#------------------------------------------------------------------------------
#$Date: 2019-11-10 00:58:42 +0200 (Sun, 10 Nov 2019) $
#$Revision: 225480 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/53/4515317.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_4515317
loop_
_publ_author_name
'Zhang, Yong-Zheng'
'He, Tao'
'Kong, Xiang-Jing'
'Lv, Xiu-Liang'
'Wu, Xue-Qian'
'Li, Jian-Rong'
_publ_section_title
;
 Tuning Water Sorption in Highly Stable Zr(IV)-Metal-Organic Frameworks
 through Local Functionalization of Metal Clusters.
;
_journal_issue                   33
_journal_name_full               'ACS applied materials & interfaces'
_journal_page_first              27868
_journal_page_last               27874
_journal_paper_doi               10.1021/acsami.8b09333
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         '0.13(C768 H480 O280 Zr48)'
_chemical_formula_sum            'C96 H60 O35 Zr6'
_chemical_formula_weight         2320.76
_space_group_crystal_system      cubic
_space_group_IT_number           212
_space_group_name_Hall           'P 4acd 2ab 3'
_space_group_name_H-M_alt        'P 43 3 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-07
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.9225(9)
_cell_length_b                   32.9225(9)
_cell_length_c                   32.9225(9)
_cell_measurement_reflns_used    1291
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      71.9430
_cell_measurement_theta_min      3.7710
_cell_volume                     35684.4(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω   -116.00 -61.00   1.00   30.00    --  -41.94 -38.00  90.00   55
  2  ω     94.00 124.00   1.00   75.00    --  105.88 125.00-180.00   30
  3  ω    125.00 169.00   1.00   75.00    --  105.88 125.00 -90.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0084551000
_diffrn_orient_matrix_UB_12      -0.0415723000
_diffrn_orient_matrix_UB_13      -0.0197861000
_diffrn_orient_matrix_UB_21      -0.0104138000
_diffrn_orient_matrix_UB_22      0.0213090000
_diffrn_orient_matrix_UB_23      -0.0403453000
_diffrn_orient_matrix_UB_31      0.0448157000
_diffrn_orient_matrix_UB_32      -0.0029156000
_diffrn_orient_matrix_UB_33      -0.0131010000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1726
_diffrn_reflns_av_unetI/netI     0.2337
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            25567
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         65.040
_diffrn_reflns_theta_min         3.798
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.864
_exptl_crystal_description       block
_exptl_crystal_F_000             9248
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.021
_refine_diff_density_min         -1.654
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 1384 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         10166
_refine_ls_number_restraints     260
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0730P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2257
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.940
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5248
_reflns_number_total             10166
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            am8b09333_si_002.cif
_cod_data_source_block           BUT-46A
_cod_original_cell_volume        35684(3)
_cod_database_code               4515317
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C H O Zr'
_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.
;
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. 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
2. Restrained planarity
 C69, C20, C18, C51, C45
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.002
Uanis(O6) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O7) = Uanis(O12)
Uanis(O1) = Uanis(O4)
4.a Rotating group:
 O11(H11A,H11B)
4.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C21(H21), C27(H27), C28(H28), C29(H29), C32(H32), C35(H35),
 C47(H47), C37(H37), C40(H40), C44(H44), C49(H49), C55(H55), C64(H64), C2(H2)
4.c Fitted hexagon refined as free rotating group:
 C35(C45,C51,C47,C39,C42)
4.d Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.857
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+3/4, x+1/4, z+3/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+1/4'
'x+3/4, -z+3/4, y+1/4'
'x+1/2, -y+1/2, -z'
'x+1/4, z+3/4, -y+3/4'
'z+1/4, y+3/4, -x+3/4'
'-x, y+1/2, -z+1/2'
'-z+3/4, y+1/4, x+3/4'
'z, x, y'
'y, z, x'
'-y+1/2, -z, x+1/2'
'z+1/2, -x+1/2, -y'
'-y, z+1/2, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'-x+3/4, z+1/4, y+3/4'
'-x+1/4, -z+1/4, -y+1/4'
'z+3/4, -y+3/4, x+1/4'
'-z+1/4, -y+1/4, -x+1/4'
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
Zr1 Zr 0.52751(4) 0.47110(4) 0.44296(4) 0.0280(3) Uani 1 1 d . U .
Zr2 Zr 0.73314(4) 0.31868(4) 0.20909(4) 0.0318(4) Uani 1 1 d . U .
O3 O 0.5613(3) 0.5063(3) 0.3978(3) 0.023(2) Uani 1 1 d . U .
O4 O 0.5707(3) 0.5693(3) 0.4188(3) 0.0279(15) Uani 1 1 d . U .
O1 O 0.3433(3) 0.7607(3) 0.1844(3) 0.0279(15) Uani 1 1 d . U .
O8 O 0.3622(3) 0.7252(3) 0.2392(3) 0.036(2) Uani 1 1 d . U .
C8 C 0.4104(5) 0.7328(5) 0.1909(5) 0.037(2) Uani 1 1 d . U .
O11 O 0.5839(3) 0.4355(4) 0.4296(3) 0.045(3) Uani 1 1 d . U .
H11A H 0.5882 0.4148 0.4475 0.068 Uiso 1 1 d GR . .
H11B H 0.6063 0.4513 0.4310 0.068 Uiso 1 1 d GR . .
O7 O 0.8325(3) 0.3551(3) 0.2544(3) 0.0393(19) Uani 1 1 d . U .
O6 O 0.7403(4) 0.4014(4) 0.2822(4) 0.055(2) Uani 1 1 d . U .
C13 C 0.4861(5) 0.7182(5) 0.1603(5) 0.040(2) Uani 1 1 d . U .
O5 O 0.7042(4) 0.3741(3) 0.2293(3) 0.047(3) Uani 1 1 d . U .
C16 C 0.6942(6) 0.4428(6) 0.2408(6) 0.050(3) Uani 1 1 d . U .
C18 C 0.5838(5) 0.6532(5) 0.1433(5) 0.041(3) Uani 1 1 d . U .
O12 O 0.7813(3) 0.3715(3) 0.2073(3) 0.0393(19) Uani 1 1 d . U .
C20 C 0.5481(5) 0.6714(5) 0.1629(5) 0.041(3) Uani 1 1 d . U .
H20 H 0.5388 0.6611 0.1876 0.049 Uiso 1 1 calc R . .
C21 C 0.4801(5) 0.7178(5) 0.2031(5) 0.040(3) Uani 1 1 d . U .
H21 H 0.5013 0.7120 0.2208 0.048 Uiso 1 1 calc R . .
C22 C 0.6592(6) 0.5165(6) 0.2175(5) 0.046(3) Uani 1 1 d . U .
C27 C 0.5898(5) 0.5925(5) 0.3398(5) 0.040(3) Uani 1 1 d . U .
H27 H 0.5874 0.6136 0.3584 0.049 Uiso 1 1 calc R . .
C28 C 0.5798(5) 0.5207(5) 0.3198(5) 0.036(3) Uani 1 1 d . U .
H28 H 0.5730 0.4941 0.3263 0.043 Uiso 1 1 calc R . .
C29 C 0.6828(5) 0.5144(5) 0.2523(5) 0.045(3) Uani 1 1 d . U .
H29 H 0.6868 0.5374 0.2682 0.055 Uiso 1 1 calc R . .
C31 C 0.3696(5) 0.7402(5) 0.2046(5) 0.035(2) Uani 1 1 d . U .
C32 C 0.5893(5) 0.5313(5) 0.2800(5) 0.040(3) Uani 1 1 d . U .
H32 H 0.5858 0.5114 0.2603 0.048 Uiso 1 1 calc R . .
C33 C 0.5708(4) 0.5449(5) 0.3909(4) 0.025(2) Uani 1 1 d . U .
C34 C 0.7114(6) 0.4045(6) 0.2526(6) 0.053(2) Uani 1 1 d . U .
C35 C 0.6539(3) 0.5687(3) 0.1634(3) 0.046(3) Uani 1 1 d . U .
H35 H 0.6741 0.5547 0.1495 0.055 Uiso 1 1 calc R . .
C45 C 0.6345(4) 0.6014(3) 0.1451(2) 0.045(3) Uani 1 1 d G U .
C51 C 0.6043(3) 0.6223(3) 0.1660(3) 0.043(3) Uani 1 1 d G U .
C47 C 0.5935(3) 0.6105(3) 0.2051(3) 0.042(3) Uani 1 1 d G U .
H47 H 0.5733 0.6245 0.2190 0.050 Uiso 1 1 calc R . .
C39 C 0.6130(3) 0.5778(3) 0.2233(2) 0.044(2) Uani 1 1 d G U .
C42 C 0.6432(3) 0.5569(3) 0.2025(3) 0.045(2) Uani 1 1 d G U .
C36 C 0.6027(5) 0.5669(5) 0.2677(5) 0.042(2) Uani 1 1 d . U .
C37 C 0.4172(5) 0.7347(5) 0.1478(5) 0.039(3) Uani 1 1 d . U .
H37 H 0.3964 0.7423 0.1303 0.047 Uiso 1 1 calc R . .
C40 C 0.4548(5) 0.7250(5) 0.1331(5) 0.039(3) Uani 1 1 d . U .
H40 H 0.4592 0.7231 0.1053 0.047 Uiso 1 1 calc R . .
C44 C 0.4429(5) 0.7261(5) 0.2165(5) 0.039(3) Uani 1 1 d . U .
H44 H 0.4387 0.7274 0.2444 0.046 Uiso 1 1 calc R . .
C49 C 0.6027(5) 0.5993(5) 0.2987(5) 0.044(3) Uani 1 1 d . U .
H49 H 0.6114 0.6252 0.2913 0.053 Uiso 1 1 calc R . .
C52 C 0.8137(6) 0.3765(5) 0.2301(6) 0.048(3) Uani 1 1 d . U .
C55 C 0.7006(6) 0.4769(5) 0.2635(6) 0.050(3) Uani 1 1 d . U .
H55 H 0.7169 0.4754 0.2865 0.060 Uiso 1 1 calc R . .
C62 C 0.5807(5) 0.5512(5) 0.3504(5) 0.034(2) Uani 1 1 d . U .
C64 C 0.6525(6) 0.4825(5) 0.1941(6) 0.048(3) Uani 1 1 d . U .
H64 H 0.6374 0.4851 0.1703 0.058 Uiso 1 1 calc R . .
C69 C 0.5276(5) 0.7046(5) 0.1446(5) 0.041(3) Uani 1 1 d . U .
O10 O 0.5747(3) 0.5080(3) 0.4761(3) 0.019(2) Uani 1 1 d . U .
O2 O 0.7029(3) 0.2774(3) 0.2450(3) 0.022(2) Uani 1 1 d . U .
O13 O 0.4629(2) 0.4629(2) 0.4629(2) 0.018(4) Uani 1 3 d S TU P
O9 O 0.7882(4) 0.2882(4) 0.2118(4) 0.065(7) Uani 1 3 d S TU P
C1AA C 0.8290(5) 0.4196(5) 0.2241(6) 0.049(3) Uani 1 1 d . U .
H1AA H 0.8322 0.4325 0.2501 0.074 Uiso 1 1 calc GR . .
H1AB H 0.8097 0.4346 0.2082 0.074 Uiso 1 1 calc GR . .
H1AC H 0.8546 0.4190 0.2103 0.074 Uiso 1 1 calc GR . .
C2 C 0.6687(6) 0.4413(6) 0.2058(5) 0.050(3) Uani 1 1 d . U .
H2 H 0.6628 0.4175 0.1917 0.060 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 '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
Zr1 Zr1 Zr1 59.997(1) 12 11
Zr1 Zr1 Zr2 60.11(4) 12 19_545
Zr1 Zr1 Zr2 60.63(4) 11 10_554
Zr1 Zr1 Zr2 90.53(3) 12 10_554
Zr1 Zr1 Zr2 90.23(3) 11 19_545
Zr2 Zr1 Zr2 60.14(5) 10_554 19_545
O3 Zr1 Zr1 163.2(2) . 12
O3 Zr1 Zr1 107.7(3) . 11
O3 Zr1 Zr2 72.9(2) . 10_554
O3 Zr1 Zr2 111.5(3) . 19_545
O3 Zr1 O1 123.4(3) . 4_455
O3 Zr1 O8 72.5(4) . 8_545
O3 Zr1 O11 73.9(4) . .
O3 Zr1 O10 72.2(3) . .
O3 Zr1 O13 138.1(3) . .
O1 Zr1 Zr1 110.2(3) 4_455 11
O1 Zr1 Zr1 73.2(2) 4_455 12
O1 Zr1 Zr2 163.7(3) 4_455 10_554
O1 Zr1 Zr2 108.7(3) 4_455 19_545
O1 Zr1 O8 79.1(4) 4_455 8_545
O1 Zr1 O11 71.4(4) 4_455 .
O1 Zr1 O10 138.7(3) 4_455 .
O1 Zr1 O13 71.5(4) 4_455 .
O8 Zr1 Zr1 74.3(3) 8_545 11
O8 Zr1 Zr1 111.7(3) 8_545 12
O8 Zr1 Zr2 164.4(3) 8_545 19_545
O8 Zr1 Zr2 109.0(3) 8_545 10_554
O8 Zr1 O11 110.1(4) 8_545 .
O8 Zr1 O10 139.2(4) 8_545 .
O8 Zr1 O13 73.0(4) 8_545 .
O11 Zr1 Zr1 117.5(3) . 12
O11 Zr1 Zr1 175.6(3) . 11
O11 Zr1 Zr2 116.7(3) . 10_554
O11 Zr1 Zr2 85.4(3) . 19_545
O11 Zr1 O10 78.8(4) . .
O11 Zr1 O13 141.3(4) . .
O10 Zr1 Zr1 97.1(2) . 12
O10 Zr1 Zr1 97.8(2) . 11
O10 Zr1 Zr2 39.6(2) . 19_545
O10 Zr1 Zr2 40.2(2) . 10_554
O2 Zr1 Zr1 85.4(3) 10_554 12
O2 Zr1 Zr1 83.9(3) 19_545 11
O2 Zr1 Zr1 34.2(2) 10_554 11
O2 Zr1 Zr1 32.3(3) 19_545 12
O2 Zr1 Zr2 31.2(2) 10_554 10_554
O2 Zr1 Zr2 84.1(2) 19_545 10_554
O2 Zr1 Zr2 83.7(2) 10_554 19_545
O2 Zr1 Zr2 32.2(2) 19_545 19_545
O2 Zr1 O3 143.3(4) 19_545 .
O2 Zr1 O3 79.0(4) 10_554 .
O2 Zr1 O1 81.4(3) 19_545 4_455
O2 Zr1 O1 143.9(4) 10_554 4_455
O2 Zr1 O8 143.4(4) 19_545 8_545
O2 Zr1 O8 82.4(4) 10_554 8_545
O2 Zr1 O11 144.6(4) 10_554 .
O2 Zr1 O11 92.4(4) 19_545 .
O2 Zr1 O10 71.8(3) 19_545 .
O2 Zr1 O10 71.4(3) 10_554 .
O2 Zr1 O2 95.9(5) 10_554 19_545
O2 Zr1 O13 71.6(3) 19_545 .
O2 Zr1 O13 73.5(3) 10_554 .
O13 Zr1 Zr1 39.3(2) . 11
O13 Zr1 Zr1 39.3(2) . 12
O13 Zr1 Zr2 96.4(3) . 19_545
O13 Zr1 Zr2 96.9(3) . 10_554
O13 Zr1 O10 125.2(4) . .
Zr1 Zr2 Zr1 59.26(5) 8_545 19_545
Zr1 Zr2 Zr2 60.19(4) 8_545 17_645
Zr1 Zr2 Zr2 89.76(3) 8_545 18_556
Zr2 Zr2 Zr1 89.47(3) 17_645 19_545
Zr2 Zr2 Zr1 59.67(4) 18_556 19_545
Zr2 Zr2 Zr2 60.0 18_556 17_645
O4 Zr2 Zr1 106.6(2) 8_545 19_545
O4 Zr2 Zr1 73.7(2) 8_545 8_545
O4 Zr2 Zr2 112.9(3) 8_545 17_645
O4 Zr2 Zr2 162.9(2) 8_545 18_556
O4 Zr2 O12 126.5(4) 8_545 .
O7 Zr2 Zr1 112.4(3) 17_645 8_545
O7 Zr2 Zr1 168.6(3) 17_645 19_545
O7 Zr2 Zr2 115.1(3) 17_645 18_556
O7 Zr2 Zr2 79.4(3) 17_645 17_645
O7 Zr2 O4 76.3(4) 17_645 8_545
O7 Zr2 O12 72.4(4) 17_645 .
O7 Zr2 O10 74.6(4) 17_645 8_545
O7 Zr2 O10 144.0(4) 17_645 19_545
O5 Zr2 Zr1 89.6(3) . 19_545
O5 Zr2 Zr1 124.6(3) . 8_545
O5 Zr2 Zr2 173.2(3) . 17_645
O5 Zr2 Zr2 113.9(3) . 18_556
O5 Zr2 O4 73.9(4) . 8_545
O5 Zr2 O7 101.7(4) . 17_645
O5 Zr2 O12 71.4(4) . .
O5 Zr2 O10 146.9(4) . 8_545
O5 Zr2 O10 78.4(4) . 19_545
O12 Zr2 Zr1 159.2(3) . 8_545
O12 Zr2 Zr1 112.5(3) . 19_545
O12 Zr2 Zr2 70.5(3) . 18_556
O12 Zr2 Zr2 102.7(3) . 17_645
O10 Zr2 Zr1 38.8(2) 19_545 19_545
O10 Zr2 Zr1 95.5(2) 8_545 19_545
O10 Zr2 Zr1 95.5(2) 19_545 8_545
O10 Zr2 Zr1 39.2(2) 8_545 8_545
O10 Zr2 Zr2 96.8(2) 19_545 17_645
O10 Zr2 Zr2 96.7(2) 8_545 18_556
O10 Zr2 Zr2 40.0(2) 19_545 18_556
O10 Zr2 Zr2 39.9(2) 8_545 17_645
O10 Zr2 O4 135.5(3) 19_545 8_545
O10 Zr2 O4 73.4(3) 8_545 8_545
O10 Zr2 O12 134.3(4) 8_545 .
O10 Zr2 O12 73.7(3) 19_545 .
O10 Zr2 O10 124.1(4) 19_545 8_545
O2 Zr2 Zr1 33.4(3) . 19_545
O2 Zr2 Zr1 30.6(3) . 8_545
O2 Zr2 Zr2 84.6(3) . 18_556
O2 Zr2 Zr2 83.3(3) . 17_645
O2 Zr2 O4 78.9(3) . 8_545
O2 Zr2 O7 141.1(4) . 17_645
O2 Zr2 O5 99.6(4) . .
O2 Zr2 O12 145.9(4) . .
O2 Zr2 O10 69.8(3) . 8_545
O2 Zr2 O10 72.3(3) . 19_545
O2 Zr2 O9 94.5(7) . .
O9 Zr2 Zr1 82.7(6) . 19_545
O9 Zr2 Zr1 83.2(6) . 8_545
O9 Zr2 Zr2 32.0(2) . 18_556
O9 Zr2 Zr2 32.0(2) . 17_645
O9 Zr2 O4 144.6(3) . 8_545
O9 Zr2 O7 88.8(6) . 17_645
O9 Zr2 O5 141.3(4) . .
O9 Zr2 O12 76.7(6) . .
O9 Zr2 O10 71.8(3) . 8_545
O9 Zr2 O10 72.0(3) . 19_545
C33 O3 Zr1 138.0(9) . .
C33 O4 Zr2 132.6(9) . 10_554
C31 O1 Zr1 135.6(9) . 2_554
C31 O8 Zr1 134.0(11) . 10_554
C37 C8 C31 116.7(16) . .
C44 C8 C31 124.0(16) . .
C44 C8 C37 119.2(16) . .
C52 O7 Zr2 124.4(11) . 18_556
C21 C13 C69 117.2(16) . .
C40 C13 C21 122.5(16) . .
C40 C13 C69 119.7(16) . .
C34 O5 Zr2 139.5(13) . .
C55 C16 C34 120.9(17) . .
C55 C16 C2 124.3(18) . .
C2 C16 C34 114.8(17) . .
C18 C18 C20 121.1(9) 20_665 .
C18 C18 C51 122.8(8) 20_665 .
C51 C18 C20 116.0(13) . .
C52 O12 Zr2 128.7(11) . .
C69 C20 C18 120.4(15) . .
C44 C21 C13 117.1(17) . .
C29 C22 C42 120.5(16) . .
C64 C22 C29 120.9(18) . .
C64 C22 C42 118.3(15) . .
C62 C27 C49 116.3(16) . .
C32 C28 C62 119.2(15) . .
C22 C29 C55 119.3(18) . .
O1 C31 C8 123.8(15) . .
O8 C31 O1 122.7(14) . .
O8 C31 C8 113.4(15) . .
C36 C32 C28 125.8(17) . .
O3 C33 C62 111.2(13) . .
O4 C33 O3 120.1(12) . .
O4 C33 C62 128.7(15) . .
O6 C34 C16 122.2(17) . .
O5 C34 O6 119.8(17) . .
O5 C34 C16 116.8(17) . .
C45 C35 C42 120.0 . .
C35 C45 C45 119.1 . 20_665
C35 C45 C51 120.0 . .
C51 C45 C45 120.73(16) . 20_665
C45 C51 C18 115.6(10) . .
C47 C51 C18 124.2(10) . .
C47 C51 C45 120.0 . .
C51 C47 C39 120.0 . .
C47 C39 C36 119.2(10) . .
C42 C39 C47 120.0 . .
C42 C39 C36 120.7(10) . .
C35 C42 C22 117.4(10) . .
C39 C42 C22 121.5(10) . .
C39 C42 C35 120.0 . .
C32 C36 C39 124.8(16) . .
C32 C36 C49 115.7(16) . .
C49 C36 C39 119.1(14) . .
C40 C37 C8 118.7(17) . .
C37 C40 C13 119.0(16) . .
C21 C44 C8 122.9(17) . .
C27 C49 C36 122.4(16) . .
O7 C52 O12 134.9(16) . .
O7 C52 C1AA 116.9(16) . .
O12 C52 C1AA 108.2(16) . .
C16 C55 C29 120.8(18) . .
C28 C62 C27 119.9(15) . .
C33 C62 C27 115.2(15) . .
C33 C62 C28 124.8(15) . .
C22 C64 C2 122.1(17) . .
C13 C69 C69 121.0(10) . 20_665
C20 C69 C13 120.3(15) . .
C20 C69 C69 118.2(10) . 20_665
Zr1 O10 Zr2 100.6(3) . 10_554
Zr1 O10 Zr2 101.5(3) . 19_545
Zr2 O10 Zr2 100.1(3) 19_545 10_554
Zr1 O2 Zr1 113.5(4) 8_545 19_545
Zr1 O2 Zr2 118.2(4) 8_545 .
Zr2 O2 Zr1 114.4(4) . 19_545
Zr1 O13 Zr1 101.4(4) 12 .
Zr1 O13 Zr1 101.4(4) 11 12
Zr1 O13 Zr1 101.4(4) 11 .
Zr2 O9 Zr2 116.1(4) 18_556 .
Zr2 O9 Zr2 116.1(4) 17_645 .
Zr2 O9 Zr2 116.1(4) 18_556 17_645
C16 C2 C64 112.5(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 Zr1 3.472(2) 12
Zr1 Zr1 3.472(2) 11
Zr1 Zr2 3.5207(19) 19_545
Zr1 Zr2 3.5025(19) 10_554
Zr1 O3 2.188(9) .
Zr1 O1 2.208(10) 4_455
Zr1 O8 2.215(10) 8_545
Zr1 O11 2.240(11) .
Zr1 O10 2.253(9) .
Zr1 O2 2.022(10) 10_554
Zr1 O2 2.129(9) 19_545
Zr1 O13 2.243(6) .
Zr2 Zr1 3.5205(19) 19_545
Zr2 Zr1 3.5024(19) 8_545
Zr2 Zr2 3.519(2) 18_556
Zr2 Zr2 3.519(2) 17_645
Zr2 O4 2.335(9) 8_545
Zr2 O7 2.200(10) 17_645
Zr2 O5 2.161(11) .
Zr2 O12 2.353(10) .
Zr2 O10 2.299(8) 8_545
Zr2 O10 2.292(9) 19_545
Zr2 O2 2.059(9) .
Zr2 O9 2.074(5) .
O3 C33 1.329(17) .
O4 Zr2 2.335(9) 10_554
O4 C33 1.219(17) .
O1 Zr1 2.208(10) 2_554
O1 C31 1.284(18) .
O8 Zr1 2.215(10) 10_554
O8 C31 1.265(18) .
C8 C31 1.44(2) .
C8 C37 1.44(2) .
C8 C44 1.38(2) .
O7 Zr2 2.200(10) 18_556
O7 C52 1.23(2) .
O6 C34 1.36(2) .
C13 C21 1.42(2) .
C13 C40 1.38(2) .
C13 C69 1.53(2) .
O5 C34 1.29(2) .
C16 C34 1.44(2) .
C16 C55 1.36(2) .
C16 C2 1.43(2) .
C18 C18 1.35(3) 20_665
C18 C20 1.47(2) .
C18 C51 1.429(17) .
O12 C52 1.31(2) .
C20 C69 1.42(2) .
C21 C44 1.33(2) .
C22 C29 1.39(2) .
C22 C42 1.514(19) .
C22 C64 1.38(2) .
C27 C49 1.44(2) .
C27 C62 1.43(2) .
C28 C32 1.39(2) .
C28 C62 1.42(2) .
C29 C55 1.42(2) .
C32 C36 1.32(2) .
C33 C62 1.39(2) .
C35 C45 1.3900 .
C35 C42 1.3900 .
C45 C45 1.481(14) 20_665
C45 C51 1.3900 .
C51 C47 1.3900 .
C47 C39 1.3900 .
C39 C42 1.3900 .
C39 C36 1.543(18) .
C36 C49 1.47(2) .
C37 C40 1.37(2) .
C52 C1AA 1.52(2) .
C64 C2 1.51(2) .
C69 C69 1.53(3) 20_665
O10 Zr2 2.299(8) 10_554
O10 Zr2 2.293(9) 19_545
O2 Zr1 2.129(9) 19_545
O2 Zr1 2.022(10) 8_545
O13 Zr1 2.243(6) 11
O13 Zr1 2.243(6) 12
O9 Zr2 2.074(5) 18_556
O9 Zr2 2.074(5) 17_645
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
1 -0.759 -0.673 -0.835 22278.4 4108.9
