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

#######################################################################
#
#                 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_compound6

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H92 Cl2 N4 O4'
_chemical_formula_sum            'C80 H92 Cl2 N4 O4'
_chemical_formula_weight         1244.48
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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)

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

_cell_length_a                   10.3062(11)
_cell_length_b                   31.646(4)
_cell_length_c                   11.0699(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.483(2)
_cell_angle_gamma                90.00
_cell_volume                     3561.2(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    5174
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      24.05

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1332
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9333
_exptl_absorpt_correction_T_max  0.9693
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17778
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.00
_diffrn_reflns_theta_max         25.25
_reflns_number_total             11028
_reflns_number_gt                9062
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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)+(0.0777P)²+1.2411P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(6)
_refine_ls_number_reflns         11028
_refine_ls_number_parameters     815
_refine_ls_number_restraints     481
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1458
_refine_ls_wR_factor_gt          0.1347
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.054
_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 0.7342(6) 0.64029(15) 0.3105(4) 0.0616(13) Uani 1 1 d U . .
C2 C 0.7468(8) 0.68657(18) 0.2692(5) 0.0879(19) Uani 1 1 d U . .
H2A H 0.7245 0.6883 0.1798 0.132 Uiso 1 1 calc R . .
H2B H 0.8374 0.6963 0.2952 0.132 Uiso 1 1 calc R . .
H2C H 0.6865 0.7045 0.3064 0.132 Uiso 1 1 calc R . .
C3 C 0.8297(7) 0.6134(2) 0.2451(5) 0.0830(18) Uani 1 1 d U . .
H3A H 0.8316 0.5843 0.2752 0.125 Uiso 1 1 calc R . .
H3B H 0.9184 0.6255 0.2627 0.125 Uiso 1 1 calc R . .
H3C H 0.7989 0.6137 0.1565 0.125 Uiso 1 1 calc R . .
C4 C 0.7793(5) 0.63931(15) 0.4482(4) 0.0529(11) Uani 1 1 d U . .
H4A H 0.7258 0.6590 0.4877 0.079 Uiso 1 1 calc R . .
H4B H 0.8720 0.6477 0.4670 0.079 Uiso 1 1 calc R . .
H4C H 0.7691 0.6106 0.4788 0.079 Uiso 1 1 calc R . .
C5 C 0.5946(6) 0.62380(14) 0.2789(3) 0.0581(13) Uani 1 1 d U . .
C6 C 0.5608(5) 0.58187(13) 0.3055(3) 0.0458(10) Uani 1 1 d U . .
C7 C 0.4318(5) 0.56712(13) 0.2795(3) 0.0504(11) Uani 1 1 d U . .
C8 C 0.3336(6) 0.59432(17) 0.2216(4) 0.0706(16) Uani 1 1 d U . .
H8 H 0.2453 0.5848 0.2014 0.085 Uiso 1 1 calc R . .
C9 C 0.3664(7) 0.63541(18) 0.1940(4) 0.0818(19) Uani 1 1 d U . .
H9 H 0.3001 0.6540 0.1548 0.098 Uiso 1 1 calc R . .
C10 C 0.4926(7) 0.64915(16) 0.2227(4) 0.0702(16) Uani 1 1 d U . .
H10 H 0.5118 0.6775 0.2034 0.084 Uiso 1 1 calc R . .
C11 C 0.3944(4) 0.52209(13) 0.3017(3) 0.0464(10) Uani 1 1 d U . .
H11A H 0.2988 0.5186 0.2730 0.056 Uiso 1 1 calc R . .
H11B H 0.4410 0.5032 0.2519 0.056 Uiso 1 1 calc R . .
C12 C 0.3709(4) 0.52962(13) 0.5315(3) 0.0403(9) Uani 1 1 d U . .
H12 H 0.3901 0.5606 0.5314 0.048 Uiso 1 1 calc R . .
C13 C 0.4538(3) 0.50851(12) 0.6475(3) 0.0332(8) Uani 1 1 d U . .
H13 H 0.3928 0.4948 0.6972 0.040 Uiso 1 1 calc R . .
C14 C 0.5060(3) 0.47833(12) 0.4731(3) 0.0347(8) Uani 1 1 d U . .
H14 H 0.5466 0.4601 0.4223 0.042 Uiso 1 1 calc R . .
C15 C 0.2261(4) 0.52281(16) 0.5206(4) 0.0526(11) Uani 1 1 d U . .
C16 C 0.1382(7) 0.5531(3) 0.5056(8) 0.119(3) Uani 1 1 d U . .
H16 H 0.1639 0.5817 0.4982 0.143 Uiso 1 1 calc R . .
C17 C -0.0060(8) 0.5415(4) 0.5005(10) 0.141(3) Uani 1 1 d U . .
H17 H -0.0702 0.5633 0.4931 0.169 Uiso 1 1 calc R . .
C18 C -0.0406(7) 0.5047(3) 0.5057(8) 0.115(3) Uani 1 1 d U . .
H18 H -0.1322 0.4988 0.4943 0.138 Uiso 1 1 calc R . .
C19 C 0.0422(5) 0.4725(2) 0.5262(5) 0.0786(17) Uani 1 1 d U . .
H19 H 0.0112 0.4446 0.5358 0.094 Uiso 1 1 calc R . .
C20 C 0.1760(4) 0.48065(19) 0.5333(5) 0.0673(15) Uani 1 1 d U . .
H20 H 0.2364 0.4578 0.5469 0.081 Uiso 1 1 calc R . .
C21 C 0.5435(3) 0.53877(12) 0.7280(3) 0.0327(8) Uani 1 1 d U . .
C22 C 0.5264(4) 0.54571(13) 0.8470(4) 0.0418(9) Uani 1 1 d U . .
H22 H 0.4588 0.5312 0.8788 0.050 Uiso 1 1 calc R . .
C23 C 0.6063(5) 0.57350(16) 0.9203(4) 0.0548(12) Uani 1 1 d U . .
H23 H 0.5941 0.5779 1.0026 0.066 Uiso 1 1 calc R . .
C24 C 0.7037(4) 0.59486(14) 0.8750(4) 0.0502(11) Uani 1 1 d U . .
H24 H 0.7583 0.6143 0.9255 0.060 Uiso 1 1 calc R . .
C25 C 0.7219(4) 0.58808(14) 0.7567(4) 0.0505(11) Uani 1 1 d U . .
H25 H 0.7895 0.6028 0.7254 0.061 Uiso 1 1 calc R . .
C26 C 0.6428(4) 0.55997(13) 0.6823(4) 0.0400(9) Uani 1 1 d U . .
H26 H 0.6564 0.5552 0.6006 0.048 Uiso 1 1 calc R . .
C27 C 0.6098(3) 0.44429(12) 0.6661(3) 0.0350(8) Uani 1 1 d U . .
H27A H 0.6902 0.4583 0.7090 0.042 Uiso 1 1 calc R . .
H27B H 0.6368 0.4223 0.6117 0.042 Uiso 1 1 calc R . .
C28 C 0.5375(3) 0.42398(12) 0.7588(3) 0.0336(8) Uani 1 1 d U . .
C29 C 0.4316(3) 0.39679(12) 0.7237(3) 0.0343(8) Uani 1 1 d U . .
C30 C 0.3608(4) 0.37953(12) 0.8118(3) 0.0382(9) Uani 1 1 d U . .
C31 C 0.4034(4) 0.39106(13) 0.9330(4) 0.0418(9) Uani 1 1 d U . .
H31 H 0.3575 0.3802 0.9939 0.050 Uiso 1 1 calc R . .
C32 C 0.5093(4) 0.41756(13) 0.9690(3) 0.0376(8) Uani 1 1 d U . .
H32 H 0.5355 0.4243 1.0531 0.045 Uiso 1 1 calc R . .
C33 C 0.5764(4) 0.43410(12) 0.8821(3) 0.0363(8) Uani 1 1 d U . .
H33 H 0.6491 0.4524 0.9062 0.044 Uiso 1 1 calc R . .
C34 C 0.2495(4) 0.34749(14) 0.7768(4) 0.0483(10) Uani 1 1 d U . .
C35 C 0.1853(5) 0.33478(19) 0.8879(5) 0.0660(13) Uani 1 1 d U . .
H35A H 0.1133 0.3149 0.8616 0.099 Uiso 1 1 calc R . .
H35B H 0.1506 0.3600 0.9228 0.099 Uiso 1 1 calc R . .
H35C H 0.2512 0.3213 0.9500 0.099 Uiso 1 1 calc R . .
C36 C 0.3080(5) 0.30761(16) 0.7284(5) 0.0624(13) Uani 1 1 d U . .
H36A H 0.3390 0.3141 0.6515 0.094 Uiso 1 1 calc R . .
H36B H 0.2405 0.2856 0.7141 0.094 Uiso 1 1 calc R . .
H36C H 0.3820 0.2976 0.7889 0.094 Uiso 1 1 calc R . .
C37 C 0.1392(4) 0.36508(17) 0.6780(4) 0.0585(12) Uani 1 1 d U . .
H37A H 0.1756 0.3719 0.6039 0.088 Uiso 1 1 calc R . .
H37B H 0.1024 0.3907 0.7088 0.088 Uiso 1 1 calc R . .
H37C H 0.0698 0.3438 0.6586 0.088 Uiso 1 1 calc R . .
C38 C 1.0637(4) 0.48870(15) -0.0482(4) 0.0507(11) Uani 1 1 d U . .
C39 C 1.1814(5) 0.5031(2) -0.1077(5) 0.0734(16) Uani 1 1 d U . .
H39A H 1.2252 0.4783 -0.1354 0.110 Uiso 1 1 calc R . .
H39B H 1.2437 0.5187 -0.0476 0.110 Uiso 1 1 calc R . .
H39C H 1.1501 0.5213 -0.1779 0.110 Uiso 1 1 calc R . .
C40 C 0.9954(5) 0.52821(17) -0.0095(5) 0.0666(14) Uani 1 1 d U . .
H40A H 0.9783 0.5479 -0.0786 0.100 Uiso 1 1 calc R . .
H40B H 1.0522 0.5418 0.0593 0.100 Uiso 1 1 calc R . .
H40C H 0.9119 0.5202 0.0156 0.100 Uiso 1 1 calc R . .
C41 C 0.9704(5) 0.4645(2) -0.1480(4) 0.0640(14) Uani 1 1 d U . .
H41A H 1.0140 0.4388 -0.1700 0.096 Uiso 1 1 calc R . .
H41B H 0.9480 0.4825 -0.2205 0.096 Uiso 1 1 calc R . .
H41C H 0.8899 0.4569 -0.1167 0.096 Uiso 1 1 calc R . .
C42 C 1.1075(4) 0.46029(12) 0.0621(4) 0.0384(9) Uani 1 1 d U . .
C43 C 1.0171(4) 0.44294(13) 0.1304(3) 0.0371(9) Uani 1 1 d U . .
C44 C 1.0563(3) 0.41855(13) 0.2337(3) 0.0364(8) Uani 1 1 d U . .
C45 C 1.1913(4) 0.41074(13) 0.2708(4) 0.0421(9) Uani 1 1 d U . .
H45 H 1.2197 0.3943 0.3421 0.051 Uiso 1 1 calc R . .
C46 C 1.2818(4) 0.42642(13) 0.2059(4) 0.0420(9) Uani 1 1 d U . .
H46 H 1.3728 0.4207 0.2306 0.050 Uiso 1 1 calc R . .
C47 C 1.2391(4) 0.45085(13) 0.1032(4) 0.0431(10) Uani 1 1 d U . .
H47 H 1.3030 0.4617 0.0586 0.052 Uiso 1 1 calc R . .
C48 C 0.9572(4) 0.39910(13) 0.3038(3) 0.0389(9) Uani 1 1 d U . .
H48A H 1.0036 0.3867 0.3810 0.047 Uiso 1 1 calc R . .
H48B H 0.8971 0.4213 0.3249 0.047 Uiso 1 1 calc R . .
C49 C 0.9402(3) 0.33170(12) 0.1701(3) 0.0325(8) Uani 1 1 d U . .
H49 H 0.9878 0.3435 0.1059 0.039 Uiso 1 1 calc R . .
C50 C 0.8164(3) 0.30664(12) 0.1076(3) 0.0304(7) Uani 1 1 d U . .
H50 H 0.8189 0.2775 0.1429 0.036 Uiso 1 1 calc R . .
C51 C 0.7530(3) 0.36290(11) 0.2127(3) 0.0307(8) Uani 1 1 d U . .
H51 H 0.6978 0.3825 0.2448 0.037 Uiso 1 1 calc R . .
C52 C 1.0344(4) 0.30673(13) 0.2610(3) 0.0374(8) Uani 1 1 d U . .
C53 C 0.9918(4) 0.28945(14) 0.3627(3) 0.0416(9) Uani 1 1 d U . .
H53 H 0.9027 0.2926 0.3734 0.050 Uiso 1 1 calc R . .
C54 C 1.0800(4) 0.26742(16) 0.4492(4) 0.0524(11) Uani 1 1 d U . .
H54 H 1.0507 0.2551 0.5181 0.063 Uiso 1 1 calc R . .
C55 C 1.2074(4) 0.26364(18) 0.4350(4) 0.0607(13) Uani 1 1 d U . .
H55 H 1.2672 0.2492 0.4956 0.073 Uiso 1 1 calc R . .
C56 C 1.2524(5) 0.28029(18) 0.3346(5) 0.0655(14) Uani 1 1 d U . .
H56 H 1.3418 0.2772 0.3249 0.079 Uiso 1 1 calc R . .
C57 C 1.1633(4) 0.30183(17) 0.2477(4) 0.0545(12) Uani 1 1 d U . .
H57 H 1.1926 0.3134 0.1777 0.065 Uiso 1 1 calc R . .
C58 C 0.8013(3) 0.30364(12) -0.0297(3) 0.0343(8) Uani 1 1 d U . .
C59 C 0.8132(5) 0.26545(15) -0.0840(4) 0.0569(12) Uani 1 1 d U . .
H59 H 0.8275 0.2405 -0.0358 0.068 Uiso 1 1 calc R . .
C60 C 0.8041(6) 0.2634(2) -0.2110(5) 0.0796(17) Uani 1 1 d U . .
H60 H 0.8133 0.2368 -0.2486 0.096 Uiso 1 1 calc R . .
C61 C 0.7824(5) 0.29834(19) -0.2821(4) 0.0625(13) Uani 1 1 d U . .
H61 H 0.7748 0.2964 -0.3686 0.075 Uiso 1 1 calc R . .
C62 C 0.7716(5) 0.33664(18) -0.2267(4) 0.0633(14) Uani 1 1 d U . .
H62 H 0.7562 0.3614 -0.2755 0.076 Uiso 1 1 calc R . .
C63 C 0.7828(5) 0.33966(16) -0.1010(4) 0.0563(13) Uani 1 1 d U . .
H63 H 0.7779 0.3665 -0.0636 0.068 Uiso 1 1 calc R . .
C64 C 0.5700(3) 0.31664(12) 0.1253(3) 0.0309(8) Uani 1 1 d U . .
H64A H 0.5332 0.3207 0.0377 0.037 Uiso 1 1 calc R . .
H64B H 0.5187 0.3344 0.1741 0.037 Uiso 1 1 calc R . .
C65 C 0.5554(3) 0.27075(12) 0.1587(3) 0.0318(8) Uani 1 1 d U . .
C66 C 0.5975(3) 0.25557(11) 0.2769(3) 0.0279(7) Uani 1 1 d U . .
C67 C 0.5838(4) 0.21271(12) 0.3067(3) 0.0371(9) Uani 1 1 d U . .
C68 C 0.5262(5) 0.18637(14) 0.2123(4) 0.0537(11) Uani 1 1 d U . .
H68 H 0.5166 0.1572 0.2292 0.064 Uiso 1 1 calc R . .
C69 C 0.4828(5) 0.20081(15) 0.0957(4) 0.0627(13) Uani 1 1 d U . .
H69 H 0.4425 0.1819 0.0341 0.075 Uiso 1 1 calc R . .
C70 C 0.4978(4) 0.24274(14) 0.0684(4) 0.0478(10) Uani 1 1 d U . .
H70 H 0.4686 0.2527 -0.0125 0.057 Uiso 1 1 calc R . .
C71 C 0.6284(4) 0.19605(12) 0.4367(3) 0.0399(9) Uani 1 1 d U . .
C72 C 0.5526(4) 0.21850(15) 0.5249(4) 0.0480(10) Uani 1 1 d U . .
H72A H 0.5669 0.2490 0.5208 0.072 Uiso 1 1 calc R . .
H72B H 0.5836 0.2085 0.6085 0.072 Uiso 1 1 calc R . .
H72C H 0.4585 0.2124 0.5022 0.072 Uiso 1 1 calc R . .
C73 C 0.6020(5) 0.14838(15) 0.4445(4) 0.0618(13) Uani 1 1 d U . .
H73A H 0.5077 0.1429 0.4203 0.093 Uiso 1 1 calc R . .
H73B H 0.6305 0.1387 0.5288 0.093 Uiso 1 1 calc R . .
H73C H 0.6511 0.1332 0.3895 0.093 Uiso 1 1 calc R . .
C74 C 0.7767(4) 0.20260(13) 0.4768(4) 0.0415(9) Uani 1 1 d U . .
H74A H 0.8245 0.1882 0.4193 0.062 Uiso 1 1 calc R . .
H74B H 0.8035 0.1909 0.5591 0.062 Uiso 1 1 calc R . .
H74C H 0.7967 0.2329 0.4777 0.062 Uiso 1 1 calc R . .
C75 C 1.0923(5) 0.19753(17) 0.1274(7) 0.131(3) Uani 1 1 d GU . .
H75 H 1.1612 0.2176 0.1473 0.157 Uiso 1 1 calc R . .
C76 C 1.0606(5) 0.18234(19) 0.0084(6) 0.125(3) Uani 1 1 d GU . .
H76 H 1.1078 0.1920 -0.0531 0.150 Uiso 1 1 calc R . .
C77 C 0.9598(5) 0.15304(18) -0.0207(4) 0.097(2) Uani 1 1 d GU . .
H77 H 0.9381 0.1427 -0.1020 0.117 Uiso 1 1 calc R . .
C78 C 0.8907(5) 0.13893(17) 0.0693(5) 0.101(2) Uani 1 1 d GU . .
H78 H 0.8219 0.1189 0.0495 0.121 Uiso 1 1 calc R . .
C79 C 0.9224(6) 0.1541(2) 0.1883(4) 0.129(3) Uani 1 1 d GU . .
H79 H 0.8752 0.1445 0.2498 0.155 Uiso 1 1 calc R . .
C80 C 1.0232(6) 0.1834(2) 0.2174(5) 0.146(3) Uani 1 1 d GU . .
H80 H 1.0449 0.1938 0.2987 0.175 Uiso 1 1 calc R . .
Cl1 Cl 0.68425(10) 0.47097(3) 0.24756(9) 0.0447(2) Uani 1 1 d . . .
Cl2 Cl 0.56279(11) 0.36873(3) 0.41936(9) 0.0505(3) Uani 1 1 d . . .
N1 N 0.4245(3) 0.50871(10) 0.4300(3) 0.0378(7) Uani 1 1 d . . .
N2 N 0.5259(3) 0.47561(10) 0.5920(3) 0.0329(7) Uani 1 1 d . . .
N3 N 0.8809(3) 0.36620(10) 0.2304(2) 0.0335(7) Uani 1 1 d . . .
N4 N 0.7082(3) 0.33056(9) 0.1475(2) 0.0305(6) Uani 1 1 d . . .
O1 O 0.6568(3) 0.55612(9) 0.3644(2) 0.0445(7) Uani 1 1 d . . .
H1 H 0.6501 0.5321 0.3316 0.067 Uiso 1 1 calc R . .
O2 O 0.3873(3) 0.38783(9) 0.6033(2) 0.0435(7) Uani 1 1 d . . .
H2 H 0.4518 0.3845 0.5667 0.065 Uiso 1 1 calc R . .
O3 O 0.8848(2) 0.44938(10) 0.0872(2) 0.0435(7) Uani 1 1 d . . .
H3 H 0.8472 0.4575 0.1450 0.065 Uiso 1 1 calc R . .
O4 O 0.6594(2) 0.28166(8) 0.3666(2) 0.0295(5) Uani 1 1 d . . .
H4 H 0.6269 0.3060 0.3570 0.044 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 C5 1.516(8) . ?
C1 C4 1.519(6) . ?
C1 C2 1.546(7) . ?
C1 C3 1.565(8) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C10 1.386(7) . ?
C5 C6 1.415(6) . ?
C6 O1 1.362(5) . ?
C6 C7 1.394(7) . ?
C7 C8 1.401(6) . ?
C7 C11 1.507(6) . ?
C8 C9 1.390(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.359(9) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 N1 1.465(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N1 1.486(5) . ?
C12 C15 1.493(6) . ?
C12 C13 1.570(5) . ?
C12 H12 1.0000 . ?
C13 N2 1.471(5) . ?
C13 C21 1.515(5) . ?
C13 H13 1.0000 . ?
C14 N2 1.301(5) . ?
C14 N1 1.313(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.310(8) . ?
C15 C20 1.446(8) . ?
C16 C17 1.522(12) . ?
C16 H16 0.9500 . ?
C17 C18 1.224(12) . ?
C17 H17 0.9500 . ?
C18 C19 1.325(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.393(7) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.375(5) . ?
C21 C26 1.388(6) . ?
C22 C23 1.375(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.372(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.371(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.383(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 N2 1.473(5) . ?
C27 C28 1.507(5) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.394(5) . ?
C28 C33 1.396(5) . ?
C29 O2 1.366(4) . ?
C29 C30 1.419(5) . ?
C30 C31 1.389(6) . ?
C30 C34 1.533(6) . ?
C31 C32 1.382(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.377(5) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C36 1.533(7) . ?
C34 C35 1.542(6) . ?
C34 C37 1.546(6) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 C42 1.524(6) . ?
C38 C40 1.530(7) . ?
C38 C39 1.541(6) . ?
C38 C41 1.543(7) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C47 1.390(5) . ?
C42 C43 1.405(5) . ?
C43 C44 1.383(6) . ?
C43 O3 1.385(4) . ?
C44 C45 1.407(5) . ?
C44 C48 1.511(5) . ?
C45 C46 1.362(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.385(6) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C48 N3 1.467(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 N3 1.465(5) . ?
C49 C52 1.502(5) . ?
C49 C50 1.564(5) . ?
C49 H49 1.0000 . ?
C50 N4 1.474(5) . ?
C50 C58 1.505(5) . ?
C50 H50 1.0000 . ?
C51 N4 1.293(5) . ?
C51 N3 1.304(4) . ?
C51 H51 0.9500 . ?
C52 C57 1.369(6) . ?
C52 C53 1.387(5) . ?
C53 C54 1.394(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.353(6) . ?
C54 H54 0.9500 . ?
C55 C56 1.377(7) . ?
C55 H55 0.9500 . ?
C56 C57 1.394(6) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
C58 C59 1.364(6) . ?
C58 C63 1.382(6) . ?
C59 C60 1.396(7) . ?
C59 H59 0.9500 . ?
C60 C61 1.354(8) . ?
C60 H60 0.9500 . ?
C61 C62 1.371(8) . ?
C61 H61 0.9500 . ?
C62 C63 1.381(6) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 N4 1.473(4) . ?
C64 C65 1.512(5) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 C70 1.394(5) . ?
C65 C66 1.394(5) . ?
C66 O4 1.366(4) . ?
C66 C67 1.409(5) . ?
C67 C68 1.391(5) . ?
C67 C71 1.531(5) . ?
C68 C69 1.372(6) . ?
C68 H68 0.9500 . ?
C69 C70 1.375(6) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
C71 C72 1.523(6) . ?
C71 C74 1.534(6) . ?
C71 C73 1.538(6) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 C76 1.3900 . ?
C75 C80 1.3900 . ?
C75 H75 0.9500 . ?
C76 C77 1.3900 . ?
C76 H76 0.9500 . ?
C77 C78 1.3900 . ?
C77 H77 0.9500 . ?
C78 C79 1.3900 . ?
C78 H78 0.9500 . ?
C79 C80 1.3900 . ?
C79 H79 0.9500 . ?
C80 H80 0.9500 . ?
O1 H1 0.8400 . ?
O2 H2 0.8400 . ?
O3 H3 0.8400 . ?
O4 H4 0.8400 . ?

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
C5 C1 C4 110.2(4) . . ?
C5 C1 C2 112.4(5) . . ?
C4 C1 C2 106.8(4) . . ?
C5 C1 C3 110.6(4) . . ?
C4 C1 C3 110.0(5) . . ?
C2 C1 C3 106.8(5) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C10 C5 C6 116.2(5) . . ?
C10 C5 C1 121.7(5) . . ?
C6 C5 C1 122.1(4) . . ?
O1 C6 C7 119.4(4) . . ?
O1 C6 C5 118.4(4) . . ?
C7 C6 C5 122.0(4) . . ?
C6 C7 C8 118.8(5) . . ?
C6 C7 C11 122.9(4) . . ?
C8 C7 C11 118.1(5) . . ?
C9 C8 C7 119.5(6) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 H8 120.3 . . ?
C10 C9 C8 120.4(5) . . ?
C10 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C9 C10 C5 123.1(5) . . ?
C9 C10 H10 118.4 . . ?
C5 C10 H10 118.4 . . ?
N1 C11 C7 114.4(3) . . ?
N1 C11 H11A 108.7 . . ?
C7 C11 H11A 108.7 . . ?
N1 C11 H11B 108.7 . . ?
C7 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
N1 C12 C15 111.5(3) . . ?
N1 C12 C13 102.0(3) . . ?
C15 C12 C13 114.0(4) . . ?
N1 C12 H12 109.7 . . ?
C15 C12 H12 109.7 . . ?
C13 C12 H12 109.7 . . ?
N2 C13 C21 113.0(3) . . ?
N2 C13 C12 101.8(3) . . ?
C21 C13 C12 114.2(3) . . ?
N2 C13 H13 109.2 . . ?
C21 C13 H13 109.2 . . ?
C12 C13 H13 109.2 . . ?
N2 C14 N1 113.6(3) . . ?
N2 C14 H14 123.2 . . ?
N1 C14 H14 123.2 . . ?
C16 C15 C20 115.9(5) . . ?
C16 C15 C12 124.5(6) . . ?
C20 C15 C12 119.6(4) . . ?
C15 C16 C17 118.7(8) . . ?
C15 C16 H16 120.7 . . ?
C17 C16 H16 120.7 . . ?
C18 C17 C16 121.1(7) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 123.9(8) . . ?
C17 C18 H18 118.1 . . ?
C19 C18 H18 118.1 . . ?
C18 C19 C20 118.0(7) . . ?
C18 C19 H19 121.0 . . ?
C20 C19 H19 121.0 . . ?
C19 C20 C15 122.1(5) . . ?
C19 C20 H20 118.9 . . ?
C15 C20 H20 118.9 . . ?
C22 C21 C26 119.4(3) . . ?
C22 C21 C13 120.2(3) . . ?
C26 C21 C13 120.5(3) . . ?
C23 C22 C21 120.6(4) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C22 120.2(4) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C25 C24 C23 119.7(4) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 120.6(4) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C25 C26 C21 119.5(4) . . ?
C25 C26 H26 120.3 . . ?
C21 C26 H26 120.3 . . ?
N2 C27 C28 110.8(3) . . ?
N2 C27 H27A 109.5 . . ?
C28 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 108.1 . . ?
C29 C28 C33 119.9(3) . . ?
C29 C28 C27 121.7(3) . . ?
C33 C28 C27 118.3(3) . . ?
O2 C29 C28 121.3(3) . . ?
O2 C29 C30 117.6(3) . . ?
C28 C29 C30 120.9(3) . . ?
C31 C30 C29 116.5(4) . . ?
C31 C30 C34 121.4(4) . . ?
C29 C30 C34 122.0(3) . . ?
C32 C31 C30 123.1(4) . . ?
C32 C31 H31 118.4 . . ?
C30 C31 H31 118.4 . . ?
C33 C32 C31 119.5(3) . . ?
C33 C32 H32 120.2 . . ?
C31 C32 H32 120.2 . . ?
C32 C33 C28 120.0(4) . . ?
C32 C33 H33 120.0 . . ?
C28 C33 H33 120.0 . . ?
C30 C34 C36 108.2(4) . . ?
C30 C34 C35 111.9(4) . . ?
C36 C34 C35 108.0(4) . . ?
C30 C34 C37 111.9(4) . . ?
C36 C34 C37 109.6(4) . . ?
C35 C34 C37 107.3(4) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C42 C38 C40 110.3(4) . . ?
C42 C38 C39 111.4(4) . . ?
C40 C38 C39 108.0(4) . . ?
C42 C38 C41 110.4(4) . . ?
C40 C38 C41 110.2(4) . . ?
C39 C38 C41 106.4(4) . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C38 C40 H40A 109.5 . . ?
C38 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C38 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C38 C41 H41A 109.5 . . ?
C38 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C38 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C47 C42 C43 115.9(4) . . ?
C47 C42 C38 122.3(4) . . ?
C43 C42 C38 121.8(3) . . ?
C44 C43 O3 120.3(3) . . ?
C44 C43 C42 122.3(3) . . ?
O3 C43 C42 117.4(3) . . ?
C43 C44 C45 118.6(4) . . ?
C43 C44 C48 121.5(3) . . ?
C45 C44 C48 119.8(4) . . ?
C46 C45 C44 120.8(4) . . ?
C46 C45 H45 119.6 . . ?
C44 C45 H45 119.6 . . ?
C45 C46 C47 119.0(4) . . ?
C45 C46 H46 120.5 . . ?
C47 C46 H46 120.5 . . ?
C46 C47 C42 123.3(4) . . ?
C46 C47 H47 118.3 . . ?
C42 C47 H47 118.3 . . ?
N3 C48 C44 110.5(3) . . ?
N3 C48 H48A 109.5 . . ?
C44 C48 H48A 109.5 . . ?
N3 C48 H48B 109.5 . . ?
C44 C48 H48B 109.5 . . ?
H48A C48 H48B 108.1 . . ?
N3 C49 C52 111.0(3) . . ?
N3 C49 C50 102.0(3) . . ?
C52 C49 C50 114.8(3) . . ?
N3 C49 H49 109.6 . . ?
C52 C49 H49 109.6 . . ?
C50 C49 H49 109.6 . . ?
N4 C50 C58 112.2(3) . . ?
N4 C50 C49 102.1(3) . . ?
C58 C50 C49 114.8(3) . . ?
N4 C50 H50 109.2 . . ?
C58 C50 H50 109.2 . . ?
C49 C50 H50 109.2 . . ?
N4 C51 N3 114.0(3) . . ?
N4 C51 H51 123.0 . . ?
N3 C51 H51 123.0 . . ?
C57 C52 C53 119.0(4) . . ?
C57 C52 C49 121.3(3) . . ?
C53 C52 C49 119.7(3) . . ?
C52 C53 C54 119.8(4) . . ?
C52 C53 H53 120.1 . . ?
C54 C53 H53 120.1 . . ?
C55 C54 C53 120.0(4) . . ?
C55 C54 H54 120.0 . . ?
C53 C54 H54 120.0 . . ?
C54 C55 C56 121.5(4) . . ?
C54 C55 H55 119.3 . . ?
C56 C55 H55 119.3 . . ?
C55 C56 C57 118.2(4) . . ?
C55 C56 H56 120.9 . . ?
C57 C56 H56 120.9 . . ?
C52 C57 C56 121.5(4) . . ?
C52 C57 H57 119.3 . . ?
C56 C57 H57 119.3 . . ?
C59 C58 C63 119.5(4) . . ?
C59 C58 C50 119.9(4) . . ?
C63 C58 C50 120.4(4) . . ?
C58 C59 C60 119.3(5) . . ?
C58 C59 H59 120.4 . . ?
C60 C59 H59 120.4 . . ?
C61 C60 C59 121.6(5) . . ?
C61 C60 H60 119.2 . . ?
C59 C60 H60 119.2 . . ?
C60 C61 C62 118.7(4) . . ?
C60 C61 H61 120.7 . . ?
C62 C61 H61 120.7 . . ?
C61 C62 C63 120.8(5) . . ?
C61 C62 H62 119.6 . . ?
C63 C62 H62 119.6 . . ?
C62 C63 C58 120.0(5) . . ?
C62 C63 H63 120.0 . . ?
C58 C63 H63 120.0 . . ?
N4 C64 C65 112.3(3) . . ?
N4 C64 H64A 109.2 . . ?
C65 C64 H64A 109.2 . . ?
N4 C64 H64B 109.2 . . ?
C65 C64 H64B 109.2 . . ?
H64A C64 H64B 107.9 . . ?
C70 C65 C66 119.0(3) . . ?
C70 C65 C64 118.9(3) . . ?
C66 C65 C64 122.2(3) . . ?
O4 C66 C65 120.7(3) . . ?
O4 C66 C67 117.7(3) . . ?
C65 C66 C67 121.6(3) . . ?
C68 C67 C66 116.6(3) . . ?
C68 C67 C71 121.7(3) . . ?
C66 C67 C71 121.7(3) . . ?
C69 C68 C67 122.7(4) . . ?
C69 C68 H68 118.7 . . ?
C67 C68 H68 118.7 . . ?
C68 C69 C70 119.8(4) . . ?
C68 C69 H69 120.1 . . ?
C70 C69 H69 120.1 . . ?
C69 C70 C65 120.4(4) . . ?
C69 C70 H70 119.8 . . ?
C65 C70 H70 119.8 . . ?
C72 C71 C67 109.6(3) . . ?
C72 C71 C74 110.1(3) . . ?
C67 C71 C74 110.9(3) . . ?
C72 C71 C73 107.9(4) . . ?
C67 C71 C73 111.2(3) . . ?
C74 C71 C73 107.0(3) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C71 C74 H74A 109.5 . . ?
C71 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C71 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C76 C75 C80 120.0 . . ?
C76 C75 H75 120.0 . . ?
C80 C75 H75 120.0 . . ?
C75 C76 C77 120.0 . . ?
C75 C76 H76 120.0 . . ?
C77 C76 H76 120.0 . . ?
C78 C77 C76 120.0 . . ?
C78 C77 H77 120.0 . . ?
C76 C77 H77 120.0 . . ?
C79 C78 C77 120.0 . . ?
C79 C78 H78 120.0 . . ?
C77 C78 H78 120.0 . . ?
C80 C79 C78 120.0 . . ?
C80 C79 H79 120.0 . . ?
C78 C79 H79 120.0 . . ?
C79 C80 C75 120.0 . . ?
C79 C80 H80 120.0 . . ?
C75 C80 H80 120.0 . . ?
C14 N1 C11 125.8(3) . . ?
C14 N1 C12 110.3(3) . . ?
C11 N1 C12 123.9(3) . . ?
C14 N2 C13 111.7(3) . . ?
C14 N2 C27 126.0(3) . . ?
C13 N2 C27 122.3(3) . . ?
C51 N3 C49 111.1(3) . . ?
C51 N3 C48 125.2(3) . . ?
C49 N3 C48 123.7(3) . . ?
C51 N4 C64 125.2(3) . . ?
C51 N4 C50 110.8(3) . . ?
C64 N4 C50 123.7(3) . . ?
C6 O1 H1 109.5 . . ?
C29 O2 H2 109.5 . . ?
C43 O3 H3 109.5 . . ?
C66 O4 H4 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.047
_database_code_depnum_ccdc_archive 'CCDC 975119'
#######################################################################
#
#                 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_compound11

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H42 Br N3 O3 Zr'
_chemical_formula_sum            'C37 H42 Br N3 O3 Zr'
_chemical_formula_weight         747.87
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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   P2(1)2(1)2(1)

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

_cell_length_a                   11.0875(7)
_cell_length_b                   14.6797(10)
_cell_length_c                   21.1257(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3438.4(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    7984
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.43

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    1.521
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5675
_exptl_absorpt_correction_T_max  0.6582
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20249
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.93
_diffrn_reflns_theta_max         27.62
_reflns_number_total             7875
_reflns_number_gt                7178
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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)+(0.0127P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.016(5)
_refine_ls_number_reflns         7875
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0611
_refine_ls_wR_factor_gt          0.0598
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.17487(2) 0.92355(2) -0.138444(12) 0.02530(7) Uani 1 1 d . . .
C1 C 0.2527(2) 0.95660(16) -0.06115(11) 0.0142(5) Uani 1 1 d . . .
C2 C 0.3277(2) 0.91111(17) -0.10407(12) 0.0177(5) Uani 1 1 d . . .
H2 H 0.2931 0.8766 -0.1375 0.021 Uiso 1 1 calc R . .
C3 C 0.4524(2) 0.91610(18) -0.09816(12) 0.0200(5) Uani 1 1 d . . .
H3 H 0.5023 0.8852 -0.1278 0.024 Uiso 1 1 calc R . .
C4 C 0.5046(2) 0.96548(18) -0.04970(12) 0.0217(6) Uani 1 1 d . . .
H4 H 0.5898 0.9686 -0.0456 0.026 Uiso 1 1 calc R . .
C5 C 0.4297(2) 1.01084(18) -0.00674(12) 0.0190(6) Uani 1 1 d . . .
H5 H 0.4651 1.0448 0.0267 0.023 Uiso 1 1 calc R . .
C6 C 0.3046(2) 1.00742(16) -0.01177(11) 0.0154(5) Uani 1 1 d . . .
C7 C 0.2282(2) 1.06522(17) 0.03236(11) 0.0155(5) Uani 1 1 d . . .
H7A H 0.2824 1.1067 0.0560 0.019 Uiso 1 1 calc R . .
H7B H 0.1739 1.1035 0.0063 0.019 Uiso 1 1 calc R . .
C8 C 0.1951(2) 0.99641(16) 0.14417(11) 0.0137(5) Uani 1 1 d . . .
H8 H 0.2606 0.9496 0.1437 0.016 Uiso 1 1 calc R . .
C9 C 0.2367(2) 1.07893(17) 0.18038(11) 0.0138(5) Uani 1 1 d . . .
C10 C 0.1712(3) 1.16017(18) 0.17853(13) 0.0230(6) Uani 1 1 d . . .
H10 H 0.1028 1.1651 0.1517 0.028 Uiso 1 1 calc R . .
C11 C 0.2053(3) 1.23375(19) 0.21566(14) 0.0268(7) Uani 1 1 d . . .
H11 H 0.1606 1.2889 0.2141 0.032 Uiso 1 1 calc R . .
C12 C 0.3051(2) 1.22646(18) 0.25510(12) 0.0217(6) Uani 1 1 d . . .
H12 H 0.3285 1.2765 0.2809 0.026 Uiso 1 1 calc R . .
C13 C 0.3702(2) 1.14633(19) 0.25676(13) 0.0218(6) Uani 1 1 d . . .
H13 H 0.4386 1.1413 0.2836 0.026 Uiso 1 1 calc R . .
C14 C 0.3361(2) 1.07340(18) 0.21956(11) 0.0177(5) Uani 1 1 d . . .
H14 H 0.3817 1.0186 0.2209 0.021 Uiso 1 1 calc R . .
C15 C 0.0788(2) 0.95430(16) 0.17181(11) 0.0144(5) Uani 1 1 d . . .
H15 H 0.0292 1.0040 0.1910 0.017 Uiso 1 1 calc R . .
C16 C 0.0991(2) 0.88143(17) 0.22101(12) 0.0147(5) Uani 1 1 d . . .
C17 C 0.0779(2) 0.90108(17) 0.28454(12) 0.0186(6) Uani 1 1 d . . .
H17 H 0.0484 0.9595 0.2960 0.022 Uiso 1 1 calc R . .
C18 C 0.0989(2) 0.8376(2) 0.33075(13) 0.0251(6) Uani 1 1 d . . .
H18 H 0.0853 0.8525 0.3739 0.030 Uiso 1 1 calc R . .
C19 C 0.1401(2) 0.75122(19) 0.31418(13) 0.0237(6) Uani 1 1 d . . .
H19 H 0.1543 0.7068 0.3460 0.028 Uiso 1 1 calc R . .
C20 C 0.1604(3) 0.73042(19) 0.25176(13) 0.0256(6) Uani 1 1 d . . .
H20 H 0.1880 0.6714 0.2405 0.031 Uiso 1 1 calc R . .
C21 C 0.1408(2) 0.79515(18) 0.20508(13) 0.0216(6) Uani 1 1 d . . .
H21 H 0.1559 0.7804 0.1620 0.026 Uiso 1 1 calc R . .
C22 C -0.1048(2) 0.88354(17) 0.11889(12) 0.0152(5) Uani 1 1 d . . .
H22A H -0.1082 0.8421 0.1558 0.018 Uiso 1 1 calc R . .
H22B H -0.1226 0.8472 0.0805 0.018 Uiso 1 1 calc R . .
C23 C -0.1989(2) 0.95651(17) 0.12623(11) 0.0155(5) Uani 1 1 d . . .
C24 C -0.2554(2) 0.97458(19) 0.18382(12) 0.0185(5) Uani 1 1 d . . .
H24 H -0.2328 0.9408 0.2203 0.022 Uiso 1 1 calc R . .
C25 C -0.3436(2) 1.04050(18) 0.18893(12) 0.0205(6) Uani 1 1 d . . .
H25 H -0.3827 1.0507 0.2283 0.025 Uiso 1 1 calc R . .
C26 C -0.3747(2) 1.09158(17) 0.13657(13) 0.0198(6) Uani 1 1 d . . .
H26 H -0.4346 1.1376 0.1401 0.024 Uiso 1 1 calc R . .
C27 C -0.3189(2) 1.07597(18) 0.07882(11) 0.0167(5) Uani 1 1 d . . .
H27 H -0.3403 1.1117 0.0430 0.020 Uiso 1 1 calc R . .
C28 C -0.2316(2) 1.00832(17) 0.07300(11) 0.0139(5) Uani 1 1 d . . .
C29 C 0.0558(2) 0.96760(17) 0.06244(11) 0.0137(5) Uani 1 1 d . . .
C30 C -0.1005(3) 0.73709(18) -0.04811(14) 0.0269(6) Uani 1 1 d . . .
H30A H -0.1708 0.7604 -0.0720 0.032 Uiso 1 1 calc R . .
H30B H -0.1292 0.6955 -0.0144 0.032 Uiso 1 1 calc R . .
C31 C -0.0116(3) 0.6893(2) -0.09174(15) 0.0363(8) Uani 1 1 d . . .
H31A H -0.0153 0.7150 -0.1350 0.044 Uiso 1 1 calc R . .
H31B H -0.0284 0.6231 -0.0938 0.044 Uiso 1 1 calc R . .
C32 C 0.1121(3) 0.7077(2) -0.06116(15) 0.0351(8) Uani 1 1 d . . .
H32A H 0.1501 0.6502 -0.0469 0.042 Uiso 1 1 calc R . .
H32B H 0.1669 0.7386 -0.0913 0.042 Uiso 1 1 calc R . .
C33 C 0.0839(2) 0.76862(18) -0.00546(14) 0.0224(6) Uani 1 1 d . . .
H33A H 0.0762 0.7325 0.0339 0.027 Uiso 1 1 calc R . .
H33B H 0.1478 0.8149 0.0004 0.027 Uiso 1 1 calc R . .
C34 C -0.1138(3) 1.17481(18) -0.04997(13) 0.0231(6) Uani 1 1 d . . .
H34A H -0.1924 1.1437 -0.0449 0.028 Uiso 1 1 calc R . .
H34B H -0.1209 1.2178 -0.0859 0.028 Uiso 1 1 calc R . .
C35 C -0.0848(3) 1.2278(2) 0.01018(15) 0.0361(8) Uani 1 1 d . . .
H35A H -0.0730 1.1851 0.0453 0.054 Uiso 1 1 calc R . .
H35B H -0.1518 1.2690 0.0201 0.054 Uiso 1 1 calc R . .
H35C H -0.0110 1.2634 0.0038 0.054 Uiso 1 1 calc R . .
C36 C 0.0740(2) 1.14579(19) -0.10537(13) 0.0222(6) Uani 1 1 d . . .
H36A H 0.1498 1.1115 -0.0986 0.027 Uiso 1 1 calc R . .
H36B H 0.0886 1.2098 -0.0928 0.027 Uiso 1 1 calc R . .
C37 C 0.0425(3) 1.1432(2) -0.17478(13) 0.0350(7) Uani 1 1 d . . .
H37A H 0.0336 1.0797 -0.1884 0.053 Uiso 1 1 calc R . .
H37B H 0.1068 1.1723 -0.1993 0.053 Uiso 1 1 calc R . .
H37C H -0.0335 1.1757 -0.1818 0.053 Uiso 1 1 calc R . .
N1 N 0.15454(18) 1.01484(14) 0.07828(9) 0.0144(4) Uani 1 1 d . . .
N2 N 0.01790(17) 0.92205(15) 0.11369(9) 0.0137(4) Uani 1 1 d . . .
N3 N -0.02056(19) 1.10711(14) -0.06422(10) 0.0168(5) Uani 1 1 d . . .
O1 O 0.13205(14) 0.95232(11) -0.06882(8) 0.0149(4) Uani 1 1 d . . .
O2 O -0.18095(15) 0.99106(11) 0.01620(7) 0.0145(4) Uani 1 1 d . . .
O3 O -0.02997(16) 0.81145(11) -0.02170(8) 0.0186(4) Uani 1 1 d . . .
Zr1 Zr -0.03815(2) 0.972555(16) -0.040721(11) 0.01262(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Zr1 2.6604(4) . ?
C1 O1 1.349(3) . ?
C1 C2 1.400(3) . ?
C1 C6 1.406(3) . ?
C2 C3 1.391(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.398(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.392(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.519(3) . ?
C7 N1 1.468(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 N1 1.487(3) . ?
C8 C9 1.505(3) . ?
C8 C15 1.544(3) . ?
C8 H8 1.0000 . ?
C9 C14 1.381(3) . ?
C9 C10 1.397(4) . ?
C10 C11 1.388(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.389(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.380(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.381(4) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 N2 1.479(3) . ?
C15 C16 1.508(3) . ?
C15 H15 1.0000 . ?
C16 C21 1.390(4) . ?
C16 C17 1.393(4) . ?
C17 C18 1.369(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.393(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.372(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.387(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 N2 1.477(3) . ?
C22 C23 1.504(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.394(3) . ?
C23 C28 1.405(3) . ?
C24 C25 1.380(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.380(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.392(4) . ?
C27 H27 0.9500 . ?
C28 O2 1.349(3) . ?
C29 N1 1.339(3) . ?
C29 N2 1.340(3) . ?
C29 Zr1 2.416(2) . ?
C30 O3 1.454(3) . ?
C30 C31 1.521(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.540(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.511(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 O3 1.451(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 N3 1.466(3) . ?
C34 C35 1.524(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 N3 1.475(3) . ?
C36 C37 1.508(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
N3 Zr1 2.046(2) . ?
O1 Zr1 2.0004(16) . ?
O2 Zr1 2.0067(17) . ?
O3 Zr1 2.4005(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 119.3(2) . . ?
O1 C1 C6 121.3(2) . . ?
C2 C1 C6 119.4(2) . . ?
C3 C2 C1 120.5(2) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 120.7(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C3 C4 C5 118.8(2) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C6 C5 C4 121.6(2) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C5 C6 C1 118.9(2) . . ?
C5 C6 C7 119.3(2) . . ?
C1 C6 C7 121.6(2) . . ?
N1 C7 C6 115.8(2) . . ?
N1 C7 H7A 108.3 . . ?
C6 C7 H7A 108.3 . . ?
N1 C7 H7B 108.3 . . ?
C6 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
N1 C8 C9 114.95(19) . . ?
N1 C8 C15 100.06(18) . . ?
C9 C8 C15 112.69(19) . . ?
N1 C8 H8 109.6 . . ?
C9 C8 H8 109.6 . . ?
C15 C8 H8 109.6 . . ?
C14 C9 C10 118.8(2) . . ?
C14 C9 C8 120.1(2) . . ?
C10 C9 C8 120.9(2) . . ?
C11 C10 C9 120.5(3) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 119.8(3) . . ?
C10 C11 H11 120.1 . . ?
C12 C11 H11 120.1 . . ?
C13 C12 C11 119.8(3) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C14 120.2(2) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C9 120.9(2) . . ?
C13 C14 H14 119.5 . . ?
C9 C14 H14 119.5 . . ?
N2 C15 C16 114.4(2) . . ?
N2 C15 C8 101.25(18) . . ?
C16 C15 C8 114.82(19) . . ?
N2 C15 H15 108.7 . . ?
C16 C15 H15 108.7 . . ?
C8 C15 H15 108.7 . . ?
C21 C16 C17 118.6(2) . . ?
C21 C16 C15 121.9(2) . . ?
C17 C16 C15 119.5(2) . . ?
C18 C17 C16 121.2(2) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 119.7(3) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C20 C19 C18 119.9(2) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 120.4(3) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C20 C21 C16 120.3(2) . . ?
C20 C21 H21 119.9 . . ?
C16 C21 H21 119.9 . . ?
N2 C22 C23 112.0(2) . . ?
N2 C22 H22A 109.2 . . ?
C23 C22 H22A 109.2 . . ?
N2 C22 H22B 109.2 . . ?
C23 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C24 C23 C28 118.6(2) . . ?
C24 C23 C22 122.5(2) . . ?
C28 C23 C22 118.8(2) . . ?
C25 C24 C23 121.4(2) . . ?
C25 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
C24 C25 C26 119.7(2) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C25 C26 C27 120.2(2) . . ?
C25 C26 H26 119.9 . . ?
C27 C26 H26 119.9 . . ?
C26 C27 C28 120.4(2) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
O2 C28 C27 120.1(2) . . ?
O2 C28 C23 120.2(2) . . ?
C27 C28 C23 119.7(2) . . ?
N1 C29 N2 108.2(2) . . ?
N1 C29 Zr1 124.22(16) . . ?
N2 C29 Zr1 127.50(16) . . ?
O3 C30 C31 103.3(2) . . ?
O3 C30 H30A 111.1 . . ?
C31 C30 H30A 111.1 . . ?
O3 C30 H30B 111.1 . . ?
C31 C30 H30B 111.1 . . ?
H30A C30 H30B 109.1 . . ?
C30 C31 C32 104.0(2) . . ?
C30 C31 H31A 111.0 . . ?
C32 C31 H31A 111.0 . . ?
C30 C31 H31B 111.0 . . ?
C32 C31 H31B 111.0 . . ?
H31A C31 H31B 109.0 . . ?
C33 C32 C31 104.2(2) . . ?
C33 C32 H32A 110.9 . . ?
C31 C32 H32A 110.9 . . ?
C33 C32 H32B 110.9 . . ?
C31 C32 H32B 110.9 . . ?
H32A C32 H32B 108.9 . . ?
O3 C33 C32 104.6(2) . . ?
O3 C33 H33A 110.8 . . ?
C32 C33 H33A 110.8 . . ?
O3 C33 H33B 110.8 . . ?
C32 C33 H33B 110.8 . . ?
H33A C33 H33B 108.9 . . ?
N3 C34 C35 111.6(2) . . ?
N3 C34 H34A 109.3 . . ?
C35 C34 H34A 109.3 . . ?
N3 C34 H34B 109.3 . . ?
C35 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N3 C36 C37 113.5(2) . . ?
N3 C36 H36A 108.9 . . ?
C37 C36 H36A 108.9 . . ?
N3 C36 H36B 108.9 . . ?
C37 C36 H36B 108.9 . . ?
H36A C36 H36B 107.7 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C29 N1 C7 123.43(19) . . ?
C29 N1 C8 112.75(19) . . ?
C7 N1 C8 122.82(19) . . ?
C29 N2 C22 122.66(19) . . ?
C29 N2 C15 111.60(19) . . ?
C22 N2 C15 118.76(19) . . ?
C34 N3 C36 111.2(2) . . ?
C34 N3 Zr1 122.52(16) . . ?
C36 N3 Zr1 125.61(17) . . ?
C1 O1 Zr1 153.25(15) . . ?
C28 O2 Zr1 152.52(15) . . ?
C33 O3 C30 103.47(19) . . ?
C33 O3 Zr1 119.95(14) . . ?
C30 O3 Zr1 130.93(16) . . ?
O1 Zr1 O2 160.43(7) . . ?
O1 Zr1 N3 88.94(8) . . ?
O2 Zr1 N3 95.16(8) . . ?
O1 Zr1 O3 82.40(6) . . ?
O2 Zr1 O3 93.61(6) . . ?
N3 Zr1 O3 171.16(7) . . ?
O1 Zr1 C29 81.76(7) . . ?
O2 Zr1 C29 78.67(7) . . ?
N3 Zr1 C29 101.94(8) . . ?
O3 Zr1 C29 78.65(7) . . ?
O1 Zr1 Br1 105.49(5) . . ?
O2 Zr1 Br1 92.98(5) . . ?
N3 Zr1 Br1 97.30(6) . . ?
O3 Zr1 Br1 83.40(4) . . ?
C29 Zr1 Br1 159.60(6) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.139
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.062
_database_code_depnum_ccdc_archive 'CCDC 975120'
#######################################################################
#
#                 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_compound15

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H42 Cl N3 O3 Zr'
_chemical_formula_sum            'C37 H42 Cl N3 O3 Zr'
_chemical_formula_weight         703.41
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P2(1)2(1)2(1)

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

_cell_length_a                   11.1599(12)
_cell_length_b                   14.8336(17)
_cell_length_c                   20.608(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3411.5(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    5896
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      27.55

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1464
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8903
_exptl_absorpt_correction_T_max  0.9656
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            20265
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         27.55
_reflns_number_total             7813
_reflns_number_gt                7149
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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)+(0.0273P)²+0.0279P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_number_reflns         7813
_refine_ls_number_parameters     408
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0653
_refine_ls_wR_factor_gt          0.0632
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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
Cl1 Cl -0.15639(6) 0.91780(5) -0.14083(3) 0.02805(15) Uani 1 1 d . . .
C1 C 0.2552(2) 0.95212(15) -0.06579(10) 0.0168(5) Uani 1 1 d . . .
C2 C 0.3294(2) 0.90582(17) -0.10846(11) 0.0211(5) Uani 1 1 d . . .
H2 H 0.2950 0.8705 -0.1421 0.025 Uiso 1 1 calc R . .
C3 C 0.4540(2) 0.91058(17) -0.10261(11) 0.0236(5) Uani 1 1 d . . .
H3 H 0.5034 0.8792 -0.1326 0.028 Uiso 1 1 calc R . .
C4 C 0.50569(19) 0.96056(17) -0.05349(12) 0.0250(5) Uani 1 1 d . . .
H4 H 0.5903 0.9633 -0.0490 0.030 Uiso 1 1 calc R . .
C5 C 0.4315(2) 1.00686(17) -0.01062(12) 0.0231(6) Uani 1 1 d . . .
H5 H 0.4667 1.0415 0.0232 0.028 Uiso 1 1 calc R . .
C6 C 0.3067(2) 1.00383(15) -0.01585(11) 0.0189(5) Uani 1 1 d . . .
C7 C 0.2307(2) 1.06191(16) 0.02847(11) 0.0190(5) Uani 1 1 d . . .
H7A H 0.2845 1.1029 0.0527 0.023 Uiso 1 1 calc R . .
H7B H 0.1778 1.0998 0.0012 0.023 Uiso 1 1 calc R . .
C8 C 0.19559(19) 0.99684(15) 0.14339(10) 0.0165(5) Uani 1 1 d . . .
H8 H 0.2621 0.9517 0.1436 0.020 Uiso 1 1 calc R . .
C9 C 0.2348(2) 1.07996(16) 0.17898(10) 0.0169(5) Uani 1 1 d . . .
C10 C 0.1650(2) 1.15773(17) 0.17848(12) 0.0249(6) Uani 1 1 d . . .
H10 H 0.0939 1.1595 0.1532 0.030 Uiso 1 1 calc R . .
C11 C 0.1982(2) 1.23290(18) 0.21457(13) 0.0269(6) Uani 1 1 d . . .
H11 H 0.1499 1.2856 0.2139 0.032 Uiso 1 1 calc R . .
C12 C 0.3014(2) 1.23062(18) 0.25137(12) 0.0244(6) Uani 1 1 d . . .
H12 H 0.3242 1.2819 0.2761 0.029 Uiso 1 1 calc R . .
C13 C 0.3718(2) 1.15379(19) 0.25232(12) 0.0254(6) Uani 1 1 d . . .
H13 H 0.4428 1.1524 0.2777 0.030 Uiso 1 1 calc R . .
C14 C 0.3389(2) 1.07916(17) 0.21637(11) 0.0213(5) Uani 1 1 d . . .
H14 H 0.3878 1.0267 0.2172 0.026 Uiso 1 1 calc R . .
C15 C 0.08147(19) 0.95360(15) 0.17207(10) 0.0154(5) Uani 1 1 d . . .
H15 H 0.0324 1.0020 0.1929 0.018 Uiso 1 1 calc R . .
C16 C 0.10194(19) 0.88010(16) 0.22098(11) 0.0166(5) Uani 1 1 d . . .
C17 C 0.0818(2) 0.89669(17) 0.28625(11) 0.0219(5) Uani 1 1 d . . .
H17 H 0.0534 0.9542 0.2995 0.026 Uiso 1 1 calc R . .
C18 C 0.1026(2) 0.83070(19) 0.33235(12) 0.0269(6) Uani 1 1 d . . .
H18 H 0.0890 0.8432 0.3770 0.032 Uiso 1 1 calc R . .
C19 C 0.1431(2) 0.74656(19) 0.31350(12) 0.0270(6) Uani 1 1 d . . .
H19 H 0.1568 0.7012 0.3452 0.032 Uiso 1 1 calc R . .
C20 C 0.1638(2) 0.72837(18) 0.24837(12) 0.0266(6) Uani 1 1 d . . .
H20 H 0.1917 0.6707 0.2352 0.032 Uiso 1 1 calc R . .
C21 C 0.1434(2) 0.79513(17) 0.20272(11) 0.0218(5) Uani 1 1 d . . .
H21 H 0.1578 0.7828 0.1582 0.026 Uiso 1 1 calc R . .
C22 C -0.1026(2) 0.88594(16) 0.11840(11) 0.0182(5) Uani 1 1 d . . .
H22A H -0.1063 0.8464 0.1571 0.022 Uiso 1 1 calc R . .
H22B H -0.1204 0.8485 0.0798 0.022 Uiso 1 1 calc R . .
C23 C -0.19617(18) 0.95850(16) 0.12443(10) 0.0173(5) Uani 1 1 d . . .
C24 C -0.25324(19) 0.97790(18) 0.18290(11) 0.0216(5) Uani 1 1 d . . .
H24 H -0.2312 0.9455 0.2208 0.026 Uiso 1 1 calc R . .
C25 C -0.3412(2) 1.04326(17) 0.18703(11) 0.0225(5) Uani 1 1 d . . .
H25 H -0.3803 1.0547 0.2271 0.027 Uiso 1 1 calc R . .
C26 C -0.3718(2) 1.09187(17) 0.13216(12) 0.0221(5) Uani 1 1 d . . .
H26 H -0.4315 1.1374 0.1347 0.026 Uiso 1 1 calc R . .
C27 C -0.3158(2) 1.07445(17) 0.07344(11) 0.0195(5) Uani 1 1 d . . .
H27 H -0.3370 1.1084 0.0361 0.023 Uiso 1 1 calc R . .
C28 C -0.22875(19) 1.00779(16) 0.06879(10) 0.0170(5) Uani 1 1 d . . .
C29 C 0.05800(17) 0.96744(16) 0.05972(9) 0.0162(5) Uani 1 1 d . . .
C30 C -0.0998(2) 0.73822(16) -0.05041(14) 0.0275(6) Uani 1 1 d . . .
H30A H -0.1690 0.7620 -0.0752 0.033 Uiso 1 1 calc R . .
H30B H -0.1296 0.6984 -0.0154 0.033 Uiso 1 1 calc R . .
C31 C -0.0131(3) 0.68818(19) -0.09478(13) 0.0392(8) Uani 1 1 d . . .
H31A H -0.0164 0.7124 -0.1395 0.047 Uiso 1 1 calc R . .
H31B H -0.0315 0.6229 -0.0959 0.047 Uiso 1 1 calc R . .
C32 C 0.1108(3) 0.70533(19) -0.06396(14) 0.0375(7) Uani 1 1 d . . .
H32A H 0.1471 0.6483 -0.0487 0.045 Uiso 1 1 calc R . .
H32B H 0.1658 0.7342 -0.0954 0.045 Uiso 1 1 calc R . .
C33 C 0.0847(2) 0.76772(17) -0.00752(13) 0.0252(6) Uani 1 1 d . . .
H33A H 0.0769 0.7332 0.0334 0.030 Uiso 1 1 calc R . .
H33B H 0.1493 0.8129 -0.0024 0.030 Uiso 1 1 calc R . .
C34 C -0.1087(2) 1.17123(17) -0.05718(12) 0.0268(6) Uani 1 1 d . . .
H34A H -0.1871 1.1409 -0.0517 0.032 Uiso 1 1 calc R . .
H34B H -0.1154 1.2131 -0.0944 0.032 Uiso 1 1 calc R . .
C35 C -0.0800(3) 1.22479(19) 0.00374(14) 0.0388(7) Uani 1 1 d . . .
H35A H -0.0689 1.1833 0.0403 0.058 Uiso 1 1 calc R . .
H35B H -0.1462 1.2661 0.0133 0.058 Uiso 1 1 calc R . .
H35C H -0.0063 1.2595 -0.0031 0.058 Uiso 1 1 calc R . .
C36 C 0.0791(2) 1.14074(18) -0.11296(12) 0.0246(6) Uani 1 1 d . . .
H36A H 0.1544 1.1073 -0.1050 0.029 Uiso 1 1 calc R . .
H36B H 0.0928 1.2044 -0.1006 0.029 Uiso 1 1 calc R . .
C37 C 0.0494(3) 1.1363(2) -0.18429(12) 0.0387(7) Uani 1 1 d . . .
H37A H 0.0354 1.0734 -0.1968 0.058 Uiso 1 1 calc R . .
H37B H 0.1163 1.1607 -0.2095 0.058 Uiso 1 1 calc R . .
H37C H -0.0230 1.1718 -0.1929 0.058 Uiso 1 1 calc R . .
N1 N 0.15588(16) 1.01291(13) 0.07549(8) 0.0172(4) Uani 1 1 d . . .
N2 N 0.01904(16) 0.92298(13) 0.11244(8) 0.0155(4) Uani 1 1 d . . .
N3 N -0.01628(17) 1.10287(13) -0.07146(9) 0.0197(4) Uani 1 1 d . . .
O1 O 0.13541(13) 0.94859(10) -0.07376(7) 0.0176(4) Uani 1 1 d . . .
O2 O -0.17780(13) 0.98895(11) 0.01094(7) 0.0175(3) Uani 1 1 d . . .
O3 O -0.02756(14) 0.81097(10) -0.02424(7) 0.0203(3) Uani 1 1 d . . .
Zr1 Zr -0.034364(18) 0.970104(15) -0.046475(10) 0.01488(5) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 Zr1 2.4976(6) . ?
C1 O1 1.348(3) . ?
C1 C2 1.390(3) . ?
C1 C6 1.407(3) . ?
C2 C3 1.397(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.397(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.515(3) . ?
C7 N1 1.471(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 N1 1.487(3) . ?
C8 C9 1.500(3) . ?
C8 C15 1.544(3) . ?
C8 H8 1.0000 . ?
C9 C10 1.392(3) . ?
C9 C14 1.394(3) . ?
C10 C11 1.391(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.379(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.385(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 N2 1.484(3) . ?
C15 C16 1.502(3) . ?
C15 H15 1.0000 . ?
C16 C17 1.386(3) . ?
C16 C21 1.394(3) . ?
C17 C18 1.383(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.383(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.388(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.385(3) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 N2 1.469(3) . ?
C22 C23 1.505(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.393(3) . ?
C23 C28 1.408(3) . ?
C24 C25 1.382(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.384(3) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.389(3) . ?
C27 H27 0.9500 . ?
C28 O2 1.350(3) . ?
C29 N1 1.324(3) . ?
C29 N2 1.343(3) . ?
C29 Zr1 2.419(2) . ?
C30 O3 1.451(3) . ?
C30 C31 1.525(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 C32 1.542(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.515(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 O3 1.449(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 N3 1.476(3) . ?
C34 C35 1.520(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 N3 1.476(3) . ?
C36 C37 1.508(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
N3 Zr1 2.046(2) . ?
O1 Zr1 2.0020(15) . ?
O2 Zr1 2.0101(14) . ?
O3 Zr1 2.4058(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 119.7(2) . . ?
O1 C1 C6 121.1(2) . . ?
C2 C1 C6 119.3(2) . . ?
C1 C2 C3 120.9(2) . . ?
C1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C4 C3 C2 120.4(2) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 118.8(2) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
C4 C5 C6 121.9(2) . . ?
C4 C5 H5 119.1 . . ?
C6 C5 H5 119.1 . . ?
C5 C6 C1 118.8(2) . . ?
C5 C6 C7 119.5(2) . . ?
C1 C6 C7 121.5(2) . . ?
N1 C7 C6 115.72(19) . . ?
N1 C7 H7A 108.4 . . ?
C6 C7 H7A 108.4 . . ?
N1 C7 H7B 108.3 . . ?
C6 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
N1 C8 C9 114.53(18) . . ?
N1 C8 C15 100.43(16) . . ?
C9 C8 C15 113.27(18) . . ?
N1 C8 H8 109.4 . . ?
C9 C8 H8 109.4 . . ?
C15 C8 H8 109.4 . . ?
C10 C9 C14 118.5(2) . . ?
C10 C9 C8 121.0(2) . . ?
C14 C9 C8 120.4(2) . . ?
C11 C10 C9 120.8(2) . . ?
C11 C10 H10 119.6 . . ?
C9 C10 H10 119.6 . . ?
C12 C11 C10 119.8(2) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C13 120.1(2) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 120.1(2) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C9 120.7(2) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?
N2 C15 C16 113.88(18) . . ?
N2 C15 C8 101.39(16) . . ?
C16 C15 C8 115.66(18) . . ?
N2 C15 H15 108.5 . . ?
C16 C15 H15 108.5 . . ?
C8 C15 H15 108.5 . . ?
C17 C16 C21 118.4(2) . . ?
C17 C16 C15 119.9(2) . . ?
C21 C16 C15 121.7(2) . . ?
C18 C17 C16 120.9(2) . . ?
C18 C17 H17 119.5 . . ?
C16 C17 H17 119.5 . . ?
C19 C18 C17 120.0(2) . . ?
C19 C18 H18 120.0 . . ?
C17 C18 H18 120.0 . . ?
C18 C19 C20 120.1(2) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C21 C20 C19 119.4(2) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C20 C21 C16 121.2(2) . . ?
C20 C21 H21 119.4 . . ?
C16 C21 H21 119.4 . . ?
N2 C22 C23 112.38(19) . . ?
N2 C22 H22A 109.1 . . ?
C23 C22 H22A 109.1 . . ?
N2 C22 H22B 109.1 . . ?
C23 C22 H22B 109.1 . . ?
H22A C22 H22B 107.9 . . ?
C24 C23 C28 118.6(2) . . ?
C24 C23 C22 122.4(2) . . ?
C28 C23 C22 118.9(2) . . ?
C25 C24 C23 121.5(2) . . ?
C25 C24 H24 119.2 . . ?
C23 C24 H24 119.2 . . ?
C24 C25 C26 119.4(2) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C25 C26 C27 120.3(2) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C26 C27 C28 120.5(2) . . ?
C26 C27 H27 119.7 . . ?
C28 C27 H27 119.7 . . ?
O2 C28 C27 120.2(2) . . ?
O2 C28 C23 120.2(2) . . ?
C27 C28 C23 119.6(2) . . ?
N1 C29 N2 108.57(17) . . ?
N1 C29 Zr1 124.41(15) . . ?
N2 C29 Zr1 127.00(14) . . ?
O3 C30 C31 103.40(19) . . ?
O3 C30 H30A 111.1 . . ?
C31 C30 H30A 111.1 . . ?
O3 C30 H30B 111.1 . . ?
C31 C30 H30B 111.1 . . ?
H30A C30 H30B 109.0 . . ?
C30 C31 C32 104.0(2) . . ?
C30 C31 H31A 111.0 . . ?
C32 C31 H31A 111.0 . . ?
C30 C31 H31B 111.0 . . ?
C32 C31 H31B 111.0 . . ?
H31A C31 H31B 109.0 . . ?
C33 C32 C31 104.2(2) . . ?
C33 C32 H32A 110.9 . . ?
C31 C32 H32A 110.9 . . ?
C33 C32 H32B 110.9 . . ?
C31 C32 H32B 110.9 . . ?
H32A C32 H32B 108.9 . . ?
O3 C33 C32 104.7(2) . . ?
O3 C33 H33A 110.8 . . ?
C32 C33 H33A 110.8 . . ?
O3 C33 H33B 110.8 . . ?
C32 C33 H33B 110.8 . . ?
H33A C33 H33B 108.9 . . ?
N3 C34 C35 112.1(2) . . ?
N3 C34 H34A 109.2 . . ?
C35 C34 H34A 109.2 . . ?
N3 C34 H34B 109.2 . . ?
C35 C34 H34B 109.2 . . ?
H34A C34 H34B 107.9 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N3 C36 C37 112.9(2) . . ?
N3 C36 H36A 109.0 . . ?
C37 C36 H36A 109.0 . . ?
N3 C36 H36B 109.0 . . ?
C37 C36 H36B 109.0 . . ?
H36A C36 H36B 107.8 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C29 N1 C7 123.93(18) . . ?
C29 N1 C8 113.27(18) . . ?
C7 N1 C8 121.99(17) . . ?
C29 N2 C22 123.38(17) . . ?
C29 N2 C15 111.57(17) . . ?
C22 N2 C15 118.62(17) . . ?
C36 N3 C34 110.97(19) . . ?
C36 N3 Zr1 125.68(16) . . ?
C34 N3 Zr1 122.83(15) . . ?
C1 O1 Zr1 153.92(14) . . ?
C28 O2 Zr1 152.12(13) . . ?
C33 O3 C30 103.87(17) . . ?
C33 O3 Zr1 120.46(13) . . ?
C30 O3 Zr1 129.89(14) . . ?
O1 Zr1 O2 160.25(6) . . ?
O1 Zr1 N3 89.39(7) . . ?
O2 Zr1 N3 95.33(7) . . ?
O1 Zr1 O3 82.37(6) . . ?
O2 Zr1 O3 92.84(6) . . ?
N3 Zr1 O3 171.68(7) . . ?
O1 Zr1 C29 81.27(6) . . ?
O2 Zr1 C29 78.99(6) . . ?
N3 Zr1 C29 101.62(8) . . ?
O3 Zr1 C29 78.36(7) . . ?
O1 Zr1 Cl1 104.35(5) . . ?
O2 Zr1 Cl1 93.86(5) . . ?
N3 Zr1 Cl1 99.03(6) . . ?
O3 Zr1 Cl1 81.99(4) . . ?
C29 Zr1 Cl1 158.67(6) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.055
_database_code_depnum_ccdc_archive 'CCDC 975123'
#######################################################################
#
#                 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_compound16

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C43 H54 Cl N3 O3 Zr'
_chemical_formula_sum            'C43 H54 Cl N3 O3 Zr'
_chemical_formula_weight         787.56
_chemical_absolute_configuration rmad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   C222(1)

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

_cell_length_a                   18.0484(6)
_cell_length_b                   24.5701(9)
_cell_length_c                   46.1636(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     20471.3(13)
_cell_formula_units_Z            16
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    9868
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      26.23

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6624
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9370
_exptl_absorpt_correction_T_max  0.9678
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18556
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0560
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         25.25
_reflns_number_total             18556
_reflns_number_gt                15790
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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)+(0.0638P)²+21.1376P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_number_reflns         18556
_refine_ls_number_parameters     962
_refine_ls_number_restraints     624
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0513
_refine_ls_wR_factor_ref         0.1249
_refine_ls_wR_factor_gt          0.1207
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.107 0.803 0.000 682 160 ' '
2 -0.025 0.618 0.250 1725 330 ' '
3 0.107 0.774 0.500 681 165 ' '
4 0.003 0.385 0.750 1726 331 ' '
5 0.393 -0.002 0.000 681 160 ' '
6 0.607 0.219 0.500 681 165 ' '
_platon_squeeze_details          
;
;


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 0.5861(2) 0.69969(16) 0.85630(8) 0.0272(9) Uani 1 1 d U . .
C2 C 0.5673(2) 0.75526(16) 0.85890(9) 0.0292(9) Uani 1 1 d U . .
C3 C 0.4915(2) 0.76751(17) 0.85726(9) 0.0348(10) Uani 1 1 d U . .
H3 H 0.4769 0.8046 0.8585 0.042 Uiso 1 1 calc R . .
C4 C 0.4371(2) 0.72854(19) 0.85395(10) 0.0417(11) Uani 1 1 d U . .
H4 H 0.3866 0.7389 0.8521 0.050 Uiso 1 1 calc R . .
C5 C 0.4571(2) 0.67456(17) 0.85329(9) 0.0339(10) Uani 1 1 d U . .
H5 H 0.4197 0.6474 0.8523 0.041 Uiso 1 1 calc R . .
C6 C 0.5312(2) 0.65914(15) 0.85410(8) 0.0262(8) Uani 1 1 d U . .
C7 C 0.6251(2) 0.79914(15) 0.86335(9) 0.0291(9) Uani 1 1 d U . .
C8 C 0.6710(2) 0.78840(17) 0.89072(10) 0.0406(11) Uani 1 1 d U . .
H8A H 0.6939 0.7523 0.8894 0.061 Uiso 1 1 calc R . .
H8B H 0.6387 0.7898 0.9078 0.061 Uiso 1 1 calc R . .
H8C H 0.7097 0.8162 0.8925 0.061 Uiso 1 1 calc R . .
C9 C 0.6751(2) 0.80343(17) 0.83753(10) 0.0408(11) Uani 1 1 d U . .
H9A H 0.7033 0.7696 0.8354 0.061 Uiso 1 1 calc R . .
H9B H 0.7094 0.8339 0.8402 0.061 Uiso 1 1 calc R . .
H9C H 0.6453 0.8096 0.8201 0.061 Uiso 1 1 calc R . .
C10 C 0.5890(2) 0.85549(18) 0.86737(11) 0.0442(11) Uani 1 1 d U . .
H10A H 0.6273 0.8823 0.8722 0.066 Uiso 1 1 calc R . .
H10B H 0.5526 0.8538 0.8831 0.066 Uiso 1 1 calc R . .
H10C H 0.5642 0.8662 0.8494 0.066 Uiso 1 1 calc R . .
C11 C 0.5523(2) 0.59987(16) 0.85584(8) 0.0284(9) Uani 1 1 d U . .
H11A H 0.5866 0.5950 0.8724 0.034 Uiso 1 1 calc R . .
H11B H 0.5071 0.5785 0.8601 0.034 Uiso 1 1 calc R . .
C12 C 0.5473(2) 0.53737(17) 0.81164(9) 0.0292(9) Uani 1 1 d U . .
H12 H 0.5366 0.5038 0.8232 0.035 Uiso 1 1 calc R . .
C13 C 0.6049(2) 0.52455(17) 0.78847(9) 0.0330(9) Uani 1 1 d U . .
H13 H 0.5943 0.5460 0.7705 0.040 Uiso 1 1 calc R . .
C14 C 0.6598(2) 0.57786(16) 0.82421(9) 0.0302(9) Uani 1 1 d U . .
C15 C 0.47540(19) 0.56098(18) 0.80025(8) 0.0310(9) Uani 1 1 d U . .
C16 C 0.4730(2) 0.6101(2) 0.78534(9) 0.0399(11) Uani 1 1 d U . .
H16 H 0.5179 0.6288 0.7813 0.048 Uiso 1 1 calc R . .
C17 C 0.4061(3) 0.6322(2) 0.77626(9) 0.0468(12) Uani 1 1 d U . .
H17 H 0.4057 0.6653 0.7657 0.056 Uiso 1 1 calc R . .
C18 C 0.3401(3) 0.6064(3) 0.78248(11) 0.0637(16) Uani 1 1 d U . .
H18 H 0.2944 0.6216 0.7763 0.076 Uiso 1 1 calc R . .
C19 C 0.3413(3) 0.5591(3) 0.79759(15) 0.082(2) Uani 1 1 d U . .
H19 H 0.2959 0.5417 0.8023 0.098 Uiso 1 1 calc R . .
C20 C 0.4080(3) 0.5353(3) 0.80647(13) 0.0634(16) Uani 1 1 d U . .
H20 H 0.4075 0.5018 0.8167 0.076 Uiso 1 1 calc R . .
C21 C 0.6106(2) 0.46362(18) 0.78112(9) 0.0395(11) Uani 1 1 d U . .
C22 C 0.6301(2) 0.42405(19) 0.80019(9) 0.0393(10) Uani 1 1 d U B .
H22 H 0.6411 0.4345 0.8195 0.047 Uiso 1 1 calc R . .
C23 C 0.6350(2) 0.36964(18) 0.79318(10) 0.0416(11) Uani 1 1 d U . .
H23 H 0.6339 0.3427 0.8079 0.050 Uiso 1 1 calc R A 1
C24A C 0.6418(6) 0.3546(5) 0.7636(3) 0.060(3) Uani 0.50 1 d PU B 1
H24A H 0.6488 0.3176 0.7583 0.072 Uiso 0.50 1 calc PR B 1
C25A C 0.6380(7) 0.3940(5) 0.7432(3) 0.069(3) Uani 0.50 1 d PU B 1
H25A H 0.6454 0.3851 0.7234 0.083 Uiso 0.50 1 calc PR B 1
C26A C 0.6231(6) 0.4486(4) 0.7514(2) 0.048(2) Uani 0.50 1 d PU B 1
H26A H 0.6213 0.4759 0.7369 0.058 Uiso 0.50 1 calc PR B 1
C24B C 0.5951(7) 0.3536(5) 0.7676(2) 0.054(2) Uani 0.50 1 d PU B 2
H24B H 0.5908 0.3163 0.7625 0.065 Uiso 0.50 1 calc PR B 2
C25B C 0.5644(7) 0.3920(5) 0.7514(3) 0.075(3) Uani 0.50 1 d PU B 2
H25B H 0.5388 0.3810 0.7344 0.091 Uiso 0.50 1 calc PR B 2
C26B C 0.5673(7) 0.4466(5) 0.7577(2) 0.063(3) Uani 0.50 1 d PU B 2
H26B H 0.5404 0.4722 0.7464 0.075 Uiso 0.50 1 calc PR B 2
C27 C 0.7461(2) 0.54033(17) 0.78791(9) 0.0361(9) Uani 1 1 d U B .
H27A H 0.7665 0.5774 0.7854 0.043 Uiso 1 1 calc R . .
H27B H 0.7388 0.5246 0.7684 0.043 Uiso 1 1 calc R . .
C28 C 0.8026(2) 0.50584(19) 0.80419(10) 0.0375(10) Uani 1 1 d U . .
C29 C 0.8209(2) 0.45448(19) 0.79493(11) 0.0471(12) Uani 1 1 d U . .
H29 H 0.7958 0.4396 0.7787 0.056 Uiso 1 1 calc R . .
C30 C 0.8738(3) 0.4242(2) 0.80822(12) 0.0568(14) Uani 1 1 d U . .
H30 H 0.8844 0.3882 0.8020 0.068 Uiso 1 1 calc R . .
C31 C 0.9120(2) 0.4480(2) 0.83135(12) 0.0508(13) Uani 1 1 d U . .
H31 H 0.9494 0.4268 0.8405 0.061 Uiso 1 1 calc R . .
C32 C 0.8997(2) 0.49948(18) 0.84196(11) 0.0420(11) Uani 1 1 d U . .
C33 C 0.8391(2) 0.52839(16) 0.82828(10) 0.0368(10) Uani 1 1 d U . .
C34 C 0.9463(2) 0.5254(2) 0.86513(12) 0.0482(12) Uani 1 1 d U . .
C35 C 1.0082(3) 0.4862(2) 0.87551(14) 0.0744(17) Uani 1 1 d U . .
H35A H 0.9858 0.4544 0.8849 0.112 Uiso 1 1 calc R . .
H35B H 1.0403 0.5051 0.8894 0.112 Uiso 1 1 calc R . .
H35C H 1.0377 0.4743 0.8588 0.112 Uiso 1 1 calc R . .
C36 C 0.9811(2) 0.5780(2) 0.85465(13) 0.0593(15) Uani 1 1 d U . .
H36A H 1.0135 0.5705 0.8381 0.089 Uiso 1 1 calc R . .
H36B H 1.0102 0.5943 0.8703 0.089 Uiso 1 1 calc R . .
H36C H 0.9420 0.6034 0.8487 0.089 Uiso 1 1 calc R . .
C37 C 0.8996(3) 0.5361(2) 0.89318(11) 0.0561(14) Uani 1 1 d U . .
H37A H 0.8603 0.5624 0.8889 0.084 Uiso 1 1 calc R . .
H37B H 0.9319 0.5507 0.9084 0.084 Uiso 1 1 calc R . .
H37C H 0.8775 0.5019 0.8998 0.084 Uiso 1 1 calc R . .
C38 C 0.7086(3) 0.7011(2) 0.78802(11) 0.0533(13) Uani 1 1 d U . .
H38A H 0.7233 0.7386 0.7836 0.080 Uiso 1 1 calc R . .
H38B H 0.6606 0.7013 0.7979 0.080 Uiso 1 1 calc R . .
H38C H 0.7046 0.6803 0.7700 0.080 Uiso 1 1 calc R . .
C39 C 0.8351(3) 0.6760(2) 0.79219(11) 0.0519(13) Uani 1 1 d U . .
H39A H 0.8303 0.6577 0.7734 0.078 Uiso 1 1 calc R . .
H39B H 0.8716 0.6567 0.8041 0.078 Uiso 1 1 calc R . .
H39C H 0.8516 0.7136 0.7892 0.078 Uiso 1 1 calc R . .
C40 C 0.7004(3) 0.61757(19) 0.91486(10) 0.0454(11) Uani 1 1 d U . .
H40A H 0.6715 0.6512 0.9114 0.055 Uiso 1 1 calc R . .
H40B H 0.7464 0.6272 0.9253 0.055 Uiso 1 1 calc R . .
C41 C 0.6561(3) 0.5776(2) 0.93164(12) 0.0542(13) Uani 1 1 d U . .
H41A H 0.6032 0.5789 0.9261 0.065 Uiso 1 1 calc R . .
H41B H 0.6605 0.5842 0.9527 0.065 Uiso 1 1 calc R . .
C42 C 0.6904(3) 0.5239(2) 0.92333(12) 0.0596(15) Uani 1 1 d U . .
H42A H 0.6556 0.4934 0.9266 0.072 Uiso 1 1 calc R . .
H42B H 0.7366 0.5171 0.9343 0.072 Uiso 1 1 calc R . .
C43 C 0.7060(2) 0.53163(17) 0.89130(11) 0.0411(11) Uani 1 1 d U . .
H43A H 0.7509 0.5112 0.8854 0.049 Uiso 1 1 calc R . .
H43B H 0.6636 0.5190 0.8795 0.049 Uiso 1 1 calc R . .
C44 C 0.8310(2) 0.91574(17) 0.92718(10) 0.0364(10) Uani 1 1 d U . .
C45 C 0.7739(2) 0.94711(18) 0.91424(11) 0.0421(11) Uani 1 1 d U . .
C46 C 0.7024(3) 0.9413(2) 0.92597(12) 0.0518(13) Uani 1 1 d U . .
H46 H 0.6629 0.9616 0.9178 0.062 Uiso 1 1 calc R . .
C47 C 0.6877(3) 0.9072(2) 0.94890(13) 0.0614(15) Uani 1 1 d U . .
H47 H 0.6383 0.9034 0.9557 0.074 Uiso 1 1 calc R . .
C48 C 0.7425(3) 0.8791(2) 0.96173(11) 0.0544(13) Uani 1 1 d U . .
H48 H 0.7317 0.8567 0.9779 0.065 Uiso 1 1 calc R . .
C49 C 0.8162(2) 0.88267(19) 0.95138(10) 0.0400(10) Uani 1 1 d U . .
C50 C 0.7882(2) 0.98740(19) 0.88950(13) 0.0521(14) Uani 1 1 d U . .
C51 C 0.8491(3) 1.0280(2) 0.89804(17) 0.0745(19) Uani 1 1 d U . .
H51A H 0.8378 1.0638 0.8898 0.112 Uiso 1 1 calc R . .
H51B H 0.8970 1.0153 0.8906 0.112 Uiso 1 1 calc R . .
H51C H 0.8515 1.0309 0.9192 0.112 Uiso 1 1 calc R . .
C52 C 0.8125(3) 0.9552(3) 0.86179(13) 0.0671(17) Uani 1 1 d U . .
H52A H 0.8635 0.9422 0.8642 0.101 Uiso 1 1 calc R . .
H52B H 0.8099 0.9792 0.8449 0.101 Uiso 1 1 calc R . .
H52C H 0.7794 0.9241 0.8589 0.101 Uiso 1 1 calc R . .
C53 C 0.7186(3) 1.0205(3) 0.88121(16) 0.0768(19) Uani 1 1 d U . .
H53A H 0.6787 0.9956 0.8756 0.115 Uiso 1 1 calc R . .
H53B H 0.7303 1.0446 0.8649 0.115 Uiso 1 1 calc R . .
H53C H 0.7027 1.0424 0.8978 0.115 Uiso 1 1 calc R . .
C54 C 0.8787(2) 0.85577(17) 0.96798(9) 0.0365(10) Uani 1 1 d U . .
H54A H 0.9201 0.8820 0.9698 0.044 Uiso 1 1 calc R . .
H54B H 0.8611 0.8472 0.9878 0.044 Uiso 1 1 calc R . .
C55 C 0.8983(2) 0.75263(17) 0.96909(9) 0.0339(10) Uani 1 1 d U . .
H55 H 0.9292 0.7522 0.9871 0.041 Uiso 1 1 calc R . .
C56 C 0.9337(2) 0.71414(16) 0.94630(9) 0.0313(9) Uani 1 1 d U . .
H56 H 0.8933 0.6976 0.9344 0.038 Uiso 1 1 calc R . .
C57 C 0.9539(2) 0.80524(16) 0.93278(9) 0.0327(9) Uani 1 1 d U . .
C58 C 0.8196(2) 0.74019(17) 0.97686(9) 0.0348(10) Uani 1 1 d U . .
C59 C 0.7647(2) 0.73373(18) 0.95586(9) 0.0373(10) Uani 1 1 d U . .
H59 H 0.7779 0.7355 0.9360 0.045 Uiso 1 1 calc R . .
C60 C 0.6918(2) 0.72483(18) 0.96329(10) 0.0384(10) Uani 1 1 d U . .
H60 H 0.6558 0.7199 0.9485 0.046 Uiso 1 1 calc R . .
C61 C 0.6706(3) 0.72304(19) 0.99189(10) 0.0430(11) Uani 1 1 d U . .
H61 H 0.6201 0.7171 0.9968 0.052 Uiso 1 1 calc R . .
C62 C 0.7232(3) 0.7299(2) 1.01352(10) 0.0518(13) Uani 1 1 d U . .
H62 H 0.7090 0.7286 1.0333 0.062 Uiso 1 1 calc R . .
C63 C 0.7961(2) 0.73872(19) 1.00597(10) 0.0404(11) Uani 1 1 d U . .
H63 H 0.8316 0.7440 1.0209 0.048 Uiso 1 1 calc R . .
C64 C 0.9801(3) 0.67032(19) 0.95819(9) 0.0404(11) Uani 1 1 d U . .
C65 C 0.9575(4) 0.6161(2) 0.95726(13) 0.0757(18) Uani 1 1 d U . .
H65 H 0.9106 0.6078 0.9491 0.091 Uiso 1 1 calc R . .
C66 C 1.0012(5) 0.5736(3) 0.96786(16) 0.104(2) Uani 1 1 d U . .
H66 H 0.9836 0.5372 0.9672 0.125 Uiso 1 1 calc R . .
C67 C 1.0669(5) 0.5845(4) 0.97877(16) 0.108(3) Uani 1 1 d U . .
H67 H 1.0964 0.5557 0.9862 0.129 Uiso 1 1 calc R . .
C68 C 1.0940(4) 0.6373(4) 0.97968(15) 0.099(2) Uani 1 1 d U . .
H68 H 1.1423 0.6445 0.9869 0.119 Uiso 1 1 calc R . .
C69 C 1.0498(3) 0.6792(3) 0.96988(13) 0.0709(17) Uani 1 1 d U . .
H69 H 1.0678 0.7155 0.9712 0.085 Uiso 1 1 calc R . .
C70 C 1.0161(2) 0.73458(16) 0.90264(9) 0.0299(9) Uani 1 1 d U . .
H70A H 0.9987 0.7555 0.8856 0.036 Uiso 1 1 calc R . .
H70B H 1.0038 0.6958 0.8992 0.036 Uiso 1 1 calc R . .
C71 C 1.0984(2) 0.73988(15) 0.90452(9) 0.0330(9) Uani 1 1 d U . .
C72 C 1.1427(2) 0.69330(17) 0.90651(11) 0.0472(12) Uani 1 1 d U . .
H72 H 1.1202 0.6585 0.9081 0.057 Uiso 1 1 calc R . .
C73 C 1.2189(3) 0.69776(19) 0.90618(13) 0.0538(13) Uani 1 1 d U . .
H73 H 1.2490 0.6664 0.9086 0.065 Uiso 1 1 calc R . .
C74 C 1.2509(3) 0.74848(17) 0.90233(10) 0.0449(11) Uani 1 1 d U . .
H74 H 1.3034 0.7504 0.9013 0.054 Uiso 1 1 calc R . .
C75 C 1.2113(2) 0.79673(17) 0.89992(9) 0.0340(10) Uani 1 1 d U . .
C76 C 1.1335(2) 0.79181(15) 0.90239(8) 0.0279(9) Uani 1 1 d U . .
C77 C 1.2492(2) 0.85148(16) 0.89490(9) 0.0340(9) Uani 1 1 d U . .
C78 C 1.3342(2) 0.84444(19) 0.89121(11) 0.0437(11) Uani 1 1 d U . .
H78A H 1.3542 0.8245 0.9078 0.066 Uiso 1 1 calc R . .
H78B H 1.3577 0.8803 0.8901 0.066 Uiso 1 1 calc R . .
H78C H 1.3443 0.8241 0.8734 0.066 Uiso 1 1 calc R . .
C79 C 1.2203(2) 0.87866(19) 0.86710(9) 0.0398(10) Uani 1 1 d U . .
H79A H 1.2295 0.8547 0.8505 0.060 Uiso 1 1 calc R . .
H79B H 1.2461 0.9133 0.8641 0.060 Uiso 1 1 calc R . .
H79C H 1.1670 0.8853 0.8689 0.060 Uiso 1 1 calc R . .
C80 C 1.2380(2) 0.88786(17) 0.92107(10) 0.0375(10) Uani 1 1 d U . .
H80A H 1.1860 0.8992 0.9221 0.056 Uiso 1 1 calc R . .
H80B H 1.2697 0.9200 0.9194 0.056 Uiso 1 1 calc R . .
H80C H 1.2510 0.8678 0.9387 0.056 Uiso 1 1 calc R . .
C81 C 1.0890(3) 0.8824(2) 0.96906(11) 0.0555(13) Uani 1 1 d U . .
H81A H 1.1312 0.9050 0.9749 0.083 Uiso 1 1 calc R . .
H81B H 1.1071 0.8491 0.9598 0.083 Uiso 1 1 calc R . .
H81C H 1.0597 0.8729 0.9862 0.083 Uiso 1 1 calc R . .
C82 C 1.0189(3) 0.96367(19) 0.96141(11) 0.0471(12) Uani 1 1 d U . .
H82A H 0.9946 0.9565 0.9800 0.071 Uiso 1 1 calc R . .
H82B H 0.9839 0.9819 0.9484 0.071 Uiso 1 1 calc R . .
H82C H 1.0621 0.9871 0.9645 0.071 Uiso 1 1 calc R . .
C83 C 0.9923(2) 0.84153(19) 0.84180(10) 0.0429(11) Uani 1 1 d U . .
H83A H 1.0436 0.8293 0.8457 0.052 Uiso 1 1 calc R . .
H83B H 0.9943 0.8765 0.8312 0.052 Uiso 1 1 calc R . .
C84 C 0.9512(3) 0.7993(2) 0.82429(11) 0.0514(13) Uani 1 1 d U . .
H84A H 0.9668 0.7619 0.8295 0.062 Uiso 1 1 calc R . .
H84B H 0.9580 0.8050 0.8032 0.062 Uiso 1 1 calc R . .
C85 C 0.8714(2) 0.8105(2) 0.83362(10) 0.0446(11) Uani 1 1 d U . .
H85A H 0.8504 0.8419 0.8229 0.053 Uiso 1 1 calc R . .
H85B H 0.8395 0.7783 0.8304 0.053 Uiso 1 1 calc R . .
C86 C 0.8787(2) 0.82297(17) 0.86521(9) 0.0358(10) Uani 1 1 d U . .
H86A H 0.8394 0.8484 0.8715 0.043 Uiso 1 1 calc R . .
H86B H 0.8751 0.7892 0.8769 0.043 Uiso 1 1 calc R . .
Cl1 Cl 0.83670(5) 0.68673(4) 0.87849(2) 0.0317(2) Uani 1 1 d . B .
Cl2 Cl 1.03838(5) 0.96133(4) 0.87697(2) 0.0355(2) Uani 1 1 d . . .
N1 N 0.58716(16) 0.57715(13) 0.82990(7) 0.0260(7) Uani 1 1 d . . .
N2 N 0.67349(17) 0.54457(14) 0.80223(8) 0.0356(9) Uani 1 1 d . . .
N3 N 0.76438(17) 0.67608(13) 0.80676(8) 0.0341(8) Uani 1 1 d . B .
N4 N 0.90636(18) 0.80605(13) 0.95463(7) 0.0305(8) Uani 1 1 d . . .
N5 N 0.97531(18) 0.75325(13) 0.92816(7) 0.0297(8) Uani 1 1 d . . .
N6 N 1.04251(17) 0.91270(14) 0.94862(8) 0.0349(8) Uani 1 1 d . . .
O1 O 0.65789(12) 0.68267(10) 0.85562(6) 0.0262(6) Uani 1 1 d . B .
O2 O 0.81934(13) 0.57781(11) 0.83774(6) 0.0317(7) Uani 1 1 d . B .
O3 O 0.71736(14) 0.59053(11) 0.88772(6) 0.0326(7) Uani 1 1 d . B .
O4 O 0.89984(13) 0.91564(11) 0.91700(6) 0.0309(6) Uani 1 1 d . . .
O5 O 1.08898(14) 0.83618(10) 0.90187(6) 0.0275(6) Uani 1 1 d . . .
O6 O 0.95193(13) 0.84784(11) 0.86848(6) 0.0304(6) Uani 1 1 d . . .
Zr1 Zr 0.74775(2) 0.638670(14) 0.845827(9) 0.02969(9) Uani 1 1 d . . .
Zr2 Zr 1.00292(2) 0.885464(15) 0.910039(9) 0.03012(9) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.361(4) . ?
C1 C6 1.409(5) . ?
C1 C2 1.412(5) . ?
C2 C3 1.402(5) . ?
C2 C7 1.514(6) . ?
C3 C4 1.381(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(5) . ?
C5 H5 0.9500 . ?
C6 C11 1.507(5) . ?
C7 C9 1.499(6) . ?
C7 C8 1.534(6) . ?
C7 C10 1.541(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 N1 1.463(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N1 1.477(5) . ?
C12 C15 1.516(5) . ?
C12 C13 1.524(6) . ?
C12 H12 1.0000 . ?
C13 N2 1.475(5) . ?
C13 C21 1.539(6) . ?
C13 H13 1.0000 . ?
C14 N2 1.327(5) . ?
C14 N1 1.337(5) . ?
C14 Zr1 2.397(4) . ?
C15 C16 1.390(6) . ?
C15 C20 1.400(6) . ?
C16 C17 1.390(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.379(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.356(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.399(8) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.358(6) . ?
C21 C26B 1.397(11) . ?
C21 C26A 1.439(11) . ?
C22 C23 1.378(6) . ?
C22 H22 0.9500 . ?
C23 C24A 1.418(12) . ?
C23 C24B 1.437(11) . ?
C23 H23 0.9500 . ?
C24A C25A 1.352(16) . ?
C24A H24A 0.9500 . ?
C25A C26A 1.420(14) . ?
C25A H25A 0.9500 . ?
C26A H26A 0.9500 . ?
C24B C25B 1.324(16) . ?
C24B H24B 0.9500 . ?
C25B C26B 1.375(15) . ?
C25B H25B 0.9500 . ?
C26B H26B 0.9500 . ?
C27 N2 1.471(5) . ?
C27 C28 1.525(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.373(6) . ?
C28 C33 1.407(6) . ?
C29 C30 1.355(7) . ?
C29 H29 0.9500 . ?
C30 C31 1.398(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.375(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.449(6) . ?
C32 C34 1.503(7) . ?
C33 O2 1.339(5) . ?
C34 C36 1.518(7) . ?
C34 C35 1.551(6) . ?
C34 C37 1.567(7) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 N3 1.463(6) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 N3 1.443(6) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 O3 1.451(5) . ?
C40 C41 1.485(7) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.506(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.517(7) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 O3 1.471(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 O4 1.328(5) . ?
C44 C49 1.407(6) . ?
C44 C45 1.419(6) . ?
C45 C46 1.406(6) . ?
C45 C50 1.533(7) . ?
C46 C47 1.376(7) . ?
C46 H46 0.9500 . ?
C47 C48 1.342(7) . ?
C47 H47 0.9500 . ?
C48 C49 1.416(6) . ?
C48 H48 0.9500 . ?
C49 C54 1.515(6) . ?
C50 C51 1.536(7) . ?
C50 C53 1.545(6) . ?
C50 C52 1.567(8) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 N4 1.456(5) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 N4 1.480(5) . ?
C55 C58 1.497(6) . ?
C55 C56 1.552(6) . ?
C55 H55 1.0000 . ?
C56 C64 1.471(6) . ?
C56 N5 1.480(5) . ?
C56 H56 1.0000 . ?
C57 N4 1.325(5) . ?
C57 N5 1.351(5) . ?
C57 Zr2 2.402(4) . ?
C58 C59 1.396(6) . ?
C58 C63 1.410(6) . ?
C59 C60 1.377(6) . ?
C59 H59 0.9500 . ?
C60 C61 1.376(6) . ?
C60 H60 0.9500 . ?
C61 C62 1.388(7) . ?
C61 H61 0.9500 . ?
C62 C63 1.378(6) . ?
C62 H62 0.9500 . ?
C63 H63 0.9500 . ?
C64 C69 1.386(7) . ?
C64 C65 1.393(7) . ?
C65 C66 1.397(9) . ?
C65 H65 0.9500 . ?
C66 C67 1.317(11) . ?
C66 H66 0.9500 . ?
C67 C68 1.387(11) . ?
C67 H67 0.9500 . ?
C68 C69 1.378(9) . ?
C68 H68 0.9500 . ?
C69 H69 0.9500 . ?
C70 N5 1.463(5) . ?
C70 C71 1.494(5) . ?
C70 H70A 0.9900 . ?
C70 H70B 0.9900 . ?
C71 C72 1.399(5) . ?
C71 C76 1.428(5) . ?
C72 C73 1.379(6) . ?
C72 H72 0.9500 . ?
C73 C74 1.386(6) . ?
C73 H73 0.9500 . ?
C74 C75 1.389(6) . ?
C74 H74 0.9500 . ?
C75 C76 1.413(5) . ?
C75 C77 1.527(6) . ?
C76 O5 1.355(4) . ?
C77 C80 1.516(6) . ?
C77 C79 1.538(6) . ?
C77 C78 1.554(6) . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 N6 1.465(6) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 N6 1.449(6) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 O6 1.440(5) . ?
C83 C84 1.510(6) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C84 C85 1.529(6) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C85 C86 1.496(6) . ?
C85 H85A 0.9900 . ?
C85 H85B 0.9900 . ?
C86 O6 1.464(5) . ?
C86 H86A 0.9900 . ?
C86 H86B 0.9900 . ?
Cl1 Zr1 2.4991(10) . ?
Cl2 Zr2 2.4929(11) . ?
N3 Zr1 2.046(4) . ?
N6 Zr2 2.032(4) . ?
O1 Zr1 2.001(2) . ?
O2 Zr1 2.011(2) . ?
O3 Zr1 2.332(3) . ?
O4 Zr2 2.028(2) . ?
O5 Zr2 2.005(2) . ?
O6 Zr2 2.320(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 116.8(3) . . ?
O1 C1 C2 121.9(3) . . ?
C6 C1 C2 121.4(3) . . ?
C3 C2 C1 115.9(4) . . ?
C3 C2 C7 121.7(3) . . ?
C1 C2 C7 122.3(3) . . ?
C4 C3 C2 123.5(4) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C5 C4 C3 119.0(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 121.0(4) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.1(4) . . ?
C5 C6 C11 120.5(3) . . ?
C1 C6 C11 120.1(3) . . ?
C9 C7 C2 110.9(3) . . ?
C9 C7 C8 110.0(3) . . ?
C2 C7 C8 111.2(3) . . ?
C9 C7 C10 106.7(3) . . ?
C2 C7 C10 111.4(3) . . ?
C8 C7 C10 106.5(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C11 C6 115.7(3) . . ?
N1 C11 H11A 108.4 . . ?
C6 C11 H11A 108.4 . . ?
N1 C11 H11B 108.4 . . ?
C6 C11 H11B 108.4 . . ?
H11A C11 H11B 107.4 . . ?
N1 C12 C15 111.2(3) . . ?
N1 C12 C13 101.9(3) . . ?
C15 C12 C13 114.8(3) . . ?
N1 C12 H12 109.6 . . ?
C15 C12 H12 109.6 . . ?
C13 C12 H12 109.6 . . ?
N2 C13 C12 101.6(3) . . ?
N2 C13 C21 111.3(3) . . ?
C12 C13 C21 113.7(4) . . ?
N2 C13 H13 110.0 . . ?
C12 C13 H13 110.0 . . ?
C21 C13 H13 110.0 . . ?
N2 C14 N1 109.0(3) . . ?
N2 C14 Zr1 125.4(3) . . ?
N1 C14 Zr1 125.1(3) . . ?
C16 C15 C20 117.8(4) . . ?
C16 C15 C12 122.0(4) . . ?
C20 C15 C12 120.0(4) . . ?
C17 C16 C15 121.0(4) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C18 C17 C16 120.6(5) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C19 C18 C17 119.1(5) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C20 121.6(5) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C19 C20 C15 119.9(5) . . ?
C19 C20 H20 120.0 . . ?
C15 C20 H20 120.0 . . ?
C22 C21 C26B 115.6(6) . . ?
C22 C21 C26A 113.2(6) . . ?
C26B C21 C26A 43.4(6) . . ?
C22 C21 C13 124.8(4) . . ?
C26B C21 C13 115.1(6) . . ?
C26A C21 C13 118.1(5) . . ?
C21 C22 C23 124.0(4) . . ?
C21 C22 H22 118.0 . . ?
C23 C22 H22 118.0 . . ?
C22 C23 C24A 119.0(7) . . ?
C22 C23 C24B 115.2(6) . . ?
C24A C23 C24B 35.2(5) . . ?
C22 C23 H23 120.5 . . ?
C24A C23 H23 120.5 . . ?
C24B C23 H23 112.7 . . ?
C25A C24A C23 118.6(10) . . ?
C25A C24A H24A 120.7 . . ?
C23 C24A H24A 120.7 . . ?
C24A C25A C26A 120.1(11) . . ?
C24A C25A H25A 119.9 . . ?
C26A C25A H25A 119.9 . . ?
C25A C26A C21 121.7(9) . . ?
C25A C26A H26A 119.2 . . ?
C21 C26A H26A 119.2 . . ?
C25B C24B C23 118.6(9) . . ?
C25B C24B H24B 120.7 . . ?
C23 C24B H24B 120.7 . . ?
C24B C25B C26B 124.1(11) . . ?
C24B C25B H25B 118.0 . . ?
C26B C25B H25B 118.0 . . ?
C25B C26B C21 118.4(10) . . ?
C25B C26B H26B 120.8 . . ?
C21 C26B H26B 120.8 . . ?
N2 C27 C28 114.5(4) . . ?
N2 C27 H27A 108.6 . . ?
C28 C27 H27A 108.6 . . ?
N2 C27 H27B 108.6 . . ?
C28 C27 H27B 108.6 . . ?
H27A C27 H27B 107.6 . . ?
C29 C28 C33 119.7(4) . . ?
C29 C28 C27 121.2(4) . . ?
C33 C28 C27 119.0(4) . . ?
C30 C29 C28 122.2(5) . . ?
C30 C29 H29 118.9 . . ?
C28 C29 H29 118.9 . . ?
C29 C30 C31 117.6(4) . . ?
C29 C30 H30 121.2 . . ?
C31 C30 H30 121.2 . . ?
C32 C31 C30 125.2(4) . . ?
C32 C31 H31 117.4 . . ?
C30 C31 H31 117.4 . . ?
C31 C32 C33 114.7(4) . . ?
C31 C32 C34 123.6(4) . . ?
C33 C32 C34 121.7(4) . . ?
O2 C33 C28 119.4(4) . . ?
O2 C33 C32 120.3(4) . . ?
C28 C33 C32 120.3(4) . . ?
C32 C34 C36 111.5(4) . . ?
C32 C34 C35 111.1(4) . . ?
C36 C34 C35 109.3(4) . . ?
C32 C34 C37 111.0(4) . . ?
C36 C34 C37 110.1(4) . . ?
C35 C34 C37 103.7(4) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N3 C38 H38A 109.5 . . ?
N3 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N3 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N3 C39 H39A 109.5 . . ?
N3 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N3 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
O3 C40 C41 105.1(4) . . ?
O3 C40 H40A 110.7 . . ?
C41 C40 H40A 110.7 . . ?
O3 C40 H40B 110.7 . . ?
C41 C40 H40B 110.7 . . ?
H40A C40 H40B 108.8 . . ?
C40 C41 C42 103.0(4) . . ?
C40 C41 H41A 111.2 . . ?
C42 C41 H41A 111.2 . . ?
C40 C41 H41B 111.2 . . ?
C42 C41 H41B 111.2 . . ?
H41A C41 H41B 109.1 . . ?
C41 C42 C43 102.4(4) . . ?
C41 C42 H42A 111.3 . . ?
C43 C42 H42A 111.3 . . ?
C41 C42 H42B 111.3 . . ?
C43 C42 H42B 111.3 . . ?
H42A C42 H42B 109.2 . . ?
O3 C43 C42 105.0(4) . . ?
O3 C43 H43A 110.7 . . ?
C42 C43 H43A 110.7 . . ?
O3 C43 H43B 110.7 . . ?
C42 C43 H43B 110.7 . . ?
H43A C43 H43B 108.8 . . ?
O4 C44 C49 117.2(4) . . ?
O4 C44 C45 122.1(4) . . ?
C49 C44 C45 120.7(4) . . ?
C46 C45 C44 116.6(4) . . ?
C46 C45 C50 120.5(4) . . ?
C44 C45 C50 122.8(4) . . ?
C47 C46 C45 122.4(5) . . ?
C47 C46 H46 118.8 . . ?
C45 C46 H46 118.8 . . ?
C48 C47 C46 120.6(5) . . ?
C48 C47 H47 119.7 . . ?
C46 C47 H47 119.7 . . ?
C47 C48 C49 120.8(5) . . ?
C47 C48 H48 119.6 . . ?
C49 C48 H48 119.6 . . ?
C44 C49 C48 118.8(4) . . ?
C44 C49 C54 120.8(4) . . ?
C48 C49 C54 120.1(4) . . ?
C45 C50 C51 110.4(5) . . ?
C45 C50 C53 112.8(4) . . ?
C51 C50 C53 107.7(4) . . ?
C45 C50 C52 109.2(4) . . ?
C51 C50 C52 109.7(4) . . ?
C53 C50 C52 106.9(5) . . ?
C50 C51 H51A 109.5 . . ?
C50 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C50 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C50 C52 H52A 109.5 . . ?
C50 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C50 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N4 C54 C49 114.0(4) . . ?
N4 C54 H54A 108.7 . . ?
C49 C54 H54A 108.7 . . ?
N4 C54 H54B 108.7 . . ?
C49 C54 H54B 108.7 . . ?
H54A C54 H54B 107.6 . . ?
N4 C55 C58 112.5(3) . . ?
N4 C55 C56 101.2(3) . . ?
C58 C55 C56 115.3(3) . . ?
N4 C55 H55 109.2 . . ?
C58 C55 H55 109.2 . . ?
C56 C55 H55 109.2 . . ?
C64 C56 N5 113.4(3) . . ?
C64 C56 C55 115.3(3) . . ?
N5 C56 C55 101.3(3) . . ?
C64 C56 H56 108.8 . . ?
N5 C56 H56 108.8 . . ?
C55 C56 H56 108.8 . . ?
N4 C57 N5 108.6(3) . . ?
N4 C57 Zr2 124.0(3) . . ?
N5 C57 Zr2 127.0(3) . . ?
C59 C58 C63 116.4(4) . . ?
C59 C58 C55 122.1(4) . . ?
C63 C58 C55 121.3(4) . . ?
C60 C59 C58 121.6(4) . . ?
C60 C59 H59 119.2 . . ?
C58 C59 H59 119.2 . . ?
C61 C60 C59 120.7(4) . . ?
C61 C60 H60 119.7 . . ?
C59 C60 H60 119.7 . . ?
C60 C61 C62 119.8(4) . . ?
C60 C61 H61 120.1 . . ?
C62 C61 H61 120.1 . . ?
C63 C62 C61 119.3(4) . . ?
C63 C62 H62 120.3 . . ?
C61 C62 H62 120.3 . . ?
C62 C63 C58 122.2(4) . . ?
C62 C63 H63 118.9 . . ?
C58 C63 H63 118.9 . . ?
C69 C64 C65 115.3(5) . . ?
C69 C64 C56 123.2(5) . . ?
C65 C64 C56 121.4(4) . . ?
C64 C65 C66 122.6(6) . . ?
C64 C65 H65 118.7 . . ?
C66 C65 H65 118.7 . . ?
C67 C66 C65 119.4(7) . . ?
C67 C66 H66 120.3 . . ?
C65 C66 H66 120.3 . . ?
C66 C67 C68 121.3(7) . . ?
C66 C67 H67 119.3 . . ?
C68 C67 H67 119.3 . . ?
C69 C68 C67 118.9(7) . . ?
C69 C68 H68 120.5 . . ?
C67 C68 H68 120.5 . . ?
C68 C69 C64 122.4(6) . . ?
C68 C69 H69 118.8 . . ?
C64 C69 H69 118.8 . . ?
N5 C70 C71 115.2(3) . . ?
N5 C70 H70A 108.5 . . ?
C71 C70 H70A 108.5 . . ?
N5 C70 H70B 108.5 . . ?
C71 C70 H70B 108.5 . . ?
H70A C70 H70B 107.5 . . ?
C72 C71 C76 118.8(4) . . ?
C72 C71 C70 120.0(4) . . ?
C76 C71 C70 121.0(3) . . ?
C73 C72 C71 120.2(4) . . ?
C73 C72 H72 119.9 . . ?
C71 C72 H72 119.9 . . ?
C72 C73 C74 119.3(4) . . ?
C72 C73 H73 120.3 . . ?
C74 C73 H73 120.3 . . ?
C73 C74 C75 124.2(5) . . ?
C73 C74 H74 117.9 . . ?
C75 C74 H74 117.9 . . ?
C74 C75 C76 115.6(4) . . ?
C74 C75 C77 122.2(4) . . ?
C76 C75 C77 122.2(4) . . ?
O5 C76 C75 121.3(3) . . ?
O5 C76 C71 117.2(3) . . ?
C75 C76 C71 121.5(4) . . ?
C80 C77 C75 109.8(3) . . ?
C80 C77 C79 111.3(3) . . ?
C75 C77 C79 111.0(3) . . ?
C80 C77 C78 106.5(3) . . ?
C75 C77 C78 111.2(3) . . ?
C79 C77 C78 106.9(3) . . ?
C77 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C77 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C77 C79 H79A 109.5 . . ?
C77 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C77 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C77 C80 H80A 109.5 . . ?
C77 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C77 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
N6 C81 H81A 109.5 . . ?
N6 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
N6 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
N6 C82 H82A 109.5 . . ?
N6 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
N6 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
O6 C83 C84 106.5(3) . . ?
O6 C83 H83A 110.4 . . ?
C84 C83 H83A 110.4 . . ?
O6 C83 H83B 110.4 . . ?
C84 C83 H83B 110.4 . . ?
H83A C83 H83B 108.6 . . ?
C83 C84 C85 100.8(4) . . ?
C83 C84 H84A 111.6 . . ?
C85 C84 H84A 111.6 . . ?
C83 C84 H84B 111.6 . . ?
C85 C84 H84B 111.6 . . ?
H84A C84 H84B 109.4 . . ?
C86 C85 C84 103.2(4) . . ?
C86 C85 H85A 111.1 . . ?
C84 C85 H85A 111.1 . . ?
C86 C85 H85B 111.1 . . ?
C84 C85 H85B 111.1 . . ?
H85A C85 H85B 109.1 . . ?
O6 C86 C85 105.4(3) . . ?
O6 C86 H86A 110.7 . . ?
C85 C86 H86A 110.7 . . ?
O6 C86 H86B 110.7 . . ?
C85 C86 H86B 110.7 . . ?
H86A C86 H86B 108.8 . . ?
C14 N1 C11 125.3(3) . . ?
C14 N1 C12 111.9(3) . . ?
C11 N1 C12 120.7(3) . . ?
C14 N2 C27 123.6(3) . . ?
C14 N2 C13 112.3(3) . . ?
C27 N2 C13 122.0(3) . . ?
C39 N3 C38 109.5(4) . . ?
C39 N3 Zr1 122.7(3) . . ?
C38 N3 Zr1 127.5(3) . . ?
C57 N4 C54 123.9(3) . . ?
C57 N4 C55 113.2(3) . . ?
C54 N4 C55 121.3(3) . . ?
C57 N5 C70 124.5(3) . . ?
C57 N5 C56 112.3(3) . . ?
C70 N5 C56 120.5(3) . . ?
C82 N6 C81 110.2(4) . . ?
C82 N6 Zr2 122.6(3) . . ?
C81 N6 Zr2 126.8(3) . . ?
C1 O1 Zr1 160.5(2) . . ?
C33 O2 Zr1 155.0(2) . . ?
C40 O3 C43 108.9(3) . . ?
C40 O3 Zr1 122.2(2) . . ?
C43 O3 Zr1 128.7(3) . . ?
C44 O4 Zr2 156.1(3) . . ?
C76 O5 Zr2 160.4(2) . . ?
C83 O6 C86 108.9(3) . . ?
C83 O6 Zr2 123.4(2) . . ?
C86 O6 Zr2 127.6(2) . . ?
O1 Zr1 O2 164.67(11) . . ?
O1 Zr1 N3 94.31(12) . . ?
O2 Zr1 N3 94.36(12) . . ?
O1 Zr1 O3 84.04(10) . . ?
O2 Zr1 O3 85.87(10) . . ?
N3 Zr1 O3 173.23(11) . . ?
O1 Zr1 C14 83.92(12) . . ?
O2 Zr1 C14 83.38(11) . . ?
N3 Zr1 C14 90.58(14) . . ?
O3 Zr1 C14 82.72(12) . . ?
O1 Zr1 Cl1 97.42(8) . . ?
O2 Zr1 Cl1 92.91(8) . . ?
N3 Zr1 Cl1 103.03(9) . . ?
O3 Zr1 Cl1 83.71(7) . . ?
C14 Zr1 Cl1 166.15(10) . . ?
O5 Zr2 O4 163.95(11) . . ?
O5 Zr2 N6 95.24(12) . . ?
O4 Zr2 N6 93.63(12) . . ?
O5 Zr2 O6 84.90(10) . . ?
O4 Zr2 O6 85.00(10) . . ?
N6 Zr2 O6 174.48(12) . . ?
O5 Zr2 C57 82.64(12) . . ?
O4 Zr2 C57 83.87(12) . . ?
N6 Zr2 C57 90.95(14) . . ?
O6 Zr2 C57 83.60(12) . . ?
O5 Zr2 Cl2 97.90(8) . . ?
O4 Zr2 Cl2 93.39(8) . . ?
N6 Zr2 Cl2 101.55(10) . . ?
O6 Zr2 Cl2 83.88(7) . . ?
C57 Zr2 Cl2 167.37(10) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.219
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.065
_database_code_depnum_ccdc_archive 'CCDC 975124'
#######################################################################
#
#                 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_compound17

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C51 H70 Cl N3 O3 Ti'
_chemical_formula_sum            'C51 H70 Cl N3 O3 Ti'
_chemical_formula_weight         856.45
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   12.3919(13)
_cell_length_b                   15.1779(16)
_cell_length_c                   29.978(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5638.4(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    7068
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      24.18

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1840
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9013
_exptl_absorpt_correction_T_max  0.9588
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      110(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10187
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         25.25
_reflns_number_total             10187
_reflns_number_gt                9028
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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)+(0.0566P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_number_reflns         10187
_refine_ls_number_parameters     561
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0397
_refine_ls_wR_factor_ref         0.1008
_refine_ls_wR_factor_gt          0.0974
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.064 0.750 0.000 629 135 ' '
2 -0.029 1.250 0.500 629 135 ' '
_platon_squeeze_details          
;
;

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 0.24265(18) 0.28145(16) 0.30055(8) 0.0208(5) Uani 1 1 d . . .
C2 C 0.24184(19) 0.27235(16) 0.34762(8) 0.0205(5) Uani 1 1 d . . .
C3 C 0.3173(2) 0.20753(17) 0.37194(8) 0.0280(6) Uani 1 1 d . . .
C4 C 0.4371(2) 0.2284(2) 0.36354(9) 0.0346(7) Uani 1 1 d . . .
H4A H 0.4527 0.2230 0.3316 0.052 Uiso 1 1 calc R . .
H4B H 0.4822 0.1869 0.3803 0.052 Uiso 1 1 calc R . .
H4C H 0.4527 0.2887 0.3734 0.052 Uiso 1 1 calc R . .
C5 C 0.2914(2) 0.11379(17) 0.35563(9) 0.0359(7) Uani 1 1 d . . .
H5A H 0.3061 0.1096 0.3236 0.054 Uiso 1 1 calc R . .
H5B H 0.2152 0.1008 0.3612 0.054 Uiso 1 1 calc R . .
H5C H 0.3366 0.0713 0.3717 0.054 Uiso 1 1 calc R . .
C6 C 0.3002(2) 0.2082(2) 0.42272(9) 0.0396(7) Uani 1 1 d . . .
H6A H 0.3503 0.1667 0.4368 0.059 Uiso 1 1 calc R . .
H6B H 0.2258 0.1907 0.4295 0.059 Uiso 1 1 calc R . .
H6C H 0.3134 0.2676 0.4343 0.059 Uiso 1 1 calc R . .
C7 C 0.16507(19) 0.31961(16) 0.37117(8) 0.0244(5) Uani 1 1 d . . .
H7 H 0.1654 0.3144 0.4027 0.029 Uiso 1 1 calc R . .
C8 C 0.0877(2) 0.37395(16) 0.35216(8) 0.0254(6) Uani 1 1 d . . .
C9 C 0.0034(2) 0.42484(19) 0.37909(9) 0.0339(7) Uani 1 1 d . . .
C10 C 0.0166(2) 0.52365(18) 0.36951(12) 0.0455(8) Uani 1 1 d . . .
H10A H -0.0345 0.5572 0.3878 0.068 Uiso 1 1 calc R . .
H10B H 0.0022 0.5350 0.3379 0.068 Uiso 1 1 calc R . .
H10C H 0.0904 0.5418 0.3767 0.068 Uiso 1 1 calc R . .
C11 C -0.1094(2) 0.3969(2) 0.36462(10) 0.0413(7) Uani 1 1 d . . .
H11A H -0.1200 0.3344 0.3715 0.062 Uiso 1 1 calc R . .
H11B H -0.1174 0.4062 0.3324 0.062 Uiso 1 1 calc R . .
H11C H -0.1632 0.4321 0.3806 0.062 Uiso 1 1 calc R . .
C12 C 0.0161(3) 0.4103(3) 0.42902(10) 0.0699(12) Uani 1 1 d U . .
H12A H 0.0902 0.4246 0.4379 0.105 Uiso 1 1 calc R . .
H12B H 0.0009 0.3485 0.4362 0.105 Uiso 1 1 calc R . .
H12C H -0.0344 0.4484 0.4451 0.105 Uiso 1 1 calc R . .
C13 C 0.08962(19) 0.38021(15) 0.30568(8) 0.0214(5) Uani 1 1 d . . .
H13 H 0.0382 0.4169 0.2913 0.026 Uiso 1 1 calc R . .
C14 C 0.16384(18) 0.33484(14) 0.27988(8) 0.0186(5) Uani 1 1 d . . .
C15 C 0.15490(19) 0.33726(15) 0.22997(8) 0.0201(5) Uani 1 1 d . . .
H15A H 0.1529 0.2760 0.2187 0.024 Uiso 1 1 calc R . .
H15B H 0.0856 0.3655 0.2219 0.024 Uiso 1 1 calc R . .
C16 C 0.21658(19) 0.46018(15) 0.17806(8) 0.0214(5) Uani 1 1 d . . .
H16 H 0.1714 0.4393 0.1525 0.026 Uiso 1 1 calc R . .
C17 C 0.16014(19) 0.53587(15) 0.20087(8) 0.0198(5) Uani 1 1 d . . .
C18 C 0.1891(2) 0.56290(16) 0.24353(8) 0.0256(5) Uani 1 1 d . . .
H18 H 0.2420 0.5312 0.2599 0.031 Uiso 1 1 calc R . .
C19 C 0.1401(2) 0.63645(16) 0.26197(9) 0.0268(6) Uani 1 1 d . . .
H19 H 0.1593 0.6545 0.2913 0.032 Uiso 1 1 calc R . .
C20 C 0.0645(2) 0.68356(16) 0.23867(9) 0.0270(6) Uani 1 1 d . . .
H20 H 0.0321 0.7341 0.2517 0.032 Uiso 1 1 calc R . .
C21 C 0.0356(2) 0.65721(18) 0.19618(9) 0.0327(6) Uani 1 1 d . . .
H21 H -0.0163 0.6899 0.1797 0.039 Uiso 1 1 calc R . .
C22 C 0.0823(2) 0.58321(16) 0.17775(9) 0.0275(6) Uani 1 1 d . . .
H22 H 0.0609 0.5644 0.1488 0.033 Uiso 1 1 calc R . .
C23 C 0.32928(19) 0.48451(15) 0.16080(8) 0.0207(5) Uani 1 1 d . . .
H23 H 0.3605 0.5323 0.1798 0.025 Uiso 1 1 calc R . .
C24 C 0.3263(2) 0.51442(18) 0.11296(9) 0.0305(6) Uani 1 1 d . . .
C25 C 0.3191(2) 0.6050(2) 0.10472(11) 0.0459(8) Uani 1 1 d . . .
H25 H 0.3230 0.6455 0.1289 0.055 Uiso 1 1 calc R . .
C26 C 0.3065(3) 0.6358(3) 0.06182(14) 0.0651(11) Uani 1 1 d U . .
H26 H 0.3003 0.6972 0.0562 0.078 Uiso 1 1 calc R . .
C27 C 0.3031(3) 0.5759(3) 0.02707(13) 0.0715(12) Uani 1 1 d U . .
H27 H 0.2952 0.5969 -0.0026 0.086 Uiso 1 1 calc R . .
C28 C 0.3107(3) 0.4897(3) 0.03401(11) 0.0665(11) Uani 1 1 d U . .
H28 H 0.3089 0.4500 0.0096 0.080 Uiso 1 1 calc R . .
C29 C 0.3213(3) 0.4576(2) 0.07799(9) 0.0491(9) Uani 1 1 d . . .
H29 H 0.3250 0.3959 0.0832 0.059 Uiso 1 1 calc R . .
C30 C 0.33868(19) 0.34945(15) 0.19813(7) 0.0196(5) Uani 1 1 d . . .
C31 C 0.50481(18) 0.39768(15) 0.15975(8) 0.0221(5) Uani 1 1 d . . .
H31A H 0.5428 0.3830 0.1878 0.027 Uiso 1 1 calc R . .
H31B H 0.5290 0.4570 0.1504 0.027 Uiso 1 1 calc R . .
C32 C 0.53822(19) 0.33236(16) 0.12452(8) 0.0231(5) Uani 1 1 d . . .
C33 C 0.5797(2) 0.36281(18) 0.08446(8) 0.0295(6) Uani 1 1 d . A .
H33 H 0.5810 0.4244 0.0787 0.035 Uiso 1 1 calc R . .
C34 C 0.6195(2) 0.30480(19) 0.05250(9) 0.0327(6) Uani 1 1 d . . .
C35A C 0.6658(15) 0.3375(15) 0.0072(10) 0.0407(10) Uani 0.50 1 d PDU A 1
C36A C 0.6567(11) 0.4379(13) 0.0031(7) 0.057(2) Uani 0.50 1 d PDU A 1
H36A H 0.5816 0.4557 0.0077 0.086 Uiso 0.50 1 calc PR A 1
H36B H 0.6801 0.4562 -0.0268 0.086 Uiso 0.50 1 calc PR A 1
H36C H 0.7026 0.4659 0.0256 0.086 Uiso 0.50 1 calc PR A 1
C37A C 0.5993(8) 0.2918(7) -0.0296(4) 0.061(2) Uani 0.50 1 d PDU A 1
H37A H 0.5243 0.3118 -0.0280 0.092 Uiso 0.50 1 calc PR A 1
H37B H 0.6021 0.2278 -0.0253 0.092 Uiso 0.50 1 calc PR A 1
H37C H 0.6294 0.3068 -0.0589 0.092 Uiso 0.50 1 calc PR A 1
C38A C 0.7870(11) 0.3115(9) 0.0029(5) 0.062(3) Uani 0.50 1 d PDU A 1
H38A H 0.8156 0.3334 -0.0255 0.092 Uiso 0.50 1 calc PR A 1
H38B H 0.7939 0.2473 0.0040 0.092 Uiso 0.50 1 calc PR A 1
H38C H 0.8277 0.3377 0.0276 0.092 Uiso 0.50 1 calc PR A 1
C35B C 0.6564(15) 0.3350(15) 0.0061(10) 0.0407(10) Uani 0.50 1 d PD A 2
C36B C 0.6882(11) 0.4336(13) 0.0056(7) 0.057(2) Uani 0.50 1 d PD A 2
H36D H 0.7152 0.4494 -0.0241 0.086 Uiso 0.50 1 calc PR A 2
H36E H 0.7446 0.4441 0.0279 0.086 Uiso 0.50 1 calc PR A 2
H36F H 0.6248 0.4696 0.0127 0.086 Uiso 0.50 1 calc PR A 2
C37B C 0.5646(8) 0.3233(7) -0.0274(4) 0.061(2) Uani 0.50 1 d PD A 2
H37D H 0.5335 0.2642 -0.0242 0.092 Uiso 0.50 1 calc PR A 2
H37E H 0.5926 0.3304 -0.0578 0.092 Uiso 0.50 1 calc PR A 2
H37F H 0.5087 0.3676 -0.0218 0.092 Uiso 0.50 1 calc PR A 2
C38B C 0.7649(11) 0.2889(9) -0.0065(5) 0.062(3) Uani 0.50 1 d PD A 2
H38D H 0.7516 0.2264 -0.0126 0.092 Uiso 0.50 1 calc PR A 2
H38E H 0.8158 0.2945 0.0184 0.092 Uiso 0.50 1 calc PR A 2
H38F H 0.7954 0.3170 -0.0331 0.092 Uiso 0.50 1 calc PR A 2
C39 C 0.6181(2) 0.21619(18) 0.06322(8) 0.0297(6) Uani 1 1 d . A .
H39 H 0.6463 0.1763 0.0418 0.036 Uiso 1 1 calc R . .
C40 C 0.5787(2) 0.18051(16) 0.10303(8) 0.0243(6) Uani 1 1 d . . .
C41 C 0.5884(2) 0.08238(16) 0.11339(8) 0.0272(6) Uani 1 1 d . A .
C42 C 0.6460(2) 0.03173(18) 0.07591(9) 0.0374(7) Uani 1 1 d . . .
H42A H 0.6540 -0.0302 0.0846 0.056 Uiso 1 1 calc R A .
H42B H 0.7174 0.0576 0.0708 0.056 Uiso 1 1 calc R . .
H42C H 0.6032 0.0355 0.0485 0.056 Uiso 1 1 calc R . .
C43 C 0.6543(2) 0.06889(17) 0.15613(9) 0.0311(6) Uani 1 1 d . . .
H43A H 0.6154 0.0943 0.1815 0.047 Uiso 1 1 calc R A .
H43B H 0.7245 0.0980 0.1530 0.047 Uiso 1 1 calc R . .
H43C H 0.6653 0.0057 0.1612 0.047 Uiso 1 1 calc R . .
C44 C 0.4770(2) 0.04104(18) 0.11887(9) 0.0336(6) Uani 1 1 d . . .
H44A H 0.4417 0.0659 0.1453 0.050 Uiso 1 1 calc R A .
H44B H 0.4845 -0.0228 0.1225 0.050 Uiso 1 1 calc R . .
H44C H 0.4333 0.0535 0.0924 0.050 Uiso 1 1 calc R . .
C45 C 0.53309(19) 0.24192(16) 0.13372(8) 0.0221(5) Uani 1 1 d . A .
C46 C 0.2559(2) 0.16500(19) 0.14525(9) 0.0325(6) Uani 1 1 d . . .
H46A H 0.2457 0.1055 0.1333 0.049 Uiso 1 1 calc R . .
H46B H 0.3158 0.1938 0.1297 0.049 Uiso 1 1 calc R . .
H46C H 0.1897 0.1993 0.1409 0.049 Uiso 1 1 calc R . .
C47 C 0.2000(2) 0.10733(16) 0.21637(9) 0.0301(6) Uani 1 1 d . . .
H47A H 0.1278 0.1301 0.2098 0.045 Uiso 1 1 calc R . .
H47B H 0.2134 0.1108 0.2485 0.045 Uiso 1 1 calc R . .
H47C H 0.2049 0.0458 0.2067 0.045 Uiso 1 1 calc R . .
C48 C 0.63890(18) 0.26989(17) 0.25267(9) 0.0281(6) Uani 1 1 d . A .
H48A H 0.6580 0.2522 0.2219 0.034 Uiso 1 1 calc R . .
H48B H 0.6558 0.2206 0.2732 0.034 Uiso 1 1 calc R . .
C49 C 0.6988(2) 0.35145(19) 0.26597(10) 0.0361(7) Uani 1 1 d . . .
H49A H 0.7086 0.3916 0.2403 0.043 Uiso 1 1 calc R . .
H49B H 0.7703 0.3370 0.2788 0.043 Uiso 1 1 calc R . .
C50 C 0.6243(2) 0.39151(19) 0.30091(9) 0.0339(7) Uani 1 1 d . . .
H50A H 0.6328 0.3620 0.3302 0.041 Uiso 1 1 calc R . .
H50B H 0.6378 0.4554 0.3045 0.041 Uiso 1 1 calc R . .
C51 C 0.5141(2) 0.37428(14) 0.28118(9) 0.0239(5) Uani 1 1 d . A .
H51A H 0.4597 0.3671 0.3051 0.029 Uiso 1 1 calc R . .
H51B H 0.4919 0.4237 0.2617 0.029 Uiso 1 1 calc R . .
Cl1 Cl 0.47992(5) 0.09152(4) 0.25740(2) 0.02522(14) Uani 1 1 d . . .
N1 N 0.24266(16) 0.38436(12) 0.20724(6) 0.0192(4) Uani 1 1 d . . .
N2 N 0.38873(16) 0.40115(12) 0.16884(6) 0.0203(4) Uani 1 1 d . . .
N3 N 0.28028(16) 0.15965(13) 0.19275(7) 0.0234(5) Uani 1 1 d . . .
O1 O 0.31488(13) 0.23971(9) 0.27475(5) 0.0204(3) Uani 1 1 d . . .
O2 O 0.48712(12) 0.21582(10) 0.17247(5) 0.0210(3) Uani 1 1 d . . .
O3 O 0.52477(12) 0.29358(10) 0.25557(5) 0.0215(4) Uani 1 1 d . . .
Ti1 Ti 0.39585(3) 0.21714(3) 0.222588(14) 0.01790(10) Uani 1 1 d . A .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.342(3) . ?
C1 C14 1.412(3) . ?
C1 C2 1.418(3) . ?
C2 C7 1.385(3) . ?
C2 C3 1.541(3) . ?
C3 C6 1.537(4) . ?
C3 C4 1.538(4) . ?
C3 C5 1.538(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.387(3) . ?
C7 H7 0.9500 . ?
C8 C13 1.397(3) . ?
C8 C9 1.529(3) . ?
C9 C12 1.521(4) . ?
C9 C11 1.523(4) . ?
C9 C10 1.536(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.385(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.501(3) . ?
C15 N1 1.469(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N1 1.481(3) . ?
C16 C17 1.509(3) . ?
C16 C23 1.534(3) . ?
C16 H16 1.0000 . ?
C17 C22 1.388(3) . ?
C17 C18 1.390(3) . ?
C18 C19 1.386(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.370(3) . ?
C19 H19 0.9500 . ?
C20 C21 1.383(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.379(3) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 N2 1.484(3) . ?
C23 C24 1.505(3) . ?
C23 H23 1.0000 . ?
C24 C29 1.359(4) . ?
C24 C25 1.400(4) . ?
C25 C26 1.378(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.384(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.327(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.412(5) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 N1 1.331(3) . ?
C30 N2 1.331(3) . ?
C30 Ti1 2.252(2) . ?
C31 N2 1.465(3) . ?
C31 C32 1.507(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.386(3) . ?
C32 C45 1.402(3) . ?
C33 C34 1.391(4) . ?
C33 H33 0.9500 . ?
C34 C39 1.383(4) . ?
C34 C35B 1.54(3) . ?
C34 C35A 1.56(3) . ?
C35A C36A 1.533(16) . ?
C35A C37A 1.541(16) . ?
C35A C38A 1.557(15) . ?
C36A H36A 0.9800 . ?
C36A H36B 0.9800 . ?
C36A H36C 0.9800 . ?
C37A H37A 0.9800 . ?
C37A H37B 0.9800 . ?
C37A H37C 0.9800 . ?
C38A H38A 0.9800 . ?
C38A H38B 0.9800 . ?
C38A H38C 0.9800 . ?
C35B C37B 1.528(15) . ?
C35B C36B 1.547(16) . ?
C35B C38B 1.561(16) . ?
C36B H36D 0.9800 . ?
C36B H36E 0.9800 . ?
C36B H36F 0.9800 . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
C39 C40 1.399(3) . ?
C39 H39 0.9500 . ?
C40 C45 1.426(3) . ?
C40 C41 1.526(3) . ?
C41 C44 1.525(4) . ?
C41 C43 1.533(4) . ?
C41 C42 1.537(3) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 O2 1.353(3) . ?
C46 N3 1.458(3) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 N3 1.456(3) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 O3 1.462(3) . ?
C48 C49 1.497(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.523(4) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.511(4) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 O3 1.451(3) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
Cl1 Ti1 2.4104(7) . ?
N3 Ti1 1.901(2) . ?
O1 Ti1 1.8893(17) . ?
O2 Ti1 1.8806(16) . ?
O3 Ti1 2.2081(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C14 118.6(2) . . ?
O1 C1 C2 122.2(2) . . ?
C14 C1 C2 119.2(2) . . ?
C7 C2 C1 117.5(2) . . ?
C7 C2 C3 120.4(2) . . ?
C1 C2 C3 121.9(2) . . ?
C6 C3 C4 107.1(2) . . ?
C6 C3 C5 107.0(2) . . ?
C4 C3 C5 109.9(2) . . ?
C6 C3 C2 112.3(2) . . ?
C4 C3 C2 112.1(2) . . ?
C5 C3 C2 108.3(2) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C2 C7 C8 125.0(2) . . ?
C2 C7 H7 117.5 . . ?
C8 C7 H7 117.5 . . ?
C7 C8 C13 116.0(2) . . ?
C7 C8 C9 123.8(2) . . ?
C13 C8 C9 120.3(2) . . ?
C12 C9 C11 109.6(3) . . ?
C12 C9 C8 112.0(2) . . ?
C11 C9 C8 109.6(2) . . ?
C12 C9 C10 108.3(3) . . ?
C11 C9 C10 108.4(2) . . ?
C8 C9 C10 108.8(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C8 122.3(2) . . ?
C14 C13 H13 118.8 . . ?
C8 C13 H13 118.8 . . ?
C13 C14 C1 120.0(2) . . ?
C13 C14 C15 119.7(2) . . ?
C1 C14 C15 120.2(2) . . ?
N1 C15 C14 114.81(19) . . ?
N1 C15 H15A 108.6 . . ?
C14 C15 H15A 108.6 . . ?
N1 C15 H15B 108.6 . . ?
C14 C15 H15B 108.6 . . ?
H15A C15 H15B 107.5 . . ?
N1 C16 C17 115.15(19) . . ?
N1 C16 C23 100.81(18) . . ?
C17 C16 C23 113.05(19) . . ?
N1 C16 H16 109.2 . . ?
C17 C16 H16 109.2 . . ?
C23 C16 H16 109.2 . . ?
C22 C17 C18 119.1(2) . . ?
C22 C17 C16 119.3(2) . . ?
C18 C17 C16 121.5(2) . . ?
C19 C18 C17 119.4(2) . . ?
C19 C18 H18 120.3 . . ?
C17 C18 H18 120.3 . . ?
C20 C19 C18 121.1(2) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C19 C20 C21 119.7(2) . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C22 C21 C20 119.7(2) . . ?
C22 C21 H21 120.1 . . ?
C20 C21 H21 120.1 . . ?
C21 C22 C17 120.9(2) . . ?
C21 C22 H22 119.6 . . ?
C17 C22 H22 119.6 . . ?
N2 C23 C24 115.1(2) . . ?
N2 C23 C16 101.07(18) . . ?
C24 C23 C16 111.8(2) . . ?
N2 C23 H23 109.5 . . ?
C24 C23 H23 109.5 . . ?
C16 C23 H23 109.5 . . ?
C29 C24 C25 119.0(3) . . ?
C29 C24 C23 123.0(3) . . ?
C25 C24 C23 117.8(3) . . ?
C26 C25 C24 120.4(4) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C25 C26 C27 118.9(4) . . ?
C25 C26 H26 120.6 . . ?
C27 C26 H26 120.6 . . ?
C28 C27 C26 121.9(3) . . ?
C28 C27 H27 119.1 . . ?
C26 C27 H27 119.1 . . ?
C27 C28 C29 119.6(4) . . ?
C27 C28 H28 120.2 . . ?
C29 C28 H28 120.2 . . ?
C24 C29 C28 120.3(3) . . ?
C24 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
N1 C30 N2 108.5(2) . . ?
N1 C30 Ti1 124.71(16) . . ?
N2 C30 Ti1 126.44(16) . . ?
N2 C31 C32 115.1(2) . . ?
N2 C31 H31A 108.5 . . ?
C32 C31 H31A 108.5 . . ?
N2 C31 H31B 108.5 . . ?
C32 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C33 C32 C45 120.9(2) . . ?
C33 C32 C31 119.3(2) . . ?
C45 C32 C31 119.6(2) . . ?
C32 C33 C34 121.1(2) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 H33 119.4 . . ?
C39 C34 C33 116.8(2) . . ?
C39 C34 C35B 120.3(8) . . ?
C33 C34 C35B 122.8(8) . . ?
C39 C34 C35A 121.1(8) . . ?
C33 C34 C35A 122.0(8) . . ?
C35B C34 C35A 4.6(12) . . ?
C36A C35A C37A 110.5(17) . . ?
C36A C35A C34 111.1(16) . . ?
C37A C35A C34 106.5(15) . . ?
C36A C35A C38A 108.4(16) . . ?
C37A C35A C38A 110.1(14) . . ?
C34 C35A C38A 110.3(16) . . ?
C37B C35B C34 109.8(16) . . ?
C37B C35B C36B 107.2(17) . . ?
C34 C35B C36B 111.9(16) . . ?
C37B C35B C38B 115.5(16) . . ?
C34 C35B C38B 110.0(16) . . ?
C36B C35B C38B 102.2(16) . . ?
C35B C36B H36D 109.5 . . ?
C35B C36B H36E 109.5 . . ?
H36D C36B H36E 109.5 . . ?
C35B C36B H36F 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
C35B C37B H37D 109.5 . . ?
C35B C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
C35B C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
C35B C38B H38D 109.5 . . ?
C35B C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C35B C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C34 C39 C40 125.4(2) . . ?
C34 C39 H39 117.3 . . ?
C40 C39 H39 117.3 . . ?
C39 C40 C45 115.8(2) . . ?
C39 C40 C41 121.6(2) . . ?
C45 C40 C41 122.5(2) . . ?
C44 C41 C40 110.6(2) . . ?
C44 C41 C43 109.7(2) . . ?
C40 C41 C43 110.0(2) . . ?
C44 C41 C42 107.0(2) . . ?
C40 C41 C42 112.1(2) . . ?
C43 C41 C42 107.3(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O2 C45 C32 118.3(2) . . ?
O2 C45 C40 122.0(2) . . ?
C32 C45 C40 119.7(2) . . ?
N3 C46 H46A 109.5 . . ?
N3 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N3 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N3 C47 H47A 109.5 . . ?
N3 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N3 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O3 C48 C49 105.1(2) . . ?
O3 C48 H48A 110.7 . . ?
C49 C48 H48A 110.7 . . ?
O3 C48 H48B 110.7 . . ?
C49 C48 H48B 110.7 . . ?
H48A C48 H48B 108.8 . . ?
C48 C49 C50 102.3(2) . . ?
C48 C49 H49A 111.3 . . ?
C50 C49 H49A 111.3 . . ?
C48 C49 H49B 111.3 . . ?
C50 C49 H49B 111.3 . . ?
H49A C49 H49B 109.2 . . ?
C51 C50 C49 102.1(2) . . ?
C51 C50 H50A 111.4 . . ?
C49 C50 H50A 111.4 . . ?
C51 C50 H50B 111.4 . . ?
C49 C50 H50B 111.4 . . ?
H50A C50 H50B 109.2 . . ?
O3 C51 C50 105.72(19) . . ?
O3 C51 H51A 110.6 . . ?
C50 C51 H51A 110.6 . . ?
O3 C51 H51B 110.6 . . ?
C50 C51 H51B 110.6 . . ?
H51A C51 H51B 108.7 . . ?
C30 N1 C15 124.28(19) . . ?
C30 N1 C16 112.53(19) . . ?
C15 N1 C16 119.37(18) . . ?
C30 N2 C31 123.99(19) . . ?
C30 N2 C23 112.24(19) . . ?
C31 N2 C23 119.21(19) . . ?
C47 N3 C46 111.3(2) . . ?
C47 N3 Ti1 122.42(16) . . ?
C46 N3 Ti1 126.18(17) . . ?
C1 O1 Ti1 156.48(15) . . ?
C45 O2 Ti1 159.38(15) . . ?
C51 O3 C48 109.08(17) . . ?
C51 O3 Ti1 127.91(13) . . ?
C48 O3 Ti1 122.96(13) . . ?
O2 Ti1 O1 169.29(7) . . ?
O2 Ti1 N3 94.14(8) . . ?
O1 Ti1 N3 94.16(8) . . ?
O2 Ti1 O3 85.89(6) . . ?
O1 Ti1 O3 85.32(6) . . ?
N3 Ti1 O3 175.63(8) . . ?
O2 Ti1 C30 86.48(8) . . ?
O1 Ti1 C30 86.60(7) . . ?
N3 Ti1 C30 91.10(8) . . ?
O3 Ti1 C30 84.54(7) . . ?
O2 Ti1 Cl1 94.45(5) . . ?
O1 Ti1 Cl1 90.84(5) . . ?
N3 Ti1 Cl1 99.57(7) . . ?
O3 Ti1 Cl1 84.78(4) . . ?
C30 Ti1 Cl1 169.19(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.044
_database_code_depnum_ccdc_archive 'CCDC 975125'
#######################################################################
#
#                 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_compound18

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C51 H70 Cl N3 O3 Zr'
_chemical_formula_sum            'C51 H70 Cl N3 O3 Zr'
_chemical_formula_weight         899.77
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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   P2(1)2(1)2(1)

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

_cell_length_a                   12.7285(15)
_cell_length_b                   15.0219(18)
_cell_length_c                   30.104(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5756.1(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    9994
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      26.84

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1912
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8531
_exptl_absorpt_correction_T_max  0.9653
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10419
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         25.25
_reflns_number_total             10419
_reflns_number_gt                9645
_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, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0414P)²+1.1045P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_number_reflns         10419
_refine_ls_number_parameters     571
_refine_ls_number_restraints     66
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0774
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.047 0.750 0.000 628 136 ' '
2 -0.094 0.250 0.500 628 136 ' '
_platon_squeeze_details          ?

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 0.25573(19) 0.22683(15) 0.30556(8) 0.0233(5) Uani 1 1 d . . .
C2 C 0.2583(2) 0.23495(17) 0.35238(8) 0.0259(5) Uani 1 1 d . . .
C3 C 0.1863(2) 0.30105(19) 0.37755(8) 0.0303(5) Uani 1 1 d . . .
C4 C 0.0694(2) 0.2803(2) 0.36983(9) 0.0375(7) Uani 1 1 d . . .
H4A H 0.0262 0.3223 0.3867 0.056 Uiso 1 1 calc R . .
H4B H 0.0543 0.2194 0.3797 0.056 Uiso 1 1 calc R . .
H4C H 0.0532 0.2858 0.3381 0.056 Uiso 1 1 calc R . .
C5 C 0.2098(2) 0.39513(19) 0.36227(10) 0.0399(7) Uani 1 1 d . . .
H5A H 0.1662 0.4372 0.3790 0.060 Uiso 1 1 calc R . .
H5B H 0.1941 0.4005 0.3305 0.060 Uiso 1 1 calc R . .
H5C H 0.2841 0.4085 0.3674 0.060 Uiso 1 1 calc R . .
C6 C 0.2025(2) 0.2971(2) 0.42821(8) 0.0420(7) Uani 1 1 d . . .
H6A H 0.2748 0.3143 0.4354 0.063 Uiso 1 1 calc R . .
H6B H 0.1895 0.2364 0.4387 0.063 Uiso 1 1 calc R . .
H6C H 0.1535 0.3382 0.4427 0.063 Uiso 1 1 calc R . .
C7 C 0.33419(19) 0.18632(18) 0.37517(8) 0.0287(6) Uani 1 1 d . . .
H7 H 0.3356 0.1909 0.4066 0.034 Uiso 1 1 calc R . .
C8 C 0.4078(2) 0.13161(17) 0.35499(8) 0.0294(5) Uani 1 1 d . . .
C9 C 0.4928(2) 0.0810(2) 0.38053(9) 0.0370(7) Uani 1 1 d . . .
C10 C 0.6019(2) 0.1156(2) 0.36692(10) 0.0449(7) Uani 1 1 d . . .
H10A H 0.6137 0.1033 0.3353 0.067 Uiso 1 1 calc R . .
H10B H 0.6559 0.0856 0.3846 0.067 Uiso 1 1 calc R . .
H10C H 0.6056 0.1799 0.3721 0.067 Uiso 1 1 calc R . .
C11 C 0.4849(3) -0.0179(2) 0.36964(12) 0.0493(8) Uani 1 1 d . . .
H11A H 0.4157 -0.0402 0.3785 0.074 Uiso 1 1 calc R . .
H11B H 0.5397 -0.0505 0.3857 0.074 Uiso 1 1 calc R . .
H11C H 0.4943 -0.0266 0.3376 0.074 Uiso 1 1 calc R . .
C12 C 0.4802(3) 0.0916(3) 0.43078(10) 0.0678(12) Uani 1 1 d . . .
H12A H 0.4888 0.1544 0.4388 0.102 Uiso 1 1 calc R . .
H12B H 0.5336 0.0559 0.4460 0.102 Uiso 1 1 calc R . .
H12C H 0.4101 0.0714 0.4397 0.102 Uiso 1 1 calc R . .
C13 C 0.4044(2) 0.12691(15) 0.30871(8) 0.0256(5) Uani 1 1 d . . .
H13 H 0.4540 0.0905 0.2937 0.031 Uiso 1 1 calc R . .
C14 C 0.33087(18) 0.17367(15) 0.28399(7) 0.0223(5) Uani 1 1 d . . .
C15 C 0.33881(18) 0.17355(15) 0.23389(7) 0.0228(5) Uani 1 1 d . . .
H15A H 0.3374 0.2360 0.2234 0.027 Uiso 1 1 calc R . .
H15B H 0.4078 0.1482 0.2255 0.027 Uiso 1 1 calc R . .
C16 C 0.28511(19) 0.04977(15) 0.18022(8) 0.0225(5) Uani 1 1 d . . .
H16 H 0.3295 0.0739 0.1556 0.027 Uiso 1 1 calc R . .
C17 C 0.34221(19) -0.02694(16) 0.20170(8) 0.0240(5) Uani 1 1 d . . .
C18 C 0.3137(2) -0.05737(16) 0.24390(8) 0.0273(6) Uani 1 1 d . . .
H18 H 0.2608 -0.0276 0.2605 0.033 Uiso 1 1 calc R . .
C19 C 0.3637(2) -0.13152(17) 0.26128(9) 0.0325(6) Uani 1 1 d . . .
H19 H 0.3457 -0.1512 0.2903 0.039 Uiso 1 1 calc R . .
C20 C 0.4386(2) -0.17727(17) 0.23775(9) 0.0336(6) Uani 1 1 d . . .
H20 H 0.4706 -0.2289 0.2500 0.040 Uiso 1 1 calc R . .
C21 C 0.4669(2) -0.1473(2) 0.19589(10) 0.0394(7) Uani 1 1 d . . .
H21 H 0.5190 -0.1781 0.1793 0.047 Uiso 1 1 calc R . .
C22 C 0.4192(2) -0.07221(18) 0.17822(9) 0.0333(6) Uani 1 1 d . . .
H22 H 0.4396 -0.0515 0.1497 0.040 Uiso 1 1 calc R . .
C23 C 0.17734(19) 0.02397(15) 0.16136(8) 0.0222(5) Uani 1 1 d . . .
H23 H 0.1471 -0.0249 0.1799 0.027 Uiso 1 1 calc R . .
C24 C 0.1813(2) -0.00664(18) 0.11355(8) 0.0272(6) Uani 1 1 d . . .
C25 C 0.1800(2) -0.0966(2) 0.10474(10) 0.0422(7) Uani 1 1 d . . .
H25 H 0.1714 -0.1377 0.1284 0.051 Uiso 1 1 calc R . .
C26 C 0.1911(3) -0.1278(3) 0.06125(13) 0.0599(10) Uani 1 1 d . . .
H26 H 0.1904 -0.1899 0.0554 0.072 Uiso 1 1 calc R . .
C27 C 0.2030(3) -0.0679(3) 0.02704(11) 0.0645(11) Uani 1 1 d . . .
H27 H 0.2108 -0.0887 -0.0026 0.077 Uiso 1 1 calc R . .
C28 C 0.2036(3) 0.0208(3) 0.03549(10) 0.0617(10) Uani 1 1 d . . .
H28 H 0.2118 0.0618 0.0117 0.074 Uiso 1 1 calc R . .
C29 C 0.1925(3) 0.0522(2) 0.07857(9) 0.0444(7) Uani 1 1 d . . .
H29 H 0.1926 0.1144 0.0841 0.053 Uiso 1 1 calc R . .
C30 C 0.16223(19) 0.15882(16) 0.20000(7) 0.0220(5) Uani 1 1 d . A .
C31 C 0.0036(2) 0.11002(16) 0.15893(8) 0.0235(5) Uani 1 1 d . . .
H31A H -0.0352 0.1245 0.1865 0.028 Uiso 1 1 calc R . .
H31B H -0.0188 0.0499 0.1494 0.028 Uiso 1 1 calc R . .
C32 C -0.02855(19) 0.17548(16) 0.12357(8) 0.0239(5) Uani 1 1 d . A .
C33 C -0.0639(2) 0.14440(18) 0.08247(8) 0.0323(6) Uani 1 1 d . . .
H33 H -0.0599 0.0825 0.0762 0.039 Uiso 1 1 calc R . .
C34 C -0.1044(2) 0.20097(19) 0.05077(8) 0.0370(6) Uani 1 1 d . A .
C35 C -0.1379(3) 0.1687(2) 0.00457(10) 0.0560(10) Uani 1 1 d D . .
C36 C -0.1447(8) 0.0671(6) 0.0026(4) 0.052(2) Uani 0.583(9) 1 d PDU A 1
H36A H -0.1546 0.0482 -0.0283 0.078 Uiso 0.583(9) 1 calc PR A 1
H36B H -0.2043 0.0468 0.0206 0.078 Uiso 0.583(9) 1 calc PR A 1
H36C H -0.0796 0.0413 0.0142 0.078 Uiso 0.583(9) 1 calc PR A 1
C37 C -0.2635(6) 0.1958(5) -0.0020(2) 0.066(2) Uani 0.583(9) 1 d PDU A 1
H37A H -0.2735 0.2586 0.0059 0.099 Uiso 0.583(9) 1 calc PR A 1
H37B H -0.3070 0.1585 0.0174 0.099 Uiso 0.583(9) 1 calc PR A 1
H37C H -0.2840 0.1864 -0.0330 0.099 Uiso 0.583(9) 1 calc PR A 1
C38 C -0.0769(8) 0.2056(7) -0.02968(19) 0.083(3) Uani 0.583(9) 1 d PDU A 1
H38A H -0.1187 0.2085 -0.0570 0.124 Uiso 0.583(9) 1 calc PR A 1
H38B H -0.0149 0.1683 -0.0347 0.124 Uiso 0.583(9) 1 calc PR A 1
H38C H -0.0547 0.2657 -0.0212 0.124 Uiso 0.583(9) 1 calc PR A 1
C39 C -0.1117(2) 0.29117(17) 0.06217(8) 0.0311(6) Uani 1 1 d . . .
H39 H -0.1411 0.3308 0.0410 0.037 Uiso 1 1 calc R A .
C40 C -0.07850(19) 0.32656(16) 0.10270(8) 0.0250(6) Uani 1 1 d . A .
C41 C -0.0942(2) 0.42613(16) 0.11292(7) 0.0284(5) Uani 1 1 d . . .
C42 C -0.1547(2) 0.47498(19) 0.07593(9) 0.0361(7) Uani 1 1 d . A .
H42A H -0.1664 0.5370 0.0847 0.054 Uiso 1 1 calc R . .
H42B H -0.2226 0.4457 0.0711 0.054 Uiso 1 1 calc R . .
H42C H -0.1137 0.4733 0.0484 0.054 Uiso 1 1 calc R . .
C43 C 0.0125(2) 0.47158(18) 0.11796(9) 0.0365(7) Uani 1 1 d . A .
H43A H 0.0532 0.4639 0.0906 0.055 Uiso 1 1 calc R . .
H43B H 0.0507 0.4448 0.1429 0.055 Uiso 1 1 calc R . .
H43C H 0.0021 0.5352 0.1236 0.055 Uiso 1 1 calc R . .
C44 C -0.1584(2) 0.43739(19) 0.15600(8) 0.0339(6) Uani 1 1 d . A .
H44A H -0.1204 0.4100 0.1808 0.051 Uiso 1 1 calc R . .
H44B H -0.2269 0.4084 0.1526 0.051 Uiso 1 1 calc R . .
H44C H -0.1686 0.5009 0.1620 0.051 Uiso 1 1 calc R . .
C45 C -0.03250(19) 0.26640(17) 0.13346(8) 0.0234(5) Uani 1 1 d . . .
C46 C -0.0194(2) 0.13521(17) 0.28588(8) 0.0292(6) Uani 1 1 d . . .
H46A H 0.0312 0.1439 0.3105 0.035 Uiso 1 1 calc R . .
H46B H 0.0055 0.0856 0.2669 0.035 Uiso 1 1 calc R . .
C47 C -0.1272(2) 0.1159(2) 0.30369(10) 0.0451(8) Uani 1 1 d . . .
H47A H -0.1384 0.1452 0.3328 0.054 Uiso 1 1 calc R . .
H47B H -0.1387 0.0510 0.3070 0.054 Uiso 1 1 calc R . .
C48 C -0.1982(2) 0.1546(2) 0.26859(12) 0.0515(8) Uani 1 1 d . . .
H48A H -0.2055 0.1137 0.2430 0.062 Uiso 1 1 calc R . .
H48B H -0.2687 0.1678 0.2808 0.062 Uiso 1 1 calc R . .
C49 C -0.1422(2) 0.23843(19) 0.25545(10) 0.0353(7) Uani 1 1 d . . .
H49A H -0.1594 0.2551 0.2245 0.042 Uiso 1 1 calc R . .
H49B H -0.1616 0.2882 0.2754 0.042 Uiso 1 1 calc R . .
C50 C 0.2441(2) 0.3573(2) 0.14665(9) 0.0427(7) Uani 1 1 d . . .
H50A H 0.2451 0.4173 0.1339 0.064 Uiso 1 1 calc R . .
H50B H 0.1905 0.3214 0.1317 0.064 Uiso 1 1 calc R . .
H50C H 0.3131 0.3294 0.1427 0.064 Uiso 1 1 calc R . .
C51 C 0.3014(2) 0.41212(18) 0.21725(10) 0.0359(6) Uani 1 1 d . . .
H51A H 0.3698 0.3843 0.2117 0.054 Uiso 1 1 calc R . .
H51B H 0.2866 0.4114 0.2492 0.054 Uiso 1 1 calc R . .
H51C H 0.3026 0.4738 0.2066 0.054 Uiso 1 1 calc R . .
C36' C -0.1840(11) 0.0787(10) 0.0044(6) 0.060(4) Uani 0.417(9) 1 d PDU A 2
H36D H -0.1847 0.0554 -0.0260 0.091 Uiso 0.417(9) 1 calc PR A 2
H36E H -0.2561 0.0815 0.0158 0.091 Uiso 0.417(9) 1 calc PR A 2
H36F H -0.1420 0.0394 0.0234 0.091 Uiso 0.417(9) 1 calc PR A 2
C37' C -0.1905(10) 0.2386(7) -0.0229(3) 0.071(4) Uani 0.417(9) 1 d PDU A 2
H37D H -0.1441 0.2904 -0.0256 0.106 Uiso 0.417(9) 1 calc PR A 2
H37E H -0.2563 0.2566 -0.0086 0.106 Uiso 0.417(9) 1 calc PR A 2
H37F H -0.2055 0.2147 -0.0525 0.106 Uiso 0.417(9) 1 calc PR A 2
C38' C -0.0190(7) 0.1587(7) -0.0218(3) 0.054(3) Uani 0.417(9) 1 d PDU A 2
H38D H -0.0289 0.1285 -0.0503 0.081 Uiso 0.417(9) 1 calc PR A 2
H38E H 0.0290 0.1240 -0.0032 0.081 Uiso 0.417(9) 1 calc PR A 2
H38F H 0.0106 0.2181 -0.0269 0.081 Uiso 0.417(9) 1 calc PR A 2
Cl1 Cl 0.00992(5) 0.42713(4) 0.264302(19) 0.02974(14) Uani 1 1 d . A .
N1 N 0.25556(16) 0.12344(13) 0.21003(6) 0.0220(4) Uani 1 1 d . . .
N2 N 0.11679(15) 0.10677(12) 0.16948(6) 0.0219(4) Uani 1 1 d . . .
N3 N 0.21999(16) 0.36283(14) 0.19378(7) 0.0250(5) Uani 1 1 d . A .
O1 O 0.18503(12) 0.27110(10) 0.28056(5) 0.0217(3) Uani 1 1 d . A .
O2 O 0.00683(12) 0.29478(11) 0.17248(5) 0.0220(3) Uani 1 1 d . A .
O3 O -0.03058(12) 0.21682(11) 0.25985(5) 0.0258(4) Uani 1 1 d . A .
Zr1 Zr 0.100027(17) 0.300189(14) 0.226370(7) 0.01972(6) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.349(3) . ?
C1 C14 1.405(3) . ?
C1 C2 1.415(3) . ?
C2 C7 1.392(3) . ?
C2 C3 1.549(4) . ?
C3 C5 1.516(4) . ?
C3 C4 1.538(4) . ?
C3 C6 1.540(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.387(4) . ?
C7 H7 0.9500 . ?
C8 C13 1.396(3) . ?
C8 C9 1.529(4) . ?
C9 C11 1.525(4) . ?
C9 C12 1.529(4) . ?
C9 C10 1.539(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.387(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.512(3) . ?
C15 N1 1.485(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N1 1.474(3) . ?
C16 C17 1.508(3) . ?
C16 C23 1.535(3) . ?
C16 H16 1.0000 . ?
C17 C22 1.387(4) . ?
C17 C18 1.398(3) . ?
C18 C19 1.385(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.372(4) . ?
C19 H19 0.9500 . ?
C20 C21 1.386(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.387(4) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 N2 1.484(3) . ?
C23 C24 1.512(3) . ?
C23 H23 1.0000 . ?
C24 C25 1.377(4) . ?
C24 C29 1.382(4) . ?
C25 C26 1.398(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.376(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.357(5) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(4) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 N1 1.336(3) . ?
C30 N2 1.338(3) . ?
C30 Zr1 2.401(2) . ?
C31 N2 1.476(3) . ?
C31 C32 1.506(3) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.397(3) . ?
C32 C45 1.399(4) . ?
C33 C34 1.378(4) . ?
C33 H33 0.9500 . ?
C34 C39 1.401(4) . ?
C34 C35 1.534(4) . ?
C35 C38 1.405(7) . ?
C35 C36' 1.473(13) . ?
C35 C37' 1.496(9) . ?
C35 C36 1.529(10) . ?
C35 C37 1.661(7) . ?
C35 C38' 1.715(9) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.397(3) . ?
C39 H39 0.9500 . ?
C40 C45 1.420(3) . ?
C40 C41 1.540(3) . ?
C41 C43 1.528(4) . ?
C41 C42 1.540(3) . ?
C41 C44 1.542(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 O2 1.346(3) . ?
C46 O3 1.462(3) . ?
C46 C47 1.501(4) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.507(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.500(4) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 O3 1.463(3) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 N3 1.454(3) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 N3 1.457(3) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C36' H36D 0.9800 . ?
C36' H36E 0.9800 . ?
C36' H36F 0.9800 . ?
C37' H37D 0.9800 . ?
C37' H37E 0.9800 . ?
C37' H37F 0.9800 . ?
C38' H38D 0.9800 . ?
C38' H38E 0.9800 . ?
C38' H38F 0.9800 . ?
Cl1 Zr1 2.5012(6) . ?
N3 Zr1 2.044(2) . ?
O1 Zr1 2.0056(15) . ?
O2 Zr1 2.0114(14) . ?
O3 Zr1 2.3125(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C14 118.4(2) . . ?
O1 C1 C2 121.9(2) . . ?
C14 C1 C2 119.6(2) . . ?
C7 C2 C1 117.5(2) . . ?
C7 C2 C3 120.4(2) . . ?
C1 C2 C3 121.9(2) . . ?
C5 C3 C4 109.5(2) . . ?
C5 C3 C6 108.0(2) . . ?
C4 C3 C6 105.7(2) . . ?
C5 C3 C2 109.5(2) . . ?
C4 C3 C2 111.6(2) . . ?
C6 C3 C2 112.4(2) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C2 124.4(2) . . ?
C8 C7 H7 117.8 . . ?
C2 C7 H7 117.8 . . ?
C7 C8 C13 116.5(2) . . ?
C7 C8 C9 123.5(2) . . ?
C13 C8 C9 119.9(2) . . ?
C11 C9 C8 109.2(2) . . ?
C11 C9 C12 107.9(3) . . ?
C8 C9 C12 111.8(2) . . ?
C11 C9 C10 109.3(2) . . ?
C8 C9 C10 109.7(2) . . ?
C12 C9 C10 108.8(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C8 122.1(2) . . ?
C14 C13 H13 119.0 . . ?
C8 C13 H13 119.0 . . ?
C13 C14 C1 119.9(2) . . ?
C13 C14 C15 119.3(2) . . ?
C1 C14 C15 120.5(2) . . ?
N1 C15 C14 115.81(19) . . ?
N1 C15 H15A 108.3 . . ?
C14 C15 H15A 108.3 . . ?
N1 C15 H15B 108.3 . . ?
C14 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
N1 C16 C17 115.8(2) . . ?
N1 C16 C23 100.77(18) . . ?
C17 C16 C23 113.36(19) . . ?
N1 C16 H16 108.8 . . ?
C17 C16 H16 108.8 . . ?
C23 C16 H16 108.8 . . ?
C22 C17 C18 119.1(2) . . ?
C22 C17 C16 119.8(2) . . ?
C18 C17 C16 121.0(2) . . ?
C19 C18 C17 119.1(2) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C20 C19 C18 121.8(3) . . ?
C20 C19 H19 119.1 . . ?
C18 C19 H19 119.1 . . ?
C19 C20 C21 119.2(2) . . ?
C19 C20 H20 120.4 . . ?
C21 C20 H20 120.4 . . ?
C20 C21 C22 119.9(3) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C17 C22 C21 120.8(3) . . ?
C17 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
N2 C23 C24 115.4(2) . . ?
N2 C23 C16 101.05(18) . . ?
C24 C23 C16 113.5(2) . . ?
N2 C23 H23 108.8 . . ?
C24 C23 H23 108.8 . . ?
C16 C23 H23 108.8 . . ?
C25 C24 C29 118.8(3) . . ?
C25 C24 C23 118.8(2) . . ?
C29 C24 C23 122.3(2) . . ?
C24 C25 C26 120.5(3) . . ?
C24 C25 H25 119.7 . . ?
C26 C25 H25 119.7 . . ?
C27 C26 C25 119.5(3) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 120.6(3) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C24 C29 C28 120.4(3) . . ?
C24 C29 H29 119.8 . . ?
C28 C29 H29 119.8 . . ?
N1 C30 N2 107.9(2) . . ?
N1 C30 Zr1 124.77(16) . . ?
N2 C30 Zr1 126.97(17) . . ?
N2 C31 C32 116.1(2) . . ?
N2 C31 H31A 108.3 . . ?
C32 C31 H31A 108.3 . . ?
N2 C31 H31B 108.3 . . ?
C32 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
C33 C32 C45 120.2(2) . . ?
C33 C32 C31 119.7(2) . . ?
C45 C32 C31 119.8(2) . . ?
C34 C33 C32 121.9(2) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C33 C34 C39 116.9(2) . . ?
C33 C34 C35 122.5(3) . . ?
C39 C34 C35 120.6(2) . . ?
C38 C35 C36' 125.5(8) . . ?
C38 C35 C37' 64.1(6) . . ?
C36' C35 C37' 117.7(8) . . ?
C38 C35 C36 113.4(6) . . ?
C36' C35 C36 20.3(6) . . ?
C37' C35 C36 130.8(6) . . ?
C38 C35 C34 112.8(4) . . ?
C36' C35 C34 113.8(8) . . ?
C37' C35 C34 113.8(4) . . ?
C36 C35 C34 111.5(5) . . ?
C38 C35 C37 110.3(5) . . ?
C36' C35 C37 80.9(6) . . ?
C37' C35 C37 48.0(5) . . ?
C36 C35 C37 100.7(5) . . ?
C34 C35 C37 107.3(3) . . ?
C38 C35 C38' 37.6(4) . . ?
C36' C35 C38' 105.7(7) . . ?
C37' C35 C38' 101.5(6) . . ?
C36 C35 C38' 86.9(5) . . ?
C34 C35 C38' 101.6(4) . . ?
C37 C35 C38' 144.6(5) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C34 124.2(2) . . ?
C40 C39 H39 117.9 . . ?
C34 C39 H39 117.9 . . ?
C39 C40 C45 116.9(2) . . ?
C39 C40 C41 120.3(2) . . ?
C45 C40 C41 122.8(2) . . ?
C43 C41 C40 109.8(2) . . ?
C43 C41 C42 107.7(2) . . ?
C40 C41 C42 112.5(2) . . ?
C43 C41 C44 109.8(2) . . ?
C40 C41 C44 110.1(2) . . ?
C42 C41 C44 106.9(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O2 C45 C32 118.8(2) . . ?
O2 C45 C40 121.4(2) . . ?
C32 C45 C40 119.8(2) . . ?
O3 C46 C47 105.4(2) . . ?
O3 C46 H46A 110.7 . . ?
C47 C46 H46A 110.7 . . ?
O3 C46 H46B 110.7 . . ?
C47 C46 H46B 110.7 . . ?
H46A C46 H46B 108.8 . . ?
C46 C47 C48 102.9(2) . . ?
C46 C47 H47A 111.2 . . ?
C48 C47 H47A 111.2 . . ?
C46 C47 H47B 111.2 . . ?
C48 C47 H47B 111.2 . . ?
H47A C47 H47B 109.1 . . ?
C49 C48 C47 103.0(2) . . ?
C49 C48 H48A 111.2 . . ?
C47 C48 H48A 111.2 . . ?
C49 C48 H48B 111.2 . . ?
C47 C48 H48B 111.2 . . ?
H48A C48 H48B 109.1 . . ?
O3 C49 C48 104.6(2) . . ?
O3 C49 H49A 110.8 . . ?
C48 C49 H49A 110.8 . . ?
O3 C49 H49B 110.8 . . ?
C48 C49 H49B 110.8 . . ?
H49A C49 H49B 108.9 . . ?
N3 C50 H50A 109.5 . . ?
N3 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
N3 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N3 C51 H51A 109.5 . . ?
N3 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
N3 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C35 C36' H36D 109.5 . . ?
C35 C36' H36E 109.5 . . ?
H36D C36' H36E 109.5 . . ?
C35 C36' H36F 109.5 . . ?
H36D C36' H36F 109.5 . . ?
H36E C36' H36F 109.5 . . ?
C35 C37' H37D 109.5 . . ?
C35 C37' H37E 109.5 . . ?
H37D C37' H37E 109.5 . . ?
C35 C37' H37F 109.5 . . ?
H37D C37' H37F 109.5 . . ?
H37E C37' H37F 109.5 . . ?
C35 C38' H38D 109.5 . . ?
C35 C38' H38E 109.5 . . ?
H38D C38' H38E 109.5 . . ?
C35 C38' H38F 109.5 . . ?
H38D C38' H38F 109.5 . . ?
H38E C38' H38F 109.5 . . ?
C30 N1 C16 112.84(19) . . ?
C30 N1 C15 122.82(19) . . ?
C16 N1 C15 119.54(19) . . ?
C30 N2 C31 123.40(19) . . ?
C30 N2 C23 112.25(19) . . ?
C31 N2 C23 119.95(18) . . ?
C50 N3 C51 110.6(2) . . ?
C50 N3 Zr1 126.85(18) . . ?
C51 N3 Zr1 122.19(16) . . ?
C1 O1 Zr1 157.13(15) . . ?
C45 O2 Zr1 159.37(15) . . ?
C46 O3 C49 109.21(18) . . ?
C46 O3 Zr1 128.15(14) . . ?
C49 O3 Zr1 122.57(14) . . ?
O1 Zr1 O2 164.88(6) . . ?
O1 Zr1 N3 95.03(7) . . ?
O2 Zr1 N3 94.13(7) . . ?
O1 Zr1 O3 85.15(6) . . ?
O2 Zr1 O3 84.59(6) . . ?
N3 Zr1 O3 174.46(7) . . ?
O1 Zr1 C30 84.17(7) . . ?
O2 Zr1 C30 83.81(7) . . ?
N3 Zr1 C30 90.12(8) . . ?
O3 Zr1 C30 84.39(7) . . ?
O1 Zr1 Cl1 92.41(5) . . ?
O2 Zr1 Cl1 97.39(5) . . ?
N3 Zr1 Cl1 102.16(6) . . ?
O3 Zr1 Cl1 83.35(4) . . ?
C30 Zr1 Cl1 167.51(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.045
_database_code_depnum_ccdc_archive 'CCDC 975126'
#######################################################################
#
#                 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_compound19

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C59 H86 Cl Hf N3 O5'
_chemical_formula_sum            'C59 H86 Cl Hf N3 O5'
_chemical_formula_weight         1131.25
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   12.7812(6)
_cell_length_b                   14.9521(8)
_cell_length_c                   30.0898(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5750.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    9933
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            xolorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2360
_exptl_absorpt_coefficient_mu    1.908
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4806
_exptl_absorpt_correction_T_max  0.6368
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28673
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         25.25
_reflns_number_total             10378
_reflns_number_gt                9927
_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, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0040P)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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(4)
_refine_ls_number_reflns         10378
_refine_ls_number_parameters     666
_refine_ls_number_restraints     243
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0482
_refine_ls_wR_factor_gt          0.0477
_refine_ls_goodness_of_fit_ref   1.011
_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
C1 C 0.2456(2) 0.7276(2) 0.69416(11) 0.0173(7) Uani 1 1 d . . .
C2 C 0.2428(2) 0.7364(2) 0.64746(11) 0.0179(7) Uani 1 1 d . . .
C3 C 0.3147(2) 0.8023(3) 0.62218(10) 0.0220(7) Uani 1 1 d . . .
C4 C 0.2895(3) 0.8979(2) 0.63773(12) 0.0301(9) Uani 1 1 d . . .
H4A H 0.3345 0.9404 0.6220 0.045 Uiso 1 1 calc R . .
H4B H 0.3020 0.9027 0.6698 0.045 Uiso 1 1 calc R . .
H4C H 0.2160 0.9114 0.6314 0.045 Uiso 1 1 calc R . .
C5 C 0.4318(2) 0.7825(3) 0.63021(11) 0.0287(9) Uani 1 1 d . . .
H5A H 0.4744 0.8250 0.6133 0.043 Uiso 1 1 calc R . .
H5B H 0.4477 0.7215 0.6205 0.043 Uiso 1 1 calc R . .
H5C H 0.4475 0.7886 0.6619 0.043 Uiso 1 1 calc R . .
C6 C 0.2976(3) 0.7980(3) 0.57164(11) 0.0327(8) Uani 1 1 d . . .
H6A H 0.2239 0.8100 0.5649 0.049 Uiso 1 1 calc R . .
H6B H 0.3164 0.7383 0.5608 0.049 Uiso 1 1 calc R . .
H6C H 0.3416 0.8429 0.5570 0.049 Uiso 1 1 calc R . .
C7 C 0.1669(2) 0.6873(2) 0.62445(11) 0.0202(7) Uani 1 1 d . . .
H7 H 0.1659 0.6914 0.5930 0.024 Uiso 1 1 calc R . .
C8 C 0.0929(3) 0.6327(2) 0.64475(10) 0.0210(7) Uani 1 1 d . . .
C9 C 0.0087(3) 0.5820(2) 0.61913(12) 0.0267(8) Uani 1 1 d . . .
C10 C 0.0211(4) 0.5918(4) 0.56894(13) 0.0553(14) Uani 1 1 d . . .
H10A H 0.0076 0.6540 0.5604 0.083 Uiso 1 1 calc R . .
H10B H -0.0289 0.5525 0.5538 0.083 Uiso 1 1 calc R . .
H10C H 0.0925 0.5754 0.5604 0.083 Uiso 1 1 calc R . .
C11 C 0.0154(3) 0.4814(2) 0.63069(14) 0.0356(10) Uani 1 1 d . . .
H11A H 0.0835 0.4579 0.6213 0.053 Uiso 1 1 calc R . .
H11B H -0.0405 0.4490 0.6153 0.053 Uiso 1 1 calc R . .
H11C H 0.0076 0.4735 0.6629 0.053 Uiso 1 1 calc R . .
C12 C -0.0999(3) 0.6180(2) 0.63274(12) 0.0345(8) Uani 1 1 d . . .
H12A H -0.1095 0.6105 0.6648 0.052 Uiso 1 1 calc R . .
H12B H -0.1544 0.5847 0.6169 0.052 Uiso 1 1 calc R . .
H12C H -0.1048 0.6816 0.6251 0.052 Uiso 1 1 calc R . .
C13 C 0.0959(3) 0.6277(2) 0.69108(10) 0.0188(7) Uani 1 1 d . . .
H13 H 0.0458 0.5920 0.7062 0.023 Uiso 1 1 calc R . .
C14 C 0.1705(2) 0.67406(19) 0.71553(10) 0.0149(7) Uani 1 1 d . . .
C15 C 0.1633(2) 0.6742(2) 0.76580(10) 0.0167(7) Uani 1 1 d . A .
H15A H 0.1653 0.7371 0.7762 0.020 Uiso 1 1 calc R . .
H15B H 0.0945 0.6492 0.7744 0.020 Uiso 1 1 calc R . .
C16 C 0.2159(2) 0.54992(19) 0.81955(11) 0.0167(7) Uani 1 1 d . A .
H16 H 0.1720 0.5746 0.8442 0.020 Uiso 1 1 calc R . .
C17 C 0.1580(2) 0.4734(2) 0.79812(12) 0.0190(8) Uani 1 1 d . . .
C18 C 0.1857(3) 0.4420(2) 0.75598(11) 0.0221(8) Uani 1 1 d . . .
H18 H 0.2385 0.4719 0.7394 0.026 Uiso 1 1 calc R . .
C19 C 0.1364(2) 0.3673(2) 0.73811(12) 0.0262(8) Uani 1 1 d . . .
H19 H 0.1549 0.3468 0.7093 0.031 Uiso 1 1 calc R . .
C20 C 0.0601(2) 0.3227(2) 0.76231(13) 0.0286(9) Uani 1 1 d . . .
H20 H 0.0271 0.2711 0.7503 0.034 Uiso 1 1 calc R . .
C21 C 0.0326(3) 0.3533(2) 0.80366(13) 0.0321(9) Uani 1 1 d . . .
H21 H -0.0202 0.3233 0.8202 0.039 Uiso 1 1 calc R . .
C22 C 0.0818(2) 0.4286(2) 0.82154(12) 0.0270(8) Uani 1 1 d . . .
H22 H 0.0625 0.4490 0.8503 0.032 Uiso 1 1 calc R . .
C23 C 0.3231(2) 0.5233(2) 0.83853(11) 0.0161(7) Uani 1 1 d . A .
H23 H 0.3530 0.4744 0.8198 0.019 Uiso 1 1 calc R . .
C24 C 0.3189(2) 0.4923(2) 0.88576(12) 0.0224(8) Uani 1 1 d . . .
C25 C 0.3179(3) 0.4002(3) 0.89409(13) 0.0320(9) Uani 1 1 d . . .
H25 H 0.3245 0.3592 0.8701 0.038 Uiso 1 1 calc R . .
C26 C 0.3073(3) 0.3688(3) 0.93709(16) 0.0491(12) Uani 1 1 d . . .
H26 H 0.3078 0.3063 0.9426 0.059 Uiso 1 1 calc R . .
C27 C 0.2959(3) 0.4282(4) 0.97220(15) 0.0529(13) Uani 1 1 d . . .
H27 H 0.2869 0.4064 1.0016 0.063 Uiso 1 1 calc R . .
C28 C 0.2978(3) 0.5186(3) 0.96416(14) 0.0481(12) Uani 1 1 d . . .
H28 H 0.2921 0.5595 0.9882 0.058 Uiso 1 1 calc R . .
C29 C 0.3079(3) 0.5504(3) 0.92107(12) 0.0339(9) Uani 1 1 d . . .
H29 H 0.3072 0.6131 0.9158 0.041 Uiso 1 1 calc R . .
C30 C 0.3391(2) 0.6593(2) 0.79969(11) 0.0172(7) Uani 1 1 d . A .
C31 C 0.4963(2) 0.6093(2) 0.84112(11) 0.0189(7) Uani 1 1 d . A .
H31A H 0.5354 0.6232 0.8136 0.023 Uiso 1 1 calc R . .
H31B H 0.5181 0.5488 0.8509 0.023 Uiso 1 1 calc R . .
C32 C 0.5282(2) 0.6757(2) 0.87651(11) 0.0181(7) Uani 1 1 d . A .
C33 C 0.5627(2) 0.6448(2) 0.91757(12) 0.0245(8) Uani 1 1 d . . .
H33 H 0.5588 0.5826 0.9239 0.029 Uiso 1 1 calc R . .
C34 C 0.6025(3) 0.7021(2) 0.94938(10) 0.0290(7) Uani 1 1 d . A .
C35 C 0.6340(3) 0.6688(3) 0.99582(13) 0.0430(11) Uani 1 1 d DU . .
C39 C 0.6116(2) 0.7917(2) 0.93779(10) 0.0227(7) Uani 1 1 d U . .
H39 H 0.6419 0.8314 0.9588 0.027 Uiso 1 1 calc R A .
C40 C 0.5787(2) 0.8273(2) 0.89710(10) 0.0185(7) Uani 1 1 d U A .
C41 C 0.5950(3) 0.9271(2) 0.88665(10) 0.0223(7) Uani 1 1 d U . .
C42 C 0.6548(3) 0.9756(2) 0.92371(12) 0.0296(9) Uani 1 1 d U A .
H42A H 0.6639 1.0386 0.9156 0.044 Uiso 1 1 calc R . .
H42B H 0.7235 0.9477 0.9277 0.044 Uiso 1 1 calc R . .
H42C H 0.6151 0.9715 0.9515 0.044 Uiso 1 1 calc R . .
C43 C 0.6589(3) 0.9382(3) 0.84381(12) 0.0275(9) Uani 1 1 d U A .
H43A H 0.6212 0.9108 0.8190 0.041 Uiso 1 1 calc R . .
H43B H 0.7271 0.9090 0.8473 0.041 Uiso 1 1 calc R . .
H43C H 0.6693 1.0020 0.8378 0.041 Uiso 1 1 calc R . .
C44 C 0.4887(3) 0.9736(2) 0.88151(13) 0.0312(9) Uani 1 1 d U A .
H44A H 0.4525 0.9496 0.8554 0.047 Uiso 1 1 calc R . .
H44B H 0.4994 1.0380 0.8778 0.047 Uiso 1 1 calc R . .
H44C H 0.4462 0.9628 0.9081 0.047 Uiso 1 1 calc R . .
C45 C 0.5326(2) 0.7670(2) 0.86628(11) 0.0178(7) Uani 1 1 d U . .
C46 C 0.1995(2) 0.9136(2) 0.78289(12) 0.0266(8) Uani 1 1 d . . .
H46A H 0.1314 0.8853 0.7880 0.040 Uiso 1 1 calc R . .
H46B H 0.2146 0.9143 0.7510 0.040 Uiso 1 1 calc R . .
H46C H 0.1979 0.9751 0.7942 0.040 Uiso 1 1 calc R . .
C47 C 0.2568(3) 0.8574(3) 0.85321(12) 0.0314(9) Uani 1 1 d . . .
H47A H 0.2520 0.9178 0.8657 0.047 Uiso 1 1 calc R . .
H47B H 0.3123 0.8242 0.8685 0.047 Uiso 1 1 calc R . .
H47C H 0.1900 0.8264 0.8573 0.047 Uiso 1 1 calc R . .
C48 C 0.6402(2) 0.7400(2) 0.74482(13) 0.0264(8) Uani 1 1 d U . .
H48A H 0.6577 0.7572 0.7757 0.032 Uiso 1 1 calc R . .
H48B H 0.6588 0.7899 0.7247 0.032 Uiso 1 1 calc R . .
C49 C 0.6963(3) 0.6555(3) 0.73169(15) 0.0410(10) Uani 1 1 d U . .
H49A H 0.7026 0.6140 0.7572 0.049 Uiso 1 1 calc R . .
H49B H 0.7671 0.6687 0.7200 0.049 Uiso 1 1 calc R . .
C50 C 0.6266(2) 0.6169(3) 0.69583(13) 0.0351(10) Uani 1 1 d U . .
H50A H 0.6383 0.5519 0.6922 0.042 Uiso 1 1 calc R . .
H50B H 0.6377 0.6472 0.6670 0.042 Uiso 1 1 calc R . .
C51 C 0.5186(3) 0.6361(2) 0.71427(11) 0.0223(8) Uani 1 1 d U . .
H51A H 0.4678 0.6454 0.6898 0.027 Uiso 1 1 calc R . .
H51B H 0.4941 0.5859 0.7330 0.027 Uiso 1 1 calc R . .
C52 C 0.8818(4) 0.6063(4) 0.8288(2) 0.0829(19) Uani 1 1 d U . .
H52A H 0.8739 0.5408 0.8324 0.099 Uiso 1 1 calc R . .
H52B H 0.8702 0.6216 0.7972 0.099 Uiso 1 1 calc R . .
C53 C 0.8060(4) 0.6533(5) 0.8569(2) 0.098(2) Uani 1 1 d U . .
H53A H 0.7668 0.6102 0.8756 0.117 Uiso 1 1 calc R . .
H53B H 0.7555 0.6868 0.8384 0.117 Uiso 1 1 calc R . .
C54 C 0.8672(4) 0.7153(5) 0.8851(2) 0.094(2) Uani 1 1 d U . .
H54A H 0.8423 0.7776 0.8816 0.113 Uiso 1 1 calc R . .
H54B H 0.8626 0.6982 0.9168 0.113 Uiso 1 1 calc R . .
C55 C 0.9700(4) 0.7057(4) 0.8690(2) 0.094(2) Uani 1 1 d U . .
H55A H 0.9903 0.7601 0.8524 0.113 Uiso 1 1 calc R . .
H55B H 1.0188 0.6989 0.8944 0.113 Uiso 1 1 calc R . .
C56 C 0.4868(8) 0.1677(6) 0.0170(3) 0.140(3) Uani 1 1 d U . .
H56A H 0.4455 0.2234 0.0199 0.168 Uiso 1 1 calc R . .
H56B H 0.5530 0.1820 0.0015 0.168 Uiso 1 1 calc R . .
C57 C 0.4330(10) 0.1072(9) -0.0062(3) 0.172(4) Uani 1 1 d U . .
H57A H 0.4655 0.1000 -0.0358 0.207 Uiso 1 1 calc R . .
H57B H 0.3605 0.1289 -0.0106 0.207 Uiso 1 1 calc R . .
C58 C 0.4304(8) 0.0277(8) 0.0144(4) 0.169(5) Uani 1 1 d U . .
H58A H 0.4627 -0.0185 -0.0047 0.203 Uiso 1 1 calc R . .
H58B H 0.3570 0.0101 0.0202 0.203 Uiso 1 1 calc R . .
C59 C 0.4855(8) 0.0337(7) 0.0548(4) 0.165(4) Uani 1 1 d U . .
H59A H 0.5509 -0.0015 0.0532 0.198 Uiso 1 1 calc R . .
H59B H 0.4423 0.0102 0.0795 0.198 Uiso 1 1 calc R . .
C36A C 0.6439(8) 0.5666(6) 0.9969(4) 0.041(2) Uani 0.50 1 d PDU A 1
H36A H 0.6741 0.5481 1.0254 0.061 Uiso 0.50 1 calc PR A 1
H36B H 0.6894 0.5468 0.9726 0.061 Uiso 0.50 1 calc PR A 1
H36C H 0.5745 0.5396 0.9935 0.061 Uiso 0.50 1 calc PR A 1
C37A C 0.5745(9) 0.7064(8) 1.0308(3) 0.071(3) Uani 0.50 1 d PDU A 1
H37A H 0.5013 0.6881 1.0278 0.107 Uiso 0.50 1 calc PR A 1
H37B H 0.5792 0.7718 1.0295 0.107 Uiso 0.50 1 calc PR A 1
H37C H 0.6019 0.6854 1.0594 0.107 Uiso 0.50 1 calc PR A 1
C38A C 0.7562(6) 0.6966(7) 1.0045(3) 0.049(2) Uani 0.50 1 d PDU A 1
H38A H 0.7650 0.7609 0.9993 0.074 Uiso 0.50 1 calc PR A 1
H38B H 0.8014 0.6632 0.9840 0.074 Uiso 0.50 1 calc PR A 1
H38C H 0.7754 0.6824 1.0352 0.074 Uiso 0.50 1 calc PR A 1
C36B C 0.6853(8) 0.5817(7) 0.9955(5) 0.053(3) Uani 0.50 1 d PDU A 2
H36D H 0.6943 0.5606 1.0261 0.080 Uiso 0.50 1 calc PR A 2
H36E H 0.7540 0.5870 0.9812 0.080 Uiso 0.50 1 calc PR A 2
H36F H 0.6422 0.5389 0.9789 0.080 Uiso 0.50 1 calc PR A 2
C37B C 0.5235(6) 0.6597(6) 1.0227(3) 0.043(2) Uani 0.50 1 d PDU A 2
H37D H 0.5375 0.6427 1.0536 0.065 Uiso 0.50 1 calc PR A 2
H37E H 0.4801 0.6137 1.0086 0.065 Uiso 0.50 1 calc PR A 2
H37F H 0.4866 0.7171 1.0221 0.065 Uiso 0.50 1 calc PR A 2
C38B C 0.6891(8) 0.7399(6) 1.0234(3) 0.054(2) Uani 0.50 1 d PDU A 2
H38D H 0.6423 0.7910 1.0277 0.081 Uiso 0.50 1 calc PR A 2
H38E H 0.7525 0.7596 1.0079 0.081 Uiso 0.50 1 calc PR A 2
H38F H 0.7081 0.7148 1.0524 0.081 Uiso 0.50 1 calc PR A 2
Cl1 Cl 0.48844(6) 0.92649(5) 0.73647(3) 0.02239(19) Uani 1 1 d . A .
Hf1 Hf 0.400049(9) 0.799631(8) 0.773841(4) 0.01427(4) Uani 1 1 d . . .
N1 N 0.24523(19) 0.62409(16) 0.78929(8) 0.0161(6) Uani 1 1 d . . .
N2 N 0.38373(18) 0.60665(16) 0.83042(8) 0.0150(6) Uani 1 1 d . . .
N3 N 0.2809(2) 0.86307(18) 0.80614(9) 0.0211(6) Uani 1 1 d . A .
O1 O 0.31637(15) 0.77156(13) 0.71932(7) 0.0165(5) Uani 1 1 d . A .
O2 O 0.49372(15) 0.79542(15) 0.82714(7) 0.0163(4) Uani 1 1 d . A .
O3 O 0.52951(15) 0.71731(13) 0.74077(7) 0.0187(5) Uani 1 1 d . A .
O4 O 0.9778(3) 0.6320(3) 0.84155(16) 0.1009(17) Uani 1 1 d . . .
O5 O 0.5095(5) 0.1299(6) 0.0621(2) 0.179(3) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.350(3) . ?
C1 C14 1.406(4) . ?
C1 C2 1.412(4) . ?
C2 C7 1.400(4) . ?
C2 C3 1.547(4) . ?
C3 C4 1.537(5) . ?
C3 C6 1.538(4) . ?
C3 C5 1.544(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.391(4) . ?
C7 H7 0.9500 . ?
C8 C13 1.397(4) . ?
C8 C9 1.525(4) . ?
C9 C10 1.526(5) . ?
C9 C12 1.544(5) . ?
C9 C11 1.547(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.389(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.516(4) . ?
C15 N1 1.469(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N1 1.483(4) . ?
C16 C17 1.507(4) . ?
C16 C23 1.536(4) . ?
C16 H16 1.0000 . ?
C17 C22 1.376(4) . ?
C17 C18 1.398(4) . ?
C18 C19 1.391(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.388(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.372(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.397(5) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 N2 1.487(4) . ?
C23 C24 1.496(4) . ?
C23 H23 1.0000 . ?
C24 C29 1.380(5) . ?
C24 C25 1.399(5) . ?
C25 C26 1.383(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.374(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.387(5) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 N2 1.341(4) . ?
C30 N1 1.347(4) . ?
C30 Hf1 2.370(3) . ?
C31 N2 1.475(4) . ?
C31 C32 1.513(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.391(5) . ?
C32 C45 1.400(5) . ?
C33 C34 1.381(5) . ?
C33 H33 0.9500 . ?
C34 C39 1.390(5) . ?
C34 C35 1.537(5) . ?
C35 C37A 1.415(9) . ?
C35 C36B 1.459(10) . ?
C35 C38B 1.521(8) . ?
C35 C36A 1.534(9) . ?
C35 C37B 1.633(8) . ?
C35 C38A 1.636(8) . ?
C39 C40 1.399(4) . ?
C39 H39 0.9500 . ?
C40 C45 1.422(4) . ?
C40 C41 1.538(4) . ?
C41 C44 1.534(5) . ?
C41 C42 1.534(4) . ?
C41 C43 1.536(5) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 O2 1.347(4) . ?
C46 N3 1.464(4) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 N3 1.452(4) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 O3 1.460(4) . ?
C48 C49 1.505(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 C50 1.514(5) . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
C50 C51 1.515(5) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 O3 1.459(4) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 O4 1.342(6) . ?
C52 C53 1.464(7) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.481(8) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.408(7) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 O4 1.382(6) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.333(12) . ?
C56 O5 1.500(9) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C58 1.342(13) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.406(13) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 O5 1.488(11) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C36A H36A 0.9800 . ?
C36A H36B 0.9800 . ?
C36A H36C 0.9800 . ?
C37A H37A 0.9800 . ?
C37A H37B 0.9800 . ?
C37A H37C 0.9800 . ?
C38A H38A 0.9800 . ?
C38A H38B 0.9800 . ?
C38A H38C 0.9800 . ?
C36B H36D 0.9800 . ?
C36B H36E 0.9800 . ?
C36B H36F 0.9800 . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
Cl1 Hf1 2.4777(7) . ?
Hf1 O2 2.0024(19) . ?
Hf1 O1 2.003(2) . ?
Hf1 N3 2.041(3) . ?
Hf1 O3 2.290(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
O1 C1 C14 118.6(3) . . ?
O1 C1 C2 122.0(3) . . ?
C14 C1 C2 119.4(3) . . ?
C7 C2 C1 117.4(3) . . ?
C7 C2 C3 120.2(3) . . ?
C1 C2 C3 122.3(3) . . ?
C4 C3 C6 108.1(3) . . ?
C4 C3 C5 109.5(3) . . ?
C6 C3 C5 106.5(3) . . ?
C4 C3 C2 108.5(3) . . ?
C6 C3 C2 112.0(3) . . ?
C5 C3 C2 112.1(3) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C2 124.2(3) . . ?
C8 C7 H7 117.9 . . ?
C2 C7 H7 117.9 . . ?
C7 C8 C13 116.8(3) . . ?
C7 C8 C9 123.3(3) . . ?
C13 C8 C9 119.8(3) . . ?
C8 C9 C10 112.3(3) . . ?
C8 C9 C12 109.1(3) . . ?
C10 C9 C12 108.8(3) . . ?
C8 C9 C11 109.3(3) . . ?
C10 C9 C11 108.1(3) . . ?
C12 C9 C11 109.2(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C8 121.4(3) . . ?
C14 C13 H13 119.3 . . ?
C8 C13 H13 119.3 . . ?
C13 C14 C1 120.7(3) . . ?
C13 C14 C15 119.2(3) . . ?
C1 C14 C15 119.8(3) . . ?
N1 C15 C14 115.8(2) . . ?
N1 C15 H15A 108.3 . . ?
C14 C15 H15A 108.3 . . ?
N1 C15 H15B 108.3 . . ?
C14 C15 H15B 108.3 . . ?
H15A C15 H15B 107.4 . . ?
N1 C16 C17 115.4(3) . . ?
N1 C16 C23 101.3(2) . . ?
C17 C16 C23 113.6(2) . . ?
N1 C16 H16 108.7 . . ?
C17 C16 H16 108.7 . . ?
C23 C16 H16 108.7 . . ?
C22 C17 C18 118.7(3) . . ?
C22 C17 C16 119.9(3) . . ?
C18 C17 C16 121.3(3) . . ?
C19 C18 C17 120.4(3) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
C20 C19 C18 120.1(3) . . ?
C20 C19 H19 119.9 . . ?
C18 C19 H19 119.9 . . ?
C21 C20 C19 119.7(3) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 120.2(3) . . ?
C20 C21 H21 119.9 . . ?
C22 C21 H21 119.9 . . ?
C17 C22 C21 120.9(3) . . ?
C17 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
N2 C23 C24 115.7(3) . . ?
N2 C23 C16 100.8(2) . . ?
C24 C23 C16 113.7(3) . . ?
N2 C23 H23 108.8 . . ?
C24 C23 H23 108.8 . . ?
C16 C23 H23 108.8 . . ?
C29 C24 C25 118.7(3) . . ?
C29 C24 C23 122.7(3) . . ?
C25 C24 C23 118.4(3) . . ?
C26 C25 C24 120.2(4) . . ?
C26 C25 H25 119.9 . . ?
C24 C25 H25 119.9 . . ?
C25 C26 C27 120.4(4) . . ?
C25 C26 H26 119.8 . . ?
C27 C26 H26 119.8 . . ?
C28 C27 C26 119.6(4) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C27 C28 C29 120.2(4) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C24 C29 C28 120.9(4) . . ?
C24 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
N2 C30 N1 108.0(3) . . ?
N2 C30 Hf1 127.3(2) . . ?
N1 C30 Hf1 124.2(2) . . ?
N2 C31 C32 115.7(3) . . ?
N2 C31 H31A 108.4 . . ?
C32 C31 H31A 108.4 . . ?
N2 C31 H31B 108.4 . . ?
C32 C31 H31B 108.4 . . ?
H31A C31 H31B 107.4 . . ?
C33 C32 C45 120.5(3) . . ?
C33 C32 C31 119.5(3) . . ?
C45 C32 C31 119.8(3) . . ?
C34 C33 C32 121.7(3) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C33 C34 C39 117.0(3) . . ?
C33 C34 C35 121.7(3) . . ?
C39 C34 C35 121.2(3) . . ?
C37A C35 C36B 127.0(8) . . ?
C37A C35 C38B 64.3(6) . . ?
C36B C35 C38B 114.8(7) . . ?
C37A C35 C36A 115.1(7) . . ?
C36B C35 C36A 22.1(5) . . ?
C38B C35 C36A 130.2(6) . . ?
C37A C35 C34 114.0(5) . . ?
C36B C35 C34 113.6(6) . . ?
C38B C35 C34 113.1(4) . . ?
C36A C35 C34 111.3(5) . . ?
C37A C35 C37B 36.9(5) . . ?
C36B C35 C37B 108.5(6) . . ?
C38B C35 C37B 100.9(6) . . ?
C36A C35 C37B 88.6(6) . . ?
C34 C35 C37B 104.5(4) . . ?
C37A C35 C38A 107.1(6) . . ?
C36B C35 C38A 78.4(6) . . ?
C38B C35 C38A 45.1(5) . . ?
C36A C35 C38A 99.8(6) . . ?
C34 C35 C38A 108.2(4) . . ?
C37B C35 C38A 140.2(5) . . ?
C34 C39 C40 124.1(3) . . ?
C34 C39 H39 117.9 . . ?
C40 C39 H39 117.9 . . ?
C39 C40 C45 117.0(3) . . ?
C39 C40 C41 120.5(3) . . ?
C45 C40 C41 122.5(3) . . ?
C44 C41 C42 107.5(3) . . ?
C44 C41 C43 109.7(3) . . ?
C42 C41 C43 107.1(3) . . ?
C44 C41 C40 109.9(3) . . ?
C42 C41 C40 112.1(3) . . ?
C43 C41 C40 110.4(3) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O2 C45 C32 119.0(3) . . ?
O2 C45 C40 121.6(3) . . ?
C32 C45 C40 119.4(3) . . ?
N3 C46 H46A 109.5 . . ?
N3 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
N3 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N3 C47 H47A 109.5 . . ?
N3 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
N3 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
O3 C48 C49 104.2(3) . . ?
O3 C48 H48A 110.9 . . ?
C49 C48 H48A 110.9 . . ?
O3 C48 H48B 110.9 . . ?
C49 C48 H48B 110.9 . . ?
H48A C48 H48B 108.9 . . ?
C48 C49 C50 103.1(3) . . ?
C48 C49 H49A 111.1 . . ?
C50 C49 H49A 111.1 . . ?
C48 C49 H49B 111.1 . . ?
C50 C49 H49B 111.1 . . ?
H49A C49 H49B 109.1 . . ?
C49 C50 C51 101.7(3) . . ?
C49 C50 H50A 111.4 . . ?
C51 C50 H50A 111.4 . . ?
C49 C50 H50B 111.4 . . ?
C51 C50 H50B 111.4 . . ?
H50A C50 H50B 109.3 . . ?
O3 C51 C50 105.7(3) . . ?
O3 C51 H51A 110.6 . . ?
C50 C51 H51A 110.6 . . ?
O3 C51 H51B 110.6 . . ?
C50 C51 H51B 110.6 . . ?
H51A C51 H51B 108.7 . . ?
O4 C52 C53 107.7(5) . . ?
O4 C52 H52A 110.2 . . ?
C53 C52 H52A 110.2 . . ?
O4 C52 H52B 110.2 . . ?
C53 C52 H52B 110.2 . . ?
H52A C52 H52B 108.5 . . ?
C52 C53 C54 106.3(4) . . ?
C52 C53 H53A 110.5 . . ?
C54 C53 H53A 110.5 . . ?
C52 C53 H53B 110.5 . . ?
C54 C53 H53B 110.5 . . ?
H53A C53 H53B 108.7 . . ?
C55 C54 C53 103.5(5) . . ?
C55 C54 H54A 111.1 . . ?
C53 C54 H54A 111.1 . . ?
C55 C54 H54B 111.1 . . ?
C53 C54 H54B 111.1 . . ?
H54A C54 H54B 109.0 . . ?
O4 C55 C54 110.7(5) . . ?
O4 C55 H55A 109.5 . . ?
C54 C55 H55A 109.5 . . ?
O4 C55 H55B 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 108.1 . . ?
C57 C56 O5 108.6(8) . . ?
C57 C56 H56A 110.0 . . ?
O5 C56 H56A 110.0 . . ?
C57 C56 H56B 110.0 . . ?
O5 C56 H56B 110.0 . . ?
H56A C56 H56B 108.3 . . ?
C56 C57 C58 111.8(10) . . ?
C56 C57 H57A 109.3 . . ?
C58 C57 H57A 109.3 . . ?
C56 C57 H57B 109.3 . . ?
C58 C57 H57B 109.3 . . ?
H57A C57 H57B 107.9 . . ?
C57 C58 C59 109.3(9) . . ?
C57 C58 H58A 109.8 . . ?
C59 C58 H58A 109.8 . . ?
C57 C58 H58B 109.8 . . ?
C59 C58 H58B 109.8 . . ?
H58A C58 H58B 108.3 . . ?
C58 C59 O5 107.1(9) . . ?
C58 C59 H59A 110.3 . . ?
O5 C59 H59A 110.3 . . ?
C58 C59 H59B 110.3 . . ?
O5 C59 H59B 110.3 . . ?
H59A C59 H59B 108.6 . . ?
C35 C36A H36A 109.5 . . ?
C35 C36A H36B 109.5 . . ?
C35 C36A H36C 109.5 . . ?
C35 C37A H37A 109.5 . . ?
C35 C37A H37B 109.5 . . ?
C35 C37A H37C 109.5 . . ?
C35 C38A H38A 109.5 . . ?
C35 C38A H38B 109.5 . . ?
C35 C38A H38C 109.5 . . ?
C35 C36B H36D 109.5 . . ?
C35 C36B H36E 109.5 . . ?
H36D C36B H36E 109.5 . . ?
C35 C36B H36F 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
C35 C37B H37D 109.5 . . ?
C35 C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
C35 C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
C35 C38B H38D 109.5 . . ?
C35 C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C35 C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
O2 Hf1 O1 165.64(8) . . ?
O2 Hf1 N3 94.56(10) . . ?
O1 Hf1 N3 95.10(10) . . ?
O2 Hf1 O3 84.21(8) . . ?
O1 Hf1 O3 85.25(8) . . ?
N3 Hf1 O3 175.01(9) . . ?
O2 Hf1 C30 84.60(10) . . ?
O1 Hf1 C30 84.70(9) . . ?
N3 Hf1 C30 90.58(11) . . ?
O3 Hf1 C30 84.49(9) . . ?
O2 Hf1 Cl1 96.60(6) . . ?
O1 Hf1 Cl1 91.84(6) . . ?
N3 Hf1 Cl1 101.57(8) . . ?
O3 Hf1 Cl1 83.38(6) . . ?
C30 Hf1 Cl1 167.63(8) . . ?
C30 N1 C15 123.2(3) . . ?
C30 N1 C16 112.0(2) . . ?
C15 N1 C16 119.8(2) . . ?
C30 N2 C31 123.3(3) . . ?
C30 N2 C23 112.5(2) . . ?
C31 N2 C23 119.7(2) . . ?
C47 N3 C46 110.2(3) . . ?
C47 N3 Hf1 126.6(2) . . ?
C46 N3 Hf1 122.9(2) . . ?
C1 O1 Hf1 156.79(19) . . ?
C45 O2 Hf1 158.5(2) . . ?
C51 O3 C48 109.4(2) . . ?
C51 O3 Hf1 127.98(17) . . ?
C48 O3 Hf1 122.63(18) . . ?
C52 O4 C55 109.5(4) . . ?
C59 O5 C56 100.9(8) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.058
_database_code_depnum_ccdc_archive 'CCDC 975127'
#######################################################################
#
#                 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_compound20

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C71 H92 Cl N3 O3 Zr'
_chemical_formula_sum            'C71 H92 Cl N3 O3 Zr'
_chemical_formula_weight         1162.15
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   15.2108(10)
_cell_length_b                   18.9002(13)
_cell_length_c                   22.5907(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6494.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    9952
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      27.40

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.39
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2480
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8930
_exptl_absorpt_correction_T_max  0.9063
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      110(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31878
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.94
_diffrn_reflns_theta_max         25.25
_reflns_number_total             11742
_reflns_number_gt                10522
_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, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0562P)²+2.9377P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_number_reflns         11742
_refine_ls_number_parameters     739
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1077
_refine_ls_wR_factor_gt          0.1017
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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
C1 C 0.6025(3) 0.43135(15) -0.01908(13) 0.0411(9) Uani 1 1 d . . .
C2 C 0.5434(3) 0.47920(16) -0.04704(15) 0.0459(9) Uani 1 1 d . . .
C3 C 0.4443(3) 0.46751(17) -0.04998(16) 0.0525(10) Uani 1 1 d . . .
C4 C 0.3993(3) 0.5207(2) -0.09254(19) 0.0680(13) Uani 1 1 d . . .
H4A H 0.4018 0.5683 -0.0754 0.102 Uiso 1 1 calc R . .
H4B H 0.3378 0.5070 -0.0984 0.102 Uiso 1 1 calc R . .
H4C H 0.4299 0.5205 -0.1307 0.102 Uiso 1 1 calc R . .
C5 C 0.4028(3) 0.4759(2) 0.01113(19) 0.0613(11) Uani 1 1 d . . .
H5A H 0.4223 0.4372 0.0369 0.092 Uiso 1 1 calc R . .
H5B H 0.3386 0.4747 0.0075 0.092 Uiso 1 1 calc R . .
H5C H 0.4208 0.5213 0.0283 0.092 Uiso 1 1 calc R . .
C6 C 0.4253(3) 0.39297(17) -0.07600(17) 0.0551(9) Uani 1 1 d . . .
H6A H 0.4592 0.3865 -0.1125 0.083 Uiso 1 1 calc R . .
H6B H 0.3624 0.3887 -0.0848 0.083 Uiso 1 1 calc R . .
H6C H 0.4422 0.3567 -0.0472 0.083 Uiso 1 1 calc R . .
C7 C 0.5827(3) 0.53887(16) -0.07451(15) 0.0508(9) Uani 1 1 d . . .
H7 H 0.5450 0.5734 -0.0915 0.061 Uiso 1 1 calc R . .
C8 C 0.6721(3) 0.54989(18) -0.07800(16) 0.0554(10) Uani 1 1 d . . .
C9 C 0.7118(4) 0.6156(2) -0.10857(18) 0.0716(14) Uani 1 1 d . . .
C10 C 0.6478(5) 0.6626(3) -0.1350(3) 0.119(3) Uani 1 1 d . . .
H10A H 0.6087 0.6354 -0.1609 0.178 Uiso 1 1 calc R . .
H10B H 0.6782 0.6989 -0.1582 0.178 Uiso 1 1 calc R . .
H10C H 0.6131 0.6853 -0.1038 0.178 Uiso 1 1 calc R . .
C11 C 0.7736(5) 0.5906(3) -0.1614(3) 0.107(2) Uani 1 1 d . . .
H11A H 0.7404 0.5596 -0.1880 0.160 Uiso 1 1 calc R . .
H11B H 0.8241 0.5647 -0.1453 0.160 Uiso 1 1 calc R . .
H11C H 0.7944 0.6321 -0.1834 0.160 Uiso 1 1 calc R . .
C12 C 0.7730(6) 0.6541(3) -0.0652(3) 0.133(3) Uani 1 1 d . . .
H12A H 0.8087 0.6887 -0.0868 0.200 Uiso 1 1 calc R . .
H12B H 0.8117 0.6196 -0.0459 0.200 Uiso 1 1 calc R . .
H12C H 0.7378 0.6786 -0.0352 0.200 Uiso 1 1 calc R . .
C13 C 0.7270(3) 0.49860(18) -0.05400(14) 0.0485(9) Uani 1 1 d . . .
H13 H 0.7889 0.5040 -0.0573 0.058 Uiso 1 1 calc R . .
C14 C 0.6933(3) 0.43970(16) -0.02534(13) 0.0415(8) Uani 1 1 d . . .
C15 C 0.7545(2) 0.38152(16) -0.00676(13) 0.0383(8) Uani 1 1 d . . .
H15A H 0.7307 0.3361 -0.0215 0.046 Uiso 1 1 calc R . .
H15B H 0.8120 0.3892 -0.0263 0.046 Uiso 1 1 calc R . .
C16 C 0.8579(2) 0.38769(14) 0.08173(13) 0.0334(7) Uani 1 1 d . . .
H16 H 0.8993 0.3515 0.0655 0.040 Uiso 1 1 calc R . .
C17 C 0.8941(2) 0.46108(16) 0.06951(13) 0.0356(7) Uani 1 1 d . . .
C18 C 0.8418(3) 0.52047(16) 0.07352(17) 0.0481(8) Uani 1 1 d . . .
H18 H 0.7815 0.5163 0.0839 0.058 Uiso 1 1 calc R . .
C19 C 0.8786(3) 0.5870(2) 0.06211(18) 0.0585(11) Uani 1 1 d . . .
H19 H 0.8429 0.6282 0.0646 0.070 Uiso 1 1 calc R . .
C20 C 0.9657(3) 0.5931(2) 0.04743(16) 0.0561(11) Uani 1 1 d . . .
H20 H 0.9904 0.6385 0.0408 0.067 Uiso 1 1 calc R . .
C21 C 1.0171(3) 0.5344(2) 0.04236(16) 0.0529(10) Uani 1 1 d . . .
H21 H 1.0770 0.5387 0.0311 0.064 Uiso 1 1 calc R . .
C22 C 0.9809(3) 0.46776(19) 0.05390(14) 0.0443(9) Uani 1 1 d . . .
H22 H 1.0168 0.4268 0.0509 0.053 Uiso 1 1 calc R . .
C23 C 0.8416(2) 0.37230(14) 0.14832(12) 0.0313(7) Uani 1 1 d . . .
H23 H 0.8272 0.4177 0.1688 0.038 Uiso 1 1 calc R . .
C24 C 0.9177(2) 0.33782(15) 0.17965(12) 0.0333(7) Uani 1 1 d . . .
C25 C 0.9691(2) 0.37569(18) 0.21836(16) 0.0459(8) Uani 1 1 d . . .
H25 H 0.9559 0.4240 0.2258 0.055 Uiso 1 1 calc R . .
C26 C 1.0404(3) 0.3440(2) 0.24683(18) 0.0575(10) Uani 1 1 d . . .
H26 H 1.0757 0.3705 0.2735 0.069 Uiso 1 1 calc R . .
C27 C 1.0593(3) 0.2730(2) 0.23566(17) 0.0579(10) Uani 1 1 d . . .
H27 H 1.1071 0.2506 0.2553 0.069 Uiso 1 1 calc R . .
C28 C 1.0093(3) 0.23572(19) 0.19668(16) 0.0550(10) Uani 1 1 d . . .
H28 H 1.0229 0.1876 0.1888 0.066 Uiso 1 1 calc R . .
C29 C 0.9390(3) 0.26720(16) 0.16845(15) 0.0464(8) Uani 1 1 d . . .
H29 H 0.9048 0.2406 0.1412 0.056 Uiso 1 1 calc R . .
C30 C 0.7185(2) 0.33719(15) 0.09400(12) 0.0344(7) Uani 1 1 d . A .
C31 C 0.7196(2) 0.30220(16) 0.19961(11) 0.0344(6) Uani 1 1 d . . .
H31A H 0.6595 0.3221 0.2021 0.041 Uiso 1 1 calc R . .
H31B H 0.7531 0.3201 0.2341 0.041 Uiso 1 1 calc R . .
C32 C 0.7135(2) 0.22248(15) 0.20420(12) 0.0339(7) Uani 1 1 d . A .
C33 C 0.7671(2) 0.18681(17) 0.24423(12) 0.0381(7) Uani 1 1 d . . .
H33 H 0.8110 0.2125 0.2651 0.046 Uiso 1 1 calc R . .
C34 C 0.7582(2) 0.11461(17) 0.25452(14) 0.0414(8) Uani 1 1 d . A .
C35 C 0.8160(3) 0.07612(18) 0.30018(16) 0.0495(9) Uani 1 1 d . . .
C36A C 0.7525(6) 0.0523(5) 0.3516(3) 0.070(3) Uani 0.553(10) 1 d P A 1
H36A H 0.7842 0.0209 0.3788 0.105 Uiso 0.553(10) 1 calc PR A 1
H36B H 0.7021 0.0271 0.3348 0.105 Uiso 0.553(10) 1 calc PR A 1
H36C H 0.7319 0.0941 0.3732 0.105 Uiso 0.553(10) 1 calc PR A 1
C37A C 0.8846(7) 0.1233(5) 0.3237(4) 0.076(4) Uani 0.553(10) 1 d P A 1
H37A H 0.9240 0.0963 0.3496 0.114 Uiso 0.553(10) 1 calc PR A 1
H37B H 0.8572 0.1615 0.3464 0.114 Uiso 0.553(10) 1 calc PR A 1
H37C H 0.9184 0.1434 0.2909 0.114 Uiso 0.553(10) 1 calc PR A 1
C38A C 0.8500(8) 0.0122(6) 0.2696(5) 0.084(4) Uani 0.553(10) 1 d P A 1
H38A H 0.8659 0.0244 0.2288 0.127 Uiso 0.553(10) 1 calc PR A 1
H38B H 0.8045 -0.0245 0.2692 0.127 Uiso 0.553(10) 1 calc PR A 1
H38C H 0.9021 -0.0054 0.2905 0.127 Uiso 0.553(10) 1 calc PR A 1
C36B C 0.7984(9) 0.1057(8) 0.3617(4) 0.080(4) Uani 0.447(10) 1 d P A 2
H36D H 0.7988 0.0670 0.3906 0.120 Uiso 0.447(10) 1 calc PR A 2
H36E H 0.7409 0.1291 0.3622 0.120 Uiso 0.447(10) 1 calc PR A 2
H36F H 0.8443 0.1400 0.3719 0.120 Uiso 0.447(10) 1 calc PR A 2
C37B C 0.9171(6) 0.0836(6) 0.2869(4) 0.059(3) Uani 0.447(10) 1 d P A 2
H37D H 0.9331 0.1338 0.2863 0.089 Uiso 0.447(10) 1 calc PR A 2
H37E H 0.9303 0.0623 0.2484 0.089 Uiso 0.447(10) 1 calc PR A 2
H37F H 0.9507 0.0594 0.3179 0.089 Uiso 0.447(10) 1 calc PR A 2
C38B C 0.8027(11) -0.0024(6) 0.3051(8) 0.092(5) Uani 0.447(10) 1 d P A 2
H38D H 0.8477 -0.0225 0.3312 0.138 Uiso 0.447(10) 1 calc PR A 2
H38E H 0.8074 -0.0239 0.2657 0.138 Uiso 0.447(10) 1 calc PR A 2
H38F H 0.7443 -0.0121 0.3215 0.138 Uiso 0.447(10) 1 calc PR A 2
C39 C 0.6918(3) 0.08027(16) 0.22315(14) 0.0413(8) Uani 1 1 d . . .
H39 H 0.6840 0.0311 0.2301 0.050 Uiso 1 1 calc R A .
C40 C 0.6361(2) 0.11241(16) 0.18254(13) 0.0343(7) Uani 1 1 d . A .
C41 C 0.5608(3) 0.07122(14) 0.15342(13) 0.0383(7) Uani 1 1 d . . .
C42 C 0.4723(2) 0.10408(18) 0.17076(16) 0.0450(8) Uani 1 1 d . A .
H42A H 0.4695 0.1529 0.1563 0.068 Uiso 1 1 calc R . .
H42B H 0.4663 0.1038 0.2140 0.068 Uiso 1 1 calc R . .
H42C H 0.4244 0.0765 0.1532 0.068 Uiso 1 1 calc R . .
C43 C 0.5693(3) 0.07140(16) 0.08565(13) 0.0438(7) Uani 1 1 d . A .
H43A H 0.5191 0.0464 0.0682 0.066 Uiso 1 1 calc R . .
H43B H 0.6239 0.0476 0.0742 0.066 Uiso 1 1 calc R . .
H43C H 0.5702 0.1203 0.0713 0.066 Uiso 1 1 calc R . .
C44 C 0.5582(3) -0.00686(16) 0.17366(15) 0.0483(9) Uani 1 1 d . A .
H44A H 0.5521 -0.0088 0.2168 0.072 Uiso 1 1 calc R . .
H44B H 0.6128 -0.0305 0.1619 0.072 Uiso 1 1 calc R . .
H44C H 0.5081 -0.0308 0.1551 0.072 Uiso 1 1 calc R . .
C45 C 0.6489(2) 0.18591(15) 0.17198(12) 0.0325(7) Uani 1 1 d . . .
C46 C 0.4822(3) 0.34185(18) 0.19547(15) 0.0449(9) Uani 1 1 d . . .
H46A H 0.5069 0.3661 0.2306 0.054 Uiso 1 1 calc R . .
H46B H 0.4951 0.2907 0.1995 0.054 Uiso 1 1 calc R . .
C47 C 0.3834(3) 0.3522(3) 0.1949(2) 0.0703(13) Uani 1 1 d . . .
H47A H 0.3700 0.4029 0.1936 0.105 Uiso 1 1 calc R . .
H47B H 0.3579 0.3315 0.2308 0.105 Uiso 1 1 calc R . .
H47C H 0.3584 0.3290 0.1600 0.105 Uiso 1 1 calc R . .
C48 C 0.5353(3) 0.44687(17) 0.14243(16) 0.0502(9) Uani 1 1 d . . .
H48A H 0.4787 0.4679 0.1550 0.060 Uiso 1 1 calc R . .
H48B H 0.5476 0.4635 0.1017 0.060 Uiso 1 1 calc R . .
C49 C 0.6073(3) 0.47296(18) 0.18312(17) 0.0505(9) Uani 1 1 d . . .
H49A H 0.5938 0.4592 0.2239 0.076 Uiso 1 1 calc R . .
H49B H 0.6113 0.5246 0.1805 0.076 Uiso 1 1 calc R . .
H49C H 0.6635 0.4519 0.1713 0.076 Uiso 1 1 calc R . .
C50 C 0.7158(2) 0.18923(17) 0.01024(14) 0.0389(7) Uani 1 1 d . . .
H50A H 0.7135 0.1599 0.0465 0.047 Uiso 1 1 calc R . .
H50B H 0.7683 0.2201 0.0121 0.047 Uiso 1 1 calc R . .
C51 C 0.7182(3) 0.14320(19) -0.04447(15) 0.0475(8) Uani 1 1 d . . .
H51A H 0.6828 0.0997 -0.0391 0.057 Uiso 1 1 calc R . .
H51B H 0.7792 0.1300 -0.0550 0.057 Uiso 1 1 calc R . .
C52 C 0.6777(3) 0.1916(2) -0.09099(14) 0.0521(9) Uani 1 1 d . . .
H52A H 0.7217 0.2256 -0.1065 0.063 Uiso 1 1 calc R . .
H52B H 0.6533 0.1640 -0.1244 0.063 Uiso 1 1 calc R . .
C53 C 0.6060(2) 0.22932(17) -0.05737(13) 0.0416(8) Uani 1 1 d . . .
H53A H 0.5975 0.2778 -0.0729 0.050 Uiso 1 1 calc R . .
H53B H 0.5497 0.2033 -0.0607 0.050 Uiso 1 1 calc R . .
C54 C 0.7727(4) 0.6277(3) 0.2044(2) 0.0771(15) Uani 1 1 d . . .
H54 H 0.7608 0.6331 0.1634 0.093 Uiso 1 1 calc R . .
C55 C 0.8413(5) 0.5865(3) 0.2216(2) 0.097(2) Uani 1 1 d . . .
H55 H 0.8760 0.5638 0.1923 0.117 Uiso 1 1 calc R . .
C56 C 0.8615(7) 0.5769(3) 0.2786(3) 0.140(4) Uani 1 1 d . . .
H56 H 0.9088 0.5472 0.2903 0.168 Uiso 1 1 calc R . .
C57 C 0.8107(9) 0.6120(7) 0.3198(3) 0.186(7) Uani 1 1 d . . .
H57 H 0.8254 0.6074 0.3605 0.223 Uiso 1 1 calc R . .
C58 C 0.7417(7) 0.6523(7) 0.3050(4) 0.194(8) Uani 1 1 d . . .
H58 H 0.7074 0.6744 0.3349 0.233 Uiso 1 1 calc R . .
C59 C 0.7201(5) 0.6618(4) 0.2447(3) 0.121(3) Uani 1 1 d . . .
H59 H 0.6717 0.6902 0.2328 0.145 Uiso 1 1 calc R . .
C60 C 0.7823(11) 0.8132(7) 0.1227(5) 0.193(7) Uani 1 1 d . . .
H60 H 0.7679 0.8118 0.1636 0.232 Uiso 1 1 calc R . .
C61 C 0.7262(8) 0.8505(7) 0.0773(7) 0.207(6) Uani 1 1 d . . .
H61 H 0.6750 0.8763 0.0880 0.249 Uiso 1 1 calc R . .
C62 C 0.7523(7) 0.8452(6) 0.0225(5) 0.172(5) Uani 1 1 d . . .
H62 H 0.7119 0.8603 -0.0070 0.206 Uiso 1 1 calc R . .
C63 C 0.8293(9) 0.8208(4) 0.0033(4) 0.151(4) Uani 1 1 d . . .
H63 H 0.8475 0.8271 -0.0366 0.181 Uiso 1 1 calc R . .
C64 C 0.8794(8) 0.7874(3) 0.0423(3) 0.163(5) Uani 1 1 d . . .
H64 H 0.9334 0.7670 0.0300 0.195 Uiso 1 1 calc R . .
C65 C 0.8537(10) 0.7823(3) 0.1006(4) 0.178(6) Uani 1 1 d . . .
H65 H 0.8892 0.7549 0.1266 0.213 Uiso 1 1 calc R . .
C66 C -0.0534(3) 0.8088(3) 0.83250(18) 0.108(2) Uani 1 1 d G . .
H66 H -0.0937 0.8187 0.8014 0.130 Uiso 1 1 calc R . .
C67 C -0.0159(3) 0.8640(2) 0.8643(3) 0.123(3) Uani 1 1 d G . .
H67 H -0.0305 0.9116 0.8550 0.148 Uiso 1 1 calc R . .
C68 C 0.0431(4) 0.8496(3) 0.9098(2) 0.120(2) Uani 1 1 d G . .
H68 H 0.0687 0.8873 0.9316 0.144 Uiso 1 1 calc R . .
C69 C 0.0644(4) 0.7799(3) 0.9234(3) 0.170(4) Uani 1 1 d G . .
H69 H 0.1047 0.7701 0.9545 0.204 Uiso 1 1 calc R . .
C70 C 0.0269(4) 0.7248(2) 0.8916(3) 0.200(6) Uani 1 1 d G . .
H70 H 0.0415 0.6772 0.9009 0.240 Uiso 1 1 calc R . .
C71 C -0.0321(4) 0.7392(3) 0.8461(3) 0.145(3) Uani 1 1 d G . .
H71 H -0.0577 0.7015 0.8243 0.174 Uiso 1 1 calc R . .
Cl1 Cl 0.42845(6) 0.24314(4) 0.04325(3) 0.04079(18) Uani 1 1 d . A .
N1 N 0.76930(19) 0.37500(13) 0.05746(11) 0.0364(6) Uani 1 1 d . . .
N2 N 0.76161(18) 0.32892(12) 0.14494(10) 0.0330(6) Uani 1 1 d . . .
N3 N 0.5264(2) 0.36901(13) 0.14172(12) 0.0403(6) Uani 1 1 d . A .
O1 O 0.57167(18) 0.37609(10) 0.01337(8) 0.0390(5) Uani 1 1 d . A .
O2 O 0.59925(14) 0.22226(10) 0.13248(8) 0.0329(5) Uani 1 1 d . A .
O3 O 0.63586(15) 0.23123(10) 0.00404(8) 0.0352(5) Uani 1 1 d . A .
Zr1 Zr 0.56860(2) 0.301412(13) 0.076589(11) 0.03247(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.359(4) . ?
C1 C14 1.398(5) . ?
C1 C2 1.422(5) . ?
C2 C7 1.419(5) . ?
C2 C3 1.526(6) . ?
C3 C5 1.526(6) . ?
C3 C4 1.550(5) . ?
C3 C6 1.554(5) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.378(6) . ?
C7 H7 0.9500 . ?
C8 C13 1.389(5) . ?
C8 C9 1.545(5) . ?
C9 C10 1.447(7) . ?
C9 C12 1.535(7) . ?
C9 C11 1.591(8) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.386(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.500(5) . ?
C15 N1 1.473(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 N1 1.474(4) . ?
C16 C17 1.518(4) . ?
C16 C23 1.552(4) . ?
C16 H16 1.0000 . ?
C17 C22 1.373(5) . ?
C17 C18 1.379(5) . ?
C18 C19 1.400(5) . ?
C18 H18 0.9500 . ?
C19 C20 1.371(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.362(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.399(5) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 N2 1.469(4) . ?
C23 C24 1.506(4) . ?
C23 H23 1.0000 . ?
C24 C25 1.374(5) . ?
C24 C29 1.396(4) . ?
C25 C26 1.396(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.397(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.360(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.380(5) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?
C30 N2 1.334(4) . ?
C30 N1 1.338(4) . ?
C30 Zr1 2.410(4) . ?
C31 N2 1.479(4) . ?
C31 C32 1.513(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.392(4) . ?
C32 C45 1.404(4) . ?
C33 C34 1.391(4) . ?
C33 H33 0.9500 . ?
C34 C39 1.394(5) . ?
C34 C35 1.538(5) . ?
C35 C37A 1.473(9) . ?
C35 C38A 1.485(9) . ?
C35 C38B 1.502(11) . ?
C35 C36B 1.521(11) . ?
C35 C37B 1.573(11) . ?
C35 C36A 1.576(9) . ?
C36A H36A 0.9800 . ?
C36A H36B 0.9800 . ?
C36A H36C 0.9800 . ?
C37A H37A 0.9800 . ?
C37A H37B 0.9800 . ?
C37A H37C 0.9800 . ?
C38A H38A 0.9800 . ?
C38A H38B 0.9800 . ?
C38A H38C 0.9800 . ?
C36B H36D 0.9800 . ?
C36B H36E 0.9800 . ?
C36B H36F 0.9800 . ?
C37B H37D 0.9800 . ?
C37B H37E 0.9800 . ?
C37B H37F 0.9800 . ?
C38B H38D 0.9800 . ?
C38B H38E 0.9800 . ?
C38B H38F 0.9800 . ?
C39 C40 1.389(5) . ?
C39 H39 0.9500 . ?
C40 C45 1.423(4) . ?
C40 C41 1.533(5) . ?
C41 C42 1.534(5) . ?
C41 C43 1.536(4) . ?
C41 C44 1.545(4) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 O2 1.356(4) . ?
C46 N3 1.480(4) . ?
C46 C47 1.515(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 N3 1.478(4) . ?
C48 C49 1.513(5) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 O3 1.458(4) . ?
C50 C51 1.512(5) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.523(5) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.509(5) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 O3 1.460(3) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 C55 1.360(8) . ?
C54 C59 1.372(8) . ?
C54 H54 0.9500 . ?
C55 C56 1.336(8) . ?
C55 H55 0.9500 . ?
C56 C57 1.378(15) . ?
C56 H56 0.9500 . ?
C57 C58 1.339(19) . ?
C57 H57 0.9500 . ?
C58 C59 1.411(13) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
C60 C65 1.331(17) . ?
C60 C61 1.511(19) . ?
C60 H60 0.9500 . ?
C61 C62 1.305(15) . ?
C61 H61 0.9500 . ?
C62 C63 1.330(13) . ?
C62 H62 0.9500 . ?
C63 C64 1.325(12) . ?
C63 H63 0.9500 . ?
C64 C65 1.376(11) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
C66 C67 1.3900 . ?
C66 C71 1.3900 . ?
C66 H66 0.9500 . ?
C67 C68 1.3900 . ?
C67 H67 0.9500 . ?
C68 C69 1.3900 . ?
C68 H68 0.9500 . ?
C69 C70 1.3900 . ?
C69 H69 0.9500 . ?
C70 C71 1.3900 . ?
C70 H70 0.9500 . ?
C71 H71 0.9500 . ?
Cl1 Zr1 2.5149(10) . ?
N3 Zr1 2.052(3) . ?
O1 Zr1 2.0085(18) . ?
O2 Zr1 2.0124(19) . ?
O3 Zr1 2.344(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
O1 C1 C14 118.8(3) . . ?
O1 C1 C2 120.7(3) . . ?
C14 C1 C2 120.5(3) . . ?
C7 C2 C1 115.7(3) . . ?
C7 C2 C3 120.8(3) . . ?
C1 C2 C3 123.5(3) . . ?
C2 C3 C5 110.8(3) . . ?
C2 C3 C4 111.7(3) . . ?
C5 C3 C4 108.1(3) . . ?
C2 C3 C6 109.4(3) . . ?
C5 C3 C6 111.1(3) . . ?
C4 C3 C6 105.8(3) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C2 124.1(3) . . ?
C8 C7 H7 118.0 . . ?
C2 C7 H7 118.0 . . ?
C7 C8 C13 117.7(3) . . ?
C7 C8 C9 122.2(4) . . ?
C13 C8 C9 120.0(4) . . ?
C10 C9 C12 112.4(5) . . ?
C10 C9 C8 114.5(4) . . ?
C12 C9 C8 109.4(3) . . ?
C10 C9 C11 105.7(5) . . ?
C12 C9 C11 105.2(5) . . ?
C8 C9 C11 109.1(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 C8 121.4(4) . . ?
C14 C13 H13 119.3 . . ?
C8 C13 H13 119.3 . . ?
C13 C14 C1 120.2(3) . . ?
C13 C14 C15 119.4(4) . . ?
C1 C14 C15 120.1(3) . . ?
N1 C15 C14 115.6(3) . . ?
N1 C15 H15A 108.4 . . ?
C14 C15 H15A 108.4 . . ?
N1 C15 H15B 108.4 . . ?
C14 C15 H15B 108.4 . . ?
H15A C15 H15B 107.4 . . ?
N1 C16 C17 114.4(3) . . ?
N1 C16 C23 100.6(2) . . ?
C17 C16 C23 113.9(2) . . ?
N1 C16 H16 109.2 . . ?
C17 C16 H16 109.2 . . ?
C23 C16 H16 109.2 . . ?
C22 C17 C18 119.8(3) . . ?
C22 C17 C16 118.7(3) . . ?
C18 C17 C16 121.5(3) . . ?
C17 C18 C19 119.2(4) . . ?
C17 C18 H18 120.4 . . ?
C19 C18 H18 120.4 . . ?
C20 C19 C18 120.4(4) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C21 C20 C19 120.4(4) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C22 119.5(4) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C17 C22 C21 120.6(4) . . ?
C17 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
N2 C23 C24 114.8(2) . . ?
N2 C23 C16 100.8(2) . . ?
C24 C23 C16 114.4(3) . . ?
N2 C23 H23 108.8 . . ?
C24 C23 H23 108.8 . . ?
C16 C23 H23 108.8 . . ?
C25 C24 C29 118.8(3) . . ?
C25 C24 C23 120.7(3) . . ?
C29 C24 C23 120.4(3) . . ?
C24 C25 C26 120.8(3) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C27 119.3(4) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
C28 C27 C26 120.0(4) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.6(3) . . ?
C27 C28 H28 119.7 . . ?
C29 C28 H28 119.7 . . ?
C28 C29 C24 120.5(4) . . ?
C28 C29 H29 119.7 . . ?
C24 C29 H29 119.7 . . ?
N2 C30 N1 108.1(3) . . ?
N2 C30 Zr1 125.0(2) . . ?
N1 C30 Zr1 126.6(2) . . ?
N2 C31 C32 115.1(2) . . ?
N2 C31 H31A 108.5 . . ?
C32 C31 H31A 108.5 . . ?
N2 C31 H31B 108.5 . . ?
C32 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C33 C32 C45 120.6(3) . . ?
C33 C32 C31 119.4(3) . . ?
C45 C32 C31 119.8(3) . . ?
C34 C33 C32 121.8(3) . . ?
C34 C33 H33 119.1 . . ?
C32 C33 H33 119.1 . . ?
C33 C34 C39 116.2(3) . . ?
C33 C34 C35 121.4(3) . . ?
C39 C34 C35 122.3(3) . . ?
C37A C35 C38A 114.4(7) . . ?
C37A C35 C38B 131.8(6) . . ?
C38A C35 C38B 43.7(7) . . ?
C37A C35 C36B 64.7(7) . . ?
C38A C35 C36B 141.8(6) . . ?
C38B C35 C36B 105.8(9) . . ?
C37A C35 C34 111.2(4) . . ?
C38A C35 C34 105.7(4) . . ?
C38B C35 C34 116.1(5) . . ?
C36B C35 C34 109.8(5) . . ?
C37A C35 C37B 47.2(5) . . ?
C38A C35 C37B 69.1(6) . . ?
C38B C35 C37B 103.6(8) . . ?
C36B C35 C37B 108.2(7) . . ?
C34 C35 C37B 112.9(4) . . ?
C37A C35 C36A 109.9(6) . . ?
C38A C35 C36A 108.9(7) . . ?
C38B C35 C36A 65.2(8) . . ?
C36B C35 C36A 47.5(6) . . ?
C34 C35 C36A 106.3(4) . . ?
C37B C35 C36A 139.8(5) . . ?
C35 C36A H36A 109.5 . . ?
C35 C36A H36B 109.5 . . ?
H36A C36A H36B 109.5 . . ?
C35 C36A H36C 109.5 . . ?
H36A C36A H36C 109.5 . . ?
H36B C36A H36C 109.5 . . ?
C35 C37A H37A 109.5 . . ?
C35 C37A H37B 109.5 . . ?
H37A C37A H37B 109.5 . . ?
C35 C37A H37C 109.5 . . ?
H37A C37A H37C 109.5 . . ?
H37B C37A H37C 109.5 . . ?
C35 C38A H38A 109.5 . . ?
C35 C38A H38B 109.5 . . ?
H38A C38A H38B 109.5 . . ?
C35 C38A H38C 109.5 . . ?
H38A C38A H38C 109.5 . . ?
H38B C38A H38C 109.5 . . ?
C35 C36B H36D 109.5 . . ?
C35 C36B H36E 109.5 . . ?
H36D C36B H36E 109.5 . . ?
C35 C36B H36F 109.5 . . ?
H36D C36B H36F 109.5 . . ?
H36E C36B H36F 109.5 . . ?
C35 C37B H37D 109.5 . . ?
C35 C37B H37E 109.5 . . ?
H37D C37B H37E 109.5 . . ?
C35 C37B H37F 109.5 . . ?
H37D C37B H37F 109.5 . . ?
H37E C37B H37F 109.5 . . ?
C35 C38B H38D 109.5 . . ?
C35 C38B H38E 109.5 . . ?
H38D C38B H38E 109.5 . . ?
C35 C38B H38F 109.5 . . ?
H38D C38B H38F 109.5 . . ?
H38E C38B H38F 109.5 . . ?
C40 C39 C34 125.0(3) . . ?
C40 C39 H39 117.5 . . ?
C34 C39 H39 117.5 . . ?
C39 C40 C45 117.0(3) . . ?
C39 C40 C41 121.1(3) . . ?
C45 C40 C41 121.7(3) . . ?
C40 C41 C42 109.9(3) . . ?
C40 C41 C43 111.3(3) . . ?
C42 C41 C43 109.1(3) . . ?
C40 C41 C44 112.1(3) . . ?
C42 C41 C44 106.8(3) . . ?
C43 C41 C44 107.4(2) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O2 C45 C32 118.8(3) . . ?
O2 C45 C40 121.9(3) . . ?
C32 C45 C40 119.3(3) . . ?
N3 C46 C47 113.5(3) . . ?
N3 C46 H46A 108.9 . . ?
C47 C46 H46A 108.9 . . ?
N3 C46 H46B 108.9 . . ?
C47 C46 H46B 108.9 . . ?
H46A C46 H46B 107.7 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
N3 C48 C49 113.4(3) . . ?
N3 C48 H48A 108.9 . . ?
C49 C48 H48A 108.9 . . ?
N3 C48 H48B 108.9 . . ?
C49 C48 H48B 108.9 . . ?
H48A C48 H48B 107.7 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O3 C50 C51 104.8(3) . . ?
O3 C50 H50A 110.8 . . ?
C51 C50 H50A 110.8 . . ?
O3 C50 H50B 110.8 . . ?
C51 C50 H50B 110.8 . . ?
H50A C50 H50B 108.9 . . ?
C50 C51 C52 102.0(3) . . ?
C50 C51 H51A 111.4 . . ?
C52 C51 H51A 111.4 . . ?
C50 C51 H51B 111.4 . . ?
C52 C51 H51B 111.4 . . ?
H51A C51 H51B 109.2 . . ?
C53 C52 C51 103.2(3) . . ?
C53 C52 H52A 111.1 . . ?
C51 C52 H52A 111.1 . . ?
C53 C52 H52B 111.1 . . ?
C51 C52 H52B 111.1 . . ?
H52A C52 H52B 109.1 . . ?
O3 C53 C52 105.3(3) . . ?
O3 C53 H53A 110.7 . . ?
C52 C53 H53A 110.7 . . ?
O3 C53 H53B 110.7 . . ?
C52 C53 H53B 110.7 . . ?
H53A C53 H53B 108.8 . . ?
C55 C54 C59 121.7(6) . . ?
C55 C54 H54 119.1 . . ?
C59 C54 H54 119.1 . . ?
C56 C55 C54 122.0(8) . . ?
C56 C55 H55 119.0 . . ?
C54 C55 H55 119.0 . . ?
C55 C56 C57 117.1(10) . . ?
C55 C56 H56 121.4 . . ?
C57 C56 H56 121.4 . . ?
C58 C57 C56 123.0(9) . . ?
C58 C57 H57 118.5 . . ?
C56 C57 H57 118.5 . . ?
C57 C58 C59 119.7(10) . . ?
C57 C58 H58 120.2 . . ?
C59 C58 H58 120.2 . . ?
C54 C59 C58 116.4(9) . . ?
C54 C59 H59 121.8 . . ?
C58 C59 H59 121.8 . . ?
C65 C60 C61 114.3(10) . . ?
C65 C60 H60 122.9 . . ?
C61 C60 H60 122.9 . . ?
C62 C61 C60 115.9(13) . . ?
C62 C61 H61 122.1 . . ?
C60 C61 H61 122.1 . . ?
C61 C62 C63 127.2(13) . . ?
C61 C62 H62 116.4 . . ?
C63 C62 H62 116.4 . . ?
C64 C63 C62 117.0(11) . . ?
C64 C63 H63 121.5 . . ?
C62 C63 H63 121.5 . . ?
C63 C64 C65 120.4(12) . . ?
C63 C64 H64 119.8 . . ?
C65 C64 H64 119.8 . . ?
C60 C65 C64 124.1(12) . . ?
C60 C65 H65 118.0 . . ?
C64 C65 H65 118.0 . . ?
C67 C66 C71 120.0 . . ?
C67 C66 H66 120.0 . . ?
C71 C66 H66 120.0 . . ?
C68 C67 C66 120.0 . . ?
C68 C67 H67 120.0 . . ?
C66 C67 H67 120.0 . . ?
C67 C68 C69 120.0 . . ?
C67 C68 H68 120.0 . . ?
C69 C68 H68 120.0 . . ?
C68 C69 C70 120.0 . . ?
C68 C69 H69 120.0 . . ?
C70 C69 H69 120.0 . . ?
C71 C70 C69 120.0 . . ?
C71 C70 H70 120.0 . . ?
C69 C70 H70 120.0 . . ?
C70 C71 C66 120.0 . . ?
C70 C71 H71 120.0 . . ?
C66 C71 H71 120.0 . . ?
C30 N1 C15 124.3(3) . . ?
C30 N1 C16 112.7(3) . . ?
C15 N1 C16 119.5(3) . . ?
C30 N2 C23 112.7(2) . . ?
C30 N2 C31 123.2(3) . . ?
C23 N2 C31 120.3(2) . . ?
C48 N3 C46 112.2(3) . . ?
C48 N3 Zr1 126.8(2) . . ?
C46 N3 Zr1 121.0(2) . . ?
C1 O1 Zr1 158.6(2) . . ?
C45 O2 Zr1 156.72(19) . . ?
C50 O3 C53 109.7(2) . . ?
C50 O3 Zr1 127.21(16) . . ?
C53 O3 Zr1 122.84(19) . . ?
O1 Zr1 O2 164.40(10) . . ?
O1 Zr1 N3 94.57(9) . . ?
O2 Zr1 N3 94.90(9) . . ?
O1 Zr1 O3 83.70(8) . . ?
O2 Zr1 O3 85.23(7) . . ?
N3 Zr1 O3 172.13(10) . . ?
O1 Zr1 C30 84.08(10) . . ?
O2 Zr1 C30 83.51(9) . . ?
N3 Zr1 C30 90.25(11) . . ?
O3 Zr1 C30 81.95(9) . . ?
O1 Zr1 Cl1 96.57(7) . . ?
O2 Zr1 Cl1 93.37(6) . . ?
N3 Zr1 Cl1 102.84(9) . . ?
O3 Zr1 Cl1 84.99(6) . . ?
C30 Zr1 Cl1 166.78(7) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.054
_database_code_depnum_ccdc_archive 'CCDC 975128'
