# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_060514b_kk
_database_code_depnum_ccdc_archive 'CCDC 1035107'
_audit_update_record             
;
2014-11-19 deposited with the CCDC.
2015-02-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ZrDMTD
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H76 O36 S12 Zr6'
_chemical_formula_weight         3025.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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      cubic
_space_group_IT_number           225
_space_group_name_H-M_alt        'F m -3 m'
_space_group_name_Hall           '-F 4 2 3'

_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'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y, x+1/2, -z+1/2'
'-y, -x+1/2, -z+1/2'
'y, -x+1/2, z+1/2'
'-y, x+1/2, z+1/2'
'x, z+1/2, -y+1/2'
'-x, z+1/2, y+1/2'
'-x, -z+1/2, -y+1/2'
'x, -z+1/2, y+1/2'
'z, y+1/2, -x+1/2'
'z, -y+1/2, x+1/2'
'-z, y+1/2, x+1/2'
'-z, -y+1/2, -x+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1/2, x, -z+1/2'
'-y+1/2, -x, -z+1/2'
'y+1/2, -x, z+1/2'
'-y+1/2, x, z+1/2'
'x+1/2, z, -y+1/2'
'-x+1/2, z, y+1/2'
'-x+1/2, -z, -y+1/2'
'x+1/2, -z, y+1/2'
'z+1/2, y, -x+1/2'
'z+1/2, -y, x+1/2'
'-z+1/2, y, x+1/2'
'-z+1/2, -y, -x+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'y+1/2, -x+1/2, z'
'-y+1/2, x+1/2, z'
'x+1/2, z+1/2, -y'
'-x+1/2, z+1/2, y'
'-x+1/2, -z+1/2, -y'
'x+1/2, -z+1/2, y'
'z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, x'
'-z+1/2, -y+1/2, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y, -x+1/2, z+1/2'
'y, x+1/2, z+1/2'
'-y, x+1/2, -z+1/2'
'y, -x+1/2, -z+1/2'
'-x, -z+1/2, y+1/2'
'x, -z+1/2, -y+1/2'
'x, z+1/2, y+1/2'
'-x, z+1/2, -y+1/2'
'-z, -y+1/2, x+1/2'
'-z, y+1/2, -x+1/2'
'z, -y+1/2, -x+1/2'
'z, y+1/2, x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y+1/2, -x, z+1/2'
'y+1/2, x, z+1/2'
'-y+1/2, x, -z+1/2'
'y+1/2, -x, -z+1/2'
'-x+1/2, -z, y+1/2'
'x+1/2, -z, -y+1/2'
'x+1/2, z, y+1/2'
'-x+1/2, z, -y+1/2'
'-z+1/2, -y, x+1/2'
'-z+1/2, y, -x+1/2'
'z+1/2, -y, -x+1/2'
'z+1/2, y, x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
'-y+1/2, x+1/2, -z'
'y+1/2, -x+1/2, -z'
'-x+1/2, -z+1/2, y'
'x+1/2, -z+1/2, -y'
'x+1/2, z+1/2, y'
'-x+1/2, z+1/2, -y'
'-z+1/2, -y+1/2, x'
'-z+1/2, y+1/2, -x'
'z+1/2, -y+1/2, -x'
'z+1/2, y+1/2, x'

_cell_length_a                   32.71650(10)
_cell_length_b                   32.71650(10)
_cell_length_c                   32.71650(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     35018.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    10457
_cell_measurement_theta_min      3.8183
_cell_measurement_theta_max      71.3753

_exptl_crystal_description       octahedral
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    0.574
_exptl_crystal_F_000             6062.4
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    2.321
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.85211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
Due to low resolution of the data, all benzene ring C-C bond distances were 
restrained to 1.39(2) Angstroms and all C, O and S atoms were restrained to 
be approximately isotropic in behaviour.  

The central benzene ring is disordered around the interesection of 
two two fold axes and mirror planes with half occupancy for the carbon atoms. 
The attached sulfur atom is additionally 1:1 disordered with a hydrogen atom. 
For refinemen t reasons, the moiety was modeled as half a benzene ring with 
one SH unit with all atoms one quarter occupied, and with two of the carvon 
atoms being symmetry equivalents of each other (C7 and C8). To overcome 
correlation, all benzene ring C atoms (and their opposite side counterparts) 
were constrained to lie within one common plane that did also include the S 
atom. C7 and C8 were constrained to have identical ADPs, and C6, C7, C8 and 
S1 were subjected to a rigid bond restraint. The C7-S1 bond was restrained 
to 1.76(2) Angstroms. 


The position of O1 was split and refined as half hydroxy and half oxy with 
slightly different Zr-O distances (shorter for the oxy-Ze bonds). Associated 
with the hydroxy unit is half a hydrogen bonded water molecule. The water H 
atoms were omitted from the refinement.
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.1270
_diffrn_reflns_number            25744
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.821
_diffrn_reflns_theta_max         71.511
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1751
_reflns_number_gt                1539
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_diffrn_orient_matrix_UB_11      0.0139919000
_diffrn_orient_matrix_UB_12      0.0389591000
_diffrn_orient_matrix_UB_13      0.0224727000
_diffrn_orient_matrix_UB_21      0.0049773000
_diffrn_orient_matrix_UB_22      0.0220303000
_diffrn_orient_matrix_UB_23      -0.0413161000
_diffrn_orient_matrix_UB_31      -0.0446941000
_diffrn_orient_matrix_UB_32      0.0145843000
_diffrn_orient_matrix_UB_33      0.0024109000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -44.00  -17.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -11.00   20.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -37.0000  150.0000 31

#__ type_ start__ end____ width___ exp.time_
  3 omega   33.00   72.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -120.0000 39

#__ type_ start__ end____ width___ exp.time_
  4 omega   78.00  119.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  120.0000 41

#__ type_ start__ end____ width___ exp.time_
  5 omega   -3.00   94.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000 -125.0000  150.0000 97

#__ type_ start__ end____ width___ exp.time_
  6 omega  -83.00  -25.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   63.0000    0.0000 58

#__ type_ start__ end____ width___ exp.time_
  7 omega  -64.00  -20.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000  -90.0000 44

#__ type_ start__ end____ width___ exp.time_
  8 omega   37.00   62.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
  9 omega   41.00   72.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -60.0000 31

#__ type_ start__ end____ width___ exp.time_
 10 omega   44.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
 11 omega   43.00   70.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -180.0000 27

#__ type_ start__ end____ width___ exp.time_
 12 omega   41.00   69.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 28

#__ type_ start__ end____ width___ exp.time_
 13 omega   52.00   78.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
 14 omega   38.00   66.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -120.0000 28

#__ type_ start__ end____ width___ exp.time_
 15 omega   37.00   64.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  150.0000 27

#__ type_ start__ end____ width___ exp.time_
 16 omega   41.00   67.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
 17 omega   42.00   67.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -30.0000 25

#__ type_ start__ end____ width___ exp.time_
 18 omega   57.00   82.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 19 omega   43.00   89.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   12.0000  120.0000 46

;

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

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  
;  
SHELXL-2013 (Sheldrick, 2013), 
SHELXLE Rev656 (Hübschle et al., 2011)
;
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1492P)²+116.6506P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1751
_refine_ls_number_parameters     69
_refine_ls_number_restraints     106
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0767
_refine_ls_wR_factor_ref         0.2569
_refine_ls_wR_factor_gt          0.2378
_refine_ls_goodness_of_fit_ref   1.300
_refine_ls_restrained_S_all      1.366
_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 0.0000 0.5000 0.07547(2) 0.0373(5) Uani 1 8 d S T P . .
O1 O 0.0316(2) 0.4684(2) 0.0316(2) 0.031(2) Uani 0.5 6 d S TU P A 1
O1B O 0.0423(2) 0.4577(2) 0.0423(2) 0.038(3) Uani 0.5 6 d S TU P A 2
H1B H 0.0600 0.4400 0.0600 0.045 Uiso 0.5 6 calc R U P A 2
O3 O 0.0904(3) 0.4096(3) 0.0904(3) 0.131(8) Uani 0.5 6 d S TU P B 2
O2 O 0.05848(17) 0.5000 0.10941(16) 0.0885(15) Uani 1 2 d S TU P A .
C1 C 0.0959(2) 0.5000 0.0959(2) 0.094(3) Uani 1 4 d S TU P . .
C2 C 0.1279(2) 0.5000 0.1279(2) 0.127(5) Uani 1 4 d DS TU P A .
C3 C 0.1157(4) 0.5000 0.1689(3) 0.179(6) Uani 1 2 d DS TU P . .
H3 H 0.0876 0.5000 0.1762 0.215 Uiso 1 2 calc R U P A .
C4 C 0.1461(4) 0.5000 0.1983(4) 0.216(7) Uani 1 2 d DS TU P A .
H4 H 0.1386 0.5000 0.2264 0.259 Uiso 1 2 calc R U P . .
C5 C 0.1880(4) 0.5000 0.1880(4) 0.166(7) Uani 1 4 d DS TU P . .
C6 C 0.2195(4) 0.5000 0.2195(4) 0.194(8) Uani 1 4 d DS TU P A .
C7 C 0.24654(13) 0.46703(16) 0.22042(13) 0.215(9) Uani 0.25 1 d D U P A -1
C8 C 0.2784(4) 0.4636(7) 0.2496(4) 0.215(9) Uani 0.25 1 d D U P A -1
H8 H 0.2968 0.4412 0.2503 0.258 Uiso 0.25 1 calc R U P A -1
S1 S 0.2531(3) 0.4220(3) 0.1913(3) 0.374(14) Uani 0.25 1 d D U P A -1
H1 H 0.2554 0.3945 0.2154 0.561 Uiso 0.25 1 d R U P A -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.049(2) . ?
Zr1 O1 2.049(2) 100 ?
Zr1 O1 2.049(2) 2_565 ?
Zr1 O1 2.049(2) 99_565 ?
Zr1 O2 2.212(4) . ?
Zr1 O2 2.212(4) 182_455 ?
Zr1 O2 2.212(4) 181 ?
Zr1 O2 2.212(4) 2_565 ?
Zr1 O1B 2.238(5) . ?
Zr1 O1B 2.238(5) 100 ?
Zr1 O1B 2.238(5) 99_565 ?
Zr1 O1B 2.238(5) 2_565 ?
O1 Zr1 2.049(2) 177 ?
O1 Zr1 2.049(2) 29_554 ?
O1B Zr1 2.238(5) 29_554 ?
O1B Zr1 2.238(5) 177 ?
O1B H1B 1.0000 . ?
O2 C1 1.301(7) . ?
C1 O2 1.301(7) 22_565 ?
C1 C2 1.481(14) . ?
C2 C3 1.398(12) . ?
C2 C3 1.398(12) 22_565 ?
C3 C4 1.385(12) . ?
C3 H3 0.9500 . ?
C4 C5 1.410(13) . ?
C4 H4 0.9500 . ?
C5 C4 1.410(13) 22_565 ?
C5 C6 1.46(2) . ?
C6 C7 1.395(10) . ?
C6 C8 1.56(2) 145_565 ?
C7 C8 1.417(15) . ?
C7 S1 1.768(11) . ?
C8 C6 1.56(2) 51 ?
C8 H8 0.9500 . ?
S1 H1 1.2000 . ?

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
O1 Zr1 O1 60.7(4) . 100 ?
O1 Zr1 O1 91.2(6) . 2_565 ?
O1 Zr1 O1 60.7(4) 100 2_565 ?
O1 Zr1 O1 60.7(4) . 99_565 ?
O1 Zr1 O1 91.2(6) 100 99_565 ?
O1 Zr1 O1 60.7(4) 2_565 99_565 ?
O1 Zr1 O2 85.1(3) . . ?
O1 Zr1 O2 142.02(10) 100 . ?
O1 Zr1 O2 142.02(10) 2_565 . ?
O1 Zr1 O2 85.1(3) 99_565 . ?
O1 Zr1 O2 142.01(10) . 182_455 ?
O1 Zr1 O2 142.01(10) 100 182_455 ?
O1 Zr1 O2 85.1(3) 2_565 182_455 ?
O1 Zr1 O2 85.1(3) 99_565 182_455 ?
O2 Zr1 O2 75.40(14) . 182_455 ?
O1 Zr1 O2 85.1(3) . 181 ?
O1 Zr1 O2 85.1(3) 100 181 ?
O1 Zr1 O2 142.01(10) 2_565 181 ?
O1 Zr1 O2 142.01(10) 99_565 181 ?
O2 Zr1 O2 75.40(14) . 181 ?
O2 Zr1 O2 119.7(3) 182_455 181 ?
O1 Zr1 O2 142.01(10) . 2_565 ?
O1 Zr1 O2 85.1(3) 100 2_565 ?
O1 Zr1 O2 85.1(3) 2_565 2_565 ?
O1 Zr1 O2 142.01(10) 99_565 2_565 ?
O2 Zr1 O2 119.7(3) . 2_565 ?
O2 Zr1 O2 75.40(14) 182_455 2_565 ?
O2 Zr1 O2 75.40(14) 181 2_565 ?
O2 Zr1 O1B 73.0(2) . . ?
O2 Zr1 O1B 141.10(7) 182_455 . ?
O2 Zr1 O1B 73.0(2) 181 . ?
O2 Zr1 O1B 141.10(7) 2_565 . ?
O2 Zr1 O1B 141.10(7) . 100 ?
O2 Zr1 O1B 141.10(7) 182_455 100 ?
O2 Zr1 O1B 73.0(2) 181 100 ?
O2 Zr1 O1B 73.0(2) 2_565 100 ?
O1B Zr1 O1B 76.4(2) . 100 ?
O2 Zr1 O1B 73.0(2) . 99_565 ?
O2 Zr1 O1B 73.0(2) 182_455 99_565 ?
O2 Zr1 O1B 141.10(7) 181 99_565 ?
O2 Zr1 O1B 141.10(7) 2_565 99_565 ?
O1B Zr1 O1B 76.4(2) . 99_565 ?
O1B Zr1 O1B 122.0(6) 100 99_565 ?
O2 Zr1 O1B 141.10(7) . 2_565 ?
O2 Zr1 O1B 73.0(2) 182_455 2_565 ?
O2 Zr1 O1B 141.10(7) 181 2_565 ?
O2 Zr1 O1B 73.0(2) 2_565 2_565 ?
O1B Zr1 O1B 122.0(6) . 2_565 ?
O1B Zr1 O1B 76.4(2) 100 2_565 ?
O1B Zr1 O1B 76.4(2) 99_565 2_565 ?
Zr1 O1 Zr1 116.87(19) . 177 ?
Zr1 O1 Zr1 116.87(19) . 29_554 ?
Zr1 O1 Zr1 116.87(19) 177 29_554 ?
Zr1 O1B Zr1 102.5(3) . 29_554 ?
Zr1 O1B Zr1 102.5(3) . 177 ?
Zr1 O1B Zr1 102.5(3) 29_554 177 ?
Zr1 O1B H1B 115.7 . . ?
Zr1 O1B H1B 115.7 29_554 . ?
Zr1 O1B H1B 115.7 177 . ?
C1 O2 Zr1 130.0(5) . . ?
O2 C1 O2 129.8(9) 22_565 . ?
O2 C1 C2 115.1(4) 22_565 . ?
O2 C1 C2 115.1(4) . . ?
C3 C2 C3 123.1(14) . 22_565 ?
C3 C2 C1 118.4(7) . . ?
C3 C2 C1 118.4(7) 22_565 . ?
C4 C3 C2 117.5(14) . . ?
C4 C3 H3 121.2 . . ?
C2 C3 H3 121.2 . . ?
C3 C4 C5 122.0(16) . . ?
C3 C4 H4 119.0 . . ?
C5 C4 H4 119.0 . . ?
C4 C5 C4 117.8(17) 22_565 . ?
C4 C5 C6 121.1(9) 22_565 . ?
C4 C5 C6 121.1(9) . . ?
C7 C6 C5 117.6(8) . . ?
C7 C6 C8 123.1(16) . 145_565 ?
C5 C6 C8 119.3(10) . 145_565 ?
C6 C7 C8 122.8(12) . . ?
C6 C7 S1 135.2(9) . . ?
C8 C7 S1 102.1(11) . . ?
C7 C8 C6 114.1(17) . 51 ?
C7 C8 H8 123.0 . . ?
C6 C8 H8 123.0 51 . ?
C7 S1 H1 106.1 . . ?

_refine_diff_density_max         1.721
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.149

_shelxl_version_number           2013-4

# start Validation Reply Form
_vrf_PLAT222_I                   
;
PROBLEM: Large Non-Solvent    H    Uiso(max)/Uiso(min) ..       10.0 Ratio 
RESPONSE: Large differences are observed between thermal parameters of atoms 
carrying hydrigen atoms due to the coexistance of rigid well defined sections 
with areas with large libration. 
;
_vrf_PLAT601_I                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of .      21809 Ang3  
RESPONSE: No substantial electron density has been found in the void areas 
of the structure. 
;
# end Validation Reply Form



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: 1:1 DMF/DEF'
_chemical_properties_physical    'sensitive to solvent loss'
_exptl_crystal_preparation       'BET surface area'
