Synthesis, characterization and anticancer mechanism studies of fluorinated cyclometalated ruthenium(ii) complexes.
Wen, Ya; Ouyang, Cheng; Li, Quanwen; Rees, Thomas W.; Qiu, Kangqiang; Ji, Liangnian; Chao, Hui; Dalton transactions (Cambridge, England : 2003) 49 (2020) 7044–7052; doi:10.1039/d0dt01412e

data_7704592
_publ_section_title
;
 Synthesis, characterization and anticancer mechanism studies of
 fluorinated cyclometalated ruthenium(ii) complexes.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7044
_journal_page_last               7052
_journal_paper_doi               10.1039/d0dt01412e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C37 H25 F N5 Ru, F6 P, C2 H3 N'
_chemical_formula_sum            'C39 H28 F7 N6 P Ru'
_chemical_formula_weight         845.71
_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
_audit_block_doi                 10.5517/ccdc.csd.cc21jjqv
_audit_creation_date             2019-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2020-05-18 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.627(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7662(2)
_cell_length_b                   18.5608(4)
_cell_length_c                   21.9662(5)
_cell_measurement_reflns_used    16198
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.4810
_cell_measurement_theta_min      3.7900
_cell_volume                     3523.74(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_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    -16.00  48.00   1.00    3.06    --   11.80  57.00 -60.00   64
  2  \w    -12.00  57.00   1.00    3.06    --   11.80  38.00 120.00   69
  3  \w    -61.00 -35.00   1.00    3.06    --   11.80 -57.00  90.00   26
  4  \w    -56.00  31.00   1.00    3.06    --   11.80 -38.00  90.00   87
  5  \w     49.00  75.00   1.00    3.06    --   11.80-178.00  60.00   26
  6  \w     35.00  99.00   1.00    3.06    --   11.80-178.00  30.00   64
  7  \w     46.00  77.00   1.00    3.06    --   11.80-178.00 -60.00   31
  8  \w    -16.00  24.00   1.00    3.06    --  -10.86 -99.00-180.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0269958000
_diffrn_orient_matrix_UB_12      -0.0307411000
_diffrn_orient_matrix_UB_13      0.0177581000
_diffrn_orient_matrix_UB_21      -0.0041489000
_diffrn_orient_matrix_UB_22      -0.0205458000
_diffrn_orient_matrix_UB_23      -0.0274664000
_diffrn_orient_matrix_UB_31      0.0773876000
_diffrn_orient_matrix_UB_32      0.0096237000
_diffrn_orient_matrix_UB_33      -0.0018569000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37298
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         3.243
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.567
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       prism
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+3.9635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6954
_reflns_number_total             7990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01412e2.cif
_cod_data_source_block           1610273
_cod_database_code               7704592
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C20 H20 N Ru'
_chemical_oxdiff_usercomment     Ru1-4
_reflns_odcompleteness_completeness 99.73
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C28(H28), C30(H30), C33(H33), C34(H34), C36(H36), C37(H37)
2.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C)
;
_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 1.227
_oxdiff_exptl_absorpt_empirical_full_min 0.816