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

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

data_dyl119
_database_code_depnum_ccdc_archive 'CCDC 1539663'
_audit_update_record             
;
2017-03-22 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C39 H58 Hf N4 O4'
_chemical_formula_sum            'C39 H58 Hf N4 O4'
_chemical_formula_weight         825.38

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'
Hf Hf -0.5830 6.1852 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'

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

_cell_length_a                   10.9194(2)
_cell_length_b                   10.6543(2)
_cell_length_c                   16.9439(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.216(2)
_cell_angle_gamma                90.00
_cell_volume                     1945.77(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4050
_cell_measurement_theta_min      3.8260
_cell_measurement_theta_max      28.9750

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             848
_exptl_absorpt_coefficient_mu    2.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87211
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7114
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5153
_reflns_number_gt                4826
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_chemical_absolute_configuration s
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0200P)²+1.2000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.026(9)
_refine_ls_number_reflns         5153
_refine_ls_number_parameters     433
_refine_ls_number_restraints     49
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0602
_refine_ls_wR_factor_gt          0.0581
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_restrained_S_all      1.015
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.009196(16) 0.14439(4) 0.208655(11) 0.01906(7) Uani 1 1 d . . .
O1 O -0.0547(4) 0.2849(5) 0.1216(3) 0.0217(13) Uani 1 1 d . . .
O2 O 0.0871(3) 0.0454(4) 0.3052(2) 0.0224(9) Uani 1 1 d . . .
O3 O -0.0133(5) 0.0193(6) 0.1265(3) 0.0326(15) Uani 1 1 d . . .
O4 O -0.1428(3) 0.1592(8) 0.2513(2) 0.0278(11) Uani 1 1 d . . .
N1 N -0.2088(5) 0.4416(5) 0.1105(3) 0.0290(12) Uani 1 1 d . . .
N2 N -0.2361(5) 0.5484(5) 0.1520(3) 0.0354(13) Uani 1 1 d . . .
N3 N 0.1051(4) 0.3219(5) 0.2666(3) 0.0230(11) Uani 1 1 d . . .
N4 N 0.2257(3) 0.1362(9) 0.1945(2) 0.0205(11) Uani 1 1 d . . .
C1 C -0.2812(7) 0.2893(6) 0.0054(4) 0.0439(19) Uani 1 1 d . . .
H1A H -0.2102 0.2413 0.0203 0.053 Uiso 1 1 calc R . .
C2 C -0.3717(7) 0.2508(7) -0.0575(5) 0.049(2) Uani 1 1 d . . .
H2B H -0.3603 0.1769 -0.0847 0.058 Uiso 1 1 calc R . .
C3 C -0.4774(7) 0.3207(8) -0.0799(4) 0.049(2) Uani 1 1 d . . .
H3A H -0.5378 0.2947 -0.1218 0.058 Uiso 1 1 calc R . .
C4 C -0.4920(6) 0.4285(8) -0.0394(4) 0.047(2) Uani 1 1 d . . .
H4A H -0.5632 0.4762 -0.0544 0.057 Uiso 1 1 calc R . .
C5 C -0.4050(6) 0.4691(7) 0.0227(4) 0.0379(17) Uani 1 1 d . . .
H5A H -0.4179 0.5429 0.0495 0.046 Uiso 1 1 calc R . .
C6 C -0.2978(6) 0.3998(6) 0.0457(4) 0.0314(15) Uani 1 1 d . . .
C7 C -0.1015(5) 0.3867(6) 0.1482(4) 0.0239(14) Uani 1 1 d . . .
C8 C -0.0575(5) 0.4603(5) 0.2152(3) 0.0234(13) Uani 1 1 d . . .
C9 C -0.1453(6) 0.5597(6) 0.2122(4) 0.0315(15) Uani 1 1 d . . .
C10 C -0.1542(6) 0.6689(8) 0.2671(4) 0.047(2) Uani 1 1 d U . .
H10A H -0.2260 0.7183 0.2470 0.070 Uiso 1 1 calc R . .
H10B H -0.0811 0.7199 0.2700 0.070 Uiso 1 1 calc R . .
H10C H -0.1612 0.6384 0.3195 0.070 Uiso 1 1 calc R . .
C11 C 0.0569(5) 0.4356(6) 0.2669(3) 0.0229(13) Uani 1 1 d . . .
C12 C 0.2328(6) 0.2950(6) 0.3052(4) 0.0231(16) Uani 1 1 d . . .
H12A H 0.2320 0.2376 0.3496 0.028 Uiso 1 1 calc R . .
H12B H 0.2734 0.3719 0.3258 0.028 Uiso 1 1 calc R . .
C13 C 0.3023(6) 0.2368(6) 0.2439(4) 0.0261(16) Uani 1 1 d U . .
H13A H 0.3777 0.1973 0.2723 0.031 Uiso 1 1 calc R . .
C14 C 0.3396(6) 0.3281(6) 0.1841(4) 0.0340(16) Uani 1 1 d . . .
H14A H 0.2777 0.3933 0.1715 0.041 Uiso 1 1 calc R . .
H14B H 0.4189 0.3667 0.2044 0.041 Uiso 1 1 calc R . .
C15 C 0.3484(6) 0.2483(7) 0.1119(4) 0.0384(17) Uani 1 1 d . . .
H15A H 0.4240 0.1989 0.1194 0.046 Uiso 1 1 calc R . .
H15B H 0.3449 0.2991 0.0641 0.046 Uiso 1 1 calc R . .
C16 C 0.2350(5) 0.1661(11) 0.1080(3) 0.031(2) Uani 1 1 d . . .
H16A H 0.2444 0.0898 0.0783 0.037 Uiso 1 1 calc R . .
H16B H 0.1614 0.2101 0.0825 0.037 Uiso 1 1 calc R . .
C17 C 0.2761(6) 0.0081(7) 0.2123(4) 0.0256(15) Uani 1 1 d . . .
H17A H 0.3576 0.0037 0.1966 0.031 Uiso 1 1 calc R . .
H17B H 0.2232 -0.0512 0.1794 0.031 Uiso 1 1 calc R . .
C18 C 0.2874(6) -0.0336(6) 0.2985(4) 0.0197(15) Uani 1 1 d . . .
C19 C 0.3911(5) -0.0992(5) 0.3340(4) 0.0263(14) Uani 1 1 d . . .
H19A H 0.4570 -0.1087 0.3059 0.032 Uiso 1 1 calc R . .
C20 C 0.4010(5) -0.1517(5) 0.4104(4) 0.0251(14) Uani 1 1 d . . .
C21 C 0.3029(5) -0.1275(5) 0.4516(4) 0.0260(14) Uani 1 1 d . . .
H21A H 0.3086 -0.1574 0.5036 0.031 Uiso 1 1 calc R . .
C22 C 0.1969(5) -0.0611(5) 0.4192(3) 0.0191(12) Uani 1 1 d . . .
C23 C 0.1879(5) -0.0152(5) 0.3408(4) 0.0199(13) Uani 1 1 d . . .
C24 C 0.1195(6) 0.5418(6) 0.3165(4) 0.0296(15) Uani 1 1 d . . .
H24A H 0.1775 0.5072 0.3604 0.036 Uiso 1 1 calc R . .
H24B H 0.0573 0.5887 0.3392 0.036 Uiso 1 1 calc R . .
C25 C 0.1881(6) 0.6307(11) 0.2697(4) 0.051(2) Uani 1 1 d . . .
H25A H 0.2258 0.6960 0.3043 0.076 Uiso 1 1 calc R . .
H25B H 0.1309 0.6671 0.2268 0.076 Uiso 1 1 calc R . .
H25C H 0.2512 0.5855 0.2480 0.076 Uiso 1 1 calc R . .
C26 C 0.5143(6) -0.2289(6) 0.4460(4) 0.0361(17) Uani 1 1 d . . .
C27 C 0.6299(7) -0.1462(8) 0.4574(5) 0.061(2) Uani 1 1 d U . .
H27A H 0.6408 -0.1108 0.4069 0.092 Uiso 1 1 calc R . .
H27B H 0.7012 -0.1958 0.4781 0.092 Uiso 1 1 calc R . .
H27C H 0.6204 -0.0799 0.4943 0.092 Uiso 1 1 calc R . .
C28 C 0.5290(7) -0.3395(12) 0.3925(4) 0.065(2) Uani 1 1 d U . .
H28A H 0.5366 -0.3099 0.3400 0.098 Uiso 1 1 calc R . .
H28B H 0.4576 -0.3930 0.3893 0.098 Uiso 1 1 calc R . .
H28C H 0.6020 -0.3859 0.4142 0.098 Uiso 1 1 calc R . .
C29 C 0.5026(7) -0.2821(7) 0.5286(5) 0.052(2) Uani 1 1 d U . .
H29A H 0.5756 -0.3298 0.5487 0.078 Uiso 1 1 calc R . .
H29B H 0.4310 -0.3355 0.5242 0.078 Uiso 1 1 calc R . .
H29C H 0.4939 -0.2143 0.5646 0.078 Uiso 1 1 calc R . .
C30 C 0.0889(5) -0.0411(5) 0.4673(3) 0.0218(13) Uani 1 1 d . . .
C31 C 0.1162(6) -0.0979(6) 0.5503(4) 0.0320(16) Uani 1 1 d . . .
H31A H 0.0472 -0.0834 0.5778 0.048 Uiso 1 1 calc R . .
H31B H 0.1893 -0.0596 0.5796 0.048 Uiso 1 1 calc R . .
H31C H 0.1295 -0.1866 0.5461 0.048 Uiso 1 1 calc R . .
C32 C -0.0297(6) -0.1020(6) 0.4222(4) 0.0299(15) Uani 1 1 d . . .
H32A H -0.0966 -0.0898 0.4519 0.045 Uiso 1 1 calc R . .
H32B H -0.0160 -0.1903 0.4161 0.045 Uiso 1 1 calc R . .
H32C H -0.0505 -0.0640 0.3704 0.045 Uiso 1 1 calc R . .
C33 C 0.0663(6) 0.0997(5) 0.4764(4) 0.0321(15) Uani 1 1 d . . .
H33A H -0.0005 0.1119 0.5062 0.048 Uiso 1 1 calc R . .
H33B H 0.0450 0.1371 0.4244 0.048 Uiso 1 1 calc R . .
H33C H 0.1402 0.1384 0.5042 0.048 Uiso 1 1 calc R . .
C34 C -0.0240(7) -0.0639(6) 0.0607(4) 0.0382(17) Uani 1 1 d . . .
H34A H 0.0591 -0.0754 0.0470 0.046 Uiso 1 1 calc R . .
C35 C -0.1049(7) -0.0091(7) -0.0110(4) 0.0455(19) Uani 1 1 d . . .
H35A H -0.0722 0.0708 -0.0236 0.068 Uiso 1 1 calc R . .
H35B H -0.1875 0.0018 0.0004 0.068 Uiso 1 1 calc R . .
H35C H -0.1066 -0.0647 -0.0557 0.068 Uiso 1 1 calc R . .
C36 C -0.0675(9) -0.1874(8) 0.0845(5) 0.069(3) Uani 1 1 d U . .
H36A H -0.0125 -0.2177 0.1305 0.103 Uiso 1 1 calc R . .
H36B H -0.0687 -0.2457 0.0412 0.103 Uiso 1 1 calc R . .
H36C H -0.1497 -0.1792 0.0973 0.103 Uiso 1 1 calc R . .
C37 C -0.2531(5) 0.1546(14) 0.2833(4) 0.0396(16) Uani 1 1 d . . .
H37A H -0.2319 0.1418 0.3411 0.047 Uiso 1 1 calc R . .
C38 C -0.3223(9) 0.2734(10) 0.2695(6) 0.047(2) Uani 1 1 d U . .
H38A H -0.2714 0.3413 0.2931 0.070 Uiso 1 1 calc R . .
H38B H -0.3962 0.2688 0.2934 0.070 Uiso 1 1 calc R . .
H38C H -0.3445 0.2875 0.2131 0.070 Uiso 1 1 calc R . .
C39 C -0.3256(11) 0.0436(11) 0.2484(7) 0.077(4) Uani 1 1 d U . .
H39A H -0.2762 -0.0308 0.2590 0.115 Uiso 1 1 calc R . .
H39B H -0.3479 0.0546 0.1917 0.115 Uiso 1 1 calc R . .
H39C H -0.3995 0.0356 0.2720 0.115 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O3 1.915(6) . ?
Hf1 O4 1.920(3) . ?
Hf1 O2 2.017(4) . ?
Hf1 O1 2.138(5) . ?
Hf1 N3 2.304(5) . ?
Hf1 N4 2.416(4) . ?
O1 C7 1.309(8) . ?
O2 C23 1.333(7) . ?
O3 C34 1.413(8) . ?
O4 C37 1.399(6) . ?
N1 C7 1.372(7) . ?
N1 N2 1.395(7) . ?
N1 C6 1.417(8) . ?
N2 C9 1.308(8) . ?
N3 C11 1.321(7) . ?
N3 C12 1.471(8) . ?
N4 C17 1.484(11) . ?
N4 C16 1.518(7) . ?
N4 C13 1.525(10) . ?
C1 C6 1.386(9) . ?
C1 C2 1.395(9) . ?
C1 H1A 0.9300 . ?
C2 C3 1.375(10) . ?
C2 H2B 0.9300 . ?
C3 C4 1.360(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.371(10) . ?
C4 H4A 0.9300 . ?
C5 C6 1.386(8) . ?
C5 H5A 0.9300 . ?
C7 C8 1.401(8) . ?
C8 C9 1.425(8) . ?
C8 C11 1.430(8) . ?
C9 C10 1.503(9) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C24 1.507(8) . ?
C12 C13 1.515(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.506(9) . ?
C13 H13A 0.9800 . ?
C14 C15 1.505(9) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.510(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.511(9) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.383(8) . ?
C18 C23 1.408(8) . ?
C19 C20 1.398(8) . ?
C19 H19A 0.9300 . ?
C20 C21 1.392(8) . ?
C20 C26 1.527(8) . ?
C21 C22 1.392(8) . ?
C21 H21A 0.9300 . ?
C22 C23 1.405(8) . ?
C22 C30 1.551(7) . ?
C24 C25 1.509(10) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C28 1.511(13) . ?
C26 C27 1.527(10) . ?
C26 C29 1.534(10) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.517(8) . ?
C30 C33 1.533(8) . ?
C30 C32 1.537(8) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C36 1.478(10) . ?
C34 C35 1.502(9) . ?
C34 H34A 0.9800 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 C38 1.474(16) . ?
C37 C39 1.492(16) . ?
C37 H37A 0.9800 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?

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 Hf1 O4 108.2(3) . . ?
O3 Hf1 O2 102.4(2) . . ?
O4 Hf1 O2 90.91(19) . . ?
O3 Hf1 O1 89.78(15) . . ?
O4 Hf1 O1 89.7(2) . . ?
O2 Hf1 O1 166.97(19) . . ?
O3 Hf1 N3 151.4(2) . . ?
O4 Hf1 N3 97.7(2) . . ?
O2 Hf1 N3 88.82(19) . . ?
O1 Hf1 N3 78.2(2) . . ?
O3 Hf1 N4 85.2(2) . . ?
O4 Hf1 N4 163.57(15) . . ?
O2 Hf1 N4 76.65(18) . . ?
O1 Hf1 N4 100.0(2) . . ?
N3 Hf1 N4 71.8(2) . . ?
C7 O1 Hf1 116.4(4) . . ?
C23 O2 Hf1 146.1(4) . . ?
C34 O3 Hf1 173.8(5) . . ?
C37 O4 Hf1 173.2(8) . . ?
C7 N1 N2 110.4(5) . . ?
C7 N1 C6 130.9(5) . . ?
N2 N1 C6 118.2(5) . . ?
C9 N2 N1 105.8(5) . . ?
C11 N3 C12 121.8(5) . . ?
C11 N3 Hf1 126.9(4) . . ?
C12 N3 Hf1 111.3(4) . . ?
C17 N4 C16 108.1(6) . . ?
C17 N4 C13 112.4(5) . . ?
C16 N4 C13 105.5(6) . . ?
C17 N4 Hf1 110.5(4) . . ?
C16 N4 Hf1 107.8(3) . . ?
C13 N4 Hf1 112.3(4) . . ?
C6 C1 C2 119.6(7) . . ?
C6 C1 H1A 120.2 . . ?
C2 C1 H1A 120.2 . . ?
C3 C2 C1 120.8(7) . . ?
C3 C2 H2B 119.6 . . ?
C1 C2 H2B 119.6 . . ?
C4 C3 C2 118.6(7) . . ?
C4 C3 H3A 120.7 . . ?
C2 C3 H3A 120.7 . . ?
C3 C4 C5 122.1(7) . . ?
C3 C4 H4A 118.9 . . ?
C5 C4 H4A 118.9 . . ?
C4 C5 C6 119.9(7) . . ?
C4 C5 H5A 120.1 . . ?
C6 C5 H5A 120.1 . . ?
C5 C6 C1 119.0(6) . . ?
C5 C6 N1 119.6(6) . . ?
C1 C6 N1 121.4(6) . . ?
O1 C7 N1 123.0(5) . . ?
O1 C7 C8 129.8(5) . . ?
N1 C7 C8 107.1(5) . . ?
C7 C8 C9 104.2(5) . . ?
C7 C8 C11 123.1(5) . . ?
C9 C8 C11 132.5(6) . . ?
N2 C9 C8 112.4(6) . . ?
N2 C9 C10 116.0(6) . . ?
C8 C9 C10 131.6(6) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 C8 118.4(5) . . ?
N3 C11 C24 123.1(5) . . ?
C8 C11 C24 118.4(5) . . ?
N3 C12 C13 108.6(5) . . ?
N3 C12 H12A 110.0 . . ?
C13 C12 H12A 110.0 . . ?
N3 C12 H12B 110.0 . . ?
C13 C12 H12B 110.0 . . ?
H12A C12 H12B 108.4 . . ?
C14 C13 C12 114.6(6) . . ?
C14 C13 N4 105.6(5) . . ?
C12 C13 N4 111.9(5) . . ?
C14 C13 H13A 108.2 . . ?
C12 C13 H13A 108.2 . . ?
N4 C13 H13A 108.2 . . ?
C15 C14 C13 104.0(6) . . ?
C15 C14 H14A 111.0 . . ?
C13 C14 H14A 111.0 . . ?
C15 C14 H14B 111.0 . . ?
C13 C14 H14B 111.0 . . ?
H14A C14 H14B 109.0 . . ?
C14 C15 C16 101.8(5) . . ?
C14 C15 H15A 111.4 . . ?
C16 C15 H15A 111.4 . . ?
C14 C15 H15B 111.4 . . ?
C16 C15 H15B 111.4 . . ?
H15A C15 H15B 109.3 . . ?
C15 C16 N4 105.1(5) . . ?
C15 C16 H16A 110.7 . . ?
N4 C16 H16A 110.7 . . ?
C15 C16 H16B 110.7 . . ?
N4 C16 H16B 110.7 . . ?
H16A C16 H16B 108.8 . . ?
N4 C17 C18 115.9(5) . . ?
N4 C17 H17A 108.3 . . ?
C18 C17 H17A 108.3 . . ?
N4 C17 H17B 108.3 . . ?
C18 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C19 C18 C23 119.5(6) . . ?
C19 C18 C17 120.2(6) . . ?
C23 C18 C17 120.0(6) . . ?
C18 C19 C20 122.8(6) . . ?
C18 C19 H19A 118.6 . . ?
C20 C19 H19A 118.6 . . ?
C21 C20 C19 116.0(5) . . ?
C21 C20 C26 122.8(6) . . ?
C19 C20 C26 121.3(6) . . ?
C20 C21 C22 123.7(6) . . ?
C20 C21 H21A 118.2 . . ?
C22 C21 H21A 118.2 . . ?
C21 C22 C23 118.5(5) . . ?
C21 C22 C30 121.2(5) . . ?
C23 C22 C30 120.3(5) . . ?
O2 C23 C22 121.6(5) . . ?
O2 C23 C18 119.1(6) . . ?
C22 C23 C18 119.4(5) . . ?
C11 C24 C25 113.4(6) . . ?
C11 C24 H24A 108.9 . . ?
C25 C24 H24A 108.9 . . ?
C11 C24 H24B 108.9 . . ?
C25 C24 H24B 108.9 . . ?
H24A C24 H24B 107.7 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28 C26 C27 111.1(6) . . ?
C28 C26 C20 109.9(6) . . ?
C27 C26 C20 109.9(6) . . ?
C28 C26 C29 107.0(7) . . ?
C27 C26 C29 106.7(6) . . ?
C20 C26 C29 112.3(6) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C33 107.9(5) . . ?
C31 C30 C32 108.5(5) . . ?
C33 C30 C32 109.1(5) . . ?
C31 C30 C22 112.3(5) . . ?
C33 C30 C22 109.6(5) . . ?
C32 C30 C22 109.4(5) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O3 C34 C36 109.5(6) . . ?
O3 C34 C35 111.0(6) . . ?
C36 C34 C35 113.2(6) . . ?
O3 C34 H34A 107.7 . . ?
C36 C34 H34A 107.7 . . ?
C35 C34 H34A 107.7 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O4 C37 C38 111.1(10) . . ?
O4 C37 C39 108.0(9) . . ?
C38 C37 C39 113.1(6) . . ?
O4 C37 H37A 108.2 . . ?
C38 C37 H37A 108.2 . . ?
C39 C37 H37A 108.2 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Hf1 O1 C7 155.8(5) . . . . ?
O4 Hf1 O1 C7 47.6(5) . . . . ?
O2 Hf1 O1 C7 -45.3(10) . . . . ?
N3 Hf1 O1 C7 -50.3(4) . . . . ?
N4 Hf1 O1 C7 -119.1(5) . . . . ?
O3 Hf1 O2 C23 70.0(7) . . . . ?
O4 Hf1 O2 C23 178.9(7) . . . . ?
O1 Hf1 O2 C23 -88.3(11) . . . . ?
N3 Hf1 O2 C23 -83.4(7) . . . . ?
N4 Hf1 O2 C23 -11.9(7) . . . . ?
O4 Hf1 O3 C34 133(4) . . . . ?
O2 Hf1 O3 C34 -132(4) . . . . ?
O1 Hf1 O3 C34 44(4) . . . . ?
N3 Hf1 O3 C34 -21(5) . . . . ?
N4 Hf1 O3 C34 -56(5) . . . . ?
O3 Hf1 O4 C37 50(3) . . . . ?
O2 Hf1 O4 C37 -53(3) . . . . ?
O1 Hf1 O4 C37 140(3) . . . . ?
N3 Hf1 O4 C37 -142(3) . . . . ?
N4 Hf1 O4 C37 -93(3) . . . . ?
C7 N1 N2 C9 1.7(7) . . . . ?
C6 N1 N2 C9 174.5(6) . . . . ?
O3 Hf1 N3 C11 106.5(6) . . . . ?
O4 Hf1 N3 C11 -48.5(5) . . . . ?
O2 Hf1 N3 C11 -139.3(5) . . . . ?
O1 Hf1 N3 C11 39.6(5) . . . . ?
N4 Hf1 N3 C11 144.4(5) . . . . ?
O3 Hf1 N3 C12 -73.1(6) . . . . ?
O4 Hf1 N3 C12 131.8(4) . . . . ?
O2 Hf1 N3 C12 41.1(4) . . . . ?
O1 Hf1 N3 C12 -140.0(5) . . . . ?
N4 Hf1 N3 C12 -35.2(4) . . . . ?
O3 Hf1 N4 C17 -60.3(4) . . . . ?
O4 Hf1 N4 C17 85.3(14) . . . . ?
O2 Hf1 N4 C17 43.6(4) . . . . ?
O1 Hf1 N4 C17 -149.2(4) . . . . ?
N3 Hf1 N4 C17 136.8(4) . . . . ?
O3 Hf1 N4 C16 57.6(6) . . . . ?
O4 Hf1 N4 C16 -156.9(11) . . . . ?
O2 Hf1 N4 C16 161.5(7) . . . . ?
O1 Hf1 N4 C16 -31.4(7) . . . . ?
N3 Hf1 N4 C16 -105.3(7) . . . . ?
O3 Hf1 N4 C13 173.3(5) . . . . ?
O4 Hf1 N4 C13 -41.1(16) . . . . ?
O2 Hf1 N4 C13 -82.8(4) . . . . ?
O1 Hf1 N4 C13 84.4(5) . . . . ?
N3 Hf1 N4 C13 10.4(4) . . . . ?
C6 C1 C2 C3 -0.3(12) . . . . ?
C1 C2 C3 C4 0.2(12) . . . . ?
C2 C3 C4 C5 -0.2(11) . . . . ?
C3 C4 C5 C6 0.4(11) . . . . ?
C4 C5 C6 C1 -0.6(10) . . . . ?
C4 C5 C6 N1 -179.4(6) . . . . ?
C2 C1 C6 C5 0.5(11) . . . . ?
C2 C1 C6 N1 179.3(7) . . . . ?
C7 N1 C6 C5 174.6(6) . . . . ?
N2 N1 C6 C5 3.5(9) . . . . ?
C7 N1 C6 C1 -4.1(11) . . . . ?
N2 N1 C6 C1 -175.2(6) . . . . ?
Hf1 O1 C7 N1 -135.6(5) . . . . ?
Hf1 O1 C7 C8 45.2(9) . . . . ?
N2 N1 C7 O1 -179.9(6) . . . . ?
C6 N1 C7 O1 8.5(10) . . . . ?
N2 N1 C7 C8 -0.6(7) . . . . ?
C6 N1 C7 C8 -172.2(6) . . . . ?
O1 C7 C8 C9 178.6(6) . . . . ?
N1 C7 C8 C9 -0.6(7) . . . . ?
O1 C7 C8 C11 2.7(11) . . . . ?
N1 C7 C8 C11 -176.6(5) . . . . ?
N1 N2 C9 C8 -2.1(7) . . . . ?
N1 N2 C9 C10 -179.5(5) . . . . ?
C7 C8 C9 N2 1.8(7) . . . . ?
C11 C8 C9 N2 177.1(6) . . . . ?
C7 C8 C9 C10 178.6(7) . . . . ?
C11 C8 C9 C10 -6.1(12) . . . . ?
C12 N3 C11 C8 167.7(6) . . . . ?
Hf1 N3 C11 C8 -11.9(8) . . . . ?
C12 N3 C11 C24 -9.7(9) . . . . ?
Hf1 N3 C11 C24 170.7(4) . . . . ?
C7 C8 C11 N3 -20.3(9) . . . . ?
C9 C8 C11 N3 165.0(6) . . . . ?
C7 C8 C11 C24 157.2(6) . . . . ?
C9 C8 C11 C24 -17.4(10) . . . . ?
C11 N3 C12 C13 -124.2(6) . . . . ?
Hf1 N3 C12 C13 55.4(6) . . . . ?
N3 C12 C13 C14 75.3(7) . . . . ?
N3 C12 C13 N4 -44.8(8) . . . . ?
C17 N4 C13 C14 123.9(6) . . . . ?
C16 N4 C13 C14 6.4(7) . . . . ?
Hf1 N4 C13 C14 -110.7(5) . . . . ?
C17 N4 C13 C12 -110.8(5) . . . . ?
C16 N4 C13 C12 131.7(6) . . . . ?
Hf1 N4 C13 C12 14.6(7) . . . . ?
C12 C13 C14 C15 -153.9(5) . . . . ?
N4 C13 C14 C15 -30.3(7) . . . . ?
C13 C14 C15 C16 42.3(7) . . . . ?
C14 C15 C16 N4 -38.3(8) . . . . ?
C17 N4 C16 C15 -100.6(7) . . . . ?
C13 N4 C16 C15 19.8(8) . . . . ?
Hf1 N4 C16 C15 140.0(5) . . . . ?
C16 N4 C17 C18 173.7(5) . . . . ?
C13 N4 C17 C18 57.7(6) . . . . ?
Hf1 N4 C17 C18 -68.6(6) . . . . ?
N4 C17 C18 C19 -138.7(6) . . . . ?
N4 C17 C18 C23 46.8(8) . . . . ?
C23 C18 C19 C20 1.6(9) . . . . ?
C17 C18 C19 C20 -172.9(6) . . . . ?
C18 C19 C20 C21 -4.0(9) . . . . ?
C18 C19 C20 C26 177.0(6) . . . . ?
C19 C20 C21 C22 3.3(9) . . . . ?
C26 C20 C21 C22 -177.7(6) . . . . ?
C20 C21 C22 C23 -0.3(9) . . . . ?
C20 C21 C22 C30 178.0(5) . . . . ?
Hf1 O2 C23 C22 173.0(5) . . . . ?
Hf1 O2 C23 C18 -7.1(10) . . . . ?
C21 C22 C23 O2 177.7(5) . . . . ?
C30 C22 C23 O2 -0.6(8) . . . . ?
C21 C22 C23 C18 -2.2(8) . . . . ?
C30 C22 C23 C18 179.5(5) . . . . ?
C19 C18 C23 O2 -178.3(5) . . . . ?
C17 C18 C23 O2 -3.7(9) . . . . ?
C19 C18 C23 C22 1.6(9) . . . . ?
C17 C18 C23 C22 176.2(6) . . . . ?
N3 C11 C24 C25 99.4(7) . . . . ?
C8 C11 C24 C25 -78.0(7) . . . . ?
C21 C20 C26 C28 122.5(7) . . . . ?
C19 C20 C26 C28 -58.5(8) . . . . ?
C21 C20 C26 C27 -114.9(7) . . . . ?
C19 C20 C26 C27 64.0(8) . . . . ?
C21 C20 C26 C29 3.6(9) . . . . ?
C19 C20 C26 C29 -177.4(6) . . . . ?
C21 C22 C30 C31 1.6(8) . . . . ?
C23 C22 C30 C31 179.8(5) . . . . ?
C21 C22 C30 C33 121.5(6) . . . . ?
C23 C22 C30 C33 -60.3(7) . . . . ?
C21 C22 C30 C32 -118.9(6) . . . . ?
C23 C22 C30 C32 59.3(7) . . . . ?
Hf1 O3 C34 C36 173(4) . . . . ?
Hf1 O3 C34 C35 -62(5) . . . . ?
Hf1 O4 C37 C38 -165(3) . . . . ?
Hf1 O4 C37 C39 -40(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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_dyl1226
_database_code_depnum_ccdc_archive 'CCDC 1539661'
_audit_update_record             
;
2017-03-22 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C43 H58 N4 O4 Zr, C3'
_chemical_formula_sum            'C46 H58 N4 O4 Zr'
_chemical_formula_weight         822.18

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'

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

_cell_length_a                   11.329(2)
_cell_length_b                   17.763(4)
_cell_length_c                   22.612(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4550.4(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6390
_cell_measurement_theta_min      3.7040
_cell_measurement_theta_max      25.2460

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1736
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17693
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.43
_diffrn_reflns_theta_max         24.99
_reflns_number_total             7987
_reflns_number_gt                6908
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_chemical_absolute_configuration s
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0100P)²+11.5000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_number_reflns         7987
_refine_ls_number_parameters     514
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0509
_refine_ls_wR_factor_ref         0.1146
_refine_ls_wR_factor_gt          0.1090
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.012
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.37950(4) -0.41418(2) -0.36548(2) 0.02744(11) Uani 1 1 d . . .
O1 O 0.5392(3) -0.38784(18) -0.31731(14) 0.0307(8) Uani 1 1 d . . .
O2 O 0.2214(3) -0.45501(18) -0.39300(15) 0.0332(8) Uani 1 1 d . . .
O3 O 0.4606(3) -0.4017(2) -0.44037(14) 0.0409(9) Uani 1 1 d . . .
O4 O 0.3168(3) -0.31729(18) -0.34577(16) 0.0409(10) Uani 1 1 d . . .
N1 N 0.6049(4) -0.3068(2) -0.24263(16) 0.0308(9) Uani 1 1 d . . .
N2 N 0.5798(4) -0.2905(2) -0.18318(18) 0.0365(11) Uani 1 1 d . . .
N3 N 0.3478(4) -0.4711(2) -0.27294(16) 0.0285(10) Uani 1 1 d . . .
N4 N 0.4169(3) -0.54978(19) -0.37281(18) 0.0259(9) Uani 1 1 d . . .
C1 C 0.6883(5) -0.2510(3) -0.3307(3) 0.0436(14) Uani 1 1 d . . .
H1A H 0.6242 -0.2682 -0.3525 0.052 Uiso 1 1 calc R . .
C2 C 0.7769(5) -0.2098(3) -0.3583(3) 0.0517(16) Uani 1 1 d . . .
H2B H 0.7715 -0.1987 -0.3984 0.062 Uiso 1 1 calc R . .
C3 C 0.8722(6) -0.1857(3) -0.3261(3) 0.0568(17) Uani 1 1 d . . .
H3A H 0.9326 -0.1591 -0.3446 0.068 Uiso 1 1 calc R . .
C4 C 0.8788(6) -0.2007(3) -0.2666(3) 0.0486(14) Uani 1 1 d . . .
H4A H 0.9428 -0.1829 -0.2450 0.058 Uiso 1 1 calc R . .
C5 C 0.7926(5) -0.2412(3) -0.2387(3) 0.0398(13) Uani 1 1 d . . .
H5A H 0.7985 -0.2521 -0.1986 0.048 Uiso 1 1 calc R . .
C6 C 0.6953(5) -0.2661(3) -0.2715(2) 0.0331(12) Uani 1 1 d . . .
C7 C 0.5322(4) -0.3617(3) -0.2644(2) 0.0286(11) Uani 1 1 d . . .
C8 C 0.4574(4) -0.3828(3) -0.2174(2) 0.0277(11) Uani 1 1 d . . .
C9 C 0.4923(5) -0.3362(3) -0.1689(2) 0.0341(12) Uani 1 1 d . . .
C10 C 0.4396(6) -0.3306(3) -0.1076(2) 0.0454(15) Uani 1 1 d . . .
H10A H 0.4830 -0.2943 -0.0848 0.068 Uiso 1 1 calc R . .
H10B H 0.4437 -0.3788 -0.0885 0.068 Uiso 1 1 calc R . .
H10C H 0.3586 -0.3151 -0.1105 0.068 Uiso 1 1 calc R . .
C11 C 0.3790(5) -0.4459(2) -0.22083(19) 0.0283(10) Uani 1 1 d . . .
C12 C 0.3005(4) -0.5483(3) -0.2787(2) 0.0298(11) Uani 1 1 d . . .
H12A H 0.2233 -0.5473 -0.2972 0.036 Uiso 1 1 calc R . .
H12B H 0.2930 -0.5715 -0.2400 0.036 Uiso 1 1 calc R . .
C13 C 0.3863(5) -0.5920(3) -0.31636(18) 0.0282(10) Uani 1 1 d . . .
H13A H 0.3499 -0.6402 -0.3271 0.034 Uiso 1 1 calc R . .
C14 C 0.5055(5) -0.6078(3) -0.2874(2) 0.0393(13) Uani 1 1 d . . .
H14A H 0.5314 -0.5654 -0.2638 0.047 Uiso 1 1 calc R . .
H14B H 0.5019 -0.6523 -0.2626 0.047 Uiso 1 1 calc R . .
C15 C 0.5869(5) -0.6201(3) -0.3402(3) 0.0481(15) Uani 1 1 d . . .
H15A H 0.6690 -0.6142 -0.3291 0.058 Uiso 1 1 calc R . .
H15B H 0.5756 -0.6697 -0.3573 0.058 Uiso 1 1 calc R . .
C16 C 0.5480(4) -0.5587(3) -0.3826(2) 0.0343(13) Uani 1 1 d . . .
H16A H 0.5889 -0.5119 -0.3741 0.041 Uiso 1 1 calc R . .
H16B H 0.5642 -0.5730 -0.4231 0.041 Uiso 1 1 calc R . .
C17 C 0.3515(4) -0.5808(3) -0.42483(19) 0.0317(11) Uani 1 1 d . . .
H17A H 0.3799 -0.6313 -0.4328 0.038 Uiso 1 1 calc R . .
H17B H 0.3690 -0.5501 -0.4592 0.038 Uiso 1 1 calc R . .
C18 C 0.2202(4) -0.5836(3) -0.41646(19) 0.0279(10) Uani 1 1 d . . .
C19 C 0.1579(5) -0.6512(3) -0.4249(2) 0.0332(13) Uani 1 1 d . . .
H19A H 0.1990 -0.6945 -0.4353 0.040 Uiso 1 1 calc R . .
C20 C 0.0356(5) -0.6544(3) -0.4178(2) 0.0348(13) Uani 1 1 d . . .
C21 C -0.0202(5) -0.5887(3) -0.3998(2) 0.0407(12) Uani 1 1 d . . .
H21A H -0.1012 -0.5905 -0.3933 0.049 Uiso 1 1 calc R . .
C22 C 0.0365(5) -0.5204(3) -0.3908(2) 0.0370(13) Uani 1 1 d . . .
C23 C 0.1597(4) -0.5184(3) -0.4008(2) 0.0304(12) Uani 1 1 d . . .
C24 C 0.3415(5) -0.4820(3) -0.1638(2) 0.0320(12) Uani 1 1 d . . .
C25 C 0.2277(6) -0.4722(3) -0.1443(2) 0.0460(15) Uani 1 1 d . . .
H25A H 0.1730 -0.4469 -0.1677 0.055 Uiso 1 1 calc R . .
C26 C 0.1947(7) -0.5001(4) -0.0892(3) 0.0590(19) Uani 1 1 d . . .
H26A H 0.1178 -0.4929 -0.0760 0.071 Uiso 1 1 calc R . .
C27 C 0.2720(8) -0.5374(4) -0.0546(3) 0.063(2) Uani 1 1 d . . .
H27A H 0.2491 -0.5555 -0.0177 0.076 Uiso 1 1 calc R . .
C28 C 0.3841(8) -0.5480(3) -0.0744(3) 0.0641(19) Uani 1 1 d . . .
H28A H 0.4377 -0.5739 -0.0509 0.077 Uiso 1 1 calc R . .
C29 C 0.4200(5) -0.5206(3) -0.1294(3) 0.0512(15) Uani 1 1 d . . .
H29A H 0.4968 -0.5286 -0.1425 0.061 Uiso 1 1 calc R . .
C30 C -0.0358(5) -0.7271(3) -0.4259(2) 0.0394(13) Uani 1 1 d . . .
C31 C 0.0374(5) -0.7894(3) -0.4545(3) 0.0502(16) Uani 1 1 d . . .
H31A H 0.0663 -0.7725 -0.4921 0.075 Uiso 1 1 calc R . .
H31B H -0.0109 -0.8333 -0.4601 0.075 Uiso 1 1 calc R . .
H31C H 0.1028 -0.8017 -0.4293 0.075 Uiso 1 1 calc R . .
C32 C -0.1430(5) -0.7132(3) -0.4653(3) 0.0539(16) Uani 1 1 d . . .
H32A H -0.1171 -0.6965 -0.5035 0.081 Uiso 1 1 calc R . .
H32B H -0.1920 -0.6752 -0.4477 0.081 Uiso 1 1 calc R . .
H32C H -0.1871 -0.7590 -0.4694 0.081 Uiso 1 1 calc R . .
C33 C -0.0820(5) -0.7543(3) -0.3656(3) 0.0537(15) Uani 1 1 d . . .
H33A H -0.1281 -0.7152 -0.3476 0.081 Uiso 1 1 calc R . .
H33B H -0.0164 -0.7665 -0.3404 0.081 Uiso 1 1 calc R . .
H33C H -0.1301 -0.7982 -0.3710 0.081 Uiso 1 1 calc R . .
C34 C -0.0316(5) -0.4492(3) -0.3713(3) 0.0515(16) Uani 1 1 d . . .
C35 C -0.1640(5) -0.4663(3) -0.3610(4) 0.0632(19) Uani 1 1 d . . .
H35A H -0.2037 -0.4212 -0.3487 0.095 Uiso 1 1 calc R . .
H35B H -0.1719 -0.5040 -0.3308 0.095 Uiso 1 1 calc R . .
H35C H -0.1986 -0.4844 -0.3970 0.095 Uiso 1 1 calc R . .
C36 C 0.0204(5) -0.4208(4) -0.3113(3) 0.068(2) Uani 1 1 d . . .
H36A H -0.0219 -0.3768 -0.2987 0.102 Uiso 1 1 calc R . .
H36B H 0.1023 -0.4085 -0.3165 0.102 Uiso 1 1 calc R . .
H36C H 0.0129 -0.4596 -0.2820 0.102 Uiso 1 1 calc R . .
C37 C -0.0200(6) -0.3878(4) -0.4179(3) 0.068(2) Uani 1 1 d . . .
H37A H -0.0629 -0.3440 -0.4054 0.103 Uiso 1 1 calc R . .
H37B H -0.0517 -0.4056 -0.4547 0.103 Uiso 1 1 calc R . .
H37C H 0.0617 -0.3752 -0.4230 0.103 Uiso 1 1 calc R . .
C38 C 0.5217(8) -0.3690(4) -0.4877(3) 0.071(2) Uani 1 1 d . . .
H38A H 0.5044 -0.3980 -0.5235 0.085 Uiso 1 1 calc R . .
C39 C 0.4829(11) -0.2906(5) -0.4974(4) 0.140(4) Uani 1 1 d U . .
H39A H 0.3996 -0.2899 -0.5052 0.210 Uiso 1 1 calc R . .
H39B H 0.5244 -0.2698 -0.5306 0.210 Uiso 1 1 calc R . .
H39C H 0.4994 -0.2612 -0.4628 0.210 Uiso 1 1 calc R . .
C40 C 0.6474(8) -0.3712(7) -0.4776(4) 0.145(4) Uani 1 1 d U . .
H40A H 0.6719 -0.4224 -0.4719 0.217 Uiso 1 1 calc R . .
H40B H 0.6662 -0.3423 -0.4430 0.217 Uiso 1 1 calc R . .
H40C H 0.6877 -0.3504 -0.5112 0.217 Uiso 1 1 calc R . .
C41 C 0.2629(9) -0.2473(4) -0.3353(4) 0.093(3) Uani 1 1 d . . .
H41A H 0.1894 -0.2481 -0.3582 0.111 Uiso 1 1 calc R . .
C42 C 0.3343(8) -0.1867(3) -0.3615(4) 0.097(3) Uani 1 1 d . . .
H42A H 0.3510 -0.1985 -0.4021 0.145 Uiso 1 1 calc R . .
H42B H 0.4070 -0.1820 -0.3400 0.145 Uiso 1 1 calc R . .
H42C H 0.2915 -0.1402 -0.3595 0.145 Uiso 1 1 calc R . .
C43 C 0.2278(8) -0.2390(4) -0.2751(3) 0.084(3) Uani 1 1 d . . .
H43A H 0.1784 -0.2805 -0.2639 0.127 Uiso 1 1 calc R . .
H43B H 0.1848 -0.1928 -0.2704 0.127 Uiso 1 1 calc R . .
H43C H 0.2966 -0.2380 -0.2503 0.127 Uiso 1 1 calc R . .
C44' C 0.364(2) 1.0038(16) 0.1059(13) 0.157(10) Uani 0.50 1 d PU A 1
C44 C 0.263(3) 0.9722(14) 0.0777(14) 0.155(10) Uani 0.50 1 d PU A 2
C45 C 0.2607(11) 0.9550(8) 0.1645(11) 0.296(15) Uani 1 1 d . . .
C46' C 0.350(2) 1.0295(7) 0.1965(10) 0.133(10) Uani 0.50 1 d P A 1
C46 C 0.372(2) 0.9593(13) 0.1561(12) 0.145(10) Uani 0.50 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O4 1.915(3) . ?
Zr1 O3 1.939(3) . ?
Zr1 O2 2.030(3) . ?
Zr1 O1 2.163(3) . ?
Zr1 N3 2.352(4) . ?
Zr1 N4 2.451(4) . ?
O1 C7 1.287(6) . ?
O2 C23 1.337(6) . ?
O3 C38 1.401(7) . ?
O4 C41 1.405(7) . ?
N1 C7 1.368(6) . ?
N1 N2 1.404(5) . ?
N1 C6 1.413(6) . ?
N2 C9 1.322(7) . ?
N3 C11 1.309(6) . ?
N3 C12 1.478(6) . ?
N4 C17 1.496(6) . ?
N4 C16 1.509(6) . ?
N4 C13 1.521(6) . ?
C1 C6 1.367(7) . ?
C1 C2 1.390(8) . ?
C1 H1A 0.9300 . ?
C2 C3 1.372(9) . ?
C2 H2B 0.9300 . ?
C3 C4 1.373(8) . ?
C3 H3A 0.9300 . ?
C4 C5 1.369(8) . ?
C4 H4A 0.9300 . ?
C5 C6 1.399(7) . ?
C5 H5A 0.9300 . ?
C7 C8 1.409(7) . ?
C8 C9 1.430(7) . ?
C8 C11 1.432(6) . ?
C9 C10 1.512(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C24 1.501(6) . ?
C12 C13 1.508(7) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.526(7) . ?
C13 H13A 0.9800 . ?
C14 C15 1.524(7) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.518(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.501(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C23 1.391(7) . ?
C18 C19 1.405(7) . ?
C19 C20 1.396(7) . ?
C19 H19A 0.9300 . ?
C20 C21 1.389(7) . ?
C20 C30 1.535(7) . ?
C21 C22 1.387(7) . ?
C21 H21A 0.9300 . ?
C22 C23 1.414(7) . ?
C22 C34 1.545(7) . ?
C24 C29 1.367(7) . ?
C24 C25 1.375(7) . ?
C25 C26 1.391(8) . ?
C25 H25A 0.9300 . ?
C26 C27 1.349(10) . ?
C26 H26A 0.9300 . ?
C27 C28 1.359(11) . ?
C27 H27A 0.9300 . ?
C28 C29 1.396(8) . ?
C28 H28A 0.9300 . ?
C29 H29A 0.9300 . ?
C30 C32 1.526(8) . ?
C30 C31 1.527(8) . ?
C30 C33 1.539(7) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 C37 1.523(9) . ?
C34 C35 1.548(8) . ?
C34 C36 1.562(9) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 C40 1.443(12) . ?
C38 C39 1.476(11) . ?
C38 H38A 0.9800 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 C43 1.428(9) . ?
C41 C42 1.470(10) . ?
C41 H41A 0.9800 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44' C45 1.97(2) . ?
C44 C45 1.99(3) . ?
C45 C46 1.28(3) . ?
C45 C46' 1.81(2) . ?

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
O4 Zr1 O3 106.06(16) . . ?
O4 Zr1 O2 93.73(15) . . ?
O3 Zr1 O2 101.01(15) . . ?
O4 Zr1 O1 89.92(14) . . ?
O3 Zr1 O1 91.09(14) . . ?
O2 Zr1 O1 165.83(13) . . ?
O4 Zr1 N3 97.05(14) . . ?
O3 Zr1 N3 153.94(15) . . ?
O2 Zr1 N3 89.10(14) . . ?
O1 Zr1 N3 76.85(13) . . ?
O4 Zr1 N4 164.40(14) . . ?
O3 Zr1 N4 88.35(15) . . ?
O2 Zr1 N4 77.33(13) . . ?
O1 Zr1 N4 95.86(12) . . ?
N3 Zr1 N4 70.36(13) . . ?
C7 O1 Zr1 119.7(3) . . ?
C23 O2 Zr1 143.4(3) . . ?
C38 O3 Zr1 161.5(4) . . ?
C41 O4 Zr1 174.7(5) . . ?
C7 N1 N2 111.6(4) . . ?
C7 N1 C6 129.5(4) . . ?
N2 N1 C6 118.9(4) . . ?
C9 N2 N1 105.1(4) . . ?
C11 N3 C12 119.6(4) . . ?
C11 N3 Zr1 127.7(3) . . ?
C12 N3 Zr1 112.1(3) . . ?
C17 N4 C16 109.5(4) . . ?
C17 N4 C13 111.4(3) . . ?
C16 N4 C13 107.2(4) . . ?
C17 N4 Zr1 109.3(3) . . ?
C16 N4 Zr1 106.4(3) . . ?
C13 N4 Zr1 112.9(3) . . ?
C6 C1 C2 120.1(6) . . ?
C6 C1 H1A 119.9 . . ?
C2 C1 H1A 119.9 . . ?
C3 C2 C1 119.6(6) . . ?
C3 C2 H2B 120.2 . . ?
C1 C2 H2B 120.2 . . ?
C2 C3 C4 120.1(6) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C5 C4 C3 121.1(6) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C4 C5 C6 118.9(5) . . ?
C4 C5 H5A 120.6 . . ?
C6 C5 H5A 120.6 . . ?
C1 C6 C5 120.2(5) . . ?
C1 C6 N1 120.7(5) . . ?
C5 C6 N1 119.1(5) . . ?
O1 C7 N1 123.7(5) . . ?
O1 C7 C8 129.9(4) . . ?
N1 C7 C8 106.4(4) . . ?
C7 C8 C9 105.0(4) . . ?
C7 C8 C11 122.7(4) . . ?
C9 C8 C11 131.7(4) . . ?
N2 C9 C8 112.0(5) . . ?
N2 C9 C10 118.7(5) . . ?
C8 C9 C10 129.2(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 C8 118.9(4) . . ?
N3 C11 C24 123.3(4) . . ?
C8 C11 C24 117.6(4) . . ?
N3 C12 C13 107.1(4) . . ?
N3 C12 H12A 110.3 . . ?
C13 C12 H12A 110.3 . . ?
N3 C12 H12B 110.3 . . ?
C13 C12 H12B 110.3 . . ?
H12A C12 H12B 108.6 . . ?
C12 C13 N4 111.6(4) . . ?
C12 C13 C14 115.0(4) . . ?
N4 C13 C14 104.4(4) . . ?
C12 C13 H13A 108.5 . . ?
N4 C13 H13A 108.5 . . ?
C14 C13 H13A 108.5 . . ?
C15 C14 C13 103.1(4) . . ?
C15 C14 H14A 111.2 . . ?
C13 C14 H14A 111.2 . . ?
C15 C14 H14B 111.2 . . ?
C13 C14 H14B 111.2 . . ?
H14A C14 H14B 109.1 . . ?
C16 C15 C14 102.4(4) . . ?
C16 C15 H15A 111.3 . . ?
C14 C15 H15A 111.3 . . ?
C16 C15 H15B 111.3 . . ?
C14 C15 H15B 111.3 . . ?
H15A C15 H15B 109.2 . . ?
N4 C16 C15 105.6(4) . . ?
N4 C16 H16A 110.6 . . ?
C15 C16 H16A 110.6 . . ?
N4 C16 H16B 110.6 . . ?
C15 C16 H16B 110.6 . . ?
H16A C16 H16B 108.8 . . ?
N4 C17 C18 113.8(4) . . ?
N4 C17 H17A 108.8 . . ?
C18 C17 H17A 108.8 . . ?
N4 C17 H17B 108.8 . . ?
C18 C17 H17B 108.8 . . ?
H17A C17 H17B 107.7 . . ?
C23 C18 C19 119.9(4) . . ?
C23 C18 C17 119.5(5) . . ?
C19 C18 C17 120.6(5) . . ?
C20 C19 C18 121.2(5) . . ?
C20 C19 H19A 119.4 . . ?
C18 C19 H19A 119.4 . . ?
C21 C20 C19 116.8(5) . . ?
C21 C20 C30 120.2(5) . . ?
C19 C20 C30 123.0(5) . . ?
C22 C21 C20 124.6(5) . . ?
C22 C21 H21A 117.7 . . ?
C20 C21 H21A 117.7 . . ?
C21 C22 C23 117.1(5) . . ?
C21 C22 C34 121.7(5) . . ?
C23 C22 C34 121.2(5) . . ?
O2 C23 C18 118.5(4) . . ?
O2 C23 C22 121.1(5) . . ?
C18 C23 C22 120.4(5) . . ?
C29 C24 C25 119.4(5) . . ?
C29 C24 C11 121.3(5) . . ?
C25 C24 C11 119.2(5) . . ?
C24 C25 C26 119.6(6) . . ?
C24 C25 H25A 120.2 . . ?
C26 C25 H25A 120.2 . . ?
C27 C26 C25 121.4(7) . . ?
C27 C26 H26A 119.3 . . ?
C25 C26 H26A 119.3 . . ?
C26 C27 C28 118.9(6) . . ?
C26 C27 H27A 120.6 . . ?
C28 C27 H27A 120.6 . . ?
C27 C28 C29 121.2(7) . . ?
C27 C28 H28A 119.4 . . ?
C29 C28 H28A 119.4 . . ?
C24 C29 C28 119.5(6) . . ?
C24 C29 H29A 120.3 . . ?
C28 C29 H29A 120.3 . . ?
C32 C30 C31 107.6(4) . . ?
C32 C30 C20 110.6(5) . . ?
C31 C30 C20 112.0(5) . . ?
C32 C30 C33 107.4(5) . . ?
C31 C30 C33 109.4(5) . . ?
C20 C30 C33 109.7(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C37 C34 C22 110.2(5) . . ?
C37 C34 C35 109.1(6) . . ?
C22 C34 C35 111.5(5) . . ?
C37 C34 C36 109.6(5) . . ?
C22 C34 C36 108.9(5) . . ?
C35 C34 C36 107.4(6) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O3 C38 C40 110.8(7) . . ?
O3 C38 C39 111.0(7) . . ?
C40 C38 C39 110.1(9) . . ?
O3 C38 H38A 108.3 . . ?
C40 C38 H38A 108.3 . . ?
C39 C38 H38A 108.3 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O4 C41 C43 111.9(6) . . ?
O4 C41 C42 109.9(6) . . ?
C43 C41 C42 117.5(7) . . ?
O4 C41 H41A 105.5 . . ?
C43 C41 H41A 105.5 . . ?
C42 C41 H41A 105.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C46 C45 C46' 57.8(15) . . ?
C46 C45 C44' 44.5(13) . . ?
C46' C45 C44' 67.5(13) . . ?
C46 C45 C44 80.1(18) . . ?
C46' C45 C44 105.8(12) . . ?
C44' C45 C44 42.1(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Zr1 O1 C7 49.5(3) . . . . ?
O3 Zr1 O1 C7 155.6(3) . . . . ?
O2 Zr1 O1 C7 -55.6(7) . . . . ?
N3 Zr1 O1 C7 -47.7(3) . . . . ?
N4 Zr1 O1 C7 -115.9(3) . . . . ?
O4 Zr1 O2 C23 -155.5(5) . . . . ?
O3 Zr1 O2 C23 97.3(5) . . . . ?
O1 Zr1 O2 C23 -50.8(9) . . . . ?
N3 Zr1 O2 C23 -58.5(5) . . . . ?
N4 Zr1 O2 C23 11.6(5) . . . . ?
O4 Zr1 O3 C38 25.7(14) . . . . ?
O2 Zr1 O3 C38 122.9(14) . . . . ?
O1 Zr1 O3 C38 -64.5(14) . . . . ?
N3 Zr1 O3 C38 -125.9(14) . . . . ?
N4 Zr1 O3 C38 -160.3(14) . . . . ?
O3 Zr1 O4 C41 74(5) . . . . ?
O2 Zr1 O4 C41 -29(5) . . . . ?
O1 Zr1 O4 C41 165(5) . . . . ?
N3 Zr1 O4 C41 -118(5) . . . . ?
N4 Zr1 O4 C41 -83(5) . . . . ?
C7 N1 N2 C9 0.6(5) . . . . ?
C6 N1 N2 C9 179.5(4) . . . . ?
O4 Zr1 N3 C11 -51.1(4) . . . . ?
O3 Zr1 N3 C11 101.5(5) . . . . ?
O2 Zr1 N3 C11 -144.8(4) . . . . ?
O1 Zr1 N3 C11 37.1(4) . . . . ?
N4 Zr1 N3 C11 138.4(5) . . . . ?
O4 Zr1 N3 C12 137.1(3) . . . . ?
O3 Zr1 N3 C12 -70.3(5) . . . . ?
O2 Zr1 N3 C12 43.4(3) . . . . ?
O1 Zr1 N3 C12 -134.6(3) . . . . ?
N4 Zr1 N3 C12 -33.4(3) . . . . ?
O4 Zr1 N4 C17 93.0(6) . . . . ?
O3 Zr1 N4 C17 -64.9(3) . . . . ?
O2 Zr1 N4 C17 36.8(3) . . . . ?
O1 Zr1 N4 C17 -155.8(3) . . . . ?
N3 Zr1 N4 C17 130.4(3) . . . . ?
O4 Zr1 N4 C16 -148.9(5) . . . . ?
O3 Zr1 N4 C16 53.3(3) . . . . ?
O2 Zr1 N4 C16 154.9(3) . . . . ?
O1 Zr1 N4 C16 -37.7(3) . . . . ?
N3 Zr1 N4 C16 -111.4(3) . . . . ?
O4 Zr1 N4 C13 -31.6(7) . . . . ?
O3 Zr1 N4 C13 170.6(3) . . . . ?
O2 Zr1 N4 C13 -87.8(3) . . . . ?
O1 Zr1 N4 C13 79.6(3) . . . . ?
N3 Zr1 N4 C13 5.9(3) . . . . ?
C6 C1 C2 C3 1.2(9) . . . . ?
C1 C2 C3 C4 -1.5(9) . . . . ?
C2 C3 C4 C5 1.6(9) . . . . ?
C3 C4 C5 C6 -1.5(8) . . . . ?
C2 C1 C6 C5 -1.0(8) . . . . ?
C2 C1 C6 N1 178.9(5) . . . . ?
C4 C5 C6 C1 1.2(8) . . . . ?
C4 C5 C6 N1 -178.8(5) . . . . ?
C7 N1 C6 C1 30.7(8) . . . . ?
N2 N1 C6 C1 -148.0(5) . . . . ?
C7 N1 C6 C5 -149.3(5) . . . . ?
N2 N1 C6 C5 32.0(7) . . . . ?
Zr1 O1 C7 N1 -141.3(4) . . . . ?
Zr1 O1 C7 C8 41.5(7) . . . . ?
N2 N1 C7 O1 -178.4(4) . . . . ?
C6 N1 C7 O1 2.9(8) . . . . ?
N2 N1 C7 C8 -0.6(5) . . . . ?
C6 N1 C7 C8 -179.4(5) . . . . ?
O1 C7 C8 C9 178.0(5) . . . . ?
N1 C7 C8 C9 0.4(5) . . . . ?
O1 C7 C8 C11 5.9(8) . . . . ?
N1 C7 C8 C11 -171.6(4) . . . . ?
N1 N2 C9 C8 -0.3(6) . . . . ?
N1 N2 C9 C10 -177.3(4) . . . . ?
C7 C8 C9 N2 -0.1(6) . . . . ?
C11 C8 C9 N2 171.0(5) . . . . ?
C7 C8 C9 C10 176.5(5) . . . . ?
C11 C8 C9 C10 -12.5(9) . . . . ?
C12 N3 C11 C8 160.4(4) . . . . ?
Zr1 N3 C11 C8 -10.8(7) . . . . ?
C12 N3 C11 C24 -16.5(7) . . . . ?
Zr1 N3 C11 C24 172.3(4) . . . . ?
C7 C8 C11 N3 -21.2(7) . . . . ?
C9 C8 C11 N3 169.1(5) . . . . ?
C7 C8 C11 C24 155.8(5) . . . . ?
C9 C8 C11 C24 -13.9(8) . . . . ?
C11 N3 C12 C13 -116.1(5) . . . . ?
Zr1 N3 C12 C13 56.4(4) . . . . ?
N3 C12 C13 N4 -49.7(5) . . . . ?
N3 C12 C13 C14 68.9(5) . . . . ?
C17 N4 C13 C12 -102.1(4) . . . . ?
C16 N4 C13 C12 138.2(4) . . . . ?
Zr1 N4 C13 C12 21.3(4) . . . . ?
C17 N4 C13 C14 133.1(4) . . . . ?
C16 N4 C13 C14 13.4(5) . . . . ?
Zr1 N4 C13 C14 -103.5(3) . . . . ?
C12 C13 C14 C15 -156.7(4) . . . . ?
N4 C13 C14 C15 -34.2(5) . . . . ?
C13 C14 C15 C16 41.9(5) . . . . ?
C17 N4 C16 C15 -108.3(4) . . . . ?
C13 N4 C16 C15 12.7(5) . . . . ?
Zr1 N4 C16 C15 133.7(3) . . . . ?
C14 C15 C16 N4 -33.7(5) . . . . ?
C16 N4 C17 C18 172.8(4) . . . . ?
C13 N4 C17 C18 54.4(5) . . . . ?
Zr1 N4 C17 C18 -71.0(5) . . . . ?
N4 C17 C18 C23 54.5(6) . . . . ?
N4 C17 C18 C19 -126.1(5) . . . . ?
C23 C18 C19 C20 0.0(8) . . . . ?
C17 C18 C19 C20 -179.3(5) . . . . ?
C18 C19 C20 C21 -2.6(8) . . . . ?
C18 C19 C20 C30 -179.3(5) . . . . ?
C19 C20 C21 C22 2.7(8) . . . . ?
C30 C20 C21 C22 179.5(5) . . . . ?
C20 C21 C22 C23 -0.1(8) . . . . ?
C20 C21 C22 C34 179.4(6) . . . . ?
Zr1 O2 C23 C18 -32.4(8) . . . . ?
Zr1 O2 C23 C22 144.6(4) . . . . ?
C19 C18 C23 O2 179.8(4) . . . . ?
C17 C18 C23 O2 -0.8(7) . . . . ?
C19 C18 C23 C22 2.8(8) . . . . ?
C17 C18 C23 C22 -177.9(5) . . . . ?
C21 C22 C23 O2 -179.7(5) . . . . ?
C34 C22 C23 O2 0.8(9) . . . . ?
C21 C22 C23 C18 -2.7(8) . . . . ?
C34 C22 C23 C18 177.8(5) . . . . ?
N3 C11 C24 C29 108.9(6) . . . . ?
C8 C11 C24 C29 -68.0(6) . . . . ?
N3 C11 C24 C25 -75.1(7) . . . . ?
C8 C11 C24 C25 107.9(6) . . . . ?
C29 C24 C25 C26 1.4(8) . . . . ?
C11 C24 C25 C26 -174.7(5) . . . . ?
C24 C25 C26 C27 -0.6(10) . . . . ?
C25 C26 C27 C28 -0.3(10) . . . . ?
C26 C27 C28 C29 0.4(10) . . . . ?
C25 C24 C29 C28 -1.3(8) . . . . ?
C11 C24 C29 C28 174.6(5) . . . . ?
C27 C28 C29 C24 0.4(9) . . . . ?
C21 C20 C30 C32 51.5(7) . . . . ?
C19 C20 C30 C32 -131.9(6) . . . . ?
C21 C20 C30 C31 171.5(5) . . . . ?
C19 C20 C30 C31 -11.9(8) . . . . ?
C21 C20 C30 C33 -66.8(7) . . . . ?
C19 C20 C30 C33 109.8(6) . . . . ?
C21 C22 C34 C37 -118.7(6) . . . . ?
C23 C22 C34 C37 60.7(8) . . . . ?
C21 C22 C34 C35 2.6(9) . . . . ?
C23 C22 C34 C35 -177.9(6) . . . . ?
C21 C22 C34 C36 121.0(6) . . . . ?
C23 C22 C34 C36 -59.6(8) . . . . ?
Zr1 O3 C38 C40 87.9(16) . . . . ?
Zr1 O3 C38 C39 -34.8(19) . . . . ?
Zr1 O4 C41 C43 124(4) . . . . ?
Zr1 O4 C41 C42 -103(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.070
####################################################################### 
# 
# 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_zr-ipr
_database_code_depnum_ccdc_archive 'CCDC 1539662'
_audit_update_record             
;
2017-03-22 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H60 N4 O4 Zr'
_chemical_formula_sum            'C40 H60 N4 O4 Zr'
_chemical_formula_weight         752.14

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'

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

_cell_length_a                   11.0439(3)
_cell_length_b                   10.3438(3)
_cell_length_c                   17.7240(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.103(3)
_cell_angle_gamma                90.00
_cell_volume                     1999.21(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2613
_cell_measurement_theta_min      3.9340
_cell_measurement_theta_max      25.8500

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.98072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7417
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.49
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5073
_reflns_number_gt                4628
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_chemical_absolute_configuration s
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0100P)²+1.4000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_number_reflns         5073
_refine_ls_number_parameters     442
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0757
_refine_ls_wR_factor_gt          0.0712
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 1.01266(3) 0.48834(5) 0.20485(2) 0.02071(10) Uani 1 1 d . . .
O1 O 0.9498(3) 0.6330(4) 0.11985(18) 0.0248(9) Uani 1 1 d . . .
O2 O 1.0949(2) 0.3899(3) 0.29744(15) 0.0221(7) Uani 1 1 d . . .
O3 O 0.9879(3) 0.3557(4) 0.12758(19) 0.0325(9) Uani 1 1 d . . .
O4 O 0.8624(2) 0.5058(4) 0.24622(15) 0.0308(8) Uani 1 1 d . . .
N1 N 0.7904(3) 0.7862(4) 0.1137(2) 0.0271(9) Uani 1 1 d . . .
N2 N 0.7593(3) 0.8909(4) 0.1556(2) 0.0376(10) Uani 1 1 d . . .
N3 N 1.1125(3) 0.6765(4) 0.25556(19) 0.0226(9) Uani 1 1 d . . .
N4 N 1.2277(3) 0.4778(5) 0.18631(15) 0.0204(8) Uani 1 1 d . . .
C1 C 0.7229(5) 0.6326(5) 0.0108(3) 0.0418(14) Uani 1 1 d . . .
H1A H 0.7940 0.5843 0.0246 0.050 Uiso 1 1 calc R . .
C2 C 0.6360(5) 0.5935(6) -0.0497(3) 0.0500(16) Uani 1 1 d . . .
H2B H 0.6489 0.5182 -0.0760 0.060 Uiso 1 1 calc R . .
C3 C 0.5304(5) 0.6641(6) -0.0718(3) 0.0465(15) Uani 1 1 d . . .
H3A H 0.4728 0.6380 -0.1130 0.056 Uiso 1 1 calc R . .
C4 C 0.5125(4) 0.7731(6) -0.0317(3) 0.0417(15) Uani 1 1 d . . .
H4A H 0.4410 0.8206 -0.0454 0.050 Uiso 1 1 calc R . .
C5 C 0.5988(4) 0.8148(5) 0.0292(3) 0.0354(13) Uani 1 1 d . . .
H5A H 0.5858 0.8902 0.0554 0.042 Uiso 1 1 calc R . .
C6 C 0.7041(4) 0.7429(5) 0.0504(3) 0.0294(11) Uani 1 1 d . . .
C7 C 0.9016(4) 0.7333(5) 0.1466(2) 0.0249(11) Uani 1 1 d . . .
C8 C 0.9442(4) 0.8117(5) 0.2106(2) 0.0274(11) Uani 1 1 d . . .
C9 C 0.8518(4) 0.9059(5) 0.2125(3) 0.0338(12) Uani 1 1 d . . .
C10 C 0.8383(4) 1.0140(6) 0.2676(3) 0.0506(18) Uani 1 1 d . . .
H10A H 0.7638 1.0605 0.2504 0.061 Uiso 1 1 calc R . .
H10B H 0.9069 1.0718 0.2701 0.061 Uiso 1 1 calc R . .
H10C H 0.8357 0.9787 0.3174 0.061 Uiso 1 1 calc R . .
C11 C 1.0639(4) 0.7912(5) 0.2565(3) 0.0286(11) Uani 1 1 d . . .
C12 C 1.2411(4) 0.6486(5) 0.2888(3) 0.0238(11) Uani 1 1 d . . .
H12A H 1.2434 0.5923 0.3328 0.029 Uiso 1 1 calc R . .
H12B H 1.2831 0.7284 0.3056 0.029 Uiso 1 1 calc R . .
C13 C 1.3046(4) 0.5836(5) 0.2287(3) 0.0268(12) Uani 1 1 d . . .
H13A H 1.3805 0.5444 0.2548 0.032 Uiso 1 1 calc R . .
C14 C 1.3381(4) 0.6750(5) 0.1667(3) 0.0337(12) Uani 1 1 d . . .
H14A H 1.2766 0.7418 0.1543 0.040 Uiso 1 1 calc R . .
H14B H 1.4172 0.7154 0.1829 0.040 Uiso 1 1 calc R . .
C15 C 1.3419(4) 0.5856(5) 0.0989(3) 0.0366(13) Uani 1 1 d . . .
H15A H 1.3339 0.6334 0.0513 0.044 Uiso 1 1 calc R . .
H15B H 1.4169 0.5352 0.1051 0.044 Uiso 1 1 calc R . .
C16 C 1.2315(3) 0.5017(7) 0.1025(2) 0.0304(11) Uani 1 1 d . . .
H16A H 1.2388 0.4205 0.0762 0.037 Uiso 1 1 calc R . .
H16B H 1.1573 0.5450 0.0788 0.037 Uiso 1 1 calc R . .
C17 C 1.2783(4) 0.3477(5) 0.2070(3) 0.0232(11) Uani 1 1 d . . .
H17A H 1.3570 0.3404 0.1896 0.028 Uiso 1 1 calc R . .
H17B H 1.2240 0.2840 0.1794 0.028 Uiso 1 1 calc R . .
C18 C 1.2956(4) 0.3146(5) 0.2906(3) 0.0218(11) Uani 1 1 d . . .
C19 C 1.4024(4) 0.2547(4) 0.3254(2) 0.0271(11) Uani 1 1 d . . .
H19A H 1.4660 0.2424 0.2975 0.033 Uiso 1 1 calc R . .
C20 C 1.4172(4) 0.2124(5) 0.4013(3) 0.0270(11) Uani 1 1 d . . .
C21 C 1.3199(4) 0.2344(5) 0.4412(2) 0.0253(11) Uani 1 1 d . . .
H21A H 1.3284 0.2073 0.4918 0.030 Uiso 1 1 calc R . .
C22 C 1.2110(4) 0.2945(4) 0.4097(2) 0.0211(10) Uani 1 1 d . . .
C23 C 1.1980(4) 0.3345(4) 0.3325(2) 0.0207(10) Uani 1 1 d . . .
C24 C 1.1254(5) 0.9082(5) 0.2986(3) 0.0470(14) Uani 1 1 d U . .
H24A H 1.0597 0.9721 0.2980 0.056 Uiso 1 1 calc R . .
C25 C 1.2179(5) 0.9717(7) 0.2547(3) 0.0685(19) Uani 1 1 d U . .
H25A H 1.1817 0.9820 0.2021 0.103 Uiso 1 1 calc R . .
H25B H 1.2895 0.9182 0.2579 0.103 Uiso 1 1 calc R . .
H25C H 1.2405 1.0549 0.2765 0.103 Uiso 1 1 calc R . .
C26 C 1.1754(5) 0.8881(6) 0.3824(3) 0.0536(16) Uani 1 1 d . . .
H26A H 1.1139 0.8479 0.4071 0.080 Uiso 1 1 calc R . .
H26B H 1.1974 0.9702 0.4059 0.080 Uiso 1 1 calc R . .
H26C H 1.2465 0.8336 0.3871 0.080 Uiso 1 1 calc R . .
C27 C 1.5334(4) 0.1416(5) 0.4366(3) 0.0354(13) Uani 1 1 d . . .
C28 C 1.6458(5) 0.2250(6) 0.4320(4) 0.074(2) Uani 1 1 d . . .
H28A H 1.7184 0.1794 0.4543 0.112 Uiso 1 1 calc R . .
H28B H 1.6397 0.3043 0.4592 0.112 Uiso 1 1 calc R . .
H28C H 1.6502 0.2439 0.3794 0.112 Uiso 1 1 calc R . .
C29 C 1.5449(5) 0.0142(7) 0.3937(3) 0.065(2) Uani 1 1 d . . .
H29A H 1.6182 -0.0300 0.4162 0.098 Uiso 1 1 calc R . .
H29B H 1.5486 0.0323 0.3410 0.098 Uiso 1 1 calc R . .
H29C H 1.4750 -0.0393 0.3972 0.098 Uiso 1 1 calc R . .
C30 C 1.5339(5) 0.1038(6) 0.5200(3) 0.0626(19) Uani 1 1 d . . .
H30A H 1.6090 0.0596 0.5391 0.094 Uiso 1 1 calc R . .
H30B H 1.4657 0.0479 0.5235 0.094 Uiso 1 1 calc R . .
H30C H 1.5275 0.1802 0.5499 0.094 Uiso 1 1 calc R . .
C31 C 1.1055(4) 0.3154(5) 0.4556(2) 0.0252(11) Uani 1 1 d . . .
C32 C 1.0779(4) 0.4590(5) 0.4607(3) 0.0363(14) Uani 1 1 d . . .
H32A H 1.0120 0.4711 0.4893 0.054 Uiso 1 1 calc R . .
H32B H 1.0547 0.4934 0.4101 0.054 Uiso 1 1 calc R . .
H32C H 1.1496 0.5032 0.4857 0.054 Uiso 1 1 calc R . .
C33 C 0.9903(4) 0.2437(5) 0.4173(2) 0.0326(12) Uani 1 1 d . . .
H33A H 1.0082 0.1532 0.4141 0.049 Uiso 1 1 calc R . .
H33B H 0.9651 0.2776 0.3668 0.049 Uiso 1 1 calc R . .
H33C H 0.9256 0.2555 0.4470 0.049 Uiso 1 1 calc R . .
C34 C 1.1378(4) 0.2615(6) 0.5372(2) 0.0395(14) Uani 1 1 d . . .
H34A H 1.1556 0.1709 0.5350 0.059 Uiso 1 1 calc R . .
H34B H 1.0697 0.2740 0.5641 0.059 Uiso 1 1 calc R . .
H34C H 1.2083 0.3060 0.5636 0.059 Uiso 1 1 calc R . .
C35 C 0.9772(5) 0.2701(6) 0.0653(3) 0.0445(14) Uani 1 1 d . . .
H35A H 1.0594 0.2568 0.0526 0.053 Uiso 1 1 calc R . .
C36 C 0.8994(5) 0.3261(6) -0.0029(3) 0.0494(15) Uani 1 1 d . . .
H36A H 0.8941 0.2663 -0.0447 0.074 Uiso 1 1 calc R . .
H36B H 0.9351 0.4056 -0.0167 0.074 Uiso 1 1 calc R . .
H36C H 0.8187 0.3427 0.0086 0.074 Uiso 1 1 calc R . .
C37 C 0.9323(7) 0.1434(6) 0.0892(3) 0.080(2) Uani 1 1 d . . .
H37A H 0.9254 0.0839 0.0472 0.120 Uiso 1 1 calc R . .
H37B H 0.8535 0.1545 0.1047 0.120 Uiso 1 1 calc R . .
H37C H 0.9892 0.1099 0.1313 0.120 Uiso 1 1 calc R . .
C38 C 0.7482(4) 0.4913(9) 0.2711(3) 0.0482(13) Uani 1 1 d . . .
H38A H 0.7623 0.4512 0.3219 0.058 Uiso 1 1 calc R . .
C39 C 0.6894(5) 0.6213(7) 0.2779(4) 0.071(2) Uani 1 1 d . . .
H39A H 0.6118 0.6098 0.2950 0.106 Uiso 1 1 calc R . .
H39B H 0.6771 0.6633 0.2291 0.106 Uiso 1 1 calc R . .
H39C H 0.7419 0.6734 0.3142 0.106 Uiso 1 1 calc R . .
C40 C 0.6711(5) 0.4010(7) 0.2173(4) 0.083(2) Uani 1 1 d . . .
H40A H 0.5926 0.3900 0.2333 0.125 Uiso 1 1 calc R . .
H40B H 0.7114 0.3187 0.2175 0.125 Uiso 1 1 calc R . .
H40C H 0.6599 0.4365 0.1666 0.125 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O4 1.926(3) . ?
Zr1 O3 1.927(3) . ?
Zr1 O2 2.021(3) . ?
Zr1 O1 2.158(3) . ?
Zr1 N3 2.345(4) . ?
Zr1 N4 2.451(3) . ?
O1 C7 1.290(6) . ?
O2 C23 1.337(5) . ?
O3 C35 1.405(6) . ?
O4 C38 1.408(4) . ?
N1 C7 1.386(5) . ?
N1 N2 1.387(5) . ?
N1 C6 1.424(5) . ?
N2 C9 1.327(5) . ?
N3 C11 1.304(6) . ?
N3 C12 1.477(5) . ?
N4 C17 1.481(7) . ?
N4 C13 1.510(6) . ?
N4 C16 1.512(4) . ?
C1 C6 1.373(7) . ?
C1 C2 1.382(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.379(7) . ?
C2 H2B 0.9300 . ?
C3 C4 1.363(8) . ?
C3 H3A 0.9300 . ?
C4 C5 1.391(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.381(6) . ?
C5 H5A 0.9300 . ?
C7 C8 1.413(6) . ?
C8 C9 1.415(6) . ?
C8 C11 1.454(6) . ?
C9 C10 1.508(7) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C24 1.524(6) . ?
C12 C13 1.522(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.539(6) . ?
C13 H13A 0.9800 . ?
C14 C15 1.521(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.507(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.504(6) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.387(6) . ?
C18 C23 1.418(6) . ?
C19 C20 1.399(6) . ?
C19 H19A 0.9300 . ?
C20 C21 1.395(6) . ?
C20 C27 1.523(6) . ?
C21 C22 1.390(6) . ?
C21 H21A 0.9300 . ?
C22 C23 1.415(6) . ?
C22 C31 1.538(6) . ?
C24 C26 1.514(7) . ?
C24 C25 1.526(7) . ?
C24 H24A 0.9800 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.524(7) . ?
C27 C30 1.529(7) . ?
C27 C29 1.536(8) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.522(6) . ?
C31 C33 1.535(6) . ?
C31 C34 1.539(6) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C36 1.486(6) . ?
C35 C37 1.486(8) . ?
C35 H35A 0.9800 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 C40 1.501(9) . ?
C38 C39 1.506(10) . ?
C38 H38A 0.9800 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?

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
O4 Zr1 O3 107.65(15) . . ?
O4 Zr1 O2 92.40(12) . . ?
O3 Zr1 O2 102.32(14) . . ?
O4 Zr1 O1 89.96(14) . . ?
O3 Zr1 O1 90.21(11) . . ?
O2 Zr1 O1 165.86(13) . . ?
O4 Zr1 N3 99.06(15) . . ?
O3 Zr1 N3 150.30(14) . . ?
O2 Zr1 N3 89.04(13) . . ?
O1 Zr1 N3 76.82(13) . . ?
O4 Zr1 N4 165.20(10) . . ?
O3 Zr1 N4 84.54(14) . . ?
O2 Zr1 N4 76.46(11) . . ?
O1 Zr1 N4 98.55(13) . . ?
N3 Zr1 N4 71.42(14) . . ?
C7 O1 Zr1 114.0(3) . . ?
C23 O2 Zr1 146.5(3) . . ?
C35 O3 Zr1 172.5(4) . . ?
C38 O4 Zr1 167.8(5) . . ?
C7 N1 N2 111.2(4) . . ?
C7 N1 C6 130.2(4) . . ?
N2 N1 C6 118.4(4) . . ?
C9 N2 N1 105.8(4) . . ?
C11 N3 C12 123.0(4) . . ?
C11 N3 Zr1 126.3(3) . . ?
C12 N3 Zr1 110.8(3) . . ?
C17 N4 C13 112.0(3) . . ?
C17 N4 C16 108.8(4) . . ?
C13 N4 C16 105.7(4) . . ?
C17 N4 Zr1 110.0(3) . . ?
C13 N4 Zr1 112.4(3) . . ?
C16 N4 Zr1 107.6(2) . . ?
C6 C1 C2 119.8(5) . . ?
C6 C1 H1A 120.1 . . ?
C2 C1 H1A 120.1 . . ?
C3 C2 C1 121.2(6) . . ?
C3 C2 H2B 119.4 . . ?
C1 C2 H2B 119.4 . . ?
C4 C3 C2 118.4(5) . . ?
C4 C3 H3A 120.8 . . ?
C2 C3 H3A 120.8 . . ?
C3 C4 C5 121.5(5) . . ?
C3 C4 H4A 119.2 . . ?
C5 C4 H4A 119.2 . . ?
C6 C5 C4 119.2(5) . . ?
C6 C5 H5A 120.4 . . ?
C4 C5 H5A 120.4 . . ?
C1 C6 C5 119.8(4) . . ?
C1 C6 N1 121.8(4) . . ?
C5 C6 N1 118.3(5) . . ?
O1 C7 N1 123.5(4) . . ?
O1 C7 C8 130.7(4) . . ?
N1 C7 C8 105.8(4) . . ?
C7 C8 C9 105.3(4) . . ?
C7 C8 C11 121.6(4) . . ?
C9 C8 C11 133.0(4) . . ?
N2 C9 C8 111.9(4) . . ?
N2 C9 C10 115.9(4) . . ?
C8 C9 C10 132.2(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 C8 117.7(4) . . ?
N3 C11 C24 125.2(4) . . ?
C8 C11 C24 117.0(4) . . ?
N3 C12 C13 109.1(3) . . ?
N3 C12 H12A 109.9 . . ?
C13 C12 H12A 109.9 . . ?
N3 C12 H12B 109.9 . . ?
C13 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
N4 C13 C12 112.6(3) . . ?
N4 C13 C14 105.6(4) . . ?
C12 C13 C14 114.7(4) . . ?
N4 C13 H13A 107.9 . . ?
C12 C13 H13A 107.9 . . ?
C14 C13 H13A 107.9 . . ?
C15 C14 C13 103.3(4) . . ?
C15 C14 H14A 111.1 . . ?
C13 C14 H14A 111.1 . . ?
C15 C14 H14B 111.1 . . ?
C13 C14 H14B 111.1 . . ?
H14A C14 H14B 109.1 . . ?
C16 C15 C14 101.1(4) . . ?
C16 C15 H15A 111.5 . . ?
C14 C15 H15A 111.5 . . ?
C16 C15 H15B 111.5 . . ?
C14 C15 H15B 111.5 . . ?
H15A C15 H15B 109.4 . . ?
C15 C16 N4 106.5(4) . . ?
C15 C16 H16A 110.4 . . ?
N4 C16 H16A 110.4 . . ?
C15 C16 H16B 110.4 . . ?
N4 C16 H16B 110.4 . . ?
H16A C16 H16B 108.6 . . ?
N4 C17 C18 115.8(4) . . ?
N4 C17 H17A 108.3 . . ?
C18 C17 H17A 108.3 . . ?
N4 C17 H17B 108.3 . . ?
C18 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
C19 C18 C23 119.7(4) . . ?
C19 C18 C17 120.5(4) . . ?
C23 C18 C17 119.6(4) . . ?
C18 C19 C20 122.0(4) . . ?
C18 C19 H19A 119.0 . . ?
C20 C19 H19A 119.0 . . ?
C21 C20 C19 117.0(4) . . ?
C21 C20 C27 122.5(4) . . ?
C19 C20 C27 120.5(4) . . ?
C22 C21 C20 123.8(4) . . ?
C22 C21 H21A 118.1 . . ?
C20 C21 H21A 118.1 . . ?
C21 C22 C23 117.8(4) . . ?
C21 C22 C31 122.0(4) . . ?
C23 C22 C31 120.1(4) . . ?
O2 C23 C22 121.5(4) . . ?
O2 C23 C18 118.7(4) . . ?
C22 C23 C18 119.7(4) . . ?
C26 C24 C11 115.8(5) . . ?
C26 C24 C25 112.9(4) . . ?
C11 C24 C25 112.0(5) . . ?
C26 C24 H24A 104.9 . . ?
C11 C24 H24A 104.9 . . ?
C25 C24 H24A 104.9 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C20 C27 C28 110.3(5) . . ?
C20 C27 C30 113.2(4) . . ?
C28 C27 C30 108.6(5) . . ?
C20 C27 C29 109.8(4) . . ?
C28 C27 C29 109.1(5) . . ?
C30 C27 C29 105.7(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 C33 109.8(4) . . ?
C32 C31 C22 110.1(4) . . ?
C33 C31 C22 110.0(4) . . ?
C32 C31 C34 108.5(4) . . ?
C33 C31 C34 107.1(4) . . ?
C22 C31 C34 111.3(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O3 C35 C36 111.1(4) . . ?
O3 C35 C37 108.8(4) . . ?
C36 C35 C37 113.6(5) . . ?
O3 C35 H35A 107.7 . . ?
C36 C35 H35A 107.7 . . ?
C37 C35 H35A 107.7 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O4 C38 C40 108.2(5) . . ?
O4 C38 C39 110.4(6) . . ?
C40 C38 C39 113.5(5) . . ?
O4 C38 H38A 108.2 . . ?
C40 C38 H38A 108.2 . . ?
C39 C38 H38A 108.2 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 Zr1 O1 C7 45.1(3) . . . . ?
O3 Zr1 O1 C7 152.7(3) . . . . ?
O2 Zr1 O1 C7 -54.6(6) . . . . ?
N3 Zr1 O1 C7 -54.2(3) . . . . ?
N4 Zr1 O1 C7 -122.8(3) . . . . ?
O4 Zr1 O2 C23 -176.2(5) . . . . ?
O3 Zr1 O2 C23 75.1(5) . . . . ?
O1 Zr1 O2 C23 -76.8(8) . . . . ?
N3 Zr1 O2 C23 -77.2(5) . . . . ?
N4 Zr1 O2 C23 -6.1(5) . . . . ?
O4 Zr1 O3 C35 134(2) . . . . ?
O2 Zr1 O3 C35 -129(2) . . . . ?
O1 Zr1 O3 C35 44(2) . . . . ?
N3 Zr1 O3 C35 -19(3) . . . . ?
N4 Zr1 O3 C35 -54(2) . . . . ?
O3 Zr1 O4 C38 24.4(14) . . . . ?
O2 Zr1 O4 C38 -79.3(14) . . . . ?
O1 Zr1 O4 C38 114.7(14) . . . . ?
N3 Zr1 O4 C38 -168.7(14) . . . . ?
N4 Zr1 O4 C38 -119.9(14) . . . . ?
C7 N1 N2 C9 2.0(5) . . . . ?
C6 N1 N2 C9 176.7(4) . . . . ?
O4 Zr1 N3 C11 -44.9(4) . . . . ?
O3 Zr1 N3 C11 109.2(4) . . . . ?
O2 Zr1 N3 C11 -137.1(4) . . . . ?
O1 Zr1 N3 C11 43.0(4) . . . . ?
N4 Zr1 N3 C11 146.8(4) . . . . ?
O4 Zr1 N3 C12 134.1(3) . . . . ?
O3 Zr1 N3 C12 -71.8(4) . . . . ?
O2 Zr1 N3 C12 41.8(3) . . . . ?
O1 Zr1 N3 C12 -138.1(3) . . . . ?
N4 Zr1 N3 C12 -34.2(3) . . . . ?
O4 Zr1 N4 C17 83.7(8) . . . . ?
O3 Zr1 N4 C17 -62.4(3) . . . . ?
O2 Zr1 N4 C17 41.7(2) . . . . ?
O1 Zr1 N4 C17 -151.8(3) . . . . ?
N3 Zr1 N4 C17 135.3(3) . . . . ?
O4 Zr1 N4 C13 -41.9(9) . . . . ?
O3 Zr1 N4 C13 172.0(3) . . . . ?
O2 Zr1 N4 C13 -83.9(3) . . . . ?
O1 Zr1 N4 C13 82.6(3) . . . . ?
N3 Zr1 N4 C13 9.7(3) . . . . ?
O4 Zr1 N4 C16 -157.8(6) . . . . ?
O3 Zr1 N4 C16 56.0(4) . . . . ?
O2 Zr1 N4 C16 160.1(4) . . . . ?
O1 Zr1 N4 C16 -33.4(4) . . . . ?
N3 Zr1 N4 C16 -106.3(4) . . . . ?
C6 C1 C2 C3 0.6(8) . . . . ?
C1 C2 C3 C4 -0.9(8) . . . . ?
C2 C3 C4 C5 1.2(8) . . . . ?
C3 C4 C5 C6 -1.1(8) . . . . ?
C2 C1 C6 C5 -0.6(8) . . . . ?
C2 C1 C6 N1 179.3(5) . . . . ?
C4 C5 C6 C1 0.8(7) . . . . ?
C4 C5 C6 N1 -179.1(4) . . . . ?
C7 N1 C6 C1 0.0(7) . . . . ?
N2 N1 C6 C1 -173.6(4) . . . . ?
C7 N1 C6 C5 179.9(5) . . . . ?
N2 N1 C6 C5 6.3(6) . . . . ?
Zr1 O1 C7 N1 -131.9(4) . . . . ?
Zr1 O1 C7 C8 48.6(6) . . . . ?
N2 N1 C7 O1 178.2(4) . . . . ?
C6 N1 C7 O1 4.3(8) . . . . ?
N2 N1 C7 C8 -2.2(5) . . . . ?
C6 N1 C7 C8 -176.1(4) . . . . ?
O1 C7 C8 C9 -178.9(5) . . . . ?
N1 C7 C8 C9 1.5(5) . . . . ?
O1 C7 C8 C11 4.2(8) . . . . ?
N1 C7 C8 C11 -175.4(4) . . . . ?
N1 N2 C9 C8 -1.0(6) . . . . ?
N1 N2 C9 C10 -179.0(4) . . . . ?
C7 C8 C9 N2 -0.3(6) . . . . ?
C11 C8 C9 N2 176.0(5) . . . . ?
C7 C8 C9 C10 177.3(5) . . . . ?
C11 C8 C9 C10 -6.3(10) . . . . ?
C12 N3 C11 C8 169.4(4) . . . . ?
Zr1 N3 C11 C8 -11.7(6) . . . . ?
C12 N3 C11 C24 -7.1(7) . . . . ?
Zr1 N3 C11 C24 171.8(4) . . . . ?
C7 C8 C11 N3 -23.8(7) . . . . ?
C9 C8 C11 N3 160.4(5) . . . . ?
C7 C8 C11 C24 153.1(5) . . . . ?
C9 C8 C11 C24 -22.8(8) . . . . ?
C11 N3 C12 C13 -126.3(5) . . . . ?
Zr1 N3 C12 C13 54.7(4) . . . . ?
C17 N4 C13 C12 -109.3(4) . . . . ?
C16 N4 C13 C12 132.4(4) . . . . ?
Zr1 N4 C13 C12 15.3(5) . . . . ?
C17 N4 C13 C14 124.8(4) . . . . ?
C16 N4 C13 C14 6.4(5) . . . . ?
Zr1 N4 C13 C14 -110.6(3) . . . . ?
N3 C12 C13 N4 -45.5(5) . . . . ?
N3 C12 C13 C14 75.4(5) . . . . ?
N4 C13 C14 C15 -30.0(5) . . . . ?
C12 C13 C14 C15 -154.5(4) . . . . ?
C13 C14 C15 C16 41.3(5) . . . . ?
C14 C15 C16 N4 -38.2(5) . . . . ?
C17 N4 C16 C15 -100.6(5) . . . . ?
C13 N4 C16 C15 19.9(6) . . . . ?
Zr1 N4 C16 C15 140.2(3) . . . . ?
C13 N4 C17 C18 56.3(4) . . . . ?
C16 N4 C17 C18 172.8(4) . . . . ?
Zr1 N4 C17 C18 -69.5(4) . . . . ?
N4 C17 C18 C19 -135.7(4) . . . . ?
N4 C17 C18 C23 49.7(6) . . . . ?
C23 C18 C19 C20 0.2(7) . . . . ?
C17 C18 C19 C20 -174.3(4) . . . . ?
C18 C19 C20 C21 -0.8(7) . . . . ?
C18 C19 C20 C27 177.3(5) . . . . ?
C19 C20 C21 C22 0.3(7) . . . . ?
C27 C20 C21 C22 -177.6(5) . . . . ?
C20 C21 C22 C23 0.6(7) . . . . ?
C20 C21 C22 C31 179.3(4) . . . . ?
Zr1 O2 C23 C22 168.0(4) . . . . ?
Zr1 O2 C23 C18 -12.6(8) . . . . ?
C21 C22 C23 O2 178.2(4) . . . . ?
C31 C22 C23 O2 -0.5(6) . . . . ?
C21 C22 C23 C18 -1.2(6) . . . . ?
C31 C22 C23 C18 -179.8(4) . . . . ?
C19 C18 C23 O2 -178.6(4) . . . . ?
C17 C18 C23 O2 -4.0(7) . . . . ?
C19 C18 C23 C22 0.8(7) . . . . ?
C17 C18 C23 C22 175.4(4) . . . . ?
N3 C11 C24 C26 -52.2(7) . . . . ?
C8 C11 C24 C26 131.2(5) . . . . ?
N3 C11 C24 C25 79.3(6) . . . . ?
C8 C11 C24 C25 -97.3(5) . . . . ?
C21 C20 C27 C28 -124.4(5) . . . . ?
C19 C20 C27 C28 57.6(7) . . . . ?
C21 C20 C27 C30 -2.6(7) . . . . ?
C19 C20 C27 C30 179.5(5) . . . . ?
C21 C20 C27 C29 115.3(5) . . . . ?
C19 C20 C27 C29 -62.6(6) . . . . ?
C21 C22 C31 C32 120.1(5) . . . . ?
C23 C22 C31 C32 -61.3(5) . . . . ?
C21 C22 C31 C33 -118.8(5) . . . . ?
C23 C22 C31 C33 59.8(5) . . . . ?
C21 C22 C31 C34 -0.2(6) . . . . ?
C23 C22 C31 C34 178.4(4) . . . . ?
Zr1 O3 C35 C36 -62(3) . . . . ?
Zr1 O3 C35 C37 172(2) . . . . ?
Zr1 O4 C38 C40 -31.9(17) . . . . ?
Zr1 O4 C38 C39 -156.7(13) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.062
####################################################################### 
# 
# 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_hf-ipr
_database_code_depnum_ccdc_archive 'CCDC 1539664'
_audit_update_record             
;
2017-03-22 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H60 Hf N4 O4'
_chemical_formula_sum            'C40 H60 Hf N4 O4'
_chemical_formula_weight         839.41

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'
Hf Hf -0.5830 6.1852 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21'

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

_cell_length_a                   11.01520(14)
_cell_length_b                   10.33345(14)
_cell_length_c                   17.7349(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.2001(13)
_cell_angle_gamma                90.00
_cell_volume                     1992.70(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5467
_cell_measurement_theta_min      3.7350
_cell_measurement_theta_max      27.9920

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             864
_exptl_absorpt_coefficient_mu    2.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96246
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7021
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         24.99
_reflns_number_total             5655
_reflns_number_gt                5381
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_chemical_absolute_configuration s
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0100P)²+1.3000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(8)
_refine_ls_number_reflns         5655
_refine_ls_number_parameters     442
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0245
_refine_ls_wR_factor_ref         0.0523
_refine_ls_wR_factor_gt          0.0511
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.014
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.013560(14) 0.31791(3) 0.704995(9) 0.01871(6) Uani 1 1 d . . .
O1 O -0.0503(4) 0.4612(5) 0.6209(3) 0.0227(11) Uani 1 1 d . . .
O2 O 0.0948(3) 0.2192(3) 0.79709(19) 0.0208(8) Uani 1 1 d . . .
O3 O -0.0124(4) 0.1853(5) 0.6285(3) 0.0310(13) Uani 1 1 d . . .
O4 O -0.1360(3) 0.3355(6) 0.74665(19) 0.0275(11) Uani 1 1 d . . .
N1 N -0.2096(4) 0.6145(4) 0.6138(3) 0.0270(10) Uani 1 1 d . . .
N2 N -0.2413(4) 0.7199(4) 0.6555(3) 0.0355(12) Uani 1 1 d . . .
N3 N 0.1118(4) 0.5029(4) 0.7558(2) 0.0206(9) Uani 1 1 d . . .
N4 N 0.2261(3) 0.3093(8) 0.68593(19) 0.0205(8) Uani 1 1 d . . .
C1 C -0.2757(5) 0.4591(6) 0.5111(3) 0.0390(15) Uani 1 1 d . . .
H1A H -0.2044 0.4108 0.5253 0.047 Uiso 1 1 calc R . .
C2 C -0.3646(6) 0.4201(7) 0.4497(4) 0.0488(17) Uani 1 1 d . . .
H2B H -0.3525 0.3448 0.4231 0.059 Uiso 1 1 calc R . .
C3 C -0.4691(6) 0.4920(7) 0.4285(4) 0.0477(17) Uani 1 1 d . . .
H3A H -0.5276 0.4661 0.3875 0.057 Uiso 1 1 calc R . .
C4 C -0.4864(5) 0.6017(6) 0.4680(3) 0.0406(15) Uani 1 1 d . . .
H4A H -0.5578 0.6498 0.4538 0.049 Uiso 1 1 calc R . .
C5 C -0.4015(5) 0.6433(6) 0.5284(3) 0.0349(14) Uani 1 1 d . . .
H5A H -0.4148 0.7191 0.5542 0.042 Uiso 1 1 calc R . .
C6 C -0.2964(5) 0.5716(5) 0.5505(3) 0.0293(13) Uani 1 1 d . . .
C7 C -0.0993(5) 0.5622(5) 0.6472(3) 0.0250(12) Uani 1 1 d . . .
C8 C -0.0566(5) 0.6390(5) 0.7116(3) 0.0267(12) Uani 1 1 d . . .
C9 C -0.1493(5) 0.7353(5) 0.7126(4) 0.0335(14) Uani 1 1 d . . .
C10 C -0.1644(5) 0.8409(7) 0.7685(4) 0.048(2) Uani 1 1 d . . .
H10A H -0.2385 0.8882 0.7508 0.072 Uiso 1 1 calc R . .
H10B H -0.0952 0.8985 0.7728 0.072 Uiso 1 1 calc R . .
H10C H -0.1690 0.8036 0.8175 0.072 Uiso 1 1 calc R . .
C11 C 0.0636(5) 0.6186(5) 0.7574(3) 0.0263(12) Uani 1 1 d . . .
C12 C 0.2404(5) 0.4759(6) 0.7893(4) 0.0229(14) Uani 1 1 d . . .
H12A H 0.2430 0.4183 0.8327 0.027 Uiso 1 1 calc R . .
H12B H 0.2819 0.5558 0.8069 0.027 Uiso 1 1 calc R . .
C13 C 0.3045(5) 0.4132(6) 0.7284(4) 0.0242(15) Uani 1 1 d . . .
H13A H 0.3806 0.3730 0.7540 0.029 Uiso 1 1 calc R . .
C14 C 0.3370(5) 0.5037(6) 0.6669(3) 0.0351(14) Uani 1 1 d U . .
H14A H 0.2747 0.5700 0.6545 0.042 Uiso 1 1 calc R . .
H14B H 0.4159 0.5449 0.6833 0.042 Uiso 1 1 calc R . .
C15 C 0.3418(5) 0.4158(6) 0.5993(3) 0.0381(15) Uani 1 1 d . . .
H15A H 0.4170 0.3654 0.6057 0.046 Uiso 1 1 calc R . .
H15B H 0.3341 0.4642 0.5519 0.046 Uiso 1 1 calc R . .
C16 C 0.2307(4) 0.3318(10) 0.6024(2) 0.0278(14) Uani 1 1 d . . .
H16A H 0.1565 0.3749 0.5780 0.033 Uiso 1 1 calc R . .
H16B H 0.2385 0.2502 0.5765 0.033 Uiso 1 1 calc R . .
C17 C 0.2770(5) 0.1759(6) 0.7063(4) 0.0245(14) Uani 1 1 d . . .
H17A H 0.3559 0.1682 0.6889 0.029 Uiso 1 1 calc R . .
H17B H 0.2222 0.1126 0.6785 0.029 Uiso 1 1 calc R . .
C18 C 0.2942(5) 0.1429(5) 0.7905(4) 0.0207(14) Uani 1 1 d . . .
C19 C 0.4019(4) 0.0843(5) 0.8248(3) 0.0240(12) Uani 1 1 d . . .
H19A H 0.4660 0.0740 0.7970 0.029 Uiso 1 1 calc R . .
C20 C 0.4167(4) 0.0407(5) 0.8996(3) 0.0246(12) Uani 1 1 d . . .
C21 C 0.3206(5) 0.0621(5) 0.9401(3) 0.0248(12) Uani 1 1 d . . .
H21A H 0.3299 0.0348 0.9906 0.030 Uiso 1 1 calc R . .
C22 C 0.2113(4) 0.1223(4) 0.9088(3) 0.0194(11) Uani 1 1 d . . .
C23 C 0.1981(5) 0.1632(4) 0.8324(3) 0.0195(11) Uani 1 1 d . . .
C24 C 0.1234(6) 0.7339(6) 0.8005(4) 0.0464(18) Uani 1 1 d . . .
H24A H 0.0567 0.7966 0.8009 0.056 Uiso 1 1 calc R . .
C25 C 0.1767(6) 0.7143(6) 0.8835(4) 0.0509(18) Uani 1 1 d . . .
H25A H 0.1172 0.6722 0.9091 0.076 Uiso 1 1 calc R . .
H25B H 0.1978 0.7967 0.9070 0.076 Uiso 1 1 calc R . .
H25C H 0.2492 0.6615 0.8872 0.076 Uiso 1 1 calc R . .
C26 C 0.2150(6) 0.8009(10) 0.7560(4) 0.067(2) Uani 1 1 d . . .
H26A H 0.1776 0.8117 0.7036 0.101 Uiso 1 1 calc R . .
H26B H 0.2876 0.7487 0.7584 0.101 Uiso 1 1 calc R . .
H26C H 0.2367 0.8842 0.7782 0.101 Uiso 1 1 calc R . .
C27 C 0.5342(5) -0.0315(5) 0.9350(3) 0.0341(14) Uani 1 1 d . . .
C28 C 0.6464(6) 0.0521(7) 0.9295(5) 0.068(2) Uani 1 1 d U . .
H28A H 0.6405 0.1316 0.9567 0.102 Uiso 1 1 calc R . .
H28B H 0.6499 0.0706 0.8769 0.102 Uiso 1 1 calc R . .
H28C H 0.7195 0.0067 0.9516 0.102 Uiso 1 1 calc R . .
C29 C 0.5437(6) -0.1595(9) 0.8911(4) 0.065(3) Uani 1 1 d . . .
H29A H 0.6170 -0.2048 0.9131 0.097 Uiso 1 1 calc R . .
H29B H 0.5468 -0.1408 0.8385 0.097 Uiso 1 1 calc R . .
H29C H 0.4731 -0.2124 0.8947 0.097 Uiso 1 1 calc R . .
C30 C 0.5343(6) -0.0682(8) 1.0184(4) 0.063(2) Uani 1 1 d . . .
H30A H 0.5285 0.0088 1.0480 0.094 Uiso 1 1 calc R . .
H30B H 0.6091 -0.1130 1.0378 0.094 Uiso 1 1 calc R . .
H30C H 0.4653 -0.1234 1.0220 0.094 Uiso 1 1 calc R . .
C31 C 0.1056(5) 0.1435(5) 0.9550(3) 0.0251(12) Uani 1 1 d . . .
C32 C 0.0778(5) 0.2879(5) 0.9603(3) 0.0329(17) Uani 1 1 d . . .
H32A H 0.1501 0.3323 0.9845 0.049 Uiso 1 1 calc R . .
H32B H 0.0127 0.2999 0.9897 0.049 Uiso 1 1 calc R . .
H32C H 0.0530 0.3222 0.9098 0.049 Uiso 1 1 calc R . .
C33 C -0.0107(5) 0.0729(5) 0.9160(3) 0.0275(12) Uani 1 1 d . . .
H33A H -0.0762 0.0864 0.9450 0.041 Uiso 1 1 calc R . .
H33B H 0.0059 -0.0181 0.9134 0.041 Uiso 1 1 calc R . .
H33C H -0.0345 0.1063 0.8653 0.041 Uiso 1 1 calc R . .
C34 C 0.1372(5) 0.0902(6) 1.0354(3) 0.0381(15) Uani 1 1 d . . .
H34A H 0.2097 0.1324 1.0613 0.057 Uiso 1 1 calc R . .
H34B H 0.1519 -0.0012 1.0332 0.057 Uiso 1 1 calc R . .
H34C H 0.0699 0.1056 1.0626 0.057 Uiso 1 1 calc R . .
C35 C -0.0224(6) 0.0978(6) 0.5675(3) 0.0404(15) Uani 1 1 d . . .
H35A H 0.0605 0.0828 0.5559 0.049 Uiso 1 1 calc R . .
C36 C -0.0978(6) 0.1555(6) 0.4978(3) 0.0475(17) Uani 1 1 d . . .
H36A H -0.0623 0.2365 0.4862 0.071 Uiso 1 1 calc R . .
H36B H -0.1802 0.1697 0.5072 0.071 Uiso 1 1 calc R . .
H36C H -0.0992 0.0974 0.4555 0.071 Uiso 1 1 calc R . .
C37 C -0.0711(8) -0.0293(6) 0.5900(4) 0.071(2) Uani 1 1 d U . .
H37A H -0.0193 -0.0614 0.6347 0.106 Uiso 1 1 calc R . .
H37B H -0.0721 -0.0901 0.5490 0.106 Uiso 1 1 calc R . .
H37C H -0.1532 -0.0178 0.6007 0.106 Uiso 1 1 calc R . .
C38 C -0.2502(4) 0.3192(13) 0.7709(3) 0.0450(13) Uani 1 1 d . . .
H38A H -0.2357 0.2781 0.8213 0.054 Uiso 1 1 calc R . .
C39 C -0.3271(6) 0.2292(8) 0.7167(5) 0.072(2) Uani 1 1 d U . .
H39A H -0.2839 0.1491 0.7141 0.107 Uiso 1 1 calc R . .
H39B H -0.3431 0.2679 0.6669 0.107 Uiso 1 1 calc R . .
H39C H -0.4035 0.2130 0.7345 0.107 Uiso 1 1 calc R . .
C40 C -0.3099(6) 0.4457(8) 0.7784(5) 0.070(2) Uani 1 1 d . . .
H40A H -0.2567 0.4992 0.8136 0.105 Uiso 1 1 calc R . .
H40B H -0.3861 0.4327 0.7971 0.105 Uiso 1 1 calc R . .
H40C H -0.3258 0.4874 0.7294 0.105 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O3 1.917(5) . ?
Hf1 O4 1.919(3) . ?
Hf1 O2 2.010(3) . ?
Hf1 O1 2.139(5) . ?
Hf1 N3 2.308(4) . ?
Hf1 N4 2.420(3) . ?
O1 C7 1.296(7) . ?
O2 C23 1.340(6) . ?
O3 C35 1.402(7) . ?
O4 C38 1.402(5) . ?
N1 C7 1.374(6) . ?
N1 N2 1.392(6) . ?
N1 C6 1.424(7) . ?
N2 C9 1.322(7) . ?
N3 C11 1.310(6) . ?
N3 C12 1.472(7) . ?
N4 C13 1.502(9) . ?
N4 C16 1.509(5) . ?
N4 C17 1.510(10) . ?
C1 C6 1.394(8) . ?
C1 C2 1.402(8) . ?
C1 H1A 0.9300 . ?
C2 C3 1.372(8) . ?
C2 H2B 0.9300 . ?
C3 C4 1.363(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.373(8) . ?
C4 H4A 0.9300 . ?
C5 C6 1.378(7) . ?
C5 H5A 0.9300 . ?
C7 C8 1.409(7) . ?
C8 C9 1.428(7) . ?
C8 C11 1.454(7) . ?
C9 C10 1.501(8) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C24 1.509(7) . ?
C12 C13 1.526(8) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 C14 1.522(7) . ?
C13 H13A 0.9800 . ?
C14 C15 1.511(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 C16 1.509(9) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.515(8) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.383(7) . ?
C18 C23 1.402(7) . ?
C19 C20 1.385(7) . ?
C19 H19A 0.9300 . ?
C20 C21 1.389(7) . ?
C20 C27 1.538(7) . ?
C21 C22 1.390(7) . ?
C21 H21A 0.9300 . ?
C22 C23 1.405(7) . ?
C22 C31 1.543(7) . ?
C24 C25 1.508(8) . ?
C24 C26 1.541(9) . ?
C24 H24A 0.9800 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.524(8) . ?
C27 C30 1.528(8) . ?
C27 C29 1.546(10) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C34 1.516(7) . ?
C31 C32 1.529(7) . ?
C31 C33 1.540(7) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C37 1.497(9) . ?
C35 C36 1.497(8) . ?
C35 H35A 0.9800 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 C40 1.480(14) . ?
C38 C39 1.497(11) . ?
C38 H38A 0.9800 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?

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 Hf1 O4 107.5(2) . . ?
O3 Hf1 O2 102.06(19) . . ?
O4 Hf1 O2 91.91(15) . . ?
O3 Hf1 O1 90.37(13) . . ?
O4 Hf1 O1 89.76(18) . . ?
O2 Hf1 O1 166.31(16) . . ?
O3 Hf1 N3 151.15(19) . . ?
O4 Hf1 N3 98.58(18) . . ?
O2 Hf1 N3 89.03(15) . . ?
O1 Hf1 N3 77.29(16) . . ?
O3 Hf1 N4 85.0(2) . . ?
O4 Hf1 N4 165.15(14) . . ?
O2 Hf1 N4 77.30(15) . . ?
O1 Hf1 N4 98.37(19) . . ?
N3 Hf1 N4 71.4(2) . . ?
C7 O1 Hf1 114.7(4) . . ?
C23 O2 Hf1 146.4(3) . . ?
C35 O3 Hf1 172.9(5) . . ?
C38 O4 Hf1 166.8(7) . . ?
C7 N1 N2 111.0(4) . . ?
C7 N1 C6 130.8(5) . . ?
N2 N1 C6 118.0(4) . . ?
C9 N2 N1 105.9(4) . . ?
C11 N3 C12 122.1(4) . . ?
C11 N3 Hf1 126.7(3) . . ?
C12 N3 Hf1 111.2(3) . . ?
C13 N4 C16 106.0(6) . . ?
C13 N4 C17 111.7(4) . . ?
C16 N4 C17 107.8(6) . . ?
C13 N4 Hf1 113.3(4) . . ?
C16 N4 Hf1 108.5(3) . . ?
C17 N4 Hf1 109.3(4) . . ?
C6 C1 C2 118.7(6) . . ?
C6 C1 H1A 120.7 . . ?
C2 C1 H1A 120.7 . . ?
C3 C2 C1 120.6(6) . . ?
C3 C2 H2B 119.7 . . ?
C1 C2 H2B 119.7 . . ?
C4 C3 C2 119.3(6) . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 H3A 120.3 . . ?
C3 C4 C5 121.9(6) . . ?
C3 C4 H4A 119.1 . . ?
C5 C4 H4A 119.1 . . ?
C4 C5 C6 119.3(6) . . ?
C4 C5 H5A 120.3 . . ?
C6 C5 H5A 120.3 . . ?
C5 C6 C1 120.2(5) . . ?
C5 C6 N1 119.0(5) . . ?
C1 C6 N1 120.8(5) . . ?
O1 C7 N1 123.6(5) . . ?
O1 C7 C8 129.8(5) . . ?
N1 C7 C8 106.6(4) . . ?
C7 C8 C9 104.8(5) . . ?
C7 C8 C11 121.9(5) . . ?
C9 C8 C11 133.1(5) . . ?
N2 C9 C8 111.6(5) . . ?
N2 C9 C10 116.1(5) . . ?
C8 C9 C10 132.0(5) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N3 C11 C8 117.1(5) . . ?
N3 C11 C24 125.9(5) . . ?
C8 C11 C24 117.0(5) . . ?
N3 C12 C13 108.6(5) . . ?
N3 C12 H12A 110.0 . . ?
C13 C12 H12A 110.0 . . ?
N3 C12 H12B 110.0 . . ?
C13 C12 H12B 110.0 . . ?
H12A C12 H12B 108.3 . . ?
N4 C13 C14 105.2(5) . . ?
N4 C13 C12 111.4(4) . . ?
C14 C13 C12 115.7(5) . . ?
N4 C13 H13A 108.1 . . ?
C14 C13 H13A 108.1 . . ?
C12 C13 H13A 108.1 . . ?
C15 C14 C13 104.0(5) . . ?
C15 C14 H14A 111.0 . . ?
C13 C14 H14A 111.0 . . ?
C15 C14 H14B 111.0 . . ?
C13 C14 H14B 111.0 . . ?
H14A C14 H14B 109.0 . . ?
C14 C15 C16 100.7(4) . . ?
C14 C15 H15A 111.6 . . ?
C16 C15 H15A 111.6 . . ?
C14 C15 H15B 111.6 . . ?
C16 C15 H15B 111.6 . . ?
H15A C15 H15B 109.4 . . ?
N4 C16 C15 106.2(5) . . ?
N4 C16 H16A 110.5 . . ?
C15 C16 H16A 110.5 . . ?
N4 C16 H16B 110.5 . . ?
C15 C16 H16B 110.5 . . ?
H16A C16 H16B 108.7 . . ?
N4 C17 C18 115.1(5) . . ?
N4 C17 H17A 108.5 . . ?
C18 C17 H17A 108.5 . . ?
N4 C17 H17B 108.5 . . ?
C18 C17 H17B 108.5 . . ?
H17A C17 H17B 107.5 . . ?
C19 C18 C23 120.0(5) . . ?
C19 C18 C17 119.7(5) . . ?
C23 C18 C17 120.2(5) . . ?
C20 C19 C18 121.6(5) . . ?
C20 C19 H19A 119.2 . . ?
C18 C19 H19A 119.2 . . ?
C19 C20 C21 117.4(5) . . ?
C19 C20 C27 120.7(5) . . ?
C21 C20 C27 121.8(5) . . ?
C20 C21 C22 123.2(5) . . ?
C20 C21 H21A 118.4 . . ?
C22 C21 H21A 118.4 . . ?
C21 C22 C23 118.0(5) . . ?
C21 C22 C31 122.0(5) . . ?
C23 C22 C31 120.0(4) . . ?
O2 C23 C18 118.3(5) . . ?
O2 C23 C22 122.0(5) . . ?
C18 C23 C22 119.7(5) . . ?
C11 C24 C25 117.3(5) . . ?
C11 C24 C26 111.3(6) . . ?
C25 C24 C26 112.1(5) . . ?
C11 C24 H24A 105.0 . . ?
C25 C24 H24A 105.0 . . ?
C26 C24 H24A 105.0 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 C30 109.1(5) . . ?
C28 C27 C20 109.7(5) . . ?
C30 C27 C20 112.7(5) . . ?
C28 C27 C29 109.4(5) . . ?
C30 C27 C29 106.6(5) . . ?
C20 C27 C29 109.3(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C34 C31 C32 108.4(5) . . ?
C34 C31 C33 107.4(4) . . ?
C32 C31 C33 109.2(4) . . ?
C34 C31 C22 111.7(4) . . ?
C32 C31 C22 110.3(4) . . ?
C33 C31 C22 109.8(4) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O3 C35 C37 110.3(6) . . ?
O3 C35 C36 110.2(5) . . ?
C37 C35 C36 113.2(5) . . ?
O3 C35 H35A 107.6 . . ?
C37 C35 H35A 107.6 . . ?
C36 C35 H35A 107.6 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
O4 C38 C40 110.8(9) . . ?
O4 C38 C39 108.8(6) . . ?
C40 C38 C39 113.1(6) . . ?
O4 C38 H38A 108.0 . . ?
C40 C38 H38A 108.0 . . ?
C39 C38 H38A 108.0 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Hf1 O1 C7 152.2(4) . . . . ?
O4 Hf1 O1 C7 44.7(4) . . . . ?
O2 Hf1 O1 C7 -52.4(8) . . . . ?
N3 Hf1 O1 C7 -54.2(4) . . . . ?
N4 Hf1 O1 C7 -122.8(4) . . . . ?
O3 Hf1 O2 C23 75.8(6) . . . . ?
O4 Hf1 O2 C23 -175.9(6) . . . . ?
O1 Hf1 O2 C23 -79.1(9) . . . . ?
N3 Hf1 O2 C23 -77.4(6) . . . . ?
N4 Hf1 O2 C23 -6.2(6) . . . . ?
O4 Hf1 O3 C35 143(4) . . . . ?
O2 Hf1 O3 C35 -121(4) . . . . ?
O1 Hf1 O3 C35 53(4) . . . . ?
N3 Hf1 O3 C35 -11(4) . . . . ?
N4 Hf1 O3 C35 -45(4) . . . . ?
O3 Hf1 O4 C38 22.9(17) . . . . ?
O2 Hf1 O4 C38 -80.4(17) . . . . ?
O1 Hf1 O4 C38 113.2(17) . . . . ?
N3 Hf1 O4 C38 -169.7(17) . . . . ?
N4 Hf1 O4 C38 -123.3(17) . . . . ?
C7 N1 N2 C9 2.1(6) . . . . ?
C6 N1 N2 C9 176.7(5) . . . . ?
O3 Hf1 N3 C11 109.5(5) . . . . ?
O4 Hf1 N3 C11 -45.0(4) . . . . ?
O2 Hf1 N3 C11 -136.8(4) . . . . ?
O1 Hf1 N3 C11 42.8(4) . . . . ?
N4 Hf1 N3 C11 146.3(5) . . . . ?
O3 Hf1 N3 C12 -71.7(5) . . . . ?
O4 Hf1 N3 C12 133.8(4) . . . . ?
O2 Hf1 N3 C12 42.0(4) . . . . ?
O1 Hf1 N3 C12 -138.4(4) . . . . ?
N4 Hf1 N3 C12 -34.9(4) . . . . ?
O3 Hf1 N4 C13 173.1(4) . . . . ?
O4 Hf1 N4 C13 -39.1(14) . . . . ?
O2 Hf1 N4 C13 -83.3(4) . . . . ?
O1 Hf1 N4 C13 83.4(4) . . . . ?
N3 Hf1 N4 C13 10.0(4) . . . . ?
O3 Hf1 N4 C16 55.7(6) . . . . ?
O4 Hf1 N4 C16 -156.5(9) . . . . ?
O2 Hf1 N4 C16 159.2(6) . . . . ?
O1 Hf1 N4 C16 -34.0(6) . . . . ?
N3 Hf1 N4 C16 -107.5(6) . . . . ?
O3 Hf1 N4 C17 -61.6(4) . . . . ?
O4 Hf1 N4 C17 86.2(12) . . . . ?
O2 Hf1 N4 C17 42.0(3) . . . . ?
O1 Hf1 N4 C17 -151.2(3) . . . . ?
N3 Hf1 N4 C17 135.3(3) . . . . ?
C6 C1 C2 C3 0.6(10) . . . . ?
C1 C2 C3 C4 -0.4(10) . . . . ?
C2 C3 C4 C5 0.5(9) . . . . ?
C3 C4 C5 C6 -0.8(9) . . . . ?
C4 C5 C6 C1 1.0(8) . . . . ?
C4 C5 C6 N1 -179.2(5) . . . . ?
C2 C1 C6 C5 -0.9(9) . . . . ?
C2 C1 C6 N1 179.3(5) . . . . ?
C7 N1 C6 C5 180.0(5) . . . . ?
N2 N1 C6 C5 6.6(7) . . . . ?
C7 N1 C6 C1 -0.2(9) . . . . ?
N2 N1 C6 C1 -173.6(5) . . . . ?
Hf1 O1 C7 N1 -132.4(4) . . . . ?
Hf1 O1 C7 C8 47.4(7) . . . . ?
N2 N1 C7 O1 178.2(5) . . . . ?
C6 N1 C7 O1 4.5(9) . . . . ?
N2 N1 C7 C8 -1.7(6) . . . . ?
C6 N1 C7 C8 -175.4(5) . . . . ?
O1 C7 C8 C9 -179.3(6) . . . . ?
N1 C7 C8 C9 0.6(6) . . . . ?
O1 C7 C8 C11 5.5(9) . . . . ?
N1 C7 C8 C11 -174.7(5) . . . . ?
N1 N2 C9 C8 -1.7(7) . . . . ?
N1 N2 C9 C10 -177.4(5) . . . . ?
C7 C8 C9 N2 0.7(7) . . . . ?
C11 C8 C9 N2 175.2(6) . . . . ?
C7 C8 C9 C10 175.5(6) . . . . ?
C11 C8 C9 C10 -10.0(11) . . . . ?
C12 N3 C11 C8 169.8(5) . . . . ?
Hf1 N3 C11 C8 -11.5(7) . . . . ?
C12 N3 C11 C24 -8.1(9) . . . . ?
Hf1 N3 C11 C24 170.7(4) . . . . ?
C7 C8 C11 N3 -24.4(8) . . . . ?
C9 C8 C11 N3 161.9(6) . . . . ?
C7 C8 C11 C24 153.7(5) . . . . ?
C9 C8 C11 C24 -20.1(9) . . . . ?
C11 N3 C12 C13 -125.7(5) . . . . ?
Hf1 N3 C12 C13 55.3(5) . . . . ?
C16 N4 C13 C14 7.8(6) . . . . ?
C17 N4 C13 C14 125.0(5) . . . . ?
Hf1 N4 C13 C14 -111.0(4) . . . . ?
C16 N4 C13 C12 134.0(5) . . . . ?
C17 N4 C13 C12 -108.9(5) . . . . ?
Hf1 N4 C13 C12 15.1(6) . . . . ?
N3 C12 C13 N4 -45.2(7) . . . . ?
N3 C12 C13 C14 74.9(6) . . . . ?
N4 C13 C14 C15 -31.4(6) . . . . ?
C12 C13 C14 C15 -154.7(5) . . . . ?
C13 C14 C15 C16 41.9(6) . . . . ?
C13 N4 C16 C15 18.6(7) . . . . ?
C17 N4 C16 C15 -101.1(7) . . . . ?
Hf1 N4 C16 C15 140.6(5) . . . . ?
C14 C15 C16 N4 -37.4(7) . . . . ?
C13 N4 C17 C18 56.7(5) . . . . ?
C16 N4 C17 C18 172.8(5) . . . . ?
Hf1 N4 C17 C18 -69.5(5) . . . . ?
N4 C17 C18 C19 -134.8(5) . . . . ?
N4 C17 C18 C23 49.6(7) . . . . ?
C23 C18 C19 C20 2.1(8) . . . . ?
C17 C18 C19 C20 -173.5(5) . . . . ?
C18 C19 C20 C21 -2.2(7) . . . . ?
C18 C19 C20 C27 176.2(5) . . . . ?
C19 C20 C21 C22 1.2(7) . . . . ?
C27 C20 C21 C22 -177.3(5) . . . . ?
C20 C21 C22 C23 0.0(7) . . . . ?
C20 C21 C22 C31 179.4(4) . . . . ?
Hf1 O2 C23 C18 -13.2(8) . . . . ?
Hf1 O2 C23 C22 168.2(4) . . . . ?
C19 C18 C23 O2 -179.5(5) . . . . ?
C17 C18 C23 O2 -3.9(7) . . . . ?
C19 C18 C23 C22 -0.8(8) . . . . ?
C17 C18 C23 C22 174.7(5) . . . . ?
C21 C22 C23 O2 178.4(4) . . . . ?
C31 C22 C23 O2 -1.0(7) . . . . ?
C21 C22 C23 C18 -0.2(7) . . . . ?
C31 C22 C23 C18 -179.6(5) . . . . ?
N3 C11 C24 C25 -49.7(8) . . . . ?
C8 C11 C24 C25 132.5(6) . . . . ?
N3 C11 C24 C26 81.3(8) . . . . ?
C8 C11 C24 C26 -96.6(6) . . . . ?
C19 C20 C27 C28 56.7(7) . . . . ?
C21 C20 C27 C28 -124.9(6) . . . . ?
C19 C20 C27 C30 178.4(5) . . . . ?
C21 C20 C27 C30 -3.2(7) . . . . ?
C19 C20 C27 C29 -63.3(7) . . . . ?
C21 C20 C27 C29 115.1(6) . . . . ?
C21 C22 C31 C34 -0.5(7) . . . . ?
C23 C22 C31 C34 178.8(4) . . . . ?
C21 C22 C31 C32 120.1(5) . . . . ?
C23 C22 C31 C32 -60.6(6) . . . . ?
C21 C22 C31 C33 -119.6(5) . . . . ?
C23 C22 C31 C33 59.7(6) . . . . ?
Hf1 O3 C35 C37 166(3) . . . . ?
Hf1 O3 C35 C36 -68(4) . . . . ?
Hf1 O4 C38 C40 -155.8(16) . . . . ?
Hf1 O4 C38 C39 -31(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.075
