#------------------------------------------------------------------------------
#$Date: 2024-03-04 04:09:35 +0200 (Mon, 04 Mar 2024) $
#$Revision: 290044 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/10/1571096.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_1571096
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-pH12
_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   mixed
_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                   28.8021(13)
_cell_length_b                   25.3660(12)
_cell_length_c                   13.6242(7)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.31
_cell_volume                     9953.8(8)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON 100'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1112
_diffrn_reflns_av_unetI/netI     0.0631
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            89747
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         1.697
_diffrn_source_current           40.0
_diffrn_source_power             1.8
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.656
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5614
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1163 before and 0.0845 after correction.
The Ratio of minimum to maximum transmission is 0.7530.
The λ/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.011
_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         0.982
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         11636
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0512
_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)+(0.0818P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7824
_reflns_number_total             11636
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc05410a2.cif
_cod_data_source_block           ph12
_cod_database_code               1571096
_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   0.937
_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
 O9-C25 = O8-C25 = O3-C17 = O4-C17
 1.25 with sigma of 0.01
3. Rigid bond restraints
 Zr1, O18A, O18B
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
 C8, C9, C10, C20
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.04
4. Uiso/Uaniso restraints and constraints
O3 \\sim O4 \\sim C17: 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
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
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
Zr1 \\sim O18A \\sim O18B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
C8 \\sim C9 \\sim C10 \\sim C20: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(O4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
5. Others
 Fixed Sof: O3(0.5) O4(0.5) O7(0.5) H7(0.5) O8(0.5) O9(0.5) O13A(0.5)
 O13B(0.5) O18A(0.5) O18B(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)
6.a Riding coordinates:
 O7(H7)
6.b 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)
6.c Fitted hexagon refined as free rotating group:
 C11(C6,C7,C8,C9,C10)
;
_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 0.42868(2) 0.52789(2) 0.40944(3) 0.03762(13) Uani 1 1 d . U . . .
Zr2 Zr 0.54873(2) 0.52914(2) 0.35861(3) 0.03699(12) Uani 1 1 d . . . . .
Zr3 Zr 0.49415(2) 0.41136(2) 0.42804(3) 0.02814(11) Uani 1 1 d . . . . .
O1 O 0.54492(8) 0.34873(9) 0.4642(2) 0.0327(6) Uani 1 1 d . . . . .
O2 O 0.59479(11) 0.38829(11) 0.5675(3) 0.0577(10) Uani 1 1 d . . . . .
O3 O 0.8951(10) 0.4703(8) 0.2005(17) 0.077(6) Uani 0.5 1 d D U P A -1
O4 O 0.9377(5) 0.3937(6) 0.1815(12) 0.031(3) Uani 0.5 1 d D U P A -1
O5 O 0.92549(11) 0.38695(11) 0.8612(3) 0.0570(10) Uani 1 1 d . . . . .
O6 O 0.95479(9) 0.34857(9) 0.9968(2) 0.0375(7) Uani 1 1 d . . . . .
O7 O 0.9038(4) 0.3138(5) 0.5006(9) 0.154(5) Uani 0.5 1 d . . P A -1
H7 H 0.887943 0.308399 0.551364 0.231 Uiso 0.5 1 d R U P A -1
O8 O 0.4389(7) 0.3851(7) 0.3346(14) 0.053(4) Uani 0.5 1 d D U P B 1
O9 O 0.3941(9) 0.4625(6) 0.3246(15) 0.054(4) Uani 0.5 1 d D U P B 1
O10 O 0.52875(12) 0.39010(12) 0.2880(2) 0.0506(8) Uani 1 1 d . . . . .
O11 O 0.56411(17) 0.46869(16) 0.2393(3) 0.0854(14) Uani 1 1 d . . . . .
O12 O 0.55733(15) 0.45715(13) 0.4381(3) 0.0670(11) Uani 1 1 d . . . . .
O13A O 0.4848(3) 0.4830(3) 0.3253(5) 0.0317(16) Uani 0.5 1 d . . P B 1
O13B O 0.4868(3) 0.4850(4) 0.3732(5) 0.0340(18) Uani 0.5 1 d . . P B 2
O14 O 0.49142(11) 0.57064(17) 0.4203(3) 0.0681(12) Uani 1 1 d . . . . .
O15 O 0.56284(16) 0.54385(13) 0.5109(3) 0.0756(13) Uani 1 1 d . . . . .
O16 O 0.62418(13) 0.52663(13) 0.3370(4) 0.0800(14) Uani 1 1 d . . . . .
O17 O 0.5280(2) 0.56375(15) 0.2187(3) 0.1074(17) Uani 1 1 d . . . . .
O18A O 0.4147(6) 0.5619(8) 0.2599(18) 0.068(4) Uani 0.5 1 d . U P B 1
O18B O 0.4306(7) 0.5617(8) 0.2640(18) 0.084(6) Uani 0.5 1 d . U P B 2
O19 O 0.35539(12) 0.52461(13) 0.4518(4) 0.0808(14) Uani 1 1 d . . . . .
N1 N 0.8310(2) 0.3008(3) 0.6054(6) 0.0445(18) Uani 0.5 1 d . . P A -1
N2 N 0.7621(2) 0.3033(3) 0.5277(5) 0.0400(17) Uani 0.5 1 d . . P A -1
H2 H 0.741150 0.309840 0.482329 0.048 Uiso 0.5 1 calc R U P A -1
C1 C 0.57969(13) 0.34905(14) 0.5224(3) 0.0367(10) Uani 1 1 d . . . . .
C2 C 0.60344(12) 0.29750(14) 0.5396(3) 0.0327(9) Uani 1 1 d . . . . .
C3 C 0.58169(18) 0.250000 0.5158(5) 0.0337(13) Uani 1 2 d S T P . .
H3 H 0.552418 0.250000 0.483681 0.040 Uiso 1 2 calc R U P . .
C4 C 0.64696(13) 0.29734(14) 0.5834(3) 0.0370(10) Uani 1 1 d . . . . .
H4 H 0.661464 0.329860 0.599355 0.044 Uiso 1 1 calc R U . . .
C5 C 0.66974(18) 0.250000 0.6043(4) 0.0298(12) Uani 1 2 d S T P . .
C11 C 0.75470(14) 0.2762(2) 0.6142(3) 0.0335(16) Uani 0.5 1 d G U P A -1
C6 C 0.71704(11) 0.2494(3) 0.6537(3) 0.0334(13) Uani 0.5 1 d G U P A -1
C7 C 0.72204(13) 0.2216(2) 0.7410(3) 0.0438(19) Uani 0.5 1 d G U P A -1
H7A H 0.696302 0.203203 0.768110 0.053 Uiso 0.5 1 calc R U P A -1
C8 C 0.76469(15) 0.2207(2) 0.7887(3) 0.0428(19) Uani 0.5 1 d G U P A -1
H8 H 0.768106 0.201671 0.848413 0.051 Uiso 0.5 1 calc R U P A -1
C9 C 0.80235(11) 0.2475(3) 0.7492(3) 0.0342(13) Uani 0.5 1 d G U P A -1
C10 C 0.79735(12) 0.2753(2) 0.6619(3) 0.0322(16) Uani 0.5 1 d G U P A -1
C12 C 0.8072(3) 0.3178(4) 0.5249(7) 0.047(2) Uani 0.5 1 d . . P A -1
C13 C 0.8317(3) 0.3417(5) 0.4445(8) 0.063(3) Uani 0.5 1 d . U P A -1
C14 C 0.8093(4) 0.3788(5) 0.3854(9) 0.083(3) Uani 0.5 1 d . U P A -1
H14 H 0.777175 0.385217 0.394964 0.100 Uiso 0.5 1 calc R U P A -1
C15 C 0.8331(4) 0.4066(5) 0.3123(9) 0.084(3) Uani 0.5 1 d . U P A -1
H15 H 0.818729 0.435652 0.280453 0.101 Uiso 0.5 1 calc R U P A -1
C16 C 0.8784(4) 0.3914(5) 0.2864(9) 0.073(3) Uani 0.5 1 d . U P A -1
C17 C 0.9050(7) 0.4214(7) 0.2170(11) 0.048(4) Uani 0.5 1 d D U P A -1
C18 C 0.9019(4) 0.3564(5) 0.3492(10) 0.084(3) Uani 0.5 1 d . U P A -1
H18 H 0.933558 0.347322 0.338832 0.100 Uiso 0.5 1 calc R U P A -1
C19 C 0.8754(4) 0.3346(5) 0.4312(9) 0.078(3) Uani 0.5 1 d . U P A -1
C20 C 0.84852(18) 0.250000 0.8071(5) 0.0335(12) Uani 1 2 d S TU P . .
C21 C 0.86923(13) 0.29694(16) 0.8324(4) 0.0408(10) Uani 1 1 d . . . . .
H21 H 0.856104 0.329327 0.811008 0.049 Uiso 1 1 calc R U . . .
C22 C 0.90942(13) 0.29706(15) 0.8892(3) 0.0363(10) Uani 1 1 d . . . . .
C23 C 0.92822(19) 0.250000 0.9213(5) 0.0356(13) Uani 1 2 d S T P . .
H23 H 0.953872 0.250001 0.965096 0.043 Uiso 1 2 calc R U P . .
C24 C 0.93165(14) 0.34799(15) 0.9189(4) 0.0405(11) Uani 1 1 d . . . . .
C25 C 0.4058(8) 0.4141(7) 0.3089(15) 0.065(4) Uani 0.5 1 d D U P B 1
H25 H 0.384225 0.396199 0.268090 0.078 Uiso 0.5 1 calc R U P B 1
C26 C 0.5545(3) 0.4192(2) 0.2322(5) 0.088(2) Uani 1 1 d . . . . .
H26 H 0.568344 0.401603 0.178084 0.106 Uiso 1 1 calc R U . . .
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 89.080(12) 5_666 . ?
O2 Zr1 Zr3 160.80(8) 5_666 . ?
O2 Zr1 Zr3 71.72(7) 5_666 5_666 ?
O2 Zr1 O9 129.3(5) 5_666 . ?
O2 Zr1 O13A 138.8(2) 5_666 . ?
O9 Zr1 Zr3 158.5(5) . 5_666 ?
O9 Zr1 Zr3 69.8(5) . . ?
O9 Zr1 O13A 71.9(6) . . ?
O12 Zr1 Zr3 88.75(11) 5_666 . ?
O12 Zr1 Zr3 35.99(9) 5_666 5_666 ?
O12 Zr1 O2 75.82(14) 5_666 5_666 ?
O12 Zr1 O9 135.1(6) 5_666 . ?
O12 Zr1 O13A 116.1(2) 5_666 . ?
O12 Zr1 O18A 147.2(6) 5_666 . ?
O12 Zr1 O18B 144.3(6) 5_666 . ?
O12 Zr1 O19 86.16(17) 5_666 . ?
O13A Zr1 Zr3 95.01(19) . 5_666 ?
O13A Zr1 Zr3 40.4(2) . . ?
O13B Zr1 Zr3 30.2(2) . . ?
O13B Zr1 O14 65.9(3) . . ?
O13B Zr1 O18B 88.2(6) . . ?
O13B Zr1 O19 145.9(3) . . ?
O14 Zr1 Zr3 35.47(10) . 5_666 ?
O14 Zr1 Zr3 88.15(11) . . ?
O14 Zr1 O2 76.26(13) . 5_666 ?
O14 Zr1 O9 142.4(6) . . ?
O14 Zr1 O12 71.44(14) . 5_666 ?
O14 Zr1 O13A 71.7(2) . . ?
O14 Zr1 O15 107.73(18) . 5_666 ?
O14 Zr1 O18A 91.1(5) . . ?
O14 Zr1 O18B 80.7(6) . . ?
O14 Zr1 O19 145.65(13) . . ?
O15 Zr1 Zr3 88.90(12) 5_666 5_666 ?
O15 Zr1 Zr3 35.37(11) 5_666 . ?
O15 Zr1 O2 140.21(14) 5_666 5_666 ?
O15 Zr1 O9 71.6(5) 5_666 . ?
O15 Zr1 O12 68.72(14) 5_666 5_666 ?
O15 Zr1 O13A 75.5(2) 5_666 . ?
O15 Zr1 O18A 144.0(6) 5_666 . ?
O15 Zr1 O18B 143.4(6) 5_666 . ?
O15 Zr1 O19 86.78(17) 5_666 . ?
O18A Zr1 Zr3 121.2(5) . 5_666 ?
O18A Zr1 Zr3 119.0(6) . . ?
O18A Zr1 O2 73.1(6) . 5_666 ?
O18A Zr1 O9 74.9(8) . . ?
O18A Zr1 O13A 82.2(6) . . ?
O18B Zr1 Zr3 112.7(6) . . ?
O18B Zr1 O19 106.3(6) . . ?
O19 Zr1 Zr3 117.58(12) . 5_666 ?
O19 Zr1 Zr3 117.79(9) . . ?
O19 Zr1 O2 73.14(13) . 5_666 ?
O19 Zr1 O9 71.4(6) . . ?
O19 Zr1 O13A 142.7(2) . . ?
O19 Zr1 O18A 94.6(5) . . ?
Zr3 Zr2 Zr1 59.979(10) . . ?
Zr3 Zr2 Zr1 59.660(11) 5_666 . ?
Zr3 Zr2 Zr3 89.150(13) 5_666 . ?
O5 Zr2 Zr1 109.17(8) 2_664 . ?
O5 Zr2 Zr3 161.44(9) 2_664 . ?
O5 Zr2 Zr3 72.32(8) 2_664 5_666 ?
O5 Zr2 O11 125.63(14) 2_664 . ?
O11 Zr2 Zr1 108.94(12) . . ?
O11 Zr2 Zr3 162.05(11) . 5_666 ?
O11 Zr2 Zr3 72.91(11) . . ?
O12 Zr2 Zr1 90.37(11) . . ?
O12 Zr2 Zr3 89.35(11) . 5_666 ?
O12 Zr2 Zr3 35.63(10) . . ?
O12 Zr2 O5 139.53(13) . 2_664 ?
O12 Zr2 O11 76.33(16) . . ?
O12 Zr2 O13A 75.5(2) . . ?
O12 Zr2 O15 68.72(13) . . ?
O12 Zr2 O16 85.90(15) . . ?
O12 Zr2 O17 144.88(14) . . ?
O13A Zr2 Zr1 39.2(2) . . ?
O13A Zr2 Zr3 95.99(19) . 5_666 ?
O13A Zr2 Zr3 40.3(2) . . ?
O13A Zr2 O5 140.5(2) . 2_664 ?
O13A Zr2 O11 70.2(2) . . ?
O13B Zr2 Zr1 31.8(2) . . ?
O13B Zr2 Zr3 31.3(2) . . ?
O13B Zr2 O11 82.8(2) . . ?
O13B Zr2 O12 66.3(3) . . ?
O13B Zr2 O14 64.6(2) . . ?
O13B Zr2 O15 99.3(2) . . ?
O13B Zr2 O16 146.3(3) . . ?
O13B Zr2 O17 93.7(3) . . ?
O14 Zr2 Zr1 33.63(9) . . ?
O14 Zr2 Zr3 35.52(10) . 5_666 ?
O14 Zr2 Zr3 88.13(11) . . ?
O14 Zr2 O5 77.44(13) . 2_664 ?
O14 Zr2 O11 139.87(15) . . ?
O14 Zr2 O12 108.20(17) . . ?
O14 Zr2 O13A 72.5(2) . . ?
O14 Zr2 O15 71.32(14) . . ?
O14 Zr2 O16 146.59(14) . . ?
O14 Zr2 O17 86.18(19) . . ?
O15 Zr2 Zr1 89.85(12) . . ?
O15 Zr2 Zr3 88.41(11) . . ?
O15 Zr2 Zr3 35.84(10) . 5_666 ?
O15 Zr2 O5 76.03(14) . 2_664 ?
O15 Zr2 O11 140.33(16) . . ?
O15 Zr2 O13A 116.4(2) . . ?
O15 Zr2 O16 86.98(18) . . ?
O15 Zr2 O17 145.70(14) . . ?
O16 Zr2 Zr1 175.79(13) . . ?
O16 Zr2 Zr3 118.27(12) . 5_666 ?
O16 Zr2 Zr3 117.11(9) . . ?
O16 Zr2 O5 72.74(12) . 2_664 ?
O16 Zr2 O11 72.07(17) . . ?
O16 Zr2 O13A 140.9(2) . . ?
O17 Zr2 Zr1 84.65(16) . . ?
O17 Zr2 Zr3 117.12(12) . . ?
O17 Zr2 Zr3 117.08(14) . 5_666 ?
O17 Zr2 O5 73.96(15) . 2_664 ?
O17 Zr2 O11 72.59(18) . . ?
O17 Zr2 O13A 78.9(2) . . ?
O17 Zr2 O16 99.5(2) . . ?
Zr1 Zr3 Zr2 60.665(12) 5_666 . ?
Zr1 Zr3 Zr2 60.543(12) 5_666 5_666 ?
Zr2 Zr3 Zr2 90.849(13) 5_666 . ?
O1 Zr3 Zr1 75.85(7) . 5_666 ?
O1 Zr3 Zr2 112.04(6) . . ?
O1 Zr3 Zr2 110.96(8) . 5_666 ?
O1 Zr3 O10 73.76(11) . . ?
O1 Zr3 O13A 140.9(2) . . ?
O6 Zr3 Zr1 110.56(8) 6_557 5_666 ?
O6 Zr3 Zr2 75.21(7) 6_557 5_666 ?
O6 Zr3 Zr2 166.06(7) 6_557 . ?
O6 Zr3 O1 73.64(10) 6_557 . ?
O6 Zr3 O10 117.01(11) 6_557 . ?
O6 Zr3 O13A 142.1(2) 6_557 . ?
O8 Zr3 Zr1 170.1(5) . 5_666 ?
O8 Zr3 Zr2 115.9(5) . . ?
O8 Zr3 Zr2 111.4(5) . 5_666 ?
O8 Zr3 O1 113.5(4) . . ?
O8 Zr3 O6 70.7(5) . 6_557 ?
O8 Zr3 O10 75.4(5) . . ?
O8 Zr3 O12 146.0(5) . . ?
O8 Zr3 O13A 78.4(5) . . ?
O8 Zr3 O14 141.0(5) . 5_666 ?
O8 Zr3 O15 80.1(5) . 5_666 ?
O10 Zr3 Zr1 111.48(9) . 5_666 ?
O10 Zr3 Zr2 76.92(8) . . ?
O10 Zr3 Zr2 167.74(9) . 5_666 ?
O10 Zr3 O13A 73.9(2) . . ?
O12 Zr3 Zr1 35.75(10) . 5_666 ?
O12 Zr3 Zr2 90.74(11) . 5_666 ?
O12 Zr3 Zr2 35.13(10) . . ?
O12 Zr3 O1 79.38(12) . . ?
O12 Zr3 O6 142.24(12) . 6_557 ?
O12 Zr3 O10 78.86(14) . . ?
O12 Zr3 O13A 73.3(2) . . ?
O13A Zr3 Zr1 96.37(19) . 5_666 ?
O13A Zr3 Zr2 38.6(2) . . ?
O13A Zr3 Zr2 97.07(19) . 5_666 ?
O13B Zr3 Zr2 32.9(2) . . ?
O13B Zr3 O1 144.4(2) . . ?
O13B Zr3 O10 87.3(2) . . ?
O13B Zr3 O12 67.4(3) . . ?
O14 Zr3 Zr1 34.63(9) 5_666 5_666 ?
O14 Zr3 Zr2 89.53(11) 5_666 . ?
O14 Zr3 Zr2 35.02(9) 5_666 5_666 ?
O14 Zr3 O1 79.14(13) 5_666 . ?
O14 Zr3 O6 78.89(13) 5_666 6_557 ?
O14 Zr3 O10 142.06(12) 5_666 . ?
O14 Zr3 O12 70.36(13) 5_666 . ?
O14 Zr3 O13A 115.9(2) 5_666 . ?
O14 Zr3 O15 70.51(14) 5_666 5_666 ?
O15 Zr3 Zr1 90.41(11) 5_666 5_666 ?
O15 Zr3 Zr2 35.52(10) 5_666 5_666 ?
O15 Zr3 Zr2 89.80(11) 5_666 . ?
O15 Zr3 O1 142.40(12) 5_666 . ?
O15 Zr3 O6 79.09(13) 5_666 6_557 ?
O15 Zr3 O10 143.07(13) 5_666 . ?
O15 Zr3 O12 109.39(17) 5_666 . ?
O15 Zr3 O13A 74.4(2) 5_666 . ?
C1 O1 Zr3 130.6(2) . . ?
C1 O2 Zr1 135.8(3) . 5_666 ?
C24 O5 Zr2 134.1(3) . 2_665 ?
C24 O6 Zr3 132.4(2) . 6_657 ?
C19 O7 H7 108.0 . . ?
C25 O8 Zr3 123.2(14) . . ?
C25 O9 Zr1 132.0(16) . . ?
C26 O10 Zr3 128.6(3) . . ?
C26 O11 Zr2 131.9(4) . . ?
Zr1 O12 Zr3 108.26(16) 5_666 . ?
Zr2 O12 Zr1 111.12(15) . 5_666 ?
Zr2 O12 Zr3 109.24(17) . . ?
Zr1 O13A Zr3 99.8(3) . . ?
Zr2 O13A Zr1 102.7(3) . . ?
Zr2 O13A Zr3 101.2(3) . . ?
Zr1 O13B Zr2 115.4(4) . . ?
Zr3 O13B Zr1 119.0(4) . . ?
Zr3 O13B Zr2 115.8(4) . . ?
Zr1 O14 Zr2 112.43(16) . . ?
Zr1 O14 Zr3 109.90(17) . 5_666 ?
Zr2 O14 Zr3 109.46(16) . 5_666 ?
Zr1 O15 Zr2 111.43(16) 5_666 . ?
Zr1 O15 Zr3 109.82(19) 5_666 5_666 ?
Zr2 O15 Zr3 108.64(17) . 5_666 ?
C12 N1 C10 104.0(6) . . ?
C11 N2 H2 126.0 . . ?
C12 N2 H2 126.0 . . ?
C12 N2 C11 108.0(6) . . ?
O1 C1 C2 116.8(3) . . ?
O2 C1 O1 125.7(3) . . ?
O2 C1 C2 117.4(4) . . ?
C3 C2 C1 120.9(3) . . ?
C4 C2 C1 118.9(3) . . ?
C4 C2 C3 120.2(4) . . ?
C2 C3 C2 119.3(5) 7_565 . ?
C2 C3 H3 120.4 . . ?
C2 C3 H3 120.4 7_565 . ?
C2 C4 H4 119.5 . . ?
C2 C4 C5 120.9(4) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C4 118.4(5) . 7_565 ?
C4 C5 C6 121.4(4) . . ?
C4 C5 C6 120.1(4) 7_565 . ?
N2 C11 C6 134.1(4) . . ?
N2 C11 C10 105.7(4) . . ?
C6 C11 C10 120.0 . . ?
C11 C6 C5 121.5(3) . . ?
C7 C6 C5 118.5(3) . . ?
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 119.5(3) . . ?
C10 C9 C20 120.3(4) . . ?
C11 C10 N1 110.4(4) . . ?
C9 C10 N1 129.4(4) . . ?
C9 C10 C11 120.0 . . ?
N1 C12 C13 120.1(8) . . ?
N2 C12 N1 111.9(7) . . ?
N2 C12 C13 127.5(8) . . ?
C14 C13 C12 119.8(9) . . ?
C19 C13 C12 121.9(9) . . ?
C19 C13 C14 117.8(10) . . ?
C13 C14 H14 119.2 . . ?
C13 C14 C15 121.6(10) . . ?
C15 C14 H14 119.2 . . ?
C14 C15 H15 120.2 . . ?
C14 C15 C16 119.6(11) . . ?
C16 C15 H15 120.2 . . ?
C15 C16 C17 121.1(11) . . ?
C15 C16 C18 117.9(10) . . ?
C18 C16 C17 118.5(11) . . ?
O3 C17 C16 120.3(13) . . ?
O4 C17 O3 128.8(17) . . ?
O4 C17 C16 110.8(14) . . ?
C16 C18 H18 121.6 . . ?
C16 C18 C19 116.8(10) . . ?
C19 C18 H18 121.6 . . ?
O7 C19 C18 111.4(10) . . ?
C13 C19 O7 123.2(11) . . ?
C13 C19 C18 124.5(10) . . ?
C21 C20 C9 117.7(4) 7_565 . ?
C21 C20 C9 122.3(4) . . ?
C21 C20 C21 119.9(5) 7_565 . ?
C20 C21 H21 120.0 . . ?
C20 C21 C22 120.1(4) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 C24 120.5(4) . . ?
C23 C22 C21 120.0(4) . . ?
C23 C22 C24 119.5(4) . . ?
C22 C23 C22 119.5(5) 7_565 . ?
C22 C23 H23 120.2 7_565 . ?
C22 C23 H23 120.2 . . ?
O5 C24 C22 116.3(4) . . ?
O6 C24 O5 125.9(4) . . ?
O6 C24 C22 117.8(4) . . ?
O8 C25 O9 135(2) . . ?
O8 C25 H25 112.3 . . ?
O9 C25 H25 112.3 . . ?
O10 C26 H26 115.3 . . ?
O11 C26 O10 129.4(6) . . ?
O11 C26 H26 115.3 . . ?
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 3.4955(6) 5_666 ?
Zr1 Zr3 3.5154(5) . ?
Zr1 O2 2.253(3) 5_666 ?
Zr1 O9 2.25(2) . ?
Zr1 O12 2.150(3) 5_666 ?
Zr1 O13A 2.286(8) . ?
Zr1 O13B 2.057(8) . ?
Zr1 O14 2.113(3) . ?
Zr1 O15 2.133(3) 5_666 ?
Zr1 O18A 2.25(2) . ?
Zr1 O18B 2.16(3) . ?
Zr1 O19 2.190(4) . ?
Zr2 Zr3 3.5003(6) 5_666 ?
Zr2 Zr3 3.5062(5) . ?
Zr2 O5 2.254(3) 2_664 ?
Zr2 O11 2.278(4) . ?
Zr2 O12 2.137(3) . ?
Zr2 O13A 2.228(8) . ?
Zr2 O13B 2.115(8) . ?
Zr2 O14 2.130(3) . ?
Zr2 O15 2.146(4) . ?
Zr2 O16 2.194(4) . ?
Zr2 O17 2.181(4) . ?
Zr3 O1 2.215(2) . ?
Zr3 O6 2.207(3) 6_557 ?
Zr3 O8 2.14(2) . ?
Zr3 O10 2.219(3) . ?
Zr3 O12 2.163(3) . ?
Zr3 O13A 2.310(8) . ?
Zr3 O13B 2.023(9) . ?
Zr3 O14 2.157(4) 5_666 ?
Zr3 O15 2.163(4) 5_666 ?
O1 C1 1.277(5) . ?
O2 C1 1.248(5) . ?
O3 C17 1.293(9) . ?
O4 C17 1.271(8) . ?
O5 C24 1.275(5) . ?
O6 C24 1.254(5) . ?
O7 H7 0.8400 . ?
O7 C19 1.357(13) . ?
O8 C25 1.253(9) . ?
O9 C25 1.291(9) . ?
O10 C26 1.294(7) . ?
O11 C26 1.288(6) . ?
N1 C10 1.395(8) . ?
N1 C12 1.363(11) . ?
N2 H2 0.8800 . ?
N2 C11 1.379(8) . ?
N2 C12 1.352(10) . ?
C1 C2 1.494(5) . ?
C2 C3 1.396(4) . ?
C2 C4 1.388(5) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C4 C5 1.398(4) . ?
C5 C6 1.520(6) . ?
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 1.548(6) . ?
C12 C13 1.436(12) . ?
C13 C14 1.395(14) . ?
C13 C19 1.284(13) . ?
C14 H14 0.9500 . ?
C14 C15 1.400(14) . ?
C15 H15 0.9500 . ?
C15 C16 1.404(14) . ?
C16 C17 1.43(2) . ?
C16 C18 1.409(15) . ?
C18 H18 0.9500 . ?
C18 C19 1.462(15) . ?
C20 C21 1.375(5) 7_565 ?
C20 C21 1.375(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.392(5) . ?
C22 C23 1.382(5) . ?
C22 C24 1.498(5) . ?
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 7.5(8) 5_666 . . . ?
Zr1 O2 C1 C2 -170.8(3) 5_666 . . . ?
Zr1 O9 C25 O8 2(4) . . . . ?
Zr2 O5 C24 O6 2.7(8) 2_665 . . . ?
Zr2 O5 C24 C22 -176.6(3) 2_665 . . . ?
Zr2 O11 C26 O10 7.7(13) . . . . ?
Zr3 O1 C1 O2 -6.0(7) . . . . ?
Zr3 O1 C1 C2 172.3(3) . . . . ?
Zr3 O6 C24 O5 0.2(7) 6_657 . . . ?
Zr3 O6 C24 C22 179.5(3) 6_657 . . . ?
Zr3 O8 C25 O9 1(4) . . . . ?
Zr3 O10 C26 O11 -5.4(11) . . . . ?
O1 C1 C2 C3 -16.9(7) . . . . ?
O1 C1 C2 C4 165.5(4) . . . . ?
O2 C1 C2 C3 161.6(5) . . . . ?
O2 C1 C2 C4 -16.0(6) . . . . ?
N1 C12 C13 C14 -151.7(11) . . . . ?
N1 C12 C13 C19 20.4(19) . . . . ?
N2 C11 C6 C5 -6.6(7) . . . . ?
N2 C11 C6 C7 174.1(7) . . . . ?
N2 C11 C10 N1 -0.8(6) . . . . ?
N2 C11 C10 C9 -175.6(5) . . . . ?
N2 C12 C13 C14 37.5(18) . . . . ?
N2 C12 C13 C19 -150.4(13) . . . . ?
C1 C2 C3 C2 -175.2(3) . . . 7_565 ?
C1 C2 C4 C5 177.6(4) . . . . ?
C2 C4 C5 C4 -2.3(9) . . . 7_565 ?
C2 C4 C5 C6 -178.9(4) . . . . ?
C3 C2 C4 C5 0.0(7) . . . . ?
C4 C2 C3 C2 2.3(9) . . . 7_565 ?
C4 C5 C6 C11 -56.1(7) . . . . ?
C4 C5 C6 C11 127.3(5) 7_565 . . . ?
C4 C5 C6 C7 123.1(5) . . . . ?
C4 C5 C6 C7 -53.5(6) 7_565 . . . ?
C5 C6 C7 C8 -179.3(6) . . . . ?
C11 N2 C12 N1 1.3(11) . . . . ?
C11 N2 C12 C13 172.7(10) . . . . ?
C11 C6 C7 C8 0.0 . . . . ?
C6 C11 C10 N1 174.8(6) . . . . ?
C6 C11 C10 C9 0.0 . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C7 C8 C9 C20 175.1(6) . . . . ?
C8 C9 C10 N1 -173.7(7) . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C8 C9 C20 C21 -123.2(5) . . . . ?
C8 C9 C20 C21 57.7(7) . . . 7_565 ?
C9 C20 C21 C22 176.5(5) . . . . ?
C10 N1 C12 N2 -1.7(10) . . . . ?
C10 N1 C12 C13 -173.9(9) . . . . ?
C10 C11 C6 C5 179.3(6) . . . . ?
C10 C11 C6 C7 0.0 . . . . ?
C10 C9 C20 C21 -127.3(5) . . . 7_565 ?
C10 C9 C20 C21 51.8(7) . . . . ?
C12 N1 C10 C11 1.5(8) . . . . ?
C12 N1 C10 C9 175.7(6) . . . . ?
C12 N2 C11 C6 -175.0(6) . . . . ?
C12 N2 C11 C10 -0.3(8) . . . . ?
C12 C13 C14 C15 173.8(13) . . . . ?
C12 C13 C19 O7 -14(2) . . . . ?
C12 C13 C19 C18 178.0(13) . . . . ?
C13 C14 C15 C16 11(2) . . . . ?
C14 C13 C19 O7 158.1(14) . . . . ?
C14 C13 C19 C18 -10(2) . . . . ?
C14 C15 C16 C17 -175.5(15) . . . . ?
C14 C15 C16 C18 -14(2) . . . . ?
C15 C16 C17 O3 22(3) . . . . ?
C15 C16 C17 O4 -160.0(15) . . . . ?
C15 C16 C18 C19 6(2) . . . . ?
C16 C18 C19 O7 -162.9(14) . . . . ?
C16 C18 C19 C13 6(2) . . . . ?
C17 C16 C18 C19 168.2(14) . . . . ?
C18 C16 C17 O3 -139.6(19) . . . . ?
C18 C16 C17 O4 38(2) . . . . ?
C19 C13 C14 C15 1(2) . . . . ?
C20 C9 C10 N1 11.3(7) . . . . ?
C20 C9 C10 C11 -175.0(6) . . . . ?
C20 C21 C22 C23 -0.8(8) . . . . ?
C20 C21 C22 C24 -178.7(5) . . . . ?
C21 C20 C21 C22 -4.4(9) 7_565 . . . ?
C21 C22 C23 C22 6.0(9) . . . 7_565 ?
C21 C22 C24 O5 -28.2(7) . . . . ?
C21 C22 C24 O6 152.5(4) . . . . ?
C23 C22 C24 O5 154.0(5) . . . . ?
C23 C22 C24 O6 -25.4(7) . . . . ?
C24 C22 C23 C22 -176.1(4) . . . 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 -0.618 -0.854 -0.415 5750.7 868.5 ?
