Cytotoxic (Salen)ruthenium(III) Anticancer Complexes Exhibit Different Modes of Cell Death Directed by Axial Ligands
Li, Cai; Ip, Kwok-Wa; Man, Wai-Lun; Song, Dan; He, Ming-Liang; Yiu, Shek-Man; Lau, Tai-Chu; ZHU, Guangyu; Chem. Sci.  (2017) –; doi:10.1039/C7SC02205K

data_1546742
_publ_section_title
;
 Cytotoxic (Salen)ruthenium(III) Anticancer Complexes Exhibit Different
 Modes of Cell Death Directed by Axial Ligands
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC02205K
_journal_year                    2017
_chemical_formula_moiety         'C22 H30 N8 O2 Ru, C4 H10 O, F6 P'
_chemical_formula_sum            'C26 H40 F6 N8 O3 P Ru'
_chemical_formula_weight         758.70
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-03-10
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2017-02-01 deposited with the CCDC.
2017-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 110.762(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1727(4)
_cell_length_b                   16.5751(4)
_cell_length_c                   14.5768(4)
_cell_measurement_reflns_used    5324
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.4790
_cell_measurement_theta_min      3.3322
_cell_volume                     3201.92(16)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12781
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.74
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.396
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         5703
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1155P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1470
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                4677
_reflns_number_total             5703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7sc02205k2.cif
_cod_data_source_block           022814a_mickey
_cod_original_cell_volume        3201.92(15)
_cod_database_code               1546742
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 P1, F1, F2, F3, F4, F5, F6, F3A, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(P1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim
Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F3A)
\\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: F3(0.5) F4(0.5) F5(0.5) F6(0.5) F3A(0.5) F4A(0.5) F5A(0.5) F6A(0.5)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C13(H13)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C24(H24A,H24B),
 C25(H25A,H25B)
5.c Aromatic/amide H refined with riding coordinates:
 N3(H3), N6(H6), C2(H2), C3(H3A), C4(H4), C5(H5), C7(H7), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19)
5.d X=CH2 refined with riding coordinates:
 N4(H4A,H4B), N5(H5A,H5B), N7(H7A,H7B), N8(H8A,H8B)
5.e Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C)
;