Cytotoxic cis-ruthenium(III) bis(amidine) complexes
Liu, Tao; Pan, Chen; Shi, Huatian; Huang, Tao; Huang, Yong-Liang; Deng, Yang-Yang; Ni, Wen-Xiu; Man, Wai-Lun; Dalton Transactions  (2023) –; doi:10.1039/D3DT00328K

data_7712658
_publ_section_title
;
 Cytotoxic cis-ruthenium(III) bis(amidine) complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00328K
_journal_year                    2023
_chemical_formula_moiety         'C26 H50 N4 O4 Ru, C F3 O3 S, 0.115(H2 O)'
_chemical_formula_sum            'C27 H50.23 F3 N4 O7.11 Ru S'
_chemical_formula_weight         734.91
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-02 deposited with the CCDC.	2023-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                105.416(2)
_cell_angle_beta                 99.450(2)
_cell_angle_gamma                106.518(2)
_cell_formula_units_Z            4
_cell_length_a                   11.1355(2)
_cell_length_b                   17.8642(3)
_cell_length_c                   19.5372(4)
_cell_measurement_reflns_used    23666
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      76.9150
_cell_measurement_theta_min      2.4500
_cell_volume                     3469.05(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.935
_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     68.00 102.00   0.50    0.24    --   45.52 139.00   1.00   68
  2  \w     75.00 121.00   0.50    0.95    --  105.42 139.00   1.00   92
  3  \w    131.00 172.00   0.50    0.95    --  105.42 125.00 -90.00   82
  4  \w     95.00 124.00   0.50    0.95    --  105.42 125.00 -90.00   58
  5  \w    100.00 125.00   0.50    0.95    --  105.42 130.00-172.00   50
  6  \w     95.00 172.00   0.50    0.95    --  105.42  37.00-120.00  154
  7  \w     23.00 117.00   0.50    0.24    --   45.52  77.00-180.00  188
  8  \w    -28.00  25.00   0.50    0.24    --  -45.52  19.00 -90.00  106
  9  \w    -64.00 -26.00   0.50    0.95    --  -97.00  77.00  30.00   76
 10  \w   -101.00 -76.00   0.50    0.95    --  -97.00  77.00  90.00   50
 11  \w    -64.00 -39.00   0.50    0.95    --  -97.00  77.00  90.00   50
 12  \w    -52.00 -27.00   0.50    0.95    --  -97.00  57.00 150.00   50
 13  \w    -29.00  25.00   0.50    0.24    --  -45.52  19.00   0.00  108
 14  \w    -29.00  22.00   0.50    0.24    --   45.52 -19.00-150.00  102
 15  \w    -26.00  12.00   0.50    0.24    --   45.52 -19.00-180.00   76
 16  \w     42.00 100.00   0.50    0.24    --   45.52-139.00 -58.00  116
 17  \w     90.00 122.00   0.50    0.95    --  105.42-139.00 -58.00   64
 18  \w     54.00  98.00   0.50    0.95    --  105.42-125.00  30.00   88
 19  \w     47.00 113.00   0.50    0.95    --  105.42-130.00 115.00  132
 20  \w     37.00  88.00   0.50    0.24    --   45.52-130.00 115.00  102
 21  \w     33.00  66.00   0.50    0.95    --  105.42 -99.00 120.00   66
 22  \w    -22.00  23.00   0.50    0.24    --   45.52 -19.00  60.00   90
 23  \w     40.00 111.00   0.50    0.95    --  105.42-125.00 -90.00  142
 24  \w     33.00 111.00   0.50    0.95    --  105.42-125.00-150.00  156
 25  \w     38.00 103.00   0.50    0.95    --  105.42 -99.00 -90.00  130
 26  \w     35.00 100.00   0.50    0.95    --  105.42 -99.00 -60.00  130
 27  \w     34.00  93.00   0.50    0.95    --  105.42 -99.00 -30.00  118
 28  \w     72.00 100.00   0.50    0.95    --  105.42 -99.00 120.00   56
 29  \w     33.00  59.00   0.50    0.95    --  105.42 -57.00 150.00   52
 30  \w     33.00  58.00   0.50    0.95    --  105.42 -57.00 120.00   50
 31  \w     33.00  60.00   0.50    0.95    --  105.42 -57.00   0.00   54
 32  \w     33.00  58.00   0.50    0.95    --  105.42 -57.00-120.00   50
 33  \w    -89.00 -63.00   0.50    0.95    --  -97.00 130.00-172.00   52
 34  \w    -85.00 -60.00   0.50    0.24    --  -45.52 130.00-172.00   50
 35  \w    -71.00 -45.00   0.50    0.24    --  -45.52 139.00   1.00   52
 36  \w   -121.00 -51.00   0.50    0.95    --  -97.00 139.00   1.00  140
 37  \w   -170.00 -91.00   0.50    0.95    --  -97.00 -99.00-120.00  158
 38  \w   -146.00-121.00   0.50    0.95    --  -97.00-139.00 -58.00   50
 39  \w   -170.00-101.00   0.50    0.95    --  -97.00-125.00   0.00  138
 40  \w   -149.00-124.00   0.50    0.95    --  -97.00-130.00 115.00   50
 41  \w   -129.00 -89.00   0.50    0.95    --  -97.00 -19.00 -30.00   80
 42  \w   -170.00 -85.00   0.50    0.95    --  -97.00 -37.00 -60.00  170
 43  \w   -169.00-110.00   0.50    0.95    --  -97.00 -77.00-150.00  118
 44  \w   -106.00 -75.00   0.50    0.95    --  -97.00 -77.00-150.00   62
 45  \w   -171.00-132.00   0.50    0.95    --  -97.00 -19.00 -30.00   78
 46  \w   -168.00 -84.00   0.50    0.95    --  -97.00 -37.00  60.00  168
 47  \w   -169.00-130.00   0.50    0.95    --  -97.00 -37.00 120.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0713223000
_diffrn_orient_matrix_UB_12      -0.0689167000
_diffrn_orient_matrix_UB_13      -0.0744137000
_diffrn_orient_matrix_UB_21      -0.0587750000
_diffrn_orient_matrix_UB_22      -0.0588490000
_diffrn_orient_matrix_UB_23      0.0403390000
_diffrn_orient_matrix_UB_31      -0.1174062000
_diffrn_orient_matrix_UB_32      0.0294959000
_diffrn_orient_matrix_UB_33      -0.0029527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0521
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48026
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.205
_diffrn_reflns_theta_min         2.429
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.760
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75222
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_description       block
_exptl_crystal_F_000             1537
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.115
_refine_diff_density_min         -1.987
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     804
_refine_ls_number_reflns         13744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0591
_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^)+(0.1180P)^2^+4.8194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11622
_reflns_number_total             13744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00328k3.cif
_cod_data_source_block           exp_10_auto
_cod_original_cell_volume        3469.04(12)
_cod_database_code               7712658
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.648
_shelx_estimated_absorpt_t_min   0.535
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(1)
3.a Free rotating group:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C38(H38A,H38B), C37(H37A,H37B), C29(H29A,H29B), C39(H39A,H39B),
 C41(H41A,H41B), C4(H4A,H4B), C5(H5A,H5B), C40(H40A,H40B), C31(H31A,H31B),
 C11(H11A,H11B), C7(H7A,H7B), C30(H30A,H30B), C32(H32A,H32B), C15(H15A,H15B),
 C33(H33A,H33B), C12(H12A,H12B), C13(H13A,H13B), C6(H6A,H6B), C14(H14A,H14B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N7(H7), N3(H3), N5(H5), N4(H4), N6(H6), N2(H2), N8(H8), C50(H50),
 C24(H24), C45(H45), C19(H19)
3.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C36(H36A,H36B,H36C), C49(H49A,H49B,H49C), C21(H21A,H21B,
 H21C), C18(H18A,H18B,H18C), C47(H47A,H47B,H47C), C52(H52A,H52B,H52C), C10(H10A,
 H10B,H10C), C23(H23A,H23B,H23C), C44(H44A,H44B,H44C), C28(H28A,H28B,H28C),
 C26(H26A,H26B,H26C), C42(H42A,H42B,H42C), C16(H16A,H16B,H16C), C8(H8A,H8B,H8C),
  C34(H34A,H34B,H34C)
;
_shelx_res_checksum              68745
_shelx_hkl_checksum              88089
_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 2.994
_oxdiff_exptl_absorpt_empirical_full_min 0.420