Direct observation by time-resolved infrared spectroscopy of the bright and the dark excited states of the [Ru(phen)2(dppz)]2+light-switch compound in solution and when bound to DNA
Poynton, Fergus E.; Hall, James P.; Keane, Páraic M.; Schwarz, Christine; Sazanovich, Igor V.; Towrie, Michael; Gunnlaugsson, Thorfinnur; Cardin, Christine J.; Cardin, David J.; Quinn, Susan J.; Long, Conor; Kelly, John M.; Chem. Sci. 7 (2016) 3075–; doi:10.1039/C5SC04514B

data_1542334
_publ_section_title
;
 Direct observation by time-resolved infrared spectroscopy of the bright
 and the dark excited states of the [Ru(phen)2(dppz)]2+light-switch
 compound in solution and when bound to DNA
;
_journal_issue                   5
_journal_name_full               'Chem. Sci.'
_journal_page_first              3075
_journal_paper_doi               10.1039/C5SC04514B
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'C42 H26 N8 Ru, 2(F6 P), 2.75(C2 H3 N)'
_chemical_formula_sum            'C47.5 H34.25 F12 N10.75 P2 Ru'
_chemical_formula_weight         1146.61
_chemical_name_systematic        '[Ru(Phen)2(DPPZ)]2PF6'
_chemical_properties_physical    Light-sensitive
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.21 svn.r3092 for OlexSys, GUI svn.r4949)
;
_audit_update_record
;
2014-12-10 deposited with the CCDC.
2016-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.6890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.7004(8)
_cell_length_b                   32.7257(12)
_cell_length_c                   14.3246(5)
_cell_measurement_reflns_used    9037
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.24
_cell_volume                     9245.2(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            436590
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         1.617
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014/3) was used for absorption correction.
wR2(int) was 0.0526 before and 0.0505 after correction.
The Ratio of minimum to maximum transmission is 0.9215.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       Needle
_exptl_crystal_F_000             4612
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1339
_refine_ls_number_reflns         21236
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0395P)^2^+22.8533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17208
_reflns_number_total             21236
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04514b6.cif
_cod_data_source_block           rup2dmono
_cod_depositor_comments
;
Adding full bibliography for 1542334.cif.

2019-07-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C42 H26 N8 Ru), 4(F6 P), 5.5(C2 H3 N)'
_cod_original_formula_sum        'C95 H68.50 F24 N21.50 P4 Ru2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     2293.23
_cod_database_code               1542334
_shelxl_version_number           2014/5
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.871
_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. Uiso/Uaniso restraints and constraints
Uanis(C502) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: N501(0.5) C501(0.5) C502(0.5) H50A(0.5) H50B(0.5) H50C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14), C15(H15),
 C16(H16), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36), C38(H38),
 C39(H39), C40(H40), C101(H101), C102(H102), C103(H103), C107(H107), C108(H108),
  C109(H109), C110(H110), C114(H114), C115(H115), C116(H116), C119(H119),
 C120(H120), C121(H121), C123(H123), C124(H124), C126(H126), C127(H127),
 C128(H128), C131(H131), C132(H132), C133(H133), C135(H135), C136(H136),
 C138(H138), C139(H139), C140(H140)
4.b Idealised Me refined as rotating group:
 C302(H30A,H30B,H30C), C402(H40A,H40B,H40C), C94(H94A,H94B,H94C), C502(H50A,
 H50B,H50C), C602(H60A,H60B,H60C), C202(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'