# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# 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_nu-406
_database_code_depnum_ccdc_archive 'CCDC 2260133'
loop_
_audit_author_name
_audit_author_address
'Haomiao Xie'
;Northwestern University
United States of America
;
_audit_update_record             
;
2023-05-01 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_audit_creation_date             2023-05-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H36 O32 P12 Zr6'
_chemical_formula_sum            'C60 H36 O32 P12 Zr6'
_chemical_formula_weight         2187.85
_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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+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+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+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+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'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'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+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+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+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+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-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'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   24.6280(3)
_cell_length_b                   24.6280(3)
_cell_length_c                   24.6280(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14937.8(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2291
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.5690
_cell_measurement_theta_min      3.0990
_shelx_estimated_absorpt_T_max   0.639
_shelx_estimated_absorpt_T_min   0.526
_exptl_absorpt_coefficient_mu    4.914
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.104a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.973
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4288
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3719
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.891
_diffrn_reflns_theta_min         3.108
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -108.00 -76.00   0.50   14.00    --  -47.56-130.00 168.00   64
  2  ω    -77.00 -41.00   0.50   55.98    -- -104.00 113.00-163.00   72
  3  ω   -119.00 -78.00   0.50   14.00    --  -47.56-125.00 -60.00   82
  4  ω    -69.00 -44.00   0.50   55.98    -- -104.00  61.00 150.00   50
  5  ω    -57.00 -32.00   0.50   55.98    -- -104.00  61.00   0.00   50
  6  ω     43.00  55.50   0.50   55.98    --  110.25 -61.00-120.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                664
_reflns_number_total             728
_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 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.336
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         728
_refine_ls_number_restraints     281
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.1082
_refine_ls_restrained_S_all      1.068
_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)+(0.1947P)²+196.9178P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2977
_refine_ls_wR_factor_ref         0.3031
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Zr1-O2
 2 with sigma of 0.02
 P1-C9 \\sim P1-C7
 with sigma of 0.01
 P1_$4-C2_$2 \\sim P1_$4-C4_$2
 with sigma of 0.01
 P1_$1-C3 \\sim P1-C8
 with sigma of 0.01
 P1_$2-O2 \\sim P1_$2-O2_$2
 with sigma of 0.01
3. Restrained planarity
 C6, C7, C8, C9, C10, C11, C2, C5, C4, C3, P1_$1, P1
 with sigma of 0.1
4. Rigid bond restraints
 O2, P1, C8
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C2 \\sim C10 \\sim C8 \\sim C3 \\sim C7 \\sim C4 \\sim C9 \\sim C5 \\sim C11
\\sim C6: within 3.2A with sigma of 0.03 and sigma for terminal atoms of 0.06
within 3.2A
P1 \\sim C8 \\sim O2 \\sim O2: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Zr1 \\sim O2: within 3A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3A
Uanis(C2) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C3) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C5)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.1 and
sigma for terminal atoms of 0.2
6. Others
 Fixed Sof: P1(0.25) C2(0.125) H2(0.125) C3(0.125) C4(0.125) H4(0.125)
 C5(0.125) H5(0.125) C6(0.125) C7(0.125) H7(0.125) C8(0.125) C9(0.125)
 H9(0.125) C10(0.125) H10(0.125) C11(0.125)
7.a Free rotating group:
 C2(C3,C4,C5,C6,C7,C8,C9,C10,C11)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10)
;
_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 0.39839(5) 0.500000 0.500000 0.0883(10) Uani 1 8 d DS TU P . .
O1 O 0.4516(4) 0.5484(4) 0.5484(4) 0.105(5) Uani 1 6 d S T P . .
P1 P 0.3707(3) 0.5313(5) 0.6294(3) 0.194(7) Uani 0.25 1 d D U P A -1
O2 O 0.3507(4) 0.500000 0.5729(5) 0.154(3) Uani 1 2 d DS TU P . .
C2 C 0.1876(13) 0.4648(15) 0.7761(11) 0.263(15) Uani 0.125 1 d G U P A -1
H2 H 0.161630 0.438912 0.764229 0.316 Uiso 0.125 1 calc R U P A -1
C3 C 0.1833(13) 0.4867(16) 0.8274(10) 0.266(16) Uani 0.125 1 d DG U P A -1
C4 C 0.2218(14) 0.525(2) 0.8458(9) 0.266(16) Uani 0.125 1 d G U P A -1
H4 H 0.218643 0.540298 0.881221 0.319 Uiso 0.125 1 calc R U P A -1
C5 C 0.2639(13) 0.541(2) 0.8125(9) 0.266(15) Uani 0.125 1 d G U P A -1
H5 H 0.289442 0.567224 0.825243 0.319 Uiso 0.125 1 calc R U P A -1
C6 C 0.2695(11) 0.5195(15) 0.7593(8) 0.263(14) Uani 0.125 1 d G U P A -1
C7 C 0.3124(12) 0.5351(16) 0.7240(8) 0.259(15) Uani 0.125 1 d DG U P A -1
H7 H 0.338454 0.560887 0.735969 0.311 Uiso 0.125 1 calc R U P A -1
C8 C 0.3168(12) 0.5132(16) 0.6726(8) 0.250(13) Uani 0.125 1 d DG U P A -1
C9 C 0.2783(14) 0.4745(18) 0.6543(10) 0.261(15) Uani 0.125 1 d DG U P A -1
H9 H 0.281515 0.459540 0.618911 0.313 Uiso 0.125 1 calc R U P A -1
C10 C 0.2362(14) 0.4585(18) 0.6876(11) 0.263(15) Uani 0.125 1 d G U P A -1
H10 H 0.210612 0.432606 0.674892 0.315 Uiso 0.125 1 calc R U P A -1
C11 C 0.2306(11) 0.4804(14) 0.7407(9) 0.263(14) Uani 0.125 1 d G U P A -1


_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 Zr1 3.5390(17) 101_666 ?
Zr1 Zr1 3.5390(17) 9 ?
Zr1 Zr1 3.5390(17) 5 ?
Zr1 Zr1 3.5390(17) 105_666 ?
Zr1 O1 2.136(5) 99_565 ?
Zr1 O1 2.136(5) 4_566 ?
Zr1 O1 2.136(5) 98_556 ?
Zr1 O1 2.136(5) . ?
Zr1 O2 2.146(10) 114_566 ?
Zr1 O2 2.146(10) . ?
Zr1 O2 2.146(10) 98_556 ?
Zr1 O2 2.146(10) 17_556 ?
P1 O2 1.665(14) . ?
P1 C8 1.760(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.3780 . ?
C2 C11 1.4232 . ?
C3 C4 1.4177 . ?
C4 H4 0.9500 . ?
C4 C5 1.3781 . ?
C5 H5 0.9500 . ?
C5 C6 1.4219 . ?
C6 C7 1.4213 . ?
C6 C11 1.4336 . ?
C7 H7 0.9500 . ?
C7 C8 1.3795 . ?
C8 C9 1.4171 . ?
C9 H9 0.9500 . ?
C9 C10 1.3797 . ?
C10 H10 0.9500 . ?
C10 C11 1.4219 . ?

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
Zr1 Zr1 Zr1 60.0 105_666 101_666 ?
Zr1 Zr1 Zr1 90.0 101_666 5 ?
Zr1 Zr1 Zr1 60.0 105_666 5 ?
Zr1 Zr1 Zr1 90.0 105_666 9 ?
Zr1 Zr1 Zr1 60.0 5 9 ?
Zr1 Zr1 Zr1 60.0 101_666 9 ?
O1 Zr1 Zr1 34.05(18) 98_556 101_666 ?
O1 Zr1 Zr1 87.8(4) 4_566 101_666 ?
O1 Zr1 Zr1 87.8(4) 99_565 101_666 ?
O1 Zr1 Zr1 34.05(18) . 101_666 ?
O1 Zr1 Zr1 34.05(18) 98_556 9 ?
O1 Zr1 Zr1 87.8(4) 4_566 105_666 ?
O1 Zr1 Zr1 34.05(18) . 105_666 ?
O1 Zr1 Zr1 34.05(19) 99_565 105_666 ?
O1 Zr1 Zr1 87.8(4) 99_565 9 ?
O1 Zr1 Zr1 87.8(4) 98_556 105_666 ?
O1 Zr1 Zr1 87.8(4) . 9 ?
O1 Zr1 Zr1 87.8(4) 98_556 5 ?
O1 Zr1 Zr1 87.8(4) . 5 ?
O1 Zr1 Zr1 34.05(18) 4_566 5 ?
O1 Zr1 Zr1 34.05(18) 99_565 5 ?
O1 Zr1 Zr1 34.05(19) 4_566 9 ?
O1 Zr1 O1 67.9(4) 4_566 99_565 ?
O1 Zr1 O1 67.9(4) 99_565 . ?
O1 Zr1 O1 104.4(8) 4_566 . ?
O1 Zr1 O1 67.9(4) 4_566 98_556 ?
O1 Zr1 O1 104.4(8) 99_565 98_556 ?
O1 Zr1 O1 67.9(4) 98_556 . ?
O1 Zr1 O2 143.42(12) 99_565 17_556 ?
O1 Zr1 O2 82.4(4) 98_556 98_556 ?
O1 Zr1 O2 82.4(4) 4_566 98_556 ?
O1 Zr1 O2 82.4(4) 98_556 17_556 ?
O1 Zr1 O2 82.4(4) 4_566 114_566 ?
O1 Zr1 O2 82.4(4) 99_565 114_566 ?
O1 Zr1 O2 143.42(12) 99_565 98_556 ?
O1 Zr1 O2 143.42(12) 98_556 114_566 ?
O1 Zr1 O2 143.42(12) . 98_556 ?
O1 Zr1 O2 143.42(12) 4_566 17_556 ?
O1 Zr1 O2 82.4(4) . 17_556 ?
O1 Zr1 O2 82.4(4) . . ?
O1 Zr1 O2 143.42(12) . 114_566 ?
O1 Zr1 O2 143.42(12) 4_566 . ?
O1 Zr1 O2 82.4(4) 99_565 . ?
O1 Zr1 O2 143.42(12) 98_556 . ?
O2 Zr1 Zr1 168.2(3) 98_556 105_666 ?
O2 Zr1 Zr1 78.2(3) . 105_666 ?
O2 Zr1 Zr1 112.8(2) 114_566 9 ?
O2 Zr1 Zr1 112.8(2) 114_566 105_666 ?
O2 Zr1 Zr1 168.2(3) . 9 ?
O2 Zr1 Zr1 112.8(2) 17_556 105_666 ?
O2 Zr1 Zr1 112.8(2) 98_556 101_666 ?
O2 Zr1 Zr1 112.8(2) . 5 ?
O2 Zr1 Zr1 112.8(2) . 101_666 ?
O2 Zr1 Zr1 112.8(2) 98_556 5 ?
O2 Zr1 Zr1 78.2(3) 98_556 9 ?
O2 Zr1 Zr1 78.2(3) 114_566 5 ?
O2 Zr1 Zr1 112.8(2) 17_556 9 ?
O2 Zr1 Zr1 168.2(3) 17_556 5 ?
O2 Zr1 Zr1 168.2(3) 114_566 101_666 ?
O2 Zr1 Zr1 78.2(3) 17_556 101_666 ?
O2 Zr1 O2 72.6(3) 98_556 17_556 ?
O2 Zr1 O2 113.7(7) . 98_556 ?
O2 Zr1 O2 72.6(3) 98_556 114_566 ?
O2 Zr1 O2 113.7(6) 114_566 17_556 ?
O2 Zr1 O2 72.6(3) . 114_566 ?
O2 Zr1 O2 72.6(3) . 17_556 ?
Zr1 O1 Zr1 111.9(4) 105_666 . ?
Zr1 O1 Zr1 111.9(4) 101_666 . ?
Zr1 O1 Zr1 111.9(4) 105_666 101_666 ?
O2 P1 C8 99.5(6) . . ?
P1 O2 Zr1 122.6(5) 99_565 . ?
P1 O2 Zr1 122.6(5) . . ?
P1 O2 Zr1 122.6(5) 24_666 . ?
P1 O2 P1 55.3(9) 24_666 . ?
P1 O2 P1 55.2(9) . 99_565 ?
P1 O2 P1 0.1(4) 24_666 99_565 ?
P1 C2 H2 86.1 70_465 . ?
C3 C2 P1 33.4(5) . 70_465 ?
C3 C2 H2 119.6 . . ?
C3 C2 C11 120.8 . . ?
C11 C2 P1 154.3(4) . 70_465 ?
C11 C2 H2 119.6 . . ?
C2 C3 P1 121.0(8) . 70_465 ?
C2 C3 C4 120.3 . . ?
C4 C3 P1 118.7(7) . 70_465 ?
P1 C4 H4 85.6 70_465 . ?
C3 C4 P1 34.3(4) . 70_465 ?
C3 C4 H4 119.9 . . ?
C5 C4 P1 154.5(4) . 70_465 ?
C5 C4 C3 120.3 . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 120.9 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C11 118.8 . . ?
C7 C6 C5 122.3 . . ?
C7 C6 C11 118.9 . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 120.9 . . ?
C8 C7 H7 119.5 . . ?
C7 C8 P1 121.0(4) . . ?
C7 C8 C9 120.2 . . ?
C9 C8 P1 118.8(4) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.3 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 119.6 . . ?
C9 C10 C11 120.8 . . ?
C11 C10 H10 119.6 . . ?
C2 C11 C6 118.9 . . ?
C10 C11 C2 122.2 . . ?
C10 C11 C6 118.9 . . ?

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
P1 C2 C3 C4 -178(2) 70_465 . . . ?
P1 C2 C11 C6 2(3) 70_465 . . . ?
P1 C2 C11 C10 -178(3) 70_465 . . . ?
P1 C3 C4 C5 -179(2) 70_465 . . . ?
P1 C4 C5 C6 -2(3) 70_465 . . . ?
P1 C8 C9 C10 179(2) . . . . ?
O2 P1 C8 C7 -173.0(17) . . . . ?
O2 P1 C8 C9 8.4(19) . . . . ?
C2 C3 C4 P1 179(2) . . . 70_465 ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C2 C11 C6 0.1 . . . . ?
C3 C2 C11 C10 179.9 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C5 C6 C7 -179.9 . . . . ?
C4 C5 C6 C11 0.1 . . . . ?
C5 C6 C7 C8 -180.0 . . . . ?
C5 C6 C11 C2 -0.1 . . . . ?
C5 C6 C11 C10 -179.9 . . . . ?
C6 C7 C8 P1 -179(2) . . . . ?
C6 C7 C8 C9 -0.1 . . . . ?
C7 C6 C11 C2 179.9 . . . . ?
C7 C6 C11 C10 0.1 . . . . ?
C7 C8 C9 C10 0.1 . . . . ?
C8 P1 O2 Zr1 -177.3(17) . . . . ?
C8 P1 O2 P1 -67.8(17) . . . 99_565 ?
C8 P1 O2 P1 -67.7(17) . . . 24_666 ?
C8 C9 C10 C11 0.0 . . . . ?
C9 C10 C11 C2 -179.9 . . . . ?
C9 C10 C11 C6 -0.1 . . . . ?
C11 C2 C3 P1 178(2) . . . 70_465 ?
C11 C2 C3 C4 0.0 . . . . ?
C11 C6 C7 C8 0.0 . . . . ?

_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 -0.139 -0.657 -0.963 7183.1 1963.7 '192 H2O'

_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
;
####################################################################### 
# 
# 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_NU-407
_database_code_depnum_ccdc_archive 'CCDC 2260134'
loop_
_audit_author_name
_audit_author_address
'Haomiao Xie'
;Northwestern University
United States of America
;
_audit_update_record             
;
2023-05-01 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_audit_creation_date             2023-01-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C60 H36 O44 P12 Zr6'
_chemical_formula_sum            'C60 H36 O44 P12 Zr6'
_chemical_formula_weight         2379.85
_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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -z+1/2, y+1/2'
'x, -y+1/2, -z+1/2'
'x, z+1/2, -y+1/2'
'z, y+1/2, -x+1/2'
'-x, y+1/2, -z+1/2'
'-z, y+1/2, x+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'z, -y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -z, y+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, z, -y+1/2'
'z+1/2, y, -x+1/2'
'-x+1/2, y, -z+1/2'
'-z+1/2, y, x+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -z+1/2, y'
'x+1/2, -y+1/2, -z'
'x+1/2, z+1/2, -y'
'z+1/2, y+1/2, -x'
'-x+1/2, y+1/2, -z'
'-z+1/2, y+1/2, x'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'z+1/2, -y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'-y, x+1/2, -z+1/2'
'-x, z+1/2, -y+1/2'
'-x, y+1/2, z+1/2'
'-x, -z+1/2, y+1/2'
'-z, -y+1/2, x+1/2'
'x, -y+1/2, z+1/2'
'z, -y+1/2, -x+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y, z+1/2, -x+1/2'
'-z, x+1/2, y+1/2'
'y, -z+1/2, x+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, z+1/2, x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-z, y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'y+1/2, -x, -z+1/2'
'x+1/2, y, -z+1/2'
'-y+1/2, x, -z+1/2'
'-x+1/2, z, -y+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -z, y+1/2'
'-z+1/2, -y, x+1/2'
'x+1/2, -y, z+1/2'
'z+1/2, -y, -x+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, z, -x+1/2'
'-z+1/2, x, y+1/2'
'y+1/2, -z, x+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, z, x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'y+1/2, -x+1/2, -z'
'x+1/2, y+1/2, -z'
'-y+1/2, x+1/2, -z'
'-x+1/2, z+1/2, -y'
'-x+1/2, y+1/2, z'
'-x+1/2, -z+1/2, y'
'-z+1/2, -y+1/2, x'
'x+1/2, -y+1/2, z'
'z+1/2, -y+1/2, -x'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/2, z+1/2, -x'
'-z+1/2, x+1/2, y'
'y+1/2, -z+1/2, x'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, z+1/2, x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-z+1/2, y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   23.832(2)
_cell_length_b                   23.832(2)
_cell_length_c                   23.832(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13536(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    509
_cell_measurement_temperature    100.02(10)
_cell_measurement_theta_max      36.0000
_cell_measurement_theta_min      5.2800
_shelx_estimated_absorpt_T_max   0.608
_shelx_estimated_absorpt_T_min   0.491
_exptl_absorpt_coefficient_mu    5.531
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            1233
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        36.366
_diffrn_reflns_theta_max         36.366
_diffrn_reflns_theta_min         5.250
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -113.00 -86.00   0.50  213.00    --  -54.78-125.00-115.00   54
  2  ω     85.00 127.00   0.50  213.00    --   56.34  90.00  33.00   84
  3  ω    -15.00  11.00   0.50  213.00    --  -54.78  19.00 -60.00   52
  4  ω    -16.00  12.00   0.50  213.00    --   56.34 -19.00-150.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                165
_reflns_number_total             201
_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 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         1.325
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         201
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.1440
_refine_ls_R_factor_gt           0.1330
_refine_ls_restrained_S_all      0.882
_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)+(0.3799P)²+824.6900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3553
_refine_ls_wR_factor_ref         0.3865
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 P8-C9
 1.7 with sigma of 0.02
 P8_$1-O2 \\sim P8_$1-O2_$1
 with sigma of 0.01
 P8_$1-O2_$1 \\sim P8_$1-O2 \\sim P8_$1-O6_$1
 with sigma of 0.01
 O6-O2_$1 \\sim O6-O2
 with sigma of 0.01
 P8-C9 \\sim P8_$23-C4
 with sigma of 0.01
 P8-C8 \\sim P8-C10
 with sigma of 0.01
 P8_$23-C5 \\sim P8_$23-C3
 with sigma of 0.01
 O2_$1-C9 \\sim O6-C9
 with sigma of 0.01
2. Restrained planarity
 P8, C9, C8, C10
 with sigma of 0.1
 P8_$23, C4, C3, C5
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
O2 \\sim Zr1 \\sim P8: within 3A with sigma of 0.03 and sigma for terminal
atoms of 0.06 within 3A
Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: P8(0.125) O6(0.125) C2(0.125) H2(0.125) C3(0.125) H3(0.125)
 C4(0.125) C5(0.125) H5(0.125) C6(0.125) C7(0.125) H7(0.125) C8(0.125)
 H8(0.125) C9(0.125) C10(0.125) H10(0.125) C11(0.125)
5.a Free rotating group:
 C2(C3,C4,C5,C6,C7,C8,C9,C10,C11)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C10(H10)
;
_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 0.500000 0.1036(3) 0.000000 0.112(7) Uani 1 8 d S TU P . .
O1 O 0.4544(14) 0.0456(14) -0.0456(14) 0.16(2) Uani 1 6 d S T P . .
O2 O 0.5761(18) 0.1532(14) 0.000000 0.170(14) Uani 1 2 d DS TU P . .
P8 P 0.6273(8) 0.1273(8) 0.0261(18) 0.25(2) Uani 0.25 1 d D U P A -1
O6 O 0.634(2) 0.134(2) 0.089(3) 0.36(5) Uani 0.25 1 d D U P A -1
C2 C 0.728(2) 0.3183(12) 0.032(4) 0.24(4) Uani 0.125 1 d G U P A -1
H2 H 0.697304 0.333332 0.052799 0.284 Uiso 0.125 1 calc R U P A -1
C3 C 0.7731(19) 0.3521(12) 0.019(4) 0.22(4) Uani 0.125 1 d DG U P A -1
H3 H 0.773499 0.390083 0.031463 0.267 Uiso 0.125 1 calc R U P A -1
C4 C 0.8190(13) 0.3303(9) -0.012(3) 0.22(4) Uani 0.125 1 d DG U P A -1
C5 C 0.8187(15) 0.2753(10) -0.029(3) 0.23(4) Uani 0.125 1 d DG U P A -1
H5 H 0.849587 0.261151 -0.050144 0.273 Uiso 0.125 1 calc R U P A -1
C6 C 0.7726(13) 0.2394(9) -0.017(2) 0.24(4) Uani 0.125 1 d G U P A -1
C7 C 0.771(2) 0.1824(13) -0.035(4) 0.24(4) Uani 0.125 1 d G U P A -1
H7 H 0.801516 0.167377 -0.055425 0.291 Uiso 0.125 1 calc R U P A -1
C8 C 0.7258(19) 0.1486(12) -0.022(4) 0.24(4) Uani 0.125 1 d DG U P A -1
H8 H 0.725355 0.110606 -0.034035 0.283 Uiso 0.125 1 calc R U P A -1
C9 C 0.6799(13) 0.1704(9) 0.009(3) 0.24(3) Uani 0.125 1 d DG U P A -1
C10 C 0.6802(15) 0.2254(9) 0.027(3) 0.24(4) Uani 0.125 1 d DG U P A -1
H10 H 0.649287 0.239537 0.047630 0.284 Uiso 0.125 1 calc R U P A -1
C11 C 0.7263(13) 0.2614(8) 0.014(2) 0.24(4) Uani 0.125 1 d G U P A -1


_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 Zr1 3.492(11) 5 ?
Zr1 Zr1 3.492(11) 101_655 ?
Zr1 Zr1 3.492(11) 74_545 ?
Zr1 O1 2.067(14) 99 ?
Zr1 O1 2.067(14) 76 ?
Zr1 O1 2.067(14) 170 ?
Zr1 O1 2.067(14) . ?
Zr1 O2 2.16(4) 102_655 ?
Zr1 O2 2.16(4) 99 ?
Zr1 O2 2.16(4) 58_554 ?
Zr1 O2 2.16(4) 56 ?
Zr1 O2 2.16(4) . ?
O2 O2 0.00(11) 99 ?
O2 P8 1.50(4) . ?
O2 P8 1.50(4) 99 ?
O2 P8 1.50(4) 91_545 ?
O2 P8 1.50(4) 188_545 ?
P8 O6 1.51(4) . ?
P8 C9 1.67(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.3785 . ?
C2 C11 1.4218 . ?
C3 H3 0.9500 . ?
C3 C4 1.4190 . ?
C4 C5 1.3772 . ?
C5 H5 0.9500 . ?
C5 C6 1.4225 . ?
C6 C7 1.4225 . ?
C6 C11 1.4331 . ?
C7 H7 0.9500 . ?
C7 C8 1.3786 . ?
C8 H8 0.9500 . ?
C8 C9 1.4188 . ?
C9 C10 1.3775 . ?
C10 H10 0.9500 . ?
C10 C11 1.4235 . ?

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
Zr1 Zr1 Zr1 90.0 101_655 5 ?
Zr1 Zr1 Zr1 60.0 74_545 101_655 ?
Zr1 Zr1 Zr1 60.0 74_545 5 ?
O1 Zr1 Zr1 84.2(14) 170 101_655 ?
O1 Zr1 Zr1 32.3(6) . 74_545 ?
O1 Zr1 Zr1 84.2(14) 76 5 ?
O1 Zr1 Zr1 32.4(6) 99 5 ?
O1 Zr1 Zr1 32.4(6) 76 101_655 ?
O1 Zr1 Zr1 84.2(14) 170 74_545 ?
O1 Zr1 Zr1 84.2(14) 99 101_655 ?
O1 Zr1 Zr1 32.4(6) 99 74_545 ?
O1 Zr1 Zr1 84.2(14) . 5 ?
O1 Zr1 Zr1 32.3(6) . 101_655 ?
O1 Zr1 Zr1 32.4(6) 170 5 ?
O1 Zr1 Zr1 84.2(14) 76 74_545 ?
O1 Zr1 O1 63.4(18) . 99 ?
O1 Zr1 O1 96(3) . 170 ?
O1 Zr1 O1 63.4(18) 76 170 ?
O1 Zr1 O1 63.4(18) . 76 ?
O1 Zr1 O1 96(3) 99 76 ?
O1 Zr1 O1 63.4(18) 99 170 ?
O1 Zr1 O2 143.7(5) 170 102_655 ?
O1 Zr1 O2 143.7(5) 76 102_655 ?
O1 Zr1 O2 85.7(15) 76 99 ?
O1 Zr1 O2 85.7(15) 170 58_554 ?
O1 Zr1 O2 143.7(5) 99 99 ?
O1 Zr1 O2 85.7(15) 76 . ?
O1 Zr1 O2 85.7(15) 76 56 ?
O1 Zr1 O2 143.7(5) . . ?
O1 Zr1 O2 85.7(15) 99 58_554 ?
O1 Zr1 O2 85.7(15) 99 102_655 ?
O1 Zr1 O2 85.7(15) 170 99 ?
O1 Zr1 O2 143.7(5) . 99 ?
O1 Zr1 O2 143.7(5) 99 . ?
O1 Zr1 O2 143.7(5) 76 58_554 ?
O1 Zr1 O2 85.7(15) 170 . ?
O1 Zr1 O2 85.7(15) . 56 ?
O1 Zr1 O2 143.7(5) 170 56 ?
O1 Zr1 O2 143.7(5) . 58_554 ?
O1 Zr1 O2 85.7(15) . 102_655 ?
O1 Zr1 O2 143.7(5) 99 56 ?
O2 Zr1 Zr1 168.1(10) 58_554 101_655 ?
O2 Zr1 Zr1 112.7(7) 58_554 74_545 ?
O2 Zr1 Zr1 112.7(7) 99 101_655 ?
O2 Zr1 Zr1 112.7(7) . 5 ?
O2 Zr1 Zr1 168.1(10) 99 74_545 ?
O2 Zr1 Zr1 112.7(7) 56 74_545 ?
O2 Zr1 Zr1 112.7(7) 102_655 101_655 ?
O2 Zr1 Zr1 112.7(7) 99 5 ?
O2 Zr1 Zr1 78.1(10) 58_554 5 ?
O2 Zr1 Zr1 168.1(10) 56 5 ?
O2 Zr1 Zr1 112.7(7) 102_655 5 ?
O2 Zr1 Zr1 112.7(7) . 101_655 ?
O2 Zr1 Zr1 78.1(10) 102_655 74_545 ?
O2 Zr1 Zr1 168.1(10) . 74_545 ?
O2 Zr1 Zr1 78.1(10) 56 101_655 ?
O2 Zr1 O2 114(2) . 102_655 ?
O2 Zr1 O2 72.7(10) . 56 ?
O2 Zr1 O2 72.7(10) 58_554 102_655 ?
O2 Zr1 O2 114(2) 58_554 56 ?
O2 Zr1 O2 72.7(10) 99 56 ?
O2 Zr1 O2 72.7(10) . 58_554 ?
O2 Zr1 O2 114(2) 99 102_655 ?
O2 Zr1 O2 72.7(10) 102_655 56 ?
O2 Zr1 O2 72.7(10) 99 58_554 ?
O2 Zr1 O2 0.0(19) 99 . ?
Zr1 O1 Zr1 115.3(11) . 74_545 ?
Zr1 O1 Zr1 115.3(11) 101_655 74_545 ?
Zr1 O1 Zr1 115.3(11) . 101_655 ?
O2 O2 Zr1 0(10) 99 . ?
O2 O2 P8 0(10) 99 188_545 ?
O2 O2 P8 0(10) 99 . ?
O2 O2 P8 0(10) 99 91_545 ?
O2 O2 P8 0(10) 99 99 ?
P8 O2 Zr1 117(2) 188_545 . ?
P8 O2 Zr1 117(2) 91_545 . ?
P8 O2 Zr1 117(2) . . ?
P8 O2 Zr1 117(2) 99 . ?
P8 O2 P8 0.0(8) 188_545 . ?
P8 O2 P8 49(3) . 99 ?
P8 O2 P8 49(3) 188_545 99 ?
P8 O2 P8 0.0(8) 91_545 99 ?
P8 O2 P8 49(3) 91_545 . ?
P8 O2 P8 49(3) 188_545 91_545 ?
O2 P8 O6 117(2) . . ?
O2 P8 C9 105(2) . . ?
O6 P8 C9 94.8(19) . . ?
C3 C2 H2 119.6 . . ?
C3 C2 C11 120.9 . . ?
C11 C2 H2 119.6 . . ?
P8 C3 H3 86.4 20_665 . ?
C2 C3 P8 153.7(4) . 20_665 ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.2 . . ?
C4 C3 P8 33.5(4) . 20_665 ?
C4 C3 H3 119.9 . . ?
C3 C4 P8 118.6(5) . 20_665 ?
C5 C4 P8 121.2(5) . 20_665 ?
C5 C4 C3 120.3 . . ?
P8 C5 H5 87.1 20_665 . ?
C4 C5 P8 32.5(4) . 20_665 ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 120.9 . . ?
C6 C5 P8 153.4(4) . 20_665 ?
C6 C5 H5 119.6 . . ?
C5 C6 C11 118.9 . . ?
C7 C6 C5 122.3 . . ?
C7 C6 C11 118.8 . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 120.9 . . ?
C8 C7 H7 119.5 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.2 . . ?
C9 C8 H8 119.9 . . ?
P8 C9 O2 39.6(9) . 91_545 ?
C8 C9 O2 79.1(10) . 91_545 ?
C8 C9 P8 118.7(5) . . ?
C10 C9 O2 160.3(12) . 91_545 ?
C10 C9 P8 121.0(5) . . ?
C10 C9 C8 120.3 . . ?
C9 C10 H10 119.6 . . ?
C9 C10 C11 120.9 . . ?
C11 C10 H10 119.6 . . ?
C2 C11 C6 118.9 . . ?
C2 C11 C10 122.2 . . ?
C10 C11 C6 118.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr1 O2 P8 O6 -86(3) . . . . ?
Zr1 O2 P8 C9 170.2(14) . . . . ?
O2 O2 P8 O6 0.0(6) 99 . . . ?
O2 O2 P8 C9 0.0(3) 99 . . . ?
O2 P8 C9 O2 -123(4) . . . 91_545 ?
O2 P8 C9 C8 -121(4) . . . . ?
O2 P8 C9 C10 62(4) . . . . ?
O2 C9 C10 C11 169(8) 91_545 . . . ?
P8 O2 P8 O6 170(3) 91_545 . . . ?
P8 O2 P8 O6 28(100) 188_545 . . . ?
P8 O2 P8 O6 170(3) 99 . . . ?
P8 O2 P8 C9 66.7(19) 99 . . . ?
P8 O2 P8 C9 -75(100) 188_545 . . . ?
P8 O2 P8 C9 66.7(19) 91_545 . . . ?
P8 C3 C4 C5 -180(3) 20_665 . . . ?
P8 C4 C5 C6 -180(3) 20_665 . . . ?
P8 C5 C6 C7 180(4) 20_665 . . . ?
P8 C5 C6 C11 0(4) 20_665 . . . ?
P8 C9 C10 C11 177(3) . . . . ?
O6 P8 C9 O2 118(2) . . . 91_545 ?
O6 P8 C9 C8 119(3) . . . . ?
O6 P8 C9 C10 -58(3) . . . . ?
C2 C3 C4 P8 180(3) . . . 20_665 ?
C2 C3 C4 C5 0.1 . . . . ?
C3 C2 C11 C6 0.0 . . . . ?
C3 C2 C11 C10 179.9 . . . . ?
C3 C4 C5 P8 180(3) . . . 20_665 ?
C3 C4 C5 C6 -0.1 . . . . ?
C4 C5 C6 C7 -180.0 . . . . ?
C4 C5 C6 C11 0.1 . . . . ?
C5 C6 C7 C8 180.0 . . . . ?
C5 C6 C11 C2 0.0 . . . . ?
C5 C6 C11 C10 -180.0 . . . . ?
C6 C7 C8 C9 0.0 . . . . ?
C7 C6 C11 C2 -180.0 . . . . ?
C7 C6 C11 C10 0.1 . . . . ?
C7 C8 C9 O2 -176(3) . . . 91_545 ?
C7 C8 C9 P8 -177(3) . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C9 C10 C11 C2 180.0 . . . . ?
C9 C10 C11 C6 -0.1 . . . . ?
C11 C2 C3 P8 0(4) . . . 20_665 ?
C11 C2 C3 C4 0.0 . . . . ?
C11 C6 C7 C8 -0.1 . . . . ?

_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 -0.110 -0.454 -0.759 5640.2 1357.9 '134.4 H2O'

_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'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_vrf_PLAT084_NU-407              
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.39 Report
RESPONSE: The crystal was from post-synthetic oxidation from which only
diffract to 1.3 angstrom and caused high wR2.
;
_vrf_PLAT088_NU-407              
;
PROBLEM: Poor Data / Parameter Ratio ....................       2.07 Note  
RESPONSE: The crystal was from post-synthetic oxidation from which only
diffract to 1.3 angstrom. The linker in asymmetric unit has positional 
disorder due to the high symmetry of the space group which require constrains
with parameters.
;
_vrf_PLAT242_NU-407              
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Zr1 Check 
RESPONSE: The relatively low 'MainMol' Ueq is resulted from the 
disorder of linkers around Zr1.
;
# start Validation Reply Form
_vrf_THETM01_NU-407              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystal was from post-synthetic oxidation from which only
diffract to 1.3 angstrom.
;
####################################################################### 
# 
# 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_NU-410
_database_code_depnum_ccdc_archive 'CCDC 2260135'
loop_
_audit_author_name
_audit_author_address
'Haomiao Xie'
;Northwestern University
United States of America
;
_audit_update_record             
;
2023-05-01 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_audit_creation_date             2023-01-25
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C72 H48 O32 P12 Zr6'
_chemical_formula_sum            'C72 H48 O32 P12 Zr6'
_chemical_formula_weight         2344.06
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'y, -x+1/2, z+1/2'
'x, -z+1/2, y+1/2'
'x, -y+1/2, -z+1/2'
'x, z+1/2, -y+1/2'
'z, y+1/2, -x+1/2'
'-x, y+1/2, -z+1/2'
'-z, y+1/2, x+1/2'
'z, x+1/2, y+1/2'
'y, z+1/2, x+1/2'
'-y, -z+1/2, x+1/2'
'z, -x+1/2, -y+1/2'
'-y, z+1/2, -x+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, -z+1/2, -x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'z, -y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-y+1/2, x, z+1/2'
'-x+1/2, -y, z+1/2'
'y+1/2, -x, z+1/2'
'x+1/2, -z, y+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, z, -y+1/2'
'z+1/2, y, -x+1/2'
'-x+1/2, y, -z+1/2'
'-z+1/2, y, x+1/2'
'z+1/2, x, y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, -z, x+1/2'
'z+1/2, -x, -y+1/2'
'-y+1/2, z, -x+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, -z, -x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-y+1/2, x+1/2, z'
'-x+1/2, -y+1/2, z'
'y+1/2, -x+1/2, z'
'x+1/2, -z+1/2, y'
'x+1/2, -y+1/2, -z'
'x+1/2, z+1/2, -y'
'z+1/2, y+1/2, -x'
'-x+1/2, y+1/2, -z'
'-z+1/2, y+1/2, x'
'z+1/2, x+1/2, y'
'y+1/2, z+1/2, x'
'-y+1/2, -z+1/2, x'
'z+1/2, -x+1/2, -y'
'-y+1/2, z+1/2, -x'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, -z+1/2, -x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'z+1/2, -y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'y, -x, -z'
'x, y, -z'
'-y, x, -z'
'-x, z, -y'
'-x, y, z'
'-x, -z, y'
'-z, -y, x'
'x, -y, z'
'z, -y, -x'
'-z, -x, -y'
'-y, -z, -x'
'y, z, -x'
'-z, x, y'
'y, -z, x'
'z, x, -y'
'z, -x, y'
'-y, z, x'
'-y, -x, z'
'y, x, z'
'x, -z, -y'
'x, z, y'
'-z, y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'-y, x+1/2, -z+1/2'
'-x, z+1/2, -y+1/2'
'-x, y+1/2, z+1/2'
'-x, -z+1/2, y+1/2'
'-z, -y+1/2, x+1/2'
'x, -y+1/2, z+1/2'
'z, -y+1/2, -x+1/2'
'-z, -x+1/2, -y+1/2'
'-y, -z+1/2, -x+1/2'
'y, z+1/2, -x+1/2'
'-z, x+1/2, y+1/2'
'y, -z+1/2, x+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, z+1/2, x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-z, y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'y+1/2, -x, -z+1/2'
'x+1/2, y, -z+1/2'
'-y+1/2, x, -z+1/2'
'-x+1/2, z, -y+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -z, y+1/2'
'-z+1/2, -y, x+1/2'
'x+1/2, -y, z+1/2'
'z+1/2, -y, -x+1/2'
'-z+1/2, -x, -y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, z, -x+1/2'
'-z+1/2, x, y+1/2'
'y+1/2, -z, x+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, z, x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'y+1/2, -x+1/2, -z'
'x+1/2, y+1/2, -z'
'-y+1/2, x+1/2, -z'
'-x+1/2, z+1/2, -y'
'-x+1/2, y+1/2, z'
'-x+1/2, -z+1/2, y'
'-z+1/2, -y+1/2, x'
'x+1/2, -y+1/2, z'
'z+1/2, -y+1/2, -x'
'-z+1/2, -x+1/2, -y'
'-y+1/2, -z+1/2, -x'
'y+1/2, z+1/2, -x'
'-z+1/2, x+1/2, y'
'y+1/2, -z+1/2, x'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, z+1/2, x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-z+1/2, y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   27.5175(5)
_cell_length_b                   27.5175(5)
_cell_length_c                   27.5175(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     20836.6(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2695
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      50.3830
_cell_measurement_theta_min      4.5350
_shelx_estimated_absorpt_T_max   0.718
_shelx_estimated_absorpt_T_min   0.637
_exptl_absorpt_coefficient_mu    3.544
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.747
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4624
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            4896
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        50.381
_diffrn_reflns_theta_max         50.381
_diffrn_reflns_theta_min         4.545
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                547
_reflns_number_total             608
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.631
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         608
_refine_ls_number_restraints     177
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0991
_refine_ls_restrained_S_all      1.077
_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)+(0.1003P)²+605.7758P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2412
_refine_ls_wR_factor_ref         0.2458
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C4-C10
 1.48 with sigma of 0.02
 P1_$1-O2_$2 \\sim P1_$1-O2_$1
 with sigma of 0.01
 P1-C2 \\sim P1-C6
 with sigma of 0.01
 P1_$3-C12 \\sim P1_$3-C8
 with sigma of 0.01
 P1_$3-C7 \\sim P1-C1
 with sigma of 0.01
 C9-C4 \\sim C5-C10 \\sim C3-C10 \\sim C4-C11
 with sigma of 0.01
2. Restrained planarity
 C6, C1, C2, P1
 with sigma of 0.1
 P1_$3, C7, C12, C8
 with sigma of 0.1
 C5, C4, C3, C10
 with sigma of 0.1
 C4, C10, C11, C9
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
P1 \\sim O2 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C10 \\sim C9 \\sim C11 \\sim C12 \\sim C7 \\sim C8 \\sim C4: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C4 \\sim C5 \\sim C3 \\sim C2 \\sim C6 \\sim C1: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C6) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
4. Others
 Fixed Sof: P1(0.125) C10(0.125) C11(0.125) H11(0.125) C12(0.0625) H12(0.125)
 C7(0.125) C8(0.125) H8(0.125) C9(0.125) H9(0.125) C1(0.125) C2(0.125)
 H2(0.125) C3(0.125) H3(0.125) C4(0.125) C5(0.125) H5(0.125) C6(0.125) H6(0.125)
5.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C8(H8), C9(H9), C2(H2), C3(H3), C5(H5), C6(H6)
5.b Fitted hexagon refined as free rotating group:
 C10(C11,C12,C7,C8,C9), C1(C2,C3,C4,C5,C6)
;
_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
Zr2 Zr 0.40897(7) 0.000000 0.000000 0.0939(13) Uani 1 8 d S T P . .
O2 O 0.3671(5) 0.000000 0.0693(7) 0.192(7) Uani 1 2 d S TU P . .
P1 P 0.3846(3) -0.0305(6) 0.1154(3) 0.217(9) Uani 0.25 1 d D U P A -1
C10 C 0.2456(10) -0.0047(19) 0.2853(10) 0.142(17) Uani 0.125 1 d DG U P A -1
C11 C 0.1984(11) -0.009(3) 0.2679(11) 0.15(2) Uani 0.125 1 d DG U P A -1
H11 H 0.193016 -0.019027 0.235132 0.175 Uiso 0.125 1 calc R U P A -1
C12 C 0.1592(9) 0.000(3) 0.2983(10) 0.14(2) Uani 0.125 1 d DG U P A -1
H12 H 0.126976 -0.003456 0.286391 0.173 Uiso 0.125 1 calc R U P A -1
C7 C 0.1672(6) 0.0138(13) 0.3462(6) 0.13(2) Uani 0.125 1 d DG U P A -1
C8 C 0.2143(6) 0.0186(19) 0.3636(7) 0.100(19) Uani 0.125 1 d DG U P A -1
H8 H 0.219759 0.028201 0.396312 0.120 Uiso 0.125 1 calc R U P A -1
C9 C 0.2536(7) 0.009(2) 0.3331(10) 0.109(18) Uani 0.125 1 d DG U P A -1
H9 H 0.285799 0.012631 0.345054 0.130 Uiso 0.125 1 calc R U P A -1
C1 C 0.3502(12) -0.0203(10) 0.1715(10) 0.204(19) Uani 0.125 1 d DG U P A -1
C2 C 0.328(3) 0.0244(10) 0.179(2) 0.21(2) Uani 0.125 1 d DG U P A -1
H2 H 0.334138 0.050729 0.158014 0.247 Uiso 0.125 1 calc R U P A -1
C3 C 0.297(3) 0.0305(13) 0.219(2) 0.19(2) Uani 0.125 1 d DG U P A -1
H3 H 0.281721 0.061040 0.224176 0.232 Uiso 0.125 1 calc R U P A -1
C4 C 0.2879(12) -0.0081(18) 0.2501(12) 0.176(19) Uani 0.125 1 d DG U P A -1
C5 C 0.310(2) -0.053(2) 0.2422(15) 0.19(2) Uani 0.125 1 d DG U P A -1
H5 H 0.303922 -0.079124 0.263609 0.225 Uiso 0.125 1 calc R U P A -1
C6 C 0.341(2) -0.0589(17) 0.2029(15) 0.19(2) Uani 0.125 1 d DG U P A -1
H6 H 0.356338 -0.089435 0.197446 0.231 Uiso 0.125 1 calc R U P A -1
O1 O 0.4571(4) 0.0429(4) 0.0429(4) 0.101(5) Uani 1 6 d S T 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
Zr2 Zr2 3.543(3) 56 ?
Zr2 Zr2 3.543(3) 152_554 ?
Zr2 Zr2 3.543(3) 74_545 ?
Zr2 Zr2 3.543(3) 170 ?
Zr2 O2 2.227(16) 117 ?
Zr2 O2 2.227(16) 99 ?
Zr2 O2 2.227(16) . ?
Zr2 O2 2.227(16) 7 ?
Zr2 O1 2.130(5) 74_545 ?
Zr2 O1 2.130(5) 99 ?
Zr2 O1 2.131(5) . ?
Zr2 O1 2.130(5) 172_545 ?
O2 P1 1.596(17) . ?
P1 C1 1.834(17) . ?
C10 C11 1.3900 . ?
C10 C9 1.3900 . ?
C10 C4 1.516(19) . ?
C11 H11 0.9500 . ?
C11 C12 1.3900 . ?
C12 H12 0.9500 . ?
C12 C7 1.3900 . ?
C7 C8 1.3900 . ?
C8 H8 0.9500 . ?
C8 C9 1.3900 . ?
C9 H9 0.9500 . ?
C1 C2 1.3900 . ?
C1 C6 1.3900 . ?
C2 H2 0.9500 . ?
C2 C3 1.3900 . ?
C3 H3 0.9500 . ?
C3 C4 1.3900 . ?
C4 C5 1.3900 . ?
C5 H5 0.9500 . ?
C5 C6 1.3900 . ?
C6 H6 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 Zr2 Zr2 60.0 74_545 152_554 ?
Zr2 Zr2 Zr2 90.0 170 74_545 ?
Zr2 Zr2 Zr2 60.0 56 74_545 ?
Zr2 Zr2 Zr2 90.0 56 152_554 ?
Zr2 Zr2 Zr2 60.0 170 56 ?
Zr2 Zr2 Zr2 60.0 170 152_554 ?
O2 Zr2 Zr2 111.5(3) 7 152_554 ?
O2 Zr2 Zr2 166.2(5) . 152_554 ?
O2 Zr2 Zr2 76.2(5) 117 74_545 ?
O2 Zr2 Zr2 111.5(3) 99 170 ?
O2 Zr2 Zr2 76.1(5) 99 152_554 ?
O2 Zr2 Zr2 111.5(3) 99 74_545 ?
O2 Zr2 Zr2 166.2(5) 99 56 ?
O2 Zr2 Zr2 76.1(5) 7 170 ?
O2 Zr2 Zr2 111.5(3) 117 56 ?
O2 Zr2 Zr2 111.5(3) . 74_545 ?
O2 Zr2 Zr2 76.2(5) . 56 ?
O2 Zr2 Zr2 166.2(5) 7 74_545 ?
O2 Zr2 Zr2 166.2(5) 117 170 ?
O2 Zr2 Zr2 111.5(3) 117 152_554 ?
O2 Zr2 Zr2 111.5(3) . 170 ?
O2 Zr2 Zr2 111.5(3) 7 56 ?
O2 Zr2 O2 74.5(4) . 7 ?
O2 Zr2 O2 74.5(4) 117 99 ?
O2 Zr2 O2 117.7(9) 117 7 ?
O2 Zr2 O2 74.5(4) 117 . ?
O2 Zr2 O2 74.5(4) 99 7 ?
O2 Zr2 O2 117.7(9) . 99 ?
O1 Zr2 Zr2 33.8(2) 74_545 74_545 ?
O1 Zr2 Zr2 33.8(2) 74_545 56 ?
O1 Zr2 Zr2 87.2(4) 99 74_545 ?
O1 Zr2 Zr2 33.8(2) 172_545 152_554 ?
O1 Zr2 Zr2 87.2(4) 172_545 56 ?
O1 Zr2 Zr2 33.8(2) 172_545 74_545 ?
O1 Zr2 Zr2 33.8(2) 99 152_554 ?
O1 Zr2 Zr2 87.2(4) 172_545 170 ?
O1 Zr2 Zr2 33.8(2) 99 170 ?
O1 Zr2 Zr2 33.8(2) . 170 ?
O1 Zr2 Zr2 87.2(4) 99 56 ?
O1 Zr2 Zr2 87.2(4) 74_545 170 ?
O1 Zr2 Zr2 33.8(2) . 56 ?
O1 Zr2 Zr2 87.2(4) . 152_554 ?
O1 Zr2 Zr2 87.2(4) . 74_545 ?
O1 Zr2 Zr2 87.2(4) 74_545 152_554 ?
O1 Zr2 O2 142.71(19) 74_545 7 ?
O1 Zr2 O2 81.3(5) 74_545 117 ?
O1 Zr2 O2 81.3(5) 99 7 ?
O1 Zr2 O2 142.71(19) 172_545 . ?
O1 Zr2 O2 81.3(5) 172_545 117 ?
O1 Zr2 O2 142.71(19) . 117 ?
O1 Zr2 O2 142.71(19) . 99 ?
O1 Zr2 O2 81.3(5) 74_545 . ?
O1 Zr2 O2 81.3(5) . . ?
O1 Zr2 O2 81.3(5) 99 99 ?
O1 Zr2 O2 81.3(5) . 7 ?
O1 Zr2 O2 142.71(19) 74_545 99 ?
O1 Zr2 O2 142.71(19) 99 117 ?
O1 Zr2 O2 81.3(5) 172_545 99 ?
O1 Zr2 O2 142.71(19) 172_545 7 ?
O1 Zr2 O2 142.71(19) 99 . ?
O1 Zr2 O1 67.2(5) 99 . ?
O1 Zr2 O1 67.2(5) 74_545 172_545 ?
O1 Zr2 O1 103.1(10) 99 74_545 ?
O1 Zr2 O1 103.1(10) 172_545 . ?
O1 Zr2 O1 67.2(5) 74_545 . ?
O1 Zr2 O1 67.2(5) 99 172_545 ?
P1 O2 Zr2 121.6(7) . . ?
O2 P1 C1 115.6(13) . . ?
C11 C10 C9 120.0 . . ?
C11 C10 C4 119.4(4) . . ?
C9 C10 C4 120.1(4) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
P1 C12 H12 85.3 145 . ?
C11 C12 P1 154.5(3) . 145 ?
C11 C12 H12 120.0 . . ?
C11 C12 C7 120.0 . . ?
C7 C12 P1 34.8(3) . 145 ?
C7 C12 H12 120.0 . . ?
C12 C7 P1 119.6(4) . 145 ?
C12 C7 C8 120.0 . . ?
C8 C7 P1 120.2(4) . 145 ?
P1 C8 H8 85.7 145 . ?
C7 C8 P1 34.4(3) . 145 ?
C7 C8 H8 120.0 . . ?
C9 C8 P1 154.2(3) . 145 ?
C9 C8 C7 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 H9 120.0 . . ?
C8 C9 C10 120.0 . . ?
C8 C9 H9 120.0 . . ?
C2 C1 P1 119.6(4) . . ?
C2 C1 C6 120.0 . . ?
C6 C1 P1 119.9(4) . . ?
C1 C2 H2 120.0 . . ?
C1 C2 C3 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C10 119.0(4) . . ?
C3 C4 C5 120.0 . . ?
C5 C4 C10 119.5(5) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 H5 120.0 . . ?
C1 C6 H6 120.0 . . ?
C5 C6 C1 120.0 . . ?
C5 C6 H6 120.0 . . ?
Zr2 O1 Zr2 112.5(4) . 56 ?
Zr2 O1 Zr2 112.5(4) 170 56 ?
Zr2 O1 Zr2 112.5(4) . 170 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zr2 O2 P1 C1 172.6(13) . . . . ?
O2 P1 C1 C2 -29(4) . . . . ?
O2 P1 C1 C6 143(4) . . . . ?
P1 C12 C7 C8 -175(2) 145 . . . ?
P1 C7 C8 C9 -175(2) 145 . . . ?
P1 C8 C9 C10 -6(3) 145 . . . ?
P1 C1 C2 C3 172(2) . . . . ?
P1 C1 C6 C5 -172(2) . . . . ?
C10 C11 C12 P1 6(3) . . . 145 ?
C10 C11 C12 C7 0.0 . . . . ?
C10 C4 C5 C6 165.8(14) . . . . ?
C11 C10 C9 C8 0.0 . . . . ?
C11 C10 C4 C3 74(5) . . . . ?
C11 C10 C4 C5 -92(5) . . . . ?
C11 C12 C7 P1 175(2) . . . 145 ?
C11 C12 C7 C8 0.0 . . . . ?
C12 C7 C8 P1 175(2) . . . 145 ?
C12 C7 C8 C9 0.0 . . . . ?
C7 C8 C9 C10 0.0 . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C9 C10 C4 C3 -98(5) . . . . ?
C9 C10 C4 C5 96(5) . . . . ?
C1 C2 C3 C4 0.0 . . . . ?
C2 C1 C6 C5 0.0 . . . . ?
C2 C3 C4 C10 -165.9(14) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C4 C10 C11 C12 -171.7(17) . . . . ?
C4 C10 C9 C8 171.6(17) . . . . ?
C4 C5 C6 C1 0.0 . . . . ?
C6 C1 C2 C3 0.0 . . . . ?

_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 -0.794 -0.759 -0.688 10010.4 2827.7 '288 H2O'

_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'
_vrf_PLAT088_NU-410              
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.74 Note  
RESPONSE: The crystal was from solvent-assisted ligand exchange conversion which 
resulted in a relatively low resolution and only diffracted to 1.0 angstrom. The 
phophinate ligand has severe disorder due to the high symmetry of Fm-3m space 
group.
;
_vrf_PLAT242_NU-410              
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Zr2 Check 
RESPONSE: The crystal was from solvent-assisted ligand exchange conversion which 
resulted in a relatively low resolution and only diffracted to 1.0 angstrom. The 
phophinate ligand has severe disorder due to the high symmetry of Fm-3m space 
group.The thermal ellipsoids around Zr2 are affected by the disorder.
;
_vrf_PLAT430_NU-410              
;
PROBLEM: Short Inter D...A Contact  O1       ..O1       .       2.36 Ang.  
RESPONSE: The O1...O1 pair is not a shourt inter D...A pair. It matches the distance
between mu3-oxygen atoms in CCDC database. 
;
# start Validation Reply Form
_vrf_THETM01_NU-410              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystal was from solvent-assisted ligand exchange conversion which 
resulted in a relatively low resolution and only diffracted to 1.0 angstrom.
;
