Enhancing CO<sub>2</sub> electroreduction to ethylene <i>via</i> microenvironment regulation in boron-imidazolate frameworks.
Lu, Chen; Hong, Qin-Long; Zhang, Hai-Xia; Zhang, Jian; Chemical communications (Cambridge, England) 60 (2024) 10204–10207; doi:10.1039/d4cc02928c

data_7133577
_publ_section_title
;
 Enhancing CO<sub>2</sub> electroreduction to ethylene <i>via</i>
 microenvironment regulation in boron-imidazolate frameworks.
;
_journal_issue                   74
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10204
_journal_page_last               10207
_journal_paper_doi               10.1039/d4cc02928c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C17 H19 B Cu N6 O2 S'
_chemical_formula_sum            'C17 H19 B Cu N6 O2 S'
_chemical_formula_weight         445.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-12
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2024-06-13 deposited with the CCDC.	2024-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9474(2)
_cell_length_b                   8.91440(10)
_cell_length_c                   17.0439(3)
_cell_measurement_reflns_used    10783
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      60.0400
_cell_measurement_theta_min      4.5280
_cell_volume                     1960.28(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_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      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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      3.00 106.00   0.50    0.05    --   76.35 -99.00-150.00  206
  2  \w      2.00 105.00   0.50    0.05    --   76.35 -77.00-120.00  206
  3  \w     20.00 111.00   0.50    0.05    --   76.35-125.00  60.00  182
  4  \w     20.00 111.00   0.50    0.05    --   76.35-125.00 120.00  182
  5  \w      2.00  96.00   0.50    0.05    --   76.35 -57.00 120.00  188
  6  \w      2.00  96.00   0.50    0.05    --   76.35 -57.00  60.00  188
  7  \w     -1.00  71.00   0.50    0.05    --   76.35 -38.00   0.00  144
  8  \w     -1.00  71.00   0.50    0.05    --   76.35 -38.00 -30.00  144
  9  \w     53.00 154.00   0.50    0.05    --   76.35  38.00 -60.00  202
 10  \w     48.00 151.00   0.50    0.05    --   76.35  77.00-180.00  206
 11  \w     54.00 151.00   0.50    0.05    --   76.35  57.00-120.00  194
 12  \w     48.00 151.00   0.50    0.05    --   76.35  77.00 120.00  206
 13  \w    -71.00  -1.00   0.50    0.05    --  -78.22  38.00-120.00  140
 14  \w   -112.00 -20.00   0.50    0.05    --  -78.22 125.00   0.00  184
 15  \w   -112.00 -20.00   0.50    0.05    --  -78.22 125.00-120.00  184
 16  \w    -71.00  -1.00   0.50    0.05    --  -78.22  38.00 -60.00  140
 17  \w     -8.00  38.00   0.50    0.05    --   -0.94 -99.00 -60.00   92
 18  \w     -8.00  38.00   0.50    0.05    --   -0.94 -99.00 -90.00   92
 19  \w     -8.00  38.00   0.50    0.05    --   -0.94 -99.00  60.00   92
 20  \w    -74.00  28.00   0.50    0.05    --   -0.94 -77.00  90.00  204
 21  \w    -74.00  28.00   0.50    0.05    --   -0.94 -77.00 150.00  204
 22  \w   -152.00 -49.00   0.50    0.05    --  -78.22 -77.00  30.00  206
 23  \w   -152.00 -55.00   0.50    0.05    --  -78.22 -57.00  90.00  194
 24  \w    -74.00  21.00   0.50    0.05    --   -0.94 -57.00-150.00  190
 25  \w   -150.00 -79.00   0.50    0.05    --  -78.22-125.00-180.00  142
 26  \w   -152.00 -88.00   0.50    0.05    --  -78.22 -99.00-180.00  128
 27  \w   -152.00 -88.00   0.50    0.05    --  -78.22 -99.00-150.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0937090000
_diffrn_orient_matrix_UB_12      -0.0642398000
_diffrn_orient_matrix_UB_13      0.0024589000
_diffrn_orient_matrix_UB_21      -0.0406058000
_diffrn_orient_matrix_UB_22      -0.1291746000
_diffrn_orient_matrix_UB_23      0.0232274000
_diffrn_orient_matrix_UB_31      -0.0185461000
_diffrn_orient_matrix_UB_32      -0.0419825000
_diffrn_orient_matrix_UB_33      -0.0752971000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16234
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         56.886
_diffrn_reflns_theta_min         4.527
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    6.795
_exptl_absorpt_correction_T_max  0.361
_exptl_absorpt_correction_T_min  0.245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear bluish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.854
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         3732
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0923P)^2^+0.0598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.886
_reflns_Friedel_fraction_max     0.880
_reflns_number_gt                3561
_reflns_number_total             3732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02928c2.cif
_cod_data_source_block           ar14-33
_cod_depositor_comments
'Adding full bibliography for 7133576--7133579.cif.'
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               7133577
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N O B S Cu'
_shelx_estimated_absorpt_t_max   0.429
_shelx_estimated_absorpt_t_min   0.235
_diffrn_oxdiff_digest_frames
;
01b5232dd3698e17f53841f518ea95c4dd04568aeaf
;
_diffrn_oxdiff_digest_hkl
;
016c13b453773e4c069f292c5a8280b67f1ef9
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{S1, C18}
{S2, C17}
3. Uiso/Uaniso restraints and constraints
Uanis(S1) = Uanis(C18)
Uanis(S2) = Uanis(C17)
4. Others
 Sof(H14A)=Sof(C18)=Sof(H18)=1-FVAR(1)
 Sof(S1)=Sof(H14)=FVAR(1)
 Sof(H16A)=Sof(C17)=Sof(H17)=1-FVAR(2)
 Sof(S2)=Sof(H16)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 B1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C7(H7), C8(H8), C10(H10), C14(H14), C14(H14A),
 C16(H16), C16(H16A), C17(H17), C18(H18)
5.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              41906
_shelx_hkl_checksum              14990
_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 1.991
_oxdiff_exptl_absorpt_empirical_full_min 0.563