#------------------------------------------------------------------------------
#$Date: 2019-08-15 03:06:52 +0300 (Thu, 15 Aug 2019) $
#$Revision: 217531 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/39/7123999.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7123999
loop_
_publ_author_name
'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'
_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, 4(H2 O)'
_chemical_formula_sum            'C14 H16 N6 O10 Zn3'
_chemical_formula_weight         624.44
_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   geom
_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                 90.176(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.544(2)
_cell_length_b                   9.0665(12)
_cell_length_c                   11.0933(13)
_cell_measurement_reflns_used    1422
_cell_measurement_temperature    120
_cell_measurement_theta_max      24.785
_cell_measurement_theta_min      2.477
_cell_volume                     1965.7(4)
_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
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1083
_diffrn_reflns_av_unetI/netI     0.1519
_diffrn_reflns_Laue_measured_fraction_full 0.912
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5727
_diffrn_reflns_point_group_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.051
_diffrn_reflns_theta_max         25.051
_diffrn_reflns_theta_min         2.476
_diffrn_source                   'high brilliance microfocus sealed tube'
_exptl_absorpt_coefficient_mu    3.702
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0727 before and 0.0539 after correction. The Ratio of minimum to maximum transmission is 0.7902. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.110
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.478
_refine_diff_density_min         -1.913
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         1588
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0618
_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/[σ²(Fo²)+(0.0111P)²+71.7093P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1490
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1123
_reflns_number_total             1588
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc04446a2.cif
_cod_data_source_block           1916082
_cod_database_code               7123999
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.708
_shelx_estimated_absorpt_t_min   0.645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(Zn2) \\sim Ueq, Uanis(Zn1) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N2)
\\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C5) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C6) \\sim
Ueq, Uanis(C11) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C2(H2), C6(H6)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Zn2 Zn 0.000000 0.14391(17) 0.250000 0.0085(4) Uani 1 2 d S TU P
Zn1 Zn -0.07424(6) -0.06092(12) 0.49400(9) 0.0106(3) Uani 1 1 d . U .
O3 O -0.0135(4) 0.1220(7) 0.4328(5) 0.0109(14) Uani 1 1 d . U .
N3 N -0.1191(4) -0.0419(8) 0.1364(7) 0.0129(17) Uani 1 1 d . U .
N2 N -0.0830(4) -0.0309(8) 0.2376(6) 0.0109(17) Uani 1 1 d . U .
N1 N -0.1215(4) -0.0702(8) 0.3329(6) 0.0124(17) Uani 1 1 d . U .
C3 C -0.1842(5) -0.1066(10) 0.2920(8) 0.011(2) Uani 1 1 d . U .
C5 C -0.2415(5) -0.1092(10) 0.0959(8) 0.014(2) Uani 1 1 d . U .
H5 H -0.240053 -0.099929 0.010660 0.017 Uiso 1 1 calc R . .
C2 C -0.2451(5) -0.1463(10) 0.3507(8) 0.012(2) Uani 1 1 d . U .
H2 H -0.246191 -0.160898 0.435469 0.015 Uiso 1 1 calc R . .
C4 C -0.1829(5) -0.0860(10) 0.1659(8) 0.010(2) Uani 1 1 d . U .
C1 C -0.3028(6) -0.1633(11) 0.2817(8) 0.016(2) Uani 1 1 d . U .
C6 C -0.3017(6) -0.1458(10) 0.1539(8) 0.014(2) Uani 1 1 d . U .
H6 H -0.342514 -0.159445 0.108448 0.017 Uiso 1 1 calc R . .
C11 C -0.3700(5) -0.2069(10) 0.3384(8) 0.013(2) Uani 1 1 d . U .
O1 O -0.3693(4) -0.2430(7) 0.4493(6) 0.0177(15) Uani 1 1 d . U .
O2 O -0.4220(4) -0.2040(7) 0.2693(6) 0.0154(15) Uani 1 1 d . U .
O2W O -0.0571(6) -0.3724(12) 0.0617(9) 0.062(3) Uani 1 1 d . . .
O1W O -0.0691(7) -0.4127(12) 0.3344(10) 0.074(4) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O3 Zn2 O3 168.9(4) . 2
O3 Zn2 N2 84.2(3) 2 2
O3 Zn2 N2 84.2(3) . .
O3 Zn2 N2 88.1(3) 2 .
O3 Zn2 N2 88.1(3) . 2
O3 Zn2 O2 93.4(3) . 3
O3 Zn2 O2 94.0(2) 2 3
O3 Zn2 O2 94.0(2) . 4_455
O3 Zn2 O2 93.4(3) 2 4_455
N2 Zn2 N2 91.5(4) . 2
O2 Zn2 N2 176.7(3) 3 .
O2 Zn2 N2 176.7(3) 4_455 2
O2 Zn2 N2 86.1(3) 3 2
O2 Zn2 N2 86.1(3) 4_455 .
O2 Zn2 O2 96.3(4) 3 4_455
O3 Zn1 Zn1 43.30(18) 5_556 5_556
O3 Zn1 Zn1 39.04(18) . 5_556
O3 Zn1 O3 82.3(3) 5_556 .
O3 Zn1 N3 100.7(3) 5_556 6_556
O3 Zn1 N1 138.6(3) 5_556 .
O3 Zn1 O1 176.0(3) . 7_446
O3 Zn1 O1 95.3(3) 5_556 7_446
N3 Zn1 Zn1 102.0(2) 6_556 5_556
N3 Zn1 O3 97.5(3) 6_556 .
N3 Zn1 O1 86.0(3) 6_556 7_446
N1 Zn1 Zn1 118.7(2) . 5_556
N1 Zn1 O3 90.2(3) . .
N1 Zn1 N3 120.7(3) . 6_556
N1 Zn1 O1 89.5(3) . 7_446
O1 Zn1 Zn1 138.5(2) 7_446 5_556
Zn2 O3 Zn1 117.3(3) . .
Zn1 O3 Zn2 108.6(3) 5_556 .
Zn1 O3 Zn1 97.7(3) 5_556 .
N2 N3 Zn1 113.1(6) . 6
N2 N3 C4 107.9(7) . .
C4 N3 Zn1 136.4(7) . 6
N3 N2 Zn2 118.8(5) . .
N3 N2 N1 110.3(8) . .
N1 N2 Zn2 122.5(6) . .
N2 N1 Zn1 115.5(6) . .
C3 N1 Zn1 136.5(6) . .
C3 N1 N2 108.1(7) . .
N1 C3 C2 132.6(8) . .
N1 C3 C4 106.4(8) . .
C2 C3 C4 120.7(9) . .
C4 C5 H5 120.8 . .
C6 C5 H5 120.8 . .
C6 C5 C4 118.3(9) . .
C3 C2 H2 121.1 . .
C1 C2 C3 117.8(8) . .
C1 C2 H2 121.1 . .
N3 C4 C3 107.4(9) . .
N3 C4 C5 131.7(8) . .
C5 C4 C3 120.9(9) . .
C2 C1 C6 121.9(9) . .
C2 C1 C11 120.8(8) . .
C6 C1 C11 117.3(9) . .
C5 C6 C1 120.3(10) . .
C5 C6 H6 119.9 . .
C1 C6 H6 119.9 . .
O1 C11 C1 117.6(9) . .
O2 C11 C1 116.0(8) . .
O2 C11 O1 126.4(9) . .
C11 O1 Zn1 118.9(6) . 7_446
C11 O2 Zn2 129.6(6) . 3_445
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn2 O3 2.055(6) .
Zn2 O3 2.055(6) 2
Zn2 N2 2.272(8) 2
Zn2 N2 2.272(8) .
Zn2 O2 2.066(7) 3
Zn2 O2 2.066(7) 4_455
Zn1 Zn1 3.108(2) 5_556
Zn1 O3 2.150(6) .
Zn1 O3 1.975(7) 5_556
Zn1 N3 2.036(7) 6_556
Zn1 N1 2.011(8) .
Zn1 O1 2.186(7) 7_446
N3 N2 1.328(11) .
N3 C4 1.351(13) .
N2 N1 1.348(10) .
N1 C3 1.347(13) .
C3 C2 1.405(13) .
C3 C4 1.412(12) .
C5 H5 0.9500 .
C5 C4 1.397(15) .
C5 C6 1.383(14) .
C2 H2 0.9500 .
C2 C1 1.370(15) .
C1 C6 1.427(13) .
C1 C11 1.510(14) .
C6 H6 0.9500 .
C11 O1 1.273(11) .
C11 O2 1.272(12) .
