Cis and trans platinum(II) N-heterocyclic carbene isomers: synthesis, characterization and biological activity
Rivera, Carolina; Bacilio-Beltrán, Héctor Alejandro; Puebla-Pérez, Ana Maria; Rangel-Salas, Irma Idalia; Alvarado–Rodríguez, José G; Flores-Moreno, Roberto; Velázquez- Juárez, Gilberto; Peregrina-Lucano, Alejandro Aarón; Becerra-Martinez, Elvia; Valdez-Ruvalcaba, Jaime; Rubio-Garcia, J. Emiliano; Cortes-Llamas, Sara Angelica; New Journal of Chemistry 46 (2022) 14221–14226; doi:10.1039/D2NJ02508F

data_7061621
_publ_section_title
;
 Cis and trans platinum(II) N-heterocyclic carbene isomers: synthesis,
 characterization and biological activity
;
_journal_issue                   29
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14221
_journal_page_last               14226
_journal_paper_doi               10.1039/D2NJ02508F
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C10 H16 Cl2 N4 Pt'
_chemical_formula_sum            'C10 H16 Cl2 N4 Pt'
_chemical_formula_weight         458.26
_chemical_melting_point          553
_chemical_name_systematic
cis-bis(N,N'-dimethylimidazole)dichloroplatinum(II)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-20
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-24 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1567(4)
_cell_length_b                   10.5298(3)
_cell_length_c                   8.7320(2)
_cell_measurement_reflns_used    37890
_cell_measurement_temperature    294.15
_cell_measurement_theta_max      29.4810
_cell_measurement_theta_min      3.8190
_cell_volume                     1393.60(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      294.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3659
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -85.00  -36.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -10.1172  153.0000   13.8025 49

  2 omega  -34.00   49.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235  -91.0000   34.9858 83

  3 omega  -17.00   85.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235   57.0000  -60.0000 102

  4 omega  -21.00   88.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235   77.0000   60.0000 109

  5 omega  -13.00   86.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235   37.0000 -150.0000 99

  6 omega  -62.00   40.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235  -57.0000  150.0000 102

  7 omega  -30.00   51.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235  -95.0000  -73.6940 81

  8 omega  -67.00  -19.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -10.1172  126.0000   11.3851 48

  9 omega  -73.00  -26.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -10.1172  136.0000   82.0000 47

 10 omega  -70.00  -24.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -10.1172  133.0000  -95.0000 46

 11 omega  -25.00   52.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235  -99.0000   60.0000 77

 12 omega  -33.00   50.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235  -92.0000 -132.8815 83

 13 omega  -16.00   58.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235 -109.0000  -87.1793 74

 14 omega  -77.00  100.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235    0.0000 -180.0000 177

 15 omega  -77.00  100.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235    0.0000 -150.0000 177

 16 omega  -77.00  100.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235    0.0000 -120.0000 177

 17 omega  -77.00  100.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235    0.0000  -90.0000 177

 18 omega  -77.00  100.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235    0.0000  -60.0000 177

 19 omega  -13.00   86.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235   37.0000  -30.0000 99

 20 omega  -77.00  100.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235    0.0000    0.0000 177

 21 omega  -77.00   53.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235    0.0000   30.0000 130

 22 omega  -77.00  100.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       11.5235    0.0000  -30.0000 177
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0291593000
_diffrn_orient_matrix_UB_12      0.0216637000
_diffrn_orient_matrix_UB_13      -0.0579102000
_diffrn_orient_matrix_UB_21      0.0365885000
_diffrn_orient_matrix_UB_22      -0.0162961000
_diffrn_orient_matrix_UB_23      0.0466509000
_diffrn_orient_matrix_UB_31      0.0005688000
_diffrn_orient_matrix_UB_32      -0.0616873000
_diffrn_orient_matrix_UB_33      -0.0326541000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            91893
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.091
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    10.436
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.184
_exptl_crystal_description       Block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
;
 Flack x determined using 1329 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.030(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         3072
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0167
_refine_ls_R_factor_gt           0.0149
_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^)+(0.0177P)^2^+1.1191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0350
_refine_ls_wR_factor_ref         0.0362
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2938
_reflns_number_total             3072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02508f3.cif
_cod_data_source_block           1a
_cod_database_code               7061621
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.146
_shelx_estimated_absorpt_t_min   0.103
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              2026