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_7711655
_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 H15 Cl N3 O3 Re'
_chemical_formula_sum            'C23 H15 Cl N3 O3 Re'
_chemical_formula_weight         603.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-27 deposited with the CCDC.	2022-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.6390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7750(9)
_cell_length_b                   15.4255(12)
_cell_length_c                   12.1047(9)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      30.42
_cell_measurement_theta_min      2.22
_cell_volume                     2127.3(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_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_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25903
_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         27.876
_diffrn_reflns_theta_min         2.156
_exptl_absorpt_coefficient_mu    5.868
_exptl_absorpt_correction_T_max  0.6606
_exptl_absorpt_correction_T_min  0.4757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0547 before and 0.0460 after correction.
The Ratio of minimum to maximum transmission is 0.7198.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.883
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1160
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM:pentane'
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.162
_exptl_crystal_size_min          0.122
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.8236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0606
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4095
_reflns_number_total             5077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02876j2.cif
_cod_data_source_block           zd-k33
_cod_database_code               7711655
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.535
_shelx_estimated_absorpt_t_min   0.405
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14),
 C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
;
_shelx_res_checksum              56108
_shelx_hkl_checksum              49583
_olex2_submission_special_instructions 'No special instructions were received'