Kinetically labile ruthenium(II) complexes of terpyridines and saccharin: effect of substituents on photoactivity, solvation kinetics, and photocytotoxicity.
Kumar, Priyaranjan; Singh, Prerana; Saren, Sanjoy; Pakira, Sandip; Sivakumar, Sri; Patra, Ashis K.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 8196–8217; doi:10.1039/d1dt00246e

data_7707292
_publ_section_title
;
 Kinetically labile ruthenium(II) complexes of terpyridines and saccharin:
 effect of substituents on photoactivity, solvation kinetics, and
 photocytotoxicity.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8196
_journal_page_last               8217
_journal_paper_doi               10.1039/d1dt00246e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C33 H23 N5 O7 Ru S3'
_chemical_formula_sum            'C33 H23 N5 O7 Ru S3'
_chemical_formula_weight         798.81
_chemical_name_systematic        Ru-ttpy-sac
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-21 deposited with the CCDC.	2021-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                78.814(3)
_cell_angle_beta                 67.894(3)
_cell_angle_gamma                68.326(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5927(18)
_cell_length_b                   13.445(2)
_cell_length_c                   13.715(2)
_cell_measurement_reflns_used    3105
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.69
_cell_measurement_theta_min      2.22
_cell_volume                     1836.7(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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_temperature      100(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker SMART CCD 1K area detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 1K area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1219
_diffrn_reflns_av_unetI/netI     0.2298
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13300
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        24.500
_diffrn_reflns_theta_max         24.500
_diffrn_reflns_theta_min         2.155
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.648
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6523
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0887 before and 0.0598 after correction. The Ratio of minimum to maximum transmission is 0.8747. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic brownish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.494
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6041
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1701
_refine_ls_R_factor_gt           0.0897
_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^)+(0.0937P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1762
_refine_ls_wR_factor_ref         0.2069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3204
_reflns_number_total             6041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00246e2.cif
_cod_data_source_block           indiumnew_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_ambient_temperature' value '100 (2)' was changed
to '100(2)' -- the value was reformatted.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7707291--7707294.cif.
;
_cod_original_cell_volume        1836.8(5)
_cod_database_code               7707292
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.903
_shelx_estimated_absorpt_t_min   0.881
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C24-C23
 1.3 with sigma of 0.02
 C23-C24
 1.2 with sigma of 0.02
 C25-C24
 1.2 with sigma of 0.02
 S3-C26
 1.8 with sigma of 0.02
 S3-C23
 1.55 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C25)
Uanis(C24) = Uanis(C23)
Uanis(C24) = Uanis(C25) = Uanis(C26) = Uanis(C23)
Uanis(C29) = Uanis(C28)
Uanis(C28) = Uanis(C27) = Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C22)
Uanis(C26) = Uanis(C25) = Uanis(C24) = Uanis(C23)
4.a Rotating group:
 O7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C21(H21), C27(H27), C3(H3), C12(H12), C9(H9), C30(H30), C15(H15),
 C33(H33), C4(H4), C16(H16), C18(H18), C31(H31), C2(H2), C11(H11), C32(H32),
 C17(H17), C5(H5), C25(H25), C10(H10), C26(H26)
;
_shelx_res_checksum              22490
_shelx_hkl_checksum              37748
_shelx_fab_checksum              24310
_olex2_submission_original_sample_id Ru-ttpy-sac
_olex2_submission_special_instructions 'No special instructions were received'