# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# 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 1446514'
_audit_update_record             
;
2016-01-09 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H21 N O16 Zr3'
_chemical_formula_weight         1045.24

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           Orthorhombic
_symmetry_space_group_name_H-M   Immm
_symmetry_Hall_group_name_H-M    -I22

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   20.194(17)
_cell_length_b                   31.65(3)
_cell_length_c                   33.78(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     21590(33)
_cell_formula_units_Z            8
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    1639
_cell_measurement_theta_min      2.178
_cell_measurement_theta_max      20.377

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4128
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9460
_exptl_absorpt_correction_T_max  0.9815
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            81198
_diffrn_reflns_av_R_equivalents  0.2231
_diffrn_reflns_av_sigmaI/netI    0.2094
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.16
_reflns_number_total             10119
_reflns_number_gt                3282
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0670P)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         10119
_refine_ls_number_parameters     286
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.2322
_refine_ls_R_factor_gt           0.0648
_refine_ls_wR_factor_ref         0.1700
_refine_ls_wR_factor_gt          0.1358
_refine_ls_goodness_of_fit_ref   0.779
_refine_ls_restrained_S_all      0.802
_refine_ls_shift/su_max          0.003
_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 0.5000 0.284001(14) 0.427802(11) 0.06659(17) Uani 1 2 d S . .
Zr2 Zr 0.41259(3) 0.339721(13) 0.5000 0.07207(19) Uani 1 2 d S . .
Zr3 Zr 0.41388(3) 0.228746(13) 0.5000 0.0780(2) Uani 1 2 d S . .
O1 O 0.41245(13) 0.28450(7) 0.46512(6) 0.1001(9) Uani 1 1 d U . .
O2 O 0.5000 0.22934(10) 0.46480(9) 0.1007(14) Uani 1 2 d S . .
O3 O 0.5000 0.34035(12) 0.46456(8) 0.1232(16) Uani 1 2 d S . .
O4 O 0.38027(12) 0.20532(6) 0.44154(6) 0.0918(9) Uani 1 1 d U . .
O5 O 0.43298(12) 0.24163(6) 0.39477(5) 0.0790(9) Uani 1 1 d . . .
O6 O 0.06444(12) 0.17450(5) 0.10471(5) 0.0733(8) Uani 1 1 d . . .
O7 O 0.12350(13) 0.13798(6) 0.06072(5) 0.0925(10) Uani 1 1 d U . .
O8 O 0.4320(2) 0.16000(10) 0.5000 0.1078(13) Uani 1 2 d SU . .
O9 O 0.3035(2) 0.23288(11) 0.5000 0.1073(15) Uani 1 2 d S . .
O10 O 0.3032(2) 0.33539(11) 0.5000 0.1276(17) Uani 1 2 d SU . .
O11 O 0.41714(17) 0.40810(9) 0.5000 0.0852(12) Uani 1 2 d S . .
N1 N 0.2395(2) 0.0000 0.21434(9) 0.0822(15) Uani 1 2 d S . .
H1 H 0.2176 0.0000 0.1918 0.099 Uiso 1 2 calc SR . .
C1 C 0.3960(2) 0.21252(10) 0.40597(9) 0.0875(14) Uani 1 1 d . . .
C2 C 0.37173(19) 0.18327(9) 0.37466(9) 0.0780(12) Uani 1 1 d U . .
C3 C 0.34082(19) 0.14659(10) 0.38702(9) 0.0946(14) Uani 1 1 d . . .
H3 H 0.3347 0.1411 0.4144 0.114 Uiso 1 1 calc R . .
C4 C 0.31876(18) 0.11771(10) 0.35854(9) 0.0813(13) Uani 1 1 d U . .
H4 H 0.2975 0.0924 0.3668 0.098 Uiso 1 1 calc R . .
C5 C 0.3275(2) 0.12538(9) 0.31852(8) 0.0792(14) Uani 1 1 d . . .
C6 C 0.3533(2) 0.16225(10) 0.30765(9) 0.0941(15) Uani 1 1 d . . .
H6 H 0.3561 0.1691 0.2803 0.113 Uiso 1 1 calc R . .
C7 C 0.37650(18) 0.19101(10) 0.33558(9) 0.0840(13) Uani 1 1 d U . .
H7 H 0.3961 0.2167 0.3269 0.101 Uiso 1 1 calc R . .
C8 C 0.30392(19) 0.09480(9) 0.29060(8) 0.0817(13) Uani 1 1 d . . .
C9 C 0.31572(19) 0.05163(9) 0.29702(9) 0.0844(14) Uani 1 1 d . . .
H9 H 0.3387 0.0423 0.3200 0.101 Uiso 1 1 calc R . .
C10 C 0.29290(17) 0.02271(8) 0.26896(8) 0.0684(12) Uani 1 1 d . . .
C11 C 0.26005(17) 0.03436(9) 0.23550(8) 0.0691(12) Uani 1 1 d . . .
C12 C 0.24789(19) 0.07790(9) 0.22700(9) 0.0759(13) Uani 1 1 d . . .
C13 C 0.27254(18) 0.10689(9) 0.25557(9) 0.0768(13) Uani 1 1 d . . .
H13 H 0.2673 0.1362 0.2505 0.092 Uiso 1 1 calc R . .
C14 C 0.21353(18) 0.09357(9) 0.19294(8) 0.0739(13) Uani 1 1 d . . .
C15 C 0.22494(18) 0.07991(10) 0.15490(9) 0.0773(12) Uani 1 1 d U . .
H15 H 0.2564 0.0583 0.1498 0.093 Uiso 1 1 calc R . .
C16 C 0.18936(17) 0.09848(10) 0.12380(9) 0.0788(12) Uani 1 1 d U . .
H16 H 0.1979 0.0885 0.0978 0.095 Uiso 1 1 calc R . .
C17 C 0.14513(19) 0.12867(9) 0.12780(8) 0.0759(13) Uani 1 1 d . . .
C18 C 0.12976(19) 0.14190(11) 0.16757(9) 0.0904(14) Uani 1 1 d U . .
H18 H 0.0962 0.1622 0.1727 0.108 Uiso 1 1 calc R . .
C19 C 0.16672(19) 0.12340(10) 0.19850(9) 0.0901(15) Uani 1 1 d . . .
H19 H 0.1581 0.1325 0.2248 0.108 Uiso 1 1 calc R . .
C20 C 0.10804(18) 0.14896(10) 0.09626(9) 0.0753(13) 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
Zr1 O2 2.134(3) . ?
Zr1 O6 2.151(2) 13 ?
Zr1 O6 2.151(2) 7 ?
Zr1 O1 2.171(3) . ?
Zr1 O1 2.171(3) 11_655 ?
Zr1 O3 2.173(4) . ?
Zr1 O5 2.208(2) . ?
Zr1 O5 2.208(2) 11_655 ?
Zr1 Zr3 3.469(2) . ?
Zr1 Zr3 3.469(2) 11_655 ?
Zr1 Zr2 3.489(2) . ?
Zr1 Zr2 3.489(2) 11_655 ?
Zr2 O1 2.108(3) . ?
Zr2 O1 2.108(3) 10_556 ?
Zr2 O3 2.133(2) . ?
Zr2 O3 2.133(2) 10_556 ?
Zr2 O11 2.166(3) . ?
Zr2 O10 2.214(5) . ?
Zr2 O7 2.288(3) 13 ?
Zr2 O7 2.288(3) 6 ?
Zr2 Zr1 3.489(2) 10_556 ?
Zr2 Zr3 3.512(3) . ?
Zr2 Zr2 3.530(3) 11_655 ?
Zr3 O2 2.107(2) . ?
Zr3 O2 2.107(2) 10_556 ?
Zr3 O1 2.122(3) . ?
Zr3 O1 2.122(3) 10_556 ?
Zr3 O8 2.206(4) . ?
Zr3 O4 2.216(3) . ?
Zr3 O4 2.216(3) 10_556 ?
Zr3 O9 2.233(4) . ?
Zr3 Zr1 3.469(2) 10_556 ?
Zr3 Zr3 3.478(3) 11_655 ?
O2 Zr3 2.107(2) 11_655 ?
O3 Zr2 2.133(2) 11_655 ?
O4 C1 1.263(4) . ?
O5 C1 1.246(4) . ?
O6 C20 1.229(4) . ?
O6 Zr1 2.151(2) 13 ?
O7 C20 1.288(4) . ?
O7 Zr2 2.288(3) 13 ?
N1 C11 1.366(4) . ?
N1 C11 1.366(4) 12 ?
N1 H1 0.8800 . ?
C1 C2 1.488(4) . ?
C2 C7 1.346(4) . ?
C2 C3 1.383(4) . ?
C3 C4 1.400(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.330(4) . ?
C5 C8 1.433(4) . ?
C6 C7 1.392(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.396(4) . ?
C8 C9 1.404(4) . ?
C9 C10 1.396(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.361(4) . ?
C10 C10 1.437(5) 12 ?
C11 C12 1.429(4) . ?
C12 C13 1.422(4) . ?
C12 C14 1.432(4) . ?
C13 H13 0.9500 . ?
C14 C19 1.349(5) . ?
C14 C15 1.375(4) . ?
C15 C16 1.402(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.315(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.441(4) . ?
C17 C20 1.452(4) . ?
C18 C19 1.411(5) . ?
C18 H18 0.9500 . ?
C19 H19 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
O2 Zr1 O6 142.58(7) . 13 ?
O2 Zr1 O6 142.58(7) . 7 ?
O6 Zr1 O6 74.47(13) 13 7 ?
O2 Zr1 O1 70.49(8) . . ?
O6 Zr1 O1 78.42(10) 13 . ?
O6 Zr1 O1 141.69(9) 7 . ?
O2 Zr1 O1 70.49(8) . 11_655 ?
O6 Zr1 O1 141.69(9) 13 11_655 ?
O6 Zr1 O1 78.42(10) 7 11_655 ?
O1 Zr1 O1 109.02(14) . 11_655 ?
O2 Zr1 O3 109.31(14) . . ?
O6 Zr1 O3 77.91(10) 13 . ?
O6 Zr1 O3 77.91(10) 7 . ?
O1 Zr1 O3 70.26(8) . . ?
O1 Zr1 O3 70.26(8) 11_655 . ?
O2 Zr1 O5 78.67(10) . . ?
O6 Zr1 O5 75.05(10) 13 . ?
O6 Zr1 O5 118.93(9) 7 . ?
O1 Zr1 O5 78.39(10) . . ?
O1 Zr1 O5 142.84(9) 11_655 . ?
O3 Zr1 O5 141.92(7) . . ?
O2 Zr1 O5 78.67(10) . 11_655 ?
O6 Zr1 O5 118.93(9) 13 11_655 ?
O6 Zr1 O5 75.05(10) 7 11_655 ?
O1 Zr1 O5 142.84(9) . 11_655 ?
O1 Zr1 O5 78.39(10) 11_655 11_655 ?
O3 Zr1 O5 141.92(7) . 11_655 ?
O5 Zr1 O5 75.61(13) . 11_655 ?
O2 Zr1 Zr3 34.87(5) . . ?
O6 Zr1 Zr3 111.32(8) 13 . ?
O6 Zr1 Zr3 166.03(5) 7 . ?
O1 Zr1 Zr3 35.64(6) . . ?
O1 Zr1 Zr3 90.22(8) 11_655 . ?
O3 Zr1 Zr3 90.69(10) . . ?
O5 Zr1 Zr3 75.04(8) . . ?
O5 Zr1 Zr3 110.89(8) 11_655 . ?
O2 Zr1 Zr3 34.87(5) . 11_655 ?
O6 Zr1 Zr3 166.03(5) 13 11_655 ?
O6 Zr1 Zr3 111.32(8) 7 11_655 ?
O1 Zr1 Zr3 90.22(8) . 11_655 ?
O1 Zr1 Zr3 35.64(6) 11_655 11_655 ?
O3 Zr1 Zr3 90.69(10) . 11_655 ?
O5 Zr1 Zr3 110.89(8) . 11_655 ?
O5 Zr1 Zr3 75.04(8) 11_655 11_655 ?
Zr3 Zr1 Zr3 60.19(6) . 11_655 ?
O2 Zr1 Zr2 90.02(10) . . ?
O6 Zr1 Zr2 75.06(8) 13 . ?
O6 Zr1 Zr2 110.75(8) 7 . ?
O1 Zr1 Zr2 34.78(6) . . ?
O1 Zr1 Zr2 90.14(8) 11_655 . ?
O3 Zr1 Zr2 35.49(5) . . ?
O5 Zr1 Zr2 110.50(8) . . ?
O5 Zr1 Zr2 166.01(5) 11_655 . ?
Zr3 Zr1 Zr2 60.64(6) . . ?
Zr3 Zr1 Zr2 90.97(6) 11_655 . ?
O2 Zr1 Zr2 90.02(10) . 11_655 ?
O6 Zr1 Zr2 110.75(8) 13 11_655 ?
O6 Zr1 Zr2 75.06(8) 7 11_655 ?
O1 Zr1 Zr2 90.14(8) . 11_655 ?
O1 Zr1 Zr2 34.78(6) 11_655 11_655 ?
O3 Zr1 Zr2 35.49(5) . 11_655 ?
O5 Zr1 Zr2 166.01(5) . 11_655 ?
O5 Zr1 Zr2 110.50(8) 11_655 11_655 ?
Zr3 Zr1 Zr2 90.97(6) . 11_655 ?
Zr3 Zr1 Zr2 60.64(6) 11_655 11_655 ?
Zr2 Zr1 Zr2 60.78(6) . 11_655 ?
O1 Zr2 O1 67.98(13) . 10_556 ?
O1 Zr2 O3 72.25(12) . . ?
O1 Zr2 O3 108.82(12) 10_556 . ?
O1 Zr2 O3 108.82(13) . 10_556 ?
O1 Zr2 O3 72.25(12) 10_556 10_556 ?
O3 Zr2 O3 68.29(14) . 10_556 ?
O1 Zr2 O11 145.94(7) . . ?
O1 Zr2 O11 145.94(7) 10_556 . ?
O3 Zr2 O11 87.46(13) . . ?
O3 Zr2 O11 87.46(13) 10_556 . ?
O1 Zr2 O10 86.97(11) . . ?
O1 Zr2 O10 86.97(11) 10_556 . ?
O3 Zr2 O10 145.75(7) . . ?
O3 Zr2 O10 145.75(7) 10_556 . ?
O11 Zr2 O10 95.98(13) . . ?
O1 Zr2 O7 75.77(9) . 13 ?
O1 Zr2 O7 139.14(8) 10_556 13 ?
O3 Zr2 O7 75.97(11) . 13 ?
O3 Zr2 O7 139.80(10) 10_556 13 ?
O11 Zr2 O7 72.87(6) . 13 ?
O10 Zr2 O7 72.61(8) . 13 ?
O1 Zr2 O7 139.14(8) . 6 ?
O1 Zr2 O7 75.77(9) 10_556 6 ?
O3 Zr2 O7 139.80(10) . 6 ?
O3 Zr2 O7 75.97(11) 10_556 6 ?
O11 Zr2 O7 72.87(6) . 6 ?
O10 Zr2 O7 72.61(8) . 6 ?
O7 Zr2 O7 127.36(12) 13 6 ?
O1 Zr2 Zr1 35.99(7) . . ?
O1 Zr2 Zr1 88.42(9) 10_556 . ?
O3 Zr2 Zr1 36.26(10) . . ?
O3 Zr2 Zr1 88.76(10) 10_556 . ?
O11 Zr2 Zr1 118.92(7) . . ?
O10 Zr2 Zr1 118.27(6) . . ?
O7 Zr2 Zr1 71.97(8) 13 . ?
O7 Zr2 Zr1 160.66(6) 6 . ?
O1 Zr2 Zr1 88.42(9) . 10_556 ?
O1 Zr2 Zr1 35.99(7) 10_556 10_556 ?
O3 Zr2 Zr1 88.76(10) . 10_556 ?
O3 Zr2 Zr1 36.26(10) 10_556 10_556 ?
O11 Zr2 Zr1 118.92(7) . 10_556 ?
O10 Zr2 Zr1 118.27(6) . 10_556 ?
O7 Zr2 Zr1 160.66(6) 13 10_556 ?
O7 Zr2 Zr1 71.97(8) 6 10_556 ?
Zr1 Zr2 Zr1 88.69(6) . 10_556 ?
O1 Zr2 Zr3 33.99(7) . . ?
O1 Zr2 Zr3 33.99(7) 10_556 . ?
O3 Zr2 Zr3 90.18(10) . . ?
O3 Zr2 Zr3 90.18(10) 10_556 . ?
O11 Zr2 Zr3 177.15(10) . . ?
O10 Zr2 Zr3 86.87(9) . . ?
O7 Zr2 Zr3 108.10(6) 13 . ?
O7 Zr2 Zr3 108.10(5) 6 . ?
Zr1 Zr2 Zr3 59.39(3) . . ?
Zr1 Zr2 Zr3 59.39(3) 10_556 . ?
O1 Zr2 Zr2 90.08(7) . 11_655 ?
O1 Zr2 Zr2 90.08(7) 10_556 11_655 ?
O3 Zr2 Zr2 34.15(7) . 11_655 ?
O3 Zr2 Zr2 34.15(7) 10_556 11_655 ?
O11 Zr2 Zr2 87.57(9) . 11_655 ?
O10 Zr2 Zr2 176.45(9) . 11_655 ?
O7 Zr2 Zr2 108.57(7) 13 11_655 ?
O7 Zr2 Zr2 108.57(7) 6 11_655 ?
Zr1 Zr2 Zr2 59.61(3) . 11_655 ?
Zr1 Zr2 Zr2 59.61(3) 10_556 11_655 ?
Zr3 Zr2 Zr2 89.578(15) . 11_655 ?
O2 Zr3 O2 68.72(15) . 10_556 ?
O2 Zr3 O1 71.97(11) . . ?
O2 Zr3 O1 108.50(12) 10_556 . ?
O2 Zr3 O1 108.50(12) . 10_556 ?
O2 Zr3 O1 71.97(11) 10_556 10_556 ?
O1 Zr3 O1 67.46(13) . 10_556 ?
O2 Zr3 O8 82.62(12) . . ?
O2 Zr3 O8 82.62(12) 10_556 . ?
O1 Zr3 O8 145.31(7) . . ?
O1 Zr3 O8 145.31(7) 10_556 . ?
O2 Zr3 O4 75.69(11) . . ?
O2 Zr3 O4 139.35(10) 10_556 . ?
O1 Zr3 O4 77.25(10) . . ?
O1 Zr3 O4 140.26(9) 10_556 . ?
O8 Zr3 O4 73.80(7) . . ?
O2 Zr3 O4 139.35(10) . 10_556 ?
O2 Zr3 O4 75.69(11) 10_556 10_556 ?
O1 Zr3 O4 140.26(9) . 10_556 ?
O1 Zr3 O4 77.25(10) 10_556 10_556 ?
O8 Zr3 O4 73.80(7) . 10_556 ?
O4 Zr3 O4 126.05(13) . 10_556 ?
O2 Zr3 O9 145.44(8) . . ?
O2 Zr3 O9 145.44(8) 10_556 . ?
O1 Zr3 O9 86.43(10) . . ?
O1 Zr3 O9 86.43(10) 10_556 . ?
O8 Zr3 O9 102.93(14) . . ?
O4 Zr3 O9 73.37(8) . . ?
O4 Zr3 O9 73.37(8) 10_556 . ?
O2 Zr3 Zr1 35.39(8) . . ?
O2 Zr3 Zr1 88.77(10) 10_556 . ?
O1 Zr3 Zr1 36.60(7) . . ?
O1 Zr3 Zr1 88.74(9) 10_556 . ?
O8 Zr3 Zr1 114.44(8) . . ?
O4 Zr3 Zr1 72.28(8) . . ?
O4 Zr3 Zr1 161.60(6) 10_556 . ?
O9 Zr3 Zr1 118.10(6) . . ?
O2 Zr3 Zr1 88.77(10) . 10_556 ?
O2 Zr3 Zr1 35.39(8) 10_556 10_556 ?
O1 Zr3 Zr1 88.74(9) . 10_556 ?
O1 Zr3 Zr1 36.60(7) 10_556 10_556 ?
O8 Zr3 Zr1 114.44(8) . 10_556 ?
O4 Zr3 Zr1 161.60(6) . 10_556 ?
O4 Zr3 Zr1 72.28(8) 10_556 10_556 ?
O9 Zr3 Zr1 118.10(6) . 10_556 ?
Zr1 Zr3 Zr1 89.36(6) . 10_556 ?
O2 Zr3 Zr3 34.36(8) . 11_655 ?
O2 Zr3 Zr3 34.36(8) 10_556 11_655 ?
O1 Zr3 Zr3 90.78(7) . 11_655 ?
O1 Zr3 Zr3 90.78(7) 10_556 11_655 ?
O8 Zr3 Zr3 80.43(11) . 11_655 ?
O4 Zr3 Zr3 107.83(7) . 11_655 ?
O4 Zr3 Zr3 107.83(7) 10_556 11_655 ?
O9 Zr3 Zr3 176.64(9) . 11_655 ?
Zr1 Zr3 Zr3 59.91(3) . 11_655 ?
Zr1 Zr3 Zr3 59.91(3) 10_556 11_655 ?
O2 Zr3 Zr2 89.84(9) . . ?
O2 Zr3 Zr2 89.84(9) 10_556 . ?
O1 Zr3 Zr2 33.73(7) . . ?
O1 Zr3 Zr2 33.73(7) 10_556 . ?
O8 Zr3 Zr2 170.85(11) . . ?
O4 Zr3 Zr2 109.41(6) . . ?
O4 Zr3 Zr2 109.41(6) 10_556 . ?
O9 Zr3 Zr2 86.22(9) . . ?
Zr1 Zr3 Zr2 59.97(3) . . ?
Zr1 Zr3 Zr2 59.97(3) 10_556 . ?
Zr3 Zr3 Zr2 90.422(15) 11_655 . ?
Zr2 O1 Zr3 112.28(11) . . ?
Zr2 O1 Zr1 109.23(11) . . ?
Zr3 O1 Zr1 107.77(11) . . ?
Zr3 O2 Zr3 111.27(15) . 11_655 ?
Zr3 O2 Zr1 109.73(10) . . ?
Zr3 O2 Zr1 109.73(10) 11_655 . ?
Zr2 O3 Zr2 111.70(14) . 11_655 ?
Zr2 O3 Zr1 108.25(12) . . ?
Zr2 O3 Zr1 108.25(12) 11_655 . ?
C1 O4 Zr3 135.3(2) . . ?
C1 O5 Zr1 131.59(19) . . ?
C20 O6 Zr1 135.79(19) . 13 ?
C20 O7 Zr2 132.5(2) . 13 ?
C11 N1 C11 105.5(3) . 12 ?
C11 N1 H1 127.3 . . ?
C11 N1 H1 127.3 12 . ?
O5 C1 O4 124.9(3) . . ?
O5 C1 C2 116.2(3) . . ?
O4 C1 C2 118.8(3) . . ?
C7 C2 C3 118.8(3) . . ?
C7 C2 C1 124.1(3) . . ?
C3 C2 C1 117.1(3) . . ?
C2 C3 C4 119.0(3) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 121.1(3) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C6 C5 C4 118.3(3) . . ?
C6 C5 C8 122.8(3) . . ?
C4 C5 C8 118.8(3) . . ?
C5 C6 C7 121.2(3) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C2 C7 C6 121.4(3) . . ?
C2 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C13 C8 C9 118.4(3) . . ?
C13 C8 C5 121.6(3) . . ?
C9 C8 C5 120.0(3) . . ?
C10 C9 C8 118.5(3) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C11 C10 C9 123.2(3) . . ?
C11 C10 C10 105.72(16) . 12 ?
C9 C10 C10 130.97(17) . 12 ?
C10 C11 N1 111.5(3) . . ?
C10 C11 C12 120.8(3) . . ?
N1 C11 C12 127.6(3) . . ?
C13 C12 C11 115.2(3) . . ?
C13 C12 C14 119.4(3) . . ?
C11 C12 C14 125.4(3) . . ?
C8 C13 C12 123.9(3) . . ?
C8 C13 H13 118.1 . . ?
C12 C13 H13 118.1 . . ?
C19 C14 C15 117.9(3) . . ?
C19 C14 C12 118.0(3) . . ?
C15 C14 C12 124.1(3) . . ?
C14 C15 C16 118.9(3) . . ?
C14 C15 H15 120.6 . . ?
C16 C15 H15 120.6 . . ?
C17 C16 C15 125.1(3) . . ?
C17 C16 H16 117.4 . . ?
C15 C16 H16 117.4 . . ?
C16 C17 C18 117.0(3) . . ?
C16 C17 C20 126.6(3) . . ?
C18 C17 C20 116.4(3) . . ?
C19 C18 C17 117.1(3) . . ?
C19 C18 H18 121.4 . . ?
C17 C18 H18 121.4 . . ?
C14 C19 C18 123.9(3) . . ?
C14 C19 H19 118.0 . . ?
C18 C19 H19 118.0 . . ?
O6 C20 O7 124.6(3) . . ?
O6 C20 C17 119.4(3) . . ?
O7 C20 C17 116.1(3) . . ?

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
O2 Zr1 Zr2 O1 -54.12(12) . . . . ?
O6 Zr1 Zr2 O1 91.16(13) 13 . . . ?
O6 Zr1 Zr2 O1 157.73(12) 7 . . . ?
O1 Zr1 Zr2 O1 -124.60(16) 11_655 . . . ?
O3 Zr1 Zr2 O1 -178.79(17) . . . . ?
O5 Zr1 Zr2 O1 23.79(12) . . . . ?
O5 Zr1 Zr2 O1 -90.0(3) 11_655 . . . ?
Zr3 Zr1 Zr2 O1 -34.43(11) . . . . ?
Zr3 Zr1 Zr2 O1 -88.98(12) 11_655 . . . ?
Zr2 Zr1 Zr2 O1 -144.13(11) 11_655 . . . ?
O2 Zr1 Zr2 O1 -1.01(8) . . . 10_556 ?
O6 Zr1 Zr2 O1 144.26(9) 13 . . 10_556 ?
O6 Zr1 Zr2 O1 -149.16(10) 7 . . 10_556 ?
O1 Zr1 Zr2 O1 53.11(12) . . . 10_556 ?
O1 Zr1 Zr2 O1 -71.50(10) 11_655 . . 10_556 ?
O3 Zr1 Zr2 O1 -125.69(15) . . . 10_556 ?
O5 Zr1 Zr2 O1 76.90(10) . . . 10_556 ?
O5 Zr1 Zr2 O1 -36.9(3) 11_655 . . 10_556 ?
Zr3 Zr1 Zr2 O1 18.67(7) . . . 10_556 ?
Zr3 Zr1 Zr2 O1 -35.87(7) 11_655 . . 10_556 ?
Zr2 Zr1 Zr2 O1 -91.02(8) 11_655 . . 10_556 ?
O2 Zr1 Zr2 O3 124.68(14) . . . . ?
O6 Zr1 Zr2 O3 -90.05(15) 13 . . . ?
O6 Zr1 Zr2 O3 -23.47(15) 7 . . . ?
O1 Zr1 Zr2 O3 178.79(17) . . . . ?
O1 Zr1 Zr2 O3 54.19(15) 11_655 . . . ?
O5 Zr1 Zr2 O3 -157.42(14) . . . . ?
O5 Zr1 Zr2 O3 88.8(3) 11_655 . . . ?
Zr3 Zr1 Zr2 O3 144.36(13) . . . . ?
Zr3 Zr1 Zr2 O3 89.82(14) 11_655 . . . ?
Zr2 Zr1 Zr2 O3 34.66(13) 11_655 . . . ?
O2 Zr1 Zr2 O3 71.26(11) . . . 10_556 ?
O6 Zr1 Zr2 O3 -143.47(11) 13 . . 10_556 ?
O6 Zr1 Zr2 O3 -76.89(12) 7 . . 10_556 ?
O1 Zr1 Zr2 O3 125.38(14) . . . 10_556 ?
O1 Zr1 Zr2 O3 0.77(11) 11_655 . . 10_556 ?
O3 Zr1 Zr2 O3 -53.41(13) . . . 10_556 ?
O5 Zr1 Zr2 O3 149.17(11) . . . 10_556 ?
O5 Zr1 Zr2 O3 35.4(3) 11_655 . . 10_556 ?
Zr3 Zr1 Zr2 O3 90.94(10) . . . 10_556 ?
Zr3 Zr1 Zr2 O3 36.40(10) 11_655 . . 10_556 ?
Zr2 Zr1 Zr2 O3 -18.75(10) 11_655 . . 10_556 ?
O2 Zr1 Zr2 O11 157.67(10) . . . . ?
O6 Zr1 Zr2 O11 -57.06(11) 13 . . . ?
O6 Zr1 Zr2 O11 9.52(11) 7 . . . ?
O1 Zr1 Zr2 O11 -148.21(14) . . . . ?
O1 Zr1 Zr2 O11 87.18(11) 11_655 . . . ?
O3 Zr1 Zr2 O11 32.99(16) . . . . ?
O5 Zr1 Zr2 O11 -124.42(11) . . . . ?
O5 Zr1 Zr2 O11 121.8(3) 11_655 . . . ?
Zr3 Zr1 Zr2 O11 177.35(9) . . . . ?
Zr3 Zr1 Zr2 O11 122.81(10) 11_655 . . . ?
Zr2 Zr1 Zr2 O11 67.66(9) 11_655 . . . ?
O2 Zr1 Zr2 O10 -86.72(10) . . . . ?
O6 Zr1 Zr2 O10 58.55(11) 13 . . . ?
O6 Zr1 Zr2 O10 125.13(11) 7 . . . ?
O1 Zr1 Zr2 O10 -32.60(13) . . . . ?
O1 Zr1 Zr2 O10 -157.21(10) 11_655 . . . ?
O3 Zr1 Zr2 O10 148.61(16) . . . . ?
O5 Zr1 Zr2 O10 -8.81(10) . . . . ?
O5 Zr1 Zr2 O10 -122.6(3) 11_655 . . . ?
Zr3 Zr1 Zr2 O10 -67.04(9) . . . . ?
Zr3 Zr1 Zr2 O10 -121.58(9) 11_655 . . . ?
Zr2 Zr1 Zr2 O10 -176.73(8) 11_655 . . . ?
O2 Zr1 Zr2 O7 -144.59(8) . . . 13 ?
O6 Zr1 Zr2 O7 0.68(9) 13 . . 13 ?
O6 Zr1 Zr2 O7 67.26(10) 7 . . 13 ?
O1 Zr1 Zr2 O7 -90.47(13) . . . 13 ?
O1 Zr1 Zr2 O7 144.92(9) 11_655 . . 13 ?
O3 Zr1 Zr2 O7 90.73(15) . . . 13 ?
O5 Zr1 Zr2 O7 -66.68(9) . . . 13 ?
O5 Zr1 Zr2 O7 179.6(3) 11_655 . . 13 ?
Zr3 Zr1 Zr2 O7 -124.91(7) . . . 13 ?
Zr3 Zr1 Zr2 O7 -179.45(6) 11_655 . . 13 ?
Zr2 Zr1 Zr2 O7 125.40(7) 11_655 . . 13 ?
O2 Zr1 Zr2 O7 33.8(2) . . . 6 ?
O6 Zr1 Zr2 O7 179.1(2) 13 . . 6 ?
O6 Zr1 Zr2 O7 -114.4(2) 7 . . 6 ?
O1 Zr1 Zr2 O7 87.9(2) . . . 6 ?
O1 Zr1 Zr2 O7 -36.7(2) 11_655 . . 6 ?
O3 Zr1 Zr2 O7 -90.9(2) . . . 6 ?
O5 Zr1 Zr2 O7 111.7(2) . . . 6 ?
O5 Zr1 Zr2 O7 -2.1(3) 11_655 . . 6 ?
Zr3 Zr1 Zr2 O7 53.47(19) . . . 6 ?
Zr3 Zr1 Zr2 O7 -1.07(19) 11_655 . . 6 ?
Zr2 Zr1 Zr2 O7 -56.2(2) 11_655 . . 6 ?
O2 Zr1 Zr2 Zr1 34.99(5) . . . 10_556 ?
O6 Zr1 Zr2 Zr1 -179.74(6) 13 . . 10_556 ?
O6 Zr1 Zr2 Zr1 -113.16(8) 7 . . 10_556 ?
O1 Zr1 Zr2 Zr1 89.11(12) . . . 10_556 ?
O1 Zr1 Zr2 Zr1 -35.50(7) 11_655 . . 10_556 ?
O3 Zr1 Zr2 Zr1 -89.69(14) . . . 10_556 ?
O5 Zr1 Zr2 Zr1 112.90(7) . . . 10_556 ?
O5 Zr1 Zr2 Zr1 -0.9(2) 11_655 . . 10_556 ?
Zr3 Zr1 Zr2 Zr1 54.67(4) . . . 10_556 ?
Zr3 Zr1 Zr2 Zr1 0.130(16) 11_655 . . 10_556 ?
Zr2 Zr1 Zr2 Zr1 -55.02(4) 11_655 . . 10_556 ?
O2 Zr1 Zr2 Zr3 -19.68(5) . . . . ?
O6 Zr1 Zr2 Zr3 125.59(7) 13 . . . ?
O6 Zr1 Zr2 Zr3 -167.83(6) 7 . . . ?
O1 Zr1 Zr2 Zr3 34.43(11) . . . . ?
O1 Zr1 Zr2 Zr3 -90.17(7) 11_655 . . . ?
O3 Zr1 Zr2 Zr3 -144.36(13) . . . . ?
O5 Zr1 Zr2 Zr3 58.23(6) . . . . ?
O5 Zr1 Zr2 Zr3 -55.5(2) 11_655 . . . ?
Zr3 Zr1 Zr2 Zr3 -54.54(4) 11_655 . . . ?
Zr2 Zr1 Zr2 Zr3 -109.70(3) 11_655 . . . ?
O2 Zr1 Zr2 Zr2 90.01(6) . . . 11_655 ?
O6 Zr1 Zr2 Zr2 -124.71(7) 13 . . 11_655 ?
O6 Zr1 Zr2 Zr2 -58.14(7) 7 . . 11_655 ?
O1 Zr1 Zr2 Zr2 144.13(11) . . . 11_655 ?
O1 Zr1 Zr2 Zr2 19.53(6) 11_655 . . 11_655 ?
O3 Zr1 Zr2 Zr2 -34.66(13) . . . 11_655 ?
O5 Zr1 Zr2 Zr2 167.92(5) . . . 11_655 ?
O5 Zr1 Zr2 Zr2 54.2(2) 11_655 . . 11_655 ?
Zr3 Zr1 Zr2 Zr2 109.70(3) . . . 11_655 ?
Zr3 Zr1 Zr2 Zr2 55.15(4) 11_655 . . 11_655 ?
O6 Zr1 Zr3 O2 158.58(14) 13 . . . ?
O6 Zr1 Zr3 O2 -89.2(3) 7 . . . ?
O1 Zr1 Zr3 O2 -177.52(17) . . . . ?
O1 Zr1 Zr3 O2 -53.87(15) 11_655 . . . ?
O3 Zr1 Zr3 O2 -124.14(14) . . . . ?
O5 Zr1 Zr3 O2 91.60(15) . . . . ?
O5 Zr1 Zr3 O2 23.77(15) 11_655 . . . ?
Zr3 Zr1 Zr3 O2 -33.74(13) 11_655 . . . ?
Zr2 Zr1 Zr3 O2 -143.91(13) . . . . ?
Zr2 Zr1 Zr3 O2 -88.64(14) 11_655 . . . ?
O2 Zr1 Zr3 O2 53.38(14) . . . 10_556 ?
O6 Zr1 Zr3 O2 -148.04(10) 13 . . 10_556 ?
O6 Zr1 Zr3 O2 -35.8(3) 7 . . 10_556 ?
O1 Zr1 Zr3 O2 -124.14(14) . . . 10_556 ?
O1 Zr1 Zr3 O2 -0.49(10) 11_655 . . 10_556 ?
O3 Zr1 Zr3 O2 -70.76(10) . . . 10_556 ?
O5 Zr1 Zr3 O2 144.98(10) . . . 10_556 ?
O5 Zr1 Zr3 O2 77.15(11) 11_655 . . 10_556 ?
Zr3 Zr1 Zr3 O2 19.64(8) 11_655 . . 10_556 ?
Zr2 Zr1 Zr3 O2 -90.53(9) . . . 10_556 ?
Zr2 Zr1 Zr3 O2 -35.26(8) 11_655 . . 10_556 ?
O2 Zr1 Zr3 O1 177.52(17) . . . . ?
O6 Zr1 Zr3 O1 -23.89(12) 13 . . . ?
O6 Zr1 Zr3 O1 88.4(3) 7 . . . ?
O1 Zr1 Zr3 O1 123.65(16) 11_655 . . . ?
O3 Zr1 Zr3 O1 53.39(12) . . . . ?
O5 Zr1 Zr3 O1 -90.87(13) . . . . ?
O5 Zr1 Zr3 O1 -158.70(12) 11_655 . . . ?
Zr3 Zr1 Zr3 O1 143.79(11) 11_655 . . . ?
Zr2 Zr1 Zr3 O1 33.61(11) . . . . ?
Zr2 Zr1 Zr3 O1 88.88(12) 11_655 . . . ?
O2 Zr1 Zr3 O1 125.37(15) . . . 10_556 ?
O6 Zr1 Zr3 O1 -76.05(9) 13 . . 10_556 ?
O6 Zr1 Zr3 O1 36.2(3) 7 . . 10_556 ?
O1 Zr1 Zr3 O1 -52.15(11) . . . 10_556 ?
O1 Zr1 Zr3 O1 71.50(10) 11_655 . . 10_556 ?
O3 Zr1 Zr3 O1 1.24(8) . . . 10_556 ?
O5 Zr1 Zr3 O1 -143.03(9) . . . 10_556 ?
O5 Zr1 Zr3 O1 149.14(10) 11_655 . . 10_556 ?
Zr3 Zr1 Zr3 O1 91.63(8) 11_655 . . 10_556 ?
Zr2 Zr1 Zr3 O1 -18.54(7) . . . 10_556 ?
Zr2 Zr1 Zr3 O1 36.73(7) 11_655 . . 10_556 ?
O2 Zr1 Zr3 O8 -27.93(16) . . . . ?
O6 Zr1 Zr3 O8 130.65(11) 13 . . . ?
O6 Zr1 Zr3 O8 -117.1(3) 7 . . . ?
O1 Zr1 Zr3 O8 154.54(14) . . . . ?
O1 Zr1 Zr3 O8 -81.81(11) 11_655 . . . ?
O3 Zr1 Zr3 O8 -152.07(10) . . . . ?
O5 Zr1 Zr3 O8 63.67(12) . . . . ?
O5 Zr1 Zr3 O8 -4.16(11) 11_655 . . . ?
Zr3 Zr1 Zr3 O8 -61.67(9) 11_655 . . . ?
Zr2 Zr1 Zr3 O8 -171.84(9) . . . . ?
Zr2 Zr1 Zr3 O8 -116.58(10) 11_655 . . . ?
O2 Zr1 Zr3 O4 -90.10(15) . . . . ?
O6 Zr1 Zr3 O4 68.49(9) 13 . . . ?
O6 Zr1 Zr3 O4 -179.3(2) 7 . . . ?
O1 Zr1 Zr3 O4 92.38(13) . . . . ?
O1 Zr1 Zr3 O4 -143.97(9) 11_655 . . . ?
O3 Zr1 Zr3 O4 145.77(8) . . . . ?
O5 Zr1 Zr3 O4 1.51(9) . . . . ?
O5 Zr1 Zr3 O4 -66.32(10) 11_655 . . . ?
Zr3 Zr1 Zr3 O4 -123.83(8) 11_655 . . . ?
Zr2 Zr1 Zr3 O4 125.99(8) . . . . ?
Zr2 Zr1 Zr3 O4 -178.74(7) 11_655 . . . ?
O2 Zr1 Zr3 O4 85.4(2) . . . 10_556 ?
O6 Zr1 Zr3 O4 -116.1(2) 13 . . 10_556 ?
O6 Zr1 Zr3 O4 -3.8(3) 7 . . 10_556 ?
O1 Zr1 Zr3 O4 -92.2(2) . . . 10_556 ?
O1 Zr1 Zr3 O4 31.5(2) 11_655 . . 10_556 ?
O3 Zr1 Zr3 O4 -38.8(2) . . . 10_556 ?
O5 Zr1 Zr3 O4 177.0(2) . . . 10_556 ?
O5 Zr1 Zr3 O4 109.1(2) 11_655 . . 10_556 ?
Zr3 Zr1 Zr3 O4 51.6(2) 11_655 . . 10_556 ?
Zr2 Zr1 Zr3 O4 -58.5(2) . . . 10_556 ?
Zr2 Zr1 Zr3 O4 -3.3(2) 11_655 . . 10_556 ?
O2 Zr1 Zr3 O9 -149.36(15) . . . . ?
O6 Zr1 Zr3 O9 9.23(10) 13 . . . ?
O6 Zr1 Zr3 O9 121.5(3) 7 . . . ?
O1 Zr1 Zr3 O9 33.12(13) . . . . ?
O1 Zr1 Zr3 O9 156.77(10) 11_655 . . . ?
O3 Zr1 Zr3 O9 86.51(10) . . . . ?
O5 Zr1 Zr3 O9 -57.75(11) . . . . ?
O5 Zr1 Zr3 O9 -125.58(10) 11_655 . . . ?
Zr3 Zr1 Zr3 O9 176.91(8) 11_655 . . . ?
Zr2 Zr1 Zr3 O9 66.73(8) . . . . ?
Zr2 Zr1 Zr3 O9 122.00(9) 11_655 . . . ?
O2 Zr1 Zr3 Zr1 88.77(14) . . . 10_556 ?
O6 Zr1 Zr3 Zr1 -112.64(7) 13 . . 10_556 ?
O6 Zr1 Zr3 Zr1 -0.4(2) 7 . . 10_556 ?
O1 Zr1 Zr3 Zr1 -88.75(12) . . . 10_556 ?
O1 Zr1 Zr3 Zr1 34.90(7) 11_655 . . 10_556 ?
O3 Zr1 Zr3 Zr1 -35.36(5) . . . 10_556 ?
O5 Zr1 Zr3 Zr1 -179.62(6) . . . 10_556 ?
O5 Zr1 Zr3 Zr1 112.55(8) 11_655 . . 10_556 ?
Zr3 Zr1 Zr3 Zr1 55.04(4) 11_655 . . 10_556 ?
Zr2 Zr1 Zr3 Zr1 -55.14(4) . . . 10_556 ?
Zr2 Zr1 Zr3 Zr1 0.131(16) 11_655 . . 10_556 ?
O2 Zr1 Zr3 Zr3 33.74(13) . . . 11_655 ?
O6 Zr1 Zr3 Zr3 -167.68(5) 13 . . 11_655 ?
O6 Zr1 Zr3 Zr3 -55.4(2) 7 . . 11_655 ?
O1 Zr1 Zr3 Zr3 -143.79(11) . . . 11_655 ?
O1 Zr1 Zr3 Zr3 -20.13(6) 11_655 . . 11_655 ?
O3 Zr1 Zr3 Zr3 -90.40(6) . . . 11_655 ?
O5 Zr1 Zr3 Zr3 125.34(7) . . . 11_655 ?
O5 Zr1 Zr3 Zr3 57.51(7) 11_655 . . 11_655 ?
Zr2 Zr1 Zr3 Zr3 -110.17(3) . . . 11_655 ?
Zr2 Zr1 Zr3 Zr3 -54.91(4) 11_655 . . 11_655 ?
O2 Zr1 Zr3 Zr2 143.91(13) . . . . ?
O6 Zr1 Zr3 Zr2 -57.51(6) 13 . . . ?
O6 Zr1 Zr3 Zr2 54.7(2) 7 . . . ?
O1 Zr1 Zr3 Zr2 -33.61(11) . . . . ?
O1 Zr1 Zr3 Zr2 90.04(7) 11_655 . . . ?
O3 Zr1 Zr3 Zr2 19.77(5) . . . . ?
O5 Zr1 Zr3 Zr2 -124.49(7) . . . . ?
O5 Zr1 Zr3 Zr2 167.68(6) 11_655 . . . ?
Zr3 Zr1 Zr3 Zr2 110.17(3) 11_655 . . . ?
Zr2 Zr1 Zr3 Zr2 55.27(4) 11_655 . . . ?
O1 Zr2 Zr3 O2 56.41(15) . . . . ?
O1 Zr2 Zr3 O2 -125.13(15) 10_556 . . . ?
O3 Zr2 Zr3 O2 -0.21(9) . . . . ?
O3 Zr2 Zr3 O2 -68.50(11) 10_556 . . . ?
O11 Zr2 Zr3 O2 -34.36(8) . . . . ?
O10 Zr2 Zr3 O2 145.64(8) . . . . ?
O7 Zr2 Zr3 O2 75.07(11) 13 . . . ?
O7 Zr2 Zr3 O2 -143.79(10) 6 . . . ?
Zr1 Zr2 Zr3 O2 19.95(7) . . . . ?
Zr1 Zr2 Zr3 O2 -88.67(10) 10_556 . . . ?
Zr2 Zr2 Zr3 O2 -34.36(8) 11_655 . . . ?
O1 Zr2 Zr3 O2 125.13(15) . . . 10_556 ?
O1 Zr2 Zr3 O2 -56.41(15) 10_556 . . 10_556 ?
O3 Zr2 Zr3 O2 68.50(11) . . . 10_556 ?
O3 Zr2 Zr3 O2 0.21(9) 10_556 . . 10_556 ?
O11 Zr2 Zr3 O2 34.36(8) . . . 10_556 ?
O10 Zr2 Zr3 O2 -145.64(8) . . . 10_556 ?
O7 Zr2 Zr3 O2 143.79(10) 13 . . 10_556 ?
O7 Zr2 Zr3 O2 -75.07(11) 6 . . 10_556 ?
Zr1 Zr2 Zr3 O2 88.67(10) . . . 10_556 ?
Zr1 Zr2 Zr3 O2 -19.95(7) 10_556 . . 10_556 ?
Zr2 Zr2 Zr3 O2 34.36(8) 11_655 . . 10_556 ?
O1 Zr2 Zr3 O1 178.5(3) 10_556 . . . ?
O3 Zr2 Zr3 O1 -56.63(15) . . . . ?
O3 Zr2 Zr3 O1 -124.92(15) 10_556 . . . ?
O11 Zr2 Zr3 O1 -90.77(13) . . . . ?
O10 Zr2 Zr3 O1 89.23(13) . . . . ?
O7 Zr2 Zr3 O1 18.66(15) 13 . . . ?
O7 Zr2 Zr3 O1 159.80(15) 6 . . . ?
Zr1 Zr2 Zr3 O1 -36.46(14) . . . . ?
Zr1 Zr2 Zr3 O1 -145.08(14) 10_556 . . . ?
Zr2 Zr2 Zr3 O1 -90.77(13) 11_655 . . . ?
O1 Zr2 Zr3 O1 -178.5(3) . . . 10_556 ?
O3 Zr2 Zr3 O1 124.92(15) . . . 10_556 ?
O3 Zr2 Zr3 O1 56.63(15) 10_556 . . 10_556 ?
O11 Zr2 Zr3 O1 90.77(13) . . . 10_556 ?
O10 Zr2 Zr3 O1 -89.23(13) . . . 10_556 ?
O7 Zr2 Zr3 O1 -159.80(15) 13 . . 10_556 ?
O7 Zr2 Zr3 O1 -18.66(15) 6 . . 10_556 ?
Zr1 Zr2 Zr3 O1 145.08(14) . . . 10_556 ?
Zr1 Zr2 Zr3 O1 36.46(14) 10_556 . . 10_556 ?
Zr2 Zr2 Zr3 O1 90.77(13) 11_655 . . 10_556 ?
O1 Zr2 Zr3 O8 90.77(13) . . . . ?
O1 Zr2 Zr3 O8 -90.77(13) 10_556 . . . ?
O3 Zr2 Zr3 O8 34.15(7) . . . . ?
O3 Zr2 Zr3 O8 -34.15(7) 10_556 . . . ?
O11 Zr2 Zr3 O8 0.0 . . . . ?
O10 Zr2 Zr3 O8 180.0 . . . . ?
O7 Zr2 Zr3 O8 109.43(7) 13 . . . ?
O7 Zr2 Zr3 O8 -109.43(7) 6 . . . ?
Zr1 Zr2 Zr3 O8 54.31(3) . . . . ?
Zr1 Zr2 Zr3 O8 -54.31(3) 10_556 . . . ?
Zr2 Zr2 Zr3 O8 0.0 11_655 . . . ?
O1 Zr2 Zr3 O4 -18.34(15) . . . . ?
O1 Zr2 Zr3 O4 160.12(15) 10_556 . . . ?
O3 Zr2 Zr3 O4 -74.96(11) . . . . ?
O3 Zr2 Zr3 O4 -143.25(10) 10_556 . . . ?
O11 Zr2 Zr3 O4 -109.11(7) . . . . ?
O10 Zr2 Zr3 O4 70.89(7) . . . . ?
O7 Zr2 Zr3 O4 0.33(10) 13 . . . ?
O7 Zr2 Zr3 O4 141.46(11) 6 . . . ?
Zr1 Zr2 Zr3 O4 -54.80(9) . . . . ?
Zr1 Zr2 Zr3 O4 -163.41(7) 10_556 . . . ?
Zr2 Zr2 Zr3 O4 -109.11(7) 11_655 . . . ?
O1 Zr2 Zr3 O4 -160.12(15) . . . 10_556 ?
O1 Zr2 Zr3 O4 18.34(15) 10_556 . . 10_556 ?
O3 Zr2 Zr3 O4 143.25(10) . . . 10_556 ?
O3 Zr2 Zr3 O4 74.96(11) 10_556 . . 10_556 ?
O11 Zr2 Zr3 O4 109.11(7) . . . 10_556 ?
O10 Zr2 Zr3 O4 -70.89(7) . . . 10_556 ?
O7 Zr2 Zr3 O4 -141.46(11) 13 . . 10_556 ?
O7 Zr2 Zr3 O4 -0.33(10) 6 . . 10_556 ?
Zr1 Zr2 Zr3 O4 163.41(7) . . . 10_556 ?
Zr1 Zr2 Zr3 O4 54.80(9) 10_556 . . 10_556 ?
Zr2 Zr2 Zr3 O4 109.11(7) 11_655 . . 10_556 ?
O1 Zr2 Zr3 O9 -89.23(13) . . . . ?
O1 Zr2 Zr3 O9 89.23(13) 10_556 . . . ?
O3 Zr2 Zr3 O9 -145.85(7) . . . . ?
O3 Zr2 Zr3 O9 145.85(7) 10_556 . . . ?
O11 Zr2 Zr3 O9 180.0 . . . . ?
O10 Zr2 Zr3 O9 0.0 . . . . ?
O7 Zr2 Zr3 O9 -70.57(7) 13 . . . ?
O7 Zr2 Zr3 O9 70.57(7) 6 . . . ?
Zr1 Zr2 Zr3 O9 -125.69(3) . . . . ?
Zr1 Zr2 Zr3 O9 125.69(3) 10_556 . . . ?
Zr2 Zr2 Zr3 O9 180.0 11_655 . . . ?
O1 Zr2 Zr3 Zr1 36.46(14) . . . . ?
O1 Zr2 Zr3 Zr1 -145.08(14) 10_556 . . . ?
O3 Zr2 Zr3 Zr1 -20.16(6) . . . . ?
O3 Zr2 Zr3 Zr1 -88.45(9) 10_556 . . . ?
O11 Zr2 Zr3 Zr1 -54.31(3) . . . . ?
O10 Zr2 Zr3 Zr1 125.69(3) . . . . ?
O7 Zr2 Zr3 Zr1 55.13(9) 13 . . . ?
O7 Zr2 Zr3 Zr1 -163.74(7) 6 . . . ?
Zr1 Zr2 Zr3 Zr1 -108.61(7) 10_556 . . . ?
Zr2 Zr2 Zr3 Zr1 -54.31(3) 11_655 . . . ?
O1 Zr2 Zr3 Zr1 145.08(14) . . . 10_556 ?
O1 Zr2 Zr3 Zr1 -36.46(14) 10_556 . . 10_556 ?
O3 Zr2 Zr3 Zr1 88.45(9) . . . 10_556 ?
O3 Zr2 Zr3 Zr1 20.16(6) 10_556 . . 10_556 ?
O11 Zr2 Zr3 Zr1 54.31(3) . . . 10_556 ?
O10 Zr2 Zr3 Zr1 -125.69(3) . . . 10_556 ?
O7 Zr2 Zr3 Zr1 163.74(7) 13 . . 10_556 ?
O7 Zr2 Zr3 Zr1 -55.13(9) 6 . . 10_556 ?
Zr1 Zr2 Zr3 Zr1 108.61(7) . . . 10_556 ?
Zr2 Zr2 Zr3 Zr1 54.31(3) 11_655 . . 10_556 ?
O1 Zr2 Zr3 Zr3 90.77(13) . . . 11_655 ?
O1 Zr2 Zr3 Zr3 -90.77(13) 10_556 . . 11_655 ?
O3 Zr2 Zr3 Zr3 34.15(7) . . . 11_655 ?
O3 Zr2 Zr3 Zr3 -34.15(7) 10_556 . . 11_655 ?
O11 Zr2 Zr3 Zr3 0.0 . . . 11_655 ?
O10 Zr2 Zr3 Zr3 180.0 . . . 11_655 ?
O7 Zr2 Zr3 Zr3 109.43(7) 13 . . 11_655 ?
O7 Zr2 Zr3 Zr3 -109.43(7) 6 . . 11_655 ?
Zr1 Zr2 Zr3 Zr3 54.31(3) . . . 11_655 ?
Zr1 Zr2 Zr3 Zr3 -54.31(3) 10_556 . . 11_655 ?
Zr2 Zr2 Zr3 Zr3 0.0 11_655 . . 11_655 ?
O1 Zr2 O1 Zr3 -0.93(16) 10_556 . . . ?
O3 Zr2 O1 Zr3 118.73(15) . . . . ?
O3 Zr2 O1 Zr3 60.03(15) 10_556 . . . ?
O11 Zr2 O1 Zr3 174.90(17) . . . . ?
O10 Zr2 O1 Zr3 -88.89(12) . . . . ?
O7 Zr2 O1 Zr3 -161.71(14) 13 . . . ?
O7 Zr2 O1 Zr3 -30.1(2) 6 . . . ?
Zr1 Zr2 O1 Zr3 119.48(18) . . . . ?
Zr1 Zr2 O1 Zr3 29.53(11) 10_556 . . . ?
Zr2 Zr2 O1 Zr3 89.12(11) 11_655 . . . ?
O1 Zr2 O1 Zr1 -120.42(7) 10_556 . . . ?
O3 Zr2 O1 Zr1 -0.75(10) . . . . ?
O3 Zr2 O1 Zr1 -59.45(13) 10_556 . . . ?
O11 Zr2 O1 Zr1 55.4(2) . . . . ?
O10 Zr2 O1 Zr1 151.63(10) . . . . ?
O7 Zr2 O1 Zr1 78.80(11) 13 . . . ?
O7 Zr2 O1 Zr1 -149.61(11) 6 . . . ?
Zr1 Zr2 O1 Zr1 -89.96(10) 10_556 . . . ?
Zr3 Zr2 O1 Zr1 -119.48(18) . . . . ?
Zr2 Zr2 O1 Zr1 -30.36(9) 11_655 . . . ?
O2 Zr3 O1 Zr2 -118.83(15) . . . . ?
O2 Zr3 O1 Zr2 -59.59(15) 10_556 . . . ?
O1 Zr3 O1 Zr2 0.93(16) 10_556 . . . ?
O8 Zr3 O1 Zr2 -163.78(19) . . . . ?
O4 Zr3 O1 Zr2 162.29(14) . . . . ?
O4 Zr3 O1 Zr2 30.1(2) 10_556 . . . ?
O9 Zr3 O1 Zr2 88.54(12) . . . . ?
Zr1 Zr3 O1 Zr2 -120.34(18) . . . . ?
Zr1 Zr3 O1 Zr2 -29.72(11) 10_556 . . . ?
Zr3 Zr3 O1 Zr2 -89.59(11) 11_655 . . . ?
O2 Zr3 O1 Zr1 1.51(10) . . . . ?
O2 Zr3 O1 Zr1 60.75(13) 10_556 . . . ?
O1 Zr3 O1 Zr1 121.27(7) 10_556 . . . ?
O8 Zr3 O1 Zr1 -43.4(3) . . . . ?
O4 Zr3 O1 Zr1 -77.37(11) . . . . ?
O4 Zr3 O1 Zr1 150.45(11) 10_556 . . . ?
O9 Zr3 O1 Zr1 -151.12(10) . . . . ?
Zr1 Zr3 O1 Zr1 90.62(10) 10_556 . . . ?
Zr3 Zr3 O1 Zr1 30.75(9) 11_655 . . . ?
Zr2 Zr3 O1 Zr1 120.34(18) . . . . ?
O2 Zr1 O1 Zr2 120.73(14) . . . . ?
O6 Zr1 O1 Zr2 -80.42(12) 13 . . . ?
O6 Zr1 O1 Zr2 -34.86(18) 7 . . . ?
O1 Zr1 O1 Zr2 60.53(15) 11_655 . . . ?
O3 Zr1 O1 Zr2 0.74(10) . . . . ?
O5 Zr1 O1 Zr2 -157.31(11) . . . . ?
O5 Zr1 O1 Zr2 156.41(10) 11_655 . . . ?
Zr3 Zr1 O1 Zr2 122.24(16) . . . . ?
Zr3 Zr1 O1 Zr2 91.40(10) 11_655 . . . ?
Zr2 Zr1 O1 Zr2 30.76(9) 11_655 . . . ?
O2 Zr1 O1 Zr3 -1.50(10) . . . . ?
O6 Zr1 O1 Zr3 157.35(11) 13 . . . ?
O6 Zr1 O1 Zr3 -157.09(10) 7 . . . ?
O1 Zr1 O1 Zr3 -61.70(14) 11_655 . . . ?
O3 Zr1 O1 Zr3 -121.49(14) . . . . ?
O5 Zr1 O1 Zr3 80.46(11) . . . . ?
O5 Zr1 O1 Zr3 34.17(19) 11_655 . . . ?
Zr3 Zr1 O1 Zr3 -30.84(9) 11_655 . . . ?
Zr2 Zr1 O1 Zr3 -122.24(16) . . . . ?
Zr2 Zr1 O1 Zr3 -91.48(10) 11_655 . . . ?
O2 Zr3 O2 Zr3 1.09(18) 10_556 . . 11_655 ?
O1 Zr3 O2 Zr3 120.09(16) . . . 11_655 ?
O1 Zr3 O2 Zr3 62.37(16) 10_556 . . 11_655 ?
O8 Zr3 O2 Zr3 -83.83(14) . . . 11_655 ?
O4 Zr3 O2 Zr3 -158.92(16) . . . 11_655 ?
O4 Zr3 O2 Zr3 -29.5(2) 10_556 . . 11_655 ?
O9 Zr3 O2 Zr3 174.07(15) . . . 11_655 ?
Zr1 Zr3 O2 Zr3 121.6(2) . . . 11_655 ?
Zr1 Zr3 O2 Zr3 31.02(13) 10_556 . . 11_655 ?
Zr2 Zr3 O2 Zr3 90.98(13) . . . 11_655 ?
O2 Zr3 O2 Zr1 -120.55(9) 10_556 . . . ?
O1 Zr3 O2 Zr1 -1.55(11) . . . . ?
O1 Zr3 O2 Zr1 -59.27(15) 10_556 . . . ?
O8 Zr3 O2 Zr1 154.53(13) . . . . ?
O4 Zr3 O2 Zr1 79.44(13) . . . . ?
O4 Zr3 O2 Zr1 -151.13(10) 10_556 . . . ?
O9 Zr3 O2 Zr1 52.4(3) . . . . ?
Zr1 Zr3 O2 Zr1 -90.63(12) 10_556 . . . ?
Zr3 Zr3 O2 Zr1 -121.6(2) 11_655 . . . ?
Zr2 Zr3 O2 Zr1 -30.66(11) . . . . ?
O6 Zr1 O2 Zr3 -34.0(2) 13 . . . ?
O6 Zr1 O2 Zr3 156.60(8) 7 . . . ?
O1 Zr1 O2 Zr3 1.53(10) . . . . ?
O1 Zr1 O2 Zr3 121.03(16) 11_655 . . . ?
O3 Zr1 O2 Zr3 61.28(11) . . . . ?
O5 Zr1 O2 Zr3 -80.03(13) . . . . ?
O5 Zr1 O2 Zr3 -157.41(13) 11_655 . . . ?
Zr3 Zr1 O2 Zr3 122.6(2) 11_655 . . . ?
Zr2 Zr1 O2 Zr3 30.89(11) . . . . ?
Zr2 Zr1 O2 Zr3 91.67(12) 11_655 . . . ?
O6 Zr1 O2 Zr3 -156.60(8) 13 . . 11_655 ?
O6 Zr1 O2 Zr3 34.0(2) 7 . . 11_655 ?
O1 Zr1 O2 Zr3 -121.03(16) . . . 11_655 ?
O1 Zr1 O2 Zr3 -1.53(10) 11_655 . . 11_655 ?
O3 Zr1 O2 Zr3 -61.28(11) . . . 11_655 ?
O5 Zr1 O2 Zr3 157.41(13) . . . 11_655 ?
O5 Zr1 O2 Zr3 80.03(13) 11_655 . . 11_655 ?
Zr3 Zr1 O2 Zr3 -122.6(2) . . . 11_655 ?
Zr2 Zr1 O2 Zr3 -91.67(12) . . . 11_655 ?
Zr2 Zr1 O2 Zr3 -30.89(11) 11_655 . . 11_655 ?
O1 Zr2 O3 Zr2 -118.34(18) . . . 11_655 ?
O1 Zr2 O3 Zr2 -60.01(18) 10_556 . . 11_655 ?
O3 Zr2 O3 Zr2 1.1(2) 10_556 . . 11_655 ?
O11 Zr2 O3 Zr2 89.42(16) . . . 11_655 ?
O10 Zr2 O3 Zr2 -173.68(16) . . . 11_655 ?
O7 Zr2 O3 Zr2 162.39(18) 13 . . 11_655 ?
O7 Zr2 O3 Zr2 30.0(3) 6 . . 11_655 ?
Zr1 Zr2 O3 Zr2 -119.1(2) . . . 11_655 ?
Zr1 Zr2 O3 Zr2 -29.60(15) 10_556 . . 11_655 ?
Zr3 Zr2 O3 Zr2 -88.98(15) . . . 11_655 ?
O1 Zr2 O3 Zr1 0.75(10) . . . . ?
O1 Zr2 O3 Zr1 59.07(14) 10_556 . . . ?
O3 Zr2 O3 Zr1 120.22(8) 10_556 . . . ?
O11 Zr2 O3 Zr1 -151.50(12) . . . . ?
O10 Zr2 O3 Zr1 -54.6(3) . . . . ?
O7 Zr2 O3 Zr1 -78.53(12) 13 . . . ?
O7 Zr2 O3 Zr1 149.13(10) 6 . . . ?
Zr1 Zr2 O3 Zr1 89.48(12) 10_556 . . . ?
Zr3 Zr2 O3 Zr1 30.10(11) . . . . ?
Zr2 Zr2 O3 Zr1 119.1(2) 11_655 . . . ?
O2 Zr1 O3 Zr2 -60.62(11) . . . . ?
O6 Zr1 O3 Zr2 81.15(13) 13 . . . ?
O6 Zr1 O3 Zr2 157.61(13) 7 . . . ?
O1 Zr1 O3 Zr2 -0.73(10) . . . . ?
O1 Zr1 O3 Zr2 -120.51(16) 11_655 . . . ?
O5 Zr1 O3 Zr2 35.7(2) . . . . ?
O5 Zr1 O3 Zr2 -156.92(8) 11_655 . . . ?
Zr3 Zr1 O3 Zr2 -30.52(11) . . . . ?
Zr3 Zr1 O3 Zr2 -90.72(12) 11_655 . . . ?
Zr2 Zr1 O3 Zr2 -121.2(2) 11_655 . . . ?
O2 Zr1 O3 Zr2 60.62(11) . . . 11_655 ?
O6 Zr1 O3 Zr2 -157.61(13) 13 . . 11_655 ?
O6 Zr1 O3 Zr2 -81.15(13) 7 . . 11_655 ?
O1 Zr1 O3 Zr2 120.51(16) . . . 11_655 ?
O1 Zr1 O3 Zr2 0.73(10) 11_655 . . 11_655 ?
O5 Zr1 O3 Zr2 156.92(8) . . . 11_655 ?
O5 Zr1 O3 Zr2 -35.7(2) 11_655 . . 11_655 ?
Zr3 Zr1 O3 Zr2 90.72(12) . . . 11_655 ?
Zr3 Zr1 O3 Zr2 30.52(11) 11_655 . . 11_655 ?
Zr2 Zr1 O3 Zr2 121.2(2) . . . 11_655 ?
O2 Zr3 O4 C1 -33.3(3) . . . . ?
O2 Zr3 O4 C1 -62.6(4) 10_556 . . . ?
O1 Zr3 O4 C1 41.0(3) . . . . ?
O1 Zr3 O4 C1 68.5(4) 10_556 . . . ?
O8 Zr3 O4 C1 -119.7(3) . . . . ?
O4 Zr3 O4 C1 -174.8(3) 10_556 . . . ?
O9 Zr3 O4 C1 131.1(3) . . . . ?
Zr1 Zr3 O4 C1 3.4(3) . . . . ?
Zr1 Zr3 O4 C1 -0.2(5) 10_556 . . . ?
Zr3 Zr3 O4 C1 -45.6(3) 11_655 . . . ?
Zr2 Zr3 O4 C1 51.3(3) . . . . ?
O2 Zr1 O5 C1 28.0(3) . . . . ?
O6 Zr1 O5 C1 -125.1(3) 13 . . . ?
O6 Zr1 O5 C1 172.6(3) 7 . . . ?
O1 Zr1 O5 C1 -44.1(3) . . . . ?
O1 Zr1 O5 C1 62.1(4) 11_655 . . . ?
O3 Zr1 O5 C1 -78.9(3) . . . . ?
O5 Zr1 O5 C1 109.1(3) 11_655 . . . ?
Zr3 Zr1 O5 C1 -7.6(3) . . . . ?
Zr3 Zr1 O5 C1 41.6(3) 11_655 . . . ?
Zr2 Zr1 O5 C1 -57.7(3) . . . . ?
Zr2 Zr1 O5 C1 -8.6(5) 11_655 . . . ?
Zr1 O5 C1 O4 12.8(6) . . . . ?
Zr1 O5 C1 C2 -164.1(2) . . . . ?
Zr3 O4 C1 O5 -10.2(6) . . . . ?
Zr3 O4 C1 C2 166.7(2) . . . . ?
O5 C1 C2 C7 -13.4(6) . . . . ?
O4 C1 C2 C7 169.5(4) . . . . ?
O5 C1 C2 C3 168.5(3) . . . . ?
O4 C1 C2 C3 -8.6(5) . . . . ?
C7 C2 C3 C4 3.4(6) . . . . ?
C1 C2 C3 C4 -178.4(3) . . . . ?
C2 C3 C4 C5 0.0(6) . . . . ?
C3 C4 C5 C6 -4.5(6) . . . . ?
C3 C4 C5 C8 -180.0(3) . . . . ?
C4 C5 C6 C7 5.5(6) . . . . ?
C8 C5 C6 C7 -179.2(4) . . . . ?
C3 C2 C7 C6 -2.5(6) . . . . ?
C1 C2 C7 C6 179.5(4) . . . . ?
C5 C6 C7 C2 -2.1(6) . . . . ?
C6 C5 C8 C13 -36.0(6) . . . . ?
C4 C5 C8 C13 139.3(4) . . . . ?
C6 C5 C8 C9 140.2(4) . . . . ?
C4 C5 C8 C9 -44.6(5) . . . . ?
C13 C8 C9 C10 -2.8(5) . . . . ?
C5 C8 C9 C10 -179.1(3) . . . . ?
C8 C9 C10 C11 0.4(5) . . . . ?
C8 C9 C10 C10 -174.5(2) . . . 12 ?
C9 C10 C11 N1 -176.1(3) . . . . ?
C10 C10 C11 N1 -0.2(3) 12 . . . ?
C9 C10 C11 C12 1.0(5) . . . . ?
C10 C10 C11 C12 176.9(3) 12 . . . ?
C11 N1 C11 C10 0.2(5) 12 . . . ?
C11 N1 C11 C12 -176.6(2) 12 . . . ?
C10 C11 C12 C13 0.2(5) . . . . ?
N1 C11 C12 C13 176.7(4) . . . . ?
C10 C11 C12 C14 -179.5(3) . . . . ?
N1 C11 C12 C14 -3.0(6) . . . . ?
C9 C8 C13 C12 4.2(6) . . . . ?
C5 C8 C13 C12 -179.6(3) . . . . ?
C11 C12 C13 C8 -2.8(5) . . . . ?
C14 C12 C13 C8 176.9(3) . . . . ?
C13 C12 C14 C19 -46.2(5) . . . . ?
C11 C12 C14 C19 133.5(4) . . . . ?
C13 C12 C14 C15 134.2(4) . . . . ?
C11 C12 C14 C15 -46.1(6) . . . . ?
C19 C14 C15 C16 2.2(5) . . . . ?
C12 C14 C15 C16 -178.3(3) . . . . ?
C14 C15 C16 C17 0.3(6) . . . . ?
C15 C16 C17 C18 -3.5(5) . . . . ?
C15 C16 C17 C20 179.2(3) . . . . ?
C16 C17 C18 C19 4.2(5) . . . . ?
C20 C17 C18 C19 -178.2(3) . . . . ?
C15 C14 C19 C18 -1.2(5) . . . . ?
C12 C14 C19 C18 179.2(3) . . . . ?
C17 C18 C19 C14 -2.0(5) . . . . ?
Zr1 O6 C20 O7 -5.8(5) 13 . . . ?
Zr1 O6 C20 C17 175.1(2) 13 . . . ?
Zr2 O7 C20 O6 4.1(5) 13 . . . ?
Zr2 O7 C20 C17 -176.8(2) 13 . . . ?
C16 C17 C20 O6 174.3(3) . . . . ?
C18 C17 C20 O6 -3.0(5) . . . . ?
C16 C17 C20 O7 -4.8(5) . . . . ?
C18 C17 C20 O7 177.9(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.977
_diffrn_reflns_theta_full        25.16
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.063
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.024 -0.010 -0.004 15809.7 3634.5
_platon_squeeze_details          
;
;
####################################################################### 
# 
# 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 1533345'
_audit_update_record             
;
2017-02-17 deposited with the CCDC.
2018-09-04 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         ?
_chemical_formula_sum            'C40 H21 N O24.50 Zr3'
_chemical_formula_weight         1181.24

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'
N N 0.0311 0.0180 '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      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'

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

_cell_length_a                   17.723(5)
_cell_length_b                   32.705(3)
_cell_length_c                   34.670(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     20096(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    975
_cell_measurement_theta_min      3.8030
_cell_measurement_theta_max      63.5330

_exptl_crystal_description       
; 
'Sat Dec 19 00:02:26 2015' 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.781
_exptl_crystal_F_000             4672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.871
_shelx_estimated_absorpt_T_min   0.611
_shelx_estimated_absorpt_T_max   0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
'Sat Dec 19 00:02:26 2015' 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_reflns_number            39298
_diffrn_reflns_av_unetI/netI     0.2558
_diffrn_reflns_av_R_equivalents  0.3270
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         3.716
_diffrn_reflns_theta_max         65.073
_diffrn_reflns_theta_full        65.073
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9189
_reflns_number_gt                2142
_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       
; 
'Sat Dec 19 00:02:26 2015' 
;
_computing_cell_refinement       
; 
'Sat Dec 19 00:02:26 2015' 
;
_computing_data_reduction        
; 
'Sat Dec 19 00:02:26 2015' 
;
_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)+(0.0500P)²+200.0000P] 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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.000009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         9189
_refine_ls_number_parameters     320
_refine_ls_number_restraints     310
_refine_ls_R_factor_all          0.2921
_refine_ls_R_factor_gt           0.1339
_refine_ls_wR_factor_ref         0.3539
_refine_ls_wR_factor_gt          0.2853
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.009
_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
C1 C 0.1210(14) 0.1545(5) 0.5934(4) 0.108(6) Uani 1 1 d . U . . .
C2 C 0.1507(12) 0.1303(4) 0.6270(4) 0.109(6) Uani 1 1 d D U . . .
C3 C 0.2075(11) 0.1012(5) 0.6221(4) 0.114(6) Uani 1 1 d D U . . .
H3 H 0.2285 0.0963 0.5974 0.136 Uiso 1 1 calc R U . . .
C4 C 0.2330(11) 0.0794(4) 0.6545(4) 0.114(6) Uani 1 1 d D U . . .
H4 H 0.2672 0.0572 0.6516 0.137 Uiso 1 1 calc R U . . .
C5 C 0.2062(13) 0.0913(5) 0.6925(4) 0.124(6) Uani 1 1 d D U . . .
C6 C 0.1532(12) 0.1226(5) 0.6958(4) 0.138(7) Uani 1 1 d D U . . .
H6 H 0.1373 0.1311 0.7207 0.165 Uiso 1 1 calc R U . . .
C7 C 0.1236(12) 0.1413(4) 0.6637(4) 0.130(7) Uani 1 1 d D U . . .
H7 H 0.0853 0.1615 0.6663 0.156 Uiso 1 1 calc R U . . .
C8 C 0.2427(14) 0.0752(4) 0.7284(4) 0.128(6) Uani 1 1 d D U . . .
C9 C 0.2525(15) 0.0336(4) 0.7359(4) 0.138(7) Uani 1 1 d D U . . .
C10 C 0.2806(14) 0.0203(4) 0.7721(4) 0.138(7) Uani 1 1 d D U . . .
C11 C 0.3063(14) 0.0499(5) 0.7999(4) 0.157(8) Uani 1 1 d D U . . .
H11 H 0.3299 0.0416 0.8232 0.188 Uiso 1 1 calc R U . . .
C12 C 0.2955(16) 0.0909(4) 0.7916(4) 0.160(7) Uani 1 1 d D U . . .
C13 C 0.2651(13) 0.1027(4) 0.7568(4) 0.139(8) Uani 1 1 d D U . . .
H13 H 0.2591 0.1311 0.7519 0.166 Uiso 1 1 calc R U . . .
C14 C 0.3157(16) 0.1221(5) 0.8219(4) 0.167(7) Uani 1 1 d D U . . .
C15 C 0.2929(14) 0.1153(5) 0.8597(4) 0.169(8) Uani 1 1 d D U . . .
H15 H 0.2610 0.0930 0.8662 0.202 Uiso 1 1 calc R U . . .
C16 C 0.3195(15) 0.1430(5) 0.8881(4) 0.179(9) Uani 1 1 d D U . . .
H16 H 0.3077 0.1382 0.9145 0.215 Uiso 1 1 calc R U . . .
C17 C 0.3630(16) 0.1777(5) 0.8782(4) 0.171(8) Uani 1 1 d D U . . .
C18 C 0.3741(16) 0.1861(5) 0.8390(4) 0.185(9) Uani 1 1 d D U . . .
H18 H 0.3977 0.2109 0.8313 0.221 Uiso 1 1 calc R U . . .
C19 C 0.3505(15) 0.1582(5) 0.8112(4) 0.175(8) Uani 1 1 d D U . . .
H19 H 0.3585 0.1640 0.7847 0.210 Uiso 1 1 calc R U . . .
C20 C 0.3847(16) 0.2093(5) 0.9065(4) 0.135(7) Uani 1 1 d . U . . .
N1 N 0.2301(16) 0.0000 0.7134(5) 0.138(9) Uani 1 2 d S TU P . .
H1 H 0.2075 0.0000 0.6907 0.166 Uiso 1 2 calc R U P . .
O5 O 0.0000 0.1674(5) 0.5333(4) 0.113(4) Uani 1 2 d S TU P . .
O9 O -0.2213(12) 0.2760(5) 0.5000 0.124(4) Uani 1 2 d S TU P . .
O7 O 0.0000 0.2732(5) 0.5325(5) 0.126(4) Uani 1 2 d S TU P . .
O8 O -0.0886(13) 0.3432(4) 0.5000 0.144(7) Uani 1 2 d S TU P . .
O1 O 0.0732(8) 0.1819(3) 0.6018(2) 0.105(4) Uani 1 1 d . U . . .
O2 O 0.1415(8) 0.1438(3) 0.5596(3) 0.106(5) Uani 1 1 d . U . . .
O3 O 0.4278(9) 0.2375(3) 0.8982(3) 0.122(5) Uani 1 1 d . U . . .
O4 O 0.3583(10) 0.2020(3) 0.9414(3) 0.146(6) Uani 1 1 d . U . . .
O11 O -0.0901(11) 0.0989(4) 0.5000 0.100(5) Uani 1 2 d S TU P . .
O6 O -0.1016(8) 0.2217(3) 0.5354(3) 0.111(3) Uani 1 1 d . U . . .
O10 O -0.2273(12) 0.1689(4) 0.5000 0.109(4) Uani 1 2 d S TU P . .
Zr01 Zr -0.10044(19) 0.16695(6) 0.5000 0.0993(11) Uani 1 2 d S TU P . .
Zr02 Zr 0.0000 0.22205(6) 0.57012(5) 0.1032(11) Uani 1 2 d S TU P . .
Zr03 Zr -0.10000(19) 0.27587(6) 0.5000 0.1054(12) Uani 1 2 d S TU P . .
O1W O 0.0000 0.3323 0.4303 0.094(11) Uiso 0.5 2 d S U P A 1
O2W O -0.235(2) 0.2203(11) 0.5826(12) 0.205(15) Uiso 0.5 1 d . U P B 1
O3W O 0.0000 0.1129 0.5708 0.28(3) Uiso 0.5 2 d S U P C 1
O4W O 0.1152(11) 0.0000 0.6566(6) 0.141(8) Uiso 1 2 d S . P . .
O5W O 0.0000 0.0749(11) 0.5780(11) 0.119(13) Uiso 0.5 2 d S U P D 2
O6W O 0.0000 0.0608(8) 0.6562(8) 0.224(13) Uiso 1 2 d S . P . .
O7W O -0.3249(16) 0.2882(8) 0.5591(8) 0.132(10) Uiso 0.5 1 d . . P . .
O8W O -0.3242(17) 0.1713(8) 0.5582(8) 0.146(11) Uiso 0.5 1 d . . P . .
O9W O 0.153(3) 0.0000 0.5792(14) 0.18(2) Uiso 0.5 2 d S . P . .
O10W O 0.0000 0.3823(12) 0.4403(12) 0.144(15) Uiso 0.5 2 d S U P E 2
O11W O -0.2352(18) 0.2254(9) 0.6252(10) 0.163(12) Uiso 0.5 1 d . U P F 2


_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
C1 O2 1.278(17) . ?
C1 O1 1.27(2) . ?
C1 C2 1.504(19) . ?
C2 C3 1.394(16) . ?
C2 C7 1.408(15) . ?
C3 C4 1.406(15) . ?
C3 H3 0.9500 . ?
C4 C5 1.452(15) . ?
C4 H4 0.9500 . ?
C5 C6 1.393(16) . ?
C5 C8 1.499(19) . ?
C6 C7 1.374(15) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.392(15) . ?
C8 C9 1.395(14) . ?
C9 N1 1.406(17) . ?
C9 C10 1.418(15) . ?
C10 C10 1.33(2) 11 ?
C10 C11 1.440(16) . ?
C11 C12 1.383(15) . ?
C11 H11 0.9500 . ?
C12 C13 1.377(15) . ?
C12 C14 1.509(19) . ?
C13 H13 0.9500 . ?
C14 C15 1.387(16) . ?
C14 C19 1.383(16) . ?
C15 C16 1.421(15) . ?
C15 H15 0.9500 . ?
C16 C17 1.413(17) . ?
C16 H16 0.9500 . ?
C17 C18 1.401(16) . ?
C17 C20 1.48(2) . ?
C18 C19 1.390(15) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 O3 1.23(2) . ?
C20 O4 1.32(2) . ?
N1 C9 1.406(17) 11 ?
N1 H1 0.8800 . ?
O5 Zr01 2.123(8) . ?
O5 Zr01 2.123(8) 3_556 ?
O5 Zr02 2.196(13) . ?
O9 Zr03 2.15(2) . ?
O7 Zr03 2.103(9) . ?
O7 Zr03 2.103(9) 3_556 ?
O7 Zr02 2.120(15) . ?
O8 Zr03 2.211(14) . ?
O1 Zr02 2.149(11) . ?
O2 Zr01 2.318(10) 3_556 ?
O3 Zr02 2.144(11) 13_556 ?
O4 Zr03 2.281(11) 15 ?
O11 Zr01 2.234(13) . ?
O6 Zr03 2.154(9) . ?
O6 Zr02 2.166(12) . ?
O6 Zr01 2.171(9) . ?
O10 Zr01 2.25(2) . ?
Zr01 O5 2.123(8) 10_556 ?
Zr01 O6 2.171(9) 10_556 ?
Zr01 O2 2.318(10) 3_556 ?
Zr01 O2 2.318(10) 12 ?
Zr01 Zr02 3.511(3) 10_556 ?
Zr01 Zr02 3.511(3) . ?
Zr01 Zr01 3.560(7) 3_556 ?
Zr01 Zr03 3.562(3) . ?
Zr02 O6 2.166(12) 12 ?
Zr02 O1 2.149(11) 12 ?
Zr02 O3 2.144(11) 13_556 ?
Zr02 O3 2.144(11) 8_456 ?
Zr02 Zr03 3.485(3) . ?
Zr02 Zr03 3.486(3) 3_556 ?
Zr02 Zr01 3.511(3) 3_556 ?
Zr03 O7 2.103(9) 10_556 ?
Zr03 O6 2.154(9) 10_556 ?
Zr03 O4 2.281(11) 8_456 ?
Zr03 O4 2.281(11) 15_454 ?
Zr03 Zr02 3.485(3) 10_556 ?
Zr03 Zr03 3.545(7) 3_556 ?

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
O2 C1 O1 126.5(16) . . ?
O2 C1 C2 117.8(17) . . ?
O1 C1 C2 115.4(13) . . ?
C3 C2 C7 122.1(13) . . ?
C3 C2 C1 121.2(14) . . ?
C7 C2 C1 116.4(15) . . ?
C2 C3 C4 118.8(13) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C3 C4 C5 118.8(13) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 119.5(13) . . ?
C6 C5 C8 118.7(14) . . ?
C4 C5 C8 121.2(17) . . ?
C7 C6 C5 121.2(14) . . ?
C7 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
C6 C7 C2 119.1(14) . . ?
C6 C7 H7 120.5 . . ?
C2 C7 H7 120.5 . . ?
C13 C8 C9 117.6(13) . . ?
C13 C8 C5 118.9(12) . . ?
C9 C8 C5 123.4(13) . . ?
C8 C9 N1 128.6(14) . . ?
C8 C9 C10 120.5(12) . . ?
N1 C9 C10 110.6(13) . . ?
C10 C10 C9 107.9(8) 11 . ?
C10 C10 C11 132.3(8) 11 . ?
C9 C10 C11 119.7(11) . . ?
C12 C11 C10 118.0(13) . . ?
C12 C11 H11 121.0 . . ?
C10 C11 H11 121.0 . . ?
C13 C12 C11 120.5(13) . . ?
C13 C12 C14 120.9(14) . . ?
C11 C12 C14 118.6(14) . . ?
C12 C13 C8 123.3(13) . . ?
C12 C13 H13 118.3 . . ?
C8 C13 H13 118.3 . . ?
C15 C14 C19 121.4(13) . . ?
C15 C14 C12 118.6(16) . . ?
C19 C14 C12 119.7(15) . . ?
C14 C15 C16 117.1(15) . . ?
C14 C15 H15 121.5 . . ?
C16 C15 H15 121.5 . . ?
C17 C16 C15 121.6(14) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C18 C17 C16 118.2(14) . . ?
C18 C17 C20 118.0(15) . . ?
C16 C17 C20 122.8(15) . . ?
C19 C18 C17 120.0(14) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C14 120.6(14) . . ?
C18 C19 H19 119.7 . . ?
C14 C19 H19 119.7 . . ?
O3 C20 O4 124.8(16) . . ?
O3 C20 C17 122.1(17) . . ?
O4 C20 C17 112.9(17) . . ?
C9 N1 C9 102.9(18) 11 . ?
C9 N1 H1 128.6 11 . ?
C9 N1 H1 128.6 . . ?
Zr01 O5 Zr01 114.0(7) . 3_556 ?
Zr01 O5 Zr02 108.8(5) . . ?
Zr01 O5 Zr02 108.8(5) 3_556 . ?
Zr03 O7 Zr03 114.9(8) . 3_556 ?
Zr03 O7 Zr02 111.3(5) . . ?
Zr03 O7 Zr02 111.3(5) 3_556 . ?
C1 O1 Zr02 135.9(9) . . ?
C1 O2 Zr01 129.8(13) . 3_556 ?
C20 O3 Zr02 135.5(10) . 13_556 ?
C20 O4 Zr03 130.1(15) . 15 ?
Zr03 O6 Zr02 107.6(5) . . ?
Zr03 O6 Zr01 110.9(4) . . ?
Zr02 O6 Zr01 108.1(5) . . ?
O5 Zr01 O5 66.0(7) 10_556 . ?
O5 Zr01 O6 72.2(5) 10_556 10_556 ?
O5 Zr01 O6 108.1(6) . 10_556 ?
O5 Zr01 O6 108.0(6) 10_556 . ?
O5 Zr01 O6 72.2(5) . . ?
O6 Zr01 O6 68.8(5) 10_556 . ?
O5 Zr01 O11 86.4(6) 10_556 . ?
O5 Zr01 O11 86.4(6) . . ?
O6 Zr01 O11 145.4(2) 10_556 . ?
O6 Zr01 O11 145.4(2) . . ?
O5 Zr01 O10 146.9(3) 10_556 . ?
O5 Zr01 O10 146.9(3) . . ?
O6 Zr01 O10 88.2(5) 10_556 . ?
O6 Zr01 O10 88.2(5) . . ?
O11 Zr01 O10 96.3(6) . . ?
O5 Zr01 O2 77.3(5) 10_556 3_556 ?
O5 Zr01 O2 138.7(5) . 3_556 ?
O6 Zr01 O2 76.3(3) 10_556 3_556 ?
O6 Zr01 O2 140.4(4) . 3_556 ?
O11 Zr01 O2 72.5(3) . 3_556 ?
O10 Zr01 O2 72.3(4) . 3_556 ?
O5 Zr01 O2 138.7(5) 10_556 12 ?
O5 Zr01 O2 77.3(5) . 12 ?
O6 Zr01 O2 140.4(4) 10_556 12 ?
O6 Zr01 O2 76.3(3) . 12 ?
O11 Zr01 O2 72.5(3) . 12 ?
O10 Zr01 O2 72.3(4) . 12 ?
O2 Zr01 O2 126.1(6) 3_556 12 ?
O5 Zr01 Zr02 36.3(4) 10_556 10_556 ?
O5 Zr01 Zr02 87.1(4) . 10_556 ?
O6 Zr01 Zr02 35.9(3) 10_556 10_556 ?
O6 Zr01 Zr02 88.4(3) . 10_556 ?
O11 Zr01 Zr02 118.0(3) . 10_556 ?
O10 Zr01 Zr02 119.5(2) . 10_556 ?
O2 Zr01 Zr02 73.1(3) 3_556 10_556 ?
O2 Zr01 Zr02 160.8(3) 12 10_556 ?
O5 Zr01 Zr02 87.1(4) 10_556 . ?
O5 Zr01 Zr02 36.3(4) . . ?
O6 Zr01 Zr02 88.4(3) 10_556 . ?
O6 Zr01 Zr02 35.9(3) . . ?
O11 Zr01 Zr02 118.0(3) . . ?
O10 Zr01 Zr02 119.5(2) . . ?
O2 Zr01 Zr02 160.8(3) 3_556 . ?
O2 Zr01 Zr02 73.1(3) 12 . ?
Zr02 Zr01 Zr02 87.65(8) 10_556 . ?
O5 Zr01 Zr01 33.0(3) 10_556 3_556 ?
O5 Zr01 Zr01 33.0(3) . 3_556 ?
O6 Zr01 Zr01 90.5(4) 10_556 3_556 ?
O6 Zr01 Zr01 90.5(4) . 3_556 ?
O11 Zr01 Zr01 85.3(5) . 3_556 ?
O10 Zr01 Zr01 178.4(4) . 3_556 ?
O2 Zr01 Zr01 108.3(4) 3_556 3_556 ?
O2 Zr01 Zr01 108.3(4) 12 3_556 ?
Zr02 Zr01 Zr01 59.53(5) 10_556 3_556 ?
Zr02 Zr01 Zr01 59.53(5) . 3_556 ?
O5 Zr01 Zr03 89.5(4) 10_556 . ?
O5 Zr01 Zr03 89.5(4) . . ?
O6 Zr01 Zr03 34.4(2) 10_556 . ?
O6 Zr01 Zr03 34.4(2) . . ?
O11 Zr01 Zr03 175.2(5) . . ?
O10 Zr01 Zr03 88.5(4) . . ?
O2 Zr01 Zr03 109.1(2) 3_556 . ?
O2 Zr01 Zr03 109.1(2) 12 . ?
Zr02 Zr01 Zr03 59.04(6) 10_556 . ?
Zr02 Zr01 Zr03 59.04(6) . . ?
Zr01 Zr01 Zr03 89.87(8) 3_556 . ?
O7 Zr02 O6 70.2(3) . . ?
O7 Zr02 O6 70.2(3) . 12 ?
O6 Zr02 O6 112.4(6) . 12 ?
O7 Zr02 O5 106.6(6) . . ?
O6 Zr02 O5 70.9(3) . . ?
O6 Zr02 O5 70.9(3) 12 . ?
O7 Zr02 O1 142.8(3) . 12 ?
O6 Zr02 O1 77.3(4) . 12 ?
O6 Zr02 O1 141.6(4) 12 12 ?
O5 Zr02 O1 78.4(4) . 12 ?
O7 Zr02 O1 142.8(4) . . ?
O6 Zr02 O1 141.6(4) . . ?
O6 Zr02 O1 77.3(4) 12 . ?
O5 Zr02 O1 78.4(4) . . ?
O1 Zr02 O1 74.2(7) 12 . ?
O7 Zr02 O3 80.1(4) . 13_556 ?
O6 Zr02 O3 141.6(4) . 13_556 ?
O6 Zr02 O3 78.0(5) 12 13_556 ?
O5 Zr02 O3 143.1(4) . 13_556 ?
O1 Zr02 O3 118.4(4) 12 13_556 ?
O1 Zr02 O3 75.8(4) . 13_556 ?
O7 Zr02 O3 80.1(4) . 8_456 ?
O6 Zr02 O3 78.0(5) . 8_456 ?
O6 Zr02 O3 141.6(4) 12 8_456 ?
O5 Zr02 O3 143.1(4) . 8_456 ?
O1 Zr02 O3 75.8(4) 12 8_456 ?
O1 Zr02 O3 118.4(4) . 8_456 ?
O3 Zr02 O3 73.3(8) 13_556 8_456 ?
O7 Zr02 Zr03 34.2(2) . . ?
O6 Zr02 Zr03 36.1(3) . . ?
O6 Zr02 Zr03 92.1(3) 12 . ?
O5 Zr02 Zr03 90.4(4) . . ?
O1 Zr02 Zr03 111.0(3) 12 . ?
O1 Zr02 Zr03 166.5(3) . . ?
O3 Zr02 Zr03 110.4(3) 13_556 . ?
O3 Zr02 Zr03 75.0(3) 8_456 . ?
O7 Zr02 Zr03 34.2(2) . 3_556 ?
O6 Zr02 Zr03 92.1(3) . 3_556 ?
O6 Zr02 Zr03 36.1(3) 12 3_556 ?
O5 Zr02 Zr03 90.4(4) . 3_556 ?
O1 Zr02 Zr03 166.5(3) 12 3_556 ?
O1 Zr02 Zr03 111.0(3) . 3_556 ?
O3 Zr02 Zr03 75.0(3) 13_556 3_556 ?
O3 Zr02 Zr03 110.4(3) 8_456 3_556 ?
Zr03 Zr02 Zr03 61.13(11) . 3_556 ?
O7 Zr02 Zr01 88.8(4) . . ?
O6 Zr02 Zr01 36.0(3) . . ?
O6 Zr02 Zr01 91.9(3) 12 . ?
O5 Zr02 Zr01 34.9(2) . . ?
O1 Zr02 Zr01 74.6(3) 12 . ?
O1 Zr02 Zr01 110.3(3) . . ?
O3 Zr02 Zr01 167.0(3) 13_556 . ?
O3 Zr02 Zr01 111.6(4) 8_456 . ?
Zr03 Zr02 Zr01 61.21(5) . . ?
Zr03 Zr02 Zr01 91.95(6) 3_556 . ?
O7 Zr02 Zr01 88.8(4) . 3_556 ?
O6 Zr02 Zr01 91.9(3) . 3_556 ?
O6 Zr02 Zr01 36.0(3) 12 3_556 ?
O5 Zr02 Zr01 34.9(2) . 3_556 ?
O1 Zr02 Zr01 110.3(3) 12 3_556 ?
O1 Zr02 Zr01 74.6(3) . 3_556 ?
O3 Zr02 Zr01 111.6(4) 13_556 3_556 ?
O3 Zr02 Zr01 167.0(3) 8_456 3_556 ?
Zr03 Zr02 Zr01 91.95(6) . 3_556 ?
Zr03 Zr02 Zr01 61.21(5) 3_556 3_556 ?
Zr01 Zr02 Zr01 60.93(10) . 3_556 ?
O7 Zr03 O7 64.9(8) . 10_556 ?
O7 Zr03 O6 70.8(5) . . ?
O7 Zr03 O6 106.4(6) 10_556 . ?
O7 Zr03 O6 106.4(6) . 10_556 ?
O7 Zr03 O6 70.8(5) 10_556 10_556 ?
O6 Zr03 O6 69.4(5) . 10_556 ?
O7 Zr03 O9 147.4(4) . . ?
O7 Zr03 O9 147.4(4) 10_556 . ?
O6 Zr03 O9 89.4(5) . . ?
O6 Zr03 O9 89.4(5) 10_556 . ?
O7 Zr03 O8 87.9(7) . . ?
O7 Zr03 O8 87.9(7) 10_556 . ?
O6 Zr03 O8 145.1(3) . . ?
O6 Zr03 O8 145.1(3) 10_556 . ?
O9 Zr03 O8 95.1(8) . . ?
O7 Zr03 O4 79.0(6) . 8_456 ?
O7 Zr03 O4 139.9(6) 10_556 8_456 ?
O6 Zr03 O4 75.5(4) . 8_456 ?
O6 Zr03 O4 139.8(5) 10_556 8_456 ?
O9 Zr03 O4 71.0(5) . 8_456 ?
O8 Zr03 O4 73.4(4) . 8_456 ?
O7 Zr03 O4 139.9(6) . 15_454 ?
O7 Zr03 O4 79.0(6) 10_556 15_454 ?
O6 Zr03 O4 139.8(5) . 15_454 ?
O6 Zr03 O4 75.5(4) 10_556 15_454 ?
O9 Zr03 O4 71.0(5) . 15_454 ?
O8 Zr03 O4 73.4(4) . 15_454 ?
O4 Zr03 O4 126.0(7) 8_456 15_454 ?
O7 Zr03 Zr02 85.7(4) . 10_556 ?
O7 Zr03 Zr02 34.5(4) 10_556 10_556 ?
O6 Zr03 Zr02 89.3(3) . 10_556 ?
O6 Zr03 Zr02 36.3(3) 10_556 10_556 ?
O9 Zr03 Zr02 120.6(3) . 10_556 ?
O8 Zr03 Zr02 117.1(4) . 10_556 ?
O4 Zr03 Zr02 161.2(4) 8_456 10_556 ?
O4 Zr03 Zr02 72.8(3) 15_454 10_556 ?
O7 Zr03 Zr02 34.5(4) . . ?
O7 Zr03 Zr02 85.7(4) 10_556 . ?
O6 Zr03 Zr02 36.3(3) . . ?
O6 Zr03 Zr02 89.3(3) 10_556 . ?
O9 Zr03 Zr02 120.6(3) . . ?
O8 Zr03 Zr02 117.1(4) . . ?
O4 Zr03 Zr02 72.8(3) 8_456 . ?
O4 Zr03 Zr02 161.2(4) 15_454 . ?
Zr02 Zr03 Zr02 88.45(8) 10_556 . ?
O7 Zr03 Zr03 32.6(4) . 3_556 ?
O7 Zr03 Zr03 32.6(4) 10_556 3_556 ?
O6 Zr03 Zr03 90.7(4) . 3_556 ?
O6 Zr03 Zr03 90.7(4) 10_556 3_556 ?
O9 Zr03 Zr03 179.9(4) . 3_556 ?
O8 Zr03 Zr03 84.7(6) . 3_556 ?
O4 Zr03 Zr03 108.9(4) 8_456 3_556 ?
O4 Zr03 Zr03 108.9(4) 15_454 3_556 ?
Zr02 Zr03 Zr03 59.44(5) 10_556 3_556 ?
Zr02 Zr03 Zr03 59.44(5) . 3_556 ?
O7 Zr03 Zr01 87.7(4) . . ?
O7 Zr03 Zr01 87.7(4) 10_556 . ?
O6 Zr03 Zr01 34.7(2) . . ?
O6 Zr03 Zr01 34.7(2) 10_556 . ?
O9 Zr03 Zr01 90.0(5) . . ?
O8 Zr03 Zr01 174.9(6) . . ?
O4 Zr03 Zr01 108.5(3) 8_456 . ?
O4 Zr03 Zr01 108.5(3) 15_454 . ?
Zr02 Zr03 Zr01 59.75(6) 10_556 . ?
Zr02 Zr03 Zr01 59.75(6) . . ?
Zr03 Zr03 Zr01 90.13(8) 3_556 . ?

_refine_diff_density_max         1.274
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.128



####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1555417'
_audit_update_record             
;
2017-06-11 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_audit_creation_date             2017-06-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_shelxl_version_number           2014-1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '0.13(C320 H168 N8 O128 Zr24)'
_chemical_formula_sum            'C40 H21 N O16 Zr3'
_chemical_formula_weight         1045.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Zr C O N H'
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'
N N 0.0311 0.0180 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   22.2490(6)
_cell_length_b                   31.0425(8)
_cell_length_c                   33.0217(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     22806.9(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5390
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.9620
_cell_measurement_theta_min      3.5990
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81454
_exptl_absorpt_correction_type   multi-scan
_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.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    0.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            34915
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.072
_diffrn_reflns_theta_min         3.625
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -96.00   -2.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605  125.0000 -150.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega  -49.00   33.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.5605   37.0000  150.0000 82

#__ type_ start__ end____ width___ exp.time_
  3 omega    1.00   57.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5605  -99.0000   60.0000 56

#__ type_ start__ end____ width___ exp.time_
  4 omega   28.00   54.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       41.5605 -125.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
  5 omega   30.00   70.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -30.0000   90.0000 40

#__ type_ start__ end____ width___ exp.time_
  6 omega   34.00   95.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -45.0000 -180.0000 61

#__ type_ start__ end____ width___ exp.time_
  7 omega  136.00  170.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  125.0000   60.0000 34

#__ type_ start__ end____ width___ exp.time_
  8 omega  142.00  176.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759   61.0000  -30.0000 34

#__ type_ start__ end____ width___ exp.time_
  9 omega   30.00   90.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759  -30.0000    0.0000 60

#__ type_ start__ end____ width___ exp.time_
 10 omega   79.00  134.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8759   61.0000  -30.0000 55
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0283014000
_diffrn_orient_matrix_UB_12      -0.0192357000
_diffrn_orient_matrix_UB_13      0.0385895000
_diffrn_orient_matrix_UB_21      -0.0616790000
_diffrn_orient_matrix_UB_22      0.0182277000
_diffrn_orient_matrix_UB_23      -0.0124355000
_diffrn_orient_matrix_UB_31      -0.0139730000
_diffrn_orient_matrix_UB_32      -0.0419390000
_diffrn_orient_matrix_UB_33      -0.0230523000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6827
_reflns_number_total             10851
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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_collection       
;
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_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         3.779
_refine_diff_density_min         -1.292
_refine_diff_density_rms         0.164
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         10851
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0780
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1610P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2297
_refine_ls_wR_factor_ref         0.2549
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
3.a Riding coordinates:
 N1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C4(H4), C16(H16), C3(H3), C6(H6), C20(H20), C12(H12), C17(H17),
 C10(H10), C19(H19)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.5000 0.29344(2) 0.42539(2) 0.01924(19) Uani 1 2 d S T P . .
Zr2 Zr 0.57937(3) 0.35023(2) 0.5000 0.0242(2) Uani 1 2 d S T P . .
Zr3 Zr 0.57815(4) 0.23666(3) 0.5000 0.0345(2) Uani 1 2 d S T P . .
O1 O 0.43942(19) 0.33546(13) 0.39172(11) 0.0254(9) Uani 1 1 d . . . . .
O2 O 0.3884(3) 0.37372(18) 0.43831(13) 0.0493(14) Uani 1 1 d . . . . .
O4 O 0.5692(4) 0.4207(2) 0.5000 0.056(2) Uani 1 2 d S T P . .
O3 O 0.5000 0.3495(3) 0.4636(2) 0.062(3) Uani 1 2 d S T P . .
O6 O 0.5793(3) 0.29368(16) 0.46349(16) 0.0590(18) Uani 1 1 d . . . . .
O8 O 0.5454(4) 0.1659(2) 0.5000 0.0517(19) Uani 1 2 d S TU P . .
O9 O 0.6772(4) 0.2430(4) 0.5000 0.074(3) Uani 1 2 d S T P . .
O7 O 0.5000 0.2381(3) 0.4631(3) 0.077(3) Uani 1 2 d S T P . .
N1 N 0.2513(4) 0.5000 0.2873(2) 0.0349(18) Uani 1 2 d S T P . .
H1 H 0.2436 0.5000 0.3128 0.042 Uiso 1 2 d RS T P . .
O5 O 0.6766(4) 0.3449(4) 0.5000 0.083(3) Uani 1 2 d S T P . .
C2 C 0.3590(3) 0.3778(2) 0.36996(18) 0.0349(15) Uani 1 1 d . . . . .
C7 C 0.3126(3) 0.4066(2) 0.3776(2) 0.0380(16) Uani 1 1 d . . . . .
H7 H 0.3062 0.4161 0.4040 0.046 Uiso 1 1 calc R . . . .
C1 C 0.3987(3) 0.3612(2) 0.40279(17) 0.0319(14) Uani 1 1 d . . . . .
C5 C 0.2831(4) 0.4059(2) 0.30729(19) 0.0371(16) Uani 1 1 d . . . . .
C4 C 0.3287(4) 0.3768(2) 0.29952(19) 0.0420(18) Uani 1 1 d . . . . .
H4 H 0.3337 0.3663 0.2734 0.050 Uiso 1 1 calc R . . . .
C16 C 0.1368(4) 0.3322(2) 0.1961(2) 0.048(2) Uani 1 1 d . . . . .
H16 H 0.1332 0.3263 0.2236 0.058 Uiso 1 1 calc R . . . .
C3 C 0.3675(4) 0.3629(2) 0.33004(19) 0.0431(18) Uani 1 1 d . . . . .
H3 H 0.3987 0.3441 0.3241 0.052 Uiso 1 1 calc R . . . .
C6 C 0.2758(3) 0.4214(2) 0.34721(18) 0.0357(15) Uani 1 1 d . . . . .
H6 H 0.2461 0.4416 0.3529 0.043 Uiso 1 1 calc R . . . .
C15 C 0.1633(4) 0.3700(2) 0.1838(2) 0.0449(19) Uani 1 1 d . . . . .
C13 C 0.1961(4) 0.47675(19) 0.23319(19) 0.0374(17) Uani 1 1 d . . . . .
C18 C 0.1216(4) 0.3109(2) 0.12647(19) 0.0425(18) Uani 1 1 d . . . . .
C8 C 0.2305(3) 0.4631(2) 0.26648(19) 0.0352(15) Uani 1 1 d . . . . .
C20 C 0.1685(4) 0.3774(2) 0.1421(2) 0.0458(19) Uani 1 1 d . . . . .
H20 H 0.1862 0.4029 0.1333 0.055 Uiso 1 1 calc R . . . .
C12 C 0.1730(4) 0.4462(2) 0.20639(19) 0.0397(18) Uani 1 1 d . . . . .
H12 H 0.1497 0.4548 0.1844 0.048 Uiso 1 1 calc R . . . .
C17 C 0.1154(4) 0.3025(3) 0.1679(2) 0.051(2) Uani 1 1 d . . . . .
H17 H 0.0970 0.2772 0.1766 0.061 Uiso 1 1 calc R . . . .
C10 C 0.2190(4) 0.3909(2) 0.2467(2) 0.0407(17) Uani 1 1 d . . . . .
H10 H 0.2254 0.3617 0.2514 0.049 Uiso 1 1 calc R . . . .
C11 C 0.1853(4) 0.4028(2) 0.2129(2) 0.0463(19) Uani 1 1 d . . . . .
C9 C 0.2435(4) 0.4203(2) 0.2737(2) 0.0373(16) Uani 1 1 d . . . . .
C19 C 0.1485(4) 0.3489(2) 0.1142(2) 0.050(2) Uani 1 1 d . . . . .
H19 H 0.1529 0.3549 0.0868 0.059 Uiso 1 1 calc R . . . .
O0AA O 0.4389(2) 0.24893(14) 0.39188(12) 0.0338(10) Uani 1 1 d . . . . .
O1AA O 0.6102(3) 0.21186(17) 0.55934(14) 0.0583(17) Uani 1 1 d . . . . .
C0AA C 0.0960(4) 0.2810(2) 0.09589(18) 0.0390(17) 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
Zr1 Zr2 3.5065(7) . ?
Zr1 Zr2 3.5064(7) 3_656 ?
Zr1 Zr3 3.4927(8) 3_656 ?
Zr1 Zr3 3.4928(8) . ?
Zr1 O1 2.180(4) . ?
Zr1 O1 2.180(4) 12_655 ?
Zr1 O3 2.151(7) . ?
Zr1 O6 2.167(5) 12_655 ?
Zr1 O6 2.167(5) . ?
Zr1 O7 2.122(8) . ?
Zr1 O0AA 2.232(4) 12_655 ?
Zr1 O0AA 2.232(4) . ?
Zr2 Zr1 3.5064(7) 10_556 ?
Zr2 Zr2 3.5319(14) 3_656 ?
Zr2 Zr3 3.5255(11) . ?
Zr2 O2 2.280(4) 3_656 ?
Zr2 O2 2.280(4) 12_655 ?
Zr2 O4 2.200(8) . ?
Zr2 O3 2.136(4) 10_556 ?
Zr2 O3 2.136(4) . ?
Zr2 O6 2.129(5) 10_556 ?
Zr2 O6 2.129(5) . ?
Zr2 O5 2.169(8) . ?
Zr3 Zr1 3.4928(8) 10_556 ?
Zr3 Zr3 3.4773(18) 3_656 ?
Zr3 O6 2.142(5) 10_556 ?
Zr3 O6 2.142(5) . ?
Zr3 O8 2.313(8) . ?
Zr3 O9 2.213(9) . ?
Zr3 O7 2.123(5) 10_556 ?
Zr3 O7 2.123(5) . ?
Zr3 O1AA 2.223(5) 10_556 ?
Zr3 O1AA 2.223(5) . ?
O1 C1 1.263(8) . ?
O2 Zr2 2.280(4) 3_656 ?
O2 C1 1.256(7) . ?
O3 Zr2 2.136(4) 3_656 ?
O7 Zr3 2.123(5) 3_656 ?
N1 H1 0.8600 . ?
N1 C8 1.415(7) 11_565 ?
N1 C8 1.415(7) . ?
C2 C7 1.389(10) . ?
C2 C1 1.490(8) . ?
C2 C3 1.409(9) . ?
C7 H7 0.9300 . ?
C7 C6 1.374(9) . ?
C5 C4 1.382(10) . ?
C5 C6 1.412(9) . ?
C5 C9 1.487(9) . ?
C4 H4 0.9300 . ?
C4 C3 1.395(9) . ?
C16 H16 0.9300 . ?
C16 C15 1.377(10) . ?
C16 C17 1.394(9) . ?
C3 H3 0.9300 . ?
C6 H6 0.9300 . ?
C15 C20 1.398(10) . ?
C15 C11 1.483(9) . ?
C13 C13 1.443(12) 11_565 ?
C13 C8 1.405(8) . ?
C13 C12 1.395(8) . ?
C18 C17 1.401(9) . ?
C18 C19 1.384(10) . ?
C18 C0AA 1.484(9) . ?
C8 C9 1.379(8) . ?
C20 H20 0.9300 . ?
C20 C19 1.353(9) . ?
C12 H12 0.9300 . ?
C12 C11 1.392(9) . ?
C17 H17 0.9300 . ?
C10 H10 0.9300 . ?
C10 C11 1.396(10) . ?
C10 C9 1.386(9) . ?
C19 H19 0.9300 . ?
O0AA C0AA 1.276(8) 13 ?
O1AA C0AA 1.267(8) 15 ?
C0AA O0AA 1.276(8) 13 ?
C0AA O1AA 1.267(8) 15_454 ?

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
Zr2 Zr1 Zr2 60.48(2) 3_656 . ?
Zr3 Zr1 Zr2 90.503(18) . 3_656 ?
Zr3 Zr1 Zr2 60.489(19) . . ?
Zr3 Zr1 Zr2 90.503(18) 3_656 . ?
Zr3 Zr1 Zr2 60.486(19) 3_656 3_656 ?
Zr3 Zr1 Zr3 59.71(3) 3_656 . ?
O1 Zr1 Zr2 111.65(10) 12_655 3_656 ?
O1 Zr1 Zr2 75.31(10) . 3_656 ?
O1 Zr1 Zr2 111.65(10) . . ?
O1 Zr1 Zr2 75.30(10) 12_655 . ?
O1 Zr1 Zr3 110.73(11) . 3_656 ?
O1 Zr1 Zr3 165.76(10) 12_655 3_656 ?
O1 Zr1 Zr3 165.77(10) . . ?
O1 Zr1 Zr3 110.73(11) 12_655 . ?
O1 Zr1 O1 76.4(2) 12_655 . ?
O1 Zr1 O0AA 74.99(16) . . ?
O1 Zr1 O0AA 74.99(16) 12_655 12_655 ?
O1 Zr1 O0AA 119.60(15) 12_655 . ?
O1 Zr1 O0AA 119.59(15) . 12_655 ?
O3 Zr1 Zr2 34.97(12) . 3_656 ?
O3 Zr1 Zr2 34.97(12) . . ?
O3 Zr1 Zr3 89.7(2) . . ?
O3 Zr1 Zr3 89.7(2) . 3_656 ?
O3 Zr1 O1 79.3(2) . . ?
O3 Zr1 O1 79.3(2) . 12_655 ?
O3 Zr1 O6 69.90(19) . 12_655 ?
O3 Zr1 O6 69.90(19) . . ?
O3 Zr1 O0AA 142.40(13) . 12_655 ?
O3 Zr1 O0AA 142.40(12) . . ?
O6 Zr1 Zr2 34.95(14) 12_655 3_656 ?
O6 Zr1 Zr2 90.03(17) 12_655 . ?
O6 Zr1 Zr2 90.03(17) . 3_656 ?
O6 Zr1 Zr2 34.95(14) . . ?
O6 Zr1 Zr3 35.60(14) 12_655 3_656 ?
O6 Zr1 Zr3 89.87(17) . 3_656 ?
O6 Zr1 Zr3 89.86(17) 12_655 . ?
O6 Zr1 Zr3 35.61(14) . . ?
O6 Zr1 O1 77.9(2) 12_655 . ?
O6 Zr1 O1 142.87(17) 12_655 12_655 ?
O6 Zr1 O1 142.87(17) . . ?
O6 Zr1 O1 77.9(2) . 12_655 ?
O6 Zr1 O6 109.0(4) . 12_655 ?
O6 Zr1 O0AA 78.1(2) 12_655 . ?
O6 Zr1 O0AA 141.80(18) . . ?
O6 Zr1 O0AA 78.1(2) . 12_655 ?
O6 Zr1 O0AA 141.80(18) 12_655 12_655 ?
O7 Zr1 Zr2 89.7(3) . 3_656 ?
O7 Zr1 Zr2 89.7(3) . . ?
O7 Zr1 Zr3 34.64(15) . . ?
O7 Zr1 Zr3 34.64(15) . 3_656 ?
O7 Zr1 O1 141.60(11) . 12_655 ?
O7 Zr1 O1 141.60(11) . . ?
O7 Zr1 O3 108.1(4) . . ?
O7 Zr1 O6 70.2(2) . 12_655 ?
O7 Zr1 O6 70.2(2) . . ?
O7 Zr1 O0AA 77.9(3) . 12_655 ?
O7 Zr1 O0AA 77.9(3) . . ?
O0AA Zr1 Zr2 165.09(11) 12_655 3_656 ?
O0AA Zr1 Zr2 110.66(12) . 3_656 ?
O0AA Zr1 Zr2 110.67(12) 12_655 . ?
O0AA Zr1 Zr2 165.08(11) . . ?
O0AA Zr1 Zr3 74.59(11) 12_655 . ?
O0AA Zr1 Zr3 109.90(12) . . ?
O0AA Zr1 Zr3 74.58(11) . 3_656 ?
O0AA Zr1 Zr3 109.91(12) 12_655 3_656 ?
O0AA Zr1 O0AA 75.0(2) 12_655 . ?
Zr1 Zr2 Zr1 89.27(2) 10_556 . ?
Zr1 Zr2 Zr2 59.759(12) . 3_656 ?
Zr1 Zr2 Zr2 59.758(12) 10_556 3_656 ?
Zr1 Zr2 Zr3 59.564(17) 10_556 . ?
Zr1 Zr2 Zr3 59.564(17) . . ?
Zr3 Zr2 Zr2 89.56(2) . 3_656 ?
O2 Zr2 Zr1 161.30(12) 3_656 . ?
O2 Zr2 Zr1 72.03(12) 12_655 . ?
O2 Zr2 Zr1 72.03(12) 3_656 10_556 ?
O2 Zr2 Zr1 161.30(12) 12_655 10_556 ?
O2 Zr2 Zr2 108.34(14) 3_656 3_656 ?
O2 Zr2 Zr2 108.34(14) 12_655 3_656 ?
O2 Zr2 Zr3 108.81(14) 3_656 . ?
O2 Zr2 Zr3 108.81(14) 12_655 . ?
O2 Zr2 O2 126.7(2) 3_656 12_655 ?
O4 Zr2 Zr1 116.64(15) . . ?
O4 Zr2 Zr1 116.64(15) . 10_556 ?
O4 Zr2 Zr2 84.1(2) . 3_656 ?
O4 Zr2 Zr3 173.7(2) . . ?
O4 Zr2 O2 73.38(17) . 12_655 ?
O4 Zr2 O2 73.38(17) . 3_656 ?
O3 Zr2 Zr1 35.3(2) . . ?
O3 Zr2 Zr1 88.5(2) 10_556 . ?
O3 Zr2 Zr1 35.2(2) 10_556 10_556 ?
O3 Zr2 Zr1 88.5(2) . 10_556 ?
O3 Zr2 Zr2 34.22(16) 10_556 3_656 ?
O3 Zr2 Zr2 34.22(16) . 3_656 ?
O3 Zr2 Zr3 89.1(3) . . ?
O3 Zr2 Zr3 89.0(3) 10_556 . ?
O3 Zr2 O2 140.0(2) 10_556 12_655 ?
O3 Zr2 O2 76.2(2) . 12_655 ?
O3 Zr2 O2 76.2(2) 10_556 3_656 ?
O3 Zr2 O2 140.0(2) . 3_656 ?
O3 Zr2 O4 85.7(3) . . ?
O3 Zr2 O4 85.7(3) 10_556 . ?
O3 Zr2 O3 68.4(3) . 10_556 ?
O3 Zr2 O5 145.45(16) . . ?
O3 Zr2 O5 145.45(16) 10_556 . ?
O6 Zr2 Zr1 35.67(16) 10_556 10_556 ?
O6 Zr2 Zr1 89.03(17) 10_556 . ?
O6 Zr2 Zr1 35.67(16) . . ?
O6 Zr2 Zr1 89.04(17) . 10_556 ?
O6 Zr2 Zr2 89.97(19) . 3_656 ?
O6 Zr2 Zr2 89.97(19) 10_556 3_656 ?
O6 Zr2 Zr3 34.48(14) 10_556 . ?
O6 Zr2 Zr3 34.49(14) . . ?
O6 Zr2 O2 76.0(2) . 12_655 ?
O6 Zr2 O2 140.3(2) 10_556 12_655 ?
O6 Zr2 O2 76.0(2) 10_556 3_656 ?
O6 Zr2 O2 140.3(2) . 3_656 ?
O6 Zr2 O4 145.07(13) 10_556 . ?
O6 Zr2 O4 145.07(13) . . ?
O6 Zr2 O3 70.9(3) 10_556 10_556 ?
O6 Zr2 O3 108.0(3) 10_556 . ?
O6 Zr2 O3 108.0(3) . 10_556 ?
O6 Zr2 O3 70.9(3) . . ?
O6 Zr2 O6 69.0(3) 10_556 . ?
O6 Zr2 O5 86.4(3) 10_556 . ?
O6 Zr2 O5 86.4(3) . . ?
O5 Zr2 Zr1 117.6(2) . 10_556 ?
O5 Zr2 Zr1 117.6(2) . . ?
O5 Zr2 Zr2 175.6(3) . 3_656 ?
O5 Zr2 Zr3 86.1(3) . . ?
O5 Zr2 O2 73.18(19) . 12_655 ?
O5 Zr2 O2 73.18(19) . 3_656 ?
O5 Zr2 O4 100.3(4) . . ?
Zr1 Zr3 Zr1 89.72(3) 10_556 . ?
Zr1 Zr3 Zr2 59.946(17) 10_556 . ?
Zr1 Zr3 Zr2 59.948(17) . . ?
Zr3 Zr3 Zr1 60.145(15) 3_656 . ?
Zr3 Zr3 Zr1 60.145(15) 3_656 10_556 ?
Zr3 Zr3 Zr2 90.441(19) 3_656 . ?
O6 Zr3 Zr1 36.10(16) 10_556 10_556 ?
O6 Zr3 Zr1 89.20(17) 10_556 . ?
O6 Zr3 Zr1 89.20(17) . 10_556 ?
O6 Zr3 Zr1 36.10(16) . . ?
O6 Zr3 Zr2 34.26(14) 10_556 . ?
O6 Zr3 Zr2 34.26(14) . . ?
O6 Zr3 Zr3 90.70(18) 10_556 3_656 ?
O6 Zr3 Zr3 90.70(18) . 3_656 ?
O6 Zr3 O6 68.5(3) 10_556 . ?
O6 Zr3 O8 142.01(16) 10_556 . ?
O6 Zr3 O8 142.01(16) . . ?
O6 Zr3 O9 85.1(3) . . ?
O6 Zr3 O9 85.1(3) 10_556 . ?
O6 Zr3 O1AA 141.1(2) 10_556 10_556 ?
O6 Zr3 O1AA 77.6(2) . 10_556 ?
O6 Zr3 O1AA 141.1(2) . . ?
O6 Zr3 O1AA 77.6(2) 10_556 . ?
O8 Zr3 Zr1 108.78(14) . 10_556 ?
O8 Zr3 Zr1 108.78(14) . . ?
O8 Zr3 Zr2 162.1(2) . . ?
O8 Zr3 Zr3 71.6(2) . 3_656 ?
O9 Zr3 Zr1 116.80(18) . . ?
O9 Zr3 Zr1 116.80(18) . 10_556 ?
O9 Zr3 Zr2 84.4(3) . . ?
O9 Zr3 Zr3 174.9(3) . 3_656 ?
O9 Zr3 O8 113.5(3) . . ?
O9 Zr3 O1AA 73.2(2) . 10_556 ?
O9 Zr3 O1AA 73.2(2) . . ?
O7 Zr3 Zr1 89.2(3) . 10_556 ?
O7 Zr3 Zr1 34.6(2) . . ?
O7 Zr3 Zr1 89.2(3) 10_556 . ?
O7 Zr3 Zr1 34.6(2) 10_556 10_556 ?
O7 Zr3 Zr2 89.1(3) . . ?
O7 Zr3 Zr2 89.1(3) 10_556 . ?
O7 Zr3 Zr3 35.0(2) 10_556 3_656 ?
O7 Zr3 Zr3 35.0(2) . 3_656 ?
O7 Zr3 O6 70.7(3) . . ?
O7 Zr3 O6 70.7(3) 10_556 10_556 ?
O7 Zr3 O6 108.4(4) 10_556 . ?
O7 Zr3 O6 108.4(4) . 10_556 ?
O7 Zr3 O8 76.2(3) 10_556 . ?
O7 Zr3 O8 76.2(3) . . ?
O7 Zr3 O9 144.47(19) 10_556 . ?
O7 Zr3 O9 144.47(19) . . ?
O7 Zr3 O7 70.0(4) 10_556 . ?
O7 Zr3 O1AA 76.4(3) . 10_556 ?
O7 Zr3 O1AA 76.4(3) 10_556 . ?
O7 Zr3 O1AA 140.8(3) . . ?
O7 Zr3 O1AA 140.8(3) 10_556 10_556 ?
O1AA Zr3 Zr1 73.29(14) 10_556 . ?
O1AA Zr3 Zr1 73.29(14) . 10_556 ?
O1AA Zr3 Zr1 162.98(14) . . ?
O1AA Zr3 Zr1 162.98(14) 10_556 10_556 ?
O1AA Zr3 Zr2 110.12(15) 10_556 . ?
O1AA Zr3 Zr2 110.12(15) . . ?
O1AA Zr3 Zr3 108.69(18) 10_556 3_656 ?
O1AA Zr3 Zr3 108.69(18) . 3_656 ?
O1AA Zr3 O8 76.84(19) . . ?
O1AA Zr3 O8 76.84(19) 10_556 . ?
O1AA Zr3 O1AA 123.7(3) . 10_556 ?
C1 O1 Zr1 132.4(4) . . ?
C1 O2 Zr2 132.7(4) . 3_656 ?
Zr2 O3 Zr1 109.8(3) . . ?
Zr2 O3 Zr1 109.8(3) 3_656 . ?
Zr2 O3 Zr2 111.6(3) 3_656 . ?
Zr2 O6 Zr1 109.4(3) . . ?
Zr2 O6 Zr3 111.3(2) . . ?
Zr3 O6 Zr1 108.3(3) . . ?
Zr1 O7 Zr3 110.7(3) . 3_656 ?
Zr1 O7 Zr3 110.7(3) . . ?
Zr3 O7 Zr3 110.0(4) 3_656 . ?
C8 N1 H1 114.3 . . ?
C8 N1 H1 114.3 11_565 . ?
C8 N1 C8 108.2(7) . 11_565 ?
C7 C2 C1 122.1(6) . . ?
C7 C2 C3 118.7(6) . . ?
C3 C2 C1 119.3(6) . . ?
C2 C7 H7 119.2 . . ?
C6 C7 C2 121.7(6) . . ?
C6 C7 H7 119.2 . . ?
O1 C1 C2 115.7(5) . . ?
O2 C1 O1 126.7(6) . . ?
O2 C1 C2 117.7(6) . . ?
C4 C5 C6 118.7(6) . . ?
C4 C5 C9 119.6(6) . . ?
C6 C5 C9 121.8(6) . . ?
C5 C4 H4 119.3 . . ?
C5 C4 C3 121.4(6) . . ?
C3 C4 H4 119.3 . . ?
C15 C16 H16 119.5 . . ?
C15 C16 C17 120.9(7) . . ?
C17 C16 H16 119.5 . . ?
C2 C3 H3 120.2 . . ?
C4 C3 C2 119.5(7) . . ?
C4 C3 H3 120.2 . . ?
C7 C6 C5 120.0(7) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C16 C15 C20 117.8(6) . . ?
C16 C15 C11 122.3(6) . . ?
C20 C15 C11 119.9(6) . . ?
C8 C13 C13 107.6(3) . 11_565 ?
C12 C13 C13 132.8(3) . 11_565 ?
C12 C13 C8 119.5(6) . . ?
C17 C18 C0AA 120.7(6) . . ?
C19 C18 C17 119.1(6) . . ?
C19 C18 C0AA 120.0(6) . . ?
C13 C8 N1 108.3(5) . . ?
C9 C8 N1 128.9(6) . . ?
C9 C8 C13 122.6(6) . . ?
C15 C20 H20 118.8 . . ?
C19 C20 C15 122.4(7) . . ?
C19 C20 H20 118.8 . . ?
C13 C12 H12 120.4 . . ?
C11 C12 C13 119.2(6) . . ?
C11 C12 H12 120.4 . . ?
C16 C17 C18 119.7(7) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C11 C10 H10 118.3 . . ?
C9 C10 H10 118.3 . . ?
C9 C10 C11 123.4(6) . . ?
C12 C11 C15 120.0(6) . . ?
C12 C11 C10 119.1(6) . . ?
C10 C11 C15 121.0(6) . . ?
C8 C9 C5 122.9(6) . . ?
C8 C9 C10 116.2(6) . . ?
C10 C9 C5 120.9(6) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.1(7) . . ?
C20 C19 H19 120.0 . . ?
C0AA O0AA Zr1 131.6(4) 13 . ?
C0AA O1AA Zr3 134.4(5) 15 . ?
O0AA C0AA C18 118.2(5) 13 . ?
O1AA C0AA C18 116.3(6) 15_454 . ?
O1AA C0AA O0AA 125.5(6) 15_454 13 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.192 -0.100 -0.922 16145.7 1255.2 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1533346'
_audit_update_record             
;
2017-02-17 deposited with the CCDC.
2018-09-04 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         ?
_chemical_formula_sum            'C56 H27 N O16 Zr3'
_chemical_formula_weight         1243.44

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'
N N 0.0311 0.0180 '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      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'

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

_cell_length_a                   24.6270(8)
_cell_length_b                   36.7534(10)
_cell_length_c                   39.9531(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     36162.6(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6511
_cell_measurement_theta_min      3.4990
_cell_measurement_theta_max      69.7610

_exptl_crystal_description       
; 
'Sat Nov 05 06:37:53 2016' 
;
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.457
_exptl_crystal_F_000             4944
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.570
_shelx_estimated_absorpt_T_min   0.787
_shelx_estimated_absorpt_T_max   0.834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55863
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
'Sat Nov 05 06:37:53 2016' 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_reflns_number            54546
_diffrn_reflns_av_unetI/netI     0.1226
_diffrn_reflns_av_R_equivalents  0.1026
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_theta_min         3.530
_diffrn_reflns_theta_max         66.593
_diffrn_reflns_theta_full        66.593
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             16898
_reflns_number_gt                6967
_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       
; 
'Sat Nov 05 06:37:53 2016' 
;
_computing_cell_refinement       
; 
'Sat Nov 05 06:37:53 2016' 
;
_computing_data_reduction        
; 
'Sat Nov 05 06:37:53 2016' 
;
_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)+(0.1113P)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         16898
_refine_ls_number_parameters     358
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1407
_refine_ls_R_factor_gt           0.0728
_refine_ls_wR_factor_ref         0.2456
_refine_ls_wR_factor_gt          0.2055
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_restrained_S_all      0.931
_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 0.0000 0.26402(2) 0.43857(2) 0.0611(2) Uani 1 2 d S T P . .
Zr2 Zr 0.07209(3) 0.31221(2) 0.5000 0.0731(3) Uani 1 2 d S T P . .
Zr3 Zr 0.07087(3) 0.21593(2) 0.5000 0.0755(3) Uani 1 2 d S T P . .
O3 O 0.44597(17) 0.27316(11) 0.08992(8) 0.0794(12) Uani 1 1 d . . . . .
O1 O 0.05423(16) 0.29942(11) 0.41025(8) 0.0797(11) Uani 1 1 d . . . . .
O4 O 0.40018(19) 0.30350(12) 0.05039(9) 0.1106(16) Uani 1 1 d . . . . .
O5 O 0.0000 0.31329(17) 0.46924(12) 0.106(2) Uani 1 2 d S T P . .
O2 O 0.1006(2) 0.33122(12) 0.44868(8) 0.1158(18) Uani 1 1 d . . . . .
O7 O 0.07204(19) 0.26413(10) 0.52997(9) 0.1059(17) Uani 1 1 d . . . . .
O6 O 0.0000 0.21516(16) 0.46882(13) 0.0974(19) Uani 1 2 d S T P . .
O8 O 0.0675(3) 0.37237(15) 0.5000 0.124(3) Uani 1 2 d S T P . .
O10 O 0.1614(3) 0.2190(2) 0.5000 0.125(2) Uani 1 2 d S T P . .
O11 O 0.0564(3) 0.15641(16) 0.5000 0.144(3) Uani 1 2 d S T P . .
O9 O 0.1602(3) 0.3081(2) 0.5000 0.136(3) Uani 1 2 d S T P . .
N1 N 0.2543(4) 0.5000 0.29632(19) 0.165(5) Uani 1 2 d S T P . .
H1 H 0.2332 0.5000 0.3141 0.198 Uiso 1 2 calc R U P . .
C1 C 0.0887(3) 0.32292(18) 0.41874(14) 0.090(2) Uani 1 1 d . . . . .
C28 C 0.4139(3) 0.29735(19) 0.07991(15) 0.100(2) Uani 1 1 d . . . . .
C2 C 0.1174(3) 0.34221(19) 0.39112(14) 0.110(2) Uani 1 1 d . . . . .
C7 C 0.1576(3) 0.36621(18) 0.39705(15) 0.117(3) Uani 1 1 d . . . . .
H7 H 0.1684 0.3710 0.4195 0.141 Uiso 1 1 calc R U . . .
C25 C 0.3893(3) 0.3227(2) 0.10530(15) 0.122(3) Uani 1 1 d . . . . .
C6 C 0.1839(4) 0.38434(19) 0.37066(17) 0.123(3) Uani 1 1 d . . . . .
C21 C 0.3751(5) 0.3416(2) 0.16268(16) 0.163(4) Uani 1 1 d . . . . .
C17 C 0.2744(5) 0.46897(16) 0.27942(19) 0.199(6) Uani 1 1 d . . . . .
C16 C 0.3074(4) 0.47929(17) 0.25276(18) 0.169(4) Uani 1 1 d . . . . .
C22 C 0.3502(4) 0.3730(2) 0.1514(2) 0.162(4) Uani 1 1 d . . . . .
C5 C 0.1653(5) 0.3758(2) 0.33715(17) 0.155(4) Uani 1 1 d . . . . .
C24 C 0.3964(3) 0.31557(19) 0.13885(16) 0.136(3) Uani 1 1 d . . . . .
H24 H 0.4147 0.2942 0.1461 0.163 Uiso 1 1 calc R U . . .
C12 C 0.2639(5) 0.4327(2) 0.28449(19) 0.191(5) Uani 1 1 d . . . . .
C15 C 0.3271(4) 0.45520(16) 0.22918(18) 0.188(5) Uani 1 1 d . . . . .
H15 H 0.3468 0.4634 0.2102 0.226 Uiso 1 1 calc R U . . .
C26 C 0.3626(4) 0.3553(2) 0.09466(18) 0.167(4) Uani 1 1 d . . . . .
H26 H 0.3586 0.3604 0.0715 0.201 Uiso 1 1 calc R U . . .
C18 C 0.3392(5) 0.3912(2) 0.2098(2) 0.201(5) Uani 1 1 d . . . . .
C14 C 0.3174(5) 0.41995(18) 0.23434(19) 0.203(6) Uani 1 1 d . . . . .
C11 C 0.2270(4) 0.4088(2) 0.37639(18) 0.175(4) Uani 1 1 d . . . . .
H11 H 0.2382 0.4148 0.3984 0.210 Uiso 1 1 calc R U . . .
C23 C 0.3322(5) 0.3989(2) 0.17524(19) 0.192(5) Uani 1 1 d . . . . .
H23 H 0.3157 0.4210 0.1682 0.231 Uiso 1 1 calc R U . . .
C13 C 0.2884(5) 0.40809(18) 0.26320(18) 0.192(5) Uani 1 1 d . . . . .
C9 C 0.2316(5) 0.4154(2) 0.31432(19) 0.167(5) Uani 1 1 d . . . . .
C3 C 0.1010(4) 0.3358(2) 0.35836(15) 0.163(4) Uani 1 1 d . . . . .
H3 H 0.0722 0.3190 0.3547 0.196 Uiso 1 1 calc R U . . .
C19 C 0.3612(5) 0.3593(2) 0.2211(2) 0.215(6) Uani 1 1 d . . . . .
H19 H 0.3622 0.3536 0.2443 0.257 Uiso 1 1 calc R U . . .
C8 C 0.1901(5) 0.3920(2) 0.3065(3) 0.210(6) Uani 1 1 d . . . . .
H8 H 0.1785 0.3867 0.2843 0.252 Uiso 1 1 calc R U . . .
C27 C 0.3428(4) 0.3793(2) 0.11810(19) 0.184(5) Uani 1 1 d . . . . .
H27 H 0.3238 0.4005 0.1110 0.220 Uiso 1 1 calc R U . . .
C4 C 0.1242(4) 0.3523(3) 0.33111(19) 0.196(5) Uani 1 1 d . . . . .
H4 H 0.1120 0.3474 0.3090 0.236 Uiso 1 1 calc R U . . .
C10 C 0.2522(4) 0.4235(2) 0.3488(2) 0.183(5) Uani 1 1 d . . . . .
H10 H 0.2828 0.4390 0.3516 0.220 Uiso 1 1 calc R U . . .
C20 C 0.3827(5) 0.3349(2) 0.1966(2) 0.226(6) Uani 1 1 d . . . . .
H20 H 0.4023 0.3139 0.2035 0.271 Uiso 1 1 calc R U . . .


_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 O6 2.164(5) . ?
Zr1 O7 2.174(4) 10_556 ?
Zr1 O7 2.174(4) 3_556 ?
Zr1 O1 2.181(4) 12 ?
Zr1 O1 2.181(4) . ?
Zr1 O5 2.187(5) . ?
Zr1 O3 2.221(4) 8_455 ?
Zr1 O3 2.221(4) 13 ?
Zr1 Zr3 3.4918(7) . ?
Zr1 Zr3 3.4919(7) 3_556 ?
Zr1 Zr2 3.5088(7) . ?
Zr1 Zr2 3.5088(7) 3_556 ?
Zr2 O7 2.134(4) 10_556 ?
Zr2 O7 2.134(4) . ?
Zr2 O5 2.160(3) 10_556 ?
Zr2 O5 2.160(3) . ?
Zr2 O9 2.175(7) . ?
Zr2 O8 2.214(6) . ?
Zr2 O2 2.277(3) 10_556 ?
Zr2 O2 2.277(3) . ?
Zr2 Zr1 3.5087(7) 10_556 ?
Zr2 Zr3 3.5386(10) . ?
Zr2 Zr2 3.5508(16) 3_556 ?
Zr3 O7 2.138(4) . ?
Zr3 O7 2.139(4) 10_556 ?
Zr3 O6 2.144(3) 10_556 ?
Zr3 O6 2.144(3) . ?
Zr3 O11 2.216(6) . ?
Zr3 O10 2.233(7) . ?
Zr3 O4 2.252(3) 6 ?
Zr3 O4 2.252(3) 13 ?
Zr3 Zr3 3.4905(16) 3_556 ?
Zr3 Zr1 3.4918(7) 10_556 ?
O3 C28 1.255(7) . ?
O3 Zr1 2.221(4) 13 ?
O1 C1 1.258(7) . ?
O4 C28 1.247(7) . ?
O4 Zr3 2.252(3) 13 ?
O5 Zr2 2.160(3) 3_556 ?
O2 C1 1.268(6) . ?
O7 Zr1 2.174(4) 10_556 ?
O6 Zr3 2.145(3) 3_556 ?
N1 C17 1.414(7) 11_565 ?
N1 C17 1.415(7) . ?
N1 H1 0.8800 . ?
C1 C2 1.489(7) . ?
C28 C25 1.506(8) . ?
C2 C7 1.348(8) . ?
C2 C3 1.390(8) . ?
C7 C6 1.405(7) . ?
C7 H7 0.9500 . ?
C25 C24 1.377(8) . ?
C25 C26 1.430(9) . ?
C6 C11 1.409(9) . ?
C6 C5 1.449(10) . ?
C21 C22 1.382(10) . ?
C21 C20 1.389(10) . ?
C21 C24 1.448(8) . ?
C17 C12 1.373(9) . ?
C17 C16 1.393(8) . ?
C16 C15 1.381(8) . ?
C16 C16 1.523(13) 11_565 ?
C22 C27 1.364(10) . ?
C22 C23 1.418(9) . ?
C5 C4 1.354(10) . ?
C5 C8 1.491(9) . ?
C24 H24 0.9500 . ?
C12 C13 1.380(9) . ?
C12 C9 1.567(10) . ?
C15 C14 1.334(8) . ?
C15 H15 0.9500 . ?
C26 C27 1.377(8) . ?
C26 H26 0.9500 . ?
C18 C19 1.367(11) . ?
C18 C23 1.422(11) . ?
C18 C14 1.537(9) . ?
C14 C13 1.425(9) . ?
C11 C10 1.376(8) . ?
C11 H11 0.9500 . ?
C23 H23 0.9500 . ?
C9 C8 1.372(13) . ?
C9 C10 1.498(12) . ?
C3 C4 1.371(9) . ?
C3 H3 0.9500 . ?
C19 C20 1.432(9) . ?
C19 H19 0.9500 . ?
C8 H8 0.9500 . ?
C27 H27 0.9500 . ?
C4 H4 0.9500 . ?
C10 H10 0.9500 . ?
C20 H20 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
O6 Zr1 O7 71.27(13) . 10_556 ?
O6 Zr1 O7 71.27(13) . 3_556 ?
O7 Zr1 O7 109.4(2) 10_556 3_556 ?
O6 Zr1 O1 141.68(11) . 12 ?
O7 Zr1 O1 142.97(14) 10_556 12 ?
O7 Zr1 O1 78.41(15) 3_556 12 ?
O6 Zr1 O1 141.68(11) . . ?
O7 Zr1 O1 78.41(15) 10_556 . ?
O7 Zr1 O1 142.98(14) 3_556 . ?
O1 Zr1 O1 75.5(2) 12 . ?
O6 Zr1 O5 112.0(2) . . ?
O7 Zr1 O5 71.00(12) 10_556 . ?
O7 Zr1 O5 71.00(12) 3_556 . ?
O1 Zr1 O5 78.26(15) 12 . ?
O1 Zr1 O5 78.27(16) . . ?
O6 Zr1 O3 77.04(16) . 8_455 ?
O7 Zr1 O3 141.83(14) 10_556 8_455 ?
O7 Zr1 O3 78.97(15) 3_556 8_455 ?
O1 Zr1 O3 74.60(15) 12 8_455 ?
O1 Zr1 O3 117.90(14) . 8_455 ?
O5 Zr1 O3 142.83(11) . 8_455 ?
O6 Zr1 O3 77.04(16) . 13 ?
O7 Zr1 O3 78.97(15) 10_556 13 ?
O7 Zr1 O3 141.83(14) 3_556 13 ?
O1 Zr1 O3 117.90(14) 12 13 ?
O1 Zr1 O3 74.60(15) . 13 ?
O5 Zr1 O3 142.83(11) . 13 ?
O3 Zr1 O3 73.6(2) 8_455 13 ?
O6 Zr1 Zr3 35.68(8) . . ?
O7 Zr1 Zr3 35.60(10) 10_556 . ?
O7 Zr1 Zr3 90.14(11) 3_556 . ?
O1 Zr1 Zr3 166.56(10) 12 . ?
O1 Zr1 Zr3 111.13(10) . . ?
O5 Zr1 Zr3 91.45(13) . . ?
O3 Zr1 Zr3 110.37(11) 8_455 . ?
O3 Zr1 Zr3 75.49(10) 13 . ?
O6 Zr1 Zr3 35.68(8) . 3_556 ?
O7 Zr1 Zr3 90.15(12) 10_556 3_556 ?
O7 Zr1 Zr3 35.60(10) 3_556 3_556 ?
O1 Zr1 Zr3 111.13(10) 12 3_556 ?
O1 Zr1 Zr3 166.57(10) . 3_556 ?
O5 Zr1 Zr3 91.45(13) . 3_556 ?
O3 Zr1 Zr3 75.49(10) 8_455 3_556 ?
O3 Zr1 Zr3 110.37(11) 13 3_556 ?
Zr3 Zr1 Zr3 59.97(3) . 3_556 ?
O6 Zr1 Zr2 91.62(14) . . ?
O7 Zr1 Zr2 35.09(10) 10_556 . ?
O7 Zr1 Zr2 90.43(11) 3_556 . ?
O1 Zr1 Zr2 111.81(11) 12 . ?
O1 Zr1 Zr2 75.63(10) . . ?
O5 Zr1 Zr2 35.90(8) . . ?
O3 Zr1 Zr2 166.43(10) 8_455 . ?
O3 Zr1 Zr2 111.47(10) 13 . ?
Zr3 Zr1 Zr2 60.725(17) . . ?
Zr3 Zr1 Zr2 90.963(16) 3_556 . ?
O6 Zr1 Zr2 91.62(14) . 3_556 ?
O7 Zr1 Zr2 90.43(11) 10_556 3_556 ?
O7 Zr1 Zr2 35.10(10) 3_556 3_556 ?
O1 Zr1 Zr2 75.63(10) 12 3_556 ?
O1 Zr1 Zr2 111.81(11) . 3_556 ?
O5 Zr1 Zr2 35.90(8) . 3_556 ?
O3 Zr1 Zr2 111.47(10) 8_455 3_556 ?
O3 Zr1 Zr2 166.43(10) 13 3_556 ?
Zr3 Zr1 Zr2 90.962(16) . 3_556 ?
Zr3 Zr1 Zr2 60.728(17) 3_556 3_556 ?
Zr2 Zr1 Zr2 60.79(3) . 3_556 ?
O7 Zr2 O7 68.3(2) 10_556 . ?
O7 Zr2 O5 109.5(2) 10_556 10_556 ?
O7 Zr2 O5 72.28(18) . 10_556 ?
O7 Zr2 O5 72.28(18) 10_556 . ?
O7 Zr2 O5 109.5(2) . . ?
O5 Zr2 O5 69.4(2) 10_556 . ?
O7 Zr2 O9 86.7(2) 10_556 . ?
O7 Zr2 O9 86.7(2) . . ?
O5 Zr2 O9 145.23(10) 10_556 . ?
O5 Zr2 O9 145.23(10) . . ?
O7 Zr2 O8 145.76(10) 10_556 . ?
O7 Zr2 O8 145.76(10) . . ?
O5 Zr2 O8 86.5(2) 10_556 . ?
O5 Zr2 O8 86.5(2) . . ?
O9 Zr2 O8 96.9(3) . . ?
O7 Zr2 O2 139.41(16) 10_556 10_556 ?
O7 Zr2 O2 75.46(15) . 10_556 ?
O5 Zr2 O2 74.65(16) 10_556 10_556 ?
O5 Zr2 O2 139.47(18) . 10_556 ?
O9 Zr2 O2 73.38(15) . 10_556 ?
O8 Zr2 O2 73.10(14) . 10_556 ?
O7 Zr2 O2 75.46(15) 10_556 . ?
O7 Zr2 O2 139.41(16) . . ?
O5 Zr2 O2 139.46(18) 10_556 . ?
O5 Zr2 O2 74.64(16) . . ?
O9 Zr2 O2 73.39(15) . . ?
O8 Zr2 O2 73.10(14) . . ?
O2 Zr2 O2 128.5(2) 10_556 . ?
O7 Zr2 Zr1 88.53(12) 10_556 10_556 ?
O7 Zr2 Zr1 35.86(11) . 10_556 ?
O5 Zr2 Zr1 36.43(14) 10_556 10_556 ?
O5 Zr2 Zr1 89.50(14) . 10_556 ?
O9 Zr2 Zr1 118.01(12) . 10_556 ?
O8 Zr2 Zr1 118.57(12) . 10_556 ?
O2 Zr2 Zr1 71.39(10) 10_556 10_556 ?
O2 Zr2 Zr1 160.15(10) . 10_556 ?
O7 Zr2 Zr1 35.85(11) 10_556 . ?
O7 Zr2 Zr1 88.52(12) . . ?
O5 Zr2 Zr1 89.50(14) 10_556 . ?
O5 Zr2 Zr1 36.42(14) . . ?
O9 Zr2 Zr1 118.01(12) . . ?
O8 Zr2 Zr1 118.57(12) . . ?
O2 Zr2 Zr1 160.15(10) 10_556 . ?
O2 Zr2 Zr1 71.39(10) . . ?
Zr1 Zr2 Zr1 88.76(2) 10_556 . ?
O7 Zr2 Zr3 34.13(10) 10_556 . ?
O7 Zr2 Zr3 34.13(10) . . ?
O5 Zr2 Zr3 90.66(17) 10_556 . ?
O5 Zr2 Zr3 90.66(17) . . ?
O9 Zr2 Zr3 86.49(19) . . ?
O8 Zr2 Zr3 176.58(19) . . ?
O2 Zr2 Zr3 108.02(12) 10_556 . ?
O2 Zr2 Zr3 108.02(12) . . ?
Zr1 Zr2 Zr3 59.401(16) 10_556 . ?
Zr1 Zr2 Zr3 59.400(16) . . ?
O7 Zr2 Zr2 89.97(13) 10_556 3_556 ?
O7 Zr2 Zr2 89.97(13) . 3_556 ?
O5 Zr2 Zr2 34.70(10) 10_556 3_556 ?
O5 Zr2 Zr2 34.70(10) . 3_556 ?
O9 Zr2 Zr2 176.00(19) . 3_556 ?
O8 Zr2 Zr2 87.07(19) . 3_556 ?
O2 Zr2 Zr2 107.94(13) 10_556 3_556 ?
O2 Zr2 Zr2 107.94(13) . 3_556 ?
Zr1 Zr2 Zr2 59.603(13) 10_556 3_556 ?
Zr1 Zr2 Zr2 59.604(13) . 3_556 ?
Zr3 Zr2 Zr2 89.512(18) . 3_556 ?
O7 Zr3 O7 68.09(19) . 10_556 ?
O7 Zr3 O6 72.34(18) . 10_556 ?
O7 Zr3 O6 110.3(2) 10_556 10_556 ?
O7 Zr3 O6 110.3(2) . . ?
O7 Zr3 O6 72.34(18) 10_556 . ?
O6 Zr3 O6 71.0(2) 10_556 . ?
O7 Zr3 O11 145.07(10) . . ?
O7 Zr3 O11 145.07(10) 10_556 . ?
O6 Zr3 O11 81.7(2) 10_556 . ?
O6 Zr3 O11 81.7(2) . . ?
O7 Zr3 O10 86.8(2) . . ?
O7 Zr3 O10 86.8(2) 10_556 . ?
O6 Zr3 O10 144.43(11) 10_556 . ?
O6 Zr3 O10 144.43(11) . . ?
O11 Zr3 O10 102.1(3) . . ?
O7 Zr3 O4 75.99(15) . 6 ?
O7 Zr3 O4 139.38(17) 10_556 6 ?
O6 Zr3 O4 74.58(17) 10_556 6 ?
O6 Zr3 O4 140.61(18) . 6 ?
O11 Zr3 O4 74.80(15) . 6 ?
O10 Zr3 O4 72.54(14) . 6 ?
O7 Zr3 O4 139.38(17) . 13 ?
O7 Zr3 O4 75.99(15) 10_556 13 ?
O6 Zr3 O4 140.61(18) 10_556 13 ?
O6 Zr3 O4 74.58(17) . 13 ?
O11 Zr3 O4 74.80(15) . 13 ?
O10 Zr3 O4 72.54(14) . 13 ?
O4 Zr3 O4 126.8(2) 6 13 ?
O7 Zr3 Zr3 90.78(13) . 3_556 ?
O7 Zr3 Zr3 90.78(13) 10_556 3_556 ?
O6 Zr3 Zr3 35.53(11) 10_556 3_556 ?
O6 Zr3 Zr3 35.53(11) . 3_556 ?
O11 Zr3 Zr3 80.8(2) . 3_556 ?
O10 Zr3 Zr3 177.10(18) . 3_556 ?
O4 Zr3 Zr3 108.45(12) 6 3_556 ?
O4 Zr3 Zr3 108.45(12) 13 3_556 ?
O7 Zr3 Zr1 36.28(12) . 10_556 ?
O7 Zr3 Zr1 88.90(11) 10_556 10_556 ?
O6 Zr3 Zr1 36.06(14) 10_556 10_556 ?
O6 Zr3 Zr1 90.47(14) . 10_556 ?
O11 Zr3 Zr1 114.80(13) . 10_556 ?
O10 Zr3 Zr1 118.26(11) . 10_556 ?
O4 Zr3 Zr1 71.97(11) 6 10_556 ?
O4 Zr3 Zr1 161.28(11) 13 10_556 ?
Zr3 Zr3 Zr1 60.014(13) 3_556 10_556 ?
O7 Zr3 Zr1 88.91(11) . . ?
O7 Zr3 Zr1 36.28(11) 10_556 . ?
O6 Zr3 Zr1 90.47(14) 10_556 . ?
O6 Zr3 Zr1 36.06(14) . . ?
O11 Zr3 Zr1 114.79(13) . . ?
O10 Zr3 Zr1 118.26(11) . . ?
O4 Zr3 Zr1 161.28(11) 6 . ?
O4 Zr3 Zr1 71.97(11) 13 . ?
Zr3 Zr3 Zr1 60.014(13) 3_556 . ?
Zr1 Zr3 Zr1 89.31(2) 10_556 . ?
O7 Zr3 Zr2 34.05(10) . . ?
O7 Zr3 Zr2 34.05(10) 10_556 . ?
O6 Zr3 Zr2 91.15(16) 10_556 . ?
O6 Zr3 Zr2 91.15(16) . . ?
O11 Zr3 Zr2 171.2(2) . . ?
O10 Zr3 Zr2 86.61(18) . . ?
O4 Zr3 Zr2 108.33(12) 6 . ?
O4 Zr3 Zr2 108.33(12) 13 . ?
Zr3 Zr3 Zr2 90.491(18) 3_556 . ?
Zr1 Zr3 Zr2 59.873(16) 10_556 . ?
Zr1 Zr3 Zr2 59.875(16) . . ?
C28 O3 Zr1 130.5(3) . 13 ?
C1 O1 Zr1 133.1(3) . . ?
C28 O4 Zr3 134.6(4) . 13 ?
Zr2 O5 Zr2 110.6(2) 3_556 . ?
Zr2 O5 Zr1 107.67(19) 3_556 . ?
Zr2 O5 Zr1 107.67(19) . . ?
C1 O2 Zr2 134.8(4) . . ?
Zr2 O7 Zr3 111.82(16) . . ?
Zr2 O7 Zr1 109.05(18) . 10_556 ?
Zr3 O7 Zr1 108.12(18) . 10_556 ?
Zr3 O6 Zr3 108.9(2) . 3_556 ?
Zr3 O6 Zr1 108.26(19) . . ?
Zr3 O6 Zr1 108.27(19) 3_556 . ?
C17 N1 C17 107.5(7) 11_565 . ?
C17 N1 H1 126.3 11_565 . ?
C17 N1 H1 126.3 . . ?
O1 C1 O2 125.1(5) . . ?
O1 C1 C2 116.5(5) . . ?
O2 C1 C2 118.4(6) . . ?
O4 C28 O3 126.9(5) . . ?
O4 C28 C25 114.6(6) . . ?
O3 C28 C25 118.5(6) . . ?
C7 C2 C3 119.4(6) . . ?
C7 C2 C1 122.0(6) . . ?
C3 C2 C1 118.6(7) . . ?
C2 C7 C6 121.1(6) . . ?
C2 C7 H7 119.4 . . ?
C6 C7 H7 119.4 . . ?
C24 C25 C26 120.5(7) . . ?
C24 C25 C28 119.1(7) . . ?
C26 C25 C28 120.2(6) . . ?
C7 C6 C11 121.8(7) . . ?
C7 C6 C5 116.5(7) . . ?
C11 C6 C5 121.7(7) . . ?
C22 C21 C20 121.7(7) . . ?
C22 C21 C24 119.9(7) . . ?
C20 C21 C24 118.3(8) . . ?
C12 C17 C16 119.2(6) . . ?
C12 C17 N1 130.3(7) . . ?
C16 C17 N1 110.5(6) . . ?
C15 C16 C17 123.6(6) . . ?
C15 C16 C16 129.9(4) . 11_565 ?
C17 C16 C16 105.8(4) . 11_565 ?
C27 C22 C21 121.3(7) . . ?
C27 C22 C23 119.9(8) . . ?
C21 C22 C23 118.8(8) . . ?
C4 C5 C6 122.6(7) . . ?
C4 C5 C8 114.5(8) . . ?
C6 C5 C8 122.9(9) . . ?
C25 C24 C21 117.8(7) . . ?
C25 C24 H24 121.1 . . ?
C21 C24 H24 121.1 . . ?
C17 C12 C13 117.6(7) . . ?
C17 C12 C9 127.0(6) . . ?
C13 C12 C9 115.1(6) . . ?
C14 C15 C16 117.0(6) . . ?
C14 C15 H15 121.5 . . ?
C16 C15 H15 121.5 . . ?
C27 C26 C25 119.8(7) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C19 C18 C23 122.6(8) . . ?
C19 C18 C14 121.2(8) . . ?
C23 C18 C14 116.0(8) . . ?
C15 C14 C13 120.8(6) . . ?
C15 C14 C18 120.5(7) . . ?
C13 C14 C18 118.7(6) . . ?
C10 C11 C6 117.4(8) . . ?
C10 C11 H11 121.3 . . ?
C6 C11 H11 121.3 . . ?
C22 C23 C18 118.7(8) . . ?
C22 C23 H23 120.7 . . ?
C18 C23 H23 120.7 . . ?
C12 C13 C14 121.2(6) . . ?
C8 C9 C10 125.9(8) . . ?
C8 C9 C12 117.3(9) . . ?
C10 C9 C12 116.6(10) . . ?
C4 C3 C2 123.5(8) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C18 C19 C20 117.4(8) . . ?
C18 C19 H19 121.3 . . ?
C20 C19 H19 121.3 . . ?
C9 C8 C5 111.6(10) . . ?
C9 C8 H8 124.2 . . ?
C5 C8 H8 124.2 . . ?
C22 C27 C26 120.5(8) . . ?
C22 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C5 C4 C3 116.9(8) . . ?
C5 C4 H4 121.5 . . ?
C3 C4 H4 121.5 . . ?
C11 C10 C9 120.4(9) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C21 C20 C19 120.3(8) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?

_refine_diff_density_max         0.903
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.063



####################################################################### 
# 
# 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_exp_481
_database_code_depnum_ccdc_archive 'CCDC 1533347'
_audit_update_record             
;
2017-02-17 deposited with the CCDC.
2018-09-04 downloaded from the CCDC.
;
_audit_creation_date             2017-01-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.13(C328 H184 N8 O128 Zr24)'
_chemical_formula_sum            'C41 H23 N O16 Zr3'
_chemical_formula_weight         1059.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Zr'
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'
N N 0.0311 0.0180 '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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'x, -y, -z'
'-x, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'-x, y, z'
'x, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   21.5401(6)
_cell_length_b                   33.1625(6)
_cell_length_c                   31.9996(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     22858.1(10)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6364
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.6700
_cell_measurement_theta_min      3.6170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.437
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.616
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_unetI/netI     0.0753
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            36277
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.939
_diffrn_reflns_theta_min         3.637
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -96.00  -2.00   1.00   12.50    --  -41.81 125.00 -60.00   94
  2  ω     23.00  98.00   1.00   12.50    --   41.81-125.00 150.00   75
  3  ω      1.00  79.00   1.00   12.50    --   41.81 -99.00 -90.00   78
  4  ω     80.00 177.00   1.00   35.00    --  105.88  77.00-120.00   97
  5  ω     38.00  64.00   1.00   35.00    --  105.88 -45.00-120.00   26
  6  ω     79.00 131.00   1.00   35.00    --  105.88 -45.00-120.00   52
  7  ω    139.00 173.00   1.00   35.00    --  105.88 125.00-120.00   34
  8  ω     99.00 126.00   1.00   35.00    --  105.88 125.00 -60.00   27
  9  ω     51.00 100.00   1.00   35.00    --  105.88-125.00  60.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0375632000
_diffrn_orient_matrix_UB_12      0.0031008000
_diffrn_orient_matrix_UB_13      -0.0409118000
_diffrn_orient_matrix_UB_21      -0.0295050000
_diffrn_orient_matrix_UB_22      -0.0396371000
_diffrn_orient_matrix_UB_23      -0.0154217000
_diffrn_orient_matrix_UB_31      -0.0531780000
_diffrn_orient_matrix_UB_32      0.0240418000
_diffrn_orient_matrix_UB_33      -0.0202084000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7534
_reflns_number_total             11951
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.687
_refine_diff_density_min         -1.073
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         11951
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0466
_refine_ls_restrained_S_all      0.941
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0625P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1229
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O7 \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: H14A(0.5) H14B(0.5) H14C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C11(H11), C16(H16), C17(H17),
 C19(H19), C20(H20)
4.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.500000 0.07396(2) 0.27802(2) 0.02042(9) Uani 1 2 d S T P . .
Zr2 Zr 0.41862(2) 0.000000 0.33332(2) 0.03085(11) Uani 1 2 d S T P . .
Zr3 Zr 0.08108(2) 0.500000 0.27708(2) 0.04133(12) Uani 1 2 d S T P . .
O1 O 0.38572(14) 0.06052(6) 0.35621(9) 0.0613(9) Uani 1 1 d . . . . .
O2 O 0.43802(10) 0.10741(6) 0.31952(6) 0.0307(5) Uani 1 1 d . U . . .
O3 O 0.11396(16) 0.43996(7) 0.29945(10) 0.0767(11) Uani 1 1 d . . . . .
O4 O 0.06280(12) 0.39196(6) 0.26404(7) 0.0388(6) Uani 1 1 d . . . . .
O5 O 0.32030(17) 0.000000 0.3293(2) 0.106(2) Uani 1 2 d S T P . .
O6 O 0.4395(3) 0.000000 0.40182(12) 0.098(2) Uani 1 2 d S T P . .
O7 O 0.500000 -0.03641(11) 0.33247(12) 0.0534(9) Uani 1 2 d S TU P . .
O8 O 0.41891(14) -0.03608(7) 0.27771(8) 0.0608(8) Uani 1 1 d . . . . .
O9 O 0.500000 0.03615(13) 0.22341(14) 0.0673(11) Uani 1 2 d S TU P . .
O10 O 0.1845(2) 0.500000 0.2735(2) 0.107(2) Uani 1 2 d S T P . .
O11 O 0.0662(4) 0.500000 0.34585(14) 0.125(3) Uani 1 2 d S T P . .
N14 N 0.2732(3) 0.21386(13) 0.500000 0.0583(14) Uani 1 2 d S T P . .
C1 C 0.39844(18) 0.09641(9) 0.34639(12) 0.0436(9) Uani 1 1 d . . . . .
C2 C 0.36249(19) 0.12942(9) 0.36694(11) 0.0451(9) Uani 1 1 d . . . . .
C3 C 0.3761(2) 0.16917(10) 0.35720(13) 0.0616(13) Uani 1 1 d . . . . .
H3 H 0.408089 0.175166 0.337729 0.074 Uiso 1 1 calc R . . . .
C4 C 0.3430(2) 0.20021(11) 0.37589(12) 0.0674(14) Uani 1 1 d . . . . .
H4 H 0.352545 0.227404 0.369118 0.081 Uiso 1 1 calc R . . . .
C5 C 0.2964(2) 0.19202(11) 0.40419(11) 0.0587(13) Uani 1 1 d . . . . .
C6 C 0.2840(2) 0.15245(12) 0.41381(12) 0.0599(12) Uani 1 1 d . . . . .
H6 H 0.252302 0.146305 0.433452 0.072 Uiso 1 1 calc R . . . .
C7 C 0.3171(2) 0.12129(11) 0.39526(13) 0.0588(12) Uani 1 1 d . . . . .
H7 H 0.308028 0.094115 0.402399 0.071 Uiso 1 1 calc R . . . .
C8 C 0.2603(2) 0.22612(12) 0.42201(11) 0.0597(13) Uani 1 1 d . . . . .
C9 C 0.2328(2) 0.25307(11) 0.39443(11) 0.0683(15) Uani 1 1 d . . . . .
H9 H 0.238874 0.248732 0.365370 0.082 Uiso 1 1 calc R . . . .
C10 C 0.1967(3) 0.28632(12) 0.40665(12) 0.0711(15) Uani 1 1 d . . . . .
C11 C 0.1856(3) 0.29194(12) 0.44897(12) 0.0741(16) Uani 1 1 d . . . . .
H11 H 0.160633 0.313796 0.458285 0.089 Uiso 1 1 calc R . . . .
C12 C 0.2115(2) 0.26496(12) 0.47772(11) 0.0653(14) Uani 1 1 d . . . . .
C13 C 0.2501(2) 0.23281(11) 0.46454(11) 0.0602(13) Uani 1 1 d . . . . .
C14 C 0.3285(3) 0.1888(2) 0.500000 0.075(2) Uani 1 2 d S T P . .
H14A H 0.318662 0.162439 0.487797 0.112 Uiso 0.5 1 calc GR . . A -1
H14B H 0.343070 0.185128 0.528764 0.112 Uiso 0.5 1 calc GR . . A -1
H14C H 0.361054 0.201846 0.483439 0.112 Uiso 0.5 1 calc GR . . A -1
C15 C 0.1737(3) 0.31556(12) 0.37585(12) 0.0712(15) Uani 1 1 d . . . . .
C16 C 0.1466(3) 0.30401(11) 0.33849(13) 0.0813(18) Uani 1 1 d . . . . .
H16 H 0.144989 0.276203 0.331444 0.098 Uiso 1 1 calc R . . . .
C17 C 0.1219(3) 0.33206(11) 0.31124(13) 0.0709(15) Uani 1 1 d . . . . .
H17 H 0.101693 0.323402 0.286430 0.085 Uiso 1 1 calc R . . . .
C18 C 0.1266(2) 0.37269(10) 0.32012(13) 0.0596(12) Uani 1 1 d . . . . .
C19 C 0.1540(2) 0.38475(12) 0.35676(14) 0.0708(15) Uani 1 1 d . . . . .
H19 H 0.157538 0.412670 0.362944 0.085 Uiso 1 1 calc R . . . .
C20 C 0.1765(3) 0.35643(12) 0.38482(13) 0.0742(16) Uani 1 1 d . . . . .
H20 H 0.193992 0.365147 0.410520 0.089 Uiso 1 1 calc R . . . .
C21 C 0.0988(2) 0.40372(10) 0.29207(12) 0.0526(11) 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
Zr1 Zr2 3.4956(4) 2_655 ?
Zr1 Zr2 3.4956(4) . ?
Zr1 Zr3 3.4892(4) 14_545 ?
Zr1 Zr3 3.4892(4) 13 ?
Zr1 O2 2.1852(19) 11_655 ?
Zr1 O2 2.1853(19) . ?
Zr1 O4 2.218(2) 13 ?
Zr1 O4 2.218(2) 7 ?
Zr1 O7 2.141(3) 2_655 ?
Zr1 O8 2.151(2) 12 ?
Zr1 O8 2.151(2) 2_655 ?
Zr1 O9 2.151(4) . ?
Zr2 Zr2 3.5057(8) 2_655 ?
Zr2 Zr3 3.5326(6) 13 ?
Zr2 O1 2.251(2) . ?
Zr2 O1 2.251(2) 12 ?
Zr2 O5 2.122(4) . ?
Zr2 O6 2.238(4) . ?
Zr2 O7 2.129(2) . ?
Zr2 O7 2.129(2) 2_655 ?
Zr2 O8 2.144(3) . ?
Zr2 O8 2.144(3) 12 ?
Zr3 Zr3 3.4929(9) 2_565 ?
Zr3 O3 2.231(2) 12_565 ?
Zr3 O3 2.231(2) . ?
Zr3 O8 2.123(3) 13 ?
Zr3 O8 2.123(3) 8 ?
Zr3 O9 2.118(2) 13 ?
Zr3 O9 2.118(2) 14_455 ?
Zr3 O10 2.231(5) . ?
Zr3 O11 2.224(5) . ?
O1 C1 1.261(4) . ?
O2 C1 1.265(4) . ?
O3 C21 1.268(4) . ?
O4 C21 1.248(4) . ?
N14 C13 1.389(4) . ?
N14 C13 1.389(4) 10_556 ?
N14 C14 1.452(7) . ?
C1 C2 1.494(4) . ?
C2 C3 1.386(5) . ?
C2 C7 1.359(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.388(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.379(6) . ?
C5 C6 1.374(5) . ?
C5 C8 1.486(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.389(5) . ?
C7 H7 0.9500 . ?
C8 C9 1.388(5) . ?
C8 C13 1.396(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.405(5) . ?
C10 C11 1.388(5) . ?
C10 C15 1.469(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.400(5) . ?
C12 C12 1.426(7) 10_556 ?
C12 C13 1.417(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.384(6) . ?
C15 C20 1.387(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.382(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.381(5) . ?
C18 C19 1.372(5) . ?
C18 C21 1.491(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.387(5) . ?
C20 H20 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
Zr2 Zr1 Zr2 60.192(13) . 2_655 ?
Zr3 Zr1 Zr2 90.776(9) 13 2_655 ?
Zr3 Zr1 Zr2 60.762(10) 13 . ?
Zr3 Zr1 Zr2 60.762(10) 14_545 2_655 ?
Zr3 Zr1 Zr2 90.776(9) 14_545 . ?
Zr3 Zr1 Zr3 60.069(16) 13 14_545 ?
O2 Zr1 Zr2 110.79(6) . 2_655 ?
O2 Zr1 Zr2 75.06(5) 11_655 2_655 ?
O2 Zr1 Zr2 110.79(6) 11_655 . ?
O2 Zr1 Zr2 75.06(5) . . ?
O2 Zr1 Zr3 165.83(5) . 14_545 ?
O2 Zr1 Zr3 110.98(6) . 13 ?
O2 Zr1 Zr3 110.98(6) 11_655 14_545 ?
O2 Zr1 Zr3 165.83(5) 11_655 13 ?
O2 Zr1 O2 75.32(12) 11_655 . ?
O2 Zr1 O4 118.87(8) . 7 ?
O2 Zr1 O4 74.78(8) . 13 ?
O2 Zr1 O4 74.78(8) 11_655 7 ?
O2 Zr1 O4 118.87(8) 11_655 13 ?
O4 Zr1 Zr2 166.07(6) 13 2_655 ?
O4 Zr1 Zr2 111.03(7) 13 . ?
O4 Zr1 Zr2 166.07(6) 7 . ?
O4 Zr1 Zr2 111.03(7) 7 2_655 ?
O4 Zr1 Zr3 110.90(6) 7 13 ?
O4 Zr1 Zr3 110.90(6) 13 14_545 ?
O4 Zr1 Zr3 75.30(6) 13 13 ?
O4 Zr1 Zr3 75.30(6) 7 14_545 ?
O4 Zr1 O4 75.18(13) 13 7 ?
O7 Zr1 Zr2 34.94(6) 2_655 2_655 ?
O7 Zr1 Zr2 34.94(6) 2_655 . ?
O7 Zr1 Zr3 90.14(10) 2_655 14_545 ?
O7 Zr1 Zr3 90.14(10) 2_655 13 ?
O7 Zr1 O2 78.50(10) 2_655 11_655 ?
O7 Zr1 O2 78.51(10) 2_655 . ?
O7 Zr1 O4 142.19(7) 2_655 13 ?
O7 Zr1 O4 142.19(7) 2_655 7 ?
O7 Zr1 O8 70.39(9) 2_655 12 ?
O7 Zr1 O8 70.39(9) 2_655 2_655 ?
O7 Zr1 O9 108.79(17) 2_655 . ?
O8 Zr1 Zr2 35.47(7) 2_655 2_655 ?
O8 Zr1 Zr2 89.99(8) 2_655 . ?
O8 Zr1 Zr2 35.47(7) 12 . ?
O8 Zr1 Zr2 89.99(8) 12 2_655 ?
O8 Zr1 Zr3 89.63(8) 12 14_545 ?
O8 Zr1 Zr3 35.00(8) 2_655 14_545 ?
O8 Zr1 Zr3 35.00(8) 12 13 ?
O8 Zr1 Zr3 89.63(8) 2_655 13 ?
O8 Zr1 O2 78.65(10) 12 . ?
O8 Zr1 O2 142.67(9) 12 11_655 ?
O8 Zr1 O2 142.67(9) 2_655 . ?
O8 Zr1 O2 78.64(10) 2_655 11_655 ?
O8 Zr1 O4 78.43(10) 2_655 7 ?
O8 Zr1 O4 78.43(10) 12 13 ?
O8 Zr1 O4 142.17(10) 12 7 ?
O8 Zr1 O4 142.17(10) 2_655 13 ?
O8 Zr1 O8 108.56(16) 12 2_655 ?
O9 Zr1 Zr2 90.13(11) . . ?
O9 Zr1 Zr2 90.13(11) . 2_655 ?
O9 Zr1 Zr3 34.88(6) . 13 ?
O9 Zr1 Zr3 34.88(6) . 14_545 ?
O9 Zr1 O2 142.14(6) . 11_655 ?
O9 Zr1 O2 142.14(6) . . ?
O9 Zr1 O4 78.69(12) . 7 ?
O9 Zr1 O4 78.69(12) . 13 ?
O9 Zr1 O8 69.87(10) . 12 ?
O9 Zr1 O8 69.87(10) . 2_655 ?
Zr1 Zr2 Zr1 89.122(13) 2_655 . ?
Zr1 Zr2 Zr2 59.904(7) . 2_655 ?
Zr1 Zr2 Zr2 59.904(7) 2_655 2_655 ?
Zr1 Zr2 Zr3 59.531(10) 2_655 13 ?
Zr1 Zr2 Zr3 59.530(10) . 13 ?
Zr2 Zr2 Zr3 89.896(10) 2_655 13 ?
O1 Zr2 Zr1 161.48(6) . 2_655 ?
O1 Zr2 Zr1 72.36(6) 12 2_655 ?
O1 Zr2 Zr1 161.48(6) 12 . ?
O1 Zr2 Zr1 72.36(6) . . ?
O1 Zr2 Zr2 108.36(8) 12 2_655 ?
O1 Zr2 Zr2 108.35(8) . 2_655 ?
O1 Zr2 Zr3 109.02(8) . 13 ?
O1 Zr2 Zr3 109.02(8) 12 13 ?
O1 Zr2 O1 126.15(13) 12 . ?
O5 Zr2 Zr1 118.03(11) . 2_655 ?
O5 Zr2 Zr1 118.03(11) . . ?
O5 Zr2 Zr2 176.53(19) . 2_655 ?
O5 Zr2 Zr3 86.63(19) . 13 ?
O5 Zr2 O1 72.86(11) . 12 ?
O5 Zr2 O1 72.87(11) . . ?
O5 Zr2 O6 105.1(2) . . ?
O5 Zr2 O7 145.20(8) . 2_655 ?
O5 Zr2 O7 145.20(8) . . ?
O5 Zr2 O8 87.29(18) . . ?
O5 Zr2 O8 87.28(18) . 12 ?
O6 Zr2 Zr1 113.26(10) . . ?
O6 Zr2 Zr1 113.26(10) . 2_655 ?
O6 Zr2 Zr2 78.39(16) . 2_655 ?
O6 Zr2 Zr3 168.28(16) . 13 ?
O6 Zr2 O1 75.21(10) . . ?
O6 Zr2 O1 75.21(10) . 12 ?
O7 Zr2 Zr1 88.78(10) 2_655 2_655 ?
O7 Zr2 Zr1 88.78(10) . . ?
O7 Zr2 Zr1 35.17(9) 2_655 . ?
O7 Zr2 Zr1 35.17(9) . 2_655 ?
O7 Zr2 Zr2 34.57(8) . 2_655 ?
O7 Zr2 Zr2 34.57(8) 2_655 2_655 ?
O7 Zr2 Zr3 89.18(11) . 13 ?
O7 Zr2 Zr3 89.18(11) 2_655 13 ?
O7 Zr2 O1 140.29(11) . . ?
O7 Zr2 O1 140.29(11) 2_655 12 ?
O7 Zr2 O1 75.98(12) . 12 ?
O7 Zr2 O1 75.97(12) 2_655 . ?
O7 Zr2 O6 81.19(17) . . ?
O7 Zr2 O6 81.18(17) 2_655 . ?
O7 Zr2 O7 69.12(16) . 2_655 ?
O7 Zr2 O8 107.68(14) 2_655 . ?
O7 Zr2 O8 70.76(11) . . ?
O7 Zr2 O8 70.76(11) 2_655 12 ?
O7 Zr2 O8 107.67(14) . 12 ?
O8 Zr2 Zr1 88.28(8) . . ?
O8 Zr2 Zr1 88.29(8) 12 2_655 ?
O8 Zr2 Zr1 35.61(7) 12 . ?
O8 Zr2 Zr1 35.61(7) . 2_655 ?
O8 Zr2 Zr2 89.84(8) 12 2_655 ?
O8 Zr2 Zr2 89.83(8) . 2_655 ?
O8 Zr2 Zr3 33.92(7) 12 13 ?
O8 Zr2 Zr3 33.92(7) . 13 ?
O8 Zr2 O1 76.90(10) 12 . ?
O8 Zr2 O1 76.90(10) . 12 ?
O8 Zr2 O1 140.22(11) 12 12 ?
O8 Zr2 O1 140.22(11) . . ?
O8 Zr2 O6 144.32(8) . . ?
O8 Zr2 O6 144.32(8) 12 . ?
O8 Zr2 O8 67.84(14) 12 . ?
Zr1 Zr3 Zr1 89.323(13) 13 14_455 ?
Zr1 Zr3 Zr2 59.705(10) 14_455 13 ?
Zr1 Zr3 Zr2 59.705(10) 13 13 ?
Zr1 Zr3 Zr3 59.965(8) 14_455 2_565 ?
Zr1 Zr3 Zr3 59.964(8) 13 2_565 ?
Zr3 Zr3 Zr2 90.103(10) 2_565 13 ?
O3 Zr3 Zr1 161.49(7) 12_565 13 ?
O3 Zr3 Zr1 161.49(7) . 14_455 ?
O3 Zr3 Zr1 72.17(6) 12_565 14_455 ?
O3 Zr3 Zr1 72.17(6) . 13 ?
O3 Zr3 Zr2 108.68(9) . 13 ?
O3 Zr3 Zr2 108.68(9) 12_565 13 ?
O3 Zr3 Zr3 108.51(9) . 2_565 ?
O3 Zr3 Zr3 108.51(9) 12_565 2_565 ?
O3 Zr3 O3 126.34(13) . 12_565 ?
O8 Zr3 Zr1 35.55(7) 13 14_455 ?
O8 Zr3 Zr1 35.55(7) 8 13 ?
O8 Zr3 Zr1 88.79(8) 8 14_455 ?
O8 Zr3 Zr1 88.79(8) 13 13 ?
O8 Zr3 Zr2 34.31(7) 8 13 ?
O8 Zr3 Zr2 34.31(7) 13 13 ?
O8 Zr3 Zr3 90.00(8) 8 2_565 ?
O8 Zr3 Zr3 90.00(8) 13 2_565 ?
O8 Zr3 O3 76.23(11) 8 . ?
O8 Zr3 O3 76.23(11) 13 12_565 ?
O8 Zr3 O3 140.18(12) 13 . ?
O8 Zr3 O3 140.18(12) 8 12_565 ?
O8 Zr3 O8 68.63(14) 8 13 ?
O8 Zr3 O10 87.57(16) 13 . ?
O8 Zr3 O10 87.57(16) 8 . ?
O8 Zr3 O11 144.82(8) 8 . ?
O8 Zr3 O11 144.82(8) 13 . ?
O9 Zr3 Zr1 88.93(12) 13 14_455 ?
O9 Zr3 Zr1 35.50(11) 14_455 14_455 ?
O9 Zr3 Zr1 88.93(12) 14_455 13 ?
O9 Zr3 Zr1 35.50(11) 13 13 ?
O9 Zr3 Zr2 89.66(13) 14_455 13 ?
O9 Zr3 Zr2 89.66(13) 13 13 ?
O9 Zr3 Zr3 34.47(9) 14_455 2_565 ?
O9 Zr3 Zr3 34.47(10) 13 2_565 ?
O9 Zr3 O3 76.06(13) 13 . ?
O9 Zr3 O3 140.26(14) 14_455 . ?
O9 Zr3 O3 140.26(14) 13 12_565 ?
O9 Zr3 O3 76.06(13) 14_455 12_565 ?
O9 Zr3 O8 71.03(13) 14_455 13 ?
O9 Zr3 O8 71.03(13) 13 8 ?
O9 Zr3 O8 108.24(15) 14_455 8 ?
O9 Zr3 O8 108.24(15) 13 13 ?
O9 Zr3 O9 68.93(19) 13 14_455 ?
O9 Zr3 O10 145.39(9) 14_455 . ?
O9 Zr3 O10 145.39(9) 13 . ?
O9 Zr3 O11 83.6(2) 14_455 . ?
O9 Zr3 O11 83.6(2) 13 . ?
O10 Zr3 Zr1 118.29(10) . 14_455 ?
O10 Zr3 Zr1 118.29(10) . 13 ?
O10 Zr3 Zr2 86.96(17) . 13 ?
O10 Zr3 Zr3 177.06(17) . 2_565 ?
O10 Zr3 O3 72.51(11) . 12_565 ?
O10 Zr3 O3 72.51(11) . . ?
O11 Zr3 Zr1 115.35(12) . 14_455 ?
O11 Zr3 Zr1 115.35(12) . 13 ?
O11 Zr3 Zr2 171.84(19) . 13 ?
O11 Zr3 Zr3 81.73(19) . 2_565 ?
O11 Zr3 O3 74.22(12) . . ?
O11 Zr3 O3 74.22(12) . 12_565 ?
O11 Zr3 O10 101.2(3) . . ?
C1 O1 Zr2 133.8(2) . . ?
C1 O2 Zr1 132.74(19) . . ?
C21 O3 Zr3 134.8(2) . . ?
C21 O4 Zr1 131.0(2) . 13 ?
Zr2 O7 Zr1 109.89(12) 2_655 2_655 ?
Zr2 O7 Zr1 109.89(12) . 2_655 ?
Zr2 O7 Zr2 110.86(16) . 2_655 ?
Zr2 O8 Zr1 108.92(12) . 2_655 ?
Zr3 O8 Zr1 109.45(13) 13 2_655 ?
Zr3 O8 Zr2 111.76(11) 13 . ?
Zr3 O9 Zr1 109.62(14) 14_545 . ?
Zr3 O9 Zr1 109.62(14) 13 . ?
Zr3 O9 Zr3 111.06(19) 13 14_545 ?
C13 N14 C13 109.5(4) . 10_556 ?
C13 N14 C14 123.6(3) 10_556 . ?
C13 N14 C14 123.6(3) . . ?
O1 C1 O2 126.0(3) . . ?
O1 C1 C2 118.0(3) . . ?
O2 C1 C2 116.0(3) . . ?
C3 C2 C1 119.2(3) . . ?
C7 C2 C1 121.4(3) . . ?
C7 C2 C3 119.4(3) . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 120.0(4) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 119.6 . . ?
C5 C4 C3 120.7(4) . . ?
C5 C4 H4 119.6 . . ?
C4 C5 C8 118.9(4) . . ?
C6 C5 C4 118.5(3) . . ?
C6 C5 C8 122.6(4) . . ?
C5 C6 H6 119.5 . . ?
C5 C6 C7 121.0(4) . . ?
C7 C6 H6 119.5 . . ?
C2 C7 C6 120.4(4) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C9 C8 C5 118.0(3) . . ?
C9 C8 C13 116.8(3) . . ?
C13 C8 C5 125.2(3) . . ?
C8 C9 H9 117.8 . . ?
C8 C9 C10 124.4(4) . . ?
C10 C9 H9 117.8 . . ?
C9 C10 C15 121.2(4) . . ?
C11 C10 C9 118.2(3) . . ?
C11 C10 C15 120.5(3) . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 119.1(3) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 C12 131.1(2) . 10_556 ?
C11 C12 C13 121.3(3) . . ?
C13 C12 C12 107.3(2) . 10_556 ?
N14 C13 C8 131.9(3) . . ?
N14 C13 C12 107.9(3) . . ?
C8 C13 C12 120.1(3) . . ?
N14 C14 H14A 109.5 . . ?
N14 C14 H14B 109.5 . . ?
N14 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C10 122.6(4) . . ?
C16 C15 C20 117.8(3) . . ?
C20 C15 C10 119.5(4) . . ?
C15 C16 H16 119.3 . . ?
C17 C16 C15 121.4(4) . . ?
C17 C16 H16 119.3 . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 119.9(4) . . ?
C18 C17 H17 120.0 . . ?
C17 C18 C21 121.3(4) . . ?
C19 C18 C17 119.5(3) . . ?
C19 C18 C21 119.1(3) . . ?
C18 C19 H19 119.8 . . ?
C18 C19 C20 120.4(4) . . ?
C20 C19 H19 119.8 . . ?
C15 C20 C19 120.9(4) . . ?
C15 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
O3 C21 C18 116.0(3) . . ?
O4 C21 O3 126.2(3) . . ?
O4 C21 C18 117.8(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O2 C1 O1 1.0(6) . . . . ?
Zr1 O2 C1 C2 -176.8(2) . . . . ?
Zr1 O4 C21 O3 -10.2(8) 13 . . . ?
Zr1 O4 C21 C18 169.3(3) 13 . . . ?
Zr2 O1 C1 O2 -2.5(7) . . . . ?
Zr2 O1 C1 C2 175.3(3) . . . . ?
Zr3 O3 C21 O4 9.8(9) . . . . ?
Zr3 O3 C21 C18 -169.7(3) . . . . ?
O1 C1 C2 C3 179.1(4) . . . . ?
O1 C1 C2 C7 -0.3(6) . . . . ?
O2 C1 C2 C3 -3.0(6) . . . . ?
O2 C1 C2 C7 177.6(4) . . . . ?
C1 C2 C3 C4 179.8(4) . . . . ?
C1 C2 C7 C6 -179.6(4) . . . . ?
C2 C3 C4 C5 -0.1(8) . . . . ?
C3 C2 C7 C6 1.0(7) . . . . ?
C3 C4 C5 C6 0.8(7) . . . . ?
C3 C4 C5 C8 -177.3(4) . . . . ?
C4 C5 C6 C7 -0.6(7) . . . . ?
C4 C5 C8 C9 53.5(7) . . . . ?
C4 C5 C8 C13 -128.4(5) . . . . ?
C5 C6 C7 C2 -0.3(7) . . . . ?
C5 C8 C9 C10 179.1(5) . . . . ?
C5 C8 C13 N14 6.6(10) . . . . ?
C5 C8 C13 C12 -175.9(5) . . . . ?
C6 C5 C8 C9 -124.6(5) . . . . ?
C6 C5 C8 C13 53.6(8) . . . . ?
C7 C2 C3 C4 -0.8(7) . . . . ?
C8 C5 C6 C7 177.4(4) . . . . ?
C8 C9 C10 C11 -2.6(9) . . . . ?
C8 C9 C10 C15 174.6(5) . . . . ?
C9 C8 C13 N14 -175.2(6) . . . . ?
C9 C8 C13 C12 2.3(8) . . . . ?
C9 C10 C11 C12 1.3(9) . . . . ?
C9 C10 C15 C16 45.7(9) . . . . ?
C9 C10 C15 C20 -137.2(6) . . . . ?
C10 C11 C12 C12 175.0(4) . . . 10_556 ?
C10 C11 C12 C13 1.7(9) . . . . ?
C10 C15 C16 C17 175.9(5) . . . . ?
C10 C15 C20 C19 -178.7(5) . . . . ?
C11 C10 C15 C16 -137.2(6) . . . . ?
C11 C10 C15 C20 39.9(9) . . . . ?
C11 C12 C13 N14 174.5(5) . . . . ?
C11 C12 C13 C8 -3.5(8) . . . . ?
C12 C12 C13 N14 -0.3(5) 10_556 . . . ?
C12 C12 C13 C8 -178.3(4) 10_556 . . . ?
C13 N14 C13 C8 178.1(4) 10_556 . . . ?
C13 N14 C13 C12 0.4(8) 10_556 . . . ?
C13 C8 C9 C10 0.8(8) . . . . ?
C14 N14 C13 C8 18.3(10) . . . . ?
C14 N14 C13 C12 -159.4(5) . . . . ?
C15 C10 C11 C12 -175.9(5) . . . . ?
C15 C16 C17 C18 3.1(9) . . . . ?
C16 C15 C20 C19 -1.4(9) . . . . ?
C16 C17 C18 C19 -2.3(9) . . . . ?
C16 C17 C18 C21 -178.1(5) . . . . ?
C17 C18 C19 C20 -0.3(9) . . . . ?
C17 C18 C21 O3 -169.3(5) . . . . ?
C17 C18 C21 O4 11.2(8) . . . . ?
C18 C19 C20 C15 2.2(9) . . . . ?
C19 C18 C21 O3 14.8(7) . . . . ?
C19 C18 C21 O4 -164.7(5) . . . . ?
C20 C15 C16 C17 -1.3(9) . . . . ?
C21 C18 C19 C20 175.6(5) . . . . ?

_shelx_SHELXL_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.578
_oxdiff_exptl_absorpt_empirical_full_min 0.801

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.010 -0.004 -0.013 17228 4271 ' '
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1533344'
_audit_update_record             
;
2017-02-17 deposited with the CCDC.
2018-09-04 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         ?
_chemical_formula_sum            'C40 H21 N O16 Zr3'
_chemical_formula_weight         1045.24

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'
N N 0.0311 0.0180 '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      orthorhombic
_space_group_IT_number           71
_space_group_name_H-M_alt        'I m m m'
_space_group_name_Hall           '-I 2 2'

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

_cell_length_a                   17.723(5)
_cell_length_b                   32.705(3)
_cell_length_c                   34.670(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     20096(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    975
_cell_measurement_theta_min      3.8030
_cell_measurement_theta_max      63.5330

_exptl_crystal_description       
; 
'Sat Dec 19 00:02:26 2015' 
;
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.691
_exptl_crystal_F_000             4128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    2.769
_shelx_estimated_absorpt_T_min   0.621
_shelx_estimated_absorpt_T_max   0.682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.71853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
'Sat Dec 19 00:02:26 2015' 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3376
_diffrn_reflns_number            39298
_diffrn_reflns_av_unetI/netI     0.2558
_diffrn_reflns_av_R_equivalents  0.3270
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         3.716
_diffrn_reflns_theta_max         65.073
_diffrn_reflns_theta_full        65.073
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9189
_reflns_number_gt                2142
_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       
; 
'Sat Dec 19 00:02:26 2015' 
;
_computing_cell_refinement       
; 
'Sat Dec 19 00:02:26 2015' 
;
_computing_data_reduction        
; 
'Sat Dec 19 00:02:26 2015' 
;
_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)+(0.0178P)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         9189
_refine_ls_number_parameters     286
_refine_ls_number_restraints     271
_refine_ls_R_factor_all          0.2695
_refine_ls_R_factor_gt           0.1153
_refine_ls_wR_factor_ref         0.2653
_refine_ls_wR_factor_gt          0.2145
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.047
_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
C1 C 0.1207(13) 0.1537(4) 0.5930(3) 0.130(6) Uani 1 1 d . U . . .
C2 C 0.1526(12) 0.1304(4) 0.6268(4) 0.126(6) Uani 1 1 d . U . . .
C3 C 0.2048(11) 0.1007(4) 0.6221(4) 0.125(6) Uani 1 1 d . U . . .
H3 H 0.2240 0.0948 0.5971 0.150 Uiso 1 1 calc R U . . .
C4 C 0.2294(12) 0.0795(4) 0.6530(4) 0.142(6) Uani 1 1 d . U . . .
H4 H 0.2618 0.0566 0.6499 0.171 Uiso 1 1 calc R U . . .
C5 C 0.2044(13) 0.0928(4) 0.6925(4) 0.142(6) Uani 1 1 d . U . . .
C6 C 0.1588(12) 0.1240(4) 0.6954(4) 0.160(7) Uani 1 1 d . U . . .
H6 H 0.1490 0.1351 0.7202 0.192 Uiso 1 1 calc R U . . .
C7 C 0.1239(12) 0.1416(4) 0.6634(4) 0.145(6) Uani 1 1 d . U . . .
H7 H 0.0830 0.1601 0.6660 0.174 Uiso 1 1 calc R U . . .
C8 C 0.2430(13) 0.0753(3) 0.7275(4) 0.141(6) Uani 1 1 d . U . . .
C9 C 0.2561(12) 0.0343(4) 0.7363(4) 0.139(6) Uani 1 1 d . U . . .
C10 C 0.2855(11) 0.0211(3) 0.7713(3) 0.134(6) Uani 1 1 d . U . . .
C11 C 0.3108(12) 0.0514(4) 0.7990(4) 0.154(7) Uani 1 1 d . U . . .
H11 H 0.3416 0.0443 0.8204 0.185 Uiso 1 1 calc R U . . .
C12 C 0.2876(13) 0.0909(4) 0.7927(4) 0.153(6) Uani 1 1 d . U . . .
C13 C 0.2641(12) 0.1019(4) 0.7569(4) 0.146(7) Uani 1 1 d . U . . .
H13 H 0.2620 0.1303 0.7514 0.175 Uiso 1 1 calc R U . . .
C14 C 0.3140(14) 0.1220(4) 0.8237(4) 0.163(7) Uani 1 1 d . U . . .
C15 C 0.2963(12) 0.1146(4) 0.8603(4) 0.155(7) Uani 1 1 d . U . . .
H15 H 0.2693 0.0908 0.8676 0.186 Uiso 1 1 calc R U . . .
C16 C 0.3197(12) 0.1441(4) 0.8879(4) 0.163(7) Uani 1 1 d . U . . .
H16 H 0.3077 0.1394 0.9142 0.195 Uiso 1 1 calc R U . . .
C17 C 0.3561(13) 0.1766(4) 0.8793(4) 0.157(7) Uani 1 1 d . U . . .
C18 C 0.3711(13) 0.1859(4) 0.8398(4) 0.193(8) Uani 1 1 d . U . . .
H18 H 0.3972 0.2101 0.8327 0.231 Uiso 1 1 calc R U . . .
C19 C 0.3459(13) 0.1578(4) 0.8115(4) 0.183(8) Uani 1 1 d . U . . .
H19 H 0.3510 0.1636 0.7848 0.219 Uiso 1 1 calc R U . . .
C20 C 0.3821(13) 0.2097(5) 0.9066(4) 0.143(6) Uani 1 1 d . U . . .
N1 N 0.2277(13) 0.0000 0.7129(4) 0.145(8) Uani 1 2 d S TU P . .
H1 H 0.2015 0.0000 0.6914 0.173 Uiso 1 2 calc R U P . .
O5 O 0.0000 0.1656(4) 0.5335(4) 0.123(3) Uani 1 2 d S TU P . .
O9 O -0.2208(9) 0.2740(4) 0.5000 0.120(4) Uani 1 2 d S TU P . .
O7 O 0.0000 0.2743(4) 0.5321(4) 0.137(4) Uani 1 2 d S TU P . .
O8 O -0.0875(10) 0.3423(3) 0.5000 0.140(5) Uani 1 2 d S TU P . .
O1 O 0.0798(7) 0.1823(2) 0.6016(2) 0.122(4) Uani 1 1 d . U . . .
O2 O 0.1415(6) 0.1438(2) 0.5588(2) 0.102(4) Uani 1 1 d . U . . .
O3 O 0.4275(7) 0.2374(2) 0.8984(2) 0.129(5) Uani 1 1 d . U . . .
O4 O 0.3553(8) 0.2017(3) 0.9427(3) 0.147(5) Uani 1 1 d . U . . .
O11 O -0.0883(9) 0.0982(3) 0.5000 0.121(5) Uani 1 2 d S TU P . .
O6 O -0.1048(6) 0.2212(2) 0.5349(2) 0.117(3) Uani 1 1 d . U . . .
O10 O -0.2235(10) 0.1685(4) 0.5000 0.119(4) Uani 1 2 d S TU P . .
Zr01 Zr -0.10067(16) 0.16690(5) 0.5000 0.1045(10) Uani 1 2 d S TU P . .
Zr02 Zr 0.0000 0.22215(5) 0.57000(4) 0.1088(10) Uani 1 2 d S TU P . .
Zr03 Zr -0.10023(16) 0.27584(5) 0.5000 0.1083(10) Uani 1 2 d S TU 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
C1 O1 1.219(17) . ?
C1 O2 1.285(14) . ?
C1 C2 1.508(18) . ?
C2 C3 1.35(2) . ?
C2 C7 1.414(18) . ?
C3 C4 1.350(16) . ?
C3 H3 0.9500 . ?
C4 C5 1.504(18) . ?
C4 H4 0.9500 . ?
C5 C6 1.31(2) . ?
C5 C8 1.506(18) . ?
C6 C7 1.395(18) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.390(16) . ?
C8 C9 1.396(15) . ?
C9 C10 1.390(16) . ?
C9 N1 1.473(16) . ?
C10 C10 1.38(2) 11 ?
C10 C11 1.450(16) . ?
C11 C12 1.374(17) . ?
C11 H11 0.9500 . ?
C12 C13 1.355(17) . ?
C12 C14 1.553(17) . ?
C13 H13 0.9500 . ?
C14 C15 1.329(19) . ?
C14 C19 1.365(19) . ?
C15 C16 1.420(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.279(18) . ?
C16 H16 0.9500 . ?
C17 C18 1.426(18) . ?
C17 C20 1.513(17) . ?
C18 C19 1.418(17) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 O3 1.245(19) . ?
C20 O4 1.362(17) . ?
N1 C9 1.473(16) 11 ?
N1 H1 0.8800 . ?
O5 Zr01 2.130(7) 3_556 ?
O5 Zr01 2.130(7) . ?
O5 Zr02 2.240(11) . ?
O9 Zr03 2.138(16) . ?
O7 Zr03 2.096(7) 3_556 ?
O7 Zr03 2.096(7) . ?
O7 Zr02 2.154(12) . ?
O8 Zr03 2.184(11) . ?
O1 Zr02 2.214(9) . ?
O2 Zr01 2.290(8) 3_556 ?
O3 Zr02 2.145(9) 13_556 ?
O4 Zr03 2.260(9) 15 ?
O11 Zr01 2.258(11) . ?
O6 Zr03 2.159(8) . ?
O6 Zr02 2.221(9) . ?
O6 Zr01 2.149(8) . ?
O10 Zr01 2.177(17) . ?
Zr01 O5 2.130(7) 10_556 ?
Zr01 O6 2.149(8) 10_556 ?
Zr01 O2 2.290(8) 3_556 ?
Zr01 O2 2.290(8) 12 ?
Zr01 Zr02 3.513(2) 10_556 ?
Zr01 Zr02 3.513(2) . ?
Zr01 Zr01 3.568(6) 3_556 ?
Zr01 Zr03 3.563(2) . ?
Zr02 O6 2.221(9) 12 ?
Zr02 O3 2.145(9) 13_556 ?
Zr02 O3 2.145(9) 8_456 ?
Zr02 O1 2.214(9) 12 ?
Zr02 Zr03 3.483(2) 3_556 ?
Zr02 Zr03 3.483(2) . ?
Zr02 Zr01 3.513(2) 3_556 ?
Zr03 O7 2.096(7) 10_556 ?
Zr03 O6 2.160(8) 10_556 ?
Zr03 O4 2.260(9) 8_456 ?
Zr03 O4 2.260(9) 15_454 ?
Zr03 Zr02 3.483(2) 10_556 ?
Zr03 Zr03 3.553(6) 3_556 ?

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
O1 C1 O2 126.1(13) . . ?
O1 C1 C2 114.9(12) . . ?
O2 C1 C2 118.9(15) . . ?
C3 C2 C7 122.7(13) . . ?
C3 C2 C1 121.8(14) . . ?
C7 C2 C1 115.5(16) . . ?
C4 C3 C2 119.7(15) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 118.6(15) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.7 . . ?
C6 C5 C8 121.1(14) . . ?
C6 C5 C4 118.6(14) . . ?
C8 C5 C4 119.3(17) . . ?
C5 C6 C7 122.5(14) . . ?
C5 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C6 C7 C2 116.6(17) . . ?
C6 C7 H7 121.7 . . ?
C2 C7 H7 121.7 . . ?
C13 C8 C9 113.3(13) . . ?
C13 C8 C5 118.5(12) . . ?
C9 C8 C5 128.1(13) . . ?
C10 C9 C8 123.5(12) . . ?
C10 C9 N1 111.9(12) . . ?
C8 C9 N1 123.7(14) . . ?
C9 C10 C10 108.1(7) . 11 ?
C9 C10 C11 118.8(11) . . ?
C10 C10 C11 133.1(7) 11 . ?
C12 C11 C10 116.4(14) . . ?
C12 C11 H11 121.8 . . ?
C10 C11 H11 121.8 . . ?
C13 C12 C11 119.1(14) . . ?
C13 C12 C14 123.6(14) . . ?
C11 C12 C14 114.5(15) . . ?
C12 C13 C8 126.1(14) . . ?
C12 C13 H13 117.0 . . ?
C8 C13 H13 117.0 . . ?
C15 C14 C19 123.3(14) . . ?
C15 C14 C12 118.1(16) . . ?
C19 C14 C12 118.1(14) . . ?
C14 C15 C16 116.9(15) . . ?
C14 C15 H15 121.6 . . ?
C16 C15 H15 121.6 . . ?
C17 C16 C15 123.5(15) . . ?
C17 C16 H16 118.2 . . ?
C15 C16 H16 118.2 . . ?
C16 C17 C18 119.7(14) . . ?
C16 C17 C20 127.0(15) . . ?
C18 C17 C20 113.1(14) . . ?
C17 C18 C19 117.9(14) . . ?
C17 C18 H18 121.1 . . ?
C19 C18 H18 121.1 . . ?
C14 C19 C18 118.1(14) . . ?
C14 C19 H19 121.0 . . ?
C18 C19 H19 121.0 . . ?
O3 C20 O4 125.1(14) . . ?
O3 C20 C17 125.0(16) . . ?
O4 C20 C17 109.4(14) . . ?
C9 N1 C9 99.2(16) . 11 ?
C9 N1 H1 130.4 . . ?
C9 N1 H1 130.4 11 . ?
Zr01 O5 Zr01 113.8(6) 3_556 . ?
Zr01 O5 Zr02 106.9(4) 3_556 . ?
Zr01 O5 Zr02 106.9(4) . . ?
Zr03 O7 Zr03 115.9(7) 3_556 . ?
Zr03 O7 Zr02 110.0(4) 3_556 . ?
Zr03 O7 Zr02 110.0(4) . . ?
C1 O1 Zr02 135.2(8) . . ?
C1 O2 Zr01 130.4(10) . 3_556 ?
C20 O3 Zr02 135.9(9) . 13_556 ?
C20 O4 Zr03 128.6(11) . 15 ?
Zr03 O6 Zr02 105.3(4) . . ?
Zr03 O6 Zr01 111.6(3) . . ?
Zr02 O6 Zr01 107.0(4) . . ?
O5 Zr01 O5 66.2(6) 10_556 . ?
O5 Zr01 O6 74.8(4) 10_556 10_556 ?
O5 Zr01 O6 110.6(5) . 10_556 ?
O5 Zr01 O6 110.6(5) 10_556 . ?
O5 Zr01 O6 74.8(4) . . ?
O6 Zr01 O6 68.5(4) 10_556 . ?
O5 Zr01 O10 146.9(3) 10_556 . ?
O5 Zr01 O10 146.9(3) . . ?
O6 Zr01 O10 86.9(4) 10_556 . ?
O6 Zr01 O10 86.9(4) . . ?
O5 Zr01 O11 84.2(5) 10_556 . ?
O5 Zr01 O11 84.2(5) . . ?
O6 Zr01 O11 145.6(2) 10_556 . ?
O6 Zr01 O11 145.6(2) . . ?
O10 Zr01 O11 97.0(5) . . ?
O5 Zr01 O2 76.8(4) 10_556 3_556 ?
O5 Zr01 O2 138.0(4) . 3_556 ?
O6 Zr01 O2 76.2(3) 10_556 3_556 ?
O6 Zr01 O2 139.6(3) . 3_556 ?
O10 Zr01 O2 72.1(3) . 3_556 ?
O11 Zr01 O2 72.7(3) . 3_556 ?
O5 Zr01 O2 138.0(4) 10_556 12 ?
O5 Zr01 O2 76.8(4) . 12 ?
O6 Zr01 O2 139.6(3) 10_556 12 ?
O6 Zr01 O2 76.2(3) . 12 ?
O10 Zr01 O2 72.1(3) . 12 ?
O11 Zr01 O2 72.7(3) . 12 ?
O2 Zr01 O2 125.7(4) 3_556 12 ?
O5 Zr01 Zr02 37.6(3) 10_556 10_556 ?
O5 Zr01 Zr02 87.8(4) . 10_556 ?
O6 Zr01 Zr02 37.2(3) 10_556 10_556 ?
O6 Zr01 Zr02 88.9(2) . 10_556 ?
O10 Zr01 Zr02 119.7(2) . 10_556 ?
O11 Zr01 Zr02 117.5(3) . 10_556 ?
O2 Zr01 Zr02 73.4(2) 3_556 10_556 ?
O2 Zr01 Zr02 160.8(2) 12 10_556 ?
O5 Zr01 Zr02 87.8(4) 10_556 . ?
O5 Zr01 Zr02 37.6(3) . . ?
O6 Zr01 Zr02 88.9(2) 10_556 . ?
O6 Zr01 Zr02 37.2(3) . . ?
O10 Zr01 Zr02 119.7(2) . . ?
O11 Zr01 Zr02 117.5(3) . . ?
O2 Zr01 Zr02 160.8(2) 3_556 . ?
O2 Zr01 Zr02 73.4(2) 12 . ?
Zr02 Zr01 Zr02 87.41(7) 10_556 . ?
O5 Zr01 Zr01 33.1(3) 10_556 3_556 ?
O5 Zr01 Zr01 33.1(3) . 3_556 ?
O6 Zr01 Zr01 91.9(3) 10_556 3_556 ?
O6 Zr01 Zr01 91.9(3) . 3_556 ?
O10 Zr01 Zr01 178.6(3) . 3_556 ?
O11 Zr01 Zr01 84.4(4) . 3_556 ?
O2 Zr01 Zr01 108.4(3) 3_556 3_556 ?
O2 Zr01 Zr01 108.4(3) 12 3_556 ?
Zr02 Zr01 Zr01 59.47(4) 10_556 3_556 ?
Zr02 Zr01 Zr01 59.47(4) . 3_556 ?
O5 Zr01 Zr03 91.1(4) 10_556 . ?
O5 Zr01 Zr03 91.1(4) . . ?
O6 Zr01 Zr03 34.3(2) 10_556 . ?
O6 Zr01 Zr03 34.3(2) . . ?
O10 Zr01 Zr03 88.7(3) . . ?
O11 Zr01 Zr03 174.3(4) . . ?
O2 Zr01 Zr03 109.3(2) 3_556 . ?
O2 Zr01 Zr03 109.3(2) 12 . ?
Zr02 Zr01 Zr03 58.97(5) 10_556 . ?
Zr02 Zr01 Zr03 58.97(5) . . ?
Zr01 Zr01 Zr03 89.87(7) 3_556 . ?
O7 Zr02 O6 71.1(3) . . ?
O7 Zr02 O6 71.1(3) . 12 ?
O6 Zr02 O6 113.4(5) . 12 ?
O7 Zr02 O3 79.9(4) . 13_556 ?
O6 Zr02 O3 142.2(3) . 13_556 ?
O6 Zr02 O3 77.8(4) 12 13_556 ?
O7 Zr02 O3 79.9(4) . 8_456 ?
O6 Zr02 O3 77.8(4) . 8_456 ?
O6 Zr02 O3 142.2(4) 12 8_456 ?
O3 Zr02 O3 73.6(6) 13_556 8_456 ?
O7 Zr02 O5 108.0(5) . . ?
O6 Zr02 O5 71.3(3) . . ?
O6 Zr02 O5 71.3(3) 12 . ?
O3 Zr02 O5 142.8(3) 13_556 . ?
O3 Zr02 O5 142.8(3) 8_456 . ?
O7 Zr02 O1 140.2(3) . . ?
O6 Zr02 O1 142.9(3) . . ?
O6 Zr02 O1 74.3(3) 12 . ?
O3 Zr02 O1 74.1(3) 13_556 . ?
O3 Zr02 O1 119.5(3) 8_456 . ?
O5 Zr02 O1 78.1(3) . . ?
O7 Zr02 O1 140.2(3) . 12 ?
O6 Zr02 O1 74.3(3) . 12 ?
O6 Zr02 O1 142.9(3) 12 12 ?
O3 Zr02 O1 119.5(3) 13_556 12 ?
O3 Zr02 O1 74.1(3) 8_456 12 ?
O5 Zr02 O1 78.1(3) . 12 ?
O1 Zr02 O1 79.4(6) . 12 ?
O7 Zr02 Zr03 34.43(17) . 3_556 ?
O6 Zr02 Zr03 92.9(2) . 3_556 ?
O6 Zr02 Zr03 36.7(2) 12 3_556 ?
O3 Zr02 Zr03 74.9(2) 13_556 3_556 ?
O3 Zr02 Zr03 110.6(2) 8_456 3_556 ?
O5 Zr02 Zr03 91.3(3) . 3_556 ?
O1 Zr02 Zr03 108.4(3) . 3_556 ?
O1 Zr02 Zr03 165.4(2) 12 3_556 ?
O7 Zr02 Zr03 34.43(17) . . ?
O6 Zr02 Zr03 36.7(2) . . ?
O6 Zr02 Zr03 92.9(2) 12 . ?
O3 Zr02 Zr03 110.6(2) 13_556 . ?
O3 Zr02 Zr03 74.9(2) 8_456 . ?
O5 Zr02 Zr03 91.3(3) . . ?
O1 Zr02 Zr03 165.4(2) . . ?
O1 Zr02 Zr03 108.4(3) 12 . ?
Zr03 Zr02 Zr03 61.34(9) 3_556 . ?
O7 Zr02 Zr01 89.2(3) . 3_556 ?
O6 Zr02 Zr01 92.2(2) . 3_556 ?
O6 Zr02 Zr01 35.8(2) 12 3_556 ?
O3 Zr02 Zr01 111.4(3) 13_556 3_556 ?
O3 Zr02 Zr01 167.0(2) 8_456 3_556 ?
O5 Zr02 Zr01 35.46(18) . 3_556 ?
O1 Zr02 Zr01 73.4(2) . 3_556 ?
O1 Zr02 Zr01 111.3(2) 12 3_556 ?
Zr03 Zr02 Zr01 61.23(4) 3_556 3_556 ?
Zr03 Zr02 Zr01 92.12(5) . 3_556 ?
O7 Zr02 Zr01 89.2(3) . . ?
O6 Zr02 Zr01 35.8(2) . . ?
O6 Zr02 Zr01 92.2(2) 12 . ?
O3 Zr02 Zr01 167.0(2) 13_556 . ?
O3 Zr02 Zr01 111.4(3) 8_456 . ?
O5 Zr02 Zr01 35.46(18) . . ?
O1 Zr02 Zr01 111.3(2) . . ?
O1 Zr02 Zr01 73.4(2) 12 . ?
Zr03 Zr02 Zr01 92.12(5) 3_556 . ?
Zr03 Zr02 Zr01 61.24(4) . . ?
Zr01 Zr02 Zr01 61.05(9) 3_556 . ?
O7 Zr03 O7 64.0(7) . 10_556 ?
O7 Zr03 O9 147.8(3) . . ?
O7 Zr03 O9 147.8(3) 10_556 . ?
O7 Zr03 O6 73.4(4) . . ?
O7 Zr03 O6 108.0(5) 10_556 . ?
O9 Zr03 O6 86.6(4) . . ?
O7 Zr03 O6 108.0(5) . 10_556 ?
O7 Zr03 O6 73.4(4) 10_556 10_556 ?
O9 Zr03 O6 86.6(4) . 10_556 ?
O6 Zr03 O6 68.1(4) . 10_556 ?
O7 Zr03 O8 86.3(6) . . ?
O7 Zr03 O8 86.3(6) 10_556 . ?
O9 Zr03 O8 97.5(6) . . ?
O6 Zr03 O8 145.8(2) . . ?
O6 Zr03 O8 145.8(2) 10_556 . ?
O7 Zr03 O4 80.6(5) . 8_456 ?
O7 Zr03 O4 140.3(5) 10_556 8_456 ?
O9 Zr03 O4 70.2(4) . 8_456 ?
O6 Zr03 O4 76.3(3) . 8_456 ?
O6 Zr03 O4 138.4(4) 10_556 8_456 ?
O8 Zr03 O4 73.3(3) . 8_456 ?
O7 Zr03 O4 140.3(5) . 15_454 ?
O7 Zr03 O4 80.6(5) 10_556 15_454 ?
O9 Zr03 O4 70.2(4) . 15_454 ?
O6 Zr03 O4 138.4(4) . 15_454 ?
O6 Zr03 O4 76.3(3) 10_556 15_454 ?
O8 Zr03 O4 73.3(3) . 15_454 ?
O4 Zr03 O4 123.2(6) 8_456 15_454 ?
O7 Zr03 Zr02 85.7(4) . 10_556 ?
O7 Zr03 Zr02 35.5(3) 10_556 10_556 ?
O9 Zr03 Zr02 119.7(2) . 10_556 ?
O6 Zr03 Zr02 89.5(2) . 10_556 ?
O6 Zr03 Zr02 38.0(3) 10_556 10_556 ?
O8 Zr03 Zr02 116.7(3) . 10_556 ?
O4 Zr03 Zr02 162.6(3) 8_456 10_556 ?
O4 Zr03 Zr02 74.2(3) 15_454 10_556 ?
O7 Zr03 Zr02 35.5(3) . . ?
O7 Zr03 Zr02 85.7(4) 10_556 . ?
O9 Zr03 Zr02 119.7(2) . . ?
O6 Zr03 Zr02 38.0(3) . . ?
O6 Zr03 Zr02 89.5(2) 10_556 . ?
O8 Zr03 Zr02 116.7(3) . . ?
O4 Zr03 Zr02 74.2(3) 8_456 . ?
O4 Zr03 Zr02 162.6(3) 15_454 . ?
Zr02 Zr03 Zr02 88.35(7) 10_556 . ?
O7 Zr03 Zr03 32.1(3) . 3_556 ?
O7 Zr03 Zr03 32.1(3) 10_556 3_556 ?
O9 Zr03 Zr03 178.4(4) . 3_556 ?
O6 Zr03 Zr03 92.1(3) . 3_556 ?
O6 Zr03 Zr03 92.1(3) 10_556 3_556 ?
O8 Zr03 Zr03 84.1(5) . 3_556 ?
O4 Zr03 Zr03 110.4(3) 8_456 3_556 ?
O4 Zr03 Zr03 110.4(3) 15_454 3_556 ?
Zr02 Zr03 Zr03 59.33(4) 10_556 3_556 ?
Zr02 Zr03 Zr03 59.33(5) . 3_556 ?
O7 Zr03 Zr01 88.7(4) . . ?
O7 Zr03 Zr01 88.7(4) 10_556 . ?
O9 Zr03 Zr01 88.3(4) . . ?
O6 Zr03 Zr01 34.1(2) . . ?
O6 Zr03 Zr01 34.1(2) 10_556 . ?
O8 Zr03 Zr01 174.2(5) . . ?
O4 Zr03 Zr01 108.9(3) 8_456 . ?
O4 Zr03 Zr01 108.9(3) 15_454 . ?
Zr02 Zr03 Zr01 59.79(5) 10_556 . ?
Zr02 Zr03 Zr01 59.79(5) . . ?
Zr03 Zr03 Zr01 90.12(7) 3_556 . ?

_refine_diff_density_max         1.428
_refine_diff_density_min         -1.598
_refine_diff_density_rms         0.102



