Nickel Metal-Organic Frameworks for Visible-Light CO2 Reduction under Mild Reaction Conditions
Chen, Liuyong; Yang, Jun; Yang, Wenqian; Xian, Jiahui; Li, Guangqin; Dalton Transactions  (2022) –; doi:10.1039/D2DT01022D

data_7710103
_publ_section_title
;
 Nickel Metal-Organic Frameworks for Visible-Light CO2 Reduction under
 Mild Reaction Conditions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01022D
_journal_year                    2022
_chemical_formula_moiety         'C32 H12 N4 Ni4 O21.333'
_chemical_formula_sum            'C32 H12 N4 Ni4 O21.33'
_chemical_formula_weight         1028.63
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-22
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2022-01-19 deposited with the CCDC.	2022-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   31.3566(3)
_cell_length_b                   31.3566(3)
_cell_length_c                   38.3643(5)
_cell_measurement_reflns_used    25444
_cell_measurement_temperature    240.00(10)
_cell_measurement_theta_max      72.5790
_cell_measurement_theta_min      3.9810
_cell_volume                     32667.5(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      240.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.918
_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   -112.00 -33.00   1.00   15.00    --  -40.20 -38.00-180.00   79
  2  \w   -116.00   0.00   1.00   15.00    --  -40.20 -19.00  60.00  116
  3  \w   -113.00 -76.00   1.00   15.00    --  -40.20-148.00 -84.00   37
  4  \w      6.00  36.00   1.00   15.00    --   40.20 -99.00 -30.00   30
  5  \w     14.00  77.00   1.00   15.00    --   40.20 -99.00 150.00   63
  6  \w     52.00  80.00   1.00   15.00    --   40.20 -99.00 -30.00   28
  7  \w     36.00  78.00   1.00   15.00    --   40.20-125.00 -30.00   42
  8  \w    100.00 150.00   1.00   40.00    --  103.61  30.00 -30.00   50
  9  \w     30.00 113.00   1.00   40.00    --  103.61-125.00  90.00   83
 10  \w     77.00 103.00   1.00   40.00    --  103.61  61.00-180.00   26
 11  \w    108.00 161.00   1.00   40.00    --  103.61  77.00 120.00   53
 12  \w     83.00 161.00   1.00   40.00    --  103.61  45.00   0.00   78
 13  \w     40.00  77.00   1.00   40.00    --  103.61 -77.00-120.00   37
 14  \w     27.00  65.00   1.00   40.00    --  103.61 -77.00  90.00   38
 15  \w    126.00 166.00   1.00   40.00    --  103.61  61.00  60.00   40
 16  \w    123.00 176.00   1.00   40.00    --  103.61  61.00 150.00   53
 17  \w     82.00 170.00   1.00   40.00    --  103.61  61.00-150.00   88
 18  \w     89.00 114.00   1.00   40.00    --  103.61  61.00 150.00   25
 19  \w     94.00 136.00   1.00   40.00    --  103.61 -77.00  90.00   42
 20  \w     81.00 165.00   1.00   40.00    --  103.61  30.00 -90.00   84
 21  \w     80.00 124.00   1.00   40.00    --  103.61  45.00-150.00   44
 22  \w    106.00 158.00   1.00   40.00    --  103.61  77.00  30.00   52
 23  \w    130.00 174.00   1.00   40.00    --  103.61 125.00 120.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0331000000
_diffrn_orient_matrix_UB_12      0.0187313000
_diffrn_orient_matrix_UB_13      -0.0152409000
_diffrn_orient_matrix_UB_21      -0.0439492333
_diffrn_orient_matrix_UB_22      -0.0391841667
_diffrn_orient_matrix_UB_23      0.0210987333
_diffrn_orient_matrix_UB_31      0.0138588000
_diffrn_orient_matrix_UB_32      0.0364815000
_diffrn_orient_matrix_UB_33      0.0305600000
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            65579
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.002
_diffrn_reflns_theta_min         3.453
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.604
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.941
_exptl_crystal_description       block
_exptl_crystal_F_000             9264
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.879
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       0.000085(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         14271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1288P)^2^+196.3417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12397
_reflns_number_total             14271
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01022d2.cif
_cod_data_source_block           exp_4716
_cod_original_cell_volume        32667.5(8)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7710103
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Co'
_shelx_estimated_absorpt_t_max   0.795
_shelx_estimated_absorpt_t_min   0.719
_reflns_odcompleteness_completeness 99.46
_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.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C18(H18), C44(H44), C10(H10), C46(H46), C20(H20), C12(H12),
 C34(H34), C42(H42), C38(H38), C8(H8), C16(H16)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24233
_shelx_hkl_checksum              99672
_shelx_fab_checksum              8490
_olex2_date_sample_data_collection 2020-10-17
_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 2.365
_oxdiff_exptl_absorpt_empirical_full_min 0.785