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_7705878
_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         '1.5(C47 H37 N6 O8 Ru), 1.5(F6 P), C H2 Cl2'
_chemical_formula_sum            'C71.5 H57.5 Cl2 F9 N9 O12 P1.5 Ru1.5'
_chemical_formula_weight         1674.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-03
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-03-03 deposited with the CCDC.	2020-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.3941(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   53.215(3)
_cell_length_b                   12.7933(6)
_cell_length_c                   21.3714(9)
_cell_measurement_reflns_used    9989
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.34
_cell_measurement_theta_min      2.48
_cell_volume                     14210.5(12)
_computing_cell_refinement       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_collection       'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker AXS, 2016)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '3-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55769
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.500
_diffrn_reflns_theta_max         24.500
_diffrn_reflns_theta_min         1.639
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0752 before and 0.0544 after correction. The Ratio of minimum to maximum transmission is 0.8198. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       block
_exptl_crystal_F_000             6792
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2, heptane'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.085
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     951
_refine_ls_number_reflns         11798
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0735
_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^)+(0.0358P)^2^+169.6408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1573
_refine_ls_wR_factor_ref         0.1610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10659
_reflns_number_total             11798
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03564e2.cif
_cod_data_source_block           ml-sm10
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        14210.4(11)
_cod_original_formula_sum        'C71.50 H57.50 Cl2 F9 N9 O12 P1.50 Ru1.50'
_cod_database_code               7705878
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.911
_computing.bruker_data_scaling   'SADABS V2012/1 (Bruker AXS Inc.)'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Ru2-Ru2_$1
 0.3 with sigma of 0.02
 Cl2-C81 \\sim Cl3-C81
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N7) = Uanis(C66)
Uanis(Cl3) = Uanis(Cl2)
Uanis(C63) = Uanis(C64) = Uanis(C65) = Uanis(C66) = Uanis(C61) = Uanis(C62) =
Uanis(N8) = Uanis(C54) = Uanis(N7)
Uanis(C53) = Uanis(C52) = Uanis(C51) = Uanis(C50) = Uanis(C49) = Uanis(C48)
Uanis(C60) = Uanis(C58) = Uanis(C57) = Uanis(C56) = Uanis(C55)
Uanis(C59) = Uanis(C60) = Uanis(C55) = Uanis(C57) = Uanis(C58)
Uanis(Cl3) = Uanis(Cl2) = Uanis(Cl1)
4. Others
 Fixed Sof: Ru2(0.5) Cl3(0.5) H81C(0.5) H81D(0.5) H81A(0.5) H81B(0.5) C61(0.5)
 C50(0.5) H50(0.5) C64(0.5) H64(0.5) N7(0.5) C56(0.5) H56(0.5) N8(0.5) C66(0.5)
 C51(0.5) H51(0.5) C63(0.5) H63(0.5) C55(0.5) C53(0.5) C48(0.5) C62(0.5)
 H62(0.5) C60(0.5) H60(0.5) C49(0.5) H49(0.5) Cl2(0.5) C52(0.5) H52(0.5)
 C65(0.5) H65(0.5) C58(0.5) H58(0.5) C57(0.5) H57(0.5) C59(0.5) H59(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C81(H81C,H81D), C81(H81A,H81B)
5.b Aromatic/amide H refined with riding coordinates:
 C73(H73), C37(H37), C23(H23), C21(H21), C42(H42), C35(H35), C26(H26),
 C18(H18), C29(H29), C5(H5), C28(H28), C70(H70), C2(H2), C20(H20), C68(H68),
 C43(H43), C75(H75), C40(H40), C17(H17), C34(H34), C76(H76), C9(H9), C16(H16),
 C3(H3), C67(H67), C15(H15), C11(H11), C12(H12), C13(H13), C4(H4), C10(H10),
 C50(H50), C64(H64), C56(H56), C51(H51), C63(H63), C62(H62), C60(H60), C49(H49),
  C52(H52), C65(H65), C58(H58), C57(H57), C59(H59)
5.c Idealised Me refined as rotating group:
 C45(H45A,H45B,H45C), C31(H31A,H31B,H31C), C80(H80A,H80B,H80C), C78(H78A,H78B,
 H78C), C47(H47A,H47B,H47C), C33(H33A,H33B,H33C)
;
_shelx_res_checksum              11687
_olex2_submission_special_instructions 'No special instructions were received'