Ce-Hydroxamate Metal-Organic Frameworks for Photocatalytic H2 Generation
Feng, Xuan; Li, Wenying; Yang, Lei; Song, Ting; Xia, Zhaoming; Lai, Qiuxue; Zhou, Xuemei; Hai, Xiao; Liu, Chong; Chemical Communications  (2022) –; doi:10.1039/D2CC05189C

data_7130973
_publ_section_title
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 Ce-Hydroxamate Metal-Organic Frameworks for Photocatalytic H2 Generation
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC05189C
_journal_year                    2022
_chemical_formula_moiety         'C14 H20 Ce N5 O9'
_chemical_formula_sum            'C14 H20 Ce N5 O9'
_chemical_formula_weight         542.47
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-03-18 deposited with the CCDC.	2022-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 124.703(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9892(7)
_cell_length_b                   20.1086(9)
_cell_length_c                   8.5463(4)
_cell_measurement_reflns_used    5738
_cell_measurement_temperature    304(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      3.52
_cell_volume                     1976.45(17)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      304.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            15794
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.495
_diffrn_reflns_theta_min         2.026
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.361
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0728 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.8766.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.406
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     153
_refine_ls_number_reflns         2267
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.167
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0650P)^2^+6.2932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1088
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1966
_reflns_number_total             2267
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc05189c2.cif
_cod_data_source_block           SUM-6
_cod_original_cell_volume        1976.44(17)
_cod_database_code               7130973
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.798
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Ce1 \\sim O3: within 3A with sigma of 0.01 and sigma for terminal atoms of
0.015 within 3A
N3 \\sim C6 \\sim C7: within 3A with sigma of 0.01 and sigma for terminal atoms
of 0.015 within 3A
3. Rigid body (RIGU) restrains
 N3, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O6)=1-FVAR(1)
 Sof(O5)=FVAR(1)
 Sof(C5B)=Sof(H5B)=1-FVAR(2)
 Sof(C5A)=Sof(H5A)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C5A(H5A), C5B(H5B)
5.b Idealised Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7449
_shelx_hkl_checksum              53218
_olex2_submission_special_instructions 'No special instructions were received'