Synthesis and characterization of novel tetradentate ruthenium complexes of a pyridine-o-phenylenediamine based chelate ligand
Stones, Maryanne K.; Sullivan, Ryan J.; Soldatov, Dmitriy V.; Schlaf, Marcel; Inorganica Chimica Acta 502 (2020) 119391–; doi:10.1016/j.ica.2019.119391

data_1565443
_publ_section_title
;
 Synthesis and characterization of novel tetradentate ruthenium complexes
 of a pyridine-o-phenylenediamine based chelate ligand
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119391
_journal_paper_doi               10.1016/j.ica.2019.119391
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         'C32 H28 N6 Ru, 2(C F3 O3 S), 0.5(H2 O)'
_chemical_formula_sum            'C34 H29 F6 N6 O6.5 Ru S2'
_chemical_formula_weight         904.82
_chemical_name_common            '[Ru(PhCN)2(L)](CF3SO3)2*0.5(H2O)'
_chemical_name_systematic
;
 (N,N'-Bis(2-pyridylmethyl)-o-phenylenediamine)-bis(benzonitrile)-
ruthenium(II) bis(triflate) hemihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.1828(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.42053(11)
_cell_length_b                   15.64518(14)
_cell_length_c                   23.5928(3)
_cell_measurement_reflns_used    49871
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      37.1810
_cell_measurement_theta_min      3.0530
_cell_volume                     3807.20(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3693
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            148529
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.035
_diffrn_reflns_theta_min         2.604
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_description       prism
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.650
_exptl_crystal_size_min          0.600
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         19380
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+4.4796P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16377
_reflns_number_total             19380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119391.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C34 H29 F6 N6 O6.50 Ru S2'
_cod_database_code               1565443
_shelx_estimated_absorpt_t_min   0.644
_shelx_estimated_absorpt_t_max   0.713
_shelxl_version_number           2013-4