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_7060100
_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, F6 P'
_chemical_formula_sum            'C42 H38 F6 N2 P2 Ru Se'
_chemical_formula_weight         926.71
_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
_audit_creation_date             2020-10-21
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-30 deposited with the CCDC.	2020-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                102.299(3)
_cell_angle_beta                 92.894(3)
_cell_angle_gamma                111.556(4)
_cell_formula_units_Z            2
_cell_length_a                   10.3258(3)
_cell_length_b                   11.4664(5)
_cell_length_c                   17.7014(7)
_cell_measurement_reflns_used    7189
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      28.7160
_cell_measurement_theta_min      3.1480
_cell_volume                     1885.31(14)
_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, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0769
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_details
'#__ type_ start__ end____ width___ exp.time_ 1 omega 0.00 25.00 1.0000 34.6900 omega____ theta____ kappa____ phi______ frames - 15.2374 57.0000 60.0000 25 #__ type_ start__ end____ width___ exp.time_ 2 omega -36.00 43.00 1.0000 34.6900 omega____ theta____ kappa____ phi______ frames - 15.2374 -19.0000 -30.0000 79 #__ type_ start__ end____ width___ exp.time_ 3 omega -20.00 30.00 1.0000 34.6900 omega____ theta____ kappa____ phi______ frames - 15.2374 -57.0000 -60.0000 50 #__ type_ start__ end____ width___ exp.time_ 4 omega -54.00 26.00 1.0000 34.6900 omega____ theta____ kappa____ phi______ frames - 15.2374 -19.0000 -120.0000 80 #__ type_ start__ end____ width___ exp.time_ 5 omega 1.00 35.00 1.0000 34.6900 omega____ theta____ kappa____ phi______ frames - 15.2374 77.0000 -90.0000 34 #__ type_ start__ end____ width___ exp.time_ 6 omega -6.00 66.00 1.0000 34.6900 omega____ theta____ kappa____ phi______ frames - 15.2374 77.0000 -180.0000 72 #__ type_ start__ end____ width___ exp.time_ 7 omega -87.00 -40.00 1.0000 34.6900 omega____ theta____ kappa____ phi______ frames - -16.0187 153.0000 -7.0000 47'
_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      0.0079375000
_diffrn_orient_matrix_UB_12      0.0444313000
_diffrn_orient_matrix_UB_13      0.0362687000
_diffrn_orient_matrix_UB_21      -0.0239866000
_diffrn_orient_matrix_UB_22      0.0378489000
_diffrn_orient_matrix_UB_23      -0.0195062000
_diffrn_orient_matrix_UB_31      -0.0702020000
_diffrn_orient_matrix_UB_32      -0.0361959000
_diffrn_orient_matrix_UB_33      0.0045270000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16267
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.177
_diffrn_reflns_theta_min         2.659
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.530
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66091
_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            orange
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       irregular
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         8622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0259P)^2^+0.8688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7395
_reflns_number_total             8622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04958a2.cif
_cod_data_source_block           ruseph
_cod_depositor_comments
'Adding full bibliography for 7060099--7060101.cif.'
_cod_original_cell_volume        1885.31(13)
_cod_database_code               7060100
_shelx_estimated_absorpt_t_max   0.803
_shelx_estimated_absorpt_t_min   0.692
_reflns_odcompleteness_completeness 99.84
_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.a Ternary CH refined with riding coordinates:
 C40(H40)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12),
 C13(H13), 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.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              75580
_olex2_submission_special_instructions 'No special instructions were received'