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_7243869
_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
'C66 H62 Cl2 Mn N6 O20 Zr6, 2(Cl), 2(C3 H7 N O)'
_chemical_formula_sum            'C72 H76 Cl4 Mn N8 O22 Zr6'
_chemical_formula_weight         2149.46
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                80.980(5)
_cell_angle_beta                 77.033(5)
_cell_angle_gamma                76.035(5)
_cell_formula_units_Z            1
_cell_length_a                   11.1927(10)
_cell_length_b                   12.9714(11)
_cell_length_c                   21.8377(19)
_cell_measurement_reflns_used    6963
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.953
_cell_volume                     2980.6(5)
_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 2014/5 (Sheldrick, 2014)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.2068
_diffrn_reflns_av_unetI/netI     0.1150
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73007
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.133
_diffrn_reflns_theta_max         25.133
_diffrn_reflns_theta_min         2.889
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.9
_diffrn_source_power             0.0405
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.748
_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    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1073
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         10595
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0926P)^2^+1.9322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5970
_reflns_number_total             10595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01198g2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7243869--7243870.cif.'
_cod_database_code               7243869
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C22 \\sim C19 \\sim C27 \\sim C21 \\sim C25: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.03 within 3.8A
C20 \\sim C11 \\sim C17 \\sim C15 \\sim C26: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.03 within 3.8A
Uanis(C32) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 O3(H3), O2(H2), O4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
  C21(H21), C22(H22), N4(H4A), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36)
3.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              14734
_shelx_hkl_checksum              65133
_shelx_fab_checksum              53007
_olex2_submission_special_instructions 'No special instructions were received'