# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_Ti2-H_121213_ben
_database_code_depnum_ccdc_archive 'CCDC 1486141'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Fri Dec 13 09:44:48 2013'
;
_audit_creation_method           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_chemical_name_common            ?
_chemical_name_systematic        Ti2-H
_chemical_formula_moiety         'C70 H78 N2 O2 Ti2'
_chemical_formula_sum            'C70 H78 N2 O2 Ti2'
_chemical_formula_weight         1075.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.09321(15)
_cell_length_b                   22.0757(3)
_cell_length_c                   28.1078(4)
_cell_angle_alpha                90.0
_cell_angle_beta                 92.8099(13)
_cell_angle_gamma                90.0
_cell_volume                     6875.05(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16884
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.5439
_cell_measurement_theta_min      3.7285
_cell_oxdiff_angle_alpha         90.037(2)
_cell_oxdiff_angle_beta          92.792(2)
_cell_oxdiff_angle_gamma         90.022(2)
_cell_oxdiff_length_a            11.0925(3)
_cell_oxdiff_length_b            22.0724(6)
_cell_oxdiff_length_c            28.1132(8)
_cell_oxdiff_measurement_reflns_used 16884
_cell_oxdiff_volume              6875.1(3)
_exptl_absorpt_coefficient_mu    2.275
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            38840
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.73
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   33.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -120.0000 33

#__ type_ start__ end____ width___ exp.time_
  2 omega   35.00   62.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
  3 omega    6.00   42.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -150.0000 36

#__ type_ start__ end____ width___ exp.time_
  4 omega   42.00   77.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   90.0000 35

#__ type_ start__ end____ width___ exp.time_
  5 omega -115.00  -37.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -57.0000  -60.0000 78

#__ type_ start__ end____ width___ exp.time_
  6 omega   78.00  117.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000 -180.0000 39

#__ type_ start__ end____ width___ exp.time_
  7 omega   99.00  126.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000   60.0000 27

#__ type_ start__ end____ width___ exp.time_
  8 omega  -72.00    9.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   25.0000  -60.0000 81

#__ type_ start__ end____ width___ exp.time_
  9 omega -113.00   -7.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000  150.0000 106

#__ type_ start__ end____ width___ exp.time_
 10 omega   40.00   71.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -150.0000 31

#__ type_ start__ end____ width___ exp.time_
 11 omega   38.00   70.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -90.0000 32

#__ type_ start__ end____ width___ exp.time_
 12 omega   39.00   68.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   90.0000 29

#__ type_ start__ end____ width___ exp.time_
 13 omega   38.00   63.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -180.0000 25

#__ type_ start__ end____ width___ exp.time_
 14 omega   38.00   71.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   60.0000 33

#__ type_ start__ end____ width___ exp.time_
 15 omega   50.00  130.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000  120.0000 80

#__ type_ start__ end____ width___ exp.time_
 16 omega   81.00  130.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -77.0000  -60.0000 49

#__ type_ start__ end____ width___ exp.time_
 17 omega   38.00   68.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -60.0000 30

#__ type_ start__ end____ width___ exp.time_
 18 omega   38.00   71.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   30.0000 33

#__ type_ start__ end____ width___ exp.time_
 19 omega   42.00   69.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -120.0000 27

#__ type_ start__ end____ width___ exp.time_
 20 omega   41.00   71.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000    0.0000 30

#__ type_ start__ end____ width___ exp.time_
 21 omega   38.00   63.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 22 omega   76.00  121.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000   60.0000 45

#__ type_ start__ end____ width___ exp.time_
 23 omega  145.00  175.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000   60.0000 30

#__ type_ start__ end____ width___ exp.time_
 24 omega  102.00  129.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000  -90.0000 27

#__ type_ start__ end____ width___ exp.time_
 25 omega   43.00   95.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000  -90.0000 52

#__ type_ start__ end____ width___ exp.time_
 26 omega  -21.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 90

#__ type_ start__ end____ width___ exp.time_
 27 omega  -21.00   69.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000   30.0000 90

#__ type_ start__ end____ width___ exp.time_
 28 omega -127.00  -29.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -37.0000  120.0000 98

#__ type_ start__ end____ width___ exp.time_
 29 omega -124.00  -47.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -70.0000 -136.0000 77
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0506656000
_diffrn_orient_matrix_UB_12      -0.0630246000
_diffrn_orient_matrix_UB_13      -0.0135165000
_diffrn_orient_matrix_UB_21      -0.0866262000
_diffrn_orient_matrix_UB_22      0.0037584000
_diffrn_orient_matrix_UB_23      0.0410990000
_diffrn_orient_matrix_UB_31      -0.0962456000
_diffrn_orient_matrix_UB_32      0.0297526000
_diffrn_orient_matrix_UB_33      -0.0337371000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                10743
_reflns_number_total             12262
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         12262
_refine_ls_number_restraints     332
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0461
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0820P)²+1.6938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1360
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
# 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 -0.025 0.500 0.000 606 85 ' '
2 -0.003 1.000 0.500 606 85 ' '
_platon_squeeze_details          
;
;

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ti1 Ti 0.11427(3) 0.841195(16) 0.122636(12) 0.03141(11) Uani 1 1 d . . . .
Ti2 Ti -0.01514(3) 0.749996(15) 0.251911(12) 0.03219(11) Uani 1 1 d . . . .
O1 O 0.22532(11) 0.89594(5) 0.10257(4) 0.0271(3) Uani 1 1 d A . . .
O2 O 0.01349(14) 0.74170(6) 0.31616(5) 0.0411(3) Uani 1 1 d A . . .
N1 N 0.24327(13) 0.82957(7) 0.18300(5) 0.0277(3) Uani 1 1 d A . . .
N2 N 0.08350(13) 0.83493(7) 0.26302(5) 0.0292(3) Uani 1 1 d A . . .
C1 C 0.13978(17) 0.73618(9) 0.19889(7) 0.0331(4) Uani 1 1 d A . . .
H1 H 0.1421 0.6974 0.2135 0.040 Uiso 1 1 calc . . R .
C2 C 0.03428(18) 0.75235(9) 0.16991(7) 0.0356(4) Uani 1 1 d A . . .
H2 H 0.0099 0.7238 0.1461 0.043 Uiso 1 1 calc . . R .
C3 C -0.03790(17) 0.80470(9) 0.17201(7) 0.0370(5) Uani 1 1 d A . . .
H3 H -0.1206 0.7993 0.1625 0.044 Uiso 1 1 calc . . R .
C4 C -0.00440(17) 0.86487(9) 0.18641(7) 0.0351(4) Uani 1 1 d A . . .
H4 H -0.0251 0.8970 0.1651 0.042 Uiso 1 1 calc . . R .
C5 C 0.24237(16) 0.77567(8) 0.20697(6) 0.0299(4) Uani 1 1 d . . . .
C6 C 0.33848(19) 0.75863(9) 0.23804(7) 0.0362(4) Uani 1 1 d A . . .
H6 H 0.3381 0.7202 0.2532 0.043 Uiso 1 1 calc . . R .
C7 C 0.43304(18) 0.79741(10) 0.24662(8) 0.0396(5) Uani 1 1 d . . . .
H7 H 0.4998 0.7858 0.2671 0.048 Uiso 1 1 calc A . R .
C8 C 0.43038(17) 0.85396(9) 0.22510(7) 0.0343(4) Uani 1 1 d A . . .
H8 H 0.4942 0.8819 0.2317 0.041 Uiso 1 1 calc . . R .
C9 C 0.33461(15) 0.86986(8) 0.19388(6) 0.0281(4) Uani 1 1 d . . . .
C10 C 0.33536(15) 0.93052(8) 0.17149(6) 0.0264(4) Uani 1 1 d A . . .
C11 C 0.39183(16) 0.97867(8) 0.19651(6) 0.0292(4) Uani 1 1 d . . . .
H11 H 0.4198 0.9726 0.2286 0.035 Uiso 1 1 calc A . R .
C12 C 0.40776(16) 1.03437(8) 0.17578(7) 0.0304(4) Uani 1 1 d A . . .
C13 C 0.37108(17) 1.04038(8) 0.12766(7) 0.0306(4) Uani 1 1 d . . . .
H13 H 0.3861 1.0779 0.1125 0.037 Uiso 1 1 calc A . R .
C14 C 0.31430(15) 0.99519(8) 0.10085(6) 0.0265(4) Uani 1 1 d A . . .
C15 C 0.28989(15) 0.94047(8) 0.12486(6) 0.0244(3) Uani 1 1 d . . . .
C16A C -0.0378(3) 0.8563(2) 0.07339(14) 0.0301(7) Uani 0.50 1 d A 2 . U
H16A H -0.0049 0.8778 0.0459 0.036 Uiso 0.50 1 calc A 2 R .
H16B H -0.0622 0.8157 0.0616 0.036 Uiso 0.50 1 calc A 2 R .
C16 C -0.0309(3) 0.8959(2) 0.08659(15) 0.0349(8) Uani 0.50 1 d A 1 . U
H16C H -0.0138 0.9385 0.0954 0.042 Uiso 0.50 1 calc A 1 R .
H16D H -0.0187 0.8926 0.0520 0.042 Uiso 0.50 1 calc A 1 R .
C17 C -0.1618(8) 0.8869(4) 0.0922(6) 0.025(2) Uani 0.50 1 d A 1 D U
C18 C -0.2342(4) 0.93151(19) 0.11107(15) 0.0376(8) Uani 0.50 1 d A 1 D U
H18 H -0.1986 0.9688 0.1211 0.045 Uiso 0.50 1 calc A 1 R .
C19 C -0.3568(6) 0.9229(3) 0.1155(3) 0.0422(16) Uani 0.50 1 d A 1 D U
H19 H -0.4029 0.9528 0.1308 0.051 Uiso 0.50 1 calc A 1 R .
C20 C -0.4119(5) 0.8714(3) 0.0979(2) 0.0451(13) Uani 0.50 1 d A 1 D U
H20 H -0.4962 0.8658 0.1005 0.054 Uiso 0.50 1 calc A 1 R .
C21 C -0.3442(4) 0.8278(2) 0.07640(15) 0.0438(9) Uani 0.50 1 d A 1 D U
H21 H -0.3817 0.7919 0.0643 0.053 Uiso 0.50 1 calc A 1 R .
C22 C -0.2215(4) 0.8364(2) 0.07246(16) 0.0363(9) Uani 0.50 1 d A 1 D U
H22 H -0.1767 0.8072 0.0559 0.044 Uiso 0.50 1 calc A 1 R .
C17A C -0.1525(8) 0.8883(4) 0.0832(6) 0.026(2) Uani 0.50 1 d A 2 . U
C18A C -0.1542(4) 0.94884(17) 0.09607(13) 0.0339(8) Uani 0.50 1 d A 2 . U
H18A H -0.0814 0.9715 0.0962 0.041 Uiso 0.50 1 calc A 2 R .
C19A C -0.2594(4) 0.9773(2) 0.10888(15) 0.0414(9) Uani 0.50 1 d A 2 . U
H19A H -0.2586 1.0195 0.1154 0.050 Uiso 0.50 1 calc A 2 R .
C20A C -0.3646(7) 0.9452(3) 0.1122(3) 0.0443(16) Uani 0.50 1 d A 2 . U
H20A H -0.4364 0.9650 0.1208 0.053 Uiso 0.50 1 calc A 2 R .
C21A C -0.3647(5) 0.8842(3) 0.1030(2) 0.0449(13) Uani 0.50 1 d A 2 . U
H21A H -0.4367 0.8615 0.1059 0.054 Uiso 0.50 1 calc A 2 R .
C22A C -0.2597(4) 0.8551(2) 0.08933(17) 0.0373(9) Uani 0.50 1 d A 2 . U
H22A H -0.2604 0.8126 0.0841 0.045 Uiso 0.50 1 calc A 2 R .
C23A C 0.1682(7) 0.7626(4) 0.0755(4) 0.0384(16) Uani 0.50 1 d A 2 . U
H23A H 0.0982 0.7349 0.0711 0.046 Uiso 0.50 1 calc A 2 R .
H23B H 0.1855 0.7789 0.0437 0.046 Uiso 0.50 1 calc A 2 R .
C23 C 0.1314(8) 0.7722(5) 0.0778(5) 0.050(2) Uani 0.50 1 d A 1 . U
H23C H 0.0533 0.7504 0.0748 0.060 Uiso 0.50 1 calc A 1 R .
H23D H 0.1472 0.7889 0.0460 0.060 Uiso 0.50 1 calc A 1 R .
C24 C 0.2288(8) 0.7269(4) 0.0909(5) 0.0515(18) Uani 0.50 1 d A 1 D U
C25 C 0.2012(7) 0.6664(3) 0.0997(3) 0.0644(16) Uani 0.50 1 d A 1 D U
H25 H 0.1199 0.6533 0.0952 0.077 Uiso 0.50 1 calc A 1 R .
C26 C 0.2892(8) 0.6244(4) 0.1150(3) 0.0789(18) Uani 0.50 1 d A 1 D U
H26 H 0.2677 0.5834 0.1202 0.095 Uiso 0.50 1 calc A 1 R .
C27 C 0.4092(9) 0.6432(4) 0.1225(5) 0.087(3) Uani 0.50 1 d A 1 D U
H27 H 0.4701 0.6160 0.1340 0.104 Uiso 0.50 1 calc A 1 R .
C28 C 0.4359(8) 0.7032(4) 0.1125(3) 0.085(2) Uani 0.50 1 d A 1 D U
H28 H 0.5173 0.7165 0.1165 0.103 Uiso 0.50 1 calc A 1 R .
C29 C 0.3493(8) 0.7440(4) 0.0972(6) 0.068(2) Uani 0.50 1 d A 1 D U
H29 H 0.3719 0.7845 0.0906 0.082 Uiso 0.50 1 calc A 1 R .
C24A C 0.2732(7) 0.7269(4) 0.0931(5) 0.0438(17) Uani 0.50 1 d A 2 . U
C25A C 0.2601(7) 0.6672(3) 0.1069(3) 0.0623(16) Uani 0.50 1 d A 2 . U
H25A H 0.1831 0.6483 0.1041 0.075 Uiso 0.50 1 calc A 2 R .
C26A C 0.3593(9) 0.6348(4) 0.1248(4) 0.073(2) Uani 0.50 1 d A 2 . U
H26A H 0.3519 0.5936 0.1341 0.087 Uiso 0.50 1 calc A 2 R .
C27A C 0.4718(8) 0.6648(4) 0.1290(3) 0.0817(18) Uani 0.50 1 d A 2 . U
H27A H 0.5402 0.6438 0.1423 0.098 Uiso 0.50 1 calc A 2 R .
C28A C 0.4845(6) 0.7231(4) 0.1145(3) 0.0752(17) Uani 0.50 1 d A 2 . U
H28A H 0.5616 0.7419 0.1164 0.090 Uiso 0.50 1 calc A 2 R .
C29A C 0.3869(7) 0.7542(4) 0.0973(6) 0.0610(18) Uani 0.50 1 d A 2 . U
H29A H 0.3956 0.7952 0.0879 0.073 Uiso 0.50 1 calc A 2 R .
C30 C 0.46789(19) 1.08812(9) 0.20207(8) 0.0383(4) Uani 1 1 d . . . .
C31 C 0.4929(2) 1.07535(11) 0.25498(8) 0.0536(6) Uani 1 1 d A . . .
H31A H 0.4171 1.0654 0.2697 0.080 Uiso 1 1 calc . . GR .
H31B H 0.5288 1.1113 0.2705 0.080 Uiso 1 1 calc . . GR .
H31C H 0.5489 1.0412 0.2588 0.080 Uiso 1 1 calc . . GR .
C32 C 0.5879(2) 1.10220(11) 0.17976(9) 0.0512(6) Uani 1 1 d A . . .
H32A H 0.6261 1.1371 0.1960 0.077 Uiso 1 1 calc . . GR .
H32B H 0.5731 1.1116 0.1459 0.077 Uiso 1 1 calc . . GR .
H32C H 0.6414 1.0670 0.1831 0.077 Uiso 1 1 calc . . GR .
C33 C 0.3851(2) 1.14340(10) 0.19759(11) 0.0578(6) Uani 1 1 d A . . .
H33A H 0.3074 1.1339 0.2110 0.087 Uiso 1 1 calc . . GR .
H33B H 0.3721 1.1542 0.1639 0.087 Uiso 1 1 calc . . GR .
H33C H 0.4227 1.1775 0.2150 0.087 Uiso 1 1 calc . . GR .
C34 C 0.28687(17) 1.00280(8) 0.04686(6) 0.0305(4) Uani 1 1 d . . . .
C35 C 0.15101(19) 0.99909(10) 0.03419(8) 0.0395(5) Uani 1 1 d A . . .
H35A H 0.1081 1.0279 0.0538 0.059 Uiso 1 1 calc . . GR .
H35B H 0.1223 0.9579 0.0402 0.059 Uiso 1 1 calc . . GR .
H35C H 0.1358 1.0091 0.0005 0.059 Uiso 1 1 calc . . GR .
C36 C 0.3525(2) 0.95314(9) 0.02010(7) 0.0398(5) Uani 1 1 d A . . .
H36A H 0.3406 0.9597 -0.0143 0.060 Uiso 1 1 calc . . GR .
H36B H 0.3199 0.9135 0.0284 0.060 Uiso 1 1 calc . . GR .
H36C H 0.4389 0.9545 0.0291 0.060 Uiso 1 1 calc . . GR .
C37 C 0.3312(2) 1.06437(9) 0.02921(7) 0.0404(5) Uani 1 1 d A . . .
H37A H 0.4181 1.0682 0.0367 0.061 Uiso 1 1 calc . . GR .
H37B H 0.2884 1.0969 0.0450 0.061 Uiso 1 1 calc . . GR .
H37C H 0.3154 1.0673 -0.0053 0.061 Uiso 1 1 calc . . GR .
C38 C 0.05857(16) 0.88022(8) 0.23100(7) 0.0317(4) Uani 1 1 d . . . .
C39 C 0.09143(18) 0.94021(9) 0.24106(8) 0.0382(4) Uani 1 1 d A . . .
H39 H 0.0705 0.9714 0.2189 0.046 Uiso 1 1 calc . . R .
C40 C 0.1535(2) 0.95392(9) 0.28278(8) 0.0424(5) Uani 1 1 d . . . .
H40 H 0.1747 0.9946 0.2902 0.051 Uiso 1 1 calc A . R .
C41 C 0.1853(2) 0.90732(9) 0.31426(8) 0.0387(4) Uani 1 1 d A . . .
H41 H 0.2306 0.9160 0.3430 0.046 Uiso 1 1 calc . . R .
C42 C 0.15106(17) 0.84817(8) 0.30378(7) 0.0319(4) Uani 1 1 d . . . .
C43 C 0.18599(18) 0.79969(8) 0.33825(7) 0.0329(4) Uani 1 1 d A . . .
C44 C 0.29419(19) 0.80498(9) 0.36557(7) 0.0378(4) Uani 1 1 d . . . .
H44 H 0.3477 0.8372 0.3591 0.045 Uiso 1 1 calc A . R .
C45 C 0.3258(2) 0.76456(10) 0.40183(8) 0.0445(5) Uani 1 1 d A . . .
C46 C 0.2419(3) 0.72047(11) 0.41181(8) 0.0521(6) Uani 1 1 d . . . .
H46 H 0.2602 0.6941 0.4379 0.062 Uiso 1 1 calc A . R .
C47 C 0.1331(2) 0.71232(10) 0.38625(8) 0.0484(5) Uani 1 1 d A . D .
C48 C 0.1103(2) 0.75056(9) 0.34676(7) 0.0366(4) Uani 1 1 d . . . .
C49 C -0.20382(19) 0.77260(10) 0.24972(9) 0.0442(5) Uani 1 1 d A . . .
H49A H -0.2378 0.7688 0.2166 0.053 Uiso 1 1 calc . . R .
H49B H -0.2471 0.7438 0.2698 0.053 Uiso 1 1 calc . . R .
C50 C -0.22229(18) 0.83504(10) 0.26692(8) 0.0426(5) Uani 1 1 d . . . .
C51 C -0.25476(18) 0.88162(10) 0.23509(9) 0.0466(5) Uani 1 1 d A . . .
H51 H -0.2681 0.8726 0.2022 0.056 Uiso 1 1 calc . . R .
C52 C -0.2677(2) 0.93996(12) 0.25045(11) 0.0591(7) Uani 1 1 d . . . .
H52 H -0.2898 0.9708 0.2281 0.071 Uiso 1 1 calc A . R .
C53 C -0.2493(3) 0.95425(14) 0.29743(14) 0.0768(9) Uani 1 1 d A . . .
H53 H -0.2580 0.9949 0.3078 0.092 Uiso 1 1 calc . . R .
C54 C -0.2177(3) 0.90906(16) 0.32993(13) 0.0831(10) Uani 1 1 d . . . .
H54 H -0.2049 0.9186 0.3627 0.100 Uiso 1 1 calc A . R .
C55 C -0.2048(3) 0.85009(13) 0.31458(10) 0.0639(7) Uani 1 1 d A . . .
H55 H -0.1836 0.8193 0.3371 0.077 Uiso 1 1 calc . . R .
C56 C -0.0377(2) 0.65348(9) 0.24313(8) 0.0428(5) Uani 1 1 d A . . .
H56A H 0.0386 0.6351 0.2559 0.051 Uiso 1 1 calc . . R .
H56B H -0.1004 0.6416 0.2652 0.051 Uiso 1 1 calc . . R .
C57 C -0.0681(2) 0.62168(10) 0.19822(8) 0.0475(5) Uani 1 1 d . . . .
C58 C -0.1813(3) 0.62758(13) 0.17496(11) 0.0631(7) Uani 1 1 d A . . .
H58 H -0.2404 0.6524 0.1886 0.076 Uiso 1 1 calc . . R .
C59 C -0.2096(4) 0.59814(17) 0.13243(13) 0.0894(11) Uani 1 1 d . . . .
H59 H -0.2874 0.6031 0.1173 0.107 Uiso 1 1 calc A . R .
C60 C -0.1260(5) 0.56165(17) 0.11194(14) 0.0995(14) Uani 1 1 d A . . .
H60 H -0.1461 0.5410 0.0830 0.119 Uiso 1 1 calc . . R .
C61 C -0.0143(4) 0.55551(14) 0.13359(14) 0.0893(12) Uani 1 1 d . . . .
H61 H 0.0444 0.5310 0.1194 0.107 Uiso 1 1 calc A . R .
C62 C 0.0146(3) 0.58485(11) 0.17628(11) 0.0650(7) Uani 1 1 d A . . .
H62 H 0.0929 0.5797 0.1909 0.078 Uiso 1 1 calc . . R .
C63 C 0.4454(2) 0.77031(11) 0.43113(9) 0.0532(6) Uani 1 1 d . . . .
C64 C 0.4839(4) 0.70994(17) 0.45413(18) 0.1175(18) Uani 1 1 d A . . .
H64A H 0.5627 0.7148 0.4711 0.176 Uiso 1 1 calc . . GR .
H64B H 0.4897 0.6790 0.4293 0.176 Uiso 1 1 calc . . GR .
H64C H 0.4240 0.6974 0.4767 0.176 Uiso 1 1 calc . . GR .
C65 C 0.5452(3) 0.7907(2) 0.40017(14) 0.1041(14) Uani 1 1 d A . . .
H65A H 0.5300 0.8325 0.3897 0.156 Uiso 1 1 calc . . GR .
H65B H 0.5478 0.7642 0.3723 0.156 Uiso 1 1 calc . . GR .
H65C H 0.6227 0.7888 0.4184 0.156 Uiso 1 1 calc . . GR .
C66 C 0.4297(3) 0.81606(18) 0.47068(13) 0.0895(11) Uani 1 1 d A . . .
H66A H 0.4037 0.8549 0.4568 0.134 Uiso 1 1 calc . . GR .
H66B H 0.5067 0.8214 0.4888 0.134 Uiso 1 1 calc . . GR .
H66C H 0.3687 0.8014 0.4919 0.134 Uiso 1 1 calc . . GR .
C67A C 0.0603(7) 0.6575(4) 0.4000(4) 0.045(2) Uani 0.50 1 d A 2 D U
C67 C 0.0257(8) 0.6700(4) 0.4016(3) 0.045(2) Uani 0.50 1 d A 1 D U
C68A C 0.1022(9) 0.6292(5) 0.4470(3) 0.088(3) Uani 0.50 1 d A 2 D U
H68A H 0.1820 0.6110 0.4440 0.132 Uiso 0.50 1 calc A 2 GR .
H68B H 0.0447 0.5979 0.4557 0.132 Uiso 0.50 1 calc A 2 GR .
H68C H 0.1070 0.6605 0.4718 0.132 Uiso 0.50 1 calc A 2 GR .
C68 C 0.0496(8) 0.6493(4) 0.4532(2) 0.0641(19) Uani 0.50 1 d A 1 D U
H68D H -0.0152 0.6221 0.4622 0.096 Uiso 0.50 1 calc A 1 GR .
H68E H 0.0523 0.6848 0.4742 0.096 Uiso 0.50 1 calc A 1 GR .
H68F H 0.1270 0.6279 0.4561 0.096 Uiso 0.50 1 calc A 1 GR .
C69 C 0.0175(8) 0.6167(4) 0.3683(3) 0.064(2) Uani 0.50 1 d A 1 D U
H69A H 0.0949 0.5952 0.3694 0.096 Uiso 0.50 1 calc A 1 GR .
H69B H -0.0015 0.6310 0.3357 0.096 Uiso 0.50 1 calc A 1 GR .
H69C H -0.0462 0.5893 0.3779 0.096 Uiso 0.50 1 calc A 1 GR .
C69A C 0.0651(8) 0.6064(4) 0.3640(4) 0.077(2) Uani 0.50 1 d A 2 D U
H69D H 0.1487 0.5927 0.3619 0.115 Uiso 0.50 1 calc A 2 GR .
H69E H 0.0344 0.6208 0.3328 0.115 Uiso 0.50 1 calc A 2 GR .
H69F H 0.0152 0.5726 0.3742 0.115 Uiso 0.50 1 calc A 2 GR .
C70 C -0.1009(8) 0.7007(4) 0.4022(4) 0.078(2) Uani 0.50 1 d A 1 D U
H70A H -0.1594 0.6720 0.4143 0.117 Uiso 0.50 1 calc A 1 GR .
H70B H -0.1268 0.7130 0.3698 0.117 Uiso 0.50 1 calc A 1 GR .
H70C H -0.0960 0.7365 0.4228 0.117 Uiso 0.50 1 calc A 1 GR .
C70A C -0.0695(9) 0.6785(5) 0.4002(4) 0.097(3) Uani 0.50 1 d A 2 D U
H70D H -0.1205 0.6451 0.4103 0.146 Uiso 0.50 1 calc A 2 GR .
H70E H -0.0965 0.6914 0.3680 0.146 Uiso 0.50 1 calc A 2 GR .
H70F H -0.0757 0.7126 0.4223 0.146 Uiso 0.50 1 calc A 2 GR .


_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
Ti1 O1 1.8343(12) . ?
Ti1 N1 2.1805(15) . ?
Ti1 C2 2.5525(18) . ?
Ti1 C3 2.3779(18) . ?
Ti1 C4 2.335(2) . ?
Ti1 C16A 2.155(4) . ?
Ti1 C16 2.218(4) . ?
Ti1 C23A 2.282(9) . ?
Ti1 C23 1.993(11) . ?
Ti2 O2 1.8273(15) . ?
Ti2 N2 2.1857(15) . ?
Ti2 C1 2.3491(19) . ?
Ti2 C2 2.396(2) . ?
Ti2 C3 2.5515(18) . ?
Ti2 C49 2.150(2) . ?
Ti2 C56 2.158(2) . ?
O1 C15 1.352(2) . ?
O2 C48 1.357(3) . ?
N1 C5 1.368(2) . ?
N1 C9 1.372(2) . ?
N2 C38 1.364(2) . ?
N2 C42 1.369(3) . ?
C1 H1 0.9500 . ?
C1 C2 1.438(3) . ?
C1 C5 1.443(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.409(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.432(3) . ?
C4 H4 0.9500 . ?
C4 C38 1.445(3) . ?
C5 C6 1.396(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.366(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.387(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.389(3) . ?
C9 C10 1.480(2) . ?
C10 C11 1.405(3) . ?
C10 C15 1.399(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.376(3) . ?
C12 C13 1.399(3) . ?
C12 C30 1.533(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(3) . ?
C14 C15 1.416(2) . ?
C14 C34 1.542(2) . ?
C16A H16A 0.9900 . ?
C16A H16B 0.9900 . ?
C16A C17A 1.492(9) . ?
C16 H16C 0.9900 . ?
C16 H16D 0.9900 . ?
C16 C17 1.481(9) . ?
C17 C18 1.392(7) . ?
C17 C22 1.399(7) . ?
C18 H18 0.9500 . ?
C18 C19 1.385(7) . ?
C19 H19 0.9500 . ?
C19 C20 1.373(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.378(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.384(5) . ?
C22 H22 0.9500 . ?
C17A C18A 1.386(8) . ?
C17A C22A 1.414(9) . ?
C18A H18A 0.9500 . ?
C18A C19A 1.389(6) . ?
C19A H19A 0.9500 . ?
C19A C20A 1.372(9) . ?
C20A H20A 0.9500 . ?
C20A C21A 1.371(9) . ?
C21A H21A 0.9500 . ?
C21A C22A 1.401(8) . ?
C22A H22A 0.9500 . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
C23A C24A 1.473(9) . ?
C23 H23C 0.9900 . ?
C23 H23D 0.9900 . ?
C23 C24 1.505(11) . ?
C24 C25 1.395(7) . ?
C24 C29 1.391(7) . ?
C25 H25 0.9500 . ?
C25 C26 1.398(7) . ?
C26 H26 0.9500 . ?
C26 C27 1.401(8) . ?
C27 H27 0.9500 . ?
C27 C28 1.388(8) . ?
C28 H28 0.9500 . ?
C28 C29 1.372(7) . ?
C29 H29 0.9500 . ?
C24A C25A 1.383(9) . ?
C24A C29A 1.398(9) . ?
C25A H25A 0.9500 . ?
C25A C26A 1.386(10) . ?
C26A H26A 0.9500 . ?
C26A C27A 1.413(11) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.359(10) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.351(9) . ?
C29A H29A 0.9500 . ?
C30 C31 1.526(3) . ?
C30 C32 1.531(3) . ?
C30 C33 1.529(3) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.534(3) . ?
C34 C36 1.533(3) . ?
C34 C37 1.536(3) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.399(3) . ?
C39 H39 0.9500 . ?
C39 C40 1.365(3) . ?
C40 H40 0.9500 . ?
C40 C41 1.391(3) . ?
C41 H41 0.9500 . ?
C41 C42 1.387(3) . ?
C42 C43 1.482(3) . ?
C43 C44 1.398(3) . ?
C43 C48 1.399(3) . ?
C44 H44 0.9500 . ?
C44 C45 1.387(3) . ?
C45 C46 1.385(3) . ?
C45 C63 1.532(3) . ?
C46 H46 0.9500 . ?
C46 C47 1.386(3) . ?
C47 C48 1.407(3) . ?
C47 C67A 1.515(10) . ?
C47 C67 1.590(9) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.478(3) . ?
C50 C51 1.399(3) . ?
C50 C55 1.385(4) . ?
C51 H51 0.9500 . ?
C51 C52 1.368(4) . ?
C52 H52 0.9500 . ?
C52 C53 1.363(5) . ?
C53 H53 0.9500 . ?
C53 C54 1.386(5) . ?
C54 H54 0.9500 . ?
C54 C55 1.381(4) . ?
C55 H55 0.9500 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.469(3) . ?
C57 C58 1.393(4) . ?
C57 C62 1.392(4) . ?
C58 H58 0.9500 . ?
C58 C59 1.383(4) . ?
C59 H59 0.9500 . ?
C59 C60 1.376(6) . ?
C60 H60 0.9500 . ?
C60 C61 1.361(6) . ?
C61 H61 0.9500 . ?
C61 C62 1.387(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.533(4) . ?
C63 C65 1.510(5) . ?
C63 C66 1.518(4) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67A C68A 1.515(11) . ?
C67A C69A 1.518(11) . ?
C67A C70A 1.513(8) . ?
C67 C68 1.530(9) . ?
C67 C69 1.503(10) . ?
C67 C70 1.561(9) . ?
C68A H68A 0.9800 . ?
C68A H68B 0.9800 . ?
C68A H68C 0.9800 . ?
C68 H68D 0.9800 . ?
C68 H68E 0.9800 . ?
C68 H68F 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C69A H69D 0.9800 . ?
C69A H69E 0.9800 . ?
C69A H69F 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C70A H70D 0.9800 . ?
C70A H70E 0.9800 . ?
C70A H70F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 N1 83.78(5) . . ?
O1 Ti1 C2 157.25(6) . . ?
O1 Ti1 C3 155.43(7) . . ?
O1 Ti1 C4 120.07(6) . . ?
O1 Ti1 C16A 102.51(11) . . ?
O1 Ti1 C16 89.12(11) . . ?
O1 Ti1 C23A 97.1(3) . . ?
O1 Ti1 C23 102.9(3) . . ?
N1 Ti1 C2 74.70(6) . . ?
N1 Ti1 C3 87.91(6) . . ?
N1 Ti1 C4 78.59(6) . . ?
N1 Ti1 C16 148.64(14) . . ?
N1 Ti1 C23A 100.5(2) . . ?
C3 Ti1 C2 32.96(7) . . ?
C4 Ti1 C2 63.18(7) . . ?
C4 Ti1 C3 35.38(7) . . ?
C16A Ti1 N1 168.90(11) . . ?
C16A Ti1 C2 99.93(12) . . ?
C16A Ti1 C3 82.64(11) . . ?
C16A Ti1 C4 90.32(11) . . ?
C16A Ti1 C16 25.05(14) . . ?
C16A Ti1 C23A 87.9(3) . . ?
C16 Ti1 C2 113.13(11) . . ?
C16 Ti1 C3 86.02(11) . . ?
C16 Ti1 C4 78.73(12) . . ?
C16 Ti1 C23A 110.7(3) . . ?
C23A Ti1 C2 80.0(3) . . ?
C23A Ti1 C3 107.2(3) . . ?
C23A Ti1 C4 142.2(3) . . ?
C23 Ti1 N1 108.9(3) . . ?
C23 Ti1 C2 77.8(3) . . ?
C23 Ti1 C3 101.7(3) . . ?
C23 Ti1 C4 137.1(3) . . ?
C23 Ti1 C16A 78.9(3) . . ?
C23 Ti1 C16 102.5(3) . . ?
C23 Ti1 C23A 9.9(4) . . ?
O2 Ti2 N2 83.30(6) . . ?
O2 Ti2 C1 121.11(7) . . ?
O2 Ti2 C2 156.35(7) . . ?
O2 Ti2 C3 157.25(7) . . ?
O2 Ti2 C49 99.99(8) . . ?
O2 Ti2 C56 91.58(8) . . ?
N2 Ti2 C1 79.94(6) . . ?
N2 Ti2 C2 88.98(6) . . ?
N2 Ti2 C3 75.34(6) . . ?
C1 Ti2 C2 35.26(7) . . ?
C1 Ti2 C3 63.06(7) . . ?
C2 Ti2 C3 32.90(7) . . ?
C49 Ti2 N2 106.55(7) . . ?
C49 Ti2 C1 138.89(8) . . ?
C49 Ti2 C2 103.64(8) . . ?
C49 Ti2 C3 79.09(7) . . ?
C49 Ti2 C56 96.82(9) . . ?
C56 Ti2 N2 156.59(8) . . ?
C56 Ti2 C1 83.31(8) . . ?
C56 Ti2 C2 86.68(8) . . ?
C56 Ti2 C3 111.14(8) . . ?
C15 O1 Ti1 133.25(10) . . ?
C48 O2 Ti2 134.89(13) . . ?
C5 N1 Ti1 117.73(12) . . ?
C5 N1 C9 118.53(15) . . ?
C9 N1 Ti1 123.14(11) . . ?
C38 N2 Ti2 116.78(13) . . ?
C38 N2 C42 118.71(16) . . ?
C42 N2 Ti2 123.52(12) . . ?
Ti2 C1 H1 81.2 . . ?
C2 C1 Ti2 74.14(11) . . ?
C2 C1 H1 118.2 . . ?
C2 C1 C5 123.58(17) . . ?
C5 C1 Ti2 114.69(13) . . ?
C5 C1 H1 118.2 . . ?
Ti1 C2 H2 103.7 . . ?
Ti2 C2 Ti1 128.27(9) . . ?
Ti2 C2 H2 126.4 . . ?
C1 C2 Ti1 101.05(12) . . ?
C1 C2 Ti2 70.60(11) . . ?
C1 C2 H2 115.5 . . ?
C3 C2 Ti1 66.69(10) . . ?
C3 C2 Ti2 79.64(12) . . ?
C3 C2 C1 128.94(19) . . ?
C3 C2 H2 115.5 . . ?
Ti1 C3 Ti2 129.17(8) . . ?
Ti1 C3 H3 125.6 . . ?
Ti2 C3 H3 103.9 . . ?
C2 C3 Ti1 80.35(11) . . ?
C2 C3 Ti2 67.46(11) . . ?
C2 C3 H3 115.4 . . ?
C2 C3 C4 129.23(18) . . ?
C4 C3 Ti1 70.66(10) . . ?
C4 C3 Ti2 100.21(13) . . ?
C4 C3 H3 115.4 . . ?
Ti1 C4 H4 79.1 . . ?
C3 C4 Ti1 73.96(11) . . ?
C3 C4 H4 117.6 . . ?
C3 C4 C38 124.76(17) . . ?
C38 C4 Ti1 116.85(12) . . ?
C38 C4 H4 117.6 . . ?
N1 C5 C1 118.23(16) . . ?
N1 C5 C6 121.24(17) . . ?
C6 C5 C1 120.53(17) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 C5 119.85(17) . . ?
C7 C6 H6 120.1 . . ?
C6 C7 H7 120.4 . . ?
C6 C7 C8 119.16(18) . . ?
C8 C7 H7 120.4 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.15(18) . . ?
C9 C8 H8 119.9 . . ?
N1 C9 C8 120.70(16) . . ?
N1 C9 C10 120.77(15) . . ?
C8 C9 C10 118.50(16) . . ?
C11 C10 C9 118.91(16) . . ?
C15 C10 C9 122.10(16) . . ?
C15 C10 C11 118.81(16) . . ?
C10 C11 H11 119.1 . . ?
C12 C11 C10 121.84(17) . . ?
C12 C11 H11 119.1 . . ?
C11 C12 C13 117.17(17) . . ?
C11 C12 C30 123.33(17) . . ?
C13 C12 C30 119.44(17) . . ?
C12 C13 H13 117.9 . . ?
C14 C13 C12 124.15(17) . . ?
C14 C13 H13 117.9 . . ?
C13 C14 C15 116.62(16) . . ?
C13 C14 C34 121.35(15) . . ?
C15 C14 C34 121.91(16) . . ?
O1 C15 C10 118.59(15) . . ?
O1 C15 C14 120.58(15) . . ?
C10 C15 C14 120.79(16) . . ?
Ti1 C16A H16A 105.5 . . ?
Ti1 C16A H16B 105.5 . . ?
H16A C16A H16B 106.1 . . ?
C17A C16A Ti1 127.1(7) . . ?
C17A C16A H16A 105.5 . . ?
C17A C16A H16B 105.5 . . ?
Ti1 C16 H16C 106.1 . . ?
Ti1 C16 H16D 106.1 . . ?
H16C C16 H16D 106.3 . . ?
C17 C16 Ti1 124.9(7) . . ?
C17 C16 H16C 106.1 . . ?
C17 C16 H16D 106.1 . . ?
C18 C17 C16 122.2(6) . . ?
C18 C17 C22 116.4(6) . . ?
C22 C17 C16 120.8(6) . . ?
C17 C18 H18 119.2 . . ?
C19 C18 C17 121.7(5) . . ?
C19 C18 H18 119.2 . . ?
C18 C19 H19 119.9 . . ?
C20 C19 C18 120.2(6) . . ?
C20 C19 H19 119.9 . . ?
C19 C20 H20 120.2 . . ?
C19 C20 C21 119.7(6) . . ?
C21 C20 H20 120.2 . . ?
C20 C21 H21 120.0 . . ?
C20 C21 C22 119.9(4) . . ?
C22 C21 H21 120.0 . . ?
C17 C22 H22 119.1 . . ?
C21 C22 C17 121.7(5) . . ?
C21 C22 H22 119.1 . . ?
C18A C17A C16A 121.8(6) . . ?
C18A C17A C22A 116.4(6) . . ?
C22A C17A C16A 120.5(7) . . ?
C17A C18A H18A 119.1 . . ?
C17A C18A C19A 121.8(5) . . ?
C19A C18A H18A 119.1 . . ?
C18A C19A H19A 119.6 . . ?
C20A C19A C18A 120.8(5) . . ?
C20A C19A H19A 119.6 . . ?
C19A C20A H20A 120.4 . . ?
C21A C20A C19A 119.2(6) . . ?
C21A C20A H20A 120.4 . . ?
C20A C21A H21A 119.7 . . ?
C20A C21A C22A 120.6(6) . . ?
C22A C21A H21A 119.7 . . ?
C17A C22A H22A 119.6 . . ?
C21A C22A C17A 120.8(6) . . ?
C21A C22A H22A 119.6 . . ?
Ti1 C23A H23A 108.3 . . ?
Ti1 C23A H23B 108.3 . . ?
H23A C23A H23B 107.4 . . ?
C24A C23A Ti1 115.9(8) . . ?
C24A C23A H23A 108.3 . . ?
C24A C23A H23B 108.3 . . ?
Ti1 C23 H23C 108.2 . . ?
Ti1 C23 H23D 108.2 . . ?
H23C C23 H23D 107.4 . . ?
C24 C23 Ti1 116.2(9) . . ?
C24 C23 H23C 108.2 . . ?
C24 C23 H23D 108.2 . . ?
C25 C24 C23 121.2(7) . . ?
C29 C24 C23 121.7(7) . . ?
C29 C24 C25 117.0(8) . . ?
C24 C25 H25 118.9 . . ?
C24 C25 C26 122.2(7) . . ?
C26 C25 H25 118.9 . . ?
C25 C26 H26 120.2 . . ?
C25 C26 C27 119.6(8) . . ?
C27 C26 H26 120.2 . . ?
C26 C27 H27 121.2 . . ?
C28 C27 C26 117.6(9) . . ?
C28 C27 H27 121.2 . . ?
C27 C28 H28 118.8 . . ?
C29 C28 C27 122.4(9) . . ?
C29 C28 H28 118.8 . . ?
C24 C29 H29 119.5 . . ?
C28 C29 C24 121.1(8) . . ?
C28 C29 H29 119.5 . . ?
C25A C24A C23A 120.8(8) . . ?
C25A C24A C29A 119.6(7) . . ?
C29A C24A C23A 119.5(7) . . ?
C24A C25A H25A 120.0 . . ?
C24A C25A C26A 120.1(7) . . ?
C26A C25A H25A 120.0 . . ?
C25A C26A H26A 121.0 . . ?
C25A C26A C27A 118.1(8) . . ?
C27A C26A H26A 121.0 . . ?
C26A C27A H27A 119.2 . . ?
C28A C27A C26A 121.5(8) . . ?
C28A C27A H27A 119.2 . . ?
C27A C28A H28A 120.1 . . ?
C29A C28A C27A 119.8(8) . . ?
C29A C28A H28A 120.1 . . ?
C24A C29A H29A 119.5 . . ?
C28A C29A C24A 120.9(7) . . ?
C28A C29A H29A 119.5 . . ?
C31 C30 C12 112.38(17) . . ?
C31 C30 C32 108.5(2) . . ?
C31 C30 C33 107.92(19) . . ?
C32 C30 C12 109.04(16) . . ?
C33 C30 C12 109.43(18) . . ?
C33 C30 C32 109.6(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C14 111.52(15) . . ?
C35 C34 C37 107.38(16) . . ?
C36 C34 C14 109.22(15) . . ?
C36 C34 C35 109.44(17) . . ?
C36 C34 C37 107.89(15) . . ?
C37 C34 C14 111.30(16) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N2 C38 C4 118.31(17) . . ?
N2 C38 C39 121.20(19) . . ?
C39 C38 C4 120.49(17) . . ?
C38 C39 H39 120.0 . . ?
C40 C39 C38 119.95(18) . . ?
C40 C39 H39 120.0 . . ?
C39 C40 H40 120.5 . . ?
C39 C40 C41 118.96(19) . . ?
C41 C40 H40 120.5 . . ?
C40 C41 H41 119.9 . . ?
C42 C41 C40 120.2(2) . . ?
C42 C41 H41 119.9 . . ?
N2 C42 C41 120.76(17) . . ?
N2 C42 C43 120.49(16) . . ?
C41 C42 C43 118.72(18) . . ?
C44 C43 C42 119.26(17) . . ?
C44 C43 C48 118.48(18) . . ?
C48 C43 C42 122.12(18) . . ?
C43 C44 H44 119.0 . . ?
C45 C44 C43 122.0(2) . . ?
C45 C44 H44 119.0 . . ?
C44 C45 C63 121.5(2) . . ?
C46 C45 C44 116.9(2) . . ?
C46 C45 C63 121.5(2) . . ?
C45 C46 H46 117.9 . . ?
C45 C46 C47 124.3(2) . . ?
C47 C46 H46 117.9 . . ?
C46 C47 C48 116.7(2) . . ?
C46 C47 C67A 115.7(4) . . ?
C46 C47 C67 125.5(3) . . ?
C48 C47 C67A 127.1(4) . . ?
C48 C47 C67 117.3(4) . . ?
C67A C47 C67 17.4(4) . . ?
O2 C48 C43 117.78(17) . . ?
O2 C48 C47 121.27(18) . . ?
C43 C48 C47 120.9(2) . . ?
Ti2 C49 H49A 109.4 . . ?
Ti2 C49 H49B 109.4 . . ?
H49A C49 H49B 108.0 . . ?
C50 C49 Ti2 110.95(14) . . ?
C50 C49 H49A 109.4 . . ?
C50 C49 H49B 109.4 . . ?
C51 C50 C49 120.8(2) . . ?
C55 C50 C49 121.7(2) . . ?
C55 C50 C51 117.5(2) . . ?
C50 C51 H51 119.4 . . ?
C52 C51 C50 121.2(3) . . ?
C52 C51 H51 119.4 . . ?
C51 C52 H52 119.7 . . ?
C53 C52 C51 120.7(3) . . ?
C53 C52 H52 119.7 . . ?
C52 C53 H53 120.2 . . ?
C52 C53 C54 119.5(3) . . ?
C54 C53 H53 120.2 . . ?
C53 C54 H54 120.0 . . ?
C55 C54 C53 120.0(3) . . ?
C55 C54 H54 120.0 . . ?
C50 C55 H55 119.4 . . ?
C54 C55 C50 121.1(3) . . ?
C54 C55 H55 119.4 . . ?
Ti2 C56 H56A 105.8 . . ?
Ti2 C56 H56B 105.8 . . ?
H56A C56 H56B 106.2 . . ?
C57 C56 Ti2 126.19(15) . . ?
C57 C56 H56A 105.8 . . ?
C57 C56 H56B 105.8 . . ?
C58 C57 C56 121.5(2) . . ?
C62 C57 C56 122.1(2) . . ?
C62 C57 C58 116.4(3) . . ?
C57 C58 H58 119.2 . . ?
C59 C58 C57 121.5(3) . . ?
C59 C58 H58 119.2 . . ?
C58 C59 H59 119.8 . . ?
C60 C59 C58 120.5(4) . . ?
C60 C59 H59 119.8 . . ?
C59 C60 H60 120.4 . . ?
C61 C60 C59 119.3(3) . . ?
C61 C60 H60 120.4 . . ?
C60 C61 H61 119.8 . . ?
C60 C61 C62 120.5(4) . . ?
C62 C61 H61 119.8 . . ?
C57 C62 H62 119.1 . . ?
C61 C62 C57 121.8(3) . . ?
C61 C62 H62 119.1 . . ?
C45 C63 C64 111.8(2) . . ?
C65 C63 C45 110.8(2) . . ?
C65 C63 C64 107.8(3) . . ?
C65 C63 C66 109.7(3) . . ?
C66 C63 C45 108.8(2) . . ?
C66 C63 C64 108.0(3) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C47 C67A C69A 112.8(8) . . ?
C68A C67A C47 114.0(7) . . ?
C68A C67A C69A 104.7(8) . . ?
C70A C67A C47 106.0(7) . . ?
C70A C67A C68A 112.0(8) . . ?
C70A C67A C69A 107.1(8) . . ?
C68 C67 C47 109.6(6) . . ?
C68 C67 C70 103.5(7) . . ?
C69 C67 C47 108.3(7) . . ?
C69 C67 C68 111.1(7) . . ?
C69 C67 C70 108.6(7) . . ?
C70 C67 C47 115.7(6) . . ?
C67A C68A H68A 109.5 . . ?
C67A C68A H68B 109.5 . . ?
C67A C68A H68C 109.5 . . ?
H68A C68A H68B 109.5 . . ?
H68A C68A H68C 109.5 . . ?
H68B C68A H68C 109.5 . . ?
C67A C69A H69D 109.5 . . ?
C67A C69A H69E 109.5 . . ?
C67A C69A H69F 109.5 . . ?
H69D C69A H69E 109.5 . . ?
H69D C69A H69F 109.5 . . ?
H69E C69A H69F 109.5 . . ?
C67A C70A H70D 109.5 . . ?
C67A C70A H70E 109.5 . . ?
C67A C70A H70F 109.5 . . ?
H70D C70A H70E 109.5 . . ?
H70D C70A H70F 109.5 . . ?
H70E C70A H70F 109.5 . . ?


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method toulene/n-pentane
_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_Zr2-H_090513a_ben
_database_code_depnum_ccdc_archive 'CCDC 1486142'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_audit_creation_date             2013-09-12
_audit_creation_method           
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_chemical_name_common            ?
_chemical_name_systematic        Zr2-H
_chemical_formula_moiety         'C70 H78 N2 O2 Zr2, 0.5(C4 H10 O)'
_chemical_formula_sum            'C72 H83 N2 O2.50 Zr2'
_chemical_formula_weight         1198.84
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   11.3506(3)
_cell_length_b                   15.5365(5)
_cell_length_c                   19.1544(6)
_cell_angle_alpha                79.469(2)
_cell_angle_beta                 79.993(2)
_cell_angle_gamma                81.353(2)
_cell_volume                     3245.81(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    14861
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.5719
_cell_measurement_theta_min      3.4480
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             1258
_exptl_crystal_size_max          0.71
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24742
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.45
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   34.00   60.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000 -150.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega   -5.00   25.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000   90.0000 30

#__ type_ start__ end____ width___ exp.time_
  3 omega    1.00   35.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 34

#__ type_ start__ end____ width___ exp.time_
  4 omega  -69.00  -30.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -60.0000 39

#__ type_ start__ end____ width___ exp.time_
  5 omega  -13.00   20.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000  -60.0000 33

#__ type_ start__ end____ width___ exp.time_
  6 omega   43.00   72.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   37.0000   90.0000 29

#__ type_ start__ end____ width___ exp.time_
  7 omega  -65.00   10.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000   57.0000  -90.0000 75

#__ type_ start__ end____ width___ exp.time_
  8 omega -123.00  -30.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -37.0000  120.0000 93

#__ type_ start__ end____ width___ exp.time_
  9 omega   73.00  126.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  120.0000 53

#__ type_ start__ end____ width___ exp.time_
 10 omega   -8.00   71.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -37.0000    0.0000 79

#__ type_ start__ end____ width___ exp.time_
 11 omega   73.00  126.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000   60.0000 53

#__ type_ start__ end____ width___ exp.time_
 12 omega   49.00   85.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  -77.0000   60.0000 36

#__ type_ start__ end____ width___ exp.time_
 13 omega -113.00  -45.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  111.0000   30.0000 68

#__ type_ start__ end____ width___ exp.time_
 14 omega  -71.00  -27.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   25.0000  -60.0000 44

#__ type_ start__ end____ width___ exp.time_
 15 omega   44.00   82.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000   60.0000 38

#__ type_ start__ end____ width___ exp.time_
 16 omega   42.00   71.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -30.0000 29

#__ type_ start__ end____ width___ exp.time_
 17 omega   38.00  153.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   12.0000   30.0000 115

#__ type_ start__ end____ width___ exp.time_
 18 omega   43.00   71.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 28

#__ type_ start__ end____ width___ exp.time_
 19 omega   42.00   88.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000 -180.0000 46

#__ type_ start__ end____ width___ exp.time_
 20 omega   38.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000   30.0000 32

#__ type_ start__ end____ width___ exp.time_
 21 omega   52.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -12.0000 53

#__ type_ start__ end____ width___ exp.time_
 22 omega   38.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  120.0000 25

#__ type_ start__ end____ width___ exp.time_
 23 omega   42.00   71.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -60.0000 29

#__ type_ start__ end____ width___ exp.time_
 24 omega   42.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
 25 omega   92.00  131.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000 -180.0000 39

#__ type_ start__ end____ width___ exp.time_
 26 omega   76.00  148.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   25.0000 -120.0000 72

#__ type_ start__ end____ width___ exp.time_
 27 omega   81.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   44.0000 27

#__ type_ start__ end____ width___ exp.time_
 28 omega   39.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -90.0000 31

#__ type_ start__ end____ width___ exp.time_
 29 omega   98.00  141.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   90.0000 43

#__ type_ start__ end____ width___ exp.time_
 30 omega   97.00  141.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -60.0000 44

#__ type_ start__ end____ width___ exp.time_
 31 omega   45.00   73.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  -60.0000 28

#__ type_ start__ end____ width___ exp.time_
 32 omega   38.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000    0.0000 32

#__ type_ start__ end____ width___ exp.time_
 33 omega   40.00   65.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 25

#__ type_ start__ end____ width___ exp.time_
 34 omega   38.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000 -150.0000 25

#__ type_ start__ end____ width___ exp.time_
 35 omega  105.00  131.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -63.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 36 omega   41.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000  154.0000 67

#__ type_ start__ end____ width___ exp.time_
 37 omega   51.00  127.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000   23.0000 76

#__ type_ start__ end____ width___ exp.time_
 38 omega   88.00  171.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   63.0000 -120.0000 83

#__ type_ start__ end____ width___ exp.time_
 39 omega   71.00  134.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -88.0000 -126.0000 63
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0853449000
_diffrn_orient_matrix_UB_12      0.0672176000
_diffrn_orient_matrix_UB_13      0.0408822000
_diffrn_orient_matrix_UB_21      -0.0091858000
_diffrn_orient_matrix_UB_22      -0.0696897000
_diffrn_orient_matrix_UB_23      0.0685357000
_diffrn_orient_matrix_UB_31      0.1091604000
_diffrn_orient_matrix_UB_32      0.0308548000
_diffrn_orient_matrix_UB_33      0.0218855000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                10741
_reflns_number_total             11537
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.218
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     806
_refine_ls_number_reflns         11537
_refine_ls_number_restraints     162
_refine_ls_R_factor_all          0.0399
_refine_ls_R_factor_gt           0.0377
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0734P)²+2.4761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1149
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.022146(18) 0.464880(13) 0.237148(11) 0.02060(8) Uani 1 1 d . B .
Zr2 Zr -0.077044(18) 0.203681(14) 0.179663(12) 0.02208(8) Uani 1 1 d . . .
O1 O 0.13389(16) 0.49981(11) 0.29253(9) 0.0228(4) Uani 1 1 d . B .
O1S O 0.7393(14) 0.0604(11) 0.4575(9) 0.190(6) Uiso 0.50 1 d PD . .
O2 O -0.05265(17) 0.07443(12) 0.21374(11) 0.0296(4) Uani 1 1 d . B .
N1 N 0.16787(18) 0.34591(13) 0.23369(11) 0.0198(4) Uani 1 1 d . B .
N2 N 0.01766(19) 0.19760(14) 0.27674(11) 0.0216(4) Uani 1 1 d . B .
C1 C 0.0698(2) 0.31471(16) 0.13878(14) 0.0230(5) Uani 1 1 d . B .
H1 H 0.0963 0.3211 0.0857 0.028 Uiso 1 1 calc R . .
C1S C 0.5956(14) 0.0341(12) 0.3831(9) 0.127(5) Uiso 0.50 1 d PD . .
H1SA H 0.5985 -0.0083 0.3506 0.190 Uiso 0.50 1 calc PR . .
H1SB H 0.5627 0.0927 0.3609 0.190 Uiso 0.50 1 calc PR . .
H1SC H 0.5439 0.0158 0.4284 0.190 Uiso 0.50 1 calc PR . .
C2 C -0.0453(2) 0.36496(17) 0.15549(14) 0.0250(5) Uani 1 1 d . B .
H2 H -0.0730 0.4050 0.1163 0.030 Uiso 1 1 calc R . .
C2S C 0.7209(16) 0.0373(14) 0.3978(10) 0.145(6) Uiso 0.50 1 d PD . .
H2SA H 0.7658 -0.0221 0.3952 0.174 Uiso 0.50 1 calc PR . .
H2SB H 0.7597 0.0781 0.3574 0.174 Uiso 0.50 1 calc PR . .
C3 C -0.1234(2) 0.36374(17) 0.22152(15) 0.0253(5) Uani 1 1 d . B .
H3 H -0.2067 0.3800 0.2184 0.030 Uiso 1 1 calc R . .
C3S C 0.8467(11) 0.0625(9) 0.4744(7) 0.092(3) Uiso 0.50 1 d PD . .
H3SA H 0.8984 0.0920 0.4325 0.111 Uiso 0.50 1 calc PR . .
H3SB H 0.8856 0.0016 0.4877 0.111 Uiso 0.50 1 calc PR . .
C4 C -0.0929(2) 0.34111(17) 0.29243(15) 0.0250(5) Uani 1 1 d . . .
H4 H -0.1614 0.3576 0.3300 0.030 Uiso 1 1 calc R B .
C4S C 0.8333(12) 0.1108(9) 0.5350(7) 0.096(4) Uiso 0.50 1 d PD . .
H4SA H 0.8173 0.1742 0.5179 0.143 Uiso 0.50 1 calc PR . .
H4SB H 0.9078 0.0987 0.5563 0.143 Uiso 0.50 1 calc PR . .
H4SC H 0.7661 0.0918 0.5712 0.143 Uiso 0.50 1 calc PR . .
C5 C 0.1726(2) 0.30242(16) 0.17710(13) 0.0215(5) Uani 1 1 d . . .
C6 C 0.2769(2) 0.24801(18) 0.15354(15) 0.0277(6) Uani 1 1 d . B .
H6 H 0.2793 0.2184 0.1140 0.033 Uiso 1 1 calc R . .
C7 C 0.3753(2) 0.2380(2) 0.18824(16) 0.0310(6) Uani 1 1 d . . .
H7 H 0.4475 0.2032 0.1718 0.037 Uiso 1 1 calc R B .
C8 C 0.3688(2) 0.27905(19) 0.24745(15) 0.0283(6) Uani 1 1 d . B .
H8 H 0.4362 0.2714 0.2722 0.034 Uiso 1 1 calc R . .
C9 C 0.2640(2) 0.33124(16) 0.27062(13) 0.0216(5) Uani 1 1 d . . .
C10 C 0.2573(2) 0.37075(17) 0.33639(14) 0.0225(5) Uani 1 1 d . B .
C11 C 0.3171(2) 0.32214(18) 0.39166(15) 0.0259(5) Uani 1 1 d . . .
H11 H 0.3547 0.2642 0.3870 0.031 Uiso 1 1 calc R B .
C12 C 0.3232(2) 0.35556(19) 0.45281(15) 0.0286(6) Uani 1 1 d . A .
C13 C 0.2717(2) 0.44217(19) 0.45603(15) 0.0282(6) Uani 1 1 d . . .
H13 H 0.2780 0.4669 0.4969 0.034 Uiso 1 1 calc R B .
C14 C 0.2116(2) 0.49471(17) 0.40298(14) 0.0241(5) Uani 1 1 d . B .
C15 C 0.1991(2) 0.45600(17) 0.34390(14) 0.0216(5) Uani 1 1 d . . .
C16 C -0.1426(2) 0.54153(18) 0.29705(16) 0.0300(6) Uani 1 1 d . . .
H16A H -0.1435 0.5208 0.3492 0.036 Uiso 1 1 calc R B .
H16B H -0.1297 0.6045 0.2878 0.036 Uiso 1 1 calc R . .
C17 C -0.2637(2) 0.53638(18) 0.28034(15) 0.0282(6) Uani 1 1 d . B .
C18 C -0.3441(3) 0.4850(2) 0.32752(16) 0.0332(6) Uani 1 1 d . . .
H18 H -0.3232 0.4567 0.3728 0.040 Uiso 1 1 calc R B .
C19 C -0.4538(3) 0.4746(2) 0.30939(19) 0.0429(8) Uani 1 1 d . B .
H19 H -0.5060 0.4381 0.3419 0.052 Uiso 1 1 calc R . .
C20 C -0.4876(3) 0.5164(3) 0.2450(2) 0.0484(8) Uani 1 1 d . . .
H20 H -0.5628 0.5093 0.2328 0.058 Uiso 1 1 calc R B .
C21 C -0.4104(3) 0.5690(2) 0.19812(18) 0.0437(8) Uani 1 1 d . B .
H21 H -0.4330 0.5984 0.1535 0.052 Uiso 1 1 calc R . .
C22 C -0.3010(3) 0.5791(2) 0.21551(17) 0.0346(6) Uani 1 1 d . . .
H22 H -0.2497 0.6159 0.1827 0.042 Uiso 1 1 calc R B .
C23 C 0.0372(3) 0.56282(19) 0.13287(16) 0.0349(6) Uani 1 1 d . . .
H23A H -0.0307 0.5633 0.1066 0.042 Uiso 1 1 calc R B .
H23B H 0.0397 0.6232 0.1419 0.042 Uiso 1 1 calc R . .
C24 C 0.1529(3) 0.52799(18) 0.09308(15) 0.0302(6) Uani 1 1 d . B .
C25 C 0.1588(3) 0.4950(3) 0.02958(17) 0.0446(8) Uani 1 1 d . . .
H25 H 0.0874 0.5005 0.0088 0.054 Uiso 1 1 calc R B .
C26 C 0.2639(4) 0.4550(3) -0.0041(2) 0.0578(11) Uani 1 1 d . B .
H26 H 0.2644 0.4348 -0.0481 0.069 Uiso 1 1 calc R . .
C27 C 0.3682(4) 0.4440(3) 0.0251(2) 0.0584(10) Uani 1 1 d . . .
H27 H 0.4402 0.4140 0.0029 0.070 Uiso 1 1 calc R B .
C28 C 0.3664(3) 0.4772(3) 0.0871(2) 0.0537(10) Uani 1 1 d . B .
H28 H 0.4386 0.4713 0.1073 0.064 Uiso 1 1 calc R . .
C29 C 0.2616(3) 0.5190(2) 0.12056(17) 0.0400(7) Uani 1 1 d . . .
H29 H 0.2631 0.5422 0.1630 0.048 Uiso 1 1 calc R B .
C30 C 0.3861(3) 0.3007(2) 0.51393(17) 0.0372(7) Uani 1 1 d . . .
C31 C 0.4425(8) 0.2084(5) 0.4986(4) 0.055(2) Uani 0.50 1 d PU A 1
H31A H 0.3797 0.1761 0.4904 0.082 Uiso 0.50 1 calc PR A 1
H31B H 0.4796 0.1762 0.5399 0.082 Uiso 0.50 1 calc PR A 1
H31C H 0.5041 0.2140 0.4559 0.082 Uiso 0.50 1 calc PR A 1
C31A C 0.5220(8) 0.2712(7) 0.4782(5) 0.067(2) Uani 0.50 1 d PU A 2
H31D H 0.5204 0.2405 0.4381 0.100 Uiso 0.50 1 calc PR A 2
H31E H 0.5647 0.2317 0.5143 0.100 Uiso 0.50 1 calc PR A 2
H31F H 0.5637 0.3236 0.4605 0.100 Uiso 0.50 1 calc PR A 2
C32 C 0.4770(8) 0.3481(6) 0.5321(5) 0.059(2) Uani 0.50 1 d PU A 1
H32A H 0.5356 0.3633 0.4892 0.088 Uiso 0.50 1 calc PR A 1
H32B H 0.5187 0.3102 0.5695 0.088 Uiso 0.50 1 calc PR A 1
H32C H 0.4372 0.4021 0.5498 0.088 Uiso 0.50 1 calc PR A 1
C32A C 0.4043(10) 0.3572(6) 0.5682(5) 0.060(2) Uani 0.50 1 d PU A 2
H32D H 0.4392 0.4102 0.5425 0.091 Uiso 0.50 1 calc PR A 2
H32E H 0.4590 0.3231 0.6004 0.091 Uiso 0.50 1 calc PR A 2
H32F H 0.3264 0.3743 0.5964 0.091 Uiso 0.50 1 calc PR A 2
C33 C 0.2857(6) 0.2827(6) 0.5824(4) 0.0488(17) Uani 0.50 1 d PU A 1
H33A H 0.2545 0.3382 0.6003 0.073 Uiso 0.50 1 calc PR A 1
H33B H 0.3211 0.2405 0.6201 0.073 Uiso 0.50 1 calc PR A 1
H33C H 0.2196 0.2584 0.5689 0.073 Uiso 0.50 1 calc PR A 1
C33A C 0.3261(11) 0.2258(7) 0.5448(6) 0.081(3) Uani 0.50 1 d PU A 2
H33D H 0.2487 0.2446 0.5728 0.121 Uiso 0.50 1 calc PR A 2
H33E H 0.3761 0.1850 0.5763 0.121 Uiso 0.50 1 calc PR A 2
H33F H 0.3119 0.1962 0.5066 0.121 Uiso 0.50 1 calc PR A 2
C34 C 0.1673(3) 0.59255(18) 0.40735(15) 0.0285(6) Uani 1 1 d . . .
C35 C 0.1998(3) 0.6202(2) 0.47358(19) 0.0450(8) Uani 1 1 d . B .
H35A H 0.1608 0.5854 0.5171 0.067 Uiso 1 1 calc R . .
H35B H 0.1720 0.6830 0.4738 0.067 Uiso 1 1 calc R . .
H35C H 0.2874 0.6098 0.4723 0.067 Uiso 1 1 calc R . .
C36 C 0.2290(3) 0.6498(2) 0.34079(19) 0.0437(8) Uani 1 1 d . B .
H36A H 0.3167 0.6381 0.3391 0.066 Uiso 1 1 calc R . .
H36B H 0.2026 0.7123 0.3436 0.066 Uiso 1 1 calc R . .
H36C H 0.2071 0.6356 0.2973 0.066 Uiso 1 1 calc R . .
C37 C 0.0304(3) 0.6114(2) 0.4123(2) 0.0429(8) Uani 1 1 d . B .
H37A H 0.0057 0.5968 0.3698 0.064 Uiso 1 1 calc R . .
H37B H 0.0050 0.6740 0.4149 0.064 Uiso 1 1 calc R . .
H37C H -0.0075 0.5755 0.4555 0.064 Uiso 1 1 calc R . .
C38 C -0.0158(2) 0.26289(17) 0.31804(14) 0.0235(5) Uani 1 1 d . B .
C39 C 0.0238(3) 0.25535(18) 0.38457(14) 0.0293(6) Uani 1 1 d . . .
H39 H -0.0054 0.2988 0.4145 0.035 Uiso 1 1 calc R B .
C40 C 0.1047(3) 0.18510(19) 0.40606(15) 0.0317(6) Uani 1 1 d . B .
H40 H 0.1334 0.1800 0.4506 0.038 Uiso 1 1 calc R . .
C41 C 0.1446(3) 0.12144(19) 0.36236(15) 0.0297(6) Uani 1 1 d . . .
H41 H 0.2027 0.0734 0.3762 0.036 Uiso 1 1 calc R B .
C42 C 0.0996(2) 0.12762(17) 0.29837(14) 0.0230(5) Uani 1 1 d . B .
C43 C 0.1341(2) 0.05300(17) 0.25780(14) 0.0237(5) Uani 1 1 d . . .
C44 C 0.2498(2) 0.00689(17) 0.25816(14) 0.0254(5) Uani 1 1 d . B .
H44 H 0.3081 0.0303 0.2769 0.031 Uiso 1 1 calc R . .
C45 C 0.2816(2) -0.07206(18) 0.23182(14) 0.0263(5) Uani 1 1 d . . .
C46 C 0.1906(3) -0.10712(18) 0.20988(15) 0.0288(6) Uani 1 1 d . B .
H46 H 0.2091 -0.1638 0.1960 0.035 Uiso 1 1 calc R . .
C47 C 0.0742(3) -0.06421(18) 0.20706(15) 0.0280(6) Uani 1 1 d . . .
C48 C 0.0502(2) 0.02151(17) 0.22578(14) 0.0249(5) Uani 1 1 d . B .
C49 C -0.2794(12) 0.2174(8) 0.2324(4) 0.0324(18) Uani 0.60 1 d PDU B 1
H49A H -0.3032 0.1652 0.2671 0.039 Uiso 0.60 1 calc PR B 1
H49B H -0.3073 0.2727 0.2523 0.039 Uiso 0.60 1 calc PR B 1
C49A C -0.2769(17) 0.2280(10) 0.2148(7) 0.029(3) Uani 0.40 1 d PDU B 2
H49C H -0.3082 0.1819 0.2536 0.035 Uiso 0.40 1 calc PR B 2
H49D H -0.3046 0.2875 0.2273 0.035 Uiso 0.40 1 calc PR B 2
C50 C -0.3065(13) 0.2201(7) 0.1598(4) 0.0302(11) Uani 0.60 1 d PDU B 1
C50A C -0.299(2) 0.2189(11) 0.1429(6) 0.0302(11) Uani 0.40 1 d PDU B 2
C51 C -0.3022(19) 0.1443(7) 0.1262(7) 0.041(2) Uani 0.60 1 d PDU B 1
H51 H -0.2896 0.0878 0.1546 0.050 Uiso 0.60 1 calc PR B 1
C51A C -0.305(3) 0.1308(12) 0.1359(10) 0.037(3) Uani 0.40 1 d PU B 2
H51A H -0.3027 0.0839 0.1753 0.045 Uiso 0.40 1 calc PR B 2
C52 C -0.3151(10) 0.1477(6) 0.0557(6) 0.0535(19) Uani 0.60 1 d PDU B 1
H52 H -0.3169 0.0948 0.0378 0.064 Uiso 0.60 1 calc PR B 1
C52A C -0.3127(15) 0.1173(9) 0.0669(8) 0.048(2) Uani 0.40 1 d PU B 2
H52A H -0.3134 0.0596 0.0573 0.058 Uiso 0.40 1 calc PR B 2
C53 C -0.3256(8) 0.2293(7) 0.0102(5) 0.0536(18) Uani 0.60 1 d PDU B 1
H53 H -0.3314 0.2328 -0.0392 0.064 Uiso 0.60 1 calc PR B 1
C53A C -0.3198(12) 0.1907(10) 0.0118(8) 0.054(3) Uani 0.40 1 d PU B 2
H53A H -0.3254 0.1807 -0.0349 0.064 Uiso 0.40 1 calc PR B 2
C54 C -0.3272(7) 0.3029(5) 0.0390(4) 0.0437(16) Uani 0.60 1 d PDU B 1
H54 H -0.3356 0.3587 0.0089 0.052 Uiso 0.60 1 calc PR B 1
C54A C -0.3190(13) 0.2748(11) 0.0214(7) 0.052(3) Uani 0.40 1 d PU B 2
H54A H -0.3258 0.3222 -0.0174 0.062 Uiso 0.40 1 calc PR B 2
C55 C -0.3172(7) 0.3006(5) 0.1107(4) 0.0330(14) Uani 0.60 1 d PDU B 1
H55 H -0.3175 0.3546 0.1275 0.040 Uiso 0.60 1 calc PR B 1
C55A C -0.3084(14) 0.2904(9) 0.0868(7) 0.045(2) Uani 0.40 1 d PU B 2
H55A H -0.3071 0.3488 0.0948 0.054 Uiso 0.40 1 calc PR B 2
C56 C -0.0211(3) 0.1910(2) 0.05961(16) 0.0348(6) Uani 1 1 d . B .
H56A H -0.0626 0.1436 0.0501 0.042 Uiso 1 1 calc R . .
H56B H -0.0528 0.2467 0.0310 0.042 Uiso 1 1 calc R . .
C57 C 0.1094(3) 0.17205(19) 0.03134(14) 0.0293(6) Uani 1 1 d . . .
C58 C 0.1766(3) 0.0921(2) 0.05479(15) 0.0340(6) Uani 1 1 d . B .
H58 H 0.1370 0.0476 0.0871 0.041 Uiso 1 1 calc R . .
C59 C 0.2990(3) 0.0760(2) 0.03220(17) 0.0410(7) Uani 1 1 d . . .
H59 H 0.3420 0.0211 0.0495 0.049 Uiso 1 1 calc R B .
C60 C 0.3599(3) 0.1388(3) -0.01536(19) 0.0472(8) Uani 1 1 d . B .
H60 H 0.4445 0.1282 -0.0300 0.057 Uiso 1 1 calc R . .
C61 C 0.2948(3) 0.2169(2) -0.04095(18) 0.0454(8) Uani 1 1 d . . .
H61 H 0.3348 0.2599 -0.0748 0.055 Uiso 1 1 calc R B .
C62 C 0.1724(3) 0.2339(2) -0.01836(16) 0.0372(7) Uani 1 1 d . B .
H62 H 0.1300 0.2885 -0.0368 0.045 Uiso 1 1 calc R . .
C63 C 0.4117(3) -0.1174(2) 0.22998(16) 0.0324(6) Uani 1 1 d . B .
C64 C 0.4389(3) -0.1464(3) 0.30719(19) 0.0486(8) Uani 1 1 d . . .
H64A H 0.4278 -0.0948 0.3314 0.073 Uiso 1 1 calc R B .
H64B H 0.5224 -0.1746 0.3061 0.073 Uiso 1 1 calc R . .
H64C H 0.3840 -0.1885 0.3333 0.073 Uiso 1 1 calc R . .
C65 C 0.4330(3) -0.1998(2) 0.1934(2) 0.0451(8) Uani 1 1 d . . .
H65A H 0.3814 -0.2434 0.2209 0.068 Uiso 1 1 calc R B .
H65B H 0.5177 -0.2251 0.1915 0.068 Uiso 1 1 calc R . .
H65C H 0.4133 -0.1834 0.1445 0.068 Uiso 1 1 calc R . .
C66 C 0.4994(3) -0.0529(2) 0.1894(2) 0.0435(8) Uani 1 1 d . . .
H66A H 0.4810 -0.0326 0.1405 0.065 Uiso 1 1 calc R B .
H66B H 0.5822 -0.0826 0.1874 0.065 Uiso 1 1 calc R . .
H66C H 0.4912 -0.0021 0.2144 0.065 Uiso 1 1 calc R . .
C67 C -0.0244(3) -0.10837(19) 0.18541(19) 0.0377(7) Uani 1 1 d . B .
C68 C 0.0202(4) -0.2045(2) 0.1756(3) 0.0560(10) Uani 1 1 d . . .
H68A H 0.0924 -0.2062 0.1391 0.084 Uiso 1 1 calc R B .
H68B H -0.0431 -0.2298 0.1600 0.084 Uiso 1 1 calc R . .
H68C H 0.0398 -0.2389 0.2212 0.084 Uiso 1 1 calc R . .
C69 C -0.1333(3) -0.1088(3) 0.2449(2) 0.0545(10) Uani 1 1 d . . .
H69A H -0.1092 -0.1426 0.2897 0.082 Uiso 1 1 calc R B .
H69B H -0.1966 -0.1360 0.2313 0.082 Uiso 1 1 calc R . .
H69C H -0.1639 -0.0481 0.2519 0.082 Uiso 1 1 calc R . .
C70 C -0.0622(3) -0.0602(2) 0.1139(2) 0.0488(9) Uani 1 1 d . . .
H70A H -0.0904 0.0018 0.1176 0.073 Uiso 1 1 calc R B .
H70B H -0.1273 -0.0880 0.1028 0.073 Uiso 1 1 calc R . .
H70C H 0.0070 -0.0638 0.0756 0.073 Uiso 1 1 calc R . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 1.9782(17) . ?
Zr1 N1 2.290(2) . ?
Zr1 C2 2.665(3) . ?
Zr1 C3 2.533(2) . ?
Zr1 C4 2.461(3) . ?
Zr1 C16 2.305(3) . ?
Zr1 C23 2.277(3) . ?
Zr2 O2 1.9879(19) . ?
Zr2 N2 2.285(2) . ?
Zr2 C1 2.507(2) . ?
Zr2 C2 2.532(3) . ?
Zr2 C3 2.700(2) . ?
Zr2 C49 2.338(13) . ?
Zr2 C49A 2.247(19) . ?
Zr2 C50 2.665(14) . ?
Zr2 C50A 2.70(2) . ?
Zr2 C56 2.313(3) . ?
O1 C15 1.355(3) . ?
O1S C2S 1.319(15) . ?
O1S C3S 1.320(14) . ?
O2 C48 1.351(3) . ?
N1 C5 1.368(3) . ?
N1 C9 1.370(3) . ?
N2 C38 1.368(3) . ?
N2 C42 1.373(3) . ?
C1 H1 1.0000 . ?
C1 C2 1.434(4) . ?
C1 C5 1.455(4) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C1S C2S 1.507(15) . ?
C2 H2 0.9500 . ?
C2 C3 1.412(4) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3 H3 0.9500 . ?
C3 C4 1.428(4) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C3S C4S 1.469(13) . ?
C4 H4 1.0000 . ?
C4 C38 1.447(4) . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?
C5 C6 1.405(4) . ?
C6 H6 0.9500 . ?
C6 C7 1.372(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.385(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.388(4) . ?
C9 C10 1.485(4) . ?
C10 C11 1.398(4) . ?
C10 C15 1.409(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.381(4) . ?
C12 C13 1.392(4) . ?
C12 C30 1.533(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.391(4) . ?
C14 C15 1.411(4) . ?
C14 C34 1.540(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.481(4) . ?
C17 C18 1.398(4) . ?
C17 C22 1.400(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.389(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.374(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.384(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.378(5) . ?
C22 H22 0.9500 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.479(4) . ?
C24 C25 1.391(4) . ?
C24 C29 1.402(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.372(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.371(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.375(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.380(5) . ?
C29 H29 0.9500 . ?
C30 C31 1.538(8) . ?
C30 C31A 1.610(9) . ?
C30 C32 1.475(8) . ?
C30 C32A 1.536(8) . ?
C30 C33 1.594(7) . ?
C30 C33A 1.419(10) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31A H31D 0.9800 . ?
C31A H31E 0.9800 . ?
C31A H31F 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C32A H32D 0.9800 . ?
C32A H32E 0.9800 . ?
C32A H32F 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33A H33D 0.9800 . ?
C33A H33E 0.9800 . ?
C33A H33F 0.9800 . ?
C34 C35 1.529(4) . ?
C34 C36 1.540(4) . ?
C34 C37 1.527(4) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C39 1.403(4) . ?
C39 H39 0.9500 . ?
C39 C40 1.367(4) . ?
C40 H40 0.9500 . ?
C40 C41 1.386(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.389(4) . ?
C42 C43 1.479(4) . ?
C43 C44 1.398(4) . ?
C43 C48 1.406(4) . ?
C44 H44 0.9500 . ?
C44 C45 1.385(4) . ?
C45 C46 1.394(4) . ?
C45 C63 1.535(4) . ?
C46 H46 0.9500 . ?
C46 C47 1.393(4) . ?
C47 C48 1.417(4) . ?
C47 C67 1.546(4) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C49 C50 1.467(9) . ?
C49A H49C 0.9900 . ?
C49A H49D 0.9900 . ?
C49A C50A 1.477(13) . ?
C50 C51 1.433(13) . ?
C50 C55 1.424(10) . ?
C50A C51A 1.41(2) . ?
C50A C55A 1.402(18) . ?
C51 H51 0.9500 . ?
C51 C52 1.374(13) . ?
C51A H51A 0.9500 . ?
C51A C52A 1.39(2) . ?
C52 H52 0.9500 . ?
C52 C53 1.404(11) . ?
C52A H52A 0.9500 . ?
C52A C53A 1.409(17) . ?
C53 H53 0.9500 . ?
C53 C54 1.354(10) . ?
C53A H53A 0.9500 . ?
C53A C54A 1.354(19) . ?
C54 H54 0.9500 . ?
C54 C55 1.392(8) . ?
C54A H54A 0.9500 . ?
C54A C55A 1.347(19) . ?
C55 H55 0.9500 . ?
C55A H55A 0.9500 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C57 1.490(4) . ?
C57 C58 1.400(4) . ?
C57 C62 1.406(4) . ?
C58 H58 0.9500 . ?
C58 C59 1.380(5) . ?
C59 H59 0.9500 . ?
C59 C60 1.385(5) . ?
C60 H60 0.9500 . ?
C60 C61 1.377(5) . ?
C61 H61 0.9500 . ?
C61 C62 1.382(5) . ?
C62 H62 0.9500 . ?
C63 C64 1.536(4) . ?
C63 C65 1.538(4) . ?
C63 C66 1.532(4) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 C68 1.538(4) . ?
C67 C69 1.529(5) . ?
C67 C70 1.534(5) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zr1 N1 80.69(7) . . ?
O1 Zr1 C2 154.86(8) . . ?
O1 Zr1 C3 151.56(8) . . ?
O1 Zr1 C4 118.54(8) . . ?
O1 Zr1 C16 92.27(9) . . ?
O1 Zr1 C23 103.92(10) . . ?
N1 Zr1 C2 74.41(8) . . ?
N1 Zr1 C3 86.91(8) . . ?
N1 Zr1 C4 77.77(8) . . ?
N1 Zr1 C16 150.72(9) . . ?
C3 Zr1 C2 31.39(9) . . ?
C4 Zr1 C2 59.60(8) . . ?
C4 Zr1 C3 33.20(9) . . ?
C16 Zr1 C2 111.22(9) . . ?
C16 Zr1 C3 86.13(9) . . ?
C16 Zr1 C4 80.91(9) . . ?
C23 Zr1 N1 112.39(9) . . ?
C23 Zr1 C2 82.74(10) . . ?
C23 Zr1 C3 104.46(10) . . ?
C23 Zr1 C4 137.52(11) . . ?
C23 Zr1 C16 96.89(11) . . ?
O2 Zr2 N2 78.70(8) . . ?
O2 Zr2 C1 131.48(8) . . ?
O2 Zr2 C2 160.71(8) . . ?
O2 Zr2 C3 144.54(8) . . ?
O2 Zr2 C49 93.2(3) . . ?
O2 Zr2 C49A 98.7(4) . . ?
O2 Zr2 C50 99.0(2) . . ?
O2 Zr2 C50A 99.6(3) . . ?
O2 Zr2 C56 94.32(10) . . ?
N2 Zr2 C1 75.65(8) . . ?
N2 Zr2 C2 84.26(8) . . ?
N2 Zr2 C3 71.97(8) . . ?
N2 Zr2 C49 101.3(2) . . ?
N2 Zr2 C50 134.56(17) . . ?
N2 Zr2 C50A 141.4(3) . . ?
N2 Zr2 C56 137.02(9) . . ?
C1 Zr2 C2 33.07(8) . . ?
C1 Zr2 C3 59.15(8) . . ?
C1 Zr2 C50 128.1(2) . . ?
C1 Zr2 C50A 125.8(3) . . ?
C2 Zr2 C3 31.10(8) . . ?
C2 Zr2 C50 99.4(2) . . ?
C2 Zr2 C50A 99.4(3) . . ?
C3 Zr2 C50A 91.4(3) . . ?
C49 Zr2 C1 131.7(3) . . ?
C49 Zr2 C2 99.0(3) . . ?
C49 Zr2 C3 73.9(3) . . ?
C49 Zr2 C50 33.3(2) . . ?
C49 Zr2 C50A 40.1(4) . . ?
C49A Zr2 N2 108.4(3) . . ?
C49A Zr2 C1 128.3(4) . . ?
C49A Zr2 C2 95.2(4) . . ?
C49A Zr2 C3 73.0(4) . . ?
C49A Zr2 C49 8.3(4) . . ?
C49A Zr2 C50 26.3(4) . . ?
C49A Zr2 C50A 33.1(4) . . ?
C49A Zr2 C56 114.6(3) . . ?
C50 Zr2 C3 88.1(2) . . ?
C50 Zr2 C50A 6.8(4) . . ?
C56 Zr2 C1 78.21(10) . . ?
C56 Zr2 C2 91.99(10) . . ?
C56 Zr2 C3 120.72(10) . . ?
C56 Zr2 C49 121.6(2) . . ?
C56 Zr2 C50 88.35(18) . . ?
C56 Zr2 C50A 81.5(3) . . ?
C15 O1 Zr1 134.03(16) . . ?
C2S O1S C3S 124.4(16) . . ?
C48 O2 Zr2 129.22(17) . . ?
C5 N1 Zr1 114.29(16) . . ?
C5 N1 C9 119.0(2) . . ?
C9 N1 Zr1 124.43(16) . . ?
C38 N2 Zr2 118.51(17) . . ?
C38 N2 C42 118.8(2) . . ?
C42 N2 Zr2 122.51(17) . . ?
Zr2 C1 H1 111.1 . . ?
C2 C1 Zr2 74.44(14) . . ?
C2 C1 H1 111.1 . . ?
C2 C1 C5 127.6(2) . . ?
C5 C1 Zr2 116.16(16) . . ?
C5 C1 H1 111.1 . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
Zr1 C2 H2 105.4 . . ?
Zr2 C2 Zr1 131.08(11) . . ?
Zr2 C2 H2 122.4 . . ?
C1 C2 Zr1 97.51(16) . . ?
C1 C2 Zr2 72.49(14) . . ?
C1 C2 H2 115.2 . . ?
C3 C2 Zr1 69.12(14) . . ?
C3 C2 Zr2 81.04(15) . . ?
C3 C2 C1 129.6(2) . . ?
C3 C2 H2 115.2 . . ?
O1S C2S C1S 121.4(17) . . ?
O1S C2S H2SA 107.0 . . ?
O1S C2S H2SB 107.0 . . ?
C1S C2S H2SA 107.0 . . ?
C1S C2S H2SB 107.0 . . ?
H2SA C2S H2SB 106.7 . . ?
Zr1 C3 Zr2 129.38(10) . . ?
Zr1 C3 H3 126.0 . . ?
Zr2 C3 H3 103.3 . . ?
C2 C3 Zr1 79.49(15) . . ?
C2 C3 Zr2 67.86(14) . . ?
C2 C3 H3 116.0 . . ?
C2 C3 C4 128.1(2) . . ?
C4 C3 Zr1 70.63(14) . . ?
C4 C3 Zr2 100.14(16) . . ?
C4 C3 H3 116.0 . . ?
O1S C3S H3SA 109.8 . . ?
O1S C3S H3SB 109.8 . . ?
O1S C3S C4S 109.3(13) . . ?
H3SA C3S H3SB 108.3 . . ?
C4S C3S H3SA 109.8 . . ?
C4S C3S H3SB 109.8 . . ?
Zr1 C4 H4 112.6 . . ?
C3 C4 Zr1 76.16(15) . . ?
C3 C4 H4 112.6 . . ?
C3 C4 C38 125.1(2) . . ?
C38 C4 Zr1 112.11(17) . . ?
C38 C4 H4 112.6 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?
N1 C5 C1 119.8(2) . . ?
N1 C5 C6 121.1(2) . . ?
C6 C5 C1 119.0(2) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 C5 119.3(2) . . ?
C7 C6 H6 120.3 . . ?
C6 C7 H7 120.2 . . ?
C6 C7 C8 119.6(2) . . ?
C8 C7 H7 120.2 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.1(3) . . ?
C9 C8 H8 119.9 . . ?
N1 C9 C8 120.7(2) . . ?
N1 C9 C10 120.3(2) . . ?
C8 C9 C10 119.0(2) . . ?
C11 C10 C9 117.8(2) . . ?
C11 C10 C15 119.0(2) . . ?
C15 C10 C9 123.1(2) . . ?
C10 C11 H11 118.9 . . ?
C12 C11 C10 122.2(3) . . ?
C12 C11 H11 118.9 . . ?
C11 C12 C13 117.1(2) . . ?
C11 C12 C30 121.7(3) . . ?
C13 C12 C30 121.2(3) . . ?
C12 C13 H13 118.0 . . ?
C14 C13 C12 123.9(3) . . ?
C14 C13 H13 118.0 . . ?
C13 C14 C15 117.3(2) . . ?
C13 C14 C34 120.6(2) . . ?
C15 C14 C34 122.0(2) . . ?
O1 C15 C10 118.4(2) . . ?
O1 C15 C14 121.5(2) . . ?
C10 C15 C14 120.1(2) . . ?
Zr1 C16 H16A 107.7 . . ?
Zr1 C16 H16B 107.7 . . ?
H16A C16 H16B 107.1 . . ?
C17 C16 Zr1 118.47(18) . . ?
C17 C16 H16A 107.7 . . ?
C17 C16 H16B 107.7 . . ?
C18 C17 C16 121.2(3) . . ?
C18 C17 C22 116.9(3) . . ?
C22 C17 C16 121.9(3) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 C17 121.2(3) . . ?
C19 C18 H18 119.4 . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.7(3) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 H20 120.5 . . ?
C19 C20 C21 119.0(3) . . ?
C21 C20 H20 120.5 . . ?
C20 C21 H21 119.7 . . ?
C22 C21 C20 120.6(3) . . ?
C22 C21 H21 119.7 . . ?
C17 C22 H22 119.2 . . ?
C21 C22 C17 121.6(3) . . ?
C21 C22 H22 119.2 . . ?
Zr1 C23 H23A 111.3 . . ?
Zr1 C23 H23B 111.3 . . ?
H23A C23 H23B 109.2 . . ?
C24 C23 Zr1 102.30(18) . . ?
C24 C23 H23A 111.3 . . ?
C24 C23 H23B 111.3 . . ?
C25 C24 C23 122.1(3) . . ?
C25 C24 C29 116.0(3) . . ?
C29 C24 C23 121.7(3) . . ?
C24 C25 H25 118.7 . . ?
C26 C25 C24 122.5(3) . . ?
C26 C25 H25 118.7 . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.5(4) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 120.7 . . ?
C26 C27 C28 118.6(4) . . ?
C28 C27 H27 120.7 . . ?
C27 C28 H28 119.5 . . ?
C27 C28 C29 121.1(3) . . ?
C29 C28 H28 119.5 . . ?
C24 C29 H29 119.4 . . ?
C28 C29 C24 121.2(3) . . ?
C28 C29 H29 119.4 . . ?
C12 C30 C31 113.3(3) . . ?
C12 C30 C31A 106.0(4) . . ?
C12 C30 C32A 112.0(4) . . ?
C12 C30 C33 107.7(3) . . ?
C31 C30 C31A 52.2(5) . . ?
C31 C30 C33 104.7(5) . . ?
C32 C30 C12 111.3(4) . . ?
C32 C30 C31 110.5(6) . . ?
C32 C30 C31A 66.0(6) . . ?
C32 C30 C32A 38.3(5) . . ?
C32 C30 C33 109.1(6) . . ?
C32A C30 C31 132.9(5) . . ?
C32A C30 C31A 102.8(6) . . ?
C32A C30 C33 72.8(6) . . ?
C33 C30 C31A 145.0(5) . . ?
C33A C30 C12 110.2(4) . . ?
C33A C30 C31 59.7(7) . . ?
C33A C30 C31A 110.8(7) . . ?
C33A C30 C32 137.3(5) . . ?
C33A C30 C32A 114.4(7) . . ?
C33A C30 C33 47.6(6) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
C30 C31A H31D 109.5 . . ?
C30 C31A H31E 109.5 . . ?
C30 C31A H31F 109.5 . . ?
H31D C31A H31E 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
C30 C32A H32D 109.5 . . ?
C30 C32A H32E 109.5 . . ?
C30 C32A H32F 109.5 . . ?
H32D C32A H32E 109.5 . . ?
H32D C32A H32F 109.5 . . ?
H32E C32A H32F 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
C30 C33A H33D 109.5 . . ?
C30 C33A H33E 109.5 . . ?
C30 C33A H33F 109.5 . . ?
H33D C33A H33E 109.5 . . ?
H33D C33A H33F 109.5 . . ?
H33E C33A H33F 109.5 . . ?
C35 C34 C14 111.9(2) . . ?
C35 C34 C36 107.4(3) . . ?
C36 C34 C14 108.9(2) . . ?
C37 C34 C14 111.4(2) . . ?
C37 C34 C35 106.7(3) . . ?
C37 C34 C36 110.5(3) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N2 C38 C4 119.4(2) . . ?
N2 C38 C39 121.1(2) . . ?
C39 C38 C4 119.6(2) . . ?
C38 C39 H39 120.2 . . ?
C40 C39 C38 119.6(3) . . ?
C40 C39 H39 120.2 . . ?
C39 C40 H40 120.3 . . ?
C39 C40 C41 119.4(3) . . ?
C41 C40 H40 120.3 . . ?
C40 C41 H41 119.9 . . ?
C40 C41 C42 120.2(3) . . ?
C42 C41 H41 119.9 . . ?
N2 C42 C41 120.7(2) . . ?
N2 C42 C43 121.0(2) . . ?
C41 C42 C43 118.1(2) . . ?
C44 C43 C42 118.7(2) . . ?
C44 C43 C48 119.2(2) . . ?
C48 C43 C42 121.7(2) . . ?
C43 C44 H44 119.1 . . ?
C45 C44 C43 121.7(3) . . ?
C45 C44 H44 119.1 . . ?
C44 C45 C46 117.0(2) . . ?
C44 C45 C63 119.4(2) . . ?
C46 C45 C63 123.6(2) . . ?
C45 C46 H46 117.9 . . ?
C47 C46 C45 124.1(3) . . ?
C47 C46 H46 117.9 . . ?
C46 C47 C48 116.7(2) . . ?
C46 C47 C67 121.6(2) . . ?
C48 C47 C67 121.6(2) . . ?
O2 C48 C43 118.6(2) . . ?
O2 C48 C47 121.5(2) . . ?
C43 C48 C47 119.9(2) . . ?
Zr2 C49 H49A 114.4 . . ?
Zr2 C49 H49B 114.4 . . ?
H49A C49 H49B 111.5 . . ?
C50 C49 Zr2 85.7(8) . . ?
C50 C49 H49A 114.4 . . ?
C50 C49 H49B 114.4 . . ?
Zr2 C49A H49C 113.5 . . ?
Zr2 C49A H49D 113.5 . . ?
H49C C49A H49D 110.8 . . ?
C50A C49A Zr2 90.6(12) . . ?
C50A C49A H49C 113.5 . . ?
C50A C49A H49D 113.5 . . ?
C49 C50 Zr2 61.0(7) . . ?
C51 C50 Zr2 99.4(11) . . ?
C51 C50 C49 124.9(10) . . ?
C55 C50 Zr2 102.2(7) . . ?
C55 C50 C49 121.5(8) . . ?
C55 C50 C51 112.6(7) . . ?
C49A C50A Zr2 56.2(10) . . ?
C51A C50A Zr2 100.2(16) . . ?
C51A C50A C49A 113.1(14) . . ?
C55A C50A Zr2 107.6(13) . . ?
C55A C50A C49A 123.0(13) . . ?
C55A C50A C51A 123.9(12) . . ?
C50 C51 H51 117.7 . . ?
C52 C51 C50 124.5(9) . . ?
C52 C51 H51 117.7 . . ?
C50A C51A H51A 122.3 . . ?
C52A C51A C50A 115.4(14) . . ?
C52A C51A H51A 122.3 . . ?
C51 C52 H52 120.0 . . ?
C51 C52 C53 119.9(8) . . ?
C53 C52 H52 120.0 . . ?
C51A C52A H52A 120.5 . . ?
C51A C52A C53A 118.9(13) . . ?
C53A C52A H52A 120.5 . . ?
C52 C53 H53 121.1 . . ?
C54 C53 C52 117.8(7) . . ?
C54 C53 H53 121.1 . . ?
C52A C53A H53A 118.1 . . ?
C54A C53A C52A 123.8(13) . . ?
C54A C53A H53A 118.1 . . ?
C53 C54 H54 118.5 . . ?
C53 C54 C55 122.9(7) . . ?
C55 C54 H54 118.5 . . ?
C53A C54A H54A 120.5 . . ?
C55A C54A C53A 119.0(13) . . ?
C55A C54A H54A 120.5 . . ?
C50 C55 H55 118.9 . . ?
C54 C55 C50 122.2(7) . . ?
C54 C55 H55 118.9 . . ?
C50A C55A H55A 120.6 . . ?
C54A C55A C50A 118.9(13) . . ?
C54A C55A H55A 120.6 . . ?
Zr2 C56 H56A 107.6 . . ?
Zr2 C56 H56B 107.6 . . ?
H56A C56 H56B 107.0 . . ?
C57 C56 Zr2 118.85(19) . . ?
C57 C56 H56A 107.6 . . ?
C57 C56 H56B 107.6 . . ?
C58 C57 C56 121.3(3) . . ?
C58 C57 C62 116.4(3) . . ?
C62 C57 C56 122.3(3) . . ?
C57 C58 H58 119.1 . . ?
C59 C58 C57 121.8(3) . . ?
C59 C58 H58 119.1 . . ?
C58 C59 H59 119.5 . . ?
C58 C59 C60 120.9(3) . . ?
C60 C59 H59 119.5 . . ?
C59 C60 H60 120.8 . . ?
C61 C60 C59 118.3(3) . . ?
C61 C60 H60 120.8 . . ?
C60 C61 H61 119.4 . . ?
C60 C61 C62 121.3(3) . . ?
C62 C61 H61 119.4 . . ?
C57 C62 H62 119.3 . . ?
C61 C62 C57 121.3(3) . . ?
C61 C62 H62 119.3 . . ?
C45 C63 C64 109.3(2) . . ?
C45 C63 C65 112.1(3) . . ?
C64 C63 C65 107.8(3) . . ?
C66 C63 C45 109.8(2) . . ?
C66 C63 C64 109.0(3) . . ?
C66 C63 C65 108.7(3) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C68 C67 C47 111.6(3) . . ?
C69 C67 C47 109.0(3) . . ?
C69 C67 C68 107.9(3) . . ?
C69 C67 C70 110.1(3) . . ?
C70 C67 C47 111.4(3) . . ?
C70 C67 C68 106.8(3) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C67 C69 H69A 109.5 . . ?
C67 C69 H69B 109.5 . . ?
C67 C69 H69C 109.5 . . ?
H69A C69 H69B 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
C67 C70 H70A 109.5 . . ?
C67 C70 H70B 109.5 . . ?
C67 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'diethyl ether/n-pentane'
_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_Hf2-Me_042313a_ben
_database_code_depnum_ccdc_archive 'CCDC 1486143'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-08-03 downloaded from the CCDC.
;
_audit_creation_date             
;
'Wed Apr 24 10:13:49 2013'
;
_audit_creation_method           
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_chemical_name_common            ?
_chemical_name_systematic        Hf2-Me
_chemical_formula_moiety         'C72 H82 Hf2 N2 O2, 0.5(C3 H7)'
_chemical_formula_sum            'C73.50 H85.50 Hf2 N2 O2'
_chemical_formula_weight         1385.92
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -6.1794 4.9776 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   14.6909(3)
_cell_length_b                   16.2174(3)
_cell_length_c                   27.5623(6)
_cell_angle_alpha                90.0
_cell_angle_beta                 103.614(2)
_cell_angle_gamma                90.0
_cell_volume                     6382.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    16358
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      71.6114
_cell_measurement_theta_min      3.1434
_cell_oxdiff_angle_alpha         90.071(2)
_cell_oxdiff_angle_beta          103.691(2)
_cell_oxdiff_angle_gamma         89.931(2)
_cell_oxdiff_length_a            14.6808(4)
_cell_oxdiff_length_b            16.2232(5)
_cell_oxdiff_length_c            27.5805(7)
_cell_oxdiff_measurement_reflns_used 16358
_cell_oxdiff_volume              6382.2(3)
_exptl_absorpt_coefficient_mu    6.244
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            indigo
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2802
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.23
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27507
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.19
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -9.00   21.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  120.0000 30

#__ type_ start__ end____ width___ exp.time_
  2 omega   32.00   63.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  120.0000 31

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   34.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  -90.0000 59

#__ type_ start__ end____ width___ exp.time_
  4 omega -112.00  -39.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  125.0000 -180.0000 73

#__ type_ start__ end____ width___ exp.time_
  5 omega -124.00  -38.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -57.0000    0.0000 86

#__ type_ start__ end____ width___ exp.time_
  6 omega  -63.00    0.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000 -180.0000 63

#__ type_ start__ end____ width___ exp.time_
  7 omega  -64.00   -7.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   37.0000  -30.0000 57

#__ type_ start__ end____ width___ exp.time_
  8 omega   37.00   66.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  120.0000 29

#__ type_ start__ end____ width___ exp.time_
  9 omega   38.00   64.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   60.0000 26

#__ type_ start__ end____ width___ exp.time_
 10 omega   45.00   71.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  -90.0000 26

#__ type_ start__ end____ width___ exp.time_
 11 omega   44.00   90.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  -60.0000 46

#__ type_ start__ end____ width___ exp.time_
 12 omega   42.00   68.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -37.0000  150.0000 26

#__ type_ start__ end____ width___ exp.time_
 13 omega   40.00   72.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000    0.0000 32

#__ type_ start__ end____ width___ exp.time_
 14 omega   47.00   87.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  120.0000 40

#__ type_ start__ end____ width___ exp.time_
 15 omega   40.00   77.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000   30.0000 37

#__ type_ start__ end____ width___ exp.time_
 16 omega   48.00   83.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000 -180.0000 35

#__ type_ start__ end____ width___ exp.time_
 17 omega   56.00   88.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000   60.0000 32

#__ type_ start__ end____ width___ exp.time_
 18 omega   40.00   66.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   90.0000 26

#__ type_ start__ end____ width___ exp.time_
 19 omega   40.00   70.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000   30.0000 30

#__ type_ start__ end____ width___ exp.time_
 20 omega   55.00   80.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   60.0000 25

#__ type_ start__ end____ width___ exp.time_
 21 omega   95.00  152.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000  150.0000 57

#__ type_ start__ end____ width___ exp.time_
 22 omega   52.00   77.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 23 omega   43.00   90.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000   90.0000 47

#__ type_ start__ end____ width___ exp.time_
 24 omega   38.00   90.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000  -30.0000 52
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0878041000
_diffrn_orient_matrix_UB_12      0.0454302000
_diffrn_orient_matrix_UB_13      0.0295781000
_diffrn_orient_matrix_UB_21      -0.0610807000
_diffrn_orient_matrix_UB_22      0.0746077000
_diffrn_orient_matrix_UB_23      0.0064604000
_diffrn_orient_matrix_UB_31      -0.0149951000
_diffrn_orient_matrix_UB_32      -0.0372466000
_diffrn_orient_matrix_UB_33      0.0488728000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                11139
_reflns_number_total             11381
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_refine_diff_density_max         1.299
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         11381
_refine_ls_number_restraints     109
_refine_ls_R_factor_all          0.0272
_refine_ls_R_factor_gt           0.0264
_refine_ls_restrained_S_all      1.182
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0319P)²+10.6768P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0694
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Hf1 Hf 0.097372(9) 0.633882(8) 0.160630(5) 0.01236(5) Uani 1 1 d B . . .
Hf2 Hf 0.414031(9) 0.739232(9) 0.187132(5) 0.01363(5) Uani 1 1 d . . . .
O1 O -0.00471(14) 0.70289(12) 0.12278(7) 0.0150(4) Uani 1 1 d . . . .
O2 O 0.48497(15) 0.73645(13) 0.25680(8) 0.0174(4) Uani 1 1 d . . . .
N1 N 0.12122(17) 0.74943(15) 0.20356(9) 0.0133(5) Uani 1 1 d . . . .
N2 N 0.32354(17) 0.81187(15) 0.22343(9) 0.0141(5) Uani 1 1 d . . . .
C1 C 0.2405(2) 0.65569(19) 0.23786(12) 0.0171(6) Uani 1 1 d . . . .
C2 C 0.2662(2) 0.64444(19) 0.19120(12) 0.0181(6) Uani 1 1 d . . . .
H2 H 0.2952 0.5928 0.1885 0.022 Uiso 1 1 calc . . R .
C3 C 0.2569(2) 0.6959(2) 0.14768(11) 0.0191(6) Uani 1 1 d . . . .
H3 H 0.2557 0.6658 0.1180 0.023 Uiso 1 1 calc . . R .
C4 C 0.2490(2) 0.7841(2) 0.14007(11) 0.0187(6) Uani 1 1 d . . . .
C5 C 0.2829(2) 0.6003(2) 0.28118(13) 0.0240(7) Uani 1 1 d . . . .
H5A H 0.2337 0.5805 0.2968 0.036 Uiso 1 1 calc . . GR .
H5B H 0.3296 0.6313 0.3057 0.036 Uiso 1 1 calc . . GR .
H5C H 0.3131 0.5532 0.2692 0.036 Uiso 1 1 calc . . GR .
C6 C 0.2134(3) 0.8156(2) 0.08744(12) 0.0285(8) Uani 1 1 d . . . .
H6A H 0.2471 0.8661 0.0829 0.043 Uiso 1 1 calc . . GR .
H6B H 0.1463 0.8276 0.0815 0.043 Uiso 1 1 calc . . GR .
H6C H 0.2236 0.7736 0.0637 0.043 Uiso 1 1 calc . . GR .
C7 C 0.1806(2) 0.72188(18) 0.24599(11) 0.0142(6) Uani 1 1 d . . . .
C8 C 0.1762(2) 0.7561(2) 0.29257(11) 0.0177(6) Uani 1 1 d . . . .
H8 H 0.2123 0.7341 0.3230 0.021 Uiso 1 1 calc . . R .
C9 C 0.1180(2) 0.8223(2) 0.29243(11) 0.0198(6) Uani 1 1 d . . . .
H9 H 0.1161 0.8479 0.3232 0.024 Uiso 1 1 calc . . R .
C10 C 0.0615(2) 0.8526(2) 0.24820(11) 0.0175(6) Uani 1 1 d . . . .
H10 H 0.0224 0.8992 0.2487 0.021 Uiso 1 1 calc . . R .
C11 C 0.0629(2) 0.81419(18) 0.20362(11) 0.0135(6) Uani 1 1 d . . . .
C12 C 0.0064(2) 0.84078(19) 0.15456(11) 0.0137(6) Uani 1 1 d . . . .
C13 C -0.0092(2) 0.92470(19) 0.14584(11) 0.0157(6) Uani 1 1 d . . . .
H13 H 0.0127 0.9625 0.1724 0.019 Uiso 1 1 calc . . R .
C14 C -0.0561(2) 0.95486(19) 0.09944(12) 0.0182(6) Uani 1 1 d . . . .
C15 C -0.0941(2) 0.8965(2) 0.06316(11) 0.0181(6) Uani 1 1 d . . . .
H15 H -0.1295 0.9156 0.0318 0.022 Uiso 1 1 calc . . R .
C16 C -0.0832(2) 0.81113(19) 0.07025(11) 0.0159(6) Uani 1 1 d . . . .
C17 C -0.0272(2) 0.78373(18) 0.11563(11) 0.0138(6) Uani 1 1 d . . . .
C18 C 0.1186(2) 0.5504(2) 0.09829(13) 0.0232(7) Uani 1 1 d . . . .
H18A H 0.1081 0.5823 0.0668 0.028 Uiso 1 1 calc . . R .
H18B H 0.1841 0.5302 0.1062 0.028 Uiso 1 1 calc . . R .
C19 C 0.0534(2) 0.4785(2) 0.09120(11) 0.0197(6) Uani 1 1 d . . . .
C20 C 0.0780(3) 0.4055(2) 0.11846(12) 0.0262(7) Uani 1 1 d . . . .
H20 H 0.1383 0.4014 0.1404 0.031 Uiso 1 1 calc . . R .
C21 C 0.0171(3) 0.3394(2) 0.11427(14) 0.0314(8) Uani 1 1 d . . . .
H21 H 0.0360 0.2909 0.1333 0.038 Uiso 1 1 calc . . R .
C22 C -0.0708(3) 0.3435(2) 0.08266(15) 0.0346(9) Uani 1 1 d . . . .
H22 H -0.1130 0.2985 0.0801 0.042 Uiso 1 1 calc . . R .
C23 C -0.0968(3) 0.4146(2) 0.05466(14) 0.0319(8) Uani 1 1 d . . . .
H23 H -0.1570 0.4179 0.0325 0.038 Uiso 1 1 calc . . R .
C24 C -0.0352(2) 0.4811(2) 0.05888(13) 0.0253(7) Uani 1 1 d . . . .
H24 H -0.0540 0.5291 0.0393 0.030 Uiso 1 1 calc . . R .
C25 C 0.0408(2) 0.5494(2) 0.21056(12) 0.0225(7) Uani 1 1 d . . . .
H25A H 0.0404 0.4917 0.1988 0.027 Uiso 1 1 calc A . R .
H25B H 0.0793 0.5525 0.2452 0.027 Uiso 1 1 calc A . R .
C26A C -0.0560(2) 0.5784(2) 0.20814(12) 0.0236(6) Uani 0.35 1 d B 2 . U
C27A C -0.0835(11) 0.6408(14) 0.2361(8) 0.034(3) Uani 0.35 1 d B 2 . U
H27A H -0.0387 0.6655 0.2626 0.041 Uiso 0.35 1 calc B 2 R .
C28A C -0.1750(11) 0.6670(10) 0.2256(6) 0.037(3) Uani 0.35 1 d B 2 . U
H28A H -0.1943 0.7097 0.2446 0.045 Uiso 0.35 1 calc B 2 R .
C29A C -0.2379(9) 0.6298(10) 0.1869(6) 0.035(3) Uani 0.35 1 d B 2 . U
H29A H -0.3013 0.6476 0.1794 0.042 Uiso 0.35 1 calc B 2 R .
C30A C -0.2127(9) 0.5682(10) 0.1588(6) 0.036(3) Uani 0.35 1 d B 2 . U
H30A H -0.2585 0.5450 0.1321 0.043 Uiso 0.35 1 calc B 2 R .
C31A C -0.1213(9) 0.5390(10) 0.1686(6) 0.028(3) Uani 0.35 1 d B 2 . U
H31A H -0.1035 0.4951 0.1499 0.034 Uiso 0.35 1 calc B 2 R .
C26 C -0.0560(2) 0.5784(2) 0.20814(12) 0.0236(6) Uani 0.65 1 d B 1 . U
C27 C -0.0666(5) 0.6399(6) 0.2438(4) 0.0229(16) Uani 0.65 1 d B 1 . U
H27 H -0.0136 0.6558 0.2690 0.027 Uiso 0.65 1 calc B 1 R .
C28 C -0.1529(5) 0.6768(4) 0.2423(3) 0.0274(14) Uani 0.65 1 d B 1 . U
H28 H -0.1588 0.7169 0.2665 0.033 Uiso 0.65 1 calc B 1 R .
C29 C -0.2309(4) 0.6542(4) 0.2048(3) 0.0260(13) Uani 0.65 1 d B 1 . U
H29 H -0.2894 0.6801 0.2034 0.031 Uiso 0.65 1 calc B 1 R .
C30 C -0.2244(5) 0.5954(5) 0.1699(3) 0.0267(13) Uani 0.65 1 d B 1 . U
H30 H -0.2777 0.5802 0.1447 0.032 Uiso 0.65 1 calc B 1 R .
C31 C -0.1377(5) 0.5588(5) 0.1726(3) 0.0264(16) Uani 0.65 1 d B 1 . U
H31 H -0.1338 0.5178 0.1486 0.032 Uiso 0.65 1 calc B 1 R .
C32 C -0.0614(2) 1.0481(2) 0.08964(12) 0.0235(7) Uani 1 1 d . . . .
C33 C -0.1102(3) 1.0694(2) 0.03578(14) 0.0392(10) Uani 1 1 d . . . .
H33A H -0.0761 1.0441 0.0130 0.059 Uiso 1 1 calc . . GR .
H33B H -0.1113 1.1294 0.0314 0.059 Uiso 1 1 calc . . GR .
H33C H -0.1745 1.0483 0.0283 0.059 Uiso 1 1 calc . . GR .
C34 C -0.1141(3) 1.0893(2) 0.12500(15) 0.0367(9) Uani 1 1 d . . . .
H34A H -0.1773 1.0661 0.1194 0.055 Uiso 1 1 calc . . GR .
H34B H -0.1181 1.1488 0.1186 0.055 Uiso 1 1 calc . . GR .
H34C H -0.0804 1.0793 0.1596 0.055 Uiso 1 1 calc . . GR .
C35 C 0.0387(3) 1.0834(2) 0.09996(17) 0.0392(9) Uani 1 1 d . . . .
H35A H 0.0693 1.0762 0.1353 0.059 Uiso 1 1 calc . . GR .
H35B H 0.0360 1.1422 0.0916 0.059 Uiso 1 1 calc . . GR .
H35C H 0.0746 1.0542 0.0795 0.059 Uiso 1 1 calc . . GR .
C36 C -0.1290(3) 0.7507(2) 0.02875(12) 0.0222(7) Uani 1 1 d . . . .
C37 C -0.1963(3) 0.7944(2) -0.01452(13) 0.0336(9) Uani 1 1 d . . . .
H37A H -0.2427 0.8256 -0.0016 0.050 Uiso 1 1 calc . . GR .
H37B H -0.2283 0.7533 -0.0387 0.050 Uiso 1 1 calc . . GR .
H37C H -0.1610 0.8322 -0.0309 0.050 Uiso 1 1 calc . . GR .
C38 C -0.1868(2) 0.6858(2) 0.04914(13) 0.0277(7) Uani 1 1 d . . . .
H38A H -0.1463 0.6570 0.0774 0.042 Uiso 1 1 calc . . GR .
H38B H -0.2129 0.6460 0.0228 0.042 Uiso 1 1 calc . . GR .
H38C H -0.2379 0.7132 0.0602 0.042 Uiso 1 1 calc . . GR .
C39 C -0.0522(3) 0.7093(2) 0.00787(12) 0.0293(8) Uani 1 1 d . . . .
H39A H -0.0186 0.7514 -0.0066 0.044 Uiso 1 1 calc . . GR .
H39B H -0.0808 0.6695 -0.0180 0.044 Uiso 1 1 calc . . GR .
H39C H -0.0082 0.6808 0.0349 0.044 Uiso 1 1 calc . . GR .
C40 C 0.2647(2) 0.84166(19) 0.18090(11) 0.0158(6) Uani 1 1 d . . . .
C41 C 0.2303(2) 0.92292(19) 0.18058(12) 0.0190(6) Uani 1 1 d . . . .
H41 H 0.1929 0.9463 0.1509 0.023 Uiso 1 1 calc . . R .
C42 C 0.2524(2) 0.96720(19) 0.22417(13) 0.0213(7) Uani 1 1 d . . . .
H42 H 0.2272 1.0210 0.2250 0.026 Uiso 1 1 calc . . R .
C43 C 0.3114(2) 0.9347(2) 0.26757(12) 0.0201(6) Uani 1 1 d . . . .
H43 H 0.3265 0.9661 0.2975 0.024 Uiso 1 1 calc . . R .
C44 C 0.3472(2) 0.85619(19) 0.26601(11) 0.0158(6) Uani 1 1 d . . . .
C45 C 0.4082(2) 0.81445(19) 0.30910(11) 0.0164(6) Uani 1 1 d . . . .
C46 C 0.3989(2) 0.8341(2) 0.35713(12) 0.0189(6) Uani 1 1 d . . . .
H46 H 0.3557 0.8758 0.3610 0.023 Uiso 1 1 calc . . R .
C47 C 0.4507(2) 0.7946(2) 0.39897(12) 0.0209(7) Uani 1 1 d . . . .
C48 C 0.5114(2) 0.7324(2) 0.39179(12) 0.0204(6) Uani 1 1 d . . . .
H48 H 0.5463 0.7040 0.4203 0.024 Uiso 1 1 calc . . R .
C49 C 0.5239(2) 0.70948(19) 0.34493(12) 0.0187(6) Uani 1 1 d . . . .
C50 C 0.4722(2) 0.75306(19) 0.30290(11) 0.0154(6) Uani 1 1 d . . . .
C51 C 0.4724(2) 0.8400(2) 0.14859(12) 0.0226(7) Uani 1 1 d . . . .
H51A H 0.4558 0.8293 0.1122 0.027 Uiso 1 1 calc . . R .
H51B H 0.4427 0.8927 0.1544 0.027 Uiso 1 1 calc . . R .
C52 C 0.5767(2) 0.8492(2) 0.16544(13) 0.0229(7) Uani 1 1 d . . . .
C53 C 0.6365(3) 0.8331(2) 0.13394(16) 0.0351(9) Uani 1 1 d . . . .
H53 H 0.6109 0.8139 0.1010 0.042 Uiso 1 1 calc . . R .
C54 C 0.7324(3) 0.8445(3) 0.14978(19) 0.0462(11) Uani 1 1 d . . . .
H54 H 0.7714 0.8348 0.1273 0.055 Uiso 1 1 calc . . R .
C55 C 0.7718(3) 0.8699(3) 0.1981(2) 0.0443(11) Uani 1 1 d . . . .
H55 H 0.8375 0.8781 0.2088 0.053 Uiso 1 1 calc . . R .
C56 C 0.7144(3) 0.8833(2) 0.23040(17) 0.0375(9) Uani 1 1 d . . . .
H56 H 0.7407 0.8992 0.2639 0.045 Uiso 1 1 calc . . R .
C57 C 0.6185(3) 0.8735(2) 0.21398(14) 0.0285(8) Uani 1 1 d . . . .
H57 H 0.5800 0.8837 0.2366 0.034 Uiso 1 1 calc . . R .
C58 C 0.4796(2) 0.6282(2) 0.15845(13) 0.0240(7) Uani 1 1 d . . . .
H58A H 0.5120 0.6496 0.1333 0.029 Uiso 1 1 calc . . R .
H58B H 0.5293 0.6082 0.1868 0.029 Uiso 1 1 calc . . R .
C59 C 0.4274(2) 0.5539(2) 0.13590(12) 0.0197(6) Uani 1 1 d . . . .
C60 C 0.3791(3) 0.5525(2) 0.08557(13) 0.0277(7) Uani 1 1 d . . . .
H60 H 0.3813 0.5995 0.0653 0.033 Uiso 1 1 calc . . R .
C61 C 0.3284(3) 0.4842(3) 0.06487(14) 0.0359(9) Uani 1 1 d . . . .
H61 H 0.2966 0.4847 0.0306 0.043 Uiso 1 1 calc . . R .
C62 C 0.3236(3) 0.4155(2) 0.09352(16) 0.0360(9) Uani 1 1 d . . . .
H62 H 0.2890 0.3684 0.0791 0.043 Uiso 1 1 calc . . R .
C63 C 0.3696(3) 0.4157(2) 0.14359(16) 0.0320(8) Uani 1 1 d . . . .
H63 H 0.3657 0.3690 0.1638 0.038 Uiso 1 1 calc . . R .
C64 C 0.4214(2) 0.4839(2) 0.16409(13) 0.0252(7) Uani 1 1 d . . . .
H64 H 0.4536 0.4828 0.1983 0.030 Uiso 1 1 calc . . R .
C65 C 0.4379(3) 0.8187(2) 0.45112(12) 0.0271(7) Uani 1 1 d . . . .
C66 C 0.3475(4) 0.7805(4) 0.45806(19) 0.0601(15) Uani 1 1 d . . . .
H66A H 0.2949 0.8006 0.4319 0.090 Uiso 1 1 calc . . GR .
H66B H 0.3378 0.7960 0.4908 0.090 Uiso 1 1 calc . . GR .
H66C H 0.3514 0.7204 0.4559 0.090 Uiso 1 1 calc . . GR .
C67 C 0.4309(4) 0.9121(3) 0.45489(16) 0.0523(13) Uani 1 1 d . . . .
H67A H 0.4849 0.9378 0.4457 0.078 Uiso 1 1 calc . . GR .
H67B H 0.4303 0.9274 0.4892 0.078 Uiso 1 1 calc . . GR .
H67C H 0.3731 0.9313 0.4322 0.078 Uiso 1 1 calc . . GR .
C68 C 0.5203(4) 0.7911(4) 0.49219(16) 0.0712(19) Uani 1 1 d . . . .
H68A H 0.5228 0.7307 0.4932 0.107 Uiso 1 1 calc . . GR .
H68B H 0.5128 0.8120 0.5244 0.107 Uiso 1 1 calc . . GR .
H68C H 0.5785 0.8127 0.4856 0.107 Uiso 1 1 calc . . GR .
C69 C 0.5922(2) 0.6403(2) 0.33904(12) 0.0216(7) Uani 1 1 d . . . .
C70 C 0.5408(2) 0.5728(2) 0.30390(13) 0.0233(7) Uani 1 1 d . . . .
H70A H 0.4931 0.5473 0.3186 0.035 Uiso 1 1 calc . . GR .
H70B H 0.5858 0.5308 0.2991 0.035 Uiso 1 1 calc . . GR .
H70C H 0.5107 0.5973 0.2716 0.035 Uiso 1 1 calc . . GR .
C71 C 0.6728(2) 0.6778(2) 0.31878(16) 0.0318(8) Uani 1 1 d . . . .
H71A H 0.6470 0.7030 0.2861 0.048 Uiso 1 1 calc . . GR .
H71B H 0.7170 0.6342 0.3153 0.048 Uiso 1 1 calc . . GR .
H71C H 0.7053 0.7198 0.3421 0.048 Uiso 1 1 calc . . GR .
C72 C 0.6360(3) 0.5974(3) 0.38882(14) 0.0359(9) Uani 1 1 d . . . .
H72A H 0.6688 0.6383 0.4129 0.054 Uiso 1 1 calc . . GR .
H72B H 0.6804 0.5553 0.3834 0.054 Uiso 1 1 calc . . GR .
H72C H 0.5865 0.5713 0.4019 0.054 Uiso 1 1 calc . . GR .
C73 C 0.5293(8) 0.5290(7) 0.5112(5) 0.066(3) Uiso 0.50 1 d . . . .
H73B H 0.5021 0.5554 0.5370 0.079 Uiso 0.50 1 calc . . R .
H73A H 0.5337 0.5717 0.4863 0.079 Uiso 0.50 1 calc . . R .
C74 C 0.6233(10) 0.5018(9) 0.5348(5) 0.080(4) Uiso 0.50 1 d . . D .
H74A H 0.6664 0.5495 0.5424 0.096 Uiso 0.50 1 calc . . R .
H74B H 0.6470 0.4634 0.5127 0.096 Uiso 0.50 1 calc . . R .
C75 C 0.6157(9) 0.4604(8) 0.5805(4) 0.074(3) Uiso 0.50 1 d . . D .
H75A H 0.5885 0.4055 0.5725 0.111 Uiso 0.50 1 calc . . GR .
H75B H 0.5754 0.4928 0.5970 0.111 Uiso 0.50 1 calc . . GR .
H75C H 0.6781 0.4551 0.6028 0.111 Uiso 0.50 1 calc . . GR .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hf1 O1 1.963(2) . ?
Hf1 N1 2.200(2) . ?
Hf1 C1 2.640(3) . ?
Hf1 C2 2.431(3) . ?
Hf1 C3 2.651(3) . ?
Hf1 C7 2.777(3) . ?
Hf1 C18 2.266(3) . ?
Hf1 C25 2.236(3) . ?
Hf2 O2 1.958(2) . ?
Hf2 N2 2.187(2) . ?
Hf2 C2 2.684(3) . ?
Hf2 C3 2.413(3) . ?
Hf2 C4 2.571(3) . ?
Hf2 C40 2.724(3) . ?
Hf2 C51 2.228(3) . ?
Hf2 C58 2.271(3) . ?
O1 C17 1.355(4) . ?
O2 C50 1.354(4) . ?
N1 C7 1.359(4) . ?
N1 C11 1.355(4) . ?
N2 C40 1.370(4) . ?
N2 C44 1.350(4) . ?
C1 C2 1.435(4) . ?
C1 C5 1.507(4) . ?
C1 C7 1.439(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.442(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.446(5) . ?
C4 C6 1.510(4) . ?
C4 C40 1.438(4) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.415(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.371(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.393(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.382(4) . ?
C11 C12 1.475(4) . ?
C12 C13 1.392(4) . ?
C12 C17 1.415(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.391(4) . ?
C14 C15 1.395(5) . ?
C14 C32 1.535(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.401(4) . ?
C16 C17 1.398(4) . ?
C16 C36 1.536(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.493(4) . ?
C19 C20 1.403(5) . ?
C19 C24 1.394(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.384(5) . ?
C21 H21 0.9500 . ?
C21 C22 1.380(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.389(6) . ?
C23 H23 0.9500 . ?
C23 C24 1.396(5) . ?
C24 H24 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26A 1.484(5) . ?
C26A C27A 1.388(13) . ?
C26A C31A 1.424(12) . ?
C27A H27A 0.9500 . ?
C27A C28A 1.374(14) . ?
C28A H28A 0.9500 . ?
C28A C29A 1.377(16) . ?
C29A H29A 0.9500 . ?
C29A C30A 1.367(16) . ?
C30A H30A 0.9500 . ?
C30A C31A 1.389(14) . ?
C31A H31A 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.394(8) . ?
C28 H28 0.9500 . ?
C28 C29 1.399(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.371(10) . ?
C30 H30 0.9500 . ?
C30 C31 1.392(10) . ?
C31 H31 0.9500 . ?
C32 C33 1.528(5) . ?
C32 C34 1.533(5) . ?
C32 C35 1.542(5) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.532(5) . ?
C36 C38 1.539(5) . ?
C36 C39 1.536(5) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.411(4) . ?
C41 H41 0.9500 . ?
C41 C42 1.371(5) . ?
C42 H42 0.9500 . ?
C42 C43 1.405(5) . ?
C43 H43 0.9500 . ?
C43 C44 1.382(4) . ?
C44 C45 1.473(4) . ?
C45 C46 1.399(4) . ?
C45 C50 1.407(4) . ?
C46 H46 0.9500 . ?
C46 C47 1.381(5) . ?
C47 C48 1.391(5) . ?
C47 C65 1.543(4) . ?
C48 H48 0.9500 . ?
C48 C49 1.397(4) . ?
C49 C50 1.415(4) . ?
C49 C69 1.540(4) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 C52 1.500(5) . ?
C52 C53 1.397(5) . ?
C52 C57 1.391(5) . ?
C53 H53 0.9500 . ?
C53 C54 1.386(6) . ?
C54 H54 0.9500 . ?
C54 C55 1.383(7) . ?
C55 H55 0.9500 . ?
C55 C56 1.381(6) . ?
C56 H56 0.9500 . ?
C56 C57 1.384(5) . ?
C57 H57 0.9500 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.484(4) . ?
C59 C60 1.402(5) . ?
C59 C64 1.390(5) . ?
C60 H60 0.9500 . ?
C60 C61 1.381(5) . ?
C61 H61 0.9500 . ?
C61 C62 1.378(6) . ?
C62 H62 0.9500 . ?
C62 C63 1.387(6) . ?
C63 H63 0.9500 . ?
C63 C64 1.385(5) . ?
C64 H64 0.9500 . ?
C65 C66 1.517(5) . ?
C65 C67 1.524(6) . ?
C65 C68 1.517(6) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 C70 1.537(4) . ?
C69 C71 1.546(5) . ?
C69 C72 1.538(5) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 C73 1.33(2) 3_666 ?
C73 H73B 0.9900 . ?
C73 H73A 0.9900 . ?
C73 C74 1.449(17) . ?
C74 H74A 0.9900 . ?
C74 H74B 0.9900 . ?
C74 C75 1.455(9) . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Hf1 N1 78.77(9) . . ?
O1 Hf1 C1 135.72(9) . . ?
O1 Hf1 C2 137.20(10) . . ?
O1 Hf1 C3 107.52(9) . . ?
O1 Hf1 C7 106.62(9) . . ?
O1 Hf1 C18 99.32(11) . . ?
O1 Hf1 C25 109.15(11) . . ?
N1 Hf1 C1 57.07(9) . . ?
N1 Hf1 C2 74.53(10) . . ?
N1 Hf1 C3 73.45(9) . . ?
N1 Hf1 C7 28.83(9) . . ?
N1 Hf1 C18 152.10(10) . . ?
N1 Hf1 C25 103.06(11) . . ?
C1 Hf1 C3 59.75(9) . . ?
C1 Hf1 C7 30.67(9) . . ?
C2 Hf1 C1 32.55(10) . . ?
C2 Hf1 C3 32.60(10) . . ?
C2 Hf1 C7 57.34(9) . . ?
C3 Hf1 C7 72.08(9) . . ?
C18 Hf1 C1 117.75(11) . . ?
C18 Hf1 C2 89.62(11) . . ?
C18 Hf1 C3 80.82(11) . . ?
C18 Hf1 C7 146.89(11) . . ?
C25 Hf1 C1 85.79(11) . . ?
C25 Hf1 C2 109.07(12) . . ?
C25 Hf1 C3 141.63(11) . . ?
C25 Hf1 C7 86.94(10) . . ?
C25 Hf1 C18 103.79(12) . . ?
O2 Hf2 N2 78.71(9) . . ?
O2 Hf2 C2 101.23(9) . . ?
O2 Hf2 C3 131.85(10) . . ?
O2 Hf2 C4 136.24(9) . . ?
O2 Hf2 C40 108.10(9) . . ?
O2 Hf2 C51 107.98(11) . . ?
O2 Hf2 C58 98.72(11) . . ?
N2 Hf2 C2 72.82(9) . . ?
N2 Hf2 C3 75.10(10) . . ?
N2 Hf2 C4 58.37(10) . . ?
N2 Hf2 C40 29.92(9) . . ?
N2 Hf2 C51 99.59(11) . . ?
N2 Hf2 C58 160.07(11) . . ?
C2 Hf2 C40 72.83(9) . . ?
C3 Hf2 C2 32.30(10) . . ?
C3 Hf2 C4 33.55(11) . . ?
C3 Hf2 C40 58.56(10) . . ?
C4 Hf2 C2 60.48(10) . . ?
C4 Hf2 C40 31.34(10) . . ?
C51 Hf2 C2 147.78(11) . . ?
C51 Hf2 C3 115.68(12) . . ?
C51 Hf2 C4 88.56(11) . . ?
C51 Hf2 C40 85.24(11) . . ?
C51 Hf2 C58 99.99(12) . . ?
C58 Hf2 C2 88.51(11) . . ?
C58 Hf2 C3 92.96(12) . . ?
C58 Hf2 C4 118.43(12) . . ?
C58 Hf2 C40 149.66(11) . . ?
C17 O1 Hf1 139.34(19) . . ?
C50 O2 Hf2 139.16(19) . . ?
C7 N1 Hf1 99.87(18) . . ?
C11 N1 Hf1 129.8(2) . . ?
C11 N1 C7 122.1(2) . . ?
C40 N2 Hf2 97.31(18) . . ?
C44 N2 Hf2 128.6(2) . . ?
C44 N2 C40 122.5(3) . . ?
C2 C1 Hf1 65.70(16) . . ?
C2 C1 C5 119.1(3) . . ?
C2 C1 C7 122.3(3) . . ?
C5 C1 Hf1 131.4(2) . . ?
C7 C1 Hf1 79.94(17) . . ?
C7 C1 C5 118.4(3) . . ?
Hf1 C2 Hf2 142.69(14) . . ?
Hf1 C2 H2 110.5 . . ?
Hf2 C2 H2 96.9 . . ?
C1 C2 Hf1 81.75(17) . . ?
C1 C2 Hf2 110.6(2) . . ?
C1 C2 H2 113.6 . . ?
C1 C2 C3 132.7(3) . . ?
C3 C2 Hf1 82.11(18) . . ?
C3 C2 Hf2 63.44(16) . . ?
C3 C2 H2 113.6 . . ?
Hf1 C3 H3 94.8 . . ?
Hf2 C3 Hf1 146.31(13) . . ?
Hf2 C3 H3 111.1 . . ?
C2 C3 Hf1 65.29(16) . . ?
C2 C3 Hf2 84.25(18) . . ?
C2 C3 H3 113.5 . . ?
C2 C3 C4 133.0(3) . . ?
C4 C3 Hf1 110.6(2) . . ?
C4 C3 Hf2 79.24(18) . . ?
C4 C3 H3 113.5 . . ?
C3 C4 Hf2 67.21(17) . . ?
C3 C4 C6 118.1(3) . . ?
C6 C4 Hf2 130.7(2) . . ?
C40 C4 Hf2 80.21(18) . . ?
C40 C4 C3 122.4(3) . . ?
C40 C4 C6 119.2(3) . . ?
C1 C5 H5A 109.5 . . ?
C1 C5 H5B 109.5 . . ?
C1 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C7 Hf1 51.30(14) . . ?
N1 C7 C1 113.8(3) . . ?
N1 C7 C8 119.7(3) . . ?
C1 C7 Hf1 69.39(16) . . ?
C8 C7 Hf1 150.0(2) . . ?
C8 C7 C1 126.5(3) . . ?
C7 C8 H8 121.1 . . ?
C9 C8 C7 117.8(3) . . ?
C9 C8 H8 121.1 . . ?
C8 C9 H9 119.3 . . ?
C8 C9 C10 121.4(3) . . ?
C10 C9 H9 119.3 . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.2(3) . . ?
C11 C10 H10 120.4 . . ?
N1 C11 C10 119.5(3) . . ?
N1 C11 C12 116.4(3) . . ?
C10 C11 C12 124.1(3) . . ?
C13 C12 C11 118.6(3) . . ?
C13 C12 C17 119.6(3) . . ?
C17 C12 C11 121.7(3) . . ?
C12 C13 H13 119.0 . . ?
C14 C13 C12 121.9(3) . . ?
C14 C13 H13 119.0 . . ?
C13 C14 C15 116.6(3) . . ?
C13 C14 C32 120.1(3) . . ?
C15 C14 C32 123.2(3) . . ?
C14 C15 H15 118.1 . . ?
C14 C15 C16 123.9(3) . . ?
C16 C15 H15 118.1 . . ?
C15 C16 C36 120.7(3) . . ?
C17 C16 C15 117.6(3) . . ?
C17 C16 C36 121.7(3) . . ?
O1 C17 C12 119.5(3) . . ?
O1 C17 C16 120.6(3) . . ?
C16 C17 C12 119.8(3) . . ?
Hf1 C18 H18A 109.3 . . ?
Hf1 C18 H18B 109.3 . . ?
H18A C18 H18B 108.0 . . ?
C19 C18 Hf1 111.5(2) . . ?
C19 C18 H18A 109.3 . . ?
C19 C18 H18B 109.3 . . ?
C20 C19 C18 120.8(3) . . ?
C24 C19 C18 122.3(3) . . ?
C24 C19 C20 116.9(3) . . ?
C19 C20 H20 119.0 . . ?
C21 C20 C19 121.9(3) . . ?
C21 C20 H20 119.0 . . ?
C20 C21 H21 119.8 . . ?
C22 C21 C20 120.4(4) . . ?
C22 C21 H21 119.8 . . ?
C21 C22 H22 120.5 . . ?
C21 C22 C23 119.0(3) . . ?
C23 C22 H22 120.5 . . ?
C22 C23 H23 119.8 . . ?
C22 C23 C24 120.4(4) . . ?
C24 C23 H23 119.8 . . ?
C19 C24 C23 121.3(3) . . ?
C19 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
Hf1 C25 H25A 110.6 . . ?
Hf1 C25 H25B 110.6 . . ?
H25A C25 H25B 108.7 . . ?
C26A C25 Hf1 105.7(2) . . ?
C26A C25 H25A 110.6 . . ?
C26A C25 H25B 110.6 . . ?
C27A C26A C25 127.4(7) . . ?
C27A C26A C31A 121.4(9) . . ?
C31A C26A C25 111.0(7) . . ?
C26A C27A H27A 119.7 . . ?
C28A C27A C26A 120.6(13) . . ?
C28A C27A H27A 119.7 . . ?
C27A C28A H28A 121.0 . . ?
C27A C28A C29A 118.1(13) . . ?
C29A C28A H28A 121.0 . . ?
C28A C29A H29A 118.7 . . ?
C30A C29A C28A 122.6(12) . . ?
C30A C29A H29A 118.7 . . ?
C29A C30A H30A 119.4 . . ?
C29A C30A C31A 121.1(13) . . ?
C31A C30A H30A 119.4 . . ?
C26A C31A H31A 121.9 . . ?
C30A C31A C26A 116.2(12) . . ?
C30A C31A H31A 121.9 . . ?
C28 C27 H27 119.2 . . ?
C27 C28 H28 120.3 . . ?
C27 C28 C29 119.4(6) . . ?
C29 C28 H28 120.3 . . ?
C28 C29 H29 119.3 . . ?
C30 C29 C28 121.3(6) . . ?
C30 C29 H29 119.3 . . ?
C29 C30 H30 120.9 . . ?
C29 C30 C31 118.2(6) . . ?
C31 C30 H30 120.9 . . ?
C30 C31 H31 117.8 . . ?
C14 C32 C35 109.0(3) . . ?
C33 C32 C14 112.7(3) . . ?
C33 C32 C34 109.1(3) . . ?
C33 C32 C35 107.7(3) . . ?
C34 C32 C14 109.3(3) . . ?
C34 C32 C35 108.9(3) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C16 C36 C38 110.3(3) . . ?
C16 C36 C39 109.0(3) . . ?
C37 C36 C16 112.0(3) . . ?
C37 C36 C38 106.9(3) . . ?
C37 C36 C39 107.9(3) . . ?
C39 C36 C38 110.8(3) . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C36 C38 H38A 109.5 . . ?
C36 C38 H38B 109.5 . . ?
C36 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C36 C39 H39A 109.5 . . ?
C36 C39 H39B 109.5 . . ?
C36 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N2 C40 Hf2 52.77(14) . . ?
N2 C40 C4 113.2(3) . . ?
N2 C40 C41 119.2(3) . . ?
C4 C40 Hf2 68.45(17) . . ?
C41 C40 Hf2 148.4(2) . . ?
C41 C40 C4 127.6(3) . . ?
C40 C41 H41 120.9 . . ?
C42 C41 C40 118.2(3) . . ?
C42 C41 H41 120.9 . . ?
C41 C42 H42 119.3 . . ?
C41 C42 C43 121.4(3) . . ?
C43 C42 H42 119.3 . . ?
C42 C43 H43 120.6 . . ?
C44 C43 C42 118.9(3) . . ?
C44 C43 H43 120.6 . . ?
N2 C44 C43 119.7(3) . . ?
N2 C44 C45 116.1(3) . . ?
C43 C44 C45 124.2(3) . . ?
C46 C45 C44 118.8(3) . . ?
C46 C45 C50 119.6(3) . . ?
C50 C45 C44 121.6(3) . . ?
C45 C46 H46 119.1 . . ?
C47 C46 C45 121.8(3) . . ?
C47 C46 H46 119.1 . . ?
C46 C47 C48 117.6(3) . . ?
C46 C47 C65 119.8(3) . . ?
C48 C47 C65 122.6(3) . . ?
C47 C48 H48 118.2 . . ?
C47 C48 C49 123.5(3) . . ?
C49 C48 H48 118.2 . . ?
C48 C49 C50 117.5(3) . . ?
C48 C49 C69 121.5(3) . . ?
C50 C49 C69 121.0(3) . . ?
O2 C50 C45 119.9(3) . . ?
O2 C50 C49 120.2(3) . . ?
C45 C50 C49 119.9(3) . . ?
Hf2 C51 H51A 108.8 . . ?
Hf2 C51 H51B 108.8 . . ?
H51A C51 H51B 107.7 . . ?
C52 C51 Hf2 113.9(2) . . ?
C52 C51 H51A 108.8 . . ?
C52 C51 H51B 108.8 . . ?
C53 C52 C51 122.3(3) . . ?
C57 C52 C51 120.9(3) . . ?
C57 C52 C53 116.8(3) . . ?
C52 C53 H53 119.3 . . ?
C54 C53 C52 121.4(4) . . ?
C54 C53 H53 119.3 . . ?
C53 C54 H54 119.8 . . ?
C55 C54 C53 120.5(4) . . ?
C55 C54 H54 119.8 . . ?
C54 C55 H55 120.4 . . ?
C56 C55 C54 119.1(4) . . ?
C56 C55 H55 120.4 . . ?
C55 C56 H56 120.0 . . ?
C55 C56 C57 120.0(4) . . ?
C57 C56 H56 120.0 . . ?
C52 C57 H57 118.9 . . ?
C56 C57 C52 122.1(4) . . ?
C56 C57 H57 118.9 . . ?
Hf2 C58 H58A 106.1 . . ?
Hf2 C58 H58B 106.1 . . ?
H58A C58 H58B 106.3 . . ?
C59 C58 Hf2 124.7(2) . . ?
C59 C58 H58A 106.1 . . ?
C59 C58 H58B 106.1 . . ?
C60 C59 C58 121.2(3) . . ?
C64 C59 C58 121.6(3) . . ?
C64 C59 C60 117.2(3) . . ?
C59 C60 H60 119.4 . . ?
C61 C60 C59 121.3(3) . . ?
C61 C60 H60 119.4 . . ?
C60 C61 H61 119.7 . . ?
C62 C61 C60 120.5(4) . . ?
C62 C61 H61 119.7 . . ?
C61 C62 H62 120.3 . . ?
C61 C62 C63 119.3(3) . . ?
C63 C62 H62 120.3 . . ?
C62 C63 H63 120.0 . . ?
C64 C63 C62 120.0(4) . . ?
C64 C63 H63 120.0 . . ?
C59 C64 H64 119.2 . . ?
C63 C64 C59 121.7(3) . . ?
C63 C64 H64 119.2 . . ?
C66 C65 C47 108.4(3) . . ?
C66 C65 C67 108.8(4) . . ?
C66 C65 C68 110.7(4) . . ?
C67 C65 C47 109.9(3) . . ?
C68 C65 C47 111.7(3) . . ?
C68 C65 C67 107.3(4) . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C65 C67 H67A 109.5 . . ?
C65 C67 H67B 109.5 . . ?
C65 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C65 C68 H68A 109.5 . . ?
C65 C68 H68B 109.5 . . ?
C65 C68 H68C 109.5 . . ?
H68A C68 H68B 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C49 C69 C71 109.0(3) . . ?
C70 C69 C49 110.4(3) . . ?
C70 C69 C71 110.9(3) . . ?
C70 C69 C72 106.3(3) . . ?
C72 C69 C49 112.4(3) . . ?
C72 C69 C71 107.8(3) . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70B 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C69 C71 H71A 109.5 . . ?
C69 C71 H71B 109.5 . . ?
C69 C71 H71C 109.5 . . ?
H71A C71 H71B 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C69 C72 H72A 109.5 . . ?
C69 C72 H72B 109.5 . . ?
C69 C72 H72C 109.5 . . ?
H72A C72 H72B 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C73 C73 H73B 108.3 3_666 . ?
C73 C73 H73A 108.3 3_666 . ?
C73 C73 C74 116.1(15) 3_666 . ?
H73B C73 H73A 107.4 . . ?
C74 C73 H73B 108.3 . . ?
C74 C73 H73A 108.3 . . ?
C73 C74 H74A 110.6 . . ?
C73 C74 H74B 110.6 . . ?
C73 C74 C75 105.6(11) . . ?
H74A C74 H74B 108.7 . . ?
C75 C74 H74A 110.6 . . ?
C75 C74 H74B 110.6 . . ?
C74 C75 H75A 109.5 . . ?
C74 C75 H75B 109.5 . . ?
C74 C75 H75C 109.5 . . ?
H75A C75 H75B 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method benzene/n-pentane
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
