Synthesis, characterization and cytotoxic activity of cationic half-sandwich Ru(ii) complexes stabilized by iminophosphorane N,N,S and N,N,Se tridentate ligands
Martínez-De-León, Carla Gabriela; Flores Vallejo, Rosario del Carmen; Rodríguez-Álvarez, Aurora; Villareal, María Luisa; Grévy, Jean-Michel; New Journal of Chemistry 44 (2020) 20676–20687; doi:10.1039/D0NJ04958A

data_7060101
_publ_section_title
;
 Synthesis, characterization and cytotoxic activity of cationic
 half-sandwich Ru(ii) complexes stabilized by iminophosphorane N,N,S and
 N,N,Se tridentate ligands
;
_journal_issue                   47
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20676
_journal_page_last               20687
_journal_paper_doi               10.1039/D0NJ04958A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C42 H38 N2 P Ru Se, Cl, C H2 Cl2'
_chemical_formula_sum            'C43 H40 Cl3 N2 P Ru Se'
_chemical_formula_weight         902.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-10-23
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-28 deposited with the CCDC.	2020-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.020(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1571(3)
_cell_length_b                   16.3864(4)
_cell_length_c                   20.0229(5)
_cell_measurement_reflns_used    14511
_cell_measurement_temperature    99.98(12)
_cell_measurement_theta_max      28.7240
_cell_measurement_theta_min      2.9980
_cell_volume                     3978.97(17)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details
;
  1 omega   -4.00   84.00   1.0000   20.3750
omega____ theta____ kappa____ phi______ frames
    -       15.2374   38.0000 -120.0000 88

  2 omega    3.00   54.00   1.0000   20.3750
omega____ theta____ kappa____ phi______ frames
    -       15.2374  -99.0000 -120.0000 51

  3 omega   -5.00   81.00   1.0000   20.3750
omega____ theta____ kappa____ phi______ frames
    -       15.2374   77.0000 -120.0000 86

  4 omega    6.00   66.00   1.0000   20.3750
omega____ theta____ kappa____ phi______ frames
    -       15.2374   77.0000  -30.0000 60

  5 omega  -26.00   74.00   1.0000   20.3750
omega____ theta____ kappa____ phi______ frames
    -       15.2374    0.0000 -180.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0377282000
_diffrn_orient_matrix_UB_12      0.0209646000
_diffrn_orient_matrix_UB_13      0.0225326000
_diffrn_orient_matrix_UB_21      -0.0179878000
_diffrn_orient_matrix_UB_22      0.0378436000
_diffrn_orient_matrix_UB_23      -0.0141009000
_diffrn_orient_matrix_UB_31      -0.0408164000
_diffrn_orient_matrix_UB_32      0.0026573000
_diffrn_orient_matrix_UB_33      0.0235348000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.886
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34326
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.886
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.219
_diffrn_reflns_theta_min         2.687
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.584
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80139
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent red'
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.065
_refine_diff_density_min         -1.721
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9574
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0226P)^2^+2.9876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8100
_reflns_number_total             9574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04958a2.cif
_cod_data_source_block           rusephcl
_cod_depositor_comments
'Adding full bibliography for 7060099--7060101.cif.'
_cod_original_cell_volume        3978.96(17)
_cod_database_code               7060101
_shelx_estimated_absorpt_t_max   0.797
_shelx_estimated_absorpt_t_min   0.570
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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.a Ternary CH refined with riding coordinates:
 C40(H40)
2.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), 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), C35(H35), C36(H36), C38(H38), C39(H39)
2.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              76813
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'