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_1565442
_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         'C22 H24 N6 Ru, 2(C F3 O3 S)'
_chemical_formula_sum            'C24 H24 F6 N6 O6 Ru S2'
_chemical_formula_weight         771.68
_chemical_name_common            '[Ru(MeCN)2(L)](CF3SO3)2'
_chemical_name_systematic
;
 (N,N'-Bis(2-pyridylmethyl)-o-phenylenediamine)-bis(acetonitrile)-
ruthenium(II) bis(triflate)
;
_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                 91.8736(9)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   9.93854(9)
_cell_length_b                   51.3735(5)
_cell_length_c                   17.6187(2)
_cell_measurement_reflns_used    58483
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.8070
_cell_measurement_theta_min      2.8200
_cell_volume                     8990.90(16)
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       73
_diffrn_reflns_limit_k_min       -73
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            193657
_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         30.508
_diffrn_reflns_theta_min         2.667
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82090
_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    1.710
_exptl_crystal_description       prism
_exptl_crystal_F_000             4656
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.177
_refine_diff_density_min         -1.929
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.370
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1368
_refine_ls_number_reflns         27420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.370
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0719
_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^)+38.9619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                25723
_reflns_number_total             27420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2020-502-119391.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1565442
_shelx_estimated_absorpt_t_min   0.706
_shelx_estimated_absorpt_t_max   0.806
_shelxl_version_number           2013-4