Electrocatalyst decomposition pathways: torsional strain in a second sphere proton relay shuts off CO2RR in a Re(2,2’-bipyridyl)(CO)3X type electrocatalyst
Dubrawski, Zack; Chang, Chia Yun; Carr, Cody; Gelfand, Benjamin Sidney; Piers, Warren; Dalton Transactions  (2022) –; doi:10.1039/D2DT02876J

data_7711656
_publ_section_title
;
 Electrocatalyst decomposition pathways: torsional strain in a second
 sphere proton relay shuts off CO2RR in a Re(2,2&#x2019;-bipyridyl)(CO)3X
 type electrocatalyst
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02876J
_journal_year                    2022
_chemical_formula_moiety         'C23 H18 N3 O3 Re, C6 D6'
_chemical_formula_sum            'C29 H18 D6 N3 O3 Re'
_chemical_formula_weight         654.75
_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     dual
_audit_creation_date             2022-02-10
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-05-27 deposited with the CCDC.	2022-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                81.0430(10)
_cell_angle_beta                 80.2040(10)
_cell_angle_gamma                67.7730(10)
_cell_formula_units_Z            2
_cell_length_a                   9.6071(9)
_cell_length_b                   11.7517(10)
_cell_length_c                   12.1793(11)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      30.042
_cell_measurement_theta_min      2.307
_cell_volume                     1248.00(19)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18767
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.277
_diffrn_reflns_theta_min         1.705
_diffrn_source                   'fine focus X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              Siemens
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.905
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0580 before and 0.0274 after correction.
The Ratio of minimum to maximum transmission is 0.9031.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       plank
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.847
_refine_diff_density_min         -1.044
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6183
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0259
_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^)+(0.0234P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0492
_refine_ls_wR_factor_ref         0.0516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5419
_reflns_number_total             6183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02876j2.cif
_cod_data_source_block           zd-n22
_cod_database_code               7711656
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.778
_shelx_estimated_absorpt_t_min   0.453
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
: within 1A with sigma of 0.003 and sigma for terminal atoms of 0.003 within 1A
3. Others
 Sof(C1S)=Sof(D1S)=Sof(C2S)=Sof(D2S)=Sof(C3S)=Sof(D3S)=Sof(C4S)=Sof(D4S)=
 Sof(C5S)=Sof(D5S)=Sof(C6S)=Sof(D6S)=1-FVAR(1)
 Sof(C1S)=Sof(D1S)=Sof(C2S)=Sof(D2S)=Sof(C3S)=Sof(D3S)=Sof(C4S)=Sof(D4S)=
 Sof(C5S)=Sof(D5S)=Sof(C6S)=Sof(D6S)=FVAR(1)
4.a :
 C1S(C2S,C3S,C4S,C5S,C6S), C1S(C2S,C3S,C4S,C5S,C6S)
4.b Ternary CH refined with riding coordinates:
 C18(H18)
4.c Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B)
4.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C20(H20), C21(H21), C22(H22), C23(H23), C1S(D1S), C2S(D2S), C3S(D3S), C4S(D4S),
  C5S(D5S), C6S(D6S), C1S(D1S), C2S(D2S), C3S(D3S), C4S(D4S), C5S(D5S), C6S(D6S)
;
_shelx_res_checksum              61863
_shelx_hkl_checksum              42952
_olex2_submission_special_instructions 'No special instructions were received'