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_7124003
_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[C3H7NO]'
_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             2019-08-06
_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                 90.71(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.94(3)
_cell_length_b                   10.098(16)
_cell_length_c                   10.957(17)
_cell_measurement_reflns_used    1145
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      18.503
_cell_measurement_theta_min      2.955
_cell_volume                     2095(6)
_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      120.0
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.2331
_diffrn_reflns_av_unetI/netI     0.1238
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7160
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        19.167
_diffrn_reflns_theta_max         19.167
_diffrn_reflns_theta_min         2.286
_diffrn_source                   'high brilliance microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.483
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.2807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1429 before and 0.1156 after correction. The Ratio of minimum to maximum transmission is 0.3771. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.215
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         4.487
_refine_diff_density_min         -3.460
_refine_diff_density_rms         0.449
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.676
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         848
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.604
_refine_ls_R_factor_all          0.2122
_refine_ls_R_factor_gt           0.1798
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4035
_refine_ls_wR_factor_ref         0.4232
_reflns_Friedel_coverage         0.000
_reflns_number_gt                568
_reflns_number_total             848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04446a2.cif
_cod_data_source_block           1916087
_cod_database_code               7124003
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(Zn1) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(N1) \\sim
Ueq, Uanis(N2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C11) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(Zn2)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Riding coordinates:
 O3(H3)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C5(H5)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 
322.0 electrons were found in a volume
of 642.0\%A^3 in 1 void. 
This is consistent with the presence of 
2[C3H7NO] per formula unit 
which account for 320.0 electrons.
;
_olex2_submission_special_instructions 'No special instructions were received'