Kinetics of the <i>Trans</i> Effect in Ruthenium Complexes Provide Insight into the Factors That Control Activity and Stability in CO<sub>2</sub> Electroreduction.
Gonell, Sergio; Assaf, Eric A.; Duffee, Kyle D.; Schauer, Cynthia K.; Miller, Alexander J. M.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c02912

data_4134904
_publ_section_title
;
 Kinetics of the <i>Trans</i> Effect in Ruthenium Complexes Provide
 Insight into the Factors That Control Activity and Stability in
 CO<sub>2</sub> Electroreduction.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c02912
_journal_year                    2020
_chemical_formula_moiety         'C29 H24 Cl N6 Ru, F6 P, 2(C3 H6 O), C2 H2 O'
_chemical_formula_sum            'C37 H38 Cl F6 N6 O3 P Ru'
_chemical_formula_weight         896.22
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                82.514(3)
_cell_angle_beta                 79.563(2)
_cell_angle_gamma                81.077(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7791(3)
_cell_length_b                   11.6967(4)
_cell_length_c                   18.8185(6)
_cell_measurement_reflns_used    7906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.601
_cell_measurement_theta_min      2.40
_cell_volume                     1867.02(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22339
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        66.710
_diffrn_reflns_theta_max         66.710
_diffrn_reflns_theta_min         2.401
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.132
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0951 before and 0.0654 after correction. The Ratio of minimum to maximum transmission is 0.8116. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       Prism
_exptl_crystal_F_000             912
_refine_diff_density_max         2.344
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         6344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0692
_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^)+(0.0867P)^2^+8.9923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5144
_reflns_number_total             6344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02912_si_003.cif
_cod_data_source_block           x1707006_1
_cod_database_code               4134904
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C38(H38A,H38B)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C23(H23), C8(H8), C28(H28), C29(H29), C21(H21), C14(H14), C22(H22),
 C6(H6), C17(H17), C13(H13), C26(H26), C27(H27), C11(H11), C15(H15), C7(H7),
 C12(H12), C5(H5), C18(H18)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C2(H2A,H2B,H2C), C35(H35A,H35B,
 H35C), C33(H33A,H33B,H33C)
;
_olex2_submission_special_instructions 'No special instructions were received'