# 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. 
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#######################################################################

data_new_sq
_database_code_depnum_ccdc_archive 'CCDC 936922'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-07-28 downloaded from the CCDC.
;
_audit_creation_date             2015-07-06
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2015.06.29 svn.r3191 for OlexSys, GUI svn.r3563)
;
_chemical_name_common            ?
_chemical_name_systematic        Hf
_chemical_formula_moiety         'C86 H88 Hf N4 O6'
_chemical_formula_sum            'C86 H88 Hf N4 O6 '
_chemical_formula_weight         1452.09
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   17.1654(6)
_cell_length_b                   20.7645(6)
_cell_length_c                   25.2494(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8999.7(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_shelx_estimated_absorpt_T_max   0.794
_shelx_estimated_absorpt_T_min   0.677
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Block
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27976
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.539
_diffrn_ambient_temperature      298.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD Area Detector'
_diffrn_measurement_method       ' Phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7211
_reflns_number_total             7909
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

The solvent used to grow the crystal was a toulene, but the resulting 
electron density was uninter-pretable. A region of disordered electron 
density, most probably disordered solvent molecules, occupying voids 
of ca 2524 Å3 for an electron count of 337, was treated using the 
SQUEEZE routine in PLATON [Spek (2009). Acta Cryst. D65, 148-155]. 
Their formula mass and unit-cell characteristics were not taken into 
account during refinement. 
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 
;
 Flack x determined using 3110 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     429
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0239
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0271P)²+0.8619P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0602
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Rigid body (RIGU) restrains
 C24, C1, C2, C6, O1, C3, C7, C5, C25, Hf1, H3, C4, H7A, H7B, N2, H5, H25A,
 H25B, N1, O3, C43, C8, C11, C26, C29, C30, H43A, H43B, H43C, H8A, H8B, C9, C10,
  H11, C12, H26A, H26B, C27, C28, H29, C31, C37, H9A, H9B, H10A, H10B, C13, C19,
  O2, H27A, H27B, H28A, H28B, C32, C36, C38, C42, C14, C18, C20, H2, H32, C33,
 C35, H36, H38, C39, C41, H42, H14, C15, C17, H18, H20, C21, C23, H24, H33, C34,
  H35, H39, C40, H41, H15, C16, H17, H21, C22, H23, H34, H40, H16, H22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C11(H11), C29(H29)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
3.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C)
3.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6056(3) 0.0229(2) 0.92019(15) 0.0463(11) Uani 1 1 d . U . . .
C2 C 0.6663(2) -0.0051(3) 0.89092(16) 0.0573(10) Uani 1 1 d . U . . .
C3 C 0.7191(4) 0.0369(3) 0.8661(2) 0.0820(18) Uani 1 1 d . U . . .
H3 H 0.7595 0.0188 0.8466 0.098 Uiso 1 1 calc R U . . .
C4 C 0.7149(4) 0.1034(3) 0.8687(3) 0.091(2) Uani 1 1 d . U . . .
C5 C 0.6522(3) 0.1283(3) 0.8951(2) 0.0662(14) Uani 1 1 d . U . . .
H5 H 0.6457 0.1728 0.8957 0.079 Uiso 1 1 calc R U . . .
C6 C 0.5981(3) 0.0904(2) 0.92069(16) 0.0473(10) Uani 1 1 d . U . . .
C7 C 0.6702(3) -0.0773(3) 0.8855(2) 0.0659(14) Uani 1 1 d . U . . .
H7A H 0.6201 -0.0946 0.8962 0.079 Uiso 1 1 calc R U . . .
H7B H 0.6770 -0.0873 0.8483 0.079 Uiso 1 1 calc R U . . .
C8 C 0.7315(4) -0.0937(3) 0.9712(2) 0.092(2) Uani 1 1 d . U . . .
H8A H 0.7223 -0.0479 0.9755 0.110 Uiso 1 1 calc R U . . .
H8B H 0.6916 -0.1171 0.9904 0.110 Uiso 1 1 calc R U . . .
C9 C 0.8089(5) -0.1110(4) 0.9904(3) 0.123(3) Uani 1 1 d . U . . .
H9A H 0.8089 -0.1547 1.0041 0.147 Uiso 1 1 calc R U . . .
H9B H 0.8249 -0.0821 1.0185 0.147 Uiso 1 1 calc R U . . .
C10 C 0.8628(4) -0.1055(3) 0.9440(2) 0.0839(17) Uani 1 1 d . U . . .
H10A H 0.9004 -0.1404 0.9441 0.101 Uiso 1 1 calc R U . . .
H10B H 0.8908 -0.0649 0.9450 0.101 Uiso 1 1 calc R U . . .
C11 C 0.8114(3) -0.1090(2) 0.89536(19) 0.0569(12) Uani 1 1 d . U . . .
H11 H 0.8188 -0.0704 0.8737 0.068 Uiso 1 1 calc R U . . .
C12 C 0.8252(3) -0.1702(2) 0.8611(2) 0.0576(12) Uani 1 1 d . U . . .
C13 C 0.9109(3) -0.1801(2) 0.84645(17) 0.0566(11) Uani 1 1 d . U . . .
C14 C 0.9405(3) -0.2419(3) 0.8416(2) 0.0682(14) Uani 1 1 d . U . . .
H14 H 0.9087 -0.2769 0.8493 0.082 Uiso 1 1 calc R U . . .
C15 C 1.0154(4) -0.2523(3) 0.8256(2) 0.0792(17) Uani 1 1 d . U . . .
H15 H 1.0342 -0.2942 0.8236 0.095 Uiso 1 1 calc R U . . .
C16 C 1.0620(4) -0.2033(3) 0.8128(2) 0.0838(17) Uani 1 1 d . U . . .
H16 H 1.1126 -0.2112 0.8013 0.101 Uiso 1 1 calc R U . . .
C17 C 1.0352(4) -0.1411(3) 0.8167(2) 0.0810(16) Uani 1 1 d . U . . .
H17 H 1.0673 -0.1067 0.8078 0.097 Uiso 1 1 calc R U . . .
C18 C 0.9598(3) -0.1303(3) 0.8340(2) 0.0710(14) Uani 1 1 d . U . . .
H18 H 0.9419 -0.0882 0.8373 0.085 Uiso 1 1 calc R U . . .
C19 C 0.7784(3) -0.1691(3) 0.8091(2) 0.0753(16) Uani 1 1 d . U . . .
C20 C 0.7262(4) -0.2161(4) 0.7967(4) 0.115(3) Uani 1 1 d . U . . .
H20 H 0.7177 -0.2492 0.8209 0.137 Uiso 1 1 calc R U . . .
C21 C 0.6855(7) -0.2164(6) 0.7497(5) 0.160(4) Uani 1 1 d . U . . .
H21 H 0.6491 -0.2483 0.7425 0.191 Uiso 1 1 calc R U . . .
C22 C 0.6999(7) -0.1696(7) 0.7148(5) 0.160(4) Uani 1 1 d . U . . .
H22 H 0.6747 -0.1710 0.6822 0.192 Uiso 1 1 calc R U . . .
C23 C 0.7492(5) -0.1203(6) 0.7245(3) 0.137(3) Uani 1 1 d . U . . .
H23 H 0.7557 -0.0874 0.6999 0.165 Uiso 1 1 calc R U . . .
C24 C 0.7900(4) -0.1197(4) 0.7721(2) 0.0943(19) Uani 1 1 d . U . . .
H24 H 0.8250 -0.0866 0.7793 0.113 Uiso 1 1 calc R U . . .
C25 C 0.5305(3) 0.1209(2) 0.94870(17) 0.0474(10) Uani 1 1 d . U . . .
H25A H 0.5419 0.1225 0.9863 0.057 Uiso 1 1 calc R U . . .
H25B H 0.5252 0.1649 0.9363 0.057 Uiso 1 1 calc R U . . .
C26 C 0.4410(3) 0.0723(2) 0.88366(16) 0.0528(12) Uani 1 1 d . U . . .
H26A H 0.4674 0.0330 0.8735 0.063 Uiso 1 1 calc R U . . .
H26B H 0.4598 0.1072 0.8615 0.063 Uiso 1 1 calc R U . . .
C27 C 0.3540(3) 0.0648(3) 0.87791(19) 0.0684(14) Uani 1 1 d . U . . .
H27A H 0.3402 0.0198 0.8734 0.082 Uiso 1 1 calc R U . . .
H27B H 0.3352 0.0888 0.8475 0.082 Uiso 1 1 calc R U . . .
C28 C 0.3193(3) 0.0913(3) 0.92864(19) 0.0572(12) Uani 1 1 d . U . . .
H28A H 0.2989 0.0567 0.9504 0.069 Uiso 1 1 calc R U . . .
H28B H 0.2775 0.1213 0.9209 0.069 Uiso 1 1 calc R U . . .
C29 C 0.3860(3) 0.1252(2) 0.95651(19) 0.0491(13) Uani 1 1 d . U . . .
H29 H 0.3909 0.1694 0.9432 0.059 Uiso 1 1 calc R U . . .
C30 C 0.3779(3) 0.1257(2) 1.01872(18) 0.0443(12) Uani 1 1 d . U . . .
C31 C 0.2925(3) 0.1410(2) 1.03298(18) 0.0527(12) Uani 1 1 d . U . . .
C32 C 0.2505(3) 0.1009(3) 1.0645(2) 0.0701(15) Uani 1 1 d . U . . .
H32 H 0.2733 0.0637 1.0780 0.084 Uiso 1 1 calc R U . . .
C33 C 0.1723(4) 0.1158(4) 1.0770(3) 0.097(2) Uani 1 1 d . U . . .
H33 H 0.1434 0.0883 1.0984 0.117 Uiso 1 1 calc R U . . .
C34 C 0.1394(4) 0.1704(4) 1.0575(3) 0.0908(19) Uani 1 1 d . U . . .
H34 H 0.0883 0.1808 1.0664 0.109 Uiso 1 1 calc R U . . .
C35 C 0.1804(4) 0.2096(3) 1.0253(2) 0.0892(19) Uani 1 1 d . U . . .
H35 H 0.1569 0.2461 1.0112 0.107 Uiso 1 1 calc R U . . .
C36 C 0.2560(3) 0.1961(3) 1.0135(3) 0.080(2) Uani 1 1 d . U . . .
H36 H 0.2838 0.2242 0.9919 0.097 Uiso 1 1 calc R U . . .
C37 C 0.4299(3) 0.1743(2) 1.04644(19) 0.0552(12) Uani 1 1 d . U . . .
C38 C 0.4426(4) 0.2360(3) 1.0272(2) 0.0786(16) Uani 1 1 d . U . . .
H38 H 0.4194 0.2487 0.9956 0.094 Uiso 1 1 calc R U . . .
C39 C 0.4890(5) 0.2783(3) 1.0542(3) 0.109(2) Uani 1 1 d . U . . .
H39 H 0.4983 0.3190 1.0402 0.131 Uiso 1 1 calc R U . . .
C40 C 0.5213(5) 0.2619(4) 1.1009(4) 0.126(3) Uani 1 1 d . U . . .
H40 H 0.5515 0.2915 1.1193 0.151 Uiso 1 1 calc R U . . .
C41 C 0.5096(5) 0.2013(4) 1.1213(3) 0.113(3) Uani 1 1 d . U . . .
H41 H 0.5321 0.1900 1.1535 0.135 Uiso 1 1 calc R U . . .
C42 C 0.4640(4) 0.1568(3) 1.0941(2) 0.0748(15) Uani 1 1 d . U . . .
H42 H 0.4565 0.1156 1.1077 0.090 Uiso 1 1 calc R U . . .
C43 C 0.7738(6) 0.1461(4) 0.8412(5) 0.166(5) Uani 1 1 d . U . . .
H43A H 0.7590 0.1904 0.8454 0.249 Uiso 1 1 calc GR U . . .
H43B H 0.7755 0.1356 0.8042 0.249 Uiso 1 1 calc GR U . . .
H43C H 0.8244 0.1394 0.8565 0.249 Uiso 1 1 calc GR U . . .
Hf1 Hf 0.46941(2) 0.0000 1.0000 0.03700(8) Uani 1 2 d S TU P . .
N1 N 0.4550(2) 0.08708(15) 0.94095(12) 0.0397(8) Uani 1 1 d . U . . .
N2 N 0.7305(3) -0.1113(2) 0.91512(17) 0.0640(12) Uani 1 1 d . U . . .
O1 O 0.55493(17) -0.01392(12) 0.94589(11) 0.0449(8) Uani 1 1 d . U . . .
O2 O 0.8024(3) -0.22245(17) 0.89315(18) 0.0831(12) Uani 1 1 d . U . . .
H2 H 0.7608 -0.2141 0.9076 0.125 Uiso 1 1 calc GR U . . .
O3 O 0.39667(18) 0.06182(13) 1.03417(10) 0.0436(7) Uani 1 1 d . 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 C2 1.404(6) . ?
C1 C6 1.407(6) . ?
C1 O1 1.327(5) . ?
C2 C3 1.404(7) . ?
C2 C7 1.506(8) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(8) . ?
C4 C5 1.368(8) . ?
C4 C43 1.514(9) . ?
C5 H5 0.9300 . ?
C5 C6 1.379(7) . ?
C6 C25 1.499(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 N2 1.459(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.460(10) . ?
C8 N2 1.462(7) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.498(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.515(7) . ?
C11 H11 0.9800 . ?
C11 C12 1.555(7) . ?
C11 N2 1.476(7) . ?
C12 C13 1.531(7) . ?
C12 C19 1.538(8) . ?
C12 O2 1.410(6) . ?
C13 C14 1.386(6) . ?
C13 C18 1.367(7) . ?
C14 H14 0.9300 . ?
C14 C15 1.365(8) . ?
C15 H15 0.9300 . ?
C15 C16 1.333(8) . ?
C16 H16 0.9300 . ?
C16 C17 1.375(8) . ?
C17 H17 0.9300 . ?
C17 C18 1.384(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.360(9) . ?
C19 C24 1.404(9) . ?
C20 H20 0.9300 . ?
C20 C21 1.377(13) . ?
C21 H21 0.9300 . ?
C21 C22 1.334(16) . ?
C22 H22 0.9300 . ?
C22 C23 1.351(15) . ?
C23 H23 0.9300 . ?
C23 C24 1.391(9) . ?
C24 H24 0.9300 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 N1 1.488(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 C27 1.508(7) . ?
C26 N1 1.498(5) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C27 C28 1.515(7) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 C29 1.517(7) . ?
C29 H29 0.9800 . ?
C29 C30 1.577(7) . ?
C29 N1 1.478(6) . ?
C30 C31 1.543(7) . ?
C30 C37 1.517(7) . ?
C30 O3 1.420(5) . ?
C31 C32 1.359(7) . ?
C31 C36 1.395(7) . ?
C32 H32 0.9300 . ?
C32 C33 1.414(8) . ?
C33 H33 0.9300 . ?
C33 C34 1.360(9) . ?
C34 H34 0.9300 . ?
C34 C35 1.348(9) . ?
C35 H35 0.9300 . ?
C35 C36 1.360(8) . ?
C36 H36 0.9300 . ?
C37 C38 1.387(7) . ?
C37 C42 1.386(7) . ?
C38 H38 0.9300 . ?
C38 C39 1.368(9) . ?
C39 H39 0.9300 . ?
C39 C40 1.347(11) . ?
C40 H40 0.9300 . ?
C40 C41 1.374(11) . ?
C41 H41 0.9300 . ?
C41 C42 1.394(8) . ?
C42 H42 0.9300 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
Hf1 N1 2.357(3) 4_557 ?
Hf1 N1 2.357(3) . ?
Hf1 O1 2.026(3) 4_557 ?
Hf1 O1 2.026(3) . ?
Hf1 O3 1.988(3) 4_557 ?
Hf1 O3 1.988(3) . ?
O2 H2 0.8200 . ?

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
C2 C1 C6 119.0(5) . . ?
O1 C1 C2 120.4(4) . . ?
O1 C1 C6 120.6(4) . . ?
C1 C2 C3 117.2(6) . . ?
C1 C2 C7 119.5(5) . . ?
C3 C2 C7 123.3(4) . . ?
C2 C3 H3 117.8 . . ?
C4 C3 C2 124.3(5) . . ?
C4 C3 H3 117.8 . . ?
C3 C4 C43 121.9(6) . . ?
C5 C4 C3 116.2(5) . . ?
C5 C4 C43 121.9(6) . . ?
C4 C5 H5 118.6 . . ?
C4 C5 C6 122.8(5) . . ?
C6 C5 H5 118.6 . . ?
C1 C6 C25 119.8(4) . . ?
C5 C6 C1 120.2(4) . . ?
C5 C6 C25 120.0(4) . . ?
C2 C7 H7A 107.9 . . ?
C2 C7 H7B 107.9 . . ?
H7A C7 H7B 107.2 . . ?
N2 C7 C2 117.8(5) . . ?
N2 C7 H7A 107.9 . . ?
N2 C7 H7B 107.9 . . ?
H8A C8 H8B 108.7 . . ?
C9 C8 H8A 110.6 . . ?
C9 C8 H8B 110.6 . . ?
C9 C8 N2 105.8(5) . . ?
N2 C8 H8A 110.6 . . ?
N2 C8 H8B 110.6 . . ?
C8 C9 H9A 110.4 . . ?
C8 C9 H9B 110.4 . . ?
C8 C9 C10 106.4(6) . . ?
H9A C9 H9B 108.6 . . ?
C10 C9 H9A 110.4 . . ?
C10 C9 H9B 110.4 . . ?
C9 C10 H10A 110.6 . . ?
C9 C10 H10B 110.6 . . ?
C9 C10 C11 105.7(6) . . ?
H10A C10 H10B 108.7 . . ?
C11 C10 H10A 110.6 . . ?
C11 C10 H10B 110.6 . . ?
C10 C11 H11 109.7 . . ?
C10 C11 C12 113.7(4) . . ?
C12 C11 H11 109.7 . . ?
N2 C11 C10 106.0(4) . . ?
N2 C11 H11 109.7 . . ?
N2 C11 C12 107.8(4) . . ?
C13 C12 C11 113.0(4) . . ?
C13 C12 C19 107.4(4) . . ?
C19 C12 C11 112.6(4) . . ?
O2 C12 C11 105.5(4) . . ?
O2 C12 C13 107.6(4) . . ?
O2 C12 C19 110.8(5) . . ?
C14 C13 C12 119.9(5) . . ?
C18 C13 C12 122.9(4) . . ?
C18 C13 C14 117.0(5) . . ?
C13 C14 H14 119.4 . . ?
C15 C14 C13 121.2(6) . . ?
C15 C14 H14 119.4 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.0(6) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 119.9(6) . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 120.4 . . ?
C16 C17 C18 119.2(6) . . ?
C18 C17 H17 120.4 . . ?
C13 C18 C17 121.6(6) . . ?
C13 C18 H18 119.2 . . ?
C17 C18 H18 119.2 . . ?
C20 C19 C12 122.0(7) . . ?
C20 C19 C24 117.7(7) . . ?
C24 C19 C12 120.3(6) . . ?
C19 C20 H20 118.8 . . ?
C19 C20 C21 122.3(11) . . ?
C21 C20 H20 118.8 . . ?
C20 C21 H21 120.9 . . ?
C22 C21 C20 118.2(13) . . ?
C22 C21 H21 120.9 . . ?
C21 C22 H22 118.4 . . ?
C21 C22 C23 123.2(12) . . ?
C23 C22 H22 118.4 . . ?
C22 C23 H23 120.7 . . ?
C22 C23 C24 118.6(12) . . ?
C24 C23 H23 120.7 . . ?
C19 C24 H24 120.1 . . ?
C23 C24 C19 119.8(9) . . ?
C23 C24 H24 120.1 . . ?
C6 C25 H25A 108.7 . . ?
C6 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
N1 C25 C6 114.3(4) . . ?
N1 C25 H25A 108.7 . . ?
N1 C25 H25B 108.7 . . ?
H26A C26 H26B 108.7 . . ?
C27 C26 H26A 110.6 . . ?
C27 C26 H26B 110.6 . . ?
N1 C26 H26A 110.6 . . ?
N1 C26 H26B 110.6 . . ?
N1 C26 C27 105.9(4) . . ?
C26 C27 H27A 110.6 . . ?
C26 C27 H27B 110.6 . . ?
C26 C27 C28 105.6(4) . . ?
H27A C27 H27B 108.7 . . ?
C28 C27 H27A 110.6 . . ?
C28 C27 H27B 110.6 . . ?
C27 C28 H28A 110.7 . . ?
C27 C28 H28B 110.7 . . ?
C27 C28 C29 105.3(4) . . ?
H28A C28 H28B 108.8 . . ?
C29 C28 H28A 110.7 . . ?
C29 C28 H28B 110.7 . . ?
C28 C29 H29 109.9 . . ?
C28 C29 C30 113.5(4) . . ?
C30 C29 H29 109.9 . . ?
N1 C29 C28 103.4(4) . . ?
N1 C29 H29 109.9 . . ?
N1 C29 C30 109.8(4) . . ?
C31 C30 C29 108.5(4) . . ?
C37 C30 C29 114.4(4) . . ?
C37 C30 C31 108.3(4) . . ?
O3 C30 C29 104.3(4) . . ?
O3 C30 C31 110.0(4) . . ?
O3 C30 C37 111.2(4) . . ?
C32 C31 C30 121.0(4) . . ?
C32 C31 C36 118.1(5) . . ?
C36 C31 C30 120.9(5) . . ?
C31 C32 H32 120.0 . . ?
C31 C32 C33 120.0(5) . . ?
C33 C32 H32 120.0 . . ?
C32 C33 H33 120.1 . . ?
C34 C33 C32 119.7(6) . . ?
C34 C33 H33 120.1 . . ?
C33 C34 H34 119.8 . . ?
C35 C34 C33 120.3(6) . . ?
C35 C34 H34 119.8 . . ?
C34 C35 H35 119.8 . . ?
C34 C35 C36 120.4(6) . . ?
C36 C35 H35 119.8 . . ?
C31 C36 H36 119.3 . . ?
C35 C36 C31 121.4(6) . . ?
C35 C36 H36 119.3 . . ?
C38 C37 C30 123.0(5) . . ?
C42 C37 C30 118.3(5) . . ?
C42 C37 C38 118.7(5) . . ?
C37 C38 H38 119.7 . . ?
C39 C38 C37 120.7(7) . . ?
C39 C38 H38 119.7 . . ?
C38 C39 H39 119.6 . . ?
C40 C39 C38 120.9(7) . . ?
C40 C39 H39 119.6 . . ?
C39 C40 H40 120.0 . . ?
C39 C40 C41 120.1(7) . . ?
C41 C40 H40 120.0 . . ?
C40 C41 H41 119.9 . . ?
C40 C41 C42 120.2(8) . . ?
C42 C41 H41 119.9 . . ?
C37 C42 C41 119.4(6) . . ?
C37 C42 H42 120.3 . . ?
C41 C42 H42 120.3 . . ?
C4 C43 H43A 109.5 . . ?
C4 C43 H43B 109.5 . . ?
C4 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N1 Hf1 N1 167.94(17) . 4_557 ?
O1 Hf1 N1 76.05(11) 4_557 4_557 ?
O1 Hf1 N1 76.05(11) . . ?
O1 Hf1 N1 113.16(12) 4_557 . ?
O1 Hf1 N1 113.16(11) . 4_557 ?
O1 Hf1 O1 87.14(16) 4_557 . ?
O3 Hf1 N1 98.92(11) . 4_557 ?
O3 Hf1 N1 73.33(11) 4_557 4_557 ?
O3 Hf1 N1 98.92(11) 4_557 . ?
O3 Hf1 N1 73.33(11) . . ?
O3 Hf1 O1 94.04(12) . 4_557 ?
O3 Hf1 O1 147.13(10) 4_557 4_557 ?
O3 Hf1 O1 94.03(12) 4_557 . ?
O3 Hf1 O1 147.13(10) . . ?
O3 Hf1 O3 102.17(18) . 4_557 ?
C25 N1 C26 111.3(3) . . ?
C25 N1 Hf1 100.8(2) . . ?
C26 N1 Hf1 118.1(3) . . ?
C29 N1 C25 114.2(3) . . ?
C29 N1 C26 103.7(3) . . ?
C29 N1 Hf1 109.1(3) . . ?
C7 N2 C8 112.5(4) . . ?
C7 N2 C11 118.6(4) . . ?
C8 N2 C11 108.0(5) . . ?
C1 O1 Hf1 136.2(2) . . ?
C12 O2 H2 109.5 . . ?
C30 O3 Hf1 128.8(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 0.0(9) . . . . ?
C1 C2 C7 N2 -107.2(5) . . . . ?
C1 C6 C25 N1 -41.0(5) . . . . ?
C2 C1 C6 C5 -3.4(7) . . . . ?
C2 C1 C6 C25 175.9(4) . . . . ?
C2 C1 O1 Hf1 169.6(3) . . . . ?
C2 C3 C4 C5 -3.8(11) . . . . ?
C2 C3 C4 C43 179.8(8) . . . . ?
C2 C7 N2 C8 51.0(6) . . . . ?
C2 C7 N2 C11 -76.4(6) . . . . ?
C3 C2 C7 N2 75.5(7) . . . . ?
C3 C4 C5 C6 4.0(10) . . . . ?
C4 C5 C6 C1 -0.6(9) . . . . ?
C4 C5 C6 C25 -179.9(6) . . . . ?
C5 C6 C25 N1 138.3(4) . . . . ?
C6 C1 C2 C3 3.6(7) . . . . ?
C6 C1 C2 C7 -173.8(4) . . . . ?
C6 C1 O1 Hf1 -12.1(6) . . . . ?
C6 C25 N1 C26 -48.1(5) . . . . ?
C6 C25 N1 C29 -165.1(3) . . . . ?
C6 C25 N1 Hf1 78.1(3) . . . . ?
C7 C2 C3 C4 177.3(6) . . . . ?
C8 C9 C10 C11 -20.5(8) . . . . ?
C9 C8 N2 C7 -159.3(6) . . . . ?
C9 C8 N2 C11 -26.4(7) . . . . ?
C9 C10 C11 C12 -114.0(6) . . . . ?
C9 C10 C11 N2 4.3(6) . . . . ?
C10 C11 C12 C13 -52.3(6) . . . . ?
C10 C11 C12 C19 -174.1(5) . . . . ?
C10 C11 C12 O2 65.0(6) . . . . ?
C10 C11 N2 C7 142.9(5) . . . . ?
C10 C11 N2 C8 13.4(6) . . . . ?
C11 C12 C13 C14 146.7(5) . . . . ?
C11 C12 C13 C18 -38.1(7) . . . . ?
C11 C12 C19 C20 -121.5(6) . . . . ?
C11 C12 C19 C24 60.1(6) . . . . ?
C12 C11 N2 C7 -94.9(5) . . . . ?
C12 C11 N2 C8 135.6(4) . . . . ?
C12 C13 C14 C15 176.2(5) . . . . ?
C12 C13 C18 C17 -174.5(5) . . . . ?
C12 C19 C20 C21 -178.3(7) . . . . ?
C12 C19 C24 C23 178.0(6) . . . . ?
C13 C12 C19 C20 113.5(6) . . . . ?
C13 C12 C19 C24 -64.9(6) . . . . ?
C13 C14 C15 C16 -1.8(9) . . . . ?
C14 C13 C18 C17 0.7(8) . . . . ?
C14 C15 C16 C17 1.3(9) . . . . ?
C15 C16 C17 C18 0.2(9) . . . . ?
C16 C17 C18 C13 -1.2(9) . . . . ?
C18 C13 C14 C15 0.7(8) . . . . ?
C19 C12 C13 C14 -88.6(6) . . . . ?
C19 C12 C13 C18 86.6(6) . . . . ?
C19 C20 C21 C22 1.8(15) . . . . ?
C20 C19 C24 C23 -0.5(9) . . . . ?
C20 C21 C22 C23 -3.6(18) . . . . ?
C21 C22 C23 C24 3.3(17) . . . . ?
C22 C23 C24 C19 -1.1(12) . . . . ?
C24 C19 C20 C21 0.1(10) . . . . ?
C26 C27 C28 C29 11.2(6) . . . . ?
C27 C26 N1 C25 -157.0(4) . . . . ?
C27 C26 N1 C29 -33.7(5) . . . . ?
C27 C26 N1 Hf1 87.1(4) . . . . ?
C27 C28 C29 C30 -151.0(4) . . . . ?
C27 C28 C29 N1 -32.0(5) . . . . ?
C28 C29 C30 C31 -42.6(6) . . . . ?
C28 C29 C30 C37 -163.6(4) . . . . ?
C28 C29 C30 O3 74.7(5) . . . . ?
C28 C29 N1 C25 161.8(3) . . . . ?
C28 C29 N1 C26 40.4(4) . . . . ?
C28 C29 N1 Hf1 -86.3(3) . . . . ?
C29 C30 C31 C32 124.7(5) . . . . ?
C29 C30 C31 C36 -54.8(6) . . . . ?
C29 C30 C37 C38 40.5(7) . . . . ?
C29 C30 C37 C42 -141.7(5) . . . . ?
C29 C30 O3 Hf1 31.1(5) . . . . ?
C30 C29 N1 C25 -76.7(5) . . . . ?
C30 C29 N1 C26 161.9(4) . . . . ?
C30 C29 N1 Hf1 35.2(5) . . . . ?
C30 C31 C32 C33 -179.9(6) . . . . ?
C30 C31 C36 C35 179.3(6) . . . . ?
C30 C37 C38 C39 178.9(6) . . . . ?
C30 C37 C42 C41 -177.6(5) . . . . ?
C31 C30 C37 C38 -80.7(6) . . . . ?
C31 C30 C37 C42 97.1(5) . . . . ?
C31 C30 O3 Hf1 147.3(3) . . . . ?
C31 C32 C33 C34 -0.3(10) . . . . ?
C32 C31 C36 C35 -0.3(9) . . . . ?
C32 C33 C34 C35 1.6(12) . . . . ?
C33 C34 C35 C36 -2.2(11) . . . . ?
C34 C35 C36 C31 1.6(10) . . . . ?
C36 C31 C32 C33 -0.3(9) . . . . ?
C37 C30 C31 C32 -110.6(5) . . . . ?
C37 C30 C31 C36 69.9(6) . . . . ?
C37 C30 O3 Hf1 -92.7(4) . . . . ?
C37 C38 C39 C40 -2.1(12) . . . . ?
C38 C37 C42 C41 0.3(9) . . . . ?
C38 C39 C40 C41 1.7(14) . . . . ?
C39 C40 C41 C42 -0.3(14) . . . . ?
C40 C41 C42 C37 -0.7(12) . . . . ?
C42 C37 C38 C39 1.1(9) . . . . ?
C43 C4 C5 C6 -179.6(8) . . . . ?
N1 C26 C27 C28 13.5(6) . . . . ?
N1 C29 C30 C31 -157.8(3) . . . . ?
N1 C29 C30 C37 81.1(5) . . . . ?
N1 C29 C30 O3 -40.6(5) . . . . ?
N2 C8 C9 C10 28.9(8) . . . . ?
N2 C11 C12 C13 -169.6(4) . . . . ?
N2 C11 C12 C19 68.6(5) . . . . ?
N2 C11 C12 O2 -52.3(5) . . . . ?
O1 C1 C2 C3 -178.1(4) . . . . ?
O1 C1 C2 C7 4.5(6) . . . . ?
O1 C1 C6 C5 178.3(4) . . . . ?
O1 C1 C6 C25 -2.4(6) . . . . ?
O2 C12 C13 C14 30.7(6) . . . . ?
O2 C12 C13 C18 -154.1(5) . . . . ?
O2 C12 C19 C20 -3.7(7) . . . . ?
O2 C12 C19 C24 177.9(5) . . . . ?
O3 C30 C31 C32 11.2(6) . . . . ?
O3 C30 C31 C36 -168.3(5) . . . . ?
O3 C30 C37 C38 158.3(5) . . . . ?
O3 C30 C37 C42 -23.9(6) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Zr
_database_code_depnum_ccdc_archive 'CCDC 958283'
_audit_update_record             
;
2015-07-20 deposited with the CCDC.
2015-07-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Zr
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C86 H88 N4 O6 Zr'
_chemical_formula_sum            'C86 H88 N4 O6 Zr'
_chemical_formula_weight         1364.82

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      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

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

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

_cell_length_a                   16.9781(12)
_cell_length_b                   20.6006(10)
_cell_length_c                   24.9765(17)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8735.8(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3816
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      22.78

_exptl_crystal_description       Block
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_F_000             2880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.173
_shelx_estimated_absorpt_T_min   0.942
_shelx_estimated_absorpt_T_max   0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(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            13755
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.139
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measured_fraction_theta_full 0.949
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_Laue_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.853
_diffrn_reflns_point_group_measured_fraction_full 0.853
_reflns_number_total             6568
_reflns_number_gt                5419
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.648
_reflns_Friedel_fraction_max     0.738
_reflns_Friedel_fraction_full    0.738

_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 SMART'
_computing_cell_refinement       'Bruker SMART'
_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          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0619P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00013(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1895 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.05(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6568
_refine_ls_number_parameters     426
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0494
_refine_ls_wR_factor_ref         0.1182
_refine_ls_wR_factor_gt          0.1118
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
C12 C 0.7223(2) 0.6673(2) 0.80673(16) 0.0487(17) Uani 1 1 d G . . . .
C13 C 0.7094(3) 0.6175(2) 0.77018(19) 0.0586(19) Uani 1 1 d G . . . .
H13 H 0.6727 0.5841 0.7782 0.070 Uiso 1 1 calc R U . . .
C14 C 0.7501(3) 0.6167(3) 0.72192(17) 0.101(2) Uani 1 1 d G . . . .
H14 H 0.7413 0.5827 0.6969 0.122 Uiso 1 1 calc R U . . .
C15 C 0.8038(3) 0.6656(3) 0.71020(19) 0.115(4) Uani 1 1 d G . . . .
H15 H 0.8316 0.6651 0.6772 0.138 Uiso 1 1 calc R U . . .
C16 C 0.8167(3) 0.7154(3) 0.7468(3) 0.101(2) Uani 1 1 d G . . . .
H16 H 0.8534 0.7488 0.7387 0.122 Uiso 1 1 calc R U . . .
C17 C 0.7760(3) 0.7162(2) 0.7950(2) 0.077(3) Uani 1 1 d G . . . .
H17 H 0.7848 0.7502 0.8200 0.092 Uiso 1 1 calc R U . . .
C1 C 0.7736(4) 0.5934(3) 0.9706(2) 0.059(2) Uani 1 1 d . . . . .
H1A H 0.8146 0.6183 0.9899 0.070 Uiso 1 1 calc R U . . .
H1B H 0.7842 0.5465 0.9751 0.070 Uiso 1 1 calc R U . . .
C2 C 0.6951(5) 0.6098(5) 0.9909(3) 0.091(3) Uani 1 1 d . . . . .
H2A H 0.6942 0.6549 1.0045 0.110 Uiso 1 1 calc R U . . .
H2B H 0.6801 0.5802 1.0204 0.110 Uiso 1 1 calc R U . . .
C3 C 0.6390(4) 0.6026(3) 0.9445(2) 0.0543(18) Uani 1 1 d . . . . .
H3A H 0.5991 0.6376 0.9448 0.065 Uiso 1 1 calc R U . . .
H3B H 0.6117 0.5601 0.9460 0.065 Uiso 1 1 calc R U . . .
C4 C 0.6910(3) 0.6072(3) 0.8940(2) 0.0366(14) Uani 1 1 d . . . . .
H4 H 0.6841 0.5675 0.8715 0.044 Uiso 1 1 calc R U . . .
C5 C 0.6757(3) 0.6687(3) 0.8599(2) 0.0331(13) Uani 1 1 d . . . . .
C6 C 0.5899(3) 0.6785(3) 0.8457(2) 0.0370(14) Uani 1 1 d . . . . .
C7 C 0.5593(4) 0.7412(3) 0.8411(2) 0.0434(16) Uani 1 1 d . . . . .
H7 H 0.5918 0.7772 0.8497 0.052 Uiso 1 1 calc R U . . .
C8 C 0.4829(4) 0.7518(3) 0.8244(2) 0.0486(17) Uani 1 1 d . . . . .
H8 H 0.4626 0.7947 0.8223 0.058 Uiso 1 1 calc R U . . .
C9 C 0.4369(4) 0.7000(4) 0.8109(2) 0.0524(17) Uani 1 1 d . . . . .
H9 H 0.3846 0.7072 0.7986 0.063 Uiso 1 1 calc R U . . .
C10 C 0.4649(4) 0.6381(3) 0.8148(2) 0.0488(15) Uani 1 1 d . . . . .
H10 H 0.4322 0.6025 0.8054 0.059 Uiso 1 1 calc R U . . .
C11 C 0.5399(4) 0.6277(3) 0.8321(2) 0.0451(15) Uani 1 1 d . . . . .
H11 H 0.5586 0.5844 0.8351 0.054 Uiso 1 1 calc R U . . .
C18 C 0.8330(4) 0.5765(3) 0.8830(2) 0.0433(15) Uani 1 1 d . . . . .
H18A H 0.8850 0.5945 0.8929 0.052 Uiso 1 1 calc R U . . .
H18B H 0.8243 0.5865 0.8447 0.052 Uiso 1 1 calc R U . . .
C19 C 0.8368(3) 0.5034(3) 0.88902(18) 0.0372(12) Uani 1 1 d . . . . .
C20 C 0.7829(4) 0.4620(3) 0.8643(3) 0.0535(19) Uani 1 1 d . . . . .
H20 H 0.7409 0.4809 0.8445 0.064 Uiso 1 1 calc R U . . .
C21 C 0.7872(4) 0.3953(3) 0.8669(3) 0.062(2) Uani 1 1 d . . . . .
C22 C 0.8506(4) 0.3692(3) 0.8948(2) 0.0430(15) Uani 1 1 d . . . . .
H22 H 0.8562 0.3234 0.8964 0.052 Uiso 1 1 calc R U . . .
C23 C 0.9054(3) 0.4073(3) 0.9202(2) 0.0315(13) Uani 1 1 d . . . . .
C24 C 0.8973(3) 0.4753(2) 0.91921(18) 0.0292(13) Uani 1 1 d . . . . .
C25 C 0.7283(5) 0.3518(4) 0.8395(4) 0.115(4) Uani 1 1 d . . . . .
H25A H 0.7024 0.3758 0.8106 0.173 Uiso 1 1 calc R U . . .
H25B H 0.6887 0.3374 0.8655 0.173 Uiso 1 1 calc R U . . .
H25C H 0.7554 0.3139 0.8246 0.173 Uiso 1 1 calc R U . . .
C26 C 0.9747(3) 0.3765(2) 0.9481(2) 0.0301(13) Uani 1 1 d . . . . .
H26A H 0.9636 0.3746 0.9870 0.036 Uiso 1 1 calc R U . . .
H26B H 0.9803 0.3313 0.9351 0.036 Uiso 1 1 calc R U . . .
C27 C 1.1294(3) 0.3728(3) 1.0175(2) 0.0297(14) Uani 1 1 d . . . . .
C28 C 1.0765(3) 0.3226(3) 1.0461(2) 0.0353(14) Uani 1 1 d . . . . .
C29 C 1.0397(4) 0.3400(3) 1.0936(2) 0.0467(15) Uani 1 1 d . . . . .
H29 H 1.0459 0.3829 1.1070 0.056 Uiso 1 1 calc R U . . .
C30 C 0.9945(4) 0.2963(4) 1.1215(3) 0.064(2) Uani 1 1 d . . . . .
H30 H 0.9706 0.3082 1.1545 0.077 Uiso 1 1 calc R U . . .
C31 C 0.9842(5) 0.2342(4) 1.1008(4) 0.084(3) Uani 1 1 d . . . . .
H31 H 0.9522 0.2037 1.1194 0.101 Uiso 1 1 calc R U . . .
C32 C 1.0201(5) 0.2165(3) 1.0533(3) 0.065(2) Uani 1 1 d . . . . .
H32 H 1.0131 0.1740 1.0393 0.078 Uiso 1 1 calc R U . . .
C33 C 1.0657(4) 0.2605(3) 1.0269(2) 0.0458(16) Uani 1 1 d . . . . .
H33 H 1.0906 0.2481 0.9944 0.055 Uiso 1 1 calc R U . . .
C34 C 1.2146(3) 0.3574(2) 1.0322(2) 0.0320(13) Uani 1 1 d . . . . .
C35 C 1.2522(3) 0.3025(3) 1.0119(3) 0.0476(18) Uani 1 1 d . . . . .
H35 H 1.2234 0.2735 0.9897 0.057 Uiso 1 1 calc R U . . .
C36 C 1.3301(4) 0.2891(3) 1.0233(3) 0.0555(18) Uani 1 1 d . . . . .
H36 H 1.3549 0.2521 1.0081 0.067 Uiso 1 1 calc R U . . .
C37 C 1.3707(4) 0.3288(3) 1.0562(3) 0.0572(18) Uani 1 1 d . . . . .
H37 H 1.4237 0.3190 1.0652 0.069 Uiso 1 1 calc R U . . .
C38 C 1.3356(4) 0.3833(4) 1.0767(3) 0.063(2) Uani 1 1 d . . . . .
H38 H 1.3649 0.4116 1.0991 0.075 Uiso 1 1 calc R U . . .
C39 C 1.2571(4) 0.3979(3) 1.0649(2) 0.0407(15) Uani 1 1 d . . . . .
H39 H 1.2333 0.4357 1.0794 0.049 Uiso 1 1 calc R U . . .
C40 C 1.0636(3) 0.5747(3) 1.11851(19) 0.0328(13) Uani 1 1 d . . . . .
H40A H 1.0350 0.5349 1.1293 0.039 Uiso 1 1 calc R U . . .
H40B H 1.0452 0.6113 1.1410 0.039 Uiso 1 1 calc R U . . .
C41 C 1.1514(4) 0.5654(3) 1.1243(2) 0.0479(17) Uani 1 1 d . . . . .
H41A H 1.1643 0.5188 1.1287 0.058 Uiso 1 1 calc R U . . .
H41B H 1.1714 0.5894 1.1559 0.058 Uiso 1 1 calc R U . . .
C42 C 1.1876(3) 0.5919(3) 1.0730(2) 0.0381(14) Uani 1 1 d . . . . .
H42A H 1.2090 0.5562 1.0509 0.046 Uiso 1 1 calc R U . . .
H42B H 1.2307 0.6227 1.0814 0.046 Uiso 1 1 calc R U . . .
C43 C 1.1206(3) 0.6266(3) 1.0437(2) 0.0321(14) Uani 1 1 d . . . . .
H43 H 1.1160 0.6721 1.0572 0.039 Uiso 1 1 calc R U . . .
N1 N 0.7730(3) 0.6107(2) 0.91398(18) 0.0385(13) Uani 1 1 d . . . . .
N2 N 1.0504(3) 0.58894(18) 1.06024(14) 0.0247(10) Uani 1 1 d . . . . .
O1 O 0.94936(19) 0.51328(14) 0.94478(12) 0.0278(8) Uani 1 1 d . . . . .
O2 O 1.1089(2) 0.43625(15) 1.03397(12) 0.0269(8) Uani 1 1 d . . . . .
Zr1 Zr 1.03588(4) 0.5000 1.0000 0.02189(19) Uani 1 2 d S T P . .
O3 O 0.6991(3) 0.7225(2) 0.8919(2) 0.0555(15) Uani 1 1 d . . . . .
H1O H 0.731(4) 0.713(4) 0.903(3) 0.05(3) Uiso 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
C12 C13 1.3900 . ?
C12 C17 1.3900 . ?
C12 C5 1.546(7) . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 C15 1.3900 . ?
C14 H14 0.9500 . ?
C15 C16 1.3900 . ?
C15 H15 0.9500 . ?
C16 C17 1.3900 . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C1 N1 1.458(7) . ?
C1 C2 1.466(10) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.507(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.542(8) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N1 1.480(7) . ?
C4 C5 1.549(7) . ?
C4 H4 1.0000 . ?
C5 O3 1.422(7) . ?
C5 C6 1.512(8) . ?
C6 C11 1.389(8) . ?
C6 C7 1.396(8) . ?
C7 C8 1.381(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.365(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.364(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.363(8) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C18 N1 1.461(7) . ?
C18 C19 1.515(9) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.396(8) . ?
C19 C24 1.400(7) . ?
C20 C21 1.378(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.390(8) . ?
C21 C25 1.508(9) . ?
C22 C23 1.373(8) . ?
C22 H22 0.9500 . ?
C23 C24 1.408(7) . ?
C23 C26 1.507(7) . ?
C24 O1 1.342(6) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 N2 1.486(7) 3_567 ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 O2 1.414(6) . ?
C27 C34 1.525(8) . ?
C27 C43 1.537(8) 3_567 ?
C27 C28 1.545(8) . ?
C28 C33 1.379(8) . ?
C28 C29 1.388(8) . ?
C29 C30 1.374(9) . ?
C29 H29 0.9500 . ?
C30 C31 1.391(11) . ?
C30 H30 0.9500 . ?
C31 C32 1.383(11) . ?
C31 H31 0.9500 . ?
C32 C33 1.363(9) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C39 1.372(8) . ?
C34 C35 1.394(7) . ?
C35 C36 1.381(8) . ?
C35 H35 0.9500 . ?
C36 C37 1.350(9) . ?
C36 H36 0.9500 . ?
C37 C38 1.371(9) . ?
C37 H37 0.9500 . ?
C38 C39 1.397(9) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 N2 1.501(6) . ?
C40 C41 1.511(8) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.523(8) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.530(8) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 N2 1.480(7) . ?
C43 C27 1.537(8) 3_567 ?
C43 H43 1.0000 . ?
N2 C26 1.486(7) 3_567 ?
N2 Zr1 2.384(4) . ?
O1 Zr1 2.033(3) . ?
O2 Zr1 1.995(3) . ?
Zr1 O2 1.995(3) 3_567 ?
Zr1 O1 2.033(3) 3_567 ?
Zr1 N2 2.384(4) 3_567 ?
O3 H1O 0.65(7) . ?

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
C13 C12 C17 120.0 . . ?
C13 C12 C5 119.8(4) . . ?
C17 C12 C5 120.1(4) . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 120.0 . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.0 . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C12 120.0 . . ?
C16 C17 H17 120.0 . . ?
C12 C17 H17 120.0 . . ?
N1 C1 C2 105.8(5) . . ?
N1 C1 H1A 110.6 . . ?
C2 C1 H1A 110.6 . . ?
N1 C1 H1B 110.6 . . ?
C2 C1 H1B 110.6 . . ?
H1A C1 H1B 108.7 . . ?
C1 C2 C3 106.6(6) . . ?
C1 C2 H2A 110.4 . . ?
C3 C2 H2A 110.4 . . ?
C1 C2 H2B 110.4 . . ?
C3 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
C2 C3 C4 105.1(6) . . ?
C2 C3 H3A 110.7 . . ?
C4 C3 H3A 110.7 . . ?
C2 C3 H3B 110.7 . . ?
C4 C3 H3B 110.7 . . ?
H3A C3 H3B 108.8 . . ?
N1 C4 C3 105.4(4) . . ?
N1 C4 C5 107.7(4) . . ?
C3 C4 C5 113.8(5) . . ?
N1 C4 H4 109.9 . . ?
C3 C4 H4 109.9 . . ?
C5 C4 H4 109.9 . . ?
O3 C5 C6 107.3(5) . . ?
O3 C5 C12 110.8(5) . . ?
C6 C5 C12 107.1(4) . . ?
O3 C5 C4 106.3(4) . . ?
C6 C5 C4 113.6(5) . . ?
C12 C5 C4 111.7(4) . . ?
C11 C6 C7 116.7(5) . . ?
C11 C6 C5 123.0(5) . . ?
C7 C6 C5 120.1(5) . . ?
C8 C7 C6 121.5(6) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C9 C8 C7 119.3(6) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C10 C9 C8 120.8(6) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C11 C10 C9 119.8(6) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C6 122.0(6) . . ?
C10 C11 H11 119.0 . . ?
C6 C11 H11 119.0 . . ?
N1 C18 C19 117.2(5) . . ?
N1 C18 H18A 108.0 . . ?
C19 C18 H18A 108.0 . . ?
N1 C18 H18B 108.0 . . ?
C19 C18 H18B 108.0 . . ?
H18A C18 H18B 107.2 . . ?
C20 C19 C24 117.9(6) . . ?
C20 C19 C18 122.4(5) . . ?
C24 C19 C18 119.8(5) . . ?
C21 C20 C19 123.6(6) . . ?
C21 C20 H20 118.2 . . ?
C19 C20 H20 118.2 . . ?
C20 C21 C22 116.8(6) . . ?
C20 C21 C25 122.3(6) . . ?
C22 C21 C25 120.8(6) . . ?
C23 C22 C21 122.4(5) . . ?
C23 C22 H22 118.8 . . ?
C21 C22 H22 118.8 . . ?
C22 C23 C24 119.6(5) . . ?
C22 C23 C26 120.1(5) . . ?
C24 C23 C26 120.3(5) . . ?
O1 C24 C19 119.9(5) . . ?
O1 C24 C23 120.5(4) . . ?
C19 C24 C23 119.6(5) . . ?
C21 C25 H25A 109.5 . . ?
C21 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C21 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2 C26 C23 114.1(4) 3_567 . ?
N2 C26 H26A 108.7 3_567 . ?
C23 C26 H26A 108.7 . . ?
N2 C26 H26B 108.7 3_567 . ?
C23 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
O2 C27 C34 110.9(4) . . ?
O2 C27 C43 104.9(4) . 3_567 ?
C34 C27 C43 109.5(4) . 3_567 ?
O2 C27 C28 109.9(4) . . ?
C34 C27 C28 107.5(4) . . ?
C43 C27 C28 114.2(5) 3_567 . ?
C33 C28 C29 118.6(5) . . ?
C33 C28 C27 122.5(5) . . ?
C29 C28 C27 118.9(5) . . ?
C30 C29 C28 121.0(6) . . ?
C30 C29 H29 119.5 . . ?
C28 C29 H29 119.5 . . ?
C29 C30 C31 119.0(7) . . ?
C29 C30 H30 120.5 . . ?
C31 C30 H30 120.5 . . ?
C32 C31 C30 120.4(7) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C33 C32 C31 119.4(7) . . ?
C33 C32 H32 120.3 . . ?
C31 C32 H32 120.3 . . ?
C32 C33 C28 121.6(6) . . ?
C32 C33 H33 119.2 . . ?
C28 C33 H33 119.2 . . ?
C39 C34 C35 118.0(5) . . ?
C39 C34 C27 121.0(5) . . ?
C35 C34 C27 121.0(5) . . ?
C36 C35 C34 121.7(6) . . ?
C36 C35 H35 119.1 . . ?
C34 C35 H35 119.1 . . ?
C37 C36 C35 119.6(6) . . ?
C37 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?
C36 C37 C38 120.1(6) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C37 C38 C39 120.8(6) . . ?
C37 C38 H38 119.6 . . ?
C39 C38 H38 119.6 . . ?
C34 C39 C38 119.8(6) . . ?
C34 C39 H39 120.1 . . ?
C38 C39 H39 120.1 . . ?
N2 C40 C41 105.3(4) . . ?
N2 C40 H40A 110.7 . . ?
C41 C40 H40A 110.7 . . ?
N2 C40 H40B 110.7 . . ?
C41 C40 H40B 110.7 . . ?
H40A C40 H40B 108.8 . . ?
C40 C41 C42 105.8(5) . . ?
C40 C41 H41A 110.6 . . ?
C42 C41 H41A 110.6 . . ?
C40 C41 H41B 110.6 . . ?
C42 C41 H41B 110.6 . . ?
H41A C41 H41B 108.7 . . ?
C41 C42 C43 105.7(5) . . ?
C41 C42 H42A 110.6 . . ?
C43 C42 H42A 110.6 . . ?
C41 C42 H42B 110.6 . . ?
C43 C42 H42B 110.6 . . ?
H42A C42 H42B 108.7 . . ?
N2 C43 C42 102.8(4) . . ?
N2 C43 C27 111.1(4) . 3_567 ?
C42 C43 C27 114.1(5) . 3_567 ?
N2 C43 H43 109.6 . . ?
C42 C43 H43 109.6 . . ?
C27 C43 H43 109.6 3_567 . ?
C1 N1 C18 113.0(4) . . ?
C1 N1 C4 108.8(5) . . ?
C18 N1 C4 117.0(4) . . ?
C43 N2 C26 114.0(4) . 3_567 ?
C43 N2 C40 104.7(4) . . ?
C26 N2 C40 111.0(4) 3_567 . ?
C43 N2 Zr1 108.1(3) . . ?
C26 N2 Zr1 101.0(3) 3_567 . ?
C40 N2 Zr1 118.5(3) . . ?
C24 O1 Zr1 136.1(3) . . ?
C27 O2 Zr1 129.7(3) . . ?
O2 Zr1 O2 103.2(2) . 3_567 ?
O2 Zr1 O1 94.13(13) . 3_567 ?
O2 Zr1 O1 145.67(12) 3_567 3_567 ?
O2 Zr1 O1 145.67(12) . . ?
O2 Zr1 O1 94.13(13) 3_567 . ?
O1 Zr1 O1 87.49(18) 3_567 . ?
O2 Zr1 N2 72.43(12) . 3_567 ?
O2 Zr1 N2 99.97(13) 3_567 3_567 ?
O1 Zr1 N2 113.56(13) 3_567 3_567 ?
O1 Zr1 N2 75.53(13) . 3_567 ?
O2 Zr1 N2 99.96(13) . . ?
O2 Zr1 N2 72.42(12) 3_567 . ?
O1 Zr1 N2 75.53(13) 3_567 . ?
O1 Zr1 N2 113.56(13) . . ?
N2 Zr1 N2 168.1(2) 3_567 . ?
C5 O3 H1O 104(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C17 C12 C13 C14 0.0 . . . . ?
C5 C12 C13 C14 178.8(4) . . . . ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 C16 0.0 . . . . ?
C14 C15 C16 C17 0.0 . . . . ?
C15 C16 C17 C12 0.0 . . . . ?
C13 C12 C17 C16 0.0 . . . . ?
C5 C12 C17 C16 -178.8(4) . . . . ?
N1 C1 C2 C3 29.4(8) . . . . ?
C1 C2 C3 C4 -21.0(8) . . . . ?
C2 C3 C4 N1 4.9(6) . . . . ?
C2 C3 C4 C5 -112.8(6) . . . . ?
C13 C12 C5 O3 178.6(3) . . . . ?
C17 C12 C5 O3 -2.6(5) . . . . ?
C13 C12 C5 C6 -64.7(5) . . . . ?
C17 C12 C5 C6 114.1(4) . . . . ?
C13 C12 C5 C4 60.3(5) . . . . ?
C17 C12 C5 C4 -120.9(4) . . . . ?
N1 C4 C5 O3 -51.0(6) . . . . ?
C3 C4 C5 O3 65.5(6) . . . . ?
N1 C4 C5 C6 -168.8(4) . . . . ?
C3 C4 C5 C6 -52.3(6) . . . . ?
N1 C4 C5 C12 70.0(5) . . . . ?
C3 C4 C5 C12 -173.6(5) . . . . ?
O3 C5 C6 C11 -156.1(5) . . . . ?
C12 C5 C6 C11 84.9(6) . . . . ?
C4 C5 C6 C11 -38.9(7) . . . . ?
O3 C5 C6 C7 29.5(7) . . . . ?
C12 C5 C6 C7 -89.4(6) . . . . ?
C4 C5 C6 C7 146.7(5) . . . . ?
C11 C6 C7 C8 0.5(8) . . . . ?
C5 C6 C7 C8 175.2(5) . . . . ?
C6 C7 C8 C9 -1.5(9) . . . . ?
C7 C8 C9 C10 1.4(9) . . . . ?
C8 C9 C10 C11 -0.3(9) . . . . ?
C9 C10 C11 C6 -0.7(9) . . . . ?
C7 C6 C11 C10 0.6(8) . . . . ?
C5 C6 C11 C10 -173.9(5) . . . . ?
N1 C18 C19 C20 76.7(7) . . . . ?
N1 C18 C19 C24 -105.0(6) . . . . ?
C24 C19 C20 C21 -1.6(10) . . . . ?
C18 C19 C20 C21 176.7(7) . . . . ?
C19 C20 C21 C22 -1.8(11) . . . . ?
C19 C20 C21 C25 -179.7(8) . . . . ?
C20 C21 C22 C23 2.0(10) . . . . ?
C25 C21 C22 C23 179.9(7) . . . . ?
C21 C22 C23 C24 1.2(9) . . . . ?
C21 C22 C23 C26 -177.6(6) . . . . ?
C20 C19 C24 O1 -178.4(5) . . . . ?
C18 C19 C24 O1 3.2(7) . . . . ?
C20 C19 C24 C23 4.9(8) . . . . ?
C18 C19 C24 C23 -173.5(5) . . . . ?
C22 C23 C24 O1 178.5(5) . . . . ?
C26 C23 C24 O1 -2.6(7) . . . . ?
C22 C23 C24 C19 -4.7(8) . . . . ?
C26 C23 C24 C19 174.1(4) . . . . ?
C22 C23 C26 N2 138.6(5) . . . 3_567 ?
C24 C23 C26 N2 -40.3(6) . . . 3_567 ?
O2 C27 C28 C33 159.6(5) . . . . ?
C34 C27 C28 C33 -79.7(6) . . . . ?
C43 C27 C28 C33 42.0(7) 3_567 . . . ?
O2 C27 C28 C29 -21.9(7) . . . . ?
C34 C27 C28 C29 98.9(6) . . . . ?
C43 C27 C28 C29 -139.4(5) 3_567 . . . ?
C33 C28 C29 C30 1.1(9) . . . . ?
C27 C28 C29 C30 -177.5(6) . . . . ?
C28 C29 C30 C31 -1.7(10) . . . . ?
C29 C30 C31 C32 1.2(12) . . . . ?
C30 C31 C32 C33 -0.2(12) . . . . ?
C31 C32 C33 C28 -0.4(11) . . . . ?
C29 C28 C33 C32 -0.1(9) . . . . ?
C27 C28 C33 C32 178.5(6) . . . . ?
O2 C27 C34 C39 10.0(7) . . . . ?
C43 C27 C34 C39 125.2(6) 3_567 . . . ?
C28 C27 C34 C39 -110.2(6) . . . . ?
O2 C27 C34 C35 -168.7(5) . . . . ?
C43 C27 C34 C35 -53.4(7) 3_567 . . . ?
C28 C27 C34 C35 71.1(6) . . . . ?
C39 C34 C35 C36 -1.0(9) . . . . ?
C27 C34 C35 C36 177.7(6) . . . . ?
C34 C35 C36 C37 2.1(10) . . . . ?
C35 C36 C37 C38 -2.3(11) . . . . ?
C36 C37 C38 C39 1.5(11) . . . . ?
C35 C34 C39 C38 0.1(9) . . . . ?
C27 C34 C39 C38 -178.6(6) . . . . ?
C37 C38 C39 C34 -0.3(10) . . . . ?
N2 C40 C41 C42 14.6(6) . . . . ?
C40 C41 C42 C43 9.8(6) . . . . ?
C41 C42 C43 N2 -30.7(5) . . . . ?
C41 C42 C43 C27 -151.1(5) . . . 3_567 ?
C2 C1 N1 C18 -158.2(6) . . . . ?
C2 C1 N1 C4 -26.6(7) . . . . ?
C19 C18 N1 C1 50.7(7) . . . . ?
C19 C18 N1 C4 -76.7(6) . . . . ?
C3 C4 N1 C1 13.1(6) . . . . ?
C5 C4 N1 C1 134.9(5) . . . . ?
C3 C4 N1 C18 142.5(5) . . . . ?
C5 C4 N1 C18 -95.6(5) . . . . ?
C42 C43 N2 C26 161.6(4) . . . 3_567 ?
C27 C43 N2 C26 -76.0(5) 3_567 . . 3_567 ?
C42 C43 N2 C40 40.1(5) . . . . ?
C27 C43 N2 C40 162.5(5) 3_567 . . . ?
C42 C43 N2 Zr1 -87.0(4) . . . . ?
C27 C43 N2 Zr1 35.4(5) 3_567 . . . ?
C41 C40 N2 C43 -34.5(5) . . . . ?
C41 C40 N2 C26 -158.0(4) . . . 3_567 ?
C41 C40 N2 Zr1 85.9(5) . . . . ?
C19 C24 O1 Zr1 169.9(3) . . . . ?
C23 C24 O1 Zr1 -13.3(7) . . . . ?
C34 C27 O2 Zr1 146.6(3) . . . . ?
C43 C27 O2 Zr1 28.6(6) 3_567 . . . ?
C28 C27 O2 Zr1 -94.6(4) . . . . ?

_refine_diff_density_max         0.699
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.059




# 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 -0.113 -0.002 -0.001 2389 412 ' '
_platon_squeeze_details          
;
;



_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
####################################################################### 
# 
# 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_Ti
_database_code_depnum_ccdc_archive 'CCDC 1414116'
_audit_update_record             
;
2015-07-21 deposited with the CCDC.
2015-07-28 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        Ti
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C129 H132 N6 O12 Ti3, 3(C7 H8)'
_chemical_formula_sum            'C150 H156 N6 O12 Ti3'
_chemical_formula_weight         2378.50

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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   19.172(3)
_cell_length_b                   22.272(3)
_cell_length_c                   30.035(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     12825(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3947
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      16.70

_exptl_crystal_description       Block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_F_000             5040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_exptl_absorpt_coefficient_mu    0.247
_shelx_estimated_absorpt_T_min   0.919
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.919
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_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            33748
_diffrn_reflns_av_unetI/netI     0.0929
_diffrn_reflns_av_R_equivalents  0.1188
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.260
_diffrn_reflns_theta_max         17.856
_diffrn_reflns_theta_full        17.856
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             8537
_reflns_number_gt                6663
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.802
_reflns_Friedel_fraction_max     0.989
_reflns_Friedel_fraction_full    0.989

_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 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)+(0.1000P)²+0.2500P] 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_abs_structure_details 
; 
 Flack x determined using 2520 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.01(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8537
_refine_ls_number_parameters     1501
_refine_ls_number_restraints     11
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0544
_refine_ls_wR_factor_ref         0.1619
_refine_ls_wR_factor_gt          0.1332
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.015
_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
C130 C 0.1350(8) 0.4397(7) 0.6302(3) 0.159(15) Uani 1 1 d G . . . .
C135 C 0.0787(8) 0.4163(8) 0.6068(3) 0.146(13) Uani 1 1 d G . . . .
H135 H 0.0356 0.4355 0.6078 0.175 Uiso 1 1 calc R U . . .
C134 C 0.0867(9) 0.3642(8) 0.5818(3) 0.19(2) Uani 1 1 d G . . . .
H134 H 0.0490 0.3486 0.5661 0.230 Uiso 1 1 calc R U . . .
C133 C 0.1510(9) 0.3355(8) 0.5803(3) 0.21(2) Uani 1 1 d G . . . .
H133 H 0.1563 0.3006 0.5636 0.255 Uiso 1 1 calc R U . . .
C132 C 0.2073(9) 0.3589(7) 0.6037(3) 0.21(2) Uani 1 1 d G . . . .
H132 H 0.2504 0.3397 0.6026 0.253 Uiso 1 1 calc R U . . .
C131 C 0.1993(8) 0.4110(7) 0.6286(3) 0.18(2) Uani 1 1 d G . . . .
H131 H 0.2370 0.4266 0.6443 0.222 Uiso 1 1 calc R U . . .
C137 C 0.4763(6) 0.4644(7) 0.9734(4) 0.157(13) Uani 1 1 d G . . . .
C138 C 0.4830(7) 0.4074(8) 0.9550(5) 0.143(13) Uani 1 1 d G . . . .
H138 H 0.5113 0.4014 0.9303 0.171 Uiso 1 1 calc R U . . .
C139 C 0.4473(9) 0.3592(7) 0.9737(5) 0.189(17) Uani 1 1 d G . . . .
H139 H 0.4518 0.3211 0.9615 0.227 Uiso 1 1 calc R U . . .
C140 C 0.4050(9) 0.3681(6) 1.0107(4) 0.23(3) Uani 1 1 d G U . . .
H140 H 0.3812 0.3358 1.0232 0.278 Uiso 1 1 calc R U . . .
C141 C 0.3984(8) 0.4251(6) 1.0291(4) 0.28(4) Uani 1 1 d G U . . .
H141 H 0.3701 0.4310 1.0538 0.333 Uiso 1 1 calc R U . . .
C142 C 0.4341(7) 0.4732(7) 1.0104(4) 0.24(3) Uani 1 1 d G U . . .
H142 H 0.4296 0.5114 1.0227 0.287 Uiso 1 1 calc R U . . .
C149 C 0.4333(10) 0.7058(7) 0.9279(4) 0.20(2) Uani 1 1 d G . . . .
C148 C 0.4748(10) 0.7234(7) 0.9635(4) 0.25(3) Uani 1 1 d DG . . . .
H148 H 0.5188 0.7066 0.9673 0.295 Uiso 1 1 calc R U . . .
C147 C 0.4505(12) 0.7661(7) 0.9935(4) 0.32(5) Uani 1 1 d G . . . .
H147 H 0.4783 0.7779 1.0173 0.383 Uiso 1 1 calc R U . . .
C146 C 0.3848(13) 0.7912(6) 0.9878(5) 0.38(6) Uani 1 1 d G . . . .
H146 H 0.3685 0.8198 1.0079 0.453 Uiso 1 1 calc R U . . .
C145 C 0.3432(12) 0.7736(5) 0.9522(5) 0.27(3) Uani 1 1 d G . . . .
H145 H 0.2992 0.7905 0.9484 0.322 Uiso 1 1 calc R U . . .
C144 C 0.3675(11) 0.7309(6) 0.9222(4) 0.21(2) Uani 1 1 d DG . . . .
H144 H 0.3397 0.7192 0.8984 0.251 Uiso 1 1 calc R U . . .
C1 C 0.7421(10) 0.4235(10) 0.6872(6) 0.048(5) Uani 1 1 d . . . . .
C2 C 0.7012(13) 0.4637(10) 0.7076(6) 0.066(5) Uani 1 1 d . . . . .
H2 H 0.7200 0.4902 0.7284 0.079 Uiso 1 1 calc R U . . .
C3 C 0.6307(14) 0.4658(11) 0.6977(9) 0.086(7) Uani 1 1 d . . . . .
H3 H 0.6034 0.4956 0.7105 0.103 Uiso 1 1 calc R U . . .
C4 C 0.6007(12) 0.4266(16) 0.6704(9) 0.095(8) Uani 1 1 d . . . . .
H4 H 0.5528 0.4278 0.6654 0.114 Uiso 1 1 calc R U . . .
C5 C 0.6413(17) 0.3840(12) 0.6494(8) 0.094(7) Uani 1 1 d . . . . .
H5 H 0.6214 0.3567 0.6298 0.112 Uiso 1 1 calc R U . . .
C6 C 0.7108(13) 0.3828(10) 0.6580(7) 0.075(6) Uani 1 1 d . . . . .
H6 H 0.7383 0.3540 0.6440 0.090 Uiso 1 1 calc R U . . .
C7 C 0.8201(9) 0.4211(7) 0.6947(6) 0.045(5) Uani 1 1 d . . . . .
C8 C 0.8553(8) 0.4556(10) 0.6568(7) 0.047(5) Uani 1 1 d . . . . .
C9 C 0.8798(11) 0.5112(12) 0.6608(7) 0.077(6) Uani 1 1 d . . . . .
H9 H 0.8780 0.5291 0.6888 0.093 Uiso 1 1 calc R U . . .
C10 C 0.9083(12) 0.5443(9) 0.6256(13) 0.102(8) Uani 1 1 d . . . . .
H10 H 0.9258 0.5828 0.6297 0.122 Uiso 1 1 calc R U . . .
C11 C 0.9089(14) 0.5171(18) 0.5850(9) 0.100(8) Uani 1 1 d . . . . .
H11 H 0.9265 0.5382 0.5608 0.120 Uiso 1 1 calc R U . . .
C12 C 0.8860(13) 0.4633(17) 0.5787(8) 0.101(9) Uani 1 1 d . . . . .
H12 H 0.8884 0.4460 0.5506 0.121 Uiso 1 1 calc R U . . .
C13 C 0.8577(10) 0.4310(11) 0.6142(9) 0.091(7) Uani 1 1 d . . . . .
H13 H 0.8401 0.3926 0.6094 0.110 Uiso 1 1 calc R U . . .
C14 C 0.8494(8) 0.3575(8) 0.7014(5) 0.045(5) Uani 1 1 d . . . . .
H14 H 0.8579 0.3388 0.6724 0.054 Uiso 1 1 calc R U . . .
C15 C 0.8036(9) 0.3178(8) 0.7289(7) 0.067(5) Uani 1 1 d . . . . .
H15A H 0.7705 0.2967 0.7102 0.080 Uiso 1 1 calc R U . . .
H15B H 0.7779 0.3414 0.7506 0.080 Uiso 1 1 calc R U . . .
C16 C 0.8512(10) 0.2739(8) 0.7521(6) 0.065(5) Uani 1 1 d . . . . .
H16A H 0.8388 0.2703 0.7833 0.078 Uiso 1 1 calc R U . . .
H16B H 0.8480 0.2346 0.7383 0.078 Uiso 1 1 calc R U . . .
C17 C 0.9234(9) 0.2987(8) 0.7473(6) 0.054(5) Uani 1 1 d . . . . .
H17A H 0.9461 0.3011 0.7761 0.065 Uiso 1 1 calc R U . . .
H17B H 0.9512 0.2733 0.7280 0.065 Uiso 1 1 calc R U . . .
C18 C 0.9778(10) 0.3749(7) 0.7010(5) 0.049(5) Uani 1 1 d . . . . .
H18A H 0.9707 0.4144 0.6881 0.058 Uiso 1 1 calc R U . . .
H18B H 0.9820 0.3465 0.6766 0.058 Uiso 1 1 calc R U . . .
C19 C 1.0447(10) 0.3752(8) 0.7265(6) 0.039(4) Uani 1 1 d . . . . .
C20 C 1.1019(12) 0.3427(7) 0.7160(6) 0.046(5) Uani 1 1 d . . . . .
H20 H 1.1001 0.3168 0.6917 0.055 Uiso 1 1 calc R U . . .
C21 C 1.1632(11) 0.3469(8) 0.7401(7) 0.054(5) Uani 1 1 d . . . . .
C22 C 1.1655(10) 0.3883(9) 0.7744(6) 0.051(4) Uani 1 1 d . . . . .
H22 H 1.2070 0.3928 0.7901 0.061 Uiso 1 1 calc R U . . .
C23 C 1.1095(11) 0.4229(7) 0.7864(6) 0.039(4) Uani 1 1 d . . . . .
C24 C 1.0468(11) 0.4165(8) 0.7624(6) 0.039(4) Uani 1 1 d . . . . .
C25 C 1.1181(8) 0.4681(8) 0.8239(5) 0.041(4) Uani 1 1 d . . . . .
H25A H 1.0787 0.4633 0.8438 0.050 Uiso 1 1 calc R U . . .
H25B H 1.1596 0.4571 0.8404 0.050 Uiso 1 1 calc R U . . .
C26 C 1.0571(9) 0.5630(7) 0.8038(6) 0.057(5) Uani 1 1 d . . . . .
H26A H 1.0186 0.5349 0.8027 0.068 Uiso 1 1 calc R U . . .
H26B H 1.0475 0.5931 0.8263 0.068 Uiso 1 1 calc R U . . .
C27 C 1.0676(16) 0.5894(14) 0.7628(11) 0.159(11) Uani 1 1 d . U . . .
H27A H 1.0451 0.6284 0.7627 0.191 Uiso 1 1 calc R U . . .
H27B H 1.0451 0.5649 0.7403 0.191 Uiso 1 1 calc R U . . .
C28 C 1.1392(8) 0.5970(8) 0.7509(6) 0.055(5) Uani 1 1 d . . . . .
H28A H 1.1556 0.6371 0.7581 0.067 Uiso 1 1 calc R U . . .
H28B H 1.1467 0.5894 0.7195 0.067 Uiso 1 1 calc R U . . .
C29 C 1.1751(9) 0.5491(7) 0.7801(6) 0.054(5) Uani 1 1 d . . . . .
H29 H 1.1880 0.5143 0.7619 0.065 Uiso 1 1 calc R U . . .
C30 C 1.2414(10) 0.5749(9) 0.8043(6) 0.056(5) Uani 1 1 d . . . . .
C31 C 1.2850(9) 0.5263(9) 0.8236(7) 0.053(5) Uani 1 1 d . . . . .
C32 C 1.3116(10) 0.4788(12) 0.7992(7) 0.072(6) Uani 1 1 d . . . . .
H32 H 1.2994 0.4760 0.7693 0.087 Uiso 1 1 calc R U . . .
C33 C 1.3541(12) 0.4362(11) 0.8162(12) 0.099(8) Uani 1 1 d . . . . .
H33 H 1.3699 0.4051 0.7981 0.119 Uiso 1 1 calc R U . . .
C34 C 1.3742(12) 0.4387(14) 0.8602(12) 0.105(8) Uani 1 1 d . . . . .
H34 H 1.4061 0.4112 0.8716 0.126 Uiso 1 1 calc R U . . .
C35 C 1.3465(15) 0.4819(16) 0.8862(9) 0.111(8) Uani 1 1 d . . . . .
H35 H 1.3556 0.4817 0.9166 0.133 Uiso 1 1 calc R U . . .
C36 C 1.3050(12) 0.5263(12) 0.8686(9) 0.091(7) Uani 1 1 d . . . . .
H36 H 1.2898 0.5573 0.8870 0.110 Uiso 1 1 calc R U . . .
C37 C 1.2857(10) 0.6145(11) 0.7752(9) 0.065(5) Uani 1 1 d . . . . .
C38 C 1.3096(12) 0.5958(11) 0.7342(10) 0.090(7) Uani 1 1 d . . . . .
H38 H 1.2934 0.5588 0.7241 0.108 Uiso 1 1 calc R U . . .
C39 C 1.3543(15) 0.6255(17) 0.7068(9) 0.119(10) Uani 1 1 d . . . . .
H39 H 1.3690 0.6105 0.6795 0.143 Uiso 1 1 calc R U . . .
C40 C 1.3759(13) 0.681(2) 0.7238(15) 0.127(12) Uani 1 1 d . . . . .
H40 H 1.4068 0.7031 0.7068 0.153 Uiso 1 1 calc R U . . .
C41 C 1.3545(17) 0.7039(13) 0.7640(15) 0.125(10) Uani 1 1 d . . . . .
H41 H 1.3699 0.7411 0.7741 0.150 Uiso 1 1 calc R U . . .
C42 C 1.3093(12) 0.6693(14) 0.7883(8) 0.091(7) Uani 1 1 d . . . . .
H42 H 1.2938 0.6842 0.8155 0.110 Uiso 1 1 calc R U . . .
C43 C 0.6418(13) 0.3424(8) 0.8147(8) 0.080(7) Uani 1 1 d . . . . .
H43 H 0.6838 0.3554 0.8026 0.096 Uiso 1 1 calc R U . . .
C44 C 0.5810(19) 0.3492(10) 0.7901(8) 0.097(7) Uani 1 1 d . . . . .
H44 H 0.5825 0.3655 0.7616 0.116 Uiso 1 1 calc R U . . .
C45 C 0.5192(16) 0.3315(13) 0.8083(11) 0.096(7) Uani 1 1 d . . . . .
H45 H 0.4781 0.3363 0.7923 0.115 Uiso 1 1 calc R U . . .
C46 C 0.5172(13) 0.3069(10) 0.8496(12) 0.088(7) Uani 1 1 d . . . . .
H46 H 0.4749 0.2953 0.8621 0.106 Uiso 1 1 calc R U . . .
C47 C 0.5773(13) 0.2996(8) 0.8724(7) 0.065(5) Uani 1 1 d . . . . .
H47 H 0.5749 0.2818 0.9004 0.077 Uiso 1 1 calc R U . . .
C48 C 0.6418(10) 0.3167(8) 0.8570(7) 0.049(5) Uani 1 1 d . . . . .
C49 C 0.7082(8) 0.3057(8) 0.8835(6) 0.041(5) Uani 1 1 d . . . . .
C50 C 0.7196(10) 0.2374(8) 0.8895(6) 0.042(5) Uani 1 1 d . . . . .
C51 C 0.7714(10) 0.2082(11) 0.8647(6) 0.058(5) Uani 1 1 d . . . . .
H51 H 0.7994 0.2298 0.8452 0.070 Uiso 1 1 calc R U . . .
C52 C 0.7805(10) 0.1469(12) 0.8696(7) 0.071(6) Uani 1 1 d . . . . .
H52 H 0.8154 0.1285 0.8530 0.086 Uiso 1 1 calc R U . . .
C53 C 0.7426(13) 0.1131(9) 0.8965(8) 0.068(6) Uani 1 1 d . . . . .
H53 H 0.7494 0.0718 0.8990 0.081 Uiso 1 1 calc R U . . .
C54 C 0.6917(11) 0.1434(13) 0.9208(6) 0.064(5) Uani 1 1 d . . . . .
H54 H 0.6634 0.1213 0.9398 0.077 Uiso 1 1 calc R U . . .
C55 C 0.6816(8) 0.2030(11) 0.9181(6) 0.047(5) Uani 1 1 d . . . . .
H55 H 0.6481 0.2211 0.9360 0.056 Uiso 1 1 calc R U . . .
C56 C 0.7043(8) 0.3409(7) 0.9293(5) 0.040(4) Uani 1 1 d . . . . .
H56 H 0.6805 0.3163 0.9517 0.048 Uiso 1 1 calc R U . . .
C57 C 0.6723(9) 0.4002(8) 0.9270(6) 0.064(5) Uani 1 1 d . . . . .
H57A H 0.6219 0.3973 0.9285 0.076 Uiso 1 1 calc R U . . .
H57B H 0.6853 0.4207 0.8998 0.076 Uiso 1 1 calc R U . . .
C58 C 0.7008(10) 0.4324(9) 0.9671(7) 0.078(6) Uani 1 1 d . . . . .
H58A H 0.7056 0.4750 0.9610 0.094 Uiso 1 1 calc R U . . .
H58B H 0.6700 0.4273 0.9924 0.094 Uiso 1 1 calc R U . . .
C59 C 0.7687(9) 0.4055(8) 0.9761(5) 0.055(5) Uani 1 1 d . . . . .
H59A H 0.7709 0.3913 1.0065 0.066 Uiso 1 1 calc R U . . .
H59B H 0.8054 0.4349 0.9716 0.066 Uiso 1 1 calc R U . . .
C60 C 0.8121(10) 0.3028(7) 0.9664(5) 0.052(5) Uani 1 1 d . . . . .
H60A H 0.8129 0.2685 0.9465 0.062 Uiso 1 1 calc R U . . .
H60B H 0.7858 0.2916 0.9927 0.062 Uiso 1 1 calc R U . . .
C61 C 0.8850(11) 0.3184(7) 0.9795(7) 0.046(5) Uani 1 1 d . . . . .
C62 C 0.9042(12) 0.3187(7) 1.0252(7) 0.058(5) Uani 1 1 d . . . . .
H62 H 0.8707 0.3099 1.0466 0.070 Uiso 1 1 calc R U . . .
C63 C 0.9693(13) 0.3312(8) 1.0381(6) 0.055(5) Uani 1 1 d . . . . .
C64 C 1.0198(10) 0.3397(7) 1.0051(8) 0.052(5) Uani 1 1 d . . . . .
H64 H 1.0661 0.3448 1.0134 0.062 Uiso 1 1 calc R U . . .
C65 C 1.0020(11) 0.3407(6) 0.9601(7) 0.039(4) Uani 1 1 d . . . . .
C66 C 0.9347(12) 0.3327(7) 0.9483(7) 0.047(5) Uani 1 1 d . . . . .
C67 C 0.9897(9) 0.3399(9) 1.0865(6) 0.077(6) Uani 1 1 d . . . . .
H67A H 0.9658 0.3109 1.1046 0.116 Uiso 1 1 calc R U . . .
H67B H 0.9771 0.3796 1.0958 0.116 Uiso 1 1 calc R U . . .
H67C H 1.0392 0.3346 1.0896 0.116 Uiso 1 1 calc R U . . .
C68 C 1.0537(9) 0.3498(7) 0.9233(6) 0.051(5) Uani 1 1 d . . . . .
H68A H 1.0431 0.3220 0.8993 0.061 Uiso 1 1 calc R U . . .
H68B H 1.0486 0.3902 0.9117 0.061 Uiso 1 1 calc R U . . .
C69 C 1.1613(11) 0.3951(8) 0.9512(6) 0.067(5) Uani 1 1 d . . . . .
H69A H 1.1409 0.4106 0.9784 0.080 Uiso 1 1 calc R U . . .
H69B H 1.1581 0.4258 0.9283 0.080 Uiso 1 1 calc R U . . .
C70 C 1.2351(11) 0.3771(10) 0.9584(7) 0.087(7) Uani 1 1 d . . . . .
H70A H 1.2411 0.3570 0.9869 0.104 Uiso 1 1 calc R U . . .
H70B H 1.2663 0.4113 0.9569 0.104 Uiso 1 1 calc R U . . .
C71 C 1.2471(9) 0.3337(9) 0.9192(7) 0.079(6) Uani 1 1 d . . . . .
H71A H 1.2699 0.3541 0.8947 0.094 Uiso 1 1 calc R U . . .
H71B H 1.2758 0.3000 0.9284 0.094 Uiso 1 1 calc R U . . .
C72 C 1.0986(11) 0.2222(7) 0.8855(8) 0.048(5) Uani 1 1 d . . . . .
C73 C 1.0923(11) 0.2276(7) 0.8397(8) 0.059(5) Uani 1 1 d . . . . .
H73 H 1.1297 0.2424 0.8233 0.071 Uiso 1 1 calc R U . . .
C74 C 1.0332(15) 0.2120(10) 0.8183(7) 0.073(6) Uani 1 1 d . . . . .
H74 H 1.0310 0.2158 0.7875 0.088 Uiso 1 1 calc R U . . .
C75 C 0.9773(14) 0.1910(10) 0.8404(12) 0.095(8) Uani 1 1 d . . . . .
H75 H 0.9369 0.1801 0.8253 0.114 Uiso 1 1 calc R U . . .
C76 C 0.9813(12) 0.1862(9) 0.8849(12) 0.087(7) Uani 1 1 d . . . . .
H76 H 0.9423 0.1731 0.9006 0.104 Uiso 1 1 calc R U . . .
C77 C 1.0410(15) 0.2000(8) 0.9082(7) 0.068(6) Uani 1 1 d . . . . .
H77 H 1.0428 0.1945 0.9389 0.082 Uiso 1 1 calc R U . . .
C78 C 1.1751(8) 0.3124(8) 0.9056(5) 0.048(5) Uani 1 1 d . . . . .
H78 H 1.1649 0.3267 0.8754 0.058 Uiso 1 1 calc R U . . .
C79 C 1.1666(9) 0.2428(8) 0.9073(6) 0.047(5) Uani 1 1 d . . . . .
C80 C 1.2251(11) 0.2079(11) 0.8848(8) 0.064(6) Uani 1 1 d . . . . .
C81 C 1.2344(12) 0.1501(15) 0.8969(7) 0.090(7) Uani 1 1 d . . . . .
H81 H 1.2081 0.1334 0.9197 0.107 Uiso 1 1 calc R U . . .
C82 C 1.286(2) 0.1148(14) 0.8739(13) 0.133(12) Uani 1 1 d . . . . .
H82 H 1.2910 0.0744 0.8808 0.160 Uiso 1 1 calc R U . . .
C83 C 1.3278(18) 0.141(2) 0.8409(13) 0.147(18) Uani 1 1 d . . . . .
H83 H 1.3625 0.1186 0.8268 0.176 Uiso 1 1 calc R U . . .
C84 C 1.3174(14) 0.1966(19) 0.8305(10) 0.129(12) Uani 1 1 d . . . . .
H84 H 1.3452 0.2138 0.8085 0.155 Uiso 1 1 calc R U . . .
C85 C 1.2657(13) 0.2323(11) 0.8511(9) 0.085(7) Uani 1 1 d . . . . .
H85 H 1.2588 0.2718 0.8421 0.102 Uiso 1 1 calc R U . . .
C86 C 1.2248(9) 0.3074(8) 0.7267(6) 0.072(6) Uani 1 1 d . . . . .
H86A H 1.2158 0.2666 0.7354 0.109 Uiso 1 1 calc R U . . .
H86B H 1.2663 0.3215 0.7412 0.109 Uiso 1 1 calc R U . . .
H86C H 1.2309 0.3092 0.6950 0.109 Uiso 1 1 calc R U . . .
C87 C 0.6099(13) 0.5368(12) 0.8326(7) 0.092(7) Uani 1 1 d . . . . .
H87 H 0.6328 0.5044 0.8455 0.110 Uiso 1 1 calc R U . . .
C88 C 0.5429(16) 0.5287(14) 0.8147(9) 0.119(9) Uani 1 1 d . . . . .
H88 H 0.5214 0.4913 0.8166 0.143 Uiso 1 1 calc R U . . .
C89 C 0.5091(14) 0.575(2) 0.7946(10) 0.144(12) Uani 1 1 d . . . . .
H89 H 0.4658 0.5689 0.7815 0.173 Uiso 1 1 calc R U . . .
C90 C 0.5379(18) 0.6299(16) 0.7938(11) 0.142(12) Uani 1 1 d . . . . .
H90 H 0.5138 0.6622 0.7816 0.170 Uiso 1 1 calc R U . . .
C91 C 0.6030(14) 0.6376(11) 0.8110(8) 0.099(7) Uani 1 1 d . . . . .
H91 H 0.6229 0.6756 0.8093 0.119 Uiso 1 1 calc R U . . .
C92 C 0.6422(11) 0.5913(12) 0.8315(7) 0.064(5) Uani 1 1 d . . . . .
C93 C 0.7124(9) 0.6028(8) 0.8526(6) 0.043(5) Uani 1 1 d . . . . .
C94 C 0.6990(9) 0.6359(12) 0.8970(8) 0.066(6) Uani 1 1 d . . . . .
C95 C 0.7036(13) 0.6029(11) 0.9356(12) 0.110(8) Uani 1 1 d . . . . .
H95 H 0.7142 0.5622 0.9342 0.131 Uiso 1 1 calc R U . . .
C96 C 0.6926(19) 0.630(2) 0.9769(13) 0.167(16) Uani 1 1 d . U . . .
H96 H 0.6949 0.6075 1.0030 0.201 Uiso 1 1 calc R U . . .
C97 C 0.679(2) 0.686(3) 0.9782(12) 0.170(18) Uani 1 1 d . U . . .
H97 H 0.6740 0.7033 1.0061 0.204 Uiso 1 1 calc R U . . .
C98 C 0.6721(15) 0.7230(14) 0.9415(16) 0.148(12) Uani 1 1 d . . . . .
H98 H 0.6604 0.7633 0.9442 0.177 Uiso 1 1 calc R U . . .
C99 C 0.6837(11) 0.6957(13) 0.8998(9) 0.092(7) Uani 1 1 d . . . . .
H99 H 0.6809 0.7186 0.8740 0.111 Uiso 1 1 calc R U . . .
C100 C 0.7610(9) 0.6370(7) 0.8221(5) 0.044(4) Uani 1 1 d . . . . .
H100 H 0.7498 0.6799 0.8225 0.053 Uiso 1 1 calc R U . . .
C101 C 0.7616(11) 0.6133(9) 0.7738(6) 0.072(6) Uani 1 1 d . . . . .
H10A H 0.7513 0.5707 0.7733 0.087 Uiso 1 1 calc R U . . .
H10B H 0.7271 0.6341 0.7560 0.087 Uiso 1 1 calc R U . . .
C102 C 0.8313(12) 0.6245(9) 0.7567(6) 0.080(6) Uani 1 1 d . . . . .
H10C H 0.8305 0.6574 0.7355 0.097 Uiso 1 1 calc R U . . .
H10D H 0.8491 0.5890 0.7418 0.097 Uiso 1 1 calc R U . . .
C103 C 0.8766(9) 0.6402(8) 0.7959(6) 0.055(5) Uani 1 1 d . . . . .
H10E H 0.9188 0.6162 0.7959 0.066 Uiso 1 1 calc R U . . .
H10F H 0.8895 0.6823 0.7951 0.066 Uiso 1 1 calc R U . . .
C104 C 0.8559(9) 0.6687(7) 0.8719(5) 0.049(5) Uani 1 1 d . . . . .
H10G H 0.8248 0.6630 0.8970 0.059 Uiso 1 1 calc R U . . .
H10H H 0.8508 0.7098 0.8618 0.059 Uiso 1 1 calc R U . . .
C105 C 0.9300(9) 0.6589(10) 0.8869(5) 0.037(4) Uani 1 1 d . . . . .
C106 C 0.9818(13) 0.7009(8) 0.8837(5) 0.054(5) Uani 1 1 d . . . . .
H106 H 0.9717 0.7380 0.8711 0.065 Uiso 1 1 calc R U . . .
C107 C 1.0494(11) 0.6898(9) 0.8988(6) 0.058(5) Uani 1 1 d . . . . .
C108 C 1.0625(9) 0.6350(11) 0.9175(5) 0.047(4) Uani 1 1 d . . . . .
H108 H 1.1072 0.6277 0.9283 0.056 Uiso 1 1 calc R U . . .
C109 C 1.0140(12) 0.5902(8) 0.9214(5) 0.043(5) Uani 1 1 d . . . . .
C110 C 0.9478(11) 0.6019(9) 0.9044(5) 0.039(4) Uani 1 1 d . . . . .
C111 C 1.1047(11) 0.7376(9) 0.8939(7) 0.095(7) Uani 1 1 d . . . . .
H11A H 1.1168 0.7419 0.8630 0.142 Uiso 1 1 calc R U . . .
H11B H 1.1454 0.7262 0.9105 0.142 Uiso 1 1 calc R U . . .
H11C H 1.0872 0.7751 0.9050 0.142 Uiso 1 1 calc R U . . .
C112 C 1.0342(8) 0.5314(8) 0.9413(5) 0.046(4) Uani 1 1 d . . . . .
H11D H 1.0191 0.4999 0.9212 0.055 Uiso 1 1 calc R U . . .
H11E H 1.0847 0.5298 0.9426 0.055 Uiso 1 1 calc R U . . .
C113 C 0.9371(10) 0.4911(7) 0.9888(6) 0.055(5) Uani 1 1 d . . . . .
H11F H 0.9173 0.4862 0.9594 0.065 Uiso 1 1 calc R U . . .
H11G H 0.9387 0.4522 1.0033 0.065 Uiso 1 1 calc R U . . .
C114 C 0.8958(10) 0.5329(10) 1.0148(8) 0.094(7) Uani 1 1 d . . . . .
H11H H 0.8580 0.5123 1.0298 0.112 Uiso 1 1 calc R U . . .
H11I H 0.8765 0.5642 0.9960 0.112 Uiso 1 1 calc R U . . .
C115 C 0.9463(9) 0.5585(9) 1.0476(6) 0.067(5) Uani 1 1 d . . . . .
H11J H 0.9517 0.5322 1.0731 0.081 Uiso 1 1 calc R U . . .
H11K H 0.9313 0.5977 1.0578 0.081 Uiso 1 1 calc R U . . .
C116 C 1.0138(8) 0.5628(7) 1.0211(5) 0.045(4) Uani 1 1 d . . . . .
H116 H 1.0183 0.6028 1.0078 0.054 Uiso 1 1 calc R U . . .
C117 C 1.0801(9) 0.5477(8) 1.0495(6) 0.050(5) Uani 1 1 d . . . . .
C118 C 1.0788(9) 0.5777(12) 1.0946(7) 0.065(6) Uani 1 1 d . . . . .
C119 C 1.0614(11) 0.6368(14) 1.1003(7) 0.084(7) Uani 1 1 d . . . . .
H119 H 1.0477 0.6576 1.0749 0.101 Uiso 1 1 calc R U . . .
C120 C 1.0622(17) 0.6682(17) 1.1391(13) 0.142(13) Uani 1 1 d . . . . .
H120 H 1.0497 0.7085 1.1403 0.171 Uiso 1 1 calc R U . . .
C121 C 1.0827(18) 0.637(2) 1.1767(17) 0.16(2) Uani 1 1 d . . . . .
H121 H 1.0840 0.6561 1.2041 0.195 Uiso 1 1 calc R U . . .
C122 C 1.1006(13) 0.579(2) 1.1738(9) 0.140(14) Uani 1 1 d . . . . .
H122 H 1.1143 0.5589 1.1997 0.168 Uiso 1 1 calc R U . . .
C123 C 1.0997(9) 0.5439(12) 1.1316(9) 0.102(8) Uani 1 1 d . . . . .
H123 H 1.1120 0.5036 1.1299 0.123 Uiso 1 1 calc R U . . .
C124 C 1.1486(10) 0.5670(12) 1.0255(5) 0.051(5) Uani 1 1 d . . . . .
C125 C 1.1576(12) 0.6245(11) 1.0105(6) 0.058(5) Uani 1 1 d . . . . .
H125 H 1.1228 0.6532 1.0140 0.070 Uiso 1 1 calc R U . . .
C126 C 1.2199(18) 0.6386(11) 0.9901(7) 0.079(6) Uani 1 1 d . . . . .
H126 H 1.2268 0.6776 0.9798 0.095 Uiso 1 1 calc R U . . .
C127 C 1.2712(16) 0.5980(19) 0.9844(8) 0.104(8) Uani 1 1 d . . . . .
H127 H 1.3126 0.6081 0.9701 0.125 Uiso 1 1 calc R U . . .
C128 C 1.2604(15) 0.5413(15) 1.0005(8) 0.090(7) Uani 1 1 d . . . . .
H128 H 1.2957 0.5129 0.9978 0.107 Uiso 1 1 calc R U . . .
C129 C 1.2002(16) 0.5254(10) 1.0202(7) 0.076(6) Uani 1 1 d . . . . .
H129 H 1.1938 0.4862 1.0301 0.092 Uiso 1 1 calc R U . . .
C136 C 0.126(3) 0.4912(14) 0.6521(10) 0.29(3) Uani 1 1 d . . . . .
H13A H 0.1071 0.5209 0.6322 0.431 Uiso 1 1 calc R U . . .
H13B H 0.1696 0.5049 0.6637 0.431 Uiso 1 1 calc R U . . .
H13C H 0.0937 0.4850 0.6763 0.431 Uiso 1 1 calc R U . . .
C143 C 0.507(2) 0.515(2) 0.9591(15) 0.26(3) Uani 1 1 d . . . . .
H14A H 0.5566 0.5091 0.9578 0.396 Uiso 1 1 calc R U . . .
H14B H 0.4967 0.5471 0.9794 0.396 Uiso 1 1 calc R U . . .
H14C H 0.4899 0.5249 0.9300 0.396 Uiso 1 1 calc R U . . .
C150 C 0.4547(16) 0.670(2) 0.9015(14) 0.39(5) Uani 1 1 d D . . . .
H15C H 0.4628 0.6323 0.9163 0.591 Uiso 1 1 calc R U . . .
H15D H 0.4976 0.6842 0.8889 0.591 Uiso 1 1 calc R U . . .
H15E H 0.4209 0.6644 0.8783 0.591 Uiso 1 1 calc R U . . .
N1 N 0.9157(7) 0.3590(6) 0.7278(4) 0.038(3) Uani 1 1 d . . . . .
N2 N 1.1235(6) 0.5317(6) 0.8132(4) 0.038(3) Uani 1 1 d . . . . .
N3 N 0.7773(6) 0.3538(5) 0.9441(4) 0.036(3) Uani 1 1 d . . . . .
N4 N 1.1264(7) 0.3408(6) 0.9373(4) 0.045(4) Uani 1 1 d . . . . .
N5 N 0.8345(7) 0.6273(5) 0.8353(4) 0.040(3) Uani 1 1 d . . . . .
N6 N 1.0072(7) 0.5171(6) 0.9860(4) 0.046(4) Uani 1 1 d . . . . .
O1 O 0.9902(6) 0.4474(5) 0.7741(3) 0.047(3) Uani 1 1 d . . . . .
O2 O 0.8769(5) 0.3807(4) 0.8199(3) 0.041(3) Uani 1 1 d . . . . .
O3 O 0.8781(5) 0.5056(4) 0.8116(3) 0.040(3) Uani 1 1 d . . . . .
O4 O 0.8349(5) 0.4514(4) 0.7350(3) 0.047(3) Uani 1 1 d . . . . .
O5 O 0.9116(5) 0.3378(4) 0.9053(4) 0.047(3) Uani 1 1 d . . . . .
O6 O 0.7635(5) 0.3313(4) 0.8601(3) 0.047(3) Uani 1 1 d . . . . .
O7 O 0.8268(4) 0.4520(4) 0.8888(3) 0.036(2) Uani 1 1 d . . . . .
O8 O 0.8978(6) 0.5584(5) 0.9032(3) 0.042(3) Uani 1 1 d . . . . .
O9 O 0.7442(5) 0.5468(5) 0.8606(4) 0.053(3) Uani 1 1 d . . . . .
O10 O 1.2123(6) 0.6124(6) 0.8392(4) 0.074(4) Uani 1 1 d . . . . .
H10I H 1.2433 0.6223 0.8565 0.112 Uiso 1 1 calc R U . . .
O11 O 1.1647(8) 0.2281(5) 0.9529(4) 0.077(4) Uani 1 1 d . . . . .
H11L H 1.1641 0.1915 0.9558 0.115 Uiso 1 1 calc R U . . .
O12 O 1.0801(7) 0.4852(6) 1.0562(4) 0.074(4) Uani 1 1 d . . . . .
H12A H 1.0609 0.4686 1.0351 0.111 Uiso 1 1 calc R U . . .
Ti1 Ti 0.89696(13) 0.43629(12) 0.78011(9) 0.0368(8) Uani 1 1 d . . . . .
Ti2 Ti 0.83864(14) 0.37442(12) 0.87721(8) 0.0394(8) Uani 1 1 d . . . . .
Ti3 Ti 0.83676(14) 0.52690(11) 0.86279(9) 0.0380(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
C130 C136 1.34(3) . ?
C130 C135 1.3900 . ?
C130 C131 1.3900 . ?
C135 C134 1.3900 . ?
C135 H135 0.9300 . ?
C134 C133 1.3900 . ?
C134 H134 0.9300 . ?
C133 C132 1.3900 . ?
C133 H133 0.9300 . ?
C132 C131 1.3900 . ?
C132 H132 0.9300 . ?
C131 H131 0.9300 . ?
C137 C143 1.34(3) . ?
C137 C142 1.3900 . ?
C137 C138 1.3900 . ?
C138 C139 1.3900 . ?
C138 H138 0.9300 . ?
C139 C140 1.3900 . ?
C139 H139 0.9300 . ?
C140 C141 1.3900 . ?
C140 H140 0.9300 . ?
C141 C142 1.3900 . ?
C141 H141 0.9300 . ?
C142 H142 0.9300 . ?
C149 C150 1.20(5) . ?
C149 C148 1.3900 . ?
C149 C144 1.3900 . ?
C148 C147 1.3900 . ?
C148 H148 0.9300 . ?
C147 C146 1.3900 . ?
C147 H147 0.9300 . ?
C146 C145 1.3900 . ?
C146 H146 0.9300 . ?
C145 C144 1.3900 . ?
C145 H145 0.9300 . ?
C144 H144 0.9300 . ?
C1 C2 1.34(2) . ?
C1 C6 1.40(2) . ?
C1 C7 1.51(2) . ?
C2 C3 1.38(2) . ?
C2 H2 0.9300 . ?
C3 C4 1.33(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.36(3) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 O4 1.413(16) . ?
C7 C8 1.53(2) . ?
C7 C14 1.54(2) . ?
C8 C9 1.33(2) . ?
C8 C13 1.39(3) . ?
C9 C10 1.40(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.36(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.29(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.40(3) . ?
C12 H12 0.9300 . ?
C13 H13 0.9300 . ?
C14 C15 1.50(2) . ?
C14 N1 1.500(18) . ?
C14 H14 0.9800 . ?
C15 C16 1.51(2) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.50(2) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 N1 1.472(18) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 N1 1.481(18) . ?
C18 C19 1.49(2) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.35(2) . ?
C19 C24 1.42(2) . ?
C20 C21 1.38(2) . ?
C20 H20 0.9300 . ?
C21 C22 1.38(2) . ?
C21 C86 1.53(2) . ?
C22 C23 1.37(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.41(2) . ?
C23 C25 1.52(2) . ?
C24 O1 1.332(18) . ?
C25 N2 1.456(18) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.38(3) . ?
C26 N2 1.478(19) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.43(3) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 C29 1.54(2) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 N2 1.455(19) . ?
C29 C30 1.57(2) . ?
C29 H29 0.9800 . ?
C30 O10 1.45(2) . ?
C30 C31 1.49(2) . ?
C30 C37 1.50(3) . ?
C31 C32 1.38(2) . ?
C31 C36 1.40(3) . ?
C32 C33 1.35(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.38(3) . ?
C33 H33 0.9300 . ?
C34 C35 1.35(3) . ?
C34 H34 0.9300 . ?
C35 C36 1.38(3) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
C37 C42 1.36(3) . ?
C37 C38 1.38(3) . ?
C38 C39 1.36(3) . ?
C38 H38 0.9300 . ?
C39 C40 1.39(4) . ?
C39 H39 0.9300 . ?
C40 C41 1.38(4) . ?
C40 H40 0.9300 . ?
C41 C42 1.37(3) . ?
C41 H41 0.9300 . ?
C42 H42 0.9300 . ?
C43 C44 1.39(3) . ?
C43 C48 1.39(2) . ?
C43 H43 0.9300 . ?
C44 C45 1.36(3) . ?
C44 H44 0.9300 . ?
C45 C46 1.36(3) . ?
C45 H45 0.9300 . ?
C46 C47 1.35(3) . ?
C46 H46 0.9300 . ?
C47 C48 1.37(2) . ?
C47 H47 0.9300 . ?
C48 C49 1.52(2) . ?
C49 O6 1.396(17) . ?
C49 C50 1.54(2) . ?
C49 C56 1.58(2) . ?
C50 C55 1.36(2) . ?
C50 C51 1.40(2) . ?
C51 C52 1.38(2) . ?
C51 H51 0.9300 . ?
C52 C53 1.32(2) . ?
C52 H52 0.9300 . ?
C53 C54 1.39(2) . ?
C53 H53 0.9300 . ?
C54 C55 1.34(2) . ?
C54 H54 0.9300 . ?
C55 H55 0.9300 . ?
C56 C57 1.46(2) . ?
C56 N3 1.496(18) . ?
C56 H56 0.9800 . ?
C57 C58 1.50(2) . ?
C57 H57A 0.9700 . ?
C57 H57B 0.9700 . ?
C58 C59 1.46(2) . ?
C58 H58A 0.9700 . ?
C58 H58B 0.9700 . ?
C59 N3 1.509(18) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 N3 1.480(19) . ?
C60 C61 1.49(2) . ?
C60 H60A 0.9700 . ?
C60 H60B 0.9700 . ?
C61 C66 1.38(2) . ?
C61 C62 1.42(2) . ?
C62 C63 1.34(2) . ?
C62 H62 0.9300 . ?
C63 C64 1.40(2) . ?
C63 C67 1.52(2) . ?
C64 C65 1.40(2) . ?
C64 H64 0.9300 . ?
C65 C66 1.35(2) . ?
C65 C68 1.50(2) . ?
C66 O5 1.37(2) . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?
C68 N4 1.469(19) . ?
C68 H68A 0.9700 . ?
C68 H68B 0.9700 . ?
C69 N4 1.444(19) . ?
C69 C70 1.49(2) . ?
C69 H69A 0.9700 . ?
C69 H69B 0.9700 . ?
C70 C71 1.54(2) . ?
C70 H70A 0.9700 . ?
C70 H70B 0.9700 . ?
C71 C78 1.52(2) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C72 C77 1.39(2) . ?
C72 C73 1.39(2) . ?
C72 C79 1.53(2) . ?
C73 C74 1.35(2) . ?
C73 H73 0.9300 . ?
C74 C75 1.34(3) . ?
C74 H74 0.9300 . ?
C75 C76 1.34(3) . ?
C75 H75 0.9300 . ?
C76 C77 1.38(3) . ?
C76 H76 0.9300 . ?
C77 H77 0.9300 . ?
C78 N4 1.477(19) . ?
C78 C79 1.56(2) . ?
C78 H78 0.9800 . ?
C79 O11 1.409(18) . ?
C79 C80 1.52(3) . ?
C80 C81 1.35(3) . ?
C80 C85 1.39(3) . ?
C81 C82 1.44(4) . ?
C81 H81 0.9300 . ?
C82 C83 1.41(4) . ?
C82 H82 0.9300 . ?
C83 C84 1.29(4) . ?
C83 H83 0.9300 . ?
C84 C85 1.41(3) . ?
C84 H84 0.9300 . ?
C85 H85 0.9300 . ?
C86 H86A 0.9600 . ?
C86 H86B 0.9600 . ?
C86 H86C 0.9600 . ?
C87 C92 1.36(3) . ?
C87 C88 1.41(3) . ?
C87 H87 0.9300 . ?
C88 C89 1.36(3) . ?
C88 H88 0.9300 . ?
C89 C90 1.34(4) . ?
C89 H89 0.9300 . ?
C90 C91 1.36(3) . ?
C90 H90 0.9300 . ?
C91 C92 1.42(3) . ?
C91 H91 0.9300 . ?
C92 C93 1.51(2) . ?
C93 O9 1.410(17) . ?
C93 C100 1.51(2) . ?
C93 C94 1.54(3) . ?
C94 C99 1.37(3) . ?
C94 C95 1.38(3) . ?
C95 C96 1.39(4) . ?
C95 H95 0.9300 . ?
C96 C97 1.27(4) . ?
C96 H96 0.9300 . ?
C97 C98 1.38(4) . ?
C97 H97 0.9300 . ?
C98 C99 1.41(3) . ?
C98 H98 0.9300 . ?
C99 H99 0.9300 . ?
C100 N5 1.480(18) . ?
C100 C101 1.54(2) . ?
C100 H100 0.9800 . ?
C101 C102 1.45(2) . ?
C101 H10A 0.9700 . ?
C101 H10B 0.9700 . ?
C102 C103 1.50(2) . ?
C102 H10C 0.9700 . ?
C102 H10D 0.9700 . ?
C103 N5 1.459(19) . ?
C103 H10E 0.9700 . ?
C103 H10F 0.9700 . ?
C104 N5 1.493(18) . ?
C104 C105 1.51(2) . ?
C104 H10G 0.9700 . ?
C104 H10H 0.9700 . ?
C105 C106 1.37(2) . ?
C105 C110 1.42(2) . ?
C106 C107 1.39(2) . ?
C106 H106 0.9300 . ?
C107 C108 1.37(2) . ?
C107 C111 1.51(2) . ?
C108 C109 1.37(2) . ?
C108 H108 0.9300 . ?
C109 C110 1.39(2) . ?
C109 C112 1.49(2) . ?
C110 O8 1.364(19) . ?
C111 H11A 0.9600 . ?
C111 H11B 0.9600 . ?
C111 H11C 0.9600 . ?
C112 N6 1.473(19) . ?
C112 H11D 0.9700 . ?
C112 H11E 0.9700 . ?
C113 C114 1.45(2) . ?
C113 N6 1.464(19) . ?
C113 H11F 0.9700 . ?
C113 H11G 0.9700 . ?
C114 C115 1.50(2) . ?
C114 H11H 0.9700 . ?
C114 H11I 0.9700 . ?
C115 C116 1.52(2) . ?
C115 H11J 0.9700 . ?
C115 H11K 0.9700 . ?
C116 N6 1.472(18) . ?
C116 C117 1.57(2) . ?
C116 H116 0.9800 . ?
C117 O12 1.407(17) . ?
C117 C118 1.51(2) . ?
C117 C124 1.56(2) . ?
C118 C119 1.37(3) . ?
C118 C123 1.40(3) . ?
C119 C120 1.36(3) . ?
C119 H119 0.9300 . ?
C120 C121 1.38(5) . ?
C120 H120 0.9300 . ?
C121 C122 1.34(4) . ?
C121 H121 0.9300 . ?
C122 C123 1.48(4) . ?
C122 H122 0.9300 . ?
C123 H123 0.9300 . ?
C124 C129 1.36(2) . ?
C124 C125 1.37(2) . ?
C125 C126 1.38(3) . ?
C125 H125 0.9300 . ?
C126 C127 1.35(3) . ?
C126 H126 0.9300 . ?
C127 C128 1.37(3) . ?
C127 H127 0.9300 . ?
C128 C129 1.34(3) . ?
C128 H128 0.9300 . ?
C129 H129 0.9300 . ?
C136 H13A 0.9600 . ?
C136 H13B 0.9600 . ?
C136 H13C 0.9600 . ?
C143 H14A 0.9600 . ?
C143 H14B 0.9600 . ?
C143 H14C 0.9600 . ?
C150 H15C 0.9600 . ?
C150 H15D 0.9600 . ?
C150 H15E 0.9600 . ?
N1 Ti1 2.358(12) . ?
N3 Ti2 2.372(12) . ?
N5 Ti3 2.384(12) . ?
O1 Ti1 1.814(11) . ?
O2 Ti1 1.764(10) . ?
O2 Ti2 1.875(9) . ?
O3 Ti3 1.792(10) . ?
O3 Ti1 1.847(10) . ?
O4 Ti1 1.835(10) . ?
O5 Ti2 1.827(12) . ?
O6 Ti2 1.806(10) . ?
O7 Ti2 1.777(9) . ?
O7 Ti3 1.853(9) . ?
O8 Ti3 1.825(11) . ?
O9 Ti3 1.829(11) . ?
O10 H10I 0.8200 . ?
O11 H11L 0.8200 . ?
O12 H12A 0.8200 . ?

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
C136 C130 C135 118(2) . . ?
C136 C130 C131 122(2) . . ?
C135 C130 C131 120.0 . . ?
C130 C135 C134 120.0 . . ?
C130 C135 H135 120.0 . . ?
C134 C135 H135 120.0 . . ?
C133 C134 C135 120.0 . . ?
C133 C134 H134 120.0 . . ?
C135 C134 H134 120.0 . . ?
C134 C133 C132 120.0 . . ?
C134 C133 H133 120.0 . . ?
C132 C133 H133 120.0 . . ?
C131 C132 C133 120.0 . . ?
C131 C132 H132 120.0 . . ?
C133 C132 H132 120.0 . . ?
C132 C131 C130 120.0 . . ?
C132 C131 H131 120.0 . . ?
C130 C131 H131 120.0 . . ?
C143 C137 C142 113(2) . . ?
C143 C137 C138 127(2) . . ?
C142 C137 C138 120.0 . . ?
C139 C138 C137 120.0 . . ?
C139 C138 H138 120.0 . . ?
C137 C138 H138 120.0 . . ?
C140 C139 C138 120.0 . . ?
C140 C139 H139 120.0 . . ?
C138 C139 H139 120.0 . . ?
C139 C140 C141 120.0 . . ?
C139 C140 H140 120.0 . . ?
C141 C140 H140 120.0 . . ?
C142 C141 C140 120.0 . . ?
C142 C141 H141 120.0 . . ?
C140 C141 H141 120.0 . . ?
C141 C142 C137 120.0 . . ?
C141 C142 H142 120.0 . . ?
C137 C142 H142 120.0 . . ?
C150 C149 C148 120.01(15) . . ?
C150 C149 C144 119.97(15) . . ?
C148 C149 C144 120.0 . . ?
C149 C148 C147 120.0 . . ?
C149 C148 H148 120.0 . . ?
C147 C148 H148 120.0 . . ?
C148 C147 C146 120.0 . . ?
C148 C147 H147 120.0 . . ?
C146 C147 H147 120.0 . . ?
C147 C146 C145 120.0 . . ?
C147 C146 H146 120.0 . . ?
C145 C146 H146 120.0 . . ?
C144 C145 C146 120.0 . . ?
C144 C145 H145 120.0 . . ?
C146 C145 H145 120.0 . . ?
C145 C144 C149 120.0 . . ?
C145 C144 H144 120.0 . . ?
C149 C144 H144 120.0 . . ?
C2 C1 C6 118.0(17) . . ?
C2 C1 C7 122(2) . . ?
C6 C1 C7 120(2) . . ?
C1 C2 C3 120(2) . . ?
C1 C2 H2 120.2 . . ?
C3 C2 H2 120.2 . . ?
C4 C3 C2 122(2) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 119(2) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 119(2) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C1 122(2) . . ?
C5 C6 H6 119.1 . . ?
C1 C6 H6 119.1 . . ?
O4 C7 C1 108.0(14) . . ?
O4 C7 C8 107.9(13) . . ?
C1 C7 C8 107.8(13) . . ?
O4 C7 C14 104.8(13) . . ?
C1 C7 C14 114.4(14) . . ?
C8 C7 C14 113.5(14) . . ?
C9 C8 C13 116.0(18) . . ?
C9 C8 C7 123.7(19) . . ?
C13 C8 C7 120(2) . . ?
C8 C9 C10 124(2) . . ?
C8 C9 H9 118.0 . . ?
C10 C9 H9 118.0 . . ?
C11 C10 C9 116(2) . . ?
C11 C10 H10 121.8 . . ?
C9 C10 H10 121.8 . . ?
C12 C11 C10 123(3) . . ?
C12 C11 H11 118.6 . . ?
C10 C11 H11 118.6 . . ?
C11 C12 C13 120(2) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C8 C13 C12 121(2) . . ?
C8 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C15 C14 N1 102.5(13) . . ?
C15 C14 C7 113.7(14) . . ?
N1 C14 C7 111.0(13) . . ?
C15 C14 H14 109.8 . . ?
N1 C14 H14 109.8 . . ?
C7 C14 H14 109.8 . . ?
C14 C15 C16 106.5(14) . . ?
C14 C15 H15A 110.4 . . ?
C16 C15 H15A 110.4 . . ?
C14 C15 H15B 110.4 . . ?
C16 C15 H15B 110.4 . . ?
H15A C15 H15B 108.6 . . ?
C17 C16 C15 106.0(14) . . ?
C17 C16 H16A 110.5 . . ?
C15 C16 H16A 110.5 . . ?
C17 C16 H16B 110.5 . . ?
C15 C16 H16B 110.5 . . ?
H16A C16 H16B 108.7 . . ?
N1 C17 C16 106.4(14) . . ?
N1 C17 H17A 110.5 . . ?
C16 C17 H17A 110.5 . . ?
N1 C17 H17B 110.5 . . ?
C16 C17 H17B 110.5 . . ?
H17A C17 H17B 108.6 . . ?
N1 C18 C19 114.3(12) . . ?
N1 C18 H18A 108.7 . . ?
C19 C18 H18A 108.7 . . ?
N1 C18 H18B 108.7 . . ?
C19 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C20 C19 C24 120.1(16) . . ?
C20 C19 C18 125.0(19) . . ?
C24 C19 C18 114.7(18) . . ?
C19 C20 C21 122.1(16) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 H20 119.0 . . ?
C22 C21 C20 117.5(15) . . ?
C22 C21 C86 124(2) . . ?
C20 C21 C86 118.6(19) . . ?
C23 C22 C21 123.1(16) . . ?
C23 C22 H22 118.5 . . ?
C21 C22 H22 118.5 . . ?
C22 C23 C24 118.6(15) . . ?
C22 C23 C25 118.9(19) . . ?
C24 C23 C25 122.5(17) . . ?
O1 C24 C23 120.6(18) . . ?
O1 C24 C19 120.8(18) . . ?
C23 C24 C19 118.6(17) . . ?
N2 C25 C23 119.3(12) . . ?
N2 C25 H25A 107.5 . . ?
C23 C25 H25A 107.5 . . ?
N2 C25 H25B 107.5 . . ?
C23 C25 H25B 107.5 . . ?
H25A C25 H25B 107.0 . . ?
C27 C26 N2 104.2(17) . . ?
C27 C26 H26A 110.9 . . ?
N2 C26 H26A 110.9 . . ?
C27 C26 H26B 110.9 . . ?
N2 C26 H26B 110.9 . . ?
H26A C26 H26B 108.9 . . ?
C26 C27 C28 115(2) . . ?
C26 C27 H27A 108.6 . . ?
C28 C27 H27A 108.6 . . ?
C26 C27 H27B 108.6 . . ?
C28 C27 H27B 108.6 . . ?
H27A C27 H27B 107.6 . . ?
C27 C28 C29 101.8(16) . . ?
C27 C28 H28A 111.4 . . ?
C29 C28 H28A 111.4 . . ?
C27 C28 H28B 111.4 . . ?
C29 C28 H28B 111.4 . . ?
H28A C28 H28B 109.3 . . ?
N2 C29 C28 105.6(13) . . ?
N2 C29 C30 109.3(13) . . ?
C28 C29 C30 111.7(14) . . ?
N2 C29 H29 110.0 . . ?
C28 C29 H29 110.0 . . ?
C30 C29 H29 110.0 . . ?
O10 C30 C31 110.7(15) . . ?
O10 C30 C37 107.5(17) . . ?
C31 C30 C37 109.7(15) . . ?
O10 C30 C29 103.4(14) . . ?
C31 C30 C29 111.6(15) . . ?
C37 C30 C29 113.6(15) . . ?
C32 C31 C36 114.1(18) . . ?
C32 C31 C30 124(2) . . ?
C36 C31 C30 122(2) . . ?
C33 C32 C31 124(2) . . ?
C33 C32 H32 118.0 . . ?
C31 C32 H32 118.0 . . ?
C32 C33 C34 120(2) . . ?
C32 C33 H33 119.9 . . ?
C34 C33 H33 119.9 . . ?
C35 C34 C33 118(2) . . ?
C35 C34 H34 120.9 . . ?
C33 C34 H34 120.9 . . ?
C34 C35 C36 121(2) . . ?
C34 C35 H35 119.4 . . ?
C36 C35 H35 119.4 . . ?
C35 C36 C31 122(2) . . ?
C35 C36 H36 119.1 . . ?
C31 C36 H36 119.1 . . ?
C42 C37 C38 115(2) . . ?
C42 C37 C30 123(2) . . ?
C38 C37 C30 122(2) . . ?
C39 C38 C37 127(2) . . ?
C39 C38 H38 116.5 . . ?
C37 C38 H38 116.5 . . ?
C38 C39 C40 113(3) . . ?
C38 C39 H39 123.3 . . ?
C40 C39 H39 123.4 . . ?
C41 C40 C39 124(3) . . ?
C41 C40 H40 117.8 . . ?
C39 C40 H40 117.8 . . ?
C42 C41 C40 116(3) . . ?
C42 C41 H41 121.9 . . ?
C40 C41 H41 121.9 . . ?
C37 C42 C41 124(3) . . ?
C37 C42 H42 117.9 . . ?
C41 C42 H42 117.9 . . ?
C44 C43 C48 122(2) . . ?
C44 C43 H43 119.0 . . ?
C48 C43 H43 119.0 . . ?
C45 C44 C43 119(2) . . ?
C45 C44 H44 120.5 . . ?
C43 C44 H44 120.5 . . ?
C46 C45 C44 121(2) . . ?
C46 C45 H45 119.7 . . ?
C44 C45 H45 119.7 . . ?
C47 C46 C45 119(2) . . ?
C47 C46 H46 120.4 . . ?
C45 C46 H46 120.4 . . ?
C46 C47 C48 124.2(19) . . ?
C46 C47 H47 117.9 . . ?
C48 C47 H47 117.9 . . ?
C47 C48 C43 114.9(17) . . ?
C47 C48 C49 122.1(19) . . ?
C43 C48 C49 122.9(19) . . ?
O6 C49 C48 107.8(14) . . ?
O6 C49 C50 110.7(14) . . ?
C48 C49 C50 109.7(13) . . ?
O6 C49 C56 105.7(12) . . ?
C48 C49 C56 109.6(13) . . ?
C50 C49 C56 113.2(14) . . ?
C55 C50 C51 116.9(17) . . ?
C55 C50 C49 123.3(19) . . ?
C51 C50 C49 119.8(19) . . ?
C52 C51 C50 119.5(16) . . ?
C52 C51 H51 120.3 . . ?
C50 C51 H51 120.3 . . ?
C53 C52 C51 123.9(18) . . ?
C53 C52 H52 118.0 . . ?
C51 C52 H52 118.0 . . ?
C52 C53 C54 115.3(18) . . ?
C52 C53 H53 122.3 . . ?
C54 C53 H53 122.3 . . ?
C55 C54 C53 123.3(18) . . ?
C55 C54 H54 118.3 . . ?
C53 C54 H54 118.3 . . ?
C54 C55 C50 121.0(16) . . ?
C54 C55 H55 119.5 . . ?
C50 C55 H55 119.5 . . ?
C57 C56 N3 103.4(12) . . ?
C57 C56 C49 115.4(14) . . ?
N3 C56 C49 108.0(12) . . ?
C57 C56 H56 109.9 . . ?
N3 C56 H56 109.9 . . ?
C49 C56 H56 109.9 . . ?
C56 C57 C58 104.0(15) . . ?
C56 C57 H57A 111.0 . . ?
C58 C57 H57A 111.0 . . ?
C56 C57 H57B 110.9 . . ?
C58 C57 H57B 111.0 . . ?
H57A C57 H57B 109.0 . . ?
C59 C58 C57 106.0(14) . . ?
C59 C58 H58A 110.5 . . ?
C57 C58 H58A 110.5 . . ?
C59 C58 H58B 110.5 . . ?
C57 C58 H58B 110.5 . . ?
H58A C58 H58B 108.7 . . ?
C58 C59 N3 107.1(13) . . ?
C58 C59 H59A 110.3 . . ?
N3 C59 H59A 110.3 . . ?
C58 C59 H59B 110.3 . . ?
N3 C59 H59B 110.3 . . ?
H59A C59 H59B 108.5 . . ?
N3 C60 C61 111.3(13) . . ?
N3 C60 H60A 109.4 . . ?
C61 C60 H60A 109.4 . . ?
N3 C60 H60B 109.4 . . ?
C61 C60 H60B 109.4 . . ?
H60A C60 H60B 108.0 . . ?
C66 C61 C62 118.6(17) . . ?
C66 C61 C60 121.5(18) . . ?
C62 C61 C60 120(2) . . ?
C63 C62 C61 121.5(17) . . ?
C63 C62 H62 119.2 . . ?
C61 C62 H62 119.3 . . ?
C62 C63 C64 118.0(16) . . ?
C62 C63 C67 123(2) . . ?
C64 C63 C67 119(2) . . ?
C65 C64 C63 121.4(16) . . ?
C65 C64 H64 119.3 . . ?
C63 C64 H64 119.3 . . ?
C66 C65 C64 119.1(17) . . ?
C66 C65 C68 117.1(19) . . ?
C64 C65 C68 124(2) . . ?
C65 C66 O5 123.1(18) . . ?
C65 C66 C61 120.9(19) . . ?
O5 C66 C61 116.0(19) . . ?
C63 C67 H67A 109.5 . . ?
C63 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C63 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N4 C68 C65 113.5(15) . . ?
N4 C68 H68A 108.9 . . ?
C65 C68 H68A 108.9 . . ?
N4 C68 H68B 108.9 . . ?
C65 C68 H68B 108.9 . . ?
H68A C68 H68B 107.7 . . ?
N4 C69 C70 104.9(14) . . ?
N4 C69 H69A 110.8 . . ?
C70 C69 H69A 110.8 . . ?
N4 C69 H69B 110.8 . . ?
C70 C69 H69B 110.8 . . ?
H69A C69 H69B 108.8 . . ?
C69 C70 C71 101.5(14) . . ?
C69 C70 H70A 111.5 . . ?
C71 C70 H70A 111.5 . . ?
C69 C70 H70B 111.5 . . ?
C71 C70 H70B 111.5 . . ?
H70A C70 H70B 109.3 . . ?
C78 C71 C70 105.5(14) . . ?
C78 C71 H71A 110.6 . . ?
C70 C71 H71A 110.6 . . ?
C78 C71 H71B 110.6 . . ?
C70 C71 H71B 110.6 . . ?
H71A C71 H71B 108.8 . . ?
C77 C72 C73 116.7(17) . . ?
C77 C72 C79 125(2) . . ?
C73 C72 C79 118(2) . . ?
C74 C73 C72 121.5(19) . . ?
C74 C73 H73 119.2 . . ?
C72 C73 H73 119.2 . . ?
C75 C74 C73 122(2) . . ?
C75 C74 H74 119.2 . . ?
C73 C74 H74 119.2 . . ?
C76 C75 C74 118(2) . . ?
C76 C75 H75 120.9 . . ?
C74 C75 H75 120.9 . . ?
C75 C76 C77 122(2) . . ?
C75 C76 H76 118.8 . . ?
C77 C76 H76 118.8 . . ?
C76 C77 C72 119.4(18) . . ?
C76 C77 H77 120.3 . . ?
C72 C77 H77 120.3 . . ?
N4 C78 C71 105.5(13) . . ?
N4 C78 C79 109.8(13) . . ?
C71 C78 C79 113.3(14) . . ?
N4 C78 H78 109.4 . . ?
C71 C78 H78 109.4 . . ?
C79 C78 H78 109.4 . . ?
O11 C79 C80 109.4(15) . . ?
O11 C79 C72 108.9(16) . . ?
C80 C79 C72 106.5(14) . . ?
O11 C79 C78 105.5(13) . . ?
C80 C79 C78 114.6(17) . . ?
C72 C79 C78 111.9(13) . . ?
C81 C80 C85 120(2) . . ?
C81 C80 C79 118(3) . . ?
C85 C80 C79 122(2) . . ?
C80 C81 C82 119(3) . . ?
C80 C81 H81 120.5 . . ?
C82 C81 H81 120.5 . . ?
C83 C82 C81 120(3) . . ?
C83 C82 H82 119.8 . . ?
C81 C82 H82 119.8 . . ?
C84 C83 C82 119(3) . . ?
C84 C83 H83 120.7 . . ?
C82 C83 H83 120.7 . . ?
C83 C84 C85 123(4) . . ?
C83 C84 H84 118.6 . . ?
C85 C84 H84 118.6 . . ?
C80 C85 C84 119(2) . . ?
C80 C85 H85 120.3 . . ?
C84 C85 H85 120.3 . . ?
C21 C86 H86A 109.5 . . ?
C21 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C21 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C92 C87 C88 121(2) . . ?
C92 C87 H87 119.3 . . ?
C88 C87 H87 119.3 . . ?
C89 C88 C87 120(2) . . ?
C89 C88 H88 119.8 . . ?
C87 C88 H88 119.8 . . ?
C90 C89 C88 120(3) . . ?
C90 C89 H89 119.9 . . ?
C88 C89 H89 119.9 . . ?
C89 C90 C91 119(3) . . ?
C89 C90 H90 120.5 . . ?
C91 C90 H90 120.5 . . ?
C90 C91 C92 124(2) . . ?
C90 C91 H91 118.0 . . ?
C92 C91 H91 118.0 . . ?
C87 C92 C91 114.8(19) . . ?
C87 C92 C93 123(2) . . ?
C91 C92 C93 122(2) . . ?
O9 C93 C92 107.8(14) . . ?
O9 C93 C100 106.4(13) . . ?
C92 C93 C100 112.2(15) . . ?
O9 C93 C94 110.3(15) . . ?
C92 C93 C94 107.2(14) . . ?
C100 C93 C94 112.8(15) . . ?
C99 C94 C95 119(2) . . ?
C99 C94 C93 124(2) . . ?
C95 C94 C93 118(2) . . ?
C94 C95 C96 121(3) . . ?
C94 C95 H95 119.7 . . ?
C96 C95 H95 119.7 . . ?
C97 C96 C95 119(4) . . ?
C97 C96 H96 120.7 . . ?
C95 C96 H96 120.7 . . ?
C96 C97 C98 126(4) . . ?
C96 C97 H97 117.2 . . ?
C98 C97 H97 117.2 . . ?
C97 C98 C99 116(3) . . ?
C97 C98 H98 122.1 . . ?
C99 C98 H98 122.1 . . ?
C94 C99 C98 121(2) . . ?
C94 C99 H99 119.7 . . ?
C98 C99 H99 119.7 . . ?
N5 C100 C93 110.5(13) . . ?
N5 C100 C101 101.2(13) . . ?
C93 C100 C101 113.7(15) . . ?
N5 C100 H100 110.4 . . ?
C93 C100 H100 110.4 . . ?
C101 C100 H100 110.4 . . ?
C102 C101 C100 106.3(15) . . ?
C102 C101 H10A 110.5 . . ?
C100 C101 H10A 110.5 . . ?
C102 C101 H10B 110.5 . . ?
C100 C101 H10B 110.5 . . ?
H10A C101 H10B 108.7 . . ?
C101 C102 C103 107.1(15) . . ?
C101 C102 H10C 110.3 . . ?
C103 C102 H10C 110.3 . . ?
C101 C102 H10D 110.3 . . ?
C103 C102 H10D 110.3 . . ?
H10C C102 H10D 108.6 . . ?
N5 C103 C102 105.6(13) . . ?
N5 C103 H10E 110.6 . . ?
C102 C103 H10E 110.6 . . ?
N5 C103 H10F 110.6 . . ?
C102 C103 H10F 110.6 . . ?
H10E C103 H10F 108.8 . . ?
N5 C104 C105 112.9(12) . . ?
N5 C104 H10G 109.0 . . ?
C105 C104 H10G 109.0 . . ?
N5 C104 H10H 109.0 . . ?
C105 C104 H10H 109.0 . . ?
H10G C104 H10H 107.8 . . ?
C106 C105 C110 117.7(17) . . ?
C106 C105 C104 124.4(19) . . ?
C110 C105 C104 117.9(17) . . ?
C105 C106 C107 122.1(16) . . ?
C105 C106 H106 119.0 . . ?
C107 C106 H106 119.0 . . ?
C108 C107 C106 117.5(15) . . ?
C108 C107 C111 123(2) . . ?
C106 C107 C111 120(2) . . ?
C107 C108 C109 124.1(16) . . ?
C107 C108 H108 118.0 . . ?
C109 C108 H108 118.0 . . ?
C108 C109 C110 116.9(15) . . ?
C108 C109 C112 119.9(19) . . ?
C110 C109 C112 123.2(17) . . ?
O8 C110 C109 121.2(18) . . ?
O8 C110 C105 117.3(18) . . ?
C109 C110 C105 121.5(16) . . ?
C107 C111 H11A 109.5 . . ?
C107 C111 H11B 109.5 . . ?
H11A C111 H11B 109.5 . . ?
C107 C111 H11C 109.5 . . ?
H11A C111 H11C 109.5 . . ?
H11B C111 H11C 109.5 . . ?
N6 C112 C109 117.7(13) . . ?
N6 C112 H11D 107.9 . . ?
C109 C112 H11D 107.9 . . ?
N6 C112 H11E 107.9 . . ?
C109 C112 H11E 107.9 . . ?
H11D C112 H11E 107.2 . . ?
C114 C113 N6 106.2(14) . . ?
C114 C113 H11F 110.5 . . ?
N6 C113 H11F 110.5 . . ?
C114 C113 H11G 110.5 . . ?
N6 C113 H11G 110.5 . . ?
H11F C113 H11G 108.7 . . ?
C113 C114 C115 104.2(15) . . ?
C113 C114 H11H 110.9 . . ?
C115 C114 H11H 110.9 . . ?
C113 C114 H11I 110.9 . . ?
C115 C114 H11I 110.9 . . ?
H11H C114 H11I 108.9 . . ?
C114 C115 C116 103.2(14) . . ?
C114 C115 H11J 111.1 . . ?
C116 C115 H11J 111.1 . . ?
C114 C115 H11K 111.1 . . ?
C116 C115 H11K 111.1 . . ?
H11J C115 H11K 109.1 . . ?
N6 C116 C115 104.9(13) . . ?
N6 C116 C117 108.2(12) . . ?
C115 C116 C117 113.1(13) . . ?
N6 C116 H116 110.2 . . ?
C115 C116 H116 110.2 . . ?
C117 C116 H116 110.2 . . ?
O12 C117 C118 107.9(16) . . ?
O12 C117 C124 109.8(15) . . ?
C118 C117 C124 107.9(14) . . ?
O12 C117 C116 106.9(13) . . ?
C118 C117 C116 112.3(15) . . ?
C124 C117 C116 112.0(14) . . ?
C119 C118 C123 119(2) . . ?
C119 C118 C117 123(2) . . ?
C123 C118 C117 118(2) . . ?
C120 C119 C118 127(3) . . ?
C120 C119 H119 116.7 . . ?
C118 C119 H119 116.7 . . ?
C119 C120 C121 116(4) . . ?
C119 C120 H120 121.9 . . ?
C121 C120 H120 121.9 . . ?
C122 C121 C120 120(4) . . ?
C122 C121 H121 119.8 . . ?
C120 C121 H121 119.8 . . ?
C121 C122 C123 124(3) . . ?
C121 C122 H122 118.2 . . ?
C123 C122 H122 118.2 . . ?
C118 C123 C122 114(2) . . ?
C118 C123 H123 123.1 . . ?
C122 C123 H123 123.1 . . ?
C129 C124 C125 120.3(18) . . ?
C129 C124 C117 119(2) . . ?
C125 C124 C117 121(2) . . ?
C124 C125 C126 117.9(18) . . ?
C124 C125 H125 121.0 . . ?
C126 C125 H125 121.0 . . ?
C127 C126 C125 122(2) . . ?
C127 C126 H126 118.8 . . ?
C125 C126 H126 118.8 . . ?
C126 C127 C128 118(3) . . ?
C126 C127 H127 121.2 . . ?
C128 C127 H127 121.2 . . ?
C129 C128 C127 122(2) . . ?
C129 C128 H128 119.0 . . ?
C127 C128 H128 119.0 . . ?
C128 C129 C124 120(2) . . ?
C128 C129 H129 120.2 . . ?
C124 C129 H129 120.2 . . ?
C130 C136 H13A 109.5 . . ?
C130 C136 H13B 109.5 . . ?
H13A C136 H13B 109.5 . . ?
C130 C136 H13C 109.5 . . ?
H13A C136 H13C 109.5 . . ?
H13B C136 H13C 109.5 . . ?
C137 C143 H14A 109.5 . . ?
C137 C143 H14B 109.5 . . ?
H14A C143 H14B 109.5 . . ?
C137 C143 H14C 109.5 . . ?
H14A C143 H14C 109.5 . . ?
H14B C143 H14C 109.5 . . ?
C149 C150 H15C 109.5 . . ?
C149 C150 H15D 109.5 . . ?
H15C C150 H15D 109.5 . . ?
C149 C150 H15E 109.5 . . ?
H15C C150 H15E 109.5 . . ?
H15D C150 H15E 109.5 . . ?
C17 N1 C18 110.7(12) . . ?
C17 N1 C14 106.0(12) . . ?
C18 N1 C14 113.5(12) . . ?
C17 N1 Ti1 114.6(9) . . ?
C18 N1 Ti1 108.1(8) . . ?
C14 N1 Ti1 103.9(9) . . ?
C29 N2 C25 117.3(12) . . ?
C29 N2 C26 109.2(13) . . ?
C25 N2 C26 116.1(12) . . ?
C60 N3 C56 114.1(12) . . ?
C60 N3 C59 110.3(12) . . ?
C56 N3 C59 103.5(11) . . ?
C60 N3 Ti2 108.0(9) . . ?
C56 N3 Ti2 104.4(9) . . ?
C59 N3 Ti2 116.5(9) . . ?
C69 N4 C68 114.1(13) . . ?
C69 N4 C78 104.6(13) . . ?
C68 N4 C78 118.3(13) . . ?
C103 N5 C100 106.3(12) . . ?
C103 N5 C104 108.8(12) . . ?
C100 N5 C104 111.5(12) . . ?
C103 N5 Ti3 117.2(10) . . ?
C100 N5 Ti3 104.3(9) . . ?
C104 N5 Ti3 108.6(8) . . ?
C113 N6 C116 108.1(13) . . ?
C113 N6 C112 117.5(13) . . ?
C116 N6 C112 118.2(13) . . ?
C24 O1 Ti1 139.3(10) . . ?
Ti1 O2 Ti2 139.5(5) . . ?
Ti3 O3 Ti1 138.4(5) . . ?
C7 O4 Ti1 132.5(9) . . ?
C66 O5 Ti2 136.1(10) . . ?
C49 O6 Ti2 132.9(9) . . ?
Ti2 O7 Ti3 141.2(5) . . ?
C110 O8 Ti3 137.8(10) . . ?
C93 O9 Ti3 129.8(9) . . ?
C30 O10 H10I 109.5 . . ?
C79 O11 H11L 109.5 . . ?
C117 O12 H12A 109.5 . . ?
O2 Ti1 O1 112.3(5) . . ?
O2 Ti1 O4 119.2(4) . . ?
O1 Ti1 O4 122.7(5) . . ?
O2 Ti1 O3 101.3(4) . . ?
O1 Ti1 O3 97.5(5) . . ?
O4 Ti1 O3 95.7(4) . . ?
O2 Ti1 N1 88.5(4) . . ?
O1 Ti1 N1 83.3(5) . . ?
O4 Ti1 N1 74.9(4) . . ?
O3 Ti1 N1 169.0(5) . . ?
O7 Ti2 O6 118.0(4) . . ?
O7 Ti2 O5 116.2(4) . . ?
O6 Ti2 O5 120.3(5) . . ?
O7 Ti2 O2 99.0(4) . . ?
O6 Ti2 O2 95.2(4) . . ?
O5 Ti2 O2 99.1(5) . . ?
O7 Ti2 N3 87.6(4) . . ?
O6 Ti2 N3 75.1(4) . . ?
O5 Ti2 N3 84.4(4) . . ?
O2 Ti2 N3 170.1(4) . . ?
O3 Ti3 O8 112.9(5) . . ?
O3 Ti3 O9 117.5(5) . . ?
O8 Ti3 O9 123.5(5) . . ?
O3 Ti3 O7 99.7(4) . . ?
O8 Ti3 O7 97.6(4) . . ?
O9 Ti3 O7 97.6(4) . . ?
O3 Ti3 N5 87.6(4) . . ?
O8 Ti3 N5 83.2(5) . . ?
O9 Ti3 N5 75.1(5) . . ?
O7 Ti3 N5 171.5(4) . . ?

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
C136 C130 C135 C134 177.2(15) . . . . ?
C131 C130 C135 C134 0.0 . . . . ?
C130 C135 C134 C133 0.0 . . . . ?
C135 C134 C133 C132 0.0 . . . . ?
C134 C133 C132 C131 0.0 . . . . ?
C133 C132 C131 C130 0.0 . . . . ?
C136 C130 C131 C132 -177.1(15) . . . . ?
C135 C130 C131 C132 0.0 . . . . ?
C143 C137 C138 C139 -179.8(18) . . . . ?
C142 C137 C138 C139 0.0 . . . . ?
C137 C138 C139 C140 0.0 . . . . ?
C138 C139 C140 C141 0.0 . . . . ?
C139 C140 C141 C142 0.0 . . . . ?
C140 C141 C142 C137 0.0 . . . . ?
C143 C137 C142 C141 179.9(16) . . . . ?
C138 C137 C142 C141 0.0 . . . . ?
C150 C149 C148 C147 178(3) . . . . ?
C144 C149 C148 C147 0.0 . . . . ?
C149 C148 C147 C146 0.0 . . . . ?
C148 C147 C146 C145 0.0 . . . . ?
C147 C146 C145 C144 0.0 . . . . ?
C146 C145 C144 C149 0.0 . . . . ?
C150 C149 C144 C145 -178(3) . . . . ?
C148 C149 C144 C145 0.0 . . . . ?
C6 C1 C2 C3 -3(3) . . . . ?
C7 C1 C2 C3 176.7(16) . . . . ?
C1 C2 C3 C4 4(3) . . . . ?
C2 C3 C4 C5 -3(3) . . . . ?
C3 C4 C5 C6 1(3) . . . . ?
C4 C5 C6 C1 0(3) . . . . ?
C2 C1 C6 C5 1(3) . . . . ?
C7 C1 C6 C5 -178.6(18) . . . . ?
C2 C1 C7 O4 19(2) . . . . ?
C6 C1 C7 O4 -160.8(14) . . . . ?
C2 C1 C7 C8 -97.1(19) . . . . ?
C6 C1 C7 C8 82.8(19) . . . . ?
C2 C1 C7 C14 135.6(16) . . . . ?
C6 C1 C7 C14 -44(2) . . . . ?
O4 C7 C8 C9 -15(2) . . . . ?
C1 C7 C8 C9 102(2) . . . . ?
C14 C7 C8 C9 -130.5(17) . . . . ?
O4 C7 C8 C13 170.8(15) . . . . ?
C1 C7 C8 C13 -73(2) . . . . ?
C14 C7 C8 C13 55(2) . . . . ?
C13 C8 C9 C10 -1(3) . . . . ?
C7 C8 C9 C10 -176.0(18) . . . . ?
C8 C9 C10 C11 1(3) . . . . ?
C9 C10 C11 C12 -1(4) . . . . ?
C10 C11 C12 C13 2(4) . . . . ?
C9 C8 C13 C12 2(3) . . . . ?
C7 C8 C13 C12 176.4(19) . . . . ?
C11 C12 C13 C8 -2(4) . . . . ?
O4 C7 C14 C15 78.5(16) . . . . ?
C1 C7 C14 C15 -40(2) . . . . ?
C8 C7 C14 C15 -164.0(15) . . . . ?
O4 C7 C14 N1 -36.5(16) . . . . ?
C1 C7 C14 N1 -154.7(14) . . . . ?
C8 C7 C14 N1 81.0(16) . . . . ?
N1 C14 C15 C16 -30.7(16) . . . . ?
C7 C14 C15 C16 -150.6(14) . . . . ?
C14 C15 C16 C17 14.6(19) . . . . ?
C15 C16 C17 N1 7.8(18) . . . . ?
N1 C18 C19 C20 123.9(15) . . . . ?
N1 C18 C19 C24 -60.5(16) . . . . ?
C24 C19 C20 C21 2(2) . . . . ?
C18 C19 C20 C21 177.5(14) . . . . ?
C19 C20 C21 C22 -4(2) . . . . ?
C19 C20 C21 C86 178.5(14) . . . . ?
C20 C21 C22 C23 3(2) . . . . ?
C86 C21 C22 C23 -179.3(15) . . . . ?
C21 C22 C23 C24 -1(2) . . . . ?
C21 C22 C23 C25 -178.6(14) . . . . ?
C22 C23 C24 O1 177.2(13) . . . . ?
C25 C23 C24 O1 -5(2) . . . . ?
C22 C23 C24 C19 -1(2) . . . . ?
C25 C23 C24 C19 176.9(13) . . . . ?
C20 C19 C24 O1 -177.9(13) . . . . ?
C18 C19 C24 O1 6(2) . . . . ?
C20 C19 C24 C23 0(2) . . . . ?
C18 C19 C24 C23 -175.6(13) . . . . ?
C22 C23 C25 N2 105.0(16) . . . . ?
C24 C23 C25 N2 -72.9(18) . . . . ?
N2 C26 C27 C28 -21(3) . . . . ?
C26 C27 C28 C29 23(3) . . . . ?
C27 C28 C29 N2 -15(2) . . . . ?
C27 C28 C29 C30 -134(2) . . . . ?
N2 C29 C30 O10 -42.3(17) . . . . ?
C28 C29 C30 O10 74.3(17) . . . . ?
N2 C29 C30 C31 76.7(18) . . . . ?
C28 C29 C30 C31 -166.7(15) . . . . ?
N2 C29 C30 C37 -158.5(16) . . . . ?
C28 C29 C30 C37 -42(2) . . . . ?
O10 C30 C31 C32 170.7(16) . . . . ?
C37 C30 C31 C32 -71(2) . . . . ?
C29 C30 C31 C32 56(2) . . . . ?
O10 C30 C31 C36 -12(2) . . . . ?
C37 C30 C31 C36 106(2) . . . . ?
C29 C30 C31 C36 -126.7(18) . . . . ?
C36 C31 C32 C33 -1(3) . . . . ?
C30 C31 C32 C33 176.4(18) . . . . ?
C31 C32 C33 C34 -1(3) . . . . ?
C32 C33 C34 C35 5(3) . . . . ?
C33 C34 C35 C36 -7(4) . . . . ?
C34 C35 C36 C31 5(4) . . . . ?
C32 C31 C36 C35 -1(3) . . . . ?
C30 C31 C36 C35 -178.6(19) . . . . ?
O10 C30 C37 C42 18(2) . . . . ?
C31 C30 C37 C42 -102(2) . . . . ?
C29 C30 C37 C42 131.8(18) . . . . ?
O10 C30 C37 C38 -166.9(17) . . . . ?
C31 C30 C37 C38 73(2) . . . . ?
C29 C30 C37 C38 -53(2) . . . . ?
C42 C37 C38 C39 1(3) . . . . ?
C30 C37 C38 C39 -174(2) . . . . ?
C37 C38 C39 C40 -1(3) . . . . ?
C38 C39 C40 C41 0(4) . . . . ?
C39 C40 C41 C42 0(4) . . . . ?
C38 C37 C42 C41 -1(3) . . . . ?
C30 C37 C42 C41 174(2) . . . . ?
C40 C41 C42 C37 1(4) . . . . ?
C48 C43 C44 C45 2(3) . . . . ?
C43 C44 C45 C46 -1(3) . . . . ?
C44 C45 C46 C47 -1(3) . . . . ?
C45 C46 C47 C48 1(3) . . . . ?
C46 C47 C48 C43 -1(3) . . . . ?
C46 C47 C48 C49 -178.1(17) . . . . ?
C44 C43 C48 C47 -1(3) . . . . ?
C44 C43 C48 C49 176.5(16) . . . . ?
C47 C48 C49 O6 -176.5(14) . . . . ?
C43 C48 C49 O6 6(2) . . . . ?
C47 C48 C49 C50 63(2) . . . . ?
C43 C48 C49 C50 -114.3(18) . . . . ?
C47 C48 C49 C56 -61.9(19) . . . . ?
C43 C48 C49 C56 120.8(17) . . . . ?
O6 C49 C50 C55 166.8(13) . . . . ?
C48 C49 C50 C55 -74.4(19) . . . . ?
C56 C49 C50 C55 48.4(19) . . . . ?
O6 C49 C50 C51 -13.0(19) . . . . ?
C48 C49 C50 C51 105.8(17) . . . . ?
C56 C49 C50 C51 -131.4(15) . . . . ?
C55 C50 C51 C52 1(2) . . . . ?
C49 C50 C51 C52 -178.9(15) . . . . ?
C50 C51 C52 C53 0(3) . . . . ?
C51 C52 C53 C54 -1(3) . . . . ?
C52 C53 C54 C55 -1(3) . . . . ?
C53 C54 C55 C50 3(3) . . . . ?
C51 C50 C55 C54 -3(2) . . . . ?
C49 C50 C55 C54 177.4(15) . . . . ?
O6 C49 C56 C57 77.3(17) . . . . ?
C48 C49 C56 C57 -38.5(19) . . . . ?
C50 C49 C56 C57 -161.3(14) . . . . ?
O6 C49 C56 N3 -37.8(16) . . . . ?
C48 C49 C56 N3 -153.7(13) . . . . ?
C50 C49 C56 N3 83.5(15) . . . . ?
N3 C56 C57 C58 -39.7(16) . . . . ?
C49 C56 C57 C58 -157.5(14) . . . . ?
C56 C57 C58 C59 28.0(19) . . . . ?
C57 C58 C59 N3 -5.2(19) . . . . ?
N3 C60 C61 C66 -62.6(19) . . . . ?
N3 C60 C61 C62 117.3(15) . . . . ?
C66 C61 C62 C63 -2(2) . . . . ?
C60 C61 C62 C63 178.6(16) . . . . ?
C61 C62 C63 C64 -5(2) . . . . ?
C61 C62 C63 C67 171.8(15) . . . . ?
C62 C63 C64 C65 6(2) . . . . ?
C67 C63 C64 C65 -170.9(15) . . . . ?
C63 C64 C65 C66 0(2) . . . . ?
C63 C64 C65 C68 179.9(14) . . . . ?
C64 C65 C66 O5 174.6(13) . . . . ?
C68 C65 C66 O5 -6(2) . . . . ?
C64 C65 C66 C61 -6(2) . . . . ?
C68 C65 C66 C61 173.7(14) . . . . ?
C62 C61 C66 C65 7(2) . . . . ?
C60 C61 C66 C65 -173.1(15) . . . . ?
C62 C61 C66 O5 -173.5(13) . . . . ?
C60 C61 C66 O5 6(2) . . . . ?
C66 C65 C68 N4 -163.5(13) . . . . ?
C64 C65 C68 N4 16(2) . . . . ?
N4 C69 C70 C71 39.7(19) . . . . ?
C69 C70 C71 C78 -22(2) . . . . ?
C77 C72 C73 C74 0(2) . . . . ?
C79 C72 C73 C74 -178.1(15) . . . . ?
C72 C73 C74 C75 1(3) . . . . ?
C73 C74 C75 C76 0(3) . . . . ?
C74 C75 C76 C77 -2(3) . . . . ?
C75 C76 C77 C72 3(3) . . . . ?
C73 C72 C77 C76 -2(2) . . . . ?
C79 C72 C77 C76 176.2(16) . . . . ?
C70 C71 C78 N4 -2(2) . . . . ?
C70 C71 C78 C79 -122.6(17) . . . . ?
C77 C72 C79 O11 8(2) . . . . ?
C73 C72 C79 O11 -174.4(13) . . . . ?
C77 C72 C79 C80 125.7(19) . . . . ?
C73 C72 C79 C80 -57(2) . . . . ?
C77 C72 C79 C78 -108.3(19) . . . . ?
C73 C72 C79 C78 69.4(19) . . . . ?
N4 C78 C79 O11 -45.6(16) . . . . ?
C71 C78 C79 O11 72.0(18) . . . . ?
N4 C78 C79 C80 -166.0(14) . . . . ?
C71 C78 C79 C80 -48(2) . . . . ?
N4 C78 C79 C72 72.6(17) . . . . ?
C71 C78 C79 C72 -169.7(16) . . . . ?
O11 C79 C80 C81 41(2) . . . . ?
C72 C79 C80 C81 -76.9(19) . . . . ?
C78 C79 C80 C81 158.8(16) . . . . ?
O11 C79 C80 C85 -143.2(17) . . . . ?
C72 C79 C80 C85 99(2) . . . . ?
C78 C79 C80 C85 -25(2) . . . . ?
C85 C80 C81 C82 -1(3) . . . . ?
C79 C80 C81 C82 175.4(17) . . . . ?
C80 C81 C82 C83 3(3) . . . . ?
C81 C82 C83 C84 -3(4) . . . . ?
C82 C83 C84 C85 0(4) . . . . ?
C81 C80 C85 C84 -2(3) . . . . ?
C79 C80 C85 C84 -177.6(17) . . . . ?
C83 C84 C85 C80 2(4) . . . . ?
C92 C87 C88 C89 2(4) . . . . ?
C87 C88 C89 C90 -3(5) . . . . ?
C88 C89 C90 C91 4(5) . . . . ?
C89 C90 C91 C92 -2(5) . . . . ?
C88 C87 C92 C91 0(3) . . . . ?
C88 C87 C92 C93 176(2) . . . . ?
C90 C91 C92 C87 0(3) . . . . ?
C90 C91 C92 C93 -176(2) . . . . ?
C87 C92 C93 O9 17(2) . . . . ?
C91 C92 C93 O9 -166.9(17) . . . . ?
C87 C92 C93 C100 133.7(19) . . . . ?
C91 C92 C93 C100 -50(2) . . . . ?
C87 C92 C93 C94 -102(2) . . . . ?
C91 C92 C93 C94 74(2) . . . . ?
O9 C93 C94 C99 164.7(16) . . . . ?
C92 C93 C94 C99 -78(2) . . . . ?
C100 C93 C94 C99 46(2) . . . . ?
O9 C93 C94 C95 -15(2) . . . . ?
C92 C93 C94 C95 103(2) . . . . ?
C100 C93 C94 C95 -133.4(19) . . . . ?
C99 C94 C95 C96 0(4) . . . . ?
C93 C94 C95 C96 180(2) . . . . ?
C94 C95 C96 C97 -1(5) . . . . ?
C95 C96 C97 C98 3(7) . . . . ?
C96 C97 C98 C99 -3(6) . . . . ?
C95 C94 C99 C98 -1(3) . . . . ?
C93 C94 C99 C98 -180(2) . . . . ?
C97 C98 C99 C94 2(4) . . . . ?
O9 C93 C100 N5 -40.3(16) . . . . ?
C92 C93 C100 N5 -158.0(14) . . . . ?
C94 C93 C100 N5 80.8(17) . . . . ?
O9 C93 C100 C101 72.7(17) . . . . ?
C92 C93 C100 C101 -45(2) . . . . ?
C94 C93 C100 C101 -166.2(15) . . . . ?
N5 C100 C101 C102 -30.7(17) . . . . ?
C93 C100 C101 C102 -149.1(15) . . . . ?
C100 C101 C102 C103 13(2) . . . . ?
C101 C102 C103 N5 9.7(19) . . . . ?
N5 C104 C105 C106 117.4(16) . . . . ?
N5 C104 C105 C110 -60.7(17) . . . . ?
C110 C105 C106 C107 -3(2) . . . . ?
C104 C105 C106 C107 179.0(15) . . . . ?
C105 C106 C107 C108 0(2) . . . . ?
C105 C106 C107 C111 179.2(16) . . . . ?
C106 C107 C108 C109 1(2) . . . . ?
C111 C107 C108 C109 -178.2(16) . . . . ?
C107 C108 C109 C110 1(2) . . . . ?
C107 C108 C109 C112 178.4(15) . . . . ?
C108 C109 C110 O8 174.3(13) . . . . ?
C112 C109 C110 O8 -3(2) . . . . ?
C108 C109 C110 C105 -5(2) . . . . ?
C112 C109 C110 C105 178.1(13) . . . . ?
C106 C105 C110 O8 -173.4(13) . . . . ?
C104 C105 C110 O8 4.8(18) . . . . ?
C106 C105 C110 C109 6(2) . . . . ?
C104 C105 C110 C109 -176.2(13) . . . . ?
C108 C109 C112 N6 108.4(17) . . . . ?
C110 C109 C112 N6 -74.3(19) . . . . ?
N6 C113 C114 C115 -33.7(19) . . . . ?
C113 C114 C115 C116 36.2(19) . . . . ?
C114 C115 C116 N6 -25.0(17) . . . . ?
C114 C115 C116 C117 -142.7(16) . . . . ?
N6 C116 C117 O12 -42.4(17) . . . . ?
C115 C116 C117 O12 73.4(17) . . . . ?
N6 C116 C117 C118 -160.5(15) . . . . ?
C115 C116 C117 C118 -45(2) . . . . ?
N6 C116 C117 C124 78.0(18) . . . . ?
C115 C116 C117 C124 -166.3(16) . . . . ?
O12 C117 C118 C119 -163.6(16) . . . . ?
C124 C117 C118 C119 78(2) . . . . ?
C116 C117 C118 C119 -46(2) . . . . ?
O12 C117 C118 C123 20(2) . . . . ?
C124 C117 C118 C123 -99(2) . . . . ?
C116 C117 C118 C123 137.4(16) . . . . ?
C123 C118 C119 C120 0(3) . . . . ?
C117 C118 C119 C120 -176(2) . . . . ?
C118 C119 C120 C121 0(4) . . . . ?
C119 C120 C121 C122 0(5) . . . . ?
C120 C121 C122 C123 0(5) . . . . ?
C119 C118 C123 C122 0(3) . . . . ?
C117 C118 C123 C122 176.5(18) . . . . ?
C121 C122 C123 C118 0(4) . . . . ?
O12 C117 C124 C129 -8(2) . . . . ?
C118 C117 C124 C129 108.9(19) . . . . ?
C116 C117 C124 C129 -127.1(16) . . . . ?
O12 C117 C124 C125 172.2(13) . . . . ?
C118 C117 C124 C125 -70(2) . . . . ?
C116 C117 C124 C125 54(2) . . . . ?
C129 C124 C125 C126 0(2) . . . . ?
C117 C124 C125 C126 179.3(14) . . . . ?
C124 C125 C126 C127 0(3) . . . . ?
C125 C126 C127 C128 -1(3) . . . . ?
C126 C127 C128 C129 2(3) . . . . ?
C127 C128 C129 C124 -2(3) . . . . ?
C125 C124 C129 C128 1(3) . . . . ?
C117 C124 C129 C128 -178.5(16) . . . . ?
C16 C17 N1 C18 -150.9(13) . . . . ?
C16 C17 N1 C14 -27.4(16) . . . . ?
C16 C17 N1 Ti1 86.5(13) . . . . ?
C19 C18 N1 C17 -59.6(16) . . . . ?
C19 C18 N1 C14 -178.7(14) . . . . ?
C19 C18 N1 Ti1 66.7(14) . . . . ?
C15 C14 N1 C17 35.8(15) . . . . ?
C7 C14 N1 C17 157.7(12) . . . . ?
C15 C14 N1 C18 157.6(12) . . . . ?
C7 C14 N1 C18 -80.6(15) . . . . ?
C15 C14 N1 Ti1 -85.2(11) . . . . ?
C7 C14 N1 Ti1 36.6(13) . . . . ?
C28 C29 N2 C25 138.7(13) . . . . ?
C30 C29 N2 C25 -101.0(15) . . . . ?
C28 C29 N2 C26 4.0(16) . . . . ?
C30 C29 N2 C26 124.3(14) . . . . ?
C23 C25 N2 C29 -51.7(18) . . . . ?
C23 C25 N2 C26 80.0(18) . . . . ?
C27 C26 N2 C29 9(2) . . . . ?
C27 C26 N2 C25 -126.1(19) . . . . ?
C61 C60 N3 C56 179.0(14) . . . . ?
C61 C60 N3 C59 -65.0(16) . . . . ?
C61 C60 N3 Ti2 63.3(15) . . . . ?
C57 C56 N3 C60 156.2(13) . . . . ?
C49 C56 N3 C60 -81.0(15) . . . . ?
C57 C56 N3 C59 36.3(14) . . . . ?
C49 C56 N3 C59 159.0(13) . . . . ?
C57 C56 N3 Ti2 -86.1(11) . . . . ?
C49 C56 N3 Ti2 36.6(13) . . . . ?
C58 C59 N3 C60 -141.4(15) . . . . ?
C58 C59 N3 C56 -18.9(16) . . . . ?
C58 C59 N3 Ti2 95.1(14) . . . . ?
C70 C69 N4 C68 -173.5(14) . . . . ?
C70 C69 N4 C78 -42.7(17) . . . . ?
C65 C68 N4 C69 -93.0(16) . . . . ?
C65 C68 N4 C78 143.3(14) . . . . ?
C71 C78 N4 C69 27.2(17) . . . . ?
C79 C78 N4 C69 149.7(13) . . . . ?
C71 C78 N4 C68 155.5(14) . . . . ?
C79 C78 N4 C68 -82.0(16) . . . . ?
C102 C103 N5 C100 -30.0(16) . . . . ?
C102 C103 N5 C104 -150.3(13) . . . . ?
C102 C103 N5 Ti3 86.0(14) . . . . ?
C93 C100 N5 C103 157.8(13) . . . . ?
C101 C100 N5 C103 37.1(15) . . . . ?
C93 C100 N5 C104 -83.7(15) . . . . ?
C101 C100 N5 C104 155.6(13) . . . . ?
C93 C100 N5 Ti3 33.4(14) . . . . ?
C101 C100 N5 Ti3 -87.4(12) . . . . ?
C105 C104 N5 C103 -64.5(16) . . . . ?
C105 C104 N5 C100 178.5(14) . . . . ?
C105 C104 N5 Ti3 64.1(14) . . . . ?
C114 C113 N6 C116 17.9(18) . . . . ?
C114 C113 N6 C112 -119.1(16) . . . . ?
C115 C116 N6 C113 5.0(15) . . . . ?
C117 C116 N6 C113 126.0(14) . . . . ?
C115 C116 N6 C112 141.6(14) . . . . ?
C117 C116 N6 C112 -97.5(15) . . . . ?
C109 C112 N6 C113 84.0(18) . . . . ?
C109 C112 N6 C116 -48.5(19) . . . . ?
C23 C24 O1 Ti1 -138.2(13) . . . . ?
C19 C24 O1 Ti1 40(2) . . . . ?
C1 C7 O4 Ti1 141.5(11) . . . . ?
C8 C7 O4 Ti1 -102.2(14) . . . . ?
C14 C7 O4 Ti1 19.1(18) . . . . ?
C65 C66 O5 Ti2 -133.7(14) . . . . ?
C61 C66 O5 Ti2 47(2) . . . . ?
C48 C49 O6 Ti2 138.6(11) . . . . ?
C50 C49 O6 Ti2 -101.5(14) . . . . ?
C56 C49 O6 Ti2 21.4(19) . . . . ?
C109 C110 O8 Ti3 -130.4(14) . . . . ?
C105 C110 O8 Ti3 48.5(19) . . . . ?
C92 C93 O9 Ti3 151.4(11) . . . . ?
C100 C93 O9 Ti3 30.8(18) . . . . ?
C94 C93 O9 Ti3 -91.9(16) . . . . ?
Ti2 O2 Ti1 O1 109.3(8) . . . . ?
Ti2 O2 Ti1 O4 -96.8(8) . . . . ?
Ti2 O2 Ti1 O3 6.3(9) . . . . ?
Ti2 O2 Ti1 N1 -168.6(8) . . . . ?
C24 O1 Ti1 O2 60.8(16) . . . . ?
C24 O1 Ti1 O4 -92.0(16) . . . . ?
C24 O1 Ti1 O3 166.3(15) . . . . ?
C24 O1 Ti1 N1 -24.7(16) . . . . ?
C7 O4 Ti1 O2 -78.5(13) . . . . ?
C7 O4 Ti1 O1 72.5(13) . . . . ?
C7 O4 Ti1 O3 175.2(12) . . . . ?
C7 O4 Ti1 N1 1.0(12) . . . . ?
Ti3 O3 Ti1 O2 -11.4(9) . . . . ?
Ti3 O3 Ti1 O1 -126.0(8) . . . . ?
Ti3 O3 Ti1 O4 109.9(8) . . . . ?
Ti3 O3 Ti1 N1 141(2) . . . . ?
Ti3 O7 Ti2 O6 -97.7(8) . . . . ?
Ti3 O7 Ti2 O5 108.0(8) . . . . ?
Ti3 O7 Ti2 O2 3.1(8) . . . . ?
Ti3 O7 Ti2 N3 -169.4(8) . . . . ?
C49 O6 Ti2 O7 -79.5(14) . . . . ?
C49 O6 Ti2 O5 73.6(14) . . . . ?
C49 O6 Ti2 O2 177.4(13) . . . . ?
C49 O6 Ti2 N3 -0.5(13) . . . . ?
C66 O5 Ti2 O7 52.1(15) . . . . ?
C66 O5 Ti2 O6 -101.5(15) . . . . ?
C66 O5 Ti2 O2 157.0(14) . . . . ?
C66 O5 Ti2 N3 -32.4(15) . . . . ?
Ti1 O2 Ti2 O7 -3.3(9) . . . . ?
Ti1 O2 Ti2 O6 116.2(8) . . . . ?
Ti1 O2 Ti2 O5 -122.0(8) . . . . ?
Ti1 O3 Ti3 O8 113.7(8) . . . . ?
Ti1 O3 Ti3 O9 -92.8(9) . . . . ?
Ti1 O3 Ti3 O7 11.1(9) . . . . ?
Ti1 O3 Ti3 N5 -164.7(8) . . . . ?
C110 O8 Ti3 O3 51.2(16) . . . . ?
C110 O8 Ti3 O9 -100.4(16) . . . . ?
C110 O8 Ti3 O7 155.2(15) . . . . ?
C110 O8 Ti3 N5 -33.3(15) . . . . ?
C93 O9 Ti3 O3 -88.7(13) . . . . ?
C93 O9 Ti3 O8 61.7(14) . . . . ?
C93 O9 Ti3 O7 166.1(12) . . . . ?
C93 O9 Ti3 N5 -9.5(12) . . . . ?
Ti2 O7 Ti3 O3 -6.1(9) . . . . ?
Ti2 O7 Ti3 O8 -120.9(8) . . . . ?
Ti2 O7 Ti3 O9 113.6(8) . . . . ?

_refine_diff_density_max         0.420
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.057





# start Validation Reply Form
_vrf_REFNR01_Ti                  
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: With the intial setting of 2 theta max at 50 degrees, the crystal
diffracted quite weakly and the resolution was less than 0.78 \%A  and the 
completness was low.

;
_vrf_THETM01_Ti                  
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: With the intial setting of 2 theta max at 50 degrees, the crystal
diffracted quite weakly and the resolution was less than 0.78 \%A  and the 
completness was low.
;
_vrf_PLAT090_Ti                  
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       3.16 Note  
RESPONSE: With the intial setting of 2 theta max at 50 degrees, the crystal
diffracted quite weakly and the resolution was less than 0.78 \%A  and the 
completness was low.
;
_vrf_PLAT234_Ti                  
;
PROBLEM: Large Hirshfeld Difference C96    --  C97     ..       0.33 Ang.  
RESPONSE: This alarm is due to the elongated ADPs of carbon atoms which suggest 
that these are probably disordered.  
;
_vrf_PLAT362_Ti                  
;
PROBLEM: Short   C(sp3)-C(sp2) Bond  C149   -   C150   ..       1.20 Ang.  
RESPONSE: This alarm is due to the elongated ADPs of carbon atoms which 
suggest that these are probably disordered. In particular, the solvent 
molecule is highly disordered.  
;
# end Validation Reply Form






_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
