Synthesis and biological evaluation of platinum complexes of highly functionalized aroylaminocarbo-N-thioyl prolinate containing tetrahydropyrrolo[3,4-c]pyrrole-1,3(2H,3aH)-dione moieties
Belveren, Samet; Poyraz, Samet; Pask, Christopher M.; Ülger, Mahmut; Sansano, José M.; Ali Döndaş, H.; Inorganica Chimica Acta 498 (2019) 119154–; doi:10.1016/j.ica.2019.119154

data_1565783
_publ_section_title
;
 Synthesis and biological evaluation of platinum complexes of highly
 functionalized aroylaminocarbo-N-thioyl prolinate containing
 tetrahydropyrrolo[3,4-c]pyrrole-1,3(2H,3aH)-dione moieties
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119154
_journal_paper_doi               10.1016/j.ica.2019.119154
_journal_volume                  498
_journal_year                    2019
_chemical_formula_moiety         'C62 H62 N4 O14 Pt S2'
_chemical_formula_sum            'C62 H62 N4 O14 Pt S2'
_chemical_formula_weight         1346.36
_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
_atom_sites_solution_primary     dual
_cell_angle_alpha                91.1570(10)
_cell_angle_beta                 105.0220(10)
_cell_angle_gamma                90.4890(10)
_cell_formula_units_Z            2
_cell_length_a                   14.3323(2)
_cell_length_b                   14.3931(2)
_cell_length_c                   15.4532(2)
_cell_measurement_reflns_used    21081
_cell_measurement_temperature    121(1)
_cell_measurement_theta_max      30.2710
_cell_measurement_theta_min      3.2740
_cell_volume                     3077.90(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      121(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     -7.00  82.00   1.00   30.00    --   13.11  37.00 -60.00   89
  2  \w    -54.00   0.00   1.00   30.00    --   13.11 -57.00-180.00   54
  3  \w    -12.00  19.00   1.00   30.00    --   13.11 -57.00  30.00   31
  4  \w    -55.00  15.00   1.00   30.00    --   13.11 -57.00 -60.00   70
  5  \w    -47.00 -19.00   1.00   30.00    --   13.11 -57.00 150.00   28
  6  \w     16.00  43.00   1.00   30.00    --   13.11  37.00   0.00   27
  7  \w     44.00  71.00   1.00   30.00    --   13.11  57.00-150.00   27
  8  \w    -34.00   7.00   1.00   30.00    --  -13.89  37.00-180.00   41
  9  \w    -82.00   8.00   1.00   30.00    --  -13.89 -62.00  14.28   90
 10  \w     21.00  46.00   1.00   30.00    --  -13.89  37.00-150.00   25
 11  \w    -35.00  11.00   1.00   30.00    --  -13.89 -57.00  90.00   46
 12  \w    -66.00 -38.00   1.00   30.00    --  -13.89 -57.00-120.00   28
 13  \w    -33.00  12.00   1.00   30.00    --  -13.89 -63.00-124.55   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0228199000
_diffrn_orient_matrix_UB_12      -0.0429874000
_diffrn_orient_matrix_UB_13      -0.0032728000
_diffrn_orient_matrix_UB_21      -0.0411642000
_diffrn_orient_matrix_UB_22      -0.0240961000
_diffrn_orient_matrix_UB_23      0.0059988000
_diffrn_orient_matrix_UB_31      -0.0202706000
_diffrn_orient_matrix_UB_32      -0.0012377000
_diffrn_orient_matrix_UB_33      -0.0470430000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            54186
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.133
_diffrn_reflns_theta_min         3.046
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.414
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.572
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.104
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     774
_refine_ls_number_reflns         17532
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+2.4382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14666
_reflns_number_total             17532
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2019-498-119154.cif
_cod_data_source_block           sk8_pt
_cod_database_code               1565783
_chemical_oxdiff_formula         'C124 H124 N8 O28 Pt2 S4'
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.699
_reflns_odcompleteness_completeness 99.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C3A-C2 = C3B-C2 = C4A-C3A = C4B-C3B = C5-C4A = C5-C4B
 1.39 with sigma of 0.01
3. Rigid body (RIGU) restrains
 C2, C7, C6, C5, C4B, C4A, C3A, C3B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H5A(0.6) H5B(0.4) C4A(0.6) H4A(0.6) C3A(0.6) H3A(0.6) C4B(0.4)
 H4B(0.4) C3B(0.4) H3B(0.4)
5.a Ternary CH refined with riding coordinates:
 C11(H11), C12(H12), C42(H42), C43(H43)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C15(H15A,H15B), C41(H41A,H41B), C46(H46A,H46B)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H5A), C5(H5B), C6(H6), C7(H7), C17(H17), C18(H18), C19(H19), C20(H20),
 C21(H21), C26(H26), C28(H28), C29(H29), C34(H34), C35(H35), C36(H36), C37(H37),
  C38(H38), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C57(H57),
 C59(H59), C60(H60), C4A(H4A), C3A(H3A), C4B(H4B), C3B(H3B)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C45(H45A,H45B,H45C), C54(H54A,H54B,H54C), C61(H61A,H61B,H61C), C62(H62A,
 H62B,H62C)
;
_olex2_date_sample_data_collection 2017-08-31
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.123
_oxdiff_exptl_absorpt_empirical_full_min 0.930