# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1852050'
_audit_update_record             
;
2018-06-27 deposited with the CCDC.
2018-08-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'Henicosa-[μ₃-oxido]-nonadeca-[μ₃-hydroxido]-octa-[μ-hydroxido]-tetraicosa-[μ-formiato-κ²O1:O2]-tetra-[formiato-κ²O1:O2]-hepta-[formiato-\kO]-pentaaqua-hexaicosazirconium(IV) penta-formic acid solvate pentadecahydrate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H72 O123 Zr26, 5(C H2 O2) [+ solvent]'
_chemical_formula_sum            'C40 H82 O133 Zr26'
_chemical_formula_weight         5062.77

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4132(8)
_cell_length_b                   18.7392(12)
_cell_length_c                   19.1989(11)
_cell_angle_alpha                71.434(5)
_cell_angle_beta                 73.347(5)
_cell_angle_gamma                81.818(5)
_cell_volume                     3723.3(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    36620
_cell_measurement_theta_min      4.025
_cell_measurement_theta_max      70.953

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.258
_exptl_crystal_F_000             2426
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    15.360
_shelx_estimated_absorpt_T_min   0.579
_shelx_estimated_absorpt_T_max   0.749
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in
F. R. Ahmed (Editor), "Crystallographic Computing",
Munksgaard, Copenhagen (1970), 255 - 270
;
_exptl_absorpt_correction_T_min  0.4903
_exptl_absorpt_correction_T_max  0.6030

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 3 2 0.0070
3 -4 1 0.0300
-5 4 -2 0.0210
1 1 -5 0.0300
-1 -1 5 0.0050
-1 -3 -2 0.0140
3 7 1 0.0080
-3 -6 4 0.0040

#-------------------------------------------------------------------------------
# EXPERIMENTAL DATA
#-------------------------------------------------------------------------------


_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_detector                 Pilatus300K
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_detector_area_resol_mean 5.81
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 3195 frames, detector distance = 60 mm
;
_diffrn_reflns_number            36620
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.025
_diffrn_reflns_theta_max         70.953
_diffrn_reflns_theta_full        67.686
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             14209
_reflns_number_gt                10370
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;


#-------------------------------------------------------------------------------
# COMPUTING DATA
#-------------------------------------------------------------------------------

_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.127.0 (STOE, 2016)
;
_computing_cell_refinement       
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_reduction        
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.77, Darmstadt 2016
;

_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 2.1e (Brandenburg, 1999)'
_computing_publication_material  'WinGX 1.70.01 (Farrugia, 1999)'


#-------------------------------------------------------------------------------
# REFINEMENT DATA
#-------------------------------------------------------------------------------


_refine_special_details          
;
All non-hydrogen atoms belonging to the cluster were refined in anisotropic 
model, while the atoms of the solvate formic acid molecules in isotropic. 
The (C)H hydrogen atoms of the formiates / formic acid molecules were placed 
geometrically and refined in a riding model. The (O)H hydrogen atoms were not 
placed explicitly.

The structure of the cluster features two major problems: a) the site-sharing 
of the H₂O/formiato ligands and b) the correct assignment of the μ₃-O²⁻/
μ₃-OH⁻ ligands. 

The first problem becomes evident after careful examination of the 
atomic thermal motion parameters and residual electron densities, which shows 
features characteristic for disorder both on the periphery of the cluster 
and in the solvate regions. Large thermal displacement parameters of the 
formiate ligands referenced further by their C6 and C7 atoms, which are 
bridging the Zr3, Zr5 and Zr5, Zr4 atoms respectively, and the residual 
peaks at 2.10-2.21 A from the Zr ions suggests partial occupancies of the 
formiate groups and presence of two aqua ligands as the second site-sharing 
components. 

The μ-HCOO⁻/ 2H₂O site-sharing was resolved smoothly with partial 
occupancies of 0.60 / 0.40 for O35-C6-O36 / (O3w, O4w) components and 
0.40 / 0.60 for O37-C7-O38 / (O1w, O2w) ones. A similar monodentate 
HCOO⁻/ H₂O site-sharing with 0.5/0.5 ratio of components was observed 
at the Zr11 ion. Additionally, all the three monodentate formiate groups 
exhibit disorders of carbon atoms, which were refined with fixed partial 
occupancies set to make their thermal parameters approximately equal. 

A set of geometry reastraints and similarity restraints for the thermal 
motion parameters was applied to disordered formiate groups in order to 
improve the refinement stability.

Disordered electron density in the solvate region was modeled using 
SQUEEZE routine.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1148P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14209
_refine_ls_number_parameters     979
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1625
_refine_ls_wR_factor_gt          0.1533
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.976
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.44841(6) 0.63645(4) 0.42434(4) 0.03204(15) Uani 1 1 d . . . . .
Zr2 Zr 0.20628(6) 0.76616(4) 0.48301(4) 0.03531(16) Uani 1 1 d . . . . .
Zr3 Zr 0.26717(7) 0.74902(4) 0.29953(4) 0.04159(18) Uani 1 1 d . . . . .
Zr4 Zr 0.56979(7) 0.78963(4) 0.26327(4) 0.04116(17) Uani 1 1 d . . . . .
Zr5 Zr 0.33567(7) 0.91439(4) 0.32481(4) 0.04276(18) Uani 1 1 d . . . . .
Zr6 Zr 0.51344(6) 0.80761(4) 0.44730(4) 0.03479(16) Uani 1 1 d . . . . .
Zr7 Zr 0.44008(6) 0.54259(4) 0.62204(4) 0.03061(15) Uani 1 1 d . . . . .
Zr8 Zr 0.19775(6) 0.67433(4) 0.67707(4) 0.03370(16) Uani 1 1 d . . . . .
Zr9 Zr 0.24987(6) 0.50465(4) 0.81245(4) 0.03502(16) Uani 1 1 d . . . . .
Zr10 Zr 0.55284(6) 0.54346(4) 0.77742(4) 0.03476(16) Uani 1 1 d . . . . .
Zr11 Zr 0.31508(6) 0.67508(4) 0.82668(4) 0.03814(17) Uani 1 1 d . . . . .
Zr12 Zr 0.50526(6) 0.71434(4) 0.64162(4) 0.03322(16) Uani 1 1 d . . . . .
Zr13 Zr 0.70256(6) 0.52912(4) 0.47683(4) 0.03346(16) Uani 1 1 d . . . . .
O1 O 0.2517(5) 0.6738(3) 0.4194(3) 0.0359(12) Uani 1 1 d . . . . .
O2 O 0.4417(5) 0.7065(3) 0.3137(3) 0.0395(12) Uani 1 1 d . . . . .
O3 O 0.5941(5) 0.7207(3) 0.3783(3) 0.0368(12) Uani 1 1 d . . . . .
O4 O 0.3875(5) 0.7280(3) 0.4705(3) 0.0333(11) Uani 1 1 d . . . . .
O5 O 0.2350(5) 0.8192(3) 0.3666(3) 0.0410(13) Uani 1 1 d . . . . .
O6 O 0.3919(6) 0.8462(4) 0.2413(4) 0.0469(14) Uani 1 1 d . . . . .
O7 O 0.4961(5) 0.8537(3) 0.3365(3) 0.0405(13) Uani 1 1 d . . . . .
O8 O 0.3238(5) 0.8641(3) 0.4527(4) 0.0401(13) Uani 1 1 d . . . . .
O9 O 0.2416(4) 0.5451(3) 0.6898(3) 0.0341(12) Uani 1 1 d . . . . .
O10 O 0.4268(5) 0.5032(3) 0.7409(3) 0.0338(11) Uani 1 1 d . . . . .
O11 O 0.5834(5) 0.5920(3) 0.6498(3) 0.0328(11) Uani 1 1 d . . . . .
O12 O 0.3809(4) 0.6533(3) 0.6277(3) 0.0331(11) Uani 1 1 d . . . . .
O13 O 0.2240(5) 0.6186(3) 0.7847(3) 0.0381(12) Uani 1 1 d . . . . .
O14 O 0.3740(5) 0.5516(3) 0.8621(3) 0.0367(12) Uani 1 1 d . . . . .
O15 O 0.4832(5) 0.6544(3) 0.7559(3) 0.0367(12) Uani 1 1 d . . . . .
O16 O 0.3160(5) 0.7437(3) 0.7049(3) 0.0366(12) Uani 1 1 d . . . . .
O17 O 0.5563(5) 0.5987(4) 0.5088(3) 0.0470(15) Uani 1 1 d . . . . .
O18 O 0.3393(5) 0.5689(4) 0.5333(3) 0.0432(14) Uani 1 1 d . . . . .
O19 O 0.6122(6) 0.5654(4) 0.3834(4) 0.0563(18) Uani 1 1 d . . . . .
O20 O 0.6037(6) 0.4660(4) 0.5901(4) 0.0524(17) Uani 1 1 d . . . . .
O21 O 0.1579(5) 0.6624(3) 0.5770(3) 0.0380(12) Uani 1 1 d . . . . .
O22 O 0.1816(5) 0.7808(3) 0.5926(3) 0.0365(12) Uani 1 1 d . . . . .
O23 O 0.6107(5) 0.7248(3) 0.5238(3) 0.0360(12) Uani 1 1 d . . . . .
O24 O 0.4574(5) 0.8163(3) 0.5619(3) 0.0381(12) Uani 1 1 d . . . . .
C1 C -0.0027(9) 0.7340(5) 0.4191(6) 0.049(2) Uani 1 1 d . . . . .
H1 H -0.0872 0.7276 0.4273 0.059 Uiso 1 1 calc R U . . .
O25 O 0.0275(5) 0.7416(4) 0.4750(4) 0.0449(14) Uani 1 1 d . . . . .
O26 O 0.0631(5) 0.7339(4) 0.3550(4) 0.0485(15) Uani 1 1 d . . . . .
C2 C 0.0805(9) 0.9392(6) 0.4397(6) 0.052(2) Uani 1 1 d . . . . .
H2 H 0.0099 0.9715 0.4502 0.063 Uiso 1 1 calc R U . . .
O27 O 0.0750(6) 0.8715(4) 0.4813(4) 0.0467(14) Uani 1 1 d . . . . .
O28 O 0.1685(6) 0.9687(3) 0.3861(4) 0.0480(15) Uani 1 1 d . . . . .
C3 C 0.4841(9) 0.9912(6) 0.3985(6) 0.052(2) Uani 1 1 d . . . . .
H3 H 0.5067 1.0363 0.4025 0.063 Uiso 1 1 calc R U . . .
O29 O 0.4088(6) 0.9991(3) 0.3591(4) 0.0510(16) Uani 1 1 d . . . . .
O30 O 0.5320(5) 0.9316(3) 0.4324(4) 0.0455(14) Uani 1 1 d . . . . .
C4 C 0.7742(8) 0.8374(6) 0.3264(6) 0.052(2) Uani 1 1 d . . . . .
H4 H 0.8549 0.8528 0.3152 0.062 Uiso 1 1 calc R U . . .
O31 O 0.7471(6) 0.8239(4) 0.2720(4) 0.0495(15) Uani 1 1 d . . . . .
O32 O 0.7121(5) 0.8334(3) 0.3904(4) 0.0461(14) Uani 1 1 d . . . . .
C5 C 0.4630(13) 0.7584(7) 0.1380(7) 0.068(3) Uani 1 1 d . . . . .
H5 H 0.4758 0.7603 0.0863 0.082 Uiso 1 1 calc R U . . .
O33 O 0.3555(8) 0.7437(4) 0.1800(4) 0.0633(19) Uani 1 1 d . . . . .
O34 O 0.5561(7) 0.7709(5) 0.1559(4) 0.067(2) Uani 1 1 d . . . . .
C6 C 0.5685(13) 0.9659(6) 0.1725(8) 0.060(2) Uani 0.6 1 d D U P A -1
H6 H 0.6041 1.0061 0.1300 0.071 Uiso 0.6 1 calc R U P A -1
O35 O 0.6187(15) 0.9008(7) 0.1752(10) 0.058(3) Uani 0.6 1 d D U P A -1
O36 O 0.4761(11) 0.9833(6) 0.2203(7) 0.059(2) Uani 0.6 1 d D U P A -1
C7 C 0.131(2) 0.9041(12) 0.2311(16) 0.067(4) Uani 0.4 1 d D U P A -2
H7 H 0.0643 0.9285 0.2104 0.081 Uiso 0.4 1 calc R U P A -2
O37 O 0.157(5) 0.8359(13) 0.233(3) 0.066(5) Uani 0.4 1 d D U P A -2
O38 O 0.184(2) 0.9433(10) 0.2544(12) 0.068(4) Uani 0.4 1 d D U P A -2
O1W O 0.640(3) 0.8762(14) 0.1612(15) 0.071(7) Uani 0.4 1 d . . P A -3
O2W O 0.409(2) 0.9963(14) 0.2217(13) 0.079(4) Uani 0.4 1 d . U P A -3
O3W O 0.164(3) 0.8249(14) 0.2197(17) 0.077(6) Uani 0.6 1 d . . P A -3
O4W O 0.2352(15) 0.9772(9) 0.2416(8) 0.076(4) Uani 0.6 1 d . U P A -3
C8 C -0.0137(8) 0.5594(5) 0.7778(5) 0.046(2) Uani 1 1 d . . . . .
H8 H -0.0976 0.5493 0.7895 0.056 Uiso 1 1 calc R U . . .
O39 O 0.0194(5) 0.6196(4) 0.7273(4) 0.0448(14) Uani 1 1 d . . . . .
O40 O 0.0516(5) 0.5103(4) 0.8151(4) 0.0430(14) Uani 1 1 d . . . . .
C9 C 0.0703(9) 0.7711(6) 0.7972(6) 0.054(2) Uani 1 1 d . . . . .
H9 H 0.0070 0.8068 0.8107 0.065 Uiso 1 1 calc R U . . .
O41 O 0.0654(5) 0.7476(4) 0.7452(4) 0.0462(14) Uani 1 1 d . . . . .
O42 O 0.1514(6) 0.7530(4) 0.8351(4) 0.0513(16) Uani 1 1 d . . . . .
C10 C 0.4727(8) 0.8245(5) 0.7484(5) 0.044(2) Uani 1 1 d . . . . .
H10 H 0.4935 0.8698 0.7530 0.052 Uiso 1 1 calc R U . . .
O43 O 0.5276(5) 0.8085(3) 0.6884(3) 0.0428(13) Uani 1 1 d . . . . .
O44 O 0.3933(6) 0.7878(4) 0.8032(4) 0.0493(15) Uani 1 1 d . . . . .
C11 C 0.7671(9) 0.6621(6) 0.6809(6) 0.056(3) Uani 1 1 d . . . . .
H11 H 0.8507 0.6721 0.6704 0.067 Uiso 1 1 calc R U . . .
O45 O 0.7027(5) 0.7107(3) 0.6434(4) 0.0458(14) Uani 1 1 d . . . . .
O46 O 0.7317(5) 0.6013(4) 0.7313(4) 0.0468(15) Uani 1 1 d . . . . .
C12 C 0.4298(9) 0.3906(6) 0.9005(5) 0.052(2) Uani 1 1 d . . . . .
H12 H 0.4399 0.3463 0.9400 0.062 Uiso 1 1 calc R U . . .
O47 O 0.3233(6) 0.4065(4) 0.8917(3) 0.0460(14) Uani 1 1 d . . . . .
O48 O 0.5253(6) 0.4262(4) 0.8632(3) 0.0458(14) Uani 1 1 d . . . . .
C13 C 0.1257(9) 0.5563(6) 0.9617(6) 0.053(2) Uani 1 1 d . . . . .
H13 H 0.0741 0.5444 1.0119 0.064 Uiso 1 1 calc R U . . .
O49 O 0.1410(6) 0.5074(4) 0.9274(3) 0.0486(15) Uani 1 1 d . . . . .
O50 O 0.1723(6) 0.6200(4) 0.9358(4) 0.0525(16) Uani 1 1 d . . . . .
C14A C 0.2485(16) 0.3323(5) 0.8092(6) 0.042(4) Uani 0.5 1 d D . P . .
H14A H 0.2449 0.3079 0.8619 0.050 Uiso 0.5 1 d R U P . .
C14B C 0.3046(9) 0.3571(6) 0.7672(10) 0.045(4) Uani 0.5 1 d D . P . .
H14B H 0.3876 0.3709 0.7546 0.054 Uiso 0.5 1 d R U P . .
O51 O 0.2175(5) 0.4016(3) 0.7885(4) 0.0469(15) Uani 1 1 d D . . . .
O52 O 0.2850(6) 0.2943(4) 0.7626(4) 0.0504(15) Uani 1 1 d D . . . .
C15A C 0.6806(9) 0.4036(6) 0.7261(10) 0.0523(13) Uani 0.6 1 d D U P . .
H15A H 0.5990 0.3871 0.7400 0.063 Uiso 0.6 1 d R U P . .
C15B C 0.744(2) 0.3996(6) 0.7518(8) 0.0516(13) Uani 0.4 1 d D U P . .
H15B H 0.7582 0.3786 0.8015 0.062 Uiso 0.4 1 d R U P . .
O53 O 0.6981(6) 0.4660(3) 0.7325(4) 0.0523(12) Uani 1 1 d D U . . .
O54 O 0.7709(6) 0.3603(4) 0.7062(4) 0.0512(12) Uani 1 1 d D U . . .
C16 C 0.6296(12) 0.5032(8) 0.9364(7) 0.075(4) Uani 1 1 d . . . . .
H16 H 0.6209 0.4508 0.9475 0.090 Uiso 1 1 calc R U . . .
O55 O 0.6210(7) 0.5459(4) 0.8717(3) 0.0537(17) Uani 1 1 d . . . . .
O56 O 0.6486(9) 0.5257(5) 0.9864(5) 0.083(3) Uani 1 1 d . . . . .
C17A C 0.3880(13) 0.7212(16) 0.9560(16) 0.060(2) Uani 0.3 1 d D U P B 4
H17A H 0.3078 0.7418 0.9753 0.072 Uiso 0.25 1 d R U P B 4
C17B C 0.4728(13) 0.694(2) 0.925(2) 0.060(2) Uani 0.2 1 d D U P B 4
H17B H 0.5534 0.6780 0.9007 0.072 Uiso 0.25 1 d R U P B 4
O57 O 0.3714(13) 0.6790(10) 0.9202(15) 0.059(2) Uani 0.5 1 d D U P B 4
O58 O 0.4893(13) 0.7370(8) 0.9604(8) 0.061(2) Uani 0.5 1 d D U P B 4
O5W O 0.4047(15) 0.6635(10) 0.9197(15) 0.057(2) Uani 0.5 1 d D U P B 5
C18 C 0.8800(9) 0.6009(6) 0.3577(6) 0.049(2) Uani 1 1 d . . . . .
H18 H 0.9408 0.6270 0.3153 0.059 Uiso 1 1 calc R U . . .
O59 O 0.8041(5) 0.6366(3) 0.3989(4) 0.0441(14) Uani 1 1 d . . . . .
O60 O 0.8742(5) 0.5295(4) 0.3734(3) 0.0419(13) Uani 1 1 d . . . . .
C19 C 0.8636(9) 0.5110(6) 0.5589(6) 0.054(2) Uani 1 1 d . . . . .
H19 H 0.9169 0.5031 0.5910 0.065 Uiso 1 1 calc R U . . .
O61 O 0.7941(5) 0.5703(4) 0.5498(3) 0.0424(13) Uani 1 1 d . . . . .
O62 O 0.8638(6) 0.4606(4) 0.5253(4) 0.0504(15) Uani 1 1 d . . . . .
C20A C 0.217(2) 0.9401(9) 0.6306(9) 0.083(3) Uiso 0.6 1 d D U P C -4
H20A H 0.1855 0.9887 0.6349 0.100 Uiso 0.6 1 calc R U P C -4
O63A O 0.2523(14) 0.8956(9) 0.6867(8) 0.085(3) Uiso 0.6 1 d D U P C -4
O64A O 0.2200(15) 0.9271(9) 0.5696(8) 0.085(3) Uiso 0.6 1 d D U P C -4
C20B C 0.236(3) 0.9518(14) 0.5993(13) 0.084(3) Uiso 0.4 1 d D U P D -5
H20B H 0.1911 0.9893 0.6214 0.101 Uiso 0.4 1 calc R U P D -5
O63B O 0.282(2) 0.8960(13) 0.6425(11) 0.084(3) Uiso 0.4 1 d D U P D -5
O64B O 0.245(2) 0.9628(13) 0.5295(11) 0.088(3) Uiso 0.4 1 d D U P D -5
C21A C 0.2388(12) 1.1245(12) 0.3945(7) 0.093(3) Uiso 0.7 1 d D U P E -6
H21A H 0.3164 1.1152 0.3626 0.111 Uiso 0.7 1 calc R U P E -6
O65A O 0.2343(12) 1.1155(8) 0.4637(7) 0.091(3) Uiso 0.7 1 d D U P E -6
O66A O 0.1500(13) 1.1445(9) 0.3641(8) 0.096(3) Uiso 0.7 1 d D U P E -6
C21B C 0.096(2) 1.164(3) 0.390(2) 0.094(3) Uiso 0.3 1 d D U P F -7
H21B H 0.0103 1.1715 0.4093 0.113 Uiso 0.3 1 calc R U P F -7
O65B O 0.163(3) 1.1667(19) 0.4313(16) 0.091(3) Uiso 0.3 1 d D U P F -7
O66B O 0.132(3) 1.151(2) 0.3262(17) 0.099(3) Uiso 0.3 1 d D U P F -7
C22 C 0.738(2) 0.674(2) 0.8994(16) 0.149(7) Uiso 0.5 1 d D U P . .
H22 H 0.6644 0.6535 0.9341 0.179 Uiso 0.5 1 calc R U P . .
O67 O 0.834(3) 0.6579(16) 0.9228(15) 0.148(8) Uiso 0.5 1 d D U P . .
O68 O 0.730(2) 0.7150(17) 0.8339(16) 0.153(8) Uiso 0.5 1 d D U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O4 2.119(5) . ?
Zr1 O2 2.129(6) . ?
Zr1 O18 2.191(6) . ?
Zr1 O17 2.193(6) . ?
Zr1 O20 2.209(6) 2_666 ?
Zr1 O19 2.236(7) . ?
Zr1 O3 2.249(5) . ?
Zr1 O1 2.274(5) . ?
Zr2 O4 2.062(5) . ?
Zr2 O5 2.086(6) . ?
Zr2 O22 2.142(5) . ?
Zr2 O21 2.201(6) . ?
Zr2 O25 2.211(6) . ?
Zr2 O8 2.254(6) . ?
Zr2 O27 2.300(6) . ?
Zr2 O1 2.341(5) . ?
Zr3 O5 2.048(6) . ?
Zr3 O2 2.097(6) . ?
Zr3 O54 2.196(6) 2_666 ?
Zr3 O37 2.21(4) . ?
Zr3 O3W 2.22(3) . ?
Zr3 O33 2.255(7) . ?
Zr3 O1 2.255(6) . ?
Zr3 O6 2.263(6) . ?
Zr3 O26 2.283(6) . ?
Zr4 O7 2.058(6) . ?
Zr4 O2 2.093(6) . ?
Zr4 O1W 2.13(3) . ?
Zr4 O52 2.180(6) 2_666 ?
Zr4 O6 2.240(6) . ?
Zr4 O3 2.248(6) . ?
Zr4 O35 2.248(15) . ?
Zr4 O34 2.249(7) . ?
Zr4 O31 2.273(6) . ?
Zr5 O7 2.044(6) . ?
Zr5 O5 2.070(6) . ?
Zr5 O2W 2.11(2) . ?
Zr5 O4W 2.172(14) . ?
Zr5 O28 2.232(6) . ?
Zr5 O29 2.239(6) . ?
Zr5 O6 2.258(6) . ?
Zr5 O8 2.303(6) . ?
Zr5 O36 2.315(11) . ?
Zr5 O38 2.392(19) . ?
Zr6 O4 2.076(5) . ?
Zr6 O7 2.081(6) . ?
Zr6 O24 2.161(6) . ?
Zr6 O23 2.188(6) . ?
Zr6 O8 2.259(5) . ?
Zr6 O32 2.263(6) . ?
Zr6 O30 2.282(6) . ?
Zr6 O3 2.346(6) . ?
Zr7 O12 2.116(5) . ?
Zr7 O10 2.129(5) . ?
Zr7 O17 2.210(6) . ?
Zr7 O18 2.213(6) . ?
Zr7 O19 2.231(6) 2_666 ?
Zr7 O11 2.249(5) . ?
Zr7 O20 2.250(7) . ?
Zr7 O9 2.268(5) . ?
Zr8 O12 2.072(5) . ?
Zr8 O13 2.085(6) . ?
Zr8 O22 2.157(6) . ?
Zr8 O21 2.181(6) . ?
Zr8 O39 2.228(5) . ?
Zr8 O16 2.270(5) . ?
Zr8 O41 2.302(6) . ?
Zr8 O9 2.350(6) . ?
Zr9 O13 2.028(6) . ?
Zr9 O10 2.094(5) . ?
Zr9 O49 2.213(6) . ?
Zr9 O47 2.216(6) . ?
Zr9 O51 2.223(6) . ?
Zr9 O40 2.238(5) . ?
Zr9 O9 2.258(5) . ?
Zr9 O14 2.314(5) . ?
Zr10 O15 2.073(6) . ?
Zr10 O10 2.087(5) . ?
Zr10 O55 2.181(6) . ?
Zr10 O53 2.211(6) . ?
Zr10 O14 2.236(5) . ?
Zr10 O46 2.261(6) . ?
Zr10 O11 2.267(5) . ?
Zr10 O48 2.287(6) . ?
Zr11 O13 2.046(5) . ?
Zr11 O15 2.075(6) . ?
Zr11 O57 2.098(17) . ?
Zr11 O42 2.201(6) . ?
Zr11 O5W 2.241(19) . ?
Zr11 O14 2.256(6) . ?
Zr11 O44 2.271(6) . ?
Zr11 O16 2.280(6) . ?
Zr11 O50 2.292(6) . ?
Zr12 O12 2.065(5) . ?
Zr12 O15 2.082(6) . ?
Zr12 O24 2.147(6) . ?
Zr12 O23 2.198(6) . ?
Zr12 O16 2.242(5) . ?
Zr12 O45 2.254(6) . ?
Zr12 O43 2.292(6) . ?
Zr12 O11 2.312(5) . ?
Zr13 O17 2.041(6) . ?
Zr13 O18 2.042(6) 2_666 ?
Zr13 O20 2.176(6) . ?
Zr13 O19 2.197(7) . ?
Zr13 O59 2.321(6) . ?
Zr13 O61 2.326(5) . ?
Zr13 O62 2.335(6) . ?
Zr13 O60 2.355(5) . ?
C1 O26 1.245(12) . ?
C1 O25 1.272(11) . ?
C1 H1 0.9500 . ?
C2 O28 1.255(12) . ?
C2 O27 1.266(12) . ?
C2 H2 0.9500 . ?
C3 O30 1.241(11) . ?
C3 O29 1.263(12) . ?
C3 H3 0.9500 . ?
C4 O32 1.215(11) . ?
C4 O31 1.274(12) . ?
C4 H4 0.9500 . ?
C5 O33 1.272(15) . ?
C5 O34 1.278(14) . ?
C5 H5 0.9500 . ?
C6 O36 1.264(5) . ?
C6 O35 1.265(5) . ?
C6 H6 0.9500 . ?
C7 O38 1.265(5) . ?
C7 O37 1.265(5) . ?
C7 H7 0.9500 . ?
C8 O39 1.254(11) . ?
C8 O40 1.267(11) . ?
C8 H8 0.9500 . ?
C9 O41 1.230(12) . ?
C9 O42 1.281(13) . ?
C9 H9 0.9500 . ?
C10 O43 1.251(11) . ?
C10 O44 1.254(11) . ?
C10 H10 0.9500 . ?
C11 O45 1.259(12) . ?
C11 O46 1.266(11) . ?
C11 H11 0.9500 . ?
C12 O47 1.255(12) . ?
C12 O48 1.265(11) . ?
C12 H12 0.9500 . ?
C13 O49 1.256(12) . ?
C13 O50 1.267(12) . ?
C13 H13 0.9500 . ?
C14A O52 1.261(5) . ?
C14A O51 1.262(5) . ?
C14A H14A 0.9600 . ?
C14B O52 1.262(5) . ?
C14B O51 1.266(5) . ?
C14B H14B 0.9600 . ?
C15A O53 1.262(5) . ?
C15A O54 1.266(5) . ?
C15A H15A 0.9600 . ?
C15B O54 1.262(5) . ?
C15B O53 1.264(5) . ?
C15B H15B 0.9599 . ?
C16 O56 1.243(14) . ?
C16 O55 1.268(14) . ?
C16 H16 0.9500 . ?
C17A O57 1.263(5) . ?
C17A O58 1.264(5) . ?
C17A H17A 0.9600 . ?
C17B O58 1.265(5) . ?
C17B O57 1.265(5) . ?
C17B H17B 0.9600 . ?
C18 O59 1.266(11) . ?
C18 O60 1.283(11) . ?
C18 H18 0.9500 . ?
C19 O61 1.265(12) . ?
C19 O62 1.303(11) . ?
C19 H19 0.9500 . ?
C20A O64A 1.262(5) . ?
C20A O63A 1.263(5) . ?
C20A H20A 0.9500 . ?
C20B O63B 1.263(5) . ?
C20B O64B 1.265(5) . ?
C20B H20B 0.9500 . ?
C21A O66A 1.265(5) . ?
C21A O65A 1.272(5) . ?
C21A H21A 0.9500 . ?
C21B O66B 1.265(5) . ?
C21B O65B 1.266(5) . ?
C21B H21B 0.9500 . ?
C22 O67 1.267(5) . ?
C22 O68 1.267(5) . ?
C22 H22 0.9500 . ?

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
O4 Zr1 O2 91.5(2) . . ?
O4 Zr1 O18 84.8(2) . . ?
O2 Zr1 O18 144.3(2) . . ?
O4 Zr1 O17 84.9(2) . . ?
O2 Zr1 O17 145.7(2) . . ?
O18 Zr1 O17 69.4(2) . . ?
O4 Zr1 O20 145.9(2) . 2_666 ?
O2 Zr1 O20 95.2(2) . 2_666 ?
O18 Zr1 O20 70.5(2) . 2_666 ?
O17 Zr1 O20 106.8(3) . 2_666 ?
O4 Zr1 O19 144.7(2) . . ?
O2 Zr1 O19 94.9(3) . . ?
O18 Zr1 O19 108.5(3) . . ?
O17 Zr1 O19 70.6(2) . . ?
O20 Zr1 O19 68.0(2) 2_666 . ?
O4 Zr1 O3 70.6(2) . . ?
O2 Zr1 O3 69.4(2) . . ?
O18 Zr1 O3 140.1(2) . . ?
O17 Zr1 O3 77.3(2) . . ?
O20 Zr1 O3 142.6(2) 2_666 . ?
O19 Zr1 O3 79.3(2) . . ?
O4 Zr1 O1 69.92(19) . . ?
O2 Zr1 O1 69.2(2) . . ?
O18 Zr1 O1 76.2(2) . . ?
O17 Zr1 O1 138.9(2) . . ?
O20 Zr1 O1 81.3(2) 2_666 . ?
O19 Zr1 O1 144.2(2) . . ?
O3 Zr1 O1 120.6(2) . . ?
O4 Zr2 O5 92.0(2) . . ?
O4 Zr2 O22 95.3(2) . . ?
O5 Zr2 O22 145.9(2) . . ?
O4 Zr2 O21 88.2(2) . . ?
O5 Zr2 O21 146.7(2) . . ?
O22 Zr2 O21 66.9(2) . . ?
O4 Zr2 O25 143.5(2) . . ?
O5 Zr2 O25 84.1(2) . . ?
O22 Zr2 O25 108.1(2) . . ?
O21 Zr2 O25 76.4(2) . . ?
O4 Zr2 O8 70.4(2) . . ?
O5 Zr2 O8 72.2(2) . . ?
O22 Zr2 O8 79.1(2) . . ?
O21 Zr2 O8 137.8(2) . . ?
O25 Zr2 O8 140.3(2) . . ?
O4 Zr2 O27 143.9(2) . . ?
O5 Zr2 O27 78.4(2) . . ?
O22 Zr2 O27 76.2(2) . . ?
O21 Zr2 O27 118.6(2) . . ?
O25 Zr2 O27 70.8(2) . . ?
O8 Zr2 O27 73.5(2) . . ?
O4 Zr2 O1 69.49(19) . . ?
O5 Zr2 O1 71.3(2) . . ?
O22 Zr2 O1 142.1(2) . . ?
O21 Zr2 O1 77.8(2) . . ?
O25 Zr2 O1 74.9(2) . . ?
O8 Zr2 O1 123.5(2) . . ?
O27 Zr2 O1 135.9(2) . . ?
O5 Zr3 O2 97.0(2) . . ?
O5 Zr3 O54 145.1(2) . 2_666 ?
O2 Zr3 O54 90.5(2) . 2_666 ?
O5 Zr3 O37 84.6(8) . . ?
O2 Zr3 O37 147.4(14) . . ?
O54 Zr3 O37 106.7(6) 2_666 . ?
O5 Zr3 O3W 93.8(5) . . ?
O2 Zr3 O3W 144.9(8) . . ?
O54 Zr3 O3W 99.4(6) 2_666 . ?
O5 Zr3 O33 142.2(3) . . ?
O2 Zr3 O33 81.9(3) . . ?
O54 Zr3 O33 72.5(3) 2_666 . ?
O37 Zr3 O33 77.5(12) . . ?
O3W Zr3 O33 69.5(7) . . ?
O5 Zr3 O1 73.7(2) . . ?
O2 Zr3 O1 70.1(2) . . ?
O54 Zr3 O1 77.0(2) 2_666 . ?
O37 Zr3 O1 139.9(14) . . ?
O3W Zr3 O1 144.9(8) . . ?
O33 Zr3 O1 138.0(2) . . ?
O5 Zr3 O6 70.8(2) . . ?
O2 Zr3 O6 73.5(2) . . ?
O54 Zr3 O6 143.5(2) 2_666 . ?
O37 Zr3 O6 76.5(11) . . ?
O3W Zr3 O6 78.9(8) . . ?
O33 Zr3 O6 72.8(3) . . ?
O1 Zr3 O6 124.5(2) . . ?
O5 Zr3 O26 80.3(2) . . ?
O2 Zr3 O26 142.7(2) . . ?
O54 Zr3 O26 73.4(2) 2_666 . ?
O37 Zr3 O26 69.7(14) . . ?
O3W Zr3 O26 72.0(8) . . ?
O33 Zr3 O26 122.4(3) . . ?
O1 Zr3 O26 73.5(2) . . ?
O6 Zr3 O26 137.1(2) . . ?
O7 Zr4 O2 96.6(2) . . ?
O7 Zr4 O1W 100.1(7) . . ?
O2 Zr4 O1W 143.5(9) . . ?
O7 Zr4 O52 143.7(2) . 2_666 ?
O2 Zr4 O52 90.8(2) . 2_666 ?
O1W Zr4 O52 94.6(7) . 2_666 ?
O7 Zr4 O6 70.9(2) . . ?
O2 Zr4 O6 74.0(2) . . ?
O1W Zr4 O6 81.1(8) . . ?
O52 Zr4 O6 144.7(2) 2_666 . ?
O7 Zr4 O3 72.8(2) . . ?
O2 Zr4 O3 70.0(2) . . ?
O1W Zr4 O3 146.2(9) . . ?
O52 Zr4 O3 76.6(2) 2_666 . ?
O6 Zr4 O3 124.4(2) . . ?
O7 Zr4 O35 84.8(4) . . ?
O2 Zr4 O35 146.2(6) . . ?
O52 Zr4 O35 108.0(3) 2_666 . ?
O6 Zr4 O35 74.6(5) . . ?
O3 Zr4 O35 140.7(6) . . ?
O7 Zr4 O34 142.8(3) . . ?
O2 Zr4 O34 82.4(3) . . ?
O1W Zr4 O34 64.8(8) . . ?
O52 Zr4 O34 73.4(3) 2_666 . ?
O6 Zr4 O34 73.1(3) . . ?
O3 Zr4 O34 138.6(3) . . ?
O35 Zr4 O34 76.7(5) . . ?
O7 Zr4 O31 81.4(2) . . ?
O2 Zr4 O31 142.5(2) . . ?
O1W Zr4 O31 72.5(9) . . ?
O52 Zr4 O31 71.6(2) 2_666 . ?
O6 Zr4 O31 137.4(2) . . ?
O3 Zr4 O31 73.7(2) . . ?
O35 Zr4 O31 71.2(6) . . ?
O34 Zr4 O31 121.2(3) . . ?
O7 Zr5 O5 93.3(2) . . ?
O7 Zr5 O2W 97.2(7) . . ?
O5 Zr5 O2W 140.9(7) . . ?
O7 Zr5 O4W 143.2(4) . . ?
O5 Zr5 O4W 96.3(5) . . ?
O2W Zr5 O4W 55.0(8) . . ?
O7 Zr5 O28 143.6(2) . . ?
O5 Zr5 O28 85.0(2) . . ?
O2W Zr5 O28 106.9(7) . . ?
O4W Zr5 O28 72.8(4) . . ?
O7 Zr5 O29 84.7(2) . . ?
O5 Zr5 O29 143.5(2) . . ?
O2W Zr5 O29 75.1(7) . . ?
O4W Zr5 O29 107.0(5) . . ?
O28 Zr5 O29 75.9(2) . . ?
O7 Zr5 O6 70.8(2) . . ?
O5 Zr5 O6 70.5(2) . . ?
O2W Zr5 O6 77.8(7) . . ?
O4W Zr5 O6 79.2(4) . . ?
O28 Zr5 O6 140.3(2) . . ?
O29 Zr5 O6 140.5(2) . . ?
O7 Zr5 O8 71.7(2) . . ?
O5 Zr5 O8 71.4(2) . . ?
O2W Zr5 O8 147.4(7) . . ?
O4W Zr5 O8 144.8(4) . . ?
O28 Zr5 O8 73.3(2) . . ?
O29 Zr5 O8 73.4(2) . . ?
O6 Zr5 O8 123.7(2) . . ?
O7 Zr5 O36 78.3(4) . . ?
O5 Zr5 O36 143.9(3) . . ?
O28 Zr5 O36 122.2(3) . . ?
O29 Zr5 O36 71.3(4) . . ?
O6 Zr5 O36 73.6(3) . . ?
O8 Zr5 O36 135.2(4) . . ?
O7 Zr5 O38 144.1(6) . . ?
O5 Zr5 O38 75.5(5) . . ?
O28 Zr5 O38 70.5(6) . . ?
O29 Zr5 O38 124.3(5) . . ?
O6 Zr5 O38 73.3(6) . . ?
O8 Zr5 O38 132.3(6) . . ?
O4 Zr6 O7 91.3(2) . . ?
O4 Zr6 O24 93.2(2) . . ?
O7 Zr6 O24 146.2(2) . . ?
O4 Zr6 O23 89.0(2) . . ?
O7 Zr6 O23 146.7(2) . . ?
O24 Zr6 O23 66.9(2) . . ?
O4 Zr6 O8 70.0(2) . . ?
O7 Zr6 O8 72.0(2) . . ?
O24 Zr6 O8 78.2(2) . . ?
O23 Zr6 O8 138.1(2) . . ?
O4 Zr6 O32 142.3(2) . . ?
O7 Zr6 O32 82.6(2) . . ?
O24 Zr6 O32 112.3(2) . . ?
O23 Zr6 O32 77.0(2) . . ?
O8 Zr6 O32 140.1(2) . . ?
O4 Zr6 O30 143.5(2) . . ?
O7 Zr6 O30 80.7(2) . . ?
O24 Zr6 O30 75.8(2) . . ?
O23 Zr6 O30 116.7(2) . . ?
O8 Zr6 O30 73.7(2) . . ?
O32 Zr6 O30 72.3(2) . . ?
O4 Zr6 O3 69.38(19) . . ?
O7 Zr6 O3 70.3(2) . . ?
O24 Zr6 O3 141.9(2) . . ?
O23 Zr6 O3 78.7(2) . . ?
O8 Zr6 O3 122.7(2) . . ?
O32 Zr6 O3 73.6(2) . . ?
O30 Zr6 O3 137.4(2) . . ?
O12 Zr7 O10 91.5(2) . . ?
O12 Zr7 O17 85.1(2) . . ?
O10 Zr7 O17 145.2(2) . . ?
O12 Zr7 O18 85.0(2) . . ?
O10 Zr7 O18 145.6(2) . . ?
O17 Zr7 O18 68.7(2) . . ?
O12 Zr7 O19 146.3(2) . 2_666 ?
O10 Zr7 O19 94.6(2) . 2_666 ?
O17 Zr7 O19 107.3(3) . 2_666 ?
O18 Zr7 O19 71.5(2) . 2_666 ?
O12 Zr7 O11 70.34(19) . . ?
O10 Zr7 O11 69.41(19) . . ?
O17 Zr7 O11 76.9(2) . . ?
O18 Zr7 O11 139.1(2) . . ?
O19 Zr7 O11 142.3(2) 2_666 . ?
O12 Zr7 O20 144.9(2) . . ?
O10 Zr7 O20 95.2(2) . . ?
O17 Zr7 O20 70.0(2) . . ?
O18 Zr7 O20 107.2(3) . . ?
O19 Zr7 O20 67.4(2) 2_666 . ?
O11 Zr7 O20 79.9(2) . . ?
O12 Zr7 O9 70.11(19) . . ?
O10 Zr7 O9 69.3(2) . . ?
O17 Zr7 O9 139.4(2) . . ?
O18 Zr7 O9 77.3(2) . . ?
O19 Zr7 O9 81.2(2) 2_666 . ?
O11 Zr7 O9 120.65(19) . . ?
O20 Zr7 O9 144.0(2) . . ?
O12 Zr8 O13 90.5(2) . . ?
O12 Zr8 O22 94.5(2) . . ?
O13 Zr8 O22 147.1(2) . . ?
O12 Zr8 O21 87.5(2) . . ?
O13 Zr8 O21 145.8(2) . . ?
O22 Zr8 O21 67.0(2) . . ?
O12 Zr8 O39 142.0(2) . . ?
O13 Zr8 O39 82.6(2) . . ?
O22 Zr8 O39 111.3(2) . . ?
O21 Zr8 O39 78.3(2) . . ?
O12 Zr8 O16 69.99(19) . . ?
O13 Zr8 O16 71.2(2) . . ?
O22 Zr8 O16 80.1(2) . . ?
O21 Zr8 O16 138.5(2) . . ?
O39 Zr8 O16 139.6(2) . . ?
O12 Zr8 O41 143.4(2) . . ?
O13 Zr8 O41 80.6(2) . . ?
O22 Zr8 O41 76.2(2) . . ?
O21 Zr8 O41 119.2(2) . . ?
O39 Zr8 O41 72.2(2) . . ?
O16 Zr8 O41 73.6(2) . . ?
O12 Zr8 O9 69.19(19) . . ?
O13 Zr8 O9 70.3(2) . . ?
O22 Zr8 O9 141.3(2) . . ?
O21 Zr8 O9 77.1(2) . . ?
O39 Zr8 O9 73.4(2) . . ?
O16 Zr8 O9 122.36(19) . . ?
O41 Zr8 O9 137.1(2) . . ?
O13 Zr9 O10 95.8(2) . . ?
O13 Zr9 O49 84.7(2) . . ?
O10 Zr9 O49 145.1(2) . . ?
O13 Zr9 O47 142.4(2) . . ?
O10 Zr9 O47 84.3(2) . . ?
O49 Zr9 O47 74.9(3) . . ?
O13 Zr9 O51 144.9(2) . . ?
O10 Zr9 O51 88.6(2) . . ?
O49 Zr9 O51 110.8(2) . . ?
O47 Zr9 O51 72.7(2) . . ?
O13 Zr9 O40 83.3(2) . . ?
O10 Zr9 O40 142.7(2) . . ?
O49 Zr9 O40 72.1(2) . . ?
O47 Zr9 O40 118.5(2) . . ?
O51 Zr9 O40 72.8(2) . . ?
O13 Zr9 O9 73.2(2) . . ?
O10 Zr9 O9 70.13(19) . . ?
O49 Zr9 O9 141.3(2) . . ?
O47 Zr9 O9 139.4(2) . . ?
O51 Zr9 O9 75.7(2) . . ?
O40 Zr9 O9 74.0(2) . . ?
O13 Zr9 O14 70.7(2) . . ?
O10 Zr9 O14 73.54(19) . . ?
O49 Zr9 O14 73.7(2) . . ?
O47 Zr9 O14 73.3(2) . . ?
O51 Zr9 O14 142.8(2) . . ?
O40 Zr9 O14 138.5(2) . . ?
O9 Zr9 O14 124.83(19) . . ?
O15 Zr10 O10 96.8(2) . . ?
O15 Zr10 O55 94.5(2) . . ?
O10 Zr10 O55 148.1(2) . . ?
O15 Zr10 O53 143.9(2) . . ?
O10 Zr10 O53 90.1(2) . . ?
O55 Zr10 O53 98.0(3) . . ?
O15 Zr10 O14 70.1(2) . . ?
O10 Zr10 O14 75.3(2) . . ?
O55 Zr10 O14 80.8(2) . . ?
O53 Zr10 O14 145.3(2) . . ?
O15 Zr10 O46 81.3(2) . . ?
O10 Zr10 O46 140.7(2) . . ?
O55 Zr10 O46 70.5(2) . . ?
O53 Zr10 O46 71.4(2) . . ?
O14 Zr10 O46 137.5(2) . . ?
O15 Zr10 O11 72.7(2) . . ?
O10 Zr10 O11 69.78(19) . . ?
O55 Zr10 O11 142.1(2) . . ?
O53 Zr10 O11 76.8(2) . . ?
O14 Zr10 O11 124.5(2) . . ?
O46 Zr10 O11 72.3(2) . . ?
O15 Zr10 O48 143.3(2) . . ?
O10 Zr10 O48 78.9(2) . . ?
O55 Zr10 O48 74.3(2) . . ?
O53 Zr10 O48 72.8(2) . . ?
O14 Zr10 O48 73.5(2) . . ?
O46 Zr10 O48 124.6(2) . . ?
O11 Zr10 O48 135.8(2) . . ?
O13 Zr11 O15 92.7(2) . . ?
O13 Zr11 O57 147.2(7) . . ?
O15 Zr11 O57 100.1(5) . . ?
O13 Zr11 O42 86.4(2) . . ?
O15 Zr11 O42 144.1(2) . . ?
O57 Zr11 O42 99.7(4) . . ?
O13 Zr11 O5W 144.0(6) . . ?
O15 Zr11 O5W 90.5(5) . . ?
O42 Zr11 O5W 110.9(4) . . ?
O13 Zr11 O14 71.7(2) . . ?
O15 Zr11 O14 69.7(2) . . ?
O57 Zr11 O14 84.6(4) . . ?
O42 Zr11 O14 141.8(2) . . ?
O5W Zr11 O14 75.9(4) . . ?
O13 Zr11 O44 143.0(2) . . ?
O15 Zr11 O44 82.9(2) . . ?
O57 Zr11 O44 69.1(6) . . ?
O42 Zr11 O44 76.7(3) . . ?
O5W Zr11 O44 73.0(6) . . ?
O14 Zr11 O44 138.0(2) . . ?
O13 Zr11 O16 71.6(2) . . ?
O15 Zr11 O16 71.6(2) . . ?
O57 Zr11 O16 141.1(6) . . ?
O42 Zr11 O16 74.1(2) . . ?
O5W Zr11 O16 142.3(7) . . ?
O14 Zr11 O16 124.2(2) . . ?
O44 Zr11 O16 72.1(2) . . ?
O13 Zr11 O50 80.1(2) . . ?
O15 Zr11 O50 142.8(2) . . ?
O57 Zr11 O50 71.4(7) . . ?
O42 Zr11 O50 72.3(3) . . ?
O5W Zr11 O50 76.0(7) . . ?
O14 Zr11 O50 73.4(2) . . ?
O44 Zr11 O50 123.8(2) . . ?
O16 Zr11 O50 136.9(2) . . ?
O12 Zr12 O15 93.4(2) . . ?
O12 Zr12 O24 93.1(2) . . ?
O15 Zr12 O24 145.8(2) . . ?
O12 Zr12 O23 89.1(2) . . ?
O15 Zr12 O23 146.6(2) . . ?
O24 Zr12 O23 67.0(2) . . ?
O12 Zr12 O16 70.7(2) . . ?
O15 Zr12 O16 72.3(2) . . ?
O24 Zr12 O16 78.3(2) . . ?
O23 Zr12 O16 138.8(2) . . ?
O12 Zr12 O45 142.1(2) . . ?
O15 Zr12 O45 82.9(2) . . ?
O24 Zr12 O45 111.0(2) . . ?
O23 Zr12 O45 75.1(2) . . ?
O16 Zr12 O45 140.9(2) . . ?
O12 Zr12 O43 145.0(2) . . ?
O15 Zr12 O43 80.0(2) . . ?
O24 Zr12 O43 75.6(2) . . ?
O23 Zr12 O43 115.2(2) . . ?
O16 Zr12 O43 74.6(2) . . ?
O45 Zr12 O43 71.6(2) . . ?
O12 Zr12 O11 69.92(19) . . ?
O15 Zr12 O11 71.6(2) . . ?
O24 Zr12 O11 141.6(2) . . ?
O23 Zr12 O11 78.2(2) . . ?
O16 Zr12 O11 123.6(2) . . ?
O45 Zr12 O11 73.2(2) . . ?
O43 Zr12 O11 136.8(2) . . ?
O17 Zr13 O18 115.6(3) . 2_666 ?
O17 Zr13 O20 74.6(2) . . ?
O18 Zr13 O20 73.9(2) 2_666 . ?
O17 Zr13 O19 74.2(2) . . ?
O18 Zr13 O19 75.5(2) 2_666 . ?
O20 Zr13 O19 120.0(3) . . ?
O17 Zr13 O59 87.6(2) . . ?
O18 Zr13 O59 137.8(2) 2_666 . ?
O20 Zr13 O59 148.3(2) . . ?
O19 Zr13 O59 78.2(2) . . ?
O17 Zr13 O61 85.4(2) . . ?
O18 Zr13 O61 139.9(2) 2_666 . ?
O20 Zr13 O61 80.2(2) . . ?
O19 Zr13 O61 144.6(2) . . ?
O59 Zr13 O61 72.3(2) . . ?
O17 Zr13 O62 137.5(2) . . ?
O18 Zr13 O62 87.5(2) 2_666 . ?
O20 Zr13 O62 79.0(3) . . ?
O19 Zr13 O62 148.2(2) . . ?
O59 Zr13 O62 98.5(2) . . ?
O61 Zr13 O62 57.5(2) . . ?
O17 Zr13 O60 139.3(2) . . ?
O18 Zr13 O60 87.0(2) 2_666 . ?
O20 Zr13 O60 146.0(2) . . ?
O19 Zr13 O60 80.2(2) . . ?
O59 Zr13 O60 56.2(2) . . ?
O61 Zr13 O60 98.5(2) . . ?
O62 Zr13 O60 72.2(2) . . ?
Zr3 O1 Zr1 104.6(2) . . ?
Zr3 O1 Zr2 99.2(2) . . ?
Zr1 O1 Zr2 102.0(2) . . ?
Zr4 O2 Zr3 111.7(3) . . ?
Zr4 O2 Zr1 115.5(3) . . ?
Zr3 O2 Zr1 116.0(3) . . ?
Zr4 O3 Zr1 105.1(2) . . ?
Zr4 O3 Zr6 100.1(2) . . ?
Zr1 O3 Zr6 102.3(2) . . ?
Zr2 O4 Zr6 116.8(2) . . ?
Zr2 O4 Zr1 118.1(2) . . ?
Zr6 O4 Zr1 117.1(2) . . ?
Zr3 O5 Zr5 116.9(3) . . ?
Zr3 O5 Zr2 115.7(3) . . ?
Zr5 O5 Zr2 115.4(3) . . ?
Zr4 O6 Zr5 101.7(3) . . ?
Zr4 O6 Zr3 100.7(2) . . ?
Zr5 O6 Zr3 101.8(3) . . ?
Zr5 O7 Zr4 116.5(3) . . ?
Zr5 O7 Zr6 116.0(3) . . ?
Zr4 O7 Zr6 116.6(3) . . ?
Zr2 O8 Zr6 102.7(2) . . ?
Zr2 O8 Zr5 100.9(2) . . ?
Zr6 O8 Zr5 100.1(2) . . ?
Zr9 O9 Zr7 104.6(2) . . ?
Zr9 O9 Zr8 99.1(2) . . ?
Zr7 O9 Zr8 102.1(2) . . ?
Zr10 O10 Zr9 111.9(2) . . ?
Zr10 O10 Zr7 116.0(2) . . ?
Zr9 O10 Zr7 115.9(2) . . ?
Zr7 O11 Zr10 104.8(2) . . ?
Zr7 O11 Zr12 102.6(2) . . ?
Zr10 O11 Zr12 100.2(2) . . ?
Zr12 O12 Zr8 116.7(2) . . ?
Zr12 O12 Zr7 116.7(2) . . ?
Zr8 O12 Zr7 118.1(2) . . ?
Zr9 O13 Zr11 117.9(3) . . ?
Zr9 O13 Zr8 117.0(3) . . ?
Zr11 O13 Zr8 116.1(3) . . ?
Zr10 O14 Zr11 103.5(2) . . ?
Zr10 O14 Zr9 99.2(2) . . ?
Zr11 O14 Zr9 99.6(2) . . ?
Zr10 O15 Zr11 116.6(3) . . ?
Zr10 O15 Zr12 115.5(3) . . ?
Zr11 O15 Zr12 114.7(3) . . ?
Zr12 O16 Zr8 102.6(2) . . ?
Zr12 O16 Zr11 101.4(2) . . ?
Zr8 O16 Zr11 100.7(2) . . ?
Zr13 O17 Zr1 111.1(3) . . ?
Zr13 O17 Zr7 110.8(3) . . ?
Zr1 O17 Zr7 110.6(2) . . ?
Zr13 O18 Zr1 110.5(3) 2_666 . ?
Zr13 O18 Zr7 109.5(3) 2_666 . ?
Zr1 O18 Zr7 110.5(2) . . ?
Zr13 O19 Zr7 103.4(3) . 2_666 ?
Zr13 O19 Zr1 104.0(3) . . ?
Zr7 O19 Zr1 112.0(3) 2_666 . ?
Zr13 O20 Zr1 105.0(3) . 2_666 ?
Zr13 O20 Zr7 104.5(3) . . ?
Zr1 O20 Zr7 112.3(3) 2_666 . ?
Zr8 O21 Zr2 108.3(2) . . ?
Zr2 O22 Zr8 111.4(2) . . ?
Zr6 O23 Zr12 108.5(2) . . ?
Zr12 O24 Zr6 111.4(2) . . ?
O26 C1 O25 128.9(9) . . ?
O26 C1 H1 115.5 . . ?
O25 C1 H1 115.5 . . ?
C1 O25 Zr2 129.9(6) . . ?
C1 O26 Zr3 132.7(6) . . ?
O28 C2 O27 127.6(9) . . ?
O28 C2 H2 116.2 . . ?
O27 C2 H2 116.2 . . ?
C2 O27 Zr2 133.7(6) . . ?
C2 O28 Zr5 129.8(6) . . ?
O30 C3 O29 127.8(9) . . ?
O30 C3 H3 116.1 . . ?
O29 C3 H3 116.1 . . ?
C3 O29 Zr5 130.9(6) . . ?
C3 O30 Zr6 133.2(6) . . ?
O32 C4 O31 129.6(8) . . ?
O32 C4 H4 115.2 . . ?
O31 C4 H4 115.2 . . ?
C4 O31 Zr4 131.3(6) . . ?
C4 O32 Zr6 131.5(6) . . ?
O33 C5 O34 128.8(10) . . ?
O33 C5 H5 115.6 . . ?
O34 C5 H5 115.6 . . ?
C5 O33 Zr3 130.6(7) . . ?
C5 O34 Zr4 130.0(7) . . ?
O36 C6 O35 126.9(8) . . ?
O36 C6 H6 116.5 . . ?
O35 C6 H6 116.5 . . ?
C6 O35 Zr4 129.7(8) . . ?
C6 O36 Zr5 134.0(8) . . ?
O38 C7 O37 126.7(8) . . ?
O38 C7 H7 116.6 . . ?
O37 C7 H7 116.6 . . ?
C7 O37 Zr3 129.5(18) . . ?
C7 O38 Zr5 133.6(15) . . ?
O39 C8 O40 127.6(8) . . ?
O39 C8 H8 116.2 . . ?
O40 C8 H8 116.2 . . ?
C8 O39 Zr8 133.2(6) . . ?
C8 O40 Zr9 131.7(5) . . ?
O41 C9 O42 127.3(9) . . ?
O41 C9 H9 116.3 . . ?
O42 C9 H9 116.3 . . ?
C9 O41 Zr8 133.5(6) . . ?
C9 O42 Zr11 131.0(6) . . ?
O43 C10 O44 127.5(8) . . ?
O43 C10 H10 116.2 . . ?
O44 C10 H10 116.2 . . ?
C10 O43 Zr12 131.9(5) . . ?
C10 O44 Zr11 132.0(6) . . ?
O45 C11 O46 126.6(8) . . ?
O45 C11 H11 116.7 . . ?
O46 C11 H11 116.7 . . ?
C11 O45 Zr12 131.8(6) . . ?
C11 O46 Zr10 133.9(6) . . ?
O47 C12 O48 128.2(9) . . ?
O47 C12 H12 115.9 . . ?
O48 C12 H12 115.9 . . ?
C12 O47 Zr9 130.2(6) . . ?
C12 O48 Zr10 131.8(6) . . ?
O49 C13 O50 126.4(9) . . ?
O49 C13 H13 116.8 . . ?
O50 C13 H13 116.8 . . ?
C13 O49 Zr9 132.1(6) . . ?
C13 O50 Zr11 133.1(6) . . ?
O52 C14A O51 121.9(9) . . ?
O52 C14A H14A 119.1 . . ?
O51 C14A H14A 119.0 . . ?
O52 C14B O51 121.5(9) . . ?
O52 C14B H14B 119.0 . . ?
O51 C14B H14B 119.5 . . ?
C14A O51 Zr9 136.1(7) . . ?
C14B O51 Zr9 122.0(5) . . ?
C14A O52 Zr4 138.8(8) . 2_666 ?
C14B O52 Zr4 123.4(6) . 2_666 ?
O53 C15A O54 120.2(9) . . ?
O53 C15A H15A 120.2 . . ?
O54 C15A H15A 119.5 . . ?
O54 C15B O53 120.3(9) . . ?
O54 C15B H15B 119.8 . . ?
O53 C15B H15B 119.9 . . ?
C15A O53 Zr10 125.1(6) . . ?
C15B O53 Zr10 141.2(9) . . ?
C15B O54 Zr3 140.1(11) . 2_666 ?
C15A O54 Zr3 117.9(5) . 2_666 ?
O56 C16 O55 124.0(13) . . ?
O56 C16 H16 118.0 . . ?
O55 C16 H16 118.0 . . ?
C16 O55 Zr10 138.9(7) . . ?
O57 C17A O58 127.2(8) . . ?
O57 C17A H17A 104.9 . . ?
O58 C17A H17A 127.7 . . ?
O58 C17B O57 127.0(8) . . ?
O58 C17B H17B 105.3 . . ?
O57 C17B H17B 127.5 . . ?
C17A O57 Zr11 145(2) . . ?
C17B O57 Zr11 131(2) . . ?
O59 C18 O60 119.6(8) . . ?
O59 C18 H18 120.2 . . ?
O60 C18 H18 120.2 . . ?
Zr13 C18 H18 178.6 . . ?
C18 O59 Zr13 93.1(6) . . ?
C18 O60 Zr13 91.1(5) . . ?
O61 C19 O62 121.6(9) . . ?
O61 C19 H19 119.2 . . ?
O62 C19 H19 119.2 . . ?
Zr13 C19 H19 176.2 . . ?
C19 O61 Zr13 91.1(5) . . ?
C19 O62 Zr13 89.7(6) . . ?
O64A C20A O63A 127.0(8) . . ?
O64A C20A H20A 116.5 . . ?
O63A C20A H20A 116.5 . . ?
O63B C20B O64B 126.7(8) . . ?
O63B C20B H20B 116.7 . . ?
O64B C20B H20B 116.7 . . ?
O66A C21A O65A 126.3(8) . . ?
O66A C21A H21A 116.9 . . ?
O65A C21A H21A 116.9 . . ?
O66B C21B O65B 126.4(8) . . ?
O66B C21B H21B 116.8 . . ?
O65B C21B H21B 116.8 . . ?
O67 C22 O68 126.0(8) . . ?
O67 C22 H22 117.0 . . ?
O68 C22 H22 117.0 . . ?

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
O26 C1 O25 Zr2 5.0(15) . . . . ?
O25 C1 O26 Zr3 -1.6(16) . . . . ?
O28 C2 O27 Zr2 -3.0(16) . . . . ?
O27 C2 O28 Zr5 13.6(16) . . . . ?
O30 C3 O29 Zr5 -4.7(17) . . . . ?
O29 C3 O30 Zr6 -1.7(18) . . . . ?
O32 C4 O31 Zr4 2.3(18) . . . . ?
O31 C4 O32 Zr6 -4.4(18) . . . . ?
O34 C5 O33 Zr3 10(2) . . . . ?
O33 C5 O34 Zr4 -10(2) . . . . ?
O36 C6 O35 Zr4 0(4) . . . . ?
O35 C6 O36 Zr5 -9(3) . . . . ?
O38 C7 O37 Zr3 18(7) . . . . ?
O37 C7 O38 Zr5 -9(6) . . . . ?
O40 C8 O39 Zr8 -1.0(15) . . . . ?
O39 C8 O40 Zr9 0.6(15) . . . . ?
O42 C9 O41 Zr8 -8.7(18) . . . . ?
O41 C9 O42 Zr11 0.4(17) . . . . ?
O44 C10 O43 Zr12 5.8(15) . . . . ?
O43 C10 O44 Zr11 3.4(15) . . . . ?
O46 C11 O45 Zr12 -2.6(18) . . . . ?
O45 C11 O46 Zr10 3.5(18) . . . . ?
O48 C12 O47 Zr9 -3.0(16) . . . . ?
O47 C12 O48 Zr10 11.6(16) . . . . ?
O50 C13 O49 Zr9 0.4(17) . . . . ?
O49 C13 O50 Zr11 -7.1(17) . . . . ?
O52 C14A O51 C14B -46.4(12) . . . . ?
O52 C14A O51 Zr9 -135.8(11) . . . . ?
O52 C14B O51 C14A 46.1(12) . . . . ?
O52 C14B O51 Zr9 171.3(11) . . . . ?
O51 C14A O52 C14B 46.5(12) . . . . ?
O51 C14A O52 Zr4 135.7(10) . . . 2_666 ?
O51 C14B O52 C14A -46.0(12) . . . . ?
O51 C14B O52 Zr4 -174.0(11) . . . 2_666 ?
O54 C15A O53 C15B -43.5(14) . . . . ?
O54 C15A O53 Zr10 -173.6(9) . . . . ?
O54 C15B O53 C15A 43.8(14) . . . . ?
O54 C15B O53 Zr10 137.1(12) . . . . ?
O53 C15B O54 C15A -43.6(14) . . . . ?
O53 C15B O54 Zr3 -124.4(15) . . . 2_666 ?
O53 C15A O54 C15B 43.6(14) . . . . ?
O53 C15A O54 Zr3 177.8(10) . . . 2_666 ?
O56 C16 O55 Zr10 -163.0(9) . . . . ?
O58 C17A O57 Zr11 -110(3) . . . . ?
O58 C17B O57 Zr11 134(3) . . . . ?
O60 C18 O59 Zr13 -1.4(9) . . . . ?
O59 C18 O60 Zr13 1.4(9) . . . . ?
O62 C19 O61 Zr13 4.3(10) . . . . ?
O61 C19 O62 Zr13 -4.3(10) . . . . ?

_refine_diff_density_max         1.416
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.209



