1,2-Azolylamidino ruthenium(II) complexes with DMSO ligands: electro- and photocatalysts for CO<sub>2</sub> reduction.
Jennings, Murphy; Cuéllar, Elena; Rojo, Ariadna; Ferrero, Sergio; García-Herbosa, Gabriel; Nganga, John; Angeles-Boza, Alfredo M; Martín-Alvarez, Jose M; Miguel, Daniel; Villafañe, Fernando; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt01122d

data_7714425
_publ_section_title
;
 1,2-Azolylamidino ruthenium(II) complexes with DMSO ligands: electro- and
 photocatalysts for CO<sub>2</sub> reduction.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt01122d
_journal_year                    2023
_chemical_formula_moiety         'C15 H27 Cl N3 O3 Ru S3, C F3 O3 S'
_chemical_formula_sum            'C16 H27 Cl F3 N3 O6 Ru S4'
_chemical_formula_weight         679.16
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2022-11-24 deposited with the CCDC.	2023-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.12(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.139(6)
_cell_length_b                   13.115(8)
_cell_length_c                   24.022(8)
_cell_measurement_reflns_used    5088
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.2540
_cell_measurement_theta_min      2.9460
_cell_volume                     2554(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.798
_diffrn_measurement_details
;
  1 omega    1.00   72.00   1.0000   59.1200
omega____ theta____ kappa____ phi______ frames
    -       10.4463   37.0000  150.0000 71

  2 omega  -55.00   25.00   1.0000   59.1200
omega____ theta____ kappa____ phi______ frames
    -       10.4463  -77.0000   30.0000 80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0564936000
_diffrn_orient_matrix_UB_12      0.0411580000
_diffrn_orient_matrix_UB_13      -0.0014174000
_diffrn_orient_matrix_UB_21      -0.0436189000
_diffrn_orient_matrix_UB_22      0.0282426000
_diffrn_orient_matrix_UB_23      0.0193538000
_diffrn_orient_matrix_UB_31      0.0496192000
_diffrn_orient_matrix_UB_32      -0.0220239000
_diffrn_orient_matrix_UB_33      0.0222677000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.798
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10434
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.798
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.390
_diffrn_reflns_theta_min         2.304
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.105
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.0695
_exptl_crystal_size_min          0.0521
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0399P)^2^+1.7535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4487
_reflns_number_total             5625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01122d2.cif
_cod_data_source_block           ec51b
_cod_original_cell_volume        2554(2)
_cod_database_code               7714425
_chemical_oxdiff_formula         'C15 H26 Cl S3 N3 Ru'
_reflns_odcompleteness_completeness 97.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              79818
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id EC51
_olex2_submission_special_instructions 'No special instructions were received'