# Electronic Supplementary Material (ESI) for Chemical Communications.
# 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_zr12_acetate_sq
_database_code_depnum_ccdc_archive 'CCDC 1830216'
_audit_update_record             
;
2018-05-14 deposited with the CCDC.
2018-05-23 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_zr12_acetate_sq     
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The data completeness up to 59 degrees were 99.5% and there
were only very weak reflections above this angle.    
;
_vrf_PLAT306_zr12_acetate_sq     
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: Two water molecules could be located from the electron difference 
map, however the positions of the corresponding hydrogen atoms could not be 
determined, and the hydrogen atoms are therefore omitted from the structural 
model.
;

_vrf_PLAT430_zr12_acetate_sq     
;
PROBLEM: Short Inter D...A Contact  O2W      ..O28              2.80 Ang.
RESPONSE: The two atoms are hydrogen bonded, O2W (a water molecule) being 
the donor. However, as positions of the hydrogen atoms could not be 
determined, the hydrogen atom is missing from the model (see above).
;
_vrf_PLAT973_zr12_acetate_sq     
;
PROBLEM: Check Calcd Positive Resid. Density on       Zr2       1.72 eA-3  
RESPONSE: This alert arises due to the presence of q peaks that are not 
assigned to any element. However, the artificial electron density peaks
around heavy atoms, (in this case Zr centres), are frequently observed in 
crystal structures, in particularly when CuKa radiation is used, and do not
correspond to unaccounted atoms.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Zr12_acetate_solvate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C51.20 H86.40 O71.20 Zr12'
_chemical_formula_weight         2935.84

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                   12.5793(8)
_cell_length_b                   15.7491(8)
_cell_length_c                   16.7679(13)
_cell_angle_alpha                116.322(6)
_cell_angle_beta                 93.693(6)
_cell_angle_gamma                106.969(5)
_cell_volume                     2774.1(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    118(2)
_cell_measurement_reflns_used    3387
_cell_measurement_theta_min      4.0420
_cell_measurement_theta_max      61.1090

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_F_000             1443
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    9.685
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.64549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      118(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Nova (Cu) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.4323
_diffrn_reflns_number            17266
_diffrn_reflns_av_unetI/netI     0.0865
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.018
_diffrn_reflns_theta_max         58.928
_diffrn_reflns_theta_full        58.928
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             7922
_reflns_number_gt                5320
_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_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;The unit cell contains additional disordered solvent molecules
which have been treated as a diffuse contribution to the overall
scattering without specific atom positions by SQUEEZE/PLATON.,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0967P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7922
_refine_ls_number_parameters     625
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0657
_refine_ls_wR_factor_ref         0.1855
_refine_ls_wR_factor_gt          0.1595
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.000
_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
Zr3 Zr 0.78052(7) 0.22604(7) 0.61519(7) 0.0328(3) Uani 1 1 d . . . . .
Zr4 Zr 0.70646(7) 0.42136(7) 0.61042(7) 0.0345(3) Uani 1 1 d . . . . .
Zr1 Zr 0.48936(7) 0.19121(7) 0.54130(7) 0.0317(3) Uani 1 1 d . . . . .
Zr2 Zr 0.58571(7) 0.20100(7) 0.75197(7) 0.0324(3) Uani 1 1 d . . . . .
Zr6 Zr 0.79761(7) 0.43579(7) 0.82047(7) 0.0359(3) Uani 1 1 d . . . . .
Zr5 Zr 0.51089(7) 0.39692(7) 0.74704(7) 0.0335(3) Uani 1 1 d . . . . .
O9 O 0.3328(6) 0.3387(6) 0.6709(6) 0.0382(18) Uani 1 1 d . . . . .
O3 O 0.6812(5) 0.4584(5) 0.7422(5) 0.0322(16) Uani 1 1 d . . . . .
O4 O 0.6229(5) 0.3784(5) 0.8384(5) 0.0319(16) Uani 1 1 d . . . . .
H4O H 0.6135 0.4034 0.9014 0.048 Uiso 1 1 calc R U . . .
O8 O 0.5226(5) 0.3636(5) 0.6068(5) 0.0342(17) Uani 1 1 d . . . . .
H8O H 0.4730 0.3836 0.5764 0.051 Uiso 1 1 calc R U . . .
O29 O 0.4699(6) 0.2260(5) 0.4286(5) 0.0373(18) Uani 1 1 d . . . . .
O1 O 0.5973(5) 0.1299(5) 0.6028(5) 0.0290(15) Uani 1 1 d . . . . .
H1O H 0.5780 0.0562 0.5709 0.044 Uiso 1 1 calc R U . . .
O6 O 0.7387(6) 0.2819(5) 0.7400(5) 0.0361(17) Uani 1 1 d . . . . .
O17 O 0.6364(6) -0.0474(5) 0.4810(5) 0.0375(18) Uani 1 1 d . . . . .
O14 O 0.4918(6) -0.0653(5) 0.5814(5) 0.0370(18) Uani 1 1 d . . . . .
O26 O 0.8074(7) 0.5800(6) 0.9484(6) 0.050(2) Uani 1 1 d . . . . .
O22 O 0.8306(6) 0.3998(6) 0.5223(5) 0.0405(19) Uani 1 1 d . . . . .
O18 O 0.7607(5) 0.0899(5) 0.4880(5) 0.0371(18) Uani 1 1 d . . . . .
O31 O 0.8188(6) 0.3992(6) 0.9320(5) 0.0423(18) Uani 1 1 d . . . . .
O16 O 0.8035(6) 0.1135(6) 0.6550(5) 0.0381(18) Uani 1 1 d . . . . .
O19 O 0.9546(6) 0.2878(6) 0.6941(6) 0.0393(18) Uani 1 1 d . . . . .
O27 O 0.4854(6) 0.5376(6) 0.7494(6) 0.048(2) Uani 1 1 d . . . . .
O13 O 0.4554(6) 0.0512(5) 0.7012(5) 0.0391(18) Uani 1 1 d . . . . .
O7 O 0.8396(6) 0.4055(5) 0.6875(5) 0.0396(18) Uani 1 1 d . . . . .
H7O H 0.9184 0.4417 0.6893 0.059 Uiso 1 1 calc R U . . .
O2 O 0.6633(5) 0.2686(5) 0.5629(5) 0.0349(17) Uani 1 1 d . . . . .
O20 O 0.9650(6) 0.4189(6) 0.8293(5) 0.0454(19) Uani 1 1 d . . . . .
O12 O 0.4510(6) 0.2205(5) 0.8301(5) 0.0395(18) Uani 1 1 d . . . . .
O5 O 0.4957(6) 0.2478(5) 0.6796(5) 0.0371(18) Uani 1 1 d . . . . .
O24 O 0.6714(7) 0.5583(6) 0.6188(6) 0.052(2) Uani 1 1 d . . . . .
O10 O 0.3207(6) 0.2093(5) 0.5350(5) 0.0400(18) Uani 1 1 d . . . . .
O32 O 0.6745(6) 0.2526(6) 0.8912(5) 0.0395(18) Uani 1 1 d . . . . .
O11 O 0.4000(6) 0.3439(5) 0.8273(5) 0.0374(17) Uani 1 1 d . . . . .
O28 O 0.5369(6) 0.5412(6) 0.8781(6) 0.0444(19) Uani 1 1 d . . . . .
O21 O 0.8804(6) 0.2758(5) 0.5287(5) 0.0392(18) Uani 1 1 d . . . . .
O15 O 0.6792(6) 0.0975(6) 0.7416(5) 0.0422(19) Uani 1 1 d . . . . .
O30 O 0.6143(7) 0.3716(6) 0.4687(6) 0.0417(19) Uani 1 1 d . . . . .
O25 O 0.9231(7) 0.5924(6) 0.8576(6) 0.049(2) Uani 1 1 d . . . . .
O23 O 0.8453(6) 0.5812(6) 0.6752(6) 0.052(2) Uani 1 1 d . U . . .
C21 C 0.5275(10) 0.2960(9) 0.4131(9) 0.042(3) Uani 1 1 d . . . . .
C11 C 1.0059(10) 0.3568(10) 0.7729(9) 0.044(3) Uani 1 1 d . . . . .
C1 C 0.2814(10) 0.2721(9) 0.5905(9) 0.040(3) Uani 1 1 d . . . . .
C3 C 0.3900(9) 0.2738(8) 0.8469(8) 0.035(3) Uani 1 1 d . . . . .
C5 C 0.4420(8) -0.0403(8) 0.6464(8) 0.035(3) Uani 1 1 d . . . . .
C13 C 0.8858(9) 0.3393(9) 0.5025(8) 0.040(3) Uani 1 1 d . . . . .
C23 C 0.7593(9) 0.3296(10) 0.9462(9) 0.046(3) Uani 1 1 d . . . . .
C9 C 0.7185(9) -0.0044(8) 0.4558(8) 0.039(3) Uani 1 1 d . . . . .
C6 C 0.3646(10) -0.1190(9) 0.6643(9) 0.043(3) Uani 1 1 d . . . . .
H6A H 0.3357 -0.1829 0.6090 0.064 Uiso 1 1 calc R U . . .
H6B H 0.3021 -0.0992 0.6854 0.064 Uiso 1 1 calc R U . . .
H6C H 0.4063 -0.1254 0.7101 0.064 Uiso 1 1 calc R U . . .
C17 C 0.8907(11) 0.6343(11) 0.9306(10) 0.059(3) Uani 1 1 d . U . . .
C14 C 0.9709(10) 0.3491(9) 0.4446(9) 0.047(3) Uani 1 1 d . . . . .
H14A H 1.0201 0.3132 0.4464 0.071 Uiso 1 1 calc R U . . .
H14B H 1.0157 0.4195 0.4678 0.071 Uiso 1 1 calc R U . . .
H14C H 0.9309 0.3209 0.3826 0.071 Uiso 1 1 calc R U . . .
C19 C 0.5128(10) 0.5872(10) 0.8373(10) 0.051(3) Uani 1 1 d . . . . .
C2 C 0.1593(9) 0.2597(10) 0.5579(9) 0.053(3) Uani 1 1 d . . . . .
H2A H 0.1125 0.2422 0.5952 0.079 Uiso 1 1 calc R U . . .
H2B H 0.1306 0.2068 0.4955 0.079 Uiso 1 1 calc R U . . .
H2C H 0.1579 0.3222 0.5624 0.079 Uiso 1 1 calc R U . . .
C22 C 0.4884(10) 0.2869(9) 0.3230(9) 0.048(3) Uani 1 1 d . . . . .
H22A H 0.4556 0.3373 0.3315 0.072 Uiso 1 1 calc R U . . .
H22B H 0.4323 0.2206 0.2840 0.072 Uiso 1 1 calc R U . . .
H22C H 0.5523 0.2968 0.2955 0.072 Uiso 1 1 calc R U . . .
C10 C 0.7732(9) -0.0657(9) 0.3840(9) 0.046(3) Uani 1 1 d . . . . .
H10A H 0.8047 -0.0296 0.3525 0.069 Uiso 1 1 calc R U . . .
H10B H 0.7166 -0.1303 0.3410 0.069 Uiso 1 1 calc R U . . .
H10C H 0.8329 -0.0760 0.4131 0.069 Uiso 1 1 calc R U . . .
C7 C 0.7566(9) 0.0758(9) 0.7022(8) 0.044(3) Uani 1 1 d . . . . .
C15 C 0.7741(10) 0.6188(9) 0.6596(9) 0.047(3) Uani 1 1 d . U . . .
C12 C 1.1280(10) 0.3734(11) 0.8089(9) 0.061(4) Uani 1 1 d . . . . .
H12A H 1.1349 0.3092 0.7939 0.092 Uiso 1 1 calc R U . . .
H12B H 1.1484 0.4159 0.8740 0.092 Uiso 1 1 calc R U . . .
H12C H 1.1780 0.4056 0.7815 0.092 Uiso 1 1 calc R U . . .
C4 C 0.2971(9) 0.2535(10) 0.8947(9) 0.050(3) Uani 1 1 d . . . . .
H4A H 0.2930 0.1953 0.9014 0.075 Uiso 1 1 calc R U . . .
H4B H 0.2256 0.2409 0.8595 0.075 Uiso 1 1 calc R U . . .
H4C H 0.3132 0.3114 0.9539 0.075 Uiso 1 1 calc R U . . .
C24 C 0.7935(11) 0.3379(10) 1.0360(9) 0.057(3) Uani 1 1 d . . . . .
H24A H 0.7434 0.3616 1.0741 0.085 Uiso 1 1 calc R U . . .
H24B H 0.8704 0.3849 1.0645 0.085 Uiso 1 1 calc R U . . .
H24C H 0.7889 0.2725 1.0279 0.085 Uiso 1 1 calc R U . . .
C8 C 0.7927(10) -0.0043(10) 0.7078(10) 0.056(4) Uani 1 1 d . . . . .
H8A H 0.7566 -0.0675 0.6525 0.084 Uiso 1 1 calc R U . . .
H8B H 0.7707 -0.0119 0.7587 0.084 Uiso 1 1 calc R U . . .
H8C H 0.8741 0.0152 0.7159 0.084 Uiso 1 1 calc R U . . .
C16 C 0.8075(12) 0.7283(9) 0.6871(12) 0.072(4) Uani 1 1 d . . . . .
H16A H 0.7698 0.7357 0.6403 0.108 Uiso 1 1 calc R U . . .
H16B H 0.8886 0.7572 0.6956 0.108 Uiso 1 1 calc R U . . .
H16C H 0.7858 0.7626 0.7432 0.108 Uiso 1 1 calc R U . . .
C20 C 0.5122(13) 0.6909(9) 0.8880(10) 0.064(4) Uani 1 1 d . . . . .
H20A H 0.4497 0.6965 0.8572 0.096 Uiso 1 1 calc R U . . .
H20B H 0.5827 0.7384 0.8911 0.096 Uiso 1 1 calc R U . . .
H20C H 0.5038 0.7053 0.9487 0.096 Uiso 1 1 calc R U . . .
C18 C 0.9503(15) 0.7460(12) 0.9996(13) 0.098(5) Uani 1 1 d . U . . .
H18A H 0.8975 0.7807 1.0056 0.147 Uiso 1 1 calc R U . . .
H18B H 1.0135 0.7750 0.9792 0.147 Uiso 1 1 calc R U . . .
H18C H 0.9775 0.7528 1.0578 0.147 Uiso 1 1 calc R U . . .
C25 C 1.1197(15) 0.5870(14) 0.7237(12) 0.069(5) Uani 0.8 1 d D . P . .
C26 C 1.2326(14) 0.6089(18) 0.6954(16) 0.093(6) Uani 0.8 1 d D U P . .
H26A H 1.2733 0.6808 0.7257 0.139 Uiso 0.8 1 calc R U P . .
H26B H 1.2772 0.5768 0.7121 0.139 Uiso 0.8 1 calc R U P . .
H26C H 1.2185 0.5829 0.6305 0.139 Uiso 0.8 1 calc R U P . .
O33 O 1.0584(10) 0.4986(12) 0.6907(10) 0.078(4) Uani 0.8 1 d D . P . .
O34 O 1.0915(10) 0.6560(11) 0.7750(10) 0.084(4) Uani 0.8 1 d D . P . .
H34 H 1.0284 0.6324 0.7832 0.126 Uiso 0.8 1 calc R U P . .
O1W O 0.3848(7) 0.4364(6) 0.5473(6) 0.057(2) Uani 1 1 d . . . . .
O2W O 0.6247(7) 0.4656(6) 1.0152(6) 0.055(2) Uani 1 1 d . . . . .


_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
Zr3 O6 2.051(7) . ?
Zr3 O2 2.079(6) . ?
Zr3 O19 2.176(8) . ?
Zr3 O18 2.184(7) . ?
Zr3 O21 2.227(7) . ?
Zr3 O16 2.234(6) . ?
Zr3 O1 2.295(6) . ?
Zr3 O7 2.373(7) . ?
Zr3 Zr6 3.4946(14) . ?
Zr3 Zr4 3.4955(11) . ?
Zr3 Zr2 3.5189(12) . ?
Zr3 Zr1 3.5904(12) . ?
Zr4 O2 2.050(7) . ?
Zr4 O3 2.092(7) . ?
Zr4 O7 2.188(7) . ?
Zr4 O8 2.211(6) . ?
Zr4 O22 2.213(6) . ?
Zr4 O30 2.251(8) . ?
Zr4 O24 2.272(7) . ?
Zr4 O23 2.308(8) . ?
Zr4 C15 2.677(11) . ?
Zr4 Zr1 3.4682(13) . ?
Zr4 Zr6 3.5198(14) . ?
Zr1 O5 2.070(7) . ?
Zr1 O2 2.086(6) . ?
Zr1 O17 2.204(7) 2_656 ?
Zr1 O29 2.207(7) . ?
Zr1 O14 2.223(7) 2_656 ?
Zr1 O10 2.224(6) . ?
Zr1 O1 2.304(6) . ?
Zr1 O8 2.321(7) . ?
Zr1 Zr5 3.4535(14) . ?
Zr1 Zr2 3.5817(13) . ?
Zr2 O6 2.053(7) . ?
Zr2 O5 2.098(7) . ?
Zr2 O13 2.181(7) . ?
Zr2 O32 2.193(8) . ?
Zr2 O12 2.218(6) . ?
Zr2 O15 2.228(6) . ?
Zr2 O1 2.279(6) . ?
Zr2 O4 2.384(7) . ?
Zr2 Zr6 3.4904(13) . ?
Zr2 Zr5 3.5106(11) . ?
Zr6 O6 2.041(7) . ?
Zr6 O3 2.114(7) . ?
Zr6 O7 2.199(7) . ?
Zr6 O20 2.202(7) . ?
Zr6 O31 2.210(7) . ?
Zr6 O4 2.215(6) . ?
Zr6 O25 2.281(8) . ?
Zr6 O26 2.293(8) . ?
Zr6 C17 2.649(15) . ?
Zr6 Zr5 3.5171(12) . ?
Zr5 O5 2.046(7) . ?
Zr5 O3 2.101(6) . ?
Zr5 O4 2.185(6) . ?
Zr5 O8 2.196(7) . ?
Zr5 O9 2.211(8) . ?
Zr5 O11 2.239(7) . ?
Zr5 O28 2.268(8) . ?
Zr5 O27 2.313(7) . ?
Zr5 C19 2.683(13) . ?
O9 C1 1.254(14) . ?
O4 H4O 0.9800 . ?
O8 H8O 0.9800 . ?
O29 C21 1.273(12) . ?
O1 H1O 0.9800 . ?
O17 C9 1.267(12) . ?
O17 Zr1 2.204(7) 2_656 ?
O14 C5 1.259(12) . ?
O14 Zr1 2.223(7) 2_656 ?
O26 C17 1.288(15) . ?
O22 C13 1.279(12) . ?
O18 C9 1.253(12) . ?
O31 C23 1.263(14) . ?
O16 C7 1.265(12) . ?
O19 C11 1.245(14) . ?
O27 C19 1.288(15) . ?
O13 C5 1.270(12) . ?
O7 H7O 0.9800 . ?
O20 C11 1.285(14) . ?
O12 C3 1.251(11) . ?
O24 C15 1.278(15) . ?
O10 C1 1.271(12) . ?
O32 C23 1.260(15) . ?
O11 C3 1.260(12) . ?
O28 C19 1.274(14) . ?
O21 C13 1.245(12) . ?
O15 C7 1.257(12) . ?
O30 C21 1.267(14) . ?
O25 C17 1.268(14) . ?
O23 C15 1.280(13) . ?
C21 C22 1.488(16) . ?
C11 C12 1.516(16) . ?
C1 C2 1.523(15) . ?
C3 C4 1.496(14) . ?
C5 C6 1.496(14) . ?
C13 C14 1.511(14) . ?
C23 C24 1.476(17) . ?
C9 C10 1.523(15) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C17 C18 1.52(2) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C19 C20 1.472(17) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C7 C8 1.497(15) . ?
C15 C16 1.486(16) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C25 O33 1.215(15) . ?
C25 O34 1.217(14) . ?
C25 C26 1.518(16) . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
O34 H34 0.8200 . ?

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
O6 Zr3 O2 91.3(3) . . ?
O6 Zr3 O19 85.0(3) . . ?
O2 Zr3 O19 140.9(3) . . ?
O6 Zr3 O18 145.7(3) . . ?
O2 Zr3 O18 96.2(3) . . ?
O19 Zr3 O18 108.5(3) . . ?
O6 Zr3 O21 141.7(3) . . ?
O2 Zr3 O21 81.3(2) . . ?
O19 Zr3 O21 78.1(3) . . ?
O18 Zr3 O21 72.6(3) . . ?
O6 Zr3 O16 81.1(3) . . ?
O2 Zr3 O16 145.4(3) . . ?
O19 Zr3 O16 72.3(3) . . ?
O18 Zr3 O16 73.7(3) . . ?
O21 Zr3 O16 124.4(2) . . ?
O6 Zr3 O1 70.2(3) . . ?
O2 Zr3 O1 69.3(2) . . ?
O19 Zr3 O1 142.6(2) . . ?
O18 Zr3 O1 81.2(2) . . ?
O21 Zr3 O1 138.0(3) . . ?
O16 Zr3 O1 76.4(2) . . ?
O6 Zr3 O7 69.3(3) . . ?
O2 Zr3 O7 69.8(3) . . ?
O19 Zr3 O7 72.6(2) . . ?
O18 Zr3 O7 144.4(2) . . ?
O21 Zr3 O7 72.9(2) . . ?
O16 Zr3 O7 135.4(3) . . ?
O1 Zr3 O7 120.3(2) . . ?
O6 Zr3 Zr6 31.26(19) . . ?
O2 Zr3 Zr6 83.21(19) . . ?
O19 Zr3 Zr6 73.68(19) . . ?
O18 Zr3 Zr6 176.66(16) . . ?
O21 Zr3 Zr6 110.48(19) . . ?
O16 Zr3 Zr6 104.9(2) . . ?
O1 Zr3 Zr6 95.49(17) . . ?
O7 Zr3 Zr6 38.33(17) . . ?
O6 Zr3 Zr4 81.65(18) . . ?
O2 Zr3 Zr4 31.9(2) . . ?
O19 Zr3 Zr4 109.47(18) . . ?
O18 Zr3 Zr4 120.28(18) . . ?
O21 Zr3 Zr4 72.31(16) . . ?
O16 Zr3 Zr4 162.45(18) . . ?
O1 Zr3 Zr4 94.52(15) . . ?
O7 Zr3 Zr4 38.07(17) . . ?
Zr6 Zr3 Zr4 60.47(3) . . ?
O6 Zr3 Zr2 31.0(2) . . ?
O2 Zr3 Zr2 82.98(18) . . ?
O19 Zr3 Zr2 110.19(19) . . ?
O18 Zr3 Zr2 116.99(16) . . ?
O21 Zr3 Zr2 162.43(16) . . ?
O16 Zr3 Zr2 73.22(17) . . ?
O1 Zr3 Zr2 39.53(17) . . ?
O7 Zr3 Zr2 94.32(16) . . ?
Zr6 Zr3 Zr2 59.69(3) . . ?
Zr4 Zr3 Zr2 90.18(3) . . ?
O6 Zr3 Zr1 81.0(2) . . ?
O2 Zr3 Zr1 30.53(18) . . ?
O19 Zr3 Zr1 162.8(2) . . ?
O18 Zr3 Zr1 88.70(17) . . ?
O21 Zr3 Zr1 107.16(18) . . ?
O16 Zr3 Zr1 115.01(18) . . ?
O1 Zr3 Zr1 38.77(15) . . ?
O7 Zr3 Zr1 92.97(16) . . ?
Zr6 Zr3 Zr1 89.17(3) . . ?
Zr4 Zr3 Zr1 58.59(2) . . ?
Zr2 Zr3 Zr1 60.49(2) . . ?
O2 Zr4 O3 96.7(3) . . ?
O2 Zr4 O7 74.2(3) . . ?
O3 Zr4 O7 70.0(2) . . ?
O2 Zr4 O8 74.4(2) . . ?
O3 Zr4 O8 69.6(3) . . ?
O7 Zr4 O8 124.5(3) . . ?
O2 Zr4 O22 83.4(2) . . ?
O3 Zr4 O22 145.0(3) . . ?
O7 Zr4 O22 76.5(3) . . ?
O8 Zr4 O22 141.9(3) . . ?
O2 Zr4 O30 83.6(3) . . ?
O3 Zr4 O30 142.1(2) . . ?
O7 Zr4 O30 143.9(3) . . ?
O8 Zr4 O30 74.1(3) . . ?
O22 Zr4 O30 72.9(3) . . ?
O2 Zr4 O24 152.6(3) . . ?
O3 Zr4 O24 91.2(3) . . ?
O7 Zr4 O24 132.9(3) . . ?
O8 Zr4 O24 84.0(3) . . ?
O22 Zr4 O24 104.7(3) . . ?
O30 Zr4 O24 74.3(3) . . ?
O2 Zr4 O23 149.3(2) . . ?
O3 Zr4 O23 86.7(3) . . ?
O7 Zr4 O23 78.5(3) . . ?
O8 Zr4 O23 134.2(2) . . ?
O22 Zr4 O23 76.8(3) . . ?
O30 Zr4 O23 112.0(3) . . ?
O24 Zr4 O23 57.0(3) . . ?
O2 Zr4 C15 174.4(3) . . ?
O3 Zr4 C15 88.5(3) . . ?
O7 Zr4 C15 105.8(4) . . ?
O8 Zr4 C15 109.5(3) . . ?
O22 Zr4 C15 91.2(3) . . ?
O30 Zr4 C15 93.6(3) . . ?
O24 Zr4 C15 28.5(3) . . ?
O23 Zr4 C15 28.5(3) . . ?
O2 Zr4 Zr1 33.35(17) . . ?
O3 Zr4 Zr1 85.76(18) . . ?
O7 Zr4 Zr1 99.81(19) . . ?
O8 Zr4 Zr1 41.26(17) . . ?
O22 Zr4 Zr1 110.1(2) . . ?
O30 Zr4 Zr1 73.75(19) . . ?
O24 Zr4 Zr1 122.2(2) . . ?
O23 Zr4 Zr1 172.4(2) . . ?
C15 Zr4 Zr1 150.0(3) . . ?
O2 Zr4 Zr3 32.41(18) . . ?
O3 Zr4 Zr3 86.05(17) . . ?
O7 Zr4 Zr3 41.95(19) . . ?
O8 Zr4 Zr3 99.15(17) . . ?
O22 Zr4 Zr3 75.37(17) . . ?
O30 Zr4 Zr3 110.46(17) . . ?
O24 Zr4 Zr3 174.8(2) . . ?
O23 Zr4 Zr3 118.32(19) . . ?
C15 Zr4 Zr3 146.8(3) . . ?
Zr1 Zr4 Zr3 62.07(2) . . ?
O2 Zr4 Zr6 82.9(2) . . ?
O3 Zr4 Zr6 33.38(17) . . ?
O7 Zr4 Zr6 36.75(18) . . ?
O8 Zr4 Zr6 94.88(18) . . ?
O22 Zr4 Zr6 113.00(19) . . ?
O30 Zr4 Zr6 164.49(19) . . ?
O24 Zr4 Zr6 116.0(2) . . ?
O23 Zr4 Zr6 83.5(2) . . ?
C15 Zr4 Zr6 100.4(3) . . ?
Zr1 Zr4 Zr6 90.75(3) . . ?
Zr3 Zr4 Zr6 59.75(3) . . ?
O5 Zr1 O2 92.9(3) . . ?
O5 Zr1 O17 87.9(3) . 2_656 ?
O2 Zr1 O17 143.4(2) . 2_656 ?
O5 Zr1 O29 142.7(2) . . ?
O2 Zr1 O29 85.2(3) . . ?
O17 Zr1 O29 115.1(3) 2_656 . ?
O5 Zr1 O14 143.7(2) . 2_656 ?
O2 Zr1 O14 86.9(3) . 2_656 ?
O17 Zr1 O14 71.8(2) 2_656 2_656 ?
O29 Zr1 O14 73.5(2) . 2_656 ?
O5 Zr1 O10 84.4(3) . . ?
O2 Zr1 O10 142.6(3) . . ?
O17 Zr1 O10 73.9(2) 2_656 . ?
O29 Zr1 O10 75.4(2) . . ?
O14 Zr1 O10 116.6(3) 2_656 . ?
O5 Zr1 O1 69.3(2) . . ?
O2 Zr1 O1 69.0(2) . . ?
O17 Zr1 O1 77.3(2) 2_656 . ?
O29 Zr1 O1 141.4(2) . . ?
O14 Zr1 O1 76.9(2) 2_656 . ?
O10 Zr1 O1 141.4(2) . . ?
O5 Zr1 O8 71.4(2) . . ?
O2 Zr1 O8 71.4(2) . . ?
O17 Zr1 O8 141.8(2) 2_656 . ?
O29 Zr1 O8 72.8(3) . . ?
O14 Zr1 O8 141.0(2) 2_656 . ?
O10 Zr1 O8 72.4(2) . . ?
O1 Zr1 O8 121.3(3) . . ?
O5 Zr1 Zr5 32.73(17) . . ?
O2 Zr1 Zr5 84.03(19) . . ?
O17 Zr1 Zr5 113.41(19) 2_656 . ?
O29 Zr1 Zr5 110.40(18) . . ?
O14 Zr1 Zr5 169.72(18) 2_656 . ?
O10 Zr1 Zr5 73.7(2) . . ?
O1 Zr1 Zr5 95.31(17) . . ?
O8 Zr1 Zr5 38.83(17) . . ?
O5 Zr1 Zr4 84.07(19) . . ?
O2 Zr1 Zr4 32.68(18) . . ?
O17 Zr1 Zr4 170.5(2) 2_656 . ?
O29 Zr1 Zr4 74.4(2) . . ?
O14 Zr1 Zr4 112.30(17) 2_656 . ?
O10 Zr1 Zr4 110.22(18) . . ?
O1 Zr1 Zr4 95.08(17) . . ?
O8 Zr1 Zr4 38.90(15) . . ?
Zr5 Zr1 Zr4 61.17(3) . . ?
O5 Zr1 Zr2 30.98(17) . . ?
O2 Zr1 Zr2 81.29(19) . . ?
O17 Zr1 Zr2 80.9(2) 2_656 . ?
O29 Zr1 Zr2 164.0(2) . . ?
O14 Zr1 Zr2 114.02(17) 2_656 . ?
O10 Zr1 Zr2 110.99(19) . . ?
O1 Zr1 Zr2 38.34(16) . . ?
O8 Zr1 Zr2 94.73(18) . . ?
Zr5 Zr1 Zr2 59.84(3) . . ?
Zr4 Zr1 Zr2 89.59(3) . . ?
O5 Zr1 Zr3 81.63(18) . . ?
O2 Zr1 Zr3 30.41(18) . . ?
O17 Zr1 Zr3 114.47(16) 2_656 . ?
O29 Zr1 Zr3 111.18(17) . . ?
O14 Zr1 Zr3 80.11(18) 2_656 . ?
O10 Zr1 Zr3 163.3(2) . . ?
O1 Zr1 Zr3 38.59(15) . . ?
O8 Zr1 Zr3 94.41(16) . . ?
Zr5 Zr1 Zr3 89.62(3) . . ?
Zr4 Zr1 Zr3 59.34(2) . . ?
Zr2 Zr1 Zr3 58.77(2) . . ?
O6 Zr2 O5 91.4(3) . . ?
O6 Zr2 O13 145.7(2) . . ?
O5 Zr2 O13 95.7(3) . . ?
O6 Zr2 O32 85.9(3) . . ?
O5 Zr2 O32 140.3(3) . . ?
O13 Zr2 O32 108.5(3) . . ?
O6 Zr2 O12 141.7(3) . . ?
O5 Zr2 O12 81.1(2) . . ?
O13 Zr2 O12 72.6(3) . . ?
O32 Zr2 O12 77.1(3) . . ?
O6 Zr2 O15 81.3(2) . . ?
O5 Zr2 O15 145.6(3) . . ?
O13 Zr2 O15 73.9(3) . . ?
O32 Zr2 O15 73.1(3) . . ?
O12 Zr2 O15 124.2(2) . . ?
O6 Zr2 O1 70.5(3) . . ?
O5 Zr2 O1 69.4(2) . . ?
O13 Zr2 O1 80.7(2) . . ?
O32 Zr2 O1 143.9(2) . . ?
O12 Zr2 O1 137.6(3) . . ?
O15 Zr2 O1 76.5(2) . . ?
O6 Zr2 O4 69.9(2) . . ?
O5 Zr2 O4 69.3(3) . . ?
O13 Zr2 O4 143.5(2) . . ?
O32 Zr2 O4 72.6(2) . . ?
O12 Zr2 O4 72.4(2) . . ?
O15 Zr2 O4 136.2(3) . . ?
O1 Zr2 O4 120.7(2) . . ?
O6 Zr2 Zr6 31.40(18) . . ?
O5 Zr2 Zr6 83.19(19) . . ?
O13 Zr2 Zr6 176.64(19) . . ?
O32 Zr2 Zr6 74.07(19) . . ?
O12 Zr2 Zr6 110.35(19) . . ?
O15 Zr2 Zr6 105.2(2) . . ?
O1 Zr2 Zr6 95.92(16) . . ?
O4 Zr2 Zr6 38.85(15) . . ?
O6 Zr2 Zr5 81.43(17) . . ?
O5 Zr2 Zr5 31.6(2) . . ?
O13 Zr2 Zr5 119.92(17) . . ?
O32 Zr2 Zr5 109.24(18) . . ?
O12 Zr2 Zr5 72.55(17) . . ?
O15 Zr2 Zr5 162.39(18) . . ?
O1 Zr2 Zr5 94.26(15) . . ?
O4 Zr2 Zr5 37.75(16) . . ?
Zr6 Zr2 Zr5 60.31(2) . . ?
O6 Zr2 Zr3 31.0(2) . . ?
O5 Zr2 Zr3 83.11(16) . . ?
O13 Zr2 Zr3 116.94(18) . . ?
O32 Zr2 Zr3 111.20(18) . . ?
O12 Zr2 Zr3 162.36(17) . . ?
O15 Zr2 Zr3 73.40(18) . . ?
O1 Zr2 Zr3 39.88(16) . . ?
O4 Zr2 Zr3 94.78(15) . . ?
Zr6 Zr2 Zr3 59.81(3) . . ?
Zr5 Zr2 Zr3 89.87(3) . . ?
O6 Zr2 Zr1 81.2(2) . . ?
O5 Zr2 Zr1 30.52(19) . . ?
O13 Zr2 Zr1 88.1(2) . . ?
O32 Zr2 Zr1 163.2(2) . . ?
O12 Zr2 Zr1 106.85(19) . . ?
O15 Zr2 Zr1 115.2(2) . . ?
O1 Zr2 Zr1 38.85(15) . . ?
O4 Zr2 Zr1 92.76(16) . . ?
Zr6 Zr2 Zr1 89.37(3) . . ?
Zr5 Zr2 Zr1 58.27(3) . . ?
Zr3 Zr2 Zr1 60.74(2) . . ?
O6 Zr6 O3 94.7(3) . . ?
O6 Zr6 O7 73.1(3) . . ?
O3 Zr6 O7 69.4(2) . . ?
O6 Zr6 O20 83.5(3) . . ?
O3 Zr6 O20 142.5(3) . . ?
O7 Zr6 O20 74.3(3) . . ?
O6 Zr6 O31 83.4(3) . . ?
O3 Zr6 O31 143.6(2) . . ?
O7 Zr6 O31 142.0(2) . . ?
O20 Zr6 O31 73.7(3) . . ?
O6 Zr6 O4 73.7(2) . . ?
O3 Zr6 O4 69.8(2) . . ?
O7 Zr6 O4 124.0(3) . . ?
O20 Zr6 O4 142.8(3) . . ?
O31 Zr6 O4 74.8(2) . . ?
O6 Zr6 O25 149.8(3) . . ?
O3 Zr6 O25 88.0(3) . . ?
O7 Zr6 O25 79.8(3) . . ?
O20 Zr6 O25 76.4(3) . . ?
O31 Zr6 O25 111.6(3) . . ?
O4 Zr6 O25 134.4(2) . . ?
O6 Zr6 O26 152.1(3) . . ?
O3 Zr6 O26 90.4(3) . . ?
O7 Zr6 O26 133.8(3) . . ?
O20 Zr6 O26 108.5(3) . . ?
O31 Zr6 O26 76.4(3) . . ?
O4 Zr6 O26 82.5(3) . . ?
O25 Zr6 O26 57.6(3) . . ?
O6 Zr6 C17 175.0(3) . . ?
O3 Zr6 C17 90.1(4) . . ?
O7 Zr6 C17 107.2(3) . . ?
O20 Zr6 C17 91.7(3) . . ?
O31 Zr6 C17 93.7(4) . . ?
O4 Zr6 C17 109.6(3) . . ?
O25 Zr6 C17 28.6(3) . . ?
O26 Zr6 C17 29.1(3) . . ?
O6 Zr6 Zr2 31.61(17) . . ?
O3 Zr6 Zr2 86.22(17) . . ?
O7 Zr6 Zr2 98.44(19) . . ?
O20 Zr6 Zr2 108.6(2) . . ?
O31 Zr6 Zr2 73.2(2) . . ?
O4 Zr6 Zr2 42.46(17) . . ?
O25 Zr6 Zr2 174.2(2) . . ?
O26 Zr6 Zr2 122.0(2) . . ?
C17 Zr6 Zr2 150.9(3) . . ?
O6 Zr6 Zr3 31.44(18) . . ?
O3 Zr6 Zr3 85.77(18) . . ?
O7 Zr6 Zr3 42.01(18) . . ?
O20 Zr6 Zr3 73.3(2) . . ?
O31 Zr6 Zr3 108.3(2) . . ?
O4 Zr6 Zr3 98.71(18) . . ?
O25 Zr6 Zr3 119.43(19) . . ?
O26 Zr6 Zr3 175.3(2) . . ?
C17 Zr6 Zr3 148.0(3) . . ?
Zr2 Zr6 Zr3 60.50(3) . . ?
O6 Zr6 Zr5 81.41(18) . . ?
O3 Zr6 Zr5 33.33(16) . . ?
O7 Zr6 Zr5 94.58(18) . . ?
O20 Zr6 Zr5 163.4(2) . . ?
O31 Zr6 Zr5 111.31(18) . . ?
O4 Zr6 Zr5 36.63(17) . . ?
O25 Zr6 Zr5 114.3(2) . . ?
O26 Zr6 Zr5 88.1(2) . . ?
C17 Zr6 Zr5 103.5(3) . . ?
Zr2 Zr6 Zr5 60.13(2) . . ?
Zr3 Zr6 Zr5 90.16(3) . . ?
O5 Zr5 O3 96.9(2) . . ?
O5 Zr5 O4 74.4(3) . . ?
O3 Zr5 O4 70.6(2) . . ?
O5 Zr5 O8 74.5(2) . . ?
O3 Zr5 O8 69.7(3) . . ?
O4 Zr5 O8 125.2(2) . . ?
O5 Zr5 O9 84.0(3) . . ?
O3 Zr5 O9 142.8(3) . . ?
O4 Zr5 O9 143.1(2) . . ?
O8 Zr5 O9 74.8(3) . . ?
O5 Zr5 O11 82.4(2) . . ?
O3 Zr5 O11 143.7(3) . . ?
O4 Zr5 O11 74.3(2) . . ?
O8 Zr5 O11 142.3(3) . . ?
O9 Zr5 O11 73.5(3) . . ?
O5 Zr5 O28 150.9(3) . . ?
O3 Zr5 O28 89.4(3) . . ?
O4 Zr5 O28 81.1(3) . . ?
O8 Zr5 O28 133.8(2) . . ?
O9 Zr5 O28 107.7(3) . . ?
O11 Zr5 O28 75.9(3) . . ?
O5 Zr5 O27 151.4(3) . . ?
O3 Zr5 O27 87.4(2) . . ?
O4 Zr5 O27 133.0(3) . . ?
O8 Zr5 O27 80.7(3) . . ?
O9 Zr5 O27 75.9(3) . . ?
O11 Zr5 O27 110.4(2) . . ?
O28 Zr5 O27 56.9(3) . . ?
O5 Zr5 C19 175.1(3) . . ?
O3 Zr5 C19 88.0(3) . . ?
O4 Zr5 C19 107.2(4) . . ?
O8 Zr5 C19 107.7(3) . . ?
O9 Zr5 C19 92.3(3) . . ?
O11 Zr5 C19 93.5(3) . . ?
O28 Zr5 C19 28.3(3) . . ?
O27 Zr5 C19 28.7(3) . . ?
O5 Zr5 Zr1 33.16(19) . . ?
O3 Zr5 Zr1 86.01(19) . . ?
O4 Zr5 Zr1 100.05(17) . . ?
O8 Zr5 Zr1 41.50(17) . . ?
O9 Zr5 Zr1 74.5(2) . . ?
O11 Zr5 Zr1 109.45(19) . . ?
O28 Zr5 Zr1 174.63(18) . . ?
O27 Zr5 Zr1 119.9(2) . . ?
C19 Zr5 Zr1 148.3(3) . . ?
O5 Zr5 Zr2 32.5(2) . . ?
O3 Zr5 Zr2 85.87(17) . . ?
O4 Zr5 Zr2 41.91(18) . . ?
O8 Zr5 Zr2 99.10(17) . . ?
O9 Zr5 Zr2 110.94(18) . . ?
O11 Zr5 Zr2 74.16(16) . . ?
O28 Zr5 Zr2 120.66(19) . . ?
O27 Zr5 Zr2 172.9(2) . . ?
C19 Zr5 Zr2 148.5(3) . . ?
Zr1 Zr5 Zr2 61.90(3) . . ?
O5 Zr5 Zr6 83.19(19) . . ?
O3 Zr5 Zr6 33.55(18) . . ?
O4 Zr5 Zr6 37.22(17) . . ?
O8 Zr5 Zr6 95.22(17) . . ?
O9 Zr5 Zr6 165.5(2) . . ?
O11 Zr5 Zr6 111.37(18) . . ?
O28 Zr5 Zr6 86.74(19) . . ?
O27 Zr5 Zr6 113.4(2) . . ?
C19 Zr5 Zr6 100.8(3) . . ?
Zr1 Zr5 Zr6 91.04(3) . . ?
Zr2 Zr5 Zr6 59.56(2) . . ?
C1 O9 Zr5 132.8(6) . . ?
Zr4 O3 Zr5 114.2(3) . . ?
Zr4 O3 Zr6 113.6(3) . . ?
Zr5 O3 Zr6 113.1(3) . . ?
Zr5 O4 Zr6 106.1(3) . . ?
Zr5 O4 Zr2 100.3(3) . . ?
Zr6 O4 Zr2 98.7(2) . . ?
Zr5 O4 H4O 116.4 . . ?
Zr6 O4 H4O 116.4 . . ?
Zr2 O4 H4O 116.4 . . ?
Zr5 O8 Zr4 106.1(3) . . ?
Zr5 O8 Zr1 99.7(2) . . ?
Zr4 O8 Zr1 99.8(2) . . ?
Zr5 O8 H8O 116.3 . . ?
Zr4 O8 H8O 116.3 . . ?
Zr1 O8 H8O 116.3 . . ?
C21 O29 Zr1 134.0(8) . . ?
Zr2 O1 Zr3 100.6(3) . . ?
Zr2 O1 Zr1 102.8(2) . . ?
Zr3 O1 Zr1 102.6(2) . . ?
Zr2 O1 H1O 116.2 . . ?
Zr3 O1 H1O 116.2 . . ?
Zr1 O1 H1O 116.2 . . ?
Zr6 O6 Zr3 117.3(3) . . ?
Zr6 O6 Zr2 117.0(3) . . ?
Zr3 O6 Zr2 118.0(4) . . ?
C9 O17 Zr1 147.1(7) . 2_656 ?
C5 O14 Zr1 146.8(7) . 2_656 ?
C17 O26 Zr6 91.0(7) . . ?
C13 O22 Zr4 130.2(6) . . ?
C9 O18 Zr3 137.9(7) . . ?
C23 O31 Zr6 132.7(8) . . ?
C7 O16 Zr3 134.1(6) . . ?
C11 O19 Zr3 134.2(7) . . ?
C19 O27 Zr5 91.8(7) . . ?
C5 O13 Zr2 137.4(6) . . ?
Zr4 O7 Zr6 106.7(3) . . ?
Zr4 O7 Zr3 100.0(3) . . ?
Zr6 O7 Zr3 99.7(3) . . ?
Zr4 O7 H7O 116.0 . . ?
Zr6 O7 H7O 116.0 . . ?
Zr3 O7 H7O 116.0 . . ?
Zr4 O2 Zr3 115.7(3) . . ?
Zr4 O2 Zr1 114.0(3) . . ?
Zr3 O2 Zr1 119.1(3) . . ?
C11 O20 Zr6 132.7(8) . . ?
C3 O12 Zr2 135.5(6) . . ?
Zr5 O5 Zr1 114.1(3) . . ?
Zr5 O5 Zr2 115.8(4) . . ?
Zr1 O5 Zr2 118.5(3) . . ?
C15 O24 Zr4 93.6(6) . . ?
C1 O10 Zr1 133.3(8) . . ?
C23 O32 Zr2 132.6(7) . . ?
C3 O11 Zr5 131.8(6) . . ?
C19 O28 Zr5 94.3(8) . . ?
C13 O21 Zr3 135.0(6) . . ?
C7 O15 Zr2 134.3(7) . . ?
C21 O30 Zr4 133.1(7) . . ?
C17 O25 Zr6 92.1(7) . . ?
C15 O23 Zr4 91.9(7) . . ?
O30 C21 O29 124.5(11) . . ?
O30 C21 C22 118.8(10) . . ?
O29 C21 C22 116.7(11) . . ?
O19 C11 O20 125.8(10) . . ?
O19 C11 C12 119.7(11) . . ?
O20 C11 C12 114.5(12) . . ?
O9 C1 O10 125.1(10) . . ?
O9 C1 C2 118.1(9) . . ?
O10 C1 C2 116.6(12) . . ?
O12 C3 O11 125.7(9) . . ?
O12 C3 C4 117.7(9) . . ?
O11 C3 C4 116.6(9) . . ?
O14 C5 O13 123.2(9) . . ?
O14 C5 C6 120.7(10) . . ?
O13 C5 C6 116.1(9) . . ?
O21 C13 O22 127.1(9) . . ?
O21 C13 C14 116.4(9) . . ?
O22 C13 C14 116.5(9) . . ?
O32 C23 O31 126.8(11) . . ?
O32 C23 C24 116.3(11) . . ?
O31 C23 C24 116.9(12) . . ?
O18 C9 O17 123.1(10) . . ?
O18 C9 C10 115.7(9) . . ?
O17 C9 C10 121.3(9) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O25 C17 O26 119.2(12) . . ?
O25 C17 C18 121.8(12) . . ?
O26 C17 C18 119.0(12) . . ?
O25 C17 Zr6 59.3(7) . . ?
O26 C17 Zr6 59.9(7) . . ?
C18 C17 Zr6 174.6(12) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O28 C19 O27 117.0(11) . . ?
O28 C19 C20 121.8(13) . . ?
O27 C19 C20 121.2(11) . . ?
O28 C19 Zr5 57.5(6) . . ?
O27 C19 Zr5 59.5(6) . . ?
C20 C19 Zr5 178.8(9) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O15 C7 O16 125.0(10) . . ?
O15 C7 C8 117.7(10) . . ?
O16 C7 C8 117.2(9) . . ?
O24 C15 O23 117.4(10) . . ?
O24 C15 C16 120.3(11) . . ?
O23 C15 C16 122.2(12) . . ?
O24 C15 Zr4 57.9(5) . . ?
O23 C15 Zr4 59.5(6) . . ?
C16 C15 Zr4 178.0(8) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O33 C25 O34 122.1(16) . . ?
O33 C25 C26 117.1(16) . . ?
O34 C25 C26 120.8(17) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 O34 H34 109.5 . . ?

_refine_diff_density_max         2.048
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.213



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetic acid'
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1837734'
_audit_update_record             
;
2018-04-17 deposited with the CCDC.
2018-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C60 H92 N4 O36 Zr6'
_chemical_formula_sum            'C60 H92 N4 O36 Zr6'
_chemical_formula_weight         1992.69

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'

_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'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   16.0037(4)
_cell_length_b                   16.0037(4)
_cell_length_c                   16.2833(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4170.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(2)
_cell_measurement_reflns_used    15748
_cell_measurement_theta_min      3.9578
_cell_measurement_theta_max      36.6070
_exptl_absorpt_correction_T_min  0.88555
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_F_000             2016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    0.806
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_diffrn_ambient_temperature      150.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measurement_device_type  
;
Oxford Diffraction Xcalibur CCD
diffractometer
;
_diffrn_measurement_method       'omega scan'

_diffrn_reflns_number            18520
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.964
_diffrn_reflns_theta_max         26.993
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             4543
_reflns_number_gt                4146
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0249P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1877 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.008(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4543
_refine_ls_number_parameters     249
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0163
_refine_ls_wR_factor_ref         0.0389
_refine_ls_wR_factor_gt          0.0386
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_restrained_S_all      0.969
_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
O4 O 0.70297(12) 0.56670(12) 0.23269(12) 0.0340(4) Uani 1 1 d . . . . .
C1 C 0.65392(16) 0.52525(17) 0.27509(17) 0.0286(6) Uani 1 1 d . . . . .
C2 C 0.66204(18) 0.52646(18) 0.36727(17) 0.0322(6) Uani 1 1 d . . . . .
C3 C 0.61067(19) 0.4802(2) 0.41264(19) 0.0420(7) Uani 1 1 d . . . . .
H3A H 0.6152 0.4808 0.4696 0.050 Uiso 1 1 calc R U . . .
H3B H 0.5702 0.4473 0.3874 0.050 Uiso 1 1 calc R U . . .
C4 C 0.7284(2) 0.5808(2) 0.4023(2) 0.0490(9) Uani 1 1 d . . . . .
H4A H 0.7230 0.5824 0.4610 0.073 Uiso 1 1 calc R U . . .
H4B H 0.7228 0.6363 0.3806 0.073 Uiso 1 1 calc R U . . .
H4C H 0.7822 0.5588 0.3879 0.073 Uiso 1 1 calc R U . . .
N1 N 0.34468(15) 0.24464(16) -0.22571(15) 0.0381(6) Uani 1 1 d . . . . .
C13 C 0.3923(2) 0.1693(2) -0.2389(3) 0.0520(9) Uani 1 1 d . . . . .
H13A H 0.4280 0.1764 -0.2858 0.078 Uiso 1 1 calc R U . . .
H13B H 0.3549 0.1234 -0.2484 0.078 Uiso 1 1 calc R U . . .
H13C H 0.4259 0.1580 -0.1913 0.078 Uiso 1 1 calc R U . . .
C14 C 0.2852(2) 0.2681(3) -0.2894(2) 0.0564(10) Uani 1 1 d . . . . .
H14A H 0.2493 0.3116 -0.2692 0.085 Uiso 1 1 calc R U . . .
H14B H 0.2521 0.2203 -0.3041 0.085 Uiso 1 1 calc R U . . .
H14C H 0.3149 0.2877 -0.3368 0.085 Uiso 1 1 calc R U . . .
C15 C 0.35781(17) 0.29286(18) -0.16154(18) 0.0324(6) Uani 1 1 d . . . . .
H15 H 0.3274 0.3423 -0.1580 0.039 Uiso 1 1 calc R U . . .
H1O H 0.649(2) 0.552(3) 0.1324(17) 0.072(13) Uiso 1 1 d D . . . .
Zr1 Zr 0.5000 0.5000 0.15504(2) 0.02068(7) Uani 1 2 d S T P . .
Zr2 Zr 0.43924(2) 0.35787(2) 0.00258(2) 0.02034(6) Uani 1 1 d . . . . .
O7 O 0.52591(9) 0.24809(9) 0.00446(16) 0.0269(3) Uani 1 1 d . . . . .
O8 O 0.30020(8) 0.34370(9) 0.00017(17) 0.0270(3) Uani 1 1 d . . . . .
O9 O 0.40786(14) 0.27714(14) -0.10530(14) 0.0299(5) Uani 1 1 d . . . . .
O1 O 0.53686(11) 0.41315(12) 0.06540(12) 0.0216(4) Uani 1 1 d . . . . .
C9 C 0.60392(13) 0.24095(12) -0.0005(2) 0.0245(4) Uani 1 1 d . . . . .
O6 O 0.41581(14) 0.29050(13) 0.11717(13) 0.0269(5) Uani 1 1 d . . . . .
C10 C 0.63700(15) 0.15351(14) -0.0062(3) 0.0313(5) Uani 1 1 d . . . . .
O2 O 0.61422(11) 0.54372(11) 0.08889(12) 0.0215(4) Uani 1 1 d D . . . .
C12 C 0.71825(16) 0.14093(16) -0.0058(3) 0.0433(7) Uani 1 1 d . . . . .
H12A H 0.7393 0.0869 -0.0090 0.052 Uiso 1 1 calc R U . . .
H12B H 0.7546 0.1861 -0.0023 0.052 Uiso 1 1 calc R U . . .
O5 O 0.47661(12) 0.37107(12) 0.21290(12) 0.0290(4) Uani 1 1 d . . . . .
O3 O 0.59436(12) 0.47932(12) 0.24623(12) 0.0301(4) Uani 1 1 d . . . . .
C7 C 0.4329(3) 0.1528(2) 0.2164(3) 0.0642(12) Uani 1 1 d . . . . .
H7A H 0.4368 0.1064 0.2506 0.077 Uiso 1 1 calc R U . . .
H7B H 0.4154 0.1464 0.1623 0.077 Uiso 1 1 calc R U . . .
C11 C 0.5741(2) 0.08525(17) -0.0116(4) 0.0644(13) Uani 1 1 d . . . . .
H11A H 0.5404 0.0930 -0.0598 0.097 Uiso 1 1 calc R U . . .
H11B H 0.5391 0.0863 0.0363 0.097 Uiso 1 1 calc R U . . .
H11C H 0.6023 0.0324 -0.0148 0.097 Uiso 1 1 calc R U . . .
C5 C 0.44759(16) 0.30287(17) 0.18696(18) 0.0287(6) Uani 1 1 d . . . . .
C8 C 0.4806(3) 0.2475(3) 0.3283(2) 0.0662(12) Uani 1 1 d . . . . .
H8A H 0.4841 0.1963 0.3589 0.099 Uiso 1 1 calc R U . . .
H8B H 0.4416 0.2844 0.3545 0.099 Uiso 1 1 calc R U . . .
H8C H 0.5346 0.2735 0.3264 0.099 Uiso 1 1 calc R U . . .
C6 C 0.45262(19) 0.22961(19) 0.2454(2) 0.0391(7) Uani 1 1 d . . . . .


_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
O4 C1 1.238(3) . ?
C1 O3 1.292(3) . ?
C1 C2 1.507(4) . ?
C2 C3 1.330(4) . ?
C2 C4 1.486(4) . ?
N1 C15 1.316(4) . ?
N1 C13 1.443(4) . ?
N1 C14 1.457(4) . ?
C15 O9 1.242(4) . ?
Zr1 O1 2.1001(18) 2_665 ?
Zr1 O1 2.1001(18) . ?
Zr1 O3 2.1436(18) 2_665 ?
Zr1 O3 2.1437(18) . ?
Zr1 O2 2.2341(18) . ?
Zr1 O2 2.2342(18) 2_665 ?
Zr1 O5 2.2989(18) 2_665 ?
Zr1 O5 2.2990(18) . ?
Zr1 Zr2 3.5045(4) 2_665 ?
Zr1 Zr2 3.5045(4) . ?
Zr1 Zr2 3.5646(4) 3_565 ?
Zr1 Zr2 3.5646(4) 4_655 ?
Zr2 O1 2.0587(18) 3_565 ?
Zr2 O1 2.0662(18) . ?
Zr2 O6 2.187(2) . ?
Zr2 O8 2.2372(14) . ?
Zr2 O9 2.238(2) . ?
Zr2 O7 2.2386(14) . ?
Zr2 O2 2.2776(19) 2_665 ?
Zr2 O2 2.2834(18) 3_565 ?
Zr2 Zr2 3.4993(3) 3_565 ?
Zr2 Zr2 3.4993(3) 4_655 ?
Zr2 Zr1 3.5646(4) 3_565 ?
O7 C9 1.256(3) . ?
O8 C9 1.266(2) 3_565 ?
O1 Zr2 2.0586(18) 4_655 ?
C9 O8 1.266(2) 4_655 ?
C9 C10 1.499(3) . ?
O6 C5 1.261(4) . ?
C10 C12 1.316(3) . ?
C10 C11 1.488(4) . ?
O2 Zr2 2.2776(19) 2_665 ?
O2 Zr2 2.2833(18) 4_655 ?
O5 C5 1.259(3) . ?
C7 C6 1.354(5) . ?
C5 C6 1.512(4) . ?
C8 C6 1.452(5) . ?

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 C1 O3 124.7(3) . . ?
O4 C1 C2 119.6(2) . . ?
O3 C1 C2 115.7(2) . . ?
C3 C2 C4 123.6(3) . . ?
C3 C2 C1 119.5(3) . . ?
C4 C2 C1 116.8(3) . . ?
C15 N1 C13 121.6(3) . . ?
C15 N1 C14 121.2(3) . . ?
C13 N1 C14 117.0(3) . . ?
O9 C15 N1 124.7(3) . . ?
O1 Zr1 O1 91.94(11) 2_665 . ?
O1 Zr1 O3 100.45(7) 2_665 2_665 ?
O1 Zr1 O3 141.40(7) . 2_665 ?
O1 Zr1 O3 141.40(7) 2_665 . ?
O1 Zr1 O3 100.45(7) . . ?
O3 Zr1 O3 92.31(11) 2_665 . ?
O1 Zr1 O2 71.79(8) 2_665 . ?
O1 Zr1 O2 69.05(8) . . ?
O3 Zr1 O2 149.55(7) 2_665 . ?
O3 Zr1 O2 78.81(8) . . ?
O1 Zr1 O2 69.05(8) 2_665 2_665 ?
O1 Zr1 O2 71.79(8) . 2_665 ?
O3 Zr1 O2 78.81(8) 2_665 2_665 ?
O3 Zr1 O2 149.55(7) . 2_665 ?
O2 Zr1 O2 122.35(10) . 2_665 ?
O1 Zr1 O5 74.72(7) 2_665 2_665 ?
O1 Zr1 O5 146.42(7) . 2_665 ?
O3 Zr1 O5 72.08(8) 2_665 2_665 ?
O3 Zr1 O5 74.93(8) . 2_665 ?
O2 Zr1 O5 77.48(7) . 2_665 ?
O2 Zr1 O5 127.72(7) 2_665 2_665 ?
O1 Zr1 O5 146.42(7) 2_665 . ?
O1 Zr1 O5 74.73(7) . . ?
O3 Zr1 O5 74.93(8) 2_665 . ?
O3 Zr1 O5 72.07(8) . . ?
O2 Zr1 O5 127.73(7) . . ?
O2 Zr1 O5 77.48(7) 2_665 . ?
O5 Zr1 O5 131.61(10) 2_665 . ?
O1 Zr1 Zr2 32.44(5) 2_665 2_665 ?
O1 Zr1 Zr2 81.91(5) . 2_665 ?
O3 Zr1 Zr2 125.87(5) 2_665 2_665 ?
O3 Zr1 Zr2 113.29(5) . 2_665 ?
O2 Zr1 Zr2 39.49(5) . 2_665 ?
O2 Zr1 Zr2 95.09(5) 2_665 2_665 ?
O5 Zr1 Zr2 70.28(5) 2_665 2_665 ?
O5 Zr1 Zr2 156.64(5) . 2_665 ?
O1 Zr1 Zr2 81.91(5) 2_665 . ?
O1 Zr1 Zr2 32.44(5) . . ?
O3 Zr1 Zr2 113.29(5) 2_665 . ?
O3 Zr1 Zr2 125.87(5) . . ?
O2 Zr1 Zr2 95.09(5) . . ?
O2 Zr1 Zr2 39.49(5) 2_665 . ?
O5 Zr1 Zr2 156.63(5) 2_665 . ?
O5 Zr1 Zr2 70.28(5) . . ?
Zr2 Zr1 Zr2 89.798(12) 2_665 . ?
O1 Zr1 Zr2 30.66(5) 2_665 3_565 ?
O1 Zr1 Zr2 81.91(5) . 3_565 ?
O3 Zr1 Zr2 90.41(6) 2_665 3_565 ?
O3 Zr1 Zr2 172.06(5) . 3_565 ?
O2 Zr1 Zr2 95.14(5) . 3_565 ?
O2 Zr1 Zr2 38.39(5) 2_665 3_565 ?
O5 Zr1 Zr2 98.87(5) 2_665 3_565 ?
O5 Zr1 Zr2 115.85(5) . 3_565 ?
Zr2 Zr1 Zr2 59.334(5) 2_665 3_565 ?
Zr2 Zr1 Zr2 59.333(5) . 3_565 ?
O1 Zr1 Zr2 81.91(5) 2_665 4_655 ?
O1 Zr1 Zr2 30.66(5) . 4_655 ?
O3 Zr1 Zr2 172.06(5) 2_665 4_655 ?
O3 Zr1 Zr2 90.41(6) . 4_655 ?
O2 Zr1 Zr2 38.39(5) . 4_655 ?
O2 Zr1 Zr2 95.14(5) 2_665 4_655 ?
O5 Zr1 Zr2 115.85(5) 2_665 4_655 ?
O5 Zr1 Zr2 98.87(5) . 4_655 ?
Zr2 Zr1 Zr2 59.334(5) 2_665 4_655 ?
Zr2 Zr1 Zr2 59.334(5) . 4_655 ?
Zr2 Zr1 Zr2 87.886(11) 3_565 4_655 ?
O1 Zr2 O1 93.97(11) 3_565 . ?
O1 Zr2 O6 145.82(8) 3_565 . ?
O1 Zr2 O6 85.32(8) . . ?
O1 Zr2 O8 82.63(7) 3_565 . ?
O1 Zr2 O8 143.53(8) . . ?
O6 Zr2 O8 78.14(9) . . ?
O1 Zr2 O9 90.28(8) 3_565 . ?
O1 Zr2 O9 143.66(8) . . ?
O6 Zr2 O9 110.27(7) . . ?
O8 Zr2 O9 72.81(9) . . ?
O1 Zr2 O7 140.83(8) 3_565 . ?
O1 Zr2 O7 82.00(7) . . ?
O6 Zr2 O7 73.00(9) . . ?
O8 Zr2 O7 122.48(5) . . ?
O9 Zr2 O7 72.34(9) . . ?
O1 Zr2 O2 71.92(7) 3_565 2_665 ?
O1 Zr2 O2 71.49(7) . 2_665 ?
O6 Zr2 O2 75.53(8) . 2_665 ?
O8 Zr2 O2 72.97(7) . 2_665 ?
O9 Zr2 O2 143.06(7) . 2_665 ?
O7 Zr2 O2 140.09(8) . 2_665 ?
O1 Zr2 O2 68.76(7) 3_565 3_565 ?
O1 Zr2 O2 71.67(7) . 3_565 ?
O6 Zr2 O2 141.11(7) . 3_565 ?
O8 Zr2 O2 137.46(8) . 3_565 ?
O9 Zr2 O2 76.42(8) . 3_565 ?
O7 Zr2 O2 73.07(7) . 3_565 ?
O2 Zr2 O2 122.85(9) 2_665 3_565 ?
O1 Zr2 Zr2 32.03(5) 3_565 3_565 ?
O1 Zr2 Zr2 84.03(5) . 3_565 ?
O6 Zr2 Zr2 114.46(6) . 3_565 ?
O8 Zr2 Zr2 73.95(4) . 3_565 ?
O9 Zr2 Zr2 115.68(6) . 3_565 ?
O7 Zr2 Zr2 163.56(4) . 3_565 ?
O2 Zr2 Zr2 39.95(5) 2_665 3_565 ?
O2 Zr2 Zr2 94.32(5) 3_565 3_565 ?
O1 Zr2 Zr2 82.57(5) 3_565 4_655 ?
O1 Zr2 Zr2 31.90(5) . 4_655 ?
O6 Zr2 Zr2 111.29(6) . 4_655 ?
O8 Zr2 Zr2 163.79(4) . 4_655 ?
O9 Zr2 Zr2 113.84(6) . 4_655 ?
O7 Zr2 Zr2 73.59(4) . 4_655 ?
O2 Zr2 Zr2 96.09(5) 2_665 4_655 ?
O2 Zr2 Zr2 39.83(5) 3_565 4_655 ?
Zr2 Zr2 Zr2 89.966(1) 3_565 4_655 ?
O1 Zr2 Zr1 84.61(5) 3_565 . ?
O1 Zr2 Zr1 33.04(5) . . ?
O6 Zr2 Zr1 76.31(6) . . ?
O8 Zr2 Zr1 110.74(6) . . ?
O9 Zr2 Zr1 173.26(6) . . ?
O7 Zr2 Zr1 109.14(6) . . ?
O2 Zr2 Zr1 38.59(4) 2_665 . ?
O2 Zr2 Zr1 97.58(5) 3_565 . ?
Zr2 Zr2 Zr1 61.189(7) 3_565 . ?
Zr2 Zr2 Zr1 61.188(7) 4_655 . ?
O1 Zr2 Zr1 31.35(5) 3_565 3_565 ?
O1 Zr2 Zr1 82.93(5) . 3_565 ?
O6 Zr2 Zr1 167.29(6) . 3_565 ?
O8 Zr2 Zr1 108.87(6) . 3_565 ?
O9 Zr2 Zr1 82.21(6) . 3_565 ?
O7 Zr2 Zr1 109.98(6) . 3_565 ?
O2 Zr2 Zr1 96.06(5) 2_665 3_565 ?
O2 Zr2 Zr1 37.42(4) 3_565 3_565 ?
Zr2 Zr2 Zr1 59.477(7) 3_565 3_565 ?
Zr2 Zr2 Zr1 59.477(7) 4_655 3_565 ?
Zr1 Zr2 Zr1 91.157(9) . 3_565 ?
C9 O7 Zr2 133.33(13) . . ?
C9 O8 Zr2 132.69(13) 3_565 . ?
C15 O9 Zr2 127.3(2) . . ?
Zr2 O1 Zr2 116.07(9) 4_655 . ?
Zr2 O1 Zr1 117.99(8) 4_655 . ?
Zr2 O1 Zr1 114.52(8) . . ?
O7 C9 O8 126.14(19) . 4_655 ?
O7 C9 C10 116.10(18) . . ?
O8 C9 C10 117.76(18) 4_655 . ?
C5 O6 Zr2 128.49(19) . . ?
C12 C10 C11 123.8(2) . . ?
C12 C10 C9 119.4(2) . . ?
C11 C10 C9 116.8(2) . . ?
Zr1 O2 Zr2 101.92(7) . 2_665 ?
Zr1 O2 Zr2 104.19(7) . 4_655 ?
Zr2 O2 Zr2 100.21(8) 2_665 4_655 ?
C5 O5 Zr1 134.47(18) . . ?
C1 O3 Zr1 133.14(17) . . ?
O5 C5 O6 126.0(3) . . ?
O5 C5 C6 116.2(3) . . ?
O6 C5 C6 117.8(3) . . ?
C7 C6 C8 125.1(3) . . ?
C7 C6 C5 118.2(3) . . ?
C8 C6 C5 116.7(3) . . ?

_refine_diff_density_max         0.228
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.038


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
