Two Zr-based heterometal–organic frameworks for efficient CO2 reduction under visible light
Wang, Ying; Fu, Yaomei; You, Siqi; Li, Xuexin; Zhao, Liang; Qin, Chao; Wang, Xinlong; CrystEngComm 23 (2021) 8115–8120; doi:10.1039/D1CE01198G

data_7243870
_publ_section_title
;
 Two Zr-based heterometal--organic frameworks for efficient CO2 reduction
 under visible light
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              8115
_journal_page_last               8120
_journal_paper_doi               10.1039/D1CE01198G
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety
'C33 H29 Cl N3 Ni O13 Zr3, 2(Cl), 1[C3H7NO], 5[H2O]'
_chemical_formula_sum            'C36 H52 Cl3 N4 Ni O19 Zr3'
_chemical_formula_weight         1283.53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-21
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.06.29 svn.r12e2184c for OlexSys, GUI svn.r6374)
;
_audit_update_record
;
2021-07-31 deposited with the CCDC.	2021-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.510(4)
_cell_length_b                   16.988(7)
_cell_length_c                   29.610(12)
_cell_measurement_reflns_used    4703
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.953
_cell_volume                     5287(4)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.02
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker D8 VENTURE'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker D8 VENTURE'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1561
_diffrn_reflns_av_unetI/netI     0.1407
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            39850
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.172
_diffrn_reflns_theta_max         25.172
_diffrn_reflns_theta_min         2.380
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.147
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.115
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.46(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         9415
_refine_ls_number_restraints     1146
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1168
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0509P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1264
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                5846
_reflns_number_total             9415
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01198g2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7243869--7243870.cif.'
_cod_database_code               7243870
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.54(5)
 0.46(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
3. Uiso/Uaniso restraints and constraints
C1 \\sim C4 \\sim C6 \\sim C7 \\sim C2 \\sim C15 \\sim C29 \\sim C31 \\sim C8
\\sim C9 \\sim C5 \\sim C11 \\sim C19 \\sim C21 \\sim C10 \\sim C12 \\sim C14
\\sim C16 \\sim C18 \\sim C20 \\sim C22 \\sim C23 \\sim C3 \\sim C13 \\sim C25
\\sim C27 \\sim C24 \\sim C26 \\sim C28 \\sim C30 \\sim C32 \\sim C34 \\sim C36
\\sim O1 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O8 \\sim O9 \\sim O10 \\sim
O11 \\sim O12 \\sim O14 \\sim O16 \\sim O18 \\sim N1 \\sim N2 \\sim N4: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03 within 3.8A
4.a :
 C7(C2,C15,C29,C31), C9(C5,C11,C19,C21), C23(C3,C13,C25,C27)
4.b Aromatic/amide H refined with riding coordinates:
 O14(H14), O16(H16), O18(H18), N2(H2), C4(H4), C7(H7), C2(H2A), C15(H15),
 C29(H29), C31(H31), C9(H9), C5(H5), C11(H11), C19(H19), C21(H21), C10(H10),
 C14(H14A), C16(H16A), C20(H20), C22(H22), C23(H23), C3(H3), C13(H13), C25(H25),
  C27(H27), C26(H26), C28(H28), C32(H32), C34(H34)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82321
_shelx_hkl_checksum              61697
_shelx_fab_checksum              1335
_olex2_submission_special_instructions 'No special instructions were received'