Quaternary Ru(II) complexes of terpyridines, saccharin and 1,2-azoles: effect of substituents on molecular structure, speciation, photoactivity, and photocytotoxicity.
Kumar, Priyaranjan; Singh, Prerana; Saren, Sanjoy; Sayala, Juhi; Sivakumar, Sri; Patra, Ashis K.; Dalton transactions (Cambridge, England : 2003)  (2022) –; doi:10.1039/d2dt02203f

data_7711841
_publ_section_title
;
 Quaternary Ru(II) complexes of terpyridines, saccharin and 1,2-azoles:
 effect of substituents on molecular structure, speciation, photoactivity,
 and photocytotoxicity.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d2dt02203f
_journal_year                    2022
_chemical_formula_moiety         'C41 H28 N8 O6 Ru S2, 1[CH3OH]'
_chemical_formula_sum            'C41 H28 N8 O6 Ru S2'
_chemical_formula_weight         893.90
_chemical_name_systematic        Ru-2pytpy-sac-in
_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     iterative
_audit_creation_date             2021-01-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-07-16 deposited with the CCDC.	2022-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                86.0730(10)
_cell_angle_beta                 78.2220(10)
_cell_angle_gamma                61.2780(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4757(5)
_cell_length_b                   12.9156(5)
_cell_length_c                   13.4640(5)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.33
_cell_volume                     1861.38(13)
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29267
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.337
_diffrn_reflns_theta_min         3.093
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1006 before and 0.0429 after correction.
The Ratio of minimum to maximum transmission is 0.9476.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic blackish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   blackish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       needle
_exptl_crystal_F_000             908
_exptl_crystal_preparation       'Synthesis at ambient condition'
_exptl_crystal_recrystallization_method 'Diffusion in diethyl ether'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0345P)^2^+2.8631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8003
_reflns_number_total             9250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02203f2.cif
_cod_data_source_block           30octc_0m
_cod_database_code               7711841
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.870
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N7(H7), C12(H12), C28(H28), C33(H33), C32(H32), C35(H35), C24(H24), C21(H21),
 C27(H27), C5(H5), C31(H31), C10(H10), C38(H38), C37(H37), C34(H34), C26(H26),
 C11(H11), C4(H4), C2(H2), C9(H9), C25(H25), C3(H3), C16(H16), C40(H40),
 C39(H39), C18(H18), C15(H15), C17(H17)
;
_smtbx_masks_special_details
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A solvent mask was calculated and 38 electrons were 
found in a volume of 93\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1[CH3OH] per Formula Unitwhich account for 36 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              36245
_shelx_fab_checksum              86737
_olex2_date_sample_completion    2017-10-30
_olex2_date_sample_data_collection 2017-10-30
_olex2_date_sample_submission    2017-10-30
_olex2_exptl_crystal_mounting_method 'Glass fiber'
_olex2_submission_original_sample_id Ru-2pytpy-sac-in
_olex2_submission_special_instructions 'No special instructions were received'