Solar energy-driven electrolysis with molecular catalysts for the reduction of carbon dioxide coupled with the oxidation of 5-hydroxymethylfurfural
Yang, Zhi-Wen; Chen, Jin-Mei; Qiu, Li-Qi; Xie, Wen-Jun; He, Liang-Nian; Catalysis Science & Technology 12 (2022) 5495–5500; doi:10.1039/D2CY01195F

data_1567446
_publ_section_title
;
 Solar energy-driven electrolysis with molecular catalysts for the
 reduction of carbon dioxide coupled with the oxidation of
 5-hydroxymethylfurfural
;
_journal_issue                   18
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              5495
_journal_page_last               5500
_journal_paper_doi               10.1039/D2CY01195F
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C29 H33 N2 O2'
_chemical_formula_sum            'C29 H33 N2 O2'
_chemical_formula_weight         441.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc29lynj
_audit_creation_date             2021-11-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-10 deposited with the CCDC.	2022-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.408(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6047(9)
_cell_length_b                   11.4378(5)
_cell_length_c                   10.1417(5)
_cell_measurement_reflns_used    9256
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      31.2620
_cell_measurement_theta_min      2.0620
_cell_volume                     2388.01(19)
_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_temperature      113.15
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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   -120.00  60.00   0.50    3.00    --  -30.00  45.00   0.00  360
  2  \w   -120.00  60.00   0.50    3.00    --  -30.00  45.00  90.00  360
  3  \w   -120.00  60.00   0.50    3.00    --  -30.00  45.00 180.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku Saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0334068000
_diffrn_orient_matrix_UB_12      -0.0050210000
_diffrn_orient_matrix_UB_13      -0.0192530000
_diffrn_orient_matrix_UB_21      -0.0014309000
_diffrn_orient_matrix_UB_22      0.0610411000
_diffrn_orient_matrix_UB_23      -0.0120781000
_diffrn_orient_matrix_UB_31      0.0083971000
_diffrn_orient_matrix_UB_32      -0.0096162000
_diffrn_orient_matrix_UB_33      -0.0661933000
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8054
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         1.978
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)'
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       block
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.0074(19)
_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   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         8054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0649
_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^)+(0.1159P)^2^+0.1083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1663
_refine_ls_wR_factor_ref         0.1760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6073
_reflns_number_total             8054
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9800\% 
 around [-0.09 0.00 1.00] (reciprocal) or [0.00 0.00 1.00] (direct)
;
_cod_data_source_file            d2cy01195f2.cif
_cod_data_source_block           r20211109a_twin1_hklf4
_cod_depositor_comments          'Adding full bibliography for 1567446.cif.'
_cod_database_code               1567446
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.983
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6880(13)
 0.3120(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C21(H21)
3.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C22(H22A,H22B), C25(H25A,H25B)
3.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C14(H14),
 C15(H15)
3.d Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C)
;
_shelx_res_checksum              49588
_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 2.234
_oxdiff_exptl_absorpt_empirical_full_min 0.310
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2