# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_VNU-23
_database_code_depnum_ccdc_archive 'CCDC 1585550'
_audit_update_record             
;
2017-12-07 deposited with the CCDC.
2017-12-21 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            'C24 H8 N0 O28 S4 Zr3'
_chemical_formula_weight         1146.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-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                   17.7174(11)
_cell_length_b                   17.7174(11)
_cell_length_c                   22.4865(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7058.7(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    150
_cell_measurement_reflns_used    1197
_cell_measurement_theta_min      3.1755
_cell_measurement_theta_max      60.6535

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_F_000             2240
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    5.183
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker four circle kappa-diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 7.314
_diffrn_reflns_number            13642
_diffrn_reflns_av_unetI/netI     0.1298
_diffrn_reflns_av_R_equivalents  0.1391
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.175
_diffrn_reflns_theta_max         65.008
_diffrn_reflns_theta_full        65.008
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             3076
_reflns_number_gt                1868
_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)+(0.1304P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3076
_refine_ls_number_parameters     167
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0714
_refine_ls_wR_factor_ref         0.2149
_refine_ls_wR_factor_gt          0.1898
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_restrained_S_all      0.940
_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
CA34 C 0.1338(13) 0.1649(13) 0.2512(11) 0.051(6) Uiso 0.5 1 d . . P A 1
HA34 H 0.0920 0.1311 0.2412 0.062 Uiso 0.5 1 calc R U P A 1
CB16 C 0.2326(13) 0.2017(13) 0.3272(10) 0.045(6) Uiso 0.5 1 d . . P A 1
HB16 H 0.2584 0.1926 0.3625 0.054 Uiso 0.5 1 calc R U P A 1
CB34 C 0.1650(16) 0.1309(16) 0.2502(13) 0.070(7) Uiso 0.5 1 d . . P A 2
HB34 H 0.1344 0.0868 0.2400 0.085 Uiso 0.5 1 calc R U P A 2
CA16 C 0.2074(11) 0.2264(11) 0.3252(9) 0.031(4) Uiso 0.5 1 d . . P A 2
HA16 H 0.2051 0.2468 0.3633 0.037 Uiso 0.5 1 calc R U P A 2
O15 O 0.3209(17) 0.102(4) 0.137(3) 0.079(18) Uiso 0.15 1 d D . P A 3
S18 S 0.2340(14) 0.1079(13) 0.1412(10) 0.063(5) Uiso 0.15 1 d D . P A 3
O13 O 0.177(4) 0.050(4) 0.142(4) 0.11(2) Uiso 0.15 1 d . . P A 3
O33 O 0.1999(15) 0.1692(18) 0.0964(13) 0.068(8) Uiso 0.3 1 d D . P A 3
S7 S 0.1305(11) 0.2041(12) 0.1312(8) 0.045(4) Uiso 0.15 1 d D . P A 3
O18 O 0.070(3) 0.150(3) 0.137(2) 0.127(14) Uiso 0.3 1 d . . P A 3
O37 O 0.117(2) 0.2920(16) 0.126(2) 0.041(11) Uiso 0.15 1 d D . P A 3
O34 O 0.2802(16) 0.117(2) 0.121(2) 0.066(12) Uiso 0.2 1 d D . P A 4
S17 S 0.1949(10) 0.1392(9) 0.1300(7) 0.047(3) Uiso 0.2 1 d D . P A 4
O12 O 0.1168(15) 0.0974(16) 0.1304(13) 0.093(8) Uiso 0.4 1 d . . P A 4
O40 O 0.1619(15) 0.2114(13) 0.0976(12) 0.069(7) Uiso 0.35 1 d D . P A 4
S6 S 0.1052(16) 0.2451(17) 0.1491(13) 0.085(7) Uiso 0.15 1 d D . P A 4
O14 O 0.086(5) 0.330(2) 0.143(4) 0.12(3) Uiso 0.15 1 d D . P A 4
O5 O 0.031(2) 0.215(5) 0.159(4) 0.12(3) Uiso 0.15 1 d D . P A 4
O38 O 0.2400(11) 0.1406(13) 0.1015(10) 0.058(6) Uiso 0.35 1 d D . P A 4
O39 O 0.1308(15) 0.2486(12) 0.1060(12) 0.070(7) Uiso 0.35 1 d D . P A 4
S5 S 0.1627(6) 0.1699(6) 0.1276(4) 0.0453(18) Uiso 0.35 1 d D . P A 4
Zr1 Zr 0.0000 0.0000 0.39119(6) 0.0192(4) Uani 1 4 d S T P . .
Zr2 Zr -0.09972(6) 0.09979(6) 0.5000 0.0255(3) Uani 1 2 d S T P . .
O1 O -0.0007(7) 0.0795(8) 0.4552(6) 0.037(3) Uiso 0.5 1 d . . P . .
O2 O -0.0928(6) 0.2230(6) 0.5000 0.056(3) Uani 1 2 d S T P . .
O3 O -0.2227(6) 0.0923(7) 0.5000 0.057(3) Uani 1 2 d S T P . .
O4 O 0.0747(3) 0.0743(3) 0.3397(3) 0.0333(14) Uani 1 1 d . . . . .
O6 O -0.1386(4) 0.1396(4) 0.4103(3) 0.059(2) Uani 1 1 d . . . . .
C7 C 0.1217(6) 0.1240(6) 0.3569(4) 0.045(3) Uani 1 1 d . . . . .
C9 C 0.1646(7) 0.1649(7) 0.3093(5) 0.066(4) Uani 1 1 d . . . . .
C12 C 0.2568(9) 0.2585(9) 0.2793(5) 0.084(5) Uani 1 1 d . . . . .
CA22 C 0.1722(19) 0.2084(19) 0.2044(15) 0.090(10) Uiso 0.5 1 d . . P . .
CB22 C 0.2052(15) 0.1740(15) 0.2062(12) 0.063(7) Uiso 0.5 1 d . . P A .
O50 O -0.0002(6) 0.1115(7) 0.4410(5) 0.023(3) Uiso 0.5 1 d . . 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
CA34 C9 1.41(3) . ?
CA34 CA22 1.47(4) . ?
CA34 CB22 1.63(3) . ?
CA34 HA34 0.9800 . ?
CB16 C9 1.43(2) . ?
CB16 C12 1.54(3) . ?
CB16 HB16 0.9300 . ?
CB34 CB22 1.44(4) . ?
CB34 C9 1.46(3) . ?
CB34 CA22 1.72(4) . ?
CB34 HB34 0.9800 . ?
CA16 C9 1.38(2) . ?
CA16 C12 1.47(2) . ?
CA16 HA16 0.9300 . ?
O15 S18 1.55(2) . ?
S18 O13 1.44(8) . ?
S18 O33 1.60(4) . ?
S18 CB22 1.94(3) . ?
S18 S7 2.51(3) . ?
O33 S7 1.584(18) . ?
S7 O18 1.45(4) . ?
S7 O37 1.580(19) . ?
S7 CA22 1.80(4) . ?
S7 CB22 2.21(3) . ?
O34 O38 0.93(4) . ?
O34 S17 1.576(19) . ?
S17 S5 0.790(14) . ?
S17 O38 1.02(2) . ?
S17 O12 1.57(3) . ?
S17 O40 1.585(17) . ?
S17 CB22 1.83(3) . ?
S17 CA22 2.11(4) . ?
S17 S6 2.50(3) . ?
O12 S5 1.52(3) . ?
O40 O39 0.88(3) . ?
O40 S5 1.00(2) . ?
O40 S6 1.64(4) . ?
S6 O39 1.07(3) . ?
S6 O5 1.44(5) . ?
S6 O14 1.55(2) . ?
S6 S5 1.75(3) . ?
S6 CA22 1.84(4) . ?
O38 S5 1.577(17) . ?
O39 S5 1.581(17) . ?
S5 CA22 1.86(4) . ?
S5 CB22 1.92(3) . ?
Zr1 O1 2.014(13) . ?
Zr1 O1 2.014(13) 4 ?
Zr1 O1 2.014(13) 3 ?
Zr1 O1 2.014(13) 2 ?
Zr1 O4 2.197(6) 2 ?
Zr1 O4 2.197(6) 4 ?
Zr1 O4 2.197(6) 3 ?
Zr1 O4 2.197(6) . ?
Zr1 O50 2.271(11) 4 ?
Zr1 O50 2.271(11) 3 ?
Zr1 O50 2.271(11) 2 ?
Zr1 O50 2.271(11) . ?
Zr2 O1 2.054(13) . ?
Zr2 O1 2.054(13) 10_556 ?
Zr2 O1 2.077(13) 3 ?
Zr2 O1 2.077(13) 12_556 ?
Zr2 O3 2.182(10) . ?
Zr2 O2 2.187(11) . ?
Zr2 O50 2.215(11) . ?
Zr2 O50 2.215(11) 10_556 ?
Zr2 O50 2.223(11) 3 ?
Zr2 O50 2.223(11) 12_556 ?
Zr2 O6 2.245(7) 10_556 ?
Zr2 O6 2.245(7) . ?
O1 O50 0.651(15) . ?
O1 Zr2 2.077(13) 11_556 ?
O4 C7 1.271(12) . ?
O6 C7 1.268(12) 3 ?
C7 O6 1.268(12) 4 ?
C7 C9 1.500(13) . ?
C12 C12 1.37(2) 13 ?
C12 CB22 1.41(3) 13 ?
C12 CA22 1.44(3) 13 ?
CA22 CB22 0.84(4) . ?
CA22 C12 1.43(3) 13 ?
CB22 C12 1.41(3) 13 ?
O50 Zr2 2.223(11) 11_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C9 CA34 CA22 119(2) . . ?
C9 CA34 CB22 105.9(18) . . ?
CA22 CA34 CB22 31.1(15) . . ?
C9 CA34 HA34 120.3 . . ?
CA22 CA34 HA34 120.3 . . ?
CB22 CA34 HA34 120.3 . . ?
C9 CB16 C12 109.7(17) . . ?
C9 CB16 HB16 125.1 . . ?
C12 CB16 HB16 125.1 . . ?
CB22 CB34 C9 114(2) . . ?
CB22 CB34 CA22 29.3(14) . . ?
C9 CB34 CA22 103(2) . . ?
CB22 CB34 HB34 122.6 . . ?
C9 CB34 HB34 122.6 . . ?
CA22 CB34 HB34 122.6 . . ?
C9 CA16 C12 116.9(15) . . ?
C9 CA16 HA16 121.5 . . ?
C12 CA16 HA16 121.5 . . ?
O13 S18 O15 131(4) . . ?
O13 S18 O33 103(4) . . ?
O15 S18 O33 113(3) . . ?
O13 S18 CB22 104(4) . . ?
O15 S18 CB22 110(3) . . ?
O33 S18 CB22 88.0(16) . . ?
O13 S18 S7 88(3) . . ?
O15 S18 S7 140(3) . . ?
O33 S18 S7 37.6(10) . . ?
CB22 S18 S7 57.8(11) . . ?
S7 O33 S18 104(2) . . ?
O18 S7 O37 124(3) . . ?
O18 S7 O33 111(3) . . ?
O37 S7 O33 118(2) . . ?
O18 S7 CA22 104(2) . . ?
O37 S7 CA22 95(2) . . ?
O33 S7 CA22 98.5(19) . . ?
O18 S7 CB22 102(2) . . ?
O37 S7 CB22 113(2) . . ?
O33 S7 CB22 79.5(16) . . ?
CA22 S7 CB22 21.4(12) . . ?
O18 S7 S18 95(2) . . ?
O37 S7 S18 142(2) . . ?
O33 S7 S18 38.1(14) . . ?
CA22 S7 S18 69.4(14) . . ?
CB22 S7 S18 48.0(10) . . ?
O38 O34 S17 38.4(17) . . ?
S5 S17 O38 120(2) . . ?
S5 S17 O12 71.8(17) . . ?
O38 S17 O12 134(2) . . ?
S5 S17 O34 149(2) . . ?
O38 S17 O34 34(2) . . ?
O12 S17 O34 137(2) . . ?
S5 S17 O40 31.3(13) . . ?
O38 S17 O40 88.8(19) . . ?
O12 S17 O40 93.3(17) . . ?
O34 S17 O40 120(2) . . ?
S5 S17 CB22 84.6(16) . . ?
O38 S17 CB22 120.1(19) . . ?
O12 S17 CB22 104.0(16) . . ?
O34 S17 CB22 97(2) . . ?
O40 S17 CB22 101.3(15) . . ?
S5 S17 CA22 61.3(15) . . ?
O38 S17 CA22 129.1(19) . . ?
O12 S17 CA22 95.9(16) . . ?
O34 S17 CA22 116(2) . . ?
O40 S17 CA22 80.0(15) . . ?
CB22 S17 CA22 23.4(11) . . ?
S5 S17 S6 15.2(12) . . ?
O38 S17 S6 125.8(19) . . ?
O12 S17 S6 78.1(15) . . ?
O34 S17 S6 145.3(19) . . ?
O40 S17 S6 40.3(13) . . ?
CB22 S17 S6 69.5(12) . . ?
CA22 S17 S6 46.1(12) . . ?
S5 O12 S17 29.5(7) . . ?
O39 O40 S5 115(3) . . ?
O39 O40 S17 137(3) . . ?
S5 O40 S17 24.3(9) . . ?
O39 O40 S6 36(2) . . ?
S5 O40 S6 79(2) . . ?
S17 O40 S6 101.2(19) . . ?
O39 S6 O5 123(4) . . ?
O39 S6 O14 87(4) . . ?
O5 S6 O14 100(5) . . ?
O39 S6 O40 29.1(14) . . ?
O5 S6 O40 122(4) . . ?
O14 S6 O40 115(4) . . ?
O39 S6 S5 63.0(17) . . ?
O5 S6 S5 107(3) . . ?
O14 S6 S5 148(4) . . ?
O40 S6 S5 34.1(9) . . ?
O39 S6 CA22 111(3) . . ?
O5 S6 CA22 111(4) . . ?
O14 S6 CA22 123(4) . . ?
O40 S6 CA22 87.3(18) . . ?
S5 S6 CA22 62.6(15) . . ?
O39 S6 S17 67.6(18) . . ?
O5 S6 S17 109(3) . . ?
O14 S6 S17 149(4) . . ?
O40 S6 S17 38.5(10) . . ?
S5 S6 S17 6.8(5) . . ?
CA22 S6 S17 55.8(14) . . ?
O34 O38 S17 107(3) . . ?
O34 O38 S5 130(3) . . ?
S17 O38 S5 25.7(10) . . ?
O40 O39 S6 115(3) . . ?
O40 O39 S5 35.0(19) . . ?
S6 O39 S5 80(2) . . ?
S17 S5 O40 124(2) . . ?
S17 S5 O12 78.6(17) . . ?
O40 S5 O12 130(2) . . ?
S17 S5 O38 34.2(14) . . ?
O40 S5 O38 90.2(19) . . ?
O12 S5 O38 101.6(15) . . ?
S17 S5 O39 152.5(17) . . ?
O40 S5 O39 30.4(18) . . ?
O12 S5 O39 124.5(16) . . ?
O38 S5 O39 119.1(15) . . ?
S17 S5 S6 158.0(17) . . ?
O40 S5 S6 67.4(19) . . ?
O12 S5 S6 108.7(16) . . ?
O38 S5 S6 149.4(14) . . ?
O39 S5 S6 37.1(12) . . ?
S17 S5 CA22 96.9(17) . . ?
O40 S5 CA22 111(2) . . ?
O12 S5 CA22 108.6(16) . . ?
O38 S5 CA22 112.7(15) . . ?
O39 S5 CA22 89.6(15) . . ?
S6 S5 CA22 61.1(14) . . ?
S17 S5 CB22 71.2(15) . . ?
O40 S5 CB22 126.7(18) . . ?
O12 S5 CB22 101.7(14) . . ?
O38 S5 CB22 90.8(13) . . ?
O39 S5 CB22 112.8(13) . . ?
S6 S5 CB22 86.8(13) . . ?
CA22 S5 CB22 25.7(11) . . ?
O1 Zr1 O1 59.2(5) . 4 ?
O1 Zr1 O1 59.2(5) . 3 ?
O1 Zr1 O1 88.7(8) 4 3 ?
O1 Zr1 O1 88.7(8) . 2 ?
O1 Zr1 O1 59.2(5) 4 2 ?
O1 Zr1 O1 59.2(5) 3 2 ?
O1 Zr1 O4 142.4(4) . 2 ?
O1 Zr1 O4 143.3(4) 4 2 ?
O1 Zr1 O4 87.3(4) 3 2 ?
O1 Zr1 O4 87.8(4) 2 2 ?
O1 Zr1 O4 143.3(4) . 4 ?
O1 Zr1 O4 87.8(4) 4 4 ?
O1 Zr1 O4 142.4(4) 3 4 ?
O1 Zr1 O4 87.3(4) 2 4 ?
O4 Zr1 O4 73.86(15) 2 4 ?
O1 Zr1 O4 87.3(4) . 3 ?
O1 Zr1 O4 142.4(4) 4 3 ?
O1 Zr1 O4 87.8(4) 3 3 ?
O1 Zr1 O4 143.3(4) 2 3 ?
O4 Zr1 O4 73.86(15) 2 3 ?
O4 Zr1 O4 116.4(3) 4 3 ?
O1 Zr1 O4 87.8(4) . . ?
O1 Zr1 O4 87.3(4) 4 . ?
O1 Zr1 O4 143.3(4) 3 . ?
O1 Zr1 O4 142.4(4) 2 . ?
O4 Zr1 O4 116.4(3) 2 . ?
O4 Zr1 O4 73.86(15) 4 . ?
O4 Zr1 O4 73.86(15) 3 . ?
O1 Zr1 O50 69.6(6) . 4 ?
O1 Zr1 O50 16.1(4) 4 4 ?
O1 Zr1 O50 104.8(6) 3 4 ?
O1 Zr1 O50 69.1(6) 2 4 ?
O4 Zr1 O50 141.7(3) 2 4 ?
O4 Zr1 O50 74.9(3) 4 4 ?
O4 Zr1 O50 141.3(3) 3 4 ?
O4 Zr1 O50 74.7(3) . 4 ?
O1 Zr1 O50 69.1(6) . 3 ?
O1 Zr1 O50 104.8(6) 4 3 ?
O1 Zr1 O50 16.1(4) 3 3 ?
O1 Zr1 O50 69.6(6) 2 3 ?
O4 Zr1 O50 74.7(3) 2 3 ?
O4 Zr1 O50 141.3(3) 4 3 ?
O4 Zr1 O50 74.9(3) 3 3 ?
O4 Zr1 O50 141.7(3) . 3 ?
O50 Zr1 O50 120.8(6) 4 3 ?
O1 Zr1 O50 104.8(6) . 2 ?
O1 Zr1 O50 69.6(6) 4 2 ?
O1 Zr1 O50 69.1(6) 3 2 ?
O1 Zr1 O50 16.1(4) 2 2 ?
O4 Zr1 O50 74.9(3) 2 2 ?
O4 Zr1 O50 74.7(3) 4 2 ?
O4 Zr1 O50 141.7(3) 3 2 ?
O4 Zr1 O50 141.3(3) . 2 ?
O50 Zr1 O50 75.9(3) 4 2 ?
O50 Zr1 O50 75.9(3) 3 2 ?
O1 Zr1 O50 16.1(4) . . ?
O1 Zr1 O50 69.1(6) 4 . ?
O1 Zr1 O50 69.6(6) 3 . ?
O1 Zr1 O50 104.8(6) 2 . ?
O4 Zr1 O50 141.3(3) 2 . ?
O4 Zr1 O50 141.7(3) 4 . ?
O4 Zr1 O50 74.7(3) 3 . ?
O4 Zr1 O50 74.9(3) . . ?
O50 Zr1 O50 75.9(3) 4 . ?
O50 Zr1 O50 75.9(3) 3 . ?
O50 Zr1 O50 120.8(6) 2 . ?
O1 Zr2 O1 58.7(8) . 10_556 ?
O1 Zr2 O1 57.6(7) . 3 ?
O1 Zr2 O1 86.5(8) 10_556 3 ?
O1 Zr2 O1 86.5(8) . 12_556 ?
O1 Zr2 O1 57.6(7) 10_556 12_556 ?
O1 Zr2 O1 58.0(7) 3 12_556 ?
O1 Zr2 O3 147.3(4) . . ?
O1 Zr2 O3 147.3(4) 10_556 . ?
O1 Zr2 O3 96.9(5) 3 . ?
O1 Zr2 O3 96.9(5) 12_556 . ?
O1 Zr2 O2 97.3(5) . . ?
O1 Zr2 O2 97.3(5) 10_556 . ?
O1 Zr2 O2 147.8(4) 3 . ?
O1 Zr2 O2 147.8(4) 12_556 . ?
O3 Zr2 O2 96.7(4) . . ?
O1 Zr2 O50 17.0(4) . . ?
O1 Zr2 O50 68.3(4) 10_556 . ?
O1 Zr2 O50 69.7(5) 3 . ?
O1 Zr2 O50 103.5(6) 12_556 . ?
O3 Zr2 O50 143.1(3) . . ?
O2 Zr2 O50 82.1(4) . . ?
O1 Zr2 O50 68.3(4) . 10_556 ?
O1 Zr2 O50 17.0(4) 10_556 10_556 ?
O1 Zr2 O50 103.5(6) 3 10_556 ?
O1 Zr2 O50 69.7(5) 12_556 10_556 ?
O3 Zr2 O50 143.1(3) . 10_556 ?
O2 Zr2 O50 82.1(4) . 10_556 ?
O50 Zr2 O50 73.5(6) . 10_556 ?
O1 Zr2 O50 69.4(5) . 3 ?
O1 Zr2 O50 103.4(6) 10_556 3 ?
O1 Zr2 O50 17.0(4) 3 3 ?
O1 Zr2 O50 67.8(4) 12_556 3 ?
O3 Zr2 O50 81.8(4) . 3 ?
O2 Zr2 O50 143.2(3) . 3 ?
O50 Zr2 O50 78.0(6) . 3 ?
O50 Zr2 O50 120.4(6) 10_556 3 ?
O1 Zr2 O50 103.4(6) . 12_556 ?
O1 Zr2 O50 69.4(5) 10_556 12_556 ?
O1 Zr2 O50 67.8(4) 3 12_556 ?
O1 Zr2 O50 17.0(4) 12_556 12_556 ?
O3 Zr2 O50 81.8(4) . 12_556 ?
O2 Zr2 O50 143.2(3) . 12_556 ?
O50 Zr2 O50 120.4(6) . 12_556 ?
O50 Zr2 O50 78.0(6) 10_556 12_556 ?
O50 Zr2 O50 73.2(6) 3 12_556 ?
O1 Zr2 O6 139.2(4) . 10_556 ?
O1 Zr2 O6 82.9(4) 10_556 10_556 ?
O1 Zr2 O6 139.3(4) 3 10_556 ?
O1 Zr2 O6 83.5(4) 12_556 10_556 ?
O3 Zr2 O6 73.3(2) . 10_556 ?
O2 Zr2 O6 72.7(2) . 10_556 ?
O50 Zr2 O6 138.8(4) . 10_556 ?
O50 Zr2 O6 71.1(4) 10_556 10_556 ?
O50 Zr2 O6 139.3(4) 3 10_556 ?
O50 Zr2 O6 71.7(4) 12_556 10_556 ?
O1 Zr2 O6 82.9(4) . . ?
O1 Zr2 O6 139.2(4) 10_556 . ?
O1 Zr2 O6 83.5(4) 3 . ?
O1 Zr2 O6 139.3(4) 12_556 . ?
O3 Zr2 O6 73.3(2) . . ?
O2 Zr2 O6 72.7(2) . . ?
O50 Zr2 O6 71.1(4) . . ?
O50 Zr2 O6 138.8(4) 10_556 . ?
O50 Zr2 O6 71.7(4) 3 . ?
O50 Zr2 O6 139.3(4) 12_556 . ?
O6 Zr2 O6 127.9(4) 10_556 . ?
O50 O1 Zr1 105.0(19) . . ?
O50 O1 Zr2 95.7(19) . . ?
Zr1 O1 Zr2 118.6(6) . . ?
O50 O1 Zr2 94.3(18) . 11_556 ?
Zr1 O1 Zr2 117.5(6) . 11_556 ?
Zr2 O1 Zr2 117.7(6) . 11_556 ?
C7 O4 Zr1 130.4(6) . . ?
C7 O6 Zr2 135.2(6) 3 . ?
O6 C7 O4 126.4(8) 4 . ?
O6 C7 C9 116.8(9) 4 . ?
O4 C7 C9 116.6(9) . . ?
CA34 C9 CB16 125.8(15) . . ?
CA16 C9 CB34 124.1(16) . . ?
CA16 C9 C7 118.5(12) . . ?
CA34 C9 C7 117.6(13) . . ?
CB16 C9 C7 116.6(13) . . ?
CB34 C9 C7 117.0(14) . . ?
C12 C12 CB22 119.5(18) 13 13 ?
C12 C12 CA22 119.3(19) 13 13 ?
CB22 C12 CA22 34.5(15) 13 13 ?
C12 C12 CA16 118.9(15) 13 . ?
CB22 C12 CA16 116.8(16) 13 . ?
CA22 C12 CA16 120.0(18) 13 . ?
C12 C12 CB16 118.6(16) 13 . ?
CB22 C12 CB16 121.8(16) 13 . ?
CA22 C12 CB16 109.5(19) 13 . ?
CB22 CA22 C12 71(3) . 13 ?
CB22 CA22 CA34 85(3) . . ?
C12 CA22 CA34 116(3) 13 . ?
CB22 CA22 CB34 56(3) . . ?
C12 CA22 CB34 104(2) 13 . ?
CB22 CA22 S7 107(4) . . ?
C12 CA22 S7 128(2) 13 . ?
CB22 CA22 S6 137(4) . . ?
C12 CA22 S6 126(3) 13 . ?
CB22 CA22 S5 81(3) . . ?
C12 CA22 S5 118(2) 13 . ?
S6 CA22 S5 56.3(14) . . ?
CB22 CA22 S17 59(3) . . ?
C12 CA22 S17 106(2) 13 . ?
S6 CA22 S17 78.1(16) . . ?
S5 CA22 S17 21.8(6) . . ?
CA22 CB22 C12 74(3) . 13 ?
CA22 CB22 CB34 94(4) . . ?
C12 CB22 CB34 122(2) 13 . ?
CA22 CB22 CA34 64(3) . . ?
C12 CB22 CA34 108.1(19) 13 . ?
CA22 CB22 S17 97(3) . . ?
C12 CB22 S17 123.4(18) 13 . ?
CA22 CB22 S5 73(3) . . ?
C12 CB22 S5 115.6(17) 13 . ?
S17 CB22 S5 24.1(6) . . ?
CA22 CB22 S18 125(4) . . ?
C12 CB22 S18 124.1(19) 13 . ?
CA22 CB22 S7 51(3) . . ?
C12 CB22 S7 105.0(17) 13 . ?
S18 CB22 S7 74.2(12) . . ?
O1 O50 Zr2 67.3(17) . . ?
O1 O50 Zr2 68.7(17) . 11_556 ?
Zr2 O50 Zr2 105.6(5) . 11_556 ?
O1 O50 Zr1 58.9(16) . . ?
Zr2 O50 Zr1 102.5(5) . . ?
Zr2 O50 Zr1 102.2(5) 11_556 . ?

_refine_diff_density_max         1.065
_refine_diff_density_min         -0.988
_refine_diff_density_rms         0.155



####################################################################### 
# 
# 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_his_sq
_database_code_depnum_ccdc_archive 'CCDC 1810933'
_audit_update_record             
;
2017-12-13 deposited with the CCDC.
2017-12-21 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            'C27 H8 N1.80 O28 S4 Zr3'
_chemical_formula_weight         1207.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 4'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-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                   17.526(3)
_cell_length_b                   17.526(3)
_cell_length_c                   22.893(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7032(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150
_cell_measurement_reflns_used    1197
_cell_measurement_theta_min      3.173
_cell_measurement_theta_max      60.622

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_F_000             2362
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    5.235
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7145
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker four circle kappa-diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13797
_diffrn_reflns_av_unetI/netI     0.1279
_diffrn_reflns_av_R_equivalents  0.1537
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.176
_diffrn_reflns_theta_max         61.160
_diffrn_reflns_theta_full        61.160
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             2750
_reflns_number_gt                1803
_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)+(0.1892P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2750
_refine_ls_number_parameters     241
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.1287
_refine_ls_R_factor_gt           0.0896
_refine_ls_wR_factor_ref         0.2752
_refine_ls_wR_factor_gt          0.2333
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.002

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
CB8 C 0.6632(16) 0.706(2) 0.7141(14) 0.069(8) Uani 0.5 1 d . U P A 1
CA7 C 0.627(2) 0.672(4) 0.7542(17) 0.097(17) Uani 0.5 1 d . . P A 1
HA7 H 0.5779 0.6533 0.7478 0.116 Uiso 0.5 1 calc R U P A 1
S5 S 0.7316(17) 0.6061(14) 0.6460(12) 0.081(8) Uani 0.2 1 d D U P A 1
O20 O 0.8185(19) 0.597(3) 0.639(2) 0.077(14) Uiso 0.2 1 d D . P A 1
O9 O 0.693(2) 0.6594(17) 0.6002(15) 0.085(8) Uiso 0.4 1 d D . P A 1
O12 O 0.710(4) 0.5209(19) 0.651(3) 0.11(2) Uiso 0.2 1 d D . P A 1
S1 S 0.6265(17) 0.7020(18) 0.6404(10) 0.064(7) Uani 0.2 1 d D U P A 1
O14 O 0.579(4) 0.624(4) 0.642(3) 0.087(16) Uiso 0.2 1 d . . P A 1
OA8 O 0.605(3) 0.784(2) 0.619(2) 0.059(11) Uiso 0.2 1 d D . P A 1
CA8 C 0.710(2) 0.6687(19) 0.7123(10) 0.065(8) Uani 0.5 1 d . U P A 2
CB7 C 0.667(2) 0.634(2) 0.7525(14) 0.075(12) Uani 0.5 1 d . . P A 2
HB7 H 0.6387 0.5904 0.7427 0.091 Uiso 0.5 1 calc R U P A 2
S2 S 0.6956(19) 0.6310(16) 0.6368(12) 0.085(11) Uani 0.2 1 d D . P A 2
O8 O 0.6549(15) 0.6983(18) 0.6044(12) 0.085(8) Uiso 0.4 1 d D . P A 2
O13 O 0.663(3) 0.555(3) 0.6470(19) 0.061(11) Uiso 0.2 1 d . . P A 2
S29 S 0.6013(13) 0.7394(17) 0.6481(10) 0.081(8) Uani 0.2 1 d D U P A 2
O16 O 0.601(5) 0.828(2) 0.648(4) 0.13(3) Uiso 0.2 1 d D . P A 2
O15 O 0.544(3) 0.672(3) 0.647(2) 0.083(15) Uiso 0.2 1 d D . P A 2
S3 S 0.6603(18) 0.6620(16) 0.6341(9) 0.057(6) Uani 0.2 1 d D U P A 2
O2 O 0.621(2) 0.585(3) 0.6404(19) 0.056(11) Uiso 0.2 1 d D . P A 2
OA9 O 0.736(3) 0.631(3) 0.607(2) 0.070(14) Uiso 0.2 1 d D . P A 2
OA2 O 0.777(2) 0.613(3) 0.614(3) 0.079(15) Uiso 0.2 1 d D . P A 2
O10 O 0.632(3) 0.740(2) 0.610(2) 0.054(10) Uiso 0.2 1 d D . P A 2
N3 N 0.761(7) 0.492(9) 0.683(6) 0.14(5) Uiso 0.15 1 d D . P B 3
C24 C 0.826(11) 0.531(12) 0.678(9) 0.15(6) Uiso 0.15 1 d . . P B 3
C33 C 0.868(5) 0.538(6) 0.739(5) 0.08(3) Uiso 0.15 1 d D . P B 3
N1 N 0.759(3) 0.500(4) 0.885(2) 0.055(16) Uiso 0.15 1 d G . P B 3
C38 C 0.821(5) 0.548(5) 0.899(3) 0.17(8) Uiso 0.15 1 d G . P B 3
N2 N 0.861(4) 0.563(5) 0.846(4) 0.12(4) Uiso 0.15 1 d G . P B 3
C39 C 0.825(4) 0.523(4) 0.800(3) 0.10(3) Uiso 0.15 1 d G . P B 3
C37 C 0.761(4) 0.484(4) 0.825(2) 0.07(3) Uiso 0.15 1 d G . P B 3
Zr1 Zr 0.5000 0.5000 0.89328(6) 0.0238(5) Uani 1 4 d S T P . .
Zr2 Zr 0.60144(8) 0.60147(8) 1.0000 0.0402(5) Uani 1 2 d S T P . .
O3 O 0.5007(5) 0.5990(7) 0.9481(4) 0.080(3) Uani 1 1 d . . . . .
O4 O 0.6422(6) 0.6409(6) 0.9107(4) 0.077(3) Uani 1 1 d . . . . .
O5 O 0.5747(4) 0.5748(4) 0.8422(3) 0.0426(18) Uani 1 1 d . . . . .
O6 O 0.5957(12) 0.7232(9) 1.0000 0.095(5) Uani 1 2 d S T P . .
O7 O 0.7239(9) 0.5924(12) 1.0000 0.099(6) Uani 1 2 d S T P . .
C11 C 0.6254(9) 0.6255(8) 0.8566(6) 0.065(4) Uani 1 1 d . . . . .
C12 C 0.6640(9) 0.6638(9) 0.8116(6) 0.076(5) Uani 1 1 d . . . . .
C21 C 0.7585(12) 0.7562(12) 0.7773(6) 0.105(7) Uani 1 1 d . . . . .
C22 C 0.7208(13) 0.7184(13) 0.8242(6) 0.128(9) Uani 1 1 d . . . . .
H22 H 0.7334 0.7296 0.8627 0.154 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
CB8 CA7 1.26(5) . ?
CB8 C21 1.54(3) 13_666 ?
CB8 S1 1.81(4) . ?
CA7 C12 1.47(4) . ?
S5 O20 1.54(2) . ?
S5 O12 1.547(15) . ?
S5 O9 1.557(19) . ?
S5 S1 2.50(4) . ?
O9 S1 1.66(4) . ?
S1 OA8 1.57(2) . ?
S1 O14 1.59(6) . ?
CA8 CB7 1.34(4) . ?
CA8 C21 1.45(3) 13_666 ?
CA8 S2 1.87(4) . ?
CA8 S3 1.99(4) . ?
CB7 C12 1.45(3) . ?
S2 S3 0.83(3) . ?
S2 OA9 0.98(4) . ?
S2 O13 1.47(5) . ?
S2 O2 1.54(2) . ?
S2 OA2 1.56(2) . ?
S2 O8 1.566(19) . ?
S2 S29 2.53(4) . ?
O8 O10 0.85(4) . ?
O8 S3 0.94(3) . ?
O8 S29 1.5501(11) . ?
O13 O2 0.93(5) . ?
O13 O15 1.74(7) 4_565 ?
O13 S3 1.90(5) . ?
S29 O10 1.01(5) . ?
S29 O16 1.55(2) . ?
S29 O15 1.55(2) . ?
S29 S3 1.74(4) . ?
O15 O13 1.74(7) 3_655 ?
O15 S3 2.07(6) . ?
S3 O2 1.52(5) . ?
S3 O10 1.56(2) . ?
S3 OA9 1.57(2) . ?
OA9 OA2 0.80(5) . ?
N3 C24 1.3(2) . ?
C24 C33 1.6(2) . ?
C33 C39 1.63(12) . ?
N1 C38 1.4200 . ?
N1 C37 1.4200 . ?
C38 N2 1.4200 . ?
N2 C39 1.4200 . ?
C39 C37 1.4200 . ?
Zr1 O3 2.141(9) 4_565 ?
Zr1 O3 2.141(9) 3_655 ?
Zr1 O3 2.141(9) 2_665 ?
Zr1 O3 2.141(9) . ?
Zr1 O5 2.190(7) . ?
Zr1 O5 2.190(7) 2_665 ?
Zr1 O5 2.190(7) 4_565 ?
Zr1 O5 2.190(7) 3_655 ?
Zr1 Zr2 3.5059(13) 3_655 ?
Zr1 Zr2 3.5059(13) 11_567 ?
Zr1 Zr2 3.5059(13) 9_667 ?
Zr1 Zr2 3.5060(13) . ?
Zr2 O3 2.129(9) 10_557 ?
Zr2 O3 2.129(9) . ?
Zr2 O6 2.137(16) . ?
Zr2 O3 2.149(9) 4_565 ?
Zr2 O3 2.149(9) 11_567 ?
Zr2 O7 2.153(17) . ?
Zr2 O4 2.273(8) 10_557 ?
Zr2 O4 2.273(8) . ?
Zr2 Zr1 3.5060(13) 9_667 ?
Zr2 Zr2 3.5560(17) 3_655 ?
Zr2 Zr2 3.5560(17) 11_567 ?
O3 Zr2 2.149(9) 3_655 ?
O4 C11 1.301(16) . ?
O5 C11 1.300(16) . ?
C11 C12 1.403(18) . ?
C12 C22 1.41(2) . ?
C21 C21 1.30(3) 13_666 ?
C21 C22 1.43(2) . ?
C21 CA8 1.45(3) 13_666 ?
C21 CB8 1.54(3) 13_666 ?

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
CA7 CB8 C21 124(3) . 13_666 ?
CA7 CB8 S1 119(3) . . ?
C21 CB8 S1 116.9(19) 13_666 . ?
CB8 CA7 C12 118(3) . . ?
O20 S5 O12 99(4) . . ?
O20 S5 O9 115(3) . . ?
O12 S5 O9 122(4) . . ?
O20 S5 S1 143(2) . . ?
O12 S5 S1 118(3) . . ?
O9 S5 S1 40.8(16) . . ?
S5 O9 S1 102(2) . . ?
OA8 S1 O14 132(4) . . ?
OA8 S1 O9 114(2) . . ?
O14 S1 O9 90(3) . . ?
OA8 S1 CB8 111(3) . . ?
O14 S1 CB8 101(3) . . ?
O9 S1 CB8 106(2) . . ?
OA8 S1 S5 144(2) . . ?
O14 S1 S5 79(3) . . ?
O9 S1 S5 37.7(12) . . ?
CB8 S1 S5 73.4(19) . . ?
CB7 CA8 C21 121(2) . 13_666 ?
CB7 CA8 S2 114(2) . . ?
C21 CA8 S2 121.6(18) 13_666 . ?
CB7 CA8 S3 110(3) . . ?
C21 CA8 S3 112(2) 13_666 . ?
S2 CA8 S3 24.4(10) . . ?
CA8 CB7 C12 119(3) . . ?
S3 S2 OA9 120(5) . . ?
S3 S2 O13 108(4) . . ?
OA9 S2 O13 113(4) . . ?
S3 S2 O2 73(3) . . ?
OA9 S2 O2 131(4) . . ?
O13 S2 O2 36(2) . . ?
S3 S2 OA2 143(4) . . ?
OA9 S2 OA2 26(4) . . ?
O13 S2 OA2 103(3) . . ?
O2 S2 OA2 134(4) . . ?
S3 S2 O8 29(2) . . ?
OA9 S2 O8 90(4) . . ?
O13 S2 O8 126(3) . . ?
O2 S2 O8 92(3) . . ?
OA2 S2 O8 115(3) . . ?
S3 S2 CA8 86(3) . . ?
OA9 S2 CA8 123(4) . . ?
O13 S2 CA8 103(2) . . ?
O2 S2 CA8 104(2) . . ?
OA2 S2 CA8 105(3) . . ?
O8 S2 CA8 103(2) . . ?
S3 S2 S29 13(2) . . ?
OA9 S2 S29 123(4) . . ?
O13 S2 S29 114(3) . . ?
O2 S2 S29 80(2) . . ?
OA2 S2 S29 142(3) . . ?
O8 S2 S29 35.4(11) . . ?
CA8 S2 S29 74.0(17) . . ?
O10 O8 S3 121(4) . . ?
O10 O8 S29 37(3) . . ?
S3 O8 S29 85(3) . . ?
O10 O8 S2 142(4) . . ?
S3 O8 S2 25.5(19) . . ?
S29 O8 S2 109(2) . . ?
O2 O13 S2 76(3) . . ?
O2 O13 O15 131(5) . 4_565 ?
S2 O13 O15 150(4) . 4_565 ?
O2 O13 S3 52(3) . . ?
S2 O13 S3 24.3(14) . . ?
O15 O13 S3 170(3) 4_565 . ?
O10 S29 O16 89(4) . . ?
O10 S29 O15 110(4) . . ?
O16 S29 O15 139(4) . . ?
O10 S29 O8 30.5(19) . . ?
O16 S29 O8 118(4) . . ?
O15 S29 O8 92(3) . . ?
O10 S29 S3 63(2) . . ?
O16 S29 S3 141(4) . . ?
O15 S29 S3 78(3) . . ?
O8 S29 S3 32.5(13) . . ?
O10 S29 S2 65(2) . . ?
O16 S29 S2 139(4) . . ?
O15 S29 S2 82(3) . . ?
O8 S29 S2 35.8(12) . . ?
S3 S29 S2 6.0(11) . . ?
S29 O15 O13 136(5) . 3_655 ?
S29 O15 S3 55.1(19) . . ?
O13 O15 S3 167(4) 3_655 . ?
S2 S3 O8 125(3) . . ?
S2 S3 O2 76(3) . . ?
O8 S3 O2 129(3) . . ?
S2 S3 O10 148(3) . . ?
O8 S3 O10 28(2) . . ?
O2 S3 O10 131(3) . . ?
S2 S3 OA9 33(3) . . ?
O8 S3 OA9 92(3) . . ?
O2 S3 OA9 97(3) . . ?
O10 S3 OA9 116(3) . . ?
S2 S3 S29 161(3) . . ?
O8 S3 S29 63(2) . . ?
O2 S3 S29 114(3) . . ?
O10 S3 S29 35.3(19) . . ?
OA9 S3 S29 148(3) . . ?
S2 S3 O13 47(3) . . ?
O8 S3 O13 142(3) . . ?
O2 S3 O13 28.8(19) . . ?
O10 S3 O13 159(3) . . ?
OA9 S3 O13 72(3) . . ?
S29 S3 O13 139(2) . . ?
S2 S3 CA8 69(3) . . ?
O8 S3 CA8 131(3) . . ?
O2 S3 CA8 99(2) . . ?
O10 S3 CA8 114(2) . . ?
OA9 S3 CA8 90(3) . . ?
S29 S3 CA8 92.6(18) . . ?
O13 S3 CA8 85(2) . . ?
S2 S3 O15 142(3) . . ?
O8 S3 O15 87(3) . . ?
O2 S3 O15 67(2) . . ?
O10 S3 O15 70(3) . . ?
OA9 S3 O15 158(3) . . ?
S29 S3 O15 46.9(14) . . ?
O13 S3 O15 95(2) . . ?
CA8 S3 O15 107(2) . . ?
O13 O2 S3 99(4) . . ?
O13 O2 S2 68(4) . . ?
S3 O2 S2 31.3(14) . . ?
OA2 OA9 S2 121(8) . . ?
OA2 OA9 S3 145(7) . . ?
S2 OA9 S3 27(2) . . ?
OA9 OA2 S2 33(4) . . ?
O8 O10 S29 112(4) . . ?
O8 O10 S3 31(2) . . ?
S29 O10 S3 82(3) . . ?
N3 C24 C33 112(10) . . ?
C24 C33 C39 122(9) . . ?
C38 N1 C37 108.0 . . ?
N1 C38 N2 108.0 . . ?
C39 N2 C38 108.0 . . ?
N2 C39 C37 108.0 . . ?
N2 C39 C33 111(6) . . ?
C37 C39 C33 141(6) . . ?
C39 C37 N1 108.0 . . ?
O3 Zr1 O3 108.2(6) 4_565 3_655 ?
O3 Zr1 O3 69.9(3) 4_565 2_665 ?
O3 Zr1 O3 69.9(3) 3_655 2_665 ?
O3 Zr1 O3 69.9(3) 4_565 . ?
O3 Zr1 O3 69.9(3) 3_655 . ?
O3 Zr1 O3 108.2(6) 2_665 . ?
O3 Zr1 O5 80.3(3) 4_565 . ?
O3 Zr1 O5 142.5(3) 3_655 . ?
O3 Zr1 O5 143.2(3) 2_665 . ?
O3 Zr1 O5 79.9(3) . . ?
O3 Zr1 O5 142.5(3) 4_565 2_665 ?
O3 Zr1 O5 80.3(3) 3_655 2_665 ?
O3 Zr1 O5 79.9(3) 2_665 2_665 ?
O3 Zr1 O5 143.2(3) . 2_665 ?
O5 Zr1 O5 115.5(4) . 2_665 ?
O3 Zr1 O5 79.9(3) 4_565 4_565 ?
O3 Zr1 O5 143.2(3) 3_655 4_565 ?
O3 Zr1 O5 80.3(3) 2_665 4_565 ?
O3 Zr1 O5 142.6(3) . 4_565 ?
O5 Zr1 O5 73.45(17) . 4_565 ?
O5 Zr1 O5 73.45(17) 2_665 4_565 ?
O3 Zr1 O5 143.2(3) 4_565 3_655 ?
O3 Zr1 O5 79.9(3) 3_655 3_655 ?
O3 Zr1 O5 142.5(3) 2_665 3_655 ?
O3 Zr1 O5 80.3(3) . 3_655 ?
O5 Zr1 O5 73.45(17) . 3_655 ?
O5 Zr1 O5 73.45(17) 2_665 3_655 ?
O5 Zr1 O5 115.5(4) 4_565 3_655 ?
O3 Zr1 Zr2 90.3(3) 4_565 3_655 ?
O3 Zr1 Zr2 34.7(3) 3_655 3_655 ?
O3 Zr1 Zr2 90.0(3) 2_665 3_655 ?
O3 Zr1 Zr2 35.3(3) . 3_655 ?
O5 Zr1 Zr2 111.83(19) . 3_655 ?
O5 Zr1 Zr2 111.84(19) 2_665 3_655 ?
O5 Zr1 Zr2 168.08(18) 4_565 3_655 ?
O5 Zr1 Zr2 76.43(18) 3_655 3_655 ?
O3 Zr1 Zr2 34.7(3) 4_565 11_567 ?
O3 Zr1 Zr2 90.3(3) 3_655 11_567 ?
O3 Zr1 Zr2 35.3(3) 2_665 11_567 ?
O3 Zr1 Zr2 90.0(3) . 11_567 ?
O5 Zr1 Zr2 111.84(19) . 11_567 ?
O5 Zr1 Zr2 111.83(19) 2_665 11_567 ?
O5 Zr1 Zr2 76.43(18) 4_565 11_567 ?
O5 Zr1 Zr2 168.08(18) 3_655 11_567 ?
Zr2 Zr1 Zr2 91.65(4) 3_655 11_567 ?
O3 Zr1 Zr2 90.0(3) 4_565 9_667 ?
O3 Zr1 Zr2 35.3(3) 3_655 9_667 ?
O3 Zr1 Zr2 34.7(3) 2_665 9_667 ?
O3 Zr1 Zr2 90.3(3) . 9_667 ?
O5 Zr1 Zr2 168.08(18) . 9_667 ?
O5 Zr1 Zr2 76.43(18) 2_665 9_667 ?
O5 Zr1 Zr2 111.84(19) 4_565 9_667 ?
O5 Zr1 Zr2 111.83(19) 3_655 9_667 ?
Zr2 Zr1 Zr2 60.95(2) 3_655 9_667 ?
Zr2 Zr1 Zr2 60.95(2) 11_567 9_667 ?
O3 Zr1 Zr2 35.3(3) 4_565 . ?
O3 Zr1 Zr2 90.0(3) 3_655 . ?
O3 Zr1 Zr2 90.3(3) 2_665 . ?
O3 Zr1 Zr2 34.7(3) . . ?
O5 Zr1 Zr2 76.43(18) . . ?
O5 Zr1 Zr2 168.08(18) 2_665 . ?
O5 Zr1 Zr2 111.83(19) 4_565 . ?
O5 Zr1 Zr2 111.84(19) 3_655 . ?
Zr2 Zr1 Zr2 60.95(2) 3_655 . ?
Zr2 Zr1 Zr2 60.95(2) 11_567 . ?
Zr2 Zr1 Zr2 91.65(4) 9_667 . ?
O3 Zr2 O3 67.9(5) 10_557 . ?
O3 Zr2 O6 89.0(6) 10_557 . ?
O3 Zr2 O6 89.0(6) . . ?
O3 Zr2 O3 105.9(7) 10_557 4_565 ?
O3 Zr2 O3 70.0(5) . 4_565 ?
O6 Zr2 O3 146.2(2) . 4_565 ?
O3 Zr2 O3 70.0(5) 10_557 11_567 ?
O3 Zr2 O3 105.9(7) . 11_567 ?
O6 Zr2 O3 146.2(2) . 11_567 ?
O3 Zr2 O3 67.1(4) 4_565 11_567 ?
O3 Zr2 O7 145.7(2) 10_557 . ?
O3 Zr2 O7 145.7(2) . . ?
O6 Zr2 O7 96.9(7) . . ?
O3 Zr2 O7 87.6(6) 4_565 . ?
O3 Zr2 O7 87.6(6) 11_567 . ?
O3 Zr2 O4 76.4(4) 10_557 10_557 ?
O3 Zr2 O4 140.3(4) . 10_557 ?
O6 Zr2 O4 73.2(3) . 10_557 ?
O3 Zr2 O4 139.2(4) 4_565 10_557 ?
O3 Zr2 O4 76.3(4) 11_567 10_557 ?
O7 Zr2 O4 73.1(3) . 10_557 ?
O3 Zr2 O4 140.3(4) 10_557 . ?
O3 Zr2 O4 76.4(4) . . ?
O6 Zr2 O4 73.2(3) . . ?
O3 Zr2 O4 76.3(4) 4_565 . ?
O3 Zr2 O4 139.2(4) 11_567 . ?
O7 Zr2 O4 73.1(3) . . ?
O4 Zr2 O4 128.1(4) 10_557 . ?
O3 Zr2 Zr1 34.9(3) 10_557 9_667 ?
O3 Zr2 Zr1 87.6(3) . 9_667 ?
O6 Zr2 Zr1 118.9(3) . 9_667 ?
O3 Zr2 Zr1 87.3(3) 4_565 9_667 ?
O3 Zr2 Zr1 35.1(3) 11_567 9_667 ?
O7 Zr2 Zr1 117.9(3) . 9_667 ?
O4 Zr2 Zr1 71.8(2) 10_557 9_667 ?
O4 Zr2 Zr1 160.1(2) . 9_667 ?
O3 Zr2 Zr1 87.6(3) 10_557 . ?
O3 Zr2 Zr1 34.9(3) . . ?
O6 Zr2 Zr1 118.9(3) . . ?
O3 Zr2 Zr1 35.1(3) 4_565 . ?
O3 Zr2 Zr1 87.3(3) 11_567 . ?
O7 Zr2 Zr1 117.9(3) . . ?
O4 Zr2 Zr1 160.1(2) 10_557 . ?
O4 Zr2 Zr1 71.8(2) . . ?
Zr1 Zr2 Zr1 88.35(4) 9_667 . ?
O3 Zr2 Zr2 34.0(2) 10_557 3_655 ?
O3 Zr2 Zr2 34.0(2) . 3_655 ?
O6 Zr2 Zr2 87.3(6) . 3_655 ?
O3 Zr2 Zr2 88.8(3) 4_565 3_655 ?
O3 Zr2 Zr2 88.8(3) 11_567 3_655 ?
O7 Zr2 Zr2 175.8(6) . 3_655 ?
O4 Zr2 Zr2 108.3(3) 10_557 3_655 ?
O4 Zr2 Zr2 108.3(3) . 3_655 ?
Zr1 Zr2 Zr2 59.526(12) 9_667 3_655 ?
Zr1 Zr2 Zr2 59.526(12) . 3_655 ?
O3 Zr2 Zr2 88.8(3) 10_557 11_567 ?
O3 Zr2 Zr2 88.8(3) . 11_567 ?
O6 Zr2 Zr2 177.3(6) . 11_567 ?
O3 Zr2 Zr2 33.6(2) 4_565 11_567 ?
O3 Zr2 Zr2 33.6(2) 11_567 11_567 ?
O7 Zr2 Zr2 85.8(6) . 11_567 ?
O4 Zr2 Zr2 107.7(3) 10_557 11_567 ?
O4 Zr2 Zr2 107.7(3) . 11_567 ?
Zr1 Zr2 Zr2 59.526(12) 9_667 11_567 ?
Zr1 Zr2 Zr2 59.526(12) . 11_567 ?
Zr2 Zr2 Zr2 89.999(1) 3_655 11_567 ?
Zr2 O3 Zr1 110.4(5) . . ?
Zr2 O3 Zr2 112.5(4) . 3_655 ?
Zr1 O3 Zr2 109.6(5) . 3_655 ?
C11 O4 Zr2 136.2(8) . . ?
C11 O5 Zr1 133.0(7) . . ?
O5 C11 O4 122.6(11) . . ?
O5 C11 C12 118.0(12) . . ?
O4 C11 C12 119.4(12) . . ?
C11 C12 C22 121.0(13) . . ?
C11 C12 CB7 121.7(18) . . ?
C22 C12 CB7 114.5(17) . . ?
C11 C12 CA7 119.3(19) . . ?
C22 C12 CA7 115(2) . . ?
C21 C21 C22 122.6(17) 13_666 . ?
C21 C21 CA8 113(2) 13_666 13_666 ?
C22 C21 CA8 118.5(16) . 13_666 ?
C21 C21 CB8 114(2) 13_666 13_666 ?
C22 C21 CB8 121.3(17) . 13_666 ?
C12 C22 C21 119.3(13) . . ?

_refine_diff_density_max         1.123
_refine_diff_density_min         -1.456
_refine_diff_density_rms         0.213



