# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_c2m
_database_code_depnum_ccdc_archive 'CCDC 2288076'
loop_
_audit_author_name
_audit_author_address
'Christopher Sumby'
;The University of Adelaide
Australia
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_audit_creation_date             2022-09-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10.5 H6.5 N4 O8 Zr1.5, 0.5(C3 H3 N O)'
_chemical_formula_sum            'C12 H8 N4.50 O8.50 Zr1.50'
_chemical_formula_weight         488.06
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   22.511(5)
_cell_length_b                   23.641(5)
_cell_length_c                   10.046(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.01(3)
_cell_angle_gamma                90
_cell_volume                     5346.3(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    33666
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.647
_cell_measurement_theta_min      1.249
_shelx_estimated_absorpt_T_max   0.988
_shelx_estimated_absorpt_T_min   0.937
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1916
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.104
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.778
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33666
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.647
_diffrn_reflns_theta_min         1.249
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '13.3 (Dectris Eiger detectors)'
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.778
_diffrn_measurement_detector_type 'Dectris Eiger 16M'
_diffrn_measurement_device_type  
;
D. Aragao, J. Aishima, H. Cherukuvada, R. Clarken, M. Clift, 
N. P. Cowieson, D. J. Ericsson, C. L. Gee, S. Macedo, N. Mudie, 
S. Panjikar, J. R. Price, A. Riboldi-Tunnicliffe, R. Rostan, R. 
Williamson and T. T. Caradoc-Davies, MX2: a high-flux 
undulator microfocus beamline serving both the chemical 
and macromolecular crystallography communities at the 
Australian Synchrotron, J. Synchrotron Rad. (2018). 25, 
885-891.
;
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4195
_reflns_number_total             5477
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'AS QEGUI'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.328
_refine_diff_density_min         -0.737
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         5477
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0560
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1039P)²+7.5198P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1705
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N4-C3
 1.34 with sigma of 0.02
 N2-N4
 1.36 with sigma of 0.02
 N2-C4
 1.35 with sigma of 0.02
 C5-C3
 1.39 with sigma of 0.02
 C4-C5
 1.38 with sigma of 0.02
 C7-N6
 1.36 with sigma of 0.02
 N6-C11
 1.46 with sigma of 0.02
 C7-O4
 1.22 with sigma of 0.02
 N6-C10
 1.45 with sigma of 0.02
 N4-C5
 2.24 with sigma of 0.04
 C4-C3
 2.19 with sigma of 0.04
 N2-C5
 2.21 with sigma of 0.04
 N2-C3
 2.16 with sigma of 0.04
 C7-C10
 2.46 with sigma of 0.04
 C7-C11
 2.45 with sigma of 0.04
 C4-N2 \\sim C3-N4
 with sigma of 0.02
 C4-C5 \\sim C5-C3
 with sigma of 0.02
 C4-N4 \\sim C3-N2
 with sigma of 0.02
 N6-C10 \\sim N6-C11
 with sigma of 0.02
3. Restrained planarity
 N2, N4, C4, C5, C3
 with sigma of 0.1
 C7, O4, N6, C10, C11
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N2 \\sim N4 \\sim C4 \\sim C5 \\sim C3: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
C7 \\sim O4 \\sim N6 \\sim C10 \\sim C11: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Uanis(N00E) = Uanis(N00L) = Uanis(C00G) = Uanis(C00J) = Uanis(C00M)
Uanis(C00F) = Uanis(C00I) = Uanis(N00H) = Uanis(C00N)
Uanis(N00H) = Uanis(N5) = Uanis(C00N) = Uanis(C00F) = Uanis(C00I)
Uanis(N00E) = Uanis(C2) = Uanis(C13) = Uanis(C00P) = Uanis(N3) = Uanis(C8)
Uanis(C00F) = Uanis(N1) = Uanis(C00M) = Uanis(C00G) = Uanis(N5) = Uanis(N00H) =
Uanis(C00N) = Uanis(C00I) = Uanis(C1) = Uanis(C00J) = Uanis(N00L)
Uanis(C3) = Uanis(C5) = Uanis(N2) = Uanis(C4) = Uanis(N4)
Uiso(C7) = Uiso(N6) = Uiso(C10) = Uiso(C11)
5. Rigid body (RIGU) restrains
 N2, N4, C4, C5, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, O4, N6, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N00E(0.5) C00F(0.5) C00G(0.5) N00H(0.5) C00I(0.5) H00I(0.5)
 C00J(0.5) H00J(0.5) N00L(0.5) C00M(0.5) H00M(0.5) C00N(0.5) H00N(0.5)
 C00P(0.5) H00P(0.5) N1(0.5) C1(0.5) H1(0.5) N5(0.5) N3(0.5) C2(0.5) H2(0.5)
 C8(0.5) C13(0.5) H13(0.5) N2(0.5) N4(0.5) C4(0.5) H4(0.5) C5(0.5) C3(0.5)
 H3(0.5) C7(0.5) O4(0.5) N6(0.5) C10(0.5) C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5)
7.a Ternary CH refined with riding coordinates:
 O009(H009), O00B(H00B), C00P(H00P), C1(H1)
7.b Aromatic/amide H refined with riding coordinates:
 C00I(H00I), C00J(H00J), C00M(H00M), C00N(H00N), C2(H2), C13(H13), C4(H4),
 C3(H3)
7.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr01 Zr 0.39086(3) 0.500000 0.49995(5) 0.03287(19) Uani 1 2 d S T P . .
Zr02 Zr 0.49998(2) 0.57506(2) 0.67533(4) 0.03342(16) Uani 1 1 d . . . . .
O003 O 0.34087(15) 0.44343(13) 0.3667(3) 0.0396(7) Uani 1 1 d . . . . .
O004 O 0.15931(15) 0.05668(13) 0.3665(3) 0.0403(7) Uani 1 1 d . . . . .
O005 O 0.50015(15) 0.56919(13) 0.8905(3) 0.0367(7) Uani 1 1 d . . . . .
O006 O 0.08927(17) 0.10705(15) 0.2584(4) 0.0515(9) Uani 1 1 d . . . . .
O007 O 0.41085(17) 0.39303(15) 0.2578(3) 0.0503(9) Uani 1 1 d . . . . .
O008 O 0.5528(3) 0.500000 0.6783(7) 0.072(2) Uani 1 2 d S T P . .
O009 O 0.4477(3) 0.500000 0.6761(7) 0.0706(19) Uani 1 2 d S T P . .
H009 H 0.422025 0.500000 0.757310 0.106 Uiso 1 2 calc R U P . .
O00A O 0.4997(2) 0.66647(18) 0.6375(5) 0.0771(14) Uani 1 1 d . . . . .
O00B O 0.4474(2) 0.5730(2) 0.4997(3) 0.0803(16) Uani 1 1 d . . . . .
H00B H 0.421441 0.607299 0.499661 0.120 Uiso 1 1 calc R U . . .
C00C C 0.1424(3) 0.0962(2) 0.2900(5) 0.0454(12) Uani 1 1 d . . . . .
C00D C 0.3580(3) 0.4038(2) 0.2907(5) 0.0452(12) Uani 1 1 d . . . . .
N00E N 0.2515(4) 0.3082(4) 0.1259(9) 0.0451(7) Uani 0.5 1 d . . P A 1
C00F C 0.1948(6) 0.1286(6) 0.2267(13) 0.0451(7) Uani 0.5 1 d . . P B 2
C00G C 0.3168(7) 0.3628(6) 0.2416(14) 0.0451(7) Uani 0.5 1 d . . P B 2
N00H N 0.2492(5) 0.1919(4) 0.1263(9) 0.0451(7) Uani 0.5 1 d . . P B 2
C00I C 0.1912(5) 0.1794(5) 0.1581(12) 0.0451(7) Uani 0.5 1 d . . P B 2
H00I H 0.156569 0.200682 0.137641 0.054 Uiso 0.5 1 calc R U P B 2
C00J C 0.3303(5) 0.3155(5) 0.1640(12) 0.0451(7) Uani 0.5 1 d . . P B 2
H00J H 0.368262 0.304452 0.131908 0.054 Uiso 0.5 1 calc R U P B 2
N00L N 0.2316(4) 0.3154(4) 0.1996(8) 0.0451(7) Uani 0.5 1 d . . P B 2
C00M C 0.2556(5) 0.3607(5) 0.2601(10) 0.0451(7) Uani 0.5 1 d . . P B 2
H00M H 0.233591 0.387866 0.309289 0.054 Uiso 0.5 1 calc R U P B 2
C00N C 0.2547(5) 0.1154(5) 0.2260(10) 0.0451(7) Uani 0.5 1 d . . P B 2
H00N H 0.270208 0.081590 0.263525 0.054 Uiso 0.5 1 calc R U P B 2
C00P C 0.2292(5) 0.2586(4) 0.0552(10) 0.0451(7) Uani 0.5 1 d . . P A 1
H00P H 0.189901 0.268439 0.014902 0.054 Uiso 0.5 1 calc R U P A 1
C00Q C 0.500000 0.5865(10) 1.000000 0.157(9) Uani 1 2 d S T P . .
C00S C 0.500000 0.6862(7) 0.500000 0.224(13) Uani 1 2 d S T P . .
C00T C 0.500000 0.6624(6) 1.000000 0.143(7) Uani 1 2 d S T P . .
N1 N 0.2792(4) 0.2894(4) 0.1445(8) 0.0451(7) Uani 0.5 1 d . . P B 2
C1 C 0.2704(5) 0.2416(4) 0.0555(9) 0.0451(7) Uani 0.5 1 d . . P B 2
H1 H 0.309751 0.231977 0.015440 0.054 Uiso 0.5 1 calc R U P B 2
N5 N 0.2882(4) 0.1540(4) 0.1686(8) 0.0451(7) Uani 0.5 1 d . . P B 2
N3 N 0.2120(4) 0.3453(4) 0.1690(8) 0.0451(7) Uani 0.5 1 d . . P A 1
C2 C 0.3086(5) 0.3206(5) 0.1607(12) 0.0451(7) Uani 0.5 1 d . . P A 1
H2 H 0.343177 0.298789 0.143544 0.054 Uiso 0.5 1 calc R U P A 1
C8 C 0.3053(7) 0.3716(6) 0.2262(14) 0.0451(7) Uani 0.5 1 d . . P A 1
C13 C 0.2457(5) 0.3841(5) 0.2293(10) 0.0451(7) Uani 0.5 1 d . . P A 1
H13 H 0.229973 0.417119 0.270279 0.054 Uiso 0.5 1 calc R U P A 1
N2 N 0.2208(4) 0.2107(3) 0.1428(7) 0.0431(11) Uani 0.5 1 d D U P A 1
N4 N 0.2680(4) 0.1840(3) 0.1995(8) 0.0431(11) Uani 0.5 1 d D U P A 1
C4 C 0.1698(4) 0.1839(4) 0.1662(11) 0.0431(11) Uani 0.5 1 d D U P A 1
H4 H 0.131495 0.194954 0.136040 0.052 Uiso 0.5 1 calc R U P A 1
C5 C 0.1833(5) 0.1368(5) 0.2428(11) 0.0431(11) Uani 0.5 1 d D U P A 1
C3 C 0.2448(4) 0.1380(4) 0.2615(9) 0.0431(11) Uani 0.5 1 d D U P A 1
H3 H 0.266991 0.110797 0.310081 0.052 Uiso 0.5 1 calc R U P A 1
C7 C 0.3265(9) 0.7017(11) 0.502(2) 0.177(6) Uiso 0.5 1 d D U P . .
O4 O 0.3814(6) 0.6891(6) 0.5003(13) 0.118(4) Uiso 0.5 1 d D U P . .
N6 N 0.3042(8) 0.7597(10) 0.500(2) 0.177(6) Uiso 0.5 1 d D U P . .
C10 C 0.2387(10) 0.7604(16) 0.500(4) 0.177(6) Uiso 0.5 1 d D U P . .
C11 C 0.3597(11) 0.7922(11) 0.501(3) 0.177(6) Uiso 0.5 1 d D U P . .
H11A H 0.380878 0.785497 0.584732 0.266 Uiso 0.5 1 calc R U P . .
H11B H 0.350641 0.832591 0.492502 0.266 Uiso 0.5 1 calc R U P . .
H11C H 0.384665 0.780273 0.426135 0.266 Uiso 0.5 1 calc R 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
Zr01 Zr02 3.5056(10) 5_666 ?
Zr01 Zr02 3.5056(10) 2_656 ?
Zr01 Zr02 3.5051(10) . ?
Zr01 Zr02 3.5051(10) 6_565 ?
Zr01 O003 2.201(3) 6_565 ?
Zr01 O003 2.201(3) . ?
Zr01 O004 2.207(3) 4_556 ?
Zr01 O004 2.207(3) 7_556 ?
Zr01 O008 2.194(6) 5_666 ?
Zr01 O009 2.184(6) . ?
Zr01 O00B 2.143(4) 6_565 ?
Zr01 O00B 2.143(4) . ?
Zr02 Zr02 3.5227(10) 2_656 ?
Zr02 Zr02 3.5488(11) 6_565 ?
Zr02 O005 2.166(3) . ?
Zr02 O006 2.248(4) 4_556 ?
Zr02 O007 2.247(4) 5_666 ?
Zr02 O008 2.137(3) . ?
Zr02 O009 2.129(3) . ?
Zr02 O00A 2.194(4) . ?
Zr02 O00B 2.121(4) 2_656 ?
Zr02 O00B 2.125(4) . ?
O003 C00D 1.270(6) . ?
O004 C00C 1.269(6) . ?
O005 C00Q 1.174(9) . ?
O006 C00C 1.263(6) . ?
O007 C00D 1.261(6) . ?
O009 H009 1.0000 . ?
O00A C00S 1.458(7) . ?
O00B H00B 1.0000 . ?
C00C C00F 1.544(15) . ?
C00C C5 1.412(13) . ?
C00D C00G 1.429(16) . ?
C00D C8 1.551(15) . ?
N00E C00P 1.459(12) . ?
N00E N3 1.323(13) . ?
N00E C2 1.364(15) . ?
C00F C00I 1.387(17) . ?
C00F C00N 1.383(17) . ?
C00G C00J 1.397(19) . ?
C00G C00M 1.389(19) . ?
N00H C00I 1.377(14) . ?
N00H C1 1.455(12) . ?
N00H N5 1.323(14) . ?
C00I H00I 0.9500 . ?
C00J H00J 0.9500 . ?
C00J N1 1.321(14) . ?
N00L C00M 1.345(13) . ?
N00L N1 1.354(14) . ?
C00M H00M 0.9500 . ?
C00N H00N 0.9500 . ?
C00N N5 1.317(12) . ?
C00P C00P 1.51(2) 7 ?
C00P H00P 1.0000 . ?
C00P N2 1.446(12) . ?
C00Q C00T 1.79(2) . ?
N1 C1 1.454(12) . ?
C1 C1 1.50(2) 7 ?
C1 H1 1.0000 . ?
N3 C13 1.335(13) . ?
C2 H2 0.9500 . ?
C2 C8 1.375(19) . ?
C8 C13 1.374(18) . ?
C13 H13 0.9500 . ?
N2 N4 1.360(11) . ?
N2 C4 1.333(10) . ?
N4 C3 1.358(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(11) . ?
C5 C3 1.398(11) . ?
C3 H3 0.9500 . ?
C7 O4 1.273(16) . ?
C7 N6 1.458(17) . ?
C7 C10 1.72(4) 7_566 ?
N6 C10 1.08(4) 7_566 ?
N6 C10 1.474(15) . ?
N6 C11 1.467(14) . ?
C10 C10 0.70(6) 7_566 ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?

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
Zr02 Zr01 Zr02 60.328(19) 6_565 5_666 ?
Zr02 Zr01 Zr02 91.00(2) 6_565 2_656 ?
Zr02 Zr01 Zr02 60.327(19) . 2_656 ?
Zr02 Zr01 Zr02 60.82(2) 2_656 5_666 ?
Zr02 Zr01 Zr02 91.00(2) . 5_666 ?
Zr02 Zr01 Zr02 60.83(2) 6_565 . ?
O003 Zr01 Zr02 110.87(9) 6_565 . ?
O003 Zr01 Zr02 110.87(9) . 6_565 ?
O003 Zr01 Zr02 75.25(9) . 5_666 ?
O003 Zr01 Zr02 111.12(8) . 2_656 ?
O003 Zr01 Zr02 166.25(9) 6_565 6_565 ?
O003 Zr01 Zr02 75.25(9) 6_565 2_656 ?
O003 Zr01 Zr02 111.13(8) 6_565 5_666 ?
O003 Zr01 Zr02 166.25(9) . . ?
O003 Zr01 O003 74.82(17) . 6_565 ?
O003 Zr01 O004 118.48(13) . 4_556 ?
O003 Zr01 O004 118.48(13) 6_565 7_556 ?
O003 Zr01 O004 74.88(12) . 7_556 ?
O003 Zr01 O004 74.88(12) 6_565 4_556 ?
O004 Zr01 Zr02 111.13(9) 7_556 . ?
O004 Zr01 Zr02 110.91(9) 4_556 2_656 ?
O004 Zr01 Zr02 75.27(9) 7_556 6_565 ?
O004 Zr01 Zr02 111.13(9) 4_556 6_565 ?
O004 Zr01 Zr02 110.91(9) 7_556 5_666 ?
O004 Zr01 Zr02 166.27(9) 4_556 5_666 ?
O004 Zr01 Zr02 75.27(9) 4_556 . ?
O004 Zr01 Zr02 166.27(9) 7_556 2_656 ?
O004 Zr01 O004 74.76(17) 4_556 7_556 ?
O008 Zr01 Zr02 35.41(10) 5_666 5_666 ?
O008 Zr01 Zr02 35.41(10) 5_666 2_656 ?
O008 Zr01 Zr02 90.31(17) 5_666 . ?
O008 Zr01 Zr02 90.31(17) 5_666 6_565 ?
O008 Zr01 O003 78.41(18) 5_666 6_565 ?
O008 Zr01 O003 78.41(18) 5_666 . ?
O008 Zr01 O004 142.36(9) 5_666 4_556 ?
O008 Zr01 O004 142.36(9) 5_666 7_556 ?
O009 Zr01 Zr02 89.79(17) . 5_666 ?
O009 Zr01 Zr02 89.79(17) . 2_656 ?
O009 Zr01 Zr02 35.12(9) . 6_565 ?
O009 Zr01 Zr02 35.12(9) . . ?
O009 Zr01 O003 142.39(9) . 6_565 ?
O009 Zr01 O003 142.39(8) . . ?
O009 Zr01 O004 78.89(17) . 4_556 ?
O009 Zr01 O004 78.89(17) . 7_556 ?
O009 Zr01 O008 108.8(3) . 5_666 ?
O00B Zr01 Zr02 89.54(15) 6_565 . ?
O00B Zr01 Zr02 89.54(15) . 6_565 ?
O00B Zr01 Zr02 34.63(11) 6_565 6_565 ?
O00B Zr01 Zr02 34.51(11) . 2_656 ?
O00B Zr01 Zr02 89.46(15) 6_565 2_656 ?
O00B Zr01 Zr02 89.46(15) . 5_666 ?
O00B Zr01 Zr02 34.63(11) . . ?
O00B Zr01 Zr02 34.51(11) 6_565 5_666 ?
O00B Zr01 O003 142.34(12) . . ?
O00B Zr01 O003 79.27(17) . 6_565 ?
O00B Zr01 O003 142.34(12) 6_565 6_565 ?
O00B Zr01 O003 79.27(17) 6_565 . ?
O00B Zr01 O004 79.39(17) 6_565 7_556 ?
O00B Zr01 O004 142.47(12) 6_565 4_556 ?
O00B Zr01 O004 79.39(17) . 4_556 ?
O00B Zr01 O004 142.47(12) . 7_556 ?
O00B Zr01 O008 69.89(16) 6_565 5_666 ?
O00B Zr01 O008 69.89(16) . 5_666 ?
O00B Zr01 O009 69.70(16) 6_565 . ?
O00B Zr01 O009 69.70(16) . . ?
O00B Zr01 O00B 107.2(3) . 6_565 ?
Zr01 Zr02 Zr01 89.00(2) . 5_666 ?
Zr01 Zr02 Zr02 59.84(2) . 2_656 ?
Zr01 Zr02 Zr02 59.83(2) 5_666 2_656 ?
Zr01 Zr02 Zr02 59.586(12) . 6_565 ?
Zr01 Zr02 Zr02 59.592(12) 5_666 6_565 ?
Zr02 Zr02 Zr02 90.0 2_656 6_565 ?
O005 Zr02 Zr01 117.89(9) . 5_666 ?
O005 Zr02 Zr01 118.05(9) . . ?
O005 Zr02 Zr02 86.33(8) . 6_565 ?
O005 Zr02 Zr02 176.32(8) . 2_656 ?
O005 Zr02 O006 74.19(13) . 4_556 ?
O005 Zr02 O007 73.85(13) . 5_666 ?
O005 Zr02 O00A 103.64(17) . . ?
O006 Zr02 Zr01 161.03(9) 4_556 5_666 ?
O006 Zr02 Zr01 72.10(9) 4_556 . ?
O006 Zr02 Zr02 109.66(10) 4_556 6_565 ?
O006 Zr02 Zr02 107.24(10) 4_556 2_656 ?
O007 Zr02 Zr01 72.17(9) 5_666 5_666 ?
O007 Zr02 Zr01 161.11(9) 5_666 . ?
O007 Zr02 Zr02 107.37(9) 5_666 2_656 ?
O007 Zr02 Zr02 109.61(10) 5_666 6_565 ?
O007 Zr02 O006 126.67(13) 5_666 4_556 ?
O008 Zr02 Zr01 36.51(16) . 5_666 ?
O008 Zr02 Zr01 88.67(18) . . ?
O008 Zr02 Zr02 90.8(2) . 2_656 ?
O008 Zr02 Zr02 33.86(14) . 6_565 ?
O008 Zr02 O005 86.1(2) . . ?
O008 Zr02 O006 140.63(17) . 4_556 ?
O008 Zr02 O007 77.12(19) . 5_666 ?
O008 Zr02 O00A 145.26(18) . . ?
O009 Zr02 Zr01 36.16(16) . . ?
O009 Zr02 Zr01 88.14(17) . 5_666 ?
O009 Zr02 Zr02 90.2(2) . 2_656 ?
O009 Zr02 Zr02 33.56(14) . 6_565 ?
O009 Zr02 O005 86.8(2) . . ?
O009 Zr02 O006 77.59(19) . 4_556 ?
O009 Zr02 O007 140.57(17) . 5_666 ?
O009 Zr02 O008 67.4(2) . . ?
O009 Zr02 O00A 145.08(19) . . ?
O00A Zr02 Zr01 114.19(15) . . ?
O00A Zr02 Zr01 114.42(14) . 5_666 ?
O00A Zr02 Zr02 170.03(15) . 6_565 ?
O00A Zr02 Zr02 80.03(15) . 2_656 ?
O00A Zr02 O006 73.60(17) . 4_556 ?
O00A Zr02 O007 73.95(18) . 5_666 ?
O00B Zr02 Zr01 34.92(12) 2_656 5_666 ?
O00B Zr02 Zr01 87.81(15) . 5_666 ?
O00B Zr02 Zr01 87.88(15) 2_656 . ?
O00B Zr02 Zr01 34.97(12) . . ?
O00B Zr02 Zr02 88.66(14) 2_656 6_565 ?
O00B Zr02 Zr02 33.98(13) 2_656 2_656 ?
O00B Zr02 Zr02 88.66(14) . 6_565 ?
O00B Zr02 Zr02 33.91(12) . 2_656 ?
O00B Zr02 O005 145.58(15) 2_656 . ?
O00B Zr02 O005 145.87(15) . . ?
O00B Zr02 O006 138.84(15) 2_656 4_556 ?
O00B Zr02 O006 75.85(17) . 4_556 ?
O00B Zr02 O007 138.91(14) . 5_666 ?
O00B Zr02 O007 75.91(17) 2_656 5_666 ?
O00B Zr02 O008 107.6(3) . . ?
O00B Zr02 O008 71.4(2) 2_656 . ?
O00B Zr02 O009 71.1(2) . . ?
O00B Zr02 O009 107.0(3) 2_656 . ?
O00B Zr02 O00A 83.2(2) 2_656 . ?
O00B Zr02 O00A 83.0(2) . . ?
O00B Zr02 O00B 67.8(2) 2_656 . ?
C00D O003 Zr01 131.3(3) . . ?
C00C O004 Zr01 131.5(3) . 7_556 ?
C00Q O005 Zr02 155.9(11) . . ?
C00C O006 Zr02 134.7(3) . 4_546 ?
C00D O007 Zr02 134.2(3) . 5_666 ?
Zr02 O008 Zr01 108.1(2) . 5_666 ?
Zr02 O008 Zr01 108.1(2) 6_565 5_666 ?
Zr02 O008 Zr02 112.3(3) 6_565 . ?
Zr01 O009 H009 108.8 . . ?
Zr02 O009 Zr01 108.7(2) . . ?
Zr02 O009 Zr01 108.7(2) 6_565 . ?
Zr02 O009 Zr02 112.9(3) 6_565 . ?
Zr02 O009 H009 108.8 6_565 . ?
Zr02 O009 H009 108.8 . . ?
C00S O00A Zr02 118.6(8) . . ?
Zr01 O00B H00B 107.9 . . ?
Zr02 O00B Zr01 110.40(19) . . ?
Zr02 O00B Zr01 110.58(19) 2_656 . ?
Zr02 O00B Zr02 112.1(2) 2_656 . ?
Zr02 O00B H00B 107.9 2_656 . ?
Zr02 O00B H00B 107.9 . . ?
O004 C00C C00F 112.6(7) . . ?
O004 C00C C5 120.6(6) . . ?
O006 C00C O004 125.8(5) . . ?
O006 C00C C00F 121.3(7) . . ?
O006 C00C C5 113.3(6) . . ?
O003 C00D C00G 120.7(8) . . ?
O003 C00D C8 112.4(7) . . ?
O007 C00D O003 126.3(4) . . ?
O007 C00D C00G 112.7(7) . . ?
O007 C00D C8 121.0(7) . . ?
N3 N00E C00P 117.5(9) . . ?
N3 N00E C2 113.9(9) . . ?
C2 N00E C00P 128.5(11) . . ?
C00I C00F C00C 126.0(11) . . ?
C00N C00F C00C 129.4(11) . . ?
C00N C00F C00I 104.5(11) . . ?
C00J C00G C00D 126.4(12) . . ?
C00M C00G C00D 128.4(12) . . ?
C00M C00G C00J 105.2(11) . . ?
C00I N00H C1 126.7(11) . . ?
N5 N00H C00I 114.2(9) . . ?
N5 N00H C1 119.1(9) . . ?
C00F C00I H00I 127.9 . . ?
N00H C00I C00F 104.1(11) . . ?
N00H C00I H00I 127.9 . . ?
C00G C00J H00J 127.3 . . ?
N1 C00J C00G 105.5(11) . . ?
N1 C00J H00J 127.3 . . ?
C00M N00L N1 103.2(9) . . ?
C00G C00M H00M 124.3 . . ?
N00L C00M C00G 111.5(11) . . ?
N00L C00M H00M 124.3 . . ?
C00F C00N H00N 123.1 . . ?
N5 C00N C00F 113.8(11) . . ?
N5 C00N H00N 123.1 . . ?
N00E C00P C00P 111.1(10) . 7 ?
N00E C00P H00P 108.3 . . ?
C00P C00P H00P 108.3 7 . ?
N2 C00P N00E 112.2(8) . . ?
N2 C00P C00P 108.5(11) . 7 ?
N2 C00P H00P 108.3 . . ?
O005 C00Q O005 139(2) . 2_657 ?
O005 C00Q C00T 110.4(11) 2_657 . ?
O005 C00Q C00T 110.4(11) . . ?
O00A C00S O00A 142.6(14) 2_656 . ?
C00J N1 N00L 114.6(9) . . ?
C00J N1 C1 124.9(10) . . ?
N00L N1 C1 119.8(9) . . ?
N00H C1 H1 107.7 . . ?
N1 C1 N00H 111.8(8) . . ?
N1 C1 H1 107.7 . . ?
C1 C1 H1 107.7 7 . ?
C00N N5 N00H 103.3(9) . . ?
N00E N3 C13 102.9(9) . . ?
N00E C2 H2 127.4 . . ?
N00E C2 C8 105.1(11) . . ?
C8 C2 H2 127.4 . . ?
C2 C8 C00D 126.0(11) . . ?
C13 C8 C00D 129.2(12) . . ?
C13 C8 C2 104.6(12) . . ?
N3 C13 C8 113.3(11) . . ?
N3 C13 H13 123.3 . . ?
C8 C13 H13 123.3 . . ?
N4 N2 C00P 121.0(8) . . ?
C4 N2 C00P 126.2(9) . . ?
C4 N2 N4 112.3(7) . . ?
C3 N4 N2 105.2(6) . . ?
N2 C4 H4 126.6 . . ?
N2 C4 C5 106.9(8) . . ?
C5 C4 H4 126.6 . . ?
C4 C5 C00C 126.1(9) . . ?
C4 C5 C3 105.9(9) . . ?
C3 C5 C00C 127.9(9) . . ?
N4 C3 C5 109.6(8) . . ?
N4 C3 H3 125.2 . . ?
C5 C3 H3 125.2 . . ?
O4 C7 N6 124(2) . . ?
O4 C7 C10 162(3) . 7_566 ?
N6 C7 C10 38.5(17) . 7_566 ?
C7 N6 C10 110.7(19) . . ?
C7 N6 C11 101.5(18) . . ?
C10 N6 C7 84(3) 7_566 . ?
C10 N6 C10 27(3) 7_566 . ?
C10 N6 C11 174(3) 7_566 . ?
C11 N6 C10 148(2) . . ?
N6 C10 C7 57.5(18) 7_566 7_566 ?
N6 C10 C7 149(3) . 7_566 ?
N6 C10 N6 153(3) 7_566 . ?
C10 C10 C7 167(7) 7_566 7_566 ?
C10 C10 N6 43(4) 7_566 . ?
C10 C10 N6 110(7) 7_566 7_566 ?
N6 C11 H11A 109.5 . . ?
N6 C11 H11B 109.5 . . ?
N6 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?

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
Zr01 O003 C00D O007 -12.1(7) . . . . ?
Zr01 O003 C00D C00G 162.5(6) . . . . ?
Zr01 O003 C00D C8 174.2(5) . . . . ?
Zr01 O004 C00C O006 -11.0(8) 7_556 . . . ?
Zr01 O004 C00C C00F 173.8(5) 7_556 . . . ?
Zr01 O004 C00C C5 162.0(6) 7_556 . . . ?
Zr02 O005 C00Q O005 179.3(7) . . . 2_657 ?
Zr02 O005 C00Q C00T -0.7(7) . . . . ?
Zr02 O006 C00C O004 7.6(8) 4_546 . . . ?
Zr02 O006 C00C C00F -177.5(6) 4_546 . . . ?
Zr02 O006 C00C C5 -165.8(6) 4_546 . . . ?
Zr02 O007 C00D O003 9.0(8) 5_666 . . . ?
Zr02 O007 C00D C00G -165.9(6) 5_666 . . . ?
Zr02 O007 C00D C8 -177.7(6) 5_666 . . . ?
Zr02 O00A C00S O00A 0.2(2) . . . 2_656 ?
O003 C00D C00G C00J -176.1(10) . . . . ?
O003 C00D C00G C00M 3.6(16) . . . . ?
O003 C00D C8 C2 -166.6(11) . . . . ?
O003 C00D C8 C13 7.8(15) . . . . ?
O004 C00C C00F C00I -168.1(10) . . . . ?
O004 C00C C00F C00N 10.8(15) . . . . ?
O004 C00C C5 C4 -175.6(9) . . . . ?
O004 C00C C5 C3 5.2(15) . . . . ?
O006 C00C C00F C00I 16.4(14) . . . . ?
O006 C00C C00F C00N -164.7(10) . . . . ?
O006 C00C C5 C4 -1.7(13) . . . . ?
O006 C00C C5 C3 179.1(10) . . . . ?
O007 C00D C00G C00J -0.8(14) . . . . ?
O007 C00D C00G C00M 178.9(10) . . . . ?
O007 C00D C8 C2 19.3(15) . . . . ?
O007 C00D C8 C13 -166.3(10) . . . . ?
C00C C00F C00I N00H 177.8(10) . . . . ?
C00C C00F C00N N5 -176.6(10) . . . . ?
C00C C5 C3 N4 179.6(9) . . . . ?
C00D C00G C00J N1 178.8(10) . . . . ?
C00D C00G C00M N00L -179.5(10) . . . . ?
C00D C8 C13 N3 -176.4(10) . . . . ?
N00E C00P N2 N4 -68.1(12) . . . . ?
N00E C00P N2 C4 119.6(11) . . . . ?
N00E N3 C13 C8 -0.7(12) . . . . ?
N00E C2 C8 C00D 177.9(10) . . . . ?
N00E C2 C8 C13 2.3(13) . . . . ?
C00F C00N N5 N00H -2.5(12) . . . . ?
C00G C00J N1 N00L 1.4(13) . . . . ?
C00G C00J N1 C1 172.2(10) . . . . ?
C00I C00F C00N N5 2.5(13) . . . . ?
C00I N00H C1 N1 84.7(13) . . . . ?
C00I N00H C1 C1 -38.9(17) . . . 7 ?
C00I N00H N5 C00N 1.6(11) . . . . ?
C00J C00G C00M N00L 0.3(13) . . . . ?
C00J N1 C1 N00H 119.8(12) . . . . ?
C00J N1 C1 C1 -115.1(14) . . . 7 ?
N00L N1 C1 N00H -69.9(13) . . . . ?
N00L N1 C1 C1 55.2(14) . . . 7 ?
C00M C00G C00J N1 -1.0(13) . . . . ?
C00M N00L N1 C00J -1.2(12) . . . . ?
C00M N00L N1 C1 -172.5(8) . . . . ?
C00N C00F C00I N00H -1.4(12) . . . . ?
C00P N00E N3 C13 179.2(8) . . . . ?
C00P N00E C2 C8 -179.4(10) . . . . ?
C00P C00P N2 N4 55.0(14) 7 . . . ?
C00P C00P N2 C4 -117.2(13) 7 . . . ?
C00P N2 N4 C3 -173.2(8) . . . . ?
C00P N2 C4 C5 172.9(10) . . . . ?
N1 N00L C00M C00G 0.5(12) . . . . ?
C1 N00H C00I C00F -178.9(9) . . . . ?
C1 N00H N5 C00N -179.5(8) . . . . ?
N5 N00H C00I C00F -0.1(12) . . . . ?
N5 N00H C1 N1 -94.0(12) . . . . ?
N5 N00H C1 C1 142.4(12) . . . 7 ?
N3 N00E C00P C00P 144.2(12) . . . 7 ?
N3 N00E C00P N2 -94.1(11) . . . . ?
N3 N00E C2 C8 -3.1(13) . . . . ?
C2 N00E C00P C00P -39.6(17) . . . 7 ?
C2 N00E C00P N2 82.1(13) . . . . ?
C2 N00E N3 C13 2.4(12) . . . . ?
C2 C8 C13 N3 -1.1(14) . . . . ?
N2 N4 C3 C5 -0.2(11) . . . . ?
N2 C4 C5 C00C -179.6(10) . . . . ?
N2 C4 C5 C3 -0.3(11) . . . . ?
N4 N2 C4 C5 0.1(11) . . . . ?
C4 N2 N4 C3 0.1(10) . . . . ?
C4 C5 C3 N4 0.3(12) . . . . ?
C7 N6 C10 C7 180(5) . . . 7_566 ?
C7 N6 C10 N6 0(10) . . . 7_566 ?
C7 N6 C10 C10 0(10) . . . 7_566 ?
O4 C7 N6 C10 178.6(19) . . . . ?
O4 C7 N6 C10 179(4) . . . 7_566 ?
O4 C7 N6 C11 -2(2) . . . . ?
C10 C7 N6 C10 0(4) 7_566 . . . ?
C10 C7 N6 C11 180(4) 7_566 . . . ?
C10 N6 C10 C7 180(15) 7_566 . . 7_566 ?
C10 N6 C10 N6 -0.004(1) 7_566 . . 7_566 ?
C11 N6 C10 C7 1(8) . . . 7_566 ?
C11 N6 C10 N6 -179(9) . . . 7_566 ?
C11 N6 C10 C10 -179(9) . . . 7_566 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.500 -0.742 1143.5 319.7 '8 DMF'
2 0.500 0.000 -0.689 1143.5 319.7 '8 DMF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT058_c2m                 
;
PROBLEM: Maximum Transmission Factor Missing ............          ?       
RESPONSE: XDS does not provide this data
;
_vrf_PLAT059_c2m                 
;
PROBLEM: Minimum Transmission Factor Missing ............          ?       
RESPONSE: XDS does not provide this data
;
_vrf_PLAT430_c2m                 
;
PROBLEM: Short Inter D...A Contact  N6       ..N6       .       2.48 Ang.  
RESPONSE: There is a disordered DMF molecule into two different orientations 
causing this shorter distance. It cannot be modelled as two different parts 
because the atoms are generated by symmetry operations.  
;
####################################################################### 
# 
# 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_uam-1002pdcl2rep_auto
_database_code_depnum_ccdc_archive 'CCDC 2288078'
loop_
_audit_author_name
_audit_author_address
'Christopher Sumby'
;The University of Adelaide
Australia
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_audit_creation_date             2023-07-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        UAM_1002PdCl2
_chemical_formula_moiety         'C22 H13 Cl2 N4 O8 Pd Zr1.5, 4[C7H8]'
_chemical_formula_sum            'C11 H7.50 Cl N2 O4 Pd0.50 Zr0.75'
_chemical_formula_weight         388.75
_chemical_melting_point          ?
_chemical_oxdiff_formula         C112H76N16O32Zr6Pd2Cl4
_chemical_oxdiff_usercomment     'Toluene RT'
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'
Cl Cl 0.3639 0.7018 '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'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_H-M_alt        'C m m m'
_space_group_name_Hall           '-C 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'

_cell_length_a                   33.4742(5)
_cell_length_b                   38.7659(6)
_cell_length_c                   9.98330(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12954.9(3)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    17234
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.6530
_cell_measurement_theta_min      2.6260
_shelx_estimated_absorpt_T_max   0.861
_shelx_estimated_absorpt_T_min   0.468
_exptl_absorpt_coefficient_mu    5.140
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    0.797
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             3032
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            34370
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.441
_diffrn_reflns_theta_min         2.640
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -121.00 -57.00   0.50    8.00    --  -48.77-148.00  70.00  128
  2  ω   -162.00 -80.00   0.50   10.00    --  -90.00 -40.00 -63.00  164
  3  ω    -85.00 -18.00   0.50   10.00    --  -90.00 124.00 -45.00  134
  4  ω   -121.00 -94.00   0.50    8.00    --  -48.77-125.00-120.00   54
  5  ω   -121.00 -94.00   0.50    8.00    --  -48.77-125.00-150.00   54
  6  ω    -16.00  26.00   0.50    8.00    --  -48.77  19.00 -30.00   84
  7  ω     -8.00  64.00   0.50    8.00    --   48.77 -82.00 120.00  144
  8  ω    -23.00  16.00   0.50    8.00    --   48.77 -19.00 120.00   78
  9  ω   -156.00-130.00   0.50   10.00    --  -90.00 -99.00   0.00   52
 10  ω   -156.00-109.00   0.50   10.00    --  -90.00 -57.00-180.00   94
 11  ω    -45.00 -19.00   0.50   10.00    --  -90.00  57.00-180.00   52
 12  ω   -161.00-111.00   0.50   10.00    --  -90.00 -77.00  60.00  100
 13  ω     41.00  67.00   0.50   10.00    --  105.66 -57.00 120.00   52
 14  ω     40.00  67.00   0.50   10.00    --  105.66 -57.00  60.00   54
 15  ω     34.00  67.00   0.50   10.00    --  105.66 -57.00-180.00   66
 16  ω     79.00 105.00   0.50   10.00    --  105.66 -82.00 120.00   52
 17  ω     35.00  73.00   0.50   10.00    --  105.66 -82.00 120.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0399337000
_diffrn_orient_matrix_UB_12      0.0195451000
_diffrn_orient_matrix_UB_13      0.0120245000
_diffrn_orient_matrix_UB_21      -0.0010829000
_diffrn_orient_matrix_UB_22      0.0046112000
_diffrn_orient_matrix_UB_23      -0.1532550000
_diffrn_orient_matrix_UB_31      -0.0228843000
_diffrn_orient_matrix_UB_32      -0.0342684000
_diffrn_orient_matrix_UB_33      -0.0137453000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5955
_reflns_number_total             6887
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.865
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     222
_refine_ls_number_reflns         6887
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0488
_refine_ls_restrained_S_all      1.134
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0923P)²+9.8026P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1477
_refine_ls_wR_factor_ref         0.1507
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C8B) = Uanis(C9A)
Uanis(N10B) = Uanis(N11B) = Uanis(C8B) = Uanis(C7B) = Uanis(C9B)
Uanis(C1A) = Uanis(C1B)
3. Others
 Fixed Sof: C4B(0.5) H4B(0.5) C6B(0.5) C5B(0.5) H5B(0.5) C3B(0.5) H3B(0.5)
 C1B(0.5) C2B(0.5) H2B(0.5) N11B(0.5) N10B(0.5) C9B(0.5) H9B(0.5) C7B(0.5)
 C8B(0.5) H8B(0.5) C8A(0.5) H8A(0.5) N11A(0.5) N10A(0.5) C9A(0.5) H9A(0.5)
 C7A(0.5) C1A(0.5) C2A(0.5) H2A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) C4A(0.5)
 H4A(0.5) C3A(0.5) H3A(0.5) Cl1(0.5) Cl3(0.5) Pd1(0.5)
4.a Ternary CH refined with riding coordinates:
 O08(H08), O09(H09)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4B(H4B), C5B(H5B), C3B(H3B), C2B(H2B), C9B(H9B), C8B(H8B),
 C8A(H8A), C9A(H9A), C2A(H2A), C5A(H5A), C4A(H4A), C3A(H3A)
4.c Fitted pentagon refined as free rotating group:
 N11B(N10B,C9B,C7B,C8B), C8A(N11A,N10A,C9A,C7A)
4.d Fitted hexagon refined as free rotating group:
 C4B(C6B,C5B,C3B,C1B,C2B), C1A(C2A,C5A,C6A,C4A,C3A)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.44686(2) 0.500000 0.67634(3) 0.03339(12) Uani 1 2 d S T P . .
Zr1 Zr 0.500000 0.43644(2) 0.500000 0.03915(14) Uani 1 4 d S T P . .
O04 O 0.44883(10) 0.500000 0.8923(3) 0.0607(9) Uani 1 2 d S T P . .
O05 O 0.42295(8) 0.44829(7) 0.2600(2) 0.0674(7) Uani 1 1 d . . . . .
O06 O 0.45980(9) 0.40874(6) 0.3654(3) 0.0693(7) Uani 1 1 d . . . . .
O07 O 0.38223(9) 0.500000 0.6147(4) 0.0715(10) Uani 1 2 d S T P . .
O08 O 0.500000 0.53012(9) 0.6808(5) 0.0826(14) Uani 1 2 d S T P . .
H08 H 0.500000 0.544902 0.762858 0.124 Uiso 1 2 calc R U P . .
O09 O 0.44907(14) 0.46925(11) 0.500000 0.0793(13) Uani 1 2 d S T P . .
H09 H 0.424846 0.454149 0.499999 0.119 Uiso 1 2 calc R U P . .
C1 C 0.42987(14) 0.41813(11) 0.2977(4) 0.0685(11) Uani 1 1 d . . . . .
C2 C 0.3664(2) 0.500000 0.500000 0.087(3) Uani 1 4 d S T P . .
H2 H 0.338007 0.500000 0.499996 0.104 Uiso 1 4 calc R U P . .
C4 C 0.250000 0.250000 0.0803(7) 0.096(2) Uani 1 2 d S T P . .
C3 C 0.4391(3) 0.500000 1.000000 0.113(4) Uani 1 4 d S T P . .
H3 H 0.410676 0.500000 1.000000 0.135 Uiso 1 4 calc R U P . .
C4B C 0.3463(2) 0.3620(2) 0.1761(10) 0.107(5) Uani 0.5 1 d G . P A 1
H4B H 0.321473 0.364900 0.131653 0.129 Uiso 0.5 1 calc R U P A 1
C6B C 0.3593(3) 0.32908(17) 0.2107(11) 0.123(6) Uani 0.5 1 d G . P A 1
C5B C 0.3957(3) 0.32478(15) 0.2758(12) 0.157(7) Uani 0.5 1 d G . P A 1
H5B H 0.404569 0.302311 0.299339 0.188 Uiso 0.5 1 calc R U P A 1
C3B C 0.4191(3) 0.35335(19) 0.3063(14) 0.111(5) Uani 0.5 1 d G . P A 1
H3B H 0.443914 0.350409 0.350838 0.134 Uiso 0.5 1 calc R U P A 1
C1B C 0.4061(3) 0.38623(16) 0.2718(13) 0.079(3) Uani 0.5 1 d G . P A 1
C2B C 0.3697(3) 0.39053(16) 0.2067(11) 0.096(4) Uani 0.5 1 d G . P A 1
H2B H 0.360818 0.412999 0.183153 0.116 Uiso 0.5 1 calc R U P A 1
N11B N 0.28415(17) 0.26264(18) 0.1296(9) 0.1102(15) Uani 0.5 1 d G . P A 1
N10B N 0.3203(2) 0.24431(14) 0.1085(7) 0.1102(15) Uani 0.5 1 d G . P A 1
C9B C 0.35257(17) 0.26695(18) 0.1371(8) 0.1102(15) Uani 0.5 1 d G . P A 1
H9B H 0.380171 0.261443 0.131222 0.132 Uiso 0.5 1 calc R U P A 1
C7B C 0.3363(2) 0.29927(15) 0.1759(9) 0.1102(15) Uani 0.5 1 d G . P A 1
C8B C 0.2940(2) 0.29660(17) 0.1713(10) 0.1102(15) Uani 0.5 1 d G . P A 1
H8B H 0.275581 0.314416 0.192434 0.132 Uiso 0.5 1 calc R U P A 1
C8A C 0.2596(2) 0.33989(14) 0.1444(10) 0.136(5) Uani 0.5 1 d G . P A 2
H8A H 0.250342 0.363062 0.144009 0.164 Uiso 0.5 1 calc R U P A 2
N11A N 0.23641(18) 0.31022(19) 0.1138(9) 0.123(4) Uani 0.5 1 d G . P A 2
N10A N 0.2615(2) 0.28083(14) 0.1261(7) 0.099(3) Uani 0.5 1 d G . P A 2
C9A C 0.3001(2) 0.29233(18) 0.1643(10) 0.1102(15) Uani 0.5 1 d G . P A 2
H9A H 0.322743 0.278100 0.179592 0.132 Uiso 0.5 1 calc R U P A 2
C7A C 0.2989(2) 0.32883(18) 0.1756(9) 0.108(4) Uani 0.5 1 d G . P A 2
C1A C 0.3948(2) 0.3962(2) 0.2610(13) 0.079(3) Uani 0.5 1 d G . P A 2
C2A C 0.3613(3) 0.40825(18) 0.1939(11) 0.096(4) Uani 0.5 1 d G . P A 2
H2A H 0.359882 0.431685 0.166499 0.115 Uiso 0.5 1 calc R U P A 2
C5A C 0.3297(2) 0.3860(2) 0.1669(10) 0.128(6) Uani 0.5 1 d G . P A 2
H5A H 0.306731 0.394270 0.120991 0.153 Uiso 0.5 1 calc R U P A 2
C6A C 0.3317(3) 0.3517(2) 0.2070(9) 0.102(4) Uani 0.5 1 d G . P A 2
C4A C 0.3653(3) 0.33966(16) 0.2741(11) 0.122(5) Uani 0.5 1 d G . P A 2
H4A H 0.366664 0.316224 0.301517 0.147 Uiso 0.5 1 calc R U P A 2
C3A C 0.3969(2) 0.3619(2) 0.3011(13) 0.110(5) Uani 0.5 1 d G . P A 2
H3A H 0.419815 0.353638 0.347027 0.132 Uiso 0.5 1 calc R U P A 2
Cl1 Cl 0.31218(19) 0.14591(15) 0.0804(11) 0.356(9) Uani 0.5 1 d . . P A .
Cl3 Cl 0.37682(18) 0.20791(19) 0.0845(10) 0.338(8) Uani 0.5 1 d . . P A .
Pd1 Pd 0.31813(3) 0.19712(3) 0.0216(5) 0.2356(15) Uani 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
Zr Zr 3.5577(6) 2_665 ?
Zr Zr 3.5208(6) 10_556 ?
Zr Zr1 3.5119(4) . ?
Zr Zr1 3.5120(4) 9_666 ?
Zr O04 2.157(3) . ?
Zr O05 2.250(2) 4_566 ?
Zr O05 2.250(2) 10_556 ?
Zr O07 2.249(3) . ?
Zr O08 2.128(2) 2_665 ?
Zr O08 2.128(2) . ?
Zr O09 2.127(2) . ?
Zr O09 2.127(2) 11_565 ?
Zr1 O06 2.184(2) . ?
Zr1 O06 2.184(2) 12_655 ?
Zr1 O06 2.184(2) 10_556 ?
Zr1 O06 2.184(2) 3_656 ?
Zr1 O08 2.222(4) 2_665 ?
Zr1 O08 2.222(4) 9_666 ?
Zr1 O09 2.127(4) 3_656 ?
Zr1 O09 2.127(4) . ?
O04 C3 1.124(4) . ?
O05 C1 1.250(5) . ?
O06 C1 1.262(5) . ?
O07 C2 1.262(5) . ?
O08 H08 1.0000 . ?
O09 H09 1.0000 . ?
C1 C1B 1.494(5) . ?
C1 C1A 1.494(6) . ?
C2 H2 0.9500 . ?
C4 C4 1.603(13) 13 ?
C4 N11B 1.338(5) 6 ?
C4 N11B 1.338(5) . ?
C4 N10A 1.336(5) . ?
C4 N10A 1.336(8) 6 ?
C3 H3 0.9500 . ?
C4B H4B 0.9500 . ?
C4B C6B 1.3900 . ?
C4B C2B 1.3900 . ?
C6B C5B 1.3900 . ?
C6B C7B 1.432(6) . ?
C5B H5B 0.9500 . ?
C5B C3B 1.3900 . ?
C3B H3B 0.9500 . ?
C3B C1B 1.3900 . ?
C1B C2B 1.3900 . ?
C2B H2B 0.9500 . ?
N11B N10B 1.4200 . ?
N11B C8B 1.4200 . ?
N10B C9B 1.4200 . ?
N10B Pd1 2.244(6) 10 ?
N10B Pd1 2.026(5) . ?
C9B H9B 0.9500 . ?
C9B C7B 1.4200 . ?
C7B C8B 1.4200 . ?
C8B H8B 0.9500 . ?
C8A H8A 0.9500 . ?
C8A N11A 1.4200 . ?
C8A C7A 1.4200 . ?
N11A N10A 1.4200 . ?
N11A Pd1 2.289(7) 13 ?
N11A Pd1 2.064(6) 6 ?
N10A C9A 1.4200 . ?
C9A H9A 0.9500 . ?
C9A C7A 1.4200 . ?
C7A C6A 1.446(6) . ?
C1A C2A 1.3900 . ?
C1A C3A 1.3900 . ?
C2A H2A 0.9500 . ?
C2A C5A 1.3900 . ?
C5A H5A 0.9500 . ?
C5A C6A 1.3900 . ?
C6A C4A 1.3900 . ?
C4A H4A 0.9500 . ?
C4A C3A 1.3900 . ?
C3A H3A 0.9500 . ?
Cl1 Cl1 1.61(2) 10 ?
Cl1 Pd1 2.080(5) . ?
Cl1 Pd1 2.240(6) 10 ?
Cl3 Cl3 1.69(2) 10 ?
Cl3 Pd1 2.104(5) . ?
Cl3 Pd1 2.271(6) 10 ?
Pd1 Pd1 0.431(9) 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
Zr Zr Zr 90.0 10_556 2_665 ?
Zr1 Zr Zr 59.567(5) . 2_665 ?
Zr1 Zr Zr 59.916(5) . 10_556 ?
Zr1 Zr Zr 59.568(5) 9_666 2_665 ?
Zr1 Zr Zr 59.916(5) 9_666 10_556 ?
Zr1 Zr Zr1 89.103(12) . 9_666 ?
O04 Zr Zr 178.25(9) . 10_556 ?
O04 Zr Zr 88.25(9) . 2_665 ?
O04 Zr Zr1 119.05(5) . 9_666 ?
O04 Zr Zr1 119.05(5) . . ?
O04 Zr O05 74.25(7) . 4_566 ?
O04 Zr O05 74.25(7) . 10_556 ?
O04 Zr O07 107.62(13) . . ?
O05 Zr Zr 110.83(7) 4_566 2_665 ?
O05 Zr Zr 110.83(7) 10_556 2_665 ?
O05 Zr Zr 106.41(7) 4_566 10_556 ?
O05 Zr Zr 106.41(7) 10_556 10_556 ?
O05 Zr Zr1 161.22(7) 10_556 9_666 ?
O05 Zr Zr1 72.34(7) 4_566 9_666 ?
O05 Zr Zr1 72.34(7) 10_556 . ?
O05 Zr Zr1 161.22(7) 4_566 . ?
O05 Zr O05 125.98(14) 10_556 4_566 ?
O07 Zr Zr 164.13(9) . 2_665 ?
O07 Zr Zr 74.13(9) . 10_556 ?
O07 Zr Zr1 110.50(6) . . ?
O07 Zr Zr1 110.50(6) . 9_666 ?
O07 Zr O05 74.64(8) . 10_556 ?
O07 Zr O05 74.64(8) . 4_566 ?
O08 Zr Zr 33.30(8) 2_665 2_665 ?
O08 Zr Zr 33.30(8) . 2_665 ?
O08 Zr Zr 91.19(13) . 10_556 ?
O08 Zr Zr 91.19(13) 2_665 10_556 ?
O08 Zr Zr1 37.08(11) 2_665 . ?
O08 Zr Zr1 88.39(11) . . ?
O08 Zr Zr1 88.39(11) 2_665 9_666 ?
O08 Zr Zr1 37.08(11) . 9_666 ?
O08 Zr O04 87.35(15) 2_665 . ?
O08 Zr O04 87.35(15) . . ?
O08 Zr O05 141.28(11) . 10_556 ?
O08 Zr O05 141.28(11) 2_665 4_566 ?
O08 Zr O05 78.62(12) . 4_566 ?
O08 Zr O05 78.61(12) 2_665 10_556 ?
O08 Zr O07 144.06(9) 2_665 . ?
O08 Zr O07 144.06(9) . . ?
O08 Zr O08 66.55(16) . 2_665 ?
O09 Zr Zr 34.15(9) 11_565 10_556 ?
O09 Zr Zr 34.15(9) . 10_556 ?
O09 Zr Zr 88.01(13) . 2_665 ?
O09 Zr Zr 88.01(13) 11_565 2_665 ?
O09 Zr Zr1 34.36(10) . . ?
O09 Zr Zr1 34.36(10) 11_565 9_666 ?
O09 Zr Zr1 87.75(12) 11_565 . ?
O09 Zr Zr1 87.75(12) . 9_666 ?
O09 Zr O04 145.70(9) 11_565 . ?
O09 Zr O04 145.70(9) . . ?
O09 Zr O05 138.18(10) 11_565 10_556 ?
O09 Zr O05 75.34(13) 11_565 4_566 ?
O09 Zr O05 138.19(10) . 4_566 ?
O09 Zr O05 75.34(13) . 10_556 ?
O09 Zr O07 78.88(14) 11_565 . ?
O09 Zr O07 78.88(14) . . ?
O09 Zr O08 107.20(19) 11_565 2_665 ?
O09 Zr O08 107.19(19) . . ?
O09 Zr O08 71.39(15) 11_565 . ?
O09 Zr O08 71.38(15) . 2_665 ?
O09 Zr O09 68.16(19) 11_565 . ?
Zr Zr1 Zr 60.864(10) 2_665 . ?
Zr Zr1 Zr 60.864(10) 9_666 10_556 ?
Zr Zr1 Zr 90.896(12) 2_665 10_556 ?
Zr Zr1 Zr 90.897(12) 9_666 . ?
Zr Zr1 Zr 60.167(10) 2_665 9_666 ?
Zr Zr1 Zr 60.167(10) 10_556 . ?
O06 Zr1 Zr 74.01(7) 12_655 9_666 ?
O06 Zr1 Zr 109.95(8) . . ?
O06 Zr1 Zr 74.01(7) . 10_556 ?
O06 Zr1 Zr 164.91(7) 3_656 10_556 ?
O06 Zr1 Zr 74.01(7) 10_556 . ?
O06 Zr1 Zr 109.95(8) 10_556 10_556 ?
O06 Zr1 Zr 109.95(8) 12_655 2_665 ?
O06 Zr1 Zr 164.90(7) . 2_665 ?
O06 Zr1 Zr 110.41(7) 3_656 . ?
O06 Zr1 Zr 110.41(7) 12_655 10_556 ?
O06 Zr1 Zr 110.41(7) . 9_666 ?
O06 Zr1 Zr 74.01(7) 3_656 2_665 ?
O06 Zr1 Zr 110.41(7) 10_556 2_665 ?
O06 Zr1 Zr 109.95(8) 3_656 9_666 ?
O06 Zr1 Zr 164.91(7) 12_655 . ?
O06 Zr1 Zr 164.91(7) 10_556 9_666 ?
O06 Zr1 O06 121.09(15) . 3_656 ?
O06 Zr1 O06 75.93(15) 3_656 12_655 ?
O06 Zr1 O06 75.93(15) . 10_556 ?
O06 Zr1 O06 121.08(15) 12_655 10_556 ?
O06 Zr1 O06 76.08(16) . 12_655 ?
O06 Zr1 O06 76.08(16) 3_656 10_556 ?
O06 Zr1 O08 141.86(8) 3_656 9_666 ?
O06 Zr1 O08 141.86(8) 12_655 2_665 ?
O06 Zr1 O08 141.86(8) . 2_665 ?
O06 Zr1 O08 77.71(12) 3_656 2_665 ?
O06 Zr1 O08 141.86(8) 10_556 9_666 ?
O06 Zr1 O08 77.71(12) 10_556 2_665 ?
O06 Zr1 O08 77.71(12) 12_655 9_666 ?
O06 Zr1 O08 77.71(12) . 9_666 ?
O08 Zr1 Zr 35.28(6) 2_665 . ?
O08 Zr1 Zr 35.28(6) 9_666 10_556 ?
O08 Zr1 Zr 89.88(11) 2_665 10_556 ?
O08 Zr1 Zr 89.88(11) 9_666 2_665 ?
O08 Zr1 Zr 35.28(6) 2_665 2_665 ?
O08 Zr1 Zr 35.28(6) 9_666 9_666 ?
O08 Zr1 Zr 89.88(11) 9_666 . ?
O08 Zr1 Zr 89.88(11) 2_665 9_666 ?
O08 Zr1 O08 108.6(2) 2_665 9_666 ?
O09 Zr1 Zr 89.23(12) . 9_666 ?
O09 Zr1 Zr 89.23(12) . 2_665 ?
O09 Zr1 Zr 89.23(12) 3_656 10_556 ?
O09 Zr1 Zr 34.36(6) 3_656 9_666 ?
O09 Zr1 Zr 34.36(6) 3_656 2_665 ?
O09 Zr1 Zr 34.36(6) . . ?
O09 Zr1 Zr 34.36(6) . 10_556 ?
O09 Zr1 Zr 89.23(12) 3_656 . ?
O09 Zr1 O06 78.47(13) . . ?
O09 Zr1 O06 142.00(7) 3_656 10_556 ?
O09 Zr1 O06 78.47(13) 3_656 3_656 ?
O09 Zr1 O06 142.00(7) 3_656 . ?
O09 Zr1 O06 78.47(13) 3_656 12_655 ?
O09 Zr1 O06 142.00(7) . 3_656 ?
O09 Zr1 O06 78.47(13) . 10_556 ?
O09 Zr1 O06 142.00(7) . 12_655 ?
O09 Zr1 O08 69.59(9) . 2_665 ?
O09 Zr1 O08 69.59(9) 3_656 2_665 ?
O09 Zr1 O08 69.59(9) . 9_666 ?
O09 Zr1 O08 69.59(9) 3_656 9_666 ?
O09 Zr1 O09 106.6(3) . 3_656 ?
C3 O04 Zr 161.3(6) . . ?
C1 O05 Zr 133.0(2) . 10_556 ?
C1 O06 Zr1 132.6(2) . . ?
C2 O07 Zr 130.7(4) . . ?
Zr O08 Zr 113.40(17) 2_665 . ?
Zr O08 Zr1 107.65(15) 2_665 9_666 ?
Zr O08 Zr1 107.65(15) . 9_666 ?
Zr O08 H08 109.4 2_665 . ?
Zr O08 H08 109.4 . . ?
Zr1 O08 H08 109.4 9_666 . ?
Zr O09 Zr 111.69(18) 10_556 . ?
Zr O09 H09 107.4 . . ?
Zr O09 H09 107.4 10_556 . ?
Zr1 O09 Zr 111.28(14) . 10_556 ?
Zr1 O09 Zr 111.28(14) . . ?
Zr1 O09 H09 107.4 . . ?
O05 C1 O06 125.3(3) . . ?
O05 C1 C1B 128.6(5) . . ?
O05 C1 C1A 108.3(5) . . ?
O06 C1 C1B 106.1(5) . . ?
O06 C1 C1A 126.2(5) . . ?
O07 C2 O07 130.3(7) . 10_556 ?
O07 C2 H2 114.8 . . ?
O07 C2 H2 114.8 10_556 . ?
N11B C4 C4 111.6(5) . 13 ?
N11B C4 C4 111.6(5) 6 13 ?
N11B C4 N11B 136.8(9) 6 . ?
O04 C3 O04 146.2(12) 10_557 . ?
O04 C3 H3 106.9 10_557 . ?
O04 C3 H3 106.9 . . ?
C6B C4B H4B 120.0 . . ?
C6B C4B C2B 120.0 . . ?
C2B C4B H4B 120.0 . . ?
C4B C6B C5B 120.0 . . ?
C4B C6B C7B 120.8(7) . . ?
C5B C6B C7B 119.2(7) . . ?
C6B C5B H5B 120.0 . . ?
C6B C5B C3B 120.0 . . ?
C3B C5B H5B 120.0 . . ?
C5B C3B H3B 120.0 . . ?
C5B C3B C1B 120.0 . . ?
C1B C3B H3B 120.0 . . ?
C3B C1B C1 123.3(5) . . ?
C2B C1B C1 116.7(5) . . ?
C2B C1B C3B 120.0 . . ?
C4B C2B H2B 120.0 . . ?
C1B C2B C4B 120.0 . . ?
C1B C2B H2B 120.0 . . ?
C4 N11B N10B 119.4(5) . . ?
C4 N11B C8B 130.3(5) . . ?
N10B N11B C8B 108.0 . . ?
N11B N10B C9B 108.0 . . ?
N11B N10B Pd1 119.0(4) . . ?
N11B N10B Pd1 117.8(4) . 10 ?
C9B N10B Pd1 132.2(4) . . ?
C9B N10B Pd1 130.2(4) . 10 ?
Pd1 N10B Pd1 10.0(2) . 10 ?
N10B C9B H9B 126.0 . . ?
C7B C9B N10B 108.0 . . ?
C7B C9B H9B 126.0 . . ?
C9B C7B C6B 124.9(7) . . ?
C9B C7B C8B 108.0 . . ?
C8B C7B C6B 127.1(7) . . ?
N11B C8B C7B 108.0 . . ?
N11B C8B H8B 126.0 . . ?
C7B C8B H8B 126.0 . . ?
N11A C8A H8A 126.0 . . ?
N11A C8A C7A 108.0 . . ?
C7A C8A H8A 126.0 . . ?
C8A N11A N10A 108.0 . . ?
Pd1 N11A Pd1 9.7(2) 6 13 ?
C4 N10A N11A 121.2(6) . . ?
C4 N10A C9A 129.4(6) . . ?
C9A N10A N11A 108.0 . . ?
N10A C9A H9A 126.0 . . ?
C7A C9A N10A 108.0 . . ?
C7A C9A H9A 126.0 . . ?
C8A C7A C6A 124.5(7) . . ?
C9A C7A C8A 108.0 . . ?
C9A C7A C6A 127.5(7) . . ?
C2A C1A C1 124.1(5) . . ?
C2A C1A C3A 120.0 . . ?
C3A C1A C1 115.8(5) . . ?
C1A C2A H2A 120.0 . . ?
C1A C2A C5A 120.0 . . ?
C5A C2A H2A 120.0 . . ?
C2A C5A H5A 120.0 . . ?
C2A C5A C6A 120.0 . . ?
C6A C5A H5A 120.0 . . ?
C5A C6A C7A 119.2(7) . . ?
C4A C6A C7A 120.8(7) . . ?
C4A C6A C5A 120.0 . . ?
C6A C4A H4A 120.0 . . ?
C6A C4A C3A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C1A C3A H3A 120.0 . . ?
C4A C3A C1A 120.0 . . ?
C4A C3A H3A 120.0 . . ?
Cl1 Cl1 Pd1 63.0(3) 10 10 ?
Cl1 Cl1 Pd1 73.6(3) 10 . ?
Pd1 Cl1 Pd1 10.6(2) . 10 ?
Cl3 Cl3 Pd1 72.6(3) 10 . ?
Cl3 Cl3 Pd1 62.2(3) 10 10 ?
Pd1 Cl3 Pd1 10.4(2) . 10 ?
N10B Pd1 N10B 60.7(6) . 10 ?
N10B Pd1 N11A 88.0(4) . 6 ?
N10B Pd1 N11A 77.6(7) 10 13 ?
N10B Pd1 N11A 113.2(4) . 13 ?
N10B Pd1 Cl1 138.1(4) . . ?
N10B Pd1 Cl1 176.5(4) . 10 ?
N10B Pd1 Cl3 70.1(3) . . ?
N10B Pd1 Cl3 90.1(3) . 10 ?
N10B Pd1 Cl3 63.4(5) 10 10 ?
N11A Pd1 Cl1 70.0(3) 6 . ?
N11A Pd1 Cl3 136.1(8) 6 . ?
Cl1 Pd1 N10B 160.8(5) . 10 ?
Cl1 Pd1 N10B 117.5(5) 10 10 ?
Cl1 Pd1 N11A 63.3(4) 10 13 ?
Cl1 Pd1 N11A 88.4(6) . 13 ?
Cl1 Pd1 Cl1 43.4(6) . 10 ?
Cl1 Pd1 Cl3 113.0(3) . 10 ?
Cl1 Pd1 Cl3 101.2(3) . . ?
Cl1 Pd1 Cl3 91.6(2) 10 10 ?
Cl3 Pd1 N10B 88.8(4) . 10 ?
Cl3 Pd1 N11A 161.0(8) . 13 ?
Cl3 Pd1 N11A 116.0(8) 10 13 ?
Cl3 Pd1 Cl1 113.2(3) . 10 ?
Cl3 Pd1 Cl3 45.1(5) . 10 ?
Pd1 Pd1 N10B 115.3(2) 10 . ?
Pd1 Pd1 N10B 54.7(4) 10 10 ?
Pd1 Pd1 N11A 53.8(7) 10 13 ?
Pd1 Pd1 N11A 116.5(7) 10 6 ?
Pd1 Pd1 Cl1 63.0(3) 10 10 ?
Pd1 Pd1 Cl1 106.4(3) 10 . ?
Pd1 Pd1 Cl3 107.4(3) 10 . ?
Pd1 Pd1 Cl3 62.2(3) 10 10 ?

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
Zr O04 C3 O04 180.000(2) . . . 10_557 ?
Zr O05 C1 O06 -16.7(7) 10_556 . . . ?
Zr O05 C1 C1B 164.5(8) 10_556 . . . ?
Zr O05 C1 C1A 157.6(6) 10_556 . . . ?
Zr O07 C2 O07 0.000(1) . . . 10_556 ?
Zr1 O06 C1 O05 23.3(7) . . . . ?
Zr1 O06 C1 C1B -157.7(6) . . . . ?
Zr1 O06 C1 C1A -150.0(7) . . . . ?
O05 C1 C1B C3B 172.5(6) . . . . ?
O05 C1 C1B C2B -5.8(12) . . . . ?
O05 C1 C1A C2A 1.2(10) . . . . ?
O05 C1 C1A C3A -177.3(5) . . . . ?
O06 C1 C1B C3B -6.4(9) . . . . ?
O06 C1 C1B C2B 175.3(6) . . . . ?
O06 C1 C1A C2A 175.5(6) . . . . ?
O06 C1 C1A C3A -3.1(11) . . . . ?
C1 C1B C2B C4B 178.4(11) . . . . ?
C1 C1A C2A C5A -178.5(12) . . . . ?
C1 C1A C3A C4A 178.6(11) . . . . ?
C4 C4 N11B N10B -66.0(6) 13 . . . ?
C4 C4 N11B C8B 94.4(6) 13 . . . ?
C4 C4 N10A N11A 70.8(6) 13 . . . ?
C4 C4 N10A C9A -94.0(6) 13 . . . ?
C4 N11B N10B C9B 164.4(8) . . . . ?
C4 N11B N10B Pd1 4.8(8) . . . 10 ?
C4 N11B N10B Pd1 -6.5(8) . . . . ?
C4 N11B C8B C7B -162.1(9) . . . . ?
C4 N10A C9A C7A 166.4(8) . . . . ?
C4B C6B C5B C3B 0.0 . . . . ?
C4B C6B C7B C9B 143.8(7) . . . . ?
C4B C6B C7B C8B -35.0(12) . . . . ?
C6B C4B C2B C1B 0.0 . . . . ?
C6B C5B C3B C1B 0.0 . . . . ?
C6B C7B C8B N11B 178.9(10) . . . . ?
C5B C6B C7B C9B -34.1(11) . . . . ?
C5B C6B C7B C8B 147.2(7) . . . . ?
C5B C3B C1B C1 -178.3(12) . . . . ?
C5B C3B C1B C2B 0.0 . . . . ?
C3B C1B C2B C4B 0.0 . . . . ?
C2B C4B C6B C5B 0.0 . . . . ?
C2B C4B C6B C7B -177.8(11) . . . . ?
N11B C4 N11B N10B 114.0(6) 6 . . . ?
N11B C4 N11B C8B -85.6(6) 6 . . . ?
N11B N10B C9B C7B 0.0 . . . . ?
N10B N11B C8B C7B 0.0 . . . . ?
N10B C9B C7B C6B -178.9(9) . . . . ?
N10B C9B C7B C8B 0.0 . . . . ?
C9B C7B C8B N11B 0.0 . . . . ?
C7B C6B C5B C3B 177.9(11) . . . . ?
C8B N11B N10B C9B 0.0 . . . . ?
C8B N11B N10B Pd1 -170.9(6) . . . . ?
C8B N11B N10B Pd1 -159.6(5) . . . 10 ?
C8A N11A N10A C4 -167.7(8) . . . . ?
C8A N11A N10A C9A 0.0 . . . . ?
C8A C7A C6A C5A -20.6(11) . . . . ?
C8A C7A C6A C4A 160.6(7) . . . . ?
N11A C8A C7A C9A 0.0 . . . . ?
N11A C8A C7A C6A 177.5(9) . . . . ?
N11A N10A C9A C7A 0.0 . . . . ?
N10A C4 N10A N11A -109.2(12) 6 . . . ?
N10A C4 N10A C9A 86.0(10) 6 . . . ?
N10A C9A C7A C8A 0.0 . . . . ?
N10A C9A C7A C6A -177.4(9) . . . . ?
C9A C7A C6A C5A 156.4(7) . . . . ?
C9A C7A C6A C4A -22.4(11) . . . . ?
C7A C8A N11A N10A 0.0 . . . . ?
C7A C8A N11A Pd1 -164.6(8) . . . 6 ?
C7A C8A N11A Pd1 -151.7(8) . . . 13 ?
C7A C6A C4A C3A 178.7(10) . . . . ?
C1A C2A C5A C6A 0.0 . . . . ?
C2A C1A C3A C4A 0.0 . . . . ?
C2A C5A C6A C7A -178.8(10) . . . . ?
C2A C5A C6A C4A 0.0 . . . . ?
C5A C6A C4A C3A 0.0 . . . . ?
C6A C4A C3A C1A 0.0 . . . . ?
C3A C1A C2A C5A 0.0 . . . . ?
Pd1 N10B C9B C7B 169.3(7) . . . . ?
Pd1 N10B C9B C7B 156.3(7) 10 . . . ?
Pd1 N11A N10A C4 -10.8(8) 13 . . . ?
Pd1 N11A N10A C4 -0.2(9) 6 . . . ?
Pd1 N11A N10A C9A 156.9(6) 13 . . . ?
Pd1 N11A N10A C9A 167.6(7) 6 . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 1555 electrons were 
found in a volume of 8326Å³ in 1 void per unit cell. 
This is consistent with the presence of 
1[C7H8] per Asymmetric Unit 
which account for 1600 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.450 -0.884 -0.575 8325.6 1555.4 '32 toluene'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.381
_oxdiff_exptl_absorpt_empirical_full_min 0.787
####################################################################### 
# 
# 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_cmmm
_database_code_depnum_ccdc_archive 'CCDC 2288079'
loop_
_audit_author_name
_audit_author_address
'Christopher Sumby'
;The University of Adelaide
Australia
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_audit_creation_date             2023-07-13
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10.5 H7 N2 O4 Zr0.75'
_chemical_formula_sum            'C10.50 H7 N2 O4 Zr0.75'
_chemical_formula_weight         293.60
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_H-M_alt        'C m m m'
_space_group_name_Hall           '-C 2 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'

_cell_length_a                   33.273(7)
_cell_length_b                   35.780(7)
_cell_length_c                   12.220(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14548(5)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    8298
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.682
_cell_measurement_theta_min      0.836
_shelx_estimated_absorpt_T_max   0.994
_shelx_estimated_absorpt_T_min   0.955
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.536
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2336
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.027
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1189
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.820
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            86300
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.820
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.682
_diffrn_reflns_theta_min         0.836
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '13.3 (Dectris Eiger detectors)'
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.820
_diffrn_measurement_detector_type 'Dectris Eiger2 9M'
_diffrn_measurement_device_type  
;
N. P. Cowieson, D. Aragao, M. Clift, D. J. Ericsson, C. Gee, 
S. J. Harrop, N. Mudie, S. Panjikar, J. R. Price, A. Riboldi-
Tunnicliffe, R. Williamson and T. Caradoc-Davies, MX1: a 
bending-magnet crystallography beamline serving both chemical 
and macromolecular crystallography communities at the 
Australian Synchrotron, J. Synchrotron Rad. (2015). 22, 187-190.
;
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2327
_reflns_number_total             8298
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'AS QEGUI'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         8298
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1894
_refine_ls_R_factor_gt           0.1144
_refine_ls_restrained_S_all      0.936
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2956
_refine_ls_wR_factor_ref         0.3759
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: C8(0.5) H8(0.5) N1(0.5) N00C(0.5) C00H(0.5) H00H(0.5) C00I(0.5)
 C2(0.5) N8(0.5) C14(0.5) H14(0.5) C24(0.5) C33(0.5) H33(0.5) N36(0.5) C7(0.5)
 H7(0.5) C00G(0.5) C00D(0.5) H00D(0.5) C00F(0.5) H00F(0.5) C00B(0.5) C20(0.5)
 H20(0.5) C26(0.5) C1(0.5) H1(0.5) C22(0.5) H22(0.5) C13(0.5) C5(0.5) H5(0.5)
 C00E(0.5) H00E(0.5)
3.a Ternary CH refined with riding coordinates:
 O003(H003), O009(H009)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C00H(H00H), C14(H14), C33(H33), C7(H7), C00D(H00D), C00F(H00F),
 C20(H20), C1(H1), C22(H22), C5(H5), C00E(H00E)
3.c Fitted pentagon refined as free rotating group:
 C8(N1,N00C,C00H,C00I)
3.d Fitted hexagon refined as free rotating group:
 C7(C00G,C00D,C00F,C00B,C20), C26(C1,C22,C13,C5,C00E)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr01 Zr 0.42542(5) 0.500000 0.500000 0.1713(7) Uani 1 4 d S T P . .
Zr02 Zr 0.500000 0.54919(2) 0.64276(10) 0.1841(7) Uani 1 2 d S T P . .
O003 O 0.4633(2) 0.500000 0.6365(6) 0.193(3) Uani 1 2 d S T P . .
H003 H 0.445923 0.500000 0.703211 0.289 Uiso 1 2 calc R U P . .
O004 O 0.39170(16) 0.46311(13) 0.3945(5) 0.1824(19) Uani 1 1 d . . . . .
O005 O 0.4384(2) 0.43119(15) 0.2972(6) 0.212(3) Uani 1 1 d . . . . .
O006 O 0.500000 0.6107(2) 0.6243(9) 0.254(4) Uani 1 2 d S T P . .
C007 C 0.4027(4) 0.4386(3) 0.3316(8) 0.191(3) Uani 1 1 d . . . . .
O008 O 0.500000 0.5431(3) 0.8226(7) 0.243(4) Uani 1 2 d S T P . .
O009 O 0.4629(3) 0.5501(2) 0.500000 0.248(4) Uani 1 2 d S T P . .
H009 H 0.445664 0.572949 0.499998 0.372 Uiso 1 2 calc R U P . .
C8 C 0.2310(6) 0.3474(4) 0.1404(15) 0.253(9) Uani 0.5 1 d G . P A 1
H8 H 0.216573 0.369601 0.156609 0.303 Uiso 0.5 1 calc R U P A 1
N1 N 0.2150(3) 0.3148(5) 0.0902(12) 0.243(7) Uani 0.5 1 d G . P A 1
N00C N 0.2465(5) 0.2882(4) 0.0810(13) 0.224(11) Uani 0.5 1 d G . P A 1
C00H C 0.2819(4) 0.3043(6) 0.1256(18) 0.219(13) Uani 0.5 1 d G . P A 1
H00H H 0.307506 0.292612 0.130021 0.262 Uiso 0.5 1 calc R U P A 1
C00I C 0.2723(5) 0.3409(5) 0.1623(16) 0.238(14) Uani 0.5 1 d G . P A 1
C2 C 0.2330(4) 0.2553(6) 0.0356(9) 0.166(9) Uani 0.5 1 d . . P . .
N8 N 0.2429(5) 0.2882(5) 0.1614(16) 0.199(7) Uani 0.5 1 d . . P A 2
C14 C 0.2525(9) 0.3215(7) 0.2216(17) 0.238(10) Uani 0.5 1 d . . P A 2
H14 H 0.235914 0.336519 0.267113 0.285 Uiso 0.5 1 calc R U P A 2
C24 C 0.2962(6) 0.3259(4) 0.1924(14) 0.157(6) Uani 0.5 1 d . . P A 2
C33 C 0.3069(5) 0.2952(5) 0.1281(19) 0.170(6) Uani 0.5 1 d . . P A 2
H33 H 0.333246 0.291135 0.100793 0.204 Uiso 0.5 1 calc R U P A 2
N36 N 0.2751(5) 0.2715(5) 0.1083(14) 0.190(6) Uani 0.5 1 d . . P A 2
C7 C 0.2963(4) 0.3938(4) 0.2806(14) 0.193(9) Uani 0.5 1 d G . P A 1
H7 H 0.269479 0.397233 0.305440 0.232 Uiso 0.5 1 calc R U P A 1
C00G C 0.3054(4) 0.3646(4) 0.2099(15) 0.170(8) Uani 0.5 1 d G . P A 1
C00D C 0.3446(4) 0.3596(4) 0.1735(13) 0.180(9) Uani 0.5 1 d G . P A 1
H00D H 0.350833 0.339644 0.125154 0.216 Uiso 0.5 1 calc R U P A 1
C00F C 0.3747(4) 0.3838(4) 0.2079(13) 0.178(8) Uani 0.5 1 d G . P A 1
H00F H 0.401529 0.380431 0.183053 0.214 Uiso 0.5 1 calc R U P A 1
C00B C 0.3656(4) 0.4131(3) 0.2786(14) 0.139(6) Uani 0.5 1 d G . P A 1
C20 C 0.3264(5) 0.4181(3) 0.3150(12) 0.169(7) Uani 0.5 1 d G . P A 1
H20 H 0.320175 0.438021 0.363341 0.203 Uiso 0.5 1 calc R U P A 1
C26 C 0.3270(5) 0.3516(4) 0.2303(17) 0.193(10) Uani 0.5 1 d G . P A 2
C1 C 0.3655(6) 0.3528(5) 0.1865(18) 0.301(19) Uani 0.5 1 d G . P A 2
H1 H 0.373263 0.335281 0.131878 0.361 Uiso 0.5 1 calc R U P A 2
C22 C 0.3928(4) 0.3795(5) 0.223(2) 0.274(16) Uani 0.5 1 d G . P A 2
H22 H 0.419098 0.380331 0.192654 0.329 Uiso 0.5 1 calc R U P A 2
C13 C 0.3815(5) 0.4051(4) 0.3025(18) 0.192(11) Uani 0.5 1 d G . P A 2
C5 C 0.3429(5) 0.4039(4) 0.3463(13) 0.196(10) Uani 0.5 1 d G . P A 2
H5 H 0.335188 0.421396 0.400857 0.235 Uiso 0.5 1 calc R U P A 2
C00E C 0.3157(4) 0.3772(5) 0.3102(16) 0.206(10) Uani 0.5 1 d G . P A 2
H00E H 0.289353 0.376346 0.340082 0.247 Uiso 0.5 1 calc R U 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
Zr01 Zr02 3.5069(15) 2_665 ?
Zr01 Zr02 3.5069(15) 9_666 ?
Zr01 Zr02 3.5069(15) 10_556 ?
Zr01 Zr02 3.5070(15) . ?
Zr01 O003 2.091(8) 10_556 ?
Zr01 O003 2.091(8) . ?
Zr01 O004 2.160(5) 11_565 ?
Zr01 O004 2.160(5) 10_556 ?
Zr01 O004 2.160(5) 4_566 ?
Zr01 O004 2.160(5) . ?
Zr01 O009 2.183(7) 11_565 ?
Zr01 O009 2.183(7) . ?
Zr02 Zr02 3.489(3) 10_556 ?
Zr02 Zr02 3.5197(18) 2_665 ?
Zr02 O003 2.143(4) 2_665 ?
Zr02 O003 2.143(4) . ?
Zr02 O005 2.287(7) 4_566 ?
Zr02 O005 2.287(7) 9_666 ?
Zr02 O006 2.212(8) . ?
Zr02 O008 2.208(9) . ?
Zr02 O009 2.137(7) 3_656 ?
Zr02 O009 2.137(7) . ?
O003 H003 1.0000 . ?
O004 C007 1.223(11) . ?
O005 C007 1.287(11) . ?
C007 C00B 1.666(14) . ?
C007 C13 1.436(15) . ?
O009 H009 1.0000 . ?
C8 H8 0.9500 . ?
C8 N1 1.4200 . ?
C8 C00I 1.4200 . ?
N1 N00C 1.4200 . ?
N00C C00H 1.4200 . ?
N00C C2 1.375(18) . ?
N00C C2 1.901(18) 10 ?
N00C C2 1.79(3) 6 ?
C00H H00H 0.9500 . ?
C00H C00I 1.4200 . ?
C00I C00G 1.507(13) . ?
C2 C2 1.48(3) 13 ?
C2 C2 0.87(2) 10 ?
C2 C2 1.19(3) 6 ?
C2 N8 1.96(2) . ?
C2 N36 1.756(19) . ?
C2 N36 1.33(2) 6 ?
N8 C14 1.44(3) . ?
N8 N36 1.39(2) . ?
C14 H14 0.9500 . ?
C14 C24 1.51(3) . ?
C24 C33 1.40(2) . ?
C24 C26 1.452(17) . ?
C33 H33 0.9500 . ?
C33 N36 1.376(17) . ?
C7 H7 0.9500 . ?
C7 C00G 1.3900 . ?
C7 C20 1.3900 . ?
C00G C00D 1.3900 . ?
C00D H00D 0.9500 . ?
C00D C00F 1.3900 . ?
C00F H00F 0.9500 . ?
C00F C00B 1.3900 . ?
C00B C20 1.3900 . ?
C20 H20 0.9500 . ?
C26 C1 1.3900 . ?
C26 C00E 1.3900 . ?
C1 H1 0.9500 . ?
C1 C22 1.3900 . ?
C22 H22 0.9500 . ?
C22 C13 1.3900 . ?
C13 C5 1.3900 . ?
C5 H5 0.9500 . ?
C5 C00E 1.3900 . ?
C00E H00E 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Zr02 Zr01 Zr02 89.92(5) 10_556 2_665 ?
Zr02 Zr01 Zr02 60.24(4) 2_665 . ?
Zr02 Zr01 Zr02 89.92(5) 9_666 . ?
Zr02 Zr01 Zr02 59.66(5) 10_556 . ?
Zr02 Zr01 Zr02 59.66(4) 2_665 9_666 ?
Zr02 Zr01 Zr02 60.24(4) 10_556 9_666 ?
O003 Zr01 Zr02 88.28(15) 10_556 . ?
O003 Zr01 Zr02 34.55(8) . . ?
O003 Zr01 Zr02 88.28(15) . 9_666 ?
O003 Zr01 Zr02 88.28(15) 10_556 2_665 ?
O003 Zr01 Zr02 34.55(8) 10_556 10_556 ?
O003 Zr01 Zr02 88.28(15) . 10_556 ?
O003 Zr01 Zr02 34.55(8) . 2_665 ?
O003 Zr01 Zr02 34.55(8) 10_556 9_666 ?
O003 Zr01 O003 105.8(3) 10_556 . ?
O003 Zr01 O004 142.15(13) . . ?
O003 Zr01 O004 142.15(14) 10_556 4_566 ?
O003 Zr01 O004 142.15(14) . 11_565 ?
O003 Zr01 O004 142.15(13) 10_556 10_556 ?
O003 Zr01 O004 80.62(19) 10_556 11_565 ?
O003 Zr01 O004 80.62(19) . 4_566 ?
O003 Zr01 O004 80.62(19) 10_556 . ?
O003 Zr01 O004 80.62(19) . 10_556 ?
O003 Zr01 O009 69.83(18) 10_556 . ?
O003 Zr01 O009 69.83(18) . 11_565 ?
O003 Zr01 O009 69.83(18) . . ?
O003 Zr01 O009 69.83(18) 10_556 11_565 ?
O004 Zr01 Zr02 76.34(15) 4_566 . ?
O004 Zr01 Zr02 166.25(16) 11_565 2_665 ?
O004 Zr01 Zr02 112.16(15) . 10_556 ?
O004 Zr01 Zr02 110.97(14) . 2_665 ?
O004 Zr01 Zr02 76.34(15) 11_565 10_556 ?
O004 Zr01 Zr02 76.34(15) . 9_666 ?
O004 Zr01 Zr02 166.25(16) . . ?
O004 Zr01 Zr02 166.25(16) 4_566 9_666 ?
O004 Zr01 Zr02 112.16(15) 4_566 2_665 ?
O004 Zr01 Zr02 110.98(14) 10_556 9_666 ?
O004 Zr01 Zr02 76.34(15) 10_556 2_665 ?
O004 Zr01 Zr02 166.25(16) 10_556 10_556 ?
O004 Zr01 Zr02 110.97(14) 11_565 . ?
O004 Zr01 Zr02 110.98(14) 4_566 10_556 ?
O004 Zr01 Zr02 112.16(15) 10_556 . ?
O004 Zr01 Zr02 112.16(15) 11_565 9_666 ?
O004 Zr01 O004 75.4(3) 11_565 . ?
O004 Zr01 O004 75.3(3) 4_566 10_556 ?
O004 Zr01 O004 117.4(3) 4_566 . ?
O004 Zr01 O004 117.4(3) 10_556 11_565 ?
O004 Zr01 O004 73.3(3) 4_566 11_565 ?
O004 Zr01 O004 73.3(3) 10_556 . ?
O004 Zr01 O009 78.2(3) 10_556 11_565 ?
O004 Zr01 O009 142.98(15) 11_565 11_565 ?
O004 Zr01 O009 142.98(15) 4_566 11_565 ?
O004 Zr01 O009 142.98(15) . . ?
O004 Zr01 O009 142.98(15) 10_556 . ?
O004 Zr01 O009 78.2(3) 11_565 . ?
O004 Zr01 O009 78.2(3) 4_566 . ?
O004 Zr01 O009 78.2(3) . 11_565 ?
O009 Zr01 Zr02 35.29(16) 11_565 2_665 ?
O009 Zr01 Zr02 90.4(3) 11_565 10_556 ?
O009 Zr01 Zr02 90.4(3) 11_565 . ?
O009 Zr01 Zr02 90.4(3) . 2_665 ?
O009 Zr01 Zr02 35.29(16) . . ?
O009 Zr01 Zr02 90.4(3) . 9_666 ?
O009 Zr01 Zr02 35.29(16) . 10_556 ?
O009 Zr01 Zr02 35.29(16) 11_565 9_666 ?
O009 Zr01 O009 110.3(6) . 11_565 ?
Zr01 Zr02 Zr01 90.08(5) 9_666 . ?
Zr01 Zr02 Zr02 59.878(18) 9_666 2_665 ?
Zr01 Zr02 Zr02 59.879(18) . 2_665 ?
Zr02 Zr02 Zr01 60.17(2) 10_556 . ?
Zr02 Zr02 Zr01 60.17(2) 10_556 9_666 ?
Zr02 Zr02 Zr02 89.998(1) 10_556 2_665 ?
O003 Zr02 Zr01 88.45(15) . 9_666 ?
O003 Zr02 Zr01 33.6(2) . . ?
O003 Zr02 Zr01 33.6(2) 2_665 9_666 ?
O003 Zr02 Zr01 88.45(15) 2_665 . ?
O003 Zr02 Zr02 88.0(2) . 10_556 ?
O003 Zr02 Zr02 88.0(2) 2_665 10_556 ?
O003 Zr02 Zr02 34.78(15) 2_665 2_665 ?
O003 Zr02 Zr02 34.78(15) . 2_665 ?
O003 Zr02 O003 69.4(3) 2_665 . ?
O003 Zr02 O005 75.7(2) . 4_566 ?
O003 Zr02 O005 140.7(3) . 9_666 ?
O003 Zr02 O005 140.7(3) 2_665 4_566 ?
O003 Zr02 O005 75.7(2) 2_665 9_666 ?
O003 Zr02 O006 144.43(18) . . ?
O003 Zr02 O006 144.43(18) 2_665 . ?
O003 Zr02 O008 87.4(3) 2_665 . ?
O003 Zr02 O008 87.4(3) . . ?
O005 Zr02 Zr01 71.30(17) 4_566 . ?
O005 Zr02 Zr01 161.37(17) 9_666 . ?
O005 Zr02 Zr01 161.37(17) 4_566 9_666 ?
O005 Zr02 Zr01 71.30(17) 9_666 9_666 ?
O005 Zr02 Zr02 108.70(18) 4_566 10_556 ?
O005 Zr02 Zr02 108.70(18) 9_666 10_556 ?
O005 Zr02 Zr02 107.87(16) 9_666 2_665 ?
O005 Zr02 Zr02 107.87(16) 4_566 2_665 ?
O005 Zr02 O005 127.3(3) 9_666 4_566 ?
O006 Zr02 Zr01 116.65(18) . 9_666 ?
O006 Zr02 Zr01 116.65(18) . . ?
O006 Zr02 Zr02 174.2(3) . 2_665 ?
O006 Zr02 Zr02 84.2(3) . 10_556 ?
O006 Zr02 O005 74.2(2) . 4_566 ?
O006 Zr02 O005 74.2(2) . 9_666 ?
O008 Zr02 Zr01 116.48(17) . . ?
O008 Zr02 Zr01 116.48(17) . 9_666 ?
O008 Zr02 Zr02 174.4(3) . 10_556 ?
O008 Zr02 Zr02 84.4(3) . 2_665 ?
O008 Zr02 O005 73.2(2) . 4_566 ?
O008 Zr02 O005 73.2(2) . 9_666 ?
O008 Zr02 O006 101.5(4) . . ?
O009 Zr02 Zr01 90.6(3) 3_656 . ?
O009 Zr02 Zr01 36.18(16) 3_656 9_666 ?
O009 Zr02 Zr01 90.6(3) . 9_666 ?
O009 Zr02 Zr01 36.17(16) . . ?
O009 Zr02 Zr02 35.3(3) . 10_556 ?
O009 Zr02 Zr02 90.8(2) . 2_665 ?
O009 Zr02 Zr02 90.8(2) 3_656 2_665 ?
O009 Zr02 Zr02 35.3(3) 3_656 10_556 ?
O009 Zr02 O003 108.2(3) . 2_665 ?
O009 Zr02 O003 69.8(3) 3_656 2_665 ?
O009 Zr02 O003 108.2(3) 3_656 . ?
O009 Zr02 O003 69.8(3) . . ?
O009 Zr02 O005 74.9(3) 3_656 9_666 ?
O009 Zr02 O005 74.9(3) . 4_566 ?
O009 Zr02 O005 140.8(3) . 9_666 ?
O009 Zr02 O005 140.8(3) 3_656 4_566 ?
O009 Zr02 O006 84.4(3) 3_656 . ?
O009 Zr02 O006 84.4(3) . . ?
O009 Zr02 O008 144.5(2) 3_656 . ?
O009 Zr02 O008 144.5(2) . . ?
O009 Zr02 O009 70.5(5) 3_656 . ?
Zr01 O003 Zr02 111.8(2) . 2_665 ?
Zr01 O003 Zr02 111.8(2) . . ?
Zr01 O003 H003 107.5 . . ?
Zr02 O003 Zr02 110.4(3) 2_665 . ?
Zr02 O003 H003 107.5 2_665 . ?
Zr02 O003 H003 107.5 . . ?
C007 O004 Zr01 131.2(7) . . ?
C007 O005 Zr02 131.2(7) . 9_666 ?
O004 C007 O005 129.0(10) . . ?
O004 C007 C00B 114.6(11) . . ?
O004 C007 C13 127.4(13) . . ?
O005 C007 C00B 116.4(10) . . ?
O005 C007 C13 101.7(12) . . ?
Zr01 O009 H009 110.1 . . ?
Zr02 O009 Zr01 108.5(2) 10_556 . ?
Zr02 O009 Zr01 108.5(2) . . ?
Zr02 O009 Zr02 109.4(5) 10_556 . ?
Zr02 O009 H009 110.1 10_556 . ?
Zr02 O009 H009 110.1 . . ?
N1 C8 H8 126.0 . . ?
N1 C8 C00I 108.0 . . ?
C00I C8 H8 126.0 . . ?
N00C N1 C8 108.0 . . ?
N1 N00C C00H 108.0 . . ?
N1 N00C C2 107.5(13) . 10 ?
N1 N00C C2 152.9(14) . 6 ?
C00H N00C C2 99.0(14) . 6 ?
C00H N00C C2 137.2(12) . 10 ?
C2 N00C N1 111.5(15) . . ?
C2 N00C C00H 140.5(15) . . ?
C2 N00C C2 41.8(10) . 6 ?
C2 N00C C2 47.0(9) 6 10 ?
C2 N00C C2 24.8(7) . 10 ?
N00C C00H H00H 126.0 . . ?
N00C C00H C00I 108.0 . . ?
C00I C00H H00H 126.0 . . ?
C8 C00I C00H 108.0 . . ?
C8 C00I C00G 133.4(17) . . ?
C00H C00I C00G 118.6(17) . . ?
N00C C2 N00C 133.0(13) 6 10 ?
N00C C2 N00C 120(2) . 6 ?
N00C C2 N00C 72.3(18) . 10 ?
N00C C2 C2 102.1(15) . 13 ?
C2 C2 N00C 62.4(16) 13 10 ?
C2 C2 N00C 113.8(9) 10 . ?
C2 C2 N00C 87.9(16) 6 . ?
C2 C2 N00C 50(2) 6 6 ?
C2 C2 N00C 41.4(10) 10 10 ?
C2 C2 N00C 71(2) 13 6 ?
C2 C2 N00C 88.5(16) 6 10 ?
C2 C2 N00C 108.1(17) 10 6 ?
C2 C2 C2 53.8(9) 10 13 ?
C2 C2 C2 90.003(7) 10 6 ?
C2 C2 C2 36.2(9) 6 13 ?
C2 C2 N8 91.9(10) 6 . ?
C2 C2 N8 141.5(7) 10 . ?
C2 C2 N8 119.2(12) 13 . ?
C2 C2 N36 131.7(9) 10 6 ?
C2 C2 N36 76.9(10) 13 . ?
C2 C2 N36 49.4(9) 6 . ?
C2 C2 N36 88.0(17) 6 6 ?
C2 C2 N36 120.3(6) 10 . ?
N36 C2 N8 86.8(8) 6 . ?
N36 C2 N8 43.4(7) . . ?
N36 C2 N36 93.6(12) 6 . ?
C14 N8 C2 159.3(16) . . ?
N36 N8 C2 60.3(12) . . ?
N36 N8 C14 115.2(17) . . ?
N8 C14 H14 129.8 . . ?
N8 C14 C24 100(2) . . ?
C24 C14 H14 129.8 . . ?
C33 C24 C14 107.3(15) . . ?
C33 C24 C26 119.9(18) . . ?
C26 C24 C14 132.2(18) . . ?
C24 C33 H33 123.5 . . ?
N36 C33 C24 112.9(17) . . ?
N36 C33 H33 123.5 . . ?
C2 N36 C2 42.7(13) 6 . ?
C2 N36 N8 117.6(13) 6 . ?
C2 N36 C33 135.8(19) 6 . ?
N8 N36 C2 76.2(10) . . ?
C33 N36 C2 154.7(14) . . ?
C33 N36 N8 104.1(17) . . ?
C00G C7 H7 120.0 . . ?
C00G C7 C20 120.0 . . ?
C20 C7 H7 120.0 . . ?
C7 C00G C00I 120.3(13) . . ?
C7 C00G C00D 120.0 . . ?
C00D C00G C00I 119.3(13) . . ?
C00G C00D H00D 120.0 . . ?
C00G C00D C00F 120.0 . . ?
C00F C00D H00D 120.0 . . ?
C00D C00F H00F 120.0 . . ?
C00B C00F C00D 120.0 . . ?
C00B C00F H00F 120.0 . . ?
C00F C00B C007 119.5(10) . . ?
C00F C00B C20 120.0 . . ?
C20 C00B C007 120.1(10) . . ?
C7 C20 H20 120.0 . . ?
C00B C20 C7 120.0 . . ?
C00B C20 H20 120.0 . . ?
C1 C26 C24 123.2(14) . . ?
C1 C26 C00E 120.0 . . ?
C00E C26 C24 116.7(14) . . ?
C26 C1 H1 120.0 . . ?
C26 C1 C22 120.0 . . ?
C22 C1 H1 120.0 . . ?
C1 C22 H22 120.0 . . ?
C1 C22 C13 120.0 . . ?
C13 C22 H22 120.0 . . ?
C22 C13 C007 126.2(13) . . ?
C5 C13 C007 112.6(13) . . ?
C5 C13 C22 120.0 . . ?
C13 C5 H5 120.0 . . ?
C13 C5 C00E 120.0 . . ?
C00E C5 H5 120.0 . . ?
C26 C00E H00E 120.0 . . ?
C5 C00E C26 120.0 . . ?
C5 C00E H00E 120.0 . . ?

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
Zr01 O004 C007 O005 -11.8(15) . . . . ?
Zr01 O004 C007 C00B 172.1(7) . . . . ?
Zr01 O004 C007 C13 149.3(12) . . . . ?
Zr02 O005 C007 O004 13.8(16) 9_666 . . . ?
Zr02 O005 C007 C00B -170.1(8) 9_666 . . . ?
Zr02 O005 C007 C13 -150.9(10) 9_666 . . . ?
O004 C007 C00B C00F -178.6(9) . . . . ?
O004 C007 C00B C20 -6.3(14) . . . . ?
O004 C007 C13 C22 173.0(12) . . . . ?
O004 C007 C13 C5 6(2) . . . . ?
O005 C007 C00B C00F 4.7(14) . . . . ?
O005 C007 C00B C20 177.1(9) . . . . ?
O005 C007 C13 C22 -21.9(15) . . . . ?
O005 C007 C13 C5 170.9(11) . . . . ?
C007 C00B C20 C7 -172.3(14) . . . . ?
C007 C13 C5 C00E 168.1(16) . . . . ?
C8 N1 N00C C00H 0.0 . . . . ?
C8 N1 N00C C2 -174(3) . . . 6 ?
C8 N1 N00C C2 178.3(15) . . . . ?
C8 N1 N00C C2 -155.7(12) . . . 10 ?
C8 C00I C00G C7 26(2) . . . . ?
C8 C00I C00G C00D -147.4(15) . . . . ?
N1 C8 C00I C00H 0.0 . . . . ?
N1 C8 C00I C00G 177(2) . . . . ?
N1 N00C C00H C00I 0.0 . . . . ?
N1 N00C C2 N00C -144.7(18) . . . 6 ?
N1 N00C C2 N00C 85.4(9) . . . 10 ?
N1 N00C C2 C2 85.4(11) . . . 10 ?
N1 N00C C2 C2 141.0(15) . . . 13 ?
N1 N00C C2 C2 174.5(13) . . . 6 ?
N00C C00H C00I C8 0.0 . . . . ?
N00C C00H C00I C00G -177.9(18) . . . . ?
C00H N00C C2 N00C -97.2(18) . . . 10 ?
C00H N00C C2 N00C 33(3) . . . 6 ?
C00H N00C C2 C2 -97.2(17) . . . 10 ?
C00H N00C C2 C2 -42(2) . . . 13 ?
C00H N00C C2 C2 -8(2) . . . 6 ?
C00H C00I C00G C7 -156.9(11) . . . . ?
C00H C00I C00G C00D 29.8(18) . . . . ?
C00I C8 N1 N00C 0.0 . . . . ?
C00I C00G C00D C00F 173.3(17) . . . . ?
C2 N00C C00H C00I -177(2) . . . . ?
C2 N00C C00H C00I 144.8(18) 10 . . . ?
C2 N00C C00H C00I 177.1(14) 6 . . . ?
C2 N00C C2 N00C 0.0(9) 10 . . 10 ?
C2 N00C C2 N00C 130(2) 10 . . 6 ?
C2 N00C C2 N00C -89.1(13) 6 . . 10 ?
C2 N00C C2 N00C 41(2) 6 . . 6 ?
C2 N00C C2 C2 89.1(7) 10 . . 6 ?
C2 N00C C2 C2 55.6(11) 10 . . 13 ?
C2 N00C C2 C2 -33.5(9) 6 . . 13 ?
C2 N00C C2 C2 -89.1(7) 6 . . 10 ?
C2 C2 N36 C2 -26.9(7) 13 . . 6 ?
C2 C2 N36 C2 -59.9(10) 10 . . 6 ?
C2 C2 N36 N8 167.5(19) 13 . . . ?
C2 C2 N36 N8 -165.6(19) 6 . . . ?
C2 C2 N36 N8 134.5(12) 10 . . . ?
C2 C2 N36 C33 73(5) 13 . . . ?
C2 C2 N36 C33 100(5) 6 . . . ?
C2 C2 N36 C33 40(5) 10 . . . ?
C2 N8 C14 C24 -68(6) . . . . ?
C2 N8 N36 C2 -10.9(16) . . . 6 ?
C2 N8 N36 C33 153.9(15) . . . . ?
N8 C2 N36 C2 165.6(19) . . . 6 ?
N8 C2 N36 C33 -94(4) . . . . ?
N8 C14 C24 C33 -3(2) . . . . ?
N8 C14 C24 C26 -174(2) . . . . ?
C14 N8 N36 C2 -157(2) . . . . ?
C14 N8 N36 C2 -168.1(16) . . . 6 ?
C14 N8 N36 C33 -3(2) . . . . ?
C14 C24 C33 N36 2(2) . . . . ?
C14 C24 C26 C1 -175.1(19) . . . . ?
C14 C24 C26 C00E 1(3) . . . . ?
C24 C33 N36 C2 88(5) . . . . ?
C24 C33 N36 C2 161(2) . . . 6 ?
C24 C33 N36 N8 1(2) . . . . ?
C24 C26 C1 C22 176.4(19) . . . . ?
C24 C26 C00E C5 -176.6(18) . . . . ?
C33 C24 C26 C1 15(2) . . . . ?
C33 C24 C26 C00E -168.2(16) . . . . ?
N36 C2 N36 C2 84(2) 6 . . 6 ?
N36 C2 N36 N8 -81.5(11) 6 . . . ?
N36 C2 N36 C33 -175(4) 6 . . . ?
N36 N8 C14 C24 4(2) . . . . ?
C7 C00G C00D C00F 0.0 . . . . ?
C00G C7 C20 C00B 0.0 . . . . ?
C00G C00D C00F C00B 0.0 . . . . ?
C00D C00F C00B C007 172.3(14) . . . . ?
C00D C00F C00B C20 0.0 . . . . ?
C00F C00B C20 C7 0.0 . . . . ?
C20 C7 C00G C00I -173.2(17) . . . . ?
C20 C7 C00G C00D 0.0 . . . . ?
C26 C24 C33 N36 173.7(16) . . . . ?
C26 C1 C22 C13 0.0 . . . . ?
C1 C26 C00E C5 0.0 . . . . ?
C1 C22 C13 C007 -166.3(18) . . . . ?
C1 C22 C13 C5 0.0 . . . . ?
C22 C13 C5 C00E 0.0 . . . . ?
C13 C5 C00E C26 0.0 . . . . ?
C00E C26 C1 C22 0.0 . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 2887 electrons were 
found in a volume of 10561Å³ in 1 void per unit cell. 
This is consistent with the presence of 
7[C7H8] per Asymmetric Unit 
which account for 2800 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.813 -0.293 -0.459 10560.9 2887.2 '56 Toluene'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
__diffrn_radiation_monochromator 'Silicon Double Crystal'
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT026_cmmm                
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..        28% Check 
RESPONSE: The crystals of the compound are weakly diffracting due 
to structural flexibility and significant porosity/large pores.
;
_vrf_PLAT058_cmmm                
;
PROBLEM: Maximum Transmission Factor Missing ............          ?       
RESPONSE: XDS does not provide this data
;
_vrf_PLAT059_cmmm                
;
PROBLEM: Minimum Transmission Factor Missing ............          ?       
RESPONSE: XDS does not provide this data
;
####################################################################### 
# 
# 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_p21n_pl
_database_code_depnum_ccdc_archive 'CCDC 2288077'
loop_
_audit_author_name
_audit_author_address
'Christopher Sumby'
;The University of Adelaide
Australia
;
_audit_update_record             
;
2023-08-11 deposited with the CCDC.	2023-12-21 downloaded from the CCDC.
;
_audit_creation_date             2022-09-14
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2019/2
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H11 N4 O8 Zr1.5'
_chemical_formula_sum            'C12 H11 N4 O8 Zr1.50'
_chemical_formula_weight         476.08
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x, -y, -z'
'-x, y+1/2, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x, y, z'
'x, -y-1/2, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -y, z-1/2'

_cell_length_a                   29.301(7)
_cell_length_b                   22.313(8)
_cell_length_c                   21.132(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13816(7)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    84271
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.684
_cell_measurement_theta_min      1.390
_shelx_estimated_absorpt_T_max   0.987
_shelx_estimated_absorpt_T_min   0.981
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.916
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.028
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2390
_diffrn_reflns_av_unetI/netI     0.1079
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.833
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            84271
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.684
_diffrn_reflns_theta_min         1.390
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '13.3 (Dectris Eiger detectors)'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.833
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'MX2 Beamline Australian Synchrotron'
_diffrn_measurement_device_type  
;
D. Aragao, J. Aishima, H. Cherukuvada, R. Clarken, M. Clift, 
N. P. Cowieson, D. J. Ericsson, C. L. Gee, S. Macedo, N. Mudie, 
S. Panjikar, J. R. Price, A. Riboldi-Tunnicliffe, R. Rostan, R. 
Williamson and T. T. Caradoc-Davies, MX2: a high-flux 
undulator microfocus beamline serving both the chemical 
and macromolecular crystallography communities at the 
Australian Synchrotron, J. Synchrotron Rad. (2018). 25, 
885-891.
;
_diffrn_measurement_detector_type 'Dectris Eiger 16M'
_diffrn_measurement_method       'Omega Scan'
_diffrn_source                   ?
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2908
_reflns_number_total             7571
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'AS QEGUI'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         7571
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1377
_refine_ls_R_factor_gt           0.0716
_refine_ls_restrained_S_all      0.878
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1203P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1882
_refine_ls_wR_factor_ref         0.2304
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Riding coordinates:
 O00C(H00C), O00E(H00E), O00H(H00A,H00B), O00N(H00N), C00S(H00S), C00T(H00T),
 C010(H010), C016(H016), C01A(H01A), C01C(H01C)
2.b Aromatic/amide H refined with riding coordinates:
 C01B(H01B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr01 Zr 0.500000 0.53013(4) 0.88817(5) 0.0746(3) Uani 1 2 d S T P . .
Zr02 Zr 0.55999(2) 0.42385(3) 0.97733(3) 0.0798(3) Uani 1 1 d . . . . .
O004 O 0.45524(16) 0.4862(2) 0.8186(2) 0.0815(13) Uani 1 1 d . . . . .
O006 O 0.45501(17) 0.5995(2) 0.8526(2) 0.0851(15) Uani 1 1 d . . . . .
O008 O 0.41760(19) 0.4168(2) 0.8765(3) 0.0955(15) Uani 1 1 d . . . . .
O00A O 0.41703(19) 0.1327(2) 0.5591(3) 0.0996(16) Uani 1 1 d . . . . .
O00C O 0.4416(2) 0.5142(2) 0.9461(3) 0.1083(18) Uani 1 1 d . . . . .
H00C H 0.414290 0.520993 0.920280 0.162 Uiso 1 1 d R U . . .
O00E O 0.500000 0.4106(3) 1.0333(3) 0.098(2) Uani 1 2 d S T P . .
H00E H 0.500000 0.369365 1.049102 0.146 Uiso 1 2 d R U P . .
O00H O 0.63501(19) 0.4315(3) 0.9788(3) 0.121(2) Uani 1 1 d . . . . .
H00A H 0.649940 0.448530 1.016398 0.181 Uiso 1 1 d R U . . .
H00B H 0.650700 0.458670 0.949378 0.181 Uiso 1 1 d R U . . .
O00L O 0.5484(2) 0.3297(3) 0.9479(3) 0.129(2) Uani 1 1 d . . . . .
O00N O 0.500000 0.4399(4) 0.9238(4) 0.122(3) Uani 1 2 d S T P . .
H00N H 0.500000 0.412476 0.887581 0.184 Uiso 1 2 d R U P . .
N00D N 0.3645(2) 0.3620(3) 0.7056(3) 0.0849(17) Uani 1 1 d . . . . .
N00F N 0.3605(2) 0.2576(3) 0.6822(3) 0.0866(17) Uani 1 1 d . . . . .
N00O N 0.3843(3) 0.4010(3) 0.6662(3) 0.103(2) Uani 1 1 d . . . . .
N00P N 0.3756(2) 0.2325(3) 0.7380(3) 0.0996(19) Uani 1 1 d . . . . .
C00S C 0.3762(2) 0.3699(3) 0.7658(3) 0.0797(19) Uani 1 1 d . . . . .
H00S H 0.365923 0.347404 0.800091 0.096 Uiso 1 1 d R U . . .
C00T C 0.3367(3) 0.3144(3) 0.6828(3) 0.082(2) Uani 1 1 d . . . . .
H00T H 0.329665 0.323899 0.638606 0.099 Uiso 1 1 d R U . . .
C00U C 0.2924(2) 0.3121(3) 0.7184(3) 0.0780(19) Uani 1 1 d . . . . .
C00V C 0.4005(3) 0.1794(4) 0.6560(4) 0.092(2) Uani 1 1 d . . . . .
C00W C 0.4293(3) 0.4431(4) 0.8259(4) 0.094(2) Uani 1 1 d . . . . .
C00Y C 0.4054(3) 0.4170(3) 0.7679(3) 0.083(2) Uani 1 1 d . . . . .
C010 C 0.3736(3) 0.2258(4) 0.6338(4) 0.093(2) Uani 1 1 d . . . . .
H010 H 0.366738 0.233080 0.591544 0.111 Uiso 1 1 d R U . . .
C012 C 0.4284(3) 0.1321(4) 0.6207(4) 0.098(3) Uani 1 1 d . . . . .
C016 C 0.4003(3) 0.1859(4) 0.7201(4) 0.100(2) Uani 1 1 d . . . . .
H016 H 0.415858 0.160837 0.747914 0.120 Uiso 1 1 d R U . . .
C01A C 0.2720(2) 0.3625(3) 0.7348(4) 0.101(3) Uani 1 1 d . . . . .
H01A H 0.286643 0.398370 0.725289 0.121 Uiso 1 1 d R U . . .
C01B C 0.4108(4) 0.4348(4) 0.7036(4) 0.119(3) Uani 1 1 d . . . . .
H01B H 0.430328 0.465937 0.689303 0.143 Uiso 1 1 calc R U . . .
C01C C 0.2719(3) 0.2592(4) 0.7328(5) 0.123(3) Uani 1 1 d . . . . .
H01C H 0.286121 0.223257 0.722507 0.147 Uiso 1 1 d 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
Zr01 Zr02 3.4959(12) 9_667 ?
Zr01 Zr02 3.5019(13) 11_655 ?
Zr01 Zr02 3.5019(13) . ?
Zr01 Zr02 3.4959(12) 3_567 ?
Zr01 O004 2.200(5) . ?
Zr01 O004 2.200(5) 11_655 ?
Zr01 O006 2.167(5) 11_655 ?
Zr01 O006 2.167(5) . ?
Zr01 O00C 2.135(5) 11_655 ?
Zr01 O00C 2.135(5) . ?
Zr01 O00E 2.121(7) 9_667 ?
Zr01 O00N 2.149(8) . ?
Zr02 Zr02 3.5156(17) 11_655 ?
Zr02 Zr02 3.5305(19) 3_567 ?
Zr02 O008 2.235(5) 11_655 ?
Zr02 O00A 2.244(5) 2_655 ?
Zr02 O00C 2.128(5) 9_667 ?
Zr02 O00C 2.122(5) 11_655 ?
Zr02 O00E 2.139(4) . ?
Zr02 O00H 2.205(6) . ?
Zr02 O00L 2.218(6) . ?
Zr02 O00N 2.121(5) . ?
O004 C00W 1.236(9) . ?
O006 C012 1.207(10) 10_567 ?
O008 C00W 1.268(9) . ?
O00A C012 1.344(10) . ?
O00C H00C 0.9798 . ?
O00E H00E 0.9795 . ?
O00H H00A 0.9832 . ?
O00H H00B 0.9831 . ?
O00N H00N 0.9795 . ?
N00D N00O 1.335(8) . ?
N00D C00S 1.329(8) . ?
N00D C00T 1.422(8) . ?
N00F N00P 1.380(8) . ?
N00F C00T 1.446(9) . ?
N00F C010 1.303(8) . ?
N00O C01B 1.340(10) . ?
N00P C016 1.322(9) . ?
C00S H00S 0.9305 . ?
C00S C00Y 1.357(9) . ?
C00T H00T 0.9805 . ?
C00T C00U 1.501(10) . ?
C00U C01A 1.320(9) . ?
C00U C01C 1.359(10) . ?
C00V C010 1.382(10) . ?
C00V C012 1.529(11) . ?
C00V C016 1.362(10) . ?
C00W C00Y 1.526(11) . ?
C00Y C01B 1.424(11) . ?
C010 H010 0.9299 . ?
C016 H016 0.9302 . ?
C01A C01A 1.439(14) 8_546 ?
C01A H01A 0.9304 . ?
C01B H01B 0.9500 . ?
C01C C01C 1.474(17) 8_546 ?
C01C H01C 0.9303 . ?

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
Zr02 Zr01 Zr02 60.26(3) . 11_655 ?
Zr02 Zr01 Zr02 60.60(3) 9_667 11_655 ?
Zr02 Zr01 Zr02 90.79(3) 3_567 11_655 ?
Zr02 Zr01 Zr02 60.60(3) 3_567 . ?
Zr02 Zr01 Zr02 90.79(3) 9_667 . ?
Zr02 Zr01 Zr02 60.37(3) 3_567 9_667 ?
O004 Zr01 Zr02 111.96(12) 11_655 3_567 ?
O004 Zr01 Zr02 76.03(13) 11_655 . ?
O004 Zr01 Zr02 110.92(14) 11_655 11_655 ?
O004 Zr01 Zr02 166.81(14) . 3_567 ?
O004 Zr01 Zr02 110.92(14) . . ?
O004 Zr01 Zr02 166.81(14) 11_655 9_667 ?
O004 Zr01 Zr02 76.03(13) . 11_655 ?
O004 Zr01 Zr02 111.97(12) . 9_667 ?
O004 Zr01 O004 73.2(2) 11_655 . ?
O006 Zr01 Zr02 111.39(13) . 11_655 ?
O006 Zr01 Zr02 112.21(15) . 3_567 ?
O006 Zr01 Zr02 111.39(13) 11_655 . ?
O006 Zr01 Zr02 167.26(14) 11_655 11_655 ?
O006 Zr01 Zr02 76.49(14) . 9_667 ?
O006 Zr01 Zr02 76.49(14) 11_655 3_567 ?
O006 Zr01 Zr02 112.21(15) 11_655 9_667 ?
O006 Zr01 Zr02 167.26(14) . . ?
O006 Zr01 O004 116.68(19) . 11_655 ?
O006 Zr01 O004 116.68(19) 11_655 . ?
O006 Zr01 O004 73.96(19) 11_655 11_655 ?
O006 Zr01 O004 73.96(19) . . ?
O006 Zr01 O006 74.9(3) . 11_655 ?
O00C Zr01 Zr02 34.84(14) 11_655 3_567 ?
O00C Zr01 Zr02 34.84(14) . 9_667 ?
O00C Zr01 Zr02 34.52(15) . 11_655 ?
O00C Zr01 Zr02 34.52(15) 11_655 . ?
O00C Zr01 Zr02 88.93(17) 11_655 11_655 ?
O00C Zr01 Zr02 89.18(16) . 3_567 ?
O00C Zr01 Zr02 88.93(17) . . ?
O00C Zr01 Zr02 89.19(16) 11_655 9_667 ?
O00C Zr01 O004 141.9(2) . 11_655 ?
O00C Zr01 O004 141.9(2) 11_655 . ?
O00C Zr01 O004 80.26(19) 11_655 11_655 ?
O00C Zr01 O004 80.26(19) . . ?
O00C Zr01 O006 143.7(2) 11_655 . ?
O00C Zr01 O006 80.2(2) . . ?
O00C Zr01 O006 80.2(2) 11_655 11_655 ?
O00C Zr01 O006 143.7(2) . 11_655 ?
O00C Zr01 O00C 106.6(3) . 11_655 ?
O00C Zr01 O00N 69.1(2) 11_655 . ?
O00C Zr01 O00N 69.1(2) . . ?
O00E Zr01 Zr02 35.03(11) 9_667 9_667 ?
O00E Zr01 Zr02 90.07(19) 9_667 . ?
O00E Zr01 Zr02 35.03(11) 9_667 3_567 ?
O00E Zr01 Zr02 90.07(19) 9_667 11_655 ?
O00E Zr01 O004 143.13(13) 9_667 . ?
O00E Zr01 O004 143.12(13) 9_667 11_655 ?
O00E Zr01 O006 80.0(2) 9_667 . ?
O00E Zr01 O006 80.0(2) 9_667 11_655 ?
O00E Zr01 O00C 69.82(18) 9_667 . ?
O00E Zr01 O00C 69.82(18) 9_667 11_655 ?
O00E Zr01 O00N 108.1(4) 9_667 . ?
O00N Zr01 Zr02 34.65(13) . 11_655 ?
O00N Zr01 Zr02 34.65(13) . . ?
O00N Zr01 Zr02 89.5(2) . 9_667 ?
O00N Zr01 Zr02 89.5(2) . 3_567 ?
O00N Zr01 O004 79.4(2) . 11_655 ?
O00N Zr01 O004 79.4(2) . . ?
O00N Zr01 O006 142.21(14) . . ?
O00N Zr01 O006 142.20(14) . 11_655 ?
Zr01 Zr02 Zr01 89.21(3) 9_667 . ?
Zr01 Zr02 Zr02 59.871(17) . 11_655 ?
Zr01 Zr02 Zr02 59.78(2) 9_667 3_567 ?
Zr01 Zr02 Zr02 59.813(16) 9_667 11_655 ?
Zr01 Zr02 Zr02 59.62(3) . 3_567 ?
Zr02 Zr02 Zr02 90.0 11_655 3_567 ?
O008 Zr02 Zr01 71.47(13) 11_655 . ?
O008 Zr02 Zr01 160.62(14) 11_655 9_667 ?
O008 Zr02 Zr02 107.08(15) 11_655 11_655 ?
O008 Zr02 Zr02 109.04(14) 11_655 3_567 ?
O008 Zr02 O00A 127.36(19) 11_655 2_655 ?
O00A Zr02 Zr01 161.09(14) 2_655 . ?
O00A Zr02 Zr01 71.92(14) 2_655 9_667 ?
O00A Zr02 Zr02 107.46(14) 2_655 11_655 ?
O00A Zr02 Zr02 109.40(15) 2_655 3_567 ?
O00C Zr02 Zr01 87.87(16) 11_655 9_667 ?
O00C Zr02 Zr01 34.97(14) 9_667 9_667 ?
O00C Zr02 Zr01 87.62(17) 9_667 . ?
O00C Zr02 Zr01 34.76(14) 11_655 . ?
O00C Zr02 Zr02 88.77(16) 11_655 11_655 ?
O00C Zr02 Zr02 33.77(14) 9_667 3_567 ?
O00C Zr02 Zr02 33.88(14) 11_655 3_567 ?
O00C Zr02 Zr02 88.77(16) 9_667 11_655 ?
O00C Zr02 O008 77.1(2) 11_655 11_655 ?
O00C Zr02 O008 140.9(2) 9_667 11_655 ?
O00C Zr02 O00A 141.3(2) 11_655 2_655 ?
O00C Zr02 O00A 77.6(2) 9_667 2_655 ?
O00C Zr02 O00C 67.6(2) 11_655 9_667 ?
O00C Zr02 O00E 106.6(3) 11_655 . ?
O00C Zr02 O00E 69.6(2) 9_667 . ?
O00C Zr02 O00H 87.3(2) 11_655 . ?
O00C Zr02 O00H 87.7(2) 9_667 . ?
O00C Zr02 O00L 145.6(2) 9_667 . ?
O00C Zr02 O00L 144.1(2) 11_655 . ?
O00E Zr02 Zr01 88.77(19) . . ?
O00E Zr02 Zr01 34.68(18) . 9_667 ?
O00E Zr02 Zr02 34.75(17) . 11_655 ?
O00E Zr02 Zr02 89.0(2) . 3_567 ?
O00E Zr02 O008 139.4(2) . 11_655 ?
O00E Zr02 O00A 75.1(2) . 2_655 ?
O00E Zr02 O00H 145.3(2) . . ?
O00E Zr02 O00L 84.2(3) . . ?
O00H Zr02 Zr01 117.84(15) . 9_667 ?
O00H Zr02 Zr01 117.12(15) . . ?
O00H Zr02 Zr02 85.52(16) . 3_567 ?
O00H Zr02 Zr02 175.50(16) . 11_655 ?
O00H Zr02 O008 74.1(2) . 11_655 ?
O00H Zr02 O00A 74.5(2) . 2_655 ?
O00H Zr02 O00L 103.3(2) . . ?
O00L Zr02 Zr01 115.45(17) . 9_667 ?
O00L Zr02 Zr01 114.45(17) . . ?
O00L Zr02 Zr02 81.21(18) . 11_655 ?
O00L Zr02 Zr02 171.18(18) . 3_567 ?
O00L Zr02 O008 73.2(2) . 11_655 ?
O00L Zr02 O00A 74.3(2) . 2_655 ?
O00N Zr02 Zr01 35.2(2) . . ?
O00N Zr02 Zr01 88.1(2) . 9_667 ?
O00N Zr02 Zr02 89.0(3) . 3_567 ?
O00N Zr02 Zr02 34.04(18) . 11_655 ?
O00N Zr02 O008 75.3(3) . 11_655 ?
O00N Zr02 O00A 139.0(2) . 2_655 ?
O00N Zr02 O00C 106.2(3) . 9_667 ?
O00N Zr02 O00C 69.9(3) . 11_655 ?
O00N Zr02 O00E 68.7(3) . . ?
O00N Zr02 O00H 145.2(2) . . ?
O00N Zr02 O00L 83.3(3) . . ?
C00W O004 Zr01 129.2(5) . . ?
C012 O006 Zr01 131.5(5) 10_567 . ?
C00W O008 Zr02 133.9(5) . 11_655 ?
C012 O00A Zr02 131.8(5) . 2_654 ?
Zr01 O00C H00C 108.0 . . ?
Zr02 O00C Zr01 110.7(2) 11_655 . ?
Zr02 O00C Zr01 110.2(2) 9_667 . ?
Zr02 O00C Zr02 112.4(2) 11_655 9_667 ?
Zr02 O00C H00C 107.8 9_667 . ?
Zr02 O00C H00C 107.6 11_655 . ?
Zr01 O00E Zr02 110.3(2) 9_667 . ?
Zr01 O00E Zr02 110.3(2) 9_667 11_655 ?
Zr01 O00E H00E 108.7 9_667 . ?
Zr02 O00E Zr02 110.5(3) 11_655 . ?
Zr02 O00E H00E 108.5 11_655 . ?
Zr02 O00E H00E 108.5 . . ?
Zr02 O00H H00A 119.0 . . ?
Zr02 O00H H00B 120.3 . . ?
H00A O00H H00B 93.7 . . ?
Zr01 O00N H00N 108.2 . . ?
Zr02 O00N Zr01 110.2(3) 11_655 . ?
Zr02 O00N Zr01 110.2(3) . . ?
Zr02 O00N Zr02 111.9(4) . 11_655 ?
Zr02 O00N H00N 108.1 . . ?
Zr02 O00N H00N 108.1 11_655 . ?
N00O N00D C00T 121.6(6) . . ?
C00S N00D N00O 113.5(6) . . ?
C00S N00D C00T 124.7(7) . . ?
N00P N00F C00T 120.2(6) . . ?
C010 N00F N00P 110.7(6) . . ?
C010 N00F C00T 128.9(7) . . ?
N00D N00O C01B 104.5(7) . . ?
C016 N00P N00F 104.5(6) . . ?
N00D C00S H00S 126.3 . . ?
N00D C00S C00Y 107.2(7) . . ?
C00Y C00S H00S 126.6 . . ?
N00D C00T N00F 112.5(6) . . ?
N00D C00T H00T 106.4 . . ?
N00D C00T C00U 110.6(6) . . ?
N00F C00T H00T 106.3 . . ?
N00F C00T C00U 113.0(6) . . ?
C00U C00T H00T 107.6 . . ?
C01A C00U C00T 119.6(7) . . ?
C01A C00U C01C 118.7(8) . . ?
C01C C00U C00T 121.6(7) . . ?
C010 C00V C012 131.0(8) . . ?
C016 C00V C010 104.8(8) . . ?
C016 C00V C012 124.0(8) . . ?
O004 C00W O008 129.1(8) . . ?
O004 C00W C00Y 118.7(7) . . ?
O008 C00W C00Y 112.2(8) . . ?
C00S C00Y C00W 127.7(7) . . ?
C00S C00Y C01B 104.8(7) . . ?
C01B C00Y C00W 127.5(8) . . ?
N00F C010 C00V 108.1(7) . . ?
N00F C010 H010 126.4 . . ?
C00V C010 H010 125.5 . . ?
O006 C012 O00A 128.1(8) 10_557 . ?
O006 C012 C00V 122.4(8) 10_557 . ?
O00A C012 C00V 109.5(9) . . ?
N00P C016 C00V 111.7(8) . . ?
N00P C016 H016 124.0 . . ?
C00V C016 H016 124.2 . . ?
C00U C01A C01A 121.5(5) . 8_546 ?
C00U C01A H01A 117.8 . . ?
C01A C01A H01A 120.6 8_546 . ?
N00O C01B C00Y 110.0(8) . . ?
N00O C01B H01B 125.0 . . ?
C00Y C01B H01B 125.0 . . ?
C00U C01C C01C 119.7(5) . 8_546 ?
C00U C01C H01C 119.9 . . ?
C01C C01C H01C 120.4 8_546 . ?

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
Zr01 O004 C00W O008 8.7(13) . . . . ?
Zr01 O004 C00W C00Y -173.8(4) . . . . ?
Zr02 O008 C00W O004 -7.2(15) 11_655 . . . ?
Zr02 O008 C00W C00Y 175.1(5) 11_655 . . . ?
Zr02 O00A C012 O006 0.2(13) 2_654 . . 10_557 ?
Zr02 O00A C012 C00V -177.6(5) 2_654 . . . ?
O004 C00W C00Y C00S 179.4(7) . . . . ?
O004 C00W C00Y C01B 3.2(13) . . . . ?
O008 C00W C00Y C00S -2.7(12) . . . . ?
O008 C00W C00Y C01B -178.9(8) . . . . ?
N00D N00O C01B C00Y -2.4(10) . . . . ?
N00D C00S C00Y C00W -178.6(7) . . . . ?
N00D C00S C00Y C01B -1.7(9) . . . . ?
N00D C00T C00U C01A 38.3(10) . . . . ?
N00D C00T C00U C01C -143.6(8) . . . . ?
N00F N00P C016 C00V -1.8(10) . . . . ?
N00F C00T C00U C01A 165.4(7) . . . . ?
N00F C00T C00U C01C -16.5(11) . . . . ?
N00O N00D C00S C00Y 0.2(9) . . . . ?
N00O N00D C00T N00F 101.4(8) . . . . ?
N00O N00D C00T C00U -131.1(7) . . . . ?
N00P N00F C00T N00D 63.1(9) . . . . ?
N00P N00F C00T C00U -63.0(9) . . . . ?
N00P N00F C010 C00V -3.3(9) . . . . ?
C00S N00D N00O C01B 1.4(10) . . . . ?
C00S N00D C00T N00F -73.5(9) . . . . ?
C00S N00D C00T C00U 53.9(9) . . . . ?
C00S C00Y C01B N00O 2.6(10) . . . . ?
C00T N00D N00O C01B -174.1(7) . . . . ?
C00T N00D C00S C00Y 175.5(6) . . . . ?
C00T N00F N00P C016 -172.3(7) . . . . ?
C00T N00F C010 C00V 171.7(7) . . . . ?
C00T C00U C01A C01A 175.9(10) . . . 8_546 ?
C00T C00U C01C C01C -179.3(10) . . . 8_546 ?
C00W C00Y C01B N00O 179.5(8) . . . . ?
C010 N00F N00P C016 3.2(9) . . . . ?
C010 N00F C00T N00D -111.4(9) . . . . ?
C010 N00F C00T C00U 122.4(8) . . . . ?
C010 C00V C012 O006 169.8(8) . . . 10_557 ?
C010 C00V C012 O00A -12.3(12) . . . . ?
C010 C00V C016 N00P -0.1(10) . . . . ?
C012 C00V C010 N00F -173.7(8) . . . . ?
C012 C00V C016 N00P 176.0(7) . . . . ?
C016 C00V C010 N00F 2.0(9) . . . . ?
C016 C00V C012 O006 -5.2(13) . . . 10_557 ?
C016 C00V C012 O00A 172.7(8) . . . . ?
C01A C00U C01C C01C -1.2(17) . . . 8_546 ?
C01C C00U C01A C01A -2.3(16) . . . 8_546 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.222 -0.053 -0.171 8974.7 2100.5 '52 DMF'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT058_p21n_pl             
;
PROBLEM: Maximum Transmission Factor Missing ............          ?       
RESPONSE: XDS does not provide this data
;
_vrf_PLAT059_p21n_pl             
;
PROBLEM: Minimum Transmission Factor Missing ............          ?       
RESPONSE: XDS does not provide this data
;
# end Validation Reply Form
