# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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 
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# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
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data_P16_054Ttg_sq
_database_code_depnum_ccdc_archive 'CCDC 1896107'
loop_
_audit_author_name
_audit_author_address
'Myoung Soo Lah'
;Ulsan National Institute of Science and Technology
South Korea
;
_audit_update_record             
;
2019-02-08 deposited with the CCDC.	2019-05-07 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 H44 F12 O40 Zr6'
_chemical_formula_weight         2132.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0024 0.0013 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0087 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0144 0.0085 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -1.8641 3.3435 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   17.445(3)
_cell_length_b                   17.445(3)
_cell_length_c                   22.934(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6979(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    243(2)
_cell_measurement_reflns_used    92597
_cell_measurement_theta_min      1.624
_cell_measurement_theta_max      33.319

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.015
_exptl_crystal_F_000             2096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    2.194
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_process_details   HKL3000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      243(2)
_diffrn_radiation_wavelength     0.650
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51191
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_av_R_equivalents  0.1437
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.624
_diffrn_reflns_theta_max         33.319
_diffrn_reflns_theta_full        22.955
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4582
_reflns_number_gt                1915
_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       'PAL BL2D-SMDC Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    SHELXS
_computing_structure_refinement  SHELXL
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_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)+(0.2000P)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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0129(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4582
_refine_ls_number_parameters     141
_refine_ls_number_restraints     147
_refine_ls_R_factor_all          0.1817
_refine_ls_R_factor_gt           0.1050
_refine_ls_wR_factor_ref         0.3324
_refine_ls_wR_factor_gt          0.2841
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.978
_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
Zr1 Zr 0.0000 0.0000 0.10696(4) 0.0485(4) Uani 1 8 d S T P . .
Zr2 Zr 0.10113(3) 0.10113(3) 0.0000 0.0553(3) Uani 1 4 d S T P . .
O1M O 0.0994(4) 0.0000 0.0516(2) 0.097(2) Uani 1 2 d S T P . .
O1 O 0.07552(19) 0.07552(19) 0.1559(2) 0.0609(11) Uani 1 2 d S T P . .
O2 O 0.1418(2) 0.1418(2) 0.0886(2) 0.0854(18) Uani 1 2 d S T P . .
O1S O 0.0985(4) 0.2270(3) 0.0000 0.0913(19) Uani 1 2 d S T P . .
C1 C 0.1252(3) 0.1252(3) 0.1405(3) 0.0686(18) Uani 1 2 d S T P . .
C2 C 0.1673(3) 0.1673(3) 0.1892(4) 0.083(2) Uani 1 2 d S T P . .
C3 C 0.1503(4) 0.1503(4) 0.2441(4) 0.142(6) Uani 1 2 d S T P . .
H3 H 0.1130 0.1130 0.2524 0.171 Uiso 1 2 calc R U P . .
C4 C 0.1872(4) 0.1872(4) 0.2884(4) 0.196(9) Uani 1 2 d S T P . .
H4 H 0.1748 0.1748 0.3271 0.235 Uiso 1 2 calc R U P . .
C5 C 0.2176(4) 0.2176(4) 0.1767(4) 0.126(5) Uani 1 2 d S T P . .
H5 H 0.2282 0.2282 0.1373 0.151 Uiso 1 2 calc R U P . .
C6 C 0.2593(3) 0.2593(3) 0.2217(3) 0.098(3) Uani 1 2 d S T P . .
C1A C 1.0000 0.3056(19) 0.1184(15) 0.147(9) Uani 0.25 2 d DS TU P A 1
F1A F 1.0000 0.2293(16) 0.1356(12) 0.115(7) Uani 0.25 2 d DS TU P A 1
F2A F 0.9323(12) 0.3201(11) 0.0890(9) 0.141(6) Uani 0.25 1 d D U P A 1
C2A C 1.0000 0.3437(14) 0.1783(15) 0.148(10) Uani 0.25 2 d DS TU P A 1
O1A O 0.9362(13) 0.3563(15) 0.1981(11) 0.142(9) Uani 0.25 1 d D U P A 1
C1B C 1.0000 0.3782(19) 0.1912(17) 0.196(11) Uani 0.25 2 d DS TU P B 2
F1B F 1.0000 0.310(2) 0.2214(18) 0.192(10) Uani 0.25 2 d DS TU P B 2
F2B F 0.9330(9) 0.4071(17) 0.1804(14) 0.222(12) Uani 0.25 1 d D U P B 2
C2B C 1.0000 0.3108(16) 0.1507(12) 0.191(11) Uani 0.25 2 d DS TU P B 2
O1B O 1.0408(17) 0.2704(17) 0.1265(13) 0.184(10) Uani 0.25 1 d D U P B 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
Zr1 O1M 2.149(6) . ?
Zr1 O1M 2.149(6) 4 ?
Zr1 O1M 2.149(6) 2 ?
Zr1 O1M 2.149(6) 3 ?
Zr1 O1 2.174(5) 2 ?
Zr1 O1 2.174(5) 4 ?
Zr1 O1 2.174(5) 3 ?
Zr1 O1 2.175(5) . ?
Zr1 Zr2 3.4989(10) 17 ?
Zr1 Zr2 3.4989(10) 19 ?
Zr1 Zr2 3.4989(10) 3 ?
Zr1 Zr2 3.4989(10) . ?
Zr2 O1M 2.125(3) . ?
Zr2 O1M 2.125(3) 20 ?
Zr2 O1M 2.125(3) 18 ?
Zr2 O1M 2.125(3) 3 ?
Zr2 O1S 2.197(6) 7 ?
Zr2 O1S 2.197(6) . ?
Zr2 O2 2.267(5) 18 ?
Zr2 O2 2.267(5) . ?
Zr2 Zr1 3.4989(10) 17 ?
Zr2 Zr2 3.5284(12) 3 ?
Zr2 Zr2 3.5284(12) 19 ?
O1M Zr2 2.125(3) 19 ?
O1 C1 1.276(9) . ?
O2 C1 1.257(9) . ?
C1 C2 1.526(10) . ?
C2 C5 1.275(12) . ?
C2 C3 1.326(14) . ?
C3 C4 1.365(12) . ?
C4 C6 1.341(14) 25 ?
C5 C6 1.457(11) . ?
C6 C4 1.341(14) 25 ?
C6 C6 1.375(16) 25 ?
C1A F2A 1.385(16) 22_755 ?
C1A F2A 1.385(16) . ?
C1A F1A 1.388(19) . ?
C1A C2A 1.524(19) . ?
C2A O1A 1.222(17) . ?
C2A O1A 1.222(17) 22_755 ?
C1B F2B 1.297(15) 22_755 ?
C1B F2B 1.297(15) . ?
C1B F1B 1.372(19) . ?
C1B C2B 1.497(19) . ?
F1B C2B 1.62(5) . ?
C2B O1B 1.146(17) . ?
C2B O1B 1.146(17) 22_755 ?
O1B O1B 1.42(6) 22_755 ?

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
O1M Zr1 O1M 69.60(19) . 4 ?
O1M Zr1 O1M 107.6(4) . 2 ?
O1M Zr1 O1M 69.60(19) 4 2 ?
O1M Zr1 O1M 69.60(19) . 3 ?
O1M Zr1 O1M 107.6(4) 4 3 ?
O1M Zr1 O1M 69.60(19) 2 3 ?
O1M Zr1 O1 142.51(5) . 2 ?
O1M Zr1 O1 79.37(17) 4 2 ?
O1M Zr1 O1 79.37(17) 2 2 ?
O1M Zr1 O1 142.51(5) 3 2 ?
O1M Zr1 O1 79.37(17) . 4 ?
O1M Zr1 O1 79.37(17) 4 4 ?
O1M Zr1 O1 142.51(5) 2 4 ?
O1M Zr1 O1 142.51(5) 3 4 ?
O1 Zr1 O1 74.58(12) 2 4 ?
O1M Zr1 O1 142.51(5) . 3 ?
O1M Zr1 O1 142.51(5) 4 3 ?
O1M Zr1 O1 79.37(17) 2 3 ?
O1M Zr1 O1 79.37(17) 3 3 ?
O1 Zr1 O1 74.58(12) 2 3 ?
O1 Zr1 O1 117.9(3) 4 3 ?
O1M Zr1 O1 79.37(17) . . ?
O1M Zr1 O1 142.51(5) 4 . ?
O1M Zr1 O1 142.51(5) 2 . ?
O1M Zr1 O1 79.37(17) 3 . ?
O1 Zr1 O1 117.9(3) 2 . ?
O1 Zr1 O1 74.58(12) 4 . ?
O1 Zr1 O1 74.58(12) 3 . ?
O1M Zr1 Zr2 89.60(16) . 17 ?
O1M Zr1 Zr2 34.83(9) 4 17 ?
O1M Zr1 Zr2 34.83(9) 2 17 ?
O1M Zr1 Zr2 89.60(16) 3 17 ?
O1 Zr1 Zr2 75.56(13) 2 17 ?
O1 Zr1 Zr2 111.19(8) 4 17 ?
O1 Zr1 Zr2 111.19(8) 3 17 ?
O1 Zr1 Zr2 166.53(13) . 17 ?
O1M Zr1 Zr2 34.82(9) . 19 ?
O1M Zr1 Zr2 34.83(9) 4 19 ?
O1M Zr1 Zr2 89.60(16) 2 19 ?
O1M Zr1 Zr2 89.60(16) 3 19 ?
O1 Zr1 Zr2 111.19(8) 2 19 ?
O1 Zr1 Zr2 75.56(13) 4 19 ?
O1 Zr1 Zr2 166.53(13) 3 19 ?
O1 Zr1 Zr2 111.19(8) . 19 ?
Zr2 Zr1 Zr2 60.558(19) 17 19 ?
O1M Zr1 Zr2 89.60(16) . 3 ?
O1M Zr1 Zr2 89.60(16) 4 3 ?
O1M Zr1 Zr2 34.83(9) 2 3 ?
O1M Zr1 Zr2 34.83(9) 3 3 ?
O1 Zr1 Zr2 111.19(8) 2 3 ?
O1 Zr1 Zr2 166.53(13) 4 3 ?
O1 Zr1 Zr2 75.56(13) 3 3 ?
O1 Zr1 Zr2 111.19(8) . 3 ?
Zr2 Zr1 Zr2 60.558(19) 17 3 ?
Zr2 Zr1 Zr2 90.97(3) 19 3 ?
O1M Zr1 Zr2 34.82(9) . . ?
O1M Zr1 Zr2 89.60(16) 4 . ?
O1M Zr1 Zr2 89.60(16) 2 . ?
O1M Zr1 Zr2 34.83(9) 3 . ?
O1 Zr1 Zr2 166.53(13) 2 . ?
O1 Zr1 Zr2 111.19(8) 4 . ?
O1 Zr1 Zr2 111.19(8) 3 . ?
O1 Zr1 Zr2 75.56(13) . . ?
Zr2 Zr1 Zr2 90.97(3) 17 . ?
Zr2 Zr1 Zr2 60.558(19) 19 . ?
Zr2 Zr1 Zr2 60.558(19) 3 . ?
O1M Zr2 O1M 106.7(4) . 20 ?
O1M Zr2 O1M 67.7(2) . 18 ?
O1M Zr2 O1M 70.5(3) 20 18 ?
O1M Zr2 O1M 70.5(3) . 3 ?
O1M Zr2 O1M 67.7(2) 20 3 ?
O1M Zr2 O1M 106.7(4) 18 3 ?
O1M Zr2 O1S 89.8(3) . 7 ?
O1M Zr2 O1S 146.07(11) 20 7 ?
O1M Zr2 O1S 89.8(3) 18 7 ?
O1M Zr2 O1S 146.07(11) 3 7 ?
O1M Zr2 O1S 146.07(11) . . ?
O1M Zr2 O1S 89.8(3) 20 . ?
O1M Zr2 O1S 146.07(11) 18 . ?
O1M Zr2 O1S 89.8(3) 3 . ?
O1S Zr2 O1S 92.4(3) 7 . ?
O1M Zr2 O2 139.81(13) . 18 ?
O1M Zr2 O2 76.36(18) 20 18 ?
O1M Zr2 O2 76.36(18) 18 18 ?
O1M Zr2 O2 139.81(13) 3 18 ?
O1S Zr2 O2 72.17(11) 7 18 ?
O1S Zr2 O2 72.17(11) . 18 ?
O1M Zr2 O2 76.37(18) . . ?
O1M Zr2 O2 139.81(13) 20 . ?
O1M Zr2 O2 139.81(13) 18 . ?
O1M Zr2 O2 76.37(18) 3 . ?
O1S Zr2 O2 72.17(11) 7 . ?
O1S Zr2 O2 72.17(11) . . ?
O2 Zr2 O2 127.5(3) 18 . ?
O1M Zr2 Zr1 35.27(15) . . ?
O1M Zr2 Zr1 88.00(16) 20 . ?
O1M Zr2 Zr1 88.00(16) 18 . ?
O1M Zr2 Zr1 35.27(15) 3 . ?
O1S Zr2 Zr1 119.58(10) 7 . ?
O1S Zr2 Zr1 119.58(10) . . ?
O2 Zr2 Zr1 160.77(14) 18 . ?
O2 Zr2 Zr1 71.74(14) . . ?
O1M Zr2 Zr1 88.00(16) . 17 ?
O1M Zr2 Zr1 35.27(15) 20 17 ?
O1M Zr2 Zr1 35.27(15) 18 17 ?
O1M Zr2 Zr1 88.00(16) 3 17 ?
O1S Zr2 Zr1 119.58(10) 7 17 ?
O1S Zr2 Zr1 119.58(10) . 17 ?
O2 Zr2 Zr1 71.74(14) 18 17 ?
O2 Zr2 Zr1 160.77(14) . 17 ?
Zr1 Zr2 Zr1 89.03(3) . 17 ?
O1M Zr2 Zr2 89.19(19) . 3 ?
O1M Zr2 Zr2 33.88(12) 20 3 ?
O1M Zr2 Zr2 89.19(19) 18 3 ?
O1M Zr2 Zr2 33.88(12) 3 3 ?
O1S Zr2 Zr2 178.81(17) 7 3 ?
O1S Zr2 Zr2 88.81(17) . 3 ?
O2 Zr2 Zr2 108.23(9) 18 3 ?
O2 Zr2 Zr2 108.23(9) . 3 ?
Zr1 Zr2 Zr2 59.721(10) . 3 ?
Zr1 Zr2 Zr2 59.721(9) 17 3 ?
O1M Zr2 Zr2 33.88(12) . 19 ?
O1M Zr2 Zr2 89.19(19) 20 19 ?
O1M Zr2 Zr2 33.88(12) 18 19 ?
O1M Zr2 Zr2 89.19(19) 3 19 ?
O1S Zr2 Zr2 88.81(17) 7 19 ?
O1S Zr2 Zr2 178.81(17) . 19 ?
O2 Zr2 Zr2 108.23(9) 18 19 ?
O2 Zr2 Zr2 108.23(9) . 19 ?
Zr1 Zr2 Zr2 59.721(10) . 19 ?
Zr1 Zr2 Zr2 59.721(9) 17 19 ?
Zr2 Zr2 Zr2 90.0 3 19 ?
Zr2 O1M Zr2 112.2(2) 19 . ?
Zr2 O1M Zr1 109.9(2) 19 . ?
Zr2 O1M Zr1 109.9(2) . . ?
C1 O1 Zr1 132.9(4) . . ?
C1 O2 Zr2 134.8(5) . . ?
O2 C1 O1 125.0(6) . . ?
O2 C1 C2 118.2(7) . . ?
O1 C1 C2 116.8(6) . . ?
C5 C2 C3 121.5(8) . . ?
C5 C2 C1 119.8(8) . . ?
C3 C2 C1 118.7(7) . . ?
C2 C3 C4 119.6(10) . . ?
C6 C4 C3 121.9(10) 25 . ?
C2 C5 C6 121.8(9) . . ?
C4 C6 C6 119.4(10) 25 25 ?
C4 C6 C5 124.8(8) 25 . ?
C6 C6 C5 115.8(10) 25 . ?
F2A C1A F2A 117(3) 22_755 . ?
F2A C1A F1A 108.3(17) 22_755 . ?
F2A C1A F1A 108.3(17) . . ?
F2A C1A C2A 111.1(17) 22_755 . ?
F2A C1A C2A 111.1(17) . . ?
F1A C1A C2A 99(2) . . ?
O1A C2A O1A 131(4) . 22_755 ?
O1A C2A C1A 114(2) . . ?
O1A C2A C1A 114(2) 22_755 . ?
F2B C1B F2B 129(3) 22_755 . ?
F2B C1B F1B 115.6(17) 22_755 . ?
F2B C1B F1B 115.6(17) . . ?
F2B C1B C2B 100.8(19) 22_755 . ?
F2B C1B C2B 100.8(19) . . ?
F1B C1B C2B 69(2) . . ?
C1B F1B C2B 59.3(16) . . ?
O1B C2B O1B 77(4) . 22_755 ?
O1B C2B C1B 141.6(19) . . ?
O1B C2B C1B 141.6(19) 22_755 . ?
O1B C2B F1B 118.8(11) . . ?
O1B C2B F1B 118.8(11) 22_755 . ?
C1B C2B F1B 52.0(13) . . ?
C2B O1B O1B 51.6(19) . 22_755 ?

_refine_diff_density_max         1.594
_refine_diff_density_min         -2.104
_refine_diff_density_rms         0.168



####################################################################### 
# 
# 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_p16_057or_sq
_database_code_depnum_ccdc_archive 'CCDC 1896108'
loop_
_audit_author_name
_audit_author_address
'Myoung Soo Lah'
;Ulsan National Institute of Science and Technology
South Korea
;
_audit_update_record             
;
2019-02-08 deposited with the CCDC.	2019-05-07 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 H68 F12 O52 Zr6'
_chemical_formula_weight         2348.42

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      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                   11.677(2)
_cell_length_b                   17.804(4)
_cell_length_c                   25.696(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5342.3(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    45359
_cell_measurement_theta_min      1.561
_cell_measurement_theta_max      26.999

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_F_000             2336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.667
_shelx_estimated_absorpt_T_min   0.974
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_process_details   HKL3000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28057
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.561
_diffrn_reflns_theta_max         29.549
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4293
_reflns_number_gt                3337
_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       'PAL BL2D-SMDC Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_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)+(0.1379P)²+3.9581P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0074(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4293
_refine_ls_number_parameters     210
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0593
_refine_ls_wR_factor_ref         0.1955
_refine_ls_wR_factor_gt          0.1848
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.105
_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 0.15162(4) 0.40064(2) 0.5000 0.02064(19) Uani 1 2 d S T P . .
Zr2 Zr 0.0000 0.5000 0.40448(2) 0.0187(2) Uani 1 4 d S T P . .
O1M O 0.1523(6) 0.5000 0.45431(16) 0.066(2) Uani 1 2 d S T P . .
O2M O 0.0000 0.3996(4) 0.4541(2) 0.081(3) Uani 1 2 d S T P . .
O1 O 0.2097(3) 0.35894(17) 0.42193(10) 0.0396(7) Uani 1 1 d . . . . .
O2 O 0.1129(2) 0.42520(15) 0.36175(9) 0.0281(5) Uani 1 1 d . . . . .
C1 C 0.1785(4) 0.3727(2) 0.37523(13) 0.0302(8) Uani 1 1 d . . . . .
C2 C 0.2203(4) 0.3216(2) 0.33345(15) 0.0384(10) Uani 1 1 d . . . . .
C3 C 0.2987(5) 0.2641(3) 0.34503(17) 0.0607(17) Uani 1 1 d . . . . .
H3 H 0.3275 0.2591 0.3786 0.073 Uiso 1 1 calc R U . . .
C4 C 0.3330(5) 0.2151(4) 0.30637(18) 0.068(2) Uani 1 1 d . . . . .
H4 H 0.3850 0.1772 0.3142 0.081 Uiso 1 1 calc R U . . .
C5 C 0.1762(4) 0.3278(3) 0.28409(16) 0.0448(12) Uani 1 1 d . . . . .
H5 H 0.1233 0.3654 0.2769 0.054 Uiso 1 1 calc R U . . .
C6 C 0.2095(4) 0.2784(3) 0.24440(15) 0.0434(11) Uani 1 1 d . . . . .
O1S O 0.3400(4) 0.4045(3) 0.5000 0.0390(11) Uani 1 2 d S T P . .
O2S O 0.1421(5) 0.2761(2) 0.5000 0.0462(11) Uani 1 2 d DS T P . .
H1S2 H 0.162(8) 0.260(5) 0.4689(2) 0.069 Uiso 0.5 1 d D U P . .
F1A F 0.0000 0.1831(11) 0.2996(6) 0.203(8) Uani 0.5 2 d DS TU P A 1
F2A F 0.0976(4) 0.0940(9) 0.3462(7) 0.231(8) Uani 0.5 1 d D U P A 1
O1A O 0.0914(4) 0.2169(13) 0.4183(9) 0.316(13) Uani 0.5 1 d D U P A 1
C1A C 0.0000 0.1440(8) 0.3474(6) 0.236(7) Uani 0.5 2 d DS TU P A 1
C2A C 0.0000 0.1923(9) 0.3965(5) 0.237(7) Uani 0.5 2 d DS TU P A 1
F1B F 0.0000 0.2703(8) 0.3914(7) 0.211(8) Uani 0.5 2 d DS TU P B 2
F2B F 0.0990(4) 0.1736(8) 0.4273(6) 0.193(6) Uani 0.5 1 d D U P B 2
O1B O 0.0914(4) 0.1222(14) 0.3241(9) 0.298(14) Uani 0.5 1 d D U P B 2
C1B C 0.0000 0.1923(9) 0.3965(5) 0.237(7) Uani 0.5 2 d DS TU P B 2
C2B C 0.0000 0.1440(8) 0.3474(6) 0.236(7) Uani 0.5 2 d DS TU P B 2
O11W O 0.0000 0.1545(9) 0.0679(5) 0.070(3) Uani 0.5 2 d S T P C 1
O21W O 0.5000 0.1942(13) 0.4435(9) 0.135(7) Uani 0.5 2 d S T P D 1
O31W O 0.307(3) 0.0933(15) 0.4283(12) 0.126(11) Uani 0.25 1 d . . P E 1
O12W O 0.0000 0.0765(18) 0.0723(7) 0.146(9) Uani 0.5 2 d S T P F 2
O22W O 0.0000 0.0675(18) 0.1829(7) 0.162(10) Uani 0.5 2 d S T P G 2
O32W O 0.1444(9) 0.0000 0.1213(9) 0.105(6) Uani 0.5 2 d S T P H 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
Zr1 O1M 2.123(2) 10_556 ?
Zr1 O1M 2.123(2) . ?
Zr1 O2M 2.128(3) . ?
Zr1 O2M 2.128(3) 10_556 ?
Zr1 O1S 2.201(4) . ?
Zr1 O2S 2.220(4) . ?
Zr1 O1 2.244(3) 10_556 ?
Zr1 O1 2.244(3) . ?
Zr1 Zr2 3.5055(6) . ?
Zr1 Zr2 3.5055(7) 9_566 ?
Zr1 Zr1 3.5380(11) 11_565 ?
Zr1 Zr1 3.5409(12) 3_556 ?
Zr2 O2 2.172(2) 12 ?
Zr2 O2 2.172(2) 11_565 ?
Zr2 O2 2.172(2) 2_565 ?
Zr2 O2 2.172(2) . ?
Zr2 O1M 2.191(5) . ?
Zr2 O1M 2.191(5) 2_565 ?
Zr2 O2M 2.196(5) 2_565 ?
Zr2 O2M 2.196(5) . ?
Zr2 Zr1 3.5055(6) 11_565 ?
Zr2 Zr1 3.5055(6) 9_566 ?
Zr2 Zr1 3.5055(7) 3_556 ?
O1M Zr1 2.123(2) 11_565 ?
O2M Zr1 2.128(3) 3_556 ?
O1 C1 1.278(4) . ?
O2 C1 1.256(5) . ?
C1 C2 1.490(5) . ?
C2 C5 1.373(5) . ?
C2 C3 1.405(6) . ?
C3 C4 1.382(6) . ?
C4 C6 1.401(6) 13 ?
C5 C6 1.402(5) . ?
C6 C4 1.401(6) 13 ?
C6 C6 1.413(8) 13 ?
F1A C1A 1.413(9) . ?
F2A C1A 1.446(8) . ?
O1A C2A 1.283(9) . ?
C1A F2A 1.446(8) 12 ?
C1A C2A 1.526(7) . ?
C2A O1A 1.283(9) 12 ?
F1B C1B 1.394(9) . ?
F2B C1B 1.441(8) . ?
O1B C2B 1.284(10) . ?
C1B F2B 1.441(8) 12 ?
C1B C2B 1.526(7) . ?
C2B O1B 1.284(10) 12 ?

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
O1M Zr1 O1M 67.14(19) 10_556 . ?
O1M Zr1 O2M 108.5(3) 10_556 . ?
O1M Zr1 O2M 72.8(2) . . ?
O1M Zr1 O2M 72.8(2) 10_556 10_556 ?
O1M Zr1 O2M 108.5(3) . 10_556 ?
O2M Zr1 O2M 67.4(3) . 10_556 ?
O1M Zr1 O1S 88.3(2) 10_556 . ?
O1M Zr1 O1S 88.3(2) . . ?
O2M Zr1 O1S 146.29(13) . . ?
O2M Zr1 O1S 146.29(13) 10_556 . ?
O1M Zr1 O2S 146.34(9) 10_556 . ?
O1M Zr1 O2S 146.34(9) . . ?
O2M Zr1 O2S 87.1(2) . . ?
O2M Zr1 O2S 87.1(2) 10_556 . ?
O1S Zr1 O2S 94.68(19) . . ?
O1M Zr1 O1 77.30(14) 10_556 10_556 ?
O1M Zr1 O1 140.25(14) . 10_556 ?
O2M Zr1 O1 138.10(14) . 10_556 ?
O2M Zr1 O1 75.66(19) 10_556 10_556 ?
O1S Zr1 O1 73.05(10) . 10_556 ?
O2S Zr1 O1 71.62(10) . 10_556 ?
O1M Zr1 O1 140.25(14) 10_556 . ?
O1M Zr1 O1 77.30(14) . . ?
O2M Zr1 O1 75.67(19) . . ?
O2M Zr1 O1 138.10(14) 10_556 . ?
O1S Zr1 O1 73.05(10) . . ?
O2S Zr1 O1 71.62(10) . . ?
O1 Zr1 O1 126.76(15) 10_556 . ?
O1M Zr1 Zr2 88.20(15) 10_556 . ?
O1M Zr1 Zr2 36.32(15) . . ?
O2M Zr1 Zr2 36.48(14) . . ?
O2M Zr1 Zr2 88.44(19) 10_556 . ?
O1S Zr1 Zr2 119.27(8) . . ?
O2S Zr1 Zr2 118.60(9) . . ?
O1 Zr1 Zr2 161.00(7) 10_556 . ?
O1 Zr1 Zr2 72.16(7) . . ?
O1M Zr1 Zr2 36.32(15) 10_556 9_566 ?
O1M Zr1 Zr2 88.20(15) . 9_566 ?
O2M Zr1 Zr2 88.44(19) . 9_566 ?
O2M Zr1 Zr2 36.48(14) 10_556 9_566 ?
O1S Zr1 Zr2 119.27(8) . 9_566 ?
O2S Zr1 Zr2 118.60(9) . 9_566 ?
O1 Zr1 Zr2 72.16(7) 10_556 9_566 ?
O1 Zr1 Zr2 161.00(7) . 9_566 ?
Zr2 Zr1 Zr2 88.88(2) . 9_566 ?
O1M Zr1 Zr1 33.57(10) 10_556 11_565 ?
O1M Zr1 Zr1 33.57(10) . 11_565 ?
O2M Zr1 Zr1 90.5(2) . 11_565 ?
O2M Zr1 Zr1 90.5(2) 10_556 11_565 ?
O1S Zr1 Zr1 88.20(13) . 11_565 ?
O2S Zr1 Zr1 177.13(14) . 11_565 ?
O1 Zr1 Zr1 109.32(8) 10_556 11_565 ?
O1 Zr1 Zr1 109.32(8) . 11_565 ?
Zr2 Zr1 Zr1 59.692(10) . 11_565 ?
Zr2 Zr1 Zr1 59.692(10) 9_566 11_565 ?
O1M Zr1 Zr1 90.22(19) 10_556 3_556 ?
O1M Zr1 Zr1 90.21(19) . 3_556 ?
O2M Zr1 Zr1 33.70(13) . 3_556 ?
O2M Zr1 Zr1 33.70(13) 10_556 3_556 ?
O1S Zr1 Zr1 178.20(13) . 3_556 ?
O2S Zr1 Zr1 87.13(14) . 3_556 ?
O1 Zr1 Zr1 107.58(9) 10_556 3_556 ?
O1 Zr1 Zr1 107.58(9) . 3_556 ?
Zr2 Zr1 Zr1 59.665(10) . 3_556 ?
Zr2 Zr1 Zr1 59.665(10) 9_566 3_556 ?
Zr1 Zr1 Zr1 90.0 11_565 3_556 ?
O2 Zr2 O2 119.27(14) 12 11_565 ?
O2 Zr2 O2 75.63(15) 12 2_565 ?
O2 Zr2 O2 74.76(15) 11_565 2_565 ?
O2 Zr2 O2 74.76(15) 12 . ?
O2 Zr2 O2 75.63(15) 11_565 . ?
O2 Zr2 O2 119.27(14) 2_565 . ?
O2 Zr2 O1M 142.00(8) 12 . ?
O2 Zr2 O1M 78.62(15) 11_565 . ?
O2 Zr2 O1M 142.00(8) 2_565 . ?
O2 Zr2 O1M 78.62(15) . . ?
O2 Zr2 O1M 78.62(15) 12 2_565 ?
O2 Zr2 O1M 142.00(8) 11_565 2_565 ?
O2 Zr2 O1M 78.62(15) 2_565 2_565 ?
O2 Zr2 O1M 142.00(8) . 2_565 ?
O1M Zr2 O1M 108.5(3) . 2_565 ?
O2 Zr2 O2M 142.43(8) 12 2_565 ?
O2 Zr2 O2M 78.11(18) 11_565 2_565 ?
O2 Zr2 O2M 78.11(18) 2_565 2_565 ?
O2 Zr2 O2M 142.44(8) . 2_565 ?
O1M Zr2 O2M 70.18(13) . 2_565 ?
O1M Zr2 O2M 70.18(13) 2_565 2_565 ?
O2 Zr2 O2M 78.11(18) 12 . ?
O2 Zr2 O2M 142.43(8) 11_565 . ?
O2 Zr2 O2M 142.43(8) 2_565 . ?
O2 Zr2 O2M 78.11(18) . . ?
O1M Zr2 O2M 70.18(13) . . ?
O1M Zr2 O2M 70.18(13) 2_565 . ?
O2M Zr2 O2M 109.1(4) 2_565 . ?
O2 Zr2 Zr1 165.92(7) 12 11_565 ?
O2 Zr2 Zr1 74.81(7) 11_565 11_565 ?
O2 Zr2 Zr1 110.56(7) 2_565 11_565 ?
O2 Zr2 Zr1 110.90(7) . 11_565 ?
O1M Zr2 Zr1 35.02(8) . 11_565 ?
O1M Zr2 Zr1 90.04(14) 2_565 11_565 ?
O2M Zr2 Zr1 35.19(10) 2_565 11_565 ?
O2M Zr2 Zr1 90.27(18) . 11_565 ?
O2 Zr2 Zr1 110.90(7) 12 9_566 ?
O2 Zr2 Zr1 110.56(7) 11_565 9_566 ?
O2 Zr2 Zr1 74.81(7) 2_565 9_566 ?
O2 Zr2 Zr1 165.92(7) . 9_566 ?
O1M Zr2 Zr1 90.04(14) . 9_566 ?
O1M Zr2 Zr1 35.02(8) 2_565 9_566 ?
O2M Zr2 Zr1 35.19(10) 2_565 9_566 ?
O2M Zr2 Zr1 90.27(18) . 9_566 ?
Zr1 Zr2 Zr1 60.67(2) 11_565 9_566 ?
O2 Zr2 Zr1 74.81(7) 12 3_556 ?
O2 Zr2 Zr1 165.92(7) 11_565 3_556 ?
O2 Zr2 Zr1 110.90(7) 2_565 3_556 ?
O2 Zr2 Zr1 110.56(7) . 3_556 ?
O1M Zr2 Zr1 90.04(14) . 3_556 ?
O1M Zr2 Zr1 35.02(8) 2_565 3_556 ?
O2M Zr2 Zr1 90.27(18) 2_565 3_556 ?
O2M Zr2 Zr1 35.19(10) . 3_556 ?
Zr1 Zr2 Zr1 91.12(2) 11_565 3_556 ?
Zr1 Zr2 Zr1 60.615(19) 9_566 3_556 ?
O2 Zr2 Zr1 110.56(7) 12 . ?
O2 Zr2 Zr1 110.90(7) 11_565 . ?
O2 Zr2 Zr1 165.92(7) 2_565 . ?
O2 Zr2 Zr1 74.81(7) . . ?
O1M Zr2 Zr1 35.02(8) . . ?
O1M Zr2 Zr1 90.04(14) 2_565 . ?
O2M Zr2 Zr1 90.27(18) 2_565 . ?
O2M Zr2 Zr1 35.19(10) . . ?
Zr1 Zr2 Zr1 60.615(19) 11_565 . ?
Zr1 Zr2 Zr1 91.12(2) 9_566 . ?
Zr1 Zr2 Zr1 60.67(2) 3_556 . ?
Zr1 O1M Zr1 112.86(19) 11_565 . ?
Zr1 O1M Zr2 108.7(2) 11_565 . ?
Zr1 O1M Zr2 108.7(2) . . ?
Zr1 O2M Zr1 112.6(3) . 3_556 ?
Zr1 O2M Zr2 108.3(2) . . ?
Zr1 O2M Zr2 108.3(2) 3_556 . ?
C1 O1 Zr1 133.6(3) . . ?
C1 O2 Zr2 133.3(2) . . ?
O2 C1 O1 125.1(3) . . ?
O2 C1 C2 117.1(3) . . ?
O1 C1 C2 117.8(3) . . ?
C5 C2 C3 119.9(4) . . ?
C5 C2 C1 119.6(4) . . ?
C3 C2 C1 120.4(3) . . ?
C4 C3 C2 119.8(4) . . ?
C3 C4 C6 121.0(4) . 13 ?
C2 C5 C6 121.2(4) . . ?
C4 C6 C5 121.8(4) 13 . ?
C4 C6 C6 119.1(4) 13 13 ?
C5 C6 C6 119.1(4) . 13 ?
F1A C1A F2A 106.5(8) . 12 ?
F1A C1A F2A 106.5(8) . . ?
F2A C1A F2A 104.0(10) 12 . ?
F1A C1A C2A 116.1(8) . . ?
F2A C1A C2A 111.4(10) 12 . ?
F2A C1A C2A 111.4(10) . . ?
O1A C2A O1A 112.5(15) . 12 ?
O1A C2A C1A 123.7(7) . . ?
O1A C2A C1A 123.7(7) 12 . ?
F1B C1B F2B 106.3(7) . . ?
F1B C1B F2B 106.3(7) . 12 ?
F2B C1B F2B 106.7(10) . 12 ?
F1B C1B C2B 119.0(9) . . ?
F2B C1B C2B 108.9(9) . . ?
F2B C1B C2B 108.9(9) 12 . ?
O1B C2B O1B 112.4(15) 12 . ?
O1B C2B C1B 123.8(7) 12 . ?
O1B C2B C1B 123.8(7) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2S H1S2 O1A 0.879(10) 1.72(8) 2.42(2) 134(10) .

_refine_diff_density_max         1.514
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.183



####################################################################### 
# 
# 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_P17_026ttg_sq
_database_code_depnum_ccdc_archive 'CCDC 1896110'
loop_
_audit_author_name
_audit_author_address
'Myoung Soo Lah'
;Ulsan National Institute of Science and Technology
South Korea
;
_audit_update_record             
;
2019-02-08 deposited with the CCDC.	2019-05-07 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            'C64 H42 N2 O40 Zr6'
_chemical_formula_weight         2026.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -3.5084 0.5477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   14.955(2)
_cell_length_b                   14.955(2)
_cell_length_c                   26.077(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5832(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    65714
_cell_measurement_theta_min      1.897
_cell_measurement_theta_max      33.456

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.154
_exptl_crystal_F_000             2000
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.047
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_process_details   HKL3000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34972
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.897
_diffrn_reflns_theta_max         33.456
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3181
_reflns_number_gt                2723
_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       'PAL BL2D-SMDC Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    SHELXS
_computing_structure_refinement  SHELXL
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_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)+(0.1266P)²+28.8964P] 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       0.0069(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3181
_refine_ls_number_parameters     109
_refine_ls_number_restraints     190
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0677
_refine_ls_wR_factor_ref         0.1995
_refine_ls_wR_factor_gt          0.1923
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.379
_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 0.5000 0.5000 0.09409(2) 0.00998(18) Uani 1 8 d S T P . .
Zr2 Zr 0.38161(2) 0.38161(2) 0.0000 0.01401(18) Uani 1 4 d S T P . .
O1M O 0.5000 0.3816(4) 0.04517(15) 0.0616(17) Uani 1 2 d S TU P A .
O1 O 0.41155(13) 0.41155(13) 0.13677(10) 0.0223(6) Uani 1 2 d S T P A .
O2 O 0.33471(16) 0.33471(16) 0.07769(12) 0.0519(13) Uani 1 2 d S TU P A .
C1 C 0.3547(2) 0.3547(2) 0.12341(15) 0.0343(11) Uani 1 2 d S T P . .
C2 C 0.3068(2) 0.3068(2) 0.16533(17) 0.0515(17) Uani 1 2 d S TU P A .
C3 C 0.3266(3) 0.3266(3) 0.21488(19) 0.062(2) Uani 1 2 d S TU P . .
H3 H 0.3701 0.3701 0.2221 0.075 Uiso 1 2 calc R U P A .
C4 C 0.2825(2) 0.2825(2) 0.25572(19) 0.063(2) Uani 1 2 d S TU P A .
C5 C 0.2422(3) 0.2422(3) 0.15378(19) 0.078(3) Uani 1 2 d S TU P . .
H5 H 0.2289 0.2289 0.1194 0.094 Uiso 1 2 calc R U P A .
C6 C 0.3020(3) 0.3020(3) 0.3077(2) 0.081(3) Uani 1 2 d S TU P . .
O4 O 0.2343(3) 0.3930(4) 0.0000 0.0648(16) Uani 0.5 2 d DS TU P A 1
O5 O 0.2258(7) 0.2431(6) 0.0000 0.303(16) Uani 0.5 2 d DS TU P A 1
C7 C 0.1854(4) 0.3250(5) 0.0000 0.174(13) Uani 0.5 2 d DS TU P A 1
C8 C 0.0886(4) 0.3343(5) 0.0000 0.144(12) Uani 0.5 2 d DS TU P A 1
C9 C 0.0475(3) 0.4198(5) 0.0000 0.32(3) Uani 0.5 2 d DS TU P A 1
C10 C 0.0472(3) 0.2523(6) 0.0000 0.27(3) Uani 0.5 2 d DS TU P A 1
N1 N 0.0971(6) 0.5000 0.0000 0.32(5) Uani 0.25 4 d DS TU P A 1
N2 N 0.0810(7) 0.1681(6) 0.0000 0.27(5) Uani 0.125 2 d DS TU P A 1
O1S O 0.2343(3) 0.3930(4) 0.0000 0.0648(16) Uani 0.5 2 d S TU P A 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
Zr1 O1 2.177(3) 2_665 ?
Zr1 O1 2.177(3) 3_655 ?
Zr1 O1 2.177(3) 4_565 ?
Zr1 O1 2.177(3) . ?
Zr1 O1M 2.182(4) 4_565 ?
Zr1 O1M 2.182(4) 3_655 ?
Zr1 O1M 2.182(4) 2_665 ?
Zr1 O1M 2.182(4) . ?
Zr1 Zr2 3.5057(7) 19_565 ?
Zr1 Zr2 3.5057(7) 3_655 ?
Zr1 Zr2 3.5057(7) 17_665 ?
Zr2 O1M 2.127(2) . ?
Zr2 O1M 2.127(2) 4_565 ?
Zr2 O1M 2.127(2) 19_565 ?
Zr2 O1M 2.127(2) 18 ?
Zr2 O4 2.210(5) 7 ?
Zr2 O1S 2.210(5) 7 ?
Zr2 O1S 2.210(5) . ?
Zr2 O4 2.210(5) . ?
Zr2 O2 2.255(3) 18 ?
Zr2 O2 2.256(3) . ?
Zr2 Zr1 3.5057(7) 17_665 ?
Zr2 Zr2 3.5411(8) 3_655 ?
O1M Zr2 2.127(2) 3_655 ?
O1 C1 1.251(5) . ?
O2 C1 1.265(5) . ?
C1 C2 1.490(6) . ?
C2 C3 1.358(7) . ?
C2 C5 1.401(8) . ?
C3 C4 1.415(7) . ?
C4 C4 1.407(11) 25 ?
C4 C6 1.418(8) . ?
C5 C6 1.371(8) 25 ?
C6 C5 1.371(8) 25 ?
O4 C7 1.253(7) . ?
O5 O5 0.367(16) 7 ?
O5 C7 1.365(7) . ?
O5 C7 1.717(12) 7 ?
C7 C8 1.454(7) . ?
C7 O5 1.717(12) 7 ?
C8 C10 1.373(7) . ?
C8 C9 1.418(6) . ?
C9 N1 1.411(7) . ?
C9 C9 1.420(8) 5 ?
C10 N2 1.358(7) . ?
C10 C10 1.413(8) 5 ?
N1 C9 1.411(7) 21_565 ?
N2 N2 1.84(2) 7 ?

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 Zr1 O1 74.84(7) 2_665 3_655 ?
O1 Zr1 O1 74.84(7) 2_665 4_565 ?
O1 Zr1 O1 118.50(15) 3_655 4_565 ?
O1 Zr1 O1 118.50(15) 2_665 . ?
O1 Zr1 O1 74.84(7) 3_655 . ?
O1 Zr1 O1 74.84(7) 4_565 . ?
O1 Zr1 O1M 142.37(3) 2_665 4_565 ?
O1 Zr1 O1M 142.37(3) 3_655 4_565 ?
O1 Zr1 O1M 78.81(13) 4_565 4_565 ?
O1 Zr1 O1M 78.81(13) . 4_565 ?
O1 Zr1 O1M 78.81(13) 2_665 3_655 ?
O1 Zr1 O1M 78.81(13) 3_655 3_655 ?
O1 Zr1 O1M 142.37(3) 4_565 3_655 ?
O1 Zr1 O1M 142.37(3) . 3_655 ?
O1M Zr1 O1M 108.5(3) 4_565 3_655 ?
O1 Zr1 O1M 78.81(13) 2_665 2_665 ?
O1 Zr1 O1M 142.37(3) 3_655 2_665 ?
O1 Zr1 O1M 78.81(13) 4_565 2_665 ?
O1 Zr1 O1M 142.37(3) . 2_665 ?
O1M Zr1 O1M 70.02(16) 4_565 2_665 ?
O1M Zr1 O1M 70.02(16) 3_655 2_665 ?
O1 Zr1 O1M 142.37(3) 2_665 . ?
O1 Zr1 O1M 78.81(13) 3_655 . ?
O1 Zr1 O1M 142.37(3) 4_565 . ?
O1 Zr1 O1M 78.81(13) . . ?
O1M Zr1 O1M 70.02(16) 4_565 . ?
O1M Zr1 O1M 70.02(16) 3_655 . ?
O1M Zr1 O1M 108.5(3) 2_665 . ?
O1 Zr1 Zr2 110.97(5) 2_665 19_565 ?
O1 Zr1 Zr2 166.33(7) 3_655 19_565 ?
O1 Zr1 Zr2 75.17(7) 4_565 19_565 ?
O1 Zr1 Zr2 110.97(5) . 19_565 ?
O1M Zr1 Zr2 35.02(7) 4_565 19_565 ?
O1M Zr1 Zr2 90.03(14) 3_655 19_565 ?
O1M Zr1 Zr2 35.02(7) 2_665 19_565 ?
O1M Zr1 Zr2 90.04(14) . 19_565 ?
O1 Zr1 Zr2 110.97(5) 2_665 3_655 ?
O1 Zr1 Zr2 75.17(7) 3_655 3_655 ?
O1 Zr1 Zr2 166.33(7) 4_565 3_655 ?
O1 Zr1 Zr2 110.97(5) . 3_655 ?
O1M Zr1 Zr2 90.03(14) 4_565 3_655 ?
O1M Zr1 Zr2 35.02(7) 3_655 3_655 ?
O1M Zr1 Zr2 90.03(14) 2_665 3_655 ?
O1M Zr1 Zr2 35.02(7) . 3_655 ?
Zr2 Zr1 Zr2 91.16(2) 19_565 3_655 ?
O1 Zr1 Zr2 75.17(7) 2_665 17_665 ?
O1 Zr1 Zr2 110.97(5) 3_655 17_665 ?
O1 Zr1 Zr2 110.97(5) 4_565 17_665 ?
O1 Zr1 Zr2 166.33(7) . 17_665 ?
O1M Zr1 Zr2 90.03(14) 4_565 17_665 ?
O1M Zr1 Zr2 35.02(7) 3_655 17_665 ?
O1M Zr1 Zr2 35.02(7) 2_665 17_665 ?
O1M Zr1 Zr2 90.04(14) . 17_665 ?
Zr2 Zr1 Zr2 60.670(12) 19_565 17_665 ?
Zr2 Zr1 Zr2 60.670(12) 3_655 17_665 ?
O1M Zr2 O1M 72.1(2) . 4_565 ?
O1M Zr2 O1M 107.9(3) . 19_565 ?
O1M Zr2 O1M 67.27(18) 4_565 19_565 ?
O1M Zr2 O1M 67.27(18) . 18 ?
O1M Zr2 O1M 107.9(3) 4_565 18 ?
O1M Zr2 O1M 72.1(2) 19_565 18 ?
O1M Zr2 O4 86.3(2) . 7 ?
O1M Zr2 O4 146.11(8) 4_565 7 ?
O1M Zr2 O4 146.11(8) 19_565 7 ?
O1M Zr2 O4 86.3(2) 18 7 ?
O1M Zr2 O1S 86.3(2) . 7 ?
O1M Zr2 O1S 146.11(8) 4_565 7 ?
O1M Zr2 O1S 146.11(8) 19_565 7 ?
O1M Zr2 O1S 86.3(2) 18 7 ?
O1M Zr2 O1S 146.11(8) . . ?
O1M Zr2 O1S 86.3(2) 4_565 . ?
O1M Zr2 O1S 86.3(2) 19_565 . ?
O1M Zr2 O1S 146.11(8) 18 . ?
O1S Zr2 O1S 98.9(3) 7 . ?
O1M Zr2 O4 146.11(8) . . ?
O1M Zr2 O4 86.3(2) 4_565 . ?
O1M Zr2 O4 86.3(2) 19_565 . ?
O1M Zr2 O4 146.11(8) 18 . ?
O4 Zr2 O4 98.9(3) 7 . ?
O1M Zr2 O2 139.15(8) . 18 ?
O1M Zr2 O2 139.15(8) 4_565 18 ?
O1M Zr2 O2 76.19(14) 19_565 18 ?
O1M Zr2 O2 76.19(14) 18 18 ?
O4 Zr2 O2 73.38(8) 7 18 ?
O1S Zr2 O2 73.38(8) 7 18 ?
O1S Zr2 O2 73.38(8) . 18 ?
O4 Zr2 O2 73.38(8) . 18 ?
O1M Zr2 O2 76.20(14) . . ?
O1M Zr2 O2 76.20(14) 4_565 . ?
O1M Zr2 O2 139.15(8) 19_565 . ?
O1M Zr2 O2 139.15(8) 18 . ?
O4 Zr2 O2 73.38(8) 7 . ?
O1S Zr2 O2 73.38(8) 7 . ?
O1S Zr2 O2 73.38(8) . . ?
O4 Zr2 O2 73.38(8) . . ?
O2 Zr2 O2 127.83(18) 18 . ?
O1M Zr2 Zr1 88.12(14) . 17_665 ?
O1M Zr2 Zr1 88.12(14) 4_565 17_665 ?
O1M Zr2 Zr1 36.08(12) 19_565 17_665 ?
O1M Zr2 Zr1 36.08(12) 18 17_665 ?
O4 Zr2 Zr1 117.68(9) 7 17_665 ?
O1S Zr2 Zr1 117.68(9) 7 17_665 ?
O1S Zr2 Zr1 117.68(9) . 17_665 ?
O4 Zr2 Zr1 117.68(9) . 17_665 ?
O2 Zr2 Zr1 71.67(9) 18 17_665 ?
O2 Zr2 Zr1 160.51(9) . 17_665 ?
O1M Zr2 Zr2 33.64(9) . 3_655 ?
O1M Zr2 Zr2 90.00(16) 4_565 3_655 ?
O1M Zr2 Zr2 90.00(16) 19_565 3_655 ?
O1M Zr2 Zr2 33.64(9) 18 3_655 ?
O4 Zr2 Zr2 85.57(15) 7 3_655 ?
O1S Zr2 Zr2 85.57(15) 7 3_655 ?
O1S Zr2 Zr2 175.57(15) . 3_655 ?
O4 Zr2 Zr2 175.57(15) . 3_655 ?
O2 Zr2 Zr2 108.11(6) 18 3_655 ?
O2 Zr2 Zr2 108.12(6) . 3_655 ?
Zr1 Zr2 Zr2 59.667(6) 17_665 3_655 ?
Zr2 O1M Zr2 112.73(18) . 3_655 ?
Zr2 O1M Zr1 108.90(18) . . ?
Zr2 O1M Zr1 108.90(18) 3_655 . ?
C1 O1 Zr1 133.1(2) . . ?
C1 O2 Zr2 134.4(3) . . ?
O1 C1 O2 125.7(4) . . ?
O1 C1 C2 116.7(4) . . ?
O2 C1 C2 117.6(4) . . ?
C3 C2 C5 120.3(4) . . ?
C3 C2 C1 119.3(4) . . ?
C5 C2 C1 120.4(4) . . ?
C2 C3 C4 120.9(5) . . ?
C4 C4 C3 118.9(6) 25 . ?
C4 C4 C6 119.2(6) 25 . ?
C3 C4 C6 121.9(5) . . ?
C6 C5 C2 120.5(5) 25 . ?
C5 C6 C4 120.1(6) 25 . ?
C7 O4 Zr2 121.3(5) . . ?
O5 O5 C7 161.3(5) 7 . ?
O5 O5 C7 14.8(4) 7 7 ?
C7 O5 C7 146.5(8) . 7 ?
O4 C7 O5 118.0(6) . . ?
O4 C7 C8 120.2(5) . . ?
O5 C7 C8 121.8(6) . . ?
O4 C7 O5 114.1(5) . 7 ?
O5 C7 O5 3.9(2) . 7 ?
C8 C7 O5 125.7(5) . 7 ?
C10 C8 C9 127.5(6) . . ?
C10 C8 C7 111.3(5) . . ?
C9 C8 C7 121.2(5) . . ?
N1 C9 C8 122.6(5) . . ?
N1 C9 C9 121.8(4) . 5 ?
C8 C9 C9 115.7(3) . 5 ?
N2 C10 C8 131.4(6) . . ?
N2 C10 C10 111.9(5) . 5 ?
C8 C10 C10 116.8(3) . 5 ?
C9 N1 C9 116.5(9) . 21_565 ?
C10 N2 N2 156.8(5) . 7 ?

_refine_diff_density_max         2.514
_refine_diff_density_min         -2.154
_refine_diff_density_rms         0.195



####################################################################### 
# 
# 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_p17_035ttg_sq
_database_code_depnum_ccdc_archive 'CCDC 1896111'
loop_
_audit_author_name
_audit_author_address
'Myoung Soo Lah'
;Ulsan National Institute of Science and Technology
South Korea
;
_audit_update_record             
;
2019-02-08 deposited with the CCDC.	2019-05-07 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            'C64 H34 N2 O36 Zr6'
_chemical_formula_weight         1954.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -3.5084 0.5477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   14.839(2)
_cell_length_b                   14.839(2)
_cell_length_c                   26.030(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5732(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4567
_cell_measurement_theta_min      1.911
_cell_measurement_theta_max      33.303

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_F_000             1920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.555
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_process_details   HKL3000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31877
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.911
_diffrn_reflns_theta_max         33.303
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3064
_reflns_number_gt                1722
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3064
_refine_ls_number_parameters     104
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0868
_refine_ls_wR_factor_ref         0.3003
_refine_ls_wR_factor_gt          0.2613
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.062
_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
Zr1 Zr 0.5000 0.5000 0.09458(3) 0.0492(4) Uani 1 8 d S T P . .
Zr2 Zr 0.38139(4) 0.38139(4) 0.0000 0.0633(4) Uani 1 4 d S T P . .
O1M O 0.3636(7) 0.5000 0.0522(4) 0.066(3) Uani 0.5 2 d S T P . .
O12M O 0.3992(6) 0.5000 0.0396(3) 0.054(2) Uani 0.5 2 d S T P . .
O1 O 0.3321(3) 0.3321(3) 0.07651(18) 0.108(2) Uani 1 2 d S T P . .
O2 O 0.4115(2) 0.4115(2) 0.13720(15) 0.0817(13) Uani 1 2 d S T P . .
O3 O 0.4107(7) 0.2345(4) 0.0000 0.130(3) Uani 1 2 d S T P . .
C1 C 0.3520(4) 0.3520(4) 0.1224(3) 0.096(3) Uani 1 2 d S T P . .
C2 C 0.3053(4) 0.3053(4) 0.1644(3) 0.106(3) Uani 1 2 d S T P . .
C3 C 0.3263(4) 0.3263(4) 0.2137(3) 0.124(4) Uani 1 2 d S T P . .
H3 H 0.3698 0.3698 0.2205 0.149 Uiso 1 2 calc R U P . .
C4 C 0.2417(5) 0.2417(5) 0.1536(3) 0.156(5) Uani 1 2 d S T P . .
H4 H 0.2284 0.2284 0.1196 0.187 Uiso 1 2 calc R U P . .
C5 C 0.1967(4) 0.1967(4) 0.1926(3) 0.197(8) Uani 1 2 d S T P . .
H5 H 0.1534 0.1534 0.1850 0.237 Uiso 1 2 calc R U P . .
C6 C 0.2182(4) 0.2182(4) 0.2450(3) 0.131(4) Uani 1 2 d S T P . .
C7 C 0.5000 0.1920(14) 0.0000 0.156(6) Uani 1 4 d S TU P . .
C8 C 0.5000 0.0944(13) 0.0000 0.147(5) Uani 1 4 d S TU P . .
C9 C 0.4202(13) 0.0461(10) 0.0000 0.201(6) Uani 1 2 d DS TU P . .
N1 N 0.3301(18) 0.0860(17) 0.0000 0.206(14) Uani 0.25 2 d DS TU P . .
O4 O 0.280(3) 0.108(2) 0.0387(7) 0.35(3) Uani 0.25 1 d D U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O12M 2.070(9) . ?
Zr1 O12M 2.070(9) 3_655 ?
Zr1 O12M 2.070(9) 4_565 ?
Zr1 O12M 2.070(9) 2_665 ?
Zr1 O2 2.164(4) 2_665 ?
Zr1 O2 2.164(4) 3_655 ?
Zr1 O2 2.164(4) 4_565 ?
Zr1 O2 2.164(4) . ?
Zr1 O1M 2.305(11) 3_655 ?
Zr1 O1M 2.305(11) 2_665 ?
Zr1 O1M 2.305(11) 4_565 ?
Zr1 O1M 2.305(11) . ?
Zr2 O12M 2.057(4) 3_655 ?
Zr2 O12M 2.057(4) 20_655 ?
Zr2 O12M 2.057(4) 18 ?
Zr2 O12M 2.057(4) . ?
Zr2 O1M 2.239(6) . ?
Zr2 O1M 2.239(6) 3_655 ?
Zr2 O1M 2.239(6) 20_655 ?
Zr2 O1M 2.239(6) 18 ?
Zr2 O3 2.223(6) . ?
Zr2 O3 2.223(6) 7 ?
Zr2 O1 2.244(5) . ?
Zr2 O1 2.244(5) 18 ?
O1M O12M 0.622(9) . ?
O1M Zr2 2.239(6) 19_565 ?
O12M Zr2 2.057(4) 19_565 ?
O1 C1 1.265(8) . ?
O2 C1 1.306(9) . ?
O3 C7 1.467(12) . ?
C1 C2 1.469(10) . ?
C2 C3 1.358(11) . ?
C2 C4 1.362(13) . ?
C3 C6 1.423(10) 25 ?
C4 C5 1.387(12) . ?
C5 C6 1.438(12) . ?
C6 C6 1.360(17) 25 ?
C6 C3 1.423(10) 25 ?
C7 C8 1.45(3) . ?
C7 O3 1.467(12) 5_655 ?
C8 C9 1.384(17) 5_655 ?
C8 C9 1.384(17) . ?
C9 C9 1.37(3) 21 ?
C9 N1 1.462(19) . ?
N1 O4 1.298(18) 18 ?
N1 O4 1.298(18) . ?

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
O12M Zr1 O12M 61.4(3) . 3_655 ?
O12M Zr1 O12M 61.4(3) . 4_565 ?
O12M Zr1 O12M 92.5(5) 3_655 4_565 ?
O12M Zr1 O12M 92.5(5) . 2_665 ?
O12M Zr1 O12M 61.4(3) 3_655 2_665 ?
O12M Zr1 O12M 61.4(3) 4_565 2_665 ?
O12M Zr1 O2 142.47(7) . 2_665 ?
O12M Zr1 O2 142.47(7) 3_655 2_665 ?
O12M Zr1 O2 85.2(2) 4_565 2_665 ?
O12M Zr1 O2 85.2(2) 2_665 2_665 ?
O12M Zr1 O2 142.47(7) . 3_655 ?
O12M Zr1 O2 85.2(2) 3_655 3_655 ?
O12M Zr1 O2 142.47(7) 4_565 3_655 ?
O12M Zr1 O2 85.2(2) 2_665 3_655 ?
O2 Zr1 O2 74.76(11) 2_665 3_655 ?
O12M Zr1 O2 85.2(2) . 4_565 ?
O12M Zr1 O2 142.47(7) 3_655 4_565 ?
O12M Zr1 O2 85.2(2) 4_565 4_565 ?
O12M Zr1 O2 142.47(7) 2_665 4_565 ?
O2 Zr1 O2 74.76(11) 2_665 4_565 ?
O2 Zr1 O2 118.3(2) 3_655 4_565 ?
O12M Zr1 O2 85.2(2) . . ?
O12M Zr1 O2 85.2(2) 3_655 . ?
O12M Zr1 O2 142.47(7) 4_565 . ?
O12M Zr1 O2 142.47(7) 2_665 . ?
O2 Zr1 O2 118.3(2) 2_665 . ?
O2 Zr1 O2 74.76(11) 3_655 . ?
O2 Zr1 O2 74.76(11) 4_565 . ?
O12M Zr1 O1M 70.68(19) . 3_655 ?
O12M Zr1 O1M 15.2(3) 3_655 3_655 ?
O12M Zr1 O1M 107.7(4) 4_565 3_655 ?
O12M Zr1 O1M 70.68(19) 2_665 3_655 ?
O2 Zr1 O1M 141.12(6) 2_665 3_655 ?
O2 Zr1 O1M 73.27(19) 3_655 3_655 ?
O2 Zr1 O1M 141.12(6) 4_565 3_655 ?
O2 Zr1 O1M 73.27(19) . 3_655 ?
O12M Zr1 O1M 107.7(4) . 2_665 ?
O12M Zr1 O1M 70.68(19) 3_655 2_665 ?
O12M Zr1 O1M 70.68(19) 4_565 2_665 ?
O12M Zr1 O1M 15.2(3) 2_665 2_665 ?
O2 Zr1 O1M 73.27(19) 2_665 2_665 ?
O2 Zr1 O1M 73.27(19) 3_655 2_665 ?
O2 Zr1 O1M 141.12(6) 4_565 2_665 ?
O2 Zr1 O1M 141.11(6) . 2_665 ?
O1M Zr1 O1M 76.76(19) 3_655 2_665 ?
O12M Zr1 O1M 70.68(19) . 4_565 ?
O12M Zr1 O1M 107.7(4) 3_655 4_565 ?
O12M Zr1 O1M 15.2(3) 4_565 4_565 ?
O12M Zr1 O1M 70.68(19) 2_665 4_565 ?
O2 Zr1 O1M 73.27(19) 2_665 4_565 ?
O2 Zr1 O1M 141.12(6) 3_655 4_565 ?
O2 Zr1 O1M 73.27(19) 4_565 4_565 ?
O2 Zr1 O1M 141.11(6) . 4_565 ?
O1M Zr1 O1M 122.8(4) 3_655 4_565 ?
O1M Zr1 O1M 76.76(19) 2_665 4_565 ?
O12M Zr1 O1M 15.1(3) . . ?
O12M Zr1 O1M 70.68(19) 3_655 . ?
O12M Zr1 O1M 70.68(19) 4_565 . ?
O12M Zr1 O1M 107.7(4) 2_665 . ?
O2 Zr1 O1M 141.12(6) 2_665 . ?
O2 Zr1 O1M 141.12(6) 3_655 . ?
O2 Zr1 O1M 73.27(19) 4_565 . ?
O2 Zr1 O1M 73.27(19) . . ?
O1M Zr1 O1M 76.76(19) 3_655 . ?
O1M Zr1 O1M 122.8(4) 2_665 . ?
O1M Zr1 O1M 76.76(19) 4_565 . ?
O12M Zr2 O12M 60.2(4) 3_655 20_655 ?
O12M Zr2 O12M 91.8(5) 3_655 18 ?
O12M Zr2 O12M 61.9(5) 20_655 18 ?
O12M Zr2 O12M 61.9(5) 3_655 . ?
O12M Zr2 O12M 91.8(5) 20_655 . ?
O12M Zr2 O12M 60.2(4) 18 . ?
O12M Zr2 O1M 72.3(3) 3_655 . ?
O12M Zr2 O1M 107.7(4) 20_655 . ?
O12M Zr2 O1M 69.3(2) 18 . ?
O12M Zr2 O1M 15.9(3) . . ?
O12M Zr2 O1M 15.9(3) 3_655 3_655 ?
O12M Zr2 O1M 69.3(2) 20_655 3_655 ?
O12M Zr2 O1M 107.7(4) 18 3_655 ?
O12M Zr2 O1M 72.3(3) . 3_655 ?
O1M Zr2 O1M 79.5(5) . 3_655 ?
O12M Zr2 O1M 69.3(2) 3_655 20_655 ?
O12M Zr2 O1M 15.9(3) 20_655 20_655 ?
O12M Zr2 O1M 72.3(3) 18 20_655 ?
O12M Zr2 O1M 107.7(4) . 20_655 ?
O1M Zr2 O1M 123.6(4) . 20_655 ?
O1M Zr2 O1M 74.7(4) 3_655 20_655 ?
O12M Zr2 O1M 107.7(4) 3_655 18 ?
O12M Zr2 O1M 72.3(3) 20_655 18 ?
O12M Zr2 O1M 15.9(3) 18 18 ?
O12M Zr2 O1M 69.3(2) . 18 ?
O1M Zr2 O1M 74.7(4) . 18 ?
O1M Zr2 O1M 123.6(4) 3_655 18 ?
O1M Zr2 O1M 79.5(5) 20_655 18 ?
O12M Zr2 O3 87.6(3) 3_655 . ?
O12M Zr2 O3 87.6(3) 20_655 . ?
O12M Zr2 O3 144.5(2) 18 . ?
O12M Zr2 O3 144.5(2) . . ?
O1M Zr2 O3 142.5(2) . . ?
O1M Zr2 O3 74.4(3) 3_655 . ?
O1M Zr2 O3 74.4(3) 20_655 . ?
O1M Zr2 O3 142.5(2) 18 . ?
O12M Zr2 O3 144.5(2) 3_655 7 ?
O12M Zr2 O3 144.5(2) 20_655 7 ?
O12M Zr2 O3 87.6(3) 18 7 ?
O12M Zr2 O3 87.6(3) . 7 ?
O1M Zr2 O3 74.4(3) . 7 ?
O1M Zr2 O3 142.5(2) 3_655 7 ?
O1M Zr2 O3 142.5(2) 20_655 7 ?
O1M Zr2 O3 74.4(3) 18 7 ?
O3 Zr2 O3 112.6(5) . 7 ?
O12M Zr2 O1 82.9(2) 3_655 . ?
O12M Zr2 O1 140.0(2) 20_655 . ?
O12M Zr2 O1 140.0(2) 18 . ?
O12M Zr2 O1 82.9(2) . . ?
O1M Zr2 O1 71.3(2) . . ?
O1M Zr2 O1 71.3(2) 3_655 . ?
O1M Zr2 O1 139.1(3) 20_655 . ?
O1M Zr2 O1 139.1(3) 18 . ?
O3 Zr2 O1 75.18(13) . . ?
O3 Zr2 O1 75.18(13) 7 . ?
O12M Zr2 O1 140.0(2) 3_655 18 ?
O12M Zr2 O1 82.9(2) 20_655 18 ?
O12M Zr2 O1 82.9(2) 18 18 ?
O12M Zr2 O1 140.0(2) . 18 ?
O1M Zr2 O1 139.1(3) . 18 ?
O1M Zr2 O1 139.1(3) 3_655 18 ?
O1M Zr2 O1 71.3(2) 20_655 18 ?
O1M Zr2 O1 71.3(2) 18 18 ?
O3 Zr2 O1 75.18(13) . 18 ?
O3 Zr2 O1 75.18(13) 7 18 ?
O1 Zr2 O1 125.1(3) . 18 ?
O12M O1M Zr2 65.2(8) . . ?
O12M O1M Zr2 65.2(8) . 19_565 ?
Zr2 O1M Zr2 103.6(4) . 19_565 ?
O12M O1M Zr1 60.4(16) . . ?
Zr2 O1M Zr1 100.8(3) . . ?
Zr2 O1M Zr1 100.8(3) 19_565 . ?
O1M O12M Zr2 98.9(9) . . ?
O1M O12M Zr2 98.9(9) . 19_565 ?
Zr2 O12M Zr2 117.7(4) . 19_565 ?
O1M O12M Zr1 104.4(17) . . ?
Zr2 O12M Zr1 116.1(3) . . ?
Zr2 O12M Zr1 116.1(3) 19_565 . ?
C1 O1 Zr2 133.3(5) . . ?
C1 O2 Zr1 132.0(4) . . ?
C7 O3 Zr2 126.7(9) . . ?
O1 C1 O2 126.5(6) . . ?
O1 C1 C2 118.8(7) . . ?
O2 C1 C2 114.7(6) . . ?
C3 C2 C4 120.9(7) . . ?
C3 C2 C1 119.1(7) . . ?
C4 C2 C1 120.0(7) . . ?
C2 C3 C6 120.0(8) . 25 ?
C2 C4 C5 121.1(8) . . ?
C4 C5 C6 118.7(8) . . ?
C6 C6 C3 120.1(9) 25 25 ?
C6 C6 C5 119.3(8) 25 . ?
C3 C6 C5 120.7(8) 25 . ?
C8 C7 O3 115.4(8) . 5_655 ?
C8 C7 O3 115.4(8) . . ?
O3 C7 O3 129.1(15) 5_655 . ?
C9 C8 C9 118(2) 5_655 . ?
C9 C8 C7 121.2(10) 5_655 . ?
C9 C8 C7 121.2(10) . . ?
C9 C9 C8 121.2(10) 21 . ?
C9 C9 N1 113.9(12) 21 . ?
C8 C9 N1 125.0(17) . . ?
O4 N1 O4 102(3) 18 . ?
O4 N1 C9 129.1(15) 18 . ?
O4 N1 C9 129.1(15) . . ?

_refine_diff_density_max         1.222
_refine_diff_density_min         -1.972
_refine_diff_density_rms         0.144



####################################################################### 
# 
# 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_p17_024ttg_sq
_database_code_depnum_ccdc_archive 'CCDC 1896109'
loop_
_audit_author_name
_audit_author_address
'Myoung Soo Lah'
;Ulsan National Institute of Science and Technology
South Korea
;
_audit_update_record             
;
2019-02-08 deposited with the CCDC.	2019-05-07 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            'C64 H50 O43 Zr6'
_chemical_formula_weight         2054.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -3.5084 0.5477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_H-M_alt        'P 4/m n c'
_space_group_name_Hall           '-P 4 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   17.439(3)
_cell_length_b                   17.439(3)
_cell_length_c                   22.592(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6871(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    82498
_cell_measurement_theta_min      1.776
_cell_measurement_theta_max      27.999

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.993
_exptl_crystal_F_000             2036
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.062
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.058
_exptl_absorpt_coefficient_mu    0.469
_shelx_estimated_absorpt_T_min   0.972
_shelx_estimated_absorpt_T_max   0.973
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.971
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_process_details   HKL3000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60100
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.776
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4460
_reflns_number_gt                3501
_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       'PAL BL2D-SMDC Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    SHELXS
_computing_structure_refinement  SHELXL
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_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)+(0.1672P)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     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0051(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4460
_refine_ls_number_parameters     292
_refine_ls_number_restraints     266
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0710
_refine_ls_wR_factor_ref         0.2150
_refine_ls_wR_factor_gt          0.2047
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.067
_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 1.0000 0.0000 -0.10842(2) 0.0157(2) Uani 1 4 d S T P . .
Zr2 Zr 0.88410(3) 0.08445(3) 0.0000 0.0242(2) Uani 1 2 d S T P . .
O1M O 0.98433(19) 0.1001(3) -0.05226(15) 0.0728(15) Uani 1 1 d . . . . .
O1 O 1.06207(16) 0.08838(15) -0.15761(11) 0.0303(6) Uani 1 1 d . . . . .
O2 O 1.1166(2) 0.1625(2) -0.08869(12) 0.0511(10) Uani 1 1 d . . . . .
C1 C 1.1043(3) 0.1424(3) -0.14154(16) 0.0393(10) Uani 1 1 d . . . . .
C2 C 1.1961(4) 0.2409(4) -0.17568(18) 0.078(2) Uani 1 1 d . . . . .
H2 H 1.2069 0.2513 -0.1357 0.094 Uiso 1 1 calc R U . . .
C3 C 1.1424(4) 0.1876(4) -0.18917(18) 0.0662(18) Uani 1 1 d . . . . .
C4 C 1.1245(4) 0.1713(4) -0.2493(2) 0.089(3) Uani 1 1 d . . . . .
H4 H 1.0871 0.1344 -0.2585 0.107 Uiso 1 1 calc R U . . .
C5 C 1.1618(4) 0.2093(4) -0.2933(2) 0.095(3) Uani 1 1 d . . . . .
H5 H 1.1491 0.1990 -0.3329 0.114 Uiso 1 1 calc R U . . .
C6 C 1.2194(4) 0.2643(4) -0.28041(18) 0.080(2) Uani 1 1 d . . . . .
O1S O 0.8611(6) 0.2053(5) 0.0000 0.048(3) Uani 0.75 2 d S T P A 1
H1S H 0.8453 0.2184 0.0331 0.072 Uiso 0.25 1 calc DR U P A 1
O11 O 0.8710(10) 0.3051(8) 0.0907(5) 0.060(4) Uani 0.25 1 d D . P B 1
O12 O 0.9568(7) 0.2332(8) 0.1393(6) 0.054(4) Uani 0.25 1 d D . P B 1
C11 C 0.9072(8) 0.2872(7) 0.1395(5) 0.080(9) Uani 0.25 1 d D . P B 1
C12 C 0.8776(8) 0.3187(8) 0.1952(5) 0.041(4) Uani 0.25 1 d D . P B 1
C13 C 0.9029(6) 0.2922(7) 0.2494(6) 0.050(4) Uani 0.25 1 d D . P B 1
O13 O 0.9604(7) 0.2364(8) 0.2534(6) 0.062(4) Uani 0.25 1 d D . P B 1
C14 C 0.8755(10) 0.3220(11) 0.3022(6) 0.053(5) Uani 0.25 1 d D . P B 1
H14 H 0.8964 0.3037 0.3378 0.064 Uiso 0.25 1 calc R U P B 1
O21 O 0.8806(11) 0.2137(9) 0.0000 0.015(4) Uani 0.25 2 d DS TU P A 2
O22 O 0.9324(9) 0.2592(10) 0.0893(7) 0.039(5) Uani 0.125 1 d D U P A 2
O23 O 0.642(3) 0.526(3) 0.1172(15) 0.19(3) Uani 0.125 1 d D U P A 2
O24 O 0.5883(17) 0.4859(19) 0.0265(16) 0.121(15) Uani 0.125 1 d D U P A 2
O25 O 0.8785(12) 0.3653(15) 0.1411(10) 0.17(2) Uani 0.125 1 d D U P A 2
O26 O 0.6418(14) 0.3763(18) -0.0278(12) 0.175(19) Uani 0.125 1 d D U P A 2
C21 C 0.8178(6) 0.3173(6) 0.0511(5) 0.028(5) Uani 0.125 1 d D U P A 2
C22 C 0.8188(8) 0.3683(8) 0.0987(6) 0.056(9) Uani 0.125 1 d D U P A 2
C23 C 0.7603(9) 0.4218(9) 0.1037(7) 0.059(9) Uani 0.125 1 d D U P A 2
H23 H 0.7601 0.4565 0.1355 0.071 Uiso 0.125 1 calc R U P A 2
C24 C 0.7024(9) 0.4246(8) 0.0623(8) 0.073(10) Uani 0.125 1 d D U P A 2
C25 C 0.7013(9) 0.3738(10) 0.0149(8) 0.117(14) Uani 0.125 1 d D U P A 2
C26 C 0.7600(9) 0.3199(10) 0.0098(7) 0.081(11) Uani 0.125 1 d D U P A 2
C27 C 0.8788(7) 0.2616(6) 0.0464(4) 0.013(4) Uani 0.125 1 d D U P A 2
C28 C 0.6418(10) 0.4807(11) 0.0688(10) 0.098(13) Uani 0.125 1 d D U P A 2
O2S O 0.7571(2) 0.0621(3) 0.0000 0.0553(13) Uani 1 2 d S T P A .


_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 O1M 2.175(3) . ?
Zr1 O1M 2.175(3) 4_665 ?
Zr1 O1M 2.175(3) 3_645 ?
Zr1 O1M 2.175(3) 2_755 ?
Zr1 O1 2.187(3) . ?
Zr1 O1 2.187(3) 2_755 ?
Zr1 O1 2.187(3) 3_645 ?
Zr1 O1 2.187(3) 4_665 ?
Zr1 Zr2 3.5006(7) 11_665 ?
Zr1 Zr2 3.5006(7) 9_755 ?
Zr1 Zr2 3.5006(7) 3_645 ?
Zr2 O1M 2.126(3) 3_645 ?
Zr2 O1M 2.126(3) 12_645 ?
Zr2 O1M 2.127(3) . ?
Zr2 O1M 2.127(3) 10 ?
Zr2 O1S 2.145(9) . ?
Zr2 O2 2.234(3) 3_645 ?
Zr2 O2 2.234(3) 12_645 ?
Zr2 O2S 2.249(4) . ?
Zr2 O21 2.256(16) . ?
Zr2 Zr1 3.5006(7) 9_755 ?
Zr2 Zr2 3.5367(8) 11_665 ?
Zr2 Zr2 3.5368(8) 3_645 ?
O1M Zr2 2.126(3) 11_665 ?
O1 C1 1.249(5) . ?
O2 C1 1.263(5) . ?
O2 Zr2 2.234(3) 11_665 ?
C1 C3 1.490(6) . ?
C2 C3 1.354(7) . ?
C2 C6 1.393(6) 8_664 ?
C3 C4 1.421(7) . ?
C4 C5 1.360(6) . ?
C5 C6 1.419(7) . ?
C6 C2 1.393(6) 8_664 ?
C6 C6 1.432(9) 8_664 ?
O11 C11 1.308(14) . ?
O12 C11 1.278(14) . ?
C11 C12 1.467(9) . ?
C12 C13 1.381(9) . ?
C12 C14 1.389(9) 7_545 ?
C13 C14 1.385(9) . ?
C13 O13 1.400(9) . ?
C14 C12 1.389(9) 7_545 ?
O21 C27 1.340(8) 10 ?
O21 C27 1.340(8) . ?
O22 C27 1.348(8) . ?
O23 C28 1.345(9) . ?
O24 O24 1.20(7) 10 ?
O24 C28 1.338(9) . ?
O25 C22 1.415(8) . ?
O26 C25 1.078(11) 10 ?
O26 O26 1.26(5) 10 ?
O26 C25 1.417(8) . ?
O26 C24 1.56(4) 10 ?
C21 C26 1.373(8) . ?
C21 C22 1.396(8) . ?
C21 C27 1.444(7) . ?
C21 C26 1.71(2) 10 ?
C22 C23 1.388(8) . ?
C23 C24 1.377(8) . ?
C24 C25 1.390(8) . ?
C24 C28 1.447(7) . ?
C24 O26 1.56(4) 10 ?
C24 C25 1.96(3) 10 ?
C25 C25 0.67(4) 10 ?
C25 O26 1.078(11) 10 ?
C25 C26 1.395(8) . ?
C25 C26 1.498(13) 10 ?
C25 C24 1.96(3) 10 ?
C26 C26 0.44(3) 10 ?
C26 C25 1.498(13) 10 ?
C26 C21 1.71(2) 10 ?

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
O1M Zr1 O1M 70.11(12) . 4_665 ?
O1M Zr1 O1M 70.11(12) . 3_645 ?
O1M Zr1 O1M 108.6(2) 4_665 3_645 ?
O1M Zr1 O1M 108.6(2) . 2_755 ?
O1M Zr1 O1M 70.11(12) 4_665 2_755 ?
O1M Zr1 O1M 70.11(12) 3_645 2_755 ?
O1M Zr1 O1 78.05(14) . . ?
O1M Zr1 O1 79.08(13) 4_665 . ?
O1M Zr1 O1 141.46(12) 3_645 . ?
O1M Zr1 O1 143.11(11) 2_755 . ?
O1M Zr1 O1 143.11(11) . 2_755 ?
O1M Zr1 O1 141.46(12) 4_665 2_755 ?
O1M Zr1 O1 79.08(13) 3_645 2_755 ?
O1M Zr1 O1 78.05(14) 2_755 2_755 ?
O1 Zr1 O1 118.92(14) . 2_755 ?
O1M Zr1 O1 79.08(13) . 3_645 ?
O1M Zr1 O1 143.11(11) 4_665 3_645 ?
O1M Zr1 O1 78.05(14) 3_645 3_645 ?
O1M Zr1 O1 141.46(12) 2_755 3_645 ?
O1 Zr1 O1 75.04(6) . 3_645 ?
O1 Zr1 O1 75.04(6) 2_755 3_645 ?
O1M Zr1 O1 141.46(12) . 4_665 ?
O1M Zr1 O1 78.05(14) 4_665 4_665 ?
O1M Zr1 O1 143.11(11) 3_645 4_665 ?
O1M Zr1 O1 79.08(13) 2_755 4_665 ?
O1 Zr1 O1 75.04(6) . 4_665 ?
O1 Zr1 O1 75.04(6) 2_755 4_665 ?
O1 Zr1 O1 118.92(14) 3_645 4_665 ?
O1M Zr1 Zr2 35.05(10) . 11_665 ?
O1M Zr1 Zr2 35.09(9) 4_665 11_665 ?
O1M Zr1 Zr2 90.12(12) 3_645 11_665 ?
O1M Zr1 Zr2 90.14(11) 2_755 11_665 ?
O1 Zr1 Zr2 74.95(7) . 11_665 ?
O1 Zr1 Zr2 166.11(7) 2_755 11_665 ?
O1 Zr1 Zr2 111.49(7) 3_645 11_665 ?
O1 Zr1 Zr2 110.17(7) 4_665 11_665 ?
O1M Zr1 Zr2 90.12(12) . 9_755 ?
O1M Zr1 Zr2 35.05(10) 4_665 9_755 ?
O1M Zr1 Zr2 90.14(11) 3_645 9_755 ?
O1M Zr1 Zr2 35.09(9) 2_755 9_755 ?
O1 Zr1 Zr2 111.49(7) . 9_755 ?
O1 Zr1 Zr2 110.17(7) 2_755 9_755 ?
O1 Zr1 Zr2 166.11(7) 3_645 9_755 ?
O1 Zr1 Zr2 74.95(7) 4_665 9_755 ?
Zr2 Zr1 Zr2 60.685(13) 11_665 9_755 ?
O1M Zr1 Zr2 90.14(11) . 3_645 ?
O1M Zr1 Zr2 90.12(12) 4_665 3_645 ?
O1M Zr1 Zr2 35.09(9) 3_645 3_645 ?
O1M Zr1 Zr2 35.05(10) 2_755 3_645 ?
O1 Zr1 Zr2 166.11(7) . 3_645 ?
O1 Zr1 Zr2 74.95(7) 2_755 3_645 ?
O1 Zr1 Zr2 110.17(7) 3_645 3_645 ?
O1 Zr1 Zr2 111.49(7) 4_665 3_645 ?
Zr2 Zr1 Zr2 91.19(2) 11_665 3_645 ?
Zr2 Zr1 Zr2 60.685(13) 9_755 3_645 ?
O1M Zr2 O1M 67.48(18) 3_645 12_645 ?
O1M Zr2 O1M 72.0(2) 3_645 . ?
O1M Zr2 O1M 107.9(3) 12_645 . ?
O1M Zr2 O1M 107.9(3) 3_645 10 ?
O1M Zr2 O1M 72.0(2) 12_645 10 ?
O1M Zr2 O1M 67.44(18) . 10 ?
O1M Zr2 O1S 146.22(9) 3_645 . ?
O1M Zr2 O1S 146.22(9) 12_645 . ?
O1M Zr2 O1S 91.6(3) . . ?
O1M Zr2 O1S 91.6(3) 10 . ?
O1M Zr2 O2 75.82(14) 3_645 3_645 ?
O1M Zr2 O2 138.72(13) 12_645 3_645 ?
O1M Zr2 O2 76.65(14) . 3_645 ?
O1M Zr2 O2 139.90(13) 10 3_645 ?
O1S Zr2 O2 71.67(13) . 3_645 ?
O1M Zr2 O2 138.72(13) 3_645 12_645 ?
O1M Zr2 O2 75.82(14) 12_645 12_645 ?
O1M Zr2 O2 139.90(13) . 12_645 ?
O1M Zr2 O2 76.65(14) 10 12_645 ?
O1S Zr2 O2 71.67(13) . 12_645 ?
O2 Zr2 O2 127.51(16) 3_645 12_645 ?
O1M Zr2 O2S 89.14(17) 3_645 . ?
O1M Zr2 O2S 89.14(17) 12_645 . ?
O1M Zr2 O2S 146.27(9) . . ?
O1M Zr2 O2S 146.27(9) 10 . ?
O1S Zr2 O2S 89.2(3) . . ?
O2 Zr2 O2S 71.64(11) 3_645 . ?
O2 Zr2 O2S 71.64(11) 12_645 . ?
O1M Zr2 O21 145.55(12) 3_645 . ?
O1M Zr2 O21 145.55(12) 12_645 . ?
O1M Zr2 O21 83.9(4) . . ?
O1M Zr2 O21 83.9(4) 10 . ?
O2 Zr2 O21 74.9(2) 3_645 . ?
O2 Zr2 O21 74.9(2) 12_645 . ?
O2S Zr2 O21 98.4(5) . . ?
O1M Zr2 Zr1 88.18(12) 3_645 9_755 ?
O1M Zr2 Zr1 36.00(10) 12_645 9_755 ?
O1M Zr2 Zr1 88.16(12) . 9_755 ?
O1M Zr2 Zr1 36.01(10) 10 9_755 ?
O1S Zr2 Zr1 121.41(16) . 9_755 ?
O2 Zr2 Zr1 160.63(8) 3_645 9_755 ?
O2 Zr2 Zr1 71.83(8) 12_645 9_755 ?
O2S Zr2 Zr1 119.71(9) . 9_755 ?
O21 Zr2 Zr1 115.9(3) . 9_755 ?
O1M Zr2 Zr2 89.97(13) 3_645 11_665 ?
O1M Zr2 Zr2 89.97(13) 12_645 11_665 ?
O1M Zr2 Zr2 33.72(9) . 11_665 ?
O1M Zr2 Zr2 33.72(9) 10 11_665 ?
O1S Zr2 Zr2 91.8(3) . 11_665 ?
O2 Zr2 Zr2 108.71(10) 3_645 11_665 ?
O2 Zr2 Zr2 108.71(10) 12_645 11_665 ?
O2S Zr2 Zr2 178.92(15) . 11_665 ?
O21 Zr2 Zr2 82.6(5) . 11_665 ?
Zr1 Zr2 Zr2 59.658(6) 9_755 11_665 ?
O1M Zr2 Zr2 33.74(9) 3_645 3_645 ?
O1M Zr2 Zr2 33.74(9) 12_645 3_645 ?
O1M Zr2 Zr2 89.96(13) . 3_645 ?
O1M Zr2 Zr2 89.97(13) 10 3_645 ?
O1S Zr2 Zr2 178.2(3) . 3_645 ?
O2 Zr2 Zr2 107.72(9) 3_645 3_645 ?
O2 Zr2 Zr2 107.72(9) 12_645 3_645 ?
O2S Zr2 Zr2 88.92(15) . 3_645 ?
O21 Zr2 Zr2 172.6(5) . 3_645 ?
Zr1 Zr2 Zr2 59.657(6) 9_755 3_645 ?
Zr2 Zr2 Zr2 90.0 11_665 3_645 ?
Zr2 O1M Zr2 112.54(15) 11_665 . ?
Zr2 O1M Zr1 108.95(18) 11_665 . ?
Zr2 O1M Zr1 108.90(17) . . ?
C1 O1 Zr1 132.5(2) . . ?
C1 O2 Zr2 134.8(3) . 11_665 ?
O1 C1 O2 125.8(4) . . ?
O1 C1 C3 116.8(3) . . ?
O2 C1 C3 117.4(4) . . ?
C3 C2 C6 121.6(4) . 8_664 ?
C2 C3 C4 120.2(4) . . ?
C2 C3 C1 120.6(4) . . ?
C4 C3 C1 119.1(4) . . ?
C5 C4 C3 119.8(4) . . ?
C4 C5 C6 121.2(4) . . ?
C2 C6 C5 122.8(4) 8_664 . ?
C2 C6 C6 119.1(5) 8_664 8_664 ?
C5 C6 C6 118.1(5) . 8_664 ?
O12 C11 O11 120.0(12) . . ?
O12 C11 C12 121.1(12) . . ?
O11 C11 C12 117.6(12) . . ?
C13 C12 C14 115.0(10) . 7_545 ?
C13 C12 C11 121.6(12) . . ?
C14 C12 C11 123.4(13) 7_545 . ?
C12 C13 C14 121.9(10) . . ?
C12 C13 O13 121.2(12) . . ?
C14 C13 O13 116.8(13) . . ?
C13 C14 C12 123.0(12) . 7_545 ?
C27 O21 C27 103.0(12) 10 . ?
C27 O21 Zr2 128.5(6) 10 . ?
C27 O21 Zr2 128.5(6) . . ?
O24 O24 C28 135.5(17) 10 . ?
C25 O26 O26 74(2) 10 10 ?
C25 O26 C25 27.2(19) 10 . ?
O26 O26 C25 47.1(7) 10 . ?
C25 O26 C24 60.4(15) 10 10 ?
O26 O26 C24 120.0(12) 10 10 ?
C25 O26 C24 82.0(10) . 10 ?
C26 C21 C22 120.7(6) . . ?
C26 C21 C27 120.9(7) . . ?
C22 C21 C27 118.4(6) . . ?
C26 C21 C26 11.0(7) . 10 ?
C22 C21 C26 127.7(6) . 10 ?
C27 C21 C26 113.2(8) . 10 ?
C23 C22 C21 118.8(6) . . ?
C23 C22 O25 120.8(8) . . ?
C21 C22 O25 120.4(8) . . ?
C24 C23 C22 120.6(7) . . ?
C23 C24 C25 120.7(6) . . ?
C23 C24 C28 119.3(7) . . ?
C25 C24 C28 119.9(7) . . ?
C23 C24 O26 144.8(11) . 10 ?
C25 C24 O26 42.4(10) . 10 ?
C28 C24 O26 85.5(8) . 10 ?
C23 C24 C25 126.6(5) . 10 ?
C25 C24 C25 12.7(6) . 10 ?
C28 C24 C25 112.9(7) . 10 ?
O26 C24 C25 45.8(9) 10 10 ?
C25 C25 O26 106(2) 10 10 ?
C25 C25 C24 140.4(6) 10 . ?
O26 C25 C24 77(2) 10 . ?
C25 C25 C26 85.3(5) 10 . ?
O26 C25 C26 139.1(10) 10 . ?
C24 C25 C26 118.8(6) . . ?
C25 C25 O26 47.1(7) 10 . ?
O26 C25 O26 59(3) 10 . ?
C24 C25 O26 121.0(8) . . ?
C26 C25 O26 120.2(8) . . ?
C25 C25 C26 68.1(12) 10 10 ?
O26 C25 C26 141.6(12) 10 10 ?
C24 C25 C26 132.6(9) . 10 ?
C26 C25 C26 17.2(12) . 10 ?
O26 C25 C26 105.4(11) . 10 ?
C25 C25 C24 26.9(5) 10 10 ?
O26 C25 C24 103.5(18) 10 10 ?
C24 C25 C24 113.5(10) . 10 ?
C26 C25 C24 103.0(7) . 10 ?
O26 C25 C24 52.2(10) . 10 ?
C26 C25 C24 86.9(14) 10 10 ?
C26 C26 C21 132.7(6) 10 . ?
C26 C26 C25 94.7(5) 10 . ?
C21 C26 C25 120.4(7) . . ?
C26 C26 C25 68.1(12) 10 10 ?
C21 C26 C25 140.9(10) . 10 ?
C25 C26 C25 26.6(13) . 10 ?
C26 C26 C21 36.2(5) 10 10 ?
C21 C26 C21 96.5(8) . 10 ?
C25 C26 C21 121.2(7) . 10 ?
C25 C26 C21 96.9(14) 10 10 ?
O21 C27 O22 121.8(8) . . ?
O21 C27 C21 119.5(8) . . ?
O22 C27 C21 118.6(7) . . ?
O24 C28 O23 122.6(9) . . ?
O24 C28 C24 118.8(8) . . ?
O23 C28 C24 118.6(8) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1S H1S O11 0.83 2.04 2.695(12) 134.8 .

_refine_diff_density_max         5.562
_refine_diff_density_min         -1.486
_refine_diff_density_rms         0.163



####################################################################### 
# 
# 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_P17_025ttg_sq
_database_code_depnum_ccdc_archive 'CCDC 1896112'
loop_
_audit_author_name
_audit_author_address
'Myoung Soo Lah'
;Ulsan National Institute of Science and Technology
South Korea
;
_audit_update_record             
;
2019-02-08 deposited with the CCDC.	2019-05-07 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            'C64 H38 N2 O32 Zr6'
_chemical_formula_weight         1894.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 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 0.0059 0.0032 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0105 0.0059 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -3.5084 0.5477 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           139
_space_group_name_H-M_alt        'I 4/m m m'
_space_group_name_Hall           '-I 4 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'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'-y+1/2, -x+1/2, z+1/2'
'y+1/2, x+1/2, z+1/2'

_cell_length_a                   14.872(2)
_cell_length_b                   14.872(2)
_cell_length_c                   26.123(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5778(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    65222
_cell_measurement_theta_min      1.907
_cell_measurement_theta_max      33.459

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_F_000             1864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.044
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.038
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_process_details   HKL3000
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.700
_diffrn_radiation_type           synchrotron
_diffrn_source                   'PLSII 2D bending magnet'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34633
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.907
_diffrn_reflns_theta_max         33.459
_diffrn_reflns_theta_full        24.835
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.868
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2908
_reflns_number_gt                2344
_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       'PAL BL2D-SMDC Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    SHELXS
_computing_structure_refinement  SHELXL
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_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)+(0.1347P)²+10.0057P] 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       0.0082(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2908
_refine_ls_number_parameters     89
_refine_ls_number_restraints     97
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0644
_refine_ls_wR_factor_ref         0.2032
_refine_ls_wR_factor_gt          0.1924
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.170
_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 0.38137(2) 0.38137(2) 0.0000 0.0262(2) Uani 1 4 d S T P . .
Zr2 Zr 0.5000 0.5000 0.09402(2) 0.0192(2) Uani 1 8 d S T P . .
O1M O 0.5000 0.3828(4) 0.04528(14) 0.0765(19) Uani 1 2 d S TU P . .
O1 O 0.33292(17) 0.33292(17) 0.07722(11) 0.0594(12) Uani 1 2 d S T P . .
O2 O 0.41067(14) 0.41067(14) 0.13637(10) 0.0360(6) Uani 1 2 d S T P . .
C1 C 0.3537(2) 0.3537(2) 0.12290(14) 0.0464(12) Uani 1 2 d S T P . .
C2 C 0.2412(3) 0.2412(3) 0.15392(17) 0.117(4) Uani 1 2 d S T P . .
H2 H 0.2275 0.2275 0.1197 0.141 Uiso 1 2 calc R U P . .
C3 C 0.3057(2) 0.3057(2) 0.16480(17) 0.0644(19) Uani 1 2 d S T P . .
C4 C 0.3267(3) 0.3267(3) 0.21434(18) 0.080(3) Uani 1 2 d S T P . .
H4 H 0.3706 0.3706 0.2213 0.096 Uiso 1 2 calc R U P . .
C5 C 0.2826(3) 0.2826(3) 0.25518(18) 0.081(2) Uani 1 2 d S T P . .
C6 C 0.3030(3) 0.3030(3) 0.3068(2) 0.132(5) Uani 1 2 d S T P . .
H6 H 0.3467 0.3467 0.3145 0.158 Uiso 1 2 calc R U P . .
O3 O 0.4058(4) 0.2335(3) 0.0000 0.094(2) Uani 1 2 d DS TU P . .
C7 C 0.5000 0.1956(6) 0.0000 0.312(17) Uani 1 4 d DS TU P A .
C8 C 0.5000 0.0961(7) 0.0000 0.248(14) Uani 1 4 d DS TU P . .
C9A C 0.4215(7) 0.0479(3) 0.0000 0.347(14) Uani 0.25 2 d DS TU P A 3
N1A N 0.3362(6) 0.086(2) 0.0000 0.30(4) Uani 0.25 2 d DS TU P A 3
H1A1 H 0.3300 0.1438 0.0000 0.356 Uiso 0.25 2 calc R U P A 3
H1A2 H 0.2890 0.0511 0.0000 0.356 Uiso 0.25 2 calc R U P A 3
C9B C 0.4215(7) 0.0479(3) 0.0000 0.347(14) Uani 0.75 2 d DS TU P A 4
H9B H 0.3663 0.0788 0.0000 0.416 Uiso 0.75 2 calc R U P A 4


_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 O1M 2.124(2) 4_565 ?
Zr1 O1M 2.124(2) 19_565 ?
Zr1 O1M 2.124(2) 18 ?
Zr1 O1M 2.124(2) . ?
Zr1 O3 2.229(4) . ?
Zr1 O3 2.229(4) 7 ?
Zr1 O1 2.260(3) 18 ?
Zr1 O1 2.260(3) . ?
Zr1 Zr2 3.5011(7) . ?
Zr1 Zr2 3.5011(7) 17_665 ?
Zr1 Zr1 3.5286(8) 19_565 ?
Zr1 Zr1 3.5286(8) 3_655 ?
Zr2 O1M 2.159(4) . ?
Zr2 O1M 2.159(4) 4_565 ?
Zr2 O1M 2.159(4) 3_655 ?
Zr2 O1M 2.159(4) 2_665 ?
Zr2 O2 2.180(3) 2_665 ?
Zr2 O2 2.180(3) 4_565 ?
Zr2 O2 2.180(3) 3_655 ?
Zr2 O2 2.180(3) . ?
Zr2 Zr1 3.5011(7) 19_565 ?
Zr2 Zr1 3.5011(7) 3_655 ?
Zr2 Zr1 3.5011(7) 17_665 ?
O1M Zr1 2.124(2) 3_655 ?
O1 C1 1.271(5) . ?
O2 C1 1.250(6) . ?
C1 C3 1.489(6) . ?
C2 C3 1.385(8) . ?
C2 C6 1.385(7) 25 ?
C3 C4 1.367(7) . ?
C4 C5 1.414(6) . ?
C5 C5 1.397(11) 25 ?
C5 C6 1.416(7) . ?
C6 C2 1.385(7) 25 ?
O3 C7 1.509(6) . ?
C7 C8 1.480(8) . ?
C7 O3 1.509(6) 5_655 ?
C8 C9B 1.371(6) . ?
C8 C9A 1.371(6) . ?
C8 C9B 1.371(6) 5_655 ?
C8 C9A 1.371(6) 5_655 ?
C9A N1A 1.386(10) . ?
C9A C9A 1.425(10) 21 ?
C9B C9B 1.425(10) 21 ?

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
O1M Zr1 O1M 67.68(17) 4_565 19_565 ?
O1M Zr1 O1M 107.1(3) 4_565 18 ?
O1M Zr1 O1M 71.0(2) 19_565 18 ?
O1M Zr1 O1M 71.0(2) 4_565 . ?
O1M Zr1 O1M 107.1(3) 19_565 . ?
O1M Zr1 O1M 67.68(17) 18 . ?
O1M Zr1 O3 144.87(8) 4_565 . ?
O1M Zr1 O3 144.87(8) 19_565 . ?
O1M Zr1 O3 82.8(2) 18 . ?
O1M Zr1 O3 82.8(2) . . ?
O1M Zr1 O3 82.8(2) 4_565 7 ?
O1M Zr1 O3 82.8(2) 19_565 7 ?
O1M Zr1 O3 144.87(8) 18 7 ?
O1M Zr1 O3 144.87(8) . 7 ?
O3 Zr1 O3 108.8(3) . 7 ?
O1M Zr1 O1 139.90(8) 4_565 18 ?
O1M Zr1 O1 76.76(13) 19_565 18 ?
O1M Zr1 O1 76.76(13) 18 18 ?
O1M Zr1 O1 139.90(8) . 18 ?
O3 Zr1 O1 74.78(8) . 18 ?
O3 Zr1 O1 74.78(8) 7 18 ?
O1M Zr1 O1 76.76(13) 4_565 . ?
O1M Zr1 O1 139.90(8) 19_565 . ?
O1M Zr1 O1 139.90(8) 18 . ?
O1M Zr1 O1 76.76(13) . . ?
O3 Zr1 O1 74.78(8) . . ?
O3 Zr1 O1 74.78(8) 7 . ?
O1 Zr1 O1 126.39(18) 18 . ?
O1M Zr1 Zr2 35.51(11) 4_565 . ?
O1M Zr1 Zr2 88.12(13) 19_565 . ?
O1M Zr1 Zr2 88.12(13) 18 . ?
O1M Zr1 Zr2 35.51(11) . . ?
O3 Zr1 Zr2 114.52(10) . . ?
O3 Zr1 Zr2 114.52(10) 7 . ?
O1 Zr1 Zr2 161.35(9) 18 . ?
O1 Zr1 Zr2 72.26(9) . . ?
O1M Zr1 Zr2 88.12(13) 4_565 17_665 ?
O1M Zr1 Zr2 35.51(11) 19_565 17_665 ?
O1M Zr1 Zr2 35.51(11) 18 17_665 ?
O1M Zr1 Zr2 88.12(13) . 17_665 ?
O3 Zr1 Zr2 114.52(10) . 17_665 ?
O3 Zr1 Zr2 114.52(10) 7 17_665 ?
O1 Zr1 Zr2 72.26(9) 18 17_665 ?
O1 Zr1 Zr2 161.35(9) . 17_665 ?
Zr2 Zr1 Zr2 89.10(2) . 17_665 ?
O1M Zr1 Zr1 33.84(8) 4_565 19_565 ?
O1M Zr1 Zr1 33.84(8) 19_565 19_565 ?
O1M Zr1 Zr1 89.45(15) 18 19_565 ?
O1M Zr1 Zr1 89.45(15) . 19_565 ?
O3 Zr1 Zr1 170.61(16) . 19_565 ?
O3 Zr1 Zr1 80.61(16) 7 19_565 ?
O1 Zr1 Zr1 108.60(6) 18 19_565 ?
O1 Zr1 Zr1 108.59(6) . 19_565 ?
Zr2 Zr1 Zr1 59.740(6) . 19_565 ?
Zr2 Zr1 Zr1 59.740(6) 17_665 19_565 ?
O1M Zr1 Zr1 89.45(15) 4_565 3_655 ?
O1M Zr1 Zr1 89.45(15) 19_565 3_655 ?
O1M Zr1 Zr1 33.84(8) 18 3_655 ?
O1M Zr1 Zr1 33.85(8) . 3_655 ?
O3 Zr1 Zr1 80.61(16) . 3_655 ?
O3 Zr1 Zr1 170.61(16) 7 3_655 ?
O1 Zr1 Zr1 108.60(6) 18 3_655 ?
O1 Zr1 Zr1 108.59(6) . 3_655 ?
Zr2 Zr1 Zr1 59.740(6) . 3_655 ?
Zr2 Zr1 Zr1 59.740(6) 17_665 3_655 ?
Zr1 Zr1 Zr1 90.0 19_565 3_655 ?
O1M Zr2 O1M 69.65(15) . 4_565 ?
O1M Zr2 O1M 69.65(15) . 3_655 ?
O1M Zr2 O1M 107.7(3) 4_565 3_655 ?
O1M Zr2 O1M 107.7(3) . 2_665 ?
O1M Zr2 O1M 69.65(15) 4_565 2_665 ?
O1M Zr2 O1M 69.65(15) 3_655 2_665 ?
O1M Zr2 O2 142.31(3) . 2_665 ?
O1M Zr2 O2 142.31(3) 4_565 2_665 ?
O1M Zr2 O2 78.88(13) 3_655 2_665 ?
O1M Zr2 O2 78.88(13) 2_665 2_665 ?
O1M Zr2 O2 142.31(3) . 4_565 ?
O1M Zr2 O2 78.88(13) 4_565 4_565 ?
O1M Zr2 O2 142.31(3) 3_655 4_565 ?
O1M Zr2 O2 78.88(13) 2_665 4_565 ?
O2 Zr2 O2 75.08(7) 2_665 4_565 ?
O1M Zr2 O2 78.88(13) . 3_655 ?
O1M Zr2 O2 142.31(3) 4_565 3_655 ?
O1M Zr2 O2 78.88(13) 3_655 3_655 ?
O1M Zr2 O2 142.31(3) 2_665 3_655 ?
O2 Zr2 O2 75.08(7) 2_665 3_655 ?
O2 Zr2 O2 119.02(15) 4_565 3_655 ?
O1M Zr2 O2 78.88(13) . . ?
O1M Zr2 O2 78.88(13) 4_565 . ?
O1M Zr2 O2 142.31(3) 3_655 . ?
O1M Zr2 O2 142.31(3) 2_665 . ?
O2 Zr2 O2 119.02(15) 2_665 . ?
O2 Zr2 O2 75.08(7) 4_565 . ?
O2 Zr2 O2 75.08(7) 3_655 . ?
O1M Zr2 Zr1 34.85(7) . . ?
O1M Zr2 Zr1 34.85(7) 4_565 . ?
O1M Zr2 Zr1 89.62(13) 3_655 . ?
O1M Zr2 Zr1 89.62(13) 2_665 . ?
O2 Zr2 Zr1 165.94(8) 2_665 . ?
O2 Zr2 Zr1 110.85(5) 4_565 . ?
O2 Zr2 Zr1 110.85(5) 3_655 . ?
O2 Zr2 Zr1 75.04(8) . . ?
O1M Zr2 Zr1 89.62(13) . 19_565 ?
O1M Zr2 Zr1 34.85(7) 4_565 19_565 ?
O1M Zr2 Zr1 89.62(13) 3_655 19_565 ?
O1M Zr2 Zr1 34.85(7) 2_665 19_565 ?
O2 Zr2 Zr1 110.85(5) 2_665 19_565 ?
O2 Zr2 Zr1 75.04(8) 4_565 19_565 ?
O2 Zr2 Zr1 165.94(8) 3_655 19_565 ?
O2 Zr2 Zr1 110.85(5) . 19_565 ?
Zr1 Zr2 Zr1 60.521(12) . 19_565 ?
O1M Zr2 Zr1 34.85(7) . 3_655 ?
O1M Zr2 Zr1 89.62(13) 4_565 3_655 ?
O1M Zr2 Zr1 34.85(7) 3_655 3_655 ?
O1M Zr2 Zr1 89.62(13) 2_665 3_655 ?
O2 Zr2 Zr1 110.85(5) 2_665 3_655 ?
O2 Zr2 Zr1 165.94(8) 4_565 3_655 ?
O2 Zr2 Zr1 75.04(8) 3_655 3_655 ?
O2 Zr2 Zr1 110.85(5) . 3_655 ?
Zr1 Zr2 Zr1 60.521(12) . 3_655 ?
Zr1 Zr2 Zr1 90.91(2) 19_565 3_655 ?
O1M Zr2 Zr1 89.62(13) . 17_665 ?
O1M Zr2 Zr1 89.62(13) 4_565 17_665 ?
O1M Zr2 Zr1 34.85(7) 3_655 17_665 ?
O1M Zr2 Zr1 34.85(7) 2_665 17_665 ?
O2 Zr2 Zr1 75.04(8) 2_665 17_665 ?
O2 Zr2 Zr1 110.85(5) 4_565 17_665 ?
O2 Zr2 Zr1 110.85(5) 3_655 17_665 ?
O2 Zr2 Zr1 165.94(8) . 17_665 ?
Zr1 Zr2 Zr1 90.90(2) . 17_665 ?
Zr1 Zr2 Zr1 60.521(12) 19_565 17_665 ?
Zr1 Zr2 Zr1 60.521(12) 3_655 17_665 ?
Zr1 O1M Zr1 112.31(16) . 3_655 ?
Zr1 O1M Zr2 109.64(16) . . ?
Zr1 O1M Zr2 109.64(16) 3_655 . ?
C1 O1 Zr1 133.1(3) . . ?
C1 O2 Zr2 133.2(2) . . ?
O2 C1 O1 126.4(4) . . ?
O2 C1 C3 116.3(4) . . ?
O1 C1 C3 117.3(4) . . ?
C3 C2 C6 120.4(5) . 25 ?
C4 C3 C2 120.7(4) . . ?
C4 C3 C1 118.5(5) . . ?
C2 C3 C1 120.8(4) . . ?
C3 C4 C5 120.1(5) . . ?
C5 C5 C4 119.8(6) 25 . ?
C5 C5 C6 118.9(5) 25 . ?
C4 C5 C6 121.3(5) . . ?
C2 C6 C5 120.1(5) 25 . ?
C7 O3 Zr1 121.3(5) . . ?
C8 C7 O3 111.9(4) . 5_655 ?
C8 C7 O3 111.9(4) . . ?
O3 C7 O3 136.2(7) 5_655 . ?
C9B C8 C9B 116.9(11) . 5_655 ?
C9A C8 C9A 116.9(11) . 5_655 ?
C9B C8 C7 121.6(6) . . ?
C9A C8 C7 121.6(6) . . ?
C9B C8 C7 121.6(6) 5_655 . ?
C9A C8 C7 121.6(6) 5_655 . ?
C8 C9A N1A 124.6(12) . . ?
C8 C9A C9A 121.6(6) . 21 ?
N1A C9A C9A 113.9(14) . 21 ?
C8 C9B C9B 121.6(6) . 21 ?

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
Zr2 O2 C1 O1 0.000(1) . . . . ?
Zr2 O2 C1 C3 180.000(0) . . . . ?
Zr1 O1 C1 O2 0.000(0) . . . . ?
Zr1 O1 C1 C3 180.000(0) . . . . ?
C6 C2 C3 C4 0.000(0) 25 . . . ?
C6 C2 C3 C1 180.000(0) 25 . . . ?
O2 C1 C3 C4 0.000(0) . . . . ?
O1 C1 C3 C4 180.000(0) . . . . ?
O2 C1 C3 C2 180.000(0) . . . . ?
O1 C1 C3 C2 0.000(1) . . . . ?
C2 C3 C4 C5 0.000(1) . . . . ?
C1 C3 C4 C5 180.000(0) . . . . ?
C3 C4 C5 C5 0.000(0) . . . 25 ?
C3 C4 C5 C6 180.000(0) . . . . ?
C5 C5 C6 C2 0.000(1) 25 . . 25 ?
C4 C5 C6 C2 180.000(0) . . . 25 ?
Zr1 O3 C7 C8 180.0 . . . . ?
Zr1 O3 C7 O3 0.0 . . . 5_655 ?
O3 C7 C8 C9B 180.0 5_655 . . . ?
O3 C7 C8 C9B 0.0 . . . . ?
O3 C7 C8 C9A 180.0 5_655 . . . ?
O3 C7 C8 C9A 0.0 . . . . ?
O3 C7 C8 C9B 0.0 5_655 . . 5_655 ?
O3 C7 C8 C9B 180.0 . . . 5_655 ?
O3 C7 C8 C9A 0.0 5_655 . . 5_655 ?
O3 C7 C8 C9A 180.0 . . . 5_655 ?
C9A C8 C9A N1A 180.0 5_655 . . . ?
C7 C8 C9A N1A 0.0 . . . . ?
C9A C8 C9A C9A 0.0 5_655 . . 21 ?
C7 C8 C9A C9A 180.0 . . . 21 ?
C9B C8 C9B C9B 0.0 5_655 . . 21 ?
C7 C8 C9B C9B 180.0 . . . 21 ?

_refine_diff_density_max         2.066
_refine_diff_density_min         -2.100
_refine_diff_density_rms         0.158



