Electrocatalytic CO2 Reduction by Imidazolium-Functionalized Molecular Catalysts.
Sung, Siyoung; Kumar, Davinder; Gil-Sepulcre, Marcos; Nippe, Michael; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b07709

data_4126486
_publ_section_title
;
 Electrocatalytic CO2 Reduction by Imidazolium-Functionalized Molecular
 Catalysts.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b07709
_journal_year                    2017
_chemical_formula_moiety         'C19 H17 Cl N4 O3 Re, F6 P'
_chemical_formula_sum            'C19 H17 Cl F6 N4 O3 P Re'
_chemical_formula_weight         715.98
_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'
_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
_audit_creation_date             2016-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.269(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.275(4)
_cell_length_b                   7.969(2)
_cell_length_c                   23.509(7)
_cell_measurement_reflns_used    76975
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.6150
_cell_measurement_theta_min      3.6496
_cell_volume                     2295.9(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0684
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            72193
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.641
_diffrn_reflns_theta_min         3.650
_exptl_absorpt_coefficient_mu    5.558
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.4659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.071
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.565
_refine_diff_density_min         -2.162
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         6446
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0146P)^2^+19.2059P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6001
_reflns_number_total             6446
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b07709_si_002.cif
_cod_data_source_block           Compound1
_cod_database_code               4126486
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.851
_shelx_estimated_absorpt_t_min   0.808
_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. Uiso/Uaniso restraints and constraints
Uanis(F5A) = Uanis(F2A) = Uanis(F6A) = Uanis(F1A) = Uanis(F4) = Uanis(F5) =
Uanis(F6) = Uanis(F1) = Uanis(F2) = Uanis(F3) = Uanis(F4A) = Uanis(F3A)
3. Others
 Fixed Sof: F1(0.7608) F2(0.7608) F3(0.7608) F4(0.7608) F5(0.7608) F6(0.7608)
 F6A(0.2392) F3A(0.2392) F2A(0.2392) F5A(0.2392) F1A(0.2392) F4A(0.2392)
4.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17),
 C18(H18)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              90185
_shelx_hkl_checksum              68704
_olex2_submission_special_instructions 'No special instructions were received'