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_4134906
_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         'C30 H24 N6 O Ru, 2(F6 P), C6 H4'
_chemical_formula_sum            'C36 H28 F12 N6 O P2 Ru'
_chemical_formula_weight         951.65
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.5370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0390(2)
_cell_length_b                   24.3020(5)
_cell_length_c                   13.6393(3)
_cell_measurement_reflns_used    9205
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.110
_cell_measurement_theta_min      3.638
_cell_volume                     3618.47(13)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.979
_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  0.0361
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29673
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.275
_diffrn_reflns_theta_min         3.637
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.288
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0704 before and 0.0452 after correction. The Ratio of minimum to maximum transmission is 0.7120. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       needle
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.248
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         7004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+5.8620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6312
_reflns_number_total             7004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02912_si_002.cif
_cod_data_source_block           x1710003
_cod_database_code               4134906
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.680
_shelx_estimated_absorpt_t_min   0.354
_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. Rigid bond restraints
3. Uiso/Uaniso restraints and constraints
Uanis(F8A) \\sim Ueq: with sigma of 0 and sigma for terminal atoms of 0
Uanis(F17) = Uanis(F18)
Uanis(F9) = Uanis(F10)
Uanis(F8A) = Uanis(F11)
4. Others
 Sof(F11)=1-FVAR(1)
 Sof(F12)=FVAR(1)
 Sof(F13)=1-FVAR(2)
 Sof(F14)=FVAR(2)
 Sof(F9)=1-FVAR(3)
 Sof(F10)=FVAR(3)
 Sof(F17)=1-FVAR(4)
 Sof(F18)=FVAR(4)
 Sof(F16)=1-FVAR(5)
 Sof(F15)=FVAR(5)
 Sof(F8A)=1-FVAR(6)
 Sof(F8)=FVAR(6)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C29(H29), C8(H8), C9(H9), C24(H24), C28(H28), C23(H23), C17(H17),
 C18(H18), C22(H22), C6(H6), C30(H30), C16(H16), C7(H7), C19(H19), C12(H12),
 C13(H13), C14(H14), C15(H15)
5.c X=CH2 refined with riding coordinates:
 C33(H33A,H33B), C36(H36A,H36B)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'