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

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1018937'
_audit_update_record             
;
2015-04-28 deposited with the CCDC.
2015-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C88 H128 N4 O8 Ti2, 4(C7 H8)'
_chemical_formula_sum            'C116 H160 N4 O8 Ti2'
_chemical_formula_weight         1834.27

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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.524(8)
_cell_length_b                   15.116(11)
_cell_length_c                   16.715(12)
_cell_angle_alpha                74.45(3)
_cell_angle_beta                 83.73(4)
_cell_angle_gamma                73.38(4)
_cell_volume                     2686(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1594
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      16.74

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_F_000             992
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    0.204
_shelx_estimated_absorpt_T_min   0.951
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24529
_diffrn_reflns_av_unetI/netI     0.2289
_diffrn_reflns_av_R_equivalents  0.1515
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.452
_diffrn_reflns_theta_max         23.180
_diffrn_reflns_theta_full        23.180
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 0.958
_reflns_number_total             7331
_reflns_number_gt                2700
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1366P)²+0.2661P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.026(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         7331
_refine_ls_number_parameters     581
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.2500
_refine_ls_R_factor_gt           0.0958
_refine_ls_wR_factor_ref         0.3125
_refine_ls_wR_factor_gt          0.2234
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2660(7) 0.6974(6) 0.3093(5) 0.059(2) Uani 1 1 d . . . . .
C2 C 0.2780(7) 0.7899(6) 0.2768(5) 0.055(2) Uani 1 1 d . . . . .
C3 C 0.2907(7) 0.8363(6) 0.3333(6) 0.064(2) Uani 1 1 d . . . . .
H3 H 0.2971 0.8983 0.3123 0.077 Uiso 1 1 calc R U . . .
C4 C 0.2951(7) 0.8007(6) 0.4188(5) 0.058(2) Uani 1 1 d . . . . .
C5 C 0.2884(7) 0.7098(6) 0.4457(5) 0.060(2) Uani 1 1 d . . . . .
H5 H 0.2931 0.6818 0.5025 0.072 Uiso 1 1 calc R U . . .
C6 C 0.2751(7) 0.6553(6) 0.3947(5) 0.058(2) Uani 1 1 d . . . . .
C7 C 0.2682(7) 0.5611(6) 0.4287(5) 0.062(2) Uani 1 1 d . . . . .
H7 H 0.2668 0.5409 0.4864 0.074 Uiso 1 1 calc R U . . .
C8 C 0.2575(9) 0.4069(6) 0.4377(5) 0.082(3) Uani 1 1 d . . . . .
H8A H 0.3294 0.3614 0.4231 0.099 Uiso 1 1 calc R U . . .
H8B H 0.1886 0.3941 0.4190 0.099 Uiso 1 1 calc R U . . .
C9 C 0.2472(9) 0.3864(5) 0.5295(5) 0.058(2) Uani 1 1 d . . . . .
C10 C 0.3497(9) 0.3508(6) 0.5763(7) 0.071(2) Uani 1 1 d . . . . .
H10 H 0.4260 0.3455 0.5502 0.085 Uiso 1 1 calc R U . . .
C11 C 0.3392(10) 0.3239(6) 0.6597(7) 0.075(3) Uani 1 1 d . . . . .
H11 H 0.4090 0.3000 0.6903 0.090 Uiso 1 1 calc R U . . .
C12 C 0.2300(11) 0.3306(6) 0.7003(5) 0.071(3) Uani 1 1 d . . . . .
H12 H 0.2254 0.3102 0.7579 0.086 Uiso 1 1 calc R U . . .
C13 C 0.1251(8) 0.3678(5) 0.6556(5) 0.053(2) Uani 1 1 d . . . . .
C14 C 0.1397(8) 0.3931(5) 0.5724(6) 0.059(2) Uani 1 1 d . . . . .
H14 H 0.0700 0.4172 0.5417 0.071 Uiso 1 1 calc R U . . .
C15 C 0.0036(8) 0.3702(6) 0.6956(6) 0.078(3) Uani 1 1 d . . . . .
H15A H 0.0139 0.3195 0.7464 0.093 Uiso 1 1 calc R U . . .
H15B H -0.0431 0.3544 0.6592 0.093 Uiso 1 1 calc R U . . .
C17 C 0.2775(9) 0.8344(6) 0.1843(5) 0.067(2) Uani 1 1 d . . . . .
C18 C 0.1549(10) 0.8444(7) 0.1514(6) 0.102(3) Uani 1 1 d . . . . .
H18A H 0.1518 0.8781 0.0938 0.153 Uiso 1 1 calc R U . . .
H18B H 0.0916 0.8792 0.1824 0.153 Uiso 1 1 calc R U . . .
H18C H 0.1441 0.7823 0.1572 0.153 Uiso 1 1 calc R U . . .
C19 C 0.3770(9) 0.7710(7) 0.1413(5) 0.093(3) Uani 1 1 d . . . . .
H19A H 0.4539 0.7634 0.1632 0.139 Uiso 1 1 calc R U . . .
H19B H 0.3784 0.7999 0.0827 0.139 Uiso 1 1 calc R U . . .
H19C H 0.3618 0.7098 0.1507 0.139 Uiso 1 1 calc R U . . .
C20 C 0.2979(11) 0.9321(7) 0.1641(5) 0.098(3) Uani 1 1 d . . . . .
H20A H 0.3787 0.9268 0.1778 0.147 Uiso 1 1 calc R U . . .
H20B H 0.2407 0.9706 0.1956 0.147 Uiso 1 1 calc R U . . .
H20C H 0.2873 0.9611 0.1058 0.147 Uiso 1 1 calc R U . . .
C21 C 0.2987(9) 0.8627(6) 0.4751(6) 0.077(3) Uani 1 1 d . . . . .
C22 C 0.4060(12) 0.9030(9) 0.4511(7) 0.135(5) Uani 1 1 d . . . . .
H22A H 0.4749 0.8546 0.4388 0.202 Uiso 1 1 calc R U . . .
H22B H 0.4236 0.9246 0.4963 0.202 Uiso 1 1 calc R U . . .
H22C H 0.3881 0.9556 0.4030 0.202 Uiso 1 1 calc R U . . .
C23 C 0.1822(10) 0.9420(7) 0.4695(7) 0.113(4) Uani 1 1 d . . . . .
H23A H 0.1713 0.9786 0.4129 0.170 Uiso 1 1 calc R U . . .
H23B H 0.1863 0.9827 0.5038 0.170 Uiso 1 1 calc R U . . .
H23C H 0.1151 0.9150 0.4883 0.170 Uiso 1 1 calc R U . . .
C24 C 0.3102(13) 0.8092(7) 0.5641(6) 0.133(5) Uani 1 1 d . . . . .
H24A H 0.2384 0.7886 0.5833 0.199 Uiso 1 1 calc R U . . .
H24B H 0.3204 0.8499 0.5965 0.199 Uiso 1 1 calc R U . . .
H24C H 0.3793 0.7547 0.5696 0.199 Uiso 1 1 calc R U . . .
C25 C 0.1973(9) 0.3504(6) 0.2517(4) 0.059(2) Uani 1 1 d . . . . .
C26 C 0.2417(8) 0.2636(6) 0.2318(5) 0.062(2) Uani 1 1 d . . . . .
C27 C 0.1624(9) 0.2185(6) 0.2183(5) 0.064(2) Uani 1 1 d . . . . .
H27 H 0.1930 0.1603 0.2046 0.077 Uiso 1 1 calc R U . . .
C28 C 0.0367(9) 0.2551(6) 0.2241(5) 0.066(2) Uani 1 1 d . . . . .
C29 C -0.0048(8) 0.3408(6) 0.2445(5) 0.067(2) Uani 1 1 d . . . . .
H29 H -0.0879 0.3662 0.2503 0.080 Uiso 1 1 calc R U . . .
C30 C 0.0714(8) 0.3911(5) 0.2568(5) 0.059(2) Uani 1 1 d . . . . .
C31 C 0.3778(8) 0.2194(6) 0.2235(6) 0.075(3) Uani 1 1 d . . . . .
C32 C 0.4368(9) 0.2845(7) 0.1549(7) 0.108(3) Uani 1 1 d . . . . .
H32A H 0.3989 0.2965 0.1033 0.162 Uiso 1 1 calc R U . . .
H32B H 0.5216 0.2540 0.1493 0.162 Uiso 1 1 calc R U . . .
H32C H 0.4268 0.3437 0.1692 0.162 Uiso 1 1 calc R U . . .
C33 C 0.4397(9) 0.2016(7) 0.3056(6) 0.111(4) Uani 1 1 d . . . . .
H33A H 0.5253 0.1746 0.2986 0.166 Uiso 1 1 calc R U . . .
H33B H 0.4067 0.1582 0.3486 0.166 Uiso 1 1 calc R U . . .
H33C H 0.4258 0.2608 0.3206 0.166 Uiso 1 1 calc R U . . .
C34 C 0.4082(9) 0.1237(6) 0.2014(7) 0.102(3) Uani 1 1 d . . . . .
H34A H 0.3829 0.1331 0.1462 0.153 Uiso 1 1 calc R U . . .
H34B H 0.3669 0.0824 0.2401 0.153 Uiso 1 1 calc R U . . .
H34C H 0.4941 0.0952 0.2040 0.153 Uiso 1 1 calc R U . . .
C35 C -0.0434(8) 0.1966(6) 0.2123(6) 0.074(3) Uani 1 1 d . . . . .
C36 C -0.0234(10) 0.1060(7) 0.2780(7) 0.114(4) Uani 1 1 d . . . . .
H36A H 0.0607 0.0718 0.2774 0.170 Uiso 1 1 calc R U . . .
H36B H -0.0715 0.0680 0.2680 0.170 Uiso 1 1 calc R U . . .
H36C H -0.0464 0.1198 0.3313 0.170 Uiso 1 1 calc R U . . .
C37 C -0.0134(10) 0.1724(8) 0.1280(6) 0.116(4) Uani 1 1 d . . . . .
H37A H 0.0707 0.1389 0.1249 0.174 Uiso 1 1 calc R U . . .
H37B H -0.0297 0.2302 0.0845 0.174 Uiso 1 1 calc R U . . .
H37C H -0.0623 0.1330 0.1217 0.174 Uiso 1 1 calc R U . . .
C38 C -0.1753(9) 0.2508(7) 0.2143(7) 0.107(4) Uani 1 1 d . . . . .
H38A H -0.2244 0.2116 0.2078 0.160 Uiso 1 1 calc R U . . .
H38B H -0.1894 0.3077 0.1699 0.160 Uiso 1 1 calc R U . . .
H38C H -0.1961 0.2676 0.2665 0.160 Uiso 1 1 calc R U . . .
C39 C 0.250(2) 0.5612(13) 0.0656(11) 0.181(6) Uani 1 1 d . U . . .
H39 H 0.1910 0.6239 0.0526 0.217 Uiso 1 1 calc R U . . .
C40 C 0.172(2) 0.5219(14) 0.0335(10) 0.254(11) Uani 1 1 d . . . . .
H40A H 0.1867 0.5308 -0.0254 0.381 Uiso 1 1 calc R U . . .
H40B H 0.0891 0.5535 0.0446 0.381 Uiso 1 1 calc R U . . .
H40C H 0.1875 0.4551 0.0597 0.381 Uiso 1 1 calc R U . . .
C41 C 0.334(2) 0.598(2) 0.0153(10) 0.323(16) Uani 1 1 d . . . . .
H41A H 0.2945 0.6486 -0.0294 0.484 Uiso 1 1 calc R U . . .
H41B H 0.3892 0.5486 -0.0071 0.484 Uiso 1 1 calc R U . . .
H41C H 0.3777 0.6216 0.0465 0.484 Uiso 1 1 calc R U . . .
C42 C 0.5324(12) 0.5127(9) 0.2626(7) 0.117(4) Uani 1 1 d . . . . .
H42 H 0.5053 0.5772 0.2714 0.141 Uiso 1 1 calc R U . . .
C43 C 0.5927(12) 0.4572(8) 0.3349(8) 0.137(5) Uani 1 1 d . . . . .
H43A H 0.5404 0.4662 0.3825 0.206 Uiso 1 1 calc R U . . .
H43B H 0.6646 0.4761 0.3378 0.206 Uiso 1 1 calc R U . . .
H43C H 0.6144 0.3913 0.3340 0.206 Uiso 1 1 calc R U . . .
C44 C 0.6114(12) 0.5220(10) 0.1888(8) 0.146(5) Uani 1 1 d . . . . .
H44A H 0.6300 0.4648 0.1698 0.219 Uiso 1 1 calc R U . . .
H44B H 0.6850 0.5321 0.2018 0.219 Uiso 1 1 calc R U . . .
H44C H 0.5714 0.5752 0.1461 0.219 Uiso 1 1 calc R U . . .
C45 C 0.2266(15) 0.1158(6) 0.6191(10) 0.191(10) Uani 1 1 d G . . . .
C46 C 0.1066(18) 0.1364(9) 0.6480(7) 0.262(15) Uani 1 1 d G . . . .
H46 H 0.0879 0.1179 0.7045 0.314 Uiso 1 1 calc R U . . .
C47 C 0.0145(10) 0.1848(9) 0.5924(12) 0.174(8) Uani 1 1 d G . . . .
H47 H -0.0659 0.1986 0.6117 0.209 Uiso 1 1 calc R U . . .
C48 C 0.0423(11) 0.2125(7) 0.5079(11) 0.160(7) Uani 1 1 d G . . . .
H48 H -0.0193 0.2449 0.4708 0.192 Uiso 1 1 calc R U . . .
C49 C 0.1624(15) 0.1919(7) 0.4791(7) 0.169(7) Uani 1 1 d G . . . .
H49 H 0.1810 0.2104 0.4226 0.203 Uiso 1 1 calc R U . . .
C50 C 0.2545(8) 0.1435(7) 0.5346(11) 0.127(6) Uani 1 1 d G . . . .
H50 H 0.3348 0.1297 0.5153 0.152 Uiso 1 1 calc R U . . .
C51 C 0.299(2) 0.0671(13) 0.6775(14) 0.298(13) Uani 1 1 d . U . . .
H51A H 0.3553 0.1020 0.6816 0.447 Uiso 1 1 calc R U . . .
H51B H 0.3433 0.0075 0.6657 0.447 Uiso 1 1 calc R U . . .
H51C H 0.2539 0.0554 0.7291 0.447 Uiso 1 1 calc R U . . .
C52 C 0.341(2) 0.143(2) 0.9425(9) 0.29(2) Uani 1 1 d G . . . .
H52 H 0.4052 0.1652 0.9506 0.350 Uiso 1 1 calc R U . . .
C53 C 0.223(3) 0.2004(13) 0.9424(8) 0.30(2) Uani 1 1 d G . . . .
C54 C 0.1275(16) 0.1670(17) 0.9303(8) 0.255(15) Uani 1 1 d G . . . .
H54 H 0.0485 0.2055 0.9303 0.306 Uiso 1 1 calc R U . . .
C55 C 0.1501(18) 0.0761(18) 0.9181(8) 0.38(3) Uani 1 1 d G . . . .
H55 H 0.0861 0.0537 0.9100 0.451 Uiso 1 1 calc R U . . .
C56 C 0.268(2) 0.0185(12) 0.9182(8) 0.308(16) Uani 1 1 d G . . . .
H56 H 0.2832 -0.0423 0.9100 0.369 Uiso 1 1 calc R U . . .
C57 C 0.3638(13) 0.052(2) 0.9303(8) 0.33(3) Uani 1 1 d G . . . .
H57 H 0.4428 0.0134 0.9303 0.396 Uiso 1 1 calc R U . . .
C58 C 0.213(5) 0.288(2) 0.9469(17) 0.42(3) Uani 1 1 d . . . . .
H58A H 0.1356 0.3279 0.9279 0.623 Uiso 1 1 calc R U . . .
H58B H 0.2760 0.3110 0.9127 0.623 Uiso 1 1 calc R U . . .
H58C H 0.2213 0.2877 1.0035 0.623 Uiso 1 1 calc R U . . .
N1 N 0.2637(6) 0.5003(5) 0.3904(4) 0.0630(19) Uani 1 1 d . . . . .
O1 O 0.2435(5) 0.6505(4) 0.2593(3) 0.0672(16) Uani 1 1 d . . . . .
O2 O 0.2693(5) 0.3957(4) 0.2676(3) 0.0689(16) Uani 1 1 d . . . . .
O3 O 0.2345(6) 0.5583(4) 0.1461(3) 0.0828(19) Uani 1 1 d . . . . .
O4 O 0.4287(6) 0.4935(4) 0.2503(4) 0.0785(18) Uani 1 1 d . . . . .
Ti1 Ti 0.26849(15) 0.52441(11) 0.25052(9) 0.0663(6) Uani 1 1 d . . . . .
N2 N -0.0708(6) 0.4592(5) 0.7172(4) 0.0638(19) Uani 1 1 d . . . . .
C16 C -0.0180(8) 0.5196(6) 0.7214(5) 0.068(2) Uani 1 1 d . . . . .
H16 H 0.0649 0.5052 0.7091 0.081 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.318(8) . ?
C1 C2 1.399(10) . ?
C1 C6 1.400(10) . ?
C2 C3 1.359(10) . ?
C2 C17 1.511(10) . ?
C3 C4 1.387(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.349(10) . ?
C4 C21 1.506(11) . ?
C5 C6 1.379(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.406(10) . ?
C7 N1 1.268(9) . ?
C7 H7 0.9300 . ?
C8 N1 1.438(9) . ?
C8 C9 1.480(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C14 1.354(11) . ?
C9 C10 1.383(11) . ?
C10 C11 1.344(11) . ?
C10 H10 0.9300 . ?
C11 C12 1.354(12) . ?
C11 H11 0.9300 . ?
C12 C13 1.385(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.345(10) . ?
C13 C15 1.479(11) . ?
C14 H14 0.9300 . ?
C15 N2 1.487(10) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C17 C20 1.505(11) . ?
C17 C19 1.521(12) . ?
C17 C18 1.525(12) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C24 1.490(11) . ?
C21 C22 1.500(13) . ?
C21 C23 1.515(12) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 O2 1.303(9) . ?
C25 C26 1.381(10) . ?
C25 C30 1.407(11) . ?
C26 C27 1.355(11) . ?
C26 C31 1.526(11) . ?
C27 C28 1.398(11) . ?
C27 H27 0.9300 . ?
C28 C29 1.367(10) . ?
C28 C35 1.508(11) . ?
C29 C30 1.378(11) . ?
C29 H29 0.9300 . ?
C30 C16 1.439(10) 2_566 ?
C31 C34 1.523(11) . ?
C31 C32 1.533(12) . ?
C31 C33 1.540(11) . ?
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 1.484(12) . ?
C35 C38 1.507(12) . ?
C35 C37 1.529(12) . ?
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 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 O3 1.329(17) . ?
C39 C41 1.35(2) . ?
C39 C40 1.425(18) . ?
C39 H39 0.9800 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 O4 1.357(13) . ?
C42 C43 1.397(12) . ?
C42 C44 1.451(14) . ?
C42 H42 0.9800 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 C51 1.280(15) . ?
C45 C46 1.3900 . ?
C45 C50 1.3900 . ?
C46 C47 1.3900 . ?
C46 H46 0.9300 . ?
C47 C48 1.3900 . ?
C47 H47 0.9300 . ?
C48 C49 1.3900 . ?
C48 H48 0.9300 . ?
C49 C50 1.3900 . ?
C49 H49 0.9300 . ?
C50 H50 0.9300 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 C53 1.3900 . ?
C52 C57 1.3900 . ?
C52 H52 0.9300 . ?
C53 C58 1.31(3) . ?
C53 C54 1.3900 . ?
C54 C55 1.3900 . ?
C54 H54 0.9300 . ?
C55 C56 1.3900 . ?
C55 H55 0.9300 . ?
C56 C57 1.3900 . ?
C56 H56 0.9300 . ?
C57 H57 0.9300 . ?
C58 H58A 0.9600 . ?
C58 H58B 0.9600 . ?
C58 H58C 0.9600 . ?
N1 Ti1 2.264(7) . ?
O1 Ti1 1.887(6) . ?
O2 Ti1 1.887(6) . ?
O3 Ti1 1.736(6) . ?
O4 Ti1 1.771(7) . ?
Ti1 N2 2.242(8) 2_566 ?
N2 C16 1.253(10) . ?
N2 Ti1 2.242(8) 2_566 ?
C16 C30 1.439(10) 2_566 ?
C16 H16 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 119.7(7) . . ?
O1 C1 C6 120.0(7) . . ?
C2 C1 C6 120.3(7) . . ?
C3 C2 C1 116.0(7) . . ?
C3 C2 C17 122.6(8) . . ?
C1 C2 C17 121.4(7) . . ?
C2 C3 C4 126.8(8) . . ?
C2 C3 H3 116.6 . . ?
C4 C3 H3 116.6 . . ?
C5 C4 C3 114.2(7) . . ?
C5 C4 C21 124.3(8) . . ?
C3 C4 C21 121.3(8) . . ?
C4 C5 C6 124.5(7) . . ?
C4 C5 H5 117.8 . . ?
C6 C5 H5 117.8 . . ?
C5 C6 C1 118.1(8) . . ?
C5 C6 C7 120.3(8) . . ?
C1 C6 C7 121.6(7) . . ?
N1 C7 C6 128.0(7) . . ?
N1 C7 H7 116.0 . . ?
C6 C7 H7 116.0 . . ?
N1 C8 C9 119.4(7) . . ?
N1 C8 H8A 107.5 . . ?
C9 C8 H8A 107.5 . . ?
N1 C8 H8B 107.5 . . ?
C9 C8 H8B 107.5 . . ?
H8A C8 H8B 107.0 . . ?
C14 C9 C10 116.2(8) . . ?
C14 C9 C8 122.9(9) . . ?
C10 C9 C8 120.6(10) . . ?
C11 C10 C9 120.0(9) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C12 122.0(9) . . ?
C10 C11 H11 119.0 . . ?
C12 C11 H11 119.0 . . ?
C11 C12 C13 119.7(8) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 116.4(9) . . ?
C14 C13 C15 121.0(9) . . ?
C12 C13 C15 122.3(9) . . ?
C13 C14 C9 125.7(8) . . ?
C13 C14 H14 117.2 . . ?
C9 C14 H14 117.2 . . ?
C13 C15 N2 119.1(7) . . ?
C13 C15 H15A 107.5 . . ?
N2 C15 H15A 107.5 . . ?
C13 C15 H15B 107.5 . . ?
N2 C15 H15B 107.5 . . ?
H15A C15 H15B 107.0 . . ?
C20 C17 C2 111.8(7) . . ?
C20 C17 C19 108.8(8) . . ?
C2 C17 C19 109.3(7) . . ?
C20 C17 C18 107.8(7) . . ?
C2 C17 C18 109.4(7) . . ?
C19 C17 C18 109.6(8) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C24 C21 C22 107.2(9) . . ?
C24 C21 C4 112.6(7) . . ?
C22 C21 C4 109.7(9) . . ?
C24 C21 C23 106.7(9) . . ?
C22 C21 C23 110.6(9) . . ?
C4 C21 C23 109.8(7) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O2 C25 C26 121.6(9) . . ?
O2 C25 C30 118.4(7) . . ?
C26 C25 C30 120.0(8) . . ?
C27 C26 C25 118.9(8) . . ?
C27 C26 C31 120.1(8) . . ?
C25 C26 C31 121.0(8) . . ?
C26 C27 C28 123.2(8) . . ?
C26 C27 H27 118.4 . . ?
C28 C27 H27 118.4 . . ?
C29 C28 C27 116.6(8) . . ?
C29 C28 C35 124.5(9) . . ?
C27 C28 C35 118.9(8) . . ?
C28 C29 C30 122.8(9) . . ?
C28 C29 H29 118.6 . . ?
C30 C29 H29 118.6 . . ?
C29 C30 C25 118.4(8) . . ?
C29 C30 C16 118.2(8) . 2_566 ?
C25 C30 C16 123.4(8) . 2_566 ?
C34 C31 C26 112.9(8) . . ?
C34 C31 C32 106.6(8) . . ?
C26 C31 C32 111.1(7) . . ?
C34 C31 C33 106.6(7) . . ?
C26 C31 C33 110.9(7) . . ?
C32 C31 C33 108.4(8) . . ?
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 . . ?
C36 C35 C38 109.3(9) . . ?
C36 C35 C28 110.4(7) . . ?
C38 C35 C28 111.1(8) . . ?
C36 C35 C37 108.3(8) . . ?
C38 C35 C37 107.9(7) . . ?
C28 C35 C37 109.7(8) . . ?
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 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
O3 C39 C41 123.9(17) . . ?
O3 C39 C40 115.8(18) . . ?
C41 C39 C40 120.3(18) . . ?
O3 C39 H39 90.2 . . ?
C41 C39 H39 90.2 . . ?
C40 C39 H39 90.2 . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
O4 C42 C43 115.9(11) . . ?
O4 C42 C44 113.0(10) . . ?
C43 C42 C44 113.8(12) . . ?
O4 C42 H42 104.2 . . ?
C43 C42 H42 104.2 . . ?
C44 C42 H42 104.2 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C51 C45 C46 112.0(18) . . ?
C51 C45 C50 127.9(18) . . ?
C46 C45 C50 120.0 . . ?
C45 C46 C47 120.0 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 H46 120.0 . . ?
C48 C47 C46 120.0 . . ?
C48 C47 H47 120.0 . . ?
C46 C47 H47 120.0 . . ?
C49 C48 C47 120.0 . . ?
C49 C48 H48 120.0 . . ?
C47 C48 H48 120.0 . . ?
C48 C49 C50 120.0 . . ?
C48 C49 H49 120.0 . . ?
C50 C49 H49 120.0 . . ?
C49 C50 C45 120.0 . . ?
C49 C50 H50 120.0 . . ?
C45 C50 H50 120.0 . . ?
C45 C51 H51A 109.5 . . ?
C45 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C45 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C53 C52 C57 120.0 . . ?
C53 C52 H52 120.0 . . ?
C57 C52 H52 120.0 . . ?
C58 C53 C54 125(3) . . ?
C58 C53 C52 115(3) . . ?
C54 C53 C52 120.0 . . ?
C53 C54 C55 120.0 . . ?
C53 C54 H54 120.0 . . ?
C55 C54 H54 120.0 . . ?
C56 C55 C54 120.0 . . ?
C56 C55 H55 120.0 . . ?
C54 C55 H55 120.0 . . ?
C55 C56 C57 120.0 . . ?
C55 C56 H56 120.0 . . ?
C57 C56 H56 120.0 . . ?
C56 C57 C52 120.0 . . ?
C56 C57 H57 120.0 . . ?
C52 C57 H57 120.0 . . ?
C53 C58 H58A 109.5 . . ?
C53 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C53 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C7 N1 C8 118.9(7) . . ?
C7 N1 Ti1 125.4(5) . . ?
C8 N1 Ti1 115.7(5) . . ?
C1 O1 Ti1 140.3(5) . . ?
C25 O2 Ti1 136.0(5) . . ?
C39 O3 Ti1 158.1(10) . . ?
C42 O4 Ti1 149.9(7) . . ?
O3 Ti1 O4 104.4(3) . . ?
O3 Ti1 O2 96.0(2) . . ?
O4 Ti1 O2 91.4(3) . . ?
O3 Ti1 O1 94.3(2) . . ?
O4 Ti1 O1 96.3(3) . . ?
O2 Ti1 O1 165.2(2) . . ?
O3 Ti1 N2 88.7(3) . 2_566 ?
O4 Ti1 N2 165.9(3) . 2_566 ?
O2 Ti1 N2 82.0(3) . 2_566 ?
O1 Ti1 N2 87.6(3) . 2_566 ?
O3 Ti1 N1 165.6(3) . . ?
O4 Ti1 N1 89.2(3) . . ?
O2 Ti1 N1 87.9(2) . . ?
O1 Ti1 N1 79.6(2) . . ?
N2 Ti1 N1 78.1(2) 2_566 . ?
C16 N2 C15 118.0(7) . . ?
C16 N2 Ti1 122.7(6) . 2_566 ?
C15 N2 Ti1 119.1(5) . 2_566 ?
N2 C16 C30 127.2(9) . 2_566 ?
N2 C16 H16 116.4 . . ?
C30 C16 H16 116.4 2_566 . ?

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
O1 C1 C2 C3 174.6(7) . . . . ?
C6 C1 C2 C3 -4.1(11) . . . . ?
O1 C1 C2 C17 -5.8(12) . . . . ?
C6 C1 C2 C17 175.6(7) . . . . ?
C1 C2 C3 C4 1.2(12) . . . . ?
C17 C2 C3 C4 -178.4(8) . . . . ?
C2 C3 C4 C5 1.6(13) . . . . ?
C2 C3 C4 C21 -174.7(9) . . . . ?
C3 C4 C5 C6 -1.6(12) . . . . ?
C21 C4 C5 C6 174.5(9) . . . . ?
C4 C5 C6 C1 -1.1(13) . . . . ?
C4 C5 C6 C7 -179.6(8) . . . . ?
O1 C1 C6 C5 -174.6(8) . . . . ?
C2 C1 C6 C5 4.0(12) . . . . ?
O1 C1 C6 C7 3.9(12) . . . . ?
C2 C1 C6 C7 -177.4(8) . . . . ?
C5 C6 C7 N1 -175.2(8) . . . . ?
C1 C6 C7 N1 6.4(14) . . . . ?
N1 C8 C9 C14 95.2(10) . . . . ?
N1 C8 C9 C10 -90.6(10) . . . . ?
C14 C9 C10 C11 0.9(11) . . . . ?
C8 C9 C10 C11 -173.6(7) . . . . ?
C9 C10 C11 C12 -0.1(13) . . . . ?
C10 C11 C12 C13 -1.3(13) . . . . ?
C11 C12 C13 C14 1.8(11) . . . . ?
C11 C12 C13 C15 175.2(7) . . . . ?
C12 C13 C14 C9 -1.0(11) . . . . ?
C15 C13 C14 C9 -174.5(7) . . . . ?
C10 C9 C14 C13 -0.3(11) . . . . ?
C8 C9 C14 C13 174.1(7) . . . . ?
C14 C13 C15 N2 -89.6(9) . . . . ?
C12 C13 C15 N2 97.3(9) . . . . ?
C3 C2 C17 C20 2.4(12) . . . . ?
C1 C2 C17 C20 -177.1(8) . . . . ?
C3 C2 C17 C19 123.0(9) . . . . ?
C1 C2 C17 C19 -56.6(11) . . . . ?
C3 C2 C17 C18 -116.9(9) . . . . ?
C1 C2 C17 C18 63.5(10) . . . . ?
C5 C4 C21 C24 7.4(13) . . . . ?
C3 C4 C21 C24 -176.8(9) . . . . ?
C5 C4 C21 C22 126.8(10) . . . . ?
C3 C4 C21 C22 -57.4(12) . . . . ?
C5 C4 C21 C23 -111.4(10) . . . . ?
C3 C4 C21 C23 64.4(12) . . . . ?
O2 C25 C26 C27 178.0(7) . . . . ?
C30 C25 C26 C27 -0.7(12) . . . . ?
O2 C25 C26 C31 -3.0(12) . . . . ?
C30 C25 C26 C31 178.3(7) . . . . ?
C25 C26 C27 C28 -0.4(12) . . . . ?
C31 C26 C27 C28 -179.4(7) . . . . ?
C26 C27 C28 C29 0.0(12) . . . . ?
C26 C27 C28 C35 -176.8(8) . . . . ?
C27 C28 C29 C30 1.7(12) . . . . ?
C35 C28 C29 C30 178.3(8) . . . . ?
C28 C29 C30 C25 -2.8(12) . . . . ?
C28 C29 C30 C16 -179.6(7) . . . 2_566 ?
O2 C25 C30 C29 -176.5(7) . . . . ?
C26 C25 C30 C29 2.3(11) . . . . ?
O2 C25 C30 C16 0.1(12) . . . 2_566 ?
C26 C25 C30 C16 178.9(7) . . . 2_566 ?
C27 C26 C31 C34 -1.1(11) . . . . ?
C25 C26 C31 C34 179.9(8) . . . . ?
C27 C26 C31 C32 118.6(9) . . . . ?
C25 C26 C31 C32 -60.4(10) . . . . ?
C27 C26 C31 C33 -120.7(9) . . . . ?
C25 C26 C31 C33 60.3(11) . . . . ?
C29 C28 C35 C36 -113.6(9) . . . . ?
C27 C28 C35 C36 62.9(10) . . . . ?
C29 C28 C35 C38 7.8(12) . . . . ?
C27 C28 C35 C38 -175.7(8) . . . . ?
C29 C28 C35 C37 127.1(9) . . . . ?
C27 C28 C35 C37 -56.4(10) . . . . ?
C51 C45 C46 C47 -176.8(12) . . . . ?
C50 C45 C46 C47 0.0 . . . . ?
C45 C46 C47 C48 0.0 . . . . ?
C46 C47 C48 C49 0.0 . . . . ?
C47 C48 C49 C50 0.0 . . . . ?
C48 C49 C50 C45 0.0 . . . . ?
C51 C45 C50 C49 176.3(14) . . . . ?
C46 C45 C50 C49 0.0 . . . . ?
C57 C52 C53 C58 -174(2) . . . . ?
C57 C52 C53 C54 0.0 . . . . ?
C58 C53 C54 C55 174(2) . . . . ?
C52 C53 C54 C55 0.0 . . . . ?
C53 C54 C55 C56 0.0 . . . . ?
C54 C55 C56 C57 0.0 . . . . ?
C55 C56 C57 C52 0.0 . . . . ?
C53 C52 C57 C56 0.0 . . . . ?
C6 C7 N1 C8 179.7(8) . . . . ?
C6 C7 N1 Ti1 1.0(13) . . . . ?
C9 C8 N1 C7 4.6(13) . . . . ?
C9 C8 N1 Ti1 -176.6(7) . . . . ?
C2 C1 O1 Ti1 152.3(6) . . . . ?
C6 C1 O1 Ti1 -29.1(13) . . . . ?
C26 C25 O2 Ti1 146.2(6) . . . . ?
C30 C25 O2 Ti1 -35.1(11) . . . . ?
C41 C39 O3 Ti1 -67(4) . . . . ?
C40 C39 O3 Ti1 113(3) . . . . ?
C43 C42 O4 Ti1 105.2(14) . . . . ?
C44 C42 O4 Ti1 -121.0(13) . . . . ?
C39 O3 Ti1 O4 28(3) . . . . ?
C39 O3 Ti1 O2 -65(3) . . . . ?
C39 O3 Ti1 O1 125(3) . . . . ?
C39 O3 Ti1 N2 -147(3) . . . 2_566 ?
C39 O3 Ti1 N1 -171(2) . . . . ?
C42 O4 Ti1 O3 109.0(13) . . . . ?
C42 O4 Ti1 O2 -154.4(13) . . . . ?
C42 O4 Ti1 O1 12.9(13) . . . . ?
C42 O4 Ti1 N2 -92.8(17) . . . 2_566 ?
C42 O4 Ti1 N1 -66.6(13) . . . . ?
C25 O2 Ti1 O3 -49.4(8) . . . . ?
C25 O2 Ti1 O4 -154.1(7) . . . . ?
C25 O2 Ti1 O1 84.5(12) . . . . ?
C25 O2 Ti1 N2 38.4(7) . . . 2_566 ?
C25 O2 Ti1 N1 116.7(7) . . . . ?
C1 O1 Ti1 O3 -164.9(8) . . . . ?
C1 O1 Ti1 O4 -59.9(8) . . . . ?
C1 O1 Ti1 O2 61.0(15) . . . . ?
C1 O1 Ti1 N2 106.5(8) . . . 2_566 ?
C1 O1 Ti1 N1 28.2(8) . . . . ?
C13 C15 N2 C16 -18.5(12) . . . . ?
C13 C15 N2 Ti1 165.7(6) . . . 2_566 ?
C15 N2 C16 C30 -178.3(7) . . . 2_566 ?
Ti1 N2 C16 C30 -2.7(12) 2_566 . . 2_566 ?

_refine_diff_density_max         0.497
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.100

####################################################################### 
# 
# 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_5a
_database_code_depnum_ccdc_archive 'CCDC 1018938'
_audit_update_record             
;
2015-04-28 deposited with the CCDC.
2015-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H96 N4 O8 Zr2'
_chemical_formula_sum            'C72 H96 N4 O8 Zr2'
_chemical_formula_weight         1327.96

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0938(12)
_cell_length_b                   14.2299(19)
_cell_length_c                   14.4174(19)
_cell_angle_alpha                68.240(6)
_cell_angle_beta                 88.659(6)
_cell_angle_gamma                82.273(6)
_cell_volume                     2093.8(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6594
_cell_measurement_theta_min      0.00
_cell_measurement_theta_max      0.00

_exptl_crystal_description       Block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_F_000             700
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.295
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24214
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.555
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_point_group_measured_fraction_full 0.979
_reflns_number_total             7194
_reflns_number_gt                4674
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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


The solvent accessible cavity associated with a toluene molecule
(estimated volume 389 Å³) contains disordered toulene molecule,
for which no reasonable model could be developed. Therefore, the observed
structure  was modified by PLATON SQUEEZE(Spek, 2009) to eliminate
the diffuse electron density (100 electrons) found in the cavity.



;

_computing_data_collection       'Bruker APEXII'
_computing_cell_refinement       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0836P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7194
_refine_ls_number_parameters     398
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1415
_refine_ls_wR_factor_gt          0.1297
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6344(2) 0.6121(2) 0.1712(2) 0.0542(7) Uani 1 1 d . . . . .
C2 C 0.5932(3) 0.6993(3) 0.1933(2) 0.0610(8) Uani 1 1 d . . . . .
C3 C 0.5512(3) 0.7869(3) 0.1128(3) 0.0778(10) Uani 1 1 d . . . . .
H3 H 0.5230 0.8452 0.1259 0.093 Uiso 1 1 calc R U . . .
C4 C 0.5477(3) 0.7947(3) 0.0144(3) 0.0821(10) Uani 1 1 d . . . . .
C5 C 0.5893(3) 0.7088(3) -0.0045(3) 0.0736(9) Uani 1 1 d . . . . .
H5 H 0.5900 0.7120 -0.0701 0.088 Uiso 1 1 calc R U . . .
C6 C 0.6310(3) 0.6159(2) 0.0732(2) 0.0597(8) Uani 1 1 d . . . . .
C7 C 0.6672(3) 0.5294(3) 0.0454(3) 0.0667(9) Uani 1 1 d . . . . .
H7 H 0.6640 0.5423 -0.0227 0.080 Uiso 1 1 calc R U . . .
C8 C 0.7351(4) 0.3606(3) 0.0549(3) 0.0864(11) Uani 1 1 d . . . . .
H8A H 0.6652 0.3253 0.0582 0.104 Uiso 1 1 calc R U . . .
H8B H 0.8007 0.3104 0.0942 0.104 Uiso 1 1 calc R U . . .
C9 C 0.7729(3) 0.4008(2) -0.0512(3) 0.0632(8) Uani 1 1 d . . . . .
C10 C 0.6952(3) 0.4124(3) -0.1288(3) 0.0868(12) Uani 1 1 d . . . . .
H10 H 0.6169 0.3954 -0.1154 0.104 Uiso 1 1 calc R U . . .
C11 C 0.7319(4) 0.4488(4) -0.2255(3) 0.1036(14) Uani 1 1 d . . . . .
H11 H 0.6776 0.4582 -0.2773 0.124 Uiso 1 1 calc R U . . .
C12 C 0.8474(4) 0.4716(3) -0.2465(3) 0.0902(12) Uani 1 1 d . . . . .
H12 H 0.8718 0.4953 -0.3125 0.108 Uiso 1 1 calc R U . . .
C13 C 0.9282(3) 0.4597(2) -0.1706(3) 0.0649(9) Uani 1 1 d . . . . .
C14 C 0.8903(3) 0.4248(2) -0.0750(3) 0.0603(8) Uani 1 1 d . . . . .
H14 H 0.9446 0.4168 -0.0236 0.072 Uiso 1 1 calc R U . . .
C15 C 0.5951(3) 0.6976(3) 0.3002(3) 0.0718(9) Uani 1 1 d . . . . .
C16 C 0.7269(3) 0.6675(4) 0.3443(3) 0.0990(13) Uani 1 1 d . . . . .
H16A H 0.7773 0.7160 0.3035 0.149 Uiso 1 1 calc R U . . .
H16B H 0.7580 0.6007 0.3456 0.149 Uiso 1 1 calc R U . . .
H16C H 0.7272 0.6672 0.4110 0.149 Uiso 1 1 calc R U . . .
C17 C 0.5154(4) 0.6207(3) 0.3657(3) 0.0974(13) Uani 1 1 d . . . . .
H17A H 0.5072 0.6271 0.4296 0.146 Uiso 1 1 calc R U . . .
H17B H 0.5522 0.5527 0.3746 0.146 Uiso 1 1 calc R U . . .
H17C H 0.4364 0.6337 0.3340 0.146 Uiso 1 1 calc R U . . .
C18 C 0.5470(5) 0.8005(3) 0.3052(3) 0.1114(15) Uani 1 1 d . . . . .
H18A H 0.4643 0.8201 0.2801 0.167 Uiso 1 1 calc R U . . .
H18B H 0.5960 0.8507 0.2653 0.167 Uiso 1 1 calc R U . . .
H18C H 0.5502 0.7959 0.3732 0.167 Uiso 1 1 calc R U . . .
C19 C 0.5018(5) 0.8945(4) -0.0681(3) 0.1252(17) Uani 1 1 d . . . . .
H19A H 0.4274 0.9242 -0.0487 0.188 Uiso 1 1 calc R U . . .
H19B H 0.4872 0.8825 -0.1279 0.188 Uiso 1 1 calc R U . . .
H19C H 0.5615 0.9403 -0.0802 0.188 Uiso 1 1 calc R U . . .
C20 C 1.0157(3) 0.3412(3) 0.2252(3) 0.0731(9) Uani 1 1 d . . . . .
H20 H 1.0878 0.3669 0.2012 0.088 Uiso 1 1 calc R U . . .
C21 C 1.0195(3) 0.2331(3) 0.2555(3) 0.0680(9) Uani 1 1 d . . . . .
C22 C 0.9165(3) 0.1830(2) 0.2854(2) 0.0637(8) Uani 1 1 d . . . . .
C23 C 0.9289(3) 0.0763(3) 0.3202(2) 0.0703(9) Uani 1 1 d . . . . .
C24 C 1.0446(4) 0.0261(3) 0.3180(3) 0.0887(11) Uani 1 1 d . . . . .
H24 H 1.0540 -0.0448 0.3398 0.106 Uiso 1 1 calc R U . . .
C25 C 1.1470(4) 0.0741(3) 0.2856(3) 0.0889(11) Uani 1 1 d . . . . .
C26 C 1.1340(3) 0.1769(3) 0.2559(3) 0.0827(11) Uani 1 1 d . . . . .
H26 H 1.2016 0.2109 0.2354 0.099 Uiso 1 1 calc R U . . .
C27 C 0.8200(4) 0.0193(3) 0.3575(3) 0.0842(11) Uani 1 1 d . . . . .
C28 C 0.7623(4) 0.0479(3) 0.4428(3) 0.1068(14) Uani 1 1 d . . . . .
H28A H 0.8222 0.0326 0.4951 0.160 Uiso 1 1 calc R U . . .
H28B H 0.6961 0.0094 0.4685 0.160 Uiso 1 1 calc R U . . .
H28C H 0.7324 0.1195 0.4181 0.160 Uiso 1 1 calc R U . . .
C29 C 0.7244(4) 0.0466(4) 0.2725(4) 0.1140(15) Uani 1 1 d . . . . .
H29A H 0.7052 0.1195 0.2419 0.171 Uiso 1 1 calc R U . . .
H29B H 0.6520 0.0174 0.2992 0.171 Uiso 1 1 calc R U . . .
H29C H 0.7564 0.0199 0.2235 0.171 Uiso 1 1 calc R U . . .
C30 C 0.8552(5) -0.0972(3) 0.3995(4) 0.1282(17) Uani 1 1 d . . . . .
H30A H 0.8908 -0.1185 0.3480 0.192 Uiso 1 1 calc R U . . .
H30B H 0.7839 -0.1296 0.4227 0.192 Uiso 1 1 calc R U . . .
H30C H 0.9130 -0.1163 0.4540 0.192 Uiso 1 1 calc R U . . .
C31 C 1.2710(4) 0.0124(4) 0.2853(4) 0.1336(19) Uani 1 1 d . . . . .
H31A H 1.2763 -0.0040 0.2263 0.200 Uiso 1 1 calc R U . . .
H31B H 1.2802 -0.0495 0.3434 0.200 Uiso 1 1 calc R U . . .
H31C H 1.3344 0.0520 0.2859 0.200 Uiso 1 1 calc R U . . .
C32 C 0.9438(3) 0.5158(3) 0.1940(3) 0.0877(12) Uani 1 1 d . . . . .
H32A H 0.9148 0.5407 0.2458 0.105 Uiso 1 1 calc R U . . .
H32B H 0.8927 0.5539 0.1348 0.105 Uiso 1 1 calc R U . . .
C34 C 0.4574(4) 0.2873(4) 0.2993(4) 0.1246(17) Uani 1 1 d . . . . .
H34A H 0.3946 0.3371 0.2557 0.150 Uiso 1 1 calc R U . . .
H34B H 0.4722 0.2304 0.2771 0.150 Uiso 1 1 calc R U . . .
C35 C 0.4177(7) 0.2540(8) 0.3933(5) 0.230(4) Uani 1 1 d . . . . .
H35A H 0.4792 0.2039 0.4367 0.346 Uiso 1 1 calc R U . . .
H35B H 0.3448 0.2238 0.3954 0.346 Uiso 1 1 calc R U . . .
H35C H 0.4008 0.3104 0.4151 0.346 Uiso 1 1 calc R U . . .
C36 C 0.8219(7) 0.3271(7) 0.5107(6) 0.195(4) Uani 1 1 d . . . . .
H36A H 0.7613 0.3510 0.5493 0.235 Uiso 1 1 calc R U . . .
H36B H 0.8384 0.2534 0.5424 0.235 Uiso 1 1 calc R U . . .
C37 C 0.9240(9) 0.3665(6) 0.5131(6) 0.232(4) Uani 1 1 d . . . . .
H37A H 0.9862 0.3402 0.4782 0.348 Uiso 1 1 calc R U . . .
H37B H 0.9505 0.3479 0.5812 0.348 Uiso 1 1 calc R U . . .
H37C H 0.9089 0.4395 0.4816 0.348 Uiso 1 1 calc R U . . .
N1 N 0.7035(2) 0.4367(2) 0.1023(2) 0.0654(7) Uani 1 1 d . . . . .
N2 N 0.9257(2) 0.4074(2) 0.2268(2) 0.0693(7) Uani 1 1 d . . . . .
O1 O 0.80813(19) 0.23688(17) 0.27991(18) 0.0755(6) Uani 1 1 d . . . . .
O2 O 0.7743(2) 0.3522(2) 0.4152(2) 0.0945(8) Uani 1 1 d . . . . .
O3 O 0.5644(2) 0.33179(19) 0.2912(2) 0.0885(7) Uani 1 1 d . . . . .
O4 O 0.67539(18) 0.52505(16) 0.24375(16) 0.0632(5) Uani 1 1 d . . . . .
Zr1 Zr 0.72430(3) 0.37236(2) 0.28155(2) 0.06692(17) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O4 1.321(3) . ?
C1 C6 1.396(4) . ?
C1 C2 1.408(4) . ?
C2 C3 1.384(5) . ?
C2 C15 1.533(5) . ?
C3 C4 1.383(5) . ?
C3 H3 0.9300 . ?
C4 C5 1.367(5) . ?
C4 C19 1.508(5) . ?
C5 C6 1.406(5) . ?
C5 H5 0.9300 . ?
C6 C7 1.435(4) . ?
C7 N1 1.283(4) . ?
C7 H7 0.9300 . ?
C8 N1 1.483(4) . ?
C8 C9 1.493(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.375(5) . ?
C9 C14 1.393(4) . ?
C10 C11 1.368(5) . ?
C10 H10 0.9300 . ?
C11 C12 1.364(5) . ?
C11 H11 0.9300 . ?
C12 C13 1.377(5) . ?
C12 H12 0.9300 . ?
C13 C14 1.358(5) . ?
C13 C32 1.508(4) 2_765 ?
C14 H14 0.9300 . ?
C15 C18 1.516(5) . ?
C15 C17 1.526(5) . ?
C15 C16 1.548(5) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N2 1.284(4) . ?
C20 C21 1.429(5) . ?
C20 H20 0.9300 . ?
C21 C22 1.404(4) . ?
C21 C26 1.406(5) . ?
C22 O1 1.323(4) . ?
C22 C23 1.398(4) . ?
C23 C24 1.388(5) . ?
C23 C27 1.523(5) . ?
C24 C25 1.387(5) . ?
C24 H24 0.9300 . ?
C25 C26 1.351(5) . ?
C25 C31 1.530(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.533(5) . ?
C27 C30 1.536(6) . ?
C27 C29 1.541(5) . ?
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 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 N2 1.477(4) . ?
C32 C13 1.508(4) 2_765 ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C34 C35 1.345(7) . ?
C34 O3 1.401(5) . ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 C37 1.336(9) . ?
C36 O2 1.386(7) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
N1 Zr1 2.406(3) . ?
N2 Zr1 2.406(2) . ?
O1 Zr1 2.033(2) . ?
O2 Zr1 1.924(3) . ?
O3 Zr1 1.924(2) . ?
O4 Zr1 2.033(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 C1 C6 119.2(3) . . ?
O4 C1 C2 120.1(3) . . ?
C6 C1 C2 120.7(3) . . ?
C3 C2 C1 116.2(3) . . ?
C3 C2 C15 121.8(3) . . ?
C1 C2 C15 122.1(3) . . ?
C4 C3 C2 125.1(3) . . ?
C4 C3 H3 117.4 . . ?
C2 C3 H3 117.4 . . ?
C5 C4 C3 117.2(3) . . ?
C5 C4 C19 121.9(4) . . ?
C3 C4 C19 120.9(4) . . ?
C4 C5 C6 121.4(3) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C1 C6 C5 119.4(3) . . ?
C1 C6 C7 123.9(3) . . ?
C5 C6 C7 116.7(3) . . ?
N1 C7 C6 128.4(3) . . ?
N1 C7 H7 115.8 . . ?
C6 C7 H7 115.8 . . ?
N1 C8 C9 116.6(3) . . ?
N1 C8 H8A 108.1 . . ?
C9 C8 H8A 108.1 . . ?
N1 C8 H8B 108.1 . . ?
C9 C8 H8B 108.1 . . ?
H8A C8 H8B 107.3 . . ?
C10 C9 C14 117.5(3) . . ?
C10 C9 C8 121.6(3) . . ?
C14 C9 C8 120.9(3) . . ?
C11 C10 C9 120.6(3) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C12 C11 C10 120.6(4) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 120.3(4) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C14 C13 C12 118.6(3) . . ?
C14 C13 C32 121.2(3) . 2_765 ?
C12 C13 C32 120.2(4) . 2_765 ?
C13 C14 C9 122.4(3) . . ?
C13 C14 H14 118.8 . . ?
C9 C14 H14 118.8 . . ?
C18 C15 C17 107.3(3) . . ?
C18 C15 C2 112.4(3) . . ?
C17 C15 C2 109.9(3) . . ?
C18 C15 C16 107.7(3) . . ?
C17 C15 C16 109.2(3) . . ?
C2 C15 C16 110.2(3) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C4 C19 H19A 109.5 . . ?
C4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N2 C20 C21 128.4(3) . . ?
N2 C20 H20 115.8 . . ?
C21 C20 H20 115.8 . . ?
C22 C21 C26 120.2(3) . . ?
C22 C21 C20 123.2(3) . . ?
C26 C21 C20 116.6(3) . . ?
O1 C22 C23 120.4(3) . . ?
O1 C22 C21 119.8(3) . . ?
C23 C22 C21 119.8(3) . . ?
C24 C23 C22 116.6(3) . . ?
C24 C23 C27 122.2(3) . . ?
C22 C23 C27 121.1(3) . . ?
C25 C24 C23 124.6(4) . . ?
C25 C24 H24 117.7 . . ?
C23 C24 H24 117.7 . . ?
C26 C25 C24 117.8(3) . . ?
C26 C25 C31 121.2(4) . . ?
C24 C25 C31 121.0(4) . . ?
C25 C26 C21 120.9(4) . . ?
C25 C26 H26 119.6 . . ?
C21 C26 H26 119.6 . . ?
C23 C27 C28 109.5(3) . . ?
C23 C27 C30 112.6(3) . . ?
C28 C27 C30 106.8(4) . . ?
C23 C27 C29 110.6(3) . . ?
C28 C27 C29 109.3(4) . . ?
C30 C27 C29 108.0(3) . . ?
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 . . ?
C25 C31 H31A 109.5 . . ?
C25 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C25 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N2 C32 C13 117.1(3) . 2_765 ?
N2 C32 H32A 108.0 . . ?
C13 C32 H32A 108.0 2_765 . ?
N2 C32 H32B 108.0 . . ?
C13 C32 H32B 108.0 2_765 . ?
H32A C32 H32B 107.3 . . ?
C35 C34 O3 112.4(5) . . ?
C35 C34 H34A 109.1 . . ?
O3 C34 H34A 109.1 . . ?
C35 C34 H34B 109.1 . . ?
O3 C34 H34B 109.1 . . ?
H34A C34 H34B 107.9 . . ?
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 . . ?
C37 C36 O2 113.9(7) . . ?
C37 C36 H36A 108.8 . . ?
O2 C36 H36A 108.8 . . ?
C37 C36 H36B 108.8 . . ?
O2 C36 H36B 108.8 . . ?
H36A C36 H36B 107.7 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C7 N1 C8 118.0(3) . . ?
C7 N1 Zr1 126.1(2) . . ?
C8 N1 Zr1 115.9(2) . . ?
C20 N2 C32 119.0(3) . . ?
C20 N2 Zr1 126.0(2) . . ?
C32 N2 Zr1 114.99(19) . . ?
C22 O1 Zr1 142.7(2) . . ?
C36 O2 Zr1 172.3(4) . . ?
C34 O3 Zr1 171.0(3) . . ?
C1 O4 Zr1 145.5(2) . . ?
O2 Zr1 O3 106.18(12) . . ?
O2 Zr1 O4 93.13(10) . . ?
O3 Zr1 O4 98.74(9) . . ?
O2 Zr1 O1 97.18(11) . . ?
O3 Zr1 O1 93.55(10) . . ?
O4 Zr1 O1 161.10(9) . . ?
O2 Zr1 N1 162.29(11) . . ?
O3 Zr1 N1 89.64(10) . . ?
O4 Zr1 N1 76.29(9) . . ?
O1 Zr1 N1 89.56(9) . . ?
O2 Zr1 N2 89.27(11) . . ?
O3 Zr1 N2 162.61(11) . . ?
O4 Zr1 N2 88.09(8) . . ?
O1 Zr1 N2 76.29(9) . . ?
N1 Zr1 N2 76.39(9) . . ?

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 C1 C2 C3 -179.6(3) . . . . ?
C6 C1 C2 C3 -0.5(4) . . . . ?
O4 C1 C2 C15 0.6(4) . . . . ?
C6 C1 C2 C15 179.7(3) . . . . ?
C1 C2 C3 C4 -0.5(5) . . . . ?
C15 C2 C3 C4 179.3(3) . . . . ?
C2 C3 C4 C5 -0.1(6) . . . . ?
C2 C3 C4 C19 -179.0(4) . . . . ?
C3 C4 C5 C6 1.6(5) . . . . ?
C19 C4 C5 C6 -179.5(4) . . . . ?
O4 C1 C6 C5 -178.9(3) . . . . ?
C2 C1 C6 C5 1.9(4) . . . . ?
O4 C1 C6 C7 1.5(4) . . . . ?
C2 C1 C6 C7 -177.7(3) . . . . ?
C4 C5 C6 C1 -2.5(5) . . . . ?
C4 C5 C6 C7 177.1(3) . . . . ?
C1 C6 C7 N1 2.6(5) . . . . ?
C5 C6 C7 N1 -177.0(3) . . . . ?
N1 C8 C9 C10 -103.0(4) . . . . ?
N1 C8 C9 C14 79.1(4) . . . . ?
C14 C9 C10 C11 -1.6(5) . . . . ?
C8 C9 C10 C11 -179.6(4) . . . . ?
C9 C10 C11 C12 1.8(7) . . . . ?
C10 C11 C12 C13 -1.0(6) . . . . ?
C11 C12 C13 C14 0.0(6) . . . . ?
C11 C12 C13 C32 179.6(4) . . . 2_765 ?
C12 C13 C14 C9 0.1(5) . . . . ?
C32 C13 C14 C9 -179.5(3) 2_765 . . . ?
C10 C9 C14 C13 0.7(5) . . . . ?
C8 C9 C14 C13 178.7(3) . . . . ?
C3 C2 C15 C18 -0.1(5) . . . . ?
C1 C2 C15 C18 179.7(3) . . . . ?
C3 C2 C15 C17 119.4(4) . . . . ?
C1 C2 C15 C17 -60.8(4) . . . . ?
C3 C2 C15 C16 -120.2(4) . . . . ?
C1 C2 C15 C16 59.6(4) . . . . ?
N2 C20 C21 C22 5.6(6) . . . . ?
N2 C20 C21 C26 -173.4(4) . . . . ?
C26 C21 C22 O1 -176.5(3) . . . . ?
C20 C21 C22 O1 4.5(5) . . . . ?
C26 C21 C22 C23 3.1(5) . . . . ?
C20 C21 C22 C23 -175.9(3) . . . . ?
O1 C22 C23 C24 176.3(3) . . . . ?
C21 C22 C23 C24 -3.2(5) . . . . ?
O1 C22 C23 C27 -3.2(5) . . . . ?
C21 C22 C23 C27 177.2(3) . . . . ?
C22 C23 C24 C25 1.0(6) . . . . ?
C27 C23 C24 C25 -179.4(4) . . . . ?
C23 C24 C25 C26 1.4(6) . . . . ?
C23 C24 C25 C31 -179.6(4) . . . . ?
C24 C25 C26 C21 -1.6(6) . . . . ?
C31 C25 C26 C21 179.4(4) . . . . ?
C22 C21 C26 C25 -0.5(6) . . . . ?
C20 C21 C26 C25 178.5(4) . . . . ?
C24 C23 C27 C28 123.4(4) . . . . ?
C22 C23 C27 C28 -57.1(4) . . . . ?
C24 C23 C27 C30 4.8(5) . . . . ?
C22 C23 C27 C30 -175.7(4) . . . . ?
C24 C23 C27 C29 -116.1(4) . . . . ?
C22 C23 C27 C29 63.4(5) . . . . ?
C6 C7 N1 C8 179.6(3) . . . . ?
C6 C7 N1 Zr1 0.0(5) . . . . ?
C9 C8 N1 C7 25.0(5) . . . . ?
C9 C8 N1 Zr1 -155.4(3) . . . . ?
C21 C20 N2 C32 178.4(3) . . . . ?
C21 C20 N2 Zr1 -0.7(6) . . . . ?
C13 C32 N2 C20 -6.3(5) 2_765 . . . ?
C13 C32 N2 Zr1 172.9(3) 2_765 . . . ?
C23 C22 O1 Zr1 154.1(3) . . . . ?
C21 C22 O1 Zr1 -26.4(5) . . . . ?
C6 C1 O4 Zr1 -11.6(5) . . . . ?
C2 C1 O4 Zr1 167.6(2) . . . . ?

_refine_diff_density_max         0.493
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.053



# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 389 100 ' '
2 0.490 -0.017 0.422 13 1 ' '
3 0.510 0.017 0.579 13 1 ' '
_platon_squeeze_details          
;
;




####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1018939'
_audit_update_record             
;
2015-04-28 deposited with the CCDC.
2015-04-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C138 H204 Hf3 N6 O12'
_chemical_formula_weight         2674.53

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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   19.1043(7)
_cell_length_b                   29.5065(11)
_cell_length_c                   30.3372(10)
_cell_angle_alpha                90
_cell_angle_beta                 97.805(2)
_cell_angle_gamma                90
_cell_volume                     16942.7(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6847
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      22.71

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_F_000             5544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.880
_shelx_estimated_absorpt_T_min   0.602
_shelx_estimated_absorpt_T_max   0.705
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6912
_exptl_absorpt_correction_T_max  0.7821
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       'ω and φ scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            116293
_diffrn_reflns_av_unetI/netI     0.1101
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         0.967
_diffrn_reflns_theta_max         27.917
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             35986
_reflns_number_gt                18642
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'APEXII (Bruker, 2008)'
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2008)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2013)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997) '
_computing_publication_material  'SHELXL-97 (Sheldrick, 2013)'

_refine_special_details          
;
 The solvent accessible cavity associated with a toluene molecule
(estimated volume 2068 Å³) contains disordered toulene molecule,
for which no reasonable model could be developed. Therefore, the observed
structure  was modified by PLATON SQUEEZE(Spek, 2009) to eliminate
the diffuse electron density (272 electrons) found in the cavity.  

;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0613P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         35986
_refine_ls_number_parameters     1544
_refine_ls_number_restraints     357
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1087
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_restrained_S_all      0.893
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 1.000 0.000 0.500 2068.2 272.0
2 0.463 0.104 0.297 11.1 0.8
3 0.854 0.208 0.756 7.1 -0.4
4 0.500 0.500 0.000 2067.8 270.5
5 0.354 0.292 0.256 7.1 -0.3
6 0.963 0.396 0.797 11.1 1.0
7 0.037 0.604 0.203 11.0 0.5
8 0.646 0.708 0.744 7.1 0.1
9 0.146 0.792 0.244 7.1 0.1
10 0.537 0.896 0.703 10.9 0.2
_platon_squeeze_details          
;
The solvent accessible cavity associated with toluene molecule
(estimated volume 2068 Å³) contains disordered toulene molecule,
for which no reasonable model could be developed. Therefore, the observed
structure  were modified by PLATON SQUEEZE(Spek, 2009) to eliminate
the diffuse electron density (272 electrons) found in the cavity.  

;

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7132(3) 0.14475(17) 0.76569(15) 0.0456(13) Uani 1 1 d . . . . .
H1 H 0.7435 0.1662 0.7562 0.055 Uiso 1 1 calc R U . . .
C2 C 0.7450(3) 0.10210(17) 0.78099(15) 0.0430(13) Uani 1 1 d . . . . .
C3 C 0.8180(3) 0.1001(2) 0.79056(18) 0.0589(15) Uani 1 1 d . . . . .
H3 H 0.8439 0.1262 0.7873 0.071 Uiso 1 1 calc R U . . .
C4 C 0.8539(3) 0.0610(2) 0.80472(18) 0.0634(17) Uani 1 1 d . . . . .
C5 C 0.8115(3) 0.0230(2) 0.80710(19) 0.0632(16) Uani 1 1 d . . . . .
H5 H 0.8344 -0.0039 0.8165 0.076 Uiso 1 1 calc R U . . .
C6 C 0.7404(3) 0.02112(18) 0.79715(18) 0.0573(15) Uani 1 1 d . . . . .
C7 C 0.7043(3) 0.06289(18) 0.78463(15) 0.0469(13) Uani 1 1 d . . . . .
C8 C 0.9337(4) 0.0588(3) 0.8175(2) 0.090(2) Uani 1 1 d D . . . .
C9 C 0.9692(8) 0.1036(4) 0.8089(5) 0.100(5) Uani 0.690(12) 1 d D U P A 1
H9A H 1.0192 0.1010 0.8179 0.151 Uiso 0.690(12) 1 calc R U P A 1
H9B H 0.9506 0.1272 0.8257 0.151 Uiso 0.690(12) 1 calc R U P A 1
H9C H 0.9602 0.1107 0.7778 0.151 Uiso 0.690(12) 1 calc R U P A 1
C10 C 0.9629(5) 0.0228(4) 0.7879(4) 0.120(5) Uani 0.690(12) 1 d D U P A 1
H10A H 1.0131 0.0204 0.7958 0.180 Uiso 0.690(12) 1 calc R U P A 1
H10B H 0.9524 0.0317 0.7572 0.180 Uiso 0.690(12) 1 calc R U P A 1
H10C H 0.9413 -0.0059 0.7921 0.180 Uiso 0.690(12) 1 calc R U P A 1
C11 C 0.9528(7) 0.0454(7) 0.8663(4) 0.141(6) Uani 0.690(12) 1 d D U P A 1
H11A H 1.0033 0.0441 0.8736 0.211 Uiso 0.690(12) 1 calc R U P A 1
H11B H 0.9331 0.0161 0.8711 0.211 Uiso 0.690(12) 1 calc R U P A 1
H11C H 0.9341 0.0674 0.8849 0.211 Uiso 0.690(12) 1 calc R U P A 1
C9' C 0.974(2) 0.0890(10) 0.7893(12) 0.118(11) Uani 0.310(12) 1 d D U P A 2
H9'1 H 1.0241 0.0861 0.7992 0.177 Uiso 0.310(12) 1 calc R U P A 2
H9'2 H 0.9602 0.1199 0.7922 0.177 Uiso 0.310(12) 1 calc R U P A 2
H9'3 H 0.9645 0.0799 0.7587 0.177 Uiso 0.310(12) 1 calc R U P A 2
C10' C 0.9554(16) 0.0121(6) 0.8361(13) 0.127(10) Uani 0.310(12) 1 d D U P A 2
H10D H 1.0057 0.0112 0.8445 0.190 Uiso 0.310(12) 1 calc R U P A 2
H10E H 0.9419 -0.0105 0.8137 0.190 Uiso 0.310(12) 1 calc R U P A 2
H10F H 0.9323 0.0060 0.8616 0.190 Uiso 0.310(12) 1 calc R U P A 2
C11' C 0.9456(14) 0.0853(11) 0.8618(7) 0.133(10) Uani 0.310(12) 1 d D U P A 2
H11D H 0.9950 0.0850 0.8733 0.199 Uiso 0.310(12) 1 calc R U P A 2
H11E H 0.9192 0.0713 0.8829 0.199 Uiso 0.310(12) 1 calc R U P A 2
H11F H 0.9300 0.1160 0.8567 0.199 Uiso 0.310(12) 1 calc R U P A 2
C12 C 0.6966(3) -0.0222(2) 0.8004(2) 0.0725(18) Uani 1 1 d . . . . .
C13 C 0.7467(4) -0.0640(2) 0.8123(3) 0.115(3) Uani 1 1 d . . . . .
H13A H 0.7187 -0.0909 0.8140 0.172 Uiso 1 1 calc R U . . .
H13B H 0.7751 -0.0589 0.8405 0.172 Uiso 1 1 calc R U . . .
H13C H 0.7769 -0.0679 0.7898 0.172 Uiso 1 1 calc R U . . .
C14 C 0.6512(4) -0.0188(2) 0.8378(2) 0.097(2) Uani 1 1 d . . . . .
H14A H 0.6243 -0.0461 0.8390 0.145 Uiso 1 1 calc R U . . .
H14B H 0.6196 0.0065 0.8325 0.145 Uiso 1 1 calc R U . . .
H14C H 0.6811 -0.0146 0.8656 0.145 Uiso 1 1 calc R U . . .
C15 C 0.6519(4) -0.0328(2) 0.7558(3) 0.101(2) Uani 1 1 d . . . . .
H15A H 0.6252 -0.0600 0.7586 0.152 Uiso 1 1 calc R U . . .
H15B H 0.6823 -0.0371 0.7334 0.152 Uiso 1 1 calc R U . . .
H15C H 0.6202 -0.0081 0.7475 0.152 Uiso 1 1 calc R U . . .
C16 C 0.6450(3) 0.1268(2) 0.89639(18) 0.0667(17) Uani 1 1 d . . . . .
C17 C 0.7146(5) 0.1015(3) 0.9018(3) 0.145(4) Uani 1 1 d . . . . .
H17A H 0.7443 0.1135 0.8815 0.218 Uiso 1 1 calc R U . . .
H17B H 0.7060 0.0699 0.8956 0.218 Uiso 1 1 calc R U . . .
H17C H 0.7377 0.1050 0.9318 0.218 Uiso 1 1 calc R U . . .
C18 C 0.5957(6) 0.1094(4) 0.9268(3) 0.186(5) Uani 1 1 d . . . . .
H18A H 0.5526 0.1265 0.9225 0.279 Uiso 1 1 calc R U . . .
H18B H 0.6173 0.1124 0.9571 0.279 Uiso 1 1 calc R U . . .
H18C H 0.5854 0.0780 0.9204 0.279 Uiso 1 1 calc R U . . .
C19 C 0.6562(5) 0.1773(3) 0.9061(3) 0.148(4) Uani 1 1 d . . . . .
H19A H 0.6116 0.1927 0.9012 0.222 Uiso 1 1 calc R U . . .
H19B H 0.6872 0.1896 0.8868 0.222 Uiso 1 1 calc R U . . .
H19C H 0.6769 0.1812 0.9365 0.222 Uiso 1 1 calc R U . . .
C20 C 0.4320(3) 0.0447(3) 0.8105(2) 0.090(2) Uani 1 1 d D . . . .
C21 C 0.4401(10) -0.0048(4) 0.7956(8) 0.154(7) Uani 0.568(10) 1 d D U P B 1
H21A H 0.4874 -0.0150 0.8056 0.231 Uiso 0.568(10) 1 calc R U P B 1
H21B H 0.4311 -0.0065 0.7638 0.231 Uiso 0.568(10) 1 calc R U P B 1
H21C H 0.4071 -0.0236 0.8083 0.231 Uiso 0.568(10) 1 calc R U P B 1
C22 C 0.4317(10) 0.0412(8) 0.8609(3) 0.131(6) Uani 0.568(10) 1 d D U P B 1
H22A H 0.4690 0.0214 0.8734 0.196 Uiso 0.568(10) 1 calc R U P B 1
H22B H 0.3871 0.0293 0.8668 0.196 Uiso 0.568(10) 1 calc R U P B 1
H22C H 0.4387 0.0707 0.8740 0.196 Uiso 0.568(10) 1 calc R U P B 1
C23 C 0.3682(6) 0.0709(6) 0.7897(8) 0.143(7) Uani 0.568(10) 1 d D U P B 1
H23A H 0.3691 0.0734 0.7582 0.215 Uiso 0.568(10) 1 calc R U P B 1
H23B H 0.3688 0.1006 0.8025 0.215 Uiso 0.568(10) 1 calc R U P B 1
H23C H 0.3260 0.0553 0.7950 0.215 Uiso 0.568(10) 1 calc R U P B 1
C21' C 0.3915(12) 0.0340(9) 0.7652(5) 0.135(8) Uani 0.432(10) 1 d D U P B 2
H21D H 0.3899 0.0605 0.7466 0.203 Uiso 0.432(10) 1 calc R U P B 2
H21E H 0.3442 0.0249 0.7685 0.203 Uiso 0.432(10) 1 calc R U P B 2
H21F H 0.4147 0.0099 0.7516 0.203 Uiso 0.432(10) 1 calc R U P B 2
C22' C 0.3858(11) 0.0764(7) 0.8342(10) 0.134(8) Uani 0.432(10) 1 d D U P B 2
H22D H 0.4077 0.0814 0.8642 0.202 Uiso 0.432(10) 1 calc R U P B 2
H22E H 0.3401 0.0628 0.8345 0.202 Uiso 0.432(10) 1 calc R U P B 2
H22F H 0.3805 0.1048 0.8187 0.202 Uiso 0.432(10) 1 calc R U P B 2
C23' C 0.4513(13) 0.0068(8) 0.8443(9) 0.150(9) Uani 0.432(10) 1 d D U P B 2
H23D H 0.4861 0.0176 0.8677 0.224 Uiso 0.432(10) 1 calc R U P B 2
H23E H 0.4702 -0.0185 0.8297 0.224 Uiso 0.432(10) 1 calc R U P B 2
H23F H 0.4099 -0.0026 0.8565 0.224 Uiso 0.432(10) 1 calc R U P B 2
C24 C 0.4540(3) 0.19119(18) 0.76723(15) 0.0438(13) Uani 1 1 d . . . . .
C25 C 0.4202(3) 0.2284(2) 0.78469(16) 0.0541(15) Uani 1 1 d . . . . .
C26 C 0.3663(3) 0.2508(2) 0.7576(2) 0.0686(17) Uani 1 1 d . . . . .
H26 H 0.3435 0.2748 0.7696 0.082 Uiso 1 1 calc R U . . .
C27 C 0.3448(3) 0.2389(2) 0.71314(19) 0.0630(16) Uani 1 1 d . . . . .
C28 C 0.3759(3) 0.2024(2) 0.69694(17) 0.0585(15) Uani 1 1 d . . . . .
H28 H 0.3610 0.1929 0.6680 0.070 Uiso 1 1 calc R U . . .
C29 C 0.4309(3) 0.1783(2) 0.72322(16) 0.0539(14) Uani 1 1 d . . . . .
C30 C 0.4605(3) 0.13995(19) 0.70271(16) 0.0538(15) Uani 1 1 d . . . . .
H30 H 0.4404 0.1337 0.6737 0.065 Uiso 1 1 calc R U . . .
C31 C 0.4413(3) 0.2431(2) 0.83333(19) 0.0750(19) Uani 1 1 d . . . . .
C32 C 0.5173(4) 0.2585(2) 0.8403(2) 0.092(2) Uani 1 1 d . . . . .
H32A H 0.5302 0.2674 0.8708 0.138 Uiso 1 1 calc R U . . .
H32B H 0.5229 0.2838 0.8213 0.138 Uiso 1 1 calc R U . . .
H32C H 0.5473 0.2341 0.8334 0.138 Uiso 1 1 calc R U . . .
C33 C 0.4311(4) 0.2038(2) 0.8650(2) 0.094(2) Uani 1 1 d . . . . .
H33A H 0.4454 0.2133 0.8951 0.142 Uiso 1 1 calc R U . . .
H33B H 0.4594 0.1785 0.8583 0.142 Uiso 1 1 calc R U . . .
H33C H 0.3823 0.1951 0.8613 0.142 Uiso 1 1 calc R U . . .
C34 C 0.3961(5) 0.2826(3) 0.8468(2) 0.128(4) Uani 1 1 d . . . . .
H34A H 0.4117 0.2908 0.8772 0.192 Uiso 1 1 calc R U . . .
H34B H 0.3474 0.2735 0.8438 0.192 Uiso 1 1 calc R U . . .
H34C H 0.4009 0.3082 0.8279 0.192 Uiso 1 1 calc R U . . .
C35 C 0.2827(3) 0.2644(2) 0.6834(2) 0.086(2) Uani 1 1 d D . . . .
C36 C 0.2528(7) 0.3023(4) 0.7105(3) 0.117(5) Uani 0.682(10) 1 d D U P C 1
H36A H 0.2330 0.2892 0.7350 0.175 Uiso 0.682(10) 1 calc R U P C 1
H36B H 0.2168 0.3185 0.6918 0.175 Uiso 0.682(10) 1 calc R U P C 1
H36C H 0.2901 0.3228 0.7217 0.175 Uiso 0.682(10) 1 calc R U P C 1
C37 C 0.2219(6) 0.2280(4) 0.6709(5) 0.134(5) Uani 0.682(10) 1 d D U P C 1
H37A H 0.2030 0.2189 0.6973 0.201 Uiso 0.682(10) 1 calc R U P C 1
H37B H 0.2410 0.2020 0.6576 0.201 Uiso 0.682(10) 1 calc R U P C 1
H37C H 0.1850 0.2411 0.6501 0.201 Uiso 0.682(10) 1 calc R U P C 1
C38 C 0.3112(7) 0.2817(5) 0.6417(4) 0.119(5) Uani 0.682(10) 1 d D U P C 1
H38A H 0.3244 0.2563 0.6247 0.178 Uiso 0.682(10) 1 calc R U P C 1
H38B H 0.3517 0.3005 0.6502 0.178 Uiso 0.682(10) 1 calc R U P C 1
H38C H 0.2752 0.2990 0.6239 0.178 Uiso 0.682(10) 1 calc R U P C 1
C36' C 0.3064(13) 0.3158(4) 0.6861(9) 0.143(10) Uani 0.318(10) 1 d D U P C 2
H36D H 0.3456 0.3198 0.6697 0.215 Uiso 0.318(10) 1 calc R U P C 2
H36E H 0.3204 0.3241 0.7166 0.215 Uiso 0.318(10) 1 calc R U P C 2
H36F H 0.2678 0.3345 0.6735 0.215 Uiso 0.318(10) 1 calc R U P C 2
C37' C 0.2158(10) 0.2542(11) 0.7056(9) 0.134(9) Uani 0.318(10) 1 d D U P C 2
H37D H 0.2215 0.2669 0.7351 0.200 Uiso 0.318(10) 1 calc R U P C 2
H37E H 0.2094 0.2221 0.7073 0.200 Uiso 0.318(10) 1 calc R U P C 2
H37F H 0.1752 0.2675 0.6882 0.200 Uiso 0.318(10) 1 calc R U P C 2
C38' C 0.2766(15) 0.2474(9) 0.6342(4) 0.135(10) Uani 0.318(10) 1 d D U P C 2
H38D H 0.3166 0.2579 0.6211 0.203 Uiso 0.318(10) 1 calc R U P C 2
H38E H 0.2340 0.2591 0.6177 0.203 Uiso 0.318(10) 1 calc R U P C 2
H38F H 0.2754 0.2149 0.6337 0.203 Uiso 0.318(10) 1 calc R U P C 2
C39 C 0.6264(3) 0.20132(17) 0.74507(17) 0.0515(14) Uani 1 1 d . . . . .
H39A H 0.6102 0.2190 0.7687 0.062 Uiso 1 1 calc R U . . .
H39B H 0.5860 0.1968 0.7224 0.062 Uiso 1 1 calc R U . . .
C40 C 0.6799(3) 0.22937(17) 0.72484(16) 0.0439(13) Uani 1 1 d . . . . .
C41 C 0.7162(3) 0.2636(2) 0.74904(17) 0.0609(16) Uani 1 1 d . . . . .
H41 H 0.7096 0.2684 0.7785 0.073 Uiso 1 1 calc R U . . .
C42 C 0.7620(3) 0.2906(2) 0.72992(19) 0.0649(17) Uani 1 1 d . . . . .
H42 H 0.7862 0.3137 0.7465 0.078 Uiso 1 1 calc R U . . .
C43 C 0.7726(3) 0.28396(19) 0.68625(17) 0.0548(15) Uani 1 1 d . . . . .
H43 H 0.8036 0.3027 0.6736 0.066 Uiso 1 1 calc R U . . .
C44 C 0.7377(3) 0.24989(16) 0.66135(15) 0.0400(12) Uani 1 1 d . . . . .
C45 C 0.6916(3) 0.22227(17) 0.68127(16) 0.0418(12) Uani 1 1 d . . . . .
H45 H 0.6684 0.1987 0.6650 0.050 Uiso 1 1 calc R U . . .
C46 C 0.7474(3) 0.24178(17) 0.61349(16) 0.0488(13) Uani 1 1 d . . . . .
H46A H 0.7760 0.2148 0.6120 0.059 Uiso 1 1 calc R U . . .
H46B H 0.7015 0.2359 0.5966 0.059 Uiso 1 1 calc R U . . .
C47 C 0.5263(3) 0.07632(18) 0.68847(16) 0.0560(15) Uani 1 1 d . . . . .
H47A H 0.4826 0.0657 0.6715 0.067 Uiso 1 1 calc R U . . .
H47B H 0.5475 0.0511 0.7059 0.067 Uiso 1 1 calc R U . . .
C48 C 0.5763(3) 0.09223(16) 0.65651(15) 0.0444(13) Uani 1 1 d . . . . .
C49 C 0.6470(3) 0.08755(19) 0.66695(17) 0.0565(15) Uani 1 1 d . . . . .
H49 H 0.6660 0.0738 0.6935 0.068 Uiso 1 1 calc R U . . .
C50 C 0.6902(3) 0.1032(2) 0.63800(19) 0.0675(17) Uani 1 1 d . . . . .
H50 H 0.7389 0.1006 0.6453 0.081 Uiso 1 1 calc R U . . .
C51 C 0.6625(4) 0.12318(19) 0.59739(19) 0.0656(17) Uani 1 1 d . . . . .
H51 H 0.6926 0.1340 0.5781 0.079 Uiso 1 1 calc R U . . .
C52 C 0.5911(4) 0.12661(18) 0.58633(17) 0.0594(16) Uani 1 1 d . . . . .
C53 C 0.5478(3) 0.11140(17) 0.61598(17) 0.0556(15) Uani 1 1 d . . . . .
H53 H 0.4991 0.1139 0.6089 0.067 Uiso 1 1 calc R U . . .
C54 C 0.5596(4) 0.14450(19) 0.54166(16) 0.075(2) Uani 1 1 d . . . . .
H54A H 0.5973 0.1470 0.5233 0.090 Uiso 1 1 calc R U . . .
H54B H 0.5265 0.1220 0.5279 0.090 Uiso 1 1 calc R U . . .
C55 C 0.7386(3) 0.31268(18) 0.58141(15) 0.0434(13) Uani 1 1 d . . . . .
H55 H 0.6923 0.3081 0.5868 0.052 Uiso 1 1 calc R U . . .
C56 C 0.7518(3) 0.35582(17) 0.56225(15) 0.0418(12) Uani 1 1 d . . . . .
C57 C 0.6942(3) 0.38531(18) 0.55416(17) 0.0525(14) Uani 1 1 d . . . . .
H57 H 0.6505 0.3758 0.5609 0.063 Uiso 1 1 calc R U . . .
C58 C 0.6999(3) 0.42738(19) 0.53681(18) 0.0579(15) Uani 1 1 d . . . . .
C59 C 0.7676(4) 0.43997(19) 0.52874(19) 0.0659(17) Uani 1 1 d . . . . .
H59 H 0.7730 0.4692 0.5182 0.079 Uiso 1 1 calc R U . . .
C60 C 0.5802(4) 0.0852(2) 0.3703(2) 0.079(2) Uani 1 1 d . . . . .
H60 H 0.5774 0.0573 0.3561 0.095 Uiso 1 1 calc R U . . .
C61 C 0.8270(3) 0.41310(19) 0.53504(17) 0.0539(14) Uani 1 1 d . . . . .
C62 C 0.8181(3) 0.36865(19) 0.55209(15) 0.0460(13) Uani 1 1 d . . . . .
C63 C 0.6373(4) 0.4596(2) 0.5272(2) 0.0786(19) Uani 1 1 d . . . . .
C64 C 0.5730(4) 0.4432(3) 0.5440(4) 0.159(5) Uani 1 1 d . . . . .
H64A H 0.5599 0.4142 0.5310 0.238 Uiso 1 1 calc R U . . .
H64B H 0.5353 0.4644 0.5362 0.238 Uiso 1 1 calc R U . . .
H64C H 0.5820 0.4402 0.5758 0.238 Uiso 1 1 calc R U . . .
C65 C 0.6237(5) 0.4678(3) 0.4770(3) 0.170(5) Uani 1 1 d . . . . .
H65A H 0.6663 0.4783 0.4669 0.255 Uiso 1 1 calc R U . . .
H65B H 0.5873 0.4901 0.4705 0.255 Uiso 1 1 calc R U . . .
H65C H 0.6090 0.4400 0.4621 0.255 Uiso 1 1 calc R U . . .
C66 C 0.6560(4) 0.5059(2) 0.5482(3) 0.115(3) Uani 1 1 d . . . . .
H66A H 0.6961 0.5181 0.5363 0.172 Uiso 1 1 calc R U . . .
H66B H 0.6671 0.5025 0.5799 0.172 Uiso 1 1 calc R U . . .
H66C H 0.6165 0.5260 0.5416 0.172 Uiso 1 1 calc R U . . .
C67 C 0.8988(3) 0.4306(2) 0.5259(2) 0.079(2) Uani 1 1 d . . . . .
C68 C 0.9269(4) 0.4020(3) 0.4903(2) 0.105(3) Uani 1 1 d . . . . .
H68A H 0.9723 0.4133 0.4852 0.157 Uiso 1 1 calc R U . . .
H68B H 0.8947 0.4035 0.4632 0.157 Uiso 1 1 calc R U . . .
H68C H 0.9316 0.3711 0.5002 0.157 Uiso 1 1 calc R U . . .
C69 C 0.9515(4) 0.4279(3) 0.5688(2) 0.115(3) Uani 1 1 d . . . . .
H69A H 0.9967 0.4389 0.5632 0.172 Uiso 1 1 calc R U . . .
H69B H 0.9560 0.3970 0.5787 0.172 Uiso 1 1 calc R U . . .
H69C H 0.9347 0.4461 0.5914 0.172 Uiso 1 1 calc R U . . .
C70 C 0.8945(5) 0.4797(2) 0.5094(4) 0.162(5) Uani 1 1 d . . . . .
H70A H 0.9405 0.4897 0.5044 0.244 Uiso 1 1 calc R U . . .
H70B H 0.8776 0.4987 0.5315 0.244 Uiso 1 1 calc R U . . .
H70C H 0.8625 0.4815 0.4822 0.244 Uiso 1 1 calc R U . . .
C71 C 0.9774(3) 0.3092(3) 0.6793(2) 0.086(2) Uani 1 1 d . . . . .
C72 C 0.9443(5) 0.3494(4) 0.6974(4) 0.196(6) Uani 1 1 d . . . . .
H72A H 0.9390 0.3730 0.6754 0.293 Uiso 1 1 calc R U . . .
H72B H 0.9738 0.3600 0.7235 0.293 Uiso 1 1 calc R U . . .
H72C H 0.8987 0.3413 0.7049 0.293 Uiso 1 1 calc R U . . .
C73 C 1.0454(4) 0.3245(5) 0.6638(3) 0.246(8) Uani 1 1 d . . . . .
H73A H 1.0357 0.3489 0.6429 0.368 Uiso 1 1 calc R U . . .
H73B H 1.0661 0.2997 0.6498 0.368 Uiso 1 1 calc R U . . .
H73C H 1.0775 0.3347 0.6889 0.368 Uiso 1 1 calc R U . . .
C74 C 0.9840(8) 0.2745(4) 0.7154(4) 0.260(9) Uani 1 1 d . . . . .
H74A H 1.0035 0.2472 0.7050 0.390 Uiso 1 1 calc R U . . .
H74B H 0.9382 0.2683 0.7237 0.390 Uiso 1 1 calc R U . . .
H74C H 1.0146 0.2858 0.7408 0.390 Uiso 1 1 calc R U . . .
C75 C 1.0498(4) 0.2674(3) 0.5374(2) 0.084(2) Uani 1 1 d . . . . .
C76 C 1.1010(4) 0.3070(4) 0.5461(3) 0.159(4) Uani 1 1 d . . . . .
H76A H 1.1118 0.3118 0.5776 0.239 Uiso 1 1 calc R U . . .
H76B H 1.0797 0.3338 0.5323 0.239 Uiso 1 1 calc R U . . .
H76C H 1.1436 0.3003 0.5339 0.239 Uiso 1 1 calc R U . . .
C77 C 1.0822(5) 0.2257(3) 0.5601(3) 0.160(5) Uani 1 1 d . . . . .
H77A H 1.0935 0.2314 0.5914 0.241 Uiso 1 1 calc R U . . .
H77B H 1.1245 0.2180 0.5479 0.241 Uiso 1 1 calc R U . . .
H77C H 1.0493 0.2010 0.5554 0.241 Uiso 1 1 calc R U . . .
C78 C 1.0323(4) 0.2597(3) 0.4887(2) 0.131(3) Uani 1 1 d . . . . .
H78A H 1.0118 0.2867 0.4748 0.197 Uiso 1 1 calc R U . . .
H78B H 0.9993 0.2351 0.4835 0.197 Uiso 1 1 calc R U . . .
H78C H 1.0746 0.2523 0.4764 0.197 Uiso 1 1 calc R U . . .
C79 C 0.8680(3) 0.1707(2) 0.57242(17) 0.0510(14) Uani 1 1 d . . . . .
C80 C 0.8753(3) 0.1303(2) 0.5965(2) 0.0647(17) Uani 1 1 d . . . . .
C81 C 0.8434(4) 0.0916(2) 0.5761(2) 0.0735(19) Uani 1 1 d . . . . .
H81 H 0.8469 0.0649 0.5926 0.088 Uiso 1 1 calc R U . . .
C82 C 0.8070(4) 0.0897(2) 0.5334(2) 0.0766(19) Uani 1 1 d . . . . .
C83 C 0.8030(3) 0.1294(2) 0.5092(2) 0.0723(18) Uani 1 1 d . . . . .
H83 H 0.7799 0.1297 0.4802 0.087 Uiso 1 1 calc R U . . .
C84 C 0.8336(3) 0.16938(19) 0.52831(17) 0.0530(14) Uani 1 1 d . . . . .
C85 C 0.8306(3) 0.2086(2) 0.50023(17) 0.0571(16) Uani 1 1 d . . . . .
H85 H 0.8134 0.2032 0.4705 0.069 Uiso 1 1 calc R U . . .
C86 C 0.9167(4) 0.1285(2) 0.6433(2) 0.082(2) Uani 1 1 d . . . . .
C87 C 0.9926(4) 0.1435(3) 0.6412(3) 0.113(3) Uani 1 1 d . . . . .
H87A H 1.0191 0.1421 0.6704 0.170 Uiso 1 1 calc R U . . .
H87B H 0.9927 0.1740 0.6303 0.170 Uiso 1 1 calc R U . . .
H87C H 1.0138 0.1238 0.6216 0.170 Uiso 1 1 calc R U . . .
C88 C 0.9198(5) 0.0809(2) 0.6634(3) 0.121(3) Uani 1 1 d . . . . .
H88A H 0.9467 0.0816 0.6926 0.181 Uiso 1 1 calc R U . . .
H88B H 0.9418 0.0606 0.6448 0.181 Uiso 1 1 calc R U . . .
H88C H 0.8727 0.0706 0.6657 0.181 Uiso 1 1 calc R U . . .
C89 C 0.8852(4) 0.1602(2) 0.6754(2) 0.092(2) Uani 1 1 d . . . . .
H89A H 0.9124 0.1582 0.7044 0.138 Uiso 1 1 calc R U . . .
H89B H 0.8372 0.1515 0.6772 0.138 Uiso 1 1 calc R U . . .
H89C H 0.8862 0.1908 0.6648 0.138 Uiso 1 1 calc R U . . .
C90 C 0.7718(4) 0.0444(2) 0.5136(3) 0.109(3) Uani 1 1 d D U . . .
C91 C 0.8345(8) 0.0096(6) 0.5161(9) 0.150(8) Uani 0.512(13) 1 d D U P D 1
H91A H 0.8514 0.0030 0.5467 0.226 Uiso 0.512(13) 1 calc R U P D 1
H91B H 0.8721 0.0224 0.5021 0.226 Uiso 0.512(13) 1 calc R U P D 1
H91C H 0.8183 -0.0178 0.5010 0.226 Uiso 0.512(13) 1 calc R U P D 1
C92 C 0.7171(11) 0.0276(6) 0.5441(7) 0.142(8) Uani 0.512(13) 1 d D U P D 1
H92A H 0.7409 0.0219 0.5735 0.213 Uiso 0.512(13) 1 calc R U P D 1
H92B H 0.6950 0.0003 0.5320 0.213 Uiso 0.512(13) 1 calc R U P D 1
H92C H 0.6817 0.0505 0.5454 0.213 Uiso 0.512(13) 1 calc R U P D 1
C93 C 0.7395(15) 0.0517(7) 0.4641(5) 0.174(9) Uani 0.512(13) 1 d D U P D 1
H93A H 0.7765 0.0589 0.4468 0.261 Uiso 0.512(13) 1 calc R U P D 1
H93B H 0.7062 0.0762 0.4623 0.261 Uiso 0.512(13) 1 calc R U P D 1
H93C H 0.7160 0.0246 0.4528 0.261 Uiso 0.512(13) 1 calc R U P D 1
C91' C 0.8177(11) 0.0302(7) 0.4773(7) 0.142(8) Uani 0.488(13) 1 d D U P D 2
H91D H 0.8136 0.0526 0.4542 0.212 Uiso 0.488(13) 1 calc R U P D 2
H91E H 0.8017 0.0015 0.4649 0.212 Uiso 0.488(13) 1 calc R U P D 2
H91F H 0.8663 0.0277 0.4903 0.212 Uiso 0.488(13) 1 calc R U P D 2
C92' C 0.7717(16) 0.0108(7) 0.5531(6) 0.180(10) Uani 0.488(13) 1 d D U P D 2
H92D H 0.7391 0.0212 0.5723 0.270 Uiso 0.488(13) 1 calc R U P D 2
H92E H 0.8183 0.0092 0.5695 0.270 Uiso 0.488(13) 1 calc R U P D 2
H92F H 0.7577 -0.0187 0.5418 0.270 Uiso 0.488(13) 1 calc R U P D 2
C93' C 0.6951(7) 0.0567(6) 0.4922(8) 0.137(8) Uani 0.488(13) 1 d D U P D 2
H93D H 0.6678 0.0657 0.5150 0.206 Uiso 0.488(13) 1 calc R U P D 2
H93E H 0.6735 0.0307 0.4768 0.206 Uiso 0.488(13) 1 calc R U P D 2
H93F H 0.6968 0.0812 0.4715 0.206 Uiso 0.488(13) 1 calc R U P D 2
C94 C 0.8402(3) 0.28154(19) 0.47166(17) 0.0569(15) Uani 1 1 d . . . . .
H94A H 0.8524 0.2658 0.4457 0.068 Uiso 1 1 calc R U . . .
H94B H 0.8740 0.3060 0.4783 0.068 Uiso 1 1 calc R U . . .
C95 C 0.7674(3) 0.30193(18) 0.46012(15) 0.0482(14) Uani 1 1 d . . . . .
C96 C 0.7592(4) 0.3398(2) 0.43338(19) 0.0703(18) Uani 1 1 d . . . . .
H96 H 0.7987 0.3538 0.4246 0.084 Uiso 1 1 calc R U . . .
C97 C 0.6932(4) 0.3571(2) 0.4196(2) 0.087(2) Uani 1 1 d . . . . .
H97 H 0.6879 0.3825 0.4013 0.104 Uiso 1 1 calc R U . . .
C98 C 0.6350(4) 0.3366(2) 0.4330(2) 0.0710(18) Uani 1 1 d . . . . .
H98 H 0.5903 0.3483 0.4233 0.085 Uiso 1 1 calc R U . . .
C99 C 0.6415(3) 0.29957(18) 0.46001(17) 0.0484(14) Uani 1 1 d . . . . .
C100 C 0.7079(3) 0.28298(16) 0.47379(15) 0.0437(13) Uani 1 1 d . . . . .
H100 H 0.7129 0.2582 0.4929 0.052 Uiso 1 1 calc R U . . .
C101 C 0.5776(3) 0.27770(17) 0.47395(18) 0.0552(15) Uani 1 1 d . . . . .
H10G H 0.5843 0.2761 0.5062 0.066 Uiso 1 1 calc R U . . .
H10H H 0.5377 0.2976 0.4653 0.066 Uiso 1 1 calc R U . . .
C102 C 0.5954(3) 0.21212(17) 0.43086(16) 0.0477(14) Uani 1 1 d . . . . .
H102 H 0.6334 0.2288 0.4235 0.057 Uiso 1 1 calc R U . . .
C103 C 0.5874(3) 0.16759(18) 0.41131(16) 0.0508(14) Uani 1 1 d . . . . .
C104 C 0.6357(3) 0.1562(2) 0.38185(19) 0.0701(17) Uani 1 1 d . . . . .
H104 H 0.6702 0.1769 0.3765 0.084 Uiso 1 1 calc R U . . .
C105 C 0.6323(4) 0.1149(2) 0.3610(2) 0.0771(19) Uani 1 1 d . . . . .
C106 C 0.5319(3) 0.0942(2) 0.39949(19) 0.0652(17) Uani 1 1 d . . . . .
C107 C 0.5359(3) 0.13676(18) 0.41965(16) 0.0504(14) Uani 1 1 d . . . . .
C108 C 0.6833(5) 0.1035(3) 0.3264(3) 0.105(3) Uani 1 1 d . . . . .
C109 C 0.7478(6) 0.1310(4) 0.3319(5) 0.246(9) Uani 1 1 d . . . . .
H0C H 0.7770 0.1223 0.3099 0.369 Uiso 1 1 calc R U . . .
H0D H 0.7731 0.1262 0.3610 0.369 Uiso 1 1 calc R U . . .
H0E H 0.7355 0.1624 0.3282 0.369 Uiso 1 1 calc R U . . .
C110 C 0.6414(8) 0.1086(5) 0.2808(3) 0.244(8) Uani 1 1 d . . . . .
H11P H 0.5994 0.0904 0.2790 0.366 Uiso 1 1 calc R U . . .
H11Q H 0.6695 0.0987 0.2587 0.366 Uiso 1 1 calc R U . . .
H11R H 0.6285 0.1398 0.2758 0.366 Uiso 1 1 calc R U . . .
C111 C 0.7039(6) 0.0543(3) 0.3286(4) 0.206(6) Uani 1 1 d . . . . .
H11S H 0.6621 0.0358 0.3247 0.309 Uiso 1 1 calc R U . . .
H11T H 0.7307 0.0479 0.3571 0.309 Uiso 1 1 calc R U . . .
H11U H 0.7321 0.0476 0.3055 0.309 Uiso 1 1 calc R U . . .
C112 C 0.4746(4) 0.0602(2) 0.4073(3) 0.086(2) Uani 1 1 d . . . . .
C113 C 0.4846(5) 0.0153(3) 0.3816(3) 0.159(4) Uani 1 1 d . . . . .
H11V H 0.4489 -0.0061 0.3870 0.238 Uiso 1 1 calc R U . . .
H11W H 0.5305 0.0029 0.3916 0.238 Uiso 1 1 calc R U . . .
H11X H 0.4806 0.0216 0.3503 0.238 Uiso 1 1 calc R U . . .
C114 C 0.3998(4) 0.0793(3) 0.3909(3) 0.129(3) Uani 1 1 d . . . . .
H11J H 0.3647 0.0574 0.3961 0.194 Uiso 1 1 calc R U . . .
H11K H 0.3958 0.0857 0.3596 0.194 Uiso 1 1 calc R U . . .
H11L H 0.3926 0.1067 0.4067 0.194 Uiso 1 1 calc R U . . .
C115 C 0.4830(5) 0.0479(2) 0.4577(3) 0.124(3) Uani 1 1 d . . . . .
H11M H 0.4477 0.0261 0.4629 0.186 Uiso 1 1 calc R U . . .
H11N H 0.4775 0.0747 0.4748 0.186 Uiso 1 1 calc R U . . .
H11O H 0.5291 0.0352 0.4666 0.186 Uiso 1 1 calc R U . . .
C116 C 0.3124(6) 0.1550(3) 0.5112(3) 0.147(4) Uani 1 1 d D . . . .
C117 C 0.3223(7) 0.1718(5) 0.5594(3) 0.281(9) Uani 1 1 d D U . E 1
H1A' H 0.3617 0.1564 0.5759 0.421 Uiso 1 1 calc R U . E 1
H1B' H 0.2803 0.1657 0.5725 0.421 Uiso 1 1 calc R U . E 1
H1C' H 0.3312 0.2038 0.5599 0.421 Uiso 1 1 calc R U . E 1
C118 C 0.2484(6) 0.1731(6) 0.4800(5) 0.329(11) Uani 1 1 d D U . F 1
H1D' H 0.2468 0.1592 0.4513 0.494 Uiso 1 1 calc R U . F 1
H1E' H 0.2524 0.2054 0.4772 0.494 Uiso 1 1 calc R U . F 1
H1F' H 0.2058 0.1660 0.4922 0.494 Uiso 1 1 calc R U . F 1
C119 C 0.3198(7) 0.1039(3) 0.5123(5) 0.296(10) Uani 1 1 d D U . G 1
H1G' H 0.3167 0.0925 0.4825 0.444 Uiso 1 1 calc R U . G 1
H1H' H 0.2826 0.0910 0.5266 0.444 Uiso 1 1 calc R U . G 1
H1I' H 0.3646 0.0958 0.5286 0.444 Uiso 1 1 calc R U . G 1
C120 C 0.3850(5) 0.2404(3) 0.3734(2) 0.113(3) Uani 1 1 d D . . . .
C121 C 0.3181(7) 0.2658(7) 0.3693(4) 0.313(12) Uani 1 1 d D . . . .
H12A H 0.3223 0.2903 0.3903 0.470 Uiso 1 1 calc R U . . .
H12B H 0.2807 0.2459 0.3751 0.470 Uiso 1 1 calc R U . . .
H12C H 0.3077 0.2777 0.3397 0.470 Uiso 1 1 calc R U . . .
C122 C 0.3881(8) 0.2014(3) 0.3436(3) 0.222(7) Uani 1 1 d D . . . .
H12D H 0.4337 0.1873 0.3496 0.334 Uiso 1 1 calc R U . . .
H12E H 0.3803 0.2115 0.3133 0.334 Uiso 1 1 calc R U . . .
H12F H 0.3523 0.1799 0.3485 0.334 Uiso 1 1 calc R U . . .
C123 C 0.4333(10) 0.2776(6) 0.3613(4) 0.369(15) Uani 1 1 d D . . . .
H12G H 0.4304 0.3031 0.3807 0.553 Uiso 1 1 calc R U . . .
H12H H 0.4191 0.2867 0.3311 0.553 Uiso 1 1 calc R U . . .
H12I H 0.4810 0.2666 0.3646 0.553 Uiso 1 1 calc R U . . .
C124 C 0.4571(3) 0.28118(17) 0.54754(15) 0.0419(12) Uani 1 1 d . . . . .
C125 C 0.4302(3) 0.32393(17) 0.55611(16) 0.0471(13) Uani 1 1 d . . . . .
C126 C 0.4550(3) 0.34342(18) 0.59689(17) 0.0544(14) Uani 1 1 d . . . . .
H126 H 0.4388 0.3723 0.6025 0.065 Uiso 1 1 calc R U . . .
C127 C 0.5021(3) 0.32305(18) 0.63008(16) 0.0497(14) Uani 1 1 d . . . . .
C128 C 0.5250(3) 0.28120(17) 0.62090(16) 0.0478(13) Uani 1 1 d . . . . .
H128 H 0.5557 0.2663 0.6426 0.057 Uiso 1 1 calc R U . . .
C129 C 0.5046(3) 0.25908(17) 0.58025(15) 0.0445(13) Uani 1 1 d . . . . .
C130 C 0.5329(3) 0.21458(17) 0.57436(16) 0.0505(14) Uani 1 1 d . . . . .
H130 H 0.5627 0.2031 0.5986 0.061 Uiso 1 1 calc R U . . .
C131 C 0.3750(3) 0.34744(18) 0.52185(18) 0.0573(15) Uani 1 1 d . . . . .
C132 C 0.4054(4) 0.3570(2) 0.47887(19) 0.082(2) Uani 1 1 d . . . . .
H13D H 0.3703 0.3715 0.4580 0.124 Uiso 1 1 calc R U . . .
H13E H 0.4193 0.3289 0.4665 0.124 Uiso 1 1 calc R U . . .
H13F H 0.4458 0.3764 0.4850 0.124 Uiso 1 1 calc R U . . .
C134 C 0.3534(4) 0.3930(2) 0.5395(2) 0.102(3) Uani 1 1 d . . . . .
H13G H 0.3339 0.3884 0.5667 0.153 Uiso 1 1 calc R U . . .
H13H H 0.3186 0.4069 0.5179 0.153 Uiso 1 1 calc R U . . .
H13I H 0.3941 0.4123 0.5450 0.153 Uiso 1 1 calc R U . . .
C133 C 0.3104(3) 0.3172(2) 0.5124(2) 0.083(2) Uani 1 1 d . . . . .
H13J H 0.2918 0.3112 0.5397 0.124 Uiso 1 1 calc R U . . .
H13K H 0.3234 0.2892 0.4996 0.124 Uiso 1 1 calc R U . . .
H13L H 0.2751 0.3322 0.4920 0.124 Uiso 1 1 calc R U . . .
C135 C 0.5276(3) 0.3469(2) 0.67433(18) 0.0628(16) Uani 1 1 d . . . . .
C136 C 0.4887(6) 0.3889(3) 0.6801(3) 0.159(5) Uani 1 1 d . . . . .
H13M H 0.4394 0.3822 0.6795 0.239 Uiso 1 1 calc R U . . .
H13N H 0.4947 0.4096 0.6565 0.239 Uiso 1 1 calc R U . . .
H13O H 0.5066 0.4025 0.7082 0.239 Uiso 1 1 calc R U . . .
C137 C 0.6048(4) 0.3581(3) 0.6755(3) 0.129(3) Uani 1 1 d . . . . .
H13P H 0.6310 0.3308 0.6726 0.193 Uiso 1 1 calc R U . . .
H13Q H 0.6219 0.3725 0.7033 0.193 Uiso 1 1 calc R U . . .
H13R H 0.6107 0.3782 0.6514 0.193 Uiso 1 1 calc R U . . .
C138 C 0.5222(4) 0.3154(2) 0.71263(19) 0.104(3) Uani 1 1 d . . . . .
H13S H 0.5475 0.2879 0.7085 0.155 Uiso 1 1 calc R U . . .
H13T H 0.4735 0.3085 0.7140 0.155 Uiso 1 1 calc R U . . .
H13U H 0.5423 0.3296 0.7399 0.155 Uiso 1 1 calc R U . . .
N1 N 0.6488(2) 0.15639(13) 0.76365(12) 0.0397(10) Uani 1 1 d . . . . .
N2 N 0.5104(2) 0.11339(14) 0.71881(13) 0.0471(11) Uani 1 1 d . . . . .
N3 N 0.8479(2) 0.24982(17) 0.50944(13) 0.0490(11) Uani 1 1 d . . . . .
N4 N 0.7808(2) 0.27940(14) 0.59225(12) 0.0394(10) Uani 1 1 d . . . . .
N5 N 0.5224(2) 0.18867(14) 0.54010(13) 0.0508(11) Uani 1 1 d . . . . .
N6 N 0.5581(2) 0.23179(14) 0.45659(13) 0.0461(11) Uani 1 1 d . . . . .
O1 O 0.63386(18) 0.06463(11) 0.77649(11) 0.0472(9) Uani 1 1 d . . . . .
O2 O 0.50529(18) 0.16940(11) 0.79103(10) 0.0480(9) Uani 1 1 d . . . . .
O3 O 0.4933(2) 0.06878(13) 0.80373(12) 0.0665(11) Uani 1 1 d . . . . .
O4 O 0.61204(18) 0.12259(12) 0.85248(10) 0.0552(10) Uani 1 1 d . . . . .
O5 O 0.87073(18) 0.33954(12) 0.55762(11) 0.0538(9) Uani 1 1 d . . . . .
O6 O 0.89334(19) 0.20926(13) 0.59036(11) 0.0554(10) Uani 1 1 d . . . . .
O7 O 0.93198(19) 0.29266(13) 0.64210(11) 0.0622(11) Uani 1 1 d . . . . .
O8 O 0.98839(19) 0.27832(13) 0.55552(12) 0.0642(11) Uani 1 1 d . . . . .
O9 O 0.49090(19) 0.14842(12) 0.44728(11) 0.0543(9) Uani 1 1 d . . . . .
O10 O 0.43883(18) 0.26080(11) 0.50857(10) 0.0500(9) Uani 1 1 d . . . . .
O11 O 0.3734(2) 0.16928(15) 0.49293(14) 0.0838(13) Uani 1 1 d . . . . .
O12 O 0.4072(2) 0.22982(14) 0.41712(12) 0.0752(12) Uani 1 1 d . . . . .
Hf1 Hf 0.56410(2) 0.11152(2) 0.79408(2) 0.04167(7) Uani 1 1 d . . . . .
Hf2 Hf 0.90158(2) 0.27732(2) 0.58070(2) 0.04776(7) Uani 1 1 d . . . . .
Hf3 Hf 0.44735(2) 0.20367(2) 0.47247(2) 0.05047(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.271(6) . ?
C1 C2 1.446(7) . ?
C1 H1 0.9300 . ?
C2 C3 1.387(7) . ?
C2 C7 1.407(7) . ?
C3 C4 1.379(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.392(8) . ?
C4 C8 1.523(9) . ?
C5 C6 1.352(8) . ?
C5 H5 0.9300 . ?
C6 C7 1.438(7) . ?
C6 C12 1.539(8) . ?
C7 O1 1.335(6) . ?
C8 C9' 1.519(10) . ?
C8 C9 1.524(8) . ?
C8 C10' 1.526(10) . ?
C8 C11 1.527(8) . ?
C8 C11' 1.544(10) . ?
C8 C10 1.545(8) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C9' H9'1 0.9600 . ?
C9' H9'2 0.9600 . ?
C9' H9'3 0.9600 . ?
C10' H10D 0.9600 . ?
C10' H10E 0.9600 . ?
C10' H10F 0.9600 . ?
C11' H11D 0.9600 . ?
C11' H11E 0.9600 . ?
C11' H11F 0.9600 . ?
C12 C14 1.524(8) . ?
C12 C15 1.530(9) . ?
C12 C13 1.573(8) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 O4 1.399(6) . ?
C16 C18 1.497(10) . ?
C16 C17 1.516(9) . ?
C16 C19 1.527(9) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O3 1.410(7) . ?
C20 C23 1.508(9) . ?
C20 C21' 1.518(9) . ?
C20 C23' 1.528(9) . ?
C20 C22' 1.529(9) . ?
C20 C22 1.532(9) . ?
C20 C21 1.543(9) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C21' H21D 0.9600 . ?
C21' H21E 0.9600 . ?
C21' H21F 0.9600 . ?
C22' H22D 0.9600 . ?
C22' H22E 0.9600 . ?
C22' H22F 0.9600 . ?
C23' H23D 0.9600 . ?
C23' H23E 0.9600 . ?
C23' H23F 0.9600 . ?
C24 O2 1.304(6) . ?
C24 C29 1.401(6) . ?
C24 C25 1.413(7) . ?
C25 C26 1.395(7) . ?
C25 C31 1.538(7) . ?
C26 C27 1.400(8) . ?
C26 H26 0.9300 . ?
C27 C28 1.356(7) . ?
C27 C35 1.579(8) . ?
C28 C29 1.419(7) . ?
C28 H28 0.9300 . ?
C29 C30 1.443(7) . ?
C30 N2 1.278(6) . ?
C30 H30 0.9300 . ?
C31 C32 1.510(9) . ?
C31 C33 1.533(9) . ?
C31 C34 1.540(8) . ?
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 C38 1.532(8) . ?
C35 C36 1.542(7) . ?
C35 C37' 1.552(9) . ?
C35 C38' 1.564(9) . ?
C35 C36' 1.580(9) . ?
C35 C37 1.590(8) . ?
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 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C36' H36D 0.9600 . ?
C36' H36E 0.9600 . ?
C36' H36F 0.9600 . ?
C37' H37D 0.9600 . ?
C37' H37E 0.9600 . ?
C37' H37F 0.9600 . ?
C38' H38D 0.9600 . ?
C38' H38E 0.9600 . ?
C38' H38F 0.9600 . ?
C39 N1 1.481(6) . ?
C39 C40 1.509(7) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C40 C41 1.379(7) . ?
C40 C45 1.386(6) . ?
C41 C42 1.369(7) . ?
C41 H41 0.9300 . ?
C42 C43 1.382(7) . ?
C42 H42 0.9300 . ?
C43 C44 1.375(7) . ?
C43 H43 0.9300 . ?
C44 C45 1.396(6) . ?
C44 C46 1.508(6) . ?
C45 H45 0.9300 . ?
C46 N4 1.472(6) . ?
C46 H46A 0.9700 . ?
C46 H46B 0.9700 . ?
C47 N2 1.487(6) . ?
C47 C48 1.525(7) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 C49 1.352(7) . ?
C48 C53 1.395(7) . ?
C49 C50 1.365(7) . ?
C49 H49 0.9300 . ?
C50 C51 1.403(8) . ?
C50 H50 0.9300 . ?
C51 C52 1.364(8) . ?
C51 H51 0.9300 . ?
C52 C53 1.377(7) . ?
C52 C54 1.502(7) . ?
C53 H53 0.9300 . ?
C54 N5 1.482(6) . ?
C54 H54A 0.9700 . ?
C54 H54B 0.9700 . ?
C55 N4 1.285(6) . ?
C55 C56 1.436(7) . ?
C55 H55 0.9300 . ?
C56 C62 1.396(7) . ?
C56 C57 1.398(7) . ?
C57 C58 1.358(7) . ?
C57 H57 0.9300 . ?
C58 C59 1.399(8) . ?
C58 C63 1.524(8) . ?
C59 C61 1.376(8) . ?
C59 H59 0.9300 . ?
C60 C105 1.384(8) . ?
C60 C106 1.387(8) . ?
C60 H60 0.9300 . ?
C61 C62 1.428(7) . ?
C61 C67 1.526(8) . ?
C62 O5 1.315(6) . ?
C63 C64 1.473(9) . ?
C63 C65 1.529(10) . ?
C63 C66 1.529(9) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C67 C68 1.523(9) . ?
C67 C70 1.532(9) . ?
C67 C69 1.536(9) . ?
C68 H68A 0.9600 . ?
C68 H68B 0.9600 . ?
C68 H68C 0.9600 . ?
C69 H69A 0.9600 . ?
C69 H69B 0.9600 . ?
C69 H69C 0.9600 . ?
C70 H70A 0.9600 . ?
C70 H70B 0.9600 . ?
C70 H70C 0.9600 . ?
C71 O7 1.414(7) . ?
C71 C72 1.485(10) . ?
C71 C74 1.491(11) . ?
C71 C73 1.509(11) . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C74 H74A 0.9600 . ?
C74 H74B 0.9600 . ?
C74 H74C 0.9600 . ?
C75 O8 1.400(7) . ?
C75 C78 1.485(9) . ?
C75 C77 1.501(10) . ?
C75 C76 1.523(11) . ?
C76 H76A 0.9600 . ?
C76 H76B 0.9600 . ?
C76 H76C 0.9600 . ?
C77 H77A 0.9600 . ?
C77 H77B 0.9600 . ?
C77 H77C 0.9600 . ?
C78 H78A 0.9600 . ?
C78 H78B 0.9600 . ?
C78 H78C 0.9600 . ?
C79 O6 1.323(6) . ?
C79 C80 1.396(7) . ?
C79 C84 1.409(7) . ?
C80 C81 1.400(8) . ?
C80 C86 1.530(8) . ?
C81 C82 1.385(9) . ?
C81 H81 0.9300 . ?
C82 C83 1.378(8) . ?
C82 C90 1.579(9) . ?
C83 C84 1.406(8) . ?
C83 H83 0.9300 . ?
C84 C85 1.433(7) . ?
C85 N3 1.281(7) . ?
C85 H85 0.9300 . ?
C86 C87 1.525(10) . ?
C86 C88 1.530(9) . ?
C86 C89 1.533(9) . ?
C87 H87A 0.9600 . ?
C87 H87B 0.9600 . ?
C87 H87C 0.9600 . ?
C88 H88A 0.9600 . ?
C88 H88B 0.9600 . ?
C88 H88C 0.9600 . ?
C89 H89A 0.9600 . ?
C89 H89B 0.9600 . ?
C89 H89C 0.9600 . ?
C90 C92' 1.552(9) . ?
C90 C91' 1.557(9) . ?
C90 C93 1.560(9) . ?
C90 C93' 1.564(9) . ?
C90 C92 1.566(9) . ?
C90 C91 1.570(9) . ?
C91 H91A 0.9600 . ?
C91 H91B 0.9600 . ?
C91 H91C 0.9600 . ?
C92 H92A 0.9600 . ?
C92 H92B 0.9600 . ?
C92 H92C 0.9600 . ?
C93 H93A 0.9600 . ?
C93 H93B 0.9600 . ?
C93 H93C 0.9600 . ?
C91' H91D 0.9600 . ?
C91' H91E 0.9600 . ?
C91' H91F 0.9600 . ?
C92' H92D 0.9600 . ?
C92' H92E 0.9600 . ?
C92' H92F 0.9600 . ?
C93' H93D 0.9600 . ?
C93' H93E 0.9600 . ?
C93' H93F 0.9600 . ?
C94 N3 1.471(6) . ?
C94 C95 1.512(7) . ?
C94 H94A 0.9700 . ?
C94 H94B 0.9700 . ?
C95 C96 1.378(7) . ?
C95 C100 1.381(7) . ?
C96 C97 1.370(9) . ?
C96 H96 0.9300 . ?
C97 C98 1.375(8) . ?
C97 H97 0.9300 . ?
C98 C99 1.363(7) . ?
C98 H98 0.9300 . ?
C99 C100 1.370(7) . ?
C99 C101 1.492(7) . ?
C100 H100 0.9300 . ?
C101 N6 1.482(6) . ?
C101 H10G 0.9700 . ?
C101 H10H 0.9700 . ?
C102 N6 1.266(6) . ?
C102 C103 1.441(7) . ?
C102 H102 0.9300 . ?
C103 C107 1.388(7) . ?
C103 C104 1.409(7) . ?
C104 C105 1.369(8) . ?
C104 H104 0.9300 . ?
C105 C108 1.564(9) . ?
C106 C107 1.395(7) . ?
C106 C112 1.527(9) . ?
C107 O9 1.325(6) . ?
C108 C109 1.464(11) . ?
C108 C111 1.505(11) . ?
C108 C110 1.508(13) . ?
C109 H0C 0.9600 . ?
C109 H0D 0.9600 . ?
C109 H0E 0.9600 . ?
C110 H11P 0.9600 . ?
C110 H11Q 0.9600 . ?
C110 H11R 0.9600 . ?
C111 H11S 0.9600 . ?
C111 H11T 0.9600 . ?
C111 H11U 0.9600 . ?
C112 C114 1.556(10) . ?
C112 C115 1.559(10) . ?
C112 C113 1.560(9) . ?
C113 H11V 0.9600 . ?
C113 H11W 0.9600 . ?
C113 H11X 0.9600 . ?
C114 H11J 0.9600 . ?
C114 H11K 0.9600 . ?
C114 H11L 0.9600 . ?
C115 H11M 0.9600 . ?
C115 H11N 0.9600 . ?
C115 H11O 0.9600 . ?
C116 O11 1.420(8) . ?
C116 C119 1.515(8) . ?
C116 C117 1.531(8) . ?
C116 C118 1.536(8) . ?
C117 H1A' 0.9600 . ?
C117 H1B' 0.9600 . ?
C117 H1C' 0.9600 . ?
C118 H1D' 0.9600 . ?
C118 H1E' 0.9600 . ?
C118 H1F' 0.9600 . ?
C119 H1G' 0.9600 . ?
C119 H1H' 0.9600 . ?
C119 H1I' 0.9600 . ?
C120 O12 1.371(7) . ?
C120 C122 1.469(7) . ?
C120 C121 1.473(8) . ?
C120 C123 1.510(9) . ?
C121 H12A 0.9600 . ?
C121 H12B 0.9600 . ?
C121 H12C 0.9600 . ?
C122 H12D 0.9600 . ?
C122 H12E 0.9600 . ?
C122 H12F 0.9600 . ?
C123 H12G 0.9600 . ?
C123 H12H 0.9600 . ?
C123 H12I 0.9600 . ?
C124 O10 1.330(5) . ?
C124 C125 1.400(6) . ?
C124 C129 1.410(7) . ?
C125 C126 1.388(7) . ?
C125 C131 1.542(7) . ?
C126 C127 1.393(7) . ?
C126 H126 0.9300 . ?
C127 C128 1.351(7) . ?
C127 C135 1.535(7) . ?
C128 C129 1.403(6) . ?
C128 H128 0.9300 . ?
C129 C130 1.440(7) . ?
C130 N5 1.284(6) . ?
C130 H130 0.9300 . ?
C131 C133 1.517(8) . ?
C131 C134 1.524(8) . ?
C131 C132 1.524(8) . ?
C132 H13D 0.9600 . ?
C132 H13E 0.9600 . ?
C132 H13F 0.9600 . ?
C134 H13G 0.9600 . ?
C134 H13H 0.9600 . ?
C134 H13I 0.9600 . ?
C133 H13J 0.9600 . ?
C133 H13K 0.9600 . ?
C133 H13L 0.9600 . ?
C135 C136 1.469(9) . ?
C135 C138 1.502(8) . ?
C135 C137 1.507(9) . ?
C136 H13M 0.9600 . ?
C136 H13N 0.9600 . ?
C136 H13O 0.9600 . ?
C137 H13P 0.9600 . ?
C137 H13Q 0.9600 . ?
C137 H13R 0.9600 . ?
C138 H13S 0.9600 . ?
C138 H13T 0.9600 . ?
C138 H13U 0.9600 . ?
N1 Hf1 2.372(4) . ?
N2 Hf1 2.374(4) . ?
N3 Hf2 2.405(4) . ?
N4 Hf2 2.381(4) . ?
N5 Hf3 2.379(4) . ?
N6 Hf3 2.383(4) . ?
O1 Hf1 2.042(3) . ?
O2 Hf1 2.039(3) . ?
O3 Hf1 1.900(4) . ?
O4 Hf1 1.909(3) . ?
O5 Hf2 2.024(4) . ?
O6 Hf2 2.039(4) . ?
O7 Hf2 1.928(3) . ?
O8 Hf2 1.918(3) . ?
O9 Hf3 2.026(3) . ?
O10 Hf3 2.029(3) . ?
O11 Hf3 1.910(4) . ?
O12 Hf3 1.912(4) . ?

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
N1 C1 C2 127.8(5) . . ?
N1 C1 H1 116.1 . . ?
C2 C1 H1 116.1 . . ?
C3 C2 C7 119.9(5) . . ?
C3 C2 C1 118.1(5) . . ?
C7 C2 C1 121.9(5) . . ?
C4 C3 C2 123.0(5) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C5 115.0(5) . . ?
C3 C4 C8 123.6(6) . . ?
C5 C4 C8 121.4(5) . . ?
C6 C5 C4 126.5(5) . . ?
C6 C5 H5 116.8 . . ?
C4 C5 H5 116.8 . . ?
C5 C6 C7 117.2(5) . . ?
C5 C6 C12 123.9(5) . . ?
C7 C6 C12 118.9(5) . . ?
O1 C7 C2 120.5(4) . . ?
O1 C7 C6 121.1(5) . . ?
C2 C7 C6 118.3(5) . . ?
C9' C8 C4 113.7(17) . . ?
C4 C8 C9 111.9(8) . . ?
C9' C8 C10' 127(2) . . ?
C4 C8 C10' 110.2(13) . . ?
C4 C8 C11 111.0(7) . . ?
C9 C8 C11 109.7(10) . . ?
C9' C8 C11' 100(2) . . ?
C4 C8 C11' 103.0(11) . . ?
C10' C8 C11' 97.9(18) . . ?
C4 C8 C10 108.0(7) . . ?
C9 C8 C10 106.9(8) . . ?
C11 C8 C10 109.1(10) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C8 C9' H9'1 109.5 . . ?
C8 C9' H9'2 109.5 . . ?
H9'1 C9' H9'2 109.5 . . ?
C8 C9' H9'3 109.5 . . ?
H9'1 C9' H9'3 109.5 . . ?
H9'2 C9' H9'3 109.5 . . ?
C8 C10' H10D 109.5 . . ?
C8 C10' H10E 109.5 . . ?
H10D C10' H10E 109.5 . . ?
C8 C10' H10F 109.5 . . ?
H10D C10' H10F 109.5 . . ?
H10E C10' H10F 109.5 . . ?
C8 C11' H11D 109.5 . . ?
C8 C11' H11E 109.5 . . ?
H11D C11' H11E 109.5 . . ?
C8 C11' H11F 109.5 . . ?
H11D C11' H11F 109.5 . . ?
H11E C11' H11F 109.5 . . ?
C14 C12 C15 111.5(6) . . ?
C14 C12 C6 111.2(5) . . ?
C15 C12 C6 110.9(5) . . ?
C14 C12 C13 105.7(5) . . ?
C15 C12 C13 107.0(6) . . ?
C6 C12 C13 110.4(5) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O4 C16 C18 108.5(6) . . ?
O4 C16 C17 109.5(5) . . ?
C18 C16 C17 112.3(7) . . ?
O4 C16 C19 107.7(5) . . ?
C18 C16 C19 107.4(7) . . ?
C17 C16 C19 111.2(7) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C16 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O3 C20 C23 108.7(8) . . ?
O3 C20 C21' 107.7(9) . . ?
O3 C20 C23' 109.7(10) . . ?
C21' C20 C23' 120.1(16) . . ?
O3 C20 C22' 107.8(9) . . ?
C21' C20 C22' 107.2(15) . . ?
C23' C20 C22' 103.7(15) . . ?
O3 C20 C22 107.2(8) . . ?
C23 C20 C22 110.0(12) . . ?
O3 C20 C21 108.4(8) . . ?
C23 C20 C21 118.0(12) . . ?
C22 C20 C21 104.0(12) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C20 C21' H21D 109.5 . . ?
C20 C21' H21E 109.5 . . ?
H21D C21' H21E 109.5 . . ?
C20 C21' H21F 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
C20 C22' H22D 109.5 . . ?
C20 C22' H22E 109.5 . . ?
H22D C22' H22E 109.5 . . ?
C20 C22' H22F 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 109.5 . . ?
C20 C23' H23D 109.5 . . ?
C20 C23' H23E 109.5 . . ?
H23D C23' H23E 109.5 . . ?
C20 C23' H23F 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
O2 C24 C29 120.7(5) . . ?
O2 C24 C25 121.5(4) . . ?
C29 C24 C25 117.8(5) . . ?
C26 C25 C24 119.1(5) . . ?
C26 C25 C31 120.6(5) . . ?
C24 C25 C31 120.3(5) . . ?
C25 C26 C27 123.1(5) . . ?
C25 C26 H26 118.4 . . ?
C27 C26 H26 118.4 . . ?
C28 C27 C26 117.5(5) . . ?
C28 C27 C35 120.3(5) . . ?
C26 C27 C35 122.0(5) . . ?
C27 C28 C29 121.5(5) . . ?
C27 C28 H28 119.3 . . ?
C29 C28 H28 119.3 . . ?
C24 C29 C28 120.9(5) . . ?
C24 C29 C30 122.1(5) . . ?
C28 C29 C30 117.0(5) . . ?
N2 C30 C29 129.1(5) . . ?
N2 C30 H30 115.4 . . ?
C29 C30 H30 115.4 . . ?
C32 C31 C33 110.0(6) . . ?
C32 C31 C25 110.0(5) . . ?
C33 C31 C25 110.5(6) . . ?
C32 C31 C34 107.3(6) . . ?
C33 C31 C34 106.4(6) . . ?
C25 C31 C34 112.6(5) . . ?
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 . . ?
C38 C35 C36 113.5(7) . . ?
C37' C35 C38' 113.2(11) . . ?
C38 C35 C27 107.8(6) . . ?
C36 C35 C27 110.1(6) . . ?
C37' C35 C27 105.0(11) . . ?
C38' C35 C27 110.2(10) . . ?
C37' C35 C36' 114.3(11) . . ?
C38' C35 C36' 109.8(10) . . ?
C27 C35 C36' 103.9(9) . . ?
C38 C35 C37 110.8(8) . . ?
C36 C35 C37 107.9(7) . . ?
C27 C35 C37 106.4(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 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C35 C36' H36D 109.5 . . ?
C35 C36' H36E 109.5 . . ?
H36D C36' H36E 109.5 . . ?
C35 C36' H36F 109.5 . . ?
H36D C36' H36F 109.5 . . ?
H36E C36' H36F 109.5 . . ?
C35 C37' H37D 109.5 . . ?
C35 C37' H37E 109.5 . . ?
H37D C37' H37E 109.5 . . ?
C35 C37' H37F 109.5 . . ?
H37D C37' H37F 109.5 . . ?
H37E C37' H37F 109.5 . . ?
C35 C38' H38D 109.5 . . ?
C35 C38' H38E 109.5 . . ?
H38D C38' H38E 109.5 . . ?
C35 C38' H38F 109.5 . . ?
H38D C38' H38F 109.5 . . ?
H38E C38' H38F 109.5 . . ?
N1 C39 C40 118.0(4) . . ?
N1 C39 H39A 107.8 . . ?
C40 C39 H39A 107.8 . . ?
N1 C39 H39B 107.8 . . ?
C40 C39 H39B 107.8 . . ?
H39A C39 H39B 107.1 . . ?
C41 C40 C45 118.9(5) . . ?
C41 C40 C39 120.3(5) . . ?
C45 C40 C39 120.7(5) . . ?
C42 C41 C40 120.3(5) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 C43 120.6(5) . . ?
C41 C42 H42 119.7 . . ?
C43 C42 H42 119.7 . . ?
C44 C43 C42 120.5(5) . . ?
C44 C43 H43 119.7 . . ?
C42 C43 H43 119.7 . . ?
C43 C44 C45 118.5(5) . . ?
C43 C44 C46 122.1(5) . . ?
C45 C44 C46 119.4(5) . . ?
C40 C45 C44 121.2(5) . . ?
C40 C45 H45 119.4 . . ?
C44 C45 H45 119.4 . . ?
N4 C46 C44 114.8(4) . . ?
N4 C46 H46A 108.6 . . ?
C44 C46 H46A 108.6 . . ?
N4 C46 H46B 108.6 . . ?
C44 C46 H46B 108.6 . . ?
H46A C46 H46B 107.5 . . ?
N2 C47 C48 111.4(4) . . ?
N2 C47 H47A 109.3 . . ?
C48 C47 H47A 109.3 . . ?
N2 C47 H47B 109.3 . . ?
C48 C47 H47B 109.3 . . ?
H47A C47 H47B 108.0 . . ?
C49 C48 C53 120.4(5) . . ?
C49 C48 C47 120.8(5) . . ?
C53 C48 C47 118.8(5) . . ?
C48 C49 C50 119.1(5) . . ?
C48 C49 H49 120.4 . . ?
C50 C49 H49 120.4 . . ?
C49 C50 C51 121.2(6) . . ?
C49 C50 H50 119.4 . . ?
C51 C50 H50 119.4 . . ?
C52 C51 C50 119.5(6) . . ?
C52 C51 H51 120.2 . . ?
C50 C51 H51 120.2 . . ?
C51 C52 C53 119.0(5) . . ?
C51 C52 C54 120.9(6) . . ?
C53 C52 C54 120.1(6) . . ?
C52 C53 C48 120.7(5) . . ?
C52 C53 H53 119.6 . . ?
C48 C53 H53 119.6 . . ?
N5 C54 C52 118.0(4) . . ?
N5 C54 H54A 107.8 . . ?
C52 C54 H54A 107.8 . . ?
N5 C54 H54B 107.8 . . ?
C52 C54 H54B 107.8 . . ?
H54A C54 H54B 107.1 . . ?
N4 C55 C56 129.9(5) . . ?
N4 C55 H55 115.0 . . ?
C56 C55 H55 115.0 . . ?
C62 C56 C57 120.6(5) . . ?
C62 C56 C55 123.0(5) . . ?
C57 C56 C55 116.4(5) . . ?
C58 C57 C56 122.3(5) . . ?
C58 C57 H57 118.8 . . ?
C56 C57 H57 118.8 . . ?
C57 C58 C59 115.8(5) . . ?
C57 C58 C63 122.8(6) . . ?
C59 C58 C63 121.4(6) . . ?
C61 C59 C58 126.0(5) . . ?
C61 C59 H59 117.0 . . ?
C58 C59 H59 117.0 . . ?
C105 C60 C106 124.6(6) . . ?
C105 C60 H60 117.7 . . ?
C106 C60 H60 117.7 . . ?
C59 C61 C62 116.3(5) . . ?
C59 C61 C67 121.7(5) . . ?
C62 C61 C67 122.0(5) . . ?
O5 C62 C56 119.7(5) . . ?
O5 C62 C61 121.3(5) . . ?
C56 C62 C61 119.0(5) . . ?
C64 C63 C58 113.5(6) . . ?
C64 C63 C65 111.1(8) . . ?
C58 C63 C65 108.2(6) . . ?
C64 C63 C66 107.9(7) . . ?
C58 C63 C66 110.1(6) . . ?
C65 C63 C66 105.8(7) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C68 C67 C61 110.7(5) . . ?
C68 C67 C70 107.6(6) . . ?
C61 C67 C70 111.6(6) . . ?
C68 C67 C69 108.6(6) . . ?
C61 C67 C69 109.3(5) . . ?
C70 C67 C69 109.0(7) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C67 C70 H70A 109.5 . . ?
C67 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C67 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
O7 C71 C72 108.9(6) . . ?
O7 C71 C74 109.4(7) . . ?
C72 C71 C74 106.0(9) . . ?
O7 C71 C73 108.4(6) . . ?
C72 C71 C73 107.6(9) . . ?
C74 C71 C73 116.4(9) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
O8 C75 C78 109.8(6) . . ?
O8 C75 C77 108.9(6) . . ?
C78 C75 C77 110.7(7) . . ?
O8 C75 C76 107.9(6) . . ?
C78 C75 C76 110.0(7) . . ?
C77 C75 C76 109.5(8) . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C75 C77 H77A 109.5 . . ?
C75 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C75 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C75 C78 H78A 109.5 . . ?
C75 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C75 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
O6 C79 C80 120.9(5) . . ?
O6 C79 C84 120.8(5) . . ?
C80 C79 C84 118.3(5) . . ?
C79 C80 C81 117.4(6) . . ?
C79 C80 C86 121.3(6) . . ?
C81 C80 C86 121.4(6) . . ?
C82 C81 C80 125.3(6) . . ?
C82 C81 H81 117.3 . . ?
C80 C81 H81 117.3 . . ?
C83 C82 C81 116.7(6) . . ?
C83 C82 C90 121.8(7) . . ?
C81 C82 C90 121.5(7) . . ?
C82 C83 C84 120.2(6) . . ?
C82 C83 H83 119.9 . . ?
C84 C83 H83 119.9 . . ?
C83 C84 C79 121.9(5) . . ?
C83 C84 C85 116.8(5) . . ?
C79 C84 C85 121.2(5) . . ?
N3 C85 C84 130.4(5) . . ?
N3 C85 H85 114.8 . . ?
C84 C85 H85 114.8 . . ?
C87 C86 C88 107.4(6) . . ?
C87 C86 C80 109.0(6) . . ?
C88 C86 C80 113.0(6) . . ?
C87 C86 C89 107.9(6) . . ?
C88 C86 C89 107.7(6) . . ?
C80 C86 C89 111.7(5) . . ?
C86 C87 H87A 109.5 . . ?
C86 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
C86 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C86 C88 H88A 109.5 . . ?
C86 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C86 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C86 C89 H89A 109.5 . . ?
C86 C89 H89B 109.5 . . ?
H89A C89 H89B 109.5 . . ?
C86 C89 H89C 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C92' C90 C91' 115.7(10) . . ?
C92' C90 C93' 111.7(10) . . ?
C91' C90 C93' 110.7(9) . . ?
C93 C90 C92 113.7(10) . . ?
C93 C90 C91 109.7(9) . . ?
C92 C90 C91 109.4(9) . . ?
C92' C90 C82 107.0(10) . . ?
C91' C90 C82 104.2(8) . . ?
C93 C90 C82 109.9(9) . . ?
C93' C90 C82 106.8(8) . . ?
C92 C90 C82 109.1(8) . . ?
C91 C90 C82 104.6(9) . . ?
C90 C91 H91A 109.5 . . ?
C90 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C90 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
C90 C92 H92A 109.5 . . ?
C90 C92 H92B 109.5 . . ?
H92A C92 H92B 109.5 . . ?
C90 C92 H92C 109.5 . . ?
H92A C92 H92C 109.5 . . ?
H92B C92 H92C 109.5 . . ?
C90 C93 H93A 109.5 . . ?
C90 C93 H93B 109.5 . . ?
H93A C93 H93B 109.5 . . ?
C90 C93 H93C 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
C90 C91' H91D 109.5 . . ?
C90 C91' H91E 109.5 . . ?
H91D C91' H91E 109.5 . . ?
C90 C91' H91F 109.5 . . ?
H91D C91' H91F 109.5 . . ?
H91E C91' H91F 109.5 . . ?
C90 C92' H92D 109.5 . . ?
C90 C92' H92E 109.5 . . ?
H92D C92' H92E 109.5 . . ?
C90 C92' H92F 109.5 . . ?
H92D C92' H92F 109.5 . . ?
H92E C92' H92F 109.5 . . ?
C90 C93' H93D 109.5 . . ?
C90 C93' H93E 109.5 . . ?
H93D C93' H93E 109.5 . . ?
C90 C93' H93F 109.5 . . ?
H93D C93' H93F 109.5 . . ?
H93E C93' H93F 109.5 . . ?
N3 C94 C95 115.1(4) . . ?
N3 C94 H94A 108.5 . . ?
C95 C94 H94A 108.5 . . ?
N3 C94 H94B 108.5 . . ?
C95 C94 H94B 108.5 . . ?
H94A C94 H94B 107.5 . . ?
C96 C95 C100 118.2(5) . . ?
C96 C95 C94 119.1(5) . . ?
C100 C95 C94 122.6(5) . . ?
C97 C96 C95 120.5(6) . . ?
C97 C96 H96 119.8 . . ?
C95 C96 H96 119.8 . . ?
C96 C97 C98 119.7(6) . . ?
C96 C97 H97 120.1 . . ?
C98 C97 H97 120.1 . . ?
C99 C98 C97 121.2(6) . . ?
C99 C98 H98 119.4 . . ?
C97 C98 H98 119.4 . . ?
C98 C99 C100 118.4(5) . . ?
C98 C99 C101 120.4(5) . . ?
C100 C99 C101 121.2(5) . . ?
C99 C100 C95 122.0(5) . . ?
C99 C100 H100 119.0 . . ?
C95 C100 H100 119.0 . . ?
N6 C101 C99 118.0(4) . . ?
N6 C101 H10G 107.8 . . ?
C99 C101 H10G 107.8 . . ?
N6 C101 H10H 107.8 . . ?
C99 C101 H10H 107.8 . . ?
H10G C101 H10H 107.1 . . ?
N6 C102 C103 129.4(5) . . ?
N6 C102 H102 115.3 . . ?
C103 C102 H102 115.3 . . ?
C107 C103 C104 120.0(5) . . ?
C107 C103 C102 124.1(5) . . ?
C104 C103 C102 115.9(5) . . ?
C105 C104 C103 120.7(6) . . ?
C105 C104 H104 119.6 . . ?
C103 C104 H104 119.6 . . ?
C104 C105 C60 117.3(6) . . ?
C104 C105 C108 120.5(7) . . ?
C60 C105 C108 122.1(6) . . ?
C60 C106 C107 116.8(6) . . ?
C60 C106 C112 121.7(5) . . ?
C107 C106 C112 121.4(6) . . ?
O9 C107 C103 118.8(5) . . ?
O9 C107 C106 120.7(5) . . ?
C103 C107 C106 120.5(5) . . ?
C109 C108 C111 108.6(9) . . ?
C109 C108 C110 112.5(10) . . ?
C111 C108 C110 103.9(8) . . ?
C109 C108 C105 113.4(6) . . ?
C111 C108 C105 111.2(7) . . ?
C110 C108 C105 107.0(8) . . ?
C108 C109 H0C 109.5 . . ?
C108 C109 H0D 109.5 . . ?
H0C C109 H0D 109.5 . . ?
C108 C109 H0E 109.5 . . ?
H0C C109 H0E 109.5 . . ?
H0D C109 H0E 109.5 . . ?
C108 C110 H11P 109.5 . . ?
C108 C110 H11Q 109.5 . . ?
H11P C110 H11Q 109.5 . . ?
C108 C110 H11R 109.5 . . ?
H11P C110 H11R 109.5 . . ?
H11Q C110 H11R 109.5 . . ?
C108 C111 H11S 109.5 . . ?
C108 C111 H11T 109.5 . . ?
H11S C111 H11T 109.5 . . ?
C108 C111 H11U 109.5 . . ?
H11S C111 H11U 109.5 . . ?
H11T C111 H11U 109.5 . . ?
C106 C112 C114 111.0(6) . . ?
C106 C112 C115 108.9(6) . . ?
C114 C112 C115 111.5(7) . . ?
C106 C112 C113 109.9(6) . . ?
C114 C112 C113 108.5(7) . . ?
C115 C112 C113 106.9(7) . . ?
C112 C113 H11V 109.5 . . ?
C112 C113 H11W 109.5 . . ?
H11V C113 H11W 109.5 . . ?
C112 C113 H11X 109.5 . . ?
H11V C113 H11X 109.5 . . ?
H11W C113 H11X 109.5 . . ?
C112 C114 H11J 109.5 . . ?
C112 C114 H11K 109.5 . . ?
H11J C114 H11K 109.5 . . ?
C112 C114 H11L 109.5 . . ?
H11J C114 H11L 109.5 . . ?
H11K C114 H11L 109.5 . . ?
C112 C115 H11M 109.5 . . ?
C112 C115 H11N 109.5 . . ?
H11M C115 H11N 109.5 . . ?
C112 C115 H11O 109.5 . . ?
H11M C115 H11O 109.5 . . ?
H11N C115 H11O 109.5 . . ?
O11 C116 C119 103.0(7) . . ?
O11 C116 C117 105.9(7) . . ?
C119 C116 C117 107.6(9) . . ?
O11 C116 C118 106.5(8) . . ?
C119 C116 C118 115.1(9) . . ?
C117 C116 C118 117.4(9) . . ?
C116 C117 H1A' 109.5 . . ?
C116 C117 H1B' 109.5 . . ?
H1A' C117 H1B' 109.5 . . ?
C116 C117 H1C' 109.5 . . ?
H1A' C117 H1C' 109.5 . . ?
H1B' C117 H1C' 109.5 . . ?
C116 C118 H1D' 109.5 . . ?
C116 C118 H1E' 109.5 . . ?
H1D' C118 H1E' 109.5 . . ?
C116 C118 H1F' 109.5 . . ?
H1D' C118 H1F' 109.5 . . ?
H1E' C118 H1F' 109.5 . . ?
C116 C119 H1G' 109.5 . . ?
C116 C119 H1H' 109.5 . . ?
H1G' C119 H1H' 109.5 . . ?
C116 C119 H1I' 109.5 . . ?
H1G' C119 H1I' 109.5 . . ?
H1H' C119 H1I' 109.5 . . ?
O12 C120 C122 112.6(7) . . ?
O12 C120 C121 110.4(7) . . ?
C122 C120 C121 116.9(10) . . ?
O12 C120 C123 106.3(7) . . ?
C122 C120 C123 110.1(11) . . ?
C121 C120 C123 99.3(11) . . ?
C120 C121 H12A 109.5 . . ?
C120 C121 H12B 109.5 . . ?
H12A C121 H12B 109.5 . . ?
C120 C121 H12C 109.5 . . ?
H12A C121 H12C 109.5 . . ?
H12B C121 H12C 109.5 . . ?
C120 C122 H12D 109.5 . . ?
C120 C122 H12E 109.5 . . ?
H12D C122 H12E 109.5 . . ?
C120 C122 H12F 109.5 . . ?
H12D C122 H12F 109.5 . . ?
H12E C122 H12F 109.5 . . ?
C120 C123 H12G 109.5 . . ?
C120 C123 H12H 109.5 . . ?
H12G C123 H12H 109.5 . . ?
C120 C123 H12I 109.5 . . ?
H12G C123 H12I 109.5 . . ?
H12H C123 H12I 109.5 . . ?
O10 C124 C125 120.9(4) . . ?
O10 C124 C129 118.9(4) . . ?
C125 C124 C129 120.2(4) . . ?
C126 C125 C124 116.7(4) . . ?
C126 C125 C131 122.3(5) . . ?
C124 C125 C131 121.0(4) . . ?
C125 C126 C127 125.1(5) . . ?
C125 C126 H126 117.5 . . ?
C127 C126 H126 117.5 . . ?
C128 C127 C126 116.1(4) . . ?
C128 C127 C135 121.7(5) . . ?
C126 C127 C135 122.1(5) . . ?
C127 C128 C129 123.2(5) . . ?
C127 C128 H128 118.4 . . ?
C129 C128 H128 118.4 . . ?
C128 C129 C124 118.6(5) . . ?
C128 C129 C130 118.0(4) . . ?
C124 C129 C130 123.4(4) . . ?
N5 C130 C129 128.6(5) . . ?
N5 C130 H130 115.7 . . ?
C129 C130 H130 115.7 . . ?
C133 C131 C134 109.4(5) . . ?
C133 C131 C132 110.0(5) . . ?
C134 C131 C132 106.9(5) . . ?
C133 C131 C125 109.1(5) . . ?
C134 C131 C125 110.7(4) . . ?
C132 C131 C125 110.7(5) . . ?
C131 C132 H13D 109.5 . . ?
C131 C132 H13E 109.5 . . ?
H13D C132 H13E 109.5 . . ?
C131 C132 H13F 109.5 . . ?
H13D C132 H13F 109.5 . . ?
H13E C132 H13F 109.5 . . ?
C131 C134 H13G 109.5 . . ?
C131 C134 H13H 109.5 . . ?
H13G C134 H13H 109.5 . . ?
C131 C134 H13I 109.5 . . ?
H13G C134 H13I 109.5 . . ?
H13H C134 H13I 109.5 . . ?
C131 C133 H13J 109.5 . . ?
C131 C133 H13K 109.5 . . ?
H13J C133 H13K 109.5 . . ?
C131 C133 H13L 109.5 . . ?
H13J C133 H13L 109.5 . . ?
H13K C133 H13L 109.5 . . ?
C136 C135 C138 110.0(6) . . ?
C136 C135 C137 108.7(7) . . ?
C138 C135 C137 106.7(6) . . ?
C136 C135 C127 112.7(5) . . ?
C138 C135 C127 110.2(5) . . ?
C137 C135 C127 108.3(5) . . ?
C135 C136 H13M 109.5 . . ?
C135 C136 H13N 109.5 . . ?
H13M C136 H13N 109.5 . . ?
C135 C136 H13O 109.5 . . ?
H13M C136 H13O 109.5 . . ?
H13N C136 H13O 109.5 . . ?
C135 C137 H13P 109.5 . . ?
C135 C137 H13Q 109.5 . . ?
H13P C137 H13Q 109.5 . . ?
C135 C137 H13R 109.5 . . ?
H13P C137 H13R 109.5 . . ?
H13Q C137 H13R 109.5 . . ?
C135 C138 H13S 109.5 . . ?
C135 C138 H13T 109.5 . . ?
H13S C138 H13T 109.5 . . ?
C135 C138 H13U 109.5 . . ?
H13S C138 H13U 109.5 . . ?
H13T C138 H13U 109.5 . . ?
C1 N1 C39 119.2(4) . . ?
C1 N1 Hf1 122.5(3) . . ?
C39 N1 Hf1 118.1(3) . . ?
C30 N2 C47 114.7(4) . . ?
C30 N2 Hf1 125.8(3) . . ?
C47 N2 Hf1 118.7(3) . . ?
C85 N3 C94 116.0(5) . . ?
C85 N3 Hf2 125.6(4) . . ?
C94 N3 Hf2 118.1(4) . . ?
C55 N4 C46 113.2(4) . . ?
C55 N4 Hf2 124.7(3) . . ?
C46 N4 Hf2 122.1(3) . . ?
C130 N5 C54 118.4(4) . . ?
C130 N5 Hf3 126.6(3) . . ?
C54 N5 Hf3 114.9(3) . . ?
C102 N6 C101 120.2(5) . . ?
C102 N6 Hf3 123.7(3) . . ?
C101 N6 Hf3 115.7(3) . . ?
C7 O1 Hf1 130.9(3) . . ?
C24 O2 Hf1 143.7(3) . . ?
C20 O3 Hf1 168.6(4) . . ?
C16 O4 Hf1 174.8(4) . . ?
C62 O5 Hf2 144.9(3) . . ?
C79 O6 Hf2 144.9(3) . . ?
C71 O7 Hf2 157.5(4) . . ?
C75 O8 Hf2 165.8(4) . . ?
C107 O9 Hf3 141.5(3) . . ?
C124 O10 Hf3 145.5(3) . . ?
C116 O11 Hf3 165.1(5) . . ?
C120 O12 Hf3 167.2(4) . . ?
O3 Hf1 O4 103.44(15) . . ?
O3 Hf1 O2 99.41(15) . . ?
O4 Hf1 O2 95.21(14) . . ?
O3 Hf1 O1 95.38(15) . . ?
O4 Hf1 O1 96.36(14) . . ?
O2 Hf1 O1 158.55(12) . . ?
O3 Hf1 N1 165.30(15) . . ?
O4 Hf1 N1 89.95(14) . . ?
O2 Hf1 N1 85.16(14) . . ?
O1 Hf1 N1 76.86(13) . . ?
O3 Hf1 N2 86.55(15) . . ?
O4 Hf1 N2 168.29(15) . . ?
O2 Hf1 N2 76.89(13) . . ?
O1 Hf1 N2 88.66(14) . . ?
N1 Hf1 N2 80.87(14) . . ?
O8 Hf2 O7 102.58(16) . . ?
O8 Hf2 O5 94.32(15) . . ?
O7 Hf2 O5 99.02(15) . . ?
O8 Hf2 O6 99.22(15) . . ?
O7 Hf2 O6 96.39(15) . . ?
O5 Hf2 O6 156.74(14) . . ?
O8 Hf2 N4 164.96(14) . . ?
O7 Hf2 N4 91.29(14) . . ?
O5 Hf2 N4 77.58(13) . . ?
O6 Hf2 N4 84.78(14) . . ?
O8 Hf2 N3 86.19(15) . . ?
O7 Hf2 N3 169.56(15) . . ?
O5 Hf2 N3 85.78(15) . . ?
O6 Hf2 N3 76.40(15) . . ?
N4 Hf2 N3 80.64(13) . . ?
O11 Hf3 O12 105.89(19) . . ?
O11 Hf3 O9 93.15(16) . . ?
O12 Hf3 O9 97.45(16) . . ?
O11 Hf3 O10 98.57(16) . . ?
O12 Hf3 O10 94.98(15) . . ?
O9 Hf3 O10 159.91(13) . . ?
O11 Hf3 N5 90.38(17) . . ?
O12 Hf3 N5 162.83(17) . . ?
O9 Hf3 N5 86.88(14) . . ?
O10 Hf3 N5 76.83(13) . . ?
O11 Hf3 N6 165.28(17) . . ?
O12 Hf3 N6 86.73(16) . . ?
O9 Hf3 N6 77.43(14) . . ?
O10 Hf3 N6 87.61(14) . . ?
N5 Hf3 N6 77.97(14) . . ?

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
N1 C1 C2 C3 -164.8(5) . . . . ?
N1 C1 C2 C7 17.7(8) . . . . ?
C7 C2 C3 C4 -1.4(8) . . . . ?
C1 C2 C3 C4 -179.0(5) . . . . ?
C2 C3 C4 C5 2.4(8) . . . . ?
C2 C3 C4 C8 -176.9(6) . . . . ?
C3 C4 C5 C6 -0.2(9) . . . . ?
C8 C4 C5 C6 179.1(6) . . . . ?
C4 C5 C6 C7 -2.8(9) . . . . ?
C4 C5 C6 C12 179.8(6) . . . . ?
C3 C2 C7 O1 178.5(5) . . . . ?
C1 C2 C7 O1 -4.0(7) . . . . ?
C3 C2 C7 C6 -1.7(7) . . . . ?
C1 C2 C7 C6 175.7(4) . . . . ?
C5 C6 C7 O1 -176.5(5) . . . . ?
C12 C6 C7 O1 0.9(8) . . . . ?
C5 C6 C7 C2 3.7(7) . . . . ?
C12 C6 C7 C2 -178.8(5) . . . . ?
C3 C4 C8 C9' -36.1(19) . . . . ?
C5 C4 C8 C9' 144.7(17) . . . . ?
C3 C4 C8 C9 -5.0(11) . . . . ?
C5 C4 C8 C9 175.7(8) . . . . ?
C3 C4 C8 C10' 174.3(18) . . . . ?
C5 C4 C8 C10' -5.0(19) . . . . ?
C3 C4 C8 C11 117.9(11) . . . . ?
C5 C4 C8 C11 -61.3(12) . . . . ?
C3 C4 C8 C11' 70.7(16) . . . . ?
C5 C4 C8 C11' -108.5(16) . . . . ?
C3 C4 C8 C10 -122.5(8) . . . . ?
C5 C4 C8 C10 58.3(9) . . . . ?
C5 C6 C12 C14 111.7(7) . . . . ?
C7 C6 C12 C14 -65.6(7) . . . . ?
C5 C6 C12 C15 -123.7(6) . . . . ?
C7 C6 C12 C15 59.0(7) . . . . ?
C5 C6 C12 C13 -5.3(9) . . . . ?
C7 C6 C12 C13 177.4(5) . . . . ?
O2 C24 C25 C26 179.3(5) . . . . ?
C29 C24 C25 C26 -0.5(8) . . . . ?
O2 C24 C25 C31 -2.6(8) . . . . ?
C29 C24 C25 C31 177.6(5) . . . . ?
C24 C25 C26 C27 -1.7(9) . . . . ?
C31 C25 C26 C27 -179.8(6) . . . . ?
C25 C26 C27 C28 3.5(10) . . . . ?
C25 C26 C27 C35 179.1(6) . . . . ?
C26 C27 C28 C29 -3.1(9) . . . . ?
C35 C27 C28 C29 -178.8(6) . . . . ?
O2 C24 C29 C28 -179.0(5) . . . . ?
C25 C24 C29 C28 0.9(8) . . . . ?
O2 C24 C29 C30 2.0(8) . . . . ?
C25 C24 C29 C30 -178.2(5) . . . . ?
C27 C28 C29 C24 1.0(9) . . . . ?
C27 C28 C29 C30 -179.9(6) . . . . ?
C24 C29 C30 N2 -1.9(9) . . . . ?
C28 C29 C30 N2 179.0(6) . . . . ?
C26 C25 C31 C32 -118.5(6) . . . . ?
C24 C25 C31 C32 63.3(8) . . . . ?
C26 C25 C31 C33 119.9(6) . . . . ?
C24 C25 C31 C33 -58.2(7) . . . . ?
C26 C25 C31 C34 1.1(9) . . . . ?
C24 C25 C31 C34 -177.0(6) . . . . ?
C28 C27 C35 C38 -59.8(10) . . . . ?
C26 C27 C35 C38 124.7(9) . . . . ?
C28 C27 C35 C36 175.8(8) . . . . ?
C26 C27 C35 C36 0.4(10) . . . . ?
C28 C27 C35 C37' 111.1(14) . . . . ?
C26 C27 C35 C37' -64.3(14) . . . . ?
C28 C27 C35 C38' -11.0(15) . . . . ?
C26 C27 C35 C38' 173.5(14) . . . . ?
C28 C27 C35 C36' -128.6(13) . . . . ?
C26 C27 C35 C36' 56.0(14) . . . . ?
C28 C27 C35 C37 59.2(9) . . . . ?
C26 C27 C35 C37 -116.3(9) . . . . ?
N1 C39 C40 C41 -98.9(6) . . . . ?
N1 C39 C40 C45 83.3(6) . . . . ?
C45 C40 C41 C42 1.3(8) . . . . ?
C39 C40 C41 C42 -176.5(5) . . . . ?
C40 C41 C42 C43 -0.1(9) . . . . ?
C41 C42 C43 C44 -0.4(9) . . . . ?
C42 C43 C44 C45 -0.2(8) . . . . ?
C42 C43 C44 C46 179.5(5) . . . . ?
C41 C40 C45 C44 -1.9(7) . . . . ?
C39 C40 C45 C44 175.9(4) . . . . ?
C43 C44 C45 C40 1.3(7) . . . . ?
C46 C44 C45 C40 -178.3(4) . . . . ?
C43 C44 C46 N4 -15.6(7) . . . . ?
C45 C44 C46 N4 164.1(4) . . . . ?
N2 C47 C48 C49 91.7(6) . . . . ?
N2 C47 C48 C53 -88.8(5) . . . . ?
C53 C48 C49 C50 2.2(8) . . . . ?
C47 C48 C49 C50 -178.4(5) . . . . ?
C48 C49 C50 C51 -1.3(8) . . . . ?
C49 C50 C51 C52 -0.7(9) . . . . ?
C50 C51 C52 C53 1.7(8) . . . . ?
C50 C51 C52 C54 -175.3(5) . . . . ?
C51 C52 C53 C48 -0.8(8) . . . . ?
C54 C52 C53 C48 176.2(5) . . . . ?
C49 C48 C53 C52 -1.2(8) . . . . ?
C47 C48 C53 C52 179.4(5) . . . . ?
C51 C52 C54 N5 -112.6(6) . . . . ?
C53 C52 C54 N5 70.4(8) . . . . ?
N4 C55 C56 C62 -0.3(8) . . . . ?
N4 C55 C56 C57 180.0(5) . . . . ?
C62 C56 C57 C58 -0.8(8) . . . . ?
C55 C56 C57 C58 178.9(5) . . . . ?
C56 C57 C58 C59 -1.9(8) . . . . ?
C56 C57 C58 C63 179.0(5) . . . . ?
C57 C58 C59 C61 2.9(9) . . . . ?
C63 C58 C59 C61 -178.0(6) . . . . ?
C58 C59 C61 C62 -1.1(9) . . . . ?
C58 C59 C61 C67 -178.9(6) . . . . ?
C57 C56 C62 O5 -176.2(4) . . . . ?
C55 C56 C62 O5 4.1(7) . . . . ?
C57 C56 C62 C61 2.6(7) . . . . ?
C55 C56 C62 C61 -177.1(4) . . . . ?
C59 C61 C62 O5 177.1(5) . . . . ?
C67 C61 C62 O5 -5.1(8) . . . . ?
C59 C61 C62 C56 -1.7(7) . . . . ?
C67 C61 C62 C56 176.1(5) . . . . ?
C57 C58 C63 C64 7.8(10) . . . . ?
C59 C58 C63 C64 -171.3(7) . . . . ?
C57 C58 C63 C65 -116.0(7) . . . . ?
C59 C58 C63 C65 64.9(9) . . . . ?
C57 C58 C63 C66 128.8(6) . . . . ?
C59 C58 C63 C66 -50.3(8) . . . . ?
C59 C61 C67 C68 -120.0(7) . . . . ?
C62 C61 C67 C68 62.3(8) . . . . ?
C59 C61 C67 C70 -0.2(9) . . . . ?
C62 C61 C67 C70 -177.9(6) . . . . ?
C59 C61 C67 C69 120.4(7) . . . . ?
C62 C61 C67 C69 -57.3(8) . . . . ?
O6 C79 C80 C81 176.3(5) . . . . ?
C84 C79 C80 C81 -4.6(8) . . . . ?
O6 C79 C80 C86 -3.7(9) . . . . ?
C84 C79 C80 C86 175.4(5) . . . . ?
C79 C80 C81 C82 2.3(10) . . . . ?
C86 C80 C81 C82 -177.7(6) . . . . ?
C80 C81 C82 C83 0.7(10) . . . . ?
C80 C81 C82 C90 -179.1(6) . . . . ?
C81 C82 C83 C84 -1.3(9) . . . . ?
C90 C82 C83 C84 178.6(6) . . . . ?
C82 C83 C84 C79 -1.2(9) . . . . ?
C82 C83 C84 C85 176.6(5) . . . . ?
O6 C79 C84 C83 -176.6(5) . . . . ?
C80 C79 C84 C83 4.2(8) . . . . ?
O6 C79 C84 C85 5.7(8) . . . . ?
C80 C79 C84 C85 -173.5(5) . . . . ?
C83 C84 C85 N3 172.8(6) . . . . ?
C79 C84 C85 N3 -9.4(9) . . . . ?
C79 C80 C86 C87 -59.5(8) . . . . ?
C81 C80 C86 C87 120.5(7) . . . . ?
C79 C80 C86 C88 -178.8(6) . . . . ?
C81 C80 C86 C88 1.2(9) . . . . ?
C79 C80 C86 C89 59.6(8) . . . . ?
C81 C80 C86 C89 -120.4(6) . . . . ?
C83 C82 C90 C92' -167.0(13) . . . . ?
C81 C82 C90 C92' 12.9(15) . . . . ?
C83 C82 C90 C91' 70.0(13) . . . . ?
C81 C82 C90 C91' -110.2(12) . . . . ?
C83 C82 C90 C93 4.2(14) . . . . ?
C81 C82 C90 C93 -176.0(13) . . . . ?
C83 C82 C90 C93' -47.2(13) . . . . ?
C81 C82 C90 C93' 132.6(12) . . . . ?
C83 C82 C90 C92 -121.2(12) . . . . ?
C81 C82 C90 C92 58.7(13) . . . . ?
C83 C82 C90 C91 121.8(12) . . . . ?
C81 C82 C90 C91 -58.3(13) . . . . ?
N3 C94 C95 C96 163.8(5) . . . . ?
N3 C94 C95 C100 -19.0(7) . . . . ?
C100 C95 C96 C97 -2.3(9) . . . . ?
C94 C95 C96 C97 175.1(6) . . . . ?
C95 C96 C97 C98 0.7(10) . . . . ?
C96 C97 C98 C99 0.5(11) . . . . ?
C97 C98 C99 C100 0.1(9) . . . . ?
C97 C98 C99 C101 -179.7(6) . . . . ?
C98 C99 C100 C95 -1.8(8) . . . . ?
C101 C99 C100 C95 178.0(5) . . . . ?
C96 C95 C100 C99 2.9(8) . . . . ?
C94 C95 C100 C99 -174.4(5) . . . . ?
C98 C99 C101 N6 111.8(6) . . . . ?
C100 C99 C101 N6 -67.9(7) . . . . ?
N6 C102 C103 C107 -2.9(9) . . . . ?
N6 C102 C103 C104 176.7(5) . . . . ?
C107 C103 C104 C105 0.3(9) . . . . ?
C102 C103 C104 C105 -179.2(6) . . . . ?
C103 C104 C105 C60 -0.4(10) . . . . ?
C103 C104 C105 C108 176.6(6) . . . . ?
C106 C60 C105 C104 -0.6(11) . . . . ?
C106 C60 C105 C108 -177.6(7) . . . . ?
C105 C60 C106 C107 1.7(10) . . . . ?
C105 C60 C106 C112 178.5(7) . . . . ?
C104 C103 C107 O9 -179.6(5) . . . . ?
C102 C103 C107 O9 -0.1(8) . . . . ?
C104 C103 C107 C106 0.8(8) . . . . ?
C102 C103 C107 C106 -179.7(5) . . . . ?
C60 C106 C107 O9 178.7(5) . . . . ?
C112 C106 C107 O9 1.9(9) . . . . ?
C60 C106 C107 C103 -1.7(9) . . . . ?
C112 C106 C107 C103 -178.5(6) . . . . ?
C104 C105 C108 C109 22.5(13) . . . . ?
C60 C105 C108 C109 -160.7(10) . . . . ?
C104 C105 C108 C111 145.1(9) . . . . ?
C60 C105 C108 C111 -38.0(12) . . . . ?
C104 C105 C108 C110 -102.1(10) . . . . ?
C60 C105 C108 C110 74.8(11) . . . . ?
C60 C106 C112 C114 -115.2(7) . . . . ?
C107 C106 C112 C114 61.4(8) . . . . ?
C60 C106 C112 C115 121.6(7) . . . . ?
C107 C106 C112 C115 -61.7(9) . . . . ?
C60 C106 C112 C113 4.8(10) . . . . ?
C107 C106 C112 C113 -178.5(7) . . . . ?
O10 C124 C125 C126 -177.0(5) . . . . ?
C129 C124 C125 C126 2.8(7) . . . . ?
O10 C124 C125 C131 3.8(8) . . . . ?
C129 C124 C125 C131 -176.4(5) . . . . ?
C124 C125 C126 C127 -2.4(8) . . . . ?
C131 C125 C126 C127 176.8(5) . . . . ?
C125 C126 C127 C128 0.4(9) . . . . ?
C125 C126 C127 C135 179.6(5) . . . . ?
C126 C127 C128 C129 1.4(8) . . . . ?
C135 C127 C128 C129 -177.8(5) . . . . ?
C127 C128 C129 C124 -1.0(8) . . . . ?
C127 C128 C129 C130 179.7(5) . . . . ?
O10 C124 C129 C128 178.5(5) . . . . ?
C125 C124 C129 C128 -1.2(8) . . . . ?
O10 C124 C129 C130 -2.1(8) . . . . ?
C125 C124 C129 C130 178.1(5) . . . . ?
C128 C129 C130 N5 -178.9(6) . . . . ?
C124 C129 C130 N5 1.8(9) . . . . ?
C126 C125 C131 C133 -120.6(6) . . . . ?
C124 C125 C131 C133 58.5(7) . . . . ?
C126 C125 C131 C134 -0.2(8) . . . . ?
C124 C125 C131 C134 179.0(5) . . . . ?
C126 C125 C131 C132 118.2(6) . . . . ?
C124 C125 C131 C132 -62.7(7) . . . . ?
C128 C127 C135 C136 -171.6(7) . . . . ?
C126 C127 C135 C136 9.2(9) . . . . ?
C128 C127 C135 C138 -48.4(8) . . . . ?
C126 C127 C135 C138 132.5(6) . . . . ?
C128 C127 C135 C137 68.0(8) . . . . ?
C126 C127 C135 C137 -111.2(7) . . . . ?
C2 C1 N1 C39 -177.5(5) . . . . ?
C2 C1 N1 Hf1 7.8(7) . . . . ?
C40 C39 N1 C1 6.4(7) . . . . ?
C40 C39 N1 Hf1 -178.7(3) . . . . ?
C29 C30 N2 C47 178.5(5) . . . . ?
C29 C30 N2 Hf1 8.9(8) . . . . ?
C48 C47 N2 C30 84.2(6) . . . . ?
C48 C47 N2 Hf1 -105.4(4) . . . . ?
C84 C85 N3 C94 177.9(5) . . . . ?
C84 C85 N3 Hf2 4.3(8) . . . . ?
C95 C94 N3 C85 85.8(6) . . . . ?
C95 C94 N3 Hf2 -100.2(5) . . . . ?
C56 C55 N4 C46 176.7(5) . . . . ?
C56 C55 N4 Hf2 -2.7(7) . . . . ?
C44 C46 N4 C55 -76.5(5) . . . . ?
C44 C46 N4 Hf2 102.9(4) . . . . ?
C129 C130 N5 C54 178.1(6) . . . . ?
C129 C130 N5 Hf3 -2.2(8) . . . . ?
C52 C54 N5 C130 16.6(9) . . . . ?
C52 C54 N5 Hf3 -163.1(5) . . . . ?
C103 C102 N6 C101 178.1(5) . . . . ?
C103 C102 N6 Hf3 -10.2(7) . . . . ?
C99 C101 N6 C102 0.3(7) . . . . ?
C99 C101 N6 Hf3 -172.0(4) . . . . ?
C2 C7 O1 Hf1 -42.3(6) . . . . ?
C6 C7 O1 Hf1 137.9(4) . . . . ?
C29 C24 O2 Hf1 -14.3(9) . . . . ?
C25 C24 O2 Hf1 165.9(4) . . . . ?
C23 C20 O3 Hf1 27(3) . . . . ?
C21' C20 O3 Hf1 86(2) . . . . ?
C23' C20 O3 Hf1 -142(2) . . . . ?
C22' C20 O3 Hf1 -29(3) . . . . ?
C22 C20 O3 Hf1 -92(2) . . . . ?
C21 C20 O3 Hf1 156(2) . . . . ?
C56 C62 O5 Hf2 -5.8(9) . . . . ?
C61 C62 O5 Hf2 175.4(4) . . . . ?
C80 C79 O6 Hf2 -176.7(4) . . . . ?
C84 C79 O6 Hf2 4.1(9) . . . . ?
C72 C71 O7 Hf2 115.7(11) . . . . ?
C74 C71 O7 Hf2 -128.9(11) . . . . ?
C73 C71 O7 Hf2 -1.1(16) . . . . ?
C78 C75 O8 Hf2 83.8(17) . . . . ?
C77 C75 O8 Hf2 -37.5(19) . . . . ?
C76 C75 O8 Hf2 -156.3(14) . . . . ?
C103 C107 O9 Hf3 24.2(8) . . . . ?
C106 C107 O9 Hf3 -156.2(4) . . . . ?
C125 C124 O10 Hf3 -175.7(4) . . . . ?
C129 C124 O10 Hf3 4.6(9) . . . . ?
C119 C116 O11 Hf3 -171.7(18) . . . . ?
C117 C116 O11 Hf3 -59(2) . . . . ?
C118 C116 O11 Hf3 67(2) . . . . ?
C122 C120 O12 Hf3 18(3) . . . . ?
C121 C120 O12 Hf3 150(2) . . . . ?
C123 C120 O12 Hf3 -103(3) . . . . ?

_refine_diff_density_max         1.103
_refine_diff_density_min         -0.803
_refine_diff_density_rms         0.096

_shelxl_version_number           2012-9

_vrf_PLAT222_7                   
;
PROBLEM: Large Non-Solvent  H     Uiso(max)/Uiso(min) ...       10.0 Ratio 
RESPONSE: The error is expected. This is due to the disorder in the 
tertiary-butyl moiety
;




