#------------------------------------------------------------------------------
#$Date: 2019-11-08 02:12:34 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224690 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/81/7058152.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_7058152
loop_
_publ_author_name
'Di, Min'
'Shen, Jingwen'
'Cui, Zheng'
'Zhang, Xiaoying'
'Zhang, Jingping'
_publ_section_title
;
 Assembly of metal--organic frameworks based on 4-connected
 3,3′,5,5′-azobenzenetetracarboxylic acid: structures,
 magnetic properties, and sensing of Fe3+ ions
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              4226
_journal_paper_doi               10.1039/C8NJ05139A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         '0.33(C156 H111 N21 O90 Zn18)'
_chemical_formula_sum            'C52 H37 N7 O30 Zn6'
_chemical_formula_weight         1632.10
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-23 deposited with the CCDC.
2019-02-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   22.8480(10)
_cell_length_b                   22.8480(10)
_cell_length_c                   20.330(2)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    170.15
_cell_measurement_theta_max      25.862
_cell_measurement_theta_min      2.682
_cell_volume                     9191.0(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       SAINT
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0781
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            78837
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.055
_diffrn_reflns_theta_min         2.252
_exptl_absorpt_coefficient_mu    1.204
_exptl_absorpt_correction_T_max  0.9172
_exptl_absorpt_correction_T_min  0.7658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.885
_exptl_crystal_description       block
_exptl_crystal_F_000             2454
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
A solvent mask was calculated and 1724 electrons were 
found in a volume of 5674Å^3 in 3 voids. 
This is consistent with the presence of 
ten N,N-dimethylacetamide and four methanol per formula unit 
which account for 1656 electrons.
;
_refine_diff_density_max         0.792
_refine_diff_density_min         -2.530
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.49(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         12112
_refine_ls_number_restraints     160
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0644
_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/[σ²(Fo²)+(0.0889P)²+20.9271P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1749
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                9667
_reflns_number_total             12112
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj05139a2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7058150--7058152.cif.'
_cod_original_cell_volume        9191.0(12)
_cod_database_code               7058152
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.51(3)
 0.49(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C20-N3 = N3A-C30
 1.4 with sigma of 0.02
 N3-N3A
 1.2 with sigma of 0.02
 O6-C9 = C9-O5
 1.2 with sigma of 0.02
 C9-C8
 1.4 with sigma of 0.02
 O6A-C9A = C9A-O5A
 1.2 with sigma of 0.02
 C9A-C8
 1.4 with sigma of 0.02
 C25-C22
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C9A) \\sim
Ueq, Uanis(O6A) \\sim Ueq, Uanis(O5A) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C14) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 N3, C20, C30, N3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, O6, C8, C9, C9A, O6A, O5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C17, C15, C16, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C22, O15, N4, C24, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O5(0.5) O6(0.5) O7(0.5) H7A(0.5) H7B(0.5) H15A(0.5) H15B(0.5)
 N3(0.5) N4(0.5) C9(0.5) C22(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
 N3A(0.5) C9A(0.5) O6A(0.5) O5A(0.5) O7A(0.5) H7AA(0.5) H7AB(0.5)
7.a Riding coordinates:
 O7(H7A,H7B), O13(H13A,H13B), O15(H15A,H15B), O7A(H7AA,H7AB)
7.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C10(H10), C13(H13), C14(H14), C17(H17), C19(H19), C21(H21),
 C28(H28), C29(H29)
7.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.25941(5) 0.11355(5) 0.84842(6) 0.0400(3) Uani 1 1 d . . . . .
Zn2 Zn 0.40760(5) 0.19925(7) 0.81936(7) 0.0593(4) Uani 1 1 d . . . . .
Zn3 Zn 0.07449(4) 0.56232(4) 0.48557(5) 0.0253(2) Uani 1 1 d . . . . .
O1 O 0.3066(4) 0.0791(5) 0.9098(5) 0.075(3) Uani 1 1 d . . . . .
O2 O 0.4166(4) 0.1381(6) 0.8857(5) 0.092(3) Uani 1 1 d . . . . .
O3 O 0.3623(4) 0.2328(5) 0.7574(4) 0.075(3) Uani 1 1 d . . . . .
O4 O 0.2499(4) 0.1746(4) 0.7816(4) 0.064(2) Uani 1 1 d . . . . .
O5 O -0.0354(12) 0.4494(16) 0.5822(18) 0.082(8) Uani 0.5 1 d D U . A 1
O6 O 0.0735(10) 0.4990(9) 0.5531(11) 0.046(4) Uani 0.5 1 d D U . A 1
O7 O 0.1724(14) 0.5964(14) 0.4747(16) 0.108(10) Uani 0.5 1 d . . . A 1
H7A H 0.203086 0.607282 0.504957 0.162 Uiso 0.5 1 d R . . A 1
H7B H 0.194446 0.604222 0.437807 0.162 Uiso 0.5 1 d R . . A 1
O8 O -0.0697(4) 0.2151(4) 0.7740(4) 0.055(2) Uani 1 1 d . . . . .
O9 O -0.1302(5) 0.2648(5) 0.7517(5) 0.079(3) Uani 1 1 d . . . . .
O10 O 0.4355(4) 0.3925(4) 0.5793(4) 0.067(3) Uani 1 1 d . . . . .
O11 O 0.3789(4) 0.4505(5) 0.5581(4) 0.073(3) Uani 1 1 d . . . . .
O12 O 0.7578(5) 0.1405(5) 0.8915(5) 0.092(3) Uani 1 1 d . . . . .
O13 O 0.4999(4) 0.2710(4) 0.8056(5) 0.095(3) Uani 1 1 d . . . . .
H13A H 0.520944 0.311187 0.822684 0.143 Uiso 1 1 d R . . . .
H13B H 0.528084 0.270888 0.780284 0.143 Uiso 1 1 d R . . . .
O14 O 0.8168(4) 0.0894(4) 0.9163(4) 0.064(2) Uani 1 1 d . . . . .
O15 O 0.1638(3) 0.0387(3) 0.8600(4) 0.0452(16) Uani 1 1 d . U . . .
H15A H 0.142305 0.021852 0.896629 0.068 Uiso 0.5 1 d R . . B 2
H15B H 0.134565 0.015792 0.829419 0.068 Uiso 0.5 1 d R . . B 2
N1 N 0.1579(5) 0.3122(5) 0.6845(5) 0.074(3) Uani 1 1 d . . . . .
N2 N 0.1505(6) 0.3549(7) 0.6534(7) 0.108(6) Uani 1 1 d . . . . .
N3 N 0.5167(12) 0.0216(18) 0.9807(18) 0.082(8) Uani 0.5 1 d D U . C -1
N4 N 0.0811(7) -0.0595(8) 0.8934(8) 0.053(4) Uani 0.5 1 d . U . D -1
C1 C 0.3662(5) 0.0917(6) 0.9182(6) 0.059(3) Uani 1 1 d . . . . .
C2 C 0.3030(7) 0.2206(6) 0.7558(5) 0.063(3) Uani 1 1 d . . . . .
C3 C 0.2904(6) 0.2688(7) 0.7131(7) 0.076(4) Uani 1 1 d . . . . .
C4 C 0.2299(6) 0.2700(6) 0.7162(6) 0.061(3) Uani 1 1 d . . . . .
H4 H 0.195065 0.240928 0.745576 0.073 Uiso 1 1 calc R . . . .
C5 C 0.2214(6) 0.3154(7) 0.6749(7) 0.083(5) Uani 1 1 d . . . . .
C6 C 0.0885(6) 0.3533(7) 0.6581(7) 0.072(4) Uani 1 1 d . . . . .
C7 C 0.0800(7) 0.4015(7) 0.6256(6) 0.072(4) Uani 1 1 d . . . . .
H7 H 0.117430 0.435848 0.602147 0.087 Uiso 1 1 calc R . . . .
C8 C 0.0225(8) 0.4027(7) 0.6252(7) 0.073(4) Uani 1 1 d D U . . .
C9 C 0.0226(13) 0.4558(17) 0.582(2) 0.075(8) Uani 0.5 1 d D U . A 1
C10 C -0.0312(7) 0.3540(6) 0.6651(5) 0.067(3) Uani 1 1 d . . . . .
H10 H -0.072874 0.353752 0.667282 0.080 Uiso 1 1 calc R . . . .
C11 C -0.0225(6) 0.3066(6) 0.7011(6) 0.064(3) Uani 1 1 d . . . . .
C12 C -0.0780(6) 0.2558(6) 0.7447(6) 0.063(3) Uani 1 1 d . . . . .
C13 C 0.0373(7) 0.3067(6) 0.7002(6) 0.071(4) Uani 1 1 d . . . . .
H13 H 0.044131 0.276483 0.726902 0.085 Uiso 1 1 calc R . . . .
C14 C 0.2725(6) 0.3607(7) 0.6360(7) 0.078(4) Uani 1 1 d . U . . .
H14 H 0.267864 0.393453 0.611388 0.093 Uiso 1 1 calc R . . . .
C15 C 0.3301(5) 0.3577(6) 0.6333(6) 0.067(3) Uani 1 1 d . U . . .
C16 C 0.3853(6) 0.4008(6) 0.5831(6) 0.068(4) Uani 1 1 d . U . . .
C17 C 0.3398(6) 0.3134(7) 0.6696(6) 0.072(4) Uani 1 1 d . U . . .
H17 H 0.380883 0.312693 0.665231 0.087 Uiso 1 1 calc R . . . .
C18 C 0.3764(6) 0.0458(8) 0.9614(7) 0.075(4) Uani 1 1 d . . . . .
C19 C 0.4382(6) 0.0437(9) 0.9627(7) 0.090(5) Uani 1 1 d . . . . .
H19 H 0.474891 0.074674 0.936074 0.108 Uiso 1 1 calc R . . . .
C20 C 0.4462(7) 0.000000 1.000000 0.118(10) Uani 1 2 d DS TU P . .
C21 C 0.3230(6) 0.000000 1.000000 0.065(5) Uani 1 2 d S T P . .
H21 H 0.281390 -0.000001 0.999999 0.078 Uiso 1 2 calc RS T P . .
C22 C 0.1358(7) -0.0046(9) 0.8979(8) 0.038(3) Uani 0.5 1 d D U . D -1
C23 C 0.0442(13) -0.1167(17) 0.9274(18) 0.142(17) Uani 0.5 1 d . U . D -1
H23A H -0.003206 -0.128102 0.927500 0.213 Uiso 0.5 1 calc GR . . D -1
H23B H 0.060897 -0.110395 0.972710 0.213 Uiso 0.5 1 calc GR . . D -1
H23C H 0.048065 -0.153396 0.906756 0.213 Uiso 0.5 1 calc GR . . D -1
C24 C 0.0619(14) -0.0739(13) 0.8259(12) 0.093(9) Uani 0.5 1 d . U . D -1
H24A H 0.066347 -0.033377 0.804572 0.139 Uiso 0.5 1 calc GR . . D -1
H24B H 0.014880 -0.110598 0.822984 0.139 Uiso 0.5 1 calc GR . . D -1
H24C H 0.091350 -0.087484 0.803793 0.139 Uiso 0.5 1 calc GR . . D -1
C25 C 0.1595(10) 0.0137(13) 0.9715(9) 0.071(7) Uani 0.5 1 d D U . D -1
H25A H 0.203086 0.055807 0.972820 0.107 Uiso 0.5 1 calc GR . . D -1
H25B H 0.164226 -0.022818 0.991264 0.107 Uiso 0.5 1 calc GR . . D -1
H25C H 0.125877 0.019525 0.996118 0.107 Uiso 0.5 1 calc GR . . D -1
C26 C 0.7675(6) 0.0975(7) 0.9205(7) 0.068(3) Uani 1 1 d . . . . .
C27 C 0.7124(6) 0.0475(7) 0.9603(7) 0.069(4) Uani 1 1 d . . . . .
C28 C 0.7178(6) 0.000000 1.000000 0.067(5) Uani 1 2 d S T P . .
H28 H 0.759339 0.000001 1.000001 0.080 Uiso 1 2 calc RS T P . .
C29 C 0.6504(7) 0.0466(9) 0.9623(10) 0.111(7) Uani 1 1 d . . . . .
H29 H 0.646043 0.079064 0.936849 0.133 Uiso 1 1 calc R . . . .
C30 C 0.5942(8) 0.000000 1.000000 0.107(9) Uani 1 2 d DS TU P . .
N3A N 0.5209(12) -0.020(2) 1.0191(18) 0.090(9) Uani 0.5 1 d D U . C -1
C9A C 0.0010(11) 0.4464(11) 0.5902(12) 0.042(4) Uani 0.5 1 d D U . A 2
O6A O 0.0477(9) 0.4865(13) 0.5538(14) 0.059(6) Uani 0.5 1 d D U . A 2
O5A O -0.0585(9) 0.4370(10) 0.5816(11) 0.040(4) Uani 0.5 1 d D U . A 2
O7A O 0.1714(10) 0.6329(11) 0.4736(11) 0.073(6) Uani 0.5 1 d . . . A 2
H7AA H 0.201136 0.654147 0.504334 0.109 Uiso 0.5 1 d R . . A 2
H7AB H 0.193656 0.648797 0.437074 0.109 Uiso 0.5 1 d R . . A 2
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
O1 Zn1 Zn2 74.4(2) . .
O1 Zn1 O8 85.9(4) . 3
O4 Zn1 Zn2 83.9(2) . .
O4 Zn1 O1 158.1(3) . .
O4 Zn1 O8 89.8(3) . 3
O8 Zn1 Zn2 70.8(2) 3 .
O14 Zn1 Zn2 86.8(2) 3_665 .
O14 Zn1 O1 89.3(4) 3_665 .
O14 Zn1 O4 86.6(4) 3_665 .
O14 Zn1 O8 157.6(3) 3_665 3
O15 Zn1 Zn2 166.4(2) . .
O15 Zn1 O1 99.2(3) . .
O15 Zn1 O4 102.6(3) . .
O15 Zn1 O8 97.1(3) . 3
O15 Zn1 O14 105.3(3) . 3_665
O2 Zn2 Zn1 83.6(2) . .
O3 Zn2 Zn1 75.2(3) . .
O3 Zn2 O2 158.4(4) . .
O9 Zn2 Zn1 87.2(2) 3 .
O9 Zn2 O2 86.5(5) 3 .
O9 Zn2 O3 88.4(4) 3 .
O12 Zn2 Zn1 70.8(2) 3_665 .
O12 Zn2 O2 90.1(5) 3_665 .
O12 Zn2 O3 86.8(4) 3_665 .
O12 Zn2 O9 157.9(3) 3_665 3
O13 Zn2 Zn1 167.2(3) . .
O13 Zn2 O2 103.7(4) . .
O13 Zn2 O3 97.9(4) . .
O13 Zn2 O9 103.5(4) . 3
O13 Zn2 O12 98.5(4) . 3_665
O5 Zn3 Zn3 76.2(7) 5_556 5_556
O6 Zn3 Zn3 81.7(6) . 5_556
O6 Zn3 O5 89.7(12) . 5_556
O6 Zn3 O10 161.4(6) . 6_566
O6 Zn3 O11 89.3(7) . 3_565
O7 Zn3 Zn3 169.1(9) . 5_556
O7 Zn3 O5 100.5(11) . 5_556
O7 Zn3 O6 87.9(11) . .
O7 Zn3 O10 110.3(10) . 6_566
O7 Zn3 O11 103.1(9) . 3_565
O10 Zn3 Zn3 79.9(3) 6_566 5_556
O10 Zn3 O5 83.7(10) 6_566 5_556
O10 Zn3 O6A 147.1(6) 6_566 .
O11 Zn3 Zn3 80.2(3) 3_565 5_556
O11 Zn3 O5 156.3(8) 3_565 5_556
O11 Zn3 O10 89.9(4) 3_565 6_566
O11 Zn3 O6A 88.5(9) 3_565 .
O6A Zn3 O5 84.7(13) . 5_556
O5A Zn3 O5 12.7(10) 5_556 5_556
O5A Zn3 O10 88.1(7) 5_556 6_566
O5A Zn3 O11 168.9(6) 5_556 3_565
O5A Zn3 O6A 87.3(11) 5_556 .
O5A Zn3 O7A 104.2(8) 5_556 .
O7A Zn3 O5 116.2(9) . 5_556
O7A Zn3 O10 92.4(8) . 6_566
O7A Zn3 O11 86.8(6) . 3_565
O7A Zn3 O6A 120.3(10) . .
C1 O1 Zn1 135.6(8) . .
C1 O2 Zn2 123.5(8) . .
C2 O3 Zn2 130.1(7) . .
C2 O4 Zn1 117.6(8) . .
C9 O5 Zn3 128(2) . 5_556
C9 O6 Zn3 125.2(17) . .
C12 O8 Zn1 139.5(9) . 2
C12 O9 Zn2 117.2(7) . 2
C16 O10 Zn3 126.0(8) . 6_666
C16 O11 Zn3 124.2(8) . 2_665
C26 O12 Zn2 137.8(9) . 2_655
C26 O14 Zn1 116.3(8) . 2_655
C22 O15 Zn1 134.9(9) . .
N2 N1 C5 115.0(10) . .
N1 N2 C6 118.5(10) . .
N3A N3 C20 93.7(15) . .
C22 N4 C23 140(2) . .
C22 N4 C24 109.7(17) . .
C23 N4 C24 107(2) . .
O1 C1 O2 122.6(12) . .
O1 C1 C18 117.2(10) . .
O2 C1 C18 119.8(10) . .
O3 C2 O4 131.8(11) . .
O3 C2 C3 115.4(9) . .
O4 C2 C3 112.7(11) . .
C4 C3 C2 121.9(9) . .
C17 C3 C2 120.5(11) . .
C17 C3 C4 117.6(11) . .
C3 C4 C5 119.0(10) . .
C4 C5 N1 112.8(9) . .
C14 C5 N1 125.6(12) . .
C14 C5 C4 121.2(12) . .
N2 C6 C13 120.5(10) . .
C7 C6 N2 119.4(11) . .
C7 C6 C13 119.9(11) . .
C8 C7 C6 123.7(12) . .
C7 C8 C9 114.9(15) . .
C7 C8 C10 117.1(10) . .
C7 C8 C9A 132.5(14) . .
C10 C8 C9 128.0(15) . .
C10 C8 C9A 110.5(13) . .
O5 C9 C8 110(2) . .
O6 C9 O5 127(2) . .
O6 C9 C8 123(2) . .
C11 C10 C8 120.0(12) . .
C10 C11 C12 120.9(11) . .
C13 C11 C10 121.4(10) . .
C13 C11 C12 117.6(9) . .
O8 C12 O9 125.1(12) . .
O8 C12 C11 119.6(12) . .
O9 C12 C11 115.0(9) . .
C11 C13 C6 117.4(9) . .
C15 C14 C5 118.2(12) . .
C14 C15 C16 120.2(12) . .
C14 C15 C17 122.8(10) . .
C17 C15 C16 116.7(12) . .
O10 C16 O11 127.6(10) . .
O10 C16 C15 117.6(13) . .
O11 C16 C15 113.5(12) . .
C15 C17 C3 120.9(12) . .
C19 C18 C1 122.8(12) . .
C21 C18 C1 118.8(10) . .
C21 C18 C19 118.3(13) . .
C20 C19 C18 122.5(14) . .
C19 C20 N3 143.7(14) 6_557 .
C19 C20 N3 97.6(11) . .
C19 C20 C19 118.7(16) . 6_557
C18 C21 C18 119.6(15) . 6_557
O15 C22 N4 130.7(17) . .
O15 C22 C25 115.7(15) . .
N4 C22 C25 111.9(16) . .
O12 C26 C27 117.0(11) . .
O14 C26 O12 127.9(13) . .
O14 C26 C27 114.9(11) . .
C28 C27 C26 123.4(10) . .
C29 C27 C26 119.9(12) . .
C29 C27 C28 116.6(13) . .
C27 C28 C27 123.5(14) . 6_557
C27 C29 C30 123.8(15) . .
C29 C30 C29 115.7(17) . 6_557
C29 C30 N3A 143.1(14) . .
C29 C30 N3A 101.1(12) 6_557 .
N3 N3A C30 95.7(16) . .
O6A C9A C8 109.1(19) . .
O6A C9A O5A 119.5(19) . .
O5A C9A C8 129.0(18) . .
C9A O6A Zn3 143.6(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 Zn2 3.0030(13) .
Zn1 O1 2.046(8) .
Zn1 O4 2.035(7) .
Zn1 O8 2.052(7) 3
Zn1 O14 2.011(8) 3_665
Zn1 O15 2.003(6) .
Zn2 O2 2.025(10) .
Zn2 O3 2.009(9) .
Zn2 O9 2.002(9) 3
Zn2 O12 1.999(9) 3_665
Zn2 O13 1.939(8) .
Zn3 Zn3 3.0058(17) 5_556
Zn3 O5 2.06(3) 5_556
Zn3 O6 1.986(19) .
Zn3 O7 1.98(3) .
Zn3 O10 2.017(7) 6_566
Zn3 O11 2.017(7) 3_565
Zn3 O6A 2.06(2) .
Zn3 O5A 1.942(18) 5_556
Zn3 O7A 1.999(19) .
O1 C1 1.255(13) .
O2 C1 1.290(13) .
O3 C2 1.239(15) .
O4 C2 1.256(14) .
O5 C9 1.26(2) .
O6 C9 1.24(2) .
O8 C12 1.196(12) .
O9 C12 1.317(15) .
O10 C16 1.254(17) .
O11 C16 1.318(17) .
O12 C26 1.258(14) .
O14 C26 1.233(14) .
O15 C22 1.163(17) .
N1 N2 1.245(13) .
N1 C5 1.428(15) .
N2 C6 1.401(15) .
N3 C20 1.483(19) .
N3 N3A 1.27(2) .
N4 C22 1.26(2) .
N4 C23 1.34(3) .
N4 C24 1.43(3) .
C1 C18 1.474(16) .
C2 C3 1.538(15) .
C3 C4 1.397(15) .
C3 C17 1.394(14) .
C4 C5 1.423(15) .
C5 C14 1.361(15) .
C6 C7 1.380(15) .
C6 C13 1.411(15) .
C7 C8 1.327(18) .
C8 C9 1.49(2) .
C8 C10 1.427(17) .
C8 C9A 1.496(19) .
C10 C11 1.400(13) .
C11 C12 1.507(15) .
C11 C13 1.366(16) .
C14 C15 1.351(17) .
C15 C16 1.537(13) .
C15 C17 1.359(18) .
C18 C19 1.437(14) .
C18 C21 1.386(13) .
C19 C20 1.337(17) .
C22 C25 1.57(2) .
C26 C27 1.451(17) .
C27 C28 1.406(12) .
C27 C29 1.405(15) .
C29 C30 1.416(18) .
C30 N3A 1.55(2) .
C9A O6A 1.24(2) .
C9A O5A 1.28(2) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Zn1 O1 C1 O2 3(2) . .
Zn1 O1 C1 C18 -169.7(10) . .
Zn1 O4 C2 O3 9(2) . .
Zn1 O4 C2 C3 -172.7(9) . .
Zn1 O8 C12 O9 -5(2) 2 .
Zn1 O8 C12 C11 167.5(9) 2 .
Zn1 O14 C26 O12 -6(2) 2_655 .
Zn1 O14 C26 C27 168.7(9) 2_655 .
Zn1 O15 C22 N4 -158.6(15) . .
Zn1 O15 C22 C25 38(2) . .
Zn2 O2 C1 O1 2(2) . .
Zn2 O2 C1 C18 174.9(10) . .
Zn2 O3 C2 O4 -17(2) . .
Zn2 O3 C2 C3 164.9(10) . .
Zn2 O9 C12 O8 2.4(19) 2 .
Zn2 O9 C12 C11 -170.9(9) 2 .
Zn2 O12 C26 O14 9(3) 2_655 .
Zn2 O12 C26 C27 -165.4(12) 2_655 .
Zn3 O5 C9 O6 19(7) 5_556 .
Zn3 O5 C9 C8 -161(2) 5_556 .
Zn3 O6 C9 O5 -10(7) . .
Zn3 O6 C9 C8 170(2) . .
Zn3 O10 C16 O11 -17.7(17) 6_666 .
Zn3 O10 C16 C15 176.0(8) 6_666 .
Zn3 O11 C16 O10 18.4(17) 2_665 .
Zn3 O11 C16 C15 -174.8(8) 2_665 .
O1 C1 C18 C19 164.2(15) . .
O1 C1 C18 C21 -12(2) . .
O2 C1 C18 C19 -9(2) . .
O2 C1 C18 C21 174.7(12) . .
O3 C2 C3 C4 -167.3(15) . .
O3 C2 C3 C17 12(2) . .
O4 C2 C3 C4 14(2) . .
O4 C2 C3 C17 -165.9(14) . .
O12 C26 C27 C28 -174.4(12) . .
O12 C26 C27 C29 3(2) . .
O14 C26 C27 C28 10(2) . .
O14 C26 C27 C29 -172.2(16) . .
N1 N2 C6 C7 178.0(15) . .
N1 N2 C6 C13 4(3) . .
N1 C5 C14 C15 178.6(15) . .
N2 N1 C5 C4 174.3(15) . .
N2 N1 C5 C14 1(3) . .
N2 C6 C7 C8 177.5(16) . .
N2 C6 C13 C11 -178.3(16) . .
C1 C18 C19 C20 -177.1(12) . .
C1 C18 C21 C18 176.9(16) . 6_557
C2 C3 C4 C5 -179.4(14) . .
C2 C3 C17 C15 -177.6(14) . .
C3 C4 C5 N1 -178.6(14) . .
C3 C4 C5 C14 -5(3) . .
C4 C3 C17 C15 2(2) . .
C4 C5 C14 C15 6(3) . .
C5 N1 N2 C6 177.4(16) . .
C5 C14 C15 C16 171.4(14) . .
C5 C14 C15 C17 -3(3) . .
C6 C7 C8 C9 -175(2) . .
C6 C7 C8 C10 5(2) . .
C6 C7 C8 C9A -175.2(19) . .
C7 C6 C13 C11 7(2) . .
C7 C8 C9 O5 175(3) . .
C7 C8 C9 O6 -5(5) . .
C7 C8 C10 C11 -2(2) . .
C7 C8 C9A O6A 3(3) . .
C7 C8 C9A O5A 165(2) . .
C8 C10 C11 C12 178.7(13) . .
C8 C10 C11 C13 2(2) . .
C8 C9A O6A Zn3 178(3) . .
C8 C9A O5A Zn3 -162.7(19) . 5_556
C9 C8 C10 C11 179(3) . .
C10 C8 C9 O5 -5(5) . .
C10 C8 C9 O6 175(3) . .
C10 C8 C9A O6A -177(2) . .
C10 C8 C9A O5A -15(3) . .
C10 C11 C12 O8 178.8(13) . .
C10 C11 C12 O9 -7.5(19) . .
C10 C11 C13 C6 -4(2) . .
C12 C11 C13 C6 178.5(13) . .
C13 C6 C7 C8 -8(3) . .
C13 C11 C12 O8 -4(2) . .
C13 C11 C12 O9 169.7(13) . .
C14 C15 C16 O10 -174.8(13) . .
C14 C15 C16 O11 17.0(18) . .
C14 C15 C17 C3 -1(2) . .
C16 C15 C17 C3 -175.4(13) . .
C17 C3 C4 C5 1(2) . .
C17 C15 C16 O10 -0.6(18) . .
C17 C15 C16 O11 -168.7(12) . .
C18 C19 C20 N3 180(2) . .
C18 C19 C20 C19 0.3(12) . 6_557
C19 C18 C21 C18 0.3(11) . 6_557
C20 N3 N3A C30 179(3) . .
C21 C18 C19 C20 -1(2) . .
C23 N4 C22 O15 172(3) . .
C23 N4 C22 C25 -23(4) . .
C24 N4 C22 O15 16(3) . .
C24 N4 C22 C25 -180(2) . .
C26 C27 C28 C27 178.6(16) . 6_557
C26 C27 C29 C30 -179.6(14) . .
C27 C29 C30 C29 0.9(14) . 6_557
C27 C29 C30 N3A 178(3) . .
C28 C27 C29 C30 -2(3) . .
C29 C27 C28 C27 0.8(12) . 6_557
C29 C30 N3A N3 5(4) . .
C29 C30 N3A N3 -177(2) 6_557 .
N3A N3 C20 C19 178.1(19) . .
N3A N3 C20 C19 -3(4) . 6_557
C9A C8 C10 C11 178.4(16) . .
O6A C9A O5A Zn3 -2(4) . 5_556
O5A C9A O6A Zn3 14(5) . .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 44 23 '0.33 methanol'
2 0.175 0.606 0.011 5630 1701 '1.66 N,N-dimethylacetamide and 0.5 methanol'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.51(3)
2 0.49(3)
