Bio-inspired bimetallic models for electrochemical CO<sub>2</sub> reduction.
Feng, Weifang; Xiong, Ying; Zhang, Ping; Li, Minghong; Zhang, Yaping; Li, Fei; Chen, Lin; Dalton transactions (Cambridge, England : 2003) 53 (2024) 8604–8607; doi:10.1039/d4dt00858h

data_7715764
_publ_section_title
;
 Bio-inspired bimetallic models for electrochemical CO<sub>2</sub>
 reduction.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8604
_journal_page_last               8607
_journal_paper_doi               10.1039/d4dt00858h
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C32 H35 Cl N3 O9 Re'
_chemical_formula_sum            'C32 H35 Cl N3 O9 Re'
_chemical_formula_weight         827.28
_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   geom
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc2gvmxw
_audit_creation_date             2023-08-18
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-08-21 deposited with the CCDC.	2024-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                80.945(2)
_cell_angle_beta                 80.953(2)
_cell_angle_gamma                75.907(2)
_cell_formula_units_Z            2
_cell_length_a                   10.0720(2)
_cell_length_b                   10.7211(3)
_cell_length_c                   15.6647(4)
_cell_measurement_reflns_used    16567
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      76.8390
_cell_measurement_theta_min      4.2620
_cell_volume                     1607.63(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -7.00  25.00   0.50    0.30    --  -48.28  19.00 120.00   64
  2  \w    -21.00  26.00   0.50    0.30    --  -48.28  19.00   0.00   94
  3  \w    -22.00  16.00   0.50    0.30    --  -48.28  19.00 -90.00   76
  4  \w     29.00 120.00   0.50    0.30    --   48.28  77.00   0.00  182
  5  \w    132.00 166.00   0.50    0.50    --  105.91  19.00 120.00   68
  6  \w    101.00 127.00   0.50    0.50    --  105.91  19.00 120.00   52
  7  \w     98.00 173.00   0.50    0.50    --  105.91  38.00   0.00  150
  8  \w     65.00 120.00   0.50    0.30    --   48.28 145.00  -2.00  110
  9  \w     93.00 118.00   0.50    0.50    --  105.91 145.00  -2.00   50
 10  \w     77.00 135.00   0.50    0.50    --  105.91 127.00-170.00  116
 11  \w     34.00  68.00   0.50    0.50    --  105.91 -57.00 -90.00   68
 12  \w     34.00  66.00   0.50    0.50    --  105.91 -57.00 -60.00   64
 13  \w     43.00  68.00   0.50    0.50    --  105.91 -57.00   0.00   50
 14  \w    -13.00  26.00   0.50    0.30    --   48.28 -19.00  30.00   78
 15  \w    -23.00  28.00   0.50    0.30    --   48.28 -19.00  90.00  102
 16  \w     34.00  67.00   0.50    0.50    --  105.91 -57.00 120.00   66
 17  \w     59.00  85.00   0.50    0.50    --  105.91 -77.00  90.00   52
 18  \w     81.00 106.00   0.50    0.50    --  105.91 -99.00 120.00   50
 19  \w     64.00 106.00   0.50    0.50    --  105.91-127.00 113.00   84
 20  \w     55.00  95.00   0.50    0.30    --   48.28-127.00 113.00   80
 21  \w     41.00 108.00   0.50    0.50    --  105.91-107.00 124.23  134
 22  \w     66.00 104.00   0.50    0.30    --   48.28-145.00 -55.00   76
 23  \w     62.00  96.00   0.50    0.50    --  105.91-125.00-150.00   68
 24  \w     95.00 126.00   0.50    0.50    --  105.91-145.00 -55.00   62
 25  \w     38.00  91.00   0.50    0.50    --  105.91-145.00 -55.00  106
 26  \w     59.00 105.00   0.50    0.50    --  105.91 -99.00 -30.00   92
 27  \w    -72.00 -44.00   0.50    0.30    --  -48.28 145.00  -2.00   56
 28  \w    -73.00 -35.00   0.50    0.50    -- -104.00 125.00 -30.00   76
 29  \w   -126.00 -32.00   0.50    0.50    -- -104.00 145.00  -2.00  188
 30  \w   -109.00 -83.00   0.50    0.50    -- -104.00 125.00 -30.00   52
 31  \w   -105.00 -73.00   0.50    0.50    -- -104.00 127.00-170.00   64
 32  \w    -80.00 -54.00   0.50    0.30    --  -48.28 127.00-170.00   52
 33  \w    -60.00 -32.00   0.50    0.50    -- -104.00  57.00 -30.00   56
 34  \w    -81.00 -33.00   0.50    0.50    -- -104.00  77.00  30.00   96
 35  \w    -64.00 -33.00   0.50    0.50    -- -104.00  57.00-120.00   62
 36  \w    -64.00 -39.00   0.50    0.50    -- -104.00  57.00-150.00   50
 37  \w    -64.00 -32.00   0.50    0.50    -- -104.00  57.00-180.00   64
 38  \w   -175.00 -95.00   0.50    0.50    -- -104.00 -38.00-180.00  160
 39  \w   -173.00-135.00   0.50    0.50    -- -104.00-125.00-180.00   76
 40  \w   -110.00 -74.00   0.50    0.50    -- -104.00-125.00-180.00   72
 41  \w   -116.00 -70.00   0.50    0.30    --  -48.28-145.00 -55.00   92
 42  \w   -139.00-114.00   0.50    0.50    -- -104.00-145.00 -55.00   50
 43  \w   -126.00-100.00   0.50    0.50    -- -104.00 -99.00  60.00   52
 44  \w   -172.00 -88.00   0.50    0.50    -- -104.00-127.00 113.00  168
 45  \w   -174.00 -88.00   0.50    0.50    -- -104.00 -99.00 150.00  172
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0318395000
_diffrn_orient_matrix_UB_12      0.0259542000
_diffrn_orient_matrix_UB_13      0.0877746000
_diffrn_orient_matrix_UB_21      0.0808606000
_diffrn_orient_matrix_UB_22      0.1005334000
_diffrn_orient_matrix_UB_23      -0.0482203000
_diffrn_orient_matrix_UB_31      -0.1330669000
_diffrn_orient_matrix_UB_32      0.1073003000
_diffrn_orient_matrix_UB_33      0.0065828000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21513
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.225
_diffrn_reflns_theta_min         2.879
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.658
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.082
_refine_diff_density_min         -1.007
_refine_diff_density_rms         0.174
_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     415
_refine_ls_number_reflns         6472
_refine_ls_number_restraints     355
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0900P)^2^+1.8724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6030
_reflns_number_total             6472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00858h2.cif
_cod_data_source_block           l1
_cod_depositor_comments          'Adding full bibliography for 7715764.cif.'
_cod_database_code               7715764
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Re Cl'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O8-C31 = O9-C32
 1.15 with sigma of 0.01
 O8-C31 \\sim O9-C32
 with sigma of 0.02
 Re1-C31 \\sim Re1-C32
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Re1, Cl1, O1, O2, O3, O4, O5, O6, O7, O8, O9, N1, N2, N3, C1, H1A, H1B, C2,
 H2A, H2B, C3, H3A, H3B, C4, H4A, H4B, C5, H5A, H5B, C6, H6A, H6B, C7, H7A, H7B,
  C8, H8A, H8B, C9, H9A, H9B, C10, H10A, H10B, C11, H11A, H11B, C12, H12A, H12B,
  C13, C14, C15, H15, C16, H16, C17, H17, C18, H18, C19, C20, C21, H21, C22,
 H22, C23, H23, C24, C25, C26, H26, C27, H27, C28, H28, C29, H29, C30, C31, C32
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
 C26(H26), C27(H27), C28(H28), C29(H29)
;
_shelx_res_checksum              37177
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.595
_oxdiff_exptl_absorpt_empirical_full_min 0.385