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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_493-MOF-BA
_database_code_depnum_ccdc_archive 'CCDC 1501750'
_audit_update_record             
;
2017-02-24 deposited with the CCDC.
2017-03-03 downloaded from the CCDC.
;

_audit_creation_date             2017-02-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.13(C808 H1282 N169 O400 Zr48)'
_chemical_formula_sum            'C105 H168 N22 O52 Zr6'
_chemical_formula_weight         3117.9185
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'O H N C Zr'
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'

_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      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   38.8511(3)
_cell_length_b                   38.8511(3)
_cell_length_c                   18.7521(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     28304.6(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    5332
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.8310
_cell_measurement_theta_min      3.5900
_shelx_estimated_absorpt_T_max   0.509
_shelx_estimated_absorpt_T_min   0.454
_exptl_absorpt_coefficient_mu    4.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68790
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             7456
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         3.217
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2542
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -77.00  -50.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -64.00  -37.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000    0.0000 27

#__ type_ start__ end____ width___ exp.time_
  3 omega  -77.00  -51.00   1.0000   50.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
  4 omega  -14.00   38.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0974  -57.0000    0.0000 52

#__ type_ start__ end____ width___ exp.time_
  5 omega   38.00   66.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0974   57.0000 -180.0000 28

#__ type_ start__ end____ width___ exp.time_
  6 omega   42.00  116.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0974   57.0000 -150.0000 74

#__ type_ start__ end____ width___ exp.time_
  7 omega   37.00   89.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1947  -25.0000  150.0000 52

#__ type_ start__ end____ width___ exp.time_
  8 omega   62.00   93.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1947  -25.0000    0.0000 31

#__ type_ start__ end____ width___ exp.time_
  9 omega   62.00   93.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1947  -50.0000   90.0000 31

#__ type_ start__ end____ width___ exp.time_
 10 omega   40.00   79.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1947  -37.0000  -90.0000 39

#__ type_ start__ end____ width___ exp.time_
 11 omega   94.00  158.00   1.0000  200.0000
omega____ theta____ kappa____ phi______ frames
    -      110.1947   50.0000 -180.0000 64
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0061227000
_diffrn_orient_matrix_UB_12      0.0249212000
_diffrn_orient_matrix_UB_13      -0.0626277000
_diffrn_orient_matrix_UB_21      0.0390435000
_diffrn_orient_matrix_UB_22      -0.0013120000
_diffrn_orient_matrix_UB_23      0.0141169000
_diffrn_orient_matrix_UB_31      0.0032710000
_diffrn_orient_matrix_UB_32      -0.0307847000
_diffrn_orient_matrix_UB_33      -0.0513377000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.878
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6580
_reflns_number_total             11323
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    ?
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 
;
 Flack x determined using 1964 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         11323
_refine_ls_number_restraints     155
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0494
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0641P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1422
_refine_special_details          
;
The remaining solvent molecules were disordered and assigned as 8 DMF and 2 water molecules per unit cell according to the TGA and elemental analysis results. The contributions of these disordered solvent to the scattering values have been removed by using the PLATON SQUEEZE program. The total  unit  cell include 8 DMF and 2 water molecules (40e*8+10e*2=340e), SQUEEZE result reveals that 4590 electrons were removed from the unit cell. This discrepancy might be owing to the low quality of low angle data caused by the small size of the Zr-MOF crystal and highly disordered nature of the lattice solvents.

 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.51(2) 0.49(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
3. Restrained distances
 C25-C26
 1.45 with sigma of 0.002
 O11-C25
 1.43 with sigma of 0.002
 C28-C31
 2.789 with sigma of 0.0001
 C31-C28
 2.789 with sigma of 0.0001
 C29-C28 = C30-C29 = C31-C30
 1.39 with sigma of 0.0001
 C28-C27 = C2-C1 = C23-C12
 1.5 with sigma of 0.01
 C31-C29 = C30-C28
 2.415 with sigma of 0.0001
4. Restrained planarity
 C28, C29, C30, C31
 with sigma of 0.001
5. Rigid bond restraints
 C26, C27, C28, C29, C30, C31
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O11, C25, C26
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Uiso/Uaniso restraints and constraints
C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31: within 1.7A with sigma
of 0.002 and sigma for terminal atoms of 0.004
O11 \\sim C25 \\sim C26: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C25) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31) \\sim Ueq: with sigma of 0.002 and
sigma for terminal atoms of 0.004
Uanis(O11) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
7. Others
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5)
8.a Riding coordinates:
 C29(H29), C30(H30), C31(H31), O17(H17A,H17B)
8.b Me refined with riding coordinates:
 C26(H26A,H26B,H26C)
8.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C17(H17), C18(H18), C20(H20), C21(H21)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr -0.00994(3) 0.81077(2) 0.08577(6) 0.0822(3) Uani 1 1 d . . . . .
Zr2 Zr -0.05510(2) 0.73612(2) 0.03495(7) 0.0778(4) Uani 1 1 d . . . . .
Zr3 Zr 0.03524(2) 0.73631(2) 0.03584(7) 0.0856(4) Uani 1 1 d . . . . .
C1 C 0.0471(3) 0.8436(3) 0.1902(9) 0.094(4) Uani 1 1 d D U . . .
C2 C 0.0634(4) 0.8761(3) 0.2214(9) 0.118(5) Uani 1 1 d D U . . .
C3 C 0.0854(4) 0.8756(3) 0.2787(10) 0.131(5) Uani 1 1 d . U . . .
H3 H 0.091258 0.854647 0.299416 0.157 Uiso 1 1 calc R . . . .
C4 C 0.0988(5) 0.9050(3) 0.3057(11) 0.171(10) Uani 1 1 d . . . . .
H4 H 0.111852 0.903984 0.347213 0.205 Uiso 1 1 calc R . . . .
C5 C 0.0936(4) 0.9356(3) 0.2738(9) 0.124(6) Uani 1 1 d . . . . .
C6 C 0.0727(4) 0.9374(4) 0.2115(10) 0.134(5) Uani 1 1 d . U . . .
H6 H 0.069858 0.958041 0.186985 0.161 Uiso 1 1 calc R . . . .
C7 C 0.0564(4) 0.9071(3) 0.1884(9) 0.130(5) Uani 1 1 d . U . . .
H7 H 0.040916 0.907929 0.150678 0.156 Uiso 1 1 calc R . . . .
C8 C 0.0647(3) 1.1538(3) 0.1912(8) 0.072(4) Uani 1 1 d . . . . .
C9 C 0.0775(3) 1.1222(3) 0.2171(9) 0.100(5) Uani 1 1 d . . . . .
C10 C 0.0686(4) 1.0909(4) 0.1881(9) 0.129(5) Uani 1 1 d . U . . .
H10 H 0.055521 1.090277 0.146590 0.155 Uiso 1 1 calc R . . . .
C11 C 0.0789(4) 1.0602(3) 0.2203(10) 0.128(6) Uani 1 1 d . . . . .
H11 H 0.068505 1.039681 0.206184 0.153 Uiso 1 1 calc R . . . .
C12 C 0.1019(4) 1.0593(3) 0.2683(9) 0.117(6) Uani 1 1 d D . . . .
C13 C 0.1123(4) 1.0900(3) 0.2980(10) 0.145(8) Uani 1 1 d . . . . .
H13 H 0.127938 1.089767 0.335441 0.174 Uiso 1 1 calc R . . . .
C14 C 0.1003(4) 1.1202(3) 0.2741(10) 0.120(6) Uani 1 1 d . . . . .
H14 H 0.107467 1.140392 0.296181 0.144 Uiso 1 1 calc R . . . .
C15 C 0.2119(3) 0.9903(3) 0.6524(8) 0.082(3) Uani 1 1 d . . . . .
C16 C 0.1955(3) 0.9915(3) 0.5806(8) 0.095(4) Uani 1 1 d . . . . .
C17 C 0.1851(4) 0.9604(3) 0.5457(10) 0.119(5) Uani 1 1 d . . . . .
H17 H 0.190078 0.939141 0.566219 0.143 Uiso 1 1 calc R . . . .
C18 C 0.1685(5) 0.9619(3) 0.4845(9) 0.138(7) Uani 1 1 d . . . . .
H18 H 0.161894 0.941460 0.462828 0.166 Uiso 1 1 calc R . . . .
C19 C 0.1603(4) 0.9938(3) 0.4499(9) 0.124(6) Uani 1 1 d . . . . .
C20 C 0.1697(5) 1.0231(3) 0.4771(13) 0.163(9) Uani 1 1 d . . . . .
H20 H 0.165785 1.043795 0.453716 0.196 Uiso 1 1 calc R . . . .
C21 C 0.1871(5) 1.0217(3) 0.5473(10) 0.140(7) Uani 1 1 d . . . . .
H21 H 0.192682 1.042309 0.569712 0.168 Uiso 1 1 calc R . . . .
C22 C 0.1394(5) 0.9947(3) 0.3835(9) 0.126(6) Uani 1 1 d . . . . .
C23 C 0.1117(4) 1.0259(3) 0.3067(10) 0.122(5) Uani 1 1 d D U . . .
C24 C 0.1080(4) 0.9672(3) 0.2972(10) 0.119(6) Uani 1 1 d . . . . .
C25 C 0.1064(4) 0.750000 0.125000 0.137(4) Uani 1 2 d DS TU P . .
C26 C 0.1437(4) 0.750000 0.125000 0.146(5) Uani 1 2 d DS TU P . .
H26A H 0.151951 0.757815 0.170469 0.219 Uiso 0.5 1 calc R . . A -1
H26B H 0.151951 0.727086 0.116288 0.219 Uiso 0.5 1 calc R . . A -1
H26C H 0.151951 0.765099 0.088243 0.219 Uiso 0.5 1 calc R . . A -1
C27 C -0.1191(3) 0.750000 0.125000 0.208(5) Uani 1 2 d DS TU P . .
C28 C -0.15790(4) 0.750000 0.125000 0.208(5) Uani 1 2 d DS TU P . .
C29 C -0.17588(4) 0.74210(17) 0.06295(9) 0.207(5) Uani 1 1 d D U . . .
H29 H -0.163943 0.737343 0.021132 0.248 Uiso 1 1 d R . . . .
C30 C -0.21173(4) 0.74210(17) 0.06295(9) 0.207(5) Uani 1 1 d D U . . .
H30 H -0.223680 0.737363 0.021132 0.249 Uiso 1 1 d R . . . .
C31 C -0.22971(4) 0.750000 0.125000 0.207(5) Uani 1 2 d DS TU P . .
H31 H -0.253639 0.750000 0.125000 0.248 Uiso 1 2 d RS T P . .
N1 N 0.1272(4) 0.9645(2) 0.3595(8) 0.136(6) Uani 1 1 d . . . . .
N2 N 0.0989(3) 0.9968(2) 0.2726(7) 0.135(5) Uani 1 1 d . . . . .
N3 N 0.1318(3) 1.0261(2) 0.3600(7) 0.109(4) Uani 1 1 d . . . . .
O1 O 0.0261(2) 0.84750(19) 0.1398(6) 0.112(3) Uani 1 1 d . . . . .
O2 O 0.0548(2) 0.81698(17) 0.2246(6) 0.104(3) Uani 1 1 d . . . . .
O3 O 0.04461(18) 1.15271(16) 0.1391(5) 0.081(3) Uani 1 1 d . . . . .
O4 O 0.07355(18) 1.18210(17) 0.2232(5) 0.085(2) Uani 1 1 d . . . . .
O5 O 0.2191(2) 1.01902(18) 0.6772(6) 0.098(3) Uani 1 1 d . . . . .
O6 O 0.2187(2) 0.96137(19) 0.6791(5) 0.093(3) Uani 1 1 d . . . . .
O7 O -0.00962(19) 0.76754(19) 0.0159(6) 0.121(3) Uani 1 1 d . U . . .
O8 O -0.00961(18) 0.7073(2) 0.0550(5) 0.112(3) Uani 1 1 d . . . . .
O9 O 0.0354(3) 0.7813(2) 0.1011(6) 0.127(4) Uani 1 1 d . . . . .
O10 O -0.0547(2) 0.77968(18) 0.1040(5) 0.098(3) Uani 1 1 d . . . . .
O11 O 0.0900(2) 0.7390(3) 0.0607(4) 0.131(3) Uani 1 1 d D U . . .
O12 O -0.11104(18) 0.7380(2) 0.0536(6) 0.120(3) Uani 1 1 d . . . . .
O13 O 0.0236(3) 0.8335(3) -0.0022(6) 0.148(5) Uani 1 1 d . . . . .
O14 O -0.0429(3) 0.8320(2) -0.0020(6) 0.137(4) Uani 1 1 d . . . . .
O15 O -0.0771(2) 0.7733(3) -0.0401(7) 0.157(5) Uani 1 1 d . . . . .
O16 O 0.0591(2) 0.7719(3) -0.0440(6) 0.139(4) Uani 1 1 d . . . . .
O17 O 0.1399(4) 0.9911(5) 0.7096(12) 0.350(13) Uani 1 1 d . . . . .
H17A H 0.150661 0.972691 0.707318 0.525 Uiso 1 1 d R . . . .
H17B H 0.154091 1.006351 0.709538 0.525 Uiso 1 1 d R . . . .


_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 3.5212(13) . ?
Zr1 Zr2 3.5033(16) 14_464 ?
Zr1 Zr3 3.4963(16) 14_464 ?
Zr1 Zr3 3.5111(13) . ?
Zr1 O1 2.242(8) . ?
Zr1 O3 2.197(7) 2_575 ?
Zr1 O7 2.131(8) . ?
Zr1 O8 2.166(8) 14_464 ?
Zr1 O9 2.122(10) . ?
Zr1 O10 2.144(8) . ?
Zr1 O13 2.281(11) . ?
Zr1 O14 2.242(10) . ?
Zr2 Zr2 3.545(2) 14_464 ?
Zr2 Zr3 3.5096(12) . ?
Zr2 O4 2.223(7) 13_444 ?
Zr2 O6 2.193(9) 16_353 ?
Zr2 O7 2.177(8) . ?
Zr2 O8 2.125(8) . ?
Zr2 O10 2.132(7) . ?
Zr2 O10 2.170(9) 14_464 ?
Zr2 O12 2.203(7) . ?
Zr2 O15 2.190(10) . ?
Zr3 Zr3 3.509(3) 14_464 ?
Zr3 O2 2.214(7) 14_464 ?
Zr3 O5 2.234(10) 16_353 ?
Zr3 O7 2.156(8) . ?
Zr3 O8 2.105(7) . ?
Zr3 O9 2.134(9) . ?
Zr3 O9 2.227(12) 14_464 ?
Zr3 O11 2.180(9) . ?
Zr3 O16 2.238(10) . ?
C1 C2 1.530(10) . ?
C1 O1 1.257(15) . ?
C1 O2 1.254(15) . ?
C2 C3 1.375(19) . ?
C2 C7 1.381(19) . ?
C3 C4 1.350(18) . ?
C4 C5 1.347(18) . ?
C5 C6 1.425(19) . ?
C5 C24 1.419(15) . ?
C6 C7 1.405(17) . ?
C8 C9 1.412(15) . ?
C8 O3 1.252(13) . ?
C8 O4 1.299(13) . ?
C9 C10 1.373(17) . ?
C9 C14 1.390(18) . ?
C10 C11 1.398(18) . ?
C11 C12 1.268(17) . ?
C12 C13 1.378(17) . ?
C12 C23 1.534(11) . ?
C13 C14 1.338(17) . ?
C15 C16 1.491(17) . ?
C15 O5 1.240(13) . ?
C15 O6 1.258(13) . ?
C16 C17 1.432(17) . ?
C16 C21 1.368(17) . ?
C17 C18 1.317(18) . ?
C18 C19 1.435(18) . ?
C19 C20 1.299(18) . ?
C19 C22 1.486(18) . ?
C20 C21 1.48(2) . ?
C22 N1 1.343(15) . ?
C22 N3 1.331(14) . ?
C23 N2 1.390(15) . ?
C23 N3 1.267(16) . ?
C24 N1 1.392(17) . ?
C24 N2 1.287(14) . ?
C25 C26 1.451(3) . ?
C25 O11 1.429(3) . ?
C25 O11 1.429(3) 14_464 ?
C27 C28 1.507(13) . ?
C27 C28 1.507(13) 14_464 ?
C27 O12 1.452(11) . ?
C27 O12 1.452(11) 14_464 ?
C28 C28 0.000(3) 14_464 ?
C28 C29 1.39134(14) . ?
C28 C29 1.39134(14) 14_464 ?
C29 C30 1.39269(12) . ?
C30 C31 1.39134(14) . ?

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 Zr2 60.62(4) 14_464 . ?
Zr2 Zr1 Zr3 90.37(3) 14_464 . ?
Zr3 Zr1 Zr2 90.31(3) 14_464 . ?
Zr3 Zr1 Zr2 59.88(2) . . ?
Zr3 Zr1 Zr2 60.19(3) 14_464 14_464 ?
Zr3 Zr1 Zr3 60.10(4) 14_464 . ?
O1 Zr1 Zr2 163.3(2) . . ?
O1 Zr1 Zr2 109.4(3) . 14_464 ?
O1 Zr1 Zr3 73.0(2) . 14_464 ?
O1 Zr1 Zr3 109.4(2) . . ?
O1 Zr1 O13 73.9(4) . . ?
O1 Zr1 O14 117.0(4) . . ?
O3 Zr1 Zr2 110.47(18) 2_575 . ?
O3 Zr1 Zr2 73.4(2) 2_575 14_464 ?
O3 Zr1 Zr3 109.4(2) 2_575 14_464 ?
O3 Zr1 Zr3 163.7(2) 2_575 . ?
O3 Zr1 O1 76.5(3) 2_575 . ?
O3 Zr1 O13 115.5(4) 2_575 . ?
O3 Zr1 O14 75.3(3) 2_575 . ?
O7 Zr1 Zr2 35.6(2) . . ?
O7 Zr1 Zr2 91.1(3) . 14_464 ?
O7 Zr1 Zr3 90.5(3) . 14_464 ?
O7 Zr1 Zr3 35.3(2) . . ?
O7 Zr1 O1 140.9(3) . . ?
O7 Zr1 O3 142.4(3) . 2_575 ?
O7 Zr1 O8 109.0(4) . 14_464 ?
O7 Zr1 O10 70.1(3) . . ?
O7 Zr1 O13 81.8(4) . . ?
O7 Zr1 O14 80.9(4) . . ?
O8 Zr1 Zr2 89.5(3) 14_464 . ?
O8 Zr1 Zr2 34.9(2) 14_464 14_464 ?
O8 Zr1 Zr3 34.5(2) 14_464 14_464 ?
O8 Zr1 Zr3 88.9(2) 14_464 . ?
O8 Zr1 O1 77.0(4) 14_464 . ?
O8 Zr1 O3 77.4(3) 14_464 2_575 ?
O8 Zr1 O13 143.7(3) 14_464 . ?
O8 Zr1 O14 144.8(4) 14_464 . ?
O9 Zr1 Zr2 90.4(3) . . ?
O9 Zr1 Zr2 92.4(3) . 14_464 ?
O9 Zr1 Zr3 37.5(3) . 14_464 ?
O9 Zr1 Zr3 34.5(3) . . ?
O9 Zr1 O1 76.3(3) . . ?
O9 Zr1 O3 142.7(4) . 2_575 ?
O9 Zr1 O7 69.7(4) . . ?
O9 Zr1 O8 72.0(4) . 14_464 ?
O9 Zr1 O10 110.3(3) . . ?
O9 Zr1 O13 80.3(4) . . ?
O9 Zr1 O14 140.6(4) . . ?
O10 Zr1 Zr2 36.0(2) . 14_464 ?
O10 Zr1 Zr2 34.4(2) . . ?
O10 Zr1 Zr3 89.1(2) . . ?
O10 Zr1 Zr3 90.1(3) . 14_464 ?
O10 Zr1 O1 142.5(4) . . ?
O10 Zr1 O3 78.1(3) . 2_575 ?
O10 Zr1 O8 70.8(3) . 14_464 ?
O10 Zr1 O13 142.9(4) . . ?
O10 Zr1 O14 82.1(4) . . ?
O13 Zr1 Zr2 114.1(3) . . ?
O13 Zr1 Zr2 171.2(3) . 14_464 ?
O13 Zr1 Zr3 80.8(3) . . ?
O13 Zr1 Zr3 114.4(3) . 14_464 ?
O14 Zr1 Zr2 79.7(3) . . ?
O14 Zr1 Zr2 114.4(3) . 14_464 ?
O14 Zr1 Zr3 170.0(3) . 14_464 ?
O14 Zr1 Zr3 113.2(3) . . ?
O14 Zr1 O13 69.7(4) . . ?
Zr1 Zr2 Zr1 89.52(4) 14_464 . ?
Zr1 Zr2 Zr2 59.94(3) 14_464 14_464 ?
Zr1 Zr2 Zr2 59.44(3) . 14_464 ?
Zr1 Zr2 Zr3 59.81(3) 14_464 . ?
Zr3 Zr2 Zr1 59.92(3) . . ?
Zr3 Zr2 Zr2 89.70(3) . 14_464 ?
O4 Zr2 Zr1 73.6(2) 13_444 14_464 ?
O4 Zr2 Zr1 163.1(2) 13_444 . ?
O4 Zr2 Zr2 110.6(2) 13_444 14_464 ?
O4 Zr2 Zr3 108.95(19) 13_444 . ?
O6 Zr2 Zr1 110.7(2) 16_353 . ?
O6 Zr2 Zr1 108.7(2) 16_353 14_464 ?
O6 Zr2 Zr2 163.00(19) 16_353 14_464 ?
O6 Zr2 Zr3 73.3(2) 16_353 . ?
O6 Zr2 O4 75.0(3) 16_353 13_444 ?
O6 Zr2 O12 116.2(3) 16_353 . ?
O7 Zr2 Zr1 34.7(2) . . ?
O7 Zr2 Zr1 89.9(3) . 14_464 ?
O7 Zr2 Zr2 89.2(3) . 14_464 ?
O7 Zr2 Zr3 35.7(2) . . ?
O7 Zr2 O4 141.2(3) . 13_444 ?
O7 Zr2 O6 77.7(3) . 16_353 ?
O7 Zr2 O12 143.9(3) . . ?
O7 Zr2 O15 80.9(4) . . ?
O8 Zr2 Zr1 88.4(2) . . ?
O8 Zr2 Zr1 35.6(2) . 14_464 ?
O8 Zr2 Zr2 89.5(2) . 14_464 ?
O8 Zr2 Zr3 33.8(2) . . ?
O8 Zr2 O4 77.5(3) . 13_444 ?
O8 Zr2 O6 75.8(3) . 16_353 ?
O8 Zr2 O7 69.5(3) . . ?
O8 Zr2 O10 107.7(4) . . ?
O8 Zr2 O10 71.0(3) . 14_464 ?
O8 Zr2 O12 144.1(3) . . ?
O8 Zr2 O15 141.8(3) . . ?
O10 Zr2 Zr1 34.7(2) . . ?
O10 Zr2 Zr1 88.3(2) 14_464 . ?
O10 Zr2 Zr1 89.3(3) . 14_464 ?
O10 Zr2 Zr1 35.4(2) 14_464 14_464 ?
O10 Zr2 Zr2 34.15(18) 14_464 14_464 ?
O10 Zr2 Zr2 34.9(2) . 14_464 ?
O10 Zr2 Zr3 89.3(3) 14_464 . ?
O10 Zr2 Zr3 89.3(3) . . ?
O10 Zr2 O4 78.5(3) 14_464 13_444 ?
O10 Zr2 O4 142.6(3) . 13_444 ?
O10 Zr2 O6 141.2(3) 14_464 16_353 ?
O10 Zr2 O6 142.4(3) . 16_353 ?
O10 Zr2 O7 108.1(4) 14_464 . ?
O10 Zr2 O7 69.4(3) . . ?
O10 Zr2 O10 69.0(3) . 14_464 ?
O10 Zr2 O12 83.4(3) . . ?
O10 Zr2 O12 82.2(4) 14_464 . ?
O10 Zr2 O15 143.7(3) 14_464 . ?
O10 Zr2 O15 82.5(4) . . ?
O12 Zr2 Zr1 114.9(2) . . ?
O12 Zr2 Zr1 113.7(3) . 14_464 ?
O12 Zr2 Zr2 80.7(3) . 14_464 ?
O12 Zr2 Zr3 170.4(3) . . ?
O12 Zr2 O4 74.0(3) . 13_444 ?
O15 Zr2 Zr1 169.4(3) . 14_464 ?
O15 Zr2 Zr1 79.9(4) . . ?
O15 Zr2 Zr2 114.3(3) . 14_464 ?
O15 Zr2 Zr3 113.1(3) . . ?
O15 Zr2 O4 116.9(4) . 13_444 ?
O15 Zr2 O6 74.7(4) . 16_353 ?
O15 Zr2 O12 72.2(4) . . ?
Zr1 Zr3 Zr1 89.80(4) 14_464 . ?
Zr1 Zr3 Zr2 60.01(3) 14_464 . ?
Zr1 Zr3 Zr3 60.16(4) 14_464 14_464 ?
Zr2 Zr3 Zr1 60.20(3) . . ?
Zr3 Zr3 Zr1 59.74(3) 14_464 . ?
Zr3 Zr3 Zr2 90.30(3) 14_464 . ?
O2 Zr3 Zr1 165.0(2) 14_464 . ?
O2 Zr3 Zr1 75.2(2) 14_464 14_464 ?
O2 Zr3 Zr2 109.9(2) 14_464 . ?
O2 Zr3 Zr3 111.6(3) 14_464 14_464 ?
O2 Zr3 O5 74.7(3) 14_464 16_353 ?
O2 Zr3 O9 78.2(4) 14_464 14_464 ?
O2 Zr3 O16 112.1(4) 14_464 . ?
O5 Zr3 Zr1 110.42(19) 16_353 . ?
O5 Zr3 Zr1 109.2(2) 16_353 14_464 ?
O5 Zr3 Zr2 73.33(18) 16_353 . ?
O5 Zr3 Zr3 163.62(18) 16_353 14_464 ?
O5 Zr3 O16 72.1(4) 16_353 . ?
O7 Zr3 Zr1 90.5(3) . 14_464 ?
O7 Zr3 Zr1 34.8(2) . . ?
O7 Zr3 Zr2 36.1(2) . . ?
O7 Zr3 Zr3 89.7(3) . 14_464 ?
O7 Zr3 O2 142.0(3) . 14_464 ?
O7 Zr3 O5 77.4(3) . 16_353 ?
O7 Zr3 O9 109.9(4) . 14_464 ?
O7 Zr3 O11 143.1(3) . . ?
O7 Zr3 O16 82.6(4) . . ?
O8 Zr3 Zr1 88.9(3) . . ?
O8 Zr3 Zr1 35.6(2) . 14_464 ?
O8 Zr3 Zr2 34.1(2) . . ?
O8 Zr3 Zr3 90.0(2) . 14_464 ?
O8 Zr3 O2 78.4(3) . 14_464 ?
O8 Zr3 O5 76.2(3) . 16_353 ?
O8 Zr3 O7 70.2(3) . . ?
O8 Zr3 O9 71.1(4) . 14_464 ?
O8 Zr3 O9 110.1(4) . . ?
O8 Zr3 O11 142.8(3) . . ?
O8 Zr3 O16 141.9(3) . . ?
O9 Zr3 Zr1 92.0(3) . 14_464 ?
O9 Zr3 Zr1 90.1(2) 14_464 . ?
O9 Zr3 Zr1 34.3(3) . . ?
O9 Zr3 Zr1 35.5(3) 14_464 14_464 ?
O9 Zr3 Zr2 90.5(3) . . ?
O9 Zr3 Zr2 90.4(3) 14_464 . ?
O9 Zr3 Zr3 35.5(2) 14_464 14_464 ?
O9 Zr3 Zr3 37.4(3) . 14_464 ?
O9 Zr3 O2 144.6(4) . 14_464 ?
O9 Zr3 O5 140.9(3) 14_464 16_353 ?
O9 Zr3 O5 140.3(4) . 16_353 ?
O9 Zr3 O7 69.0(4) . . ?
O9 Zr3 O9 72.9(4) . 14_464 ?
O9 Zr3 O11 80.5(4) . . ?
O9 Zr3 O16 82.9(4) . . ?
O9 Zr3 O16 145.6(4) 14_464 . ?
O11 Zr3 Zr1 111.5(3) . 14_464 ?
O11 Zr3 Zr1 113.1(3) . . ?
O11 Zr3 Zr2 167.6(2) . . ?
O11 Zr3 Zr3 77.4(2) . 14_464 ?
O11 Zr3 O2 74.2(4) . 14_464 ?
O11 Zr3 O5 119.0(3) . 16_353 ?
O11 Zr3 O9 78.9(4) . 14_464 ?
O11 Zr3 O16 73.1(4) . . ?
O16 Zr3 Zr1 172.5(3) . 14_464 ?
O16 Zr3 Zr1 82.9(3) . . ?
O16 Zr3 Zr2 114.4(3) . . ?
O16 Zr3 Zr3 116.8(3) . 14_464 ?
O1 C1 C2 117.1(13) . . ?
O2 C1 C2 112.6(13) . . ?
O2 C1 O1 129.9(10) . . ?
C3 C2 C1 123.0(14) . . ?
C3 C2 C7 119.0(12) . . ?
C7 C2 C1 117.9(14) . . ?
C4 C3 C2 121.3(14) . . ?
C5 C4 C3 121.5(16) . . ?
C4 C5 C6 119.6(14) . . ?
C4 C5 C24 124.7(15) . . ?
C24 C5 C6 115.7(14) . . ?
C7 C6 C5 117.9(15) . . ?
C2 C7 C6 120.3(15) . . ?
O3 C8 C9 117.3(12) . . ?
O3 C8 O4 123.6(10) . . ?
O4 C8 C9 119.1(13) . . ?
C10 C9 C8 123.0(15) . . ?
C10 C9 C14 114.6(12) . . ?
C14 C9 C8 122.4(12) . . ?
C9 C10 C11 120.8(15) . . ?
C12 C11 C10 122.0(13) . . ?
C11 C12 C13 118.0(13) . . ?
C11 C12 C23 122.1(14) . . ?
C13 C12 C23 118.0(13) . . ?
C14 C13 C12 121.5(15) . . ?
C13 C14 C9 121.7(13) . . ?
O5 C15 C16 114.0(11) . . ?
O5 C15 O6 127.4(12) . . ?
O6 C15 C16 118.4(11) . . ?
C17 C16 C15 120.4(12) . . ?
C21 C16 C15 122.7(13) . . ?
C21 C16 C17 116.7(13) . . ?
C18 C17 C16 119.8(14) . . ?
C17 C18 C19 122.9(14) . . ?
C18 C19 C22 121.5(12) . . ?
C20 C19 C18 120.9(16) . . ?
C20 C19 C22 117.5(15) . . ?
C19 C20 C21 116.6(15) . . ?
C16 C21 C20 123.0(13) . . ?
N1 C22 C19 116.8(12) . . ?
N3 C22 C19 114.9(12) . . ?
N3 C22 N1 127.7(14) . . ?
N2 C23 C12 112.5(13) . . ?
N3 C23 C12 121.1(12) . . ?
N3 C23 N2 126.1(11) . . ?
N1 C24 C5 114.0(12) . . ?
N2 C24 C5 123.7(15) . . ?
N2 C24 N1 120.9(12) . . ?
O11 C25 C26 116.5(7) 14_464 . ?
O11 C25 C26 116.5(7) . . ?
O11 C25 O11 127.1(15) . 14_464 ?
O12 C27 C28 102.5(6) 14_464 14_464 ?
O12 C27 C28 102.5(6) . . ?
O12 C27 C28 102.5(6) 14_464 . ?
O12 C27 C28 102.5(6) . 14_464 ?
O12 C27 O12 155.0(12) . 14_464 ?
C29 C28 C27 120.134(6) . . ?
C29 C28 C27 120.134(6) 14_464 . ?
C29 C28 C29 119.732(12) . 14_464 ?
C28 C29 C30 120.134(12) . . ?
C28 C29 C30 120.134(12) 14_464 . ?
C31 C30 C29 120.134(12) . . ?
C30 C31 C30 119.732(12) 14_464 . ?
C22 N1 C24 113.9(11) . . ?
C24 N2 C23 117.6(12) . . ?
C23 N3 C22 113.0(11) . . ?
C1 O1 Zr1 131.9(8) . . ?
C1 O2 Zr3 130.0(8) . 14_464 ?
C8 O3 Zr1 135.7(7) . 2_575 ?
C8 O4 Zr2 133.1(8) . 13_454 ?
C15 O5 Zr3 131.5(9) . 8_465 ?
C15 O6 Zr2 133.2(9) . 8_465 ?
Zr1 O7 Zr2 109.6(4) . . ?
Zr1 O7 Zr3 110.0(4) . . ?
Zr3 O7 Zr2 108.2(4) . . ?
Zr2 O8 Zr1 109.5(4) . 14_464 ?
Zr3 O8 Zr1 109.9(4) . 14_464 ?
Zr3 O8 Zr2 112.1(4) . . ?
Zr1 O9 Zr3 107.0(5) . 14_464 ?
Zr1 O9 Zr3 111.2(5) . . ?
Zr3 O9 Zr3 107.1(4) . 14_464 ?
Zr1 O10 Zr2 108.6(4) . 14_464 ?
Zr2 O10 Zr1 110.9(4) . . ?
Zr2 O10 Zr2 111.0(3) . 14_464 ?
C25 O11 Zr3 129.0(10) . . ?
C27 O12 Zr2 111.7(7) . . ?

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
C1 C2 C3 C4 -178.7(18) . . . . ?
C1 C2 C7 C6 -175.3(15) . . . . ?
C2 C1 O1 Zr1 -170.2(10) . . . . ?
C2 C1 O2 Zr3 172.5(9) . . . 14_464 ?
C2 C3 C4 C5 -6(4) . . . . ?
C3 C2 C7 C6 2(3) . . . . ?
C3 C4 C5 C6 2(3) . . . . ?
C3 C4 C5 C24 -177.1(19) . . . . ?
C4 C5 C6 C7 4(3) . . . . ?
C4 C5 C24 N1 -3(3) . . . . ?
C4 C5 C24 N2 -170(2) . . . . ?
C5 C6 C7 C2 -6(3) . . . . ?
C5 C24 N1 C22 -177.0(17) . . . . ?
C5 C24 N2 C23 171.6(18) . . . . ?
C6 C5 C24 N1 177.8(17) . . . . ?
C6 C5 C24 N2 11(3) . . . . ?
C7 C2 C3 C4 4(3) . . . . ?
C8 C9 C10 C11 -172.9(15) . . . . ?
C8 C9 C14 C13 -179.9(17) . . . . ?
C9 C8 O3 Zr1 167.7(9) . . . 2_575 ?
C9 C8 O4 Zr2 -169.2(9) . . . 13_454 ?
C9 C10 C11 C12 -14(3) . . . . ?
C10 C9 C14 C13 0(3) . . . . ?
C10 C11 C12 C13 12(3) . . . . ?
C10 C11 C12 C23 176.4(17) . . . . ?
C11 C12 C13 C14 -4(3) . . . . ?
C11 C12 C23 N2 14(3) . . . . ?
C11 C12 C23 N3 -172(2) . . . . ?
C12 C13 C14 C9 -2(3) . . . . ?
C12 C23 N2 C24 174.5(16) . . . . ?
C12 C23 N3 C22 -175.4(17) . . . . ?
C13 C12 C23 N2 178.3(17) . . . . ?
C13 C12 C23 N3 -7(3) . . . . ?
C14 C9 C10 C11 7(3) . . . . ?
C15 C16 C17 C18 175.4(16) . . . . ?
C15 C16 C21 C20 -177.8(16) . . . . ?
C16 C15 O5 Zr3 169.7(7) . . . 8_465 ?
C16 C15 O6 Zr2 -170.9(8) . . . 8_465 ?
C16 C17 C18 C19 0(3) . . . . ?
C17 C16 C21 C20 -3(3) . . . . ?
C17 C18 C19 C20 2(3) . . . . ?
C17 C18 C19 C22 -175.7(19) . . . . ?
C18 C19 C20 C21 -4(3) . . . . ?
C18 C19 C22 N1 3(3) . . . . ?
C18 C19 C22 N3 175.6(18) . . . . ?
C19 C20 C21 C16 5(3) . . . . ?
C19 C22 N1 C24 -180.0(16) . . . . ?
C19 C22 N3 C23 -174.6(16) . . . . ?
C20 C19 C22 N1 -174(2) . . . . ?
C20 C19 C22 N3 -2(3) . . . . ?
C21 C16 C17 C18 0(2) . . . . ?
C22 C19 C20 C21 173.6(17) . . . . ?
C23 C12 C13 C14 -169.5(18) . . . . ?
C24 C5 C6 C7 -176.8(17) . . . . ?
C26 C25 O11 Zr3 -178.0(5) . . . . ?
C27 C28 C29 C28 0.0(17) . . . 14_464 ?
C27 C28 C29 C30 180.00(2) . . . . ?
C28 C27 C28 C29 0(100) 14_464 . . . ?
C28 C27 C28 C29 0(100) 14_464 . . 14_464 ?
C28 C27 O12 Zr2 178.7(3) 14_464 . . . ?
C28 C27 O12 Zr2 178.7(3) . . . . ?
C28 C28 C29 C30 0(62) 14_464 . . . ?
C28 C29 C30 C31 0.00(4) . . . . ?
C28 C29 C30 C31 0.00(4) 14_464 . . . ?
C29 C28 C29 C28 0(100) 14_464 . . 14_464 ?
C29 C28 C29 C30 0.00(2) 14_464 . . . ?
C29 C30 C31 C30 0.00(2) . . . 14_464 ?
N1 C22 N3 C23 -4(3) . . . . ?
N1 C24 N2 C23 6(3) . . . . ?
N2 C23 N3 C22 -2(3) . . . . ?
N2 C24 N1 C22 -10(3) . . . . ?
N3 C22 N1 C24 9(3) . . . . ?
N3 C23 N2 C24 0(3) . . . . ?
O1 C1 C2 C3 176.7(16) . . . . ?
O1 C1 C2 C7 -6(2) . . . . ?
O1 C1 O2 Zr3 0(2) . . . 14_464 ?
O2 C1 C2 C3 3(2) . . . . ?
O2 C1 C2 C7 -179.2(15) . . . . ?
O2 C1 O1 Zr1 2(2) . . . . ?
O3 C8 C9 C10 -1(2) . . . . ?
O3 C8 C9 C14 179.2(14) . . . . ?
O3 C8 O4 Zr2 9.0(18) . . . 13_454 ?
O4 C8 C9 C10 177.7(14) . . . . ?
O4 C8 C9 C14 -2(2) . . . . ?
O4 C8 O3 Zr1 -10.5(18) . . . 2_575 ?
O5 C15 C16 C17 -178.8(13) . . . . ?
O5 C15 C16 C21 -4(2) . . . . ?
O5 C15 O6 Zr2 14(2) . . . 8_465 ?
O6 C15 C16 C17 5.2(18) . . . . ?
O6 C15 C16 C21 -179.9(15) . . . . ?
O6 C15 O5 Zr3 -15(2) . . . 8_465 ?
O11 C25 O11 Zr3 2.0(5) 14_464 . . . ?
O12 C27 C28 C28 0(7) 14_464 . . 14_464 ?
O12 C27 C28 C28 0.0 . . . 14_464 ?
O12 C27 C28 C29 -4.4(5) . . . . ?
O12 C27 C28 C29 175.6(5) 14_464 . . . ?
O12 C27 C28 C29 -4.4(5) 14_464 . . 14_464 ?
O12 C27 C28 C29 175.6(5) . . . 14_464 ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 2 0 2.274
0 1 1 2.616
0 3 1 4.149
0 5 1 6.165

_platon_squeeze_details          
;
TITL 1 in I-42d
CELL   38.8511   38.8511   18.7521     90.00     90.00     90.00
SPGR I-42d
# Solvent Accessible Volume =     18119
# Electrons Found in S.A.V. =      4555
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.586 0.485 0.108 !       2.28 eA-3
C102 0.345 0.249 0.279 !       2.21 eA-3
C103 0.326 0.624 0.438 !       2.07 eA-3
Q104 0.789 0.912 0.154 !       2.04 eA-3
Q105 0.547 0.722 0.356 !       1.98 eA-3
Q106 0.047 0.222 0.856 !       1.98 eA-3
C107 0.364 0.226 0.297 !       1.97 eA-3
C108 0.860 0.828 0.418 !       1.91 eA-3
Q109 0.547 0.791 0.872 !       1.89 eA-3
Q110 0.602 0.728 0.330 !       1.88 eA-3
C111 0.369 0.262 0.313 !       1.87 eA-3
C112 0.024 0.291 0.464 !       1.85 eA-3
C113 0.790 0.009 0.217 !       1.84 eA-3
C114 0.265 0.627 0.126 !       1.82 eA-3
Q115 0.587 0.008 0.093 !       1.80 eA-3
C116 0.697 0.257 0.093 !       1.79 eA-3
C117 0.782 0.530 0.017 !       1.73 eA-3
C118 0.334 0.226 0.283 !       1.73 eA-3
C119 0.141 0.236 0.420 !       1.69 eA-3
C120 0.670 0.765 0.128 !       1.67 eA-3
C121 0.273 0.823 0.154 !       1.67 eA-3
C122 0.356 0.227 0.048 !       1.67 eA-3
C123 0.336 0.662 0.046 !       1.58 eA-3
C124 0.023 0.717 0.436 !       1.58 eA-3
C125 0.155 0.182 0.401 !       1.57 eA-3
Q126 0.835 0.408 0.280 !       1.57 eA-3
C127 0.344 0.356 0.920 !       1.56 eA-3
C128 0.844 0.856 0.420 !       1.56 eA-3
Q129 0.493 0.360 0.421 !       1.56 eA-3
C130 0.368 0.224 0.411 !       1.55 eA-3
C131 0.482 0.216 0.032 !       1.55 eA-3
C132 0.991 0.282 0.503 !       1.55 eA-3
C133 0.491 0.782 0.003 !       1.55 eA-3
C134 0.125 0.848 0.096 !       1.51 eA-3
C135 0.695 0.839 0.400 !       1.50 eA-3
C136 0.514 0.443 0.059 !       1.50 eA-3
C137 0.005 0.570 0.860 !       1.49 eA-3
C138 0.505 0.070 0.360 !       1.49 eA-3
Q139 0.393 0.495 0.124 !       1.49 eA-3
C140 0.976 0.914 0.438 !       1.49 eA-3
C141 0.839 0.356 0.203 !       1.48 eA-3
C142 0.275 0.315 0.879 !       1.48 eA-3
C143 0.775 0.815 0.379 !       1.48 eA-3
C144 0.656 0.636 0.924 !       1.48 eA-3
C145 0.228 0.845 0.407 !       1.47 eA-3
C146 0.305 0.220 0.358 !       1.47 eA-3
C147 0.634 0.223 0.263 !       1.47 eA-3
C148 0.782 0.892 0.300 !       1.47 eA-3
C149 0.998 0.306 0.403 !       1.45 eA-3
C150 0.947 0.484 0.261 !       1.45 eA-3
C151 0.662 0.765 0.190 !       1.45 eA-3
C152 0.844 0.644 0.830 !       1.45 eA-3
Q153 0.905 0.664 0.277 !       1.44 eA-3
C154 0.859 0.144 0.045 !       1.43 eA-3
C155 0.367 0.702 0.392 !       1.42 eA-3
C156 0.509 0.062 0.246 !       1.41 eA-3
C157 0.672 0.175 0.138 !       1.40 eA-3
C158 0.133 0.818 0.434 !       1.40 eA-3
C159 0.719 0.894 0.390 !       1.39 eA-3
C160 0.319 0.365 0.016 !       1.38 eA-3
C161 0.272 0.006 0.453 !       1.38 eA-3
C162 0.725 0.673 0.871 !       1.38 eA-3
Q163 0.522 0.889 0.397 !       1.38 eA-3
C164 0.336 0.640 0.124 !       1.37 eA-3
C165 0.366 0.180 0.373 !       1.37 eA-3
C166 0.140 0.336 0.874 !       1.37 eA-3
C167 0.350 0.783 0.043 !       1.36 eA-3
C168 0.961 0.940 0.002 !       1.35 eA-3
C169 0.298 0.889 0.434 !       1.34 eA-3
C170 0.882 0.735 0.487 !       1.34 eA-3
C171 0.637 0.315 0.032 !       1.34 eA-3
Q172 0.330 0.626 0.386 !       1.34 eA-3
C173 0.600 0.785 0.015 !       1.33 eA-3
Q174 0.594 0.180 0.663 !       1.33 eA-3
Q175 0.094 0.680 0.163 !       1.33 eA-3
Q176 0.263 0.781 0.281 !       1.33 eA-3
C177 0.108 0.679 0.190 !       1.32 eA-3
C178 0.507 0.250 0.125 !       1.32 eA-3
C179 0.648 0.798 0.298 !       1.32 eA-3
C180 0.180 0.199 0.374 !       1.32 eA-3
C181 0.586 0.799-0.005 !       1.31 eA-3
C182 0.227 0.459 0.954 !       1.31 eA-3
C183 0.727 0.959 0.454 !       1.31 eA-3
C184 0.585 0.515 0.094 !       1.31 eA-3
C185 0.085 0.015 0.594 !       1.31 eA-3
C186 0.838 0.652 0.317 !       1.30 eA-3
C187 0.749 1.004 0.421 !       1.30 eA-3
C188 0.227 0.165 0.262 !       1.30 eA-3
C189 0.016 0.586 0.843 !       1.30 eA-3
C190 0.667 0.249 0.080 !       1.30 eA-3
C191 0.751 0.663 0.834 !       1.
;
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 -0.008 -0.003 -0.007 18123 4590 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.51(2)
2 0.49(2)

_vrf_CHEMW03_ALERT_2_A           
;PROBLEM: 
ALERT: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside the range 0.90 <> 1.10


RESPONSE: This is the consequence of the use of SQUEEZE. Some guest solvents are highly disordered that 
they could not be assigned. Therefore, the solvent is included in formula, but is not in the model.
;



#===END
####################################################################### 
# 
# 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_493-MOF-TATB
_database_code_depnum_ccdc_archive 'CCDC 1501751'
_audit_update_record             
;
2017-02-24 deposited with the CCDC.
2017-03-03 downloaded from the CCDC.
;

_audit_creation_date             2017-02-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.13(C800 H1115 N146 O423 Zr48)'
_chemical_formula_sum            'C104 H145 N19 O55 Zr6'
_chemical_formula_weight         3088.7039
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O N Zr'
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'

_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      tetragonal
_space_group_IT_number           122
_space_group_name_H-M_alt        'I -4 2 d'
_space_group_name_Hall           'I -4 2bw'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y, -z+3/4'
'x+1/2, -y, -z+3/4'
'-y+1/2, -x, z+3/4'
'y+1/2, x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1, y+1/2, -z+5/4'
'x+1, -y+1/2, -z+5/4'
'-y+1, -x+1/2, z+5/4'
'y+1, x+1/2, z+5/4'

_cell_length_a                   38.9025(7)
_cell_length_b                   38.9025(7)
_cell_length_c                   18.9223(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     28637.1(19)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    7860
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.9130
_cell_measurement_theta_min      4.7170
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.220
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             8464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23798
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        64.995
_diffrn_reflns_theta_max         64.995
_diffrn_reflns_theta_min         4.133
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3031
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -97.00   -6.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5455  -19.0000   60.0000 91

#__ type_ start__ end____ width___ exp.time_
  2 omega   67.00   92.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       40.5455 -144.0000 -144.0000 25

#__ type_ start__ end____ width___ exp.time_
  3 omega   37.00   98.00   1.0000  400.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -45.0000 -120.0000 61

#__ type_ start__ end____ width___ exp.time_
  4 omega   54.00   87.00   1.0000  400.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000 -180.0000 33

#__ type_ start__ end____ width___ exp.time_
  5 omega  111.00  177.00   1.0000  400.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  125.0000 -120.0000 66

#__ type_ start__ end____ width___ exp.time_
  6 omega   34.00   70.00   1.0000  400.0000
omega____ theta____ kappa____ phi______ frames
    -      107.1410  -30.0000   90.0000 36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0184049000
_diffrn_orient_matrix_UB_12      0.0334677000
_diffrn_orient_matrix_UB_13      -0.0214693000
_diffrn_orient_matrix_UB_21      -0.0349199000
_diffrn_orient_matrix_UB_22      -0.0167104000
_diffrn_orient_matrix_UB_23      0.0170496000
_diffrn_orient_matrix_UB_31      0.0025898000
_diffrn_orient_matrix_UB_32      0.0130567000
_diffrn_orient_matrix_UB_33      0.0766607000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.876
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                9210
_reflns_number_total             10644
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         0.893
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details 
;
 Flack x determined using 2979 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.040(11)
_refine_ls_extinction_coef       0.000024(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         10644
_refine_ls_number_restraints     331
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0558
_refine_ls_restrained_S_all      1.024
_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)+(0.1120P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1611
_refine_special_details          
;

The remaining solvent molecules were disordered and assigned as 5 DMF and 5.5 water molecules per unit cell according to the TGA and elemental analysis results. The contributions of these disordered solvent to the scattering values have been removed by using the PLATON SQUEEZE program. The total  unit  cell include 5 DMF and 5.5 water molecules (40e*5+10e*5.5=255e), SQUEEZE result reveals that 5669 electrons were removed from the unit cell. This discrepancy might be owing to the low quality of low angle data caused by the small size of the Zr-MOF crystal and highly disordered nature of the lattice solvents.
 
Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.54(2) 0.46(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C26-C25
 1.51 with sigma of 0.01
 O7_$1-C25 = O7-C25
 1.26 with sigma of 0.01
 C30-C31 = C31-C32 = N4-C32
 1.39 with sigma of 0.01
 N4-C32 = N4-C33 = N5-C33
 1.39 with sigma of 0.01
 C32-C33
 2.38 with sigma of 0.01
 C32-N5
 2.78 with sigma of 0.01
 C33_$1-C45_$1 = C33_$1-C34_$1 = C33-C34 = C33-C45
 1.39 with sigma of 0.01
 O0AA-C46
 1.25 with sigma of 0.01
 O17-C46 = O0AA-C47
 1.24 with sigma of 0.01
 O16_$3-C46 = O16_$3-C47
 1.24 with sigma of 0.01
 C47-C42 = C46-C37
 1.51 with sigma of 0.01
 C29-C28
 1.39 with sigma of 0.01
4. Rigid bond restraints
 C26, C25, O7, O7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
C38 \\sim C39 \\sim C34 \\sim C35 \\sim C36 \\sim C37: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C36 \\sim C35 \\sim C34 \\sim C39 \\sim C38 \\sim C37 \\sim C43 \\sim C44 \\sim
C45 \\sim C40 \\sim C41 \\sim C42 \\sim N4 \\sim C33 \\sim N4 \\sim C32 \\sim
N5 \\sim C33 \\sim C36 \\sim C35 \\sim C34 \\sim C39 \\sim C38 \\sim C37 \\sim
C43 \\sim C44 \\sim C45 \\sim C40 \\sim C41 \\sim C42 \\sim C29 \\sim C30 \\sim
C28 \\sim C29 \\sim C30 \\sim C31 \\sim C27 \\sim C47 \\sim C46: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002
Zr3 \\sim Zr2 \\sim O11: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C26) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O17) \\sim Ueq, Uanis(O0AA) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C46)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
6. Others
 Fixed Sof: H26A(0.5) H26B(0.5) H26C(0.5) O0AA(0.5) O17(0.5) C47(0.5) C46(0.5)
 C36(0.5) H36(0.5) C35(0.5) H35(0.5) C34(0.5) C39(0.5) H39(0.5) C38(0.5)
 H38(0.5) C37(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5) C45(0.5) C40(0.5)
 H40(0.5) C41(0.5) H41(0.5) C42(0.5)
7.a Me refined with riding coordinates:
 C26(H26A,H26B,H26C)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C6(H6), C4(H4), C16(H16), C15(H15), C13(H13), C12(H12),
 C23(H23), C22(H22), C20(H20), C19(H19), C29(H29), C30(H30), C36(H36), C35(H35),
  C39(H39), C38(H38), C43(H43), C44(H44), C40(H40), C41(H41)
7.c Fitted hexagon refined as free rotating group:
 C3(C2,C7,C6,C5,C4), C16(C15,C14,C13,C12,C11), C18(C23,C22,C21,C20,C19),
 C36(C35,C34,C39,C38,C37), C43(C44,C45,C40,C41,C42)
;
_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 0.26363(2) 0.46466(2) 0.78595(5) 0.0487(2) Uani 1 1 d . . . . .
Zr2 Zr 0.18925(2) 0.50987(2) 0.83637(4) 0.0488(2) Uani 1 1 d . U . . .
Zr3 Zr 0.23566(2) 0.55545(2) 0.96369(5) 0.0504(2) Uani 1 1 d . U . . .
C1 C 0.3438(3) 0.4527(3) 0.8087(6) 0.057(3) Uani 1 1 d . . . . .
C3 C 0.37455(14) 0.4129(3) 0.7255(6) 0.119(7) Uani 1 1 d . . . . .
H3 H 0.353291 0.406481 0.707259 0.142 Uiso 1 1 calc R . . . .
C2 C 0.37640(14) 0.4371(3) 0.7793(5) 0.074(3) Uani 1 1 d G . . . .
C7 C 0.40817(17) 0.4467(2) 0.8065(4) 0.081(4) Uani 1 1 d G . . . .
H7 H 0.409415 0.462933 0.842585 0.097 Uiso 1 1 calc R . . . .
C6 C 0.43809(13) 0.4321(3) 0.7798(5) 0.101(5) Uani 1 1 d G . . . .
H6 H 0.459345 0.438570 0.798018 0.121 Uiso 1 1 calc R . . . .
C5 C 0.43623(15) 0.4079(3) 0.7259(6) 0.103(6) Uani 1 1 d G . . . .
C4 C 0.40446(18) 0.3983(3) 0.6987(6) 0.126(8) Uani 1 1 d G . . . .
H4 H 0.403221 0.382117 0.662692 0.152 Uiso 1 1 calc R . . . .
C8 C 0.4681(2) 0.3946(4) 0.6933(7) 0.090(5) Uani 1 1 d . . . . .
C9 C 0.4944(3) 0.3610(4) 0.6128(7) 0.083(4) Uani 1 1 d . . . . .
C10 C 0.5258(3) 0.3894(4) 0.6946(8) 0.088(5) Uani 1 1 d . . . . .
C16 C 0.52418(14) 0.3309(3) 0.5146(5) 0.113(7) Uani 1 1 d . . . . .
H16 H 0.545147 0.335674 0.536047 0.136 Uiso 1 1 calc R . . . .
C15 C 0.52325(15) 0.3122(3) 0.4520(5) 0.101(6) Uani 1 1 d G . . . .
H15 H 0.543591 0.304560 0.431499 0.121 Uiso 1 1 calc R . . . .
C14 C 0.49192(19) 0.3050(2) 0.4199(4) 0.080(4) Uani 1 1 d G . . . .
C13 C 0.46152(15) 0.3165(3) 0.4505(5) 0.105(6) Uani 1 1 d G . . . .
H13 H 0.440552 0.311699 0.429001 0.127 Uiso 1 1 calc R . . . .
C12 C 0.46245(14) 0.3351(3) 0.5131(5) 0.111(7) Uani 1 1 d G . . . .
H12 H 0.442108 0.342813 0.533549 0.133 Uiso 1 1 calc R . . . .
C11 C 0.49378(17) 0.3423(3) 0.5452(4) 0.087(5) Uani 1 1 d G . . . .
C17 C 0.4910(3) 0.2881(2) 0.3489(6) 0.061(3) Uani 1 1 d . . . . .
C18 C 0.55913(13) 0.3996(3) 0.7259(5) 0.079(4) Uani 1 1 d . . . . .
C23 C 0.55960(13) 0.4222(3) 0.7828(5) 0.106(6) Uani 1 1 d G . . . .
H23 H 0.539060 0.430050 0.802014 0.127 Uiso 1 1 calc R . . . .
C22 C 0.59078(16) 0.4331(2) 0.8108(4) 0.097(5) Uani 1 1 d G . . . .
H22 H 0.591096 0.448206 0.848855 0.116 Uiso 1 1 calc R . . . .
C21 C 0.62148(13) 0.4213(2) 0.7821(4) 0.064(3) Uani 1 1 d G . . . .
C20 C 0.62101(13) 0.3987(2) 0.7252(4) 0.077(3) Uani 1 1 d G U . . .
H20 H 0.641550 0.390820 0.705965 0.092 Uiso 1 1 calc R . . . .
C19 C 0.58983(17) 0.3878(2) 0.6972(4) 0.091(4) Uani 1 1 d G U . . .
H19 H 0.589515 0.372664 0.659122 0.109 Uiso 1 1 calc R . . . .
C24 C 0.6552(3) 0.4346(3) 0.8092(6) 0.060(3) Uani 1 1 d . . . . .
C25 C 0.250000 0.3940(5) 0.875000 0.115(6) Uani 1 2 d DS TU P . .
C26 C 0.250000 0.3545(5) 0.875000 0.109(5) Uani 1 2 d DS TU P . .
H26A H 0.259474 0.346253 0.831313 0.164 Uiso 0.5 1 calc R . . A -1
H26B H 0.263666 0.346253 0.913711 0.164 Uiso 0.5 1 calc R . . A -1
H26C H 0.226860 0.346253 0.879976 0.164 Uiso 0.5 1 calc R . . A -1
C27 C 0.250000 0.6267(7) 0.875000 0.136(3) Uani 1 2 d S TU P . .
N1 N 0.4649(2) 0.3743(4) 0.6364(6) 0.104(5) Uani 1 1 d . . . . .
N2 N 0.5259(2) 0.3698(4) 0.6388(7) 0.104(5) Uani 1 1 d . . . . .
N3 N 0.4970(2) 0.4037(3) 0.7224(6) 0.087(4) Uani 1 1 d . . . . .
O1 O 0.31691(18) 0.4458(2) 0.7792(4) 0.0645(19) Uani 1 1 d . . . . .
O2 O 0.34783(17) 0.4739(2) 0.8594(4) 0.066(2) Uani 1 1 d . . . . .
O3 O 0.4621(2) 0.2827(2) 0.3222(4) 0.074(2) Uani 1 1 d . . . . .
O4 O 0.52027(18) 0.2803(2) 0.3211(4) 0.0629(19) Uani 1 1 d . . . . .
O5 O 0.68184(16) 0.42497(19) 0.7789(5) 0.0643(19) Uani 1 1 d . . . . .
O6 O 0.65247(16) 0.4555(2) 0.8604(4) 0.0596(18) Uani 1 1 d . . . . .
O7 O 0.2620(2) 0.4087(2) 0.8198(5) 0.082(2) Uani 1 1 d D U . . .
O8 O 0.2390(3) 0.6110(2) 0.9325(5) 0.084(3) Uani 1 1 d . . . . .
O9 O 0.2199(2) 0.4662(3) 0.8544(5) 0.086(3) Uani 1 1 d . U . . .
O10 O 0.23290(19) 0.5113(2) 0.7656(4) 0.075(2) Uani 1 1 d . . . . .
O11 O 0.2059(3) 0.5101(3) 0.9459(6) 0.098(3) Uani 1 1 d . U . . .
O12 O 0.2282(3) 0.4397(3) 0.7124(5) 0.108(4) Uani 1 1 d . . . . .
O13 O 0.1678(3) 0.4779(3) 0.7471(6) 0.102(3) Uani 1 1 d . . . . .
O14 O 0.1648(2) 0.5401(3) 0.7490(5) 0.092(3) Uani 1 1 d . . . . .
O15 O 0.2796(2) 0.5554(3) 0.8965(6) 0.104(4) Uani 1 1 d . . . . .
O16 O 0.2644(2) 0.5836(2) 1.0418(4) 0.073(2) Uani 1 1 d D . . . .
C28 C 0.250000 0.6641(6) 0.875000 0.136(3) Uani 1 2 d DS TU P . .
C29 C 0.2470(7) 0.6825(4) 0.9369(8) 0.136(2) Uani 1 1 d D U . . .
H29 H 0.244777 0.670533 0.979216 0.163 Uiso 1 1 calc R . . . .
N4 N 0.2559(6) 0.7896(3) 0.9373(6) 0.138(2) Uani 1 1 d D U . . .
C30 C 0.2472(7) 0.7181(4) 0.9389(8) 0.136(2) Uani 1 1 d D U . . .
H30 H 0.245442 0.729700 0.981668 0.164 Uiso 1 1 calc R . . . .
C32 C 0.250000 0.7719(3) 0.875000 0.138(2) Uani 1 2 d DS TU P . .
C31 C 0.250000 0.7362(4) 0.875000 0.137(2) Uani 1 2 d DS TU P . .
N5 N 0.250000 0.8433(4) 0.875000 0.138(2) Uani 1 2 d DS TU P . .
C33 C 0.2595(7) 0.8253(3) 0.9349(6) 0.138(2) Uani 1 1 d D U . . .
O0AA O 0.3048(5) 0.8812(5) 1.2426(11) 0.101(6) Uani 0.5 1 d D U . B 1
O17 O 0.2826(8) 0.9548(6) 1.1229(18) 0.153(11) Uani 0.5 1 d D U . C 2
C47 C 0.2832(9) 0.8910(7) 1.1986(13) 0.138(2) Uani 0.5 1 d D U . B 1
C46 C 0.2727(13) 0.9262(5) 1.1477(9) 0.138(2) Uani 0.5 1 d D U . C 2
C36 C 0.2846(8) 0.9062(5) 1.0250(12) 0.138(2) Uani 0.5 1 d . U . C 2
H36 H 0.296343 0.926658 1.017298 0.166 Uiso 0.5 1 calc R . . C 2
C35 C 0.2785(8) 0.8839(5) 0.9690(9) 0.138(2) Uani 0.5 1 d G U . C 2
H35 H 0.286191 0.889369 0.923921 0.166 Uiso 0.5 1 calc R . . C 2
C34 C 0.2609(8) 0.8533(4) 0.9805(9) 0.138(2) Uani 0.5 1 d DG U . C 2
C39 C 0.2494(8) 0.8450(5) 1.0480(12) 0.138(2) Uani 0.5 1 d G U . C 2
H39 H 0.237572 0.824560 1.055650 0.166 Uiso 0.5 1 calc R . . C 2
C38 C 0.2554(8) 0.8674(5) 1.1039(10) 0.138(2) Uani 0.5 1 d G U . C 2
H38 H 0.247723 0.861849 1.149029 0.166 Uiso 0.5 1 calc R . . C 2
C37 C 0.2730(8) 0.8980(4) 1.0924(9) 0.138(2) Uani 0.5 1 d DG U . C 2
C43 C 0.2877(8) 0.8396(5) 1.1215(10) 0.138(2) Uani 0.5 1 d . U . B 1
H43 H 0.299364 0.828961 1.158463 0.166 Uiso 0.5 1 calc R . . B 1
C44 C 0.2814(9) 0.8218(5) 1.0592(10) 0.138(2) Uani 0.5 1 d G U . B 1
H44 H 0.288832 0.799173 1.054478 0.166 Uiso 0.5 1 calc R . . B 1
C45 C 0.2641(9) 0.8377(5) 1.0041(8) 0.138(2) Uani 0.5 1 d DG U . B 1
C40 C 0.2530(8) 0.8715(5) 1.0112(8) 0.138(2) Uani 0.5 1 d G U . B 1
H40 H 0.241373 0.882206 0.974257 0.166 Uiso 0.5 1 calc R . . B 1
C41 C 0.2593(9) 0.8894(5) 1.0735(8) 0.138(2) Uani 0.5 1 d G U . B 1
H41 H 0.251905 0.911995 1.078240 0.166 Uiso 0.5 1 calc R . . B 1
C42 C 0.2767(9) 0.8734(5) 1.1287(8) 0.138(2) Uani 0.5 1 d DG U . B 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 3.5329(17) 5_556 ?
Zr1 Zr2 3.5059(12) 5_556 ?
Zr1 Zr2 3.5178(10) . ?
Zr1 Zr3 3.5321(11) 5_556 ?
Zr1 O1 2.203(7) . ?
Zr1 O4 2.207(7) 3_566 ?
Zr1 O7 2.269(8) . ?
Zr1 O9 2.173(10) 5_556 ?
Zr1 O9 2.139(7) . ?
Zr1 O10 2.207(9) . ?
Zr1 O11 2.157(10) 5_556 ?
Zr1 O12 2.185(10) . ?
Zr2 Zr3 3.4940(12) . ?
Zr2 Zr3 3.5461(11) 5_556 ?
Zr2 O2 2.256(7) 5_556 ?
Zr2 O6 2.209(7) 6_466 ?
Zr2 O9 2.101(9) . ?
Zr2 O10 2.164(6) . ?
Zr2 O11 2.172(10) . ?
Zr2 O13 2.258(10) . ?
Zr2 O14 2.239(10) . ?
Zr2 O15 2.171(8) 5_556 ?
Zr3 Zr3 3.5371(17) 5_556 ?
Zr3 O3 2.279(8) 7_565 ?
Zr3 O5 2.233(6) 6_466 ?
Zr3 O8 2.244(8) . ?
Zr3 O10 2.144(8) 5_556 ?
Zr3 O11 2.136(11) . ?
Zr3 O15 2.130(7) . ?
Zr3 O15 2.167(11) 5_556 ?
Zr3 O16 2.152(8) . ?
C1 C2 1.513(11) . ?
C1 O1 1.215(13) . ?
C1 O2 1.274(13) . ?
C3 H3 0.9300 . ?
C3 C2 1.3900 . ?
C3 C4 1.3900 . ?
C2 C7 1.3900 . ?
C7 H7 0.9300 . ?
C7 C6 1.3900 . ?
C6 H6 0.9300 . ?
C6 C5 1.3900 . ?
C5 C4 1.3900 . ?
C5 C8 1.478(11) . ?
C4 H4 0.9300 . ?
C8 N1 1.342(14) . ?
C8 N3 1.302(14) . ?
C9 C11 1.471(11) . ?
C9 N1 1.337(14) . ?
C9 N2 1.366(14) . ?
C10 C18 1.479(12) . ?
C10 N2 1.303(15) . ?
C10 N3 1.357(14) . ?
C16 H16 0.9300 . ?
C16 C15 1.3900 . ?
C16 C11 1.3900 . ?
C15 H15 0.9300 . ?
C15 C14 1.3900 . ?
C14 C13 1.3900 . ?
C14 C17 1.497(11) . ?
C13 H13 0.9300 . ?
C13 C12 1.3900 . ?
C12 H12 0.9300 . ?
C12 C11 1.3900 . ?
C17 O3 1.249(14) . ?
C17 O4 1.290(13) . ?
C18 C23 1.3900 . ?
C18 C19 1.3900 . ?
C23 H23 0.9300 . ?
C23 C22 1.3900 . ?
C22 H22 0.9300 . ?
C22 C21 1.3900 . ?
C21 C20 1.3900 . ?
C21 C24 1.501(10) . ?
C20 H20 0.9300 . ?
C20 C19 1.3900 . ?
C19 H19 0.9300 . ?
C24 O5 1.242(14) . ?
C24 O6 1.269(14) . ?
C25 C26 1.538(13) . ?
C25 O7 1.279(8) . ?
C25 O7 1.279(8) 5_556 ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 O8 1.319(15) . ?
C27 O8 1.319(15) 5_556 ?
C27 C28 1.45(3) . ?
O16 C47 1.243(13) 14_466 ?
O16 C46 1.248(13) 14_466 ?
C28 C29 1.379(12) 5_556 ?
C28 C29 1.379(12) . ?
C29 H29 0.9300 . ?
C29 C30 1.38(2) . ?
N4 C32 1.383(8) . ?
N4 C33 1.396(11) . ?
C30 H30 0.9300 . ?
C30 C31 1.405(11) . ?
C32 C31 1.390(12) . ?
N5 N5 0.00(3) 5_556 ?
N5 C33 1.383(11) 5_556 ?
N5 C33 1.383(11) . ?
C33 C34 1.390(10) . ?
C33 C45 1.406(11) . ?
O0AA C47 1.243(12) . ?
O17 C46 1.265(13) . ?
C47 C42 1.511(12) . ?
C46 C37 1.519(13) . ?
C36 H36 0.9300 . ?
C36 C35 1.3900 . ?
C36 C37 1.3900 . ?
C35 H35 0.9300 . ?
C35 C34 1.3900 . ?
C34 C39 1.3900 . ?
C39 H39 0.9300 . ?
C39 C38 1.3900 . ?
C38 H38 0.9300 . ?
C38 C37 1.3900 . ?
C43 H43 0.9300 . ?
C43 C44 1.3900 . ?
C43 C42 1.3900 . ?
C44 H44 0.9300 . ?
C44 C45 1.3900 . ?
C45 C40 1.3900 . ?
C40 H40 0.9300 . ?
C40 C41 1.3900 . ?
C41 H41 0.9300 . ?
C41 C42 1.3900 . ?

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 Zr1 59.97(3) 5_556 5_556 ?
Zr2 Zr1 Zr1 59.63(2) . 5_556 ?
Zr2 Zr1 Zr2 89.56(3) 5_556 . ?
Zr2 Zr1 Zr3 60.40(2) . 5_556 ?
Zr2 Zr1 Zr3 59.53(2) 5_556 5_556 ?
Zr3 Zr1 Zr1 90.03(2) 5_556 5_556 ?
O1 Zr1 Zr1 109.7(2) . 5_556 ?
O1 Zr1 Zr2 73.4(2) . 5_556 ?
O1 Zr1 Zr2 163.0(2) . . ?
O1 Zr1 Zr3 109.0(2) . 5_556 ?
O1 Zr1 O4 76.0(3) . 3_566 ?
O1 Zr1 O7 73.9(3) . . ?
O1 Zr1 O10 140.7(3) . . ?
O4 Zr1 Zr1 164.60(18) 3_566 5_556 ?
O4 Zr1 Zr2 111.00(19) 3_566 . ?
O4 Zr1 Zr2 110.2(2) 3_566 5_556 ?
O4 Zr1 Zr3 74.57(18) 3_566 5_556 ?
O4 Zr1 O7 121.5(3) 3_566 . ?
O7 Zr1 Zr1 73.9(2) . 5_556 ?
O7 Zr1 Zr2 107.5(2) . 5_556 ?
O7 Zr1 Zr2 112.3(2) . . ?
O7 Zr1 Zr3 163.5(2) . 5_556 ?
O9 Zr1 Zr1 34.7(2) 5_556 5_556 ?
O9 Zr1 Zr1 35.3(3) . 5_556 ?
O9 Zr1 Zr2 89.1(3) . 5_556 ?
O9 Zr1 Zr2 34.2(3) 5_556 5_556 ?
O9 Zr1 Zr2 33.6(3) . . ?
O9 Zr1 Zr2 88.3(2) 5_556 . ?
O9 Zr1 Zr3 88.6(3) . 5_556 ?
O9 Zr1 Zr3 88.1(3) 5_556 5_556 ?
O9 Zr1 O1 142.5(3) . . ?
O9 Zr1 O1 77.7(3) 5_556 . ?
O9 Zr1 O4 141.5(3) 5_556 3_566 ?
O9 Zr1 O4 141.5(3) . 3_566 ?
O9 Zr1 O7 76.5(4) 5_556 . ?
O9 Zr1 O7 80.5(3) . . ?
O9 Zr1 O9 69.9(4) . 5_556 ?
O9 Zr1 O10 69.6(3) . . ?
O9 Zr1 O10 107.7(4) 5_556 . ?
O9 Zr1 O11 108.5(5) . 5_556 ?
O9 Zr1 O12 84.0(4) . . ?
O9 Zr1 O12 143.8(3) 5_556 . ?
O10 Zr1 Zr1 90.23(19) . 5_556 ?
O10 Zr1 Zr2 35.98(17) . . ?
O10 Zr1 Zr2 89.5(2) . 5_556 ?
O10 Zr1 Zr3 35.1(2) . 5_556 ?
O10 Zr1 O4 77.3(3) . 3_566 ?
O10 Zr1 O7 145.3(3) . . ?
O11 Zr1 Zr1 90.8(3) 5_556 5_556 ?
O11 Zr1 Zr2 36.1(3) 5_556 5_556 ?
O11 Zr1 Zr2 89.9(3) 5_556 . ?
O11 Zr1 Zr3 34.4(3) 5_556 5_556 ?
O11 Zr1 O1 76.4(4) 5_556 . ?
O11 Zr1 O4 76.5(4) 5_556 3_566 ?
O11 Zr1 O7 139.2(4) 5_556 . ?
O11 Zr1 O9 70.3(4) 5_556 5_556 ?
O11 Zr1 O10 69.6(4) 5_556 . ?
O11 Zr1 O12 144.3(4) 5_556 . ?
O12 Zr1 Zr1 114.7(3) . 5_556 ?
O12 Zr1 Zr2 82.9(4) . . ?
O12 Zr1 Zr2 172.4(4) . 5_556 ?
O12 Zr1 Zr3 116.7(3) . 5_556 ?
O12 Zr1 O1 114.1(4) . . ?
O12 Zr1 O4 73.7(3) . 3_566 ?
O12 Zr1 O7 74.7(4) . . ?
O12 Zr1 O10 85.0(4) . . ?
Zr1 Zr2 Zr1 60.40(3) 5_556 . ?
Zr1 Zr2 Zr3 60.00(2) . 5_556 ?
Zr1 Zr2 Zr3 90.24(3) 5_556 5_556 ?
Zr3 Zr2 Zr1 90.90(3) . . ?
Zr3 Zr2 Zr1 60.61(2) . 5_556 ?
Zr3 Zr2 Zr3 60.31(3) . 5_556 ?
O2 Zr2 Zr1 73.1(2) 5_556 5_556 ?
O2 Zr2 Zr1 109.8(2) 5_556 . ?
O2 Zr2 Zr3 163.4(2) 5_556 5_556 ?
O2 Zr2 Zr3 109.3(2) 5_556 . ?
O2 Zr2 O13 76.3(4) 5_556 . ?
O6 Zr2 Zr1 109.3(2) 6_466 5_556 ?
O6 Zr2 Zr1 164.07(19) 6_466 . ?
O6 Zr2 Zr3 73.18(19) 6_466 . ?
O6 Zr2 Zr3 110.49(19) 6_466 5_556 ?
O6 Zr2 O2 75.9(3) 6_466 5_556 ?
O6 Zr2 O13 116.0(4) 6_466 . ?
O6 Zr2 O14 75.0(3) 6_466 . ?
O9 Zr2 Zr1 35.6(3) . 5_556 ?
O9 Zr2 Zr1 34.3(2) . . ?
O9 Zr2 Zr3 88.9(3) . 5_556 ?
O9 Zr2 Zr3 90.3(3) . . ?
O9 Zr2 O2 77.8(3) . 5_556 ?
O9 Zr2 O6 141.9(3) . 6_466 ?
O9 Zr2 O10 71.1(3) . . ?
O9 Zr2 O11 71.3(4) . . ?
O9 Zr2 O13 83.5(5) . . ?
O9 Zr2 O14 141.6(4) . . ?
O9 Zr2 O15 108.6(4) . 5_556 ?
O10 Zr2 Zr1 91.7(3) . 5_556 ?
O10 Zr2 Zr1 36.8(2) . . ?
O10 Zr2 Zr3 90.5(2) . . ?
O10 Zr2 Zr3 34.4(2) . 5_556 ?
O10 Zr2 O2 143.1(3) . 5_556 ?
O10 Zr2 O6 140.8(3) . 6_466 ?
O10 Zr2 O11 110.9(4) . . ?
O10 Zr2 O13 80.9(3) . . ?
O10 Zr2 O14 82.1(4) . . ?
O10 Zr2 O15 68.5(3) . 5_556 ?
O11 Zr2 Zr1 35.8(3) . 5_556 ?
O11 Zr2 Zr1 90.9(3) . . ?
O11 Zr2 Zr3 35.5(3) . . ?
O11 Zr2 Zr3 90.4(3) . 5_556 ?
O11 Zr2 O2 76.1(4) . 5_556 ?
O11 Zr2 O6 75.8(3) . 6_466 ?
O11 Zr2 O13 145.8(4) . . ?
O11 Zr2 O14 146.0(4) . . ?
O13 Zr2 Zr1 80.0(3) . . ?
O13 Zr2 Zr1 115.7(3) . 5_556 ?
O13 Zr2 Zr3 170.6(3) . . ?
O13 Zr2 Zr3 112.3(3) . 5_556 ?
O14 Zr2 Zr1 173.5(3) . 5_556 ?
O14 Zr2 Zr1 114.3(2) . . ?
O14 Zr2 Zr3 117.5(3) . . ?
O14 Zr2 Zr3 83.7(3) . 5_556 ?
O14 Zr2 O2 112.9(3) . 5_556 ?
O14 Zr2 O13 65.1(4) . . ?
O15 Zr2 Zr1 89.4(3) 5_556 . ?
O15 Zr2 Zr1 90.8(4) 5_556 5_556 ?
O15 Zr2 Zr3 34.1(2) 5_556 5_556 ?
O15 Zr2 Zr3 36.3(3) 5_556 . ?
O15 Zr2 O2 142.6(3) 5_556 5_556 ?
O15 Zr2 O6 78.2(3) 5_556 6_466 ?
O15 Zr2 O11 71.7(4) 5_556 . ?
O15 Zr2 O13 140.1(4) 5_556 . ?
O15 Zr2 O14 85.4(5) 5_556 . ?
Zr1 Zr3 Zr2 59.60(2) 5_556 5_556 ?
Zr1 Zr3 Zr3 89.96(2) 5_556 5_556 ?
Zr2 Zr3 Zr1 59.86(2) . 5_556 ?
Zr2 Zr3 Zr2 89.29(3) . 5_556 ?
Zr2 Zr3 Zr3 60.57(3) . 5_556 ?
Zr3 Zr3 Zr2 59.11(2) 5_556 5_556 ?
O3 Zr3 Zr1 72.6(2) 7_565 5_556 ?
O3 Zr3 Zr2 107.9(2) 7_565 . ?
O3 Zr3 Zr2 110.4(2) 7_565 5_556 ?
O3 Zr3 Zr3 162.5(2) 7_565 5_556 ?
O5 Zr3 Zr1 110.40(19) 6_466 5_556 ?
O5 Zr3 Zr2 163.7(2) 6_466 5_556 ?
O5 Zr3 Zr2 74.5(2) 6_466 . ?
O5 Zr3 Zr3 110.8(2) 6_466 5_556 ?
O5 Zr3 O3 75.7(3) 6_466 7_565 ?
O5 Zr3 O8 75.1(4) 6_466 . ?
O8 Zr3 Zr1 164.4(2) . 5_556 ?
O8 Zr3 Zr2 111.3(3) . 5_556 ?
O8 Zr3 Zr2 109.7(2) . . ?
O8 Zr3 Zr3 74.4(2) . 5_556 ?
O8 Zr3 O3 123.0(3) . 7_565 ?
O10 Zr3 Zr1 36.3(2) 5_556 5_556 ?
O10 Zr3 Zr2 90.8(3) 5_556 . ?
O10 Zr3 Zr2 34.78(17) 5_556 5_556 ?
O10 Zr3 Zr3 89.6(2) 5_556 5_556 ?
O10 Zr3 O3 76.9(3) 5_556 7_565 ?
O10 Zr3 O5 142.8(3) 5_556 6_466 ?
O10 Zr3 O8 141.8(3) 5_556 . ?
O10 Zr3 O15 109.3(4) 5_556 5_556 ?
O10 Zr3 O16 89.1(4) 5_556 . ?
O11 Zr3 Zr1 34.8(3) . 5_556 ?
O11 Zr3 Zr2 36.1(3) . . ?
O11 Zr3 Zr2 89.5(3) . 5_556 ?
O11 Zr3 Zr3 91.2(3) . 5_556 ?
O11 Zr3 O3 74.0(4) . 7_565 ?
O11 Zr3 O5 77.5(3) . 6_466 ?
O11 Zr3 O8 141.7(4) . . ?
O11 Zr3 O10 71.1(4) . 5_556 ?
O11 Zr3 O15 72.5(4) . 5_556 ?
O11 Zr3 O16 144.0(4) . . ?
O15 Zr3 Zr1 89.6(3) . 5_556 ?
O15 Zr3 Zr1 90.2(3) 5_556 5_556 ?
O15 Zr3 Zr2 90.1(4) . . ?
O15 Zr3 Zr2 34.8(2) . 5_556 ?
O15 Zr3 Zr2 36.4(2) 5_556 . ?
O15 Zr3 Zr2 88.2(3) 5_556 5_556 ?
O15 Zr3 Zr3 34.3(2) 5_556 5_556 ?
O15 Zr3 Zr3 34.9(3) . 5_556 ?
O15 Zr3 O3 141.3(3) 5_556 7_565 ?
O15 Zr3 O3 142.1(3) . 7_565 ?
O15 Zr3 O5 78.7(3) 5_556 6_466 ?
O15 Zr3 O5 142.2(3) . 6_466 ?
O15 Zr3 O8 78.3(4) . . ?
O15 Zr3 O8 76.3(4) 5_556 . ?
O15 Zr3 O10 69.6(3) . 5_556 ?
O15 Zr3 O11 109.9(5) . . ?
O15 Zr3 O15 69.2(4) . 5_556 ?
O15 Zr3 O16 89.6(4) . . ?
O16 Zr3 Zr1 120.2(2) . 5_556 ?
O16 Zr3 Zr2 90.5(2) . 5_556 ?
O16 Zr3 Zr2 179.8(2) . . ?
O16 Zr3 Zr3 119.2(2) . 5_556 ?
O16 Zr3 O3 72.3(3) . 7_565 ?
O16 Zr3 O5 105.7(3) . 6_466 ?
O16 Zr3 O8 70.2(3) . . ?
O16 Zr3 O15 143.5(3) . 5_556 ?
O1 C1 C2 117.6(9) . . ?
O1 C1 O2 126.6(9) . . ?
O2 C1 C2 115.6(9) . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C2 C1 119.8(6) . . ?
C7 C2 C1 120.2(6) . . ?
C7 C2 C3 120.0 . . ?
C2 C7 H7 120.0 . . ?
C2 C7 C6 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C6 H6 120.0 . . ?
C7 C6 C5 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C5 C4 120.0 . . ?
C6 C5 C8 120.0(6) . . ?
C4 C5 C8 119.8(6) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C8 C5 117.6(8) . . ?
N3 C8 C5 116.9(9) . . ?
N3 C8 N1 125.4(10) . . ?
N1 C9 C11 117.9(9) . . ?
N1 C9 N2 123.6(9) . . ?
N2 C9 C11 116.9(9) . . ?
N2 C10 C18 118.5(9) . . ?
N2 C10 N3 124.0(11) . . ?
N3 C10 C18 117.2(9) . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C11 120.0 . . ?
C11 C16 H16 120.0 . . ?
C16 C15 H15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C14 C17 120.1(6) . . ?
C13 C14 C15 120.0 . . ?
C13 C14 C17 119.6(6) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C12 H12 120.0 . . ?
C13 C12 C11 120.0 . . ?
C11 C12 H12 120.0 . . ?
C16 C11 C9 120.4(6) . . ?
C12 C11 C9 119.6(6) . . ?
C12 C11 C16 120.0 . . ?
O3 C17 C14 117.3(9) . . ?
O3 C17 O4 126.1(9) . . ?
O4 C17 C14 116.6(9) . . ?
C23 C18 C10 119.4(6) . . ?
C23 C18 C19 120.0 . . ?
C19 C18 C10 120.5(6) . . ?
C18 C23 H23 120.0 . . ?
C18 C23 C22 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C21 C24 120.3(6) . . ?
C20 C21 C22 120.0 . . ?
C20 C21 C24 119.6(7) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 C21 120.0 . . ?
C19 C20 H20 120.0 . . ?
C18 C19 H19 120.0 . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
O5 C24 C21 117.9(10) . . ?
O5 C24 O6 128.0(9) . . ?
O6 C24 C21 114.1(10) . . ?
O7 C25 C26 116.6(8) . . ?
O7 C25 C26 116.6(8) 5_556 . ?
O7 C25 O7 126.9(16) 5_556 . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
O8 C27 O8 125(2) . 5_556 ?
O8 C27 C28 117.7(11) 5_556 . ?
O8 C27 C28 117.7(11) . . ?
C9 N1 C8 114.7(9) . . ?
C10 N2 C9 115.8(9) . . ?
C8 N3 C10 115.9(9) . . ?
C1 O1 Zr1 135.1(7) . . ?
C1 O2 Zr2 131.6(7) . 5_556 ?
C17 O3 Zr3 133.4(7) . 15_553 ?
C17 O4 Zr1 132.7(7) . 4_656 ?
C24 O5 Zr3 130.6(7) . 6_566 ?
C24 O6 Zr2 133.2(7) . 6_566 ?
C25 O7 Zr1 132.0(9) . . ?
C27 O8 Zr3 133.1(12) . . ?
Zr1 O9 Zr1 110.0(4) . 5_556 ?
Zr2 O9 Zr1 112.1(4) . . ?
Zr2 O9 Zr1 110.2(4) . 5_556 ?
Zr2 O10 Zr1 107.2(3) . . ?
Zr3 O10 Zr1 108.5(4) 5_556 . ?
Zr3 O10 Zr2 110.8(3) 5_556 . ?
Zr1 O11 Zr2 108.2(5) 5_556 . ?
Zr3 O11 Zr1 110.7(5) . 5_556 ?
Zr3 O11 Zr2 108.4(5) . . ?
Zr3 O15 Zr2 107.3(5) 5_556 5_556 ?
Zr3 O15 Zr2 111.1(4) . 5_556 ?
Zr3 O15 Zr3 110.8(4) . 5_556 ?
C47 O16 Zr3 144.1(16) 14_466 . ?
C47 O16 C46 88(2) 14_466 14_466 ?
C46 O16 Zr3 127.5(17) 14_466 . ?
C29 C28 C27 121.3(12) . . ?
C29 C28 C27 121.3(12) 5_556 . ?
C29 C28 C29 117(2) . 5_556 ?
C28 C29 H29 118.6 . . ?
C28 C29 C30 122.8(19) . . ?
C30 C29 H29 118.6 . . ?
C32 N4 C33 118.9(11) . . ?
C29 C30 H30 120.7 . . ?
C29 C30 C31 118.7(16) . . ?
C31 C30 H30 120.7 . . ?
N4 C32 N4 120.4(13) 5_556 . ?
N4 C32 C31 119.8(6) 5_556 . ?
N4 C32 C31 119.8(6) . . ?
C30 C31 C30 119.6(19) . 5_556 ?
C32 C31 C30 120.2(9) . 5_556 ?
C32 C31 C30 120.2(9) . . ?
C33 N5 C33 119.1(11) 5_556 . ?
N4 C33 C45 109.0(13) . . ?
N5 C33 N4 120.2(11) 5_556 . ?
N5 C33 N4 120.2(11) . . ?
N5 C33 C34 97.0(10) 5_556 . ?
N5 C33 C34 97.0(10) . . ?
N5 C33 C45 128.5(12) . . ?
N5 C33 C45 128.5(12) 5_556 . ?
C34 C33 N4 139.7(14) . . ?
O16 C47 O0AA 122.9(16) 14_466 . ?
O16 C47 C42 113.0(16) 14_466 . ?
O0AA C47 C42 124.2(18) . . ?
O16 C46 O17 133(2) 14_466 . ?
O16 C46 C37 114.4(17) 14_466 . ?
O17 C46 C37 112(2) . . ?
C35 C36 H36 120.0 . . ?
C35 C36 C37 120.0 . . ?
C37 C36 H36 120.0 . . ?
C36 C35 H35 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35 120.0 . . ?
C33 C34 C35 126(2) . . ?
C33 C34 C39 112.1(16) . . ?
C35 C34 C39 120.0 . . ?
C34 C39 H39 120.0 . . ?
C38 C39 C34 120.0 . . ?
C38 C39 H39 120.0 . . ?
C39 C38 H38 120.0 . . ?
C39 C38 C37 120.0 . . ?
C37 C38 H38 120.0 . . ?
C36 C37 C46 117.9(16) . . ?
C38 C37 C46 120.5(19) . . ?
C38 C37 C36 120.0 . . ?
C44 C43 H43 120.0 . . ?
C44 C43 C42 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 H44 120.0 . . ?
C43 C44 C45 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C33 127.4(15) . . ?
C40 C45 C33 112.1(14) . . ?
C40 C45 C44 120.0 . . ?
C45 C40 H40 120.0 . . ?
C45 C40 C41 120.0 . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 120.0 . . ?
C40 C41 C42 120.0 . . ?
C42 C41 H41 120.0 . . ?
C43 C42 C47 117.5(14) . . ?
C41 C42 C47 122.5(14) . . ?
C41 C42 C43 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C7 C6 179.5(11) . . . . ?
C3 C2 C7 C6 0.0 . . . . ?
C2 C1 O1 Zr1 -170.1(7) . . . . ?
C2 C1 O2 Zr2 170.7(7) . . . 5_556 ?
C2 C3 C4 C5 0.0 . . . . ?
C2 C7 C6 C5 0.0 . . . . ?
C7 C6 C5 C4 0.0 . . . . ?
C7 C6 C5 C8 174.7(14) . . . . ?
C6 C5 C4 C3 0.0 . . . . ?
C6 C5 C8 N1 -172.7(13) . . . . ?
C6 C5 C8 N3 7(2) . . . . ?
C5 C8 N1 C9 -175.0(16) . . . . ?
C5 C8 N3 C10 175.8(15) . . . . ?
C4 C3 C2 C1 -179.5(11) . . . . ?
C4 C3 C2 C7 0.0 . . . . ?
C4 C5 C8 N1 2(2) . . . . ?
C4 C5 C8 N3 -178.0(13) . . . . ?
C8 C5 C4 C3 -174.7(14) . . . . ?
C10 C18 C23 C22 -177.3(13) . . . . ?
C10 C18 C19 C20 177.2(13) . . . . ?
C16 C15 C14 C13 0.0 . . . . ?
C16 C15 C14 C17 173.9(10) . . . . ?
C15 C16 C11 C9 177.8(12) . . . . ?
C15 C16 C11 C12 0.0 . . . . ?
C15 C14 C13 C12 0.0 . . . . ?
C15 C14 C17 O3 -179.0(9) . . . . ?
C15 C14 C17 O4 1.0(14) . . . . ?
C14 C13 C12 C11 0.0 . . . . ?
C14 C17 O3 Zr3 171.4(7) . . . 15_553 ?
C14 C17 O4 Zr1 -168.2(7) . . . 4_656 ?
C13 C14 C17 O3 -5.1(14) . . . . ?
C13 C14 C17 O4 175.0(9) . . . . ?
C13 C12 C11 C9 -177.8(12) . . . . ?
C13 C12 C11 C16 0.0 . . . . ?
C11 C9 N1 C8 -171.8(15) . . . . ?
C11 C9 N2 C10 172.9(15) . . . . ?
C11 C16 C15 C14 0.0 . . . . ?
C17 C14 C13 C12 -174.0(10) . . . . ?
C18 C10 N2 C9 179.3(15) . . . . ?
C18 C10 N3 C8 179.3(15) . . . . ?
C18 C23 C22 C21 0.0 . . . . ?
C23 C18 C19 C20 0.0 . . . . ?
C23 C22 C21 C20 0.0 . . . . ?
C23 C22 C21 C24 176.3(10) . . . . ?
C22 C21 C20 C19 0.0 . . . . ?
C22 C21 C24 O5 -175.5(8) . . . . ?
C22 C21 C24 O6 2.6(12) . . . . ?
C21 C20 C19 C18 0.0 . . . . ?
C21 C24 O5 Zr3 167.2(7) . . . 6_566 ?
C21 C24 O6 Zr2 -168.8(7) . . . 6_566 ?
C20 C21 C24 O5 0.8(13) . . . . ?
C20 C21 C24 O6 178.9(7) . . . . ?
C19 C18 C23 C22 0.0 . . . . ?
C24 C21 C20 C19 -176.4(10) . . . . ?
C26 C25 O7 Zr1 173.1(5) . . . . ?
C27 C28 C29 C30 180(2) . . . . ?
N1 C8 N3 C10 -4(3) . . . . ?
N1 C9 C11 C16 173.6(13) . . . . ?
N1 C9 C11 C12 -9(2) . . . . ?
N1 C9 N2 C10 8(3) . . . . ?
N2 C9 C11 C16 7.5(19) . . . . ?
N2 C9 C11 C12 -174.7(13) . . . . ?
N2 C9 N1 C8 -7(3) . . . . ?
N2 C10 C18 C23 176.1(13) . . . . ?
N2 C10 C18 C19 -1(2) . . . . ?
N2 C10 N3 C8 5(3) . . . . ?
N3 C8 N1 C9 5(3) . . . . ?
N3 C10 C18 C23 2(2) . . . . ?
N3 C10 C18 C19 -175.6(12) . . . . ?
N3 C10 N2 C9 -7(3) . . . . ?
O1 C1 C2 C3 -6.8(14) . . . . ?
O1 C1 C2 C7 173.8(9) . . . . ?
O1 C1 O2 Zr2 -4.0(17) . . . 5_556 ?
O2 C1 C2 C3 178.0(8) . . . . ?
O2 C1 C2 C7 -1.4(14) . . . . ?
O2 C1 O1 Zr1 4.4(19) . . . . ?
O3 C17 O4 Zr1 11.8(18) . . . 4_656 ?
O4 C17 O3 Zr3 -8.7(19) . . . 15_553 ?
O5 C24 O6 Zr2 9.0(17) . . . 6_566 ?
O6 C24 O5 Zr3 -10.5(17) . . . 6_566 ?
O7 C25 O7 Zr1 -6.9(5) 5_556 . . . ?
O8 C27 O8 Zr3 3.3(6) 5_556 . . . ?
O8 C27 C28 C29 15.8(14) 5_556 . . 5_556 ?
O8 C27 C28 C29 -164.2(14) . . . 5_556 ?
O8 C27 C28 C29 -164.2(14) 5_556 . . . ?
O8 C27 C28 C29 15.8(14) . . . . ?
O16 C47 C42 C43 -160(3) 14_466 . . . ?
O16 C47 C42 C41 17(5) 14_466 . . . ?
O16 C46 C37 C36 -175(3) 14_466 . . . ?
O16 C46 C37 C38 19(5) 14_466 . . . ?
C28 C27 O8 Zr3 -176.7(6) . . . . ?
C28 C29 C30 C31 1(4) . . . . ?
C29 C28 C29 C30 0(2) 5_556 . . . ?
C29 C30 C31 C30 -0.5(19) . . . 5_556 ?
C29 C30 C31 C32 180(2) . . . . ?
N4 C32 C31 C30 16.3(15) 5_556 . . 5_556 ?
N4 C32 C31 C30 -163.7(15) 5_556 . . . ?
N4 C32 C31 C30 16.3(15) . . . . ?
N4 C32 C31 C30 -163.7(15) . . . 5_556 ?
N4 C33 C34 C35 151(3) . . . . ?
N4 C33 C34 C39 -15(5) . . . . ?
N4 C33 C45 C44 35(4) . . . . ?
N4 C33 C45 C40 -154(2) . . . . ?
C32 N4 C33 N5 14(3) . . . . ?
C32 N4 C33 N5 14(3) . . . 5_556 ?
C32 N4 C33 C34 169(3) . . . . ?
C32 N4 C33 C45 178(2) . . . . ?
N5 N5 C33 N4 0.0(4) 5_556 . . . ?
N5 N5 C33 C34 0.0(4) 5_556 . . . ?
N5 N5 C33 C45 0.0(3) 5_556 . . . ?
N5 C33 C34 C35 -51(2) . . . . ?
N5 C33 C34 C35 -51(2) 5_556 . . . ?
N5 C33 C34 C39 143.3(16) 5_556 . . . ?
N5 C33 C34 C39 143.3(16) . . . . ?
N5 C33 C45 C44 -163(2) 5_556 . . . ?
N5 C33 C45 C44 -163(2) . . . . ?
N5 C33 C45 C40 9(4) 5_556 . . . ?
N5 C33 C45 C40 9(4) . . . . ?
C33 N4 C32 N4 -6.8(17) . . . 5_556 ?
C33 N4 C32 C31 173.2(17) . . . . ?
C33 N5 C33 N4 -6.9(17) 5_556 . . . ?
C33 N5 C33 N5 0(100) 5_556 . . 5_556 ?
C33 N5 C33 C34 -171(2) 5_556 . . . ?
C33 N5 C33 C45 -168(4) 5_556 . . . ?
C33 C34 C39 C38 167(2) . . . . ?
C33 C45 C40 C41 -172(3) . . . . ?
O0AA C47 C42 C43 19(5) . . . . ?
O0AA C47 C42 C41 -163(3) . . . . ?
O17 C46 C37 C36 2(5) . . . . ?
O17 C46 C37 C38 -164(3) . . . . ?
C36 C35 C34 C33 -165(2) . . . . ?
C36 C35 C34 C39 0.0 . . . . ?
C35 C36 C37 C46 -166(3) . . . . ?
C35 C36 C37 C38 0.0 . . . . ?
C35 C34 C39 C38 0.0 . . . . ?
C34 C39 C38 C37 0.0 . . . . ?
C39 C38 C37 C46 166(3) . . . . ?
C39 C38 C37 C36 0.0 . . . . ?
C37 C36 C35 C34 0.0 . . . . ?
C43 C44 C45 C33 171(3) . . . . ?
C43 C44 C45 C40 0.0 . . . . ?
C44 C43 C42 C47 178(3) . . . . ?
C44 C43 C42 C41 0.0 . . . . ?
C44 C45 C40 C41 0.0 . . . . ?
C45 C40 C41 C42 0.0 . . . . ?
C40 C41 C42 C47 -178(3) . . . . ?
C40 C41 C42 C43 0.0 . . . . ?
C42 C43 C44 C45 0.0 . . . . ?

loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
0 2 0 2.271
2 2 0 3.213
0 1 1 2.597

_platon_squeeze_details          
;
TITL 20150821ZH3.res in I-42d
CELL   38.9025   38.9025   18.9223     90.00     90.00     90.00
SPGR I-42d
# Solvent Accessible Volume =     15351
# Electrons Found in S.A.V. =      5640
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.507 0.641 0.296 !       2.98 eA-3
Q102 0.596 0.188 0.239 !       2.92 eA-3
Q103 0.484 0.804 0.429 !       2.30 eA-3
Q104 0.507 0.849 0.368 !       2.27 eA-3
C105 0.631 0.877 0.261 !       2.22 eA-3
Q106 0.660 0.015 0.137 !       2.21 eA-3
Q107 0.160 0.515 0.637 !       2.21 eA-3
Q108 0.662 0.984 0.109 !       2.11 eA-3
Q109 0.852 0.412 0.700 !       2.02 eA-3
Q110 0.352 0.912 0.200 !       2.02 eA-3
C111 0.041 0.812 0.331 !       1.99 eA-3
Q112 0.986 0.665 0.835 !       1.98 eA-3
C113 0.510 0.279 0.765 !       1.97 eA-3
C114 0.010 0.779 0.265 !       1.97 eA-3
Q115 0.691 0.587 0.144 !       1.96 eA-3
C116 0.996 0.726 0.093 !       1.93 eA-3
Q117 0.508 0.859 0.306 !       1.88 eA-3
Q118 1.000 0.662 0.839 !       1.87 eA-3
Q119 0.853 0.077 0.568 !       1.86 eA-3
Q120 1.002 0.352 0.824 !       1.84 eA-3
Q121 0.023 0.205 0.265 !       1.80 eA-3
C122 0.861 0.193 0.403 !       1.80 eA-3
C123 0.033 0.358 0.886 !       1.79 eA-3
C124 0.533 0.858 0.386 !       1.79 eA-3
C125 0.987 0.264 0.107 !       1.75 eA-3
Q126 0.641 0.989 0.084 !       1.73 eA-3
Q127 0.119 0.780 0.409 !       1.73 eA-3
Q128 0.619 0.280 0.909 !       1.73 eA-3
C129 0.342 0.338 0.467 !       1.73 eA-3
C130 0.960 0.963 0.486 !       1.69 eA-3
C131 0.320 0.368 0.089 !       1.69 eA-3
C132 0.571 0.197 0.420 !       1.66 eA-3
Q133 0.562 0.171 0.342 !       1.65 eA-3
C134 0.991 0.248 0.170 !       1.63 eA-3
C135 0.774 0.522 0.460 !       1.63 eA-3
C136 0.274 0.022 0.960 !       1.63 eA-3
C137 0.555 0.054 0.230 !       1.61 eA-3
C138 0.834 0.161 0.100 !       1.61 eA-3
C139 0.462 0.355 0.847 !       1.61 eA-3
C140 0.712 0.468 0.345 !       1.59 eA-3
C141 0.212 0.968 0.845 !       1.59 eA-3
C142 0.757 0.546 0.374 !       1.59 eA-3
C143 0.257 0.046 0.874 !       1.59 eA-3
Q144 0.991 0.875 0.464 !       1.58 eA-3
C145 0.867 0.866 0.409 !       1.58 eA-3
Q146 0.522 0.615 0.001 !       1.58 eA-3
C147 0.500 0.818 0.457 !       1.57 eA-3
C148 0.953 0.282 0.059 !       1.57 eA-3
C149 0.972 0.740 0.124 !       1.57 eA-3
C150 0.405 0.786 0.427 !       1.57 eA-3
C151 0.790 0.641 0.045 !       1.56 eA-3
Q152 0.362 0.843 0.265 !       1.54 eA-3
Q153 0.888 0.288 0.863 !       1.54 eA-3
Q154 0.342 0.697 0.184 !       1.54 eA-3
C155 0.568 0.249 0.458 !       1.53 eA-3
C156 0.040 0.842 0.324 !       1.52 eA-3
C157 0.540 0.342 0.824 !       1.52 eA-3
C158 0.479 0.021 0.356 !       1.51 eA-3
Q159 0.362 0.150 0.299 !       1.51 eA-3
Q160 0.662 0.953 0.132 !       1.51 eA-3
Q161 0.638 0.958 0.139 !       1.51 eA-3
Q162 0.460 0.638 0.886 !       1.51 eA-3
C163 0.113 0.836 0.455 !       1.50 eA-3
Q164 0.444 0.164 0.371 !       1.50 eA-3
Q165 0.944 0.664 0.871 !       1.50 eA-3
Q166 0.556 0.666 0.870 !       1.49 eA-3
Q167 0.892 0.185 0.407 !       1.49 eA-3
Q168 0.970 0.808 0.295 !       1.49 eA-3
C169 0.540 0.016 0.258 !       1.48 eA-3
C170 0.829 0.881 0.077 !       1.48 eA-3
Q171 0.038 0.179 0.281 !       1.47 eA-3
Q172 0.691 0.959 0.142 !       1.46 eA-3
Q173 0.073 0.868 0.471 !       1.46 eA-3
C174 0.493 0.062 0.184 !       1.46 eA-3
C175 0.903 0.565 0.698 !       1.46 eA-3
C176 0.403 0.065 0.198 !       1.46 eA-3
C177 0.852 0.172 0.048 !       1.45 eA-3
C178 0.740 0.579 0.346 !       1.45 eA-3
C179 0.240 0.079 0.846 !       1.45 eA-3
C180 0.258 0.445 0.185 !       1.44 eA-3
C181 0.827 0.310 0.172 !       1.44 eA-3
C182 0.860 0.161 0.061 !       1.44 eA-3
Q183 0.291 0.559 0.317 !       1.44 eA-3
C184 0.733 0.469 0.308 !       1.44 eA-3
Q185 0.524 0.115 0.345 !       1.43 eA-3
Q186 0.931 0.727 0.076 !       1.43 eA-3
C187 0.874 0.242 0.407 !       1.42 eA-3
C188 0.312 0.343 0.168 !       1.42 eA-3
C189 0.575 1.000 0.250 !       1.42 eA-3
C190 0.445 0.580-0.001 !       1.42 eA-3
C191 0.448 0.969 0.268 !       1.42 eA-3
C192 0.948 0.469 0.768 !       1.42 eA-3
C193 0.268 0.127 0.104 !       1.42 eA-3
C194 0.453 1.000 0.309 !       1.42 eA-3
C195 0.762 0.920 0.864 !       1.42 eA-3
C196 0.744 0.862 0.174 !       1.41 eA-3
Q197 0.840 0.951 0.694 !       1.41 eA-3
C198 0.961 0.272 0.083 !       1.41 eA-3
Q199 0.331 0.865 0.060 !       1.41 eA-3
;
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 -0.028 0.015 0.000 15360 5669 ' '

_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.54(2)
2 0.46(2)

_vrf_CHEMW03_ALERT_2_A           
;PROBLEM:
ALERT: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside  the range 0.90 <> 1.10

RESPONSE: This is the consequence of the use of SQUEEZE. Some guest solvents are highly disordered that they could not be assigned. 
Therefore, the solvent is included in formula, but is not in the model.
;

_vrf_PLAT430                     
;
PROBLEM: 
Short Inter D...A Contact  O3     ..  O17     ..       2.76 Ang. 
Short Inter D...A Contact  O5     ..  O15     ..       2.79 Ang.  
Short Inter D...A Contact  O6     ..  O15     ..       2.76 Ang.
RESPONSE: In the crystal structure, there are a number of short connections
between the O atoms and OH atoms in the range 2.50-2.90 Ang,
which indicate extensive H bonding interactions among them. 
;
_vrf_PLAT987                     
;
PROBLEM: The Flack x is >> 0 - Do a BASF/TWIN Refinement Please Check
RESPONSE: The struture was refined as a racemic twin.
;



#===END
