Copper phenanthroline for selective electrochemical CO<sub>2</sub> reduction on carbon paper.
Du, Jiehao; Cheng, Banggui; Jiang, Long; Han, Zhiji; Chemical communications (Cambridge, England) 59 (2023) 4778–4781; doi:10.1039/d2cc06943a

data_7131460
_publ_section_title
;
 Copper phenanthroline for selective electrochemical CO<sub>2</sub>
 reduction on carbon paper.
;
_journal_issue                   32
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4778
_journal_page_last               4781
_journal_paper_doi               10.1039/d2cc06943a
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'Cl, C17 H12 N3'
_chemical_formula_sum            'C17 H12 Cl N3'
_chemical_formula_weight         293.75
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-09-20 deposited with the CCDC.	2023-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                98.018(11)
_cell_angle_beta                 98.510(9)
_cell_angle_gamma                96.695(10)
_cell_formula_units_Z            2
_cell_length_a                   6.9329(7)
_cell_length_b                   10.2901(14)
_cell_length_c                   11.7596(14)
_cell_measurement_reflns_used    1881
_cell_measurement_temperature    149.98(10)
_cell_measurement_theta_max      73.0480
_cell_measurement_theta_min      3.8150
_cell_volume                     813.48(17)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      149.98(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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   -115.00 -35.00   1.00    4.00    --  -41.14 -38.00 150.00   80
  2  \w   -113.00  -8.00   1.00    4.00    --  -41.14 -19.00-150.00  105
  3  \w    -92.00  -4.00   1.00    4.00    --  -41.14 125.00 -60.00   88
  4  \w     25.00  50.00   1.00    4.00    --   41.14-125.00 120.00   25
  5  \w     41.00  87.00   1.00    4.00    --   41.14-125.00-150.00   46
  6  \w     45.00 109.00   1.00   16.00    --  106.54 -94.00 -30.00   64
  7  \w     79.00 174.00   1.00   16.00    --  106.54  30.00   0.00   95
  8  \w     48.00  81.00   1.00   16.00    --  106.54 -45.00 -60.00   33
  9  \w     34.00 117.00   1.00   16.00    --  106.54-125.00-180.00   83
 10  \w     87.00 174.00   1.00   16.00    --  106.54  45.00-120.00   87
 11  \w     35.00 134.00   1.00   16.00    --  106.54 -61.00 150.00   99
 12  \w    104.00 174.00   1.00   16.00    --  106.54 125.00-180.00   70
 13  \w     79.00 109.00   1.00   16.00    --  106.54  61.00 -60.00   30
 14  \w    140.00 172.00   1.00   16.00    --  106.54  61.00 -60.00   32
 15  \w     35.00  62.00   1.00   16.00    --  106.54 -61.00   0.00   27
 16  \w     74.00 109.00   1.00   16.00    --  106.54 -94.00-120.00   35
 17  \w     90.00 130.00   1.00   16.00    --  106.54 -61.00   0.00   40
 18  \w     97.00 159.00   1.00   16.00    --  106.54  30.00 -60.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1360029000
_diffrn_orient_matrix_UB_12      -0.0186911000
_diffrn_orient_matrix_UB_13      -0.0916679000
_diffrn_orient_matrix_UB_21      -0.1721026000
_diffrn_orient_matrix_UB_22      0.0081223000
_diffrn_orient_matrix_UB_23      -0.0967596000
_diffrn_orient_matrix_UB_31      0.0581190000
_diffrn_orient_matrix_UB_32      0.1513319000
_diffrn_orient_matrix_UB_33      0.0154769000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4388
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        62.999
_diffrn_reflns_theta_max         62.999
_diffrn_reflns_theta_min         4.382
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.039
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       prism
_exptl_crystal_F_000             304
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.1000
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1879P)^2^+0.4580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2689
_refine_ls_wR_factor_ref         0.2833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2024
_reflns_number_total             2544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc06943a2.cif
_cod_data_source_block           exp_2203
_cod_depositor_comments
'Adding full bibliography for 7131459--7131460.cif.'
_cod_database_code               7131460
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     RED
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.535
_reflns_odcompleteness_completeness 99.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Cl1(0.85) Cl1A(0.15)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17)
;
_olex2_date_sample_data_collection 2021-10-01
_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 1.853
_oxdiff_exptl_absorpt_empirical_full_min 0.448