Transformation of carbon dioxide catalyzed using an N-heterocyclic carbene copper(i)-embedded metal–organic framework
You, Li-Xin; Wang, Xin-Yu; Li, Jin-Rong; Guo, Jie; Xiong, Gang; ding, Fu; Sun, Ya-Guang; CrystEngComm 27 (2025) 5625–5632; doi:10.1039/D5CE00627A

data_7250697
_publ_section_title
;
 Transformation of carbon dioxide catalyzed using an N-heterocyclic
 carbene copper(i)-embedded metal--organic framework
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              5625
_journal_page_last               5632
_journal_paper_doi               10.1039/D5CE00627A
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety
'0.25(C320 H272 N32 O68 Zn16), 4(H2 O), 2(N O3)'
_chemical_formula_sum            'C80 H76 N10 O27 Zn4'
_chemical_formula_weight         1870.98
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-06-18
_audit_creation_method
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_audit_update_record
;
2025-06-19 deposited with the CCDC.	2025-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.8779(6)
_cell_length_b                   25.8779(6)
_cell_length_c                   11.7846(5)
_cell_measurement_reflns_used    7432
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      23.4560
_cell_measurement_theta_min      2.2900
_cell_volume                     7891.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.105a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      4.00  30.00   0.50   33.12    --    9.80  21.00  72.00   52
  2  \w    -35.00 -10.00   0.50   33.12    --  -10.50 -21.00 -93.00   50
  3  \w    -14.00  40.00   0.50   33.12    --    9.80  77.00-150.00  108
  4  \w     45.00  97.00   0.50   33.12    --    9.80  77.00-150.00  104
  5  \w    -56.00  40.00   0.50   33.12    --    9.80 -57.00   0.00  192
  6  \w    -23.00   3.00   0.50   33.12    --  -10.50  77.00   0.00   52
  7  \w    -53.00 -12.00   0.50   33.12    --  -10.50 -77.00-150.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Pro II AFC12 (RINC): Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0085335000
_diffrn_orient_matrix_UB_12      -0.0248501000
_diffrn_orient_matrix_UB_13      0.0169046000
_diffrn_orient_matrix_UB_21      -0.0259984000
_diffrn_orient_matrix_UB_22      0.0085019000
_diffrn_orient_matrix_UB_23      -0.0031064000
_diffrn_orient_matrix_UB_31      -0.0010774000
_diffrn_orient_matrix_UB_32      -0.0077527000
_diffrn_orient_matrix_UB_33      -0.0577977000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19299
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.007
_diffrn_reflns_theta_max         25.007
_diffrn_reflns_theta_min         1.899
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38168
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.105a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       prism
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         1.479
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         3458
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.1426
_refine_ls_R_factor_gt           0.1196
_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^)+(0.2600P)^2^+20.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3583
_refine_ls_wR_factor_ref         0.3892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2585
_reflns_number_total             3458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00627a2.cif
_cod_data_source_block           20250604a_auto
_cod_depositor_comments          'Adding full bibliography for 7250697.cif.'
_cod_original_cell_volume        7891.7(5)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7250697
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H O N Zn'
_chemical_oxdiff_usercomment     'YOULIXIN wangxinyu-'
_diffrn_oxdiff_digest_frames
;
0136632bff5ba8ad7d546527ca9352b0320002567f5
;
_diffrn_oxdiff_digest_hkl
;
0100776310e0a99227340bb453f9a39ea363aa
;
_reflns_odcompleteness_completeness 99.39
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 O9-N3
 1.3 with sigma of 0.01
 O10-N3
 1.3 with sigma of 0.01
 O8-N3
 1.3 with sigma of 0.01
 C20-C17
 1.5 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
O8 \\sim O9 \\sim N3 \\sim O10: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 2A
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O3) = Uanis(O2)
3. Others
 Sof(Zn)=1-FVAR(1)
 Sof(Zn1)=FVAR(1)
 Sof(O2)=1-FVAR(2)
 Sof(O3)=FVAR(2)
 Fixed Sof: O9(0.5) N3(0.5) O8(0.5) O10(0.5)
4.a Free rotating group:
 O1AA(H1AA,H1AB)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C8(H8A,H8B)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C9(H9), C19(H19), C18(H18), C16(H16), C10(H10), C6(H6), C3(H3),
 C4(H4), C7(H7)
4.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              34499
_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 1.543
_oxdiff_exptl_absorpt_empirical_full_min 0.613