10(C15,C14,C13,C12,C11), C17(C18,C19,C20,C21,C22),
 C25(C30,C29,C28,C27,C26)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C23(H23A,H23B,H23C)
5.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_shelx_res_checksum              47262
_shelx_hkl_checksum              53529
_shelx_fab_checksum              34422