Structural investigations into the deactivation pathway of the CO2 reduction electrocatalyst Re(bpy)(CO)3Cl
Eric Benson; Clifford Kubiak; Chem.Commun. 48 (2012) 7374–; doi:10.1039/c2cc32617e

data_7108008
_publ_section_title
;
 Structural investigations into the deactivation pathway of the CO2
 reduction electrocatalyst Re(bpy)(CO)3Cl
;
_journal_name_full               Chem.Commun.
_journal_page_first              7374
_journal_paper_doi               10.1039/c2cc32617e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C29 H40 K N2 O10 Re'
_chemical_formula_weight         801.94
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 73.240(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.3023(13)
_cell_length_b                   18.0705(9)
_cell_length_c                   16.0034(8)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.51
_cell_measurement_theta_min      2.79
_cell_volume                     6452.5(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44779
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.56
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    3.952
_exptl_absorpt_correction_T_max  0.6933
_exptl_absorpt_correction_T_min  0.5054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.705
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     798
_refine_ls_number_reflns         11977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0131P)^2^+15.2106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0578
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                8870
_reflns_number_total             11977
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32617e.txt
_cod_data_source_block           '[Re(bpy)(CO)3][K(18-crown-6)(THF)]'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7108008