# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Moshe Kol'
'Israel Goldberg'
'Jacob Kopilov'
'Ekaterina Sergeeva'

_publ_contact_author_name        'Moshe Kol'
_publ_contact_author_email       MOSHEKOL@POST.TAU.AC.IL

_publ_section_title              
;
Salan ligands assembled around chiral bipyrrolidine:
predetermination of chirality around octahedral Ti and Zr centres
;

# Attachment 'mk192.cif'

data_mk192
_database_code_depnum_ccdc_archive 'CCDC 715079'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H76 N2 O4 Zr'
_chemical_formula_sum            'C46 H76 N2 O4 Zr'
_chemical_formula_weight         812.31
_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'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 65'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'x-y, x, z+5/6'
'y, -x+y, z+1/6'

_cell_length_a                   23.4652(5)
_cell_length_b                   23.4652(5)
_cell_length_c                   15.7143(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     7493.3(2)
_cell_formula_units_Z            6
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    10995
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      27.88

_exptl_crystal_description       needles
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2628
_exptl_absorpt_coefficient_mu    0.257
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. \f scans'
_diffrn_detector_area_resol_mean 12.8
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            43878
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_sigmaI/netI    0.1183
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.39
_diffrn_reflns_theta_max         27.88
_reflns_number_total             11342
_reflns_number_gt                7834
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Nonius B.V.'
_computing_cell_refinement       Denzo
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_solution    Sir-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

The structure contains traces of disordered pentane solvent, which
couldn't be modeled by discrete atoms. Two of the t-butyl residues
reveal ADP's of larger amplitude, which are indicative of their partial
disorder.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/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(4)
_refine_ls_number_reflns         11341
_refine_ls_number_parameters     500
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1549
_refine_ls_wR_factor_gt          0.1376
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.980
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.62753(2) 0.09653(2) 0.08522(3) 0.02120(11) Uani 1 1 d . . .
O2 O 0.52715(15) 0.05507(14) 0.0851(2) 0.0240(7) Uani 1 1 d . . .
O3 O 0.72091(15) 0.11104(16) 0.10379(18) 0.0248(7) Uani 1 1 d . . .
O4 O 0.64021(17) 0.11220(17) -0.03636(19) 0.0287(8) Uani 1 1 d . . .
O5 O 0.64134(16) 0.17831(15) 0.1351(2) 0.0268(7) Uani 1 1 d . . .
N6 N 0.58771(18) -0.02234(18) 0.0751(2) 0.0229(8) Uani 1 1 d . . .
N7 N 0.62059(19) 0.0518(2) 0.2282(2) 0.0241(9) Uani 1 1 d . . .
C8 C 0.5632(2) 0.0422(2) 0.2813(3) 0.0272(11) Uani 1 1 d . . .
H8A H 0.5220 0.0209 0.2476 0.033 Uiso 1 1 calc R . .
H8B H 0.5703 0.0849 0.3028 0.033 Uiso 1 1 calc R . .
C9 C 0.5594(3) -0.0022(3) 0.3553(3) 0.0304(11) Uani 1 1 d . . .
H9A H 0.5133 -0.0311 0.3737 0.036 Uiso 1 1 calc R . .
H9B H 0.5856 0.0243 0.4045 0.036 Uiso 1 1 calc R . .
C10 C 0.5891(3) -0.0435(3) 0.3172(3) 0.0301(11) Uani 1 1 d . . .
H10A H 0.6256 -0.0393 0.3532 0.036 Uiso 1 1 calc R . .
H10B H 0.5550 -0.0905 0.3135 0.036 Uiso 1 1 calc R . .
C11 C 0.6141(2) -0.0154(2) 0.2292(2) 0.0209(10) Uani 1 1 d . . .
H11 H 0.6579 -0.0116 0.2189 0.025 Uiso 1 1 calc R . .
C12 C 0.5654(2) -0.0570(2) 0.1585(3) 0.0233(10) Uani 1 1 d . . .
H12 H 0.5202 -0.0656 0.1723 0.028 Uiso 1 1 calc R . .
C13 C 0.5648(2) -0.1233(2) 0.1463(3) 0.0267(11) Uani 1 1 d . . .
H13A H 0.5811 -0.1346 0.1981 0.032 Uiso 1 1 calc R . .
H13B H 0.5197 -0.1595 0.1339 0.032 Uiso 1 1 calc R . .
C14 C 0.6107(2) -0.1121(2) 0.0705(3) 0.0273(10) Uani 1 1 d . . .
H14A H 0.6470 -0.1200 0.0871 0.033 Uiso 1 1 calc R . .
H14B H 0.5862 -0.1416 0.0225 0.033 Uiso 1 1 calc R . .
C15 C 0.6373(2) -0.0402(2) 0.0463(3) 0.0259(10) Uani 1 1 d . . .
H15A H 0.6801 -0.0119 0.0746 0.031 Uiso 1 1 calc R . .
H15B H 0.6437 -0.0345 -0.0160 0.031 Uiso 1 1 calc R . .
C16 C 0.5319(2) -0.0513(2) 0.0112(3) 0.0256(10) Uani 1 1 d . . .
H16A H 0.5462 -0.0239 -0.0409 0.031 Uiso 1 1 calc R . .
H16B H 0.5229 -0.0959 -0.0046 0.031 Uiso 1 1 calc R . .
C17 C 0.4691(2) -0.0561(2) 0.0422(3) 0.0213(10) Uani 1 1 d . . .
C18 C 0.4104(2) -0.1151(2) 0.0327(3) 0.0247(10) Uani 1 1 d . . .
H18 H 0.4117 -0.1525 0.0120 0.030 Uiso 1 1 calc R . .
C19 C 0.3495(2) -0.1212(2) 0.0527(3) 0.0254(11) Uani 1 1 d . . .
C20 C 0.3513(2) -0.0634(2) 0.0805(3) 0.0253(10) Uani 1 1 d . . .
H20 H 0.3105 -0.0657 0.0926 0.030 Uiso 1 1 calc R . .
C21 C 0.4088(2) -0.0029(2) 0.0914(3) 0.0236(9) Uani 1 1 d . . .
C22 C 0.4690(2) -0.0005(2) 0.0735(3) 0.0221(9) Uani 1 1 d . . .
C23 C 0.6825(2) 0.0998(2) 0.2754(3) 0.0266(11) Uani 1 1 d . . .
H23A H 0.6884 0.1445 0.2692 0.032 Uiso 1 1 calc R . .
H23B H 0.6760 0.0885 0.3366 0.032 Uiso 1 1 calc R . .
C24 C 0.7445(2) 0.1020(2) 0.2471(3) 0.0249(9) Uani 1 1 d . . .
C25 C 0.7862(3) 0.0999(2) 0.3087(3) 0.0339(12) Uani 1 1 d . . .
H25 H 0.7728 0.0938 0.3665 0.041 Uiso 1 1 calc R . .
C26 C 0.8463(3) 0.1063(2) 0.2884(3) 0.0330(12) Uani 1 1 d . . .
C27 C 0.8631(3) 0.1143(2) 0.2021(3) 0.0343(12) Uani 1 1 d . . .
H27 H 0.9042 0.1187 0.1866 0.041 Uiso 1 1 calc R . .
C28 C 0.8235(2) 0.1161(2) 0.1375(3) 0.0293(11) Uani 1 1 d . . .
C29 C 0.7626(2) 0.1095(2) 0.1604(3) 0.0240(10) Uani 1 1 d . . .
C30 C 0.2859(2) -0.1888(2) 0.0473(3) 0.0297(11) Uani 1 1 d . . .
C31 C 0.2797(3) -0.2195(3) -0.0409(3) 0.0419(14) Uani 1 1 d . . .
H31A H 0.2742 -0.1924 -0.0840 0.063 Uiso 1 1 calc R . .
H31B H 0.2413 -0.2640 -0.0417 0.063 Uiso 1 1 calc R . .
H31C H 0.3195 -0.2217 -0.0533 0.063 Uiso 1 1 calc R . .
C32 C 0.2245(3) -0.1828(3) 0.0638(4) 0.0446(15) Uani 1 1 d . . .
H32A H 0.2241 -0.1706 0.1233 0.067 Uiso 1 1 calc R . .
H32B H 0.1848 -0.2251 0.0520 0.067 Uiso 1 1 calc R . .
H32C H 0.2253 -0.1489 0.0264 0.067 Uiso 1 1 calc R . .
C33 C 0.2889(3) -0.2341(3) 0.1145(3) 0.0350(12) Uani 1 1 d . . .
H33A H 0.3274 -0.2391 0.1041 0.053 Uiso 1 1 calc R . .
H33B H 0.2488 -0.2773 0.1115 0.053 Uiso 1 1 calc R . .
H33C H 0.2924 -0.2151 0.1711 0.053 Uiso 1 1 calc R . .
C34 C 0.4064(2) 0.0597(2) 0.1174(3) 0.0266(10) Uani 1 1 d . . .
C35 C 0.4452(3) 0.0892(3) 0.2002(3) 0.0323(12) Uani 1 1 d . . .
H35A H 0.4424 0.1281 0.2160 0.049 Uiso 1 1 calc R . .
H35B H 0.4914 0.1018 0.1914 0.049 Uiso 1 1 calc R . .
H35C H 0.4265 0.0564 0.2458 0.049 Uiso 1 1 calc R . .
C36 C 0.4366(3) 0.1103(3) 0.0453(3) 0.0362(12) Uani 1 1 d . . .
H36A H 0.4101 0.0926 -0.0064 0.054 Uiso 1 1 calc R . .
H36B H 0.4816 0.1197 0.0343 0.054 Uiso 1 1 calc R . .
H36C H 0.4375 0.1510 0.0619 0.054 Uiso 1 1 calc R . .
C37 C 0.3354(3) 0.0447(3) 0.1316(3) 0.0373(12) Uani 1 1 d . . .
H37A H 0.3141 0.0099 0.1743 0.056 Uiso 1 1 calc R . .
H37B H 0.3110 0.0301 0.0779 0.056 Uiso 1 1 calc R . .
H37C H 0.3359 0.0845 0.1515 0.056 Uiso 1 1 calc R . .
C38 C 0.8938(3) 0.1105(3) 0.3597(4) 0.0436(14) Uani 1 1 d U . .
C39 C 0.9237(3) 0.1778(3) 0.4003(4) 0.0468(15) Uani 1 1 d U . .
H39A H 0.8889 0.1833 0.4263 0.070 Uiso 1 1 calc R . .
H39B H 0.9464 0.2117 0.3568 0.070 Uiso 1 1 calc R . .
H39C H 0.9553 0.1819 0.4441 0.070 Uiso 1 1 calc R . .
C40 C 0.9497(4) 0.1019(5) 0.3246(6) 0.058(3) Uani 1 1 d U . .
H40A H 0.9788 0.1049 0.3712 0.087 Uiso 1 1 calc R . .
H40B H 0.9749 0.1365 0.2828 0.087 Uiso 1 1 calc R . .
H40C H 0.9314 0.0588 0.2971 0.087 Uiso 1 1 calc R . .
C41 C 0.8581(4) 0.0579(4) 0.4261(5) 0.058(3) Uani 1 1 d U . .
H41A H 0.8892 0.0616 0.4703 0.087 Uiso 1 1 calc R . .
H41B H 0.8386 0.0145 0.3993 0.087 Uiso 1 1 calc R . .
H41C H 0.8232 0.0637 0.4517 0.087 Uiso 1 1 calc R . .
C42 C 0.8482(3) 0.1313(3) 0.0437(3) 0.0368(13) Uani 1 1 d . . .
C43 C 0.7986(3) 0.0792(3) -0.0175(3) 0.0369(13) Uani 1 1 d . . .
H43A H 0.7579 0.0813 -0.0178 0.055 Uiso 1 1 calc R . .
H43B H 0.7889 0.0354 0.0012 0.055 Uiso 1 1 calc R . .
H43C H 0.8172 0.0876 -0.0750 0.055 Uiso 1 1 calc R . .
C44 C 0.8582(3) 0.1991(3) 0.0195(3) 0.0357(13) Uani 1 1 d . . .
H44A H 0.8686 0.2071 -0.0413 0.054 Uiso 1 1 calc R . .
H44B H 0.8945 0.2332 0.0529 0.054 Uiso 1 1 calc R . .
H44C H 0.8177 0.2002 0.0314 0.054 Uiso 1 1 calc R . .
C45 C 0.9143(3) 0.1328(4) 0.0338(4) 0.0539(17) Uani 1 1 d . . .
H45A H 0.9084 0.0895 0.0483 0.081 Uiso 1 1 calc R . .
H45B H 0.9470 0.1662 0.0719 0.081 Uiso 1 1 calc R . .
H45C H 0.9295 0.1436 -0.0252 0.081 Uiso 1 1 calc R . .
C46 C 0.6546(3) 0.1381(3) -0.1202(3) 0.0335(12) Uani 1 1 d . . .
C47 C 0.7273(3) 0.1904(3) -0.1249(4) 0.0480(15) Uani 1 1 d . . .
H47A H 0.7374 0.2235 -0.0805 0.072 Uiso 1 1 calc R . .
H47B H 0.7369 0.2117 -0.1809 0.072 Uiso 1 1 calc R . .
H47C H 0.7542 0.1697 -0.1164 0.072 Uiso 1 1 calc R . .
C48 C 0.6390(3) 0.0832(3) -0.1820(3) 0.0450(15) Uani 1 1 d . . .
H48A H 0.6655 0.0628 -0.1683 0.067 Uiso 1 1 calc R . .
H48B H 0.6491 0.1009 -0.2400 0.067 Uiso 1 1 calc R . .
H48C H 0.5922 0.0501 -0.1780 0.067 Uiso 1 1 calc R . .
C49 C 0.6133(3) 0.1698(3) -0.1390(3) 0.0436(14) Uani 1 1 d . . .
H49A H 0.5672 0.1389 -0.1249 0.065 Uiso 1 1 calc R . .
H49B H 0.6168 0.1811 -0.1995 0.065 Uiso 1 1 calc R . .
H49C H 0.6291 0.2098 -0.1047 0.065 Uiso 1 1 calc R . .
C50 C 0.6612(3) 0.2446(3) 0.1540(3) 0.0342(12) Uani 1 1 d U . .
C51 C 0.6253(3) 0.2670(3) 0.0980(4) 0.0477(15) Uani 1 1 d U . .
H51A H 0.6380 0.2667 0.0387 0.072 Uiso 1 1 calc R . .
H51B H 0.6363 0.3117 0.1140 0.072 Uiso 1 1 calc R . .
H51C H 0.5778 0.2373 0.1043 0.072 Uiso 1 1 calc R . .
C52 C 0.6441(6) 0.2486(4) 0.2458(4) 0.060(3) Uani 1 1 d U . .
H52A H 0.5975 0.2169 0.2557 0.090 Uiso 1 1 calc R . .
H52B H 0.6526 0.2931 0.2579 0.090 Uiso 1 1 calc R . .
H52C H 0.6712 0.2384 0.2832 0.090 Uiso 1 1 calc R . .
C53 C 0.7340(4) 0.2848(4) 0.1395(8) 0.055(3) Uani 1 1 d U . .
H53A H 0.7561 0.2652 0.1708 0.082 Uiso 1 1 calc R . .
H53B H 0.7501 0.3298 0.1598 0.082 Uiso 1 1 calc R . .
H53C H 0.7433 0.2856 0.0786 0.082 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zr1 0.0240(2) 0.0195(2) 0.01833(18) -0.00048(17) -0.00046(17) 0.0096(2)
O2 0.0273(17) 0.0228(17) 0.0237(15) -0.0013(14) 0.0005(14) 0.0138(14)
O3 0.0252(18) 0.0262(18) 0.0223(16) 0.0008(12) 0.0007(12) 0.0123(15)
O4 0.031(2) 0.031(2) 0.0179(16) 0.0030(13) 0.0012(13) 0.0106(17)
O5 0.0301(19) 0.0208(18) 0.0292(17) -0.0035(13) -0.0023(14) 0.0125(16)
N6 0.025(2) 0.025(2) 0.0199(18) -0.0011(15) 0.0000(15) 0.0128(18)
N7 0.024(2) 0.026(2) 0.0202(19) -0.0019(15) 0.0001(14) 0.0116(19)
C8 0.030(3) 0.031(3) 0.024(2) -0.0019(19) -0.0009(18) 0.018(2)
C9 0.037(3) 0.035(3) 0.019(2) 0.0031(19) 0.0066(19) 0.018(3)
C10 0.037(3) 0.034(3) 0.021(2) 0.001(2) -0.003(2) 0.019(3)
C11 0.025(3) 0.015(2) 0.019(2) -0.0004(16) -0.0022(16) 0.008(2)
C12 0.025(3) 0.024(3) 0.021(2) 0.0016(18) 0.0015(18) 0.012(2)
C13 0.028(3) 0.015(2) 0.029(3) -0.0040(18) -0.0030(19) 0.005(2)
C14 0.026(3) 0.023(3) 0.035(3) -0.0001(19) 0.000(2) 0.014(2)
C15 0.022(3) 0.026(3) 0.028(2) -0.0038(19) -0.0003(19) 0.011(2)
C16 0.030(3) 0.023(3) 0.021(2) -0.0018(18) -0.0052(18) 0.011(2)
C17 0.020(2) 0.027(3) 0.019(2) 0.0003(18) 0.0007(17) 0.013(2)
C18 0.031(3) 0.020(3) 0.022(2) -0.0027(17) -0.0029(18) 0.012(2)
C19 0.027(3) 0.021(3) 0.025(2) 0.0030(18) -0.0005(19) 0.010(2)
C20 0.027(3) 0.030(3) 0.022(2) 0.005(2) 0.0052(19) 0.016(2)
C21 0.028(3) 0.026(2) 0.017(2) 0.0002(19) -0.0018(19) 0.014(2)
C22 0.024(2) 0.024(2) 0.018(2) 0.0009(17) -0.0031(17) 0.012(2)
C23 0.030(3) 0.026(3) 0.020(2) -0.0053(17) -0.0009(18) 0.011(2)
C24 0.025(2) 0.017(2) 0.029(2) -0.0020(19) -0.004(2) 0.0071(19)
C25 0.039(3) 0.027(3) 0.030(3) -0.003(2) -0.007(2) 0.012(3)
C26 0.029(3) 0.019(3) 0.047(3) -0.003(2) -0.013(2) 0.009(2)
C27 0.025(3) 0.024(3) 0.053(3) -0.005(2) -0.007(2) 0.011(2)
C28 0.023(3) 0.019(3) 0.037(3) -0.001(2) 0.001(2) 0.004(2)
C29 0.023(3) 0.017(2) 0.030(2) -0.0015(18) -0.0059(19) 0.008(2)
C30 0.028(3) 0.026(3) 0.029(2) 0.0034(19) -0.001(2) 0.009(2)
C31 0.041(3) 0.035(3) 0.026(3) -0.001(2) -0.005(2) 0.002(3)
C32 0.026(3) 0.030(3) 0.070(4) 0.001(3) 0.002(3) 0.008(3)
C33 0.039(3) 0.025(3) 0.035(3) 0.006(2) 0.002(2) 0.012(3)
C34 0.026(3) 0.027(3) 0.028(2) -0.0037(19) -0.0050(19) 0.015(2)
C35 0.042(3) 0.032(3) 0.029(3) -0.005(2) -0.004(2) 0.024(3)
C36 0.053(4) 0.030(3) 0.034(3) 0.000(2) -0.003(2) 0.027(3)
C37 0.038(3) 0.037(3) 0.046(3) -0.006(2) -0.002(2) 0.025(3)
C38 0.038(3) 0.029(3) 0.059(4) -0.004(2) -0.026(3) 0.013(3)
C39 0.043(4) 0.044(3) 0.047(3) -0.014(2) -0.021(3) 0.017(3)
C40 0.050(5) 0.065(7) 0.059(6) -0.027(5) -0.033(4) 0.034(6)
C41 0.062(5) 0.060(4) 0.053(6) 0.012(4) -0.029(4) 0.009(4)
C42 0.027(3) 0.038(3) 0.039(3) -0.002(2) 0.006(2) 0.012(3)
C43 0.037(3) 0.029(3) 0.037(3) -0.009(2) 0.007(2) 0.011(3)
C44 0.032(3) 0.029(3) 0.034(3) 0.001(2) 0.003(2) 0.006(2)
C45 0.038(4) 0.066(5) 0.060(4) -0.003(3) 0.013(3) 0.027(3)
C46 0.036(3) 0.029(3) 0.022(2) 0.001(2) 0.000(2) 0.006(3)
C47 0.041(4) 0.050(4) 0.035(3) 0.012(3) 0.004(2) 0.010(3)
C48 0.054(4) 0.051(4) 0.024(3) -0.006(2) 0.000(2) 0.021(3)
C49 0.046(4) 0.042(4) 0.039(3) 0.011(3) -0.004(3) 0.019(3)
C50 0.038(3) 0.026(3) 0.039(3) -0.010(2) -0.013(2) 0.016(2)
C51 0.070(4) 0.041(3) 0.050(3) -0.001(3) -0.009(3) 0.041(3)
C52 0.071(10) 0.074(5) 0.034(3) -0.012(3) -0.014(5) 0.031(6)
C53 0.047(4) 0.055(4) 0.062(11) -0.018(6) -0.026(5) 0.009(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O4 1.940(3) . ?
Zr1 O5 1.944(3) . ?
Zr1 O2 2.050(3) . ?
Zr1 O3 2.063(3) . ?
Zr1 N7 2.450(4) . ?
Zr1 N6 2.464(4) . ?
O2 C22 1.348(5) . ?
O3 C29 1.336(5) . ?
O4 C46 1.419(6) . ?
O5 C50 1.414(6) . ?
N6 C12 1.493(6) . ?
N6 C15 1.491(6) . ?
N6 C16 1.516(6) . ?
N7 C8 1.504(6) . ?
N7 C11 1.507(6) . ?
N7 C23 1.514(6) . ?
C8 C9 1.534(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.568(7) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C11 1.518(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.541(6) . ?
C11 H11 1.0000 . ?
C12 C13 1.560(6) . ?
C12 H12 1.0000 . ?
C13 C14 1.538(6) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.525(6) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.501(6) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.389(6) . ?
C17 C22 1.396(6) . ?
C18 C19 1.398(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.406(7) . ?
C19 C30 1.543(7) . ?
C20 C21 1.398(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.412(6) . ?
C21 C34 1.553(7) . ?
C23 C24 1.497(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.394(7) . ?
C24 C29 1.412(7) . ?
C25 C26 1.379(8) . ?
C25 H25 0.9500 . ?
C26 C27 1.397(8) . ?
C26 C38 1.549(7) . ?
C27 C28 1.391(7) . ?
C27 H27 0.9500 . ?
C28 C29 1.405(7) . ?
C28 C42 1.559(7) . ?
C30 C33 1.525(7) . ?
C30 C31 1.534(7) . ?
C30 C32 1.540(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.535(7) . ?
C34 C37 1.536(7) . ?
C34 C35 1.539(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 C39 1.512(8) . ?
C38 C41 1.509(9) . ?
C38 C40 1.526(10) . ?
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 C44 1.536(8) . ?
C42 C43 1.533(7) . ?
C42 C45 1.542(8) . ?
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 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C48 1.506(7) . ?
C46 C49 1.517(8) . ?
C46 C47 1.526(8) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.484(7) . ?
C50 C53 1.500(9) . ?
C50 C52 1.512(9) . ?
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 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Zr1 O5 105.99(14) . . ?
O4 Zr1 O2 96.90(13) . . ?
O5 Zr1 O2 93.08(13) . . ?
O4 Zr1 O3 93.35(13) . . ?
O5 Zr1 O3 98.10(13) . . ?
O2 Zr1 O3 162.15(12) . . ?
O4 Zr1 N7 162.74(14) . . ?
O5 Zr1 N7 89.78(13) . . ?
O2 Zr1 N7 89.02(12) . . ?
O3 Zr1 N7 77.21(12) . . ?
O4 Zr1 N6 94.95(13) . . ?
O5 Zr1 N6 157.69(13) . . ?
O2 Zr1 N6 76.55(12) . . ?
O3 Zr1 N6 88.07(12) . . ?
N7 Zr1 N6 70.61(12) . . ?
C22 O2 Zr1 145.8(3) . . ?
C29 O3 Zr1 145.2(3) . . ?
C46 O4 Zr1 167.5(3) . . ?
C50 O5 Zr1 166.2(3) . . ?
C12 N6 C15 102.8(3) . . ?
C12 N6 C16 110.4(3) . . ?
C15 N6 C16 107.1(3) . . ?
C12 N6 Zr1 113.1(3) . . ?
C15 N6 Zr1 115.5(3) . . ?
C16 N6 Zr1 107.7(3) . . ?
C8 N7 C11 102.9(3) . . ?
C8 N7 C23 107.1(3) . . ?
C11 N7 C23 109.4(3) . . ?
C8 N7 Zr1 115.9(3) . . ?
C11 N7 Zr1 114.1(2) . . ?
C23 N7 Zr1 107.2(3) . . ?
N7 C8 C9 105.4(4) . . ?
N7 C8 H8A 110.7 . . ?
C9 C8 H8A 110.7 . . ?
N7 C8 H8B 110.7 . . ?
C9 C8 H8B 110.7 . . ?
H8A C8 H8B 108.8 . . ?
C8 C9 C10 103.7(4) . . ?
C8 C9 H9A 111.0 . . ?
C10 C9 H9A 111.0 . . ?
C8 C9 H9B 111.0 . . ?
C10 C9 H9B 111.0 . . ?
H9A C9 H9B 109.0 . . ?
C11 C10 C9 106.0(4) . . ?
C11 C10 H10A 110.5 . . ?
C9 C10 H10A 110.5 . . ?
C11 C10 H10B 110.5 . . ?
C9 C10 H10B 110.5 . . ?
H10A C10 H10B 108.7 . . ?
N7 C11 C10 106.2(4) . . ?
N7 C11 C12 108.1(3) . . ?
C10 C11 C12 112.3(4) . . ?
N7 C11 H11 110.1 . . ?
C10 C11 H11 110.1 . . ?
C12 C11 H11 110.1 . . ?
N6 C12 C11 109.9(4) . . ?
N6 C12 C13 105.2(3) . . ?
C11 C12 C13 110.8(4) . . ?
N6 C12 H12 110.3 . . ?
C11 C12 H12 110.3 . . ?
C13 C12 H12 110.3 . . ?
C14 C13 C12 105.6(4) . . ?
C14 C13 H13A 110.6 . . ?
C12 C13 H13A 110.6 . . ?
C14 C13 H13B 110.6 . . ?
C12 C13 H13B 110.6 . . ?
H13A C13 H13B 108.8 . . ?
C15 C14 C13 104.2(4) . . ?
C15 C14 H14A 110.9 . . ?
C13 C14 H14A 110.9 . . ?
C15 C14 H14B 110.9 . . ?
C13 C14 H14B 110.9 . . ?
H14A C14 H14B 108.9 . . ?
N6 C15 C14 106.9(4) . . ?
N6 C15 H15A 110.3 . . ?
C14 C15 H15A 110.3 . . ?
N6 C15 H15B 110.3 . . ?
C14 C15 H15B 110.3 . . ?
H15A C15 H15B 108.6 . . ?
C17 C16 N6 114.5(4) . . ?
C17 C16 H16A 108.6 . . ?
N6 C16 H16A 108.6 . . ?
C17 C16 H16B 108.6 . . ?
N6 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
C18 C17 C22 120.3(4) . . ?
C18 C17 C16 119.1(4) . . ?
C22 C17 C16 120.4(4) . . ?
C17 C18 C19 122.1(4) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C18 C19 C20 115.8(4) . . ?
C18 C19 C30 120.5(4) . . ?
C20 C19 C30 123.7(4) . . ?
C21 C20 C19 124.5(4) . . ?
C21 C20 H20 117.8 . . ?
C19 C20 H20 117.8 . . ?
C20 C21 C22 117.0(4) . . ?
C20 C21 C34 121.3(4) . . ?
C22 C21 C34 121.6(4) . . ?
O2 C22 C17 118.5(4) . . ?
O2 C22 C21 121.3(4) . . ?
C17 C22 C21 120.2(4) . . ?
C24 C23 N7 115.8(4) . . ?
C24 C23 H23A 108.3 . . ?
N7 C23 H23A 108.3 . . ?
C24 C23 H23B 108.3 . . ?
N7 C23 H23B 108.3 . . ?
H23A C23 H23B 107.4 . . ?
C25 C24 C29 120.1(4) . . ?
C25 C24 C23 118.8(4) . . ?
C29 C24 C23 121.1(4) . . ?
C26 C25 C24 122.2(5) . . ?
C26 C25 H25 118.9 . . ?
C24 C25 H25 118.9 . . ?
C25 C26 C27 116.3(5) . . ?
C25 C26 C38 120.3(5) . . ?
C27 C26 C38 123.2(5) . . ?
C28 C27 C26 124.4(5) . . ?
C28 C27 H27 117.8 . . ?
C26 C27 H27 117.8 . . ?
C27 C28 C29 117.9(4) . . ?
C27 C28 C42 121.3(5) . . ?
C29 C28 C42 120.6(4) . . ?
O3 C29 C28 123.0(4) . . ?
O3 C29 C24 117.9(4) . . ?
C28 C29 C24 119.1(4) . . ?
C33 C30 C31 109.0(4) . . ?
C33 C30 C32 108.6(4) . . ?
C31 C30 C32 108.7(4) . . ?
C33 C30 C19 108.7(4) . . ?
C31 C30 C19 110.4(4) . . ?
C32 C30 C19 111.5(4) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C34 C37 108.3(4) . . ?
C36 C34 C35 109.6(4) . . ?
C37 C34 C35 108.1(4) . . ?
C36 C34 C21 108.4(4) . . ?
C37 C34 C21 111.7(4) . . ?
C35 C34 C21 110.8(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 . . ?
C39 C38 C41 109.9(6) . . ?
C39 C38 C40 108.1(5) . . ?
C41 C38 C40 107.8(7) . . ?
C39 C38 C26 108.3(4) . . ?
C41 C38 C26 111.1(5) . . ?
C40 C38 C26 111.6(5) . . ?
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 . . ?
C44 C42 C43 109.4(5) . . ?
C44 C42 C45 108.8(5) . . ?
C43 C42 C45 108.0(5) . . ?
C44 C42 C28 108.5(4) . . ?
C43 C42 C28 111.3(4) . . ?
C45 C42 C28 110.9(5) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C42 C45 H45A 109.5 . . ?
C42 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C42 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O4 C46 C48 109.2(4) . . ?
O4 C46 C49 108.5(4) . . ?
C48 C46 C49 110.6(5) . . ?
O4 C46 C47 108.7(4) . . ?
C48 C46 C47 110.7(5) . . ?
C49 C46 C47 109.1(5) . . ?
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 . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C46 C49 H49A 109.5 . . ?
C46 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C46 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O5 C50 C51 109.4(4) . . ?
O5 C50 C53 107.7(5) . . ?
C51 C50 C53 110.9(6) . . ?
O5 C50 C52 108.6(5) . . ?
C51 C50 C52 109.2(5) . . ?
C53 C50 C52 111.0(7) . . ?
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 . . ?

# start Validation Reply Form
_vrf_PLAT601_mk192               
;
PROBLEM: Structure Contains Sovent Accessible VOIDS of ... 1065.00 A**3
RESPONSE: These voids accommodate disordered pentane solvent; one
molecular fragment of partial occupancy per asymmetric unit.
This is reflected by the presence of several diffused residual
electron-density peaks, 0.5-1.0 e/A**3, within these voids.
The pentane solvent couldn't be reliably modeled by discrete
atoms.
;
# end Validation Reply Form

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        27.88
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.091