#------------------------------------------------------------------------------
#$Date: 2024-03-04 04:09:35 +0200 (Mon, 04 Mar 2024) $
#$Revision: 290044 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/10/1571094.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_1571094
loop_
_publ_author_name
'Peng, Tianyou'
'Han, Chao-Qin'
'Xia, Hai-Lun'
'Zhou, Kang'
'Zhang, Jian'
'Si, Jincheng'
'Wang, Lei'
'Miao, Jiafeng'
'Guo, Fu-An'
'Wang, Hao'
'Qu, Lu-Lu'
'Xu, Guozhong'
'Li, Jing'
'Liu, Xiao-Yuan'
_publ_section_title
;
 Reticular chemistry guided precise construction of
 zirconium-pentacarboxylate frameworks with 5-connected Zr₆
 clusters.
;
_journal_issue                   9
_journal_name_full               'Chemical science'
_journal_page_first              3174
_journal_page_last               3181
_journal_paper_doi               10.1039/d3sc05410a
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C33 H16 N2 O33 Zr6'
_chemical_formula_sum            'C33 H16 N2 O33 Zr6'
_chemical_formula_weight         1515.80
_chemical_name_systematic        HIAM-4040-OH
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-08-23 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.6081(13)
_cell_length_b                   25.3758(13)
_cell_length_c                   13.7747(7)
_cell_measurement_reflns_used    9526
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.066
_cell_measurement_theta_min      2.296
_cell_volume                     9999.8(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX4 V2022.10-1 (Bruker, 2022)'
_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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.1083
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43414
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.514
_diffrn_reflns_theta_min         1.682
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1352 before and 0.0946 after correction.
The Ratio of minimum to maximum transmission is 0.7870.
The λ/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.007
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         11462
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0734
_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)+(0.0848P)²+6.2726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1763
_refine_ls_wR_factor_ref         0.1972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6966
_reflns_number_total             11462
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc05410a2.cif
_cod_data_source_block           a
_cod_database_code               1571094
_shelx_shelxl_version_number     2017/1
_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   0.938
_shelx_estimated_absorpt_t_min   0.920
_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 O(H) groups
2. Restrained distances
 O8-C25 = O9-C25
 1.25 with sigma of 0.01
 O4-C17 = O3-C17
 1.25 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
O3 \\sim O4 \\sim C17: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O7 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C18 \\sim C19: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O8 \\sim O9 \\sim C25: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O9: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O18A) = Uanis(O18B)
4. Others
 Fixed Sof: O3(0.5) O4(0.5) O7(0.5) H7(0.5) O8(0.5) O9(0.5) O13B(0.5)
 O18A(0.5) N1(0.5) N2(0.5) H2(0.5) C11(0.5) C6(0.5) C7(0.5) H7A(0.5) C8(0.5)
 H8(0.5) C9(0.5) C10(0.5) C12(0.5) C13(0.5) C14(0.5) H14(0.5) C15(0.5) H15(0.5)
 C16(0.5) C17(0.5) C18(0.5) H18(0.5) C19(0.5) C25(0.5) H25(0.5) O18B(0.5)
 O13A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2), C3(H3), C4(H4), C7(H7A), C8(H8), C14(H14), C15(H15), C18(H18),
 C21(H21), C23(H23), C25(H25), C26(H26)
5.b Fitted hexagon refined as free rotating group:
 C11(C6,C7,C8,C9,C10)
5.c Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.42827(2) 0.52767(3) 0.40972(5) 0.03888(18) Uani 1 1 d . . . . .
Zr2 Zr 0.54963(2) 0.52901(3) 0.36088(5) 0.03891(18) Uani 1 1 d . . . . .
Zr3 Zr 0.49442(2) 0.41159(2) 0.42861(4) 0.02951(15) Uani 1 1 d . . . . .
O1 O 0.54527(12) 0.34895(17) 0.4640(3) 0.0354(9) Uani 1 1 d . . . . .
O2 O 0.59496(15) 0.3876(2) 0.5674(4) 0.0584(14) Uani 1 1 d . . . . .
O3 O 0.8959(8) 0.4682(7) 0.2026(10) 0.047(4) Uani 0.5 1 d D U P A -1
O4 O 0.9384(9) 0.3948(11) 0.1839(18) 0.035(4) Uani 0.5 1 d D U P A -1
O5 O 0.92476(17) 0.3872(2) 0.8666(4) 0.0631(15) Uani 1 1 d . . . . .
O6 O 0.95477(12) 0.34857(16) 0.9991(3) 0.0352(10) Uani 1 1 d . . . . .
O7 O 0.9077(4) 0.3155(6) 0.5053(9) 0.091(4) Uani 0.5 1 d . U P A -1
H7 H 0.896781 0.320306 0.561235 0.137 Uiso 0.5 1 calc R U P A -1
O8 O 0.4386(10) 0.3884(12) 0.335(2) 0.043(5) Uani 0.5 1 d D U P B 1
O9 O 0.3918(8) 0.4614(8) 0.3317(10) 0.048(4) Uani 0.5 1 d D U P B 1
O10 O 0.52958(17) 0.3918(2) 0.2902(3) 0.0530(12) Uani 1 1 d . . . . .
O11 O 0.5649(2) 0.4679(3) 0.2448(4) 0.085(2) Uani 1 1 d . . . . .
O12 O 0.55780(19) 0.4578(2) 0.4408(4) 0.0660(15) Uani 1 1 d . . . . .
O13B O 0.4851(7) 0.4855(8) 0.3286(9) 0.040(4) Uani 0.5 1 d . . P B 2
O14 O 0.49154(15) 0.5719(3) 0.4181(4) 0.081(2) Uani 1 1 d . . . . .
O15 O 0.5633(2) 0.5433(2) 0.5103(4) 0.082(2) Uani 1 1 d . . . . .
O16 O 0.62553(18) 0.5275(2) 0.3366(4) 0.0782(18) Uani 1 1 d . . . . .
O17 O 0.5322(2) 0.5642(3) 0.2186(4) 0.0840(18) Uani 1 1 d . . . . .
O18A O 0.4115(10) 0.5631(18) 0.277(3) 0.056(4) Uani 0.5 1 d . . P B 1
O19 O 0.35435(15) 0.5259(2) 0.4495(4) 0.0668(15) Uani 1 1 d . . . . .
N1 N 0.8324(3) 0.3046(4) 0.6056(7) 0.036(2) Uani 0.5 1 d . . P A -1
N2 N 0.7642(3) 0.3067(4) 0.5308(8) 0.039(3) Uani 0.5 1 d . . P A -1
H2 H 0.742887 0.315709 0.487931 0.047 Uiso 0.5 1 calc R U P A -1
C1 C 0.57959(19) 0.3489(2) 0.5232(5) 0.0396(15) Uani 1 1 d . . . . .
C2 C 0.60412(18) 0.2978(3) 0.5377(4) 0.0350(14) Uani 1 1 d . . . . .
C3 C 0.5821(3) 0.250000 0.5156(6) 0.036(2) Uani 1 2 d S T P . .
H3 H 0.552228 0.250000 0.485524 0.044 Uiso 1 2 calc R U P . .
C4 C 0.64848(18) 0.2968(2) 0.5803(4) 0.0354(14) Uani 1 1 d . . . . .
H4 H 0.663459 0.329236 0.595396 0.043 Uiso 1 1 calc R U . . .
C5 C 0.6712(2) 0.250000 0.6013(5) 0.0279(17) Uani 1 2 d S T P . .
C11 C 0.7561(2) 0.2776(3) 0.6143(4) 0.035(2) Uani 0.5 1 d G U P A -1
C6 C 0.71852(16) 0.2489(4) 0.6505(4) 0.0343(18) Uani 0.5 1 d G U P A -1
C7 C 0.72366(19) 0.2194(4) 0.7347(5) 0.040(2) Uani 0.5 1 d G U P A -1
H7A H 0.697978 0.199768 0.759421 0.048 Uiso 0.5 1 calc R U P A -1
C8 C 0.7664(2) 0.2184(4) 0.7828(4) 0.041(3) Uani 0.5 1 d G U P A -1
H8 H 0.769874 0.198193 0.840375 0.049 Uiso 0.5 1 calc R U P A -1
C9 C 0.80393(16) 0.2471(4) 0.7466(5) 0.0340(19) Uani 0.5 1 d G U P A -1
C10 C 0.79880(19) 0.2767(3) 0.6624(5) 0.032(2) Uani 0.5 1 d G U P A -1
C12 C 0.8107(4) 0.3191(6) 0.5255(9) 0.043(3) Uani 0.5 1 d . . P A -1
C13 C 0.8338(4) 0.3467(7) 0.4470(10) 0.055(3) Uani 0.5 1 d . U P A -1
C14 C 0.8085(5) 0.3777(7) 0.3837(11) 0.063(3) Uani 0.5 1 d . U P A -1
H14 H 0.775697 0.382009 0.391389 0.076 Uiso 0.5 1 calc R U P A -1
C15 C 0.8328(4) 0.4031(7) 0.3068(10) 0.061(3) Uani 0.5 1 d . U P A -1
H15 H 0.816457 0.425634 0.263299 0.073 Uiso 0.5 1 calc R U P A -1
C16 C 0.8806(5) 0.3948(7) 0.2954(10) 0.057(3) Uani 0.5 1 d . U P A -1
C17 C 0.9075(7) 0.4217(7) 0.2260(11) 0.041(4) Uani 0.5 1 d D U P A -1
C18 C 0.9043(5) 0.3676(7) 0.3647(11) 0.063(3) Uani 0.5 1 d . U P A -1
H18 H 0.937482 0.366339 0.361998 0.076 Uiso 0.5 1 calc R U P A -1
C19 C 0.8812(5) 0.3415(7) 0.4399(11) 0.065(3) Uani 0.5 1 d . U P A -1
C20 C 0.8491(2) 0.250000 0.8039(6) 0.0292(17) Uani 1 2 d S T P . .
C21 C 0.8699(2) 0.2963(3) 0.8328(5) 0.0455(16) Uani 1 1 d . . . . .
H21 H 0.857030 0.328735 0.811192 0.055 Uiso 1 1 calc R U . . .
C22 C 0.9097(2) 0.2974(3) 0.8933(5) 0.0424(15) Uani 1 1 d . . . . .
C23 C 0.9281(3) 0.250000 0.9252(6) 0.036(2) Uani 1 2 d S T P . .
H23 H 0.953613 0.250001 0.969373 0.043 Uiso 1 2 calc R U P . .
C24 C 0.9314(2) 0.3488(3) 0.9220(5) 0.0405(15) Uani 1 1 d . . . . .
C25 C 0.4044(8) 0.4157(7) 0.3068(12) 0.046(4) Uani 0.5 1 d D U P B 1
H25 H 0.385233 0.399359 0.259252 0.055 Uiso 0.5 1 calc R U P B 1
C26 C 0.5544(4) 0.4213(4) 0.2370(7) 0.087(3) Uani 1 1 d . . . . .
H26 H 0.567110 0.404420 0.181358 0.105 Uiso 1 1 calc R U . . .
O18B O 0.4248(10) 0.5610(18) 0.255(3) 0.056(4) Uani 0.5 1 d . . P B 2
O13A O 0.4870(6) 0.4860(8) 0.3704(9) 0.034(3) Uani 0.5 1 d . . P B 1
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'
Zr Zr -2.9673 0.5597 '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
_geom_angle_publ_flag
Zr3 Zr1 Zr3 88.950(19) 5_666 . ?
O2 Zr1 Zr3 71.32(11) 5_666 5_666 ?
O2 Zr1 Zr3 160.26(11) 5_666 . ?
O2 Zr1 O18B 76.6(10) 5_666 . ?
O9 Zr1 Zr3 70.0(5) . . ?
O9 Zr1 Zr3 157.8(4) . 5_666 ?
O9 Zr1 O2 129.6(5) . 5_666 ?
O12 Zr1 Zr3 88.42(16) 5_666 . ?
O12 Zr1 Zr3 35.86(14) 5_666 5_666 ?
O12 Zr1 O2 76.0(2) 5_666 5_666 ?
O12 Zr1 O9 132.6(4) 5_666 . ?
O12 Zr1 O13B 115.3(4) 5_666 . ?
O12 Zr1 O14 72.4(2) 5_666 . ?
O12 Zr1 O19 86.7(2) 5_666 . ?
O12 Zr1 O18B 147.4(11) 5_666 . ?
O13B Zr1 Zr3 41.1(4) . . ?
O13B Zr1 O18B 75.2(8) . . ?
O14 Zr1 Zr3 36.56(15) . 5_666 ?
O14 Zr1 Zr3 88.88(18) . . ?
O14 Zr1 O2 75.1(2) . 5_666 ?
O14 Zr1 O9 144.3(5) . . ?
O14 Zr1 O13B 70.3(5) . . ?
O14 Zr1 O19 144.9(2) . . ?
O14 Zr1 O18B 83.9(10) . . ?
O15 Zr1 Zr3 88.34(17) 5_666 5_666 ?
O15 Zr1 Zr3 35.84(15) 5_666 . ?
O15 Zr1 O2 139.74(19) 5_666 5_666 ?
O15 Zr1 O9 70.6(4) 5_666 . ?
O15 Zr1 O12 67.9(2) 5_666 5_666 ?
O15 Zr1 O13B 76.8(5) 5_666 . ?
O15 Zr1 O14 108.8(3) 5_666 . ?
O15 Zr1 O19 87.8(2) 5_666 . ?
O15 Zr1 O18B 143.0(10) 5_666 . ?
O18A Zr1 Zr3 120.8(12) . 5_666 ?
O18A Zr1 Zr3 123.2(9) . . ?
O18A Zr1 O2 69.4(11) . 5_666 ?
O18A Zr1 O9 78.3(13) . . ?
O18A Zr1 O12 144.5(12) . 5_666 ?
O18A Zr1 O14 90.9(10) . . ?
O18A Zr1 O15 147.4(12) . 5_666 ?
O18A Zr1 O19 90.4(6) . . ?
O19 Zr1 Zr3 119.04(15) . . ?
O19 Zr1 Zr3 117.48(14) . 5_666 ?
O19 Zr1 O2 72.68(19) . 5_666 ?
O19 Zr1 O9 69.9(5) . . ?
O19 Zr1 O13B 144.7(5) . . ?
O19 Zr1 O18B 101.5(7) . . ?
O18B Zr1 Zr3 113.6(8) . . ?
O13A Zr1 Zr3 31.6(5) . . ?
O13A Zr1 Zr3 83.0(4) . 5_666 ?
O13A Zr1 O2 139.6(5) . 5_666 ?
O13A Zr1 O9 82.5(7) . . ?
O13A Zr1 O12 101.0(4) . 5_666 ?
O13A Zr1 O14 65.9(6) . . ?
O13A Zr1 O15 66.9(5) . 5_666 ?
O13A Zr1 O18A 100.2(7) . . ?
O13A Zr1 O19 147.7(5) . . ?
Zr3 Zr2 Zr1 59.903(17) 5_666 5_666 ?
Zr3 Zr2 Zr1 59.675(17) . 5_666 ?
Zr3 Zr2 Zr3 89.044(19) . 5_666 ?
O5 Zr2 Zr1 107.18(15) 2_664 5_666 ?
O5 Zr2 Zr3 71.43(12) 2_664 5_666 ?
O5 Zr2 Zr3 160.44(12) 2_664 . ?
O5 Zr2 O11 127.39(19) 2_664 . ?
O11 Zr2 Zr1 108.52(18) . 5_666 ?
O11 Zr2 Zr3 161.18(15) . 5_666 ?
O11 Zr2 Zr3 72.13(15) . . ?
O12 Zr2 Zr1 34.03(14) . 5_666 ?
O12 Zr2 Zr3 35.80(14) . . ?
O12 Zr2 Zr3 88.66(16) . 5_666 ?
O12 Zr2 O5 138.4(2) . 2_664 ?
O12 Zr2 O11 76.3(2) . . ?
O12 Zr2 O13B 76.7(5) . . ?
O12 Zr2 O14 109.1(3) . . ?
O12 Zr2 O16 87.5(2) . . ?
O12 Zr2 O17 145.7(2) . . ?
O13B Zr2 Zr3 41.1(4) . . ?
O13B Zr2 O11 71.1(5) . . ?
O13B Zr2 O16 142.3(5) . . ?
O13B Zr2 O17 80.4(4) . . ?
O14 Zr2 Zr1 90.96(18) . 5_666 ?
O14 Zr2 Zr3 36.46(15) . 5_666 ?
O14 Zr2 Zr3 89.13(18) . . ?
O14 Zr2 O5 76.0(2) . 2_664 ?
O14 Zr2 O11 139.3(2) . . ?
O14 Zr2 O13B 71.2(5) . . ?
O14 Zr2 O16 146.4(2) . . ?
O14 Zr2 O17 86.9(2) . . ?
O15 Zr2 Zr1 33.85(15) . 5_666 ?
O15 Zr2 Zr3 36.04(14) . 5_666 ?
O15 Zr2 Zr3 88.26(18) . . ?
O15 Zr2 O5 75.3(2) . 2_664 ?
O15 Zr2 O11 139.7(2) . . ?
O15 Zr2 O12 67.9(2) . . ?
O15 Zr2 O13B 115.9(4) . . ?
O15 Zr2 O14 72.5(2) . . ?
O15 Zr2 O16 88.2(2) . . ?
O15 Zr2 O17 146.2(2) . . ?
O16 Zr2 Zr1 87.28(17) . 5_666 ?
O16 Zr2 Zr3 118.19(16) . . ?
O16 Zr2 Zr3 119.28(16) . 5_666 ?
O16 Zr2 O5 72.5(2) . 2_664 ?
O16 Zr2 O11 72.0(2) . . ?
O16 Zr2 O17 95.4(2) . . ?
O17 Zr2 Zr1 177.27(17) . 5_666 ?
O17 Zr2 Zr3 118.63(17) . 5_666 ?
O17 Zr2 Zr3 118.56(17) . . ?
O17 Zr2 O5 73.9(2) . 2_664 ?
O17 Zr2 O11 72.2(2) . . ?
O13A Zr2 Zr1 83.4(3) . 5_666 ?
O13A Zr2 Zr3 82.2(4) . 5_666 ?
O13A Zr2 Zr3 32.5(5) . . ?
O13A Zr2 O5 140.0(5) . 2_664 ?
O13A Zr2 O11 81.6(5) . . ?
O13A Zr2 O12 67.7(5) . . ?
O13A Zr2 O14 65.1(5) . . ?
O13A Zr2 O15 100.6(4) . . ?
O13A Zr2 O16 147.5(5) . . ?
O13A Zr2 O17 94.1(4) . . ?
Zr1 Zr3 Zr2 60.698(17) 5_666 5_666 ?
Zr1 Zr3 Zr2 60.590(18) 5_666 . ?
Zr2 Zr3 Zr2 90.954(19) . 5_666 ?
O1 Zr3 Zr1 76.13(10) . 5_666 ?
O1 Zr3 Zr2 111.97(10) . . ?
O1 Zr3 Zr2 111.35(11) . 5_666 ?
O1 Zr3 O10 74.16(17) . . ?
O1 Zr3 O13B 141.3(5) . . ?
O6 Zr3 Zr1 110.99(10) 6_557 5_666 ?
O6 Zr3 Zr2 75.66(10) 6_557 5_666 ?
O6 Zr3 Zr2 166.61(11) 6_557 . ?
O6 Zr3 O1 73.54(14) 6_557 . ?
O6 Zr3 O10 117.34(17) 6_557 . ?
O6 Zr3 O13B 142.2(5) 6_557 . ?
O8 Zr3 Zr1 168.3(7) . 5_666 ?
O8 Zr3 Zr2 114.4(8) . . ?
O8 Zr3 Zr2 110.4(8) . 5_666 ?
O8 Zr3 O1 115.3(7) . . ?
O8 Zr3 O6 71.7(8) . 6_557 ?
O8 Zr3 O10 76.1(8) . . ?
O8 Zr3 O12 145.4(8) . . ?
O8 Zr3 O14 140.4(8) . 5_666 ?
O8 Zr3 O15 79.1(8) . 5_666 ?
O10 Zr3 Zr1 111.18(13) . 5_666 ?
O10 Zr3 Zr2 76.04(13) . . ?
O10 Zr3 Zr2 166.99(13) . 5_666 ?
O10 Zr3 O13B 74.1(4) . . ?
O12 Zr3 Zr1 35.16(14) . 5_666 ?
O12 Zr3 Zr2 35.08(14) . . ?
O12 Zr3 Zr2 90.22(16) . 5_666 ?
O12 Zr3 O1 79.71(18) . . ?
O12 Zr3 O6 142.23(17) . 6_557 ?
O12 Zr3 O10 79.0(2) . . ?
O12 Zr3 O13B 72.9(5) . . ?
O12 Zr3 O14 70.6(2) . 5_666 ?
O12 Zr3 O15 108.6(3) . 5_666 ?
O13B Zr3 Zr2 38.0(5) . . ?
O14 Zr3 Zr1 35.48(14) 5_666 5_666 ?
O14 Zr3 Zr2 35.47(14) 5_666 5_666 ?
O14 Zr3 Zr2 90.68(18) 5_666 . ?
O14 Zr3 O1 78.7(2) 5_666 . ?
O14 Zr3 O6 78.3(2) 5_666 6_557 ?
O14 Zr3 O10 142.24(17) 5_666 . ?
O14 Zr3 O13B 115.8(5) 5_666 . ?
O15 Zr3 Zr1 90.07(16) 5_666 5_666 ?
O15 Zr3 Zr2 35.03(14) 5_666 5_666 ?
O15 Zr3 Zr2 89.84(18) 5_666 . ?
O15 Zr3 O1 142.39(17) 5_666 . ?
O15 Zr3 O6 79.4(2) 5_666 6_557 ?
O15 Zr3 O10 142.82(19) 5_666 . ?
O15 Zr3 O13B 73.8(5) 5_666 . ?
O15 Zr3 O14 70.48(19) 5_666 5_666 ?
O13A Zr3 Zr1 84.8(4) . 5_666 ?
O13A Zr3 Zr2 33.2(5) . . ?
O13A Zr3 Zr2 83.7(4) . 5_666 ?
O13A Zr3 O1 144.3(5) . . ?
O13A Zr3 O6 142.0(5) . 6_557 ?
O13A Zr3 O8 86.6(9) . . ?
O13A Zr3 O10 85.4(4) . . ?
O13A Zr3 O12 67.7(5) . . ?
O13A Zr3 O14 102.7(4) . 5_666 ?
O13A Zr3 O15 65.8(5) . 5_666 ?
C1 O1 Zr3 130.4(4) . . ?
C1 O2 Zr1 135.7(4) . 5_666 ?
C24 O5 Zr2 135.0(4) . 2_665 ?
C24 O6 Zr3 130.9(4) . 6_657 ?
C19 O7 H7 109.5 . . ?
C25 O8 Zr3 128(2) . . ?
C25 O9 Zr1 133.1(16) . . ?
C26 O10 Zr3 128.2(5) . . ?
C26 O11 Zr2 132.4(6) . . ?
Zr1 O12 Zr3 109.0(2) 5_666 . ?
Zr2 O12 Zr1 112.0(2) . 5_666 ?
Zr2 O12 Zr3 109.1(2) . . ?
Zr1 O13B Zr3 99.8(6) . . ?
Zr2 O13B Zr1 105.6(8) . . ?
Zr2 O13B Zr3 100.9(7) . . ?
Zr1 O14 Zr2 111.8(3) . . ?
Zr1 O14 Zr3 108.0(2) . 5_666 ?
Zr2 O14 Zr3 108.1(2) . 5_666 ?
Zr1 O15 Zr2 112.3(3) 5_666 . ?
Zr1 O15 Zr3 109.3(3) 5_666 5_666 ?
Zr2 O15 Zr3 108.9(2) . 5_666 ?
C12 N1 C10 106.3(9) . . ?
C11 N2 H2 125.4 . . ?
C12 N2 H2 125.4 . . ?
C12 N2 C11 109.3(8) . . ?
O1 C1 C2 116.7(5) . . ?
O2 C1 O1 126.0(5) . . ?
O2 C1 C2 117.3(5) . . ?
C3 C2 C1 120.9(5) . . ?
C4 C2 C1 120.0(5) . . ?
C4 C2 C3 118.9(6) . . ?
C2 C3 C2 120.1(7) 7_565 . ?
C2 C3 H3 119.9 7_565 . ?
C2 C3 H3 119.9 . . ?
C2 C4 H4 119.0 . . ?
C5 C4 C2 121.9(5) . . ?
C5 C4 H4 119.0 . . ?
C4 C5 C4 118.2(7) 7_565 . ?
C4 C5 C6 119.8(5) 7_565 . ?
C4 C5 C6 121.9(5) . . ?
N2 C11 C6 134.9(6) . . ?
N2 C11 C10 104.9(6) . . ?
C6 C11 C10 120.0 . . ?
C11 C6 C5 121.4(5) . . ?
C7 C6 C5 118.5(5) . . ?
C7 C6 C11 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7A 120.0 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 C20 119.9(5) . . ?
C10 C9 C20 119.9(5) . . ?
C11 C10 N1 108.8(6) . . ?
C9 C10 N1 130.9(6) . . ?
C9 C10 C11 120.0 . . ?
N1 C12 N2 110.4(11) . . ?
N1 C12 C13 123.1(11) . . ?
N2 C12 C13 126.4(11) . . ?
C14 C13 C12 120.6(11) . . ?
C19 C13 C12 117.3(12) . . ?
C19 C13 C14 122.1(12) . . ?
C13 C14 H14 120.9 . . ?
C13 C14 C15 118.2(12) . . ?
C15 C14 H14 120.9 . . ?
C14 C15 H15 120.2 . . ?
C16 C15 C14 119.7(13) . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C17 122.7(13) . . ?
C18 C16 C15 119.2(12) . . ?
C18 C16 C17 116.9(13) . . ?
O3 C17 C16 118.9(15) . . ?
O4 C17 O3 124.9(19) . . ?
O4 C17 C16 115.7(19) . . ?
C16 C18 H18 119.1 . . ?
C16 C18 C19 121.7(13) . . ?
C19 C18 H18 119.1 . . ?
O7 C19 C13 123.9(12) . . ?
O7 C19 C18 117.4(12) . . ?
C13 C19 C18 118.5(13) . . ?
C21 C20 C9 124.1(5) . . ?
C21 C20 C9 118.5(5) 7_565 . ?
C21 C20 C21 117.3(7) . 7_565 ?
C20 C21 H21 118.8 . . ?
C20 C21 C22 122.5(6) . . ?
C22 C21 H21 118.8 . . ?
C21 C22 C24 120.5(6) . . ?
C23 C22 C21 118.5(6) . . ?
C23 C22 C24 121.0(5) . . ?
C22 C23 C22 120.6(7) . 7_565 ?
C22 C23 H23 119.7 7_565 . ?
C22 C23 H23 119.7 . . ?
O5 C24 O6 126.9(6) . . ?
O5 C24 C22 117.0(5) . . ?
O6 C24 C22 116.1(6) . . ?
O8 C25 O9 130(2) . . ?
O8 C25 H25 115.0 . . ?
O9 C25 H25 115.0 . . ?
O10 C26 H26 114.4 . . ?
O11 C26 O10 131.1(8) . . ?
O11 C26 H26 114.4 . . ?
Zr1 O13A Zr2 116.5(9) . . ?
Zr1 O13A Zr3 116.9(8) . . ?
Zr3 O13A Zr2 114.3(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 Zr3 3.5106(8) . ?
Zr1 Zr3 3.4967(8) 5_666 ?
Zr1 O2 2.273(5) 5_666 ?
Zr1 O9 2.25(2) . ?
Zr1 O12 2.129(5) 5_666 ?
Zr1 O13B 2.245(19) . ?
Zr1 O14 2.134(5) . ?
Zr1 O15 2.124(5) 5_666 ?
Zr1 O18A 2.10(4) . ?
Zr1 O19 2.185(5) . ?
Zr1 O18B 2.29(4) . ?
Zr1 O13A 2.057(19) . ?
Zr2 Zr3 3.4988(8) . ?
Zr2 Zr3 3.5026(8) 5_666 ?
Zr2 O5 2.251(5) 2_664 ?
Zr2 O11 2.270(5) . ?
Zr2 O12 2.128(5) . ?
Zr2 O13B 2.20(2) . ?
Zr2 O14 2.138(5) . ?
Zr2 O15 2.125(5) . ?
Zr2 O16 2.197(5) . ?
Zr2 O17 2.210(6) . ?
Zr2 O13A 2.103(18) . ?
Zr3 O1 2.209(4) . ?
Zr3 O6 2.199(4) 6_557 ?
Zr3 O8 2.13(3) . ?
Zr3 O10 2.213(5) . ?
Zr3 O12 2.166(5) . ?
Zr3 O13B 2.342(18) . ?
Zr3 O14 2.190(5) 5_666 ?
Zr3 O15 2.179(5) 5_666 ?
Zr3 O13A 2.063(18) . ?
O1 C1 1.277(7) . ?
O2 C1 1.235(7) . ?
O3 C17 1.266(9) . ?
O4 C17 1.258(9) . ?
O5 C24 1.251(8) . ?
O6 C24 1.255(7) . ?
O7 H7 0.8400 . ?
O7 C19 1.350(16) . ?
O8 C25 1.260(9) . ?
O9 C25 1.262(9) . ?
O10 C26 1.267(10) . ?
O11 C26 1.224(11) . ?
N1 C10 1.428(11) . ?
N1 C12 1.317(14) . ?
N2 H2 0.8800 . ?
N2 C11 1.386(11) . ?
N2 C12 1.369(14) . ?
C1 C2 1.487(8) . ?
C2 C3 1.401(7) . ?
C2 C4 1.398(7) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.385(7) . ?
C5 C6 1.514(8) . ?
C11 C6 1.3900 . ?
C11 C10 1.3900 . ?
C6 C7 1.3900 . ?
C7 H7A 0.9500 . ?
C7 C8 1.3900 . ?
C8 H8 0.9500 . ?
C8 C9 1.3900 . ?
C9 C10 1.3900 . ?
C9 C20 1.516(8) . ?
C12 C13 1.449(17) . ?
C13 C14 1.379(19) . ?
C13 C19 1.365(17) . ?
C14 H14 0.9500 . ?
C14 C15 1.422(17) . ?
C15 H15 0.9500 . ?
C15 C16 1.395(17) . ?
C16 C17 1.40(2) . ?
C16 C18 1.359(19) . ?
C18 H18 0.9500 . ?
C18 C19 1.396(18) . ?
C20 C21 1.376(7) 7_565 ?
C20 C21 1.376(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.411(8) . ?
C22 C23 1.385(7) . ?
C22 C24 1.498(9) . ?
C23 H23 0.9500 . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O2 C1 O1 9.2(12) 5_666 . . . ?
Zr1 O2 C1 C2 -172.9(4) 5_666 . . . ?
Zr1 O9 C25 O8 17(3) . . . . ?
Zr2 O5 C24 O6 4.4(12) 2_665 . . . ?
Zr2 O5 C24 C22 -175.1(5) 2_665 . . . ?
Zr2 O11 C26 O10 3(2) . . . . ?
Zr3 O1 C1 O2 -8.5(10) . . . . ?
Zr3 O1 C1 C2 173.6(4) . . . . ?
Zr3 O6 C24 O5 -0.8(10) 6_657 . . . ?
Zr3 O6 C24 C22 178.6(4) 6_657 . . . ?
Zr3 O8 C25 O9 -7(4) . . . . ?
Zr3 O10 C26 O11 -2.0(18) . . . . ?
O1 C1 C2 C3 -21.2(9) . . . . ?
O1 C1 C2 C4 163.4(6) . . . . ?
O2 C1 C2 C3 160.7(7) . . . . ?
O2 C1 C2 C4 -14.7(9) . . . . ?
N1 C12 C13 C14 -155.7(16) . . . . ?
N1 C12 C13 C19 23(2) . . . . ?
N2 C11 C6 C5 -7.9(11) . . . . ?
N2 C11 C6 C7 173.5(11) . . . . ?
N2 C11 C10 N1 -1.1(9) . . . . ?
N2 C11 C10 C9 -175.2(8) . . . . ?
N2 C12 C13 C14 21(3) . . . . ?
N2 C12 C13 C19 -160.4(15) . . . . ?
C1 C2 C3 C2 -174.3(5) . . . 7_565 ?
C1 C2 C4 C5 175.5(6) . . . . ?
C2 C4 C5 C4 -1.1(12) . . . 7_565 ?
C2 C4 C5 C6 -177.9(6) . . . . ?
C3 C2 C4 C5 0.0(10) . . . . ?
C4 C2 C3 C2 1.1(12) . . . 7_565 ?
C4 C5 C6 C11 130.2(7) 7_565 . . . ?
C4 C5 C6 C11 -53.0(9) . . . . ?
C4 C5 C6 C7 -51.2(9) 7_565 . . . ?
C4 C5 C6 C7 125.6(7) . . . . ?
C5 C6 C7 C8 -178.7(8) . . . . ?
C11 N2 C12 N1 -6.5(15) . . . . ?
C11 N2 C12 C13 176.6(15) . . . . ?
C11 C6 C7 C8 0.0 . . . . ?
C6 C11 C10 N1 174.1(8) . . . . ?
C6 C11 C10 C9 0.0 . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C7 C8 C9 C20 174.5(8) . . . . ?
C8 C9 C10 N1 -172.6(10) . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C8 C9 C20 C21 53.4(9) . . . 7_565 ?
C8 C9 C20 C21 -123.7(8) . . . . ?
C9 C20 C21 C22 174.2(7) . . . . ?
C10 N1 C12 N2 5.6(14) . . . . ?
C10 N1 C12 C13 -177.4(14) . . . . ?
C10 C11 C6 C5 178.6(8) . . . . ?
C10 C11 C6 C7 0.0 . . . . ?
C10 C9 C20 C21 50.8(10) . . . . ?
C10 C9 C20 C21 -132.1(7) . . . 7_565 ?
C12 N1 C10 C11 -2.8(11) . . . . ?
C12 N1 C10 C9 170.5(9) . . . . ?
C12 N2 C11 C6 -169.7(9) . . . . ?
C12 N2 C11 C10 4.5(11) . . . . ?
C12 C13 C14 C15 -178.8(16) . . . . ?
C12 C13 C19 O7 -5(3) . . . . ?
C12 C13 C19 C18 179.9(17) . . . . ?
C13 C14 C15 C16 2(3) . . . . ?
C14 C13 C19 O7 173.7(19) . . . . ?
C14 C13 C19 C18 -1(3) . . . . ?
C14 C15 C16 C17 -174.9(17) . . . . ?
C14 C15 C16 C18 -8(3) . . . . ?
C15 C16 C17 O3 31(3) . . . . ?
C15 C16 C17 O4 -141(2) . . . . ?
C15 C16 C18 C19 9(3) . . . . ?
C16 C18 C19 O7 -180.0(18) . . . . ?
C16 C18 C19 C13 -5(3) . . . . ?
C17 C16 C18 C19 177.0(17) . . . . ?
C18 C16 C17 O3 -136.2(19) . . . . ?
C18 C16 C17 O4 52(2) . . . . ?
C19 C13 C14 C15 2(3) . . . . ?
C20 C9 C10 N1 12.9(10) . . . . ?
C20 C9 C10 C11 -174.5(8) . . . . ?
C20 C21 C22 C23 -0.5(11) . . . . ?
C20 C21 C22 C24 179.3(7) . . . . ?
C21 C20 C21 C22 -2.9(13) 7_565 . . . ?
C21 C22 C23 C22 4.1(13) . . . 7_565 ?
C21 C22 C24 O5 -24.6(10) . . . . ?
C21 C22 C24 O6 155.9(6) . . . . ?
C23 C22 C24 O5 155.2(7) . . . . ?
C23 C22 C24 O6 -24.3(10) . . . . ?
C24 C22 C23 C22 -175.7(5) . . . 7_565 ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.148 -0.619 -0.631 5757.4 784.3 ?
