Rationally Designed Long-Wavelength Absorbing Ru(II) Polypyridyl Complexes as Photosensitizers for Photodynamic Therapy.
Karges, Johannes; Heinemann, Franz; Jakubaszek, Marta; Maschietto, Federica; Subecz, Chloé; Dotou, Mazzarine; Vinck, Robin; Blacque, Olivier; Tharaud, Mickaël; Goud, Bruno; Viñuelas Zahı Nos, Emilio; Spingler, Bernhard; Ciofini, Ilaria; Gasser, Gilles; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13620

data_4134555
_publ_section_title
;
 Rationally Designed Long-Wavelength Absorbing Ru(II) Polypyridyl
 Complexes as Photosensitizers for Photodynamic Therapy.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13620
_journal_year                    2020
_chemical_formula_moiety         'C34 H24 N6 Ru, 2(F6 P), C2 H3 N [+ C2 H3 N]'
_chemical_formula_sum            'C38 H30 F12 N8 P2 Ru'
_chemical_formula_weight         989.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 118.159(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4678(3)
_cell_length_b                   27.4167(4)
_cell_length_c                   13.2004(3)
_cell_measurement_reflns_used    13485
_cell_measurement_temperature    183(1)
_cell_measurement_theta_max      75.3590
_cell_measurement_theta_min      3.9940
_cell_volume                     3978.18(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      183(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -80.00  34.30   0.90   10.00    --  -42.61  19.00 150.00  127
  2  \w    -96.00  -3.30   0.90   10.00    --  -42.61 125.00 -60.00  103
  3  \w     23.00  96.80   0.90   10.00    --   42.61-125.00 120.00   82
  4  \w     87.00 177.00   0.90   40.00    --  111.00  30.00 120.00  100
  5  \w     87.00 177.00   0.90   40.00    --  111.00  45.00  60.00  100
  6  \w     36.00 114.30   0.90   40.00    --  111.00-111.00   0.00   87
  7  \w     40.00 133.60   0.90   40.00    --  111.00 -45.00  60.00  104
  8  \w     36.00 135.00   0.90   40.00    --  111.00 -30.00-120.00  110
  9  \w     87.00 177.00   0.90   40.00    --  111.00  45.00 150.00  100
 10  \w     57.00 149.70   0.90   40.00    --  111.00 178.00-120.00  103
 11  \w     87.00 177.00   0.90   40.00    --  111.00  45.00  90.00  100
 12  \w     57.00 144.30   0.90   40.00    --  111.00 178.00 -60.00   97
 13  \w     86.00 177.80   0.90   40.00    --  111.00  61.00   0.00  102
 14  \w    143.00 166.40   0.90   40.00    --  111.00 111.00 -90.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0567100000
_diffrn_orient_matrix_UB_12      -0.0276526000
_diffrn_orient_matrix_UB_13      0.1152328000
_diffrn_orient_matrix_UB_21      0.1282395000
_diffrn_orient_matrix_UB_22      0.0122589000
_diffrn_orient_matrix_UB_23      0.0173910000
_diffrn_orient_matrix_UB_31      -0.0000391000
_diffrn_orient_matrix_UB_32      0.0473171000
_diffrn_orient_matrix_UB_33      0.0628225000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30861
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.495
_diffrn_reflns_theta_min         3.224
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.832
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.13a (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.652
_exptl_crystal_description       prism
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.129
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8116
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0756
_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^)+(0.0476P)^2^+10.1320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.1799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7644
_reflns_number_total             8116
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13620_si_002.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        3978.16(16)
_cod_database_code               4134555
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.619
_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. Rigid body (RIGU) restrains
 C23, C24, C25, C26, C27, C28, C29, C30, C31, C32, C33, C34, N5, N6
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34)
3.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              13837
_shelx_hkl_checksum              89618
_shelx_fab_checksum              61013
_platon_squeeze_void_probe_radius 1.20
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.611
_oxdiff_exptl_absorpt_empirical_full_min 0.678