Design of cost-efficient and photocatalytically active Zn-based MOFs decorated with Cu2O nanoparticles for CO2 methanation
Cabrero-Antonino, Maria; Remiro-Buenamañana, Sonia; Souto, Manuel; García-Valdivia, Antonio Andres; Choquesillo-Lazarte, Duane; Navalon, Sergio; Rodríguez Diéguez, Antonio; Minguez Espallargas, Guillermo; Garcia, Hermenegildo; Chemical Communications  (2019) –; doi:10.1039/C9CC04446A

data_7124002
_publ_section_title
;
 Design of cost-efficient and photocatalytically active Zn-based MOFs
 decorated with Cu2O nanoparticles for CO2 methanation
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04446A
_journal_year                    2019
_chemical_formula_moiety         'C14 H8 N6 O6 Zn3, 2(C3 H7 N O)'
_chemical_formula_sum            'C20 H22 N8 O8 Zn3'
_chemical_formula_weight         698.56
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-07 deposited with the CCDC.    2019-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.046(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.037(2)
_cell_length_b                   12.5871(13)
_cell_length_c                   11.0828(13)
_cell_measurement_reflns_used    1552
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.068
_cell_measurement_theta_min      2.740
_cell_volume                     2512.6(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker Apex3, 2016'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7245
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.197
_diffrn_reflns_theta_max         25.197
_diffrn_reflns_theta_min         2.658
_diffrn_source                   'high brilliance microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.904
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6536
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0687 before and 0.0594 after correction. The Ratio of minimum to maximum transmission is 0.8771. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2238
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0508
_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^)+(0.0274P)^2^+18.8964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1642
_reflns_number_total             2238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04446a2.cif
_cod_data_source_block           1916086
_cod_database_code               7124002
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.760
_shelx_estimated_absorpt_t_min   0.722
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Restrained distances
 N4-C8 \\sim N4-C9
 with sigma of 0.02
3. Restrained planarity
 C7, O4, N4, C8, C9
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7 \\sim O4 \\sim N4 \\sim C8 \\sim C9: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C7, O4, N4, C8, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4, N2, N1, C3, C5, C6, C2, C1, N3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N4A, C9A, C7A, C8A, O4A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(C9A)=Sof(N4A)=Sof(C7A)=Sof(O4A)=Sof(C8A)=1-FVAR(1)
 Sof(C7)=Sof(O4)=Sof(N4)=Sof(C8)=Sof(C9)=FVAR(1)
7.a Riding coordinates:
 O3(H3)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'