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

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

data_TPPZrX
_database_code_depnum_ccdc_archive 'CCDC 2015704'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2020-07-12 deposited with the CCDC.	2020-08-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'Tetraphenylporphyrin-(9,9-dimethylxanthene-4,5-bis(iminium)bis(4,6-ditertbutylcatecholato))zirconium(IV) hepta-tetrahydrofuran solvate'
_chemical_name_common            (TPP)Zr(XbicH2).7(THF)
_chemical_melting_point          .
_chemical_formula_moiety         'C89 H82 N6 O5 Zr, 7(C4 H8 O)'
_chemical_formula_sum            'C117 H138 N6 O12 Zr'
_chemical_formula_weight         1911.55

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   20.745(3)
_cell_length_b                   17.732(2)
_cell_length_c                   28.218(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.6014(18)
_cell_angle_gamma                90
_cell_volume                     9838(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9307
_cell_measurement_theta_min      2.277
_cell_measurement_theta_max      28.353

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_F_000             4072
_exptl_transmission_factor_min   0.674300
_exptl_transmission_factor_max   0.745700
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.192
_exptl_absorpt_coefficient_mu    0.179
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6743
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;
_exptl_crystal_recrystallization_method 
;
Crystals deposited from THF at room temperature after 5 days. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans '
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            326985
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.378
_diffrn_reflns_theta_max         28.453
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             24610
_reflns_number_gt                19848
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;
One tetrahydrofuran of crystallization was found to be  
disordered. The carbons were treated with 
SIMU to take into account the different vibration motions. 
The molecule was modeled with the carbon atoms refined with occupancies 
summed to unity yielding an approximately 0.65:0.35 ratio.

The hydrogen atoms on lattice tetrahydrofuran were placed in calculated
positions. All other hydrogens were found on the difference map and 
refined isotropically.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0415P)²+11.7298P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         24610
_refine_ls_number_parameters     1563
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0469
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.1024
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.002
_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
Zr Zr 0.27999(2) 0.29897(2) 0.58631(2) 0.00881(4) Uani 1 1 d . . . . .
O1 O 0.34871(6) 0.23287(7) 0.56128(4) 0.0134(2) Uani 1 1 d . . . . .
O2 O 0.36721(6) 0.37080(7) 0.58233(4) 0.0117(2) Uani 1 1 d . . . . .
O3 O 0.21865(6) 0.25571(7) 0.51557(4) 0.0121(2) Uani 1 1 d . . . . .
O4 O 0.23878(6) 0.39582(7) 0.53363(4) 0.0118(2) Uani 1 1 d . . . . .
O5 O 0.33509(6) 0.59647(7) 0.56992(4) 0.0132(2) Uani 1 1 d . . . . .
N1 N 0.43669(7) 0.49481(8) 0.59839(5) 0.0126(3) Uani 1 1 d . . . . .
H1 H 0.3972(12) 0.4712(13) 0.5942(8) 0.020(6) Uiso 1 1 d . . . . .
N2 N 0.22068(7) 0.53762(9) 0.50866(6) 0.0134(3) Uani 1 1 d . . . . .
H2 H 0.2398(12) 0.5037(14) 0.5296(9) 0.025(6) Uiso 1 1 d . . . . .
N3 N 0.24917(7) 0.17964(8) 0.60656(5) 0.0117(3) Uani 1 1 d . . . . .
N4 N 0.16774(7) 0.31383(8) 0.59048(5) 0.0120(3) Uani 1 1 d . . . . .
N5 N 0.28683(7) 0.40140(8) 0.64127(5) 0.0113(3) Uani 1 1 d . . . . .
N6 N 0.36563(7) 0.26623(8) 0.66216(5) 0.0121(3) Uani 1 1 d . . . . .
C11 C 0.40856(8) 0.25900(10) 0.56129(6) 0.0129(3) Uani 1 1 d . . . . .
C12 C 0.41870(8) 0.33778(10) 0.57392(6) 0.0119(3) Uani 1 1 d . . . . .
C13 C 0.47966(8) 0.37752(10) 0.57588(6) 0.0131(3) Uani 1 1 d . . . . .
C14 C 0.53268(8) 0.33596(11) 0.56327(6) 0.0152(3) Uani 1 1 d . . . . .
C15 C 0.51916(9) 0.26218(11) 0.54997(7) 0.0171(4) Uani 1 1 d . . . . .
H15 H 0.5512(10) 0.2360(12) 0.5403(7) 0.012(5) Uiso 1 1 d . . . . .
C16 C 0.45882(9) 0.22107(10) 0.54775(6) 0.0151(3) Uani 1 1 d . . . . .
C17 C 0.45387(10) 0.14009(11) 0.52712(7) 0.0200(4) Uani 1 1 d . . . . .
C171 C 0.39229(10) 0.09560(12) 0.53078(9) 0.0257(4) Uani 1 1 d . . . . .
H17A H 0.3497(13) 0.1188(15) 0.5109(10) 0.036(7) Uiso 1 1 d . . . . .
H17B H 0.3961(13) 0.0437(15) 0.5171(10) 0.038(7) Uiso 1 1 d . . . . .
H17C H 0.3909(13) 0.0911(15) 0.5666(10) 0.039(7) Uiso 1 1 d . . . . .
C172 C 0.51826(11) 0.09516(13) 0.55463(11) 0.0317(5) Uani 1 1 d . . . . .
H17D H 0.5271(13) 0.0966(15) 0.5914(10) 0.036(7) Uiso 1 1 d . . . . .
H17E H 0.5132(13) 0.0429(16) 0.5446(9) 0.035(7) Uiso 1 1 d . . . . .
H17F H 0.5590(14) 0.1145(15) 0.5471(10) 0.041(7) Uiso 1 1 d . . . . .
C173 C 0.44854(17) 0.14513(15) 0.47158(9) 0.0401(6) Uani 1 1 d . . . . .
H17G H 0.4048(17) 0.1742(19) 0.4523(12) 0.061(9) Uiso 1 1 d . . . . .
H17H H 0.4880(17) 0.1691(19) 0.4663(12) 0.062(10) Uiso 1 1 d . . . . .
H17I H 0.4462(14) 0.0945(17) 0.4573(10) 0.047(8) Uiso 1 1 d . . . . .
C18 C 0.60047(9) 0.37199(11) 0.56313(7) 0.0193(4) Uani 1 1 d . . . . .
C181 C 0.64581(11) 0.31512(14) 0.54728(10) 0.0289(5) Uani 1 1 d . . . . .
H18A H 0.6573(12) 0.2730(14) 0.5695(9) 0.025(6) Uiso 1 1 d . . . . .
H18B H 0.6235(12) 0.2957(14) 0.5121(9) 0.028(6) Uiso 1 1 d . . . . .
H18C H 0.6877(13) 0.3404(14) 0.5492(9) 0.033(7) Uiso 1 1 d . . . . .
C182 C 0.58744(11) 0.43650(13) 0.52453(8) 0.0235(4) Uani 1 1 d . . . . .
H18D H 0.5583(12) 0.4771(14) 0.5294(8) 0.025(6) Uiso 1 1 d . . . . .
H18E H 0.6291(12) 0.4586(14) 0.5249(9) 0.028(6) Uiso 1 1 d . . . . .
H18F H 0.5645(12) 0.4157(13) 0.4911(9) 0.026(6) Uiso 1 1 d . . . . .
C183 C 0.64241(10) 0.39878(13) 0.61607(8) 0.0240(4) Uani 1 1 d . . . . .
H18G H 0.6191(12) 0.4358(14) 0.6310(9) 0.026(6) Uiso 1 1 d . . . . .
H18H H 0.6849(14) 0.4217(15) 0.6155(10) 0.039(7) Uiso 1 1 d . . . . .
H18I H 0.6535(13) 0.3575(15) 0.6394(10) 0.034(7) Uiso 1 1 d . . . . .
C19 C 0.48531(8) 0.45431(10) 0.58968(6) 0.0129(3) Uani 1 1 d . . . . .
H19 H 0.5246(10) 0.4806(11) 0.5931(7) 0.010(5) Uiso 1 1 d . . . . .
C21 C 0.19038(8) 0.30070(10) 0.47729(6) 0.0113(3) Uani 1 1 d . . . . .
C22 C 0.20047(8) 0.37926(10) 0.48824(6) 0.0108(3) Uani 1 1 d . . . . .
C23 C 0.17295(8) 0.43592(10) 0.45085(6) 0.0118(3) Uani 1 1 d . . . . .
C24 C 0.13443(8) 0.41226(10) 0.40042(6) 0.0127(3) Uani 1 1 d . . . . .
C25 C 0.12823(8) 0.33606(10) 0.39207(6) 0.0132(3) Uani 1 1 d . . . . .
H25 H 0.1045(10) 0.3194(12) 0.3605(8) 0.015(5) Uiso 1 1 d . . . . .
C26 C 0.15639(8) 0.27871(10) 0.42810(6) 0.0121(3) Uani 1 1 d . . . . .
C27 C 0.15148(9) 0.19547(10) 0.41240(6) 0.0147(3) Uani 1 1 d . . . . .
C271 C 0.22355(11) 0.16203(12) 0.42694(9) 0.0247(4) Uani 1 1 d . . . . .
H27A H 0.2206(12) 0.1091(15) 0.4161(9) 0.031(6) Uiso 1 1 d . . . . .
H27B H 0.2500(14) 0.1880(15) 0.4075(10) 0.041(7) Uiso 1 1 d . . . . .
H27C H 0.2482(14) 0.1644(16) 0.4630(11) 0.046(8) Uiso 1 1 d . . . . .
C272 C 0.11821(13) 0.18439(12) 0.35594(8) 0.0283(5) Uani 1 1 d . . . . .
H27D H 0.0697(14) 0.2028(15) 0.3446(10) 0.039(7) Uiso 1 1 d . . . . .
H27E H 0.1444(14) 0.2121(16) 0.3358(10) 0.042(7) Uiso 1 1 d . . . . .
H27F H 0.1197(12) 0.1293(15) 0.3481(9) 0.033(7) Uiso 1 1 d . . . . .
C273 C 0.10970(11) 0.15240(13) 0.43927(8) 0.0251(4) Uani 1 1 d . . . . .
H27G H 0.1311(13) 0.1550(14) 0.4763(10) 0.035(7) Uiso 1 1 d . . . . .
H27H H 0.0598(14) 0.1726(15) 0.4273(10) 0.038(7) Uiso 1 1 d . . . . .
H27I H 0.1085(13) 0.0982(16) 0.4295(10) 0.039(7) Uiso 1 1 d . . . . .
C28 C 0.10329(9) 0.46867(10) 0.35756(6) 0.0152(3) Uani 1 1 d . . . . .
C281 C 0.06439(11) 0.42653(12) 0.30914(7) 0.0234(4) Uani 1 1 d . . . . .
H28A H 0.0941(11) 0.3960(13) 0.2983(8) 0.021(6) Uiso 1 1 d . . . . .
H28B H 0.0456(13) 0.4630(15) 0.2837(10) 0.035(7) Uiso 1 1 d . . . . .
H28C H 0.0257(12) 0.3959(14) 0.3130(9) 0.025(6) Uiso 1 1 d . . . . .
C282 C 0.05054(10) 0.52092(11) 0.36898(7) 0.0185(4) Uani 1 1 d . . . . .
H28D H 0.0260(13) 0.5482(15) 0.3394(10) 0.035(7) Uiso 1 1 d . . . . .
H28E H 0.0695(12) 0.5580(14) 0.3950(9) 0.031(6) Uiso 1 1 d . . . . .
H28F H 0.0191(13) 0.4936(15) 0.3796(9) 0.034(7) Uiso 1 1 d . . . . .
C283 C 0.15857(11) 0.51525(12) 0.34522(8) 0.0224(4) Uani 1 1 d . . . . .
H28G H 0.1875(11) 0.5438(13) 0.3732(8) 0.021(6) Uiso 1 1 d . . . . .
H28H H 0.1880(12) 0.4838(13) 0.3343(8) 0.024(6) Uiso 1 1 d . . . . .
H28I H 0.1367(12) 0.5505(14) 0.3184(9) 0.031(6) Uiso 1 1 d . . . . .
C29 C 0.18422(8) 0.51201(10) 0.46408(6) 0.0132(3) Uani 1 1 d . . . . .
H29 H 0.1651(10) 0.5505(12) 0.4410(8) 0.015(5) Uiso 1 1 d . . . . .
C31 C 0.44703(9) 0.56872(10) 0.61894(6) 0.0133(3) Uani 1 1 d . . . . .
C32 C 0.39451(9) 0.62187(10) 0.60448(6) 0.0133(3) Uani 1 1 d . . . . .
C33 C 0.40247(9) 0.69443(10) 0.62438(6) 0.0157(3) Uani 1 1 d . . . . .
C34 C 0.46505(10) 0.71254(11) 0.65969(7) 0.0215(4) Uani 1 1 d . . . . .
H34 H 0.4713(10) 0.7626(13) 0.6739(8) 0.017(5) Uiso 1 1 d . . . . .
C35 C 0.51712(10) 0.66022(12) 0.67482(7) 0.0231(4) Uani 1 1 d . . . . .
H35 H 0.5578(11) 0.6726(13) 0.6996(8) 0.021(6) Uiso 1 1 d . . . . .
C36 C 0.50814(9) 0.58821(11) 0.65466(7) 0.0179(4) Uani 1 1 d . . . . .
H36 H 0.5414(11) 0.5507(13) 0.6657(8) 0.023(6) Uiso 1 1 d . . . . .
C41 C 0.22151(9) 0.61493(10) 0.52149(6) 0.0138(3) Uani 1 1 d . . . . .
C42 C 0.16465(10) 0.66023(11) 0.50194(7) 0.0197(4) Uani 1 1 d . . . . .
H42 H 0.1235(12) 0.6380(13) 0.4792(9) 0.026(6) Uiso 1 1 d . . . . .
C43 C 0.16690(10) 0.73559(11) 0.51586(8) 0.0232(4) Uani 1 1 d . . . . .
H43 H 0.1279(12) 0.7651(14) 0.5040(9) 0.026(6) Uiso 1 1 d . . . . .
C44 C 0.22509(10) 0.76445(11) 0.55023(7) 0.0208(4) Uani 1 1 d . . . . .
H44 H 0.2244(11) 0.8158(13) 0.5608(8) 0.021(6) Uiso 1 1 d . . . . .
C45 C 0.28328(9) 0.72038(10) 0.57047(7) 0.0154(3) Uani 1 1 d . . . . .
C46 C 0.28084(9) 0.64573(10) 0.55494(6) 0.0133(3) Uani 1 1 d . . . . .
C51 C 0.29446(9) 0.12049(10) 0.62136(6) 0.0129(3) Uani 1 1 d . . . . .
C52 C 0.26164(9) 0.05018(10) 0.60286(7) 0.0152(3) Uani 1 1 d . . . . .
H52 H 0.2841(10) 0.0022(12) 0.6084(8) 0.016(5) Uiso 1 1 d . . . . .
C53 C 0.19497(9) 0.06593(10) 0.57978(7) 0.0150(3) Uani 1 1 d . . . . .
H53 H 0.1587(11) 0.0318(12) 0.5650(8) 0.018(5) Uiso 1 1 d . . . . .
C54 C 0.18669(8) 0.14613(10) 0.58395(6) 0.0121(3) Uani 1 1 d . . . . .
C61 C 0.11619(8) 0.26095(10) 0.57752(6) 0.0129(3) Uani 1 1 d . . . . .
C62 C 0.05200(9) 0.29620(11) 0.57349(7) 0.0172(4) Uani 1 1 d . . . . .
H62 H 0.0092(11) 0.2694(12) 0.5667(8) 0.018(5) Uiso 1 1 d . . . . .
C63 C 0.06453(9) 0.37029(11) 0.58331(7) 0.0175(4) Uani 1 1 d . . . . .
H63 H 0.0339(11) 0.4083(13) 0.5849(8) 0.020(5) Uiso 1 1 d . . . . .
C64 C 0.13688(8) 0.38133(10) 0.59405(6) 0.0131(3) Uani 1 1 d . . . . .
C71 C 0.23972(8) 0.45937(10) 0.63157(6) 0.0117(3) Uani 1 1 d . . . . .
C72 C 0.27270(9) 0.52954(10) 0.65130(6) 0.0140(3) Uani 1 1 d . . . . .
H72 H 0.2510(11) 0.5754(13) 0.6487(8) 0.017(5) Uiso 1 1 d . . . . .
C73 C 0.33894(9) 0.51365(10) 0.67530(6) 0.0136(3) Uani 1 1 d . . . . .
H73 H 0.3745(11) 0.5497(12) 0.6937(8) 0.019(5) Uiso 1 1 d . . . . .
C74 C 0.34765(8) 0.43364(10) 0.67032(6) 0.0120(3) Uani 1 1 d . . . . .
C81 C 0.41232(8) 0.31455(10) 0.69315(6) 0.0135(3) Uani 1 1 d . . . . .
C82 C 0.46675(9) 0.27204(11) 0.72764(7) 0.0175(4) Uani 1 1 d . . . . .
H82 H 0.5024(11) 0.2933(13) 0.7540(8) 0.022(6) Uiso 1 1 d . . . . .
C83 C 0.45319(9) 0.19838(11) 0.71715(7) 0.0179(4) Uani 1 1 d . . . . .
H83 H 0.4782(11) 0.1569(13) 0.7328(8) 0.023(6) Uiso 1 1 d . . . . .
C84 C 0.39045(8) 0.19470(10) 0.67597(6) 0.0140(3) Uani 1 1 d . . . . .
C91 C 0.39708(9) 0.05510(11) 0.67656(7) 0.0194(4) Uani 1 1 d . . . . .
C92 C 0.37524(12) 0.01098(13) 0.70874(9) 0.0340(5) Uani 1 1 d . . . . .
H92 H 0.3392(13) 0.0261(14) 0.7181(9) 0.029(7) Uiso 1 1 d . . . . .
C93 C 0.41099(16) -0.05425(14) 0.72996(12) 0.0515(9) Uani 1 1 d . . . . .
H93 H 0.3958(16) -0.0772(19) 0.7524(12) 0.060(10) Uiso 1 1 d . . . . .
C94 C 0.46794(16) -0.07508(14) 0.71931(11) 0.0540(9) Uani 1 1 d . . . . .
H94 H 0.4935(16) -0.1190(18) 0.7335(12) 0.060(9) Uiso 1 1 d . . . . .
C95 C 0.49058(16) -0.03193(18) 0.68752(10) 0.0551(9) Uani 1 1 d . . . . .
H95 H 0.531(2) -0.048(2) 0.6784(14) 0.089(12) Uiso 1 1 d . . . . .
C96 C 0.45586(13) 0.03370(16) 0.66627(9) 0.0384(6) Uani 1 1 d . . . . .
H96 H 0.4714(15) 0.0653(18) 0.6427(12) 0.058(9) Uiso 1 1 d . . . . .
C101 C 0.06093(8) 0.13509(10) 0.55800(7) 0.0135(3) Uani 1 1 d . . . . .
C102 C 0.00834(9) 0.14503(11) 0.51288(7) 0.0155(3) Uani 1 1 d . . . . .
H102 H 0.0118(11) 0.1822(13) 0.4897(8) 0.021(6) Uiso 1 1 d . . . . .
C103 C -0.04869(9) 0.09839(11) 0.50004(7) 0.0181(4) Uani 1 1 d . . . . .
H103 H -0.0832(11) 0.1057(12) 0.4688(8) 0.017(5) Uiso 1 1 d . . . . .
C104 C -0.05438(9) 0.04197(11) 0.53245(7) 0.0194(4) Uani 1 1 d . . . . .
H104 H -0.0929(12) 0.0094(13) 0.5230(8) 0.023(6) Uiso 1 1 d . . . . .
C105 C -0.00365(10) 0.03293(11) 0.57822(7) 0.0203(4) Uani 1 1 d . . . . .
H105 H -0.0083(12) -0.0049(14) 0.6009(9) 0.028(6) Uiso 1 1 d . . . . .
C106 C 0.05331(9) 0.07922(11) 0.59094(7) 0.0172(4) Uani 1 1 d . . . . .
H106 H 0.0862(11) 0.0740(13) 0.6226(9) 0.023(6) Uiso 1 1 d . . . . .
C111 C 0.12494(9) 0.51860(10) 0.60537(7) 0.0163(4) Uani 1 1 d . . . . .
C112 C 0.08003(10) 0.54096(12) 0.55915(8) 0.0231(4) Uani 1 1 d . . . . .
H112 H 0.0777(12) 0.5128(13) 0.5294(9) 0.026(6) Uiso 1 1 d . . . . .
C113 C 0.03765(11) 0.60349(13) 0.55558(10) 0.0333(5) Uani 1 1 d . . . . .
H113 H 0.0082(13) 0.6178(14) 0.5245(9) 0.032(7) Uiso 1 1 d . . . . .
C114 C 0.04004(11) 0.64437(13) 0.59787(11) 0.0365(6) Uani 1 1 d . . . . .
H114 H 0.0092(14) 0.6868(16) 0.5952(10) 0.043(8) Uiso 1 1 d . . . . .
C115 C 0.08414(11) 0.62274(12) 0.64380(10) 0.0326(5) Uani 1 1 d . . . . .
H115 H 0.0853(13) 0.6494(15) 0.6734(10) 0.036(7) Uiso 1 1 d . . . . .
C116 C 0.12592(10) 0.56001(12) 0.64778(8) 0.0227(4) Uani 1 1 d . . . . .
H116 H 0.1554(11) 0.5445(12) 0.6798(8) 0.018(5) Uiso 1 1 d . . . . .
C121 C 0.47043(9) 0.43431(10) 0.72443(6) 0.0150(3) Uani 1 1 d . . . . .
C122 C 0.47150(10) 0.48567(11) 0.76246(7) 0.0192(4) Uani 1 1 d . . . . .
H122 H 0.4300(11) 0.4950(12) 0.7693(8) 0.015(5) Uiso 1 1 d . . . . .
C123 C 0.53217(11) 0.52043(12) 0.79014(7) 0.0250(4) Uani 1 1 d . . . . .
H123 H 0.5312(12) 0.5551(14) 0.8157(9) 0.027(6) Uiso 1 1 d . . . . .
C124 C 0.59256(10) 0.50432(12) 0.78091(8) 0.0263(5) Uani 1 1 d . . . . .
H124 H 0.6335(13) 0.5271(14) 0.8004(9) 0.034(7) Uiso 1 1 d . . . . .
C125 C 0.59235(10) 0.45337(12) 0.74362(7) 0.0230(4) Uani 1 1 d . . . . .
H125 H 0.6329(12) 0.4411(13) 0.7362(9) 0.026(6) Uiso 1 1 d . . . . .
C126 C 0.53190(9) 0.41889(11) 0.71554(7) 0.0177(4) Uani 1 1 d . . . . .
H126 H 0.5320(11) 0.3866(13) 0.6908(8) 0.020(6) Uiso 1 1 d . . . . .
C1 C 0.34581(9) 0.75297(10) 0.60954(7) 0.0166(4) Uani 1 1 d . . . . .
C2 C 0.37047(11) 0.82376(12) 0.58876(9) 0.0259(4) Uani 1 1 d . . . . .
H2A H 0.3347(12) 0.8624(14) 0.5780(9) 0.028(6) Uiso 1 1 d . . . . .
H2B H 0.3837(12) 0.8118(14) 0.5590(10) 0.031(6) Uiso 1 1 d . . . . .
H2C H 0.4104(13) 0.8452(14) 0.6144(9) 0.033(7) Uiso 1 1 d . . . . .
C3 C 0.32581(11) 0.77435(13) 0.65606(8) 0.0256(4) Uani 1 1 d . . . . .
C4 C 0.12378(8) 0.18306(10) 0.57197(6) 0.0129(3) Uani 1 1 d . . . . .
H3A H 0.2909(13) 0.8116(14) 0.6474(9) 0.029(6) Uiso 1 1 d . . . . .
H3B H 0.3654(12) 0.7964(14) 0.6814(9) 0.029(6) Uiso 1 1 d . . . . .
H3C H 0.3103(12) 0.7295(15) 0.6700(9) 0.030(6) Uiso 1 1 d . . . . .
C5 C 0.16923(8) 0.45074(10) 0.60931(6) 0.0132(3) Uani 1 1 d . . . . .
C6 C 0.40748(8) 0.39350(10) 0.69424(6) 0.0127(3) Uani 1 1 d . . . . .
C7 C 0.36010(9) 0.12658(10) 0.65549(6) 0.0141(3) Uani 1 1 d . . . . .
O6 O 0.64313(9) 0.38853(12) 0.21710(7) 0.0498(5) Uani 1 1 d . . . . .
C1S C 0.71272(12) 0.38885(14) 0.22041(8) 0.0323(5) Uani 1 1 d . . . . .
H1S H 0.7376 0.4283 0.2440 0.039 Uiso 1 1 calc R U . . .
H1' H 0.7176 0.3991 0.1872 0.039 Uiso 1 1 calc R U . . .
C2S C 0.74058(12) 0.31165(14) 0.23884(9) 0.0355(5) Uani 1 1 d . . . . .
H2S H 0.7553 0.3087 0.2758 0.043 Uiso 1 1 calc R U . . .
H2' H 0.7793 0.2982 0.2271 0.043 Uiso 1 1 calc R U . . .
C3S C 0.67939(15) 0.26126(17) 0.21519(9) 0.0462(7) Uani 1 1 d . . . . .
H3S H 0.6791 0.2431 0.1819 0.055 Uiso 1 1 calc R U . . .
H3' H 0.6793 0.2172 0.2367 0.055 Uiso 1 1 calc R U . . .
C4S C 0.61918(13) 0.31231(19) 0.21070(10) 0.0505(8) Uani 1 1 d . . . . .
H4S H 0.5845 0.3061 0.1774 0.061 Uiso 1 1 calc R U . . .
H4' H 0.5982 0.2993 0.2366 0.061 Uiso 1 1 calc R U . . .
O7 O 0.66651(8) 0.61985(9) 0.12343(5) 0.0308(3) Uani 1 1 d . . . . .
C5S C 0.68837(12) 0.57642(13) 0.16858(8) 0.0301(5) Uani 1 1 d . . . . .
H5S H 0.7374 0.5643 0.1774 0.036 Uiso 1 1 calc R U . . .
H5' H 0.6625 0.5286 0.1644 0.036 Uiso 1 1 calc R U . . .
C6S C 0.67547(14) 0.62360(15) 0.20856(9) 0.0392(6) Uani 1 1 d . . . . .
H6S H 0.7143 0.6575 0.2244 0.047 Uiso 1 1 calc R U . . .
H6' H 0.6663 0.5919 0.2346 0.047 Uiso 1 1 calc R U . . .
C7S C 0.61279(16) 0.66766(16) 0.17903(11) 0.0483(7) Uani 1 1 d . . . . .
H7S H 0.5708 0.6375 0.1735 0.058 Uiso 1 1 calc R U . . .
H7' H 0.6087 0.7154 0.1961 0.058 Uiso 1 1 calc R U . . .
C8S C 0.62678(14) 0.68222(15) 0.13088(10) 0.0413(6) Uani 1 1 d . . . . .
H8S H 0.5836 0.6859 0.1028 0.050 Uiso 1 1 calc R U . . .
H8' H 0.6522 0.7300 0.1329 0.050 Uiso 1 1 calc R U . . .
O8 O 0.77451(9) 0.06280(12) 0.61683(6) 0.0469(5) Uani 1 1 d . . . . .
C9S C 0.81635(12) 0.06067(14) 0.58541(9) 0.0350(5) Uani 1 1 d . . . . .
H9S H 0.8461 0.0157 0.5930 0.042 Uiso 1 1 calc R U . . .
H9' H 0.8453 0.1063 0.5905 0.042 Uiso 1 1 calc R U . . .
C10S C 0.76850(13) 0.05749(15) 0.53213(9) 0.0373(5) Uani 1 1 d . . . . .
H10S H 0.7881 0.0834 0.5089 0.045 Uiso 1 1 calc R U . . .
H10' H 0.7576 0.0048 0.5209 0.045 Uiso 1 1 calc R U . . .
C11S C 0.70600(13) 0.0767(2) 0.58719(10) 0.0571(9) Uani 1 1 d . . . . .
H11S H 0.6865 0.1179 0.6020 0.069 Uiso 1 1 calc R U . . .
H11' H 0.6781 0.0308 0.5854 0.069 Uiso 1 1 calc R U . . .
C12S C 0.70633(12) 0.09857(16) 0.53589(9) 0.0384(6) Uani 1 1 d . . . . .
H12S H 0.7109 0.1538 0.5330 0.046 Uiso 1 1 calc R U . . .
H12' H 0.6645 0.0813 0.5098 0.046 Uiso 1 1 calc R U . . .
O9 O 0.3619(2) 0.8794(2) 0.30561(14) 0.1277(13) Uani 1 1 d . . . . .
C13S C 0.3514(4) 0.7612(4) 0.2737(2) 0.059(2) Uani 0.644(13) 1 d . U P A 1
H13A H 0.3438 0.7076 0.2802 0.070 Uiso 0.644(13) 1 calc R U P A 1
H13B H 0.3812 0.7634 0.2524 0.070 Uiso 0.644(13) 1 calc R U P A 1
C13T C 0.3164(6) 0.7467(5) 0.2883(4) 0.053(3) Uani 0.356(13) 1 d . U P A 2
H13C H 0.3306 0.6992 0.2761 0.063 Uiso 0.356(13) 1 calc R U P A 2
H13D H 0.2861 0.7355 0.3083 0.063 Uiso 0.356(13) 1 calc R U P A 2
C14S C 0.3819(2) 0.7996(2) 0.31899(15) 0.0804(12) Uani 1 1 d . . . . .
H14A H 0.4320 0.7937 0.3303 0.096 Uiso 0.644(13) 1 calc R U P A 1
H14B H 0.3641 0.7814 0.3456 0.096 Uiso 0.644(13) 1 calc R U P A 1
H14C H 0.3930 0.7920 0.3555 0.096 Uiso 0.356(13) 1 calc R U P A 2
H14D H 0.4223 0.7864 0.3093 0.096 Uiso 0.356(13) 1 calc R U P A 2
C15S C 0.2907(2) 0.8710(3) 0.26834(18) 0.0934(14) Uani 1 1 d . . . . .
H15S H 0.2560 0.8782 0.2852 0.112 Uiso 1 1 calc R U . . .
H15' H 0.2830 0.9089 0.2414 0.112 Uiso 1 1 calc R U . . .
C16S C 0.2866(2) 0.7984(2) 0.24874(15) 0.0821(12) Uani 1 1 d . . . . .
H16A H 0.2782 0.8006 0.2122 0.099 Uiso 0.644(13) 1 calc R U P A 1
H16B H 0.2488 0.7703 0.2549 0.099 Uiso 0.644(13) 1 calc R U P A 1
H16C H 0.3108 0.7962 0.2237 0.099 Uiso 0.356(13) 1 calc R U P A 2
H16D H 0.2384 0.7849 0.2319 0.099 Uiso 0.356(13) 1 calc R U P A 2
O10 O 0.39384(7) 0.41798(9) 0.40161(5) 0.0274(3) Uani 1 1 d . . . . .
C17S C 0.40739(11) 0.36102(13) 0.43938(8) 0.0294(5) Uani 1 1 d . . . . .
H17S H 0.4353 0.3814 0.4722 0.035 Uiso 1 1 calc R U . . .
H17' H 0.4316 0.3178 0.4306 0.035 Uiso 1 1 calc R U . . .
C18S C 0.33798(12) 0.33769(15) 0.44058(9) 0.0348(5) Uani 1 1 d . . . . .
H18S H 0.3207 0.3730 0.4609 0.042 Uiso 1 1 calc R U . . .
H18' H 0.3387 0.2860 0.4540 0.042 Uiso 1 1 calc R U . . .
C19S C 0.29557(11) 0.34155(16) 0.38569(9) 0.0387(6) Uani 1 1 d . . . . .
H19S H 0.2913 0.2911 0.3700 0.046 Uiso 1 1 calc R U . . .
H19' H 0.2495 0.3613 0.3817 0.046 Uiso 1 1 calc R U . . .
C20S C 0.33413(11) 0.39484(14) 0.36246(8) 0.0313(5) Uani 1 1 d . . . . .
H20S H 0.3468 0.3690 0.3356 0.038 Uiso 1 1 calc R U . . .
H20' H 0.3057 0.4391 0.3479 0.038 Uiso 1 1 calc R U . . .
O11 O 0.1214(2) 0.7011(2) 0.38203(11) 0.1208(13) Uani 1 1 d . . . . .
C21S C 0.0738(2) 0.7535(2) 0.30585(14) 0.0773(11) Uani 1 1 d . . . . .
H21S H 0.0442 0.7956 0.2886 0.093 Uiso 1 1 calc R U . . .
H21' H 0.0636 0.7086 0.2839 0.093 Uiso 1 1 calc R U . . .
C22S C 0.1448(2) 0.7741(2) 0.31844(19) 0.0876(14) Uani 1 1 d . . . . .
H22S H 0.1514 0.8292 0.3236 0.105 Uiso 1 1 calc R U . . .
H22' H 0.1642 0.7577 0.2923 0.105 Uiso 1 1 calc R U . . .
C23S C 0.0638(2) 0.7376(2) 0.35250(16) 0.0751(11) Uani 1 1 d . . . . .
H23S H 0.0567 0.7850 0.3687 0.090 Uiso 1 1 calc R U . . .
H23' H 0.0233 0.7051 0.3473 0.090 Uiso 1 1 calc R U . . .
C24S C 0.1758(2) 0.7313(2) 0.3666(3) 0.136(3) Uani 1 1 d . . . . .
H24S H 0.2049 0.6899 0.3614 0.164 Uiso 1 1 calc R U . . .
H24' H 0.2044 0.7654 0.3927 0.164 Uiso 1 1 calc R U . . .
O12 O 0.3633(2) 0.1503(3) 0.28295(19) 0.1353(17) Uani 1 1 d . . . . .
C25S C 0.3763(3) 0.1594(2) 0.3340(2) 0.1038(18) Uani 1 1 d . . . . .
H25S H 0.3597 0.2092 0.3412 0.125 Uiso 1 1 calc R U . . .
H25' H 0.4257 0.1560 0.3520 0.125 Uiso 1 1 calc R U . . .
C26S C 0.34058(16) 0.0996(2) 0.34954(13) 0.0660(10) Uani 1 1 d . . . . .
H26S H 0.3293 0.1142 0.3798 0.079 Uiso 1 1 calc R U . . .
H26' H 0.3683 0.0530 0.3567 0.079 Uiso 1 1 calc R U . . .
C27S C 0.27799(17) 0.0885(3) 0.30650(12) 0.0719(10) Uani 1 1 d . . . . .
H27S H 0.2592 0.0372 0.3065 0.086 Uiso 1 1 calc R U . . .
H27' H 0.2428 0.1262 0.3064 0.086 Uiso 1 1 calc R U . . .
C28S C 0.3035(3) 0.0994(4) 0.26390(16) 0.122(2) Uani 1 1 d . . . . .
H28S H 0.2682 0.1227 0.2354 0.146 Uiso 1 1 calc R U . . .
H28' H 0.3172 0.0506 0.2529 0.146 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr O1 2.1324(12) . ?
Zr O3 2.1381(12) . ?
Zr O2 2.2448(12) . ?
Zr O4 2.2537(12) . ?
Zr N3 2.3335(15) . ?
Zr N5 2.3631(15) . ?
Zr N6 2.3768(14) . ?
Zr N4 2.3834(14) . ?
O1 C11 1.325(2) . ?
O2 C12 1.305(2) . ?
O3 C21 1.320(2) . ?
O4 C22 1.3072(19) . ?
O5 C46 1.380(2) . ?
O5 C32 1.381(2) . ?
N1 C19 1.323(2) . ?
N1 C31 1.422(2) . ?
N1 H1 0.89(2) . ?
N2 C29 1.324(2) . ?
N2 C41 1.417(2) . ?
N2 H2 0.85(2) . ?
N3 C51 1.381(2) . ?
N3 C54 1.383(2) . ?
N4 C64 1.376(2) . ?
N4 C61 1.381(2) . ?
N5 C71 1.384(2) . ?
N5 C74 1.390(2) . ?
N6 C81 1.377(2) . ?
N6 C84 1.377(2) . ?
C11 C16 1.393(2) . ?
C11 C12 1.440(2) . ?
C12 C13 1.433(2) . ?
C13 C19 1.411(3) . ?
C13 C14 1.459(2) . ?
C14 C15 1.365(3) . ?
C14 C18 1.546(2) . ?
C15 C16 1.433(3) . ?
C15 H15 0.92(2) . ?
C16 C17 1.541(3) . ?
C17 C171 1.533(3) . ?
C17 C172 1.536(3) . ?
C17 C173 1.538(3) . ?
C171 H17A 0.97(3) . ?
C171 H17B 1.01(3) . ?
C171 H17C 1.02(3) . ?
C172 H17D 1.00(3) . ?
C172 H17E 0.96(3) . ?
C172 H17F 1.00(3) . ?
C173 H17G 1.03(3) . ?
C173 H17H 0.98(3) . ?
C173 H17I 0.98(3) . ?
C18 C181 1.540(3) . ?
C18 C182 1.543(3) . ?
C18 C183 1.544(3) . ?
C181 H18A 0.96(2) . ?
C181 H18B 1.01(2) . ?
C181 H18C 0.96(3) . ?
C182 H18D 0.98(2) . ?
C182 H18E 0.95(2) . ?
C182 H18F 0.98(2) . ?
C183 H18G 0.99(2) . ?
C183 H18H 0.97(3) . ?
C183 H18I 0.96(3) . ?
C19 H19 0.92(2) . ?
C21 C26 1.397(2) . ?
C21 C22 1.428(2) . ?
C22 C23 1.437(2) . ?
C23 C29 1.400(2) . ?
C23 C24 1.454(2) . ?
C24 C25 1.371(2) . ?
C24 C28 1.543(2) . ?
C25 C26 1.425(2) . ?
C25 H25 0.92(2) . ?
C26 C27 1.535(2) . ?
C27 C273 1.526(3) . ?
C27 C272 1.534(3) . ?
C27 C271 1.537(3) . ?
C271 H27A 0.98(3) . ?
C271 H27B 1.00(3) . ?
C271 H27C 0.98(3) . ?
C272 H27D 1.01(3) . ?
C272 H27E 1.03(3) . ?
C272 H27F 1.00(3) . ?
C273 H27G 1.00(3) . ?
C273 H27H 1.04(3) . ?
C273 H27I 1.00(3) . ?
C28 C281 1.540(3) . ?
C28 C283 1.541(3) . ?
C28 C282 1.544(3) . ?
C281 H28A 0.94(2) . ?
C281 H28B 0.95(3) . ?
C281 H28C 1.00(2) . ?
C282 H28D 0.96(3) . ?
C282 H28E 0.97(3) . ?
C282 H28F 0.94(3) . ?
C283 H28G 0.97(2) . ?
C283 H28H 0.95(2) . ?
C283 H28I 0.98(3) . ?
C29 H29 0.94(2) . ?
C31 C36 1.388(2) . ?
C31 C32 1.399(2) . ?
C32 C33 1.393(2) . ?
C33 C34 1.399(2) . ?
C33 C1 1.523(3) . ?
C34 C35 1.384(3) . ?
C34 H34 0.97(2) . ?
C35 C36 1.386(3) . ?
C35 H35 0.93(2) . ?
C36 H36 0.94(2) . ?
C41 C42 1.388(2) . ?
C41 C46 1.401(2) . ?
C42 C43 1.389(3) . ?
C42 H42 0.97(2) . ?
C43 C44 1.383(3) . ?
C43 H43 0.93(2) . ?
C44 C45 1.398(3) . ?
C44 H44 0.96(2) . ?
C45 C46 1.390(2) . ?
C45 C1 1.523(2) . ?
C51 C7 1.399(2) . ?
C51 C52 1.437(2) . ?
C52 C53 1.357(2) . ?
C52 H52 0.96(2) . ?
C53 C54 1.442(2) . ?
C53 H53 0.95(2) . ?
C54 C4 1.402(2) . ?
C61 C4 1.404(2) . ?
C61 C62 1.442(2) . ?
C62 C63 1.351(3) . ?
C62 H62 0.97(2) . ?
C63 C64 1.447(2) . ?
C63 H63 0.94(2) . ?
C64 C5 1.402(2) . ?
C71 C5 1.404(2) . ?
C71 C72 1.443(2) . ?
C72 C73 1.354(2) . ?
C72 H72 0.92(2) . ?
C73 C74 1.443(2) . ?
C73 H73 0.99(2) . ?
C74 C6 1.403(2) . ?
C81 C6 1.405(2) . ?
C81 C82 1.445(2) . ?
C82 C83 1.349(3) . ?
C82 H82 0.94(2) . ?
C83 C84 1.444(2) . ?
C83 H83 0.93(2) . ?
C84 C7 1.399(2) . ?
C91 C92 1.380(3) . ?
C91 C96 1.393(3) . ?
C91 C7 1.502(2) . ?
C92 C93 1.401(3) . ?
C92 H92 0.91(3) . ?
C93 C94 1.360(5) . ?
C93 H93 0.89(3) . ?
C94 C95 1.371(5) . ?
C94 H94 0.96(3) . ?
C95 C96 1.399(4) . ?
C95 H95 1.00(4) . ?
C96 H96 1.00(3) . ?
C101 C102 1.399(2) . ?
C101 C106 1.402(3) . ?
C101 C4 1.500(2) . ?
C102 C103 1.393(2) . ?
C102 H102 0.95(2) . ?
C103 C104 1.386(3) . ?
C103 H103 0.95(2) . ?
C104 C105 1.391(3) . ?
C104 H104 0.95(2) . ?
C105 C106 1.389(3) . ?
C105 H105 0.95(2) . ?
C106 H106 0.94(2) . ?
C111 C112 1.397(3) . ?
C111 C116 1.399(3) . ?
C111 C5 1.496(2) . ?
C112 C113 1.398(3) . ?
C112 H112 0.97(2) . ?
C113 C114 1.383(4) . ?
C113 H113 0.93(2) . ?
C114 C115 1.381(4) . ?
C114 H114 0.97(3) . ?
C115 C116 1.392(3) . ?
C115 H115 0.95(3) . ?
C116 H116 0.95(2) . ?
C121 C122 1.402(3) . ?
C121 C126 1.403(3) . ?
C121 C6 1.498(2) . ?
C122 C123 1.395(3) . ?
C122 H122 0.96(2) . ?
C123 C124 1.388(3) . ?
C123 H123 0.95(2) . ?
C124 C125 1.386(3) . ?
C124 H124 0.94(3) . ?
C125 C126 1.393(3) . ?
C125 H125 0.95(2) . ?
C126 H126 0.90(2) . ?
C1 C2 1.540(3) . ?
C1 C3 1.545(3) . ?
C2 H2A 0.98(2) . ?
C2 H2B 0.99(3) . ?
C2 H2C 0.99(3) . ?
C3 H3A 0.95(3) . ?
C3 H3B 0.98(2) . ?
C3 H3C 0.99(3) . ?
O6 C1S 1.416(3) . ?
O6 C4S 1.431(4) . ?
C1S C2S 1.512(3) . ?
C1S H1S 0.9900 . ?
C1S H1' 0.9900 . ?
C2S C3S 1.521(4) . ?
C2S H2S 0.9900 . ?
C2S H2' 0.9900 . ?
C3S C4S 1.515(4) . ?
C3S H3S 0.9900 . ?
C3S H3' 0.9900 . ?
C4S H4S 0.9900 . ?
C4S H4' 0.9900 . ?
O7 C5S 1.433(3) . ?
O7 C8S 1.434(3) . ?
C5S C6S 1.496(3) . ?
C5S H5S 0.9900 . ?
C5S H5' 0.9900 . ?
C6S C7S 1.518(4) . ?
C6S H6S 0.9900 . ?
C6S H6' 0.9900 . ?
C7S C8S 1.499(4) . ?
C7S H7S 0.9900 . ?
C7S H7' 0.9900 . ?
C8S H8S 0.9900 . ?
C8S H8' 0.9900 . ?
O8 C11S 1.422(3) . ?
O8 C9S 1.426(3) . ?
C9S C10S 1.515(3) . ?
C9S H9S 0.9900 . ?
C9S H9' 0.9900 . ?
C10S C12S 1.514(3) . ?
C10S H10S 0.9900 . ?
C10S H10' 0.9900 . ?
C11S C12S 1.501(4) . ?
C11S H11S 0.9900 . ?
C11S H11' 0.9900 . ?
C12S H12S 0.9900 . ?
C12S H12' 0.9900 . ?
O9 C14S 1.488(5) . ?
O9 C15S 1.522(5) . ?
C13S C14S 1.408(6) . ?
C13S C16S 1.462(7) . ?
C13S H13A 0.9900 . ?
C13S H13B 0.9900 . ?
C13T C16S 1.424(10) . ?
C13T C14S 1.651(10) . ?
C13T H13C 0.9900 . ?
C13T H13D 0.9900 . ?
C14S H14A 0.9900 . ?
C14S H14B 0.9900 . ?
C14S H14C 0.9900 . ?
C14S H14D 0.9900 . ?
C15S C16S 1.392(6) . ?
C15S H15S 0.9900 . ?
C15S H15' 0.9900 . ?
C16S H16A 0.9900 . ?
C16S H16B 0.9900 . ?
C16S H16C 0.9900 . ?
C16S H16D 0.9900 . ?
O10 C17S 1.430(3) . ?
O10 C20S 1.432(2) . ?
C17S C18S 1.509(3) . ?
C17S H17S 0.9900 . ?
C17S H17' 0.9900 . ?
C18S C19S 1.520(3) . ?
C18S H18S 0.9900 . ?
C18S H18' 0.9900 . ?
C19S C20S 1.516(3) . ?
C19S H19S 0.9900 . ?
C19S H19' 0.9900 . ?
C20S H20S 0.9900 . ?
C20S H20' 0.9900 . ?
O11 C23S 1.381(5) . ?
O11 C24S 1.437(7) . ?
C21S C23S 1.425(5) . ?
C21S C22S 1.449(5) . ?
C21S H21S 0.9900 . ?
C21S H21' 0.9900 . ?
C22S C24S 1.511(7) . ?
C22S H22S 0.9900 . ?
C22S H22' 0.9900 . ?
C23S H23S 0.9900 . ?
C23S H23' 0.9900 . ?
C24S H24S 0.9900 . ?
C24S H24' 0.9900 . ?
O12 C25S 1.389(6) . ?
O12 C28S 1.489(7) . ?
C25S C26S 1.439(6) . ?
C25S H25S 0.9900 . ?
C25S H25' 0.9900 . ?
C26S C27S 1.481(4) . ?
C26S H26S 0.9900 . ?
C26S H26' 0.9900 . ?
C27S C28S 1.473(6) . ?
C27S H27S 0.9900 . ?
C27S H27' 0.9900 . ?
C28S H28S 0.9900 . ?
C28S H28' 0.9900 . ?

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 Zr O3 75.84(5) . . ?
O1 Zr O2 70.16(5) . . ?
O3 Zr O2 113.96(4) . . ?
O1 Zr O4 110.70(5) . . ?
O3 Zr O4 70.73(4) . . ?
O2 Zr O4 71.14(4) . . ?
O1 Zr N3 81.20(5) . . ?
O3 Zr N3 77.02(5) . . ?
O2 Zr N3 144.58(5) . . ?
O4 Zr N3 140.95(4) . . ?
O1 Zr N5 137.16(5) . . ?
O3 Zr N5 141.42(5) . . ?
O2 Zr N5 73.50(5) . . ?
O4 Zr N5 77.17(5) . . ?
N3 Zr N5 120.00(5) . . ?
O1 Zr N6 77.13(5) . . ?
O3 Zr N6 143.55(5) . . ?
O2 Zr N6 78.50(5) . . ?
O4 Zr N6 142.89(5) . . ?
N3 Zr N6 75.08(5) . . ?
N5 Zr N6 74.07(5) . . ?
O1 Zr N4 147.57(5) . . ?
O3 Zr N4 77.63(5) . . ?
O2 Zr N4 139.07(5) . . ?
O4 Zr N4 77.13(5) . . ?
N3 Zr N4 74.92(5) . . ?
N5 Zr N4 74.79(5) . . ?
N6 Zr N4 116.36(5) . . ?
C11 O1 Zr 122.21(11) . . ?
C12 O2 Zr 118.31(11) . . ?
C21 O3 Zr 121.58(11) . . ?
C22 O4 Zr 117.33(11) . . ?
C46 O5 C32 117.83(13) . . ?
C19 N1 C31 123.45(15) . . ?
C19 N1 H1 116.2(15) . . ?
C31 N1 H1 119.9(15) . . ?
C29 N2 C41 122.09(15) . . ?
C29 N2 H2 114.6(16) . . ?
C41 N2 H2 123.0(16) . . ?
C51 N3 C54 105.09(14) . . ?
C51 N3 Zr 123.34(11) . . ?
C54 N3 Zr 124.49(11) . . ?
C64 N4 C61 105.72(14) . . ?
C64 N4 Zr 125.77(11) . . ?
C61 N4 Zr 126.73(11) . . ?
C71 N5 C74 105.19(14) . . ?
C71 N5 Zr 123.38(10) . . ?
C74 N5 Zr 123.81(11) . . ?
C81 N6 C84 105.64(14) . . ?
C81 N6 Zr 126.31(11) . . ?
C84 N6 Zr 125.74(11) . . ?
O1 C11 C16 127.91(16) . . ?
O1 C11 C12 113.71(15) . . ?
C16 C11 C12 118.24(16) . . ?
O2 C12 C13 122.39(16) . . ?
O2 C12 C11 114.64(15) . . ?
C13 C12 C11 122.95(15) . . ?
C19 C13 C12 118.68(15) . . ?
C19 C13 C14 123.49(16) . . ?
C12 C13 C14 117.82(16) . . ?
C15 C14 C13 116.50(16) . . ?
C15 C14 C18 120.18(16) . . ?
C13 C14 C18 123.30(16) . . ?
C14 C15 C16 126.83(17) . . ?
C14 C15 H15 117.4(13) . . ?
C16 C15 H15 115.7(13) . . ?
C11 C16 C15 117.56(16) . . ?
C11 C16 C17 126.04(16) . . ?
C15 C16 C17 116.28(16) . . ?
C171 C17 C172 107.94(17) . . ?
C171 C17 C173 107.94(19) . . ?
C172 C17 C173 108.3(2) . . ?
C171 C17 C16 114.26(16) . . ?
C172 C17 C16 110.49(16) . . ?
C173 C17 C16 107.78(17) . . ?
C17 C171 H17A 111.5(15) . . ?
C17 C171 H17B 105.9(15) . . ?
H17A C171 H17B 109(2) . . ?
C17 C171 H17C 113.2(15) . . ?
H17A C171 H17C 107(2) . . ?
H17B C171 H17C 110(2) . . ?
C17 C172 H17D 110.8(15) . . ?
C17 C172 H17E 110.8(15) . . ?
H17D C172 H17E 107(2) . . ?
C17 C172 H17F 112.0(16) . . ?
H17D C172 H17F 109(2) . . ?
H17E C172 H17F 107(2) . . ?
C17 C173 H17G 109.3(18) . . ?
C17 C173 H17H 112.9(19) . . ?
H17G C173 H17H 110(3) . . ?
C17 C173 H17I 110.1(17) . . ?
H17G C173 H17I 109(2) . . ?
H17H C173 H17I 106(2) . . ?
C181 C18 C182 105.44(17) . . ?
C181 C18 C183 105.94(16) . . ?
C182 C18 C183 111.89(17) . . ?
C181 C18 C14 111.75(17) . . ?
C182 C18 C14 110.71(15) . . ?
C183 C18 C14 110.92(16) . . ?
C18 C181 H18A 111.6(14) . . ?
C18 C181 H18B 112.1(14) . . ?
H18A C181 H18B 109(2) . . ?
C18 C181 H18C 107.7(15) . . ?
H18A C181 H18C 107(2) . . ?
H18B C181 H18C 110(2) . . ?
C18 C182 H18D 115.1(14) . . ?
C18 C182 H18E 110.2(15) . . ?
H18D C182 H18E 107(2) . . ?
C18 C182 H18F 108.8(14) . . ?
H18D C182 H18F 106.2(19) . . ?
H18E C182 H18F 109(2) . . ?
C18 C183 H18G 114.7(13) . . ?
C18 C183 H18H 110.3(15) . . ?
H18G C183 H18H 107(2) . . ?
C18 C183 H18I 111.5(15) . . ?
H18G C183 H18I 105(2) . . ?
H18H C183 H18I 108(2) . . ?
N1 C19 C13 125.01(16) . . ?
N1 C19 H19 114.1(13) . . ?
C13 C19 H19 120.8(13) . . ?
O3 C21 C26 126.57(16) . . ?
O3 C21 C22 114.60(14) . . ?
C26 C21 C22 118.70(15) . . ?
O4 C22 C21 115.63(15) . . ?
O4 C22 C23 122.50(15) . . ?
C21 C22 C23 121.79(15) . . ?
C29 C23 C22 119.00(15) . . ?
C29 C23 C24 122.14(15) . . ?
C22 C23 C24 118.86(15) . . ?
C25 C24 C23 116.40(15) . . ?
C25 C24 C28 120.76(15) . . ?
C23 C24 C28 122.82(15) . . ?
C24 C25 C26 125.91(16) . . ?
C24 C25 H25 118.4(13) . . ?
C26 C25 H25 115.7(13) . . ?
C21 C26 C25 118.15(16) . . ?
C21 C26 C27 121.42(15) . . ?
C25 C26 C27 120.39(15) . . ?
C273 C27 C272 108.26(16) . . ?
C273 C27 C26 109.48(15) . . ?
C272 C27 C26 112.92(15) . . ?
C273 C27 C271 109.42(17) . . ?
C272 C27 C271 107.77(17) . . ?
C26 C27 C271 108.93(15) . . ?
C27 C271 H27A 109.1(14) . . ?
C27 C271 H27B 109.4(15) . . ?
H27A C271 H27B 105(2) . . ?
C27 C271 H27C 113.6(16) . . ?
H27A C271 H27C 109(2) . . ?
H27B C271 H27C 111(2) . . ?
C27 C272 H27D 111.1(15) . . ?
C27 C272 H27E 111.8(15) . . ?
H27D C272 H27E 109(2) . . ?
C27 C272 H27F 108.6(14) . . ?
H27D C272 H27F 110(2) . . ?
H27E C272 H27F 107(2) . . ?
C27 C273 H27G 111.3(15) . . ?
C27 C273 H27H 109.2(15) . . ?
H27G C273 H27H 113(2) . . ?
C27 C273 H27I 108.2(15) . . ?
H27G C273 H27I 107(2) . . ?
H27H C273 H27I 108(2) . . ?
C281 C28 C283 106.06(16) . . ?
C281 C28 C24 110.52(15) . . ?
C283 C28 C24 111.64(15) . . ?
C281 C28 C282 105.70(15) . . ?
C283 C28 C282 110.72(16) . . ?
C24 C28 C282 111.88(15) . . ?
C28 C281 H28A 110.8(14) . . ?
C28 C281 H28B 108.2(15) . . ?
H28A C281 H28B 107(2) . . ?
C28 C281 H28C 112.2(13) . . ?
H28A C281 H28C 110.6(19) . . ?
H28B C281 H28C 108(2) . . ?
C28 C282 H28D 109.6(15) . . ?
C28 C282 H28E 114.9(14) . . ?
H28D C282 H28E 107(2) . . ?
C28 C282 H28F 111.6(16) . . ?
H28D C282 H28F 108(2) . . ?
H28E C282 H28F 105(2) . . ?
C28 C283 H28G 114.0(13) . . ?
C28 C283 H28H 111.2(14) . . ?
H28G C283 H28H 106.1(19) . . ?
C28 C283 H28I 108.9(14) . . ?
H28G C283 H28I 108.3(19) . . ?
H28H C283 H28I 108(2) . . ?
N2 C29 C23 125.46(16) . . ?
N2 C29 H29 113.3(13) . . ?
C23 C29 H29 121.2(13) . . ?
C36 C31 C32 119.33(16) . . ?
C36 C31 N1 120.64(16) . . ?
C32 C31 N1 119.99(15) . . ?
O5 C32 C33 123.41(16) . . ?
O5 C32 C31 115.02(15) . . ?
C33 C32 C31 121.57(16) . . ?
C32 C33 C34 117.59(17) . . ?
C32 C33 C1 122.47(15) . . ?
C34 C33 C1 119.93(16) . . ?
C35 C34 C33 121.43(18) . . ?
C35 C34 H34 120.0(13) . . ?
C33 C34 H34 118.6(12) . . ?
C34 C35 C36 120.11(17) . . ?
C34 C35 H35 120.2(14) . . ?
C36 C35 H35 119.6(14) . . ?
C35 C36 C31 119.95(18) . . ?
C35 C36 H36 122.0(14) . . ?
C31 C36 H36 118.0(14) . . ?
C42 C41 C46 119.66(17) . . ?
C42 C41 N2 121.27(16) . . ?
C46 C41 N2 119.06(15) . . ?
C41 C42 C43 119.78(17) . . ?
C41 C42 H42 118.9(14) . . ?
C43 C42 H42 121.3(14) . . ?
C44 C43 C42 119.82(18) . . ?
C44 C43 H43 120.5(15) . . ?
C42 C43 H43 119.4(15) . . ?
C43 C44 C45 121.77(18) . . ?
C43 C44 H44 118.2(13) . . ?
C45 C44 H44 120.0(13) . . ?
C46 C45 C44 117.61(16) . . ?
C46 C45 C1 121.76(16) . . ?
C44 C45 C1 120.58(16) . . ?
O5 C46 C45 124.19(15) . . ?
O5 C46 C41 114.52(15) . . ?
C45 C46 C41 121.29(16) . . ?
N3 C51 C7 124.65(16) . . ?
N3 C51 C52 110.58(15) . . ?
C7 C51 C52 124.16(16) . . ?
C53 C52 C51 106.75(16) . . ?
C53 C52 H52 128.9(13) . . ?
C51 C52 H52 124.2(13) . . ?
C52 C53 C54 107.07(16) . . ?
C52 C53 H53 128.5(13) . . ?
C54 C53 H53 124.4(13) . . ?
N3 C54 C4 125.03(16) . . ?
N3 C54 C53 110.06(15) . . ?
C4 C54 C53 124.55(15) . . ?
N4 C61 C4 126.32(15) . . ?
N4 C61 C62 110.12(15) . . ?
C4 C61 C62 123.43(16) . . ?
C63 C62 C61 107.03(16) . . ?
C63 C62 H62 128.4(13) . . ?
C61 C62 H62 124.5(13) . . ?
C62 C63 C64 107.07(16) . . ?
C62 C63 H63 128.4(14) . . ?
C64 C63 H63 124.5(14) . . ?
N4 C64 C5 126.70(15) . . ?
N4 C64 C63 110.04(15) . . ?
C5 C64 C63 123.10(16) . . ?
N5 C71 C5 125.21(16) . . ?
N5 C71 C72 110.24(14) . . ?
C5 C71 C72 124.37(16) . . ?
C73 C72 C71 107.10(16) . . ?
C73 C72 H72 128.0(13) . . ?
C71 C72 H72 124.8(13) . . ?
C72 C73 C74 107.14(15) . . ?
C72 C73 H73 126.6(13) . . ?
C74 C73 H73 126.2(13) . . ?
N5 C74 C6 124.93(16) . . ?
N5 C74 C73 110.10(15) . . ?
C6 C74 C73 124.83(15) . . ?
N6 C81 C6 126.39(15) . . ?
N6 C81 C82 110.07(15) . . ?
C6 C81 C82 123.44(16) . . ?
C83 C82 C81 107.08(15) . . ?
C83 C82 H82 128.0(14) . . ?
C81 C82 H82 124.8(14) . . ?
C82 C83 C84 106.97(16) . . ?
C82 C83 H83 128.2(14) . . ?
C84 C83 H83 124.8(14) . . ?
N6 C84 C7 126.86(15) . . ?
N6 C84 C83 110.22(15) . . ?
C7 C84 C83 122.89(16) . . ?
C92 C91 C96 118.4(2) . . ?
C92 C91 C7 120.35(19) . . ?
C96 C91 C7 121.2(2) . . ?
C91 C92 C93 120.6(3) . . ?
C91 C92 H92 119.9(16) . . ?
C93 C92 H92 119.4(16) . . ?
C94 C93 C92 120.6(3) . . ?
C94 C93 H93 124(2) . . ?
C92 C93 H93 115(2) . . ?
C93 C94 C95 119.8(2) . . ?
C93 C94 H94 122(2) . . ?
C95 C94 H94 118.0(19) . . ?
C94 C95 C96 120.5(3) . . ?
C94 C95 H95 120(2) . . ?
C96 C95 H95 119(2) . . ?
C91 C96 C95 120.2(3) . . ?
C91 C96 H96 118.5(18) . . ?
C95 C96 H96 121.3(18) . . ?
C102 C101 C106 118.20(16) . . ?
C102 C101 C4 121.86(16) . . ?
C106 C101 C4 119.93(15) . . ?
C103 C102 C101 120.86(17) . . ?
C103 C102 H102 118.6(13) . . ?
C101 C102 H102 120.5(13) . . ?
C104 C103 C102 120.06(17) . . ?
C104 C103 H103 120.8(13) . . ?
C102 C103 H103 119.1(13) . . ?
C103 C104 C105 119.85(17) . . ?
C103 C104 H104 119.5(14) . . ?
C105 C104 H104 120.6(14) . . ?
C106 C105 C104 120.08(18) . . ?
C106 C105 H105 120.1(14) . . ?
C104 C105 H105 119.8(14) . . ?
C105 C106 C101 120.87(17) . . ?
C105 C106 H106 119.1(14) . . ?
C101 C106 H106 119.9(14) . . ?
C112 C111 C116 118.24(18) . . ?
C112 C111 C5 120.58(17) . . ?
C116 C111 C5 121.16(17) . . ?
C111 C112 C113 120.6(2) . . ?
C111 C112 H112 119.9(14) . . ?
C113 C112 H112 119.5(14) . . ?
C114 C113 C112 120.3(2) . . ?
C114 C113 H113 120.2(16) . . ?
C112 C113 H113 119.5(16) . . ?
C115 C114 C113 119.6(2) . . ?
C115 C114 H114 120.6(16) . . ?
C113 C114 H114 119.7(16) . . ?
C114 C115 C116 120.4(2) . . ?
C114 C115 H115 120.6(16) . . ?
C116 C115 H115 119.0(16) . . ?
C115 C116 C111 120.8(2) . . ?
C115 C116 H116 120.0(13) . . ?
C111 C116 H116 119.2(13) . . ?
C122 C121 C126 118.03(16) . . ?
C122 C121 C6 123.17(16) . . ?
C126 C121 C6 118.78(16) . . ?
C123 C122 C121 120.44(19) . . ?
C123 C122 H122 121.4(13) . . ?
C121 C122 H122 118.1(13) . . ?
C124 C123 C122 120.72(19) . . ?
C124 C123 H123 120.9(14) . . ?
C122 C123 H123 118.3(14) . . ?
C125 C124 C123 119.49(18) . . ?
C125 C124 H124 120.4(16) . . ?
C123 C124 H124 120.1(16) . . ?
C124 C125 C126 120.2(2) . . ?
C124 C125 H125 121.8(14) . . ?
C126 C125 H125 118.1(14) . . ?
C125 C126 C121 121.17(19) . . ?
C125 C126 H126 119.6(14) . . ?
C121 C126 H126 119.2(14) . . ?
C45 C1 C33 110.17(15) . . ?
C45 C1 C2 110.08(15) . . ?
C33 C1 C2 109.82(16) . . ?
C45 C1 C3 108.09(16) . . ?
C33 C1 C3 109.06(16) . . ?
C2 C1 C3 109.59(17) . . ?
C1 C2 H2A 112.1(14) . . ?
C1 C2 H2B 111.5(15) . . ?
H2A C2 H2B 106(2) . . ?
C1 C2 H2C 109.7(15) . . ?
H2A C2 H2C 109(2) . . ?
H2B C2 H2C 108(2) . . ?
C1 C3 H3A 110.0(15) . . ?
C1 C3 H3B 109.1(14) . . ?
H3A C3 H3B 108(2) . . ?
C1 C3 H3C 110.5(14) . . ?
H3A C3 H3C 110(2) . . ?
H3B C3 H3C 110(2) . . ?
C54 C4 C61 124.15(15) . . ?
C54 C4 C101 117.56(15) . . ?
C61 C4 C101 117.89(15) . . ?
C64 C5 C71 124.14(16) . . ?
C64 C5 C111 117.42(15) . . ?
C71 C5 C111 118.23(16) . . ?
C74 C6 C81 123.62(15) . . ?
C74 C6 C121 120.36(16) . . ?
C81 C6 C121 116.00(15) . . ?
C51 C7 C84 124.19(16) . . ?
C51 C7 C91 118.00(16) . . ?
C84 C7 C91 117.33(15) . . ?
C1S O6 C4S 108.5(2) . . ?
O6 C1S C2S 106.8(2) . . ?
O6 C1S H1S 110.4 . . ?
C2S C1S H1S 110.4 . . ?
O6 C1S H1' 110.4 . . ?
C2S C1S H1' 110.4 . . ?
H1S C1S H1' 108.6 . . ?
C1S C2S C3S 101.9(2) . . ?
C1S C2S H2S 111.4 . . ?
C3S C2S H2S 111.4 . . ?
C1S C2S H2' 111.4 . . ?
C3S C2S H2' 111.4 . . ?
H2S C2S H2' 109.2 . . ?
C4S C3S C2S 103.7(2) . . ?
C4S C3S H3S 111.0 . . ?
C2S C3S H3S 111.0 . . ?
C4S C3S H3' 111.0 . . ?
C2S C3S H3' 111.0 . . ?
H3S C3S H3' 109.0 . . ?
O6 C4S C3S 108.0(2) . . ?
O6 C4S H4S 110.1 . . ?
C3S C4S H4S 110.1 . . ?
O6 C4S H4' 110.1 . . ?
C3S C4S H4' 110.1 . . ?
H4S C4S H4' 108.4 . . ?
C5S O7 C8S 108.52(17) . . ?
O7 C5S C6S 106.74(18) . . ?
O7 C5S H5S 110.4 . . ?
C6S C5S H5S 110.4 . . ?
O7 C5S H5' 110.4 . . ?
C6S C5S H5' 110.4 . . ?
H5S C5S H5' 108.6 . . ?
C5S C6S C7S 101.7(2) . . ?
C5S C6S H6S 111.4 . . ?
C7S C6S H6S 111.4 . . ?
C5S C6S H6' 111.4 . . ?
C7S C6S H6' 111.4 . . ?
H6S C6S H6' 109.3 . . ?
C8S C7S C6S 101.9(2) . . ?
C8S C7S H7S 111.4 . . ?
C6S C7S H7S 111.4 . . ?
C8S C7S H7' 111.4 . . ?
C6S C7S H7' 111.4 . . ?
H7S C7S H7' 109.3 . . ?
O7 C8S C7S 106.6(2) . . ?
O7 C8S H8S 110.4 . . ?
C7S C8S H8S 110.4 . . ?
O7 C8S H8' 110.4 . . ?
C7S C8S H8' 110.4 . . ?
H8S C8S H8' 108.6 . . ?
C11S O8 C9S 109.34(18) . . ?
O8 C9S C10S 106.38(19) . . ?
O8 C9S H9S 110.5 . . ?
C10S C9S H9S 110.5 . . ?
O8 C9S H9' 110.5 . . ?
C10S C9S H9' 110.5 . . ?
H9S C9S H9' 108.6 . . ?
C12S C10S C9S 102.5(2) . . ?
C12S C10S H10S 111.3 . . ?
C9S C10S H10S 111.3 . . ?
C12S C10S H10' 111.3 . . ?
C9S C10S H10' 111.3 . . ?
H10S C10S H10' 109.2 . . ?
O8 C11S C12S 107.5(2) . . ?
O8 C11S H11S 110.2 . . ?
C12S C11S H11S 110.2 . . ?
O8 C11S H11' 110.2 . . ?
C12S C11S H11' 110.2 . . ?
H11S C11S H11' 108.5 . . ?
C11S C12S C10S 102.1(2) . . ?
C11S C12S H12S 111.4 . . ?
C10S C12S H12S 111.4 . . ?
C11S C12S H12' 111.4 . . ?
C10S C12S H12' 111.4 . . ?
H12S C12S H12' 109.2 . . ?
C14S O9 C15S 102.3(3) . . ?
C14S C13S C16S 107.2(4) . . ?
C14S C13S H13A 110.3 . . ?
C16S C13S H13A 110.3 . . ?
C14S C13S H13B 110.3 . . ?
C16S C13S H13B 110.3 . . ?
H13A C13S H13B 108.5 . . ?
C16S C13T C14S 97.2(6) . . ?
C16S C13T H13C 112.3 . . ?
C14S C13T H13C 112.3 . . ?
C16S C13T H13D 112.3 . . ?
C14S C13T H13D 112.3 . . ?
H13C C13T H13D 109.9 . . ?
C13S C14S O9 102.8(4) . . ?
O9 C14S C13T 106.9(4) . . ?
C13S C14S H14A 111.2 . . ?
O9 C14S H14A 111.2 . . ?
C13S C14S H14B 111.2 . . ?
O9 C14S H14B 111.2 . . ?
H14A C14S H14B 109.1 . . ?
O9 C14S H14C 110.3 . . ?
C13T C14S H14C 110.3 . . ?
O9 C14S H14D 110.3 . . ?
C13T C14S H14D 110.3 . . ?
H14C C14S H14D 108.6 . . ?
C16S C15S O9 106.8(4) . . ?
C16S C15S H15S 110.4 . . ?
O9 C15S H15S 110.4 . . ?
C16S C15S H15' 110.4 . . ?
O9 C15S H15' 110.4 . . ?
H15S C15S H15' 108.6 . . ?
C15S C16S C13T 109.1(5) . . ?
C15S C16S C13S 107.2(4) . . ?
C15S C16S H16A 110.3 . . ?
C13S C16S H16A 110.3 . . ?
C15S C16S H16B 110.3 . . ?
C13S C16S H16B 110.3 . . ?
H16A C16S H16B 108.5 . . ?
C15S C16S H16C 109.9 . . ?
C13T C16S H16C 109.9 . . ?
C15S C16S H16D 109.9 . . ?
C13T C16S H16D 109.9 . . ?
H16C C16S H16D 108.3 . . ?
C17S O10 C20S 106.78(16) . . ?
O10 C17S C18S 104.39(17) . . ?
O10 C17S H17S 110.9 . . ?
C18S C17S H17S 110.9 . . ?
O10 C17S H17' 110.9 . . ?
C18S C17S H17' 110.9 . . ?
H17S C17S H17' 108.9 . . ?
C17S C18S C19S 102.19(18) . . ?
C17S C18S H18S 111.3 . . ?
C19S C18S H18S 111.3 . . ?
C17S C18S H18' 111.3 . . ?
C19S C18S H18' 111.3 . . ?
H18S C18S H18' 109.2 . . ?
C20S C19S C18S 104.77(18) . . ?
C20S C19S H19S 110.8 . . ?
C18S C19S H19S 110.8 . . ?
C20S C19S H19' 110.8 . . ?
C18S C19S H19' 110.8 . . ?
H19S C19S H19' 108.9 . . ?
O10 C20S C19S 106.93(18) . . ?
O10 C20S H20S 110.3 . . ?
C19S C20S H20S 110.3 . . ?
O10 C20S H20' 110.3 . . ?
C19S C20S H20' 110.3 . . ?
H20S C20S H20' 108.6 . . ?
C23S O11 C24S 104.8(3) . . ?
C23S C21S C22S 105.1(4) . . ?
C23S C21S H21S 110.7 . . ?
C22S C21S H21S 110.7 . . ?
C23S C21S H21' 110.7 . . ?
C22S C21S H21' 110.7 . . ?
H21S C21S H21' 108.8 . . ?
C21S C22S C24S 101.6(3) . . ?
C21S C22S H22S 111.4 . . ?
C24S C22S H22S 111.4 . . ?
C21S C22S H22' 111.4 . . ?
C24S C22S H22' 111.4 . . ?
H22S C22S H22' 109.3 . . ?
O11 C23S C21S 107.3(3) . . ?
O11 C23S H23S 110.3 . . ?
C21S C23S H23S 110.3 . . ?
O11 C23S H23' 110.3 . . ?
C21S C23S H23' 110.3 . . ?
H23S C23S H23' 108.5 . . ?
O11 C24S C22S 108.0(3) . . ?
O11 C24S H24S 110.1 . . ?
C22S C24S H24S 110.1 . . ?
O11 C24S H24' 110.1 . . ?
C22S C24S H24' 110.1 . . ?
H24S C24S H24' 108.4 . . ?
C25S O12 C28S 108.0(3) . . ?
O12 C25S C26S 106.3(4) . . ?
O12 C25S H25S 110.5 . . ?
C26S C25S H25S 110.5 . . ?
O12 C25S H25' 110.5 . . ?
C26S C25S H25' 110.5 . . ?
H25S C25S H25' 108.7 . . ?
C25S C26S C27S 104.5(4) . . ?
C25S C26S H26S 110.8 . . ?
C27S C26S H26S 110.8 . . ?
C25S C26S H26' 110.8 . . ?
C27S C26S H26' 110.8 . . ?
H26S C26S H26' 108.9 . . ?
C28S C27S C26S 101.7(3) . . ?
C28S C27S H27S 111.4 . . ?
C26S C27S H27S 111.4 . . ?
C28S C27S H27' 111.4 . . ?
C26S C27S H27' 111.4 . . ?
H27S C27S H27' 109.3 . . ?
C27S C28S O12 105.0(4) . . ?
C27S C28S H28S 110.7 . . ?
O12 C28S H28S 110.7 . . ?
C27S C28S H28' 110.7 . . ?
O12 C28S H28' 110.7 . . ?
H28S C28S H28' 108.8 . . ?

_refine_diff_density_max         0.894
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_zrxbic_sq
_database_code_depnum_ccdc_archive 'CCDC 2015705'
loop_
_audit_author_name
_audit_author_address
'Seth Brown'
;University of Notre Dame
United States of America
;
_audit_update_record             
;
2020-07-12 deposited with the CCDC.	2020-08-05 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT934_zrxbic_sq           
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW > 10 Outliers ....2 Check 
RESPONSE: There is no systematic reason to discard these reflections. 
The reflections could disagree because SQUEEZE was run to remove
disordered solvent molecules. 
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2016/4
_shelx_SHELXL_version_number     2016/4
_chemical_name_systematic        
'Bis(9,9-dimethylxanthene-4,5-bis(4,6-di-tert-butylcatecholatoaldiminium))zirconium(IV) tri-chloroform mono-hexane solvate'
_chemical_name_common            '(XbicH2)2Zr . 3 CHCl3 . C6H14'
_chemical_melting_point          .
_chemical_formula_moiety         'C90 H108 N4 O10 Zr, 3(C H Cl3), C6 H14'
_chemical_formula_sum            'C99 H125 Cl9 N4 O10 Zr'
_chemical_formula_weight         1941.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

_cell_length_a                   35.0034(17)
_cell_length_b                   15.2378(7)
_cell_length_c                   24.6829(12)
_cell_angle_alpha                90
_cell_angle_beta                 133.9561(12)
_cell_angle_gamma                90
_cell_volume                     9477.3(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9887
_cell_measurement_theta_min      2.245
_cell_measurement_theta_max      29.216

_exptl_crystal_description       block
_exptl_crystal_colour            blue
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_F_000             4080
_exptl_transmission_factor_min   0.7096
_exptl_transmission_factor_max   0.7458
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.255
_exptl_absorpt_coefficient_mu    0.430
_shelx_estimated_absorpt_T_min   0.893
_shelx_estimated_absorpt_T_max   0.918
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7096
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;
_exptl_crystal_recrystallization_method 
'Crystals deposited from solvent layering of CHCl3 and hexanes.'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa X8-APEX-II'
_diffrn_measurement_method       'combination of ω and φ-scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            99143
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.562
_diffrn_reflns_theta_max         29.333
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12983
_reflns_number_gt                11050
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_refine_special_details          
;
Solution of the structure yielded one ordered chloroform and an
area of electron density with indistinguishable solvent. The 
structure was analyzed using SQUEEZE (P. van der Sluis and A. L. Spek, 
Acta Cryst. A, 1990, 46, 194-201), which showed that the void volume
was 1415 cubic angstroms with 421 electrons per unit cell. 
This corresponds to about 4 CHCl3 and 4 hexane molecules per unit cell
(432 electrons, predicted V = 1400 cubic angstroms, based on the
molar volumes of the liquids). 

The hydrogens on N1, N2, C19, and C29 were found on 
the difference map and refined isotropically.
The remaining hydrogens were placed in calculated positions.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0519P)²+21.2066P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12983
_refine_ls_number_parameters     528
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1151
_refine_ls_wR_factor_gt          0.1077
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_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
ZR Zr 0.500000 0.09713(2) 0.250000 0.01031(6) Uani 1 2 d S T P . .
O1 O 0.46492(5) -0.00784(8) 0.16990(7) 0.0165(2) Uani 1 1 d . . . . .
H1 H 0.3901(10) 0.0634(17) 0.2450(14) 0.027(6) Uiso 1 1 d . . . . .
O2 O 0.42890(5) 0.04440(8) 0.22443(7) 0.0146(2) Uani 1 1 d . . . . .
H2 H 0.3917(10) 0.2577(17) 0.1871(14) 0.027(6) Uiso 1 1 d . . . . .
O3 O 0.49653(5) 0.15191(8) 0.16663(7) 0.0152(2) Uani 1 1 d . . . . .
O4 O 0.43750(5) 0.20121(8) 0.18605(7) 0.0148(2) Uani 1 1 d . . . . .
O5 O 0.34516(5) 0.20760(8) 0.22944(7) 0.0166(2) Uani 1 1 d . . . . .
N1 N 0.36744(6) 0.03540(10) 0.24413(8) 0.0161(3) Uani 1 1 d . . . . .
N2 N 0.36903(6) 0.30033(10) 0.16220(8) 0.0166(3) Uani 1 1 d . . . . .
C11 C 0.43405(6) -0.06479(11) 0.16480(9) 0.0150(3) Uani 1 1 d . . . . .
C12 C 0.41332(6) -0.03312(11) 0.19457(9) 0.0136(3) Uani 1 1 d . . . . .
C13 C 0.37668(6) -0.08343(11) 0.18977(9) 0.0157(3) Uani 1 1 d . . . . .
C14 C 0.36344(7) -0.17106(12) 0.15865(9) 0.0182(3) Uani 1 1 d . . . . .
C15 C 0.38533(7) -0.19785(12) 0.13248(10) 0.0200(3) Uani 1 1 d . . . . .
H15 H 0.376871 -0.255388 0.112117 0.024 Uiso 1 1 calc R U . . .
C16 C 0.41975(7) -0.14724(12) 0.13296(9) 0.0172(3) Uani 1 1 d . . . . .
C17 C 0.44032(8) -0.18363(13) 0.09935(10) 0.0227(4) Uani 1 1 d . . . . .
C171 C 0.42039(12) -0.27695(16) 0.06848(16) 0.0424(6) Uani 1 1 d . . . . .
H17A H 0.431782 -0.316007 0.109011 0.064 Uiso 1 1 calc R U . . .
H17B H 0.381556 -0.276735 0.028158 0.064 Uiso 1 1 calc R U . . .
H17C H 0.435110 -0.297759 0.048527 0.064 Uiso 1 1 calc R U . . .
C172 C 0.42216(10) -0.12427(16) 0.03543(13) 0.0355(5) Uani 1 1 d . . . . .
H17D H 0.383294 -0.122054 -0.003489 0.053 Uiso 1 1 calc R U . . .
H17E H 0.436275 -0.065027 0.054900 0.053 Uiso 1 1 calc R U . . .
H17F H 0.435216 -0.147534 0.013755 0.053 Uiso 1 1 calc R U . . .
C173 C 0.50075(9) -0.18729(18) 0.16004(12) 0.0371(5) Uani 1 1 d . . . . .
H17G H 0.512305 -0.225527 0.201083 0.056 Uiso 1 1 calc R U . . .
H17H H 0.513867 -0.210603 0.138463 0.056 Uiso 1 1 calc R U . . .
H17I H 0.514927 -0.128096 0.179607 0.056 Uiso 1 1 calc R U . . .
C18 C 0.32806(8) -0.23348(13) 0.15670(11) 0.0233(4) Uani 1 1 d . . . . .
C181 C 0.35321(8) -0.25299(13) 0.23717(11) 0.0248(4) Uani 1 1 d . . . . .
H18A H 0.357626 -0.198022 0.261630 0.037 Uiso 1 1 calc R U . . .
H18B H 0.330034 -0.292615 0.234820 0.037 Uiso 1 1 calc R U . . .
H18C H 0.387924 -0.280737 0.266164 0.037 Uiso 1 1 calc R U . . .
C182 C 0.27138(8) -0.19722(17) 0.10729(12) 0.0355(5) Uani 1 1 d . . . . .
H18D H 0.272743 -0.140008 0.126719 0.053 Uiso 1 1 calc R U . . .
H18E H 0.255096 -0.190544 0.055444 0.053 Uiso 1 1 calc R U . . .
H18F H 0.250216 -0.238019 0.108258 0.053 Uiso 1 1 calc R U . . .
C183 C 0.32267(10) -0.32242(15) 0.12299(13) 0.0372(5) Uani 1 1 d . . . . .
H18G H 0.299965 -0.361059 0.122330 0.056 Uiso 1 1 calc R U . . .
H18H H 0.306752 -0.313969 0.071473 0.056 Uiso 1 1 calc R U . . .
H18I H 0.357827 -0.349128 0.153589 0.056 Uiso 1 1 calc R U . . .
C19 C 0.35593(7) -0.04440(12) 0.21587(10) 0.0170(3) Uani 1 1 d . . . . .
H19 H 0.3306(9) -0.0724(16) 0.2123(13) 0.022(6) Uiso 1 1 d . . . . .
C21 C 0.45903(6) 0.20792(11) 0.11667(9) 0.0142(3) Uani 1 1 d . . . . .
C22 C 0.42689(6) 0.23717(11) 0.12917(9) 0.0137(3) Uani 1 1 d . . . . .
C23 C 0.38602(7) 0.30082(11) 0.08248(9) 0.0156(3) Uani 1 1 d . . . . .
C24 C 0.37516(7) 0.33401(12) 0.01779(9) 0.0170(3) Uani 1 1 d . . . . .
C25 C 0.40558(7) 0.30080(12) 0.00667(10) 0.0193(3) Uani 1 1 d . . . . .
H25 H 0.398632 0.321844 -0.035699 0.023 Uiso 1 1 calc R U . . .
C26 C 0.44678(7) 0.23741(12) 0.05302(10) 0.0183(3) Uani 1 1 d . . . . .
C27 C 0.47633(8) 0.20102(16) 0.03296(11) 0.0287(4) Uani 1 1 d . . . . .
C271 C 0.53506(9) 0.2246(2) 0.09514(14) 0.0430(6) Uani 1 1 d . . . . .
H27A H 0.554096 0.201290 0.082385 0.064 Uiso 1 1 calc R U . . .
H27B H 0.538971 0.288543 0.100114 0.064 Uiso 1 1 calc R U . . .
H27C H 0.549814 0.199032 0.142843 0.064 Uiso 1 1 calc R U . . .
C272 C 0.45481(11) 0.2367(2) -0.04192(14) 0.0528(8) Uani 1 1 d . . . . .
H27D H 0.417087 0.221991 -0.082327 0.079 Uiso 1 1 calc R U . . .
H27E H 0.459127 0.300619 -0.038581 0.079 Uiso 1 1 calc R U . . .
H27F H 0.474449 0.210385 -0.052755 0.079 Uiso 1 1 calc R U . . .
C273 C 0.47008(12) 0.10087(18) 0.02575(15) 0.0435(6) Uani 1 1 d . . . . .
H27G H 0.432370 0.085826 -0.014172 0.065 Uiso 1 1 calc R U . . .
H27H H 0.489175 0.076938 0.013271 0.065 Uiso 1 1 calc R U . . .
H27I H 0.484715 0.075893 0.073554 0.065 Uiso 1 1 calc R U . . .
C28 C 0.33101(7) 0.40057(13) -0.03754(11) 0.0225(4) Uani 1 1 d . . . . .
C281 C 0.27675(8) 0.36230(16) -0.07439(12) 0.0303(4) Uani 1 1 d . . . . .
H28A H 0.248798 0.405224 -0.109627 0.045 Uiso 1 1 calc R U . . .
H28B H 0.270002 0.308441 -0.101613 0.045 Uiso 1 1 calc R U . . .
H28C H 0.276967 0.348888 -0.035346 0.045 Uiso 1 1 calc R U . . .
C282 C 0.34158(10) 0.48958(14) 0.00038(13) 0.0345(5) Uani 1 1 d . . . . .
H28D H 0.312612 0.530226 -0.036633 0.052 Uiso 1 1 calc R U . . .
H28E H 0.343679 0.481339 0.041769 0.052 Uiso 1 1 calc R U . . .
H28F H 0.375166 0.513808 0.020145 0.052 Uiso 1 1 calc R U . . .
C283 C 0.32632(9) 0.42049(16) -0.10319(12) 0.0310(5) Uani 1 1 d . . . . .
H28G H 0.297795 0.463129 -0.137220 0.046 Uiso 1 1 calc R U . . .
H28H H 0.359924 0.444786 -0.083322 0.046 Uiso 1 1 calc R U . . .
H28I H 0.318258 0.366211 -0.130768 0.046 Uiso 1 1 calc R U . . .
C29 C 0.36023(7) 0.33008(11) 0.10395(10) 0.0171(3) Uani 1 1 d . . . . .
H29 H 0.3356(9) 0.3775(15) 0.0791(13) 0.022(6) Uiso 1 1 d . . . . .
C31 C 0.34732(7) 0.06934(12) 0.27319(9) 0.0170(3) Uani 1 1 d . . . . .
C32 C 0.33546(6) 0.15858(12) 0.26575(9) 0.0164(3) Uani 1 1 d . . . . .
C33 C 0.31464(7) 0.19318(13) 0.29263(10) 0.0196(3) Uani 1 1 d . . . . .
C34 C 0.30473(8) 0.13569(14) 0.32566(11) 0.0243(4) Uani 1 1 d . . . . .
H34 H 0.289179 0.157858 0.342639 0.029 Uiso 1 1 calc R U . . .
C35 C 0.31682(8) 0.04776(14) 0.33436(11) 0.0259(4) Uani 1 1 d . . . . .
H35 H 0.310075 0.010096 0.357605 0.031 Uiso 1 1 calc R U . . .
C36 C 0.33888(8) 0.01464(13) 0.30898(10) 0.0223(4) Uani 1 1 d . . . . .
H36 H 0.348253 -0.045642 0.316074 0.027 Uiso 1 1 calc R U . . .
C41 C 0.34989(7) 0.34405(12) 0.18984(10) 0.0180(3) Uani 1 1 d . . . . .
C42 C 0.34440(9) 0.43450(13) 0.18451(12) 0.0259(4) Uani 1 1 d . . . . .
H42 H 0.353361 0.467351 0.161924 0.031 Uiso 1 1 calc R U . . .
C43 C 0.32590(9) 0.47700(14) 0.21200(13) 0.0302(4) Uani 1 1 d . . . . .
H43 H 0.321862 0.538983 0.207848 0.036 Uiso 1 1 calc R U . . .
C44 C 0.31334(8) 0.42991(14) 0.24531(12) 0.0268(4) Uani 1 1 d . . . . .
H44 H 0.300717 0.459969 0.264046 0.032 Uiso 1 1 calc R U . . .
C45 C 0.31873(7) 0.33912(12) 0.25217(10) 0.0197(3) Uani 1 1 d . . . . .
C46 C 0.33754(7) 0.29686(11) 0.22484(9) 0.0166(3) Uani 1 1 d . . . . .
C1 C 0.30355(8) 0.28991(13) 0.28827(11) 0.0229(4) Uani 1 1 d . . . . .
C2 C 0.33686(11) 0.32448(16) 0.36884(13) 0.0358(5) Uani 1 1 d . . . . .
H2A H 0.329991 0.387268 0.367047 0.054 Uiso 1 1 calc R U . . .
H2B H 0.374624 0.315396 0.398376 0.054 Uiso 1 1 calc R U . . .
H2C H 0.327142 0.292755 0.392365 0.054 Uiso 1 1 calc R U . . .
C3 C 0.24424(9) 0.30438(17) 0.24153(14) 0.0361(5) Uani 1 1 d . . . . .
H3A H 0.223215 0.283032 0.190140 0.054 Uiso 1 1 calc R U . . .
H3B H 0.237494 0.367135 0.240187 0.054 Uiso 1 1 calc R U . . .
H3C H 0.234205 0.272193 0.264464 0.054 Uiso 1 1 calc R U . . .
C4 C 0.16971(8) 0.44352(13) -0.01661(11) 0.0245(4) Uani 1 1 d . . . . .
H4 H 0.130783 0.455108 -0.058202 0.029 Uiso 1 1 calc R U . . .
CL1 Cl 0.18065(2) 0.37831(4) 0.05136(3) 0.03401(12) Uani 1 1 d . . . . .
CL2 Cl 0.20297(2) 0.54441(4) 0.02228(3) 0.04053(14) Uani 1 1 d . . . . .
CL3 Cl 0.19113(2) 0.38894(4) -0.05386(3) 0.04063(14) Uani 1 1 d . . . . .


_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
ZR O3 2.1446(11) . ?
ZR O3 2.1446(11) 2_655 ?
ZR O1 2.1459(12) 2_655 ?
ZR O1 2.1459(12) . ?
ZR O4 2.2358(12) 2_655 ?
ZR O4 2.2359(11) . ?
ZR O2 2.2489(11) . ?
ZR O2 2.2490(11) 2_655 ?
O1 C11 1.322(2) . ?
O2 C12 1.295(2) . ?
O3 C21 1.313(2) . ?
O4 C22 1.2983(19) . ?
O5 C46 1.375(2) . ?
O5 C32 1.3783(19) . ?
N1 C19 1.318(2) . ?
N1 C31 1.407(2) . ?
N1 H1 0.89(3) . ?
N2 C29 1.324(2) . ?
N2 C41 1.412(2) . ?
N2 H2 0.87(3) . ?
C11 C16 1.379(2) . ?
C11 C12 1.428(2) . ?
C12 C13 1.427(2) . ?
C13 C19 1.395(2) . ?
C13 C14 1.447(2) . ?
C14 C15 1.363(3) . ?
C14 C18 1.536(2) . ?
C15 C16 1.423(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.531(2) . ?
C17 C172 1.523(3) . ?
C17 C173 1.524(3) . ?
C17 C171 1.534(3) . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C173 H17G 0.9800 . ?
C173 H17H 0.9800 . ?
C173 H17I 0.9800 . ?
C18 C183 1.532(3) . ?
C18 C182 1.540(3) . ?
C18 C181 1.543(3) . ?
C181 H18A 0.9800 . ?
C181 H18B 0.9800 . ?
C181 H18C 0.9800 . ?
C182 H18D 0.9800 . ?
C182 H18E 0.9800 . ?
C182 H18F 0.9800 . ?
C183 H18G 0.9800 . ?
C183 H18H 0.9800 . ?
C183 H18I 0.9800 . ?
C19 H19 0.93(2) . ?
C21 C26 1.385(2) . ?
C21 C22 1.429(2) . ?
C22 C23 1.424(2) . ?
C23 C29 1.400(2) . ?
C23 C24 1.451(2) . ?
C24 C25 1.368(2) . ?
C24 C28 1.534(2) . ?
C25 C26 1.425(2) . ?
C25 H25 0.9500 . ?
C26 C27 1.527(2) . ?
C27 C271 1.527(3) . ?
C27 C272 1.532(3) . ?
C27 C273 1.534(4) . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C273 H27G 0.9800 . ?
C273 H27H 0.9800 . ?
C273 H27I 0.9800 . ?
C28 C282 1.540(3) . ?
C28 C283 1.541(3) . ?
C28 C281 1.542(3) . ?
C281 H28A 0.9800 . ?
C281 H28B 0.9800 . ?
C281 H28C 0.9800 . ?
C282 H28D 0.9800 . ?
C282 H28E 0.9800 . ?
C282 H28F 0.9800 . ?
C283 H28G 0.9800 . ?
C283 H28H 0.9800 . ?
C283 H28I 0.9800 . ?
C29 H29 0.95(2) . ?
C31 C36 1.387(2) . ?
C31 C32 1.396(3) . ?
C32 C33 1.386(2) . ?
C33 C34 1.395(3) . ?
C33 C1 1.509(3) . ?
C34 C35 1.376(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.384(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C41 C42 1.385(3) . ?
C41 C46 1.403(2) . ?
C42 C43 1.382(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.373(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.391(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.386(2) . ?
C45 C1 1.515(3) . ?
C1 C3 1.538(3) . ?
C1 C2 1.540(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 CL3 1.748(2) . ?
C4 CL1 1.748(2) . ?
C4 CL2 1.757(2) . ?
C4 H4 1.0000 . ?

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
O3 ZR O3 134.19(7) . 2_655 ?
O3 ZR O1 142.12(4) . 2_655 ?
O3 ZR O1 77.93(5) 2_655 2_655 ?
O3 ZR O1 77.93(5) . . ?
O3 ZR O1 142.12(4) 2_655 . ?
O1 ZR O1 83.62(7) 2_655 . ?
O3 ZR O4 77.14(4) . 2_655 ?
O3 ZR O4 70.76(4) 2_655 2_655 ?
O1 ZR O4 102.97(5) 2_655 2_655 ?
O1 ZR O4 146.40(4) . 2_655 ?
O3 ZR O4 70.77(4) . . ?
O3 ZR O4 77.13(4) 2_655 . ?
O1 ZR O4 146.39(4) 2_655 . ?
O1 ZR O4 102.97(5) . . ?
O4 ZR O4 89.64(6) 2_655 . ?
O3 ZR O2 123.72(4) . . ?
O3 ZR O2 73.91(4) 2_655 . ?
O1 ZR O2 78.83(4) 2_655 . ?
O1 ZR O2 70.19(4) . . ?
O4 ZR O2 143.28(4) 2_655 . ?
O4 ZR O2 72.86(4) . . ?
O3 ZR O2 73.91(4) . 2_655 ?
O3 ZR O2 123.72(4) 2_655 2_655 ?
O1 ZR O2 70.19(4) 2_655 2_655 ?
O1 ZR O2 78.83(4) . 2_655 ?
O4 ZR O2 72.86(4) 2_655 2_655 ?
O4 ZR O2 143.28(4) . 2_655 ?
O2 ZR O2 138.13(6) . 2_655 ?
C11 O1 ZR 118.96(10) . . ?
C12 O2 ZR 115.61(10) . . ?
C21 O3 ZR 120.53(10) . . ?
C22 O4 ZR 117.91(10) . . ?
C46 O5 C32 117.93(13) . . ?
C19 N1 C31 122.11(15) . . ?
C19 N1 H1 113.4(16) . . ?
C31 N1 H1 124.4(16) . . ?
C29 N2 C41 122.18(15) . . ?
C29 N2 H2 115.8(16) . . ?
C41 N2 H2 121.3(16) . . ?
O1 C11 C16 127.01(15) . . ?
O1 C11 C12 113.75(15) . . ?
C16 C11 C12 119.22(15) . . ?
O2 C12 C13 122.43(15) . . ?
O2 C12 C11 115.93(14) . . ?
C13 C12 C11 121.62(15) . . ?
C19 C13 C12 117.32(15) . . ?
C19 C13 C14 124.13(15) . . ?
C12 C13 C14 118.55(15) . . ?
C15 C14 C13 116.73(15) . . ?
C15 C14 C18 120.40(16) . . ?
C13 C14 C18 122.84(16) . . ?
C14 C15 C16 125.78(16) . . ?
C14 C15 H15 117.1 . . ?
C16 C15 H15 117.1 . . ?
C11 C16 C15 117.96(15) . . ?
C11 C16 C17 121.18(15) . . ?
C15 C16 C17 120.86(16) . . ?
C172 C17 C173 109.67(18) . . ?
C172 C17 C16 109.34(16) . . ?
C173 C17 C16 109.55(15) . . ?
C172 C17 C171 108.49(18) . . ?
C173 C17 C171 107.26(19) . . ?
C16 C17 C171 112.49(16) . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C17 C173 H17G 109.5 . . ?
C17 C173 H17H 109.5 . . ?
H17G C173 H17H 109.5 . . ?
C17 C173 H17I 109.5 . . ?
H17G C173 H17I 109.5 . . ?
H17H C173 H17I 109.5 . . ?
C183 C18 C14 110.96(16) . . ?
C183 C18 C182 106.38(18) . . ?
C14 C18 C182 111.74(16) . . ?
C183 C18 C181 105.90(17) . . ?
C14 C18 C181 110.61(15) . . ?
C182 C18 C181 111.03(17) . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C18 C182 H18D 109.5 . . ?
C18 C182 H18E 109.5 . . ?
H18D C182 H18E 109.5 . . ?
C18 C182 H18F 109.5 . . ?
H18D C182 H18F 109.5 . . ?
H18E C182 H18F 109.5 . . ?
C18 C183 H18G 109.5 . . ?
C18 C183 H18H 109.5 . . ?
H18G C183 H18H 109.5 . . ?
C18 C183 H18I 109.5 . . ?
H18G C183 H18I 109.5 . . ?
H18H C183 H18I 109.5 . . ?
N1 C19 C13 124.87(15) . . ?
N1 C19 H19 113.2(14) . . ?
C13 C19 H19 121.8(14) . . ?
O3 C21 C26 126.63(15) . . ?
O3 C21 C22 115.05(14) . . ?
C26 C21 C22 118.26(15) . . ?
O4 C22 C23 122.37(14) . . ?
O4 C22 C21 115.14(14) . . ?
C23 C22 C21 122.48(14) . . ?
C29 C23 C22 117.40(15) . . ?
C29 C23 C24 124.08(15) . . ?
C22 C23 C24 118.47(14) . . ?
C25 C24 C23 116.48(15) . . ?
C25 C24 C28 120.63(15) . . ?
C23 C24 C28 122.87(15) . . ?
C24 C25 C26 125.76(16) . . ?
C24 C25 H25 117.1 . . ?
C26 C25 H25 117.1 . . ?
C21 C26 C25 118.33(15) . . ?
C21 C26 C27 120.24(16) . . ?
C25 C26 C27 121.42(15) . . ?
C271 C27 C26 109.33(18) . . ?
C271 C27 C272 108.7(2) . . ?
C26 C27 C272 112.69(16) . . ?
C271 C27 C273 109.5(2) . . ?
C26 C27 C273 108.95(17) . . ?
C272 C27 C273 107.6(2) . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C27 C273 H27G 109.5 . . ?
C27 C273 H27H 109.5 . . ?
H27G C273 H27H 109.5 . . ?
C27 C273 H27I 109.5 . . ?
H27G C273 H27I 109.5 . . ?
H27H C273 H27I 109.5 . . ?
C24 C28 C282 111.88(16) . . ?
C24 C28 C283 111.88(15) . . ?
C282 C28 C283 105.73(17) . . ?
C24 C28 C281 110.02(16) . . ?
C282 C28 C281 111.69(17) . . ?
C283 C28 C281 105.41(16) . . ?
C28 C281 H28A 109.5 . . ?
C28 C281 H28B 109.5 . . ?
H28A C281 H28B 109.5 . . ?
C28 C281 H28C 109.5 . . ?
H28A C281 H28C 109.5 . . ?
H28B C281 H28C 109.5 . . ?
C28 C282 H28D 109.5 . . ?
C28 C282 H28E 109.5 . . ?
H28D C282 H28E 109.5 . . ?
C28 C282 H28F 109.5 . . ?
H28D C282 H28F 109.5 . . ?
H28E C282 H28F 109.5 . . ?
C28 C283 H28G 109.5 . . ?
C28 C283 H28H 109.5 . . ?
H28G C283 H28H 109.5 . . ?
C28 C283 H28I 109.5 . . ?
H28G C283 H28I 109.5 . . ?
H28H C283 H28I 109.5 . . ?
N2 C29 C23 125.25(16) . . ?
N2 C29 H29 112.6(14) . . ?
C23 C29 H29 122.0(14) . . ?
C36 C31 C32 119.57(16) . . ?
C36 C31 N1 120.47(17) . . ?
C32 C31 N1 119.96(15) . . ?
O5 C32 C33 123.65(16) . . ?
O5 C32 C31 115.36(14) . . ?
C33 C32 C31 120.99(16) . . ?
C32 C33 C34 117.88(17) . . ?
C32 C33 C1 122.15(16) . . ?
C34 C33 C1 119.96(16) . . ?
C35 C34 C33 121.89(17) . . ?
C35 C34 H34 119.1 . . ?
C33 C34 H34 119.1 . . ?
C34 C35 C36 119.49(17) . . ?
C34 C35 H35 120.3 . . ?
C36 C35 H35 120.3 . . ?
C35 C36 C31 120.11(18) . . ?
C35 C36 H36 119.9 . . ?
C31 C36 H36 119.9 . . ?
C42 C41 C46 119.12(16) . . ?
C42 C41 N2 120.31(16) . . ?
C46 C41 N2 120.54(16) . . ?
C43 C42 C41 120.07(18) . . ?
C43 C42 H42 120.0 . . ?
C41 C42 H42 120.0 . . ?
C44 C43 C42 120.21(19) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 121.32(17) . . ?
C43 C44 H44 119.3 . . ?
C45 C44 H44 119.3 . . ?
C46 C45 C44 118.24(17) . . ?
C46 C45 C1 122.38(17) . . ?
C44 C45 C1 119.38(16) . . ?
O5 C46 C45 123.35(15) . . ?
O5 C46 C41 115.63(14) . . ?
C45 C46 C41 121.02(16) . . ?
C33 C1 C45 110.34(14) . . ?
C33 C1 C3 109.88(17) . . ?
C45 C1 C3 109.25(16) . . ?
C33 C1 C2 108.37(16) . . ?
C45 C1 C2 109.27(17) . . ?
C3 C1 C2 109.72(17) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
CL3 C4 CL1 110.25(11) . . ?
CL3 C4 CL2 109.89(11) . . ?
CL1 C4 CL2 110.62(11) . . ?
CL3 C4 H4 108.7 . . ?
CL1 C4 H4 108.7 . . ?
CL2 C4 H4 108.7 . . ?

_refine_diff_density_max         0.861
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.074



