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_7711837
_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         'C35.931 H24.908 N7 O6.977 Ru S2'
_chemical_formula_sum            'C35.93 H24.91 N7 O6.97 Ru S2'
_chemical_formula_weight         831.49
_chemical_name_systematic        Ru-ftpy-sac-pz
_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     iterative
_audit_creation_date             2022-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-09-26 deposited with the CCDC.	2022-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                105.076(2)
_cell_angle_beta                 114.080(2)
_cell_angle_gamma                92.307(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7775(8)
_cell_length_b                   13.4849(9)
_cell_length_c                   14.2982(9)
_cell_measurement_reflns_used    5766
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.60
_cell_volume                     1974.1(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0881
_diffrn_reflns_av_unetI/netI     0.1116
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30386
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.367
_diffrn_reflns_theta_min         2.993
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0877 before and 0.0584 after correction. The Ratio of minimum to maximum transmission is 0.8966. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic brownish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       block
_exptl_crystal_F_000             843
_exptl_crystal_preparation       'Synthesis at ambient conditions'
_exptl_crystal_recrystallization_method 'Diffusion in Diethyl Ether'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.289
_refine_diff_density_min         -1.324
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9791
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0671
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1610
_refine_ls_wR_factor_ref         0.1826
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6546
_reflns_number_total             9791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02203f2.cif
_cod_data_source_block           23octc_0m
_cod_database_code               7711837
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.887
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N6B) = Uanis(N6A)
Uanis(N6A) = Uanis(N6B)
3. Rigid body (RIGU) restrains
 C36B, C35B, C34B, N7B, N6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C35A, C36A, C34A, N7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C34A)=Sof(H34A)=Sof(N7A)=Sof(H7A)=
 Sof(N6B)=1-FVAR(1)
 Sof(C36B)=Sof(H36B)=Sof(C35B)=Sof(H35B)=Sof(C34B)=Sof(H34B)=Sof(N7B)=Sof(H7B)=
 Sof(N6A)=FVAR(1)
 Sof(H32)=Sof(O7)=Sof(C26)=Sof(H26)=Sof(C25)=Sof(H25)=Sof(C24)=Sof(H24)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C27(H27), C11(H11), C21(H21), C15(H15), C12(H12), C17(H17),
 C33(H33), C10(H10), C18(H18), C32(H32), C9(H9), C30(H30), C5(H5), C3(H3),
 C4(H4), C2(H2), C36B(H36B), C35B(H35B), C34B(H34B), N7B(H7B), C35A(H35A),
 C36A(H36A), C34A(H34A), N7A(H7A), C26(H26), C25(H25), C24(H24)
5.b Fitted pentagon refined as free rotating group:
 C36B(C35B,C34B,N7B,N6A)
;
_shelx_res_checksum              95569
_shelx_fab_checksum              88629
_olex2_submission_original_sample_id Ru-ftpy-sac-pz
_olex2_submission_special_instructions 'No special instructions were received'