# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1849328'
loop_
_audit_author_name
_audit_author_address
'Aleksander Shkurenko'
;King Abdullah University of Science & Technology
Saudi Arabia
;
_audit_update_record             
;
2018-06-14 deposited with the CCDC.	2020-01-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(Zr 4+)6 (O H 1-)16 (C54 H26 N2 O12 4-)2'
_chemical_formula_sum            'C108 H68 N4 O40 Zr6'
_chemical_formula_weight         2608.98

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_H-M_alt        'C m m m'
_space_group_name_Hall           '-C 2 2'

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

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

_cell_length_a                   20.7974(9)
_cell_length_b                   34.3196(13)
_cell_length_c                   24.2844(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     17333(1)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    8317
_cell_measurement_theta_min      4.41
_cell_measurement_theta_max      51.24

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.500
_exptl_crystal_F_000             2608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.003
_exptl_absorpt_coefficient_mu    1.666
_shelx_estimated_absorpt_T_min   0.788
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0414
_exptl_absorpt_correction_T_max  0.1249
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1216 before and 0.0634 after correction.
The Ratio of minimum to maximum transmission is 0.3315.
The λ/2 correction factor is Not present.
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Incoatec I\ms'
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            22259
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.409
_diffrn_reflns_theta_max         50.421
_diffrn_reflns_theta_full        50.421
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4918
_reflns_number_gt                3701
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material  
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'

_refine_special_details          
;A full list of restraints and constraints is contained
 within the CIF file.
 A set of restraints and constraints was applied to make
 both geometry and thermal parameters of organic and solvent
 molecules reasonable.
 Hydrogen atoms are placed at the calculated positions and refined using
 a riding model with Uiso(H) = 1.2Ueq(C, O) or 1.5Ueq(C,O).
 The PLATON SQUEEZE procedure was applied to exclude the diffused
 solvent contribution from the structure factors. 5406 Electrons
 were found in the voids of the total volume of 13337 A^3.,SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1207P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4918
_refine_ls_number_parameters     216
_refine_ls_number_restraints     192
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0517
_refine_ls_wR_factor_ref         0.1767
_refine_ls_wR_factor_gt          0.1716
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.5000 0.57120(2) 0.5000 0.0641(3) Uani 1 4 d S T P . .
Zr2 Zr 0.58490(3) 0.5000 0.57300(2) 0.0686(3) Uani 1 2 d S T P A .
O1 O 0.56398(17) 0.60361(8) 0.55409(12) 0.0703(9) Uani 1 1 d . U . . .
O2 O 0.61794(19) 0.55894(8) 0.60284(13) 0.0877(11) Uani 1 1 d D U . . .
O1H O 0.5000 0.53424(14) 0.5718(2) 0.0982(17) Uani 1 2 d S T P A 2
H1H H 0.5000 0.5513 0.6052 0.118 Uiso 1 2 calc R U P A 2
O2H O 0.5848(3) 0.53431(14) 0.5000 0.0994(18) Uani 1 2 d S T P A 2
H2H H 0.6239 0.5513 0.5000 0.119 Uiso 1 2 calc R U P A 2
O3H O 0.5774(3) 0.5000 0.66308(18) 0.0908(16) Uani 1 2 d S T P . .
H3H H 0.5958 0.4802 0.6758 0.136 Uiso 0.5 1 calc R U P A .
O4H O 0.6907(3) 0.5000 0.5684(3) 0.1033(17) Uani 1 2 d S T P . .
H4H H 0.7038 0.4772 0.5631 0.155 Uiso 0.5 1 calc R U P A .
C1 C 0.6030(3) 0.59357(12) 0.58979(19) 0.0770(13) Uani 1 1 d D U . . .
C2 C 0.63563(18) 0.62547(6) 0.62183(11) 0.0816(14) Uani 1 1 d DG U . . .
C3 C 0.62942(19) 0.66362(7) 0.60337(11) 0.0965(18) Uani 1 1 d G U . . .
H3 H 0.6053 0.6690 0.5711 0.116 Uiso 1 1 calc R U . . .
C4 C 0.65851(19) 0.69384(5) 0.63220(12) 0.1035(19) Uani 1 1 d G U . . .
H4 H 0.6543 0.7199 0.6196 0.124 Uiso 1 1 calc R U . . .
C5 C 0.69382(18) 0.68591(7) 0.67949(11) 0.0898(16) Uani 1 1 d DG U . . .
C6 C 0.70004(18) 0.64776(8) 0.69795(11) 0.0974(18) Uani 1 1 d G U . . .
H6 H 0.7242 0.6423 0.7303 0.117 Uiso 1 1 calc R U . . .
C7 C 0.67095(18) 0.61754(6) 0.66912(12) 0.0919(16) Uani 1 1 d G U . . .
H7 H 0.6752 0.5915 0.6817 0.110 Uiso 1 1 calc R U . . .
C8 C 0.7500 0.7500 0.6829(2) 0.092(2) Uani 1 2 d DS TU P . .
H8 H 0.7500 0.7500 0.6437 0.110 Uiso 1 2 calc R U P . .
C9 C 0.7233(3) 0.71862(13) 0.71078(15) 0.0881(16) Uani 1 1 d D U . . .
C10 C 0.7251(3) 0.71843(14) 0.76897(16) 0.0985(19) Uani 1 1 d D U . . .
H10 H 0.7092 0.6967 0.7890 0.118 Uiso 1 1 calc R U . . .
C11 C 0.7500 0.7500 0.7960(2) 0.100(2) Uani 1 2 d DS TU P . .
N1 N 0.7500 0.7500 0.8568(2) 0.0943(16) Uani 1 2 d S TU P . .
O3A O 0.8333(6) 0.7088(4) 0.8561(5) 0.147(5) Uani 0.5 1 d D U P B 1
C12A C 0.7953(6) 0.7275(3) 0.8839(5) 0.103(3) Uani 0.5 1 d D U P B 1
C13A C 0.7944(4) 0.7278(2) 0.9423(4) 0.096(3) Uani 0.5 1 d D U P B 1
O3B O 0.8559(7) 0.7318(4) 0.8560(6) 0.181(7) Uani 0.5 1 d D U P B 2
C12B C 0.8081(8) 0.7400(2) 0.8833(5) 0.128(5) Uani 0.5 1 d D U P B 2
C13B C 0.8047(5) 0.7406(2) 0.9415(5) 0.125(5) Uani 0.5 1 d D U P B 2
C14 C 0.7500 0.7500 0.97119(16) 0.0903(19) Uani 1 2 d DS TU P . .
C15A C 0.8377(7) 0.7062(4) 0.97108(19) 0.154(8) Uani 0.5 1 d D U P B 1
H15A H 0.8685 0.6910 0.9518 0.185 Uiso 0.5 1 calc R U P B 1
C15B C 0.8586(8) 0.7316(4) 0.9713(2) 0.169(9) Uani 0.5 1 d D U P B 2
H15B H 0.8970 0.7251 0.9523 0.202 Uiso 0.5 1 calc R U P B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1H 2.156(5) 10_556 ?
Zr1 O1H 2.156(5) . ?
Zr1 O2H 2.171(5) . ?
Zr1 O2H 2.171(5) 3_656 ?
Zr1 O1 2.176(3) 3_656 ?
Zr1 O1 2.176(3) 10_556 ?
Zr1 O1 2.176(3) 12_655 ?
Zr1 O1 2.176(3) . ?
Zr1 Zr2 3.4973(6) 9_666 ?
Zr1 Zr2 3.4973(6) 2_665 ?
Zr1 Zr2 3.4973(6) 10_556 ?
Zr1 Zr2 3.4974(6) . ?
Zr2 O1H 2.121(3) . ?
Zr2 O1H 2.121(3) 2_665 ?
Zr2 O2H 2.128(3) 11_565 ?
Zr2 O2H 2.128(3) . ?
Zr2 O3H 2.193(4) . ?
Zr2 O4H 2.203(6) . ?
Zr2 O2 2.256(3) . ?
Zr2 O2 2.256(3) 11_565 ?
Zr2 Zr1 3.4973(6) 9_666 ?
Zr2 Zr2 3.5315(14) 2_665 ?
Zr2 Zr2 3.5454(10) 10_556 ?
O1 C1 1.237(5) . ?
O2 C1 1.268(5) . ?
O1H Zr2 2.121(3) 2_665 ?
O1H H1H 1.0000 . ?
O2H Zr2 2.128(3) 10_556 ?
O2H H2H 1.0000 . ?
O3H H3H 0.8400 . ?
O4H H4H 0.8400 . ?
C1 C2 1.504(5) . ?
C2 C3 1.3900 . ?
C2 C7 1.3900 . ?
C3 C4 1.3900 . ?
C3 H3 0.9500 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 C9 1.488(4) . ?
C6 C7 1.3900 . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.388(5) 6_665 ?
C8 C9 1.388(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.414(5) . ?
C10 C11 1.369(5) . ?
C10 H10 0.9500 . ?
C11 C10 1.369(5) 6_665 ?
C11 N1 1.476(7) . ?
N1 C12A 1.385(15) 6_665 ?
N1 C12A 1.385(16) . ?
N1 C12B 1.410(17) 6_665 ?
N1 C12B 1.410(17) . ?
O3A C12A 1.221(9) . ?
C12A C13A 1.418(8) . ?
C13A C15A 1.358(9) . ?
C13A C14 1.388(8) . ?
O3B C12B 1.228(9) . ?
C12B C13B 1.416(9) . ?
C13B C15B 1.369(9) . ?
C13B C14 1.385(8) . ?
C14 C13B 1.385(8) 6_665 ?
C14 C13A 1.388(8) 6_665 ?
C14 C14 1.399(8) 10_557 ?
C15A C15A 1.404(9) 10_557 ?
C15A H15A 0.9500 . ?
C15B C15B 1.396(10) 10_557 ?
C15B H15B 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
O1H Zr1 O1H 107.9(3) 10_556 . ?
O1H Zr1 O2H 69.93(10) 10_556 . ?
O1H Zr1 O2H 69.93(10) . . ?
O1H Zr1 O2H 69.93(10) 10_556 3_656 ?
O1H Zr1 O2H 69.93(10) . 3_656 ?
O2H Zr1 O2H 108.7(3) . 3_656 ?
O1H Zr1 O1 79.20(13) 10_556 3_656 ?
O1H Zr1 O1 142.09(9) . 3_656 ?
O2H Zr1 O1 142.65(8) . 3_656 ?
O2H Zr1 O1 78.54(14) 3_656 3_656 ?
O1H Zr1 O1 79.20(13) 10_556 10_556 ?
O1H Zr1 O1 142.09(9) . 10_556 ?
O2H Zr1 O1 78.54(14) . 10_556 ?
O2H Zr1 O1 142.65(8) 3_656 10_556 ?
O1 Zr1 O1 75.41(17) 3_656 10_556 ?
O1H Zr1 O1 142.09(9) 10_556 12_655 ?
O1H Zr1 O1 79.20(13) . 12_655 ?
O2H Zr1 O1 142.65(8) . 12_655 ?
O2H Zr1 O1 78.54(14) 3_656 12_655 ?
O1 Zr1 O1 74.29(15) 3_656 12_655 ?
O1 Zr1 O1 118.51(15) 10_556 12_655 ?
O1H Zr1 O1 142.09(9) 10_556 . ?
O1H Zr1 O1 79.20(13) . . ?
O2H Zr1 O1 78.54(14) . . ?
O2H Zr1 O1 142.66(8) 3_656 . ?
O1 Zr1 O1 118.51(15) 3_656 . ?
O1 Zr1 O1 74.28(15) 10_556 . ?
O1 Zr1 O1 75.42(17) 12_655 . ?
O1H Zr1 Zr2 34.82(7) 10_556 9_666 ?
O1H Zr1 Zr2 89.93(12) . 9_666 ?
O2H Zr1 Zr2 90.15(13) . 9_666 ?
O2H Zr1 Zr2 35.16(7) 3_656 9_666 ?
O1 Zr1 Zr2 75.07(8) 3_656 9_666 ?
O1 Zr1 Zr2 111.10(7) 10_556 9_666 ?
O1 Zr1 Zr2 110.76(9) 12_655 9_666 ?
O1 Zr1 Zr2 166.42(8) . 9_666 ?
O1H Zr1 Zr2 89.93(12) 10_556 2_665 ?
O1H Zr1 Zr2 34.82(7) . 2_665 ?
O2H Zr1 Zr2 90.15(13) . 2_665 ?
O2H Zr1 Zr2 35.16(7) 3_656 2_665 ?
O1 Zr1 Zr2 110.76(9) 3_656 2_665 ?
O1 Zr1 Zr2 166.42(8) 10_556 2_665 ?
O1 Zr1 Zr2 75.07(8) 12_655 2_665 ?
O1 Zr1 Zr2 111.10(7) . 2_665 ?
Zr2 Zr1 Zr2 60.912(18) 9_666 2_665 ?
O1H Zr1 Zr2 34.82(7) 10_556 10_556 ?
O1H Zr1 Zr2 89.93(12) . 10_556 ?
O2H Zr1 Zr2 35.16(7) . 10_556 ?
O2H Zr1 Zr2 90.15(13) 3_656 10_556 ?
O1 Zr1 Zr2 111.10(7) 3_656 10_556 ?
O1 Zr1 Zr2 75.07(8) 10_556 10_556 ?
O1 Zr1 Zr2 166.42(8) 12_655 10_556 ?
O1 Zr1 Zr2 110.76(9) . 10_556 ?
Zr2 Zr1 Zr2 60.65(2) 9_666 10_556 ?
Zr2 Zr1 Zr2 91.35(2) 2_665 10_556 ?
O1H Zr1 Zr2 89.93(12) 10_556 . ?
O1H Zr1 Zr2 34.82(7) . . ?
O2H Zr1 Zr2 35.15(7) . . ?
O2H Zr1 Zr2 90.15(13) 3_656 . ?
O1 Zr1 Zr2 166.42(8) 3_656 . ?
O1 Zr1 Zr2 110.76(9) 10_556 . ?
O1 Zr1 Zr2 111.10(7) 12_655 . ?
O1 Zr1 Zr2 75.07(8) . . ?
Zr2 Zr1 Zr2 91.36(2) 9_666 . ?
Zr2 Zr1 Zr2 60.65(2) 2_665 . ?
Zr2 Zr1 Zr2 60.912(18) 10_556 . ?
O1H Zr2 O1H 67.3(2) . 2_665 ?
O1H Zr2 O2H 107.1(2) . 11_565 ?
O1H Zr2 O2H 71.40(19) 2_665 11_565 ?
O1H Zr2 O2H 71.40(19) . . ?
O1H Zr2 O2H 107.1(2) 2_665 . ?
O2H Zr2 O2H 67.2(2) 11_565 . ?
O1H Zr2 O3H 87.4(2) . . ?
O1H Zr2 O3H 87.4(2) 2_665 . ?
O2H Zr2 O3H 146.18(11) 11_565 . ?
O2H Zr2 O3H 146.18(11) . . ?
O1H Zr2 O4H 146.17(10) . . ?
O1H Zr2 O4H 146.16(10) 2_665 . ?
O2H Zr2 O4H 87.6(2) 11_565 . ?
O2H Zr2 O4H 87.6(2) . . ?
O3H Zr2 O4H 97.0(2) . . ?
O1H Zr2 O2 76.19(15) . . ?
O1H Zr2 O2 139.00(15) 2_665 . ?
O2H Zr2 O2 139.82(15) 11_565 . ?
O2H Zr2 O2 76.80(14) . . ?
O3H Zr2 O2 72.62(10) . . ?
O4H Zr2 O2 73.27(12) . . ?
O1H Zr2 O2 139.00(15) . 11_565 ?
O1H Zr2 O2 76.18(15) 2_665 11_565 ?
O2H Zr2 O2 76.80(14) 11_565 11_565 ?
O2H Zr2 O2 139.82(14) . 11_565 ?
O3H Zr2 O2 72.62(10) . 11_565 ?
O4H Zr2 O2 73.27(12) . 11_565 ?
O2 Zr2 O2 127.46(17) . 11_565 ?
O1H Zr2 Zr1 87.69(13) . 9_666 ?
O1H Zr2 Zr1 35.47(12) 2_665 9_666 ?
O2H Zr2 Zr1 35.97(14) 11_565 9_666 ?
O2H Zr2 Zr1 87.93(13) . 9_666 ?
O3H Zr2 Zr1 118.01(10) . 9_666 ?
O4H Zr2 Zr1 118.59(10) . 9_666 ?
O2 Zr2 Zr1 160.58(9) . 9_666 ?
O2 Zr2 Zr1 71.94(8) 11_565 9_666 ?
O1H Zr2 Zr1 35.48(12) . . ?
O1H Zr2 Zr1 87.69(13) 2_665 . ?
O2H Zr2 Zr1 87.93(13) 11_565 . ?
O2H Zr2 Zr1 35.97(14) . . ?
O3H Zr2 Zr1 118.01(10) . . ?
O4H Zr2 Zr1 118.59(10) . . ?
O2 Zr2 Zr1 71.94(8) . . ?
O2 Zr2 Zr1 160.58(9) 11_565 . ?
Zr1 Zr2 Zr1 88.64(2) 9_666 . ?
O1H Zr2 Zr2 33.65(11) . 2_665 ?
O1H Zr2 Zr2 33.65(11) 2_665 2_665 ?
O2H Zr2 Zr2 89.94(16) 11_565 2_665 ?
O2H Zr2 Zr2 89.94(16) . 2_665 ?
O3H Zr2 Zr2 85.91(16) . 2_665 ?
O4H Zr2 Zr2 177.09(16) . 2_665 ?
O2 Zr2 Zr2 107.73(10) . 2_665 ?
O2 Zr2 Zr2 107.73(10) 11_565 2_665 ?
Zr1 Zr2 Zr2 59.676(11) 9_666 2_665 ?
Zr1 Zr2 Zr2 59.676(11) . 2_665 ?
O1H Zr2 Zr2 89.20(14) . 10_556 ?
O1H Zr2 Zr2 89.20(14) 2_665 10_556 ?
O2H Zr2 Zr2 33.59(11) 11_565 10_556 ?
O2H Zr2 Zr2 33.59(11) . 10_556 ?
O3H Zr2 Zr2 175.91(16) . 10_556 ?
O4H Zr2 Zr2 87.09(16) . 10_556 ?
O2 Zr2 Zr2 108.74(8) . 10_556 ?
O2 Zr2 Zr2 108.74(8) 11_565 10_556 ?
Zr1 Zr2 Zr2 59.543(9) 9_666 10_556 ?
Zr1 Zr2 Zr2 59.544(9) . 10_556 ?
Zr2 Zr2 Zr2 90.0 2_665 10_556 ?
C1 O1 Zr1 133.0(3) . . ?
C1 O2 Zr2 133.3(3) . . ?
Zr2 O1H Zr2 112.7(2) 2_665 . ?
Zr2 O1H Zr1 109.70(16) 2_665 . ?
Zr2 O1H Zr1 109.70(16) . . ?
Zr2 O1H H1H 108.2 2_665 . ?
Zr2 O1H H1H 108.2 . . ?
Zr1 O1H H1H 108.2 . . ?
Zr2 O2H Zr2 112.8(2) 10_556 . ?
Zr2 O2H Zr1 108.87(18) 10_556 . ?
Zr2 O2H Zr1 108.87(18) . . ?
Zr2 O2H H2H 108.7 10_556 . ?
Zr2 O2H H2H 108.7 . . ?
Zr1 O2H H2H 108.7 . . ?
Zr2 O3H H3H 109.5 . . ?
Zr2 O4H H4H 109.5 . . ?
O1 C1 O2 126.6(4) . . ?
O1 C1 C2 117.1(4) . . ?
O2 C1 C2 116.3(4) . . ?
C3 C2 C7 120.0 . . ?
C3 C2 C1 118.5(3) . . ?
C7 C2 C1 121.5(3) . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 C9 119.5(3) . . ?
C6 C5 C9 120.5(3) . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C2 120.0 . . ?
C6 C7 H7 120.0 . . ?
C2 C7 H7 120.0 . . ?
C9 C8 C9 121.5(5) 6_665 . ?
C9 C8 H8 119.2 6_665 . ?
C9 C8 H8 119.2 . . ?
C8 C9 C10 118.8(4) . . ?
C8 C9 C5 120.0(3) . . ?
C10 C9 C5 121.2(4) . . ?
C11 C10 C9 119.1(4) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C10 122.6(6) 6_665 . ?
C10 C11 N1 118.7(3) 6_665 . ?
C10 C11 N1 118.7(3) . . ?
C12A N1 C12A 123.3(10) 6_665 . ?
C12B N1 C12B 125.8(11) 6_665 . ?
C12A N1 C11 118.4(5) 6_665 . ?
C12A N1 C11 118.4(5) . . ?
C12B N1 C11 117.1(6) 6_665 . ?
C12B N1 C11 117.1(6) . . ?
O3A C12A N1 118.1(11) . . ?
O3A C12A C13A 124.4(13) . . ?
N1 C12A C13A 117.5(11) . . ?
C15A C13A C14 118.7(10) . . ?
C15A C13A C12A 120.1(9) . . ?
C14 C13A C12A 121.1(10) . . ?
O3B C12B N1 120.3(12) . . ?
O3B C12B C13B 125.6(15) . . ?
N1 C12B C13B 114.1(12) . . ?
C15B C13B C14 116.7(12) . . ?
C15B C13B C12B 118.9(10) . . ?
C14 C13B C12B 124.4(12) . . ?
C13B C14 C13B 117.2(12) . 6_665 ?
C13A C14 C13A 119.3(11) . 6_665 ?
C13B C14 C14 121.4(6) . 10_557 ?
C13B C14 C14 121.4(6) 6_665 10_557 ?
C13A C14 C14 120.3(5) . 10_557 ?
C13A C14 C14 120.3(5) 6_665 10_557 ?
C13A C15A C15A 121.0(6) . 10_557 ?
C13A C15A H15A 119.5 . . ?
C15A C15A H15A 119.5 10_557 . ?
C13B C15B C15B 121.9(6) . 10_557 ?
C13B C15B H15B 119.1 . . ?
C15B C15B H15B 119.1 10_557 . ?

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 O1 C1 O2 3.2(9) . . . . ?
Zr1 O1 C1 C2 -175.8(3) . . . . ?
Zr2 O2 C1 O1 -0.9(9) . . . . ?
Zr2 O2 C1 C2 178.0(3) . . . . ?
O1 C1 C2 C3 -11.5(6) . . . . ?
O2 C1 C2 C3 169.4(4) . . . . ?
O1 C1 C2 C7 168.0(4) . . . . ?
O2 C1 C2 C7 -11.0(6) . . . . ?
C7 C2 C3 C4 0.0 . . . . ?
C1 C2 C3 C4 179.5(4) . . . . ?
C2 C3 C4 C5 0.0 . . . . ?
C3 C4 C5 C6 0.0 . . . . ?
C3 C4 C5 C9 -178.4(4) . . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C9 C5 C6 C7 178.4(4) . . . . ?
C5 C6 C7 C2 0.0 . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C1 C2 C7 C6 -179.5(4) . . . . ?
C9 C8 C9 C10 -1.6(4) 6_665 . . . ?
C9 C8 C9 C5 178.6(6) 6_665 . . . ?
C4 C5 C9 C8 -38.4(6) . . . . ?
C6 C5 C9 C8 143.2(4) . . . . ?
C4 C5 C9 C10 141.9(5) . . . . ?
C6 C5 C9 C10 -36.6(7) . . . . ?
C8 C9 C10 C11 3.3(9) . . . . ?
C5 C9 C10 C11 -176.9(4) . . . . ?
C9 C10 C11 C10 -1.7(4) . . . 6_665 ?
C9 C10 C11 N1 178.3(4) . . . . ?
C10 C11 N1 C12A 76.1(4) 6_665 . . 6_665 ?
C10 C11 N1 C12A -103.9(4) . . . 6_665 ?
C10 C11 N1 C12A -103.9(4) 6_665 . . . ?
C10 C11 N1 C12A 76.1(4) . . . . ?
C10 C11 N1 C12B 99.7(5) 6_665 . . 6_665 ?
C10 C11 N1 C12B -80.3(5) . . . 6_665 ?
C10 C11 N1 C12B -80.3(5) 6_665 . . . ?
C10 C11 N1 C12B 99.7(5) . . . . ?
C12A N1 C12A O3A -179.6(3) 6_665 . . . ?
C11 N1 C12A O3A 0.4(3) . . . . ?
C12A N1 C12A C13A 0.14(13) 6_665 . . . ?
C11 N1 C12A C13A -179.86(13) . . . . ?
O3A C12A C13A C15A -0.2(4) . . . . ?
N1 C12A C13A C15A -179.9(3) . . . . ?
O3A C12A C13A C14 179.4(4) . . . . ?
N1 C12A C13A C14 -0.3(3) . . . . ?
C12B N1 C12B O3B -180.0(3) 6_665 . . . ?
C11 N1 C12B O3B 0.0(3) . . . . ?
C12B N1 C12B C13B 0.02(13) 6_665 . . . ?
C11 N1 C12B C13B -179.98(13) . . . . ?
O3B C12B C13B C15B 0.4(4) . . . . ?
N1 C12B C13B C15B -179.6(3) . . . . ?
O3B C12B C13B C14 180.0(4) . . . . ?
N1 C12B C13B C14 0.0(3) . . . . ?
C15B C13B C14 C13B 179.6(3) . . . 6_665 ?
C12B C13B C14 C13B 0.02(15) . . . 6_665 ?
C15B C13B C14 C14 -0.4(3) . . . 10_557 ?
C12B C13B C14 C14 -179.97(15) . . . 10_557 ?
C15A C13A C14 C13A 179.8(3) . . . 6_665 ?
C12A C13A C14 C13A 0.15(14) . . . 6_665 ?
C15A C13A C14 C14 -0.2(3) . . . 10_557 ?
C12A C13A C14 C14 -179.85(14) . . . 10_557 ?
C14 C13A C15A C15A 0.2(3) . . . 10_557 ?
C12A C13A C15A C15A 179.85(14) . . . 10_557 ?
C14 C13B C15B C15B 0.4(3) . . . 10_557 ?
C12B C13B C15B C15B 180.00(13) . . . 10_557 ?

_refine_diff_density_max         0.494
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.058

# SQUEEZE RESULTS (Version =  41016)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.046 -0.004 -0.006 13337 5406 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?




# start Validation Reply Form
_vrf_THETM01_shelx               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: This alert is caused by poor diffraction.
;
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Without Acceptor       O1H    --  H1H    ...     Please Check 
RESPONSE: It was not possible to localize an acceptor for it in the channel.
;
_vrf_PLAT241_shelx               
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of        O1H Check 
RESPONSE: This atom is bound to Zr - the heaviest element in the structure.
;
_vrf_PLAT242_shelx               
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Zr1 Check 
RESPONSE: Zr is the heaviest element in the structure. N1 and C14 are
 the 'pivot' atoms of the disordered
 benzo[lmn][3,8]phenanthroline-1,3,6,8(2H,7H)-tetrone moiety.
;
_vrf_PLAT250_shelx               
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        2.5 Note  
RESPONSE: There are significant thermal motion of the flexible organic
 ligand towards channels in the structure.
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).          7 Note  
RESPONSE: These reflexes were omitted due to bad statistics.
;
_vrf_PLAT911_shelx               
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.500         24 Report
RESPONSE: These reflexes were omitted due to bad statistics.
;
_vrf_PLAT913_shelx               
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....          4 Note  
RESPONSE: These reflexes were omitted due to bad statistics.
;
_vrf_PLAT934_shelx               
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....          1 Check 
RESPONSE: It was not possible to localize this reflex since PLATON
 used weighed values when SHELXL not.
;
_vrf_PLAT977_shelx               
;
PROBLEM: Check the Negative Difference Density on     H2H      -0.38 eA-3  
RESPONSE: It is an artifact due to poor diffraction. Zr-O distances
 corresponds to m3-OH and the H-atom was placed using geometrical
 considerations.
;
# end Validation Reply Form




