Characterization and Biological Activity of a Hydrogen Sulfide-Releasing Red Light-Activated Ruthenium(II) Complex.
Woods, Joshua J.; Cao, Jian; Lippert, Alexander R.; Wilson, Justin J.; Journal of the American Chemical Society 140 (2018) 12383–12387; doi:10.1021/jacs.8b08695

data_4133152
_publ_section_title
;
 Characterization and Biological Activity of a Hydrogen Sulfide-Releasing
 Red Light-Activated Ruthenium(II) Complex.
;
_journal_issue                   39
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12383
_journal_page_last               12387
_journal_paper_doi               10.1021/jacs.8b08695
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C44 H38 N6 O2 P Ru S2, F6 P'
_chemical_formula_sum            'C44 H38 F6 N6 O2 P2 Ru S2'
_chemical_formula_weight         1023.93
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-08-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                69.733(2)
_cell_angle_beta                 69.229(2)
_cell_angle_gamma                78.640(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9001(2)
_cell_length_b                   13.9565(3)
_cell_length_c                   15.9207(3)
_cell_measurement_reflns_used    18658
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      71.3960
_cell_measurement_theta_min      3.1130
_cell_volume                     2310.95(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_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      8.00 145.00   0.50    2.70    --   56.58  77.00  60.00  274
  2  \w    103.00 178.00   0.50    2.70    --  113.17  98.00 124.00  150
  3  \w    100.00 178.00   0.50    2.70    --  113.17 111.00   0.00  156
  4  \w    100.00 178.00   0.50    2.70    --  113.17 111.00-120.00  156
  5  \w    100.00 178.00   0.50    2.70    --  113.17 111.00  30.00  156
  6  \w    100.00 178.00   0.50    2.70    --  113.17 111.00 -60.00  156
  7  \w     92.00 145.00   0.50    2.70    --   56.58 125.00  90.00  106
  8  \w     92.00 145.00   0.50    2.70    --   56.58 125.00   0.00  106
  9  \w     63.00 178.00   0.50    2.70    --  113.17  50.00 -30.00  230
 10  \w     71.00 178.00   0.50    2.70    --  113.17  63.00-180.00  214
 11  \w     60.00 150.00   0.50    2.70    --  113.17 178.00  60.00  180
 12  \w     60.00 150.00   0.50    2.70    --  113.17 178.00   0.00  180
 13  \w     60.00 150.00   0.50    2.70    --  113.17 178.00-150.00  180
 14  \w     60.00 150.00   0.50    2.70    --  113.17 178.00 -30.00  180
 15  \w     60.00 150.00   0.50    2.70    --  113.17 178.00  30.00  180
 16  \w      8.00 145.00   0.50    2.70    --   56.58  77.00 120.00  274
 17  \w     16.00 109.00   0.50    2.70    --  113.17 -98.00  16.00  186
 18  \w     31.00 121.00   0.50    2.70    --   56.58-125.00-120.00  180
 19  \w     22.00 178.00   0.50    2.70    --  113.17 -37.00 -30.00  312
 20  \w     21.00 114.00   0.50    2.70    --  113.17-111.00  60.00  186
 21  \w     -7.00  59.00   0.50    0.67    --    0.00 -98.00  16.00  132
 22  \w     15.00 117.00   0.50    2.70    --   56.58  61.00 150.00  204
 23  \w      8.00 145.00   0.50    2.70    --   56.58  77.00 -30.00  274
 24  \w     21.00 114.00   0.50    2.70    --  113.17-111.00-180.00  186
 25  \w     -4.00  61.00   0.50    0.67    --    0.00 -99.00-180.00  130
 26  \w     -8.00 110.00   0.50    2.70    --   56.58 -98.00  16.00  236
 27  \w     -4.00 145.00   0.50    2.70    --   56.58  45.00 -90.00  298
 28  \w      8.00 145.00   0.50    2.70    --   56.58  77.00-180.00  274
 29  \w      8.00 145.00   0.50    2.70    --   56.58  77.00 -60.00  274
 30  \w      8.00 145.00   0.50    2.70    --   56.58  77.00-120.00  274
 31  \w      8.00 145.00   0.50    2.70    --   56.58  77.00  30.00  274
 32  \w    -49.00  89.00   0.50    0.67    --    0.00  77.00-120.00  276
 33  \w    -49.00  89.00   0.50    0.67    --    0.00  77.00-120.00  276
 34  \w    -49.00  89.00   0.50    0.67    --    0.00  77.00 150.00  276
 35  \w    -60.00  30.00   0.50    0.67    --    0.00  98.00 124.00  180
 36  \w    -84.00 -17.00   0.50    2.70    -- -106.00  98.00 124.00  134
 37  \w    -84.00  30.00   0.50    2.70    --  -56.58  98.00 124.00  228
 38  \w    -89.00 -17.00   0.50    2.70    -- -106.00 111.00 -90.00  144
 39  \w    -89.00 -17.00   0.50    2.70    -- -106.00 111.00-180.00  144
 40  \w    -89.00 -17.00   0.50    2.70    -- -106.00 111.00 -30.00  144
 41  \w    -94.00 -10.00   0.50    2.70    --  -56.58 125.00 120.00  168
 42  \w   -103.00 -36.00   0.50    0.67    --    0.00 178.00 -90.00  134
 43  \w   -144.00   2.00   0.50    2.70    --  -56.58 -45.00  30.00  292
 44  \w   -105.00 -38.00   0.50    0.67    --    0.00-178.00 -30.00  134
 45  \w   -145.00 -70.00   0.50    2.70    --  -56.58-125.00 -90.00  150
 46  \w   -152.00 -83.00   0.50    2.70    --  -56.58 -98.00  16.00  138
 47  \w   -145.00 -70.00   0.50    2.70    --  -56.58-125.00 150.00  150
 48  \w   -154.00 -80.00   0.50    2.70    --  -56.58 -94.00  60.00  148
 49  \w   -154.00 -80.00   0.50    2.70    --  -56.58 -94.00 -30.00  148
 50  \w   -154.00 -80.00   0.50    2.70    --  -56.58 -94.00-180.00  148
 51  \w   -154.00 -80.00   0.50    2.70    --  -56.58 -94.00-150.00  148
 52  \w   -154.00 -80.00   0.50    2.70    --  -56.58 -94.00 -90.00  148
 53  \w   -177.00 -82.00   0.50    2.70    -- -106.00 -98.00  16.00  190
 54  \w   -154.00 -80.00   0.50    2.70    --  -56.58 -94.00 120.00  148
 55  \w   -177.00 -76.00   0.50    2.70    -- -106.00 -91.00 120.00  202
 56  \w   -177.00 -78.00   0.50    2.70    -- -106.00-111.00 -60.00  198
 57  \w   -177.00 -57.00   0.50    2.70    -- -106.00 -77.00  60.00  240
 58  \w   -177.00 -76.00   0.50    2.70    -- -106.00 -91.00 -30.00  202
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0234539000
_diffrn_orient_matrix_UB_12      0.1140311000
_diffrn_orient_matrix_UB_13      -0.0344127000
_diffrn_orient_matrix_UB_21      -0.0106390000
_diffrn_orient_matrix_UB_22      0.0102123000
_diffrn_orient_matrix_UB_23      -0.0964479000
_diffrn_orient_matrix_UB_31      -0.1365466000
_diffrn_orient_matrix_UB_32      0.0289469000
_diffrn_orient_matrix_UB_33      0.0360021000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40236
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.313
_diffrn_reflns_theta_min         3.114
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.830
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.036
_refine_diff_density_max         1.225
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         8776
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+2.6142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1258
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7827
_reflns_number_total             8776
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08695_si_002.cif
_cod_data_source_block           1_Cl
_cod_database_code               4133152
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C47 H42 F6 N6 O3 P2 Ru S2'
_chemical_oxdiff_usercomment     'grown from either diffusion into acetone'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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 Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B), C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C43(H43), C28(H28), C42(H42), C34(H34), C8(H8), C37(H37), C40(H40),
 C41(H41), C26(H26), C7(H7), C10(H10), C23(H23), C33(H33), C24(H24), C29(H29),
 C25(H25), C18(H18), C11(H11), C15(H15), C12(H12), C31(H31), C30(H30), C20(H20),
  C19(H19), C14(H14), C13(H13)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              49578
_shelx_hkl_checksum              57041
_shelx_fab_checksum              22391
_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 1.317
_oxdiff_exptl_absorpt_empirical_full_min 0.808