# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_jgmm023_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H50 Si2'
_chemical_formula_weight         635.02

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3973(11)
_cell_length_b                   12.1375(14)
_cell_length_c                   18.422(2)
_cell_angle_alpha                103.273(6)
_cell_angle_beta                 93.615(7)
_cell_angle_gamma                92.848(6)
_cell_volume                     1819.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       blocks
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             684
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9738
_exptl_absorpt_correction_T_max  0.9799
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            42063
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.14
_diffrn_reflns_theta_max         31.12
_reflns_number_total             11574
_reflns_number_gt                8550
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'


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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0504P)²+0.5099P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11574
_refine_ls_number_parameters     415
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1202
_refine_ls_wR_factor_gt          0.1062
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.42233(4) 0.79742(3) 0.12797(2) 0.01983(8) Uani 1 1 d . . .
Si2 Si -0.08201(4) 0.50349(3) 0.311867(19) 0.01841(8) Uani 1 1 d . . .
C1 C 0.19432(14) 0.78932(10) 0.31829(7) 0.0165(2) Uani 1 1 d . . .
C2 C 0.18444(14) 0.69958(10) 0.25692(7) 0.0166(2) Uani 1 1 d . . .
C3 C 0.13975(15) 0.71437(10) 0.18123(7) 0.0175(2) Uani 1 1 d . . .
C4 C 0.03948(16) 0.64199(11) 0.12888(7) 0.0212(3) Uani 1 1 d . . .
H15A H -0.0058 0.5712 0.1341 0.025 Uiso 1 1 calc R . .
C5 C 0.01185(16) 0.68874(11) 0.06400(7) 0.0216(3) Uani 1 1 d . . .
C6 C -0.08490(18) 0.64827(13) -0.00232(8) 0.0293(3) Uani 1 1 d . . .
H39A H -0.1432 0.5767 -0.0117 0.035 Uiso 1 1 calc R . .
C7 C -0.09385(19) 0.71477(14) -0.05410(8) 0.0330(3) Uani 1 1 d . . .
H38A H -0.1583 0.6881 -0.0997 0.040 Uiso 1 1 calc R . .
C8 C -0.00989(18) 0.81998(14) -0.04038(8) 0.0306(3) Uani 1 1 d . . .
H32A H -0.0200 0.8650 -0.0762 0.037 Uiso 1 1 calc R . .
C9 C 0.08863(16) 0.86046(12) 0.02483(7) 0.0242(3) Uani 1 1 d . . .
H29A H 0.1465 0.9322 0.0337 0.029 Uiso 1 1 calc R . .
C10 C 0.10076(15) 0.79376(11) 0.07686(7) 0.0193(2) Uani 1 1 d . . .
C11 C 0.20175(15) 0.81079(11) 0.14922(7) 0.0175(2) Uani 1 1 d . . .
H8A H 0.1860 0.8859 0.1831 0.021 Uiso 1 1 calc R . .
C12 C 0.21373(14) 0.58351(10) 0.26433(7) 0.0175(2) Uani 1 1 d . . .
C13 C 0.29764(15) 0.50808(11) 0.21849(7) 0.0200(2) Uani 1 1 d . . .
H13A H 0.3427 0.5207 0.1748 0.024 Uiso 1 1 calc R . .
C14 C 0.30899(15) 0.40542(11) 0.24535(7) 0.0206(2) Uani 1 1 d . . .
C15 C 0.38613(17) 0.30609(12) 0.21822(8) 0.0266(3) Uani 1 1 d . . .
H37A H 0.4423 0.2974 0.1743 0.032 Uiso 1 1 calc R . .
C16 C 0.37875(18) 0.22104(12) 0.25673(9) 0.0306(3) Uani 1 1 d . . .
H33A H 0.4294 0.1529 0.2387 0.037 Uiso 1 1 calc R . .
C17 C 0.29845(17) 0.23374(12) 0.32140(9) 0.0305(3) Uani 1 1 d . . .
H35A H 0.2955 0.1744 0.3472 0.037 Uiso 1 1 calc R . .
C18 C 0.22197(16) 0.33243(12) 0.34900(8) 0.0261(3) Uani 1 1 d . . .
H26A H 0.1681 0.3409 0.3936 0.031 Uiso 1 1 calc R . .
C19 C 0.22547(15) 0.41816(11) 0.31052(7) 0.0197(2) Uani 1 1 d . . .
C20 C 0.14756(15) 0.52932(11) 0.32344(7) 0.0179(2) Uani 1 1 d . . .
H10A H 0.1821 0.5766 0.3745 0.022 Uiso 1 1 calc R . .
C21 C 0.11202(14) 0.89618(10) 0.32680(7) 0.0172(2) Uani 1 1 d . . .
C22 C -0.00223(15) 0.93208(11) 0.28011(7) 0.0208(2) Uani 1 1 d . . .
H14A H -0.0323 0.8871 0.2313 0.025 Uiso 1 1 calc R . .
C23 C -0.07122(16) 1.03415(11) 0.30590(8) 0.0245(3) Uani 1 1 d . . .
H27A H -0.1454 1.0602 0.2735 0.029 Uiso 1 1 calc R . .
C24 C -0.03370(17) 1.09881(12) 0.37813(9) 0.0273(3) Uani 1 1 d . . .
H28A H -0.0819 1.1685 0.3946 0.033 Uiso 1 1 calc R . .
C25 C 0.07381(17) 1.06222(11) 0.42641(8) 0.0252(3) Uani 1 1 d . . .
H23A H 0.0974 1.1052 0.4763 0.030 Uiso 1 1 calc R . .
C26 C 0.14654(15) 0.96153(11) 0.40065(7) 0.0195(2) Uani 1 1 d . . .
C27 C 0.25552(15) 0.90104(11) 0.44009(7) 0.0191(2) Uani 1 1 d . . .
C28 C 0.32864(17) 0.93253(12) 0.51213(7) 0.0253(3) Uani 1 1 d . . .
H25A H 0.3072 1.0020 0.5449 0.030 Uiso 1 1 calc R . .
C29 C 0.43371(17) 0.86056(13) 0.53542(8) 0.0284(3) Uani 1 1 d . . .
H31A H 0.4820 0.8797 0.5851 0.034 Uiso 1 1 calc R . .
C30 C 0.46885(16) 0.76042(13) 0.48646(8) 0.0252(3) Uani 1 1 d . . .
H18A H 0.5435 0.7133 0.5028 0.030 Uiso 1 1 calc R . .
C31 C 0.39662(15) 0.72833(11) 0.41408(7) 0.0209(3) Uani 1 1 d . . .
H17A H 0.4232 0.6609 0.3807 0.025 Uiso 1 1 calc R . .
C32 C 0.28415(14) 0.79716(11) 0.39130(7) 0.0176(2) Uani 1 1 d . . .
C33 C 0.54326(17) 0.80245(13) 0.21769(8) 0.0273(3) Uani 1 1 d . . .
H19A H 0.5039 0.7392 0.2389 0.033 Uiso 1 1 calc R . .
H19B H 0.6560 0.7908 0.2069 0.033 Uiso 1 1 calc R . .
C34 C 0.53697(19) 0.91429(15) 0.27636(8) 0.0347(4) Uani 1 1 d . . .
H41A H 0.6024 0.9112 0.3217 0.052 Uiso 1 1 calc R . .
H41B H 0.4261 0.9257 0.2884 0.052 Uiso 1 1 calc R . .
H41C H 0.5784 0.9773 0.2564 0.052 Uiso 1 1 calc R . .
C35 C 0.4485(2) 0.66166(13) 0.05771(8) 0.0319(3) Uani 1 1 d . . .
H34A H 0.5596 0.6404 0.0654 0.038 Uiso 1 1 calc R . .
H34B H 0.3765 0.6014 0.0686 0.038 Uiso 1 1 calc R . .
C36 C 0.4169(3) 0.66221(16) -0.02460(9) 0.0476(5) Uani 1 1 d . . .
H44A H 0.4335 0.5871 -0.0556 0.071 Uiso 1 1 calc R . .
H44B H 0.4904 0.7190 -0.0372 0.071 Uiso 1 1 calc R . .
H44C H 0.3063 0.6809 -0.0339 0.071 Uiso 1 1 calc R . .
C37 C 0.48839(17) 0.92279(12) 0.09135(8) 0.0269(3) Uani 1 1 d . . .
H20A H 0.4370 0.9144 0.0403 0.032 Uiso 1 1 calc R . .
H20B H 0.4513 0.9923 0.1235 0.032 Uiso 1 1 calc R . .
C38 C 0.67052(19) 0.93715(16) 0.08861(10) 0.0403(4) Uani 1 1 d . . .
H42A H 0.6975 1.0035 0.0688 0.060 Uiso 1 1 calc R . .
H42B H 0.7081 0.8692 0.0561 0.060 Uiso 1 1 calc R . .
H42C H 0.7222 0.9479 0.1392 0.060 Uiso 1 1 calc R . .
C39 C -0.17816(16) 0.64019(11) 0.31472(8) 0.0242(3) Uani 1 1 d . . .
H22A H -0.1343 0.6754 0.2762 0.029 Uiso 1 1 calc R . .
H22B H -0.2943 0.6232 0.3014 0.029 Uiso 1 1 calc R . .
C40 C -0.15483(19) 0.72651(13) 0.39046(9) 0.0322(3) Uani 1 1 d . . .
H36A H -0.2089 0.7951 0.3871 0.048 Uiso 1 1 calc R . .
H36B H -0.0404 0.7461 0.4036 0.048 Uiso 1 1 calc R . .
H36C H -0.2004 0.6935 0.4290 0.048 Uiso 1 1 calc R . .
C41 C -0.14379(17) 0.44926(13) 0.39405(8) 0.0277(3) Uani 1 1 d . . .
H30A H -0.1069 0.3719 0.3895 0.033 Uiso 1 1 calc R . .
H30B H -0.0897 0.4984 0.4403 0.033 Uiso 1 1 calc R . .
C42 C -0.32514(18) 0.44524(15) 0.40141(10) 0.0367(4) Uani 1 1 d . . .
H43A H -0.3489 0.4159 0.4451 0.055 Uiso 1 1 calc R . .
H43B H -0.3797 0.3954 0.3563 0.055 Uiso 1 1 calc R . .
H43C H -0.3624 0.5218 0.4075 0.055 Uiso 1 1 calc R . .
C43 C -0.14853(18) 0.40041(12) 0.22121(8) 0.0279(3) Uani 1 1 d . . .
H24A H -0.2559 0.4194 0.2044 0.033 Uiso 1 1 calc R . .
H24B H -0.0747 0.4120 0.1834 0.033 Uiso 1 1 calc R . .
C44 C -0.1569(2) 0.27439(13) 0.22208(10) 0.0353(3) Uani 1 1 d . . .
H40A H -0.1928 0.2289 0.1720 0.053 Uiso 1 1 calc R . .
H40B H -0.2325 0.2605 0.2579 0.053 Uiso 1 1 calc R . .
H40C H -0.0507 0.2531 0.2369 0.053 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
Si1 C33 1.8715(14) . ?
Si1 C37 1.8744(14) . ?
Si1 C35 1.8792(15) . ?
Si1 C11 1.9242(13) . ?
Si2 C39 1.8724(14) . ?
Si2 C41 1.8755(14) . ?
Si2 C43 1.8762(15) . ?
Si2 C20 1.9281(13) . ?
C1 C2 1.3730(17) . ?
C1 C32 1.4810(17) . ?
C1 C21 1.4811(17) . ?
C2 C3 1.4742(16) . ?
C2 C12 1.4774(17) . ?
C3 C4 1.3586(18) . ?
C3 C11 1.5111(17) . ?
C4 C5 1.4470(17) . ?
C5 C6 1.3977(18) . ?
C5 C10 1.4082(19) . ?
C6 C7 1.385(2) . ?
C7 C8 1.390(2) . ?
C8 C9 1.390(2) . ?
C9 C10 1.3917(17) . ?
C10 C11 1.5007(17) . ?
C12 C13 1.3535(18) . ?
C12 C20 1.5153(17) . ?
C13 C14 1.4475(18) . ?
C14 C15 1.4017(19) . ?
C14 C19 1.4101(18) . ?
C15 C16 1.381(2) . ?
C16 C17 1.387(2) . ?
C17 C18 1.394(2) . ?
C18 C19 1.3872(18) . ?
C19 C20 1.5049(17) . ?
C21 C22 1.4000(17) . ?
C21 C26 1.4128(17) . ?
C22 C23 1.3900(19) . ?
C23 C24 1.389(2) . ?
C24 C25 1.387(2) . ?
C25 C26 1.3915(19) . ?
C26 C27 1.4602(18) . ?
C27 C28 1.3876(18) . ?
C27 C32 1.4115(18) . ?
C28 C29 1.388(2) . ?
C29 C30 1.394(2) . ?
C30 C31 1.3905(18) . ?
C31 C32 1.3983(17) . ?
C33 C34 1.534(2) . ?
C35 C36 1.524(2) . ?
C37 C38 1.536(2) . ?
C39 C40 1.535(2) . ?
C41 C42 1.537(2) . ?
C43 C44 1.532(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C33 Si1 C37 108.61(7) . . ?
C33 Si1 C35 110.48(7) . . ?
C37 Si1 C35 110.46(7) . . ?
C33 Si1 C11 108.22(6) . . ?
C37 Si1 C11 107.98(6) . . ?
C35 Si1 C11 110.99(7) . . ?
C39 Si2 C41 107.70(7) . . ?
C39 Si2 C43 109.08(6) . . ?
C41 Si2 C43 111.41(7) . . ?
C39 Si2 C20 110.29(6) . . ?
C41 Si2 C20 107.15(6) . . ?
C43 Si2 C20 111.14(6) . . ?
C2 C1 C32 127.00(11) . . ?
C2 C1 C21 127.48(11) . . ?
C32 C1 C21 105.47(10) . . ?
C1 C2 C3 121.46(11) . . ?
C1 C2 C12 121.31(11) . . ?
C3 C2 C12 117.21(10) . . ?
C4 C3 C2 125.25(11) . . ?
C4 C3 C11 109.51(11) . . ?
C2 C3 C11 125.23(11) . . ?
C3 C4 C5 109.93(11) . . ?
C6 C5 C10 120.49(13) . . ?
C6 C5 C4 131.22(13) . . ?
C10 C5 C4 108.28(11) . . ?
C7 C6 C5 118.55(14) . . ?
C6 C7 C8 120.94(13) . . ?
C7 C8 C9 121.08(13) . . ?
C8 C9 C10 118.60(14) . . ?
C9 C10 C5 120.29(12) . . ?
C9 C10 C11 131.07(12) . . ?
C5 C10 C11 108.61(11) . . ?
C10 C11 C3 102.73(10) . . ?
C10 C11 Si1 108.93(8) . . ?
C3 C11 Si1 111.52(8) . . ?
C13 C12 C2 125.85(11) . . ?
C13 C12 C20 109.59(11) . . ?
C2 C12 C20 124.52(11) . . ?
C12 C13 C14 110.42(11) . . ?
C15 C14 C19 120.69(12) . . ?
C15 C14 C13 131.30(13) . . ?
C19 C14 C13 108.00(11) . . ?
C16 C15 C14 118.58(14) . . ?
C15 C16 C17 120.95(13) . . ?
C16 C17 C18 120.88(13) . . ?
C19 C18 C17 119.16(14) . . ?
C18 C19 C14 119.72(12) . . ?
C18 C19 C20 131.40(12) . . ?
C14 C19 C20 108.84(11) . . ?
C19 C20 C12 102.58(10) . . ?
C19 C20 Si2 110.37(9) . . ?
C12 C20 Si2 113.06(8) . . ?
C22 C21 C26 118.79(12) . . ?
C22 C21 C1 131.82(11) . . ?
C26 C21 C1 108.77(11) . . ?
C23 C22 C21 119.32(12) . . ?
C24 C23 C22 121.21(13) . . ?
C25 C24 C23 120.35(13) . . ?
C24 C25 C26 118.96(13) . . ?
C25 C26 C21 121.25(12) . . ?
C25 C26 C27 130.24(12) . . ?
C21 C26 C27 108.39(11) . . ?
C28 C27 C32 121.23(12) . . ?
C28 C27 C26 130.12(12) . . ?
C32 C27 C26 108.63(11) . . ?
C27 C28 C29 118.72(13) . . ?
C28 C29 C30 120.49(13) . . ?
C31 C30 C29 121.18(13) . . ?
C30 C31 C32 118.80(12) . . ?
C31 C32 C27 119.39(11) . . ?
C31 C32 C1 131.52(12) . . ?
C27 C32 C1 108.70(11) . . ?
C34 C33 Si1 113.68(10) . . ?
C36 C35 Si1 116.97(11) . . ?
C38 C37 Si1 113.30(11) . . ?
C40 C39 Si2 114.79(10) . . ?
C42 C41 Si2 113.81(10) . . ?
C44 C43 Si2 116.69(11) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        31.12
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.053
_database_code_depnum_ccdc_archive 'CCDC 1003249'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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data_t1_compound_9a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H70 Cl8 Ti3'
_chemical_formula_weight         1794.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   20.627(5)
_cell_length_b                   15.990(5)
_cell_length_c                   25.582(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.08(3)
_cell_angle_gamma                90.00
_cell_volume                     8390(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       blocks
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3680
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9173
_exptl_absorpt_correction_T_max  0.9546
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            64896
_diffrn_reflns_av_R_equivalents  0.1308
_diffrn_reflns_av_sigmaI/netI    0.1112
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.61
_diffrn_reflns_theta_max         27.76
_reflns_number_total             9744
_reflns_number_gt                5374
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1855P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9744
_refine_ls_number_parameters     517
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0574
_refine_ls_wR_factor_ref         0.2183
_refine_ls_wR_factor_gt          0.1607
_refine_ls_goodness_of_fit_ref   0.728
_refine_ls_restrained_S_all      0.728
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 1.03919(3) 0.27157(4) 0.46139(3) 0.01992(19) Uani 1 1 d . . .
Ti2 Ti 1.0000 -0.02385(6) 0.2500 0.0199(2) Uani 1 2 d S . .
Cl1 Cl 1.07012(5) 0.15125(6) 0.42015(4) 0.0320(3) Uani 1 1 d . . .
Cl2 Cl 1.09421(5) 0.25092(7) 0.54295(4) 0.0309(3) Uani 1 1 d . . .
Cl3 Cl 1.04658(5) -0.11720(7) 0.31120(4) 0.0339(3) Uani 1 1 d . . .
C1 C 0.91671(19) 0.4747(3) 0.40333(15) 0.0247(9) Uani 1 1 d . . .
C2 C 0.95511(19) 0.4129(3) 0.42367(15) 0.0235(8) Uani 1 1 d . . .
C3 C 1.02685(19) 0.4026(3) 0.42274(16) 0.0264(9) Uani 1 1 d . . .
C4 C 1.07274(19) 0.4142(2) 0.46701(15) 0.0234(8) Uani 1 1 d . . .
H4A H 1.0672 0.4526 0.4971 0.028 Uiso 1 1 calc R . .
C5 C 1.13319(18) 0.3774(2) 0.45575(16) 0.0237(8) Uani 1 1 d . . .
C6 C 1.1956(2) 0.3756(3) 0.48511(17) 0.0286(9) Uani 1 1 d . . .
H6A H 1.2032 0.4028 0.5182 0.034 Uiso 1 1 calc R . .
C7 C 1.24429(19) 0.3336(3) 0.46417(18) 0.0316(10) Uani 1 1 d . . .
H7A H 1.2867 0.3324 0.4827 0.038 Uiso 1 1 calc R . .
C8 C 1.2329(2) 0.2921(3) 0.41594(18) 0.0329(10) Uani 1 1 d . . .
H8A H 1.2676 0.2619 0.4032 0.039 Uiso 1 1 calc R . .
C9 C 1.1732(2) 0.2933(3) 0.38626(16) 0.0286(9) Uani 1 1 d . . .
H9A H 1.1667 0.2654 0.3533 0.034 Uiso 1 1 calc R . .
C10 C 1.12160(18) 0.3375(2) 0.40624(15) 0.0229(8) Uani 1 1 d . . .
C11 C 1.05444(19) 0.3511(3) 0.38654(16) 0.0261(9) Uani 1 1 d . . .
H11A H 1.0347 0.3387 0.3500 0.031 Uiso 1 1 calc R . .
C12 C 0.93656(17) 0.3332(2) 0.44891(15) 0.0219(8) Uani 1 1 d . . .
C13 C 0.94956(18) 0.3154(3) 0.50302(15) 0.0248(9) Uani 1 1 d . . .
H13A H 0.9509 0.3575 0.5320 0.030 Uiso 1 1 calc R . .
C14 C 0.94281(18) 0.2267(2) 0.50915(15) 0.0225(8) Uani 1 1 d . . .
C15 C 0.94783(19) 0.1750(3) 0.55437(16) 0.0281(9) Uani 1 1 d . . .
H15A H 0.9579 0.1979 0.5885 0.034 Uiso 1 1 calc R . .
C16 C 0.9377(2) 0.0908(3) 0.54719(17) 0.0295(10) Uani 1 1 d . . .
H16A H 0.9407 0.0553 0.5771 0.035 Uiso 1 1 calc R . .
C17 C 0.9232(2) 0.0551(3) 0.49697(17) 0.0319(10) Uani 1 1 d . . .
H17A H 0.9160 -0.0035 0.4937 0.038 Uiso 1 1 calc R . .
C18 C 0.91921(19) 0.1042(3) 0.45287(17) 0.0285(9) Uani 1 1 d . . .
H18A H 0.9098 0.0801 0.4190 0.034 Uiso 1 1 calc R . .
C19 C 0.92933(17) 0.1909(3) 0.45846(15) 0.0230(8) Uani 1 1 d . . .
C20 C 0.92980(18) 0.2575(2) 0.42110(15) 0.0227(8) Uani 1 1 d . . .
H20A H 0.9168 0.2522 0.3825 0.027 Uiso 1 1 calc R . .
C21 C 0.84435(19) 0.4811(2) 0.40336(15) 0.0229(8) Uani 1 1 d . . .
C22 C 0.8009(2) 0.4292(3) 0.42538(16) 0.0288(9) Uani 1 1 d . . .
H22A H 0.8156 0.3801 0.4439 0.035 Uiso 1 1 calc R . .
C23 C 0.7347(2) 0.4510(3) 0.41963(18) 0.0365(11) Uani 1 1 d . . .
H23A H 0.7039 0.4164 0.4344 0.044 Uiso 1 1 calc R . .
C24 C 0.7139(2) 0.5227(3) 0.39246(18) 0.0364(11) Uani 1 1 d . . .
H24A H 0.6689 0.5370 0.3892 0.044 Uiso 1 1 calc R . .
C25 C 0.7569(2) 0.5733(3) 0.37019(16) 0.0306(10) Uani 1 1 d . . .
H25A H 0.7419 0.6218 0.3512 0.037 Uiso 1 1 calc R . .
C26 C 0.8232(2) 0.5531(3) 0.37556(15) 0.0261(9) Uani 1 1 d . . .
C27 C 0.8797(2) 0.5948(2) 0.35687(15) 0.0260(9) Uani 1 1 d . . .
C28 C 0.8837(2) 0.6651(3) 0.32632(17) 0.0355(11) Uani 1 1 d . . .
H28A H 0.8455 0.6953 0.3139 0.043 Uiso 1 1 calc R . .
C29 C 0.9443(3) 0.6911(3) 0.31398(18) 0.0412(12) Uani 1 1 d . . .
H29A H 0.9474 0.7397 0.2930 0.049 Uiso 1 1 calc R . .
C30 C 1.0007(3) 0.6476(3) 0.33169(18) 0.0386(11) Uani 1 1 d . . .
H30A H 1.0418 0.6665 0.3229 0.046 Uiso 1 1 calc R . .
C31 C 0.9968(2) 0.5760(3) 0.36242(16) 0.0310(10) Uani 1 1 d . . .
H31A H 1.0350 0.5458 0.3748 0.037 Uiso 1 1 calc R . .
C32 C 0.9362(2) 0.5496(2) 0.37452(15) 0.0235(8) Uani 1 1 d . . .
C33 C 1.0000 0.2445(3) 0.2500 0.0221(12) Uani 1 2 d S . .
C34 C 1.0000 0.1618(3) 0.2500 0.0216(11) Uani 1 2 d S . .
C35 C 1.04913(19) 0.1026(2) 0.23205(16) 0.0236(8) Uani 1 1 d . . .
C36 C 1.03703(19) 0.0591(2) 0.18367(15) 0.0227(8) Uani 1 1 d . . .
H36A H 1.0096 0.0800 0.1518 0.027 Uiso 1 1 calc R . .
C37 C 1.08399(19) -0.0076(3) 0.18440(15) 0.0240(8) Uani 1 1 d . . .
C38 C 1.0957(2) -0.0682(3) 0.14608(16) 0.0269(9) Uani 1 1 d . . .
H38A H 1.0698 -0.0703 0.1131 0.032 Uiso 1 1 calc R . .
C39 C 1.1451(2) -0.1231(3) 0.15815(17) 0.0307(10) Uani 1 1 d . . .
H39A H 1.1543 -0.1633 0.1326 0.037 Uiso 1 1 calc R . .
C40 C 1.1833(2) -0.1226(3) 0.20748(18) 0.0316(10) Uani 1 1 d . . .
H40A H 1.2181 -0.1614 0.2138 0.038 Uiso 1 1 calc R . .
C41 C 1.1714(2) -0.0676(3) 0.24608(17) 0.0282(9) Uani 1 1 d . . .
H41A H 1.1960 -0.0692 0.2796 0.034 Uiso 1 1 calc R . .
C42 C 1.12130(19) -0.0081(2) 0.23460(15) 0.0235(8) Uani 1 1 d . . .
C43 C 1.09653(18) 0.0576(2) 0.26473(16) 0.0235(8) Uani 1 1 d . . .
H43A H 1.1167 0.0768 0.3000 0.028 Uiso 1 1 calc R . .
C44 C 1.0532(2) 0.3007(2) 0.23744(14) 0.0238(8) Uani 1 1 d . . .
C45 C 1.1156(2) 0.2822(3) 0.22416(15) 0.0273(9) Uani 1 1 d . . .
H45A H 1.1288 0.2260 0.2195 0.033 Uiso 1 1 calc R . .
C46 C 1.1578(2) 0.3482(3) 0.21805(17) 0.0352(11) Uani 1 1 d . . .
H46A H 1.1999 0.3369 0.2079 0.042 Uiso 1 1 calc R . .
C47 C 1.1398(2) 0.4302(3) 0.22645(17) 0.0356(11) Uani 1 1 d . . .
H47A H 1.1704 0.4740 0.2236 0.043 Uiso 1 1 calc R . .
C48 C 1.0777(2) 0.4488(3) 0.23897(17) 0.0357(11) Uani 1 1 d . . .
H48A H 1.0652 0.5051 0.2443 0.043 Uiso 1 1 calc R . .
C49 C 1.0338(2) 0.3838(2) 0.24360(15) 0.0273(9) Uani 1 1 d . . .
Cl4 Cl 1.23755(19) 0.7310(2) 0.47505(12) 0.0748(10) Uani 0.50 1 d P . 2
C56 C 1.2260(7) 0.5646(5) 0.3588(5) 0.140(10) Uiso 0.50 1 d PG A 2
H56A H 1.2363 0.5074 0.3540 0.168 Uiso 0.50 1 calc PR A 2
C51 C 1.1997(6) 0.6123(7) 0.3164(4) 0.131(7) Uiso 0.50 1 d PG A 2
H51A H 1.1921 0.5877 0.2825 0.157 Uiso 0.50 1 calc PR A 2
C52 C 1.1847(5) 0.6960(7) 0.3235(3) 0.069(4) Uiso 0.50 1 d PG A 2
H52A H 1.1667 0.7286 0.2945 0.082 Uiso 0.50 1 calc PR A 2
C55 C 1.1959(4) 0.7319(5) 0.3731(3) 0.061(3) Uiso 0.50 1 d PG A 2
H55A H 1.1856 0.7891 0.3780 0.073 Uiso 0.50 1 calc PR A 2
C54 C 1.2221(4) 0.6842(6) 0.4156(3) 0.059(3) Uiso 0.50 1 d PG A 2
C53 C 1.2372(6) 0.6005(6) 0.4084(4) 0.102(6) Uiso 0.50 1 d PG A 2
H53A H 1.2552 0.5679 0.4375 0.122 Uiso 0.50 1 calc PR A 2
Cl5 Cl 1.25130(15) 0.6393(2) 0.26316(12) 0.0666(8) Uani 0.50 1 d P B 3
C66 C 1.2444(5) 0.5667(5) 0.3533(4) 0.069(4) Uiso 0.50 1 d PG B 3
H66A H 1.2672 0.5224 0.3387 0.083 Uiso 0.50 1 calc PR B 3
C61 C 1.2300(4) 0.6393(5) 0.3245(3) 0.049(3) Uiso 0.50 1 d PG B 3
C62 C 1.1965(4) 0.7041(5) 0.3459(4) 0.068(3) Uiso 0.50 1 d PG B 3
H62A H 1.1867 0.7537 0.3262 0.081 Uiso 0.50 1 calc PR B 3
C65 C 1.1774(5) 0.6963(6) 0.3962(4) 0.097(5) Uiso 0.50 1 d PG B 3
H65A H 1.1545 0.7406 0.4108 0.116 Uiso 0.50 1 calc PR B 3
C64 C 1.1917(6) 0.6238(8) 0.4250(3) 0.118(6) Uiso 0.50 1 d PG B 3
H64A H 1.1786 0.6185 0.4594 0.142 Uiso 0.50 1 calc PR B 3
C63 C 1.2252(6) 0.5590(6) 0.4036(4) 0.108(6) Uiso 0.50 1 d PG B 3
H63A H 1.2350 0.5094 0.4233 0.129 Uiso 0.50 1 calc PR B 3


_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 Cl2 2.2910(13) . ?
Ti1 Cl1 2.3158(13) . ?
Ti1 C3 2.319(4) . ?
Ti1 C12 2.326(4) . ?
Ti1 C13 2.337(4) . ?
Ti1 C11 2.347(4) . ?
Ti1 C4 2.384(4) . ?
Ti1 C20 2.390(4) . ?
Ti1 C14 2.545(4) . ?
Ti1 C10 2.549(4) . ?
Ti1 C5 2.589(4) . ?
Ti1 C19 2.602(4) . ?
Ti2 Cl3 2.2988(13) 2_755 ?
Ti2 Cl3 2.2988(13) . ?
Ti2 C35 2.328(4) . ?
Ti2 C35 2.328(4) 2_755 ?
Ti2 C36 2.345(4) 2_755 ?
Ti2 C36 2.345(4) . ?
Ti2 C43 2.376(4) . ?
Ti2 C43 2.376(4) 2_755 ?
Ti2 C37 2.550(4) . ?
Ti2 C37 2.550(4) 2_755 ?
Ti2 C42 2.586(4) . ?
Ti2 C42 2.586(4) 2_755 ?
C1 C2 1.337(5) . ?
C1 C32 1.484(6) . ?
C1 C21 1.496(5) . ?
C2 C3 1.492(5) . ?
C2 C12 1.496(6) . ?
C3 C11 1.404(6) . ?
C3 C4 1.409(6) . ?
C4 C5 1.436(5) . ?
C4 H4A 1.0000 . ?
C5 C10 1.416(6) . ?
C5 C6 1.420(6) . ?
C6 C7 1.364(6) . ?
C6 H6A 0.9500 . ?
C7 C8 1.399(6) . ?
C7 H7A 0.9500 . ?
C8 C9 1.377(6) . ?
C8 H8A 0.9500 . ?
C9 C10 1.417(6) . ?
C9 H9A 0.9500 . ?
C10 C11 1.440(5) . ?
C11 H11A 1.0000 . ?
C12 C20 1.403(6) . ?
C12 C13 1.411(5) . ?
C13 C14 1.436(6) . ?
C13 H13A 1.0000 . ?
C14 C15 1.416(5) . ?
C14 C19 1.418(5) . ?
C15 C16 1.373(6) . ?
C15 H15A 0.9500 . ?
C16 C17 1.409(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.370(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.406(6) . ?
C18 H18A 0.9500 . ?
C19 C20 1.433(5) . ?
C20 H20A 1.0000 . ?
C21 C22 1.384(6) . ?
C21 C26 1.399(5) . ?
C22 C23 1.403(6) . ?
C22 H22A 0.9500 . ?
C23 C24 1.385(6) . ?
C23 H23A 0.9500 . ?
C24 C25 1.370(7) . ?
C24 H24A 0.9500 . ?
C25 C26 1.396(6) . ?
C25 H25A 0.9500 . ?
C26 C27 1.467(6) . ?
C27 C28 1.377(6) . ?
C27 C32 1.406(6) . ?
C28 C29 1.385(7) . ?
C28 H28A 0.9500 . ?
C29 C30 1.390(7) . ?
C29 H29A 0.9500 . ?
C30 C31 1.396(6) . ?
C30 H30A 0.9500 . ?
C31 C32 1.384(6) . ?
C31 H31A 0.9500 . ?
C33 C34 1.322(8) . ?
C33 C44 1.481(5) . ?
C33 C44 1.481(5) 2_755 ?
C34 C35 1.494(5) 2_755 ?
C34 C35 1.494(5) . ?
C35 C43 1.413(5) . ?
C35 C36 1.418(5) . ?
C36 C37 1.440(6) . ?
C36 H36A 1.0000 . ?
C37 C38 1.417(6) . ?
C37 C42 1.426(5) . ?
C38 C39 1.356(6) . ?
C38 H38A 0.9500 . ?
C39 C40 1.416(6) . ?
C39 H39A 0.9500 . ?
C40 C41 1.364(6) . ?
C40 H40A 0.9500 . ?
C41 C42 1.412(6) . ?
C41 H41A 0.9500 . ?
C42 C43 1.430(6) . ?
C43 H43A 1.0000 . ?
C44 C45 1.397(6) . ?
C44 C49 1.401(6) . ?
C45 C46 1.386(6) . ?
C45 H45A 0.9500 . ?
C46 C47 1.385(7) . ?
C46 H46A 0.9500 . ?
C47 C48 1.387(7) . ?
C47 H47A 0.9500 . ?
C48 C49 1.391(6) . ?
C48 H48A 0.9500 . ?
C49 C49 1.467(9) 2_755 ?
Cl4 Cl4 1.458(7) 7_766 ?
Cl4 C54 1.695(8) . ?
C56 C51 1.3900 . ?
C56 C53 1.3900 . ?
C56 H56A 0.9500 . ?
C51 C52 1.3900 . ?
C51 H51A 0.9500 . ?
C52 C55 1.3900 . ?
C52 H52A 0.9500 . ?
C55 C54 1.3900 . ?
C55 H55A 0.9500 . ?
C54 C53 1.3900 . ?
C53 H53A 0.9500 . ?
Cl5 C61 1.673(7) . ?
C66 C61 1.3900 . ?
C66 C63 1.3900 . ?
C66 H66A 0.9500 . ?
C61 C62 1.3900 . ?
C62 C65 1.3900 . ?
C62 H62A 0.9500 . ?
C65 C64 1.3900 . ?
C65 H65A 0.9500 . ?
C64 C63 1.3900 . ?
C64 H64A 0.9500 . ?
C63 H63A 0.9500 . ?

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
Cl2 Ti1 Cl1 99.29(5) . . ?
Cl2 Ti1 C3 122.67(11) . . ?
Cl1 Ti1 C3 125.41(11) . . ?
Cl2 Ti1 C12 122.81(10) . . ?
Cl1 Ti1 C12 125.45(10) . . ?
C3 Ti1 C12 60.10(14) . . ?
Cl2 Ti1 C13 88.15(10) . . ?
Cl1 Ti1 C13 136.58(11) . . ?
C3 Ti1 C13 82.34(14) . . ?
C12 Ti1 C13 35.22(13) . . ?
Cl2 Ti1 C11 136.45(11) . . ?
Cl1 Ti1 C11 90.65(11) . . ?
C3 Ti1 C11 35.02(14) . . ?
C12 Ti1 C11 81.79(14) . . ?
C13 Ti1 C11 112.95(14) . . ?
Cl2 Ti1 C4 88.30(10) . . ?
Cl1 Ti1 C4 136.91(11) . . ?
C3 Ti1 C4 34.84(14) . . ?
C12 Ti1 C4 81.78(14) . . ?
C13 Ti1 C4 85.63(14) . . ?
C11 Ti1 C4 57.84(14) . . ?
Cl2 Ti1 C20 137.16(10) . . ?
Cl1 Ti1 C20 91.07(10) . . ?
C3 Ti1 C20 81.08(14) . . ?
C12 Ti1 C20 34.58(13) . . ?
C13 Ti1 C20 57.88(13) . . ?
C11 Ti1 C20 84.32(14) . . ?
C4 Ti1 C20 111.75(13) . . ?
Cl2 Ti1 C14 81.89(10) . . ?
Cl1 Ti1 C14 104.56(10) . . ?
C3 Ti1 C14 113.78(13) . . ?
C12 Ti1 C14 55.90(13) . . ?
C13 Ti1 C14 33.87(13) . . ?
C11 Ti1 C14 136.34(13) . . ?
C4 Ti1 C14 118.52(13) . . ?
C20 Ti1 C14 55.29(13) . . ?
Cl2 Ti1 C10 105.58(9) . . ?
Cl1 Ti1 C10 81.93(10) . . ?
C3 Ti1 C10 55.94(13) . . ?
C12 Ti1 C10 113.53(13) . . ?
C13 Ti1 C10 137.22(14) . . ?
C11 Ti1 C10 33.87(13) . . ?
C4 Ti1 C10 55.33(13) . . ?
C20 Ti1 C10 117.04(13) . . ?
C14 Ti1 C10 169.41(13) . . ?
Cl2 Ti1 C5 80.98(9) . . ?
Cl1 Ti1 C5 105.88(10) . . ?
C3 Ti1 C5 55.59(13) . . ?
C12 Ti1 C5 113.05(13) . . ?
C13 Ti1 C5 117.55(14) . . ?
C11 Ti1 C5 55.58(13) . . ?
C4 Ti1 C5 33.23(13) . . ?
C20 Ti1 C5 135.71(13) . . ?
C14 Ti1 C5 147.02(13) . . ?
C10 Ti1 C5 31.97(12) . . ?
Cl2 Ti1 C19 107.50(9) . . ?
Cl1 Ti1 C19 81.72(10) . . ?
C3 Ti1 C19 112.32(13) . . ?
C12 Ti1 C19 55.18(13) . . ?
C13 Ti1 C19 55.48(14) . . ?
C11 Ti1 C19 115.89(13) . . ?
C4 Ti1 C19 136.27(13) . . ?
C20 Ti1 C19 33.01(12) . . ?
C14 Ti1 C19 31.96(12) . . ?
C10 Ti1 C19 144.98(12) . . ?
C5 Ti1 C19 167.86(12) . . ?
Cl3 Ti2 Cl3 99.02(7) 2_755 . ?
Cl3 Ti2 C35 126.06(10) 2_755 . ?
Cl3 Ti2 C35 122.60(10) . . ?
Cl3 Ti2 C35 122.60(10) 2_755 2_755 ?
Cl3 Ti2 C35 126.06(10) . 2_755 ?
C35 Ti2 C35 59.5(2) . 2_755 ?
Cl3 Ti2 C36 135.70(10) 2_755 2_755 ?
Cl3 Ti2 C36 91.10(10) . 2_755 ?
C35 Ti2 C36 80.41(14) . 2_755 ?
C35 Ti2 C36 35.33(13) 2_755 2_755 ?
Cl3 Ti2 C36 91.10(10) 2_755 . ?
Cl3 Ti2 C36 135.70(10) . . ?
C35 Ti2 C36 35.33(13) . . ?
C35 Ti2 C36 80.41(14) 2_755 . ?
C36 Ti2 C36 111.08(19) 2_755 . ?
Cl3 Ti2 C43 138.33(10) 2_755 . ?
Cl3 Ti2 C43 88.01(10) . . ?
C35 Ti2 C43 34.95(13) . . ?
C35 Ti2 C43 82.39(14) 2_755 . ?
C36 Ti2 C43 84.64(14) 2_755 . ?
C36 Ti2 C43 58.18(13) . . ?
Cl3 Ti2 C43 88.01(10) 2_755 2_755 ?
Cl3 Ti2 C43 138.33(10) . 2_755 ?
C35 Ti2 C43 82.39(14) . 2_755 ?
C35 Ti2 C43 34.95(13) 2_755 2_755 ?
C36 Ti2 C43 58.18(13) 2_755 2_755 ?
C36 Ti2 C43 84.64(14) . 2_755 ?
C43 Ti2 C43 113.48(19) . 2_755 ?
Cl3 Ti2 C37 83.22(9) 2_755 . ?
Cl3 Ti2 C37 104.50(9) . . ?
C35 Ti2 C37 56.05(13) . . ?
C35 Ti2 C37 112.43(14) 2_755 . ?
C36 Ti2 C37 135.63(14) 2_755 . ?
C36 Ti2 C37 33.89(13) . . ?
C43 Ti2 C37 55.40(13) . . ?
C43 Ti2 C37 117.14(14) 2_755 . ?
Cl3 Ti2 C37 104.50(10) 2_755 2_755 ?
Cl3 Ti2 C37 83.22(9) . 2_755 ?
C35 Ti2 C37 112.43(14) . 2_755 ?
C35 Ti2 C37 56.05(13) 2_755 2_755 ?
C36 Ti2 C37 33.89(13) 2_755 2_755 ?
C36 Ti2 C37 135.63(14) . 2_755 ?
C43 Ti2 C37 117.14(14) . 2_755 ?
C43 Ti2 C37 55.40(13) 2_755 2_755 ?
C37 Ti2 C37 168.31(19) . 2_755 ?
Cl3 Ti2 C42 107.51(9) 2_755 . ?
Cl3 Ti2 C42 79.95(9) . . ?
C35 Ti2 C42 55.75(13) . . ?
C35 Ti2 C42 113.20(14) 2_755 . ?
C36 Ti2 C42 116.73(13) 2_755 . ?
C36 Ti2 C42 55.95(13) . . ?
C43 Ti2 C42 33.15(13) . . ?
C43 Ti2 C42 136.93(14) 2_755 . ?
C37 Ti2 C42 32.23(12) . . ?
C37 Ti2 C42 145.70(12) 2_755 . ?
Cl3 Ti2 C42 79.95(9) 2_755 2_755 ?
Cl3 Ti2 C42 107.51(9) . 2_755 ?
C35 Ti2 C42 113.20(14) . 2_755 ?
C35 Ti2 C42 55.75(13) 2_755 2_755 ?
C36 Ti2 C42 55.95(13) 2_755 2_755 ?
C36 Ti2 C42 116.73(13) . 2_755 ?
C43 Ti2 C42 136.93(14) . 2_755 ?
C43 Ti2 C42 33.15(13) 2_755 2_755 ?
C37 Ti2 C42 145.70(12) . 2_755 ?
C37 Ti2 C42 32.23(12) 2_755 2_755 ?
C42 Ti2 C42 168.83(18) . 2_755 ?
C2 C1 C32 127.5(4) . . ?
C2 C1 C21 126.9(4) . . ?
C32 C1 C21 105.6(3) . . ?
C1 C2 C3 128.5(4) . . ?
C1 C2 C12 129.0(4) . . ?
C3 C2 C12 102.3(3) . . ?
C11 C3 C4 108.8(4) . . ?
C11 C3 C2 123.2(4) . . ?
C4 C3 C2 123.8(4) . . ?
C11 C3 Ti1 73.6(2) . . ?
C4 C3 Ti1 75.1(2) . . ?
C2 C3 Ti1 99.0(2) . . ?
C3 C4 C5 108.0(3) . . ?
C3 C4 Ti1 70.1(2) . . ?
C5 C4 Ti1 81.3(2) . . ?
C3 C4 H4A 125.3 . . ?
C5 C4 H4A 125.3 . . ?
Ti1 C4 H4A 125.3 . . ?
C10 C5 C6 121.5(4) . . ?
C10 C5 C4 107.2(3) . . ?
C6 C5 C4 131.3(4) . . ?
C10 C5 Ti1 72.5(2) . . ?
C6 C5 Ti1 126.9(3) . . ?
C4 C5 Ti1 65.5(2) . . ?
C7 C6 C5 117.8(4) . . ?
C7 C6 H6A 121.1 . . ?
C5 C6 H6A 121.1 . . ?
C6 C7 C8 121.2(4) . . ?
C6 C7 H7A 119.4 . . ?
C8 C7 H7A 119.4 . . ?
C9 C8 C7 122.4(4) . . ?
C9 C8 H8A 118.8 . . ?
C7 C8 H8A 118.8 . . ?
C8 C9 C10 118.1(4) . . ?
C8 C9 H9A 121.0 . . ?
C10 C9 H9A 121.0 . . ?
C5 C10 C9 119.0(3) . . ?
C5 C10 C11 108.1(3) . . ?
C9 C10 C11 132.9(4) . . ?
C5 C10 Ti1 75.6(2) . . ?
C9 C10 Ti1 124.3(3) . . ?
C11 C10 Ti1 65.3(2) . . ?
C3 C11 C10 107.4(4) . . ?
C3 C11 Ti1 71.4(2) . . ?
C10 C11 Ti1 80.8(2) . . ?
C3 C11 H11A 125.4 . . ?
C10 C11 H11A 125.4 . . ?
Ti1 C11 H11A 125.4 . . ?
C20 C12 C13 108.8(3) . . ?
C20 C12 C2 122.1(3) . . ?
C13 C12 C2 124.3(4) . . ?
C20 C12 Ti1 75.2(2) . . ?
C13 C12 Ti1 72.8(2) . . ?
C2 C12 Ti1 98.6(2) . . ?
C12 C13 C14 107.2(3) . . ?
C12 C13 Ti1 72.0(2) . . ?
C14 C13 Ti1 81.0(2) . . ?
C12 C13 H13A 125.4 . . ?
C14 C13 H13A 125.4 . . ?
Ti1 C13 H13A 125.4 . . ?
C15 C14 C19 120.1(4) . . ?
C15 C14 C13 131.8(4) . . ?
C19 C14 C13 108.1(3) . . ?
C15 C14 Ti1 124.3(3) . . ?
C19 C14 Ti1 76.3(2) . . ?
C13 C14 Ti1 65.1(2) . . ?
C16 C15 C14 117.8(4) . . ?
C16 C15 H15A 121.1 . . ?
C14 C15 H15A 121.1 . . ?
C15 C16 C17 122.3(4) . . ?
C15 C16 H16A 118.9 . . ?
C17 C16 H16A 118.9 . . ?
C18 C17 C16 120.5(4) . . ?
C18 C17 H17A 119.8 . . ?
C16 C17 H17A 119.8 . . ?
C17 C18 C19 119.1(4) . . ?
C17 C18 H18A 120.5 . . ?
C19 C18 H18A 120.5 . . ?
C18 C19 C14 120.2(4) . . ?
C18 C19 C20 132.6(4) . . ?
C14 C19 C20 107.2(4) . . ?
C18 C19 Ti1 127.7(3) . . ?
C14 C19 Ti1 71.8(2) . . ?
C20 C19 Ti1 65.3(2) . . ?
C12 C20 C19 108.1(3) . . ?
C12 C20 Ti1 70.2(2) . . ?
C19 C20 Ti1 81.7(2) . . ?
C12 C20 H20A 125.2 . . ?
C19 C20 H20A 125.2 . . ?
Ti1 C20 H20A 125.2 . . ?
C22 C21 C26 121.3(4) . . ?
C22 C21 C1 130.4(4) . . ?
C26 C21 C1 108.3(4) . . ?
C21 C22 C23 118.3(4) . . ?
C21 C22 H22A 120.9 . . ?
C23 C22 H22A 120.9 . . ?
C24 C23 C22 120.3(4) . . ?
C24 C23 H23A 119.9 . . ?
C22 C23 H23A 119.9 . . ?
C25 C24 C23 121.2(4) . . ?
C25 C24 H24A 119.4 . . ?
C23 C24 H24A 119.4 . . ?
C24 C25 C26 119.5(4) . . ?
C24 C25 H25A 120.2 . . ?
C26 C25 H25A 120.2 . . ?
C25 C26 C21 119.4(4) . . ?
C25 C26 C27 131.7(4) . . ?
C21 C26 C27 108.9(3) . . ?
C28 C27 C32 120.3(4) . . ?
C28 C27 C26 130.9(4) . . ?
C32 C27 C26 108.8(3) . . ?
C27 C28 C29 119.0(4) . . ?
C27 C28 H28A 120.5 . . ?
C29 C28 H28A 120.5 . . ?
C28 C29 C30 121.3(4) . . ?
C28 C29 H29A 119.3 . . ?
C30 C29 H29A 119.3 . . ?
C29 C30 C31 119.8(4) . . ?
C29 C30 H30A 120.1 . . ?
C31 C30 H30A 120.1 . . ?
C32 C31 C30 118.9(4) . . ?
C32 C31 H31A 120.5 . . ?
C30 C31 H31A 120.5 . . ?
C31 C32 C27 120.6(4) . . ?
C31 C32 C1 131.0(4) . . ?
C27 C32 C1 108.4(3) . . ?
C34 C33 C44 127.4(2) . . ?
C34 C33 C44 127.4(2) . 2_755 ?
C44 C33 C44 105.2(5) . 2_755 ?
C33 C34 C35 129.3(2) . 2_755 ?
C33 C34 C35 129.3(2) . . ?
C35 C34 C35 101.3(4) 2_755 . ?
C43 C35 C36 108.3(3) . . ?
C43 C35 C34 126.1(3) . . ?
C36 C35 C34 121.1(3) . . ?
C43 C35 Ti2 74.4(2) . . ?
C36 C35 Ti2 73.0(2) . . ?
C34 C35 Ti2 99.6(3) . . ?
C35 C36 C37 107.2(3) . . ?
C35 C36 Ti2 71.7(2) . . ?
C37 C36 Ti2 80.9(2) . . ?
C35 C36 H36A 125.5 . . ?
C37 C36 H36A 125.5 . . ?
Ti2 C36 H36A 125.5 . . ?
C38 C37 C42 120.3(4) . . ?
C38 C37 C36 131.4(4) . . ?
C42 C37 C36 108.3(3) . . ?
C38 C37 Ti2 124.2(3) . . ?
C42 C37 Ti2 75.3(2) . . ?
C36 C37 Ti2 65.2(2) . . ?
C39 C38 C37 117.6(4) . . ?
C39 C38 H38A 121.2 . . ?
C37 C38 H38A 121.2 . . ?
C38 C39 C40 122.3(4) . . ?
C38 C39 H39A 118.9 . . ?
C40 C39 H39A 118.9 . . ?
C41 C40 C39 121.5(4) . . ?
C41 C40 H40A 119.3 . . ?
C39 C40 H40A 119.3 . . ?
C40 C41 C42 117.9(4) . . ?
C40 C41 H41A 121.0 . . ?
C42 C41 H41A 121.0 . . ?
C41 C42 C37 120.3(4) . . ?
C41 C42 C43 132.7(4) . . ?
C37 C42 C43 107.0(3) . . ?
C41 C42 Ti2 127.0(3) . . ?
C37 C42 Ti2 72.5(2) . . ?
C43 C42 Ti2 65.3(2) . . ?
C35 C43 C42 108.6(3) . . ?
C35 C43 Ti2 70.7(2) . . ?
C42 C43 Ti2 81.5(2) . . ?
C35 C43 H43A 125.0 . . ?
C42 C43 H43A 125.0 . . ?
Ti2 C43 H43A 125.0 . . ?
C45 C44 C49 120.6(4) . . ?
C45 C44 C33 130.3(4) . . ?
C49 C44 C33 108.9(4) . . ?
C46 C45 C44 118.1(4) . . ?
C46 C45 H45A 120.9 . . ?
C44 C45 H45A 120.9 . . ?
C47 C46 C45 121.4(4) . . ?
C47 C46 H46A 119.3 . . ?
C45 C46 H46A 119.3 . . ?
C46 C47 C48 120.5(4) . . ?
C46 C47 H47A 119.7 . . ?
C48 C47 H47A 119.7 . . ?
C47 C48 C49 119.0(4) . . ?
C47 C48 H48A 120.5 . . ?
C49 C48 H48A 120.5 . . ?
C48 C49 C44 120.2(4) . . ?
C48 C49 C49 131.4(3) . 2_755 ?
C44 C49 C49 108.4(2) . 2_755 ?
Cl4 Cl4 C54 170.2(5) 7_766 . ?
C51 C56 C53 120.0 . . ?
C51 C56 H56A 120.0 . . ?
C53 C56 H56A 120.0 . . ?
C52 C51 C56 120.0 . . ?
C52 C51 H51A 120.0 . . ?
C56 C51 H51A 120.0 . . ?
C51 C52 C55 120.0 . . ?
C51 C52 H52A 120.0 . . ?
C55 C52 H52A 120.0 . . ?
C54 C55 C52 120.0 . . ?
C54 C55 H55A 120.0 . . ?
C52 C55 H55A 120.0 . . ?
C53 C54 C55 120.0 . . ?
C53 C54 Cl4 121.3(6) . . ?
C55 C54 Cl4 118.7(6) . . ?
C54 C53 C56 120.0 . . ?
C54 C53 H53A 120.0 . . ?
C56 C53 H53A 120.0 . . ?
C61 C66 C63 120.0 . . ?
C61 C66 H66A 120.0 . . ?
C63 C66 H66A 120.0 . . ?
C62 C61 C66 120.0 . . ?
C62 C61 Cl5 124.1(5) . . ?
C66 C61 Cl5 115.8(5) . . ?
C65 C62 C61 120.0 . . ?
C65 C62 H62A 120.0 . . ?
C61 C62 H62A 120.0 . . ?
C62 C65 C64 120.0 . . ?
C62 C65 H65A 120.0 . . ?
C64 C65 H65A 120.0 . . ?
C65 C64 C63 120.0 . . ?
C65 C64 H64A 120.0 . . ?
C63 C64 H64A 120.0 . . ?
C64 C63 C66 120.0 . . ?
C64 C63 H63A 120.0 . . ?
C66 C63 H63A 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C32 C1 C2 C3 -0.2(7) . . . . ?
C21 C1 C2 C3 177.5(4) . . . . ?
C32 C1 C2 C12 -174.3(4) . . . . ?
C21 C1 C2 C12 3.4(7) . . . . ?
C1 C2 C3 C11 -98.8(5) . . . . ?
C12 C2 C3 C11 76.5(4) . . . . ?
C1 C2 C3 C4 106.9(5) . . . . ?
C12 C2 C3 C4 -77.8(5) . . . . ?
C1 C2 C3 Ti1 -175.1(4) . . . . ?
C12 C2 C3 Ti1 0.2(3) . . . . ?
Cl2 Ti1 C3 C11 125.8(2) . . . . ?
Cl1 Ti1 C3 C11 -7.9(3) . . . . ?
C12 Ti1 C3 C11 -122.2(3) . . . . ?
C13 Ti1 C3 C11 -151.4(3) . . . . ?
C4 Ti1 C3 C11 115.3(3) . . . . ?
C20 Ti1 C3 C11 -92.8(2) . . . . ?
C14 Ti1 C3 C11 -138.5(2) . . . . ?
C10 Ti1 C3 C11 38.6(2) . . . . ?
C5 Ti1 C3 C11 77.5(2) . . . . ?
C19 Ti1 C3 C11 -103.7(2) . . . . ?
Cl2 Ti1 C3 C4 10.6(3) . . . . ?
Cl1 Ti1 C3 C4 -123.2(2) . . . . ?
C12 Ti1 C3 C4 122.5(3) . . . . ?
C13 Ti1 C3 C4 93.4(2) . . . . ?
C11 Ti1 C3 C4 -115.3(3) . . . . ?
C20 Ti1 C3 C4 151.9(3) . . . . ?
C14 Ti1 C3 C4 106.3(2) . . . . ?
C10 Ti1 C3 C4 -76.7(2) . . . . ?
C5 Ti1 C3 C4 -37.8(2) . . . . ?
C19 Ti1 C3 C4 141.0(2) . . . . ?
Cl2 Ti1 C3 C2 -112.1(2) . . . . ?
Cl1 Ti1 C3 C2 114.2(2) . . . . ?
C12 Ti1 C3 C2 -0.2(2) . . . . ?
C13 Ti1 C3 C2 -29.3(2) . . . . ?
C11 Ti1 C3 C2 122.1(4) . . . . ?
C4 Ti1 C3 C2 -122.7(4) . . . . ?
C20 Ti1 C3 C2 29.2(2) . . . . ?
C14 Ti1 C3 C2 -16.4(3) . . . . ?
C10 Ti1 C3 C2 160.7(3) . . . . ?
C5 Ti1 C3 C2 -160.4(3) . . . . ?
C19 Ti1 C3 C2 18.4(3) . . . . ?
C11 C3 C4 C5 6.9(5) . . . . ?
C2 C3 C4 C5 164.3(4) . . . . ?
Ti1 C3 C4 C5 73.3(3) . . . . ?
C11 C3 C4 Ti1 -66.4(3) . . . . ?
C2 C3 C4 Ti1 91.0(4) . . . . ?
Cl2 Ti1 C4 C3 -171.1(2) . . . . ?
Cl1 Ti1 C4 C3 87.1(3) . . . . ?
C12 Ti1 C4 C3 -47.6(2) . . . . ?
C13 Ti1 C4 C3 -82.9(2) . . . . ?
C11 Ti1 C4 C3 37.8(2) . . . . ?
C20 Ti1 C4 C3 -30.1(3) . . . . ?
C14 Ti1 C4 C3 -91.3(3) . . . . ?
C10 Ti1 C4 C3 78.6(2) . . . . ?
C5 Ti1 C4 C3 112.8(3) . . . . ?
C19 Ti1 C4 C3 -57.3(3) . . . . ?
Cl2 Ti1 C4 C5 76.1(2) . . . . ?
Cl1 Ti1 C4 C5 -25.7(3) . . . . ?
C3 Ti1 C4 C5 -112.8(3) . . . . ?
C12 Ti1 C4 C5 -160.4(2) . . . . ?
C13 Ti1 C4 C5 164.3(2) . . . . ?
C11 Ti1 C4 C5 -75.0(2) . . . . ?
C20 Ti1 C4 C5 -142.9(2) . . . . ?
C14 Ti1 C4 C5 155.9(2) . . . . ?
C10 Ti1 C4 C5 -34.3(2) . . . . ?
C19 Ti1 C4 C5 -170.1(2) . . . . ?
C3 C4 C5 C10 -4.8(4) . . . . ?
Ti1 C4 C5 C10 60.8(3) . . . . ?
C3 C4 C5 C6 175.9(4) . . . . ?
Ti1 C4 C5 C6 -118.5(4) . . . . ?
C3 C4 C5 Ti1 -65.6(3) . . . . ?
Cl2 Ti1 C5 C10 140.2(2) . . . . ?
Cl1 Ti1 C5 C10 43.0(2) . . . . ?
C3 Ti1 C5 C10 -79.4(2) . . . . ?
C12 Ti1 C5 C10 -97.9(2) . . . . ?
C13 Ti1 C5 C10 -136.7(2) . . . . ?
C11 Ti1 C5 C10 -36.6(2) . . . . ?
C4 Ti1 C5 C10 -119.0(3) . . . . ?
C20 Ti1 C5 C10 -65.6(3) . . . . ?
C14 Ti1 C5 C10 -160.3(2) . . . . ?
C19 Ti1 C5 C10 -84.6(6) . . . . ?
Cl2 Ti1 C5 C6 23.6(3) . . . . ?
Cl1 Ti1 C5 C6 -73.6(4) . . . . ?
C3 Ti1 C5 C6 164.1(4) . . . . ?
C12 Ti1 C5 C6 145.5(3) . . . . ?
C13 Ti1 C5 C6 106.7(4) . . . . ?
C11 Ti1 C5 C6 -153.2(4) . . . . ?
C4 Ti1 C5 C6 124.4(5) . . . . ?
C20 Ti1 C5 C6 177.8(3) . . . . ?
C14 Ti1 C5 C6 83.1(4) . . . . ?
C10 Ti1 C5 C6 -116.6(5) . . . . ?
C19 Ti1 C5 C6 158.8(5) . . . . ?
Cl2 Ti1 C5 C4 -100.8(2) . . . . ?
Cl1 Ti1 C5 C4 162.0(2) . . . . ?
C3 Ti1 C5 C4 39.7(2) . . . . ?
C12 Ti1 C5 C4 21.1(3) . . . . ?
C13 Ti1 C5 C4 -17.7(3) . . . . ?
C11 Ti1 C5 C4 82.4(2) . . . . ?
C20 Ti1 C5 C4 53.4(3) . . . . ?
C14 Ti1 C5 C4 -41.3(3) . . . . ?
C10 Ti1 C5 C4 119.0(3) . . . . ?
C19 Ti1 C5 C4 34.4(7) . . . . ?
C10 C5 C6 C7 -0.4(6) . . . . ?
C4 C5 C6 C7 178.8(4) . . . . ?
Ti1 C5 C6 C7 90.6(5) . . . . ?
C5 C6 C7 C8 -1.3(6) . . . . ?
C6 C7 C8 C9 2.1(7) . . . . ?
C7 C8 C9 C10 -1.0(6) . . . . ?
C6 C5 C10 C9 1.5(6) . . . . ?
C4 C5 C10 C9 -177.9(4) . . . . ?
Ti1 C5 C10 C9 -121.5(4) . . . . ?
C6 C5 C10 C11 -179.5(4) . . . . ?
C4 C5 C10 C11 1.1(4) . . . . ?
Ti1 C5 C10 C11 57.5(3) . . . . ?
C6 C5 C10 Ti1 123.0(4) . . . . ?
C4 C5 C10 Ti1 -56.4(3) . . . . ?
C8 C9 C10 C5 -0.7(6) . . . . ?
C8 C9 C10 C11 -179.4(4) . . . . ?
C8 C9 C10 Ti1 -92.6(4) . . . . ?
Cl2 Ti1 C10 C5 -41.0(2) . . . . ?
Cl1 Ti1 C10 C5 -138.5(2) . . . . ?
C3 Ti1 C10 C5 78.2(2) . . . . ?
C12 Ti1 C10 C5 96.3(2) . . . . ?
C13 Ti1 C10 C5 63.5(3) . . . . ?
C11 Ti1 C10 C5 118.1(3) . . . . ?
C4 Ti1 C10 C5 35.6(2) . . . . ?
C20 Ti1 C10 C5 134.4(2) . . . . ?
C14 Ti1 C10 C5 92.9(7) . . . . ?
C19 Ti1 C10 C5 158.6(2) . . . . ?
Cl2 Ti1 C10 C9 74.5(3) . . . . ?
Cl1 Ti1 C10 C9 -23.0(3) . . . . ?
C3 Ti1 C10 C9 -166.3(4) . . . . ?
C12 Ti1 C10 C9 -148.2(3) . . . . ?
C13 Ti1 C10 C9 179.1(3) . . . . ?
C11 Ti1 C10 C9 -126.4(4) . . . . ?
C4 Ti1 C10 C9 151.2(4) . . . . ?
C20 Ti1 C10 C9 -110.0(3) . . . . ?
C14 Ti1 C10 C9 -151.6(6) . . . . ?
C5 Ti1 C10 C9 115.5(4) . . . . ?
C19 Ti1 C10 C9 -85.9(4) . . . . ?
Cl2 Ti1 C10 C11 -159.2(2) . . . . ?
Cl1 Ti1 C10 C11 103.4(2) . . . . ?
C3 Ti1 C10 C11 -39.9(2) . . . . ?
C12 Ti1 C10 C11 -21.9(3) . . . . ?
C13 Ti1 C10 C11 -54.6(3) . . . . ?
C4 Ti1 C10 C11 -82.5(3) . . . . ?
C20 Ti1 C10 C11 16.3(3) . . . . ?
C14 Ti1 C10 C11 -25.2(8) . . . . ?
C5 Ti1 C10 C11 -118.1(3) . . . . ?
C19 Ti1 C10 C11 40.5(3) . . . . ?
C4 C3 C11 C10 -6.1(5) . . . . ?
C2 C3 C11 C10 -163.8(4) . . . . ?
Ti1 C3 C11 C10 -73.6(3) . . . . ?
C4 C3 C11 Ti1 67.4(3) . . . . ?
C2 C3 C11 Ti1 -90.2(4) . . . . ?
C5 C10 C11 C3 3.1(5) . . . . ?
C9 C10 C11 C3 -178.1(4) . . . . ?
Ti1 C10 C11 C3 67.1(3) . . . . ?
C5 C10 C11 Ti1 -64.0(3) . . . . ?
C9 C10 C11 Ti1 114.8(5) . . . . ?
Cl2 Ti1 C11 C3 -82.2(3) . . . . ?
Cl1 Ti1 C11 C3 173.6(2) . . . . ?
C12 Ti1 C11 C3 47.8(2) . . . . ?
C13 Ti1 C11 C3 31.0(3) . . . . ?
C4 Ti1 C11 C3 -37.6(2) . . . . ?
C20 Ti1 C11 C3 82.6(2) . . . . ?
C14 Ti1 C11 C3 61.5(3) . . . . ?
C10 Ti1 C11 C3 -112.0(3) . . . . ?
C5 Ti1 C11 C3 -77.5(3) . . . . ?
C19 Ti1 C11 C3 92.5(3) . . . . ?
Cl2 Ti1 C11 C10 29.8(3) . . . . ?
Cl1 Ti1 C11 C10 -74.4(2) . . . . ?
C3 Ti1 C11 C10 112.0(3) . . . . ?
C12 Ti1 C11 C10 159.8(3) . . . . ?
C13 Ti1 C11 C10 143.1(2) . . . . ?
C4 Ti1 C11 C10 74.4(2) . . . . ?
C20 Ti1 C11 C10 -165.4(2) . . . . ?
C14 Ti1 C11 C10 173.5(2) . . . . ?
C5 Ti1 C11 C10 34.5(2) . . . . ?
C19 Ti1 C11 C10 -155.5(2) . . . . ?
C1 C2 C12 C20 97.2(5) . . . . ?
C3 C2 C12 C20 -78.1(4) . . . . ?
C1 C2 C12 C13 -110.0(5) . . . . ?
C3 C2 C12 C13 74.7(4) . . . . ?
C1 C2 C12 Ti1 175.1(4) . . . . ?
C3 C2 C12 Ti1 -0.2(3) . . . . ?
Cl2 Ti1 C12 C20 -127.0(2) . . . . ?
Cl1 Ti1 C12 C20 7.0(3) . . . . ?
C3 Ti1 C12 C20 121.3(3) . . . . ?
C13 Ti1 C12 C20 -115.5(3) . . . . ?
C11 Ti1 C12 C20 91.9(2) . . . . ?
C4 Ti1 C12 C20 150.4(2) . . . . ?
C14 Ti1 C12 C20 -76.7(2) . . . . ?
C10 Ti1 C12 C20 104.0(2) . . . . ?
C5 Ti1 C12 C20 138.9(2) . . . . ?
C19 Ti1 C12 C20 -37.7(2) . . . . ?
Cl2 Ti1 C12 C13 -11.5(3) . . . . ?
Cl1 Ti1 C12 C13 122.5(2) . . . . ?
C3 Ti1 C12 C13 -123.2(3) . . . . ?
C11 Ti1 C12 C13 -152.6(3) . . . . ?
C4 Ti1 C12 C13 -94.1(2) . . . . ?
C20 Ti1 C12 C13 115.5(3) . . . . ?
C14 Ti1 C12 C13 38.8(2) . . . . ?
C10 Ti1 C12 C13 -140.5(2) . . . . ?
C5 Ti1 C12 C13 -105.6(2) . . . . ?
C19 Ti1 C12 C13 77.8(3) . . . . ?
Cl2 Ti1 C12 C2 111.9(2) . . . . ?
Cl1 Ti1 C12 C2 -114.1(2) . . . . ?
C3 Ti1 C12 C2 0.2(2) . . . . ?
C13 Ti1 C12 C2 123.4(4) . . . . ?
C11 Ti1 C12 C2 -29.2(2) . . . . ?
C4 Ti1 C12 C2 29.3(2) . . . . ?
C20 Ti1 C12 C2 -121.1(3) . . . . ?
C14 Ti1 C12 C2 162.2(3) . . . . ?
C10 Ti1 C12 C2 -17.1(3) . . . . ?
C5 Ti1 C12 C2 17.8(3) . . . . ?
C19 Ti1 C12 C2 -158.8(3) . . . . ?
C20 C12 C13 C14 -7.0(4) . . . . ?
C2 C12 C13 C14 -162.9(3) . . . . ?
Ti1 C12 C13 C14 -74.2(3) . . . . ?
C20 C12 C13 Ti1 67.2(3) . . . . ?
C2 C12 C13 Ti1 -88.7(3) . . . . ?
Cl2 Ti1 C13 C12 170.4(2) . . . . ?
Cl1 Ti1 C13 C12 -88.1(3) . . . . ?
C3 Ti1 C13 C12 47.0(2) . . . . ?
C11 Ti1 C13 C12 29.7(3) . . . . ?
C4 Ti1 C13 C12 81.9(2) . . . . ?
C20 Ti1 C13 C12 -37.2(2) . . . . ?
C14 Ti1 C13 C12 -111.5(3) . . . . ?
C10 Ti1 C13 C12 59.2(3) . . . . ?
C5 Ti1 C13 C12 91.5(3) . . . . ?
C19 Ti1 C13 C12 -76.9(2) . . . . ?
Cl2 Ti1 C13 C14 -78.2(2) . . . . ?
Cl1 Ti1 C13 C14 23.4(3) . . . . ?
C3 Ti1 C13 C14 158.5(2) . . . . ?
C12 Ti1 C13 C14 111.5(3) . . . . ?
C11 Ti1 C13 C14 141.1(2) . . . . ?
C4 Ti1 C13 C14 -166.6(2) . . . . ?
C20 Ti1 C13 C14 74.3(2) . . . . ?
C10 Ti1 C13 C14 170.7(2) . . . . ?
C5 Ti1 C13 C14 -157.0(2) . . . . ?
C19 Ti1 C13 C14 34.6(2) . . . . ?
C12 C13 C14 C15 -177.4(4) . . . . ?
Ti1 C13 C14 C15 114.7(4) . . . . ?
C12 C13 C14 C19 3.2(4) . . . . ?
Ti1 C13 C14 C19 -64.7(3) . . . . ?
C12 C13 C14 Ti1 67.9(3) . . . . ?
Cl2 Ti1 C14 C15 -26.1(3) . . . . ?
Cl1 Ti1 C14 C15 71.5(3) . . . . ?
C3 Ti1 C14 C15 -148.3(3) . . . . ?
C12 Ti1 C14 C15 -165.3(4) . . . . ?
C13 Ti1 C14 C15 -124.9(4) . . . . ?
C11 Ti1 C14 C15 178.3(3) . . . . ?
C4 Ti1 C14 C15 -109.7(3) . . . . ?
C20 Ti1 C14 C15 152.5(4) . . . . ?
C10 Ti1 C14 C15 -161.6(6) . . . . ?
C5 Ti1 C14 C15 -85.4(4) . . . . ?
C19 Ti1 C14 C15 117.3(4) . . . . ?
Cl2 Ti1 C14 C19 -143.3(2) . . . . ?
Cl1 Ti1 C14 C19 -45.8(2) . . . . ?
C3 Ti1 C14 C19 94.4(2) . . . . ?
C12 Ti1 C14 C19 77.4(2) . . . . ?
C13 Ti1 C14 C19 117.8(3) . . . . ?
C11 Ti1 C14 C19 61.0(3) . . . . ?
C4 Ti1 C14 C19 133.1(2) . . . . ?
C20 Ti1 C14 C19 35.2(2) . . . . ?
C10 Ti1 C14 C19 81.1(7) . . . . ?
C5 Ti1 C14 C19 157.4(2) . . . . ?
Cl2 Ti1 C14 C13 98.8(2) . . . . ?
Cl1 Ti1 C14 C13 -163.6(2) . . . . ?
C3 Ti1 C14 C13 -23.4(3) . . . . ?
C12 Ti1 C14 C13 -40.4(2) . . . . ?
C11 Ti1 C14 C13 -56.8(3) . . . . ?
C4 Ti1 C14 C13 15.2(3) . . . . ?
C20 Ti1 C14 C13 -82.6(2) . . . . ?
C10 Ti1 C14 C13 -36.7(8) . . . . ?
C5 Ti1 C14 C13 39.5(3) . . . . ?
C19 Ti1 C14 C13 -117.8(3) . . . . ?
C19 C14 C15 C16 -1.5(6) . . . . ?
C13 C14 C15 C16 179.1(4) . . . . ?
Ti1 C14 C15 C16 -95.1(4) . . . . ?
C14 C15 C16 C17 0.4(6) . . . . ?
C15 C16 C17 C18 0.7(6) . . . . ?
C16 C17 C18 C19 -0.6(6) . . . . ?
C17 C18 C19 C14 -0.6(6) . . . . ?
C17 C18 C19 C20 178.6(4) . . . . ?
C17 C18 C19 Ti1 89.0(4) . . . . ?
C15 C14 C19 C18 1.6(6) . . . . ?
C13 C14 C19 C18 -178.9(3) . . . . ?
Ti1 C14 C19 C18 123.6(3) . . . . ?
C15 C14 C19 C20 -177.8(3) . . . . ?
C13 C14 C19 C20 1.7(4) . . . . ?
Ti1 C14 C19 C20 -55.9(3) . . . . ?
C15 C14 C19 Ti1 -121.9(3) . . . . ?
C13 C14 C19 Ti1 57.6(3) . . . . ?
Cl2 Ti1 C19 C18 -76.3(4) . . . . ?
Cl1 Ti1 C19 C18 20.9(3) . . . . ?
C3 Ti1 C19 C18 145.9(3) . . . . ?
C12 Ti1 C19 C18 165.5(4) . . . . ?
C13 Ti1 C19 C18 -151.3(4) . . . . ?
C11 Ti1 C19 C18 107.6(4) . . . . ?
C4 Ti1 C19 C18 177.2(3) . . . . ?
C20 Ti1 C19 C18 125.9(5) . . . . ?
C14 Ti1 C19 C18 -114.6(4) . . . . ?
C10 Ti1 C19 C18 83.9(4) . . . . ?
C5 Ti1 C19 C18 150.6(5) . . . . ?
Cl2 Ti1 C19 C14 38.3(2) . . . . ?
Cl1 Ti1 C19 C14 135.5(2) . . . . ?
C3 Ti1 C19 C14 -99.5(2) . . . . ?
C12 Ti1 C19 C14 -79.9(2) . . . . ?
C13 Ti1 C19 C14 -36.7(2) . . . . ?
C11 Ti1 C19 C14 -137.8(2) . . . . ?
C4 Ti1 C19 C14 -68.2(3) . . . . ?
C20 Ti1 C19 C14 -119.5(3) . . . . ?
C10 Ti1 C19 C14 -161.6(2) . . . . ?
C5 Ti1 C19 C14 -94.8(6) . . . . ?
Cl2 Ti1 C19 C20 157.8(2) . . . . ?
Cl1 Ti1 C19 C20 -105.0(2) . . . . ?
C3 Ti1 C19 C20 20.0(3) . . . . ?
C12 Ti1 C19 C20 39.6(2) . . . . ?
C13 Ti1 C19 C20 82.8(3) . . . . ?
C11 Ti1 C19 C20 -18.3(3) . . . . ?
C4 Ti1 C19 C20 51.3(3) . . . . ?
C14 Ti1 C19 C20 119.5(3) . . . . ?
C10 Ti1 C19 C20 -42.0(3) . . . . ?
C5 Ti1 C19 C20 24.7(7) . . . . ?
C13 C12 C20 C19 8.2(4) . . . . ?
C2 C12 C20 C19 164.7(3) . . . . ?
Ti1 C12 C20 C19 73.8(3) . . . . ?
C13 C12 C20 Ti1 -65.6(3) . . . . ?
C2 C12 C20 Ti1 90.9(3) . . . . ?
C18 C19 C20 C12 174.6(4) . . . . ?
C14 C19 C20 C12 -6.1(4) . . . . ?
Ti1 C19 C20 C12 -65.9(3) . . . . ?
C18 C19 C20 Ti1 -119.4(4) . . . . ?
C14 C19 C20 Ti1 59.9(3) . . . . ?
Cl2 Ti1 C20 C12 80.8(3) . . . . ?
Cl1 Ti1 C20 C12 -174.3(2) . . . . ?
C3 Ti1 C20 C12 -48.6(2) . . . . ?
C13 Ti1 C20 C12 37.9(2) . . . . ?
C11 Ti1 C20 C12 -83.8(2) . . . . ?
C4 Ti1 C20 C12 -31.8(3) . . . . ?
C14 Ti1 C20 C12 78.7(2) . . . . ?
C10 Ti1 C20 C12 -92.8(2) . . . . ?
C5 Ti1 C20 C12 -60.0(3) . . . . ?
C19 Ti1 C20 C12 112.7(3) . . . . ?
Cl2 Ti1 C20 C19 -32.0(3) . . . . ?
Cl1 Ti1 C20 C19 73.0(2) . . . . ?
C3 Ti1 C20 C19 -161.3(2) . . . . ?
C12 Ti1 C20 C19 -112.7(3) . . . . ?
C13 Ti1 C20 C19 -74.8(2) . . . . ?
C11 Ti1 C20 C19 163.5(2) . . . . ?
C4 Ti1 C20 C19 -144.5(2) . . . . ?
C14 Ti1 C20 C19 -34.1(2) . . . . ?
C10 Ti1 C20 C19 154.4(2) . . . . ?
C5 Ti1 C20 C19 -172.8(2) . . . . ?
C2 C1 C21 C22 3.1(7) . . . . ?
C32 C1 C21 C22 -178.8(4) . . . . ?
C2 C1 C21 C26 -176.8(4) . . . . ?
C32 C1 C21 C26 1.3(4) . . . . ?
C26 C21 C22 C23 -0.6(6) . . . . ?
C1 C21 C22 C23 179.5(4) . . . . ?
C21 C22 C23 C24 0.1(6) . . . . ?
C22 C23 C24 C25 0.7(7) . . . . ?
C23 C24 C25 C26 -0.9(7) . . . . ?
C24 C25 C26 C21 0.4(6) . . . . ?
C24 C25 C26 C27 -179.4(4) . . . . ?
C22 C21 C26 C25 0.4(6) . . . . ?
C1 C21 C26 C25 -179.7(4) . . . . ?
C22 C21 C26 C27 -179.8(4) . . . . ?
C1 C21 C26 C27 0.1(4) . . . . ?
C25 C26 C27 C28 -3.1(8) . . . . ?
C21 C26 C27 C28 177.1(4) . . . . ?
C25 C26 C27 C32 178.1(4) . . . . ?
C21 C26 C27 C32 -1.7(4) . . . . ?
C32 C27 C28 C29 -1.0(6) . . . . ?
C26 C27 C28 C29 -179.6(4) . . . . ?
C27 C28 C29 C30 0.2(7) . . . . ?
C28 C29 C30 C31 0.2(7) . . . . ?
C29 C30 C31 C32 0.2(6) . . . . ?
C30 C31 C32 C27 -1.0(6) . . . . ?
C30 C31 C32 C1 176.2(4) . . . . ?
C28 C27 C32 C31 1.4(6) . . . . ?
C26 C27 C32 C31 -179.7(4) . . . . ?
C28 C27 C32 C1 -176.4(4) . . . . ?
C26 C27 C32 C1 2.5(4) . . . . ?
C2 C1 C32 C31 -1.7(7) . . . . ?
C21 C1 C32 C31 -179.8(4) . . . . ?
C2 C1 C32 C27 175.7(4) . . . . ?
C21 C1 C32 C27 -2.4(4) . . . . ?
C44 C33 C34 C35 172.5(3) . . . 2_755 ?
C44 C33 C34 C35 -7.5(3) 2_755 . . 2_755 ?
C44 C33 C34 C35 -7.5(3) . . . . ?
C44 C33 C34 C35 172.5(3) 2_755 . . . ?
C33 C34 C35 C43 102.4(4) . . . . ?
C35 C34 C35 C43 -77.6(4) 2_755 . . . ?
C33 C34 C35 C36 -104.2(3) . . . . ?
C35 C34 C35 C36 75.8(3) 2_755 . . . ?
C33 C34 C35 Ti2 180.0 . . . . ?
C35 C34 C35 Ti2 0.0 2_755 . . . ?
Cl3 Ti2 C35 C43 -124.8(2) 2_755 . . . ?
Cl3 Ti2 C35 C43 9.3(3) . . . . ?
C35 Ti2 C35 C43 125.0(3) 2_755 . . . ?
C36 Ti2 C35 C43 94.4(2) 2_755 . . . ?
C36 Ti2 C35 C43 -115.3(3) . . . . ?
C43 Ti2 C35 C43 153.3(2) 2_755 . . . ?
C37 Ti2 C35 C43 -76.6(2) . . . . ?
C37 Ti2 C35 C43 105.7(2) 2_755 . . . ?
C42 Ti2 C35 C43 -37.4(2) . . . . ?
C42 Ti2 C35 C43 140.7(2) 2_755 . . . ?
Cl3 Ti2 C35 C36 -9.6(3) 2_755 . . . ?
Cl3 Ti2 C35 C36 124.5(2) . . . . ?
C35 Ti2 C35 C36 -119.7(3) 2_755 . . . ?
C36 Ti2 C35 C36 -150.3(2) 2_755 . . . ?
C43 Ti2 C35 C36 115.3(3) . . . . ?
C43 Ti2 C35 C36 -91.5(2) 2_755 . . . ?
C37 Ti2 C35 C36 38.7(2) . . . . ?
C37 Ti2 C35 C36 -139.0(2) 2_755 . . . ?
C42 Ti2 C35 C36 77.8(2) . . . . ?
C42 Ti2 C35 C36 -104.0(2) 2_755 . . . ?
Cl3 Ti2 C35 C34 110.17(17) 2_755 . . . ?
Cl3 Ti2 C35 C34 -115.75(16) . . . . ?
C35 Ti2 C35 C34 0.0 2_755 . . . ?
C36 Ti2 C35 C34 -30.62(18) 2_755 . . . ?
C36 Ti2 C35 C34 119.7(3) . . . . ?
C43 Ti2 C35 C34 -125.0(3) . . . . ?
C43 Ti2 C35 C34 28.25(19) 2_755 . . . ?
C37 Ti2 C35 C34 158.4(3) . . . . ?
C37 Ti2 C35 C34 -19.3(2) 2_755 . . . ?
C42 Ti2 C35 C34 -162.4(3) . . . . ?
C42 Ti2 C35 C34 15.7(2) 2_755 . . . ?
C43 C35 C36 C37 -7.4(4) . . . . ?
C34 C35 C36 C37 -165.0(3) . . . . ?
Ti2 C35 C36 C37 -73.9(3) . . . . ?
C43 C35 C36 Ti2 66.5(3) . . . . ?
C34 C35 C36 Ti2 -91.0(3) . . . . ?
Cl3 Ti2 C36 C35 172.3(2) 2_755 . . . ?
Cl3 Ti2 C36 C35 -83.6(2) . . . . ?
C35 Ti2 C36 C35 49.4(3) 2_755 . . . ?
C36 Ti2 C36 C35 31.53(19) 2_755 . . . ?
C43 Ti2 C36 C35 -37.6(2) . . . . ?
C43 Ti2 C36 C35 84.4(2) 2_755 . . . ?
C37 Ti2 C36 C35 -111.6(3) . . . . ?
C37 Ti2 C36 C35 60.1(3) 2_755 . . . ?
C42 Ti2 C36 C35 -77.2(2) . . . . ?
C42 Ti2 C36 C35 93.0(2) 2_755 . . . ?
Cl3 Ti2 C36 C37 -76.1(2) 2_755 . . . ?
Cl3 Ti2 C36 C37 28.0(3) . . . . ?
C35 Ti2 C36 C37 111.6(3) . . . . ?
C35 Ti2 C36 C37 161.0(2) 2_755 . . . ?
C36 Ti2 C36 C37 143.1(3) 2_755 . . . ?
C43 Ti2 C36 C37 74.1(2) . . . . ?
C43 Ti2 C36 C37 -164.0(2) 2_755 . . . ?
C37 Ti2 C36 C37 171.72(15) 2_755 . . . ?
C42 Ti2 C36 C37 34.4(2) . . . . ?
C42 Ti2 C36 C37 -155.4(2) 2_755 . . . ?
C35 C36 C37 C38 -177.7(4) . . . . ?
Ti2 C36 C37 C38 114.8(4) . . . . ?
C35 C36 C37 C42 4.1(4) . . . . ?
Ti2 C36 C37 C42 -63.4(3) . . . . ?
C35 C36 C37 Ti2 67.5(3) . . . . ?
Cl3 Ti2 C37 C38 -22.3(3) 2_755 . . . ?
Cl3 Ti2 C37 C38 75.3(3) . . . . ?
C35 Ti2 C37 C38 -164.9(4) . . . . ?
C35 Ti2 C37 C38 -144.8(3) 2_755 . . . ?
C36 Ti2 C37 C38 -177.7(3) 2_755 . . . ?
C36 Ti2 C37 C38 -124.5(4) . . . . ?
C43 Ti2 C37 C38 152.5(4) . . . . ?
C43 Ti2 C37 C38 -106.6(3) 2_755 . . . ?
C37 Ti2 C37 C38 -154.3(3) 2_755 . . . ?
C42 Ti2 C37 C38 116.9(4) . . . . ?
C42 Ti2 C37 C38 -83.2(4) 2_755 . . . ?
Cl3 Ti2 C37 C42 -139.2(2) 2_755 . . . ?
Cl3 Ti2 C37 C42 -41.6(2) . . . . ?
C35 Ti2 C37 C42 78.2(2) . . . . ?
C35 Ti2 C37 C42 98.3(2) 2_755 . . . ?
C36 Ti2 C37 C42 65.4(3) 2_755 . . . ?
C36 Ti2 C37 C42 118.6(3) . . . . ?
C43 Ti2 C37 C42 35.6(2) . . . . ?
C43 Ti2 C37 C42 136.6(2) 2_755 . . . ?
C37 Ti2 C37 C42 88.8(2) 2_755 . . . ?
C42 Ti2 C37 C42 159.9(3) 2_755 . . . ?
Cl3 Ti2 C37 C36 102.2(2) 2_755 . . . ?
Cl3 Ti2 C37 C36 -160.2(2) . . . . ?
C35 Ti2 C37 C36 -40.4(2) . . . . ?
C35 Ti2 C37 C36 -20.3(3) 2_755 . . . ?
C36 Ti2 C37 C36 -53.2(4) 2_755 . . . ?
C43 Ti2 C37 C36 -83.0(2) . . . . ?
C43 Ti2 C37 C36 18.0(3) 2_755 . . . ?
C37 Ti2 C37 C36 -29.8(2) 2_755 . . . ?
C42 Ti2 C37 C36 -118.6(3) . . . . ?
C42 Ti2 C37 C36 41.3(3) 2_755 . . . ?
C42 C37 C38 C39 -3.1(6) . . . . ?
C36 C37 C38 C39 178.9(4) . . . . ?
Ti2 C37 C38 C39 -95.5(4) . . . . ?
C37 C38 C39 C40 1.5(6) . . . . ?
C38 C39 C40 C41 1.5(7) . . . . ?
C39 C40 C41 C42 -2.9(6) . . . . ?
C40 C41 C42 C37 1.3(6) . . . . ?
C40 C41 C42 C43 -179.4(4) . . . . ?
C40 C41 C42 Ti2 91.5(5) . . . . ?
C38 C37 C42 C41 1.7(6) . . . . ?
C36 C37 C42 C41 -179.8(4) . . . . ?
Ti2 C37 C42 C41 123.1(4) . . . . ?
C38 C37 C42 C43 -177.7(3) . . . . ?
C36 C37 C42 C43 0.7(4) . . . . ?
Ti2 C37 C42 C43 -56.4(3) . . . . ?
C38 C37 C42 Ti2 -121.4(4) . . . . ?
C36 C37 C42 Ti2 57.1(3) . . . . ?
Cl3 Ti2 C42 C41 -72.2(3) 2_755 . . . ?
Cl3 Ti2 C42 C41 24.1(3) . . . . ?
C35 Ti2 C42 C41 165.6(4) . . . . ?
C35 Ti2 C42 C41 149.2(3) 2_755 . . . ?
C36 Ti2 C42 C41 110.3(3) 2_755 . . . ?
C36 Ti2 C42 C41 -151.3(4) . . . . ?
C43 Ti2 C42 C41 126.1(5) . . . . ?
C43 Ti2 C42 C41 -178.7(3) 2_755 . . . ?
C37 Ti2 C42 C41 -115.1(4) . . . . ?
C37 Ti2 C42 C41 85.9(4) 2_755 . . . ?
C42 Ti2 C42 C41 157.0(3) 2_755 . . . ?
Cl3 Ti2 C42 C37 42.9(2) 2_755 . . . ?
Cl3 Ti2 C42 C37 139.3(2) . . . . ?
C35 Ti2 C42 C37 -79.2(3) . . . . ?
C35 Ti2 C42 C37 -95.7(2) 2_755 . . . ?
C36 Ti2 C42 C37 -134.6(2) 2_755 . . . ?
C36 Ti2 C42 C37 -36.2(2) . . . . ?
C43 Ti2 C42 C37 -118.8(3) . . . . ?
C43 Ti2 C42 C37 -63.6(3) 2_755 . . . ?
C37 Ti2 C42 C37 -158.9(3) 2_755 . . . ?
C42 Ti2 C42 C37 -87.9(2) 2_755 . . . ?
Cl3 Ti2 C42 C43 161.7(2) 2_755 . . . ?
Cl3 Ti2 C42 C43 -101.9(2) . . . . ?
C35 Ti2 C42 C43 39.6(2) . . . . ?
C35 Ti2 C42 C43 23.1(3) 2_755 . . . ?
C36 Ti2 C42 C43 -15.8(3) 2_755 . . . ?
C36 Ti2 C42 C43 82.6(2) . . . . ?
C43 Ti2 C42 C43 55.2(4) 2_755 . . . ?
C37 Ti2 C42 C43 118.8(3) . . . . ?
C37 Ti2 C42 C43 -40.1(3) 2_755 . . . ?
C42 Ti2 C42 C43 30.9(2) 2_755 . . . ?
C36 C35 C43 C42 8.0(5) . . . . ?
C34 C35 C43 C42 164.1(4) . . . . ?
Ti2 C35 C43 C42 73.6(3) . . . . ?
C36 C35 C43 Ti2 -65.6(3) . . . . ?
C34 C35 C43 Ti2 90.5(4) . . . . ?
C41 C42 C43 C35 175.3(4) . . . . ?
C37 C42 C43 C35 -5.3(4) . . . . ?
Ti2 C42 C43 C35 -66.2(3) . . . . ?
C41 C42 C43 Ti2 -118.5(5) . . . . ?
C37 C42 C43 Ti2 60.9(3) . . . . ?
Cl3 Ti2 C43 C35 86.4(3) 2_755 . . . ?
Cl3 Ti2 C43 C35 -172.2(2) . . . . ?
C35 Ti2 C43 C35 -45.4(3) 2_755 . . . ?
C36 Ti2 C43 C35 -80.9(2) 2_755 . . . ?
C36 Ti2 C43 C35 38.0(2) . . . . ?
C43 Ti2 C43 C35 -29.1(2) 2_755 . . . ?
C37 Ti2 C43 C35 78.6(3) . . . . ?
C37 Ti2 C43 C35 -90.9(3) 2_755 . . . ?
C42 Ti2 C43 C35 113.2(3) . . . . ?
C42 Ti2 C43 C35 -58.4(3) 2_755 . . . ?
Cl3 Ti2 C43 C42 -26.8(3) 2_755 . . . ?
Cl3 Ti2 C43 C42 74.6(2) . . . . ?
C35 Ti2 C43 C42 -113.2(3) . . . . ?
C35 Ti2 C43 C42 -158.6(2) 2_755 . . . ?
C36 Ti2 C43 C42 165.9(2) 2_755 . . . ?
C36 Ti2 C43 C42 -75.2(2) . . . . ?
C43 Ti2 C43 C42 -142.3(3) 2_755 . . . ?
C37 Ti2 C43 C42 -34.6(2) . . . . ?
C37 Ti2 C43 C42 155.9(2) 2_755 . . . ?
C42 Ti2 C43 C42 -171.62(15) 2_755 . . . ?
C34 C33 C44 C45 -1.9(5) . . . . ?
C44 C33 C44 C45 178.1(5) 2_755 . . . ?
C34 C33 C44 C49 -178.37(19) . . . . ?
C44 C33 C44 C49 1.63(19) 2_755 . . . ?
C49 C44 C45 C46 0.9(6) . . . . ?
C33 C44 C45 C46 -175.3(3) . . . . ?
C44 C45 C46 C47 2.1(6) . . . . ?
C45 C46 C47 C48 -3.0(6) . . . . ?
C46 C47 C48 C49 0.8(6) . . . . ?
C47 C48 C49 C44 2.1(6) . . . . ?
C47 C48 C49 C49 179.7(5) . . . 2_755 ?
C45 C44 C49 C48 -3.0(6) . . . . ?
C33 C44 C49 C48 173.9(3) . . . . ?
C45 C44 C49 C49 178.9(4) . . . 2_755 ?
C33 C44 C49 C49 -4.2(5) . . . 2_755 ?
C53 C56 C51 C52 0.0 . . . . ?
C56 C51 C52 C55 0.0 . . . . ?
C51 C52 C55 C54 0.0 . . . . ?
C52 C55 C54 C53 0.0 . . . . ?
C52 C55 C54 Cl4 177.9(7) . . . . ?
Cl4 Cl4 C54 C53 66(3) 7_766 . . . ?
Cl4 Cl4 C54 C55 -112(3) 7_766 . . . ?
C55 C54 C53 C56 0.0 . . . . ?
Cl4 C54 C53 C56 -177.9(8) . . . . ?
C51 C56 C53 C54 0.0 . . . . ?
C63 C66 C61 C62 0.0 . . . . ?
C63 C66 C61 Cl5 -176.3(7) . . . . ?
C66 C61 C62 C65 0.0 . . . . ?
Cl5 C61 C62 C65 176.0(8) . . . . ?
C61 C62 C65 C64 0.0 . . . . ?
C62 C65 C64 C63 0.0 . . . . ?
C65 C64 C63 C66 0.0 . . . . ?
C61 C66 C63 C64 0.0 . . . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        27.76
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.096
_database_code_depnum_ccdc_archive 'CCDC 1003250'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_jgmm015_0m_Compound_9b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H26 Cl2 Zr'
_chemical_formula_weight         644.71

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   10.2021(9)
_cell_length_b                   9.6547(8)
_cell_length_c                   30.541(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3008.2(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       blocks
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1312
_exptl_absorpt_coefficient_mu    0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4831
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19014
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_av_sigmaI/netI    0.0827
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.33
_diffrn_reflns_theta_max         27.52
_reflns_number_total             3661
_reflns_number_gt                2572
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0388P)²+18.5417P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3661
_refine_ls_number_parameters     211
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0623
_refine_ls_wR_factor_ref         0.1525
_refine_ls_wR_factor_gt          0.1416
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_restrained_S_all      0.964
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.67303(6) 0.2500 0.37844(2) 0.02125(18) Uani 1 2 d S . .
Cl1 Cl 0.73323(12) 0.05359(18) 0.33425(4) 0.0417(4) Uani 1 1 d . . .
C1 C 0.4970(6) 0.2500 0.5094(2) 0.0207(14) Uani 1 2 d S . .
C2 C 0.5492(6) 0.2500 0.4697(2) 0.0217(14) Uani 1 2 d S . .
C3 C 0.6936(6) 0.2500 0.4584(2) 0.0221(14) Uani 1 2 d S . .
C4 C 0.7617(4) 0.1298(6) 0.44382(14) 0.0234(10) Uani 1 1 d . . .
H4A H 0.7417 0.0324 0.4527 0.028 Uiso 1 1 calc R . .
C5 C 0.8810(4) 0.1763(6) 0.42343(15) 0.0299(12) Uani 1 1 d . . .
C6 C 0.9866(5) 0.1024(8) 0.40399(17) 0.0413(15) Uani 1 1 d . . .
H6A H 0.9868 0.0040 0.4034 0.050 Uiso 1 1 calc R . .
C7 C 1.0873(5) 0.1758(7) 0.38619(18) 0.0463(17) Uani 1 1 d . . .
H7A H 1.1591 0.1276 0.3735 0.056 Uiso 1 1 calc R . .
C8 C 0.4811(6) 0.2500 0.4265(2) 0.0212(14) Uani 1 2 d S . .
C9 C 0.4687(4) 0.1294(6) 0.39977(14) 0.0224(10) Uani 1 1 d . . .
H9A H 0.4624 0.0319 0.4106 0.027 Uiso 1 1 calc R . .
C10 C 0.4350(4) 0.1765(5) 0.35602(15) 0.0232(10) Uani 1 1 d . . .
C11 C 0.4069(4) 0.1030(6) 0.31719(16) 0.0297(12) Uani 1 1 d . . .
H11A H 0.4081 0.0046 0.3168 0.036 Uiso 1 1 calc R . .
C12 C 0.3781(5) 0.1761(6) 0.28031(16) 0.0322(13) Uani 1 1 d . . .
H12A H 0.3576 0.1278 0.2541 0.039 Uiso 1 1 calc R . .
C13 C 0.5656(6) 0.2500 0.5524(2) 0.0226(14) Uani 1 2 d S . .
C14 C 0.6996(6) 0.2500 0.5622(2) 0.0319(18) Uani 1 2 d S . .
H14A H 0.7636 0.2500 0.5396 0.038 Uiso 1 2 calc SR . .
C15 C 0.7360(7) 0.2500 0.6061(2) 0.0368(19) Uani 1 2 d S . .
H15A H 0.8265 0.2500 0.6135 0.044 Uiso 1 2 calc SR . .
C16 C 0.6440(7) 0.2500 0.6394(2) 0.0347(18) Uani 1 2 d S . .
H16A H 0.6720 0.2500 0.6690 0.042 Uiso 1 2 calc SR . .
C17 C 0.5109(7) 0.2500 0.6297(2) 0.0295(17) Uani 1 2 d S . .
H17A H 0.4472 0.2500 0.6524 0.035 Uiso 1 2 calc SR . .
C18 C 0.4736(6) 0.2500 0.5861(2) 0.0202(14) Uani 1 2 d S . .
C19 C 0.3414(7) 0.2500 0.5663(2) 0.0245(15) Uani 1 2 d S . .
C20 C 0.2185(7) 0.2500 0.5855(2) 0.0331(18) Uani 1 2 d S . .
H20A H 0.2091 0.2500 0.6164 0.040 Uiso 1 2 calc SR . .
C21 C 0.1099(7) 0.2500 0.5586(3) 0.043(2) Uani 1 2 d S . .
H21A H 0.0250 0.2500 0.5713 0.052 Uiso 1 2 calc SR . .
C22 C 0.1220(7) 0.2500 0.5136(3) 0.044(2) Uani 1 2 d S . .
H22A H 0.0454 0.2500 0.4959 0.053 Uiso 1 2 calc SR . .
C23 C 0.2444(7) 0.2500 0.4938(2) 0.0341(19) Uani 1 2 d S . .
H23A H 0.2524 0.2500 0.4629 0.041 Uiso 1 2 calc SR . .
C24 C 0.3550(6) 0.2500 0.5203(2) 0.0221(14) Uani 1 2 d S . .
C25 C 0.9915(6) 0.1798(8) 0.6932(2) 0.070(3) Uani 1 1 d D . .
H25A H 1.0500 0.1305 0.6747 0.084 Uiso 1 1 calc R . .
C26 C 0.9071(7) 0.1096(7) 0.7198(3) 0.082(3) Uani 1 1 d D . .
H26A H 0.9063 0.0112 0.7202 0.098 Uiso 1 1 calc R . .
C27 C 0.8241(7) 0.1828(8) 0.7459(2) 0.079(3) Uani 1 1 d D . .
H27A H 0.7649 0.1346 0.7644 0.095 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 Cl1 2.4071(15) 7_565 ?
Zr1 Cl1 2.4071(15) . ?
Zr1 C8 2.448(6) . ?
Zr1 C3 2.451(6) . ?
Zr1 C9 2.475(4) 7_565 ?
Zr1 C9 2.475(4) . ?
Zr1 C4 2.480(5) . ?
Zr1 C4 2.480(5) 7_565 ?
Zr1 C10 2.621(4) 7_565 ?
Zr1 C10 2.621(4) . ?
Zr1 C5 2.626(5) 7_565 ?
Zr1 C5 2.626(5) . ?
C1 C2 1.324(9) . ?
C1 C24 1.487(8) . ?
C1 C13 1.487(9) . ?
C2 C8 1.492(9) . ?
C2 C3 1.514(8) . ?
C3 C4 1.424(6) 7_565 ?
C3 C4 1.424(6) . ?
C4 C5 1.439(6) . ?
C5 C5 1.423(12) 7_565 ?
C5 C6 1.422(7) . ?
C6 C7 1.362(8) . ?
C7 C7 1.433(14) 7_565 ?
C8 C9 1.428(6) . ?
C8 C9 1.428(6) 7_565 ?
C9 C10 1.452(6) . ?
C10 C10 1.419(10) 7_565 ?
C10 C11 1.412(7) . ?
C11 C12 1.361(7) . ?
C12 C12 1.427(11) 7_565 ?
C13 C18 1.393(9) . ?
C13 C14 1.399(9) . ?
C14 C15 1.393(10) . ?
C15 C16 1.382(10) . ?
C16 C17 1.390(10) . ?
C17 C18 1.385(9) . ?
C18 C19 1.478(9) . ?
C19 C20 1.384(9) . ?
C19 C24 1.410(9) . ?
C20 C21 1.379(10) . ?
C21 C22 1.378(11) . ?
C22 C23 1.387(10) . ?
C23 C24 1.388(9) . ?
C25 C26 1.365(8) . ?
C25 C25 1.355(16) 7_565 ?
C26 C27 1.360(8) . ?
C27 C27 1.297(16) 7_565 ?

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
Cl1 Zr1 Cl1 103.96(8) 7_565 . ?
Cl1 Zr1 C8 122.71(6) 7_565 . ?
Cl1 Zr1 C8 122.71(7) . . ?
Cl1 Zr1 C3 122.46(6) 7_565 . ?
Cl1 Zr1 C3 122.46(6) . . ?
C8 Zr1 C3 58.1(2) . . ?
Cl1 Zr1 C9 89.53(12) 7_565 7_565 ?
Cl1 Zr1 C9 137.14(12) . 7_565 ?
C8 Zr1 C9 33.72(13) . 7_565 ?
C3 Zr1 C9 79.05(16) . 7_565 ?
Cl1 Zr1 C9 137.14(12) 7_565 . ?
Cl1 Zr1 C9 89.53(12) . . ?
C8 Zr1 C9 33.72(13) . . ?
C3 Zr1 C9 79.05(16) . . ?
C9 Zr1 C9 56.1(2) 7_565 . ?
Cl1 Zr1 C4 136.62(12) 7_565 . ?
Cl1 Zr1 C4 89.41(12) . . ?
C8 Zr1 C4 78.99(16) . . ?
C3 Zr1 C4 33.55(13) . . ?
C9 Zr1 C4 108.39(15) 7_565 . ?
C9 Zr1 C4 82.84(15) . . ?
Cl1 Zr1 C4 89.41(12) 7_565 7_565 ?
Cl1 Zr1 C4 136.62(12) . 7_565 ?
C8 Zr1 C4 78.99(16) . 7_565 ?
C3 Zr1 C4 33.55(13) . 7_565 ?
C9 Zr1 C4 82.84(15) 7_565 7_565 ?
C9 Zr1 C4 108.39(15) . 7_565 ?
C4 Zr1 C4 55.8(2) . 7_565 ?
Cl1 Zr1 C10 82.92(11) 7_565 7_565 ?
Cl1 Zr1 C10 107.65(11) . 7_565 ?
C8 Zr1 C10 54.22(16) . 7_565 ?
C3 Zr1 C10 109.85(17) . 7_565 ?
C9 Zr1 C10 32.96(14) 7_565 7_565 ?
C9 Zr1 C10 54.24(15) . 7_565 ?
C4 Zr1 C10 132.44(14) . 7_565 ?
C4 Zr1 C10 114.94(15) 7_565 7_565 ?
Cl1 Zr1 C10 107.65(11) 7_565 . ?
Cl1 Zr1 C10 82.92(11) . . ?
C8 Zr1 C10 54.22(16) . . ?
C3 Zr1 C10 109.85(17) . . ?
C9 Zr1 C10 54.24(16) 7_565 . ?
C9 Zr1 C10 32.96(14) . . ?
C4 Zr1 C10 114.94(15) . . ?
C4 Zr1 C10 132.44(14) 7_565 . ?
C10 Zr1 C10 31.4(2) 7_565 . ?
Cl1 Zr1 C5 82.74(12) 7_565 7_565 ?
Cl1 Zr1 C5 107.49(12) . 7_565 ?
C8 Zr1 C5 109.43(17) . 7_565 ?
C3 Zr1 C5 53.81(17) . 7_565 ?
C9 Zr1 C5 114.55(16) 7_565 7_565 ?
C9 Zr1 C5 132.10(15) . 7_565 ?
C4 Zr1 C5 53.90(16) . 7_565 ?
C4 Zr1 C5 32.58(14) 7_565 7_565 ?
C10 Zr1 C5 144.29(16) 7_565 7_565 ?
C10 Zr1 C5 163.47(14) . 7_565 ?
Cl1 Zr1 C5 107.49(12) 7_565 . ?
Cl1 Zr1 C5 82.74(12) . . ?
C8 Zr1 C5 109.43(17) . . ?
C3 Zr1 C5 53.81(17) . . ?
C9 Zr1 C5 132.10(15) 7_565 . ?
C9 Zr1 C5 114.55(16) . . ?
C4 Zr1 C5 32.58(14) . . ?
C4 Zr1 C5 53.90(16) 7_565 . ?
C10 Zr1 C5 163.47(14) 7_565 . ?
C10 Zr1 C5 144.29(16) . . ?
C5 Zr1 C5 31.4(3) 7_565 . ?
C2 C1 C24 126.6(6) . . ?
C2 C1 C13 128.3(6) . . ?
C24 C1 C13 105.1(5) . . ?
C1 C2 C8 128.5(6) . . ?
C1 C2 C3 126.9(6) . . ?
C8 C2 C3 104.5(5) . . ?
C4 C3 C4 109.2(6) 7_565 . ?
C4 C3 C2 123.1(3) 7_565 . ?
C4 C3 C2 123.1(3) . . ?
C4 C3 Zr1 74.4(3) 7_565 . ?
C4 C3 Zr1 74.4(3) . . ?
C2 C3 Zr1 98.3(4) . . ?
C3 C4 C5 107.1(5) . . ?
C3 C4 Zr1 72.1(3) . . ?
C5 C4 Zr1 79.3(3) . . ?
C5 C5 C6 120.1(4) 7_565 . ?
C5 C5 C4 108.2(3) 7_565 . ?
C6 C5 C4 131.7(6) . . ?
C5 C5 Zr1 74.28(12) 7_565 . ?
C6 C5 Zr1 122.0(3) . . ?
C4 C5 Zr1 68.1(2) . . ?
C7 C6 C5 118.5(6) . . ?
C6 C7 C7 121.4(4) . 7_565 ?
C9 C8 C9 109.2(6) . 7_565 ?
C9 C8 C2 123.2(3) . . ?
C9 C8 C2 123.2(3) 7_565 . ?
C9 C8 Zr1 74.2(3) . . ?
C9 C8 Zr1 74.2(3) 7_565 . ?
C2 C8 Zr1 99.1(4) . . ?
C8 C9 C10 107.0(4) . . ?
C8 C9 Zr1 72.1(3) . . ?
C10 C9 Zr1 79.1(3) . . ?
C10 C10 C11 120.2(3) 7_565 . ?
C10 C10 C9 108.2(3) 7_565 . ?
C11 C10 C9 131.6(5) . . ?
C10 C10 Zr1 74.30(11) 7_565 . ?
C11 C10 Zr1 122.9(3) . . ?
C9 C10 Zr1 68.0(2) . . ?
C12 C11 C10 118.6(5) . . ?
C11 C12 C12 121.2(3) . 7_565 ?
C18 C13 C14 120.0(6) . . ?
C18 C13 C1 109.6(6) . . ?
C14 C13 C1 130.4(6) . . ?
C15 C14 C13 117.8(7) . . ?
C16 C15 C14 121.8(7) . . ?
C15 C16 C17 120.5(7) . . ?
C18 C17 C16 118.2(7) . . ?
C17 C18 C13 121.7(6) . . ?
C17 C18 C19 130.1(6) . . ?
C13 C18 C19 108.2(5) . . ?
C20 C19 C24 120.7(6) . . ?
C20 C19 C18 130.8(6) . . ?
C24 C19 C18 108.5(6) . . ?
C19 C20 C21 118.4(7) . . ?
C22 C21 C20 121.4(7) . . ?
C21 C22 C23 121.0(7) . . ?
C22 C23 C24 118.5(7) . . ?
C23 C24 C19 120.0(6) . . ?
C23 C24 C1 131.4(6) . . ?
C19 C24 C1 108.6(6) . . ?
C26 C25 C25 119.8(5) . 7_565 ?
C25 C26 C27 118.9(7) . . ?
C26 C27 C27 121.3(5) . 7_565 ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.527
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.103
_database_code_depnum_ccdc_archive 'CCDC 1003251'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_jgmm016_0m_compound_10a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C33 H24 Cl4 Ti'
_chemical_formula_weight         610.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1722(9)
_cell_length_b                   10.6755(10)
_cell_length_c                   13.8213(11)
_cell_angle_alpha                83.362(4)
_cell_angle_beta                 72.459(4)
_cell_angle_gamma                72.561(4)
_cell_volume                     1364.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       blocks
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.8390
_exptl_absorpt_correction_T_max  0.8390
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24287
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         27.44
_reflns_number_total             6044
_reflns_number_gt                4845
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0394P)²+0.7071P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6044
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.1001
_refine_ls_wR_factor_gt          0.0938
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.29011(4) 0.31950(3) 0.31740(3) 0.01705(10) Uani 1 1 d . . .
Cl1 Cl 0.15389(5) 0.29397(5) 0.48168(4) 0.02906(14) Uani 1 1 d . . .
Cl2 Cl 0.34969(6) 0.10514(5) 0.26613(4) 0.02988(14) Uani 1 1 d . . .
Cl3 Cl 0.17032(7) 0.83264(7) 0.40779(6) 0.04738(18) Uani 1 1 d . . .
Cl4 Cl 0.00695(9) 0.89394(7) 0.26008(6) 0.0552(2) Uani 1 1 d . . .
C12 C 0.2463(2) 0.49966(18) 0.20585(15) 0.0196(4) Uani 1 1 d . . .
C2 C 0.3759(2) 0.54496(19) 0.19320(15) 0.0188(4) Uani 1 1 d . . .
C1 C 0.4217(2) 0.64375(18) 0.13819(14) 0.0172(4) Uani 1 1 d . . .
C21 C 0.5595(2) 0.65905(18) 0.14727(14) 0.0173(4) Uani 1 1 d . . .
C26 C 0.5597(2) 0.7616(2) 0.20092(16) 0.0245(5) Uani 1 1 d . . .
H5 H 0.4719 0.8253 0.2297 0.029 Uiso 1 1 calc R . .
C25 C 0.6869(2) 0.7719(2) 0.21278(17) 0.0305(5) Uani 1 1 d . . .
H6 H 0.6853 0.8418 0.2502 0.037 Uiso 1 1 calc R . .
C24 C 0.8162(3) 0.6806(2) 0.17043(18) 0.0326(5) Uani 1 1 d . . .
H7 H 0.9032 0.6881 0.1782 0.039 Uiso 1 1 calc R . .
C23 C 0.8172(2) 0.5783(2) 0.11648(18) 0.0316(5) Uani 1 1 d . . .
H8 H 0.9054 0.5157 0.0868 0.038 Uiso 1 1 calc R . .
C22 C 0.6902(2) 0.5669(2) 0.10566(16) 0.0244(5) Uani 1 1 d . . .
H9 H 0.6920 0.4957 0.0695 0.029 Uiso 1 1 calc R . .
C27 C 0.3454(2) 0.73890(18) 0.07134(14) 0.0188(4) Uani 1 1 d . . .
C32 C 0.2216(2) 0.7278(2) 0.05212(15) 0.0228(4) Uani 1 1 d . . .
H11 H 0.1854 0.6555 0.0811 0.027 Uiso 1 1 calc R . .
C31 C 0.1510(2) 0.8193(2) -0.00786(16) 0.0269(5) Uani 1 1 d . . .
H12 H 0.0676 0.8090 -0.0197 0.032 Uiso 1 1 calc R . .
C30 C 0.2013(2) 0.9265(2) -0.05111(16) 0.0274(5) Uani 1 1 d . . .
H13 H 0.1514 0.9907 -0.0910 0.033 Uiso 1 1 calc R . .
C29 C 0.3240(3) 0.9382(2) -0.03534(18) 0.0336(5) Uani 1 1 d . . .
H14 H 0.3601 1.0102 -0.0656 0.040 Uiso 1 1 calc R . .
C28 C 0.3963(2) 0.8457(2) 0.02452(17) 0.0278(5) Uani 1 1 d . . .
H15 H 0.4817 0.8551 0.0338 0.033 Uiso 1 1 calc R . .
C3 C 0.4485(2) 0.45012(18) 0.26225(15) 0.0186(4) Uani 1 1 d . . .
C11 C 0.4014(2) 0.45609(19) 0.36932(15) 0.0200(4) Uani 1 1 d . . .
H17 H 0.3366 0.5296 0.4073 0.024 Uiso 1 1 calc R . .
C10 C 0.4683(2) 0.33218(19) 0.41077(15) 0.0200(4) Uani 1 1 d . . .
C5 C 0.5469(2) 0.24725(19) 0.32825(15) 0.0193(4) Uani 1 1 d . . .
C6 C 0.6250(2) 0.1159(2) 0.34630(17) 0.0238(4) Uani 1 1 d . . .
H20 H 0.6766 0.0578 0.2918 0.029 Uiso 1 1 calc R . .
C7 C 0.6237(2) 0.0756(2) 0.44395(17) 0.0271(5) Uani 1 1 d . . .
H21 H 0.6766 -0.0112 0.4571 0.033 Uiso 1 1 calc R . .
C8 C 0.5446(2) 0.1609(2) 0.52651(17) 0.0286(5) Uani 1 1 d . . .
H22 H 0.5455 0.1294 0.5935 0.034 Uiso 1 1 calc R . .
C9 C 0.4676(2) 0.2868(2) 0.51183(16) 0.0253(5) Uani 1 1 d . . .
H23 H 0.4148 0.3426 0.5676 0.030 Uiso 1 1 calc R . .
C4 C 0.5297(2) 0.31920(19) 0.23641(15) 0.0199(4) Uani 1 1 d . . .
H24 H 0.5662 0.2851 0.1700 0.024 Uiso 1 1 calc R . .
C13 C 0.2480(2) 0.3883(2) 0.15786(15) 0.0213(4) Uani 1 1 d . . .
H25 H 0.3224 0.3445 0.1023 0.026 Uiso 1 1 calc R . .
C14 C 0.1174(2) 0.35373(19) 0.20809(16) 0.0216(4) Uani 1 1 d . . .
C19 C 0.0420(2) 0.43720(19) 0.29201(15) 0.0202(4) Uani 1 1 d . . .
C20 C 0.1265(2) 0.52301(19) 0.29364(15) 0.0203(4) Uani 1 1 d . . .
H28 H 0.1059 0.5845 0.3445 0.024 Uiso 1 1 calc R . .
C18 C -0.0924(2) 0.4254(2) 0.35662(17) 0.0257(5) Uani 1 1 d . . .
H29 H -0.1418 0.4785 0.4143 0.031 Uiso 1 1 calc R . .
C17 C -0.1480(2) 0.3351(2) 0.33307(18) 0.0307(5) Uani 1 1 d . . .
H30 H -0.2389 0.3274 0.3742 0.037 Uiso 1 1 calc R . .
C16 C -0.0739(2) 0.2528(2) 0.24894(18) 0.0309(5) Uani 1 1 d . . .
H31 H -0.1170 0.1921 0.2347 0.037 Uiso 1 1 calc R . .
C15 C 0.0585(2) 0.2581(2) 0.18729(17) 0.0264(5) Uani 1 1 d . . .
H32 H 0.1089 0.1999 0.1327 0.032 Uiso 1 1 calc R . .
C33 C 0.0310(3) 0.9457(3) 0.3678(2) 0.0447(7) Uani 1 1 d . . .
H33A H 0.0526 1.0315 0.3522 0.054 Uiso 1 1 calc R . .
H33B H -0.0593 0.9581 0.4235 0.054 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
Ti1 Cl1 2.3101(6) . ?
Ti1 Cl2 2.3219(6) . ?
Ti1 C3 2.3417(18) . ?
Ti1 C12 2.3429(19) . ?
Ti1 C4 2.3547(19) . ?
Ti1 C13 2.365(2) . ?
Ti1 C20 2.3653(19) . ?
Ti1 C11 2.3757(19) . ?
Ti1 C5 2.5385(19) . ?
Ti1 C10 2.5628(19) . ?
Ti1 C14 2.567(2) . ?
Ti1 C19 2.569(2) . ?
Cl3 C33 1.750(3) . ?
Cl4 C33 1.752(3) . ?
C12 C13 1.420(3) . ?
C12 C20 1.420(3) . ?
C12 C2 1.492(3) . ?
C2 C1 1.343(3) . ?
C2 C3 1.495(3) . ?
C1 C27 1.493(3) . ?
C1 C21 1.502(3) . ?
C21 C26 1.393(3) . ?
C21 C22 1.397(3) . ?
C26 C25 1.389(3) . ?
C26 H5 0.9500 . ?
C25 C24 1.386(3) . ?
C25 H6 0.9500 . ?
C24 C23 1.388(3) . ?
C24 H7 0.9500 . ?
C23 C22 1.386(3) . ?
C23 H8 0.9500 . ?
C22 H9 0.9500 . ?
C27 C28 1.403(3) . ?
C27 C32 1.404(3) . ?
C32 C31 1.381(3) . ?
C32 H11 0.9500 . ?
C31 C30 1.391(3) . ?
C31 H12 0.9500 . ?
C30 C29 1.374(3) . ?
C30 H13 0.9500 . ?
C29 C28 1.394(3) . ?
C29 H14 0.9500 . ?
C28 H15 0.9500 . ?
C3 C11 1.414(3) . ?
C3 C4 1.417(3) . ?
C11 C10 1.436(3) . ?
C11 H17 0.9500 . ?
C10 C5 1.420(3) . ?
C10 C9 1.423(3) . ?
C5 C6 1.425(3) . ?
C5 C4 1.435(3) . ?
C6 C7 1.366(3) . ?
C6 H20 0.9500 . ?
C7 C8 1.423(3) . ?
C7 H21 0.9500 . ?
C8 C9 1.365(3) . ?
C8 H22 0.9500 . ?
C9 H23 0.9500 . ?
C4 H24 0.9500 . ?
C13 C14 1.436(3) . ?
C13 H25 0.9500 . ?
C14 C19 1.422(3) . ?
C14 C15 1.423(3) . ?
C19 C18 1.423(3) . ?
C19 C20 1.438(3) . ?
C20 H28 0.9500 . ?
C18 C17 1.365(3) . ?
C18 H29 0.9500 . ?
C17 C16 1.416(3) . ?
C17 H30 0.9500 . ?
C16 C15 1.373(3) . ?
C16 H31 0.9500 . ?
C15 H32 0.9500 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Ti1 Cl2 98.49(2) . . ?
Cl1 Ti1 C3 126.84(5) . . ?
Cl2 Ti1 C3 122.51(5) . . ?
Cl1 Ti1 C12 127.27(5) . . ?
Cl2 Ti1 C12 121.72(5) . . ?
C3 Ti1 C12 59.10(7) . . ?
Cl1 Ti1 C4 136.51(5) . . ?
Cl2 Ti1 C4 88.14(5) . . ?
C3 Ti1 C4 35.13(7) . . ?
C12 Ti1 C4 81.57(7) . . ?
Cl1 Ti1 C13 136.97(5) . . ?
Cl2 Ti1 C13 87.28(5) . . ?
C3 Ti1 C13 81.72(7) . . ?
C12 Ti1 C13 35.10(7) . . ?
C4 Ti1 C13 85.99(7) . . ?
Cl1 Ti1 C20 92.30(5) . . ?
Cl2 Ti1 C20 136.86(5) . . ?
C3 Ti1 C20 80.33(7) . . ?
C12 Ti1 C20 35.10(7) . . ?
C4 Ti1 C20 111.79(7) . . ?
C13 Ti1 C20 58.11(7) . . ?
Cl1 Ti1 C11 92.09(5) . . ?
Cl2 Ti1 C11 137.87(5) . . ?
C3 Ti1 C11 34.87(7) . . ?
C12 Ti1 C11 80.39(7) . . ?
C4 Ti1 C11 57.91(7) . . ?
C13 Ti1 C11 111.84(7) . . ?
C20 Ti1 C11 82.73(7) . . ?
Cl1 Ti1 C5 104.26(5) . . ?
Cl2 Ti1 C5 82.17(5) . . ?
C3 Ti1 C5 56.23(6) . . ?
C12 Ti1 C5 113.09(6) . . ?
C4 Ti1 C5 33.85(6) . . ?
C13 Ti1 C5 118.77(7) . . ?
C20 Ti1 C5 135.11(6) . . ?
C11 Ti1 C5 55.71(7) . . ?
Cl1 Ti1 C10 81.52(5) . . ?
Cl2 Ti1 C10 108.09(5) . . ?
C3 Ti1 C10 56.00(6) . . ?
C12 Ti1 C10 112.14(6) . . ?
C4 Ti1 C10 55.84(7) . . ?
C13 Ti1 C10 137.07(7) . . ?
C20 Ti1 C10 114.79(7) . . ?
C11 Ti1 C10 33.53(6) . . ?
C5 Ti1 C10 32.33(6) . . ?
Cl1 Ti1 C14 104.97(5) . . ?
Cl2 Ti1 C14 81.22(5) . . ?
C3 Ti1 C14 112.84(6) . . ?
C12 Ti1 C14 55.91(6) . . ?
C4 Ti1 C14 118.52(7) . . ?
C13 Ti1 C14 33.53(7) . . ?
C20 Ti1 C14 55.66(7) . . ?
C11 Ti1 C14 134.89(6) . . ?
C5 Ti1 C14 148.12(7) . . ?
C10 Ti1 C14 168.03(6) . . ?
Cl1 Ti1 C19 82.23(5) . . ?
Cl2 Ti1 C19 106.88(5) . . ?
C3 Ti1 C19 111.99(6) . . ?
C12 Ti1 C19 55.88(6) . . ?
C4 Ti1 C19 136.80(7) . . ?
C13 Ti1 C19 55.59(7) . . ?
C20 Ti1 C19 33.55(6) . . ?
C11 Ti1 C19 114.94(7) . . ?
C5 Ti1 C19 168.21(6) . . ?
C10 Ti1 C19 143.15(7) . . ?
C14 Ti1 C19 32.14(7) . . ?
C13 C12 C20 107.99(17) . . ?
C13 C12 C2 123.88(18) . . ?
C20 C12 C2 123.43(18) . . ?
C13 C12 Ti1 73.29(11) . . ?
C20 C12 Ti1 73.31(11) . . ?
C2 C12 Ti1 99.78(12) . . ?
C1 C2 C12 132.39(18) . . ?
C1 C2 C3 126.26(18) . . ?
C12 C2 C3 101.34(15) . . ?
C2 C1 C27 125.20(18) . . ?
C2 C1 C21 116.27(17) . . ?
C27 C1 C21 118.52(16) . . ?
C26 C21 C22 118.39(18) . . ?
C26 C21 C1 121.04(18) . . ?
C22 C21 C1 120.51(17) . . ?
C25 C26 C21 120.7(2) . . ?
C25 C26 H5 119.6 . . ?
C21 C26 H5 119.6 . . ?
C24 C25 C26 120.5(2) . . ?
C24 C25 H6 119.8 . . ?
C26 C25 H6 119.8 . . ?
C25 C24 C23 119.3(2) . . ?
C25 C24 H7 120.4 . . ?
C23 C24 H7 120.4 . . ?
C22 C23 C24 120.4(2) . . ?
C22 C23 H8 119.8 . . ?
C24 C23 H8 119.8 . . ?
C23 C22 C21 120.8(2) . . ?
C23 C22 H9 119.6 . . ?
C21 C22 H9 119.6 . . ?
C28 C27 C32 116.74(18) . . ?
C28 C27 C1 120.29(18) . . ?
C32 C27 C1 122.97(17) . . ?
C31 C32 C27 121.71(19) . . ?
C31 C32 H11 119.1 . . ?
C27 C32 H11 119.1 . . ?
C32 C31 C30 120.5(2) . . ?
C32 C31 H12 119.8 . . ?
C30 C31 H12 119.8 . . ?
C29 C30 C31 119.0(2) . . ?
C29 C30 H13 120.5 . . ?
C31 C30 H13 120.5 . . ?
C30 C29 C28 120.8(2) . . ?
C30 C29 H14 119.6 . . ?
C28 C29 H14 119.6 . . ?
C29 C28 C27 121.2(2) . . ?
C29 C28 H15 119.4 . . ?
C27 C28 H15 119.4 . . ?
C11 C3 C4 107.99(17) . . ?
C11 C3 C2 123.89(18) . . ?
C4 C3 C2 123.50(18) . . ?
C11 C3 Ti1 73.88(11) . . ?
C4 C3 Ti1 72.94(10) . . ?
C2 C3 Ti1 99.73(12) . . ?
C3 C11 C10 108.35(18) . . ?
C3 C11 Ti1 71.25(10) . . ?
C10 C11 Ti1 80.40(11) . . ?
C3 C11 H17 125.8 . . ?
C10 C11 H17 125.8 . . ?
Ti1 C11 H17 114.7 . . ?
C5 C10 C9 120.21(18) . . ?
C5 C10 C11 107.31(17) . . ?
C9 C10 C11 132.48(19) . . ?
C5 C10 Ti1 72.90(11) . . ?
C9 C10 Ti1 126.49(13) . . ?
C11 C10 Ti1 66.07(10) . . ?
C10 C5 C6 120.14(18) . . ?
C10 C5 C4 107.97(17) . . ?
C6 C5 C4 131.89(19) . . ?
C10 C5 Ti1 74.78(11) . . ?
C6 C5 Ti1 125.43(13) . . ?
C4 C5 Ti1 66.04(10) . . ?
C7 C6 C5 118.3(2) . . ?
C7 C6 H20 120.8 . . ?
C5 C6 H20 120.8 . . ?
C6 C7 C8 121.4(2) . . ?
C6 C7 H21 119.3 . . ?
C8 C7 H21 119.3 . . ?
C9 C8 C7 121.67(19) . . ?
C9 C8 H22 119.2 . . ?
C7 C8 H22 119.2 . . ?
C8 C9 C10 118.2(2) . . ?
C8 C9 H23 120.9 . . ?
C10 C9 H23 120.9 . . ?
C3 C4 C5 107.89(17) . . ?
C3 C4 Ti1 71.93(11) . . ?
C5 C4 Ti1 80.11(11) . . ?
C3 C4 H24 126.1 . . ?
C5 C4 H24 126.1 . . ?
Ti1 C4 H24 114.2 . . ?
C12 C13 C14 107.98(18) . . ?
C12 C13 Ti1 71.61(11) . . ?
C14 C13 Ti1 80.98(12) . . ?
C12 C13 H25 126.0 . . ?
C14 C13 H25 126.0 . . ?
Ti1 C13 H25 113.7 . . ?
C19 C14 C15 120.23(18) . . ?
C19 C14 C13 107.75(17) . . ?
C15 C14 C13 132.0(2) . . ?
C19 C14 Ti1 74.03(11) . . ?
C15 C14 Ti1 126.62(14) . . ?
C13 C14 Ti1 65.49(11) . . ?
C14 C19 C18 120.50(18) . . ?
C14 C19 C20 107.73(17) . . ?
C18 C19 C20 131.8(2) . . ?
C14 C19 Ti1 73.84(11) . . ?
C18 C19 Ti1 126.21(14) . . ?
C20 C19 Ti1 65.41(10) . . ?
C12 C20 C19 107.88(17) . . ?
C12 C20 Ti1 71.59(11) . . ?
C19 C20 Ti1 81.03(11) . . ?
C12 C20 H28 126.1 . . ?
C19 C20 H28 126.1 . . ?
Ti1 C20 H28 113.6 . . ?
C17 C18 C19 117.9(2) . . ?
C17 C18 H29 121.1 . . ?
C19 C18 H29 121.1 . . ?
C18 C17 C16 121.7(2) . . ?
C18 C17 H30 119.1 . . ?
C16 C17 H30 119.1 . . ?
C15 C16 C17 121.9(2) . . ?
C15 C16 H31 119.0 . . ?
C17 C16 H31 119.0 . . ?
C16 C15 C14 117.7(2) . . ?
C16 C15 H32 121.2 . . ?
C14 C15 H32 121.2 . . ?
Cl3 C33 Cl4 112.11(14) . . ?
Cl3 C33 H33A 109.2 . . ?
Cl4 C33 H33A 109.2 . . ?
Cl3 C33 H33B 109.2 . . ?
Cl4 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?

_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.972
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.067
_database_code_depnum_ccdc_archive 'CCDC 1003252'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_jgmm012_compound_10b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H28 Cl2 Zr'
_chemical_formula_weight         646.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.519
_cell_length_b                   23.219
_cell_length_c                   11.225
_cell_angle_alpha                90.00
_cell_angle_beta                 92.85
_cell_angle_gamma                90.00
_cell_volume                     2998.8
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       blocks
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1320
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28620
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         29.30
_reflns_number_total             8173
_reflns_number_gt                5539
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0434P)²+0.3315P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8173
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0724
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1019
_refine_ls_wR_factor_gt          0.0897
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.23049(2) 0.400389(9) 0.737807(19) 0.02004(7) Uani 1 1 d . . .
Cl1 Cl 0.26303(6) 0.46946(3) 0.89768(5) 0.02934(15) Uani 1 1 d . . .
Cl2 Cl 0.20452(6) 0.46525(2) 0.56934(5) 0.02911(14) Uani 1 1 d . . .
C1 C 0.2236(2) 0.20981(10) 0.73833(19) 0.0231(5) Uani 1 1 d . . .
C2 C 0.2255(2) 0.26757(10) 0.7395(2) 0.0248(5) Uani 1 1 d . . .
C3 C 0.3272(2) 0.30640(9) 0.7266(2) 0.0234(5) Uani 1 1 d . . .
C4 C 0.3844(2) 0.33700(9) 0.8220(2) 0.0244(5) Uani 1 1 d . . .
H4 H 0.3778 0.3294 0.9045 0.029 Uiso 1 1 calc R . .
C5 C 0.4538(2) 0.38124(10) 0.7723(2) 0.0271(5) Uani 1 1 d . . .
C6 C 0.5327(2) 0.42170(10) 0.8247(3) 0.0328(6) Uani 1 1 d . . .
H6 H 0.5457 0.4238 0.9088 0.039 Uiso 1 1 calc R . .
C7 C 0.5895(2) 0.45759(11) 0.7509(3) 0.0406(7) Uani 1 1 d . . .
H7 H 0.6441 0.4844 0.7847 0.049 Uiso 1 1 calc R . .
C8 C 0.5694(3) 0.45599(11) 0.6253(3) 0.0429(8) Uani 1 1 d . . .
H8 H 0.6110 0.4816 0.5771 0.052 Uiso 1 1 calc R . .
C9 C 0.4919(2) 0.41855(11) 0.5722(3) 0.0370(7) Uani 1 1 d . . .
H9 H 0.4778 0.4184 0.4881 0.044 Uiso 1 1 calc R . .
C10 C 0.4329(2) 0.37993(10) 0.6458(2) 0.0282(6) Uani 1 1 d . . .
C11 C 0.3503(2) 0.33486(10) 0.6187(2) 0.0266(5) Uani 1 1 d . . .
H11 H 0.3170 0.3258 0.5419 0.032 Uiso 1 1 calc R . .
C12 C 0.1257(2) 0.30825(9) 0.7529(2) 0.0226(5) Uani 1 1 d . . .
C13 C 0.1070(2) 0.33817(10) 0.8608(2) 0.0251(5) Uani 1 1 d . . .
H13 H 0.1404 0.3288 0.9375 0.030 Uiso 1 1 calc R . .
C14 C 0.0289(2) 0.38476(10) 0.8337(2) 0.0246(5) Uani 1 1 d . . .
C15 C -0.0243(2) 0.42604(11) 0.9072(2) 0.0317(6) Uani 1 1 d . . .
H15 H -0.0097 0.4259 0.9913 0.038 Uiso 1 1 calc R . .
C16 C -0.0969(2) 0.46598(11) 0.8536(2) 0.0345(6) Uani 1 1 d . . .
H16 H -0.1336 0.4936 0.9015 0.041 Uiso 1 1 calc R . .
C17 C -0.1187(2) 0.46707(10) 0.7279(2) 0.0321(6) Uani 1 1 d . . .
H17 H -0.1695 0.4955 0.6937 0.038 Uiso 1 1 calc R . .
C18 C -0.0686(2) 0.42826(10) 0.6550(2) 0.0274(5) Uani 1 1 d . . .
H18 H -0.0833 0.4297 0.5711 0.033 Uiso 1 1 calc R . .
C19 C 0.0059(2) 0.38587(9) 0.7072(2) 0.0230(5) Uani 1 1 d . . .
C20 C 0.0704(2) 0.33968(9) 0.6579(2) 0.0233(5) Uani 1 1 d . . .
H20 H 0.0753 0.3315 0.5754 0.028 Uiso 1 1 calc R . .
C21 C 0.3331(2) 0.17569(9) 0.7311(2) 0.0240(5) Uani 1 1 d . . .
C22 C 0.4339(2) 0.18895(10) 0.7996(2) 0.0288(6) Uani 1 1 d . . .
H22 H 0.4342 0.2209 0.8525 0.035 Uiso 1 1 calc R . .
C23 C 0.5334(2) 0.15630(11) 0.7915(2) 0.0339(6) Uani 1 1 d . . .
H23 H 0.6014 0.1660 0.8387 0.041 Uiso 1 1 calc R . .
C24 C 0.5350(2) 0.10956(11) 0.7152(2) 0.0356(6) Uani 1 1 d . . .
H24 H 0.6035 0.0871 0.7102 0.043 Uiso 1 1 calc R . .
C25 C 0.4364(2) 0.09590(10) 0.6465(2) 0.0318(6) Uani 1 1 d . . .
H25 H 0.4375 0.0642 0.5929 0.038 Uiso 1 1 calc R . .
C26 C 0.3354(2) 0.12800(10) 0.6548(2) 0.0263(5) Uani 1 1 d . . .
H26 H 0.2674 0.1175 0.6084 0.032 Uiso 1 1 calc R . .
C27 C 0.1122(2) 0.17671(9) 0.7427(2) 0.0221(5) Uani 1 1 d . . .
C28 C 0.0146(2) 0.19062(10) 0.6715(2) 0.0276(5) Uani 1 1 d . . .
H28 H 0.0167 0.2229 0.6197 0.033 Uiso 1 1 calc R . .
C29 C -0.0867(2) 0.15796(11) 0.6744(2) 0.0337(6) Uani 1 1 d . . .
H29 H -0.1530 0.1680 0.6250 0.040 Uiso 1 1 calc R . .
C30 C -0.0906(2) 0.11082(11) 0.7496(2) 0.0337(6) Uani 1 1 d . . .
H30 H -0.1594 0.0884 0.7517 0.040 Uiso 1 1 calc R . .
C31 C 0.0059(2) 0.09658(10) 0.8214(2) 0.0305(6) Uani 1 1 d . . .
H31 H 0.0029 0.0645 0.8737 0.037 Uiso 1 1 calc R . .
C32 C 0.1071(2) 0.12878(9) 0.8177(2) 0.0258(5) Uani 1 1 d . . .
H32 H 0.1734 0.1182 0.8666 0.031 Uiso 1 1 calc R . .
C33 C 0.6508(4) 0.23502(17) 1.0800(4) 0.0744(12) Uani 1 1 d . . .
H33 H 0.5997 0.2275 1.1420 0.089 Uiso 1 1 calc R . .
C34 C 0.6357(3) 0.28247(17) 1.0071(4) 0.0707(12) Uani 1 1 d . . .
H34 H 0.5722 0.3075 1.0197 0.085 Uiso 1 1 calc R . .
C35 C 0.7085(4) 0.29543(18) 0.9163(4) 0.0842(14) Uani 1 1 d . . .
H35 H 0.6948 0.3286 0.8681 0.101 Uiso 1 1 calc R . .
C36 C 0.8000(4) 0.26002(19) 0.8969(4) 0.0837(14) Uani 1 1 d . . .
H36 H 0.8511 0.2682 0.8352 0.100 Uiso 1 1 calc R . .
C37 C 0.8171(4) 0.21245(19) 0.9680(4) 0.0842(15) Uani 1 1 d . . .
H37 H 0.8811 0.1879 0.9547 0.101 Uiso 1 1 calc R . .
C38 C 0.7434(4) 0.19860(17) 1.0598(4) 0.0859(15) Uani 1 1 d . . .
H38 H 0.7566 0.1651 1.1070 0.103 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 Cl1 2.4219(6) . ?
Zr1 Cl2 2.4244(6) . ?
Zr1 C20 2.455(2) . ?
Zr1 C3 2.457(2) . ?
Zr1 C4 2.457(2) . ?
Zr1 C12 2.467(2) . ?
Zr1 C11 2.488(2) . ?
Zr1 C13 2.493(2) . ?
Zr1 C19 2.615(2) . ?
Zr1 C5 2.620(2) . ?
Zr1 C14 2.633(2) . ?
Zr1 C10 2.640(2) . ?
C1 C2 1.341(3) . ?
C1 C21 1.496(3) . ?
C1 C27 1.498(3) . ?
C2 C3 1.492(3) . ?
C2 C12 1.501(3) . ?
C3 C11 1.416(3) . ?
C3 C4 1.420(3) . ?
C4 C5 1.432(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.415(4) . ?
C5 C10 1.429(4) . ?
C6 C7 1.365(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.418(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.362(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.416(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.437(3) . ?
C11 H11 0.9500 . ?
C12 C20 1.417(3) . ?
C12 C13 1.422(3) . ?
C13 C14 1.430(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.423(3) . ?
C14 C19 1.432(3) . ?
C15 C16 1.368(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.421(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.364(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.413(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.432(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.395(4) . ?
C21 C26 1.401(3) . ?
C22 C23 1.381(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.383(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.378(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.385(3) . ?
C27 C32 1.399(3) . ?
C28 C29 1.394(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.384(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.380(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.387(3) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C34 1.379(5) . ?
C33 C38 1.389(5) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.363(5) . ?
C35 H35 0.9500 . ?
C36 C37 1.371(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.404(6) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?

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
Cl1 Zr1 Cl2 100.09(2) . . ?
Cl1 Zr1 C20 137.45(5) . . ?
Cl2 Zr1 C20 90.59(6) . . ?
Cl1 Zr1 C3 124.92(6) . . ?
Cl2 Zr1 C3 123.40(6) . . ?
C20 Zr1 C3 78.79(8) . . ?
Cl1 Zr1 C4 91.70(6) . . ?
Cl2 Zr1 C4 136.95(6) . . ?
C20 Zr1 C4 108.12(8) . . ?
C3 Zr1 C4 33.59(8) . . ?
Cl1 Zr1 C12 125.56(5) . . ?
Cl2 Zr1 C12 123.41(6) . . ?
C20 Zr1 C12 33.47(7) . . ?
C3 Zr1 C12 57.18(8) . . ?
C4 Zr1 C12 78.48(8) . . ?
Cl1 Zr1 C11 137.18(6) . . ?
Cl2 Zr1 C11 90.63(6) . . ?
C20 Zr1 C11 83.06(8) . . ?
C3 Zr1 C11 33.27(7) . . ?
C4 Zr1 C11 55.34(8) . . ?
C12 Zr1 C11 78.06(7) . . ?
Cl1 Zr1 C13 92.56(6) . . ?
Cl2 Zr1 C13 137.77(6) . . ?
C20 Zr1 C13 55.30(8) . . ?
C3 Zr1 C13 77.68(7) . . ?
C4 Zr1 C13 81.99(8) . . ?
C12 Zr1 C13 33.32(7) . . ?
C11 Zr1 C13 106.89(8) . . ?
Cl1 Zr1 C19 107.36(5) . . ?
Cl2 Zr1 C19 83.96(5) . . ?
C20 Zr1 C19 32.62(7) . . ?
C3 Zr1 C19 109.10(8) . . ?
C4 Zr1 C19 131.59(7) . . ?
C12 Zr1 C19 54.03(7) . . ?
C11 Zr1 C19 114.98(8) . . ?
C13 Zr1 C19 53.83(8) . . ?
Cl1 Zr1 C5 83.58(6) . . ?
Cl2 Zr1 C5 107.62(6) . . ?
C20 Zr1 C5 132.11(7) . . ?
C3 Zr1 C5 54.00(8) . . ?
C4 Zr1 C5 32.55(7) . . ?
C12 Zr1 C5 108.85(8) . . ?
C11 Zr1 C5 53.77(8) . . ?
C13 Zr1 C5 113.77(8) . . ?
C19 Zr1 C5 162.80(7) . . ?
Cl1 Zr1 C14 83.99(5) . . ?
Cl2 Zr1 C14 109.12(6) . . ?
C20 Zr1 C14 53.75(7) . . ?
C3 Zr1 C14 108.07(7) . . ?
C4 Zr1 C14 113.23(8) . . ?
C12 Zr1 C14 53.67(7) . . ?
C11 Zr1 C14 131.26(7) . . ?
C13 Zr1 C14 32.24(7) . . ?
C19 Zr1 C14 31.67(7) . . ?
C5 Zr1 C14 142.71(8) . . ?
Cl1 Zr1 C10 107.57(6) . . ?
Cl2 Zr1 C10 83.32(6) . . ?
C20 Zr1 C10 114.56(8) . . ?
C3 Zr1 C10 53.72(7) . . ?
C4 Zr1 C10 53.70(8) . . ?
C12 Zr1 C10 108.41(7) . . ?
C11 Zr1 C10 32.37(8) . . ?
C13 Zr1 C10 130.70(7) . . ?
C19 Zr1 C10 144.38(8) . . ?
C5 Zr1 C10 31.51(8) . . ?
C14 Zr1 C10 161.69(7) . . ?
C2 C1 C21 121.1(2) . . ?
C2 C1 C27 121.7(2) . . ?
C21 C1 C27 117.13(19) . . ?
C1 C2 C3 128.0(2) . . ?
C1 C2 C12 128.2(2) . . ?
C3 C2 C12 103.83(19) . . ?
C11 C3 C4 108.2(2) . . ?
C11 C3 C2 123.2(2) . . ?
C4 C3 C2 124.5(2) . . ?
C11 C3 Zr1 74.58(13) . . ?
C4 C3 Zr1 73.21(13) . . ?
C2 C3 Zr1 99.85(14) . . ?
C3 C4 C5 108.2(2) . . ?
C3 C4 Zr1 73.20(13) . . ?
C5 C4 Zr1 80.02(14) . . ?
C3 C4 H4 125.9 . . ?
C5 C4 H4 125.9 . . ?
Zr1 C4 H4 113.2 . . ?
C6 C5 C10 120.0(2) . . ?
C6 C5 C4 132.4(2) . . ?
C10 C5 C4 107.6(2) . . ?
C6 C5 Zr1 123.67(16) . . ?
C10 C5 Zr1 75.00(14) . . ?
C4 C5 Zr1 67.42(13) . . ?
C7 C6 C5 118.1(3) . . ?
C7 C6 H6 121.0 . . ?
C5 C6 H6 121.0 . . ?
C6 C7 C8 121.9(3) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C9 C8 C7 121.6(3) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C10 118.1(3) . . ?
C8 C9 H9 120.9 . . ?
C10 C9 H9 120.9 . . ?
C9 C10 C5 120.3(2) . . ?
C9 C10 C11 132.0(3) . . ?
C5 C10 C11 107.6(2) . . ?
C9 C10 Zr1 124.98(17) . . ?
C5 C10 Zr1 73.49(13) . . ?
C11 C10 Zr1 67.99(13) . . ?
C3 C11 C10 108.0(2) . . ?
C3 C11 Zr1 72.15(13) . . ?
C10 C11 Zr1 79.64(13) . . ?
C3 C11 H11 126.0 . . ?
C10 C11 H11 126.0 . . ?
Zr1 C11 H11 114.4 . . ?
C20 C12 C13 108.0(2) . . ?
C20 C12 C2 124.5(2) . . ?
C13 C12 C2 122.8(2) . . ?
C20 C12 Zr1 72.82(13) . . ?
C13 C12 Zr1 74.36(13) . . ?
C2 C12 Zr1 99.14(14) . . ?
C12 C13 C14 108.0(2) . . ?
C12 C13 Zr1 72.32(12) . . ?
C14 C13 Zr1 79.27(13) . . ?
C12 C13 H13 126.0 . . ?
C14 C13 H13 126.0 . . ?
Zr1 C13 H13 114.6 . . ?
C15 C14 C13 132.1(2) . . ?
C15 C14 C19 119.9(2) . . ?
C13 C14 C19 108.0(2) . . ?
C15 C14 Zr1 123.93(16) . . ?
C13 C14 Zr1 68.49(12) . . ?
C19 C14 Zr1 73.46(13) . . ?
C16 C15 C14 118.2(2) . . ?
C16 C15 H15 120.9 . . ?
C14 C15 H15 120.9 . . ?
C15 C16 C17 121.6(2) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C18 C17 C16 121.6(2) . . ?
C18 C17 H17 119.2 . . ?
C16 C17 H17 119.2 . . ?
C17 C18 C19 118.6(2) . . ?
C17 C18 H18 120.7 . . ?
C19 C18 H18 120.7 . . ?
C18 C19 C20 132.6(2) . . ?
C18 C19 C14 120.1(2) . . ?
C20 C19 C14 107.2(2) . . ?
C18 C19 Zr1 122.74(16) . . ?
C20 C19 Zr1 67.55(13) . . ?
C14 C19 Zr1 74.87(14) . . ?
C12 C20 C19 108.5(2) . . ?
C12 C20 Zr1 73.71(14) . . ?
C19 C20 Zr1 79.83(13) . . ?
C12 C20 H20 125.8 . . ?
C19 C20 H20 125.8 . . ?
Zr1 C20 H20 113.0 . . ?
C22 C21 C26 118.1(2) . . ?
C22 C21 C1 122.3(2) . . ?
C26 C21 C1 119.6(2) . . ?
C23 C22 C21 120.9(2) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C22 C23 C24 120.5(3) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C25 C24 C23 119.5(2) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C26 120.6(2) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 120.5(2) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C28 C27 C32 118.4(2) . . ?
C28 C27 C1 122.2(2) . . ?
C32 C27 C1 119.3(2) . . ?
C27 C28 C29 121.1(2) . . ?
C27 C28 H28 119.5 . . ?
C29 C28 H28 119.5 . . ?
C30 C29 C28 119.8(3) . . ?
C30 C29 H29 120.1 . . ?
C28 C29 H29 120.1 . . ?
C31 C30 C29 119.7(2) . . ?
C31 C30 H30 120.1 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 120.5(2) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C31 C32 C27 120.5(2) . . ?
C31 C32 H32 119.8 . . ?
C27 C32 H32 119.8 . . ?
C34 C33 C38 117.7(4) . . ?
C34 C33 H33 121.1 . . ?
C38 C33 H33 121.1 . . ?
C33 C34 C35 123.2(4) . . ?
C33 C34 H34 118.4 . . ?
C35 C34 H34 118.4 . . ?
C36 C35 C34 119.2(4) . . ?
C36 C35 H35 120.4 . . ?
C34 C35 H35 120.4 . . ?
C35 C36 C37 118.8(5) . . ?
C35 C36 H36 120.6 . . ?
C37 C36 H36 120.6 . . ?
C36 C37 C38 122.5(4) . . ?
C36 C37 H37 118.7 . . ?
C38 C37 H37 118.7 . . ?
C33 C38 C37 118.5(4) . . ?
C33 C38 H38 120.7 . . ?
C37 C38 H38 120.7 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        29.30
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.081
_database_code_depnum_ccdc_archive 'CCDC 1003253'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_jgmm018_0m_compound_11a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H26 Cl2 Ti'
_chemical_formula_weight         457.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   10.312(3)
_cell_length_b                   20.895(8)
_cell_length_c                   10.999(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.539(15)
_cell_angle_gamma                90.00
_cell_volume                     2219.3(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       blocks
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             952
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19859
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_sigmaI/netI    0.0900
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         27.70
_reflns_number_total             5147
_reflns_number_gt                3010
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1144P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5147
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1274
_refine_ls_R_factor_gt           0.0702
_refine_ls_wR_factor_ref         0.2051
_refine_ls_wR_factor_gt          0.1693
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.63676(7) 0.22162(3) 0.21516(6) 0.0181(2) Uani 1 1 d . . .
Cl1 Cl 0.78236(10) 0.14889(5) 0.35849(9) 0.0250(3) Uani 1 1 d . . .
Cl2 Cl 0.48952(10) 0.15232(5) 0.06672(9) 0.0250(3) Uani 1 1 d . . .
C1 C 0.6640(5) 0.4260(2) 0.2471(4) 0.0283(10) Uani 1 1 d . . .
C2 C 0.6478(4) 0.3631(2) 0.2291(4) 0.0228(9) Uani 1 1 d . . .
C3 C 0.7146(4) 0.31880(19) 0.1621(4) 0.0208(9) Uani 1 1 d . . .
C4 C 0.6424(4) 0.28770(19) 0.0427(4) 0.0222(9) Uani 1 1 d . . .
H4A H 0.5595 0.3051 -0.0279 0.027 Uiso 1 1 calc R . .
C5 C 0.7271(4) 0.23646(19) 0.0287(4) 0.0209(9) Uani 1 1 d . . .
C6 C 0.7111(5) 0.1917(2) -0.0732(4) 0.0277(10) Uani 1 1 d . . .
H6A H 0.6325 0.1936 -0.1509 0.033 Uiso 1 1 calc R . .
C7 C 0.8097(5) 0.1465(2) -0.0576(5) 0.0329(11) Uani 1 1 d . . .
H7A H 0.8000 0.1167 -0.1253 0.040 Uiso 1 1 calc R . .
C8 C 0.9292(5) 0.1429(2) 0.0603(5) 0.0347(11) Uani 1 1 d . . .
H8A H 0.9980 0.1113 0.0683 0.042 Uiso 1 1 calc R . .
C9 C 0.9443(4) 0.1838(2) 0.1589(4) 0.0277(10) Uani 1 1 d . . .
H9A H 1.0217 0.1801 0.2372 0.033 Uiso 1 1 calc R . .
C10 C 0.8448(4) 0.2323(2) 0.1456(4) 0.0224(9) Uani 1 1 d . . .
C11 C 0.8325(4) 0.2824(2) 0.2293(4) 0.0228(9) Uani 1 1 d . . .
H11A H 0.9066 0.2955 0.3120 0.027 Uiso 1 1 calc R . .
C12 C 0.5698(4) 0.31796(19) 0.2824(4) 0.0211(9) Uani 1 1 d . . .
C13 C 0.6355(4) 0.2822(2) 0.3971(4) 0.0232(9) Uani 1 1 d . . .
H13A H 0.7197 0.2960 0.4707 0.028 Uiso 1 1 calc R . .
C14 C 0.5448(4) 0.2310(2) 0.4020(4) 0.0234(9) Uani 1 1 d . . .
C15 C 0.5526(5) 0.1838(2) 0.4964(4) 0.0270(10) Uani 1 1 d . . .
H15A H 0.6302 0.1820 0.5749 0.032 Uiso 1 1 calc R . .
C16 C 0.4480(5) 0.1410(2) 0.4736(5) 0.0329(11) Uani 1 1 d . . .
H16A H 0.4525 0.1094 0.5370 0.040 Uiso 1 1 calc R . .
C17 C 0.3315(5) 0.1427(2) 0.3561(5) 0.0310(10) Uani 1 1 d . . .
H17A H 0.2597 0.1121 0.3429 0.037 Uiso 1 1 calc R . .
C18 C 0.3202(5) 0.1870(2) 0.2620(4) 0.0270(10) Uani 1 1 d . . .
H18A H 0.2423 0.1871 0.1836 0.032 Uiso 1 1 calc R . .
C19 C 0.4273(4) 0.2330(2) 0.2837(4) 0.0222(9) Uani 1 1 d . . .
C20 C 0.4467(4) 0.28484(19) 0.2080(4) 0.0213(9) Uani 1 1 d . . .
H20A H 0.3750 0.3015 0.1270 0.026 Uiso 1 1 calc R . .
C21 C 0.7601(5) 0.4622(2) 0.1959(5) 0.0352(11) Uani 1 1 d . . .
H21A H 0.7166 0.5035 0.1598 0.042 Uiso 1 1 calc R . .
H21B H 0.7728 0.4374 0.1242 0.042 Uiso 1 1 calc R . .
C22 C 0.9012(6) 0.4751(3) 0.2986(6) 0.0559(16) Uani 1 1 d . . .
H22A H 0.8888 0.5021 0.3677 0.067 Uiso 1 1 calc R . .
H22B H 0.9420 0.4339 0.3386 0.067 Uiso 1 1 calc R . .
C23 C 1.0002(6) 0.5075(3) 0.2470(6) 0.0554(16) Uani 1 1 d . . .
H23A H 1.0886 0.5144 0.3178 0.083 Uiso 1 1 calc R . .
H23B H 0.9618 0.5489 0.2092 0.083 Uiso 1 1 calc R . .
H23C H 1.0151 0.4806 0.1801 0.083 Uiso 1 1 calc R . .
C24 C 0.5900(5) 0.4629(2) 0.3213(5) 0.0398(12) Uani 1 1 d . . .
H24A H 0.6561 0.4928 0.3819 0.048 Uiso 1 1 calc R . .
H24B H 0.5575 0.4326 0.3736 0.048 Uiso 1 1 calc R . .
C25 C 0.4644(6) 0.5014(3) 0.2311(6) 0.0509(15) Uani 1 1 d . . .
H25A H 0.4242 0.5262 0.2859 0.061 Uiso 1 1 calc R . .
H25B H 0.4983 0.5324 0.1810 0.061 Uiso 1 1 calc R . .
C26 C 0.3528(6) 0.4623(3) 0.1383(5) 0.0529(15) Uani 1 1 d . . .
H26A H 0.2789 0.4905 0.0848 0.079 Uiso 1 1 calc R . .
H26B H 0.3152 0.4327 0.1866 0.079 Uiso 1 1 calc R . .
H26C H 0.3908 0.4379 0.0824 0.079 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
Ti1 Cl2 2.3084(13) . ?
Ti1 Cl1 2.3213(13) . ?
Ti1 C12 2.331(4) . ?
Ti1 C3 2.332(4) . ?
Ti1 C20 2.342(4) . ?
Ti1 C11 2.343(4) . ?
Ti1 C4 2.364(4) . ?
Ti1 C13 2.371(4) . ?
Ti1 C10 2.527(4) . ?
Ti1 C19 2.537(4) . ?
Ti1 C5 2.551(4) . ?
Ti1 C14 2.555(4) . ?
C1 C2 1.332(6) . ?
C1 C21 1.504(6) . ?
C1 C24 1.509(6) . ?
C2 C12 1.487(5) . ?
C2 C3 1.493(5) . ?
C3 C11 1.404(6) . ?
C3 C4 1.419(5) . ?
C4 C5 1.423(6) . ?
C5 C6 1.424(5) . ?
C5 C10 1.428(5) . ?
C6 C7 1.354(6) . ?
C7 C8 1.444(7) . ?
C8 C9 1.347(6) . ?
C9 C10 1.413(6) . ?
C10 C11 1.428(6) . ?
C12 C13 1.417(5) . ?
C12 C20 1.425(6) . ?
C13 C14 1.434(6) . ?
C14 C15 1.415(6) . ?
C14 C19 1.434(6) . ?
C15 C16 1.354(6) . ?
C16 C17 1.423(7) . ?
C17 C18 1.363(6) . ?
C18 C19 1.420(6) . ?
C19 C20 1.423(6) . ?
C21 C22 1.521(7) . ?
C22 C23 1.493(7) . ?
C24 C25 1.551(7) . ?
C25 C26 1.486(8) . ?

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
Cl2 Ti1 Cl1 100.24(5) . . ?
Cl2 Ti1 C12 124.87(11) . . ?
Cl1 Ti1 C12 122.88(11) . . ?
Cl2 Ti1 C3 124.61(11) . . ?
Cl1 Ti1 C3 122.88(11) . . ?
C12 Ti1 C3 59.58(14) . . ?
Cl2 Ti1 C20 89.72(11) . . ?
Cl1 Ti1 C20 136.58(10) . . ?
C12 Ti1 C20 35.52(14) . . ?
C3 Ti1 C20 81.83(14) . . ?
Cl2 Ti1 C11 136.42(11) . . ?
Cl1 Ti1 C11 88.46(11) . . ?
C12 Ti1 C11 81.65(14) . . ?
C3 Ti1 C11 34.96(14) . . ?
C20 Ti1 C11 112.81(15) . . ?
Cl2 Ti1 C4 89.66(11) . . ?
Cl1 Ti1 C4 137.33(11) . . ?
C12 Ti1 C4 81.01(14) . . ?
C3 Ti1 C4 35.18(13) . . ?
C20 Ti1 C4 84.24(14) . . ?
C11 Ti1 C4 58.21(14) . . ?
Cl2 Ti1 C13 137.28(11) . . ?
Cl1 Ti1 C13 88.29(11) . . ?
C12 Ti1 C13 35.07(13) . . ?
C3 Ti1 C13 81.41(14) . . ?
C20 Ti1 C13 58.33(14) . . ?
C11 Ti1 C13 85.08(15) . . ?
C4 Ti1 C13 111.99(15) . . ?
Cl2 Ti1 C10 105.01(10) . . ?
Cl1 Ti1 C10 81.26(10) . . ?
C12 Ti1 C10 113.37(14) . . ?
C3 Ti1 C10 56.21(14) . . ?
C20 Ti1 C10 136.81(14) . . ?
C11 Ti1 C10 33.83(14) . . ?
C4 Ti1 C10 56.13(13) . . ?
C13 Ti1 C10 117.68(14) . . ?
Cl2 Ti1 C19 81.47(10) . . ?
Cl1 Ti1 C19 105.95(10) . . ?
C12 Ti1 C19 56.43(14) . . ?
C3 Ti1 C19 113.37(14) . . ?
C20 Ti1 C19 33.62(13) . . ?
C11 Ti1 C19 137.14(14) . . ?
C4 Ti1 C19 116.58(14) . . ?
C13 Ti1 C19 56.08(14) . . ?
C10 Ti1 C19 169.54(14) . . ?
Cl2 Ti1 C5 80.95(10) . . ?
Cl1 Ti1 C5 107.09(10) . . ?
C12 Ti1 C5 112.48(13) . . ?
C3 Ti1 C5 55.82(13) . . ?
C20 Ti1 C5 116.21(14) . . ?
C11 Ti1 C5 55.85(14) . . ?
C4 Ti1 C5 33.39(13) . . ?
C13 Ti1 C5 136.46(14) . . ?
C10 Ti1 C5 32.65(12) . . ?
C19 Ti1 C5 144.76(14) . . ?
Cl2 Ti1 C14 106.22(10) . . ?
Cl1 Ti1 C14 80.70(10) . . ?
C12 Ti1 C14 56.20(13) . . ?
C3 Ti1 C14 113.08(14) . . ?
C20 Ti1 C14 56.03(13) . . ?
C11 Ti1 C14 117.34(14) . . ?
C4 Ti1 C14 136.17(14) . . ?
C13 Ti1 C14 33.59(14) . . ?
C10 Ti1 C14 146.16(14) . . ?
C19 Ti1 C14 32.71(13) . . ?
C5 Ti1 C14 168.61(13) . . ?
C2 C1 C21 120.3(4) . . ?
C2 C1 C24 121.6(4) . . ?
C21 C1 C24 118.0(4) . . ?
C1 C2 C12 128.6(4) . . ?
C1 C2 C3 129.1(4) . . ?
C12 C2 C3 102.0(3) . . ?
C11 C3 C4 108.4(4) . . ?
C11 C3 C2 122.7(4) . . ?
C4 C3 C2 123.9(4) . . ?
C11 C3 Ti1 73.0(2) . . ?
C4 C3 Ti1 73.6(2) . . ?
C2 C3 Ti1 99.0(2) . . ?
C3 C4 C5 107.6(4) . . ?
C3 C4 Ti1 71.2(2) . . ?
C5 C4 Ti1 80.6(2) . . ?
C4 C5 C6 132.3(4) . . ?
C4 C5 C10 107.9(3) . . ?
C6 C5 C10 119.8(4) . . ?
C4 C5 Ti1 66.0(2) . . ?
C6 C5 Ti1 125.4(3) . . ?
C10 C5 Ti1 72.7(2) . . ?
C7 C6 C5 118.9(4) . . ?
C6 C7 C8 121.2(4) . . ?
C9 C8 C7 120.7(4) . . ?
C8 C9 C10 119.9(4) . . ?
C9 C10 C5 119.6(4) . . ?
C9 C10 C11 133.2(4) . . ?
C5 C10 C11 107.2(4) . . ?
C9 C10 Ti1 124.6(3) . . ?
C5 C10 Ti1 74.6(2) . . ?
C11 C10 Ti1 66.0(2) . . ?
C3 C11 C10 108.3(4) . . ?
C3 C11 Ti1 72.1(2) . . ?
C10 C11 Ti1 80.2(2) . . ?
C13 C12 C20 107.8(3) . . ?
C13 C12 C2 122.0(4) . . ?
C20 C12 C2 125.3(4) . . ?
C13 C12 Ti1 74.0(2) . . ?
C20 C12 Ti1 72.7(2) . . ?
C2 C12 Ti1 99.3(2) . . ?
C12 C13 C14 108.2(4) . . ?
C12 C13 Ti1 70.9(2) . . ?
C14 C13 Ti1 80.3(2) . . ?
C15 C14 C19 119.9(4) . . ?
C15 C14 C13 132.7(4) . . ?
C19 C14 C13 107.4(4) . . ?
C15 C14 Ti1 126.5(3) . . ?
C19 C14 Ti1 72.9(2) . . ?
C13 C14 Ti1 66.2(2) . . ?
C16 C15 C14 119.2(4) . . ?
C15 C16 C17 121.0(4) . . ?
C18 C17 C16 121.8(4) . . ?
C17 C18 C19 118.5(4) . . ?
C18 C19 C20 132.7(4) . . ?
C18 C19 C14 119.5(4) . . ?
C20 C19 C14 107.8(4) . . ?
C18 C19 Ti1 125.5(3) . . ?
C20 C19 Ti1 65.6(2) . . ?
C14 C19 Ti1 74.4(2) . . ?
C19 C20 C12 108.3(4) . . ?
C19 C20 Ti1 80.7(2) . . ?
C12 C20 Ti1 71.8(2) . . ?
C1 C21 C22 113.3(4) . . ?
C23 C22 C21 113.7(5) . . ?
C1 C24 C25 112.7(4) . . ?
C26 C25 C24 115.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.70
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.049
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.122
_database_code_depnum_ccdc_archive 'CCDC 1003254'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_jz001_0m_compound_13

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H32'
_chemical_formula_weight         512.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   9.7792(5)
_cell_length_b                   18.3385(9)
_cell_length_c                   15.3858(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.060(2)
_cell_angle_gamma                90.00
_cell_volume                     2687.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       blocks
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9894
_exptl_absorpt_correction_T_max  0.9929
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22384
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6133
_reflns_number_gt                3798
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0434P)²+0.4080P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6133
_refine_ls_number_parameters     362
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1140
_refine_ls_wR_factor_gt          0.0967
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.43269(19) -0.21970(10) 0.30490(12) 0.0326(5) Uani 1 1 d . . .
H1 H 0.3799 -0.2381 0.2497 0.039 Uiso 1 1 calc R . .
C2 C 0.47475(18) -0.14707(10) 0.31079(11) 0.0291(4) Uani 1 1 d . . .
H32 H 0.4511 -0.1159 0.2603 0.035 Uiso 1 1 calc R . .
C3 C 0.55150(17) -0.12102(9) 0.39127(11) 0.0235(4) Uani 1 1 d . . .
C4 C 0.61098(18) -0.04689(9) 0.41787(10) 0.0241(4) Uani 1 1 d . . .
H7 H 0.5352 -0.0108 0.4163 0.029 Uiso 1 1 calc R . .
H6 H 0.6711 -0.0303 0.3779 0.029 Uiso 1 1 calc R . .
C5 C 0.69655(18) -0.05767(9) 0.51222(11) 0.0225(4) Uani 1 1 d . . .
C6 C 0.77978(17) 0.00138(9) 0.56173(10) 0.0216(4) Uani 1 1 d . . .
C7 C 0.88045(17) -0.00824(9) 0.65245(10) 0.0211(4) Uani 1 1 d . . .
C8 C 0.80240(18) 0.01931(9) 0.72634(11) 0.0224(4) Uani 1 1 d . . .
H31 H 0.7092 0.0374 0.6923 0.027 Uiso 1 1 calc R . .
C9 C 0.76879(18) -0.03070(9) 0.79769(11) 0.0259(4) Uani 1 1 d . . .
C10 C 0.70034(19) -0.09750(10) 0.78841(13) 0.0345(5) Uani 1 1 d . . .
H26 H 0.6734 -0.1200 0.7315 0.041 Uiso 1 1 calc R . .
C11 C 0.6715(2) -0.13127(11) 0.86341(14) 0.0431(5) Uani 1 1 d . . .
H27 H 0.6261 -0.1774 0.8575 0.052 Uiso 1 1 calc R . .
C12 C 0.7081(2) -0.09845(12) 0.94620(14) 0.0465(6) Uani 1 1 d . . .
H2 H 0.6901 -0.1226 0.9971 0.056 Uiso 1 1 calc R . .
C13 C 0.4663(2) -0.26550(10) 0.37791(13) 0.0347(5) Uani 1 1 d . . .
H3 H 0.4356 -0.3148 0.3728 0.042 Uiso 1 1 calc R . .
C14 C 0.58896(18) -0.16753(9) 0.46494(11) 0.0253(4) Uani 1 1 d . . .
C15 C 0.5447(2) -0.23984(10) 0.45851(12) 0.0323(4) Uani 1 1 d . . .
H4 H 0.5680 -0.2712 0.5088 0.039 Uiso 1 1 calc R . .
C16 C 0.67874(18) -0.12728(9) 0.53734(11) 0.0277(4) Uani 1 1 d . . .
H5 H 0.7194 -0.1470 0.5944 0.033 Uiso 1 1 calc R . .
C17 C 0.87044(18) 0.08449(9) 0.77990(11) 0.0238(4) Uani 1 1 d . . .
C18 C 0.93669(18) 0.13726(9) 0.74575(11) 0.0253(4) Uani 1 1 d . . .
C19 C 0.96755(17) 0.12379(9) 0.65418(11) 0.0227(4) Uani 1 1 d . . .
C20 C 1.00740(17) 0.04309(9) 0.65216(11) 0.0208(4) Uani 1 1 d . . .
H14 H 1.0360 0.0346 0.5945 0.025 Uiso 1 1 calc R . .
C21 C 1.12259(17) 0.01192(9) 0.72544(10) 0.0223(4) Uani 1 1 d . . .
C22 C 1.24475(18) 0.04315(10) 0.77575(11) 0.0268(4) Uani 1 1 d . . .
H8 H 1.2635 0.0935 0.7699 0.032 Uiso 1 1 calc R . .
C23 C 1.33872(19) -0.00030(11) 0.83454(12) 0.0333(5) Uani 1 1 d . . .
H13 H 1.4229 0.0204 0.8687 0.040 Uiso 1 1 calc R . .
C24 C 1.3110(2) -0.07366(10) 0.84387(12) 0.0357(5) Uani 1 1 d . . .
H12 H 1.3766 -0.1029 0.8841 0.043 Uiso 1 1 calc R . .
C25 C 1.18819(19) -0.10477(10) 0.79490(12) 0.0317(4) Uani 1 1 d . . .
H11 H 1.1691 -0.1550 0.8015 0.038 Uiso 1 1 calc R . .
C26 C 1.09387(18) -0.06145(9) 0.73615(11) 0.0245(4) Uani 1 1 d . . .
C27 C 0.95571(18) -0.08262(9) 0.67519(11) 0.0251(4) Uani 1 1 d . . .
H10 H 0.9013 -0.1153 0.7059 0.030 Uiso 1 1 calc R . .
H9 H 0.9705 -0.1071 0.6207 0.030 Uiso 1 1 calc R . .
C28 C 0.83473(18) 0.13696(9) 0.57499(10) 0.0229(4) Uani 1 1 d . . .
H15 H 0.7635 0.1641 0.5999 0.027 Uiso 1 1 calc R . .
C29 C 0.88613(18) 0.18774(8) 0.51180(11) 0.0226(4) Uani 1 1 d . . .
C30 C 1.02250(18) 0.21063(9) 0.54595(11) 0.0235(4) Uani 1 1 d . . .
C31 C 1.0849(2) 0.26120(9) 0.50013(12) 0.0289(4) Uani 1 1 d . . .
H19 H 1.1772 0.2783 0.5248 0.035 Uiso 1 1 calc R . .
C32 C 1.0115(2) 0.28631(10) 0.41838(12) 0.0342(5) Uani 1 1 d . . .
H18 H 1.0533 0.3212 0.3867 0.041 Uiso 1 1 calc R . .
C33 C 0.8779(2) 0.26115(10) 0.38223(12) 0.0345(5) Uani 1 1 d . . .
H17 H 0.8298 0.2774 0.3248 0.041 Uiso 1 1 calc R . .
C34 C 0.81270(19) 0.21228(9) 0.42892(11) 0.0293(4) Uani 1 1 d . . .
H16 H 0.7197 0.1960 0.4046 0.035 Uiso 1 1 calc R . .
C35 C 1.08543(19) 0.17301(9) 0.63212(11) 0.0284(4) Uani 1 1 d . . .
H20 H 1.1174 0.2092 0.6802 0.034 Uiso 1 1 calc R . .
H21 H 1.1669 0.1430 0.6259 0.034 Uiso 1 1 calc R . .
C36 C 0.76460(18) 0.06972(9) 0.52964(11) 0.0246(4) Uani 1 1 d . . .
H22 H 0.7035 0.0762 0.4727 0.029 Uiso 1 1 calc R . .
C37 C 0.9889(2) 0.20369(10) 0.79968(12) 0.0403(5) Uani 1 1 d . . .
H24 H 0.9287 0.2136 0.8414 0.060 Uiso 1 1 calc R . .
H23 H 0.9866 0.2455 0.7598 0.060 Uiso 1 1 calc R . .
H25 H 1.0854 0.1954 0.8332 0.060 Uiso 1 1 calc R . .
C38 C 0.8539(2) 0.07930(10) 0.87484(11) 0.0327(5) Uani 1 1 d . . .
H30 H 0.9451 0.0862 0.9177 0.039 Uiso 1 1 calc R . .
H29 H 0.7865 0.1162 0.8869 0.039 Uiso 1 1 calc R . .
C39 C 0.79907(19) 0.00356(10) 0.88063(12) 0.0311(4) Uani 1 1 d . . .
C40 C 0.7707(2) -0.03068(12) 0.95508(13) 0.0431(5) Uani 1 1 d . . .
H28 H 0.7942 -0.0076 1.0118 0.052 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
C1 C13 1.381(3) . ?
C1 C2 1.391(2) . ?
C1 H1 0.9500 . ?
C2 C3 1.380(2) . ?
C2 H32 0.9500 . ?
C3 C14 1.400(2) . ?
C3 C4 1.499(2) . ?
C4 C5 1.516(2) . ?
C4 H7 0.9900 . ?
C4 H6 0.9900 . ?
C5 C16 1.356(2) . ?
C5 C6 1.461(2) . ?
C6 C36 1.343(2) . ?
C6 C7 1.526(2) . ?
C7 C27 1.552(2) . ?
C7 C20 1.559(2) . ?
C7 C8 1.588(2) . ?
C8 C17 1.517(2) . ?
C8 C9 1.522(2) . ?
C8 H31 1.0000 . ?
C9 C10 1.388(2) . ?
C9 C39 1.393(2) . ?
C10 C11 1.394(2) . ?
C10 H26 0.9500 . ?
C11 C12 1.381(3) . ?
C11 H27 0.9500 . ?
C12 C40 1.378(3) . ?
C12 H2 0.9500 . ?
C13 C15 1.385(2) . ?
C13 H3 0.9500 . ?
C14 C15 1.391(2) . ?
C14 C16 1.454(2) . ?
C15 H4 0.9500 . ?
C16 H5 0.9500 . ?
C17 C18 1.336(2) . ?
C17 C38 1.508(2) . ?
C18 C37 1.497(2) . ?
C18 C19 1.526(2) . ?
C19 C20 1.532(2) . ?
C19 C35 1.561(2) . ?
C19 C28 1.586(2) . ?
C20 C21 1.514(2) . ?
C20 H14 1.0000 . ?
C21 C22 1.392(2) . ?
C21 C26 1.392(2) . ?
C22 C23 1.386(2) . ?
C22 H8 0.9500 . ?
C23 C24 1.386(3) . ?
C23 H13 0.9500 . ?
C24 C25 1.388(3) . ?
C24 H12 0.9500 . ?
C25 C26 1.386(2) . ?
C25 H11 0.9500 . ?
C26 C27 1.511(2) . ?
C27 H10 0.9900 . ?
C27 H9 0.9900 . ?
C28 C36 1.504(2) . ?
C28 C29 1.512(2) . ?
C28 H15 1.0000 . ?
C29 C30 1.383(2) . ?
C29 C34 1.389(2) . ?
C30 C31 1.387(2) . ?
C30 C35 1.498(2) . ?
C31 C32 1.379(2) . ?
C31 H19 0.9500 . ?
C32 C33 1.379(3) . ?
C32 H18 0.9500 . ?
C33 C34 1.390(2) . ?
C33 H17 0.9500 . ?
C34 H16 0.9500 . ?
C35 H20 0.9900 . ?
C35 H21 0.9900 . ?
C36 H22 0.9500 . ?
C37 H24 0.9800 . ?
C37 H23 0.9800 . ?
C37 H25 0.9800 . ?
C38 C39 1.499(3) . ?
C38 H30 0.9900 . ?
C38 H29 0.9900 . ?
C39 C40 1.388(2) . ?
C40 H28 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C13 C1 C2 121.11(17) . . ?
C13 C1 H1 119.4 . . ?
C2 C1 H1 119.4 . . ?
C3 C2 C1 118.86(17) . . ?
C3 C2 H32 120.6 . . ?
C1 C2 H32 120.6 . . ?
C2 C3 C14 120.36(16) . . ?
C2 C3 C4 131.13(16) . . ?
C14 C3 C4 108.50(14) . . ?
C3 C4 C5 103.85(13) . . ?
C3 C4 H7 111.0 . . ?
C5 C4 H7 111.0 . . ?
C3 C4 H6 111.0 . . ?
C5 C4 H6 111.0 . . ?
H7 C4 H6 109.0 . . ?
C16 C5 C6 129.88(15) . . ?
C16 C5 C4 108.48(14) . . ?
C6 C5 C4 121.64(14) . . ?
C36 C6 C5 119.85(15) . . ?
C36 C6 C7 116.06(14) . . ?
C5 C6 C7 124.02(14) . . ?
C6 C7 C27 118.89(13) . . ?
C6 C7 C20 106.09(12) . . ?
C27 C7 C20 101.19(13) . . ?
C6 C7 C8 107.64(13) . . ?
C27 C7 C8 113.48(13) . . ?
C20 C7 C8 108.77(13) . . ?
C17 C8 C9 102.86(13) . . ?
C17 C8 C7 114.63(13) . . ?
C9 C8 C7 122.79(14) . . ?
C17 C8 H31 105.0 . . ?
C9 C8 H31 105.0 . . ?
C7 C8 H31 105.0 . . ?
C10 C9 C39 119.36(16) . . ?
C10 C9 C8 129.44(16) . . ?
C39 C9 C8 110.67(15) . . ?
C9 C10 C11 119.36(18) . . ?
C9 C10 H26 120.3 . . ?
C11 C10 H26 120.3 . . ?
C12 C11 C10 120.75(19) . . ?
C12 C11 H27 119.6 . . ?
C10 C11 H27 119.6 . . ?
C40 C12 C11 120.07(18) . . ?
C40 C12 H2 120.0 . . ?
C11 C12 H2 120.0 . . ?
C1 C13 C15 120.24(17) . . ?
C1 C13 H3 119.9 . . ?
C15 C13 H3 119.9 . . ?
C15 C14 C3 120.20(16) . . ?
C15 C14 C16 131.48(16) . . ?
C3 C14 C16 108.26(15) . . ?
C13 C15 C14 119.19(17) . . ?
C13 C15 H4 120.4 . . ?
C14 C15 H4 120.4 . . ?
C5 C16 C14 110.71(15) . . ?
C5 C16 H5 124.6 . . ?
C14 C16 H5 124.6 . . ?
C18 C17 C38 126.43(15) . . ?
C18 C17 C8 123.29(15) . . ?
C38 C17 C8 110.27(14) . . ?
C17 C18 C37 120.40(16) . . ?
C17 C18 C19 117.40(14) . . ?
C37 C18 C19 121.98(15) . . ?
C18 C19 C20 106.22(13) . . ?
C18 C19 C35 114.64(13) . . ?
C20 C19 C35 110.51(14) . . ?
C18 C19 C28 112.72(13) . . ?
C20 C19 C28 107.42(13) . . ?
C35 C19 C28 105.18(13) . . ?
C21 C20 C19 119.96(13) . . ?
C21 C20 C7 103.22(13) . . ?
C19 C20 C7 112.13(13) . . ?
C21 C20 H14 106.9 . . ?
C19 C20 H14 106.9 . . ?
C7 C20 H14 106.9 . . ?
C22 C21 C26 120.19(16) . . ?
C22 C21 C20 131.26(16) . . ?
C26 C21 C20 108.49(14) . . ?
C23 C22 C21 119.05(17) . . ?
C23 C22 H8 120.5 . . ?
C21 C22 H8 120.5 . . ?
C22 C23 C24 120.59(17) . . ?
C22 C23 H13 119.7 . . ?
C24 C23 H13 119.7 . . ?
C23 C24 C25 120.55(17) . . ?
C23 C24 H12 119.7 . . ?
C25 C24 H12 119.7 . . ?
C26 C25 C24 119.00(17) . . ?
C26 C25 H11 120.5 . . ?
C24 C25 H11 120.5 . . ?
C25 C26 C21 120.59(16) . . ?
C25 C26 C27 128.85(16) . . ?
C21 C26 C27 110.54(14) . . ?
C26 C27 C7 103.07(13) . . ?
C26 C27 H10 111.1 . . ?
C7 C27 H10 111.1 . . ?
C26 C27 H9 111.1 . . ?
C7 C27 H9 111.1 . . ?
H10 C27 H9 109.1 . . ?
C36 C28 C29 112.94(13) . . ?
C36 C28 C19 116.11(13) . . ?
C29 C28 C19 104.73(13) . . ?
C36 C28 H15 107.6 . . ?
C29 C28 H15 107.6 . . ?
C19 C28 H15 107.6 . . ?
C30 C29 C34 120.28(16) . . ?
C30 C29 C28 112.01(14) . . ?
C34 C29 C28 127.71(16) . . ?
C29 C30 C31 120.46(16) . . ?
C29 C30 C35 111.37(15) . . ?
C31 C30 C35 128.16(16) . . ?
C32 C31 C30 119.26(17) . . ?
C32 C31 H19 120.4 . . ?
C30 C31 H19 120.4 . . ?
C31 C32 C33 120.45(18) . . ?
C31 C32 H18 119.8 . . ?
C33 C32 H18 119.8 . . ?
C32 C33 C34 120.71(17) . . ?
C32 C33 H17 119.6 . . ?
C34 C33 H17 119.6 . . ?
C29 C34 C33 118.74(17) . . ?
C29 C34 H16 120.6 . . ?
C33 C34 H16 120.6 . . ?
C30 C35 C19 106.43(14) . . ?
C30 C35 H20 110.4 . . ?
C19 C35 H20 110.4 . . ?
C30 C35 H21 110.4 . . ?
C19 C35 H21 110.4 . . ?
H20 C35 H21 108.6 . . ?
C6 C36 C28 126.42(15) . . ?
C6 C36 H22 116.8 . . ?
C28 C36 H22 116.8 . . ?
C18 C37 H24 109.5 . . ?
C18 C37 H23 109.5 . . ?
H24 C37 H23 109.5 . . ?
C18 C37 H25 109.5 . . ?
H24 C37 H25 109.5 . . ?
H23 C37 H25 109.5 . . ?
C39 C38 C17 103.54(14) . . ?
C39 C38 H30 111.1 . . ?
C17 C38 H30 111.1 . . ?
C39 C38 H29 111.1 . . ?
C17 C38 H29 111.1 . . ?
H30 C38 H29 109.0 . . ?
C40 C39 C9 120.74(18) . . ?
C40 C39 C38 127.54(17) . . ?
C9 C39 C38 111.62(15) . . ?
C12 C40 C39 119.56(19) . . ?
C12 C40 H28 120.2 . . ?
C39 C40 H28 120.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C13 C1 C2 C3 0.1(3) . . . . ?
C1 C2 C3 C14 1.5(3) . . . . ?
C1 C2 C3 C4 179.84(17) . . . . ?
C2 C3 C4 C5 -173.93(17) . . . . ?
C14 C3 C4 C5 4.57(18) . . . . ?
C3 C4 C5 C16 -3.96(19) . . . . ?
C3 C4 C5 C6 176.45(14) . . . . ?
C16 C5 C6 C36 -169.00(18) . . . . ?
C4 C5 C6 C36 10.5(2) . . . . ?
C16 C5 C6 C7 7.6(3) . . . . ?
C4 C5 C6 C7 -172.91(15) . . . . ?
C36 C6 C7 C27 -152.60(15) . . . . ?
C5 C6 C7 C27 30.7(2) . . . . ?
C36 C6 C7 C20 -39.66(19) . . . . ?
C5 C6 C7 C20 143.61(15) . . . . ?
C36 C6 C7 C8 76.64(18) . . . . ?
C5 C6 C7 C8 -100.09(17) . . . . ?
C6 C7 C8 C17 -116.95(15) . . . . ?
C27 C7 C8 C17 109.36(16) . . . . ?
C20 C7 C8 C17 -2.42(18) . . . . ?
C6 C7 C8 C9 117.15(16) . . . . ?
C27 C7 C8 C9 -16.5(2) . . . . ?
C20 C7 C8 C9 -128.32(16) . . . . ?
C17 C8 C9 C10 177.07(17) . . . . ?
C7 C8 C9 C10 -52.0(3) . . . . ?
C17 C8 C9 C39 5.60(18) . . . . ?
C7 C8 C9 C39 136.56(16) . . . . ?
C39 C9 C10 C11 -4.2(3) . . . . ?
C8 C9 C10 C11 -175.03(17) . . . . ?
C9 C10 C11 C12 1.1(3) . . . . ?
C10 C11 C12 C40 1.7(3) . . . . ?
C2 C1 C13 C15 -0.8(3) . . . . ?
C2 C3 C14 C15 -2.3(3) . . . . ?
C4 C3 C14 C15 178.98(16) . . . . ?
C2 C3 C14 C16 175.10(15) . . . . ?
C4 C3 C14 C16 -3.58(19) . . . . ?
C1 C13 C15 C14 0.0(3) . . . . ?
C3 C14 C15 C13 1.6(3) . . . . ?
C16 C14 C15 C13 -175.20(18) . . . . ?
C6 C5 C16 C14 -178.49(16) . . . . ?
C4 C5 C16 C14 2.0(2) . . . . ?
C15 C14 C16 C5 178.05(18) . . . . ?
C3 C14 C16 C5 1.0(2) . . . . ?
C9 C8 C17 C18 169.18(16) . . . . ?
C7 C8 C17 C18 33.5(2) . . . . ?
C9 C8 C17 C38 -9.79(18) . . . . ?
C7 C8 C17 C38 -145.49(14) . . . . ?
C38 C17 C18 C37 -7.4(3) . . . . ?
C8 C17 C18 C37 173.85(16) . . . . ?
C38 C17 C18 C19 167.43(16) . . . . ?
C8 C17 C18 C19 -11.4(2) . . . . ?
C17 C18 C19 C20 -38.0(2) . . . . ?
C37 C18 C19 C20 136.69(16) . . . . ?
C17 C18 C19 C35 -160.34(15) . . . . ?
C37 C18 C19 C35 14.4(2) . . . . ?
C17 C18 C19 C28 79.37(19) . . . . ?
C37 C18 C19 C28 -105.93(18) . . . . ?
C18 C19 C20 C21 -53.34(19) . . . . ?
C35 C19 C20 C21 71.58(18) . . . . ?
C28 C19 C20 C21 -174.19(13) . . . . ?
C18 C19 C20 C7 67.95(16) . . . . ?
C35 C19 C20 C7 -167.13(13) . . . . ?
C28 C19 C20 C7 -52.90(16) . . . . ?
C6 C7 C20 C21 -160.04(12) . . . . ?
C27 C7 C20 C21 -35.32(15) . . . . ?
C8 C7 C20 C21 84.43(15) . . . . ?
C6 C7 C20 C19 69.47(16) . . . . ?
C27 C7 C20 C19 -165.81(13) . . . . ?
C8 C7 C20 C19 -46.06(17) . . . . ?
C19 C20 C21 C22 -32.8(3) . . . . ?
C7 C20 C21 C22 -158.36(16) . . . . ?
C19 C20 C21 C26 150.29(15) . . . . ?
C7 C20 C21 C26 24.70(16) . . . . ?
C26 C21 C22 C23 1.8(2) . . . . ?
C20 C21 C22 C23 -174.84(16) . . . . ?
C21 C22 C23 C24 -0.7(3) . . . . ?
C22 C23 C24 C25 -0.4(3) . . . . ?
C23 C24 C25 C26 0.3(3) . . . . ?
C24 C25 C26 C21 0.9(3) . . . . ?
C24 C25 C26 C27 179.03(16) . . . . ?
C22 C21 C26 C25 -1.9(2) . . . . ?
C20 C21 C26 C25 175.40(15) . . . . ?
C22 C21 C26 C27 179.59(14) . . . . ?
C20 C21 C26 C27 -3.06(18) . . . . ?
C25 C26 C27 C7 161.78(17) . . . . ?
C21 C26 C27 C7 -19.92(17) . . . . ?
C6 C7 C27 C26 148.93(14) . . . . ?
C20 C7 C27 C26 33.35(15) . . . . ?
C8 C7 C27 C26 -82.97(16) . . . . ?
C18 C19 C28 C36 -105.87(16) . . . . ?
C20 C19 C28 C36 10.79(19) . . . . ?
C35 C19 C28 C36 128.54(15) . . . . ?
C18 C19 C28 C29 128.84(14) . . . . ?
C20 C19 C28 C29 -114.50(14) . . . . ?
C35 C19 C28 C29 3.25(16) . . . . ?
C36 C28 C29 C30 -132.63(15) . . . . ?
C19 C28 C29 C30 -5.38(18) . . . . ?
C36 C28 C29 C34 48.2(2) . . . . ?
C19 C28 C29 C34 175.45(15) . . . . ?
C34 C29 C30 C31 3.4(2) . . . . ?
C28 C29 C30 C31 -175.83(15) . . . . ?
C34 C29 C30 C35 -175.35(15) . . . . ?
C28 C29 C30 C35 5.4(2) . . . . ?
C29 C30 C31 C32 -2.6(3) . . . . ?
C35 C30 C31 C32 175.98(17) . . . . ?
C30 C31 C32 C33 -0.4(3) . . . . ?
C31 C32 C33 C34 2.5(3) . . . . ?
C30 C29 C34 C33 -1.3(2) . . . . ?
C28 C29 C34 C33 177.81(16) . . . . ?
C32 C33 C34 C29 -1.6(3) . . . . ?
C29 C30 C35 C19 -3.00(19) . . . . ?
C31 C30 C35 C19 178.36(16) . . . . ?
C18 C19 C35 C30 -124.77(15) . . . . ?
C20 C19 C35 C30 115.25(15) . . . . ?
C28 C19 C35 C30 -0.39(17) . . . . ?
C5 C6 C36 C28 175.70(16) . . . . ?
C7 C6 C36 C28 -1.2(3) . . . . ?
C29 C28 C36 C6 138.46(17) . . . . ?
C19 C28 C36 C6 17.5(2) . . . . ?
C18 C17 C38 C39 -168.75(17) . . . . ?
C8 C17 C38 C39 10.18(18) . . . . ?
C10 C9 C39 C40 4.6(3) . . . . ?
C8 C9 C39 C40 177.09(17) . . . . ?
C10 C9 C39 C38 -171.83(16) . . . . ?
C8 C9 C39 C38 0.6(2) . . . . ?
C17 C38 C39 C40 177.22(19) . . . . ?
C17 C38 C39 C9 -6.6(2) . . . . ?
C11 C12 C40 C39 -1.3(3) . . . . ?
C9 C39 C40 C12 -1.9(3) . . . . ?
C38 C39 C40 C12 173.97(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.045
_database_code_depnum_ccdc_archive 'CCDC 1003255'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_t1_compound_14
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H41 Cl2 Zr'
_chemical_formula_weight         707.87

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma

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

_cell_length_a                   8.6369(5)
_cell_length_b                   11.7633(8)
_cell_length_c                   33.907(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3444.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1468
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9060
_exptl_absorpt_correction_T_max  0.9514
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            49060
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3196
_reflns_number_gt                2730
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0567P)²+35.1465P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3196
_refine_ls_number_parameters     202
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.1008
_refine_ls_wR_factor_ref         0.2457
_refine_ls_wR_factor_gt          0.2372
_refine_ls_goodness_of_fit_ref   1.251
_refine_ls_restrained_S_all      1.251
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.78689(12) 0.2500 0.42618(3) 0.0410(4) Uani 1 2 d S . .
Cl1 Cl 0.7039(4) 0.2500 0.49461(8) 0.0633(10) Uani 1 2 d S . .
Cl2 Cl 1.0644(3) 0.2500 0.42990(10) 0.0616(10) Uani 1 2 d S . .
C1 C 0.7024(10) 0.0369(9) 0.4299(2) 0.049(2) Uani 1 1 d . . .
C2 C 0.5816(9) 0.1054(8) 0.4130(2) 0.0397(19) Uani 1 1 d . . .
C3 C 0.6385(8) 0.1481(8) 0.3764(2) 0.0370(19) Uani 1 1 d . . .
C4 C 0.7942(9) 0.1086(8) 0.3711(2) 0.0408(19) Uani 1 1 d . . .
C5 C 0.8321(9) 0.0385(8) 0.4045(2) 0.041(2) Uani 1 1 d . . .
C6 C 0.7087(12) -0.0285(10) 0.4650(3) 0.065(3) Uani 1 1 d . . .
H6A H 0.6227 -0.0312 0.4824 0.078 Uiso 1 1 calc R . .
C7 C 0.8390(14) -0.0865(12) 0.4731(3) 0.081(4) Uani 1 1 d . . .
H7A H 0.8440 -0.1299 0.4967 0.098 Uiso 1 1 calc R . .
C8 C 0.9684(13) -0.0852(10) 0.4478(3) 0.072(3) Uani 1 1 d . . .
H8A H 1.0577 -0.1279 0.4547 0.086 Uiso 1 1 calc R . .
C9 C 0.9685(10) -0.0237(9) 0.4134(3) 0.054(2) Uani 1 1 d . . .
H9A H 1.0557 -0.0229 0.3963 0.065 Uiso 1 1 calc R . .
C10 C 0.5694(12) 0.2500 0.3569(3) 0.038(3) Uani 1 2 d S . .
C11 C 0.4537(12) 0.2500 0.3300(3) 0.042(3) Uani 1 2 d S . .
C12 C 0.3774(8) 0.1495(9) 0.3120(2) 0.042(2) Uani 1 1 d . . .
C13 C 0.3999(10) 0.0355(10) 0.3178(2) 0.055(3) Uani 1 1 d . . .
H13A H 0.4731 0.0091 0.3366 0.066 Uiso 1 1 calc R . .
C14 C 0.3134(12) -0.0408(11) 0.2957(3) 0.070(3) Uani 1 1 d . . .
H14A H 0.3284 -0.1202 0.2990 0.084 Uiso 1 1 calc R . .
C15 C 0.2049(13) -0.0017(13) 0.2685(3) 0.077(4) Uani 1 1 d . . .
H15A H 0.1457 -0.0549 0.2538 0.093 Uiso 1 1 calc R . .
C16 C 0.1824(10) 0.1115(12) 0.2628(2) 0.065(3) Uani 1 1 d . . .
H16A H 0.1087 0.1376 0.2441 0.078 Uiso 1 1 calc R . .
C17 C 0.2677(8) 0.1878(9) 0.2845(2) 0.052(3) Uani 1 1 d . . .
C18 C 0.8936(11) 0.1147(10) 0.3342(2) 0.058(3) Uani 1 1 d . . .
H18A H 0.9167 0.0378 0.3249 0.087 Uiso 1 1 d . . .
H18B H 0.9912 0.1541 0.3403 0.087 Uiso 1 1 d . . .
H18C H 0.8386 0.1568 0.3136 0.087 Uiso 1 1 d . . .
C19 C 0.4198(10) 0.1102(10) 0.4287(3) 0.059(3) Uani 1 1 d . . .
H19A H 0.3785 0.0328 0.4309 0.088 Uiso 1 1 d . . .
H19B H 0.3549 0.1549 0.4110 0.088 Uiso 1 1 d . . .
H19C H 0.4208 0.1455 0.4550 0.088 Uiso 1 1 d . . .
C51 C -0.025(3) -0.2500 0.3101(8) 0.144(10) Uiso 0.50 1 d PD A 2
H51A H 0.0638 -0.2500 0.3279 0.216 Uiso 0.25 1 calc PR A 2
H51B H -0.0221 -0.1820 0.2934 0.216 Uiso 0.50 1 calc PR A 2
H51C H -0.0221 -0.3180 0.2934 0.216 Uiso 0.50 1 calc PR A 2
C52 C -0.175(3) -0.2500 0.3342(12) 0.26(2) Uiso 0.50 1 d PD A 2
H52A H -0.1611 -0.3167 0.3516 0.308 Uiso 0.50 1 calc PR A 2
H52B H -0.1611 -0.1833 0.3516 0.308 Uiso 0.50 1 calc PR A 2
C53 C -0.348(4) -0.2500 0.3270(9) 0.218(17) Uiso 0.50 1 d PD A 2
H53A H -0.3848 -0.3191 0.3131 0.261 Uiso 0.50 1 calc PR A 2
H53B H -0.3848 -0.1809 0.3131 0.261 Uiso 0.50 1 calc PR A 2
C54 C -0.389(4) -0.2500 0.3713(10) 0.25(2) Uiso 0.50 1 d PD A 2
H54A H -0.3308 -0.3167 0.3811 0.294 Uiso 0.50 1 calc PR A 2
H54B H -0.3308 -0.1833 0.3811 0.294 Uiso 0.50 1 calc PR A 2
C55 C -0.532(2) -0.2500 0.3984(9) 0.168(12) Uiso 0.50 1 d PD A 2
H55A H -0.5179 -0.1829 0.4156 0.202 Uiso 0.50 1 calc PR A 2
H55B H -0.5179 -0.3171 0.4156 0.202 Uiso 0.50 1 calc PR A 2
C56 C -0.707(2) -0.2500 0.3885(6) 0.104(6) Uiso 0.50 1 d PD A 2
H56A H -0.7672 -0.2500 0.4130 0.156 Uiso 0.25 1 calc PR A 2
H56B H -0.7323 -0.3180 0.3731 0.156 Uiso 0.50 1 calc PR A 2
H56C H -0.7323 -0.1820 0.3731 0.156 Uiso 0.50 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 Cl2 2.400(3) . ?
Zr1 Cl1 2.428(3) . ?
Zr1 C3 2.436(7) . ?
Zr1 C3 2.436(7) 7_565 ?
Zr1 C2 2.498(9) . ?
Zr1 C2 2.498(8) 7_565 ?
Zr1 C4 2.502(8) . ?
Zr1 C4 2.502(8) 7_565 ?
Zr1 C1 2.614(10) . ?
Zr1 C1 2.614(10) 7_565 ?
Zr1 C5 2.624(9) . ?
Zr1 C5 2.624(9) 7_565 ?
C1 C5 1.414(11) . ?
C1 C6 1.418(12) . ?
C1 C2 1.437(11) . ?
C2 C3 1.429(10) . ?
C2 C19 1.496(11) . ?
C3 C4 1.434(11) . ?
C3 C10 1.492(10) . ?
C4 C5 1.438(11) . ?
C4 C18 1.518(11) . ?
C5 C9 1.419(11) . ?
C6 C7 1.345(14) . ?
C7 C8 1.409(15) . ?
C8 C9 1.374(14) . ?
C10 C11 1.354(14) . ?
C10 C3 1.492(10) 7_565 ?
C11 C12 1.485(11) . ?
C11 C12 1.485(11) 7_565 ?
C12 C13 1.369(14) . ?
C12 C17 1.403(11) . ?
C13 C14 1.388(13) . ?
C14 C15 1.392(16) . ?
C15 C16 1.360(17) . ?
C16 C17 1.375(13) . ?
C17 C17 1.46(2) 7_565 ?
C51 C52 1.529(10) . ?
C52 C53 1.518(10) . ?
C53 C54 1.545(10) . ?
C54 C55 1.539(10) . ?
C55 C56 1.546(10) . ?

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
Cl2 Zr1 Cl1 104.16(12) . . ?
Cl2 Zr1 C3 124.19(19) . . ?
Cl1 Zr1 C3 120.49(19) . . ?
Cl2 Zr1 C3 124.2(2) . 7_565 ?
Cl1 Zr1 C3 120.49(19) . 7_565 ?
C3 Zr1 C3 58.9(4) . 7_565 ?
Cl2 Zr1 C2 135.91(19) . . ?
Cl1 Zr1 C2 87.77(18) . . ?
C3 Zr1 C2 33.6(2) . . ?
C3 Zr1 C2 80.7(3) 7_565 . ?
Cl2 Zr1 C2 135.9(2) . 7_565 ?
Cl1 Zr1 C2 87.77(18) . 7_565 ?
C3 Zr1 C2 80.7(3) . 7_565 ?
C3 Zr1 C2 33.6(2) 7_565 7_565 ?
C2 Zr1 C2 85.9(4) . 7_565 ?
Cl2 Zr1 C4 90.81(18) . . ?
Cl1 Zr1 C4 136.1(2) . . ?
C3 Zr1 C4 33.7(2) . . ?
C3 Zr1 C4 79.8(3) 7_565 . ?
C2 Zr1 C4 55.4(3) . . ?
C2 Zr1 C4 109.7(3) 7_565 . ?
Cl2 Zr1 C4 90.81(19) . 7_565 ?
Cl1 Zr1 C4 136.1(2) . 7_565 ?
C3 Zr1 C4 79.8(3) . 7_565 ?
C3 Zr1 C4 33.7(2) 7_565 7_565 ?
C2 Zr1 C4 109.7(3) . 7_565 ?
C2 Zr1 C4 55.4(3) 7_565 7_565 ?
C4 Zr1 C4 83.3(4) . 7_565 ?
Cl2 Zr1 C1 106.03(18) . . ?
Cl1 Zr1 C1 82.62(17) . . ?
C3 Zr1 C1 54.2(3) . . ?
C3 Zr1 C1 111.0(3) 7_565 . ?
C2 Zr1 C1 32.6(3) . . ?
C2 Zr1 C1 117.6(3) 7_565 . ?
C4 Zr1 C1 53.5(3) . . ?
C4 Zr1 C1 132.9(3) 7_565 . ?
Cl2 Zr1 C1 106.03(18) . 7_565 ?
Cl1 Zr1 C1 82.62(17) . 7_565 ?
C3 Zr1 C1 111.0(3) . 7_565 ?
C3 Zr1 C1 54.2(3) 7_565 7_565 ?
C2 Zr1 C1 117.6(3) . 7_565 ?
C2 Zr1 C1 32.6(3) 7_565 7_565 ?
C4 Zr1 C1 132.9(3) . 7_565 ?
C4 Zr1 C1 53.5(3) 7_565 7_565 ?
C1 Zr1 C1 147.1(4) . 7_565 ?
Cl2 Zr1 C5 82.30(17) . . ?
Cl1 Zr1 C5 108.19(17) . . ?
C3 Zr1 C5 54.4(3) . . ?
C3 Zr1 C5 110.5(3) 7_565 . ?
C2 Zr1 C5 53.8(3) . . ?
C2 Zr1 C5 134.6(2) 7_565 . ?
C4 Zr1 C5 32.5(3) . . ?
C4 Zr1 C5 114.7(3) 7_565 . ?
C1 Zr1 C5 31.3(2) . . ?
C1 Zr1 C5 164.7(2) 7_565 . ?
Cl2 Zr1 C5 82.30(17) . 7_565 ?
Cl1 Zr1 C5 108.19(17) . 7_565 ?
C3 Zr1 C5 110.5(3) . 7_565 ?
C3 Zr1 C5 54.4(3) 7_565 7_565 ?
C2 Zr1 C5 134.6(2) . 7_565 ?
C2 Zr1 C5 53.8(3) 7_565 7_565 ?
C4 Zr1 C5 114.7(3) . 7_565 ?
C4 Zr1 C5 32.5(3) 7_565 7_565 ?
C1 Zr1 C5 164.7(2) . 7_565 ?
C1 Zr1 C5 31.3(2) 7_565 7_565 ?
C5 Zr1 C5 142.9(3) . 7_565 ?
C5 C1 C6 119.3(8) . . ?
C5 C1 C2 109.0(7) . . ?
C6 C1 C2 131.8(8) . . ?
C5 C1 Zr1 74.7(6) . . ?
C6 C1 Zr1 123.3(7) . . ?
C2 C1 Zr1 69.3(5) . . ?
C3 C2 C1 107.1(7) . . ?
C3 C2 C19 128.1(7) . . ?
C1 C2 C19 123.9(7) . . ?
C3 C2 Zr1 70.8(4) . . ?
C1 C2 Zr1 78.2(5) . . ?
C19 C2 Zr1 125.0(7) . . ?
C2 C3 C4 108.4(7) . . ?
C2 C3 C10 122.0(8) . . ?
C4 C3 C10 125.5(8) . . ?
C2 C3 Zr1 75.5(4) . . ?
C4 C3 Zr1 75.7(4) . . ?
C10 C3 Zr1 97.0(5) . . ?
C3 C4 C5 107.6(7) . . ?
C3 C4 C18 128.1(7) . . ?
C5 C4 C18 123.1(7) . . ?
C3 C4 Zr1 70.6(4) . . ?
C5 C4 Zr1 78.4(5) . . ?
C18 C4 Zr1 126.7(6) . . ?
C1 C5 C9 121.4(8) . . ?
C1 C5 C4 107.9(7) . . ?
C9 C5 C4 130.7(8) . . ?
C1 C5 Zr1 73.9(6) . . ?
C9 C5 Zr1 123.6(6) . . ?
C4 C5 Zr1 69.1(5) . . ?
C7 C6 C1 118.6(10) . . ?
C6 C7 C8 122.2(10) . . ?
C9 C8 C7 121.6(9) . . ?
C8 C9 C5 116.9(9) . . ?
C11 C10 C3 126.4(4) . 7_565 ?
C11 C10 C3 126.4(4) . . ?
C3 C10 C3 106.9(8) 7_565 . ?
C10 C11 C12 127.2(5) . . ?
C10 C11 C12 127.2(5) . 7_565 ?
C12 C11 C12 105.6(9) . 7_565 ?
C13 C12 C17 120.4(8) . . ?
C13 C12 C11 131.1(8) . . ?
C17 C12 C11 108.4(9) . . ?
C12 C13 C14 118.6(10) . . ?
C13 C14 C15 120.5(12) . . ?
C16 C15 C14 120.9(10) . . ?
C15 C16 C17 119.1(10) . . ?
C16 C17 C12 120.5(10) . . ?
C16 C17 C17 130.7(7) . 7_565 ?
C12 C17 C17 108.7(6) . 7_565 ?
C53 C52 C51 138(4) . . ?
C52 C53 C54 94(2) . . ?
C55 C54 C53 140(4) . . ?
C54 C55 C56 131(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.229
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.124
_database_code_depnum_ccdc_archive 'CCDC 1003256'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_tao009_0m_compound_16
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H28,0.5(C5 H12)'
_chemical_formula_sum            'C38.50 H34'
_chemical_formula_weight         496.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   8.9310(4)
_cell_length_b                   13.1050(7)
_cell_length_c                   23.2702(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.581(3)
_cell_angle_gamma                90.00
_cell_volume                     2722.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1060
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9865
_exptl_absorpt_correction_T_max  0.9966
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26802
_diffrn_reflns_av_R_equivalents  0.0438
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4804
_reflns_number_gt                3689
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0683P)²+3.0652P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4804
_refine_ls_number_parameters     345
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0569
_refine_ls_wR_factor_ref         0.1555
_refine_ls_wR_factor_gt          0.1408
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3407(3) 0.38207(19) -0.06304(11) 0.0307(6) Uani 1 1 d . . .
H1A H 0.2737 0.3880 -0.0953 0.037 Uiso 1 1 calc R . .
C2 C 0.2949(3) 0.41271(18) -0.00893(10) 0.0280(6) Uani 1 1 d . . .
H2A H 0.1976 0.4407 -0.0048 0.034 Uiso 1 1 calc R . .
C2A C 0.6540(3) 0.36217(16) 0.13288(9) 0.0198(5) Uani 1 1 d . . .
C3 C 0.3896(3) 0.40277(18) 0.03902(10) 0.0245(5) Uani 1 1 d . . .
H3A H 0.3581 0.4247 0.0757 0.029 Uiso 1 1 calc R . .
C4 C 0.5311(3) 0.36036(17) 0.03289(10) 0.0224(5) Uani 1 1 d . . .
C5 C 0.6568(3) 0.34504(17) 0.07466(9) 0.0202(5) Uani 1 1 d . . .
C7 C 0.5202(3) 0.36156(17) 0.16833(9) 0.0195(5) Uani 1 1 d . . .
C8 C 0.5531(2) 0.41256(16) 0.22644(9) 0.0183(5) Uani 1 1 d . . .
C9 C 0.4322(2) 0.36809(17) 0.26317(10) 0.0205(5) Uani 1 1 d . . .
C10 C 0.4011(3) 0.38367(18) 0.32022(10) 0.0256(5) Uani 1 1 d . . .
H10A H 0.4619 0.4277 0.3434 0.031 Uiso 1 1 calc R . .
C11 C 0.2788(3) 0.3336(2) 0.34321(11) 0.0290(6) Uani 1 1 d . . .
H11A H 0.2579 0.3422 0.3827 0.035 Uiso 1 1 calc R . .
C12 C 0.1873(3) 0.27135(19) 0.30925(11) 0.0291(6) Uani 1 1 d . . .
H12A H 0.1034 0.2390 0.3256 0.035 Uiso 1 1 calc R . .
C13 C 0.7822(3) 0.30667(17) 0.04076(10) 0.0223(5) Uani 1 1 d . . .
C14 C 0.9228(3) 0.26932(19) 0.05738(11) 0.0270(6) Uani 1 1 d . . .
H14A H 0.9550 0.2707 0.0966 0.032 Uiso 1 1 calc R . .
C15 C 1.0151(3) 0.2301(2) 0.01581(11) 0.0338(6) Uani 1 1 d . . .
H15A H 1.1118 0.2056 0.0268 0.041 Uiso 1 1 calc R . .
C16 C 0.9691(3) 0.2260(2) -0.04145(11) 0.0366(7) Uani 1 1 d . . .
H16A H 1.0350 0.1998 -0.0692 0.044 Uiso 1 1 calc R . .
C17 C 0.8278(3) 0.2597(2) -0.05859(11) 0.0316(6) Uani 1 1 d . . .
H17A H 0.7957 0.2559 -0.0978 0.038 Uiso 1 1 calc R . .
C18 C 0.7340(3) 0.29916(18) -0.01758(10) 0.0235(5) Uani 1 1 d . . .
C19 C 0.5782(3) 0.33339(17) -0.02246(10) 0.0232(5) Uani 1 1 d . . .
C20 C 0.4831(3) 0.34313(19) -0.07020(10) 0.0285(6) Uani 1 1 d . . .
H20A H 0.5151 0.3234 -0.1072 0.034 Uiso 1 1 calc R . .
C21 C 0.7760(2) 0.38592(16) 0.17477(9) 0.0188(5) Uani 1 1 d . . .
C22 C 0.7194(2) 0.37533(16) 0.23594(9) 0.0187(5) Uani 1 1 d . . .
C23 C 0.7261(3) 0.26416(17) 0.25701(10) 0.0232(5) Uani 1 1 d . . .
H23A H 0.8310 0.2434 0.2625 0.035 Uiso 1 1 calc R . .
H23B H 0.6769 0.2197 0.2284 0.035 Uiso 1 1 calc R . .
H23C H 0.6747 0.2585 0.2935 0.035 Uiso 1 1 calc R . .
C24 C 0.8296(2) 0.43963(16) 0.27028(10) 0.0197(5) Uani 1 1 d . . .
C25 C 0.8387(3) 0.46115(17) 0.32832(10) 0.0235(5) Uani 1 1 d . . .
H25A H 0.7643 0.4369 0.3533 0.028 Uiso 1 1 calc R . .
C26 C 0.9591(3) 0.51914(18) 0.34970(10) 0.0271(6) Uani 1 1 d . . .
H26A H 0.9651 0.5362 0.3894 0.032 Uiso 1 1 calc R . .
C27 C 1.0697(3) 0.55198(18) 0.31356(11) 0.0279(6) Uani 1 1 d . . .
H27A H 1.1513 0.5909 0.3288 0.033 Uiso 1 1 calc R . .
C28 C 1.0632(3) 0.52881(17) 0.25513(10) 0.0246(5) Uani 1 1 d . . .
H28A H 1.1400 0.5508 0.2306 0.030 Uiso 1 1 calc R . .
C29 C 0.9421(3) 0.47283(16) 0.23352(10) 0.0197(5) Uani 1 1 d . . .
C30 C 0.9044(3) 0.44191(17) 0.17396(10) 0.0204(5) Uani 1 1 d . . .
C31 C 0.4006(3) 0.29786(17) 0.17075(10) 0.0215(5) Uani 1 1 d . . .
C32 C 0.3461(3) 0.22211(19) 0.12728(10) 0.0303(6) Uani 1 1 d . . .
H32A H 0.4009 0.2309 0.0917 0.046 Uiso 1 1 calc R . .
H32B H 0.2389 0.2326 0.1194 0.046 Uiso 1 1 calc R . .
H32C H 0.3627 0.1529 0.1421 0.046 Uiso 1 1 calc R . .
C33 C 0.3396(3) 0.30453(17) 0.22867(10) 0.0210(5) Uani 1 1 d . . .
C34 C 0.2166(3) 0.25575(18) 0.25169(10) 0.0249(5) Uani 1 1 d . . .
H34A H 0.1541 0.2128 0.2285 0.030 Uiso 1 1 calc R . .
C35 C 0.5427(3) 0.52944(17) 0.22404(10) 0.0229(5) Uani 1 1 d . . .
H35A H 0.4378 0.5498 0.2180 0.034 Uiso 1 1 calc R . .
H35B H 0.6019 0.5549 0.1922 0.034 Uiso 1 1 calc R . .
H35C H 0.5816 0.5583 0.2603 0.034 Uiso 1 1 calc R . .
C36 C 0.9916(3) 0.47942(19) 0.12437(10) 0.0272(6) Uani 1 1 d . . .
H36A H 0.9494 0.4506 0.0886 0.041 Uiso 1 1 calc R . .
H36B H 1.0964 0.4582 0.1293 0.041 Uiso 1 1 calc R . .
H36C H 0.9862 0.5541 0.1227 0.041 Uiso 1 1 calc R . .
C101 C 0.7476(13) 0.5102(9) 0.5021(5) 0.089(3) Uiso 0.50 1 d P A -2
H10B H 0.8475 0.4806 0.5084 0.133 Uiso 0.50 1 calc PR A -2
H10C H 0.7515 0.5836 0.5102 0.133 Uiso 0.50 1 calc PR A -2
H10D H 0.7147 0.4994 0.4621 0.133 Uiso 0.50 1 calc PR A -2
C102 C 0.6388(10) 0.4596(7) 0.5416(4) 0.075(2) Uiso 0.50 1 d P A -2
H10E H 0.6725 0.4711 0.5820 0.090 Uiso 0.50 1 calc PR A -2
H10F H 0.6390 0.3852 0.5345 0.090 Uiso 0.50 1 calc PR A -2
C103 C 0.4799(9) 0.5001(6) 0.5332(3) 0.070(2) Uiso 0.50 1 d P A -2
H10G H 0.4272 0.4863 0.5693 0.085 Uiso 0.50 1 calc PR A -2
H10H H 0.4874 0.5751 0.5296 0.085 Uiso 0.50 1 calc PR A -2
C104 C 0.3911(14) 0.4680(10) 0.4904(5) 0.117(4) Uiso 0.50 1 d P A -2
H10L H 0.3732 0.3945 0.4973 0.140 Uiso 0.50 1 calc PR A -2
H10M H 0.4506 0.4722 0.4552 0.140 Uiso 0.50 1 calc PR A -2
C105 C 0.2405(9) 0.5140(6) 0.4752(4) 0.058(2) Uiso 0.50 1 d P A -2
H10I H 0.1949 0.4771 0.4426 0.087 Uiso 0.50 1 calc PR A -2
H10J H 0.2532 0.5859 0.4650 0.087 Uiso 0.50 1 calc PR A -2
H10K H 0.1755 0.5089 0.5084 0.087 Uiso 0.50 1 calc PR A -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C20 1.385(4) . ?
C1 C2 1.394(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.387(3) . ?
C2 H2A 0.9500 . ?
C2A C5 1.374(3) . ?
C2A C7 1.471(3) . ?
C2A C21 1.475(3) . ?
C3 C4 1.392(3) . ?
C3 H3A 0.9500 . ?
C4 C19 1.411(3) . ?
C4 C5 1.478(3) . ?
C5 C13 1.476(3) . ?
C7 C31 1.358(3) . ?
C7 C8 1.530(3) . ?
C8 C9 1.512(3) . ?
C8 C35 1.535(3) . ?
C8 C22 1.573(3) . ?
C9 C10 1.379(3) . ?
C9 C33 1.409(3) . ?
C10 C11 1.393(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.386(4) . ?
C11 H11A 0.9500 . ?
C12 C34 1.387(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.393(3) . ?
C13 C18 1.416(3) . ?
C14 C15 1.387(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.384(4) . ?
C15 H15A 0.9500 . ?
C16 C17 1.386(4) . ?
C16 H16A 0.9500 . ?
C17 C18 1.387(3) . ?
C17 H17A 0.9500 . ?
C18 C19 1.463(3) . ?
C19 C20 1.386(3) . ?
C20 H20A 0.9500 . ?
C21 C30 1.362(3) . ?
C21 C22 1.530(3) . ?
C22 C24 1.508(3) . ?
C22 C23 1.538(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.380(3) . ?
C24 C29 1.406(3) . ?
C25 C26 1.397(3) . ?
C25 H25A 0.9500 . ?
C26 C27 1.383(4) . ?
C26 H26A 0.9500 . ?
C27 C28 1.393(3) . ?
C27 H27A 0.9500 . ?
C28 C29 1.389(3) . ?
C28 H28A 0.9500 . ?
C29 C30 1.474(3) . ?
C30 C36 1.493(3) . ?
C31 C33 1.470(3) . ?
C31 C32 1.490(3) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C34 1.391(3) . ?
C34 H34A 0.9500 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C101 C102 1.509(13) . ?
C101 H10B 0.9800 . ?
C101 H10C 0.9800 . ?
C101 H10D 0.9800 . ?
C102 C103 1.523(11) . ?
C102 H10E 0.9900 . ?
C102 H10F 0.9900 . ?
C103 C104 1.325(12) . ?
C103 H10G 0.9900 . ?
C103 H10H 0.9900 . ?
C104 C105 1.507(14) . ?
C104 H10L 0.9900 . ?
C104 H10M 0.9900 . ?
C105 H10I 0.9800 . ?
C105 H10J 0.9800 . ?
C105 H10K 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
C20 C1 C2 120.6(2) . . ?
C20 C1 H1A 119.7 . . ?
C2 C1 H1A 119.7 . . ?
C3 C2 C1 120.8(2) . . ?
C3 C2 H2A 119.6 . . ?
C1 C2 H2A 119.6 . . ?
C5 C2A C7 126.1(2) . . ?
C5 C2A C21 130.8(2) . . ?
C7 C2A C21 103.13(18) . . ?
C2 C3 C4 119.4(2) . . ?
C2 C3 H3A 120.3 . . ?
C4 C3 H3A 120.3 . . ?
C3 C4 C19 119.2(2) . . ?
C3 C4 C5 131.5(2) . . ?
C19 C4 C5 109.0(2) . . ?
C2A C5 C13 128.1(2) . . ?
C2A C5 C4 126.3(2) . . ?
C13 C5 C4 105.58(19) . . ?
C31 C7 C2A 132.8(2) . . ?
C31 C7 C8 111.34(19) . . ?
C2A C7 C8 110.76(19) . . ?
C9 C8 C7 102.04(18) . . ?
C9 C8 C35 111.18(18) . . ?
C7 C8 C35 113.18(18) . . ?
C9 C8 C22 119.17(18) . . ?
C7 C8 C22 98.41(17) . . ?
C35 C8 C22 111.76(18) . . ?
C10 C9 C33 120.4(2) . . ?
C10 C9 C8 130.7(2) . . ?
C33 C9 C8 108.83(19) . . ?
C9 C10 C11 118.7(2) . . ?
C9 C10 H10A 120.6 . . ?
C11 C10 H10A 120.6 . . ?
C12 C11 C10 120.9(2) . . ?
C12 C11 H11A 119.5 . . ?
C10 C11 H11A 119.5 . . ?
C11 C12 C34 120.9(2) . . ?
C11 C12 H12A 119.6 . . ?
C34 C12 H12A 119.6 . . ?
C14 C13 C18 119.3(2) . . ?
C14 C13 C5 131.5(2) . . ?
C18 C13 C5 108.7(2) . . ?
C15 C14 C13 119.0(2) . . ?
C15 C14 H14A 120.5 . . ?
C13 C14 H14A 120.5 . . ?
C16 C15 C14 121.3(2) . . ?
C16 C15 H15A 119.3 . . ?
C14 C15 H15A 119.3 . . ?
C15 C16 C17 120.5(2) . . ?
C15 C16 H16A 119.7 . . ?
C17 C16 H16A 119.7 . . ?
C16 C17 C18 118.9(2) . . ?
C16 C17 H17A 120.5 . . ?
C18 C17 H17A 120.5 . . ?
C17 C18 C13 120.8(2) . . ?
C17 C18 C19 130.7(2) . . ?
C13 C18 C19 108.4(2) . . ?
C20 C19 C4 121.1(2) . . ?
C20 C19 C18 130.6(2) . . ?
C4 C19 C18 108.2(2) . . ?
C1 C20 C19 118.8(2) . . ?
C1 C20 H20A 120.6 . . ?
C19 C20 H20A 120.6 . . ?
C30 C21 C2A 135.3(2) . . ?
C30 C21 C22 111.21(19) . . ?
C2A C21 C22 109.80(19) . . ?
C24 C22 C21 102.40(18) . . ?
C24 C22 C23 109.96(18) . . ?
C21 C22 C23 111.81(18) . . ?
C24 C22 C8 120.08(18) . . ?
C21 C22 C8 100.14(17) . . ?
C23 C22 C8 111.52(18) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 C29 120.6(2) . . ?
C25 C24 C22 130.7(2) . . ?
C29 C24 C22 108.50(19) . . ?
C24 C25 C26 118.9(2) . . ?
C24 C25 H25A 120.5 . . ?
C26 C25 H25A 120.5 . . ?
C27 C26 C25 120.5(2) . . ?
C27 C26 H26A 119.7 . . ?
C25 C26 H26A 119.7 . . ?
C26 C27 C28 121.0(2) . . ?
C26 C27 H27A 119.5 . . ?
C28 C27 H27A 119.5 . . ?
C29 C28 C27 118.7(2) . . ?
C29 C28 H28A 120.7 . . ?
C27 C28 H28A 120.7 . . ?
C28 C29 C24 120.3(2) . . ?
C28 C29 C30 129.8(2) . . ?
C24 C29 C30 109.79(19) . . ?
C21 C30 C29 107.79(19) . . ?
C21 C30 C36 130.2(2) . . ?
C29 C30 C36 121.7(2) . . ?
C7 C31 C33 108.2(2) . . ?
C7 C31 C32 128.6(2) . . ?
C33 C31 C32 122.7(2) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C34 C33 C9 120.6(2) . . ?
C34 C33 C31 129.9(2) . . ?
C9 C33 C31 109.35(19) . . ?
C12 C34 C33 118.4(2) . . ?
C12 C34 H34A 120.8 . . ?
C33 C34 H34A 120.8 . . ?
C8 C35 H35A 109.5 . . ?
C8 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C8 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C30 C36 H36A 109.5 . . ?
C30 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C30 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C102 C101 H10B 109.5 . . ?
C102 C101 H10C 109.5 . . ?
H10B C101 H10C 109.5 . . ?
C102 C101 H10D 109.5 . . ?
H10B C101 H10D 109.5 . . ?
H10C C101 H10D 109.5 . . ?
C101 C102 C103 112.5(8) . . ?
C101 C102 H10E 109.1 . . ?
C103 C102 H10E 109.1 . . ?
C101 C102 H10F 109.1 . . ?
C103 C102 H10F 109.1 . . ?
H10E C102 H10F 107.8 . . ?
C104 C103 C102 121.5(9) . . ?
C104 C103 H10G 107.0 . . ?
C102 C103 H10G 107.0 . . ?
C104 C103 H10H 107.0 . . ?
C102 C103 H10H 107.0 . . ?
H10G C103 H10H 106.7 . . ?
C103 C104 C105 124.1(10) . . ?
C103 C104 H10L 106.3 . . ?
C105 C104 H10L 106.3 . . ?
C103 C104 H10M 106.3 . . ?
C105 C104 H10M 106.3 . . ?
H10L C104 H10M 106.4 . . ?
C104 C105 H10I 109.5 . . ?
C104 C105 H10J 109.5 . . ?
H10I C105 H10J 109.5 . . ?
C104 C105 H10K 109.5 . . ?
H10I C105 H10K 109.5 . . ?
H10J C105 H10K 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C20 C1 C2 C3 -1.4(4) . . . . ?
C1 C2 C3 C4 -0.9(4) . . . . ?
C2 C3 C4 C19 3.4(3) . . . . ?
C2 C3 C4 C5 176.5(2) . . . . ?
C7 C2A C5 C13 -154.7(2) . . . . ?
C21 C2A C5 C13 26.0(4) . . . . ?
C7 C2A C5 C4 24.3(4) . . . . ?
C21 C2A C5 C4 -155.0(2) . . . . ?
C3 C4 C5 C2A 6.9(4) . . . . ?
C19 C4 C5 C2A -179.4(2) . . . . ?
C3 C4 C5 C13 -173.9(2) . . . . ?
C19 C4 C5 C13 -0.3(2) . . . . ?
C5 C2A C7 C31 44.4(4) . . . . ?
C21 C2A C7 C31 -136.2(3) . . . . ?
C5 C2A C7 C8 -163.9(2) . . . . ?
C21 C2A C7 C8 15.5(2) . . . . ?
C31 C7 C8 C9 -0.1(2) . . . . ?
C2A C7 C8 C9 -158.20(18) . . . . ?
C31 C7 C8 C35 -119.7(2) . . . . ?
C2A C7 C8 C35 82.3(2) . . . . ?
C31 C7 C8 C22 122.2(2) . . . . ?
C2A C7 C8 C22 -35.8(2) . . . . ?
C7 C8 C9 C10 179.9(2) . . . . ?
C35 C8 C9 C10 -59.2(3) . . . . ?
C22 C8 C9 C10 73.0(3) . . . . ?
C7 C8 C9 C33 -2.7(2) . . . . ?
C35 C8 C9 C33 118.3(2) . . . . ?
C22 C8 C9 C33 -109.5(2) . . . . ?
C33 C9 C10 C11 1.5(3) . . . . ?
C8 C9 C10 C11 178.7(2) . . . . ?
C9 C10 C11 C12 -1.8(4) . . . . ?
C10 C11 C12 C34 1.2(4) . . . . ?
C2A C5 C13 C14 6.6(4) . . . . ?
C4 C5 C13 C14 -172.5(2) . . . . ?
C2A C5 C13 C18 178.9(2) . . . . ?
C4 C5 C13 C18 -0.2(2) . . . . ?
C18 C13 C14 C15 3.1(4) . . . . ?
C5 C13 C14 C15 174.7(2) . . . . ?
C13 C14 C15 C16 -1.1(4) . . . . ?
C14 C15 C16 C17 -1.0(4) . . . . ?
C15 C16 C17 C18 1.0(4) . . . . ?
C16 C17 C18 C13 1.1(4) . . . . ?
C16 C17 C18 C19 -175.3(2) . . . . ?
C14 C13 C18 C17 -3.1(3) . . . . ?
C5 C13 C18 C17 -176.5(2) . . . . ?
C14 C13 C18 C19 174.0(2) . . . . ?
C5 C13 C18 C19 0.6(3) . . . . ?
C3 C4 C19 C20 -3.6(3) . . . . ?
C5 C4 C19 C20 -178.2(2) . . . . ?
C3 C4 C19 C18 175.2(2) . . . . ?
C5 C4 C19 C18 0.6(2) . . . . ?
C17 C18 C19 C20 -5.3(4) . . . . ?
C13 C18 C19 C20 177.9(2) . . . . ?
C17 C18 C19 C4 176.0(2) . . . . ?
C13 C18 C19 C4 -0.8(3) . . . . ?
C2 C1 C20 C19 1.2(4) . . . . ?
C4 C19 C20 C1 1.3(3) . . . . ?
C18 C19 C20 C1 -177.2(2) . . . . ?
C5 C2A C21 C30 36.4(4) . . . . ?
C7 C2A C21 C30 -143.0(3) . . . . ?
C5 C2A C21 C22 -167.9(2) . . . . ?
C7 C2A C21 C22 12.7(2) . . . . ?
C30 C21 C22 C24 3.5(2) . . . . ?
C2A C21 C22 C24 -158.48(18) . . . . ?
C30 C21 C22 C23 -114.2(2) . . . . ?
C2A C21 C22 C23 83.8(2) . . . . ?
C30 C21 C22 C8 127.56(19) . . . . ?
C2A C21 C22 C8 -34.4(2) . . . . ?
C9 C8 C22 C24 -100.5(2) . . . . ?
C7 C8 C22 C24 150.6(2) . . . . ?
C35 C8 C22 C24 31.4(3) . . . . ?
C9 C8 C22 C21 148.68(19) . . . . ?
C7 C8 C22 C21 39.78(19) . . . . ?
C35 C8 C22 C21 -79.4(2) . . . . ?
C9 C8 C22 C23 30.2(3) . . . . ?
C7 C8 C22 C23 -78.7(2) . . . . ?
C35 C8 C22 C23 162.17(18) . . . . ?
C21 C22 C24 C25 179.7(2) . . . . ?
C23 C22 C24 C25 -61.3(3) . . . . ?
C8 C22 C24 C25 70.1(3) . . . . ?
C21 C22 C24 C29 -5.4(2) . . . . ?
C23 C22 C24 C29 113.6(2) . . . . ?
C8 C22 C24 C29 -115.0(2) . . . . ?
C29 C24 C25 C26 1.9(3) . . . . ?
C22 C24 C25 C26 176.3(2) . . . . ?
C24 C25 C26 C27 -1.8(3) . . . . ?
C25 C26 C27 C28 0.5(4) . . . . ?
C26 C27 C28 C29 0.7(3) . . . . ?
C27 C28 C29 C24 -0.6(3) . . . . ?
C27 C28 C29 C30 177.1(2) . . . . ?
C25 C24 C29 C28 -0.7(3) . . . . ?
C22 C24 C29 C28 -176.2(2) . . . . ?
C25 C24 C29 C30 -178.9(2) . . . . ?
C22 C24 C29 C30 5.6(2) . . . . ?
C2A C21 C30 C29 155.2(2) . . . . ?
C22 C21 C30 C29 -0.3(2) . . . . ?
C2A C21 C30 C36 -18.5(4) . . . . ?
C22 C21 C30 C36 -174.0(2) . . . . ?
C28 C29 C30 C21 178.7(2) . . . . ?
C24 C29 C30 C21 -3.4(3) . . . . ?
C28 C29 C30 C36 -6.9(4) . . . . ?
C24 C29 C30 C36 171.0(2) . . . . ?
C2A C7 C31 C33 154.3(2) . . . . ?
C8 C7 C31 C33 2.8(3) . . . . ?
C2A C7 C31 C32 -18.0(4) . . . . ?
C8 C7 C31 C32 -169.5(2) . . . . ?
C10 C9 C33 C34 -0.7(3) . . . . ?
C8 C9 C33 C34 -178.4(2) . . . . ?
C10 C9 C33 C31 -177.8(2) . . . . ?
C8 C9 C33 C31 4.4(2) . . . . ?
C7 C31 C33 C34 178.7(2) . . . . ?
C32 C31 C33 C34 -8.5(4) . . . . ?
C7 C31 C33 C9 -4.5(3) . . . . ?
C32 C31 C33 C9 168.3(2) . . . . ?
C11 C12 C34 C33 -0.4(4) . . . . ?
C9 C33 C34 C12 0.1(3) . . . . ?
C31 C33 C34 C12 176.6(2) . . . . ?
C101 C102 C103 C104 80.0(13) . . . . ?
C102 C103 C104 C105 -172.0(9) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.054
_database_code_depnum_ccdc_archive 'CCDC 1003257'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_yus001_0m_compund_22
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H28 Zr,0.5(C5 H12)'
_chemical_formula_sum            'C42.50 H34 Zr'
_chemical_formula_weight         635.92

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   15.6928(11)
_cell_length_b                   12.8853(10)
_cell_length_c                   16.2474(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.001(2)
_cell_angle_gamma                90.00
_cell_volume                     3024.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1316
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9432
_exptl_absorpt_correction_T_max  0.9616
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23365
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5316
_reflns_number_gt                4152
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0271P)²+2.3376P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5316
_refine_ls_number_parameters     390
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0766
_refine_ls_wR_factor_gt          0.0690
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.225785(17) 0.34610(2) 0.254122(16) 0.01497(9) Uani 1 1 d . . .
C1 C 0.35026(17) 0.4114(2) 0.22465(17) 0.0176(6) Uani 1 1 d . . .
H1A H 0.3784 0.3506 0.2062 0.021 Uiso 1 1 calc R . .
C2 C 0.34505(17) 0.4957(2) 0.16166(18) 0.0183(6) Uani 1 1 d . . .
C3 C 0.29756(18) 0.5039(2) 0.06968(18) 0.0224(6) Uani 1 1 d . . .
H3A H 0.2626 0.4470 0.0361 0.027 Uiso 1 1 calc R . .
C4 C 0.30178(19) 0.5961(2) 0.02724(19) 0.0253(7) Uani 1 1 d . . .
H4A H 0.2690 0.6025 -0.0356 0.030 Uiso 1 1 calc R . .
C5 C 0.3537(2) 0.6791(2) 0.0762(2) 0.0281(7) Uani 1 1 d . . .
H5A H 0.3548 0.7422 0.0463 0.034 Uiso 1 1 calc R . .
C6 C 0.40379(19) 0.6719(2) 0.16755(19) 0.0258(7) Uani 1 1 d . . .
H6A H 0.4396 0.7288 0.2001 0.031 Uiso 1 1 calc R . .
C7 C 0.40060(18) 0.5792(2) 0.21083(18) 0.0210(6) Uani 1 1 d . . .
C8 C 0.44525(18) 0.5468(2) 0.30280(18) 0.0217(6) Uani 1 1 d . . .
H8A H 0.4858 0.5884 0.3502 0.026 Uiso 1 1 calc R . .
C9 C 0.42034(17) 0.4478(2) 0.31109(17) 0.0183(6) Uani 1 1 d . . .
C10 C 0.44615(18) 0.3842(2) 0.39243(17) 0.0179(6) Uani 1 1 d . . .
C11 C 0.52565(19) 0.3915(2) 0.46311(19) 0.0252(7) Uani 1 1 d . . .
H11A H 0.5709 0.4407 0.4635 0.030 Uiso 1 1 calc R . .
H11B H 0.5373 0.3475 0.5133 0.030 Uiso 1 1 calc R . .
C12 C 0.36949(18) 0.3132(2) 0.38986(16) 0.0185(6) Uani 1 1 d . . .
C13 C 0.29943(18) 0.3428(2) 0.41919(16) 0.0212(6) Uani 1 1 d . . .
H13A H 0.3029 0.4028 0.4595 0.025 Uiso 1 1 calc R . .
C14 C 0.23302(18) 0.2603(2) 0.39789(17) 0.0213(6) Uani 1 1 d . . .
C15 C 0.1516(2) 0.2443(3) 0.41461(18) 0.0298(7) Uani 1 1 d . . .
H15A H 0.1312 0.2954 0.4449 0.036 Uiso 1 1 calc R . .
C16 C 0.1034(2) 0.1541(3) 0.38640(19) 0.0351(8) Uani 1 1 d . . .
H16A H 0.0489 0.1428 0.3973 0.042 Uiso 1 1 calc R . .
C17 C 0.1327(2) 0.0771(3) 0.34132(19) 0.0349(8) Uani 1 1 d . . .
H17A H 0.0972 0.0155 0.3224 0.042 Uiso 1 1 calc R . .
C18 C 0.2102(2) 0.0886(2) 0.32432(18) 0.0268(7) Uani 1 1 d . . .
H18A H 0.2292 0.0356 0.2945 0.032 Uiso 1 1 calc R . .
C19 C 0.26250(18) 0.1816(2) 0.35186(17) 0.0202(6) Uani 1 1 d . . .
C20 C 0.34569(18) 0.2178(2) 0.34481(17) 0.0195(6) Uani 1 1 d . . .
H20A H 0.3862 0.1760 0.3227 0.023 Uiso 1 1 calc R . .
C21 C 0.18054(17) 0.2320(2) 0.13212(16) 0.0163(6) Uani 1 1 d . . .
H21A H 0.1924 0.2696 0.0838 0.020 Uiso 1 1 calc R . .
C22 C 0.21477(18) 0.1259(2) 0.13223(16) 0.0174(6) Uani 1 1 d . . .
C23 C 0.30320(19) 0.0866(2) 0.15048(18) 0.0226(6) Uani 1 1 d . . .
H23A H 0.3539 0.1324 0.1611 0.027 Uiso 1 1 calc R . .
C24 C 0.3161(2) -0.0198(2) 0.15288(19) 0.0291(7) Uani 1 1 d . . .
H24A H 0.3763 -0.0469 0.1659 0.035 Uiso 1 1 calc R . .
C25 C 0.2422(2) -0.0876(2) 0.13649(19) 0.0305(7) Uani 1 1 d . . .
H25A H 0.2530 -0.1604 0.1402 0.037 Uiso 1 1 calc R . .
C26 C 0.1537(2) -0.0509(2) 0.11497(18) 0.0273(7) Uani 1 1 d . . .
H26A H 0.1035 -0.0977 0.1029 0.033 Uiso 1 1 calc R . .
C27 C 0.13909(18) 0.0562(2) 0.11112(17) 0.0201(6) Uani 1 1 d . . .
C28 C 0.05629(19) 0.1169(2) 0.09079(18) 0.0227(6) Uani 1 1 d . . .
H28A H -0.0044 0.0896 0.0744 0.027 Uiso 1 1 calc R . .
C29 C 0.07869(18) 0.2191(2) 0.09877(17) 0.0197(6) Uani 1 1 d . . .
C30 C 0.01788(18) 0.3086(2) 0.08808(18) 0.0218(6) Uani 1 1 d . . .
C31 C -0.0701(2) 0.3155(2) 0.0309(2) 0.0334(8) Uani 1 1 d . . .
H31A H -0.0984 0.2589 -0.0076 0.040 Uiso 1 1 calc R . .
H31B H -0.1044 0.3769 0.0285 0.040 Uiso 1 1 calc R . .
C32 C 0.06420(17) 0.3936(2) 0.15248(18) 0.0203(6) Uani 1 1 d . . .
C33 C 0.12093(18) 0.4715(2) 0.14040(19) 0.0220(6) Uani 1 1 d . . .
H33A H 0.1250 0.4901 0.0823 0.026 Uiso 1 1 calc R . .
C34 C 0.15721(18) 0.5317(2) 0.22072(19) 0.0241(7) Uani 1 1 d . . .
C35 C 0.2113(2) 0.6236(2) 0.2436(2) 0.0340(8) Uani 1 1 d . . .
H35A H 0.2330 0.6547 0.2024 0.041 Uiso 1 1 calc R . .
C36 C 0.2314(2) 0.6663(3) 0.3262(3) 0.0449(9) Uani 1 1 d . . .
H36A H 0.2662 0.7288 0.3416 0.054 Uiso 1 1 calc R . .
C37 C 0.2015(2) 0.6196(3) 0.3889(2) 0.0446(9) Uani 1 1 d . . .
H37A H 0.2172 0.6512 0.4457 0.053 Uiso 1 1 calc R . .
C38 C 0.1513(2) 0.5312(3) 0.3704(2) 0.0343(8) Uani 1 1 d . . .
H38A H 0.1329 0.5003 0.4140 0.041 Uiso 1 1 calc R . .
C39 C 0.12623(19) 0.4852(2) 0.28445(19) 0.0249(7) Uani 1 1 d . . .
C40 C 0.07078(18) 0.3970(2) 0.24193(18) 0.0231(6) Uani 1 1 d . . .
H40A H 0.0312 0.3565 0.2660 0.028 Uiso 1 1 calc R . .
C41 C 0.5179(6) 0.3550(5) 0.0955(6) 0.051(2) Uiso 0.50 1 d PD A -2
H41A H 0.5496 0.3412 0.1597 0.076 Uiso 0.50 1 calc PR A -2
H41B H 0.5425 0.3090 0.0621 0.076 Uiso 0.50 1 calc PR A -2
H41C H 0.4514 0.3424 0.0771 0.076 Uiso 0.50 1 calc PR A -2
C42 C 0.5337(4) 0.4683(4) 0.0764(3) 0.0317(15) Uiso 0.50 1 d PD A -2
H42A H 0.5099 0.5142 0.1114 0.038 Uiso 0.50 1 calc PR A -2
H42B H 0.6011 0.4809 0.0966 0.038 Uiso 0.50 1 calc PR A -2
C43 C 0.4867(4) 0.4963(5) -0.0222(3) 0.0246(14) Uiso 0.50 1 d PD A -2
H43A H 0.5104 0.4502 -0.0572 0.029 Uiso 0.50 1 calc PR A -2
H43B H 0.4193 0.4839 -0.0423 0.029 Uiso 0.50 1 calc PR A -2
C44 C 0.5025(4) 0.6080(4) -0.0410(4) 0.0289(14) Uiso 0.50 1 d PD A -2
H44A H 0.5696 0.6195 -0.0242 0.035 Uiso 0.50 1 calc PR A -2
H44B H 0.4819 0.6541 -0.0036 0.035 Uiso 0.50 1 calc PR A -2
C45 C 0.4504(5) 0.6363(6) -0.1394(4) 0.0415(18) Uiso 0.50 1 d PD A -2
H45A H 0.4626 0.7090 -0.1487 0.062 Uiso 0.50 1 calc PR A -2
H45B H 0.3838 0.6264 -0.1560 0.062 Uiso 0.50 1 calc PR A -2
H45C H 0.4714 0.5917 -0.1766 0.062 Uiso 0.50 1 calc PR A -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 C1 2.342(2) . ?
Zr1 C21 2.344(2) . ?
Zr1 C40 2.451(3) . ?
Zr1 C13 2.471(2) . ?
Zr1 C12 2.498(2) . ?
Zr1 C32 2.502(3) . ?
Zr1 C20 2.506(3) . ?
Zr1 C33 2.521(3) . ?
Zr1 C14 2.547(3) . ?
Zr1 C39 2.549(3) . ?
Zr1 C19 2.576(3) . ?
Zr1 C34 2.592(3) . ?
C1 C2 1.473(4) . ?
C1 C9 1.482(4) . ?
C1 H1A 1.0000 . ?
C2 C3 1.389(4) . ?
C2 C7 1.419(4) . ?
C3 C4 1.388(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.391(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.385(4) . ?
C5 H5A 0.9500 . ?
C6 C7 1.397(4) . ?
C6 H6A 0.9500 . ?
C7 C8 1.442(4) . ?
C8 C9 1.356(4) . ?
C8 H8A 0.9500 . ?
C9 C10 1.471(4) . ?
C10 C11 1.328(4) . ?
C10 C12 1.499(4) . ?
C11 H11A 0.9500 . ?
C11 H11B 0.9500 . ?
C12 C20 1.405(4) . ?
C12 C13 1.411(4) . ?
C13 C14 1.433(4) . ?
C13 H13A 1.0000 . ?
C14 C15 1.421(4) . ?
C14 C19 1.440(4) . ?
C15 C16 1.365(4) . ?
C15 H15A 0.9500 . ?
C16 C17 1.413(4) . ?
C16 H16A 0.9500 . ?
C17 C18 1.356(4) . ?
C17 H17A 0.9500 . ?
C18 C19 1.422(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.433(4) . ?
C20 H20A 1.0000 . ?
C21 C22 1.469(4) . ?
C21 C29 1.483(3) . ?
C21 H21A 1.0000 . ?
C22 C23 1.396(4) . ?
C22 C27 1.419(4) . ?
C23 C24 1.384(4) . ?
C23 H23A 0.9500 . ?
C24 C25 1.392(4) . ?
C24 H24A 0.9500 . ?
C25 C26 1.376(4) . ?
C25 H25A 0.9500 . ?
C26 C27 1.397(4) . ?
C26 H26A 0.9500 . ?
C27 C28 1.440(4) . ?
C28 C29 1.357(4) . ?
C28 H28A 0.9500 . ?
C29 C30 1.463(4) . ?
C30 C31 1.332(4) . ?
C30 C32 1.493(4) . ?
C31 H31A 0.9500 . ?
C31 H31B 0.9500 . ?
C32 C33 1.405(4) . ?
C32 C40 1.417(4) . ?
C33 C34 1.432(4) . ?
C33 H33A 1.0000 . ?
C34 C35 1.418(4) . ?
C34 C39 1.436(4) . ?
C35 C36 1.369(4) . ?
C35 H35A 0.9500 . ?
C36 C37 1.412(5) . ?
C36 H36A 0.9500 . ?
C37 C38 1.351(5) . ?
C37 H37A 0.9500 . ?
C38 C39 1.424(4) . ?
C38 H38A 0.9500 . ?
C39 C40 1.434(4) . ?
C40 H40A 1.0000 . ?
C41 C42 1.532(7) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.523(7) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.512(7) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.528(7) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 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
C1 Zr1 C21 93.06(9) . . ?
C1 Zr1 C40 140.20(9) . . ?
C21 Zr1 C40 97.83(9) . . ?
C1 Zr1 C13 98.88(9) . . ?
C21 Zr1 C13 139.96(9) . . ?
C40 Zr1 C13 96.94(9) . . ?
C1 Zr1 C12 72.78(9) . . ?
C21 Zr1 C12 120.72(9) . . ?
C40 Zr1 C12 129.91(9) . . ?
C13 Zr1 C12 32.98(8) . . ?
C1 Zr1 C32 119.24(9) . . ?
C21 Zr1 C32 72.62(9) . . ?
C40 Zr1 C32 33.22(9) . . ?
C13 Zr1 C32 130.10(9) . . ?
C12 Zr1 C32 163.06(9) . . ?
C1 Zr1 C20 82.09(9) . . ?
C21 Zr1 C20 89.61(9) . . ?
C40 Zr1 C20 135.84(9) . . ?
C13 Zr1 C20 54.92(9) . . ?
C12 Zr1 C20 32.62(8) . . ?
C32 Zr1 C20 152.15(9) . . ?
C1 Zr1 C33 88.72(9) . . ?
C21 Zr1 C33 83.50(9) . . ?
C40 Zr1 C33 55.01(9) . . ?
C13 Zr1 C33 134.50(9) . . ?
C12 Zr1 C33 149.44(9) . . ?
C32 Zr1 C33 32.48(9) . . ?
C20 Zr1 C33 168.22(9) . . ?
C1 Zr1 C14 127.00(9) . . ?
C21 Zr1 C14 113.18(9) . . ?
C40 Zr1 C14 82.96(9) . . ?
C13 Zr1 C14 33.15(9) . . ?
C12 Zr1 C14 54.22(9) . . ?
C32 Zr1 C14 112.47(9) . . ?
C20 Zr1 C14 54.55(9) . . ?
C33 Zr1 C14 137.14(9) . . ?
C1 Zr1 C39 114.23(9) . . ?
C21 Zr1 C39 126.76(9) . . ?
C40 Zr1 C39 33.26(9) . . ?
C13 Zr1 C39 82.20(9) . . ?
C12 Zr1 C39 111.01(9) . . ?
C32 Zr1 C39 54.25(9) . . ?
C20 Zr1 C39 136.59(9) . . ?
C33 Zr1 C39 54.36(9) . . ?
C14 Zr1 C39 86.50(9) . . ?
C1 Zr1 C19 114.72(9) . . ?
C21 Zr1 C19 85.76(9) . . ?
C40 Zr1 C19 104.23(9) . . ?
C13 Zr1 C19 54.53(9) . . ?
C12 Zr1 C19 53.77(8) . . ?
C32 Zr1 C19 122.23(9) . . ?
C20 Zr1 C19 32.71(8) . . ?
C33 Zr1 C19 154.70(9) . . ?
C14 Zr1 C19 32.64(8) . . ?
C39 Zr1 C19 117.77(9) . . ?
C1 Zr1 C34 86.39(9) . . ?
C21 Zr1 C34 115.97(9) . . ?
C40 Zr1 C34 54.45(9) . . ?
C13 Zr1 C34 102.88(9) . . ?
C12 Zr1 C34 119.93(9) . . ?
C32 Zr1 C34 53.49(9) . . ?
C20 Zr1 C34 152.51(9) . . ?
C33 Zr1 C34 32.48(9) . . ?
C14 Zr1 C34 117.31(9) . . ?
C39 Zr1 C34 32.43(9) . . ?
C19 Zr1 C34 149.69(9) . . ?
C2 C1 C9 104.1(2) . . ?
C2 C1 Zr1 125.64(17) . . ?
C9 C1 Zr1 106.83(16) . . ?
C2 C1 H1A 106.3 . . ?
C9 C1 H1A 106.3 . . ?
Zr1 C1 H1A 106.3 . . ?
C3 C2 C7 120.1(2) . . ?
C3 C2 C1 131.7(2) . . ?
C7 C2 C1 108.3(2) . . ?
C4 C3 C2 119.3(3) . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 H3A 120.3 . . ?
C3 C4 C5 120.4(3) . . ?
C3 C4 H4A 119.8 . . ?
C5 C4 H4A 119.8 . . ?
C6 C5 C4 121.4(3) . . ?
C6 C5 H5A 119.3 . . ?
C4 C5 H5A 119.3 . . ?
C5 C6 C7 118.7(3) . . ?
C5 C6 H6A 120.6 . . ?
C7 C6 H6A 120.6 . . ?
C6 C7 C2 120.0(3) . . ?
C6 C7 C8 132.1(3) . . ?
C2 C7 C8 107.9(2) . . ?
C9 C8 C7 109.4(2) . . ?
C9 C8 H8A 125.3 . . ?
C7 C8 H8A 125.3 . . ?
C8 C9 C10 128.6(3) . . ?
C8 C9 C1 109.9(2) . . ?
C10 C9 C1 121.1(2) . . ?
C11 C10 C9 125.0(3) . . ?
C11 C10 C12 122.7(3) . . ?
C9 C10 C12 112.2(2) . . ?
C10 C11 H11A 120.0 . . ?
C10 C11 H11B 120.0 . . ?
H11A C11 H11B 120.0 . . ?
C20 C12 C13 109.2(2) . . ?
C20 C12 C10 126.6(2) . . ?
C13 C12 C10 123.3(2) . . ?
C20 C12 Zr1 73.98(14) . . ?
C13 C12 Zr1 72.46(14) . . ?
C10 C12 Zr1 111.04(16) . . ?
C12 C13 C14 107.9(2) . . ?
C12 C13 Zr1 74.56(14) . . ?
C14 C13 Zr1 76.30(14) . . ?
C12 C13 H13A 125.4 . . ?
C14 C13 H13A 125.4 . . ?
Zr1 C13 H13A 125.4 . . ?
C15 C14 C13 133.2(3) . . ?
C15 C14 C19 119.5(3) . . ?
C13 C14 C19 107.3(2) . . ?
C15 C14 Zr1 121.14(18) . . ?
C13 C14 Zr1 70.54(14) . . ?
C19 C14 Zr1 74.79(14) . . ?
C16 C15 C14 118.8(3) . . ?
C16 C15 H15A 120.6 . . ?
C14 C15 H15A 120.6 . . ?
C15 C16 C17 121.4(3) . . ?
C15 C16 H16A 119.3 . . ?
C17 C16 H16A 119.3 . . ?
C18 C17 C16 121.9(3) . . ?
C18 C17 H17A 119.0 . . ?
C16 C17 H17A 119.0 . . ?
C17 C18 C19 118.8(3) . . ?
C17 C18 H18A 120.6 . . ?
C19 C18 H18A 120.6 . . ?
C18 C19 C20 132.9(3) . . ?
C18 C19 C14 119.6(3) . . ?
C20 C19 C14 107.5(2) . . ?
C18 C19 Zr1 122.46(18) . . ?
C20 C19 Zr1 70.96(14) . . ?
C14 C19 Zr1 72.57(15) . . ?
C12 C20 C19 108.0(2) . . ?
C12 C20 Zr1 73.40(15) . . ?
C19 C20 Zr1 76.32(15) . . ?
C12 C20 H20A 125.5 . . ?
C19 C20 H20A 125.5 . . ?
Zr1 C20 H20A 125.5 . . ?
C22 C21 C29 103.7(2) . . ?
C22 C21 Zr1 126.37(17) . . ?
C29 C21 Zr1 107.83(16) . . ?
C22 C21 H21A 105.8 . . ?
C29 C21 H21A 105.8 . . ?
Zr1 C21 H21A 105.8 . . ?
C23 C22 C27 119.4(2) . . ?
C23 C22 C21 132.1(2) . . ?
C27 C22 C21 108.5(2) . . ?
C24 C23 C22 119.1(3) . . ?
C24 C23 H23A 120.4 . . ?
C22 C23 H23A 120.4 . . ?
C23 C24 C25 121.0(3) . . ?
C23 C24 H24A 119.5 . . ?
C25 C24 H24A 119.5 . . ?
C26 C25 C24 121.0(3) . . ?
C26 C25 H25A 119.5 . . ?
C24 C25 H25A 119.5 . . ?
C25 C26 C27 118.9(3) . . ?
C25 C26 H26A 120.6 . . ?
C27 C26 H26A 120.6 . . ?
C26 C27 C22 120.4(3) . . ?
C26 C27 C28 131.7(3) . . ?
C22 C27 C28 107.9(2) . . ?
C29 C28 C27 109.2(2) . . ?
C29 C28 H28A 125.4 . . ?
C27 C28 H28A 125.4 . . ?
C28 C29 C30 128.4(2) . . ?
C28 C29 C21 110.2(2) . . ?
C30 C29 C21 121.0(2) . . ?
C31 C30 C29 125.8(3) . . ?
C31 C30 C32 121.9(3) . . ?
C29 C30 C32 112.3(2) . . ?
C30 C31 H31A 120.0 . . ?
C30 C31 H31B 120.0 . . ?
H31A C31 H31B 120.0 . . ?
C33 C32 C40 109.0(2) . . ?
C33 C32 C30 126.0(2) . . ?
C40 C32 C30 124.2(2) . . ?
C33 C32 Zr1 74.51(15) . . ?
C40 C32 Zr1 71.42(14) . . ?
C30 C32 Zr1 111.93(17) . . ?
C32 C33 C34 107.9(2) . . ?
C32 C33 Zr1 73.01(15) . . ?
C34 C33 Zr1 76.48(16) . . ?
C32 C33 H33A 125.5 . . ?
C34 C33 H33A 125.5 . . ?
Zr1 C33 H33A 125.5 . . ?
C35 C34 C33 132.5(3) . . ?
C35 C34 C39 119.8(3) . . ?
C33 C34 C39 107.7(2) . . ?
C35 C34 Zr1 123.94(19) . . ?
C33 C34 Zr1 71.04(15) . . ?
C39 C34 Zr1 72.13(15) . . ?
C36 C35 C34 118.5(3) . . ?
C36 C35 H35A 120.7 . . ?
C34 C35 H35A 120.7 . . ?
C35 C36 C37 121.4(3) . . ?
C35 C36 H36A 119.3 . . ?
C37 C36 H36A 119.3 . . ?
C38 C37 C36 121.9(3) . . ?
C38 C37 H37A 119.0 . . ?
C36 C37 H37A 119.0 . . ?
C37 C38 C39 118.9(3) . . ?
C37 C38 H38A 120.6 . . ?
C39 C38 H38A 120.6 . . ?
C38 C39 C40 133.3(3) . . ?
C38 C39 C34 119.4(3) . . ?
C40 C39 C34 107.2(2) . . ?
C38 C39 Zr1 121.84(19) . . ?
C40 C39 Zr1 69.63(15) . . ?
C34 C39 Zr1 75.44(15) . . ?
C32 C40 C39 107.8(2) . . ?
C32 C40 Zr1 75.36(15) . . ?
C39 C40 Zr1 77.10(15) . . ?
C32 C40 H40A 125.3 . . ?
C39 C40 H40A 125.3 . . ?
Zr1 C40 H40A 125.3 . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C41 112.9(5) . . ?
C43 C42 H42A 109.0 . . ?
C41 C42 H42A 109.0 . . ?
C43 C42 H42B 109.0 . . ?
C41 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
C44 C43 C42 112.9(4) . . ?
C44 C43 H43A 109.0 . . ?
C42 C43 H43A 109.0 . . ?
C44 C43 H43B 109.0 . . ?
C42 C43 H43B 109.0 . . ?
H43A C43 H43B 107.8 . . ?
C43 C44 C45 112.1(5) . . ?
C43 C44 H44A 109.2 . . ?
C45 C44 H44A 109.2 . . ?
C43 C44 H44B 109.2 . . ?
C45 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C21 Zr1 C1 C2 84.9(2) . . . . ?
C40 Zr1 C1 C2 -21.2(3) . . . . ?
C13 Zr1 C1 C2 -133.5(2) . . . . ?
C12 Zr1 C1 C2 -153.9(2) . . . . ?
C32 Zr1 C1 C2 13.1(3) . . . . ?
C20 Zr1 C1 C2 174.1(2) . . . . ?
C33 Zr1 C1 C2 1.5(2) . . . . ?
C14 Zr1 C1 C2 -152.9(2) . . . . ?
C39 Zr1 C1 C2 -48.1(2) . . . . ?
C19 Zr1 C1 C2 171.6(2) . . . . ?
C34 Zr1 C1 C2 -31.0(2) . . . . ?
C21 Zr1 C1 C9 -153.08(18) . . . . ?
C40 Zr1 C1 C9 100.8(2) . . . . ?
C13 Zr1 C1 C9 -11.42(19) . . . . ?
C12 Zr1 C1 C9 -31.82(17) . . . . ?
C32 Zr1 C1 C9 135.14(17) . . . . ?
C20 Zr1 C1 C9 -63.91(18) . . . . ?
C33 Zr1 C1 C9 123.50(18) . . . . ?
C14 Zr1 C1 C9 -30.8(2) . . . . ?
C39 Zr1 C1 C9 73.97(19) . . . . ?
C19 Zr1 C1 C9 -66.35(19) . . . . ?
C34 Zr1 C1 C9 91.06(18) . . . . ?
C9 C1 C2 C3 174.2(3) . . . . ?
Zr1 C1 C2 C3 -62.6(4) . . . . ?
C9 C1 C2 C7 -6.0(3) . . . . ?
Zr1 C1 C2 C7 117.2(2) . . . . ?
C7 C2 C3 C4 -2.9(4) . . . . ?
C1 C2 C3 C4 176.9(3) . . . . ?
C2 C3 C4 C5 0.6(4) . . . . ?
C3 C4 C5 C6 1.3(4) . . . . ?
C4 C5 C6 C7 -0.8(4) . . . . ?
C5 C6 C7 C2 -1.5(4) . . . . ?
C5 C6 C7 C8 178.6(3) . . . . ?
C3 C2 C7 C6 3.4(4) . . . . ?
C1 C2 C7 C6 -176.5(2) . . . . ?
C3 C2 C7 C8 -176.7(2) . . . . ?
C1 C2 C7 C8 3.5(3) . . . . ?
C6 C7 C8 C9 -179.3(3) . . . . ?
C2 C7 C8 C9 0.8(3) . . . . ?
C7 C8 C9 C10 -177.7(2) . . . . ?
C7 C8 C9 C1 -4.7(3) . . . . ?
C2 C1 C9 C8 6.6(3) . . . . ?
Zr1 C1 C9 C8 -128.11(19) . . . . ?
C2 C1 C9 C10 -179.8(2) . . . . ?
Zr1 C1 C9 C10 45.5(3) . . . . ?
C8 C9 C10 C11 -31.0(4) . . . . ?
C1 C9 C10 C11 156.7(3) . . . . ?
C8 C9 C10 C12 145.3(3) . . . . ?
C1 C9 C10 C12 -27.0(3) . . . . ?
C11 C10 C12 C20 -103.6(3) . . . . ?
C9 C10 C12 C20 80.0(3) . . . . ?
C11 C10 C12 C13 88.8(3) . . . . ?
C9 C10 C12 C13 -87.6(3) . . . . ?
C11 C10 C12 Zr1 171.1(2) . . . . ?
C9 C10 C12 Zr1 -5.3(3) . . . . ?
C1 Zr1 C12 C20 -102.54(17) . . . . ?
C21 Zr1 C12 C20 -19.37(19) . . . . ?
C40 Zr1 C12 C20 115.34(17) . . . . ?
C13 Zr1 C12 C20 116.7(2) . . . . ?
C32 Zr1 C12 C20 119.9(3) . . . . ?
C33 Zr1 C12 C20 -157.74(17) . . . . ?
C14 Zr1 C12 C20 78.45(17) . . . . ?
C39 Zr1 C12 C20 147.51(15) . . . . ?
C19 Zr1 C12 C20 37.80(15) . . . . ?
C34 Zr1 C12 C20 -177.80(14) . . . . ?
C1 Zr1 C12 C13 140.75(18) . . . . ?
C21 Zr1 C12 C13 -136.08(16) . . . . ?
C40 Zr1 C12 C13 -1.4(2) . . . . ?
C32 Zr1 C12 C13 3.2(4) . . . . ?
C20 Zr1 C12 C13 -116.7(2) . . . . ?
C33 Zr1 C12 C13 85.6(2) . . . . ?
C14 Zr1 C12 C13 -38.26(16) . . . . ?
C39 Zr1 C12 C13 30.80(18) . . . . ?
C19 Zr1 C12 C13 -78.91(17) . . . . ?
C34 Zr1 C12 C13 65.49(18) . . . . ?
C1 Zr1 C12 C10 21.08(17) . . . . ?
C21 Zr1 C12 C10 104.24(18) . . . . ?
C40 Zr1 C12 C10 -121.05(18) . . . . ?
C13 Zr1 C12 C10 -119.7(3) . . . . ?
C32 Zr1 C12 C10 -116.4(3) . . . . ?
C20 Zr1 C12 C10 123.6(3) . . . . ?
C33 Zr1 C12 C10 -34.1(3) . . . . ?
C14 Zr1 C12 C10 -157.9(2) . . . . ?
C39 Zr1 C12 C10 -88.88(18) . . . . ?
C19 Zr1 C12 C10 161.4(2) . . . . ?
C34 Zr1 C12 C10 -54.2(2) . . . . ?
C20 C12 C13 C14 4.3(3) . . . . ?
C10 C12 C13 C14 173.7(2) . . . . ?
Zr1 C12 C13 C14 69.68(18) . . . . ?
C20 C12 C13 Zr1 -65.39(18) . . . . ?
C10 C12 C13 Zr1 104.1(2) . . . . ?
C1 Zr1 C13 C12 -37.71(17) . . . . ?
C21 Zr1 C13 C12 68.0(2) . . . . ?
C40 Zr1 C13 C12 178.94(16) . . . . ?
C32 Zr1 C13 C12 -178.77(15) . . . . ?
C20 Zr1 C13 C12 36.04(15) . . . . ?
C33 Zr1 C13 C12 -134.71(16) . . . . ?
C14 Zr1 C13 C12 113.3(2) . . . . ?
C39 Zr1 C13 C12 -151.16(17) . . . . ?
C19 Zr1 C13 C12 76.39(17) . . . . ?
C34 Zr1 C13 C12 -126.01(16) . . . . ?
C1 Zr1 C13 C14 -150.98(16) . . . . ?
C21 Zr1 C13 C14 -45.3(2) . . . . ?
C40 Zr1 C13 C14 65.66(17) . . . . ?
C12 Zr1 C13 C14 -113.3(2) . . . . ?
C32 Zr1 C13 C14 67.96(19) . . . . ?
C20 Zr1 C13 C14 -77.24(17) . . . . ?
C33 Zr1 C13 C14 112.01(18) . . . . ?
C39 Zr1 C13 C14 95.57(17) . . . . ?
C19 Zr1 C13 C14 -36.88(15) . . . . ?
C34 Zr1 C13 C14 120.71(16) . . . . ?
C12 C13 C14 C15 176.6(3) . . . . ?
Zr1 C13 C14 C15 -114.9(3) . . . . ?
C12 C13 C14 C19 -2.2(3) . . . . ?
Zr1 C13 C14 C19 66.34(18) . . . . ?
C12 C13 C14 Zr1 -68.50(17) . . . . ?
C1 Zr1 C14 C15 166.3(2) . . . . ?
C21 Zr1 C14 C15 -80.4(2) . . . . ?
C40 Zr1 C14 C15 15.1(2) . . . . ?
C13 Zr1 C14 C15 129.4(3) . . . . ?
C12 Zr1 C14 C15 167.5(3) . . . . ?
C32 Zr1 C14 C15 -0.5(3) . . . . ?
C20 Zr1 C14 C15 -152.1(3) . . . . ?
C33 Zr1 C14 C15 25.8(3) . . . . ?
C39 Zr1 C14 C15 48.3(2) . . . . ?
C19 Zr1 C14 C15 -115.6(3) . . . . ?
C34 Zr1 C14 C15 58.8(3) . . . . ?
C1 Zr1 C14 C13 36.9(2) . . . . ?
C21 Zr1 C14 C13 150.16(16) . . . . ?
C40 Zr1 C14 C13 -114.31(17) . . . . ?
C12 Zr1 C14 C13 38.05(15) . . . . ?
C32 Zr1 C14 C13 -129.89(16) . . . . ?
C20 Zr1 C14 C13 78.46(17) . . . . ?
C33 Zr1 C14 C13 -103.56(18) . . . . ?
C39 Zr1 C14 C13 -81.09(17) . . . . ?
C19 Zr1 C14 C13 115.0(2) . . . . ?
C34 Zr1 C14 C13 -70.62(18) . . . . ?
C1 Zr1 C14 C19 -78.13(18) . . . . ?
C21 Zr1 C14 C19 35.15(17) . . . . ?
C40 Zr1 C14 C19 130.69(16) . . . . ?
C13 Zr1 C14 C19 -115.0(2) . . . . ?
C12 Zr1 C14 C19 -76.96(16) . . . . ?
C32 Zr1 C14 C19 115.11(16) . . . . ?
C20 Zr1 C14 C19 -36.54(15) . . . . ?
C33 Zr1 C14 C19 141.43(16) . . . . ?
C39 Zr1 C14 C19 163.91(16) . . . . ?
C34 Zr1 C14 C19 174.38(15) . . . . ?
C13 C14 C15 C16 -178.6(3) . . . . ?
C19 C14 C15 C16 0.0(4) . . . . ?
Zr1 C14 C15 C16 89.4(3) . . . . ?
C14 C15 C16 C17 0.0(4) . . . . ?
C15 C16 C17 C18 0.4(5) . . . . ?
C16 C17 C18 C19 -0.8(4) . . . . ?
C17 C18 C19 C20 179.8(3) . . . . ?
C17 C18 C19 C14 0.8(4) . . . . ?
C17 C18 C19 Zr1 -86.5(3) . . . . ?
C15 C14 C19 C18 -0.4(4) . . . . ?
C13 C14 C19 C18 178.5(2) . . . . ?
Zr1 C14 C19 C18 -117.9(2) . . . . ?
C15 C14 C19 C20 -179.7(2) . . . . ?
C13 C14 C19 C20 -0.7(3) . . . . ?
Zr1 C14 C19 C20 62.80(17) . . . . ?
C15 C14 C19 Zr1 117.5(2) . . . . ?
C13 C14 C19 Zr1 -63.50(18) . . . . ?
C1 Zr1 C19 C18 -124.9(2) . . . . ?
C21 Zr1 C19 C18 -33.5(2) . . . . ?
C40 Zr1 C19 C18 63.5(2) . . . . ?
C13 Zr1 C19 C18 151.9(3) . . . . ?
C12 Zr1 C19 C18 -167.1(3) . . . . ?
C32 Zr1 C19 C18 32.9(3) . . . . ?
C20 Zr1 C19 C18 -129.4(3) . . . . ?
C33 Zr1 C19 C18 31.5(4) . . . . ?
C14 Zr1 C19 C18 114.4(3) . . . . ?
C39 Zr1 C19 C18 96.2(2) . . . . ?
C34 Zr1 C19 C18 104.5(3) . . . . ?
C1 Zr1 C19 C20 4.47(18) . . . . ?
C21 Zr1 C19 C20 95.90(16) . . . . ?
C40 Zr1 C19 C20 -167.09(15) . . . . ?
C13 Zr1 C19 C20 -78.67(16) . . . . ?
C12 Zr1 C19 C20 -37.68(15) . . . . ?
C32 Zr1 C19 C20 162.27(15) . . . . ?
C33 Zr1 C19 C20 160.90(19) . . . . ?
C14 Zr1 C19 C20 -116.2(2) . . . . ?
C39 Zr1 C19 C20 -134.38(15) . . . . ?
C34 Zr1 C19 C20 -126.09(19) . . . . ?
C1 Zr1 C19 C14 120.63(16) . . . . ?
C21 Zr1 C19 C14 -147.94(16) . . . . ?
C40 Zr1 C19 C14 -50.93(17) . . . . ?
C13 Zr1 C19 C14 37.49(15) . . . . ?
C12 Zr1 C19 C14 78.48(17) . . . . ?
C32 Zr1 C19 C14 -81.57(17) . . . . ?
C20 Zr1 C19 C14 116.2(2) . . . . ?
C33 Zr1 C19 C14 -82.9(2) . . . . ?
C39 Zr1 C19 C14 -18.22(18) . . . . ?
C34 Zr1 C19 C14 -9.9(3) . . . . ?
C13 C12 C20 C19 -4.7(3) . . . . ?
C10 C12 C20 C19 -173.7(2) . . . . ?
Zr1 C12 C20 C19 -69.14(18) . . . . ?
C13 C12 C20 Zr1 64.41(18) . . . . ?
C10 C12 C20 Zr1 -104.6(3) . . . . ?
C18 C19 C20 C12 -175.8(3) . . . . ?
C14 C19 C20 C12 3.3(3) . . . . ?
Zr1 C19 C20 C12 67.17(18) . . . . ?
C18 C19 C20 Zr1 117.0(3) . . . . ?
C14 C19 C20 Zr1 -63.85(18) . . . . ?
C1 Zr1 C20 C12 70.28(16) . . . . ?
C21 Zr1 C20 C12 163.43(16) . . . . ?
C40 Zr1 C20 C12 -95.71(18) . . . . ?
C13 Zr1 C20 C12 -36.46(15) . . . . ?
C32 Zr1 C20 C12 -147.28(19) . . . . ?
C33 Zr1 C20 C12 109.4(4) . . . . ?
C14 Zr1 C20 C12 -77.36(17) . . . . ?
C39 Zr1 C20 C12 -46.9(2) . . . . ?
C19 Zr1 C20 C12 -113.8(2) . . . . ?
C34 Zr1 C20 C12 4.1(3) . . . . ?
C1 Zr1 C20 C19 -175.90(16) . . . . ?
C21 Zr1 C20 C19 -82.75(16) . . . . ?
C40 Zr1 C20 C19 18.1(2) . . . . ?
C13 Zr1 C20 C19 77.36(16) . . . . ?
C12 Zr1 C20 C19 113.8(2) . . . . ?
C32 Zr1 C20 C19 -33.5(3) . . . . ?
C33 Zr1 C20 C19 -136.8(4) . . . . ?
C14 Zr1 C20 C19 36.46(15) . . . . ?
C39 Zr1 C20 C19 67.0(2) . . . . ?
C34 Zr1 C20 C19 118.0(2) . . . . ?
C1 Zr1 C21 C22 87.8(2) . . . . ?
C40 Zr1 C21 C22 -130.6(2) . . . . ?
C13 Zr1 C21 C22 -19.9(3) . . . . ?
C12 Zr1 C21 C22 16.0(3) . . . . ?
C32 Zr1 C21 C22 -152.5(2) . . . . ?
C20 Zr1 C21 C22 5.7(2) . . . . ?
C33 Zr1 C21 C22 176.2(2) . . . . ?
C14 Zr1 C21 C22 -44.9(2) . . . . ?
C39 Zr1 C21 C22 -148.6(2) . . . . ?
C19 Zr1 C21 C22 -26.8(2) . . . . ?
C34 Zr1 C21 C22 175.3(2) . . . . ?
C1 Zr1 C21 C29 -149.06(18) . . . . ?
C40 Zr1 C21 C29 -7.43(18) . . . . ?
C13 Zr1 C21 C29 103.25(19) . . . . ?
C12 Zr1 C21 C29 139.19(16) . . . . ?
C32 Zr1 C21 C29 -29.33(17) . . . . ?
C20 Zr1 C21 C29 128.88(18) . . . . ?
C33 Zr1 C21 C29 -60.69(17) . . . . ?
C14 Zr1 C21 C29 78.22(18) . . . . ?
C39 Zr1 C21 C29 -25.5(2) . . . . ?
C19 Zr1 C21 C29 96.37(18) . . . . ?
C34 Zr1 C21 C29 -61.58(19) . . . . ?
C29 C21 C22 C23 175.0(3) . . . . ?
Zr1 C21 C22 C23 -60.2(4) . . . . ?
C29 C21 C22 C27 -6.6(3) . . . . ?
Zr1 C21 C22 C27 118.2(2) . . . . ?
C27 C22 C23 C24 -3.9(4) . . . . ?
C21 C22 C23 C24 174.4(3) . . . . ?
C22 C23 C24 C25 0.7(4) . . . . ?
C23 C24 C25 C26 1.8(4) . . . . ?
C24 C25 C26 C27 -1.0(4) . . . . ?
C25 C26 C27 C22 -2.2(4) . . . . ?
C25 C26 C27 C28 179.9(3) . . . . ?
C23 C22 C27 C26 4.7(4) . . . . ?
C21 C22 C27 C26 -173.9(2) . . . . ?
C23 C22 C27 C28 -177.0(2) . . . . ?
C21 C22 C27 C28 4.4(3) . . . . ?
C26 C27 C28 C29 178.0(3) . . . . ?
C22 C27 C28 C29 -0.1(3) . . . . ?
C27 C28 C29 C30 -177.3(2) . . . . ?
C27 C28 C29 C21 -4.3(3) . . . . ?
C22 C21 C29 C28 6.8(3) . . . . ?
Zr1 C21 C29 C28 -129.3(2) . . . . ?
C22 C21 C29 C30 -179.6(2) . . . . ?
Zr1 C21 C29 C30 44.3(3) . . . . ?
C28 C29 C30 C31 -34.3(5) . . . . ?
C21 C29 C30 C31 153.3(3) . . . . ?
C28 C29 C30 C32 143.3(3) . . . . ?
C21 C29 C30 C32 -29.1(3) . . . . ?
C31 C30 C32 C33 -97.1(3) . . . . ?
C29 C30 C32 C33 85.2(3) . . . . ?
C31 C30 C32 C40 94.7(3) . . . . ?
C29 C30 C32 C40 -83.0(3) . . . . ?
C31 C30 C32 Zr1 176.5(2) . . . . ?
C29 C30 C32 Zr1 -1.1(3) . . . . ?
C1 Zr1 C32 C33 -22.08(19) . . . . ?
C21 Zr1 C32 C33 -105.70(17) . . . . ?
C40 Zr1 C32 C33 116.7(2) . . . . ?
C13 Zr1 C32 C33 112.56(17) . . . . ?
C12 Zr1 C32 C33 110.3(3) . . . . ?
C20 Zr1 C32 C33 -158.29(18) . . . . ?
C14 Zr1 C32 C33 145.82(16) . . . . ?
C39 Zr1 C32 C33 78.10(18) . . . . ?
C19 Zr1 C32 C33 -178.91(15) . . . . ?
C34 Zr1 C32 C33 37.66(16) . . . . ?
C1 Zr1 C32 C40 -138.79(16) . . . . ?
C21 Zr1 C32 C40 137.59(18) . . . . ?
C13 Zr1 C32 C40 -4.2(2) . . . . ?
C12 Zr1 C32 C40 -6.5(4) . . . . ?
C20 Zr1 C32 C40 85.0(2) . . . . ?
C33 Zr1 C32 C40 -116.7(2) . . . . ?
C14 Zr1 C32 C40 29.11(19) . . . . ?
C39 Zr1 C32 C40 -38.61(16) . . . . ?
C19 Zr1 C32 C40 64.38(19) . . . . ?
C34 Zr1 C32 C40 -79.05(18) . . . . ?
C1 Zr1 C32 C30 100.99(19) . . . . ?
C21 Zr1 C32 C30 17.36(17) . . . . ?
C40 Zr1 C32 C30 -120.2(3) . . . . ?
C13 Zr1 C32 C30 -124.38(18) . . . . ?
C12 Zr1 C32 C30 -126.7(3) . . . . ?
C20 Zr1 C32 C30 -35.2(3) . . . . ?
C33 Zr1 C32 C30 123.1(3) . . . . ?
C14 Zr1 C32 C30 -91.11(19) . . . . ?
C39 Zr1 C32 C30 -158.8(2) . . . . ?
C19 Zr1 C32 C30 -55.8(2) . . . . ?
C34 Zr1 C32 C30 160.7(2) . . . . ?
C40 C32 C33 C34 -5.6(3) . . . . ?
C30 C32 C33 C34 -175.3(2) . . . . ?
Zr1 C32 C33 C34 -69.16(18) . . . . ?
C40 C32 C33 Zr1 63.57(18) . . . . ?
C30 C32 C33 Zr1 -106.1(3) . . . . ?
C1 Zr1 C33 C32 160.85(17) . . . . ?
C21 Zr1 C33 C32 67.62(17) . . . . ?
C40 Zr1 C33 C32 -36.68(16) . . . . ?
C13 Zr1 C33 C32 -97.93(19) . . . . ?
C12 Zr1 C33 C32 -147.47(18) . . . . ?
C20 Zr1 C33 C32 122.2(4) . . . . ?
C14 Zr1 C33 C32 -49.7(2) . . . . ?
C39 Zr1 C33 C32 -77.74(17) . . . . ?
C19 Zr1 C33 C32 2.2(3) . . . . ?
C34 Zr1 C33 C32 -113.9(2) . . . . ?
C1 Zr1 C33 C34 -85.29(16) . . . . ?
C21 Zr1 C33 C34 -178.52(17) . . . . ?
C40 Zr1 C33 C34 77.18(17) . . . . ?
C13 Zr1 C33 C34 15.9(2) . . . . ?
C12 Zr1 C33 C34 -33.6(3) . . . . ?
C32 Zr1 C33 C34 113.9(2) . . . . ?
C20 Zr1 C33 C34 -124.0(4) . . . . ?
C14 Zr1 C33 C34 64.1(2) . . . . ?
C39 Zr1 C33 C34 36.12(15) . . . . ?
C19 Zr1 C33 C34 116.0(2) . . . . ?
C32 C33 C34 C35 -174.1(3) . . . . ?
Zr1 C33 C34 C35 119.1(3) . . . . ?
C32 C33 C34 C39 3.6(3) . . . . ?
Zr1 C33 C34 C39 -63.23(19) . . . . ?
C32 C33 C34 Zr1 66.82(18) . . . . ?
C1 Zr1 C34 C35 -35.7(3) . . . . ?
C21 Zr1 C34 C35 -127.4(3) . . . . ?
C40 Zr1 C34 C35 152.0(3) . . . . ?
C13 Zr1 C34 C35 62.6(3) . . . . ?
C12 Zr1 C34 C35 32.1(3) . . . . ?
C32 Zr1 C34 C35 -166.7(3) . . . . ?
C20 Zr1 C34 C35 29.5(4) . . . . ?
C33 Zr1 C34 C35 -129.0(3) . . . . ?
C14 Zr1 C34 C35 94.5(3) . . . . ?
C39 Zr1 C34 C35 114.3(3) . . . . ?
C19 Zr1 C34 C35 100.6(3) . . . . ?
C1 Zr1 C34 C33 93.29(16) . . . . ?
C21 Zr1 C34 C33 1.64(18) . . . . ?
C40 Zr1 C34 C33 -79.05(17) . . . . ?
C13 Zr1 C34 C33 -168.41(15) . . . . ?
C12 Zr1 C34 C33 161.05(15) . . . . ?
C32 Zr1 C34 C33 -37.67(15) . . . . ?
C20 Zr1 C34 C33 158.48(18) . . . . ?
C14 Zr1 C34 C33 -136.46(15) . . . . ?
C39 Zr1 C34 C33 -116.7(2) . . . . ?
C19 Zr1 C34 C33 -130.45(19) . . . . ?
C1 Zr1 C34 C39 -150.02(17) . . . . ?
C21 Zr1 C34 C39 118.33(17) . . . . ?
C40 Zr1 C34 C39 37.65(16) . . . . ?
C13 Zr1 C34 C39 -51.72(17) . . . . ?
C12 Zr1 C34 C39 -82.26(18) . . . . ?
C32 Zr1 C34 C39 79.03(17) . . . . ?
C20 Zr1 C34 C39 -84.8(2) . . . . ?
C33 Zr1 C34 C39 116.7(2) . . . . ?
C14 Zr1 C34 C39 -19.77(19) . . . . ?
C19 Zr1 C34 C39 -13.8(3) . . . . ?
C33 C34 C35 C36 176.6(3) . . . . ?
C39 C34 C35 C36 -0.9(4) . . . . ?
Zr1 C34 C35 C36 -88.6(3) . . . . ?
C34 C35 C36 C37 1.6(5) . . . . ?
C35 C36 C37 C38 -0.5(5) . . . . ?
C36 C37 C38 C39 -1.3(5) . . . . ?
C37 C38 C39 C40 -176.2(3) . . . . ?
C37 C38 C39 C34 1.9(4) . . . . ?
C37 C38 C39 Zr1 92.5(3) . . . . ?
C35 C34 C39 C38 -0.8(4) . . . . ?
C33 C34 C39 C38 -178.8(2) . . . . ?
Zr1 C34 C39 C38 118.6(2) . . . . ?
C35 C34 C39 C40 177.8(2) . . . . ?
C33 C34 C39 C40 -0.3(3) . . . . ?
Zr1 C34 C39 C40 -62.80(18) . . . . ?
C35 C34 C39 Zr1 -119.4(2) . . . . ?
C33 C34 C39 Zr1 62.51(18) . . . . ?
C1 Zr1 C39 C38 -82.7(3) . . . . ?
C21 Zr1 C39 C38 163.1(2) . . . . ?
C40 Zr1 C39 C38 129.1(3) . . . . ?
C13 Zr1 C39 C38 13.5(2) . . . . ?
C12 Zr1 C39 C38 -2.8(3) . . . . ?
C32 Zr1 C39 C38 167.6(3) . . . . ?
C20 Zr1 C39 C38 22.1(3) . . . . ?
C33 Zr1 C39 C38 -152.1(3) . . . . ?
C14 Zr1 C39 C38 46.6(3) . . . . ?
C19 Zr1 C39 C38 56.3(3) . . . . ?
C34 Zr1 C39 C38 -115.9(3) . . . . ?
C1 Zr1 C39 C40 148.19(16) . . . . ?
C21 Zr1 C39 C40 34.0(2) . . . . ?
C13 Zr1 C39 C40 -115.54(17) . . . . ?
C12 Zr1 C39 C40 -131.88(16) . . . . ?
C32 Zr1 C39 C40 38.56(15) . . . . ?
C20 Zr1 C39 C40 -106.96(18) . . . . ?
C33 Zr1 C39 C40 78.85(17) . . . . ?
C14 Zr1 C39 C40 -82.49(17) . . . . ?
C19 Zr1 C39 C40 -72.76(18) . . . . ?
C34 Zr1 C39 C40 115.0(2) . . . . ?
C1 Zr1 C39 C34 33.16(19) . . . . ?
C21 Zr1 C39 C34 -81.00(19) . . . . ?
C40 Zr1 C39 C34 -115.0(2) . . . . ?
C13 Zr1 C39 C34 129.43(17) . . . . ?
C12 Zr1 C39 C34 113.09(17) . . . . ?
C32 Zr1 C39 C34 -76.47(17) . . . . ?
C20 Zr1 C39 C34 138.01(16) . . . . ?
C33 Zr1 C39 C34 -36.18(16) . . . . ?
C14 Zr1 C39 C34 162.48(17) . . . . ?
C19 Zr1 C39 C34 172.20(15) . . . . ?
C33 C32 C40 C39 5.4(3) . . . . ?
C30 C32 C40 C39 175.3(2) . . . . ?
Zr1 C32 C40 C39 70.97(18) . . . . ?
C33 C32 C40 Zr1 -65.56(19) . . . . ?
C30 C32 C40 Zr1 104.4(2) . . . . ?
C38 C39 C40 C32 175.2(3) . . . . ?
C34 C39 C40 C32 -3.1(3) . . . . ?
Zr1 C39 C40 C32 -69.77(18) . . . . ?
C38 C39 C40 Zr1 -115.1(3) . . . . ?
C34 C39 C40 Zr1 66.67(18) . . . . ?
C1 Zr1 C40 C32 63.9(2) . . . . ?
C21 Zr1 C40 C32 -40.52(17) . . . . ?
C13 Zr1 C40 C32 176.80(16) . . . . ?
C12 Zr1 C40 C32 177.55(15) . . . . ?
C20 Zr1 C40 C32 -138.08(16) . . . . ?
C33 Zr1 C40 C32 35.84(16) . . . . ?
C14 Zr1 C40 C32 -153.06(17) . . . . ?
C39 Zr1 C40 C32 112.6(2) . . . . ?
C19 Zr1 C40 C32 -128.11(16) . . . . ?
C34 Zr1 C40 C32 75.90(17) . . . . ?
C1 Zr1 C40 C39 -48.7(2) . . . . ?
C21 Zr1 C40 C39 -153.09(16) . . . . ?
C13 Zr1 C40 C39 64.23(17) . . . . ?
C12 Zr1 C40 C39 65.0(2) . . . . ?
C32 Zr1 C40 C39 -112.6(2) . . . . ?
C20 Zr1 C40 C39 109.35(18) . . . . ?
C33 Zr1 C40 C39 -76.72(17) . . . . ?
C14 Zr1 C40 C39 94.37(17) . . . . ?
C19 Zr1 C40 C39 119.32(16) . . . . ?
C34 Zr1 C40 C39 -36.66(16) . . . . ?
C41 C42 C43 C44 -179.9(6) . . . . ?
C42 C43 C44 C45 -176.8(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.066
#===end

_database_code_depnum_ccdc_archive 'CCDC 1003258'
