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_7060944
_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 H24 Gd2 N6 Ni O16, 2(N O3)'
_chemical_formula_sum            'C40 H33 Gd2 N9 Ni O23'
_chemical_formula_weight         1380.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-05
_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                90
_cell_angle_beta                 110.266(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5924(13)
_cell_length_b                   16.7807(12)
_cell_length_c                   20.6012(15)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.953
_cell_volume                     5705.2(7)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0970
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40832
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.146
_diffrn_reflns_theta_max         25.146
_diffrn_reflns_theta_min         2.238
_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    2.704
_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    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.677
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5072
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0516P)^2^+43.7649P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4187
_reflns_number_total             5072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj03479k2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7060944--7060945.cif.'
_cod_database_code               7060944
_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
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O10-N7 = O11-N7 = O9-N7 = O15-N5 = O12-N5 = O13-N5
 1.3 with sigma of 0.01
 O7-H7 = O3-H3A = O3-H3B
 0.85 with sigma of 0.01
 O3-H3B = O3-H3A = O7-H7
 0.85 with sigma of 0.01
 O9-O10 \\sim O9-O11 \\sim O11-O10 \\sim O13-O12 \\sim O15-O12 \\sim O15-O13
 with sigma of 0.02
 O10-N7 \\sim O11-N7 \\sim O9-N7 \\sim O13-N5 \\sim O15-N5 \\sim O12-N5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O15 \\sim O12 \\sim N5 \\sim O13 \\sim O10 \\sim O9 \\sim N7 \\sim O11: within
3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03 within 3.8A
4. Rigid body (RIGU) restrains
 O9, N7, O10, O11, O15, O12, N5, O13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: O9(0.5) O12(0.5) O10(0.5) O11(0.5) N7(0.5) N5(0.5) O13(0.5) O15(0.5)
6.a Riding coordinates:
 O7(H7)
6.b Rotating group:
 O3(H3A,H3B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7A), C9(H9), C11(H11), C14(H14), C16(H16), C17(H17)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95988
_shelx_fab_checksum              35513
_olex2_submission_special_instructions 'No special instructions were received'