Versatile coordination ability of thioamide ligand in Ru(ii) complexes: synthesis, computational studies, in vitro anticancer activity and apoptosis induction
Kumar, Ramasamy Raj; Ramesh, Rengan; Małecki, Jan Grzegorz; New J. Chem. 41 (2017) 9130–9141; doi:10.1039/C7NJ01828B

data_7056469
_publ_section_title
;
 Versatile coordination ability of thioamide ligand in Ru(ii) complexes:
 synthesis, computational studies, in vitro anticancer activity and
 apoptosis induction
;
_journal_issue                   17
_journal_name_full               'New J. Chem.'
_journal_page_first              9130
_journal_page_last               9141
_journal_paper_doi               10.1039/C7NJ01828B
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         '2(C44 H34 Cl N O4 P2 Ru S), C H5 O'
_chemical_formula_sum            'C89 H73 Cl2 N2 O9 P4 Ru2 S2'
_chemical_formula_weight         1775.53
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-12 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.726(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.4223(6)
_cell_length_b                   18.0430(5)
_cell_length_c                   16.9397(6)
_cell_measurement_reflns_used    7169
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.3950
_cell_measurement_theta_min      3.7250
_cell_volume                     4035.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.869
_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  84.00   1.00    7.93    --    9.90  38.00  60.00   77
  2  \w     -9.00  50.00   1.00    7.93    --  -11.78  77.00 -60.00   59
  3  \w    -22.00  66.00   1.00    7.93    --  -11.78  19.00 -90.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0286183000
_diffrn_orient_matrix_UB_12      -0.0275796000
_diffrn_orient_matrix_UB_13      0.0100153000
_diffrn_orient_matrix_UB_21      0.0442834000
_diffrn_orient_matrix_UB_22      -0.0118919000
_diffrn_orient_matrix_UB_23      0.0352265000
_diffrn_orient_matrix_UB_31      -0.0103505000
_diffrn_orient_matrix_UB_32      0.0253529000
_diffrn_orient_matrix_UB_33      0.0274085000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.869
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24488
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.869
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.569
_diffrn_reflns_theta_min         3.465
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       block
_exptl_crystal_F_000             1814
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         9819
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0304P)^2^+1.6925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0903
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7319
_reflns_number_total             9819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj01828b2.cif
_cod_data_source_block           rrk62
_cod_database_code               7056469
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'Ru1 P2 N2 S1 O4 Cl1 C48 H42'
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 H5-O5
 0.98 with sigma of 0.02
3. Others
 Fixed Sof: O5(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5)
4.a Riding coordinates:
 O5(H5)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44)
4.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C)
;
_shelx_res_checksum              675
_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 1.110
_oxdiff_exptl_absorpt_empirical_full_min 0.840