Cyclometalated Ru(II) complexes with tunable redox and optical properties for dye-sensitized solar cells.
Lavrova, Maria A.; Mishurinskiy, Sergey A.; Smirnov, Daniil E.; Kalle, Paulina; Krivogina, Ekaterina V.; Kozyukhin, Sergey A.; Emets, Viktor V.; Mariasina, Sofia S.; Dolzhenko, Vladimir D.; Bezzubov, Stanislav I.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16935–16945; doi:10.1039/d0dt03564e

data_7705877
_publ_section_title
;
 Cyclometalated Ru(II) complexes with tunable redox and optical properties
 for dye-sensitized solar cells.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16935
_journal_page_last               16945
_journal_paper_doi               10.1039/d0dt03564e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C48 H39 N6 O4 Ru, F6 P, 3(C H Cl3)'
_chemical_formula_sum            'C51 H42 Cl9 F6 N6 O4 P Ru'
_chemical_formula_weight         1367.99
_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             2020-03-16
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-03-17 deposited with the CCDC.	2020-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                83.218(2)
_cell_angle_beta                 85.892(2)
_cell_angle_gamma                79.659(2)
_cell_formula_units_Z            4
_cell_length_a                   16.4300(7)
_cell_length_b                   17.9246(9)
_cell_length_c                   19.3808(7)
_cell_measurement_reflns_used    8263
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.167
_cell_volume                     5568.2(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.1143
_diffrn_reflns_av_unetI/netI     0.1660
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            53144
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.857
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.813
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0989 before and 0.0671 after correction.
The Ratio of minimum to maximum transmission is 0.7918.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       needle
_exptl_crystal_F_000             2752
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CDCl3'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.549
_refine_diff_density_min         -1.455
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1413
_refine_ls_number_reflns         19298
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.1621
_refine_ls_R_factor_gt           0.0841
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1011P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.2179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9904
_reflns_number_total             19298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03564e2.cif
_cod_data_source_block           sm17
_cod_database_code               7705877
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.848
_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. Restrained distances
 Cl13-C043 \\sim Cl12-C043
 with sigma of 0.01
 Cl17-C03P \\sim Cl16-C03P
 with sigma of 0.01
 Cl20-C3B \\sim Cl21-C3B \\sim Cl19-C3B \\sim Cl18-C3B
 with sigma of 0.01
 Cl21-C49 \\sim Cl21-C3B \\sim Cl19-C49 \\sim Cl20-C49 \\sim Cl19-C3B \\sim
Cl18-C3B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(N6) = Uanis(O4)
Uanis(Cl13) = Uanis(Cl12)
Uiso(C49) = Uiso(C3B)
4. Others
 Fixed Sof: Cl12(0.4) Cl16(0.45) H03A(0.45) H03P(0.55) H04A(0.4) H043(0.6)
 Cl20(0.4) Cl18(0.6) C3B(0.6) H3B(0.6) Cl13(0.6) Cl17(0.55) C49(0.4) H49(0.4)
5.a Ternary CH refined with riding coordinates:
 C88(H88), C03P(H03A), C03P(H03P), C44(H44), C042(H042), C043(H04A),
 C043(H043), C04A(H04B), C04C(H04C), C3B(H3B), C49(H49)
5.b Aromatic/amide H refined with riding coordinates:
 C79(H79), C36(H36), C37(H37), C61(H61), C78(H78), C77(H77), C62(H62), C2(H2),
 C59(H59), C86(H86), C35(H35), C83(H83), C93(H93), C91(H91), C63(H63), C52(H52),
  C97(H97), C75(H75), C85(H85), C80(H80), C4(H4), C53(H53), C32(H32), C41(H41),
 C20(H20), C51(H51), C18(H18), C42(H42), C66(H66), C34(H34), C54(H54), C58(H58),
  C47(H47), C74(H74), C56(H56), C5(H5), C17(H17), C65(H65), C28(H28), C92(H92),
 C21(H21), C24(H24), C23(H23), C9(H9), C48(H48), C13(H13), C71(H71), C70(H70),
 C12(H12), C31(H31), C57(H57), C15(H15), C29(H29), C73(H73), C11(H11), C10(H10),
  C30(H30), C16(H16)
5.c Idealised Me refined as rotating group:
 C89(H89A,H89B,H89C), C39(H39A,H39B,H39C), C90(H90A,H90B,H90C), C82(H82A,H82B,
 H82C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              59667
_olex2_submission_special_instructions 'No special instructions were received'