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_7714426
_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         'C11 H25 Cl N3 O3 Ru S3, C F3 O3 S'
_chemical_formula_sum            'C12 H25 Cl F3 N3 O6 Ru S4'
_chemical_formula_weight         629.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2022-11-24 deposited with the CCDC.	2023-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.275(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8611(3)
_cell_length_b                   16.6923(7)
_cell_length_c                   16.0264(6)
_cell_measurement_reflns_used    5768
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.6810
_cell_measurement_theta_min      2.6110
_cell_volume                     2368.63(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4757
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -14.00  85.00   1.00  127.68    --   11.82  57.00  90.00   99
  2  \w    -63.00  22.00   1.00  127.68    --   11.82 -37.00 -60.00   85
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0134811000
_diffrn_orient_matrix_UB_12      0.0380378000
_diffrn_orient_matrix_UB_13      -0.0185801000
_diffrn_orient_matrix_UB_21      0.0444776000
_diffrn_orient_matrix_UB_22      0.0184225000
_diffrn_orient_matrix_UB_23      0.0323551000
_diffrn_orient_matrix_UB_31      0.0653268000
_diffrn_orient_matrix_UB_32      -0.0046915000
_diffrn_orient_matrix_UB_33      -0.0237444000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12231
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.747
_diffrn_reflns_theta_min         2.300
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.076
_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     278
_refine_ls_number_reflns         5650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0308P)^2^+0.6994P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4507
_reflns_number_total             5650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01122d2.cif
_cod_data_source_block           ec60a
_cod_original_cell_volume        2368.62(15)
_cod_database_code               7714426
_chemical_oxdiff_formula         'C11 H25 Ru S3 N3 Cl O3'
_reflns_odcompleteness_completeness 99.94
_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), C2(H2), C1(H1), C3(H3A)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C),
 C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              2590
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.176
_oxdiff_exptl_absorpt_empirical_full_min 0.914