# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 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. 
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data_cu_zhaoyang2023021101_0m
_database_code_depnum_ccdc_archive 'CCDC 2270600'
loop_
_audit_author_name
_audit_author_address
'Dongxu Cui'
;Northeast Normal University
China
;
_audit_update_record             
;
2023-06-18 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_audit_creation_date             2023-06-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H33 O13 Zr3, Cl, C4 H7 O'
_chemical_formula_sum            'C43 H40 Cl O14 Zr3'
_chemical_formula_weight         1089.86
_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 0.0181 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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.4744(4)
_cell_length_b                   10.9063(4)
_cell_length_c                   21.5947(8)
_cell_angle_alpha                83.359(2)
_cell_angle_beta                 86.050(2)
_cell_angle_gamma                72.183(2)
_cell_volume                     2331.37(15)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      62.444
_cell_measurement_theta_min      4.125
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.459
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56280
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        62.638
_diffrn_reflns_theta_max         62.638
_diffrn_reflns_theta_min         2.061
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5710
_reflns_number_total             7324
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.494
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         7324
_refine_ls_number_restraints     874
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0667
_refine_ls_restrained_S_all      1.093
_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)+(0.0870P)²+17.0615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1879
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{O01K, H01A}
{O2, H01E}
{O3, H9A}
{O40, H9B}
{O11, H01F}
{O01H, H01H}
3. Restrained distances
 C9-C01I
 1.5 with sigma of 0.02
 C9-O3
 1.2 with sigma of 0.02
 C01F-C011
 1.5 with sigma of 0.02
 C01F-O01K
 1.2 with sigma of 0.02
 O01K-C011
 2.5 with sigma of 0.02
 C01I-O3
 2.5 with sigma of 0.02
 C01M-O11
 1.2 with sigma of 0.02
 C01F-O2
 1.2 with sigma of 0.02
 O2-C011
 2.5 with sigma of 0.02
 O40-C01I
 2.5 with sigma of 0.02
 O11-C01A
 2.5 with sigma of 0.02
 O40-C9
 1.2 with sigma of 0.02
 O3-C9
 1.2 with sigma of 0.02
 O3-O40
 1.9 with sigma of 0.02
 O3-C01N
 2.8 with sigma of 0.02
 O40-C01L
 2.8 with sigma of 0.02
 O40-C01N
 3.5 with sigma of 0.02
 O3-C01L
 3.5 with sigma of 0.02
4. Restrained planarity
 O3, O40, C9, C01I
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C00F \\sim C00H \\sim C00I \\sim C00J \\sim C00K \\sim C00L \\sim C00M \\sim
C00N \\sim C00O \\sim C00P \\sim C00Q \\sim C00R \\sim C00S \\sim C00T \\sim
C00U \\sim C00V \\sim C00W \\sim C00X \\sim C00Y \\sim C00Z \\sim C010 \\sim
C011 \\sim C012 \\sim C013 \\sim C014 \\sim C015 \\sim C016 \\sim C017 \\sim
C018 \\sim C019 \\sim C01A \\sim C01B \\sim C01C \\sim C01D \\sim C01E \\sim
C01G \\sim C01I \\sim C01J \\sim O01K \\sim C01L \\sim C01M \\sim C01N \\sim
C9: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
Cl00 \\sim O005 \\sim O006 \\sim O007 \\sim O008 \\sim O009 \\sim O00A \\sim
O00B \\sim O00C \\sim O00D \\sim O00E \\sim O00G \\sim C01F \\sim O01H \\sim
O3: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
C00F \\sim C00H \\sim C00I \\sim C00J \\sim C00K \\sim C00L \\sim C00M \\sim
C00N \\sim C00O \\sim C00P \\sim C00Q \\sim C00R \\sim C00S \\sim C00T \\sim
C00U \\sim C00V \\sim C00W \\sim C00X \\sim C00Y \\sim C00Z \\sim C010 \\sim
C011 \\sim C012 \\sim C013 \\sim C014 \\sim C015 \\sim C016 \\sim C017 \\sim
C018 \\sim C019 \\sim C01A \\sim C01B \\sim C01C \\sim C01D \\sim C01E \\sim
C01F \\sim C01G \\sim C01I \\sim C01J \\sim C01L \\sim C01M \\sim C01N \\sim
C9: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03
O005 \\sim O006 \\sim O007 \\sim O008 \\sim O009 \\sim O00A \\sim O00B \\sim
O00C \\sim O00D \\sim O00E \\sim O00G \\sim O01H \\sim O01K \\sim O3 \\sim O2
\\sim O11 \\sim O40: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.03
: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C01F) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uiso(O01K) = Uiso(H01A)
Uiso(O2) = Uiso(H01E)
Uiso(O3) = Uiso(H9A)
Uiso(O40) = Uiso(H9B)
Uiso(O11) = Uiso(H01F)
Uiso(O01H) = Uiso(H01H)
6. Others
 Fixed Sof: O01H(0.5) O01K(0.5) O3(0.5) O2(0.5) O11(0.5) O40(0.5) H01A(0.5)
 H01E(0.5) H9A(0.5) H9B(0.5) H01F(0.5) H01H(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 O005(H005), O007(H007), O009(H009), C00K(H00K), C00N(H00N), C00O(H00O),
 C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U), C00V(H00V),
 C00W(H00W), C00Y(H00Y), C00Z(H00Z), C010(H010), C012(H012), C013(H013),
 C014(H014), C015(H015), C016(H016), C017(H017), C018(H018), C019(H019),
 C01B(H01B), C01C(H01C), C01D(H01D), C01G(H01G), C01J(H01J), C01L(H01L),
 C01N(H01N)
7.b Idealised Me refined as rotating group:
 C00P(H00A,H00B,H00C), C00X(H00D,H00E,H00F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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 0.51971(7) 0.65763(6) 0.86666(3) 0.0350(2) Uani 1 1 d . . . . .
Zr02 Zr 0.58352(7) 0.38977(7) 0.79404(3) 0.0401(2) Uani 1 1 d . . . . .
Zr03 Zr 0.26590(7) 0.56859(7) 0.81953(3) 0.0409(2) Uani 1 1 d . . . . .
Cl00 Cl 0.1815(2) 0.6943(2) 1.02151(10) 0.0565(6) Uani 1 1 d . U . . .
O005 O 0.3359(5) 0.6243(5) 0.8988(2) 0.0399(12) Uani 1 1 d . U . . .
H005 H 0.295318 0.632204 0.938431 0.048 Uiso 1 1 calc R . . . .
O006 O 0.4586(5) 0.5769(5) 0.7958(2) 0.0388(11) Uani 1 1 d . U . . .
O007 O 0.6265(5) 0.4573(5) 0.8758(2) 0.0391(12) Uani 1 1 d . U . . .
H007 H 0.680006 0.409982 0.908231 0.047 Uiso 1 1 calc R . . . .
O008 O 0.6665(6) 0.6764(6) 0.7929(3) 0.0484(13) Uani 1 1 d . U . . .
O009 O 0.3953(6) 0.3771(5) 0.8329(3) 0.0447(12) Uani 1 1 d . U . . .
H009 H 0.374698 0.303958 0.851534 0.054 Uiso 1 1 calc R . . . .
O00A O 0.3934(6) 0.8336(5) 0.8140(3) 0.0487(13) Uani 1 1 d . U . . .
O00B O 0.2231(6) 0.7733(6) 0.7840(3) 0.0518(14) Uani 1 1 d . U . . .
O00C O 0.4916(7) 0.4217(6) 0.7032(3) 0.0559(15) Uani 1 1 d . U . . .
O00D O 0.7115(6) 0.4995(6) 0.7427(3) 0.0518(14) Uani 1 1 d . U . . .
O00E O 0.2796(7) 0.5428(6) 0.7191(3) 0.0561(14) Uani 1 1 d . U . . .
C00F C 0.1962(8) 0.0859(8) 0.9461(4) 0.0362(17) Uani 1 1 d . U . . .
O00G O 0.3251(8) 0.1680(7) 0.8756(4) 0.075(2) Uani 1 1 d . U . . .
C00H C 0.7117(12) 0.6135(12) 0.7465(5) 0.068(2) Uani 1 1 d . U . . .
C00I C 0.2929(12) 0.8499(10) 0.7815(5) 0.062(2) Uani 1 1 d . U . . .
C00J C 0.2517(12) 0.9687(10) 0.7371(5) 0.068(2) Uani 1 1 d . U . . .
C00K C 0.4797(11) 0.7770(10) 0.9635(5) 0.062(2) Uani 1 1 d . U . . .
H00K H 0.392314 0.805751 0.979726 0.074 Uiso 1 1 calc R . . . .
C00L C 0.7678(13) 0.6834(12) 0.6937(5) 0.076(2) Uani 1 1 d . U . . .
C00M C 0.3830(17) 0.5037(15) 0.6862(6) 0.100(3) Uani 1 1 d . U . . .
C00N C 0.2867(11) 0.1440(10) 0.9305(5) 0.064(2) Uani 1 1 d . U . . .
H00N H 0.325383 0.169537 0.962248 0.076 Uiso 1 1 calc R . . . .
C00O C 0.5421(11) 0.8442(10) 0.9198(5) 0.063(2) Uani 1 1 d . U . . .
H00O H 0.502993 0.927454 0.901160 0.076 Uiso 1 1 calc R . . . .
C00P C 0.1556(11) 0.0626(11) 1.0103(5) 0.067(3) Uani 1 1 d . U . . .
H00A H 0.173742 -0.028748 1.021281 0.100 Uiso 1 1 calc GR . . . .
H00B H 0.061225 0.104987 1.015882 0.100 Uiso 1 1 calc GR . . . .
H00C H 0.204635 0.096207 1.036480 0.100 Uiso 1 1 calc GR . . . .
C00Q C 0.3148(13) 1.0621(11) 0.7352(6) 0.080(2) Uani 1 1 d . U . . .
H00Q H 0.384758 1.049977 0.761753 0.096 Uiso 1 1 calc R . . . .
C00R C 0.6928(11) 0.6554(11) 0.9449(5) 0.068(2) Uani 1 1 d . U . . .
H00R H 0.773302 0.588666 0.947046 0.082 Uiso 1 1 calc R . . . .
C00S C 0.5758(11) 0.6551(10) 0.9788(5) 0.064(2) Uani 1 1 d . U . . .
H00S H 0.562567 0.587635 1.006333 0.077 Uiso 1 1 calc R . . . .
C00T C 0.7635(14) 0.8113(13) 0.6966(6) 0.088(2) Uani 1 1 d . U . . .
H00T H 0.725908 0.852770 0.731701 0.105 Uiso 1 1 calc R . . . .
C00U C 0.6706(11) 0.7691(11) 0.9081(5) 0.064(2) Uani 1 1 d . U . . .
H00U H 0.732387 0.792094 0.879787 0.077 Uiso 1 1 calc R . . . .
C00V C 0.1436(13) 0.9897(11) 0.6989(5) 0.080(2) Uani 1 1 d . U . . .
H00V H 0.097585 0.928661 0.700508 0.096 Uiso 1 1 calc R . . . .
C00W C 0.0986(11) 0.4927(13) 0.8918(6) 0.081(2) Uani 1 1 d . U . . .
H00W H 0.128763 0.443653 0.929008 0.098 Uiso 1 1 calc R . . . .
C00X C 0.1271(12) 0.0467(12) 0.9012(5) 0.077(3) Uani 1 1 d . U . . .
H00D H 0.036411 0.102774 0.899263 0.116 Uiso 1 1 calc GR . . . .
H00E H 0.126619 -0.040730 0.913130 0.116 Uiso 1 1 calc GR . . . .
H00F H 0.171559 0.051709 0.861060 0.116 Uiso 1 1 calc GR . . . .
C00Y C 0.0432(11) 0.5423(14) 0.7955(6) 0.082(2) Uani 1 1 d . U . . .
H00Y H 0.027832 0.533734 0.754525 0.098 Uiso 1 1 calc R . . . .
C00Z C 0.0140(11) 0.6572(14) 0.8196(6) 0.082(3) Uani 1 1 d . U . . .
H00Z H -0.021556 0.739190 0.798901 0.099 Uiso 1 1 calc R . . . .
C010 C 0.0501(11) 0.6256(14) 0.8846(6) 0.082(2) Uani 1 1 d . U . . .
H010 H 0.042064 0.682441 0.914631 0.098 Uiso 1 1 calc R . . . .
C011 C 0.1736(14) 1.1912(11) 0.6581(6) 0.087(2) Uani 1 1 d D U . . .
C012 C 0.0965(12) 0.4426(14) 0.8373(6) 0.083(2) Uani 1 1 d . U . . .
H012 H 0.126557 0.355582 0.830381 0.099 Uiso 1 1 calc R . . . .
C013 C 0.8091(16) 0.2193(12) 0.8024(8) 0.099(3) Uani 1 1 d . U . . .
H013 H 0.881811 0.246701 0.810093 0.119 Uiso 1 1 calc R . . . .
C014 C 0.7261(16) 0.1786(11) 0.8463(7) 0.097(3) Uani 1 1 d . U . . .
H014 H 0.731165 0.172942 0.889407 0.116 Uiso 1 1 calc R . . . .
C015 C 0.1053(14) 1.1011(12) 0.6588(6) 0.084(2) Uani 1 1 d . U . . .
H015 H 0.034339 1.115495 0.632568 0.101 Uiso 1 1 calc R . . . .
C016 C 0.6643(16) 0.1702(11) 0.7513(7) 0.092(3) Uani 1 1 d . U . . .
H016 H 0.619784 0.157536 0.717938 0.110 Uiso 1 1 calc R . . . .
C017 C 0.8285(14) 0.6202(14) 0.6420(6) 0.093(2) Uani 1 1 d . U . . .
H017 H 0.833745 0.534031 0.640037 0.112 Uiso 1 1 calc R . . . .
C018 C 0.6303(15) 0.1468(11) 0.8124(7) 0.095(3) Uani 1 1 d . U . . .
H018 H 0.559712 0.116534 0.828665 0.114 Uiso 1 1 calc R . . . .
C019 C 0.2777(14) 1.1723(12) 0.6954(6) 0.087(2) Uani 1 1 d . U . . .
H019 H 0.323346 1.233599 0.693849 0.104 Uiso 1 1 calc R . . . .
C01A C 0.8690(15) 0.8159(14) 0.5974(6) 0.098(2) Uani 1 1 d D U . . .
C01B C 0.8151(15) 0.8774(14) 0.6473(6) 0.094(2) Uani 1 1 d . U . . .
H01B H 0.812191 0.963055 0.649053 0.113 Uiso 1 1 calc R . . . .
C01C C 0.7662(16) 0.2121(12) 0.7464(8) 0.100(3) Uani 1 1 d . U . . .
H01C H 0.805564 0.234714 0.708602 0.120 Uiso 1 1 calc R . . . .
C01D C 0.8807(15) 0.6865(14) 0.5937(6) 0.096(2) Uani 1 1 d . U . . .
H01D H 0.923093 0.645298 0.559146 0.115 Uiso 1 1 calc R . . . .
C01E C 0.388(2) 0.5713(18) 0.6213(7) 0.137(3) Uani 1 1 d . U . . .
C01F C 0.1339(14) 1.3150(13) 0.6130(7) 0.096(3) Uani 1 1 d D U . . .
C01G C 0.269(2) 0.6460(18) 0.5922(8) 0.145(3) Uani 1 1 d . U . . .
H01G H 0.187184 0.658371 0.614005 0.174 Uiso 1 1 calc R . . . .
O01H O 0.965(3) 0.852(2) 0.4974(12) 0.150(8) Uiso 0.5 1 d . U P A 3
C01I C 0.400(2) 0.692(2) 0.5051(7) 0.156(4) Uani 1 1 d D U . . .
C01J C 0.521(2) 0.5553(19) 0.5886(8) 0.142(3) Uani 1 1 d . U . . .
H01J H 0.600642 0.504811 0.606791 0.171 Uiso 1 1 calc R . . . .
O01K O 0.202(2) 1.3867(18) 0.5979(10) 0.129(6) Uiso 0.5 1 d D U P B 3
C01L C 0.519(2) 0.6231(19) 0.5268(7) 0.156(4) Uani 1 1 d D U . . .
H01L H 0.598084 0.618692 0.503258 0.188 Uiso 1 1 calc R . . . .
C01M C 0.9194(18) 0.8975(16) 0.5454(7) 0.111(3) Uani 1 1 d D U . . .
C01N C 0.273(2) 0.7022(19) 0.5302(7) 0.154(4) Uani 1 1 d D U . . .
H01N H 0.195715 0.742941 0.508022 0.184 Uiso 1 1 calc R . . . .
O3 O 0.308(2) 0.809(3) 0.4066(10) 0.267(17) Uiso 0.5 1 d D U P C 3
C9 C 0.4029(19) 0.7612(16) 0.4384(7) 0.163(4) Uani 1 1 d D U . . .
O2 O 0.029(3) 1.357(3) 0.5850(14) 0.209(12) Uiso 0.5 1 d D U P B 3
O11 O 0.904(5) 1.016(2) 0.5423(19) 0.302(18) Uiso 0.5 1 d D U P A 3
O40 O 0.496(3) 0.783(4) 0.4118(13) 0.36(2) Uiso 0.5 1 d D U P C 3
H01A H 0.202(2) 1.3867(18) 0.5979(10) 0.129(6) Uiso 0.5 1 d . . P D 4
H01E H 0.029(3) 1.357(3) 0.5850(14) 0.209(12) Uiso 0.5 1 d . . P E 4
H9A H 0.308(2) 0.809(3) 0.4066(10) 0.267(17) Uiso 0.5 1 d . . P F 4
H9B H 0.496(3) 0.783(4) 0.4118(13) 0.36(2) Uiso 0.5 1 d . . P G 4
H01F H 0.904(5) 1.016(2) 0.5423(19) 0.302(18) Uiso 0.5 1 d . . P H 4
H01H H 0.965(3) 0.852(2) 0.4974(12) 0.150(8) Uiso 0.5 1 d . . P I 4


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr01 Zr02 3.3407(10) . ?
Zr01 Zr03 3.3508(10) . ?
Zr01 O005 2.123(5) . ?
Zr01 O006 2.077(5) . ?
Zr01 O007 2.121(5) . ?
Zr01 O008 2.173(6) . ?
Zr01 O00A 2.208(6) . ?
Zr01 C00K 2.534(10) . ?
Zr01 C00O 2.526(10) . ?
Zr01 C00R 2.555(10) . ?
Zr01 C00S 2.525(10) . ?
Zr01 C00U 2.530(10) . ?
Zr02 Zr03 3.3466(11) . ?
Zr02 O006 2.063(5) . ?
Zr02 O007 2.115(5) . ?
Zr02 O009 2.126(6) . ?
Zr02 O00C 2.190(6) . ?
Zr02 O00D 2.220(6) . ?
Zr02 C013 2.523(13) . ?
Zr02 C014 2.517(11) . ?
Zr02 C016 2.543(12) . ?
Zr02 C018 2.532(12) . ?
Zr02 C01C 2.530(13) . ?
Zr03 O005 2.127(5) . ?
Zr03 O006 2.075(5) . ?
Zr03 O009 2.113(6) . ?
Zr03 O00B 2.194(6) . ?
Zr03 O00E 2.208(6) . ?
Zr03 C00W 2.530(11) . ?
Zr03 C00Y 2.531(11) . ?
Zr03 C00Z 2.517(11) . ?
Zr03 C010 2.526(12) . ?
Zr03 C012 2.541(11) . ?
O008 C00H 1.263(13) . ?
O00A C00I 1.261(12) . ?
O00B C00I 1.262(12) . ?
O00C C00M 1.261(16) . ?
O00D C00H 1.255(12) . ?
O00E C00M 1.242(16) . ?
C00F C00N 1.300(13) . ?
C00F C00P 1.439(13) . ?
C00F C00X 1.423(13) . ?
O00G C00N 1.248(12) . ?
C00H C00L 1.486(14) . ?
C00I C00J 1.488(13) . ?
C00J C00Q 1.369(16) . ?
C00J C00V 1.393(16) . ?
C00K C00O 1.380(15) . ?
C00K C00S 1.419(15) . ?
C00L C00T 1.390(17) . ?
C00L C017 1.392(17) . ?
C00M C01E 1.511(19) . ?
C00O C00U 1.368(15) . ?
C00Q C019 1.363(15) . ?
C00R C00S 1.383(15) . ?
C00R C00U 1.359(15) . ?
C00T C01B 1.387(16) . ?
C00V C015 1.376(15) . ?
C00W C010 1.375(18) . ?
C00W C012 1.358(18) . ?
C00Y C00Z 1.353(18) . ?
C00Y C012 1.333(17) . ?
C00Z C010 1.455(18) . ?
C011 C015 1.380(17) . ?
C011 C019 1.350(17) . ?
C011 C01F 1.534(13) . ?
C013 C014 1.37(2) . ?
C013 C01C 1.34(2) . ?
C014 C018 1.43(2) . ?
C016 C018 1.359(19) . ?
C016 C01C 1.28(2) . ?
C017 C01D 1.378(16) . ?
C01A C01B 1.336(19) . ?
C01A C01D 1.390(19) . ?
C01A C01M 1.518(17) . ?
C01E C01G 1.41(2) . ?
C01E C01J 1.49(3) . ?
C01F O01K 1.214(14) . ?
C01F O2 1.222(16) . ?
C01G C01N 1.41(2) . ?
O01H C01M 1.21(3) . ?
C01I C01L 1.33(2) . ?
C01I C01N 1.38(2) . ?
C01I C9 1.549(14) . ?
C01J C01L 1.45(2) . ?
C01M O11 1.241(18) . ?
O3 C9 1.197(13) . ?
C9 O40 1.168(16) . ?

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 Zr03 60.02(2) . . ?
O005 Zr01 Zr02 86.73(15) . . ?
O005 Zr01 Zr03 38.00(15) . . ?
O005 Zr01 O008 151.8(2) . . ?
O005 Zr01 O00A 85.5(2) . . ?
O005 Zr01 C00K 81.6(3) . . ?
O005 Zr01 C00O 107.9(3) . . ?
O005 Zr01 C00R 119.9(3) . . ?
O005 Zr01 C00S 88.8(3) . . ?
O005 Zr01 C00U 134.1(3) . . ?
O006 Zr01 Zr02 36.05(15) . . ?
O006 Zr01 Zr03 36.17(15) . . ?
O006 Zr01 O005 73.6(2) . . ?
O006 Zr01 O007 73.2(2) . . ?
O006 Zr01 O008 79.1(2) . . ?
O006 Zr01 O00A 79.4(2) . . ?
O006 Zr01 C00K 153.5(3) . . ?
O006 Zr01 C00O 153.9(3) . . ?
O006 Zr01 C00R 150.9(3) . . ?
O006 Zr01 C00S 151.7(3) . . ?
O006 Zr01 C00U 151.7(3) . . ?
O007 Zr01 Zr02 37.87(14) . . ?
O007 Zr01 Zr03 85.86(15) . . ?
O007 Zr01 O005 92.8(2) . . ?
O007 Zr01 O008 86.2(2) . . ?
O007 Zr01 O00A 151.9(2) . . ?
O007 Zr01 C00K 118.0(3) . . ?
O007 Zr01 C00O 131.8(3) . . ?
O007 Zr01 C00R 80.2(3) . . ?
O007 Zr01 C00S 86.0(3) . . ?
O007 Zr01 C00U 105.8(3) . . ?
O008 Zr01 Zr02 75.18(16) . . ?
O008 Zr01 Zr03 113.90(16) . . ?
O008 Zr01 O00A 82.4(2) . . ?
O008 Zr01 C00K 123.6(3) . . ?
O008 Zr01 C00O 93.4(3) . . ?
O008 Zr01 C00R 87.8(3) . . ?
O008 Zr01 C00S 119.2(3) . . ?
O008 Zr01 C00U 72.6(3) . . ?
O00A Zr01 Zr02 114.06(16) . . ?
O00A Zr01 Zr03 75.56(16) . . ?
O00A Zr01 C00K 89.6(3) . . ?
O00A Zr01 C00O 74.7(3) . . ?
O00A Zr01 C00R 124.7(3) . . ?
O00A Zr01 C00S 122.0(3) . . ?
O00A Zr01 C00U 95.2(3) . . ?
C00K Zr01 Zr02 152.7(3) . . ?
C00K Zr01 Zr03 117.8(2) . . ?
C00K Zr01 C00R 52.6(4) . . ?
C00O Zr01 Zr02 163.9(3) . . ?
C00O Zr01 Zr03 136.0(3) . . ?
C00O Zr01 C00K 31.7(3) . . ?
C00O Zr01 C00R 51.6(3) . . ?
C00O Zr01 C00U 31.4(3) . . ?
C00R Zr01 Zr02 115.5(3) . . ?
C00R Zr01 Zr03 153.4(3) . . ?
C00S Zr01 Zr02 123.2(2) . . ?
C00S Zr01 Zr03 125.4(3) . . ?
C00S Zr01 C00K 32.6(3) . . ?
C00S Zr01 C00O 52.6(3) . . ?
C00S Zr01 C00R 31.6(3) . . ?
C00S Zr01 C00U 52.3(4) . . ?
C00U Zr01 Zr02 132.6(3) . . ?
C00U Zr01 Zr03 167.3(3) . . ?
C00U Zr01 C00K 52.6(3) . . ?
C00U Zr01 C00R 31.0(3) . . ?
Zr01 Zr02 Zr03 60.14(2) . . ?
O006 Zr02 Zr01 36.35(15) . . ?
O006 Zr02 Zr03 36.13(14) . . ?
O006 Zr02 O007 73.6(2) . . ?
O006 Zr02 O009 73.2(2) . . ?
O006 Zr02 O00C 78.9(2) . . ?
O006 Zr02 O00D 79.3(2) . . ?
O006 Zr02 C013 152.9(4) . . ?
O006 Zr02 C014 152.3(4) . . ?
O006 Zr02 C016 153.3(4) . . ?
O006 Zr02 C018 152.2(4) . . ?
O006 Zr02 C01C 153.8(4) . . ?
O007 Zr02 Zr01 38.01(14) . . ?
O007 Zr02 Zr03 86.07(15) . . ?
O007 Zr02 O009 91.8(2) . . ?
O007 Zr02 O00C 151.8(2) . . ?
O007 Zr02 O00D 86.6(2) . . ?
O007 Zr02 C013 87.7(4) . . ?
O007 Zr02 C014 81.0(4) . . ?
O007 Zr02 C016 132.6(3) . . ?
O007 Zr02 C018 108.7(4) . . ?
O007 Zr02 C01C 117.9(4) . . ?
O009 Zr02 Zr01 85.93(16) . . ?
O009 Zr02 Zr03 37.72(15) . . ?
O009 Zr02 O00C 86.2(2) . . ?
O009 Zr02 O00D 151.7(2) . . ?
O009 Zr02 C013 128.0(4) . . ?
O009 Zr02 C014 97.1(4) . . ?
O009 Zr02 C016 97.9(4) . . ?
O009 Zr02 C018 79.1(4) . . ?
O009 Zr02 C01C 126.5(4) . . ?
O00C Zr02 Zr01 113.88(17) . . ?
O00C Zr02 Zr03 75.24(18) . . ?
O00C Zr02 O00D 82.1(2) . . ?
O00C Zr02 C013 115.5(4) . . ?
O00C Zr02 C014 127.1(4) . . ?
O00C Zr02 C016 75.3(4) . . ?
O00C Zr02 C018 98.5(4) . . ?
O00C Zr02 C01C 85.0(4) . . ?
O00D Zr02 Zr01 75.51(17) . . ?
O00D Zr02 Zr03 114.02(16) . . ?
O00D Zr02 C013 80.3(4) . . ?
O00D Zr02 C014 110.5(4) . . ?
O00D Zr02 C016 103.9(4) . . ?
O00D Zr02 C018 128.1(4) . . ?
O00D Zr02 C01C 78.1(4) . . ?
C013 Zr02 Zr01 120.4(4) . . ?
C013 Zr02 Zr03 164.0(4) . . ?
C013 Zr02 C016 50.5(5) . . ?
C013 Zr02 C018 52.5(5) . . ?
C013 Zr02 C01C 30.7(5) . . ?
C014 Zr02 Zr01 119.0(3) . . ?
C014 Zr02 Zr03 132.6(4) . . ?
C014 Zr02 C013 31.5(4) . . ?
C014 Zr02 C016 51.9(5) . . ?
C014 Zr02 C018 32.8(5) . . ?
C014 Zr02 C01C 51.2(5) . . ?
C016 Zr02 Zr01 170.3(3) . . ?
C016 Zr02 Zr03 127.4(4) . . ?
C018 Zr02 Zr01 143.3(4) . . ?
C018 Zr02 Zr03 116.2(4) . . ?
C018 Zr02 C016 31.1(4) . . ?
C01C Zr02 Zr01 144.7(4) . . ?
C01C Zr02 Zr03 154.6(4) . . ?
C01C Zr02 C016 29.2(4) . . ?
C01C Zr02 C018 50.6(5) . . ?
Zr02 Zr03 Zr01 59.84(2) . . ?
O005 Zr03 Zr01 37.92(14) . . ?
O005 Zr03 Zr02 86.51(15) . . ?
O005 Zr03 O00B 84.7(2) . . ?
O005 Zr03 O00E 151.2(2) . . ?
O005 Zr03 C00W 88.0(3) . . ?
O005 Zr03 C00Y 132.9(3) . . ?
O005 Zr03 C00Z 109.0(4) . . ?
O005 Zr03 C010 80.7(3) . . ?
O005 Zr03 C012 118.2(3) . . ?
O006 Zr03 Zr01 36.22(15) . . ?
O006 Zr03 Zr02 35.89(15) . . ?
O006 Zr03 O005 73.6(2) . . ?
O006 Zr03 O009 73.2(2) . . ?
O006 Zr03 O00B 79.6(2) . . ?
O006 Zr03 O00E 78.8(2) . . ?
O006 Zr03 C00W 151.8(3) . . ?
O006 Zr03 C00Y 153.3(3) . . ?
O006 Zr03 C00Z 153.7(3) . . ?
O006 Zr03 C010 152.6(3) . . ?
O006 Zr03 C012 150.7(4) . . ?
O009 Zr03 Zr01 85.88(16) . . ?
O009 Zr03 Zr02 38.00(15) . . ?
O009 Zr03 O005 92.7(2) . . ?
O009 Zr03 O00B 152.2(2) . . ?
O009 Zr03 O00E 86.8(2) . . ?
O009 Zr03 C00W 86.9(3) . . ?
O009 Zr03 C00Y 104.3(4) . . ?
O009 Zr03 C00Z 131.6(4) . . ?
O009 Zr03 C010 117.8(4) . . ?
O009 Zr03 C012 79.3(4) . . ?
O00B Zr03 Zr01 75.15(16) . . ?
O00B Zr03 Zr02 114.21(17) . . ?
O00B Zr03 O00E 82.5(2) . . ?
O00B Zr03 C00W 120.6(4) . . ?
O00B Zr03 C00Y 97.5(4) . . ?
O00B Zr03 C00Z 74.7(3) . . ?
O00B Zr03 C010 89.2(4) . . ?
O00B Zr03 C012 126.1(4) . . ?
O00E Zr03 Zr01 113.49(18) . . ?
O00E Zr03 Zr02 75.48(18) . . ?
O00E Zr03 C00W 120.7(4) . . ?
O00E Zr03 C00Y 74.5(4) . . ?
O00E Zr03 C00Z 92.4(4) . . ?
O00E Zr03 C010 124.7(3) . . ?
O00E Zr03 C012 90.0(4) . . ?
C00W Zr03 Zr01 124.7(3) . . ?
C00W Zr03 Zr02 124.1(3) . . ?
C00W Zr03 C00Y 50.5(4) . . ?
C00W Zr03 C012 31.1(4) . . ?
C00Y Zr03 Zr01 167.7(3) . . ?
C00Y Zr03 Zr02 132.4(3) . . ?
C00Y Zr03 C012 30.5(4) . . ?
C00Z Zr03 Zr01 136.8(3) . . ?
C00Z Zr03 Zr02 163.3(3) . . ?
C00Z Zr03 C00W 52.6(4) . . ?
C00Z Zr03 C00Y 31.1(4) . . ?
C00Z Zr03 C010 33.5(4) . . ?
C00Z Zr03 C012 52.3(4) . . ?
C010 Zr03 Zr01 116.8(3) . . ?
C010 Zr03 Zr02 152.2(3) . . ?
C010 Zr03 C00W 31.6(4) . . ?
C010 Zr03 C00Y 52.5(4) . . ?
C010 Zr03 C012 52.8(4) . . ?
C012 Zr03 Zr01 151.4(3) . . ?
C012 Zr03 Zr02 115.2(3) . . ?
Zr01 O005 Zr03 104.1(2) . . ?
Zr02 O006 Zr01 107.6(2) . . ?
Zr02 O006 Zr03 108.0(2) . . ?
Zr03 O006 Zr01 107.6(2) . . ?
Zr02 O007 Zr01 104.1(2) . . ?
C00H O008 Zr01 132.0(6) . . ?
Zr03 O009 Zr02 104.3(2) . . ?
C00I O00A Zr01 130.5(6) . . ?
C00I O00B Zr03 131.6(6) . . ?
C00M O00C Zr02 128.1(7) . . ?
C00H O00D Zr02 129.4(6) . . ?
C00M O00E Zr03 127.5(7) . . ?
C00N C00F C00P 121.4(9) . . ?
C00N C00F C00X 122.6(9) . . ?
C00X C00F C00P 115.9(8) . . ?
O008 C00H C00L 115.5(10) . . ?
O00D C00H O008 124.7(9) . . ?
O00D C00H C00L 119.8(11) . . ?
O00A C00I O00B 125.0(9) . . ?
O00A C00I C00J 118.0(9) . . ?
O00B C00I C00J 116.9(9) . . ?
C00Q C00J C00I 120.7(10) . . ?
C00Q C00J C00V 118.9(10) . . ?
C00V C00J C00I 120.3(10) . . ?
C00O C00K Zr01 73.9(6) . . ?
C00O C00K C00S 106.2(10) . . ?
C00S C00K Zr01 73.4(6) . . ?
C00T C00L C00H 120.1(11) . . ?
C00T C00L C017 119.7(11) . . ?
C017 C00L C00H 120.3(11) . . ?
O00C C00M C01E 114.9(14) . . ?
O00E C00M O00C 126.6(11) . . ?
O00E C00M C01E 118.0(13) . . ?
O00G C00N C00F 124.4(10) . . ?
C00K C00O Zr01 74.5(6) . . ?
C00U C00O Zr01 74.5(6) . . ?
C00U C00O C00K 109.3(10) . . ?
C019 C00Q C00J 121.7(12) . . ?
C00S C00R Zr01 73.0(6) . . ?
C00U C00R Zr01 73.5(6) . . ?
C00U C00R C00S 108.8(10) . . ?
C00K C00S Zr01 74.0(6) . . ?
C00R C00S Zr01 75.4(6) . . ?
C00R C00S C00K 107.2(10) . . ?
C01B C00T C00L 120.4(13) . . ?
C00O C00U Zr01 74.1(6) . . ?
C00R C00U Zr01 75.5(6) . . ?
C00R C00U C00O 108.5(11) . . ?
C015 C00V C00J 119.6(12) . . ?
C010 C00W Zr03 74.0(7) . . ?
C012 C00W Zr03 74.9(7) . . ?
C012 C00W C010 111.0(13) . . ?
C00Z C00Y Zr03 73.9(7) . . ?
C012 C00Y Zr03 75.2(7) . . ?
C012 C00Y C00Z 112.2(13) . . ?
C00Y C00Z Zr03 75.0(7) . . ?
C00Y C00Z C010 105.5(12) . . ?
C010 C00Z Zr03 73.6(6) . . ?
C00W C010 Zr03 74.4(7) . . ?
C00W C010 C00Z 104.4(12) . . ?
C00Z C010 Zr03 72.9(7) . . ?
C015 C011 C01F 119.9(11) . . ?
C019 C011 C015 121.7(11) . . ?
C019 C011 C01F 118.4(12) . . ?
C00W C012 Zr03 74.0(7) . . ?
C00Y C012 Zr03 74.3(7) . . ?
C00Y C012 C00W 106.7(13) . . ?
C014 C013 Zr02 74.0(8) . . ?
C01C C013 Zr02 74.9(8) . . ?
C01C C013 C014 107.2(16) . . ?
C013 C014 Zr02 74.5(7) . . ?
C013 C014 C018 106.0(14) . . ?
C018 C014 Zr02 74.2(7) . . ?
C00V C015 C011 119.1(12) . . ?
C018 C016 Zr02 74.0(7) . . ?
C01C C016 Zr02 74.8(8) . . ?
C01C C016 C018 110.2(15) . . ?
C01D C017 C00L 119.4(13) . . ?
C014 C018 Zr02 73.0(7) . . ?
C016 C018 Zr02 74.9(7) . . ?
C016 C018 C014 105.2(14) . . ?
C011 C019 C00Q 119.0(13) . . ?
C01B C01A C01D 122.7(12) . . ?
C01B C01A C01M 114.8(13) . . ?
C01D C01A C01M 122.5(13) . . ?
C01A C01B C00T 118.8(14) . . ?
C013 C01C Zr02 74.4(8) . . ?
C016 C01C Zr02 76.0(9) . . ?
C016 C01C C013 111.4(16) . . ?
C017 C01D C01A 119.0(14) . . ?
C01G C01E C00M 120.4(18) . . ?
C01G C01E C01J 120.9(16) . . ?
C01J C01E C00M 118.7(15) . . ?
O01K C01F C011 126.0(14) . . ?
O01K C01F O2 108(2) . . ?
O2 C01F C011 125.7(17) . . ?
C01N C01G C01E 120.6(19) . . ?
C01L C01I C01N 130.0(14) . . ?
C01L C01I C9 115.2(15) . . ?
C01N C01I C9 114.5(14) . . ?
C01L C01J C01E 116.0(17) . . ?
C01I C01L C01J 117.1(18) . . ?
O01H C01M C01A 119.7(19) . . ?
O01H C01M O11 113(3) . . ?
O11 C01M C01A 127(2) . . ?
C01I C01N C01G 114.8(17) . . ?
O3 C9 C01I 125.4(15) . . ?
O40 C9 C01I 126.5(15) . . ?
O40 C9 O3 107.9(15) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT220_cu_zhaoyang2023021101_0m 
;
PROBLEM: NonSolvent   Resd 1  O   Ueq(max)/Ueq(min) Range        9.3 Ratio 
RESPONSE: The molecules in the crystal are not packed very tightly, owing to 
the presence of a lot of disord ered solvent molecules. Consequently, high 
thermal motion of some atoms in the molecules is expected.
;
_vrf_PLAT242_cu_zhaoyang2023021101_0m 
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         C9 Check 
RESPONSE: The molecules in the crystal are not packed very tightly, owing to
 the presence of a lot of disord ered solvent molecules. Consequently, high
 thermal motion of some atoms in the molecules is expected.
;
_vrf_PLAT601_cu_zhaoyang2023021101_0m 
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        144 Ang**3
RESPONSE: Structure is porous.
;
# end Validation Reply Form
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 2270602'
loop_
_audit_author_name
_audit_author_address
'Dongxu Cui'
;Northeast Normal University
China
;
_audit_update_record             
;
2023-06-18 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_audit_creation_date             2023-06-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C78 H66 N6 O20 Zr6, 2(Cl), 2(O)'
_chemical_formula_sum            'C78 H66 Cl2 N6 O22 Zr6'
_chemical_formula_weight         2057.58
_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 0.0181 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'
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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   45.504(9)
_cell_length_b                   17.800(3)
_cell_length_c                   15.373(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.940(10)
_cell_angle_gamma                90
_cell_volume                     12265(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      37.638
_cell_measurement_theta_min      2.671
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.861
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            ?
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4104
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            25401
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        38.080
_diffrn_reflns_theta_max         38.080
_diffrn_reflns_theta_min         2.671
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2538
_reflns_number_total             3250
_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       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.925
_refine_diff_density_min         -1.340
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         3250
_refine_ls_number_restraints     1266
_refine_ls_R_factor_all          0.1364
_refine_ls_R_factor_gt           0.1154
_refine_ls_restrained_S_all      0.900
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1727P)²+1312.5455P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2962
_refine_ls_wR_factor_ref         0.3153
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Restrained distances
 C31-C19
 1.45 with sigma of 0.01
 N2-C19
 1.25 with sigma of 0.01
 N2-N2_$1
 1.45 with sigma of 0.01
 C31-N2
 2.3 with sigma of 0.02
 O8-C2AA \\sim O9-C0AA \\sim O10-C0AA \\sim O6-C2AA \\sim O2-C22 \\sim O7-C22
 with sigma of 0.02
 C38-C22 \\sim C29-C32 \\sim C27-C21 \\sim C17-C0AA \\sim C2AA-C3
 with sigma of 0.02
 C33-C0AA \\sim C35-C0AA \\sim C19-C15 \\sim C19-C2
 with sigma of 0.02
3. Restrained planarity
 C0AA, C2, C15, C17, C31, C33, C35
 with sigma of 0.01
 C2, C15, C17, C19, C31, C33, C35
 with sigma of 0.01
 N2, C2, C15, C17, C19, C31, C33, C35
 with sigma of 0.01
 O9, O10, C0AA, C2, C15, C17, C31, C33, C35
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C0AA \\sim C2AA \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C12 \\sim
C14 \\sim C15 \\sim C31 \\sim C2 \\sim C33 \\sim C17 \\sim C35 \\sim C16 \\sim
C18 \\sim C19 \\sim C20 \\sim C21 \\sim C1AA \\sim C23 \\sim C3 \\sim C25 \\sim
C13 \\sim C22 \\sim C24 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim
C32 \\sim C34 \\sim C36 \\sim C38 \\sim C39 \\sim C5 \\sim C37 \\sim N1 \\sim
N2 \\sim N3 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O6 \\sim O7 \\sim O8
\\sim O9 \\sim O10 \\sim O11 \\sim O5: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.03
5.a Aromatic/amide H refined with riding coordinates:
 O1(H1), O4(H4), O11(H11), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C14(H14), C15(H15), C2(H2), C33(H33), C35(H35), C16(H16), C18(H18), C19(H19),
 C20(H20), C1AA(H1AA), C23(H23), C25(H25), C13(H13), C24(H24), C26(H26),
 C27(H27), C28(H28), C29(H29), C30(H30), C34(H34), C36(H36), C39(H39), C5(H5),
 C37(H37)
5.b Fitted hexagon refined as free rotating group:
 C15(C31,C2,C33,C17,C35), C21(C1AA,C23,C3,C25,C13), C32(C34,C36,C38,C39,C5)
;
_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
Zr1 Zr 0.31569(6) 0.23541(15) 0.96206(18) 0.0359(12) Uani 1 1 d . . . . .
Zr2 Zr 0.31251(6) 0.41939(15) 0.91376(18) 0.0345(12) Uani 1 1 d . . . . .
Zr3 Zr 0.29313(6) 0.29261(15) 0.75299(18) 0.0331(12) Uani 1 1 d . . . . .
O1 O 0.2805(4) 0.2255(11) 0.8544(13) 0.054(3) Uani 1 1 d . U . . .
H1 H 0.262768 0.196904 0.851663 0.065 Uiso 1 1 calc R . . . .
O2 O 0.6436(4) 0.4015(11) 0.5060(14) 0.059(4) Uani 1 1 d D U . . .
O3 O 0.3228(4) 0.3140(11) 0.8706(13) 0.054(3) Uani 1 1 d . U . . .
O4 O 0.2983(4) 0.3378(11) 0.9999(13) 0.052(3) Uani 1 1 d . U . . .
H4 H 0.286703 0.345804 1.044910 0.062 Uiso 1 1 calc R . . . .
O6 O 0.3258(4) 0.3684(12) 0.7079(14) 0.055(3) Uani 1 1 d D U . . .
O7 O 0.6394(4) 0.2814(12) 0.4783(15) 0.060(4) Uani 1 1 d D U . . .
O8 O 0.3390(4) 0.4461(11) 0.8154(14) 0.054(3) Uani 1 1 d D U . . .
O9 O 0.3411(4) 0.1633(8) 0.8780(13) 0.060(3) Uani 1 1 d D U . . .
O10 O 0.3287(4) 0.2081(8) 0.7467(13) 0.059(3) Uani 1 1 d D U . . .
O11 O 0.2783(4) 0.3911(11) 0.8092(13) 0.052(3) Uani 1 1 d . U . . .
H11 H 0.259977 0.416917 0.790969 0.063 Uiso 1 1 calc R . . . .
N1 N 0.4661(6) 0.3924(15) 0.5885(19) 0.063(3) Uani 1 1 d . U . . .
N2 N 0.4850(2) 0.1567(10) 0.7240(12) 0.084(4) Uani 1 1 d D U . . .
N3 N 0.4951(6) 0.4073(15) 0.5733(19) 0.065(3) Uani 1 1 d . U . . .
C0AA C 0.3483(4) 0.1827(6) 0.8058(12) 0.063(3) Uani 1 1 d D U . . .
C2AA C 0.3454(5) 0.4110(16) 0.7510(17) 0.057(3) Uani 1 1 d D U . . .
C6 C 0.2789(7) 0.5294(17) 0.919(2) 0.053(3) Uani 1 1 d . U . . .
H6 H 0.260152 0.525369 0.880447 0.063 Uiso 1 1 calc R . . . .
C7 C 0.3224(7) 0.1105(19) 1.038(2) 0.057(3) Uani 1 1 d . U . . .
H7 H 0.334773 0.075229 1.014622 0.068 Uiso 1 1 calc R . . . .
C8 C 0.3069(7) 0.1985(19) 1.118(2) 0.056(4) Uani 1 1 d . U . . .
H8 H 0.306509 0.235332 1.162711 0.067 Uiso 1 1 calc R . . . .
C9 C 0.2927(7) 0.1186(19) 1.011(2) 0.057(3) Uani 1 1 d . U . . .
H9 H 0.280534 0.090331 0.966505 0.068 Uiso 1 1 calc R . . . .
C10 C 0.3140(7) 0.5157(17) 1.033(2) 0.053(4) Uani 1 1 d . U . . .
H10 H 0.324623 0.502067 1.089709 0.063 Uiso 1 1 calc R . . . .
C12 C 0.3254(8) 0.5516(17) 0.963(2) 0.052(4) Uani 1 1 d . U . . .
H12 H 0.345451 0.566905 0.963907 0.062 Uiso 1 1 calc R . . . .
C14 C 0.2767(7) 0.2988(18) 0.587(2) 0.055(3) Uani 1 1 d . U . . .
H14 H 0.289750 0.320066 0.551359 0.066 Uiso 1 1 calc R . . . .
C15 C 0.4292(3) 0.1353(8) 0.8613(11) 0.075(3) Uani 1 1 d D U . . .
H15 H 0.442815 0.115265 0.909585 0.090 Uiso 1 1 calc R . . . .
C31 C 0.4392(3) 0.1554(6) 0.7840(12) 0.075(4) Uani 1 1 d DG U . . .
C2 C 0.4193(4) 0.1846(8) 0.7133(10) 0.074(3) Uani 1 1 d DG U . . .
H2 H 0.426063 0.198352 0.660469 0.089 Uiso 1 1 calc R . . . .
C33 C 0.3894(4) 0.1937(7) 0.7200(10) 0.069(3) Uani 1 1 d DG U . . .
H33 H 0.375781 0.213732 0.671664 0.083 Uiso 1 1 calc R . . . .
C17 C 0.3794(3) 0.1736(5) 0.7973(10) 0.068(3) Uani 1 1 d DG U . . .
C35 C 0.3993(4) 0.1444(7) 0.8679(10) 0.070(3) Uani 1 1 d DG U . . .
H35 H 0.392532 0.130645 0.920781 0.085 Uiso 1 1 calc R . . . .
C16 C 0.2533(7) 0.2155(19) 0.660(2) 0.056(3) Uani 1 1 d . U . . .
H16 H 0.246949 0.169832 0.682952 0.067 Uiso 1 1 calc R . . . .
C18 C 0.3318(8) 0.1626(18) 1.104(2) 0.056(3) Uani 1 1 d . U . . .
H18 H 0.351624 0.171152 1.133017 0.067 Uiso 1 1 calc R . . . .
C19 C 0.4705(4) 0.1444(8) 0.7816(15) 0.078(4) Uani 1 1 d D U . . .
H19 H 0.481597 0.123966 0.834311 0.094 Uiso 1 1 calc R . . . .
C20 C 0.2757(7) 0.2221(19) 0.612(2) 0.055(3) Uani 1 1 d . U . . .
H20 H 0.288202 0.182827 0.597757 0.066 Uiso 1 1 calc R . . . .
C21 C 0.4291(4) 0.4245(13) 0.6676(15) 0.061(3) Uani 1 1 d D U . . .
C1AA C 0.4063(5) 0.3828(12) 0.6183(12) 0.061(3) Uani 1 1 d G U . . .
H1AA H 0.409746 0.356167 0.567521 0.073 Uiso 1 1 calc R . . . .
C23 C 0.3784(4) 0.3801(12) 0.6434(14) 0.060(3) Uani 1 1 d G U . . .
H23 H 0.362761 0.351582 0.609662 0.072 Uiso 1 1 calc R . . . .
C3 C 0.3733(4) 0.4190(13) 0.7177(15) 0.058(3) Uani 1 1 d DG U . . .
C25 C 0.3961(5) 0.4607(12) 0.7670(12) 0.060(3) Uani 1 1 d G U . . .
H25 H 0.392621 0.487344 0.817837 0.072 Uiso 1 1 calc R . . . .
C13 C 0.4240(4) 0.4634(12) 0.7420(14) 0.062(3) Uani 1 1 d G U . . .
H13 H 0.439607 0.491930 0.775698 0.074 Uiso 1 1 calc R . . . .
C22 C 0.6280(5) 0.3436(13) 0.490(2) 0.062(4) Uani 1 1 d D U . . .
C24 C 0.2409(7) 0.2872(18) 0.671(2) 0.055(3) Uani 1 1 d . U . . .
H24 H 0.225815 0.299294 0.703932 0.066 Uiso 1 1 calc R . . . .
C26 C 0.2839(7) 0.5051(17) 1.000(2) 0.052(3) Uani 1 1 d . U . . .
H26 H 0.269587 0.484091 1.031402 0.062 Uiso 1 1 calc R . . . .
C27 C 0.4589(5) 0.432(2) 0.645(2) 0.062(3) Uani 1 1 d D U . . .
H27 H 0.472399 0.468544 0.673654 0.075 Uiso 1 1 calc R . . . .
C28 C 0.3027(7) 0.5600(18) 0.895(2) 0.053(3) Uani 1 1 d . U . . .
H28 H 0.303679 0.583700 0.840677 0.063 Uiso 1 1 calc R . . . .
C29 C 0.5068(5) 0.350(2) 0.541(2) 0.065(3) Uani 1 1 d D U . . .
H29 H 0.494688 0.308111 0.521210 0.078 Uiso 1 1 calc R . . . .
C30 C 0.2556(7) 0.3363(19) 0.622(2) 0.055(3) Uani 1 1 d . U . . .
H30 H 0.251404 0.388402 0.615021 0.066 Uiso 1 1 calc R . . . .
C32 C 0.5385(3) 0.3500(13) 0.5340(15) 0.064(3) Uani 1 1 d D U . . .
C34 C 0.5513(4) 0.2808(11) 0.5219(15) 0.065(3) Uani 1 1 d G U . . .
H34 H 0.540380 0.235848 0.525764 0.078 Uiso 1 1 calc R . . . .
C36 C 0.5802(5) 0.2774(10) 0.5041(15) 0.064(3) Uani 1 1 d G U . . .
H36 H 0.589024 0.230080 0.495748 0.076 Uiso 1 1 calc R . . . .
C38 C 0.5963(3) 0.3431(13) 0.4984(15) 0.063(4) Uani 1 1 d DG U . . .
C39 C 0.5834(4) 0.4123(11) 0.5105(15) 0.063(3) Uani 1 1 d G U . . .
H39 H 0.594361 0.457264 0.506668 0.076 Uiso 1 1 calc R . . . .
C5 C 0.5545(5) 0.4157(10) 0.5284(15) 0.064(3) Uani 1 1 d G U . . .
H5 H 0.545717 0.463033 0.536684 0.077 Uiso 1 1 calc R . . . .
C37 C 0.2830(8) 0.1754(18) 1.061(2) 0.056(3) Uani 1 1 d . U . . .
H37 H 0.263270 0.194266 1.056119 0.067 Uiso 1 1 calc R . . . .
Cl1 Cl 0.2753(2) 0.3770(5) 1.1696(6) 0.068(3) Uani 1 1 d . . . . .
O5 O 0.2640(6) -0.0092(13) 0.7776(15) 0.097(9) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 Zr2 3.356(4) . ?
Zr1 Zr3 3.359(4) . ?
Zr1 O1 2.10(2) . ?
Zr1 O3 2.05(2) . ?
Zr1 O4 2.108(19) . ?
Zr1 O7 2.25(2) 2_656 ?
Zr1 O9 2.274(18) . ?
Zr1 C7 2.50(3) . ?
Zr1 C8 2.58(3) . ?
Zr1 C9 2.50(3) . ?
Zr1 C18 2.53(3) . ?
Zr1 C37 2.54(3) . ?
Zr2 Zr3 3.351(4) . ?
Zr2 O2 2.18(2) 2_656 ?
Zr2 O3 2.07(2) . ?
Zr2 O4 2.140(19) . ?
Zr2 O8 2.14(2) . ?
Zr2 O11 2.10(2) . ?
Zr2 C6 2.49(3) . ?
Zr2 C10 2.50(3) . ?
Zr2 C12 2.51(3) . ?
Zr2 C26 2.53(3) . ?
Zr2 C28 2.55(3) . ?
Zr3 O1 2.120(19) . ?
Zr3 O3 2.10(2) . ?
Zr3 O6 2.21(2) . ?
Zr3 O10 2.225(18) . ?
Zr3 O11 2.12(2) . ?
Zr3 C14 2.54(3) . ?
Zr3 C16 2.51(3) . ?
Zr3 C20 2.51(3) . ?
Zr3 C24 2.49(3) . ?
Zr3 C30 2.53(3) . ?
O1 H1 0.9500 . ?
O2 C22 1.252(16) . ?
O4 H4 0.9500 . ?
O6 C2AA 1.265(16) . ?
O7 C22 1.249(16) . ?
O8 C2AA 1.247(16) . ?
O9 C0AA 1.257(16) . ?
O10 C0AA 1.241(16) . ?
O11 H11 0.9500 . ?
N1 N3 1.40(3) . ?
N1 C27 1.21(3) . ?
N2 N2 1.460(11) 2_656 ?
N2 C19 1.214(10) . ?
N3 C29 1.28(3) . ?
C0AA C17 1.456(14) . ?
C2AA C3 1.455(19) . ?
C6 H6 0.9500 . ?
C6 C26 1.31(4) . ?
C6 C28 1.32(4) . ?
C7 H7 0.9500 . ?
C7 C9 1.35(4) . ?
C7 C18 1.39(4) . ?
C8 H8 0.9500 . ?
C8 C18 1.35(4) . ?
C8 C37 1.34(4) . ?
C9 H9 0.9500 . ?
C9 C37 1.39(4) . ?
C10 H10 0.9500 . ?
C10 C12 1.43(4) . ?
C10 C26 1.39(4) . ?
C12 H12 0.9500 . ?
C12 C28 1.34(4) . ?
C14 H14 0.9500 . ?
C14 C20 1.42(4) . ?
C14 C30 1.36(4) . ?
C15 H15 0.9500 . ?
C15 C31 1.3900 . ?
C15 C35 1.3900 . ?
C31 C2 1.3900 . ?
C31 C19 1.444(9) . ?
C2 H2 0.9500 . ?
C2 C33 1.3900 . ?
C33 H33 0.9500 . ?
C33 C17 1.3900 . ?
C17 C35 1.3900 . ?
C35 H35 0.9500 . ?
C16 H16 0.9500 . ?
C16 C20 1.36(4) . ?
C16 C24 1.42(4) . ?
C18 H18 0.9500 . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C1AA 1.3900 . ?
C21 C13 1.3900 . ?
C21 C27 1.465(19) . ?
C1AA H1AA 0.9500 . ?
C1AA C23 1.3900 . ?
C23 H23 0.9500 . ?
C23 C3 1.3900 . ?
C3 C25 1.3900 . ?
C25 H25 0.9500 . ?
C25 C13 1.3900 . ?
C13 H13 0.9500 . ?
C22 C38 1.470(19) . ?
C24 H24 0.9500 . ?
C24 C30 1.39(4) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C29 C32 1.465(19) . ?
C30 H30 0.9500 . ?
C32 C34 1.3900 . ?
C32 C5 1.3900 . ?
C34 H34 0.9500 . ?
C34 C36 1.3900 . ?
C36 H36 0.9500 . ?
C36 C38 1.3900 . ?
C38 C39 1.3900 . ?
C39 H39 0.9500 . ?
C39 C5 1.3900 . ?
C5 H5 0.9500 . ?
C37 H37 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Zr2 Zr1 Zr3 59.87(8) . . ?
O1 Zr1 Zr2 84.8(5) . . ?
O1 Zr1 Zr3 37.5(5) . . ?
O1 Zr1 O4 91.1(8) . . ?
O1 Zr1 O7 150.2(8) . 2_656 ?
O1 Zr1 O9 84.1(7) . . ?
O1 Zr1 C7 107.8(10) . . ?
O1 Zr1 C8 119.5(9) . . ?
O1 Zr1 C9 82.4(10) . . ?
O1 Zr1 C18 134.6(10) . . ?
O1 Zr1 C37 89.6(10) . . ?
O3 Zr1 Zr2 35.7(6) . . ?
O3 Zr1 Zr3 36.3(6) . . ?
O3 Zr1 O1 72.9(8) . . ?
O3 Zr1 O4 73.2(8) . . ?
O3 Zr1 O7 77.9(8) . 2_656 ?
O3 Zr1 O9 80.7(7) . . ?
O3 Zr1 C7 154.7(10) . . ?
O3 Zr1 C8 151.5(10) . . ?
O3 Zr1 C9 154.0(10) . . ?
O3 Zr1 C18 152.1(10) . . ?
O3 Zr1 C37 151.3(10) . . ?
O4 Zr1 Zr2 38.2(5) . . ?
O4 Zr1 Zr3 86.2(5) . . ?
O4 Zr1 O7 86.1(7) . 2_656 ?
O4 Zr1 O9 153.7(7) . . ?
O4 Zr1 C7 131.4(10) . . ?
O4 Zr1 C8 80.7(9) . . ?
O4 Zr1 C9 115.9(9) . . ?
O4 Zr1 C18 105.8(9) . . ?
O4 Zr1 C37 84.9(9) . . ?
O7 Zr1 Zr2 74.7(5) 2_656 . ?
O7 Zr1 Zr3 112.7(6) 2_656 . ?
O7 Zr1 O9 85.5(7) 2_656 . ?
O7 Zr1 C7 96.0(9) 2_656 . ?
O7 Zr1 C8 89.4(9) 2_656 . ?
O7 Zr1 C9 125.3(10) 2_656 . ?
O7 Zr1 C18 74.2(10) 2_656 . ?
O7 Zr1 C37 119.6(10) 2_656 . ?
O9 Zr1 Zr2 115.6(4) . . ?
O9 Zr1 Zr3 74.3(5) . . ?
O9 Zr1 C7 74.3(9) . . ?
O9 Zr1 C8 124.0(9) . . ?
O9 Zr1 C9 89.1(9) . . ?
O9 Zr1 C18 95.8(9) . . ?
O9 Zr1 C37 120.8(9) . . ?
C7 Zr1 Zr2 165.2(8) . . ?
C7 Zr1 Zr3 134.9(8) . . ?
C7 Zr1 C8 50.9(11) . . ?
C7 Zr1 C9 31.3(9) . . ?
C7 Zr1 C18 32.0(9) . . ?
C7 Zr1 C37 52.1(11) . . ?
C8 Zr1 Zr2 116.5(8) . . ?
C8 Zr1 Zr3 153.5(7) . . ?
C9 Zr1 Zr2 150.8(8) . . ?
C9 Zr1 Zr3 117.8(8) . . ?
C9 Zr1 C8 50.8(11) . . ?
C9 Zr1 C18 52.3(11) . . ?
C9 Zr1 C37 31.9(9) . . ?
C18 Zr1 Zr2 133.2(8) . . ?
C18 Zr1 Zr3 166.8(8) . . ?
C18 Zr1 C8 30.6(9) . . ?
C18 Zr1 C37 51.7(11) . . ?
C37 Zr1 Zr2 122.4(8) . . ?
C37 Zr1 Zr3 126.0(8) . . ?
C37 Zr1 C8 30.2(9) . . ?
Zr3 Zr2 Zr1 60.11(8) . . ?
O2 Zr2 Zr1 74.5(5) 2_656 . ?
O2 Zr2 Zr3 114.7(6) 2_656 . ?
O2 Zr2 C6 127.2(10) 2_656 . ?
O2 Zr2 C10 77.3(9) 2_656 . ?
O2 Zr2 C12 79.8(10) 2_656 . ?
O2 Zr2 C26 107.1(9) 2_656 . ?
O2 Zr2 C28 109.3(9) 2_656 . ?
O3 Zr2 Zr1 35.2(5) . . ?
O3 Zr2 Zr3 36.7(6) . . ?
O3 Zr2 O2 79.2(8) . 2_656 ?
O3 Zr2 O4 72.1(8) . . ?
O3 Zr2 O8 77.8(7) . . ?
O3 Zr2 O11 73.5(8) . . ?
O3 Zr2 C6 153.5(10) . . ?
O3 Zr2 C10 151.2(10) . . ?
O3 Zr2 C12 153.2(9) . . ?
O3 Zr2 C26 151.8(9) . . ?
O3 Zr2 C28 154.0(10) . . ?
O4 Zr2 Zr1 37.5(5) . . ?
O4 Zr2 Zr3 86.0(5) . . ?
O4 Zr2 O2 84.1(7) . 2_656 ?
O4 Zr2 O8 148.7(8) . . ?
O4 Zr2 C6 105.2(9) . . ?
O4 Zr2 C10 89.1(9) . . ?
O4 Zr2 C12 122.0(9) . . ?
O4 Zr2 C26 81.1(9) . . ?
O4 Zr2 C28 132.0(9) . . ?
O8 Zr2 Zr1 111.4(5) . . ?
O8 Zr2 Zr3 74.7(5) . . ?
O8 Zr2 O2 82.0(8) . 2_656 ?
O8 Zr2 C6 105.6(9) . . ?
O8 Zr2 C10 114.7(9) . . ?
O8 Zr2 C12 82.8(9) . . ?
O8 Zr2 C26 129.8(9) . . ?
O8 Zr2 C28 79.2(9) . . ?
O11 Zr2 Zr1 86.2(5) . . ?
O11 Zr2 Zr3 37.5(5) . . ?
O11 Zr2 O2 152.2(8) . 2_656 ?
O11 Zr2 O4 92.7(7) . . ?
O11 Zr2 O8 86.9(7) . . ?
O11 Zr2 C6 80.4(10) . . ?
O11 Zr2 C10 130.5(9) . . ?
O11 Zr2 C12 124.1(10) . . ?
O11 Zr2 C26 99.6(9) . . ?
O11 Zr2 C28 93.4(9) . . ?
C6 Zr2 Zr1 139.7(8) . . ?
C6 Zr2 Zr3 117.8(8) . . ?
C6 Zr2 C10 51.7(11) . . ?
C6 Zr2 C12 50.8(11) . . ?
C6 Zr2 C26 30.2(9) . . ?
C6 Zr2 C28 30.2(8) . . ?
C10 Zr2 Zr1 120.7(8) . . ?
C10 Zr2 Zr3 166.5(7) . . ?
C10 Zr2 C12 33.1(9) . . ?
C10 Zr2 C26 32.0(9) . . ?
C10 Zr2 C28 52.5(11) . . ?
C12 Zr2 Zr1 148.2(8) . . ?
C12 Zr2 Zr3 150.7(8) . . ?
C12 Zr2 C26 52.4(10) . . ?
C12 Zr2 C28 30.7(9) . . ?
C26 Zr2 Zr1 118.6(8) . . ?
C26 Zr2 Zr3 134.5(7) . . ?
C26 Zr2 C28 50.9(11) . . ?
C28 Zr2 Zr1 169.3(7) . . ?
C28 Zr2 Zr3 124.1(8) . . ?
Zr2 Zr3 Zr1 60.02(8) . . ?
O1 Zr3 Zr1 37.1(6) . . ?
O1 Zr3 Zr2 84.7(6) . . ?
O1 Zr3 O6 149.1(8) . . ?
O1 Zr3 O10 86.7(7) . . ?
O1 Zr3 C14 134.0(9) . . ?
O1 Zr3 C16 81.4(10) . . ?
O1 Zr3 C20 105.5(9) . . ?
O1 Zr3 C24 89.8(9) . . ?
O1 Zr3 C30 121.8(9) . . ?
O3 Zr3 Zr1 35.4(5) . . ?
O3 Zr3 Zr2 36.2(5) . . ?
O3 Zr3 O1 71.6(7) . . ?
O3 Zr3 O6 77.9(8) . . ?
O3 Zr3 O10 78.2(7) . . ?
O3 Zr3 O11 72.6(8) . . ?
O3 Zr3 C14 153.4(9) . . ?
O3 Zr3 C16 152.1(10) . . ?
O3 Zr3 C20 153.6(10) . . ?
O3 Zr3 C24 149.3(9) . . ?
O3 Zr3 C30 151.3(10) . . ?
O6 Zr3 Zr1 112.0(6) . . ?
O6 Zr3 Zr2 73.4(5) . . ?
O6 Zr3 O10 82.2(7) . . ?
O6 Zr3 C14 75.8(9) . . ?
O6 Zr3 C16 127.9(9) . . ?
O6 Zr3 C20 99.4(9) . . ?
O6 Zr3 C24 119.9(9) . . ?
O6 Zr3 C30 87.9(9) . . ?
O10 Zr3 Zr1 74.5(5) . . ?
O10 Zr3 Zr2 112.7(5) . . ?
O10 Zr3 C14 94.4(9) . . ?
O10 Zr3 C16 93.7(9) . . ?
O10 Zr3 C20 75.4(9) . . ?
O10 Zr3 C24 126.1(9) . . ?
O10 Zr3 C30 124.8(9) . . ?
O11 Zr3 Zr1 85.8(5) . . ?
O11 Zr3 Zr2 37.1(5) . . ?
O11 Zr3 O1 91.2(7) . . ?
O11 Zr3 O6 84.4(7) . . ?
O11 Zr3 O10 149.8(7) . . ?
O11 Zr3 C14 108.4(9) . . ?
O11 Zr3 C16 115.7(9) . . ?
O11 Zr3 C20 133.7(10) . . ?
O11 Zr3 C24 84.0(9) . . ?
O11 Zr3 C30 81.4(9) . . ?
C14 Zr3 Zr1 164.8(8) . . ?
C14 Zr3 Zr2 135.0(8) . . ?
C16 Zr3 Zr1 116.7(8) . . ?
C16 Zr3 Zr2 149.2(7) . . ?
C16 Zr3 C14 52.6(11) . . ?
C16 Zr3 C20 31.5(9) . . ?
C16 Zr3 C30 52.6(11) . . ?
C20 Zr3 Zr1 132.3(8) . . ?
C20 Zr3 Zr2 167.6(8) . . ?
C20 Zr3 C14 32.7(9) . . ?
C20 Zr3 C30 52.9(11) . . ?
C24 Zr3 Zr1 125.5(8) . . ?
C24 Zr3 Zr2 120.5(8) . . ?
C24 Zr3 C14 53.2(10) . . ?
C24 Zr3 C16 32.8(9) . . ?
C24 Zr3 C20 53.9(11) . . ?
C24 Zr3 C30 32.1(9) . . ?
C30 Zr3 Zr1 155.2(7) . . ?
C30 Zr3 Zr2 115.8(8) . . ?
C30 Zr3 C14 31.1(9) . . ?
Zr1 O1 Zr3 105.4(8) . . ?
Zr1 O1 H1 127.3 . . ?
Zr3 O1 H1 127.3 . . ?
C22 O2 Zr2 132(2) . 2_656 ?
Zr1 O3 Zr2 109.1(9) . . ?
Zr1 O3 Zr3 108.3(9) . . ?
Zr2 O3 Zr3 107.1(9) . . ?
Zr1 O4 Zr2 104.3(8) . . ?
Zr1 O4 H4 127.8 . . ?
Zr2 O4 H4 127.8 . . ?
C2AA O6 Zr3 130.8(18) . . ?
C22 O7 Zr1 129(2) . 2_656 ?
C2AA O8 Zr2 133.3(18) . . ?
C0AA O9 Zr1 125.5(11) . . ?
C0AA O10 Zr3 130.4(12) . . ?
Zr2 O11 Zr3 105.3(9) . . ?
Zr2 O11 H11 127.3 . . ?
Zr3 O11 H11 127.3 . . ?
C27 N1 N3 113(3) . . ?
C19 N2 N2 100.1(18) . 2_656 ?
C29 N3 N1 112(3) . . ?
O9 C0AA C17 117.0(15) . . ?
O10 C0AA O9 119(2) . . ?
O10 C0AA C17 124.0(16) . . ?
O6 C2AA C3 117(2) . . ?
O8 C2AA O6 118(2) . . ?
O8 C2AA C3 125(2) . . ?
Zr2 C6 H6 114.3 . . ?
C26 C6 Zr2 76(2) . . ?
C26 C6 H6 123.9 . . ?
C26 C6 C28 112(4) . . ?
C28 C6 Zr2 77(2) . . ?
C28 C6 H6 123.9 . . ?
Zr1 C7 H7 116.6 . . ?
C9 C7 Zr1 74(2) . . ?
C9 C7 H7 125.9 . . ?
C9 C7 C18 108(3) . . ?
C18 C7 Zr1 75.2(19) . . ?
C18 C7 H7 125.9 . . ?
Zr1 C8 H8 121.3 . . ?
C18 C8 Zr1 72.6(19) . . ?
C18 C8 H8 124.6 . . ?
C37 C8 Zr1 73(2) . . ?
C37 C8 H8 124.6 . . ?
C37 C8 C18 111(4) . . ?
Zr1 C9 H9 116.2 . . ?
C7 C9 Zr1 74.3(19) . . ?
C7 C9 H9 126.0 . . ?
C7 C9 C37 108(3) . . ?
C37 C9 Zr1 75.6(19) . . ?
C37 C9 H9 126.0 . . ?
Zr2 C10 H10 116.2 . . ?
C12 C10 Zr2 73.7(18) . . ?
C12 C10 H10 127.8 . . ?
C26 C10 Zr2 74.9(19) . . ?
C26 C10 H10 127.8 . . ?
C26 C10 C12 104(3) . . ?
Zr2 C12 H12 116.5 . . ?
C10 C12 Zr2 73.2(18) . . ?
C10 C12 H12 126.2 . . ?
C28 C12 Zr2 76.2(19) . . ?
C28 C12 C10 108(3) . . ?
C28 C12 H12 126.2 . . ?
Zr3 C14 H14 119.2 . . ?
C20 C14 Zr3 72.7(19) . . ?
C20 C14 H14 126.2 . . ?
C30 C14 Zr3 74(2) . . ?
C30 C14 H14 126.2 . . ?
C30 C14 C20 108(3) . . ?
C31 C15 H15 120.0 . . ?
C31 C15 C35 120.0 . . ?
C35 C15 H15 120.0 . . ?
C15 C31 C19 117.0(8) . . ?
C2 C31 C15 120.0 . . ?
C2 C31 C19 123.0(8) . . ?
C31 C2 H2 120.0 . . ?
C31 C2 C33 120.0 . . ?
C33 C2 H2 120.0 . . ?
C2 C33 H33 120.0 . . ?
C17 C33 C2 120.0 . . ?
C17 C33 H33 120.0 . . ?
C33 C17 C0AA 121.0(8) . . ?
C33 C17 C35 120.0 . . ?
C35 C17 C0AA 119.0(8) . . ?
C15 C35 H35 120.0 . . ?
C17 C35 C15 120.0 . . ?
C17 C35 H35 120.0 . . ?
Zr3 C16 H16 119.4 . . ?
C20 C16 Zr3 74.3(19) . . ?
C20 C16 H16 125.3 . . ?
C20 C16 C24 109(3) . . ?
C24 C16 Zr3 72.8(19) . . ?
C24 C16 H16 125.3 . . ?
Zr1 C18 H18 115.8 . . ?
C7 C18 Zr1 72.8(19) . . ?
C7 C18 H18 126.9 . . ?
C8 C18 Zr1 77(2) . . ?
C8 C18 C7 106(3) . . ?
C8 C18 H18 126.9 . . ?
N2 C19 C31 131.1(14) . . ?
N2 C19 H19 114.5 . . ?
C31 C19 H19 114.5 . . ?
Zr3 C20 H20 116.8 . . ?
C14 C20 Zr3 74.6(19) . . ?
C14 C20 H20 126.5 . . ?
C16 C20 Zr3 74.2(19) . . ?
C16 C20 C14 107(3) . . ?
C16 C20 H20 126.5 . . ?
C1AA C21 C13 120.0 . . ?
C1AA C21 C27 124(2) . . ?
C13 C21 C27 116(2) . . ?
C21 C1AA H1AA 120.0 . . ?
C23 C1AA C21 120.0 . . ?
C23 C1AA H1AA 120.0 . . ?
C1AA C23 H23 120.0 . . ?
C1AA C23 C3 120.0 . . ?
C3 C23 H23 120.0 . . ?
C23 C3 C2AA 121.3(17) . . ?
C23 C3 C25 120.0 . . ?
C25 C3 C2AA 118.4(17) . . ?
C3 C25 H25 120.0 . . ?
C13 C25 C3 120.0 . . ?
C13 C25 H25 120.0 . . ?
C21 C13 H13 120.0 . . ?
C25 C13 C21 120.0 . . ?
C25 C13 H13 120.0 . . ?
O2 C22 C38 121(2) . . ?
O7 C22 O2 121(2) . . ?
O7 C22 C38 117(2) . . ?
Zr3 C24 H24 115.7 . . ?
C16 C24 Zr3 74.4(19) . . ?
C16 C24 H24 127.2 . . ?
C30 C24 Zr3 75.2(18) . . ?
C30 C24 C16 106(3) . . ?
C30 C24 H24 127.2 . . ?
Zr2 C26 H26 119.2 . . ?
C6 C26 Zr2 73(2) . . ?
C6 C26 C10 108(3) . . ?
C6 C26 H26 126.2 . . ?
C10 C26 Zr2 73.1(18) . . ?
C10 C26 H26 126.2 . . ?
N1 C27 C21 120(3) . . ?
N1 C27 H27 120.1 . . ?
C21 C27 H27 120.1 . . ?
Zr2 C28 H28 120.0 . . ?
C6 C28 Zr2 73(2) . . ?
C6 C28 C12 108(3) . . ?
C6 C28 H28 126.1 . . ?
C12 C28 Zr2 73.1(19) . . ?
C12 C28 H28 126.1 . . ?
N3 C29 H29 119.7 . . ?
N3 C29 C32 121(3) . . ?
C32 C29 H29 119.7 . . ?
Zr3 C30 H30 119.2 . . ?
C14 C30 Zr3 75(2) . . ?
C14 C30 C24 110(3) . . ?
C14 C30 H30 124.9 . . ?
C24 C30 Zr3 72.6(19) . . ?
C24 C30 H30 124.9 . . ?
C34 C32 C29 117(2) . . ?
C34 C32 C5 120.0 . . ?
C5 C32 C29 122(2) . . ?
C32 C34 H34 120.0 . . ?
C36 C34 C32 120.0 . . ?
C36 C34 H34 120.0 . . ?
C34 C36 H36 120.0 . . ?
C34 C36 C38 120.0 . . ?
C38 C36 H36 120.0 . . ?
C36 C38 C22 122.9(17) . . ?
C39 C38 C22 116.7(17) . . ?
C39 C38 C36 120.0 . . ?
C38 C39 H39 120.0 . . ?
C5 C39 C38 120.0 . . ?
C5 C39 H39 120.0 . . ?
C32 C5 H5 120.0 . . ?
C39 C5 C32 120.0 . . ?
C39 C5 H5 120.0 . . ?
Zr1 C37 H37 116.4 . . ?
C8 C37 Zr1 76.7(19) . . ?
C8 C37 C9 107(3) . . ?
C8 C37 H37 126.7 . . ?
C9 C37 Zr1 72.5(18) . . ?
C9 C37 H37 126.7 . . ?

_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 -0.139 2566.4 660.1 ?
2 0.000 0.183 0.250 10.7 0.0 ?
3 0.000 0.817 0.750 10.7 0.0 ?
4 0.500 0.000 -0.158 2566.4 660.1 ?
5 0.500 0.317 0.750 10.7 0.0 ?
6 0.500 0.683 0.250 10.7 0.0 ?

_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_THETM01_1                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystals were weakly diffracting at high angle which is not 
uncommon for structures of this type.
;
_vrf_PLAT088_1                   
;
PROBLEM: Poor Data / Parameter Ratio ....................       6.80 Note  
RESPONSE: The crystals were weakly diffracting at high angle which is not 
uncommon for structures of this type.
;
_vrf_PLAT306_1                   
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......         O5 Check 
RESPONSE: The H atoms of water molecules were unable to locate. These alerts 
are due to the lack of H at om of water molecules.
;
_vrf_PLAT342_1                   
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.03487 Ang.  
RESPONSE: The crystals were weakly diffracting at high angle which is not 
uncommon for structures of this type.
;
# end Validation Reply Form
