Synthesis and CO2 photoreduction of two 3d–4f heterometal–organic frameworks
Yang, Yu; Fu, Yaomei; You, Siqi; Li, Mingyue; Qin, Chao; Zhao, Liang; Su, Zhongmin; New Journal of Chemistry 45 (2021) 18790–18795; doi:10.1039/D1NJ03479K

data_7060945
_publ_section_title
;
 Synthesis and CO2 photoreduction of two 3d--4f heterometal--organic
 frameworks
;
_journal_issue                   40
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18790
_journal_page_last               18795
_journal_paper_doi               10.1039/D1NJ03479K
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C36 H18 Co Gd2 N6 O18, N O3'
_chemical_formula_sum            'C35 H51 Co Gd2 N9 O25'
_chemical_formula_weight         1371.27
_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             2021-06-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-16 deposited with the CCDC.	2021-09-07 downloaded from the CCDC.
;
_cell_angle_alpha                101.704(3)
_cell_angle_beta                 103.402(3)
_cell_angle_gamma                95.429(3)
_cell_formula_units_Z            2
_cell_length_a                   11.0599(10)
_cell_length_b                   12.4532(10)
_cell_length_c                   22.2391(18)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.953
_cell_volume                     2885.2(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 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_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  0.0557
_diffrn_reflns_av_unetI/netI     0.0326
_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       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66861
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.142
_diffrn_reflns_theta_max         25.142
_diffrn_reflns_theta_min         2.254
_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    2.636
_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    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1358
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.983
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10259
_refine_ls_number_restraints     2030
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+4.1620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8487
_reflns_number_total             10259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03479k2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7060944--7060945.cif.'
_cod_database_code               7060945
_shelx_shelxl_version_number     2018/3
_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
2. Restrained distances
 O19-N7 = O21-N7 = O20-N7 = O23-N8 = O24-N8 = O22-N8
 1.3 with sigma of 0.02
 O21-N7 \\sim O19-N7 \\sim O20-N7 \\sim O23-N8 \\sim O22-N8 \\sim O24-N8
 with sigma of 0.02
 O20-O19 \\sim O21-O19 \\sim O21-O20 \\sim O23-O22 \\sim O24-O23 \\sim O24-O22
 with sigma of 0.02
3. Restrained planarity
 N8, O23, O22, O24
 with sigma of 0.1
 N7, O21, O19, O20
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O19 \\sim N7 \\sim O21 \\sim O20 \\sim O23 \\sim N8 \\sim O22 \\sim O24: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03 within 3.8A
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O21 \\sim O19 \\sim O20 \\sim O23 \\sim O22 \\sim O24 \\sim O7A
\\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.03 within 3.8A
Uanis(O8) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
5. Rigid body (RIGU) restrains
 O19, N7, O21, O20, O23, N8, O22, O24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: O7(0.65) N7(0.5) O21(0.5) O19(0.5) O20(0.5) O23(0.5) O22(0.5)
 N8(0.5) O24(0.5) O7A(0.35)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15), C17(H17),
 C18(H18), C24(H24), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31),
  C32(H32), C35(H35)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38279
_shelx_fab_checksum              56157
_olex2_submission_special_instructions 'No special instructions were received'