Electrocatalytic properties of a novel ruthenium(II) terpyridine-based complex towards CO2 reduction
Faustino, Leandro A.; Machado, Antonio; da Silva Maia, Pedro Ivo; Concepcion, Javier; Patrocinio, Antonio Otavio; Dalton Transactions  (2023) –; doi:10.1039/D3DT00121K

data_7712535
_publ_section_title
;
 Electrocatalytic properties of a novel ruthenium(II) terpyridine-based
 complex towards CO2 reduction
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00121K
_journal_year                    2023
_chemical_formula_moiety         'C22 H17 Cl N4 O2 Ru, 2(H2 O)'
_chemical_formula_sum            'C22 H21 Cl N4 O4 Ru'
_chemical_formula_weight         541.95
_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     direct
_audit_creation_date             2022-12-03
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-03 deposited with the CCDC.	2023-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                92.649(8)
_cell_angle_beta                 99.764(7)
_cell_angle_gamma                98.885(7)
_cell_formula_units_Z            2
_cell_length_a                   8.9094(8)
_cell_length_b                   8.9354(9)
_cell_length_c                   13.7859(13)
_cell_measurement_reflns_used    12719
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      4.70
_cell_volume                     1065.65(18)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
 215 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11922
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.160
_diffrn_reflns_theta_min         4.762
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_description       Plate
_exptl_crystal_F_000             548
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2 and MeOH'
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.957
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5673
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0326
_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^)+(0.0383P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4518
_reflns_number_total             5673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00121k2.cif
_cod_data_source_block           pirutpi
_cod_database_code               7712535
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 H1SB-O1S
 0.9 with sigma of 0.02
 O1S-H1SA
 0.9 with sigma of 0.02
 H2SB-O2S
 0.9 with sigma of 0.02
 O2S-H2SA
 0.9 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C22(H22), C23(H23), C4(H4), C32(H32), C27(H27), C34(H34), C33(H33),
 C1(H1), C24(H24), C21(H21), C28(H28), C35(H35), C2(H2), C3(H3)
;
_shelx_res_checksum              77159
_shelx_hkl_checksum              40001
_olex2_submission_special_instructions 'No special instructions were received'