# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# 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_aaa
_database_code_depnum_ccdc_archive 'CCDC 1585933'
_audit_update_record             
;
2017-11-16 deposited with the CCDC.
2018-03-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C115 H155 N9 O53 Zr6'
_chemical_formula_sum            'C115 H155 N9 O53 Zr6'
_chemical_formula_weight         3058.80

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.624(2)
_cell_length_b                   19.309(4)
_cell_length_c                   19.483(4)
_cell_angle_alpha                63.46(3)
_cell_angle_beta                 77.79(3)
_cell_angle_gamma                83.38(3)
_cell_volume                     3493.7(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    13036
_cell_measurement_theta_min      1.18
_cell_measurement_theta_max      25.78

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1572
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7357
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            23440
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0913
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.18
_diffrn_reflns_theta_max         25.78
_reflns_number_total             13036
_reflns_number_gt                8941
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  SHELXTL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0650P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13036
_refine_ls_number_parameters     586
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1455
_refine_ls_wR_factor_gt          0.1370
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.44265(3) 0.93356(3) 0.14295(2) 0.02758(12) Uani 1 1 d . . .
Zr2 Zr 0.56479(4) 1.11588(3) 0.00880(2) 0.03124(13) Uani 1 1 d . . .
Zr3 Zr 0.72425(3) 0.94554(3) 0.00650(2) 0.03044(13) Uani 1 1 d . . .
O1 O 0.4640(3) 0.99218(19) 0.21326(16) 0.0354(7) Uani 1 1 d . . .
O2 O 0.5417(3) 1.10882(19) 0.12979(16) 0.0457(9) Uani 1 1 d . . .
O3 O -0.2481(2) 1.05736(19) 0.79614(16) 0.0375(8) Uani 1 1 d . . .
O4 O -0.1377(3) 0.9820(2) 0.89057(16) 0.0517(10) Uani 1 1 d . . .
O5 O 0.5856(3) 0.86338(18) 0.21125(15) 0.0368(8) Uani 1 1 d . . .
O6 O 0.7681(3) 0.8647(2) 0.12797(16) 0.0493(10) Uani 1 1 d . . .
O7 O 0.6296(3) 0.18487(19) 0.79874(16) 0.0406(8) Uani 1 1 d . . .
O8 O 0.6342(4) 0.2170(2) 0.89403(19) 0.0720(13) Uani 1 1 d . . .
O9 O 0.6193(4) 0.9990(2) 0.0773(2) 0.0836(15) Uani 1 1 d . . .
O10 O 0.3934(4) 1.0527(2) 0.0706(2) 0.0837(16) Uani 1 1 d U . .
O11 O 0.5518(3) 0.8829(3) 0.0683(2) 0.0653(13) Uani 1 1 d . . .
O12 O 0.3268(4) 0.9367(3) 0.06142(19) 0.0716(13) Uani 1 1 d . . .
O13 O 0.8976(3) 0.9851(2) 0.01750(18) 0.0530(11) Uani 1 1 d D . .
O14 O 0.4496(5) 1.2182(3) 0.0110(2) 0.0917(16) Uani 1 1 d . . .
O15 O 0.7445(3) 1.1508(2) 0.0193(2) 0.0597(11) Uani 1 1 d . . .
O16 O 0.8082(4) 0.8379(2) -0.0003(2) 0.0775(13) Uani 1 1 d . . .
C1 C 0.4451(4) 1.1216(3) 0.4659(3) 0.0440(12) Uani 1 1 d . . .
C2 C 0.3337(4) 1.1033(3) 0.5214(3) 0.0438(13) Uani 1 1 d . . .
H2 H 0.2627 1.0878 0.5112 0.053 Uiso 1 1 calc R . .
C3 C 0.3243(4) 1.1071(3) 0.5913(3) 0.0422(12) Uani 1 1 d . . .
C4 C 0.4299(4) 1.1303(3) 0.6068(3) 0.0529(15) Uani 1 1 d . . .
H4 H 0.4253 1.1314 0.6545 0.063 Uiso 1 1 calc R . .
C5 C 0.5409(4) 1.1516(4) 0.5521(3) 0.0523(14) Uani 1 1 d . . .
C6 C 0.5474(5) 1.1471(3) 0.4827(3) 0.0537(15) Uani 1 1 d . . .
H6 H 0.6227 1.1617 0.4457 0.064 Uiso 1 1 calc R . .
C7 C 0.4542(4) 1.1091(3) 0.3953(2) 0.0441(13) Uani 1 1 d . . .
C8 C 0.3896(5) 1.0506(3) 0.3972(3) 0.0512(14) Uani 1 1 d . . .
H8 H 0.3359 1.0201 0.4431 0.061 Uiso 1 1 calc R . .
C9 C 0.4015(5) 1.0353(3) 0.3333(3) 0.0480(13) Uani 1 1 d . . .
H9 H 0.3559 0.9950 0.3372 0.058 Uiso 1 1 calc R . .
C10 C 0.4795(4) 1.0786(3) 0.2643(2) 0.0407(12) Uani 1 1 d . . .
C11 C 0.5437(5) 1.1399(3) 0.2591(3) 0.0601(16) Uani 1 1 d . . .
H11 H 0.5947 1.1710 0.2122 0.072 Uiso 1 1 calc R . .
C12 C 0.5322(5) 1.1552(4) 0.3237(3) 0.0617(16) Uani 1 1 d . . .
H12 H 0.5763 1.1962 0.3195 0.074 Uiso 1 1 calc R . .
C13 C 0.4961(4) 1.0589(3) 0.1970(3) 0.0383(11) Uani 1 1 d . . .
C14 C 0.2035(4) 1.0859(3) 0.6505(3) 0.0423(12) Uani 1 1 d . . .
C15 C 0.0845(4) 1.1086(3) 0.6286(3) 0.0533(16) Uani 1 1 d . . .
H15 H 0.0798 1.1374 0.5761 0.064 Uiso 1 1 calc R . .
C16 C -0.0290(4) 1.0892(3) 0.6840(3) 0.0547(16) Uani 1 1 d . . .
H16 H -0.1082 1.1059 0.6682 0.066 Uiso 1 1 calc R . .
C17 C -0.0243(4) 1.0457(3) 0.7615(2) 0.0384(11) Uani 1 1 d . . .
C18 C 0.0949(4) 1.0224(3) 0.7843(3) 0.0475(14) Uani 1 1 d . . .
H18 H 0.0990 0.9932 0.8368 0.057 Uiso 1 1 calc R . .
C19 C 0.2072(4) 1.0424(3) 0.7297(3) 0.0480(14) Uani 1 1 d . . .
H19 H 0.2862 1.0266 0.7459 0.058 Uiso 1 1 calc R . .
C20 C -0.1458(4) 1.0269(3) 0.8206(2) 0.0373(11) Uani 1 1 d . . .
C21 C 0.6557(5) 1.1774(4) 0.5700(3) 0.081(2) Uani 1 1 d . . .
H21A H 0.7251 1.1905 0.5261 0.122 Uiso 1 1 calc R . .
H21B H 0.6833 1.1360 0.6150 0.122 Uiso 1 1 calc R . .
H21C H 0.6310 1.2218 0.5801 0.122 Uiso 1 1 calc R . .
C22 C 0.9005(5) 0.6302(3) 0.4691(3) 0.0487(14) Uani 1 1 d . . .
C23 C 0.8447(4) 0.5626(3) 0.5234(3) 0.0484(14) Uani 1 1 d . . .
H23 H 0.7770 0.5452 0.5122 0.058 Uiso 1 1 calc R . .
C24 C 0.8831(5) 0.5189(3) 0.5938(3) 0.0549(15) Uani 1 1 d . . .
C25 C 0.9863(6) 0.5451(4) 0.6088(3) 0.084(2) Uani 1 1 d U A .
H25 H 1.0158 0.5160 0.6555 0.101 Uiso 1 1 calc R . .
C26 C 1.0454(6) 0.6130(4) 0.5562(4) 0.090(2) Uani 1 1 d U . .
C27 C 1.0010(6) 0.6548(4) 0.4873(3) 0.079(2) Uani 1 1 d . A .
H27 H 1.0397 0.7013 0.4517 0.095 Uiso 1 1 calc R . .
C28 C 0.8511(4) 0.6789(3) 0.3976(3) 0.0454(13) Uani 1 1 d . . .
C29 C 0.7206(4) 0.6854(3) 0.3965(3) 0.0442(13) Uani 1 1 d . . .
C30 C 0.6731(4) 0.7359(3) 0.3306(3) 0.0516(14) Uani 1 1 d . . .
H30 H 0.5847 0.7395 0.3317 0.062 Uiso 1 1 calc R . .
C31 C 0.7550(4) 0.7816(3) 0.2622(2) 0.0378(11) Uani 1 1 d . . .
C32 C 0.8851(4) 0.7721(3) 0.2613(3) 0.0523(15) Uani 1 1 d . . .
H32 H 0.9421 0.7990 0.2154 0.063 Uiso 1 1 calc R . .
C33 C 0.9322(4) 0.7230(3) 0.3279(3) 0.0555(16) Uani 1 1 d . . .
H33 H 1.0207 0.7192 0.3265 0.067 Uiso 1 1 calc R . .
C34 C 0.7008(4) 0.8402(3) 0.1948(2) 0.0406(12) Uani 1 1 d . . .
C35 C 0.8193(5) 0.4468(3) 0.6532(3) 0.0521(14) Uani 1 1 d . . .
C36 C 0.7629(5) 0.3998(3) 0.6322(3) 0.0556(15) Uani 1 1 d . . .
H36 H 0.7618 0.4153 0.5797 0.067 Uiso 1 1 calc R . .
C37 C 0.7079(5) 0.3303(3) 0.6871(3) 0.0508(14) Uani 1 1 d . . .
H37 H 0.6724 0.2995 0.6709 0.061 Uiso 1 1 calc R . .
C38 C 0.7052(5) 0.3064(3) 0.7651(3) 0.0517(14) Uani 1 1 d . . .
C39 C 0.7565(7) 0.3526(4) 0.7868(3) 0.079(2) Uani 1 1 d . . .
H39 H 0.7529 0.3379 0.8396 0.095 Uiso 1 1 calc R . .
C40 C 0.8142(7) 0.4212(4) 0.7325(3) 0.080(2) Uani 1 1 d . . .
H40 H 0.8506 0.4509 0.7496 0.096 Uiso 1 1 calc R . .
C41 C 0.6513(5) 0.2306(3) 0.8233(3) 0.0457(13) Uani 1 1 d . . .
C42 C 1.1846(12) 0.6247(9) 0.5657(8) 0.067(4) Uani 0.50 1 d PU A 1
H42A H 1.2157 0.6741 0.5260 0.101 Uiso 0.50 1 calc PR A 1
H42B H 1.2418 0.5844 0.5605 0.101 Uiso 0.50 1 calc PR A 1
H42C H 1.1807 0.6228 0.6162 0.101 Uiso 0.50 1 calc PR A 1
C42' C 1.1307(14) 0.6532(9) 0.5828(9) 0.080(5) Uani 0.50 1 d PU A 2
H42D H 1.1635 0.7001 0.5393 0.121 Uiso 0.50 1 calc PR A 2
H42E H 1.2014 0.6192 0.6021 0.121 Uiso 0.50 1 calc PR A 2
H42F H 1.0802 0.6652 0.6233 0.121 Uiso 0.50 1 calc PR A 2
C43 C 1.000(2) 1.0338(12) -0.0064(12) 0.036(5) Uani 0.25 1 d PDU . 1
C43' C 1.0296(15) 0.9895(19) -0.0012(14) 0.037(5) Uani 0.25 1 d PDU . 2
C44 C 0.8486(12) 1.1670(8) -0.0093(9) 0.095(5) Uani 0.50 1 d PU . .


_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 O5 2.164(3) . ?
Zr1 O10 2.165(4) . ?
Zr1 O11 2.171(4) . ?
Zr1 O12 2.183(4) . ?
Zr1 O3 2.185(3) 2_576 ?
Zr1 O1 2.187(3) . ?
Zr1 O7 2.196(3) 2_666 ?
Zr1 O9 2.201(4) . ?
Zr1 Zr3 3.4966(15) 2_675 ?
Zr1 Zr2 3.5066(9) 2_675 ?
Zr1 Zr2 3.5078(17) . ?
Zr1 Zr3 3.5097(14) . ?
Zr2 O10 2.128(4) . ?
Zr2 O12 2.130(4) 2_675 ?
Zr2 O11 2.130(3) 2_675 ?
Zr2 O9 2.131(4) . ?
Zr2 O15 2.174(3) . ?
Zr2 O14 2.213(5) . ?
Zr2 O8 2.256(3) 1_564 ?
Zr2 O2 2.261(3) . ?
Zr2 Zr1 3.5066(9) 2_675 ?
Zr2 Zr3 3.5308(10) 2_675 ?
Zr2 Zr3 3.5361(12) . ?
Zr3 O12 2.132(4) 2_675 ?
Zr3 O11 2.133(3) . ?
Zr3 O10 2.134(3) 2_675 ?
Zr3 O9 2.137(4) . ?
Zr3 O13 2.158(3) . ?
Zr3 O16 2.214(4) . ?
Zr3 O4 2.273(3) 1_654 ?
Zr3 O6 2.292(3) . ?
Zr3 Zr1 3.4966(15) 2_675 ?
Zr3 Zr2 3.5308(10) 2_675 ?
O1 C13 1.252(6) . ?
O2 C13 1.261(5) . ?
O3 C20 1.255(5) . ?
O3 Zr1 2.185(3) 2_576 ?
O4 C20 1.263(5) . ?
O4 Zr3 2.273(3) 1_456 ?
O5 C34 1.279(5) . ?
O6 C34 1.251(5) . ?
O7 C41 1.238(6) . ?
O7 Zr1 2.196(3) 2_666 ?
O8 C41 1.259(6) . ?
O8 Zr2 2.256(3) 1_546 ?
O10 Zr3 2.134(3) 2_675 ?
O11 Zr2 2.130(3) 2_675 ?
O12 Zr2 2.130(4) 2_675 ?
O12 Zr3 2.132(4) 2_675 ?
O13 C43' 0.89(2) 2_775 ?
O13 C43 1.12(3) 2_775 ?
O13 C43' 1.375(17) . ?
O13 C43 1.381(16) . ?
O15 C44 1.137(11) . ?
C1 C2 1.381(6) . ?
C1 C6 1.396(7) . ?
C1 C7 1.482(7) . ?
C2 C3 1.380(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.389(7) . ?
C3 C14 1.490(6) . ?
C4 C5 1.373(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.381(7) . ?
C5 C21 1.526(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.372(7) . ?
C7 C12 1.413(6) . ?
C8 C9 1.380(7) . ?
C8 H8 0.9300 . ?
C9 C10 1.370(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.388(7) . ?
C10 C13 1.492(7) . ?
C11 C12 1.395(7) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C14 C15 1.381(6) . ?
C14 C19 1.395(6) . ?
C15 C16 1.397(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.370(6) . ?
C16 H16 0.9300 . ?
C17 C18 1.389(6) . ?
C17 C20 1.494(5) . ?
C18 C19 1.381(6) . ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 C23 1.361(6) . ?
C22 C27 1.386(7) . ?
C22 C28 1.459(6) . ?
C23 C24 1.373(6) . ?
C23 H23 0.9300 . ?
C24 C25 1.392(7) . ?
C24 C35 1.477(7) . ?
C25 C26 1.371(8) . ?
C25 H25 0.9300 . ?
C26 C27 1.374(7) . ?
C26 C42' 1.553(17) . ?
C26 C42 1.581(13) . ?
C27 H27 0.9300 . ?
C28 C29 1.381(6) . ?
C28 C33 1.397(6) . ?
C29 C30 1.377(6) . ?
C30 C31 1.395(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.371(6) . ?
C31 C34 1.477(6) . ?
C32 C33 1.378(6) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C35 C36 1.382(8) . ?
C35 C40 1.388(7) . ?
C36 C37 1.386(7) . ?
C36 H36 0.9300 . ?
C37 C38 1.371(7) . ?
C37 H37 0.9300 . ?
C38 C39 1.349(8) . ?
C38 C41 1.480(7) . ?
C39 C40 1.382(7) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C42' H42D 0.9600 . ?
C42' H42E 0.9600 . ?
C42' H42F 0.9600 . ?
C43 O13 1.12(3) 2_775 ?
C43 C43 1.21(4) 2_775 ?
C43' C43' 0.71(4) 2_775 ?
C43' O13 0.89(2) 2_775 ?

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
O5 Zr1 O10 141.81(12) . . ?
O5 Zr1 O11 78.24(13) . . ?
O10 Zr1 O11 108.65(18) . . ?
O5 Zr1 O12 141.99(14) . . ?
O10 Zr1 O12 70.62(16) . . ?
O11 Zr1 O12 70.09(14) . . ?
O5 Zr1 O3 118.53(11) . 2_576 ?
O10 Zr1 O3 79.69(15) . 2_576 ?
O11 Zr1 O3 142.08(12) . 2_576 ?
O12 Zr1 O3 78.84(13) . 2_576 ?
O5 Zr1 O1 76.02(12) . . ?
O10 Zr1 O1 77.58(14) . . ?
O11 Zr1 O1 142.74(11) . . ?
O12 Zr1 O1 141.62(13) . . ?
O3 Zr1 O1 74.77(12) 2_576 . ?
O5 Zr1 O7 74.55(12) . 2_666 ?
O10 Zr1 O7 143.32(12) . 2_666 ?
O11 Zr1 O7 78.12(14) . 2_666 ?
O12 Zr1 O7 78.76(14) . 2_666 ?
O3 Zr1 O7 74.90(13) 2_576 2_666 ?
O1 Zr1 O7 119.41(11) . 2_666 ?
O5 Zr1 O9 77.80(14) . . ?
O10 Zr1 O9 70.12(16) . . ?
O11 Zr1 O9 70.38(15) . . ?
O12 Zr1 O9 109.39(17) . . ?
O3 Zr1 O9 142.97(14) 2_576 . ?
O1 Zr1 O9 78.15(14) . . ?
O7 Zr1 O9 141.50(14) 2_666 . ?
O5 Zr1 Zr3 165.58(7) . 2_675 ?
O10 Zr1 Zr3 35.28(10) . 2_675 ?
O11 Zr1 Zr3 90.05(11) . 2_675 ?
O12 Zr1 Zr3 35.37(11) . 2_675 ?
O3 Zr1 Zr3 75.89(8) 2_576 2_675 ?
O1 Zr1 Zr3 110.00(8) . 2_675 ?
O7 Zr1 Zr3 111.53(8) 2_666 2_675 ?
O9 Zr1 Zr3 90.44(13) . 2_675 ?
O5 Zr1 Zr2 110.56(9) . 2_675 ?
O10 Zr1 Zr2 90.25(13) . 2_675 ?
O11 Zr1 Zr2 35.00(9) . 2_675 ?
O12 Zr1 Zr2 35.10(10) . 2_675 ?
O3 Zr1 Zr2 111.05(9) 2_576 2_675 ?
O1 Zr1 Zr2 165.54(8) . 2_675 ?
O7 Zr1 Zr2 75.05(9) 2_666 2_675 ?
O9 Zr1 Zr2 90.47(12) . 2_675 ?
Zr3 Zr1 Zr2 60.65(2) 2_675 2_675 ?
O5 Zr1 Zr2 110.53(8) . . ?
O10 Zr1 Zr2 34.86(10) . . ?
O11 Zr1 Zr2 90.01(12) . . ?
O12 Zr1 Zr2 90.34(12) . . ?
O3 Zr1 Zr2 111.82(9) 2_576 . ?
O1 Zr1 Zr2 74.56(8) . . ?
O7 Zr1 Zr2 166.02(9) 2_666 . ?
O9 Zr1 Zr2 35.27(11) . . ?
Zr3 Zr1 Zr2 60.54(3) 2_675 . ?
Zr2 Zr1 Zr2 90.99(3) 2_675 . ?
O5 Zr1 Zr3 74.72(8) . . ?
O10 Zr1 Zr3 89.86(13) . . ?
O11 Zr1 Zr3 35.01(10) . . ?
O12 Zr1 Zr3 90.05(10) . . ?
O3 Zr1 Zr3 166.74(7) 2_576 . ?
O1 Zr1 Zr3 111.14(7) . . ?
O7 Zr1 Zr3 110.27(9) 2_666 . ?
O9 Zr1 Zr3 35.38(11) . . ?
Zr3 Zr1 Zr3 90.86(3) 2_675 . ?
Zr2 Zr1 Zr3 60.43(2) 2_675 . ?
Zr2 Zr1 Zr3 60.52(3) . . ?
O10 Zr2 O12 108.4(2) . 2_675 ?
O10 Zr2 O11 68.21(14) . 2_675 ?
O12 Zr2 O11 71.87(15) 2_675 2_675 ?
O10 Zr2 O9 72.16(17) . . ?
O12 Zr2 O9 68.02(14) 2_675 . ?
O11 Zr2 O9 108.7(2) 2_675 . ?
O10 Zr2 O15 145.38(13) . . ?
O12 Zr2 O15 88.84(16) 2_675 . ?
O11 Zr2 O15 146.35(13) 2_675 . ?
O9 Zr2 O15 87.97(18) . . ?
O10 Zr2 O14 85.89(19) . . ?
O12 Zr2 O14 146.54(14) 2_675 . ?
O11 Zr2 O14 86.79(18) 2_675 . ?
O9 Zr2 O14 145.02(14) . . ?
O15 Zr2 O14 95.94(18) . . ?
O10 Zr2 O8 138.82(14) . 1_564 ?
O12 Zr2 O8 76.01(16) 2_675 1_564 ?
O11 Zr2 O8 75.13(15) 2_675 1_564 ?
O9 Zr2 O8 139.76(15) . 1_564 ?
O15 Zr2 O8 73.54(15) . 1_564 ?
O14 Zr2 O8 73.72(17) . 1_564 ?
O10 Zr2 O2 75.75(14) . . ?
O12 Zr2 O2 140.21(13) 2_675 . ?
O11 Zr2 O2 139.17(11) 2_675 . ?
O9 Zr2 O2 76.49(14) . . ?
O15 Zr2 O2 72.12(13) . . ?
O14 Zr2 O2 71.80(15) . . ?
O8 Zr2 O2 127.55(14) 1_564 . ?
O10 Zr2 Zr1 88.61(13) . 2_675 ?
O12 Zr2 Zr1 36.10(10) 2_675 2_675 ?
O11 Zr2 Zr1 35.78(10) 2_675 2_675 ?
O9 Zr2 Zr1 88.85(13) . 2_675 ?
O15 Zr2 Zr1 119.79(10) . 2_675 ?
O14 Zr2 Zr1 118.18(12) . 2_675 ?
O8 Zr2 Zr1 71.27(10) 1_564 2_675 ?
O2 Zr2 Zr1 161.15(9) . 2_675 ?
O10 Zr2 Zr1 35.56(12) . . ?
O12 Zr2 Zr1 88.71(12) 2_675 . ?
O11 Zr2 Zr1 88.37(12) 2_675 . ?
O9 Zr2 Zr1 36.61(11) . . ?
O15 Zr2 Zr1 119.27(11) . . ?
O14 Zr2 Zr1 116.81(12) . . ?
O8 Zr2 Zr1 160.25(10) 1_564 . ?
O2 Zr2 Zr1 72.16(9) . . ?
Zr1 Zr2 Zr1 89.01(3) 2_675 . ?
O10 Zr2 Zr3 34.11(10) . 2_675 ?
O12 Zr2 Zr3 90.35(12) 2_675 2_675 ?
O11 Zr2 Zr3 34.11(9) 2_675 2_675 ?
O9 Zr2 Zr3 90.68(14) . 2_675 ?
O15 Zr2 Zr3 178.61(11) . 2_675 ?
O14 Zr2 Zr3 85.36(14) . 2_675 ?
O8 Zr2 Zr3 107.35(11) 1_564 2_675 ?
O2 Zr2 Zr3 107.88(9) . 2_675 ?
Zr1 Zr2 Zr3 59.83(3) 2_675 2_675 ?
Zr1 Zr2 Zr3 59.57(3) . 2_675 ?
O10 Zr2 Zr3 89.76(15) . . ?
O12 Zr2 Zr3 33.94(10) 2_675 . ?
O11 Zr2 Zr3 89.66(12) 2_675 . ?
O9 Zr2 Zr3 34.10(10) . . ?
O15 Zr2 Zr3 88.83(12) . . ?
O14 Zr2 Zr3 175.18(14) . . ?
O8 Zr2 Zr3 108.50(12) 1_564 . ?
O2 Zr2 Zr3 109.14(9) . . ?
Zr1 Zr2 Zr3 59.53(3) 2_675 . ?
Zr1 Zr2 Zr3 59.77(3) . . ?
Zr3 Zr2 Zr3 89.87(3) 2_675 . ?
O12 Zr3 O11 108.49(17) 2_675 . ?
O12 Zr3 O10 72.21(17) 2_675 2_675 ?
O11 Zr3 O10 68.06(14) . 2_675 ?
O12 Zr3 O9 67.89(14) 2_675 . ?
O11 Zr3 O9 72.34(16) . . ?
O10 Zr3 O9 108.9(2) 2_675 . ?
O12 Zr3 O13 88.55(16) 2_675 . ?
O11 Zr3 O13 145.17(12) . . ?
O10 Zr3 O13 146.69(13) 2_675 . ?
O9 Zr3 O13 87.40(17) . . ?
O12 Zr3 O16 143.83(14) 2_675 . ?
O11 Zr3 O16 86.75(17) . . ?
O10 Zr3 O16 84.42(19) 2_675 . ?
O9 Zr3 O16 147.72(14) . . ?
O13 Zr3 O16 97.13(17) . . ?
O12 Zr3 O4 74.79(14) 2_675 1_654 ?
O11 Zr3 O4 140.95(14) . 1_654 ?
O10 Zr3 O4 76.75(14) 2_675 1_654 ?
O9 Zr3 O4 137.62(14) . 1_654 ?
O13 Zr3 O4 71.99(13) . 1_654 ?
O16 Zr3 O4 73.19(15) . 1_654 ?
O12 Zr3 O6 140.86(14) 2_675 . ?
O11 Zr3 O6 75.39(13) . . ?
O10 Zr3 O6 138.31(13) 2_675 . ?
O9 Zr3 O6 77.07(15) . . ?
O13 Zr3 O6 72.57(12) . . ?
O16 Zr3 O6 73.95(14) . . ?
O4 Zr3 O6 127.29(11) 1_654 . ?
O12 Zr3 Zr1 36.35(11) 2_675 2_675 ?
O11 Zr3 Zr1 88.63(11) . 2_675 ?
O10 Zr3 Zr1 35.88(12) 2_675 2_675 ?
O9 Zr3 Zr1 89.03(13) . 2_675 ?
O13 Zr3 Zr1 119.79(10) . 2_675 ?
O16 Zr3 Zr1 115.37(11) . 2_675 ?
O4 Zr3 Zr1 71.35(8) 1_654 2_675 ?
O6 Zr3 Zr1 161.32(7) . 2_675 ?
O12 Zr3 Zr1 88.63(11) 2_675 . ?
O11 Zr3 Zr1 35.73(11) . . ?
O10 Zr3 Zr1 88.44(13) 2_675 . ?
O9 Zr3 Zr1 36.61(11) . . ?
O13 Zr3 Zr1 118.75(9) . . ?
O16 Zr3 Zr1 118.57(11) . . ?
O4 Zr3 Zr1 160.42(8) 1_654 . ?
O6 Zr3 Zr1 72.26(8) . . ?
Zr1 Zr3 Zr1 89.14(3) 2_675 . ?
O12 Zr3 Zr2 90.57(12) 2_675 2_675 ?
O11 Zr3 Zr2 34.06(9) . 2_675 ?
O10 Zr3 Zr2 34.00(10) 2_675 2_675 ?
O9 Zr3 Zr2 90.90(14) . 2_675 ?
O13 Zr3 Zr2 178.28(11) . 2_675 ?
O16 Zr3 Zr2 84.45(13) . 2_675 ?
O4 Zr3 Zr2 109.19(9) 1_654 2_675 ?
O6 Zr3 Zr2 107.30(9) . 2_675 ?
Zr1 Zr3 Zr2 59.89(3) 2_675 2_675 ?
Zr1 Zr3 Zr2 59.74(2) . 2_675 ?
O12 Zr3 Zr2 33.90(10) 2_675 . ?
O11 Zr3 Zr2 89.88(12) . . ?
O10 Zr3 Zr2 89.97(15) 2_675 . ?
O9 Zr3 Zr2 34.00(10) . . ?
O13 Zr3 Zr2 88.31(11) . . ?
O16 Zr3 Zr2 174.23(12) . . ?
O4 Zr3 Zr2 106.90(10) 1_654 . ?
O6 Zr3 Zr2 109.71(10) . . ?
Zr1 Zr3 Zr2 59.81(3) 2_675 . ?
Zr1 Zr3 Zr2 59.72(3) . . ?
Zr2 Zr3 Zr2 90.13(3) 2_675 . ?
C13 O1 Zr1 133.7(3) . . ?
C13 O2 Zr2 133.6(3) . . ?
C20 O3 Zr1 131.9(3) . 2_576 ?
C20 O4 Zr3 134.6(3) . 1_456 ?
C34 O5 Zr1 134.4(3) . . ?
C34 O6 Zr3 132.9(3) . . ?
C41 O7 Zr1 133.0(3) . 2_666 ?
C41 O8 Zr2 135.6(4) . 1_546 ?
Zr2 O9 Zr3 111.90(16) . . ?
Zr2 O9 Zr1 108.12(19) . . ?
Zr3 O9 Zr1 108.0(2) . . ?
Zr2 O10 Zr3 111.89(17) . 2_675 ?
Zr2 O10 Zr1 109.58(19) . . ?
Zr3 O10 Zr1 108.8(2) 2_675 . ?
Zr2 O11 Zr3 111.84(15) 2_675 . ?
Zr2 O11 Zr1 109.21(15) 2_675 . ?
Zr3 O11 Zr1 109.26(18) . . ?
Zr2 O12 Zr3 112.16(15) 2_675 2_675 ?
Zr2 O12 Zr1 108.80(16) 2_675 . ?
Zr3 O12 Zr1 108.3(2) 2_675 . ?
C43' O13 C43 48.2(18) 2_775 2_775 ?
C43' O13 C43' 27(3) 2_775 . ?
C43 O13 C43' 21.2(19) 2_775 . ?
C43' O13 C43 9(3) 2_775 . ?
C43 O13 C43 56.9(19) 2_775 . ?
C43' O13 C43 35.7(11) . . ?
C43' O13 Zr3 156.6(16) 2_775 . ?
C43 O13 Zr3 130.3(11) 2_775 . ?
C43' O13 Zr3 148.0(13) . . ?
C43 O13 Zr3 155.4(9) . . ?
C44 O15 Zr2 145.9(9) . . ?
C2 C1 C6 116.8(4) . . ?
C2 C1 C7 119.9(4) . . ?
C6 C1 C7 123.2(4) . . ?
C3 C2 C1 122.1(5) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C2 C3 C4 119.3(4) . . ?
C2 C3 C14 121.0(4) . . ?
C4 C3 C14 119.7(4) . . ?
C5 C4 C3 120.4(5) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 119.0(5) . . ?
C4 C5 C21 119.7(5) . . ?
C6 C5 C21 121.3(4) . . ?
C5 C6 C1 122.4(4) . . ?
C5 C6 H6 118.8 . . ?
C1 C6 H6 118.8 . . ?
C8 C7 C12 116.9(5) . . ?
C8 C7 C1 121.2(4) . . ?
C12 C7 C1 121.9(5) . . ?
C7 C8 C9 122.4(4) . . ?
C7 C8 H8 118.8 . . ?
C9 C8 H8 118.8 . . ?
C10 C9 C8 121.0(5) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 118.6(5) . . ?
C9 C10 C13 120.3(5) . . ?
C11 C10 C13 121.1(4) . . ?
C10 C11 C12 120.5(4) . . ?
C10 C11 H11 119.8 . . ?
C12 C11 H11 119.8 . . ?
C11 C12 C7 120.7(5) . . ?
C11 C12 H12 119.7 . . ?
C7 C12 H12 119.7 . . ?
O1 C13 O2 125.4(4) . . ?
O1 C13 C10 115.7(4) . . ?
O2 C13 C10 118.9(5) . . ?
C15 C14 C19 118.0(4) . . ?
C15 C14 C3 121.0(4) . . ?
C19 C14 C3 121.1(4) . . ?
C14 C15 C16 121.2(4) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C17 C16 C15 120.3(4) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C16 C17 C18 119.1(4) . . ?
C16 C17 C20 120.1(4) . . ?
C18 C17 C20 120.8(4) . . ?
C19 C18 C17 120.6(4) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 C14 120.8(4) . . ?
C18 C19 H19 119.6 . . ?
C14 C19 H19 119.6 . . ?
O3 C20 O4 125.4(4) . . ?
O3 C20 C17 116.8(4) . . ?
O4 C20 C17 117.8(4) . . ?
C5 C21 H21A 109.5 . . ?
C5 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C5 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C27 117.1(4) . . ?
C23 C22 C28 122.3(5) . . ?
C27 C22 C28 120.3(4) . . ?
C22 C23 C24 123.3(5) . . ?
C22 C23 H23 118.3 . . ?
C24 C23 H23 118.3 . . ?
C23 C24 C25 117.5(5) . . ?
C23 C24 C35 122.8(5) . . ?
C25 C24 C35 119.8(4) . . ?
C26 C25 C24 121.4(5) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C25 C26 C27 118.3(6) . . ?
C25 C26 C42' 120.2(7) . . ?
C27 C26 C42' 119.2(7) . . ?
C25 C26 C42 117.0(7) . . ?
C27 C26 C42 121.8(7) . . ?
C42' C26 C42 32.1(7) . . ?
C26 C27 C22 122.3(5) . . ?
C26 C27 H27 118.8 . . ?
C22 C27 H27 118.8 . . ?
C29 C28 C33 116.9(4) . . ?
C29 C28 C22 121.1(4) . . ?
C33 C28 C22 122.0(4) . . ?
C30 C29 C28 121.1(4) . . ?
C29 C30 C31 121.3(4) . . ?
C29 C30 H30 119.4 . . ?
C31 C30 H30 119.4 . . ?
C32 C31 C30 118.0(4) . . ?
C32 C31 C34 121.9(4) . . ?
C30 C31 C34 120.1(4) . . ?
C31 C32 C33 120.5(4) . . ?
C31 C32 H32 119.7 . . ?
C33 C32 H32 119.7 . . ?
C32 C33 C28 122.0(4) . . ?
C32 C33 H33 119.0 . . ?
C28 C33 H33 119.0 . . ?
O6 C34 O5 125.1(4) . . ?
O6 C34 C31 119.8(4) . . ?
O5 C34 C31 115.1(4) . . ?
C36 C35 C40 115.9(5) . . ?
C36 C35 C24 121.3(5) . . ?
C40 C35 C24 122.7(5) . . ?
C35 C36 C37 121.9(5) . . ?
C35 C36 H36 119.1 . . ?
C37 C36 H36 119.1 . . ?
C38 C37 C36 120.8(5) . . ?
C38 C37 H37 119.6 . . ?
C36 C37 H37 119.6 . . ?
C39 C38 C37 118.2(5) . . ?
C39 C38 C41 121.1(5) . . ?
C37 C38 C41 120.6(5) . . ?
C38 C39 C40 121.6(5) . . ?
C38 C39 H39 119.2 . . ?
C40 C39 H39 119.2 . . ?
C39 C40 C35 121.6(6) . . ?
C39 C40 H40 119.2 . . ?
C35 C40 H40 119.2 . . ?
O7 C41 O8 125.1(4) . . ?
O7 C41 C38 117.5(4) . . ?
O8 C41 C38 117.3(5) . . ?
C26 C42 H42A 109.5 . . ?
C26 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C26 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C26 C42' H42D 109.5 . . ?
C26 C42' H42E 109.5 . . ?
H42D C42' H42E 109.5 . . ?
C26 C42' H42F 109.5 . . ?
H42D C42' H42F 109.5 . . ?
H42E C42' H42F 109.5 . . ?
O13 C43 C43 73(2) 2_775 2_775 ?
O13 C43 O13 123.1(19) 2_775 . ?
C43 C43 O13 50.5(14) 2_775 . ?
C43' C43' O13 118(7) 2_775 2_775 ?
C43' C43' O13 35(4) 2_775 . ?
O13 C43' O13 153(3) 2_775 . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        25.78
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         1.165
_refine_diff_density_min         -0.855
_refine_diff_density_rms         0.093
