# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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#  This CIF contains data from an original supplementary publication 
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#  as required by the journal to which it was submitted. 
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data_jfc3_complex4
_database_code_depnum_ccdc_archive 'CCDC 919740'
#TrackingRef '16852_web_deposit_cif_file_0_StephenA.Miller_1358192858.complex4.cif'
_audit_update_record             
;
2009-08-25 # Formatted by publCIF
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H41 Cl2 N Si Zr'
_chemical_formula_weight         593.84
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/n
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a                   14.702(2)
_cell_length_b                   11.0049(18)
_cell_length_c                   18.445(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.953(2)
_cell_angle_gamma                90.00
_cell_volume                     2955.6(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    87
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      28.0
_exptl_crystal_description       plates
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_type   Numerical
_exptl_absorpt_correction_T_min  0.8490
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_process_details   
'based on measured indexed crystal faces, Bruker SHELXTL v6.12 (Bruker 2007)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(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       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27817
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6770
_reflns_number_gt                4953
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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.
;
_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^)+(0.0353P)^2^+0.3478P] 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_number_reflns         6770
_refine_ls_number_parameters     317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0808
_refine_ls_wR_factor_gt          0.0734
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_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 0.410974(15) 0.77263(2) 0.096724(12) 0.01473(7) Uani 1 1 d . . .
Cl1 Cl 0.38872(4) 0.77774(6) -0.03478(3) 0.02276(14) Uani 1 1 d . . .
Cl2 Cl 0.57129(4) 0.73100(6) 0.13061(3) 0.02650(14) Uani 1 1 d . . .
Si1 Si 0.26483(5) 0.69848(6) 0.18517(4) 0.01669(15) Uani 1 1 d . . .
N1 N 0.33883(13) 0.63036(17) 0.13067(10) 0.0175(4) Uani 1 1 d . . .
C1 C 0.30854(15) 0.8552(2) 0.17233(12) 0.0153(5) Uani 1 1 d . . .
C2 C 0.39780(16) 0.8982(2) 0.20746(12) 0.0154(5) Uani 1 1 d . . .
C3 C 0.45303(16) 0.8650(2) 0.27341(12) 0.0168(5) Uani 1 1 d . . .
H3A H 0.4316 0.8044 0.3036 0.020 Uiso 1 1 calc R . .
C4 C 0.53738(16) 0.9186(2) 0.29507(12) 0.0179(5) Uani 1 1 d . . .
C5 C 0.59118(17) 0.8774(2) 0.36781(13) 0.0225(5) Uani 1 1 d . . .
C6 C 0.6896(2) 0.9246(3) 0.37504(19) 0.0568(10) Uani 1 1 d . . .
H6A H 0.7168 0.9182 0.4271 0.068 Uiso 1 1 calc R . .
H6B H 0.7251 0.8703 0.3467 0.068 Uiso 1 1 calc R . .
C7 C 0.7016(2) 1.0457(4) 0.35175(18) 0.0610(11) Uani 1 1 d . . .
H7A H 0.7681 1.0644 0.3593 0.073 Uiso 1 1 calc R . .
H7B H 0.6718 1.1010 0.3837 0.073 Uiso 1 1 calc R . .
C8 C 0.66390(18) 1.0741(3) 0.27233(14) 0.0295(6) Uani 1 1 d . . .
C9 C 0.57164(17) 1.0092(2) 0.24998(13) 0.0202(5) Uani 1 1 d . . .
C10 C 0.52074(17) 1.0395(2) 0.18413(13) 0.0205(5) Uani 1 1 d . . .
H10A H 0.5441 1.0977 0.1534 0.025 Uiso 1 1 calc R . .
C11 C 0.43466(16) 0.9856(2) 0.16170(12) 0.0162(5) Uani 1 1 d . . .
C12 C 0.36667(16) 1.0046(2) 0.09832(12) 0.0162(5) Uani 1 1 d . . .
C13 C 0.36500(17) 1.0847(2) 0.03789(13) 0.0199(5) Uani 1 1 d . . .
H13A H 0.4174 1.1319 0.0316 0.024 Uiso 1 1 calc R . .
C14 C 0.28659(17) 1.0924(2) -0.01092(13) 0.0229(6) Uani 1 1 d . . .
H14A H 0.2850 1.1459 -0.0515 0.027 Uiso 1 1 calc R . .
C15 C 0.20712(17) 1.0226(2) -0.00292(13) 0.0211(5) Uani 1 1 d . . .
C16 C 0.20942(16) 0.9396(2) 0.05336(12) 0.0189(5) Uani 1 1 d . . .
H16A H 0.1579 0.8889 0.0566 0.023 Uiso 1 1 calc R . .
C17 C 0.28889(16) 0.9301(2) 0.10652(12) 0.0165(5) Uani 1 1 d . . .
C18 C 0.5972(2) 0.7399(3) 0.37164(17) 0.0461(8) Uani 1 1 d . . .
H18A H 0.5360 0.7060 0.3737 0.069 Uiso 1 1 calc R . .
H18B H 0.6386 0.7158 0.4156 0.069 Uiso 1 1 calc R . .
H18C H 0.6210 0.7090 0.3281 0.069 Uiso 1 1 calc R . .
C19 C 0.5428(2) 0.9237(3) 0.43056(15) 0.0453(8) Uani 1 1 d . . .
H19A H 0.4805 0.8903 0.4257 0.068 Uiso 1 1 calc R . .
H19B H 0.5398 1.0126 0.4289 0.068 Uiso 1 1 calc R . .
H19C H 0.5772 0.8979 0.4774 0.068 Uiso 1 1 calc R . .
C20 C 0.73042(19) 1.0366(3) 0.21991(18) 0.0446(8) Uani 1 1 d . . .
H20A H 0.7365 0.9479 0.2201 0.067 Uiso 1 1 calc R . .
H20B H 0.7906 1.0735 0.2356 0.067 Uiso 1 1 calc R . .
H20C H 0.7070 1.0644 0.1704 0.067 Uiso 1 1 calc R . .
C21 C 0.6516(2) 1.2126(3) 0.2675(2) 0.0543(10) Uani 1 1 d . . .
H21A H 0.6309 1.2358 0.2166 0.082 Uiso 1 1 calc R . .
H21B H 0.7103 1.2524 0.2844 0.082 Uiso 1 1 calc R . .
H21C H 0.6058 1.2379 0.2983 0.082 Uiso 1 1 calc R . .
C22 C 0.11956(18) 1.0495(3) -0.05290(15) 0.0316(6) Uani 1 1 d . . .
H22A H 0.0750 0.9831 -0.0494 0.038 Uiso 1 1 calc R . .
H22B H 0.1325 1.0533 -0.1041 0.038 Uiso 1 1 calc R . .
C23 C 0.0776(2) 1.1703(3) -0.03268(18) 0.0463(8) Uani 1 1 d . . .
H23A H 0.0210 1.1858 -0.0661 0.069 Uiso 1 1 calc R . .
H23B H 0.1214 1.2363 -0.0366 0.069 Uiso 1 1 calc R . .
H23C H 0.0635 1.1660 0.0177 0.069 Uiso 1 1 calc R . .
C24 C 0.35102(18) 0.4973(2) 0.11711(14) 0.0233(6) Uani 1 1 d . . .
C25 C 0.4046(2) 0.4814(2) 0.05205(16) 0.0333(7) Uani 1 1 d . . .
H25A H 0.4653 0.5190 0.0636 0.050 Uiso 1 1 calc R . .
H25B H 0.3710 0.5204 0.0086 0.050 Uiso 1 1 calc R . .
H25C H 0.4118 0.3946 0.0424 0.050 Uiso 1 1 calc R . .
C26 C 0.4052(2) 0.4392(3) 0.18497(16) 0.0377(7) Uani 1 1 d . . .
H26A H 0.3706 0.4474 0.2265 0.057 Uiso 1 1 calc R . .
H26B H 0.4646 0.4800 0.1964 0.057 Uiso 1 1 calc R . .
H26C H 0.4150 0.3529 0.1755 0.057 Uiso 1 1 calc R . .
C27 C 0.25740(19) 0.4361(2) 0.09898(16) 0.0343(7) Uani 1 1 d . . .
H27A H 0.2245 0.4404 0.1416 0.051 Uiso 1 1 calc R . .
H27B H 0.2659 0.3509 0.0862 0.051 Uiso 1 1 calc R . .
H27C H 0.2217 0.4779 0.0575 0.051 Uiso 1 1 calc R . .
C28 C 0.28188(19) 0.6461(2) 0.28194(13) 0.0266(6) Uani 1 1 d . . .
H28A H 0.2543 0.5655 0.2850 0.040 Uiso 1 1 calc R . .
H28B H 0.2526 0.7035 0.3121 0.040 Uiso 1 1 calc R . .
H28C H 0.3478 0.6416 0.2998 0.040 Uiso 1 1 calc R . .
C29 C 0.13957(16) 0.6845(2) 0.15146(14) 0.0259(6) Uani 1 1 d . . .
H29A H 0.1178 0.6044 0.1647 0.039 Uiso 1 1 calc R . .
H29B H 0.1293 0.6938 0.0981 0.039 Uiso 1 1 calc R . .
H29C H 0.1059 0.7479 0.1739 0.039 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 0.01516(12) 0.01681(12) 0.01297(11) 0.00136(10) 0.00460(8) 0.00095(10)
Cl1 0.0270(3) 0.0280(3) 0.0139(3) 0.0008(3) 0.0053(2) -0.0004(3)
Cl2 0.0175(3) 0.0347(4) 0.0274(3) 0.0001(3) 0.0034(2) 0.0055(3)
Si1 0.0182(3) 0.0171(4) 0.0157(3) 0.0005(3) 0.0056(3) -0.0022(3)
N1 0.0210(11) 0.016(1) 0.0163(10) 0.0011(8) 0.0051(8) 0.0010(8)
C1 0.0163(12) 0.0163(12) 0.0140(11) -0.0020(9) 0.0049(9) 0.0017(9)
C2 0.0183(12) 0.0149(12) 0.0140(11) -0.0001(9) 0.0053(9) -0.0005(9)
C3 0.0208(13) 0.0165(12) 0.0141(12) 0.0018(9) 0.0061(10) 0.001(1)
C4 0.0207(13) 0.0206(13) 0.0130(12) -0.0016(9) 0.0043(10) 0.0027(10)
C5 0.0205(13) 0.0295(15) 0.0171(12) 0.0045(11) 0.0007(10) 0.0014(11)
C6 0.039(2) 0.074(3) 0.050(2) 0.0304(19) -0.0182(16) -0.0186(18)
C7 0.049(2) 0.091(3) 0.0373(19) 0.0187(19) -0.0162(16) -0.038(2)
C8 0.0258(15) 0.0376(17) 0.0235(14) 0.0048(12) -0.0022(11) -0.0144(12)
C9 0.0206(13) 0.0226(13) 0.0177(12) -0.0033(10) 0.0033(10) -0.0035(10)
C10 0.0236(13) 0.0202(13) 0.0185(12) 0.0031(10) 0.0054(10) -0.0052(10)
C11 0.0206(13) 0.0157(12) 0.0130(11) 0.0013(9) 0.0052(10) 0.0003(9)
C12 0.0199(13) 0.0155(12) 0.0136(12) -0.0006(9) 0.0038(10) -0.0006(10)
C13 0.0225(13) 0.0185(13) 0.0193(12) 0.0022(10) 0.0051(10) -0.0025(10)
C14 0.0271(14) 0.0223(14) 0.0198(13) 0.0063(10) 0.0051(11) 0.0023(11)
C15 0.0218(13) 0.0231(14) 0.0179(12) -0.0002(10) 0.0011(10) 0.0032(10)
C16 0.0182(12) 0.0198(13) 0.0190(12) -0.0025(10) 0.0037(10) 0.001(1)
C17 0.0189(12) 0.0161(12) 0.0156(12) -0.0009(9) 0.0057(10) 0.0023(10)
C18 0.059(2) 0.0386(19) 0.0370(17) 0.0090(14) -0.0065(15) 0.0128(16)
C19 0.051(2) 0.068(2) 0.0163(14) 0.0025(14) 0.0015(13) 0.0161(17)
C20 0.0202(16) 0.060(2) 0.053(2) 0.0013(17) 0.0062(14) -0.0107(15)
C21 0.052(2) 0.046(2) 0.064(2) -0.0182(18) 0.0060(18) -0.0259(17)
C22 0.0286(15) 0.0351(16) 0.0297(15) 0.0068(13) -0.0005(12) 0.0024(13)
C23 0.0308(17) 0.0433(19) 0.063(2) 0.0135(17) 0.0013(16) 0.0111(15)
C24 0.0300(15) 0.0145(12) 0.0274(14) 0.001(1) 0.0110(11) 0.0025(11)
C25 0.0427(18) 0.0224(14) 0.0388(17) -0.0033(12) 0.0197(14) 0.0041(13)
C26 0.051(2) 0.0251(15) 0.0370(17) 0.0074(13) 0.0078(15) 0.0119(14)
C27 0.0409(17) 0.0193(14) 0.0450(18) -0.0068(13) 0.0138(14) -0.0062(12)
C28 0.0383(16) 0.0217(14) 0.0216(14) 0.0013(11) 0.0101(12) -0.0078(12)
C29 0.0206(14) 0.0242(14) 0.0332(15) -0.0015(11) 0.0051(11) -0.0028(11)
_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 N1 2.0376(19) . ?
Zr1 C1 2.370(2) . ?
Zr1 Cl2 2.3975(7) . ?
Zr1 Cl1 2.4029(7) . ?
Zr1 C2 2.496(2) . ?
Zr1 C17 2.519(2) . ?
Zr1 C11 2.633(2) . ?
Zr1 C12 2.635(2) . ?
Zr1 Si1 2.9855(7) . ?
Si1 N1 1.749(2) . ?
Si1 C28 1.860(2) . ?
Si1 C1 1.867(2) . ?
Si1 C29 1.867(2) . ?
N1 C24 1.500(3) . ?
C1 C2 1.460(3) . ?
C1 C17 1.463(3) . ?
C2 C3 1.414(3) . ?
C2 C11 1.435(3) . ?
C3 C4 1.381(3) . ?
C3 H3A 0.9500 . ?
C4 C9 1.434(3) . ?
C4 C5 1.529(3) . ?
C5 C18 1.517(4) . ?
C5 C6 1.527(4) . ?
C5 C19 1.527(4) . ?
C6 C7 1.418(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.525(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C20 1.524(4) . ?
C8 C21 1.535(4) . ?
C8 C9 1.538(3) . ?
C9 C10 1.377(3) . ?
C10 C11 1.407(3) . ?
C10 H10A 0.9500 . ?
C11 C12 1.444(3) . ?
C12 C13 1.419(3) . ?
C12 C17 1.432(3) . ?
C13 C14 1.364(3) . ?
C13 H13A 0.9500 . ?
C14 C15 1.423(3) . ?
C14 H14A 0.9500 . ?
C15 C16 1.379(3) . ?
C15 C22 1.505(3) . ?
C16 C17 1.422(3) . ?
C16 H16A 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.533(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C27 1.527(4) . ?
C24 C26 1.527(4) . ?
C24 C25 1.534(3) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 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
N1 Zr1 C1 73.36(8) . . ?
N1 Zr1 Cl2 107.93(6) . . ?
C1 Zr1 Cl2 126.98(6) . . ?
N1 Zr1 Cl1 108.92(6) . . ?
C1 Zr1 Cl1 125.17(6) . . ?
Cl2 Zr1 Cl1 105.03(2) . . ?
N1 Zr1 C2 94.09(7) . . ?
C1 Zr1 C2 34.79(7) . . ?
Cl2 Zr1 C2 94.43(6) . . ?
Cl1 Zr1 C2 142.95(6) . . ?
N1 Zr1 C17 95.75(8) . . ?
C1 Zr1 C17 34.64(7) . . ?
Cl2 Zr1 C17 142.86(6) . . ?
Cl1 Zr1 C17 93.29(5) . . ?
C2 Zr1 C17 54.81(7) . . ?
N1 Zr1 C11 125.85(7) . . ?
C1 Zr1 C11 56.36(7) . . ?
Cl2 Zr1 C11 89.32(5) . . ?
Cl1 Zr1 C11 115.44(5) . . ?
C2 Zr1 C11 32.35(7) . . ?
C17 Zr1 C11 53.55(7) . . ?
N1 Zr1 C12 126.93(7) . . ?
C1 Zr1 C12 56.23(7) . . ?
Cl2 Zr1 C12 114.69(5) . . ?
Cl1 Zr1 C12 89.39(5) . . ?
C2 Zr1 C12 53.66(7) . . ?
C17 Zr1 C12 32.15(7) . . ?
C11 Zr1 C12 31.82(7) . . ?
N1 Zr1 Si1 34.67(5) . . ?
C1 Zr1 Si1 38.69(6) . . ?
Cl2 Zr1 Si1 124.14(2) . . ?
Cl1 Zr1 Si1 123.38(2) . . ?
C2 Zr1 Si1 63.95(5) . . ?
C17 Zr1 Si1 64.85(5) . . ?
C11 Zr1 Si1 93.12(5) . . ?
C12 Zr1 Si1 93.49(5) . . ?
N1 Si1 C28 114.00(11) . . ?
N1 Si1 C1 94.05(9) . . ?
C28 Si1 C1 113.91(11) . . ?
N1 Si1 C29 115.89(11) . . ?
C28 Si1 C29 106.84(12) . . ?
C1 Si1 C29 112.03(11) . . ?
N1 Si1 Zr1 41.51(6) . . ?
C28 Si1 Zr1 126.70(9) . . ?
C1 Si1 Zr1 52.54(7) . . ?
C29 Si1 Zr1 126.30(9) . . ?
C24 N1 Si1 127.75(15) . . ?
C24 N1 Zr1 128.27(15) . . ?
Si1 N1 Zr1 103.82(9) . . ?
C2 C1 C17 104.36(19) . . ?
C2 C1 Si1 123.18(17) . . ?
C17 C1 Si1 126.44(17) . . ?
C2 C1 Zr1 77.30(12) . . ?
C17 C1 Zr1 78.25(12) . . ?
Si1 C1 Zr1 88.77(9) . . ?
C3 C2 C11 117.4(2) . . ?
C3 C2 C1 132.3(2) . . ?
C11 C2 C1 110.2(2) . . ?
C3 C2 Zr1 117.45(15) . . ?
C11 C2 Zr1 79.12(13) . . ?
C1 C2 Zr1 67.91(12) . . ?
C4 C3 C2 121.6(2) . . ?
C4 C3 H3A 119.2 . . ?
C2 C3 H3A 119.2 . . ?
C3 C4 C9 120.2(2) . . ?
C3 C4 C5 117.5(2) . . ?
C9 C4 C5 122.3(2) . . ?
C18 C5 C6 106.7(3) . . ?
C18 C5 C19 109.2(2) . . ?
C6 C5 C19 110.8(3) . . ?
C18 C5 C4 110.9(2) . . ?
C6 C5 C4 110.2(2) . . ?
C19 C5 C4 109.1(2) . . ?
C7 C6 C5 116.7(3) . . ?
C7 C6 H6A 108.1 . . ?
C5 C6 H6A 108.1 . . ?
C7 C6 H6B 108.1 . . ?
C5 C6 H6B 108.1 . . ?
H6A C6 H6B 107.3 . . ?
C6 C7 C8 116.1(3) . . ?
C6 C7 H7A 108.3 . . ?
C8 C7 H7A 108.3 . . ?
C6 C7 H7B 108.3 . . ?
C8 C7 H7B 108.3 . . ?
H7A C7 H7B 107.4 . . ?
C20 C8 C7 111.9(3) . . ?
C20 C8 C21 108.2(3) . . ?
C7 C8 C21 106.5(3) . . ?
C20 C8 C9 108.9(2) . . ?
C7 C8 C9 110.6(2) . . ?
C21 C8 C9 110.7(2) . . ?
C10 C9 C4 119.2(2) . . ?
C10 C9 C8 118.4(2) . . ?
C4 C9 C8 122.4(2) . . ?
C9 C10 C11 120.9(2) . . ?
C9 C10 H10A 119.5 . . ?
C11 C10 H10A 119.5 . . ?
C10 C11 C2 120.5(2) . . ?
C10 C11 C12 132.1(2) . . ?
C2 C11 C12 107.3(2) . . ?
C10 C11 Zr1 124.48(16) . . ?
C2 C11 Zr1 68.53(13) . . ?
C12 C11 Zr1 74.17(13) . . ?
C13 C12 C17 120.8(2) . . ?
C13 C12 C11 131.3(2) . . ?
C17 C12 C11 107.77(19) . . ?
C13 C12 Zr1 124.79(15) . . ?
C17 C12 Zr1 69.45(12) . . ?
C11 C12 Zr1 74.01(13) . . ?
C14 C13 C12 118.6(2) . . ?
C14 C13 H13A 120.7 . . ?
C12 C13 H13A 120.7 . . ?
C13 C14 C15 122.0(2) . . ?
C13 C14 H14A 119.0 . . ?
C15 C14 H14A 119.0 . . ?
C16 C15 C14 120.0(2) . . ?
C16 C15 C22 121.4(2) . . ?
C14 C15 C22 118.4(2) . . ?
C15 C16 C17 120.0(2) . . ?
C15 C16 H16A 120.0 . . ?
C17 C16 H16A 120.0 . . ?
C16 C17 C12 118.5(2) . . ?
C16 C17 C1 131.5(2) . . ?
C12 C17 C1 110.0(2) . . ?
C16 C17 Zr1 121.82(15) . . ?
C12 C17 Zr1 78.39(13) . . ?
C1 C17 Zr1 67.10(12) . . ?
C5 C18 H18A 109.5 . . ?
C5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C5 C19 H19A 109.5 . . ?
C5 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C5 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C8 C20 H20A 109.5 . . ?
C8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C21 H21A 109.5 . . ?
C8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C15 C22 C23 111.1(2) . . ?
C15 C22 H22A 109.4 . . ?
C23 C22 H22A 109.4 . . ?
C15 C22 H22B 109.4 . . ?
C23 C22 H22B 109.4 . . ?
H22A C22 H22B 108.0 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1 C24 C27 110.0(2) . . ?
N1 C24 C26 109.4(2) . . ?
C27 C24 C26 110.3(2) . . ?
N1 C24 C25 109.1(2) . . ?
C27 C24 C25 108.9(2) . . ?
C26 C24 C25 109.1(2) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si1 C28 H28A 109.5 . . ?
Si1 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
Si1 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si1 C29 H29A 109.5 . . ?
Si1 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
Si1 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.041
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.075


data_jfc5_complex5
_database_code_depnum_ccdc_archive 'CCDC 919741'
#TrackingRef '16853_web_deposit_cif_file_1_StephenA.Miller_1358192858.complex5.cif'
_audit_update_record             
;
2009-11-02 # Formatted by publCIF
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H45 Cl2 N Si Zr'
_chemical_formula_weight         621.89
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'
Si Si 0.0817 0.0704 '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   P212121
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
_cell_length_a                   8.4408(15)
_cell_length_b                   12.349(2)
_cell_length_c                   30.170(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3144.8(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    815
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      28.0
_exptl_crystal_description       cubes
_exptl_crystal_colour            gold
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1304
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8997
_exptl_absorpt_correction_T_max  0.9472
_exptl_absorpt_process_details   
'based on measured indexed crystal faces, Bruker SHELXTL v6.12 (Bruker 2007)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(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       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25282
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         1.35
_diffrn_reflns_theta_max         27.50
_reflns_number_total             7190
_reflns_number_gt                6794
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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.
;
_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^)+(0.0268P)^2^+0.8478P] 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   -0.01(2)
_refine_ls_number_reflns         7190
_refine_ls_number_parameters     337
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0224
_refine_ls_wR_factor_ref         0.0547
_refine_ls_wR_factor_gt          0.0535
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.004
_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 0.921311(18) 0.000477(13) 0.908669(4) 0.01400(4) Uani 1 1 d . . .
Cl1 Cl 1.12562(6) -0.01518(4) 0.963310(15) 0.02816(11) Uani 1 1 d . . .
Cl2 Cl 1.06171(6) 0.02487(3) 0.840335(14) 0.02504(10) Uani 1 1 d . . .
Si1 Si 0.60964(6) -0.11106(4) 0.922116(15) 0.01582(10) Uani 1 1 d . . .
N1 N 0.80210(18) -0.14243(11) 0.90493(5) 0.0149(3) Uani 1 1 d . . .
C1 C 0.6503(2) 0.03749(13) 0.92535(5) 0.0148(3) Uani 1 1 d . . .
C2 C 0.6813(2) 0.10208(14) 0.88585(6) 0.0159(4) Uani 1 1 d . . .
C3 C 0.6340(2) 0.08811(13) 0.84152(6) 0.0176(4) Uani 1 1 d . . .
H3 H 0.5648 0.0302 0.8341 0.021 Uiso 1 1 calc R . .
C4 C 0.6862(2) 0.15705(14) 0.80846(6) 0.0187(4) Uani 1 1 d . . .
C5 C 0.6242(3) 0.13652(15) 0.76150(6) 0.0247(4) Uani 1 1 d . . .
C6 C 0.7234(4) 0.20090(19) 0.72754(7) 0.0390(6) Uani 1 1 d . . .
H6A H 0.8256 0.1632 0.7229 0.047 Uiso 1 1 calc R . .
H6B H 0.6665 0.2018 0.6988 0.047 Uiso 1 1 calc R . .
C7 C 0.7554(3) 0.31402(19) 0.74133(7) 0.0406(6) Uani 1 1 d . . .
H7A H 0.6533 0.3517 0.7461 0.049 Uiso 1 1 calc R . .
H7B H 0.8117 0.3518 0.7171 0.049 Uiso 1 1 calc R . .
C8 C 0.8548(3) 0.32184(15) 0.78370(6) 0.0244(4) Uani 1 1 d . . .
C9 C 0.7896(2) 0.24485(14) 0.81903(6) 0.0192(4) Uani 1 1 d . . .
C10 C 0.8395(2) 0.25866(14) 0.86229(6) 0.0183(4) Uani 1 1 d . . .
H10 H 0.9089 0.3167 0.8694 0.022 Uiso 1 1 calc R . .
C11 C 0.7888(2) 0.18779(14) 0.89599(6) 0.0161(4) Uani 1 1 d . . .
C12 C 0.8208(2) 0.18272(14) 0.94306(6) 0.0166(4) Uani 1 1 d . . .
C13 C 0.9118(2) 0.24942(13) 0.97131(6) 0.0197(4) Uani 1 1 d . . .
H13 H 0.9696 0.3091 0.9597 0.024 Uiso 1 1 calc R . .
C14 C 0.9153(3) 0.22673(13) 1.01546(6) 0.0205(4) Uani 1 1 d . . .
H14 H 0.9763 0.2716 1.0345 0.025 Uiso 1 1 calc R . .
C15 C 0.8302(2) 0.13773(14) 1.03404(6) 0.0177(4) Uani 1 1 d . . .
C16 C 0.7422(2) 0.07225(14) 1.00683(5) 0.0158(4) Uani 1 1 d . . .
H16 H 0.6875 0.0119 1.0189 0.019 Uiso 1 1 calc R . .
C17 C 0.7322(2) 0.09402(13) 0.96063(6) 0.0153(3) Uani 1 1 d . . .
C18 C 0.6425(3) 0.01692(17) 0.74900(6) 0.0383(6) Uani 1 1 d . . .
H18A H 0.5737 -0.0272 0.7679 0.057 Uiso 1 1 calc R . .
H18B H 0.7530 -0.0052 0.7532 0.057 Uiso 1 1 calc R . .
H18C H 0.6124 0.0067 0.7179 0.057 Uiso 1 1 calc R . .
C19 C 0.4495(3) 0.1680(2) 0.75948(8) 0.0458(6) Uani 1 1 d . . .
H19A H 0.3897 0.1250 0.7811 0.069 Uiso 1 1 calc R . .
H19B H 0.4085 0.1541 0.7296 0.069 Uiso 1 1 calc R . .
H19C H 0.4381 0.2451 0.7665 0.069 Uiso 1 1 calc R . .
C20 C 0.8495(4) 0.44042(16) 0.79917(8) 0.0429(7) Uani 1 1 d . . .
H20A H 0.7426 0.4578 0.8097 0.064 Uiso 1 1 calc R . .
H20B H 0.8769 0.4881 0.7744 0.064 Uiso 1 1 calc R . .
H20C H 0.9256 0.4510 0.8233 0.064 Uiso 1 1 calc R . .
C21 C 1.0280(3) 0.29295(19) 0.77488(8) 0.0366(5) Uani 1 1 d . . .
H21A H 1.0896 0.3024 0.8021 0.055 Uiso 1 1 calc R . .
H21B H 1.0704 0.3405 0.7517 0.055 Uiso 1 1 calc R . .
H21C H 1.0352 0.2174 0.7651 0.055 Uiso 1 1 calc R . .
C22 C 0.8452(3) 0.11752(15) 1.08390(6) 0.0234(4) Uani 1 1 d . . .
C23 C 0.8062(3) 0.22146(17) 1.10963(7) 0.0336(5) Uani 1 1 d . . .
H23A H 0.6969 0.2434 1.1033 0.050 Uiso 1 1 calc R . .
H23B H 0.8788 0.2792 1.1006 0.050 Uiso 1 1 calc R . .
H23C H 0.8179 0.2081 1.1415 0.050 Uiso 1 1 calc R . .
C24 C 1.0172(3) 0.08357(19) 1.09342(8) 0.0376(5) Uani 1 1 d . . .
H24A H 1.0313 0.0733 1.1254 0.056 Uiso 1 1 calc R . .
H24B H 1.0895 0.1402 1.0830 0.056 Uiso 1 1 calc R . .
H24C H 1.0404 0.0156 1.0780 0.056 Uiso 1 1 calc R . .
C25 C 0.7355(3) 0.02710(16) 1.09977(6) 0.0306(5) Uani 1 1 d . . .
H25A H 0.6256 0.0457 1.0926 0.046 Uiso 1 1 calc R . .
H25B H 0.7466 0.0183 1.1319 0.046 Uiso 1 1 calc R . .
H25C H 0.7640 -0.0408 1.0849 0.046 Uiso 1 1 calc R . .
C26 C 0.5539(3) -0.16899(15) 0.97695(6) 0.0274(5) Uani 1 1 d . . .
H26A H 0.5191 -0.2441 0.9731 0.041 Uiso 1 1 calc R . .
H26B H 0.4675 -0.1263 0.9898 0.041 Uiso 1 1 calc R . .
H26C H 0.6457 -0.1670 0.9968 0.041 Uiso 1 1 calc R . .
C27 C 0.4497(2) -0.14725(16) 0.88225(6) 0.0251(4) Uani 1 1 d . . .
H27A H 0.4875 -0.1360 0.8519 0.038 Uiso 1 1 calc R . .
H27B H 0.3569 -0.1014 0.8876 0.038 Uiso 1 1 calc R . .
H27C H 0.4205 -0.2234 0.8862 0.038 Uiso 1 1 calc R . .
C28 C 0.8610(2) -0.24824(14) 0.88817(6) 0.0200(4) Uani 1 1 d . . .
C29 C 0.8136(3) -0.25872(17) 0.83952(7) 0.0319(5) Uani 1 1 d . . .
H29A H 0.6981 -0.2644 0.8373 0.048 Uiso 1 1 calc R . .
H29B H 0.8626 -0.3237 0.8269 0.048 Uiso 1 1 calc R . .
H29C H 0.8498 -0.1947 0.8232 0.048 Uiso 1 1 calc R . .
C30 C 1.0410(3) -0.25176(16) 0.89197(7) 0.0286(5) Uani 1 1 d . . .
H30A H 1.0871 -0.1931 0.8743 0.043 Uiso 1 1 calc R . .
H30B H 1.0799 -0.3216 0.8810 0.043 Uiso 1 1 calc R . .
H30C H 1.0719 -0.2429 0.9231 0.043 Uiso 1 1 calc R . .
C31 C 0.7893(3) -0.34112(15) 0.91495(7) 0.0308(5) Uani 1 1 d . . .
H31A H 0.8169 -0.3324 0.9463 0.046 Uiso 1 1 calc R . .
H31B H 0.8312 -0.4102 0.9041 0.046 Uiso 1 1 calc R . .
H31C H 0.6738 -0.3404 0.9117 0.046 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 0.01224(8) 0.01410(7) 0.01567(7) -0.00113(7) 0.00104(6) -0.00028(8)
Cl1 0.0189(2) 0.0370(3) 0.0285(2) -0.0096(2) -0.00782(17) 0.0048(2)
Cl2 0.0272(3) 0.0231(2) 0.0248(2) 0.00286(15) 0.01192(19) 0.00421(18)
Si1 0.0156(3) 0.0163(2) 0.0155(2) -0.00059(16) 0.00082(19) -0.00324(19)
N1 0.0162(8) 0.0137(6) 0.0147(7) -0.0007(5) -0.0002(6) 0.0001(6)
C1 0.0117(9) 0.0174(8) 0.0154(7) -0.0015(6) 0.0006(7) 0.0015(6)
C2 0.0132(9) 0.0162(8) 0.0183(8) 0.0008(6) 0.0033(7) 0.0034(7)
C3 0.0168(10) 0.0169(8) 0.0190(8) 0.0003(6) 0.0001(7) 0.0015(7)
C4 0.0198(11) 0.0189(8) 0.0174(8) 0.0008(7) 0.0012(7) 0.0051(7)
C5 0.0306(12) 0.0269(9) 0.0165(8) 0.0025(7) -0.0033(8) -0.0017(8)
C6 0.0565(18) 0.0428(12) 0.0176(9) 0.0056(9) -0.0022(10) -0.0114(12)
C7 0.0527(18) 0.0427(13) 0.0263(11) 0.0168(9) -0.0033(11) -0.0101(12)
C8 0.0313(13) 0.0221(9) 0.0197(9) 0.0052(7) 0.0037(8) -0.0030(8)
C9 0.0207(11) 0.0156(8) 0.0212(9) 0.0032(7) 0.0046(8) 0.0045(7)
C10 0.0193(11) 0.0144(8) 0.0211(9) 0.0013(7) 0.0029(8) 0.0005(7)
C11 0.0156(10) 0.0149(8) 0.0177(8) -0.0018(6) 0.0024(7) 0.0038(7)
C12 0.0167(10) 0.0147(8) 0.0185(8) -0.0015(6) 0.0026(7) 0.0011(7)
C13 0.0208(11) 0.0166(7) 0.0217(8) -0.0013(6) 0.0037(8) -0.0054(8)
C14 0.0213(11) 0.0183(8) 0.0220(8) -0.0052(6) -0.0005(8) -0.0029(8)
C15 0.0171(10) 0.0179(8) 0.0182(8) -0.0012(6) 0.0005(7) 0.0014(7)
C16 0.015(1) 0.0160(8) 0.0165(8) -0.0005(6) 0.0030(7) 0.0009(7)
C17 0.0114(9) 0.0149(8) 0.0197(8) -0.0015(6) 0.0012(7) 0.0012(6)
C18 0.0571(16) 0.0355(12) 0.0221(9) -0.0060(8) -0.0033(9) -0.0028(11)
C19 0.0360(16) 0.0677(17) 0.0336(12) 0.0065(11) -0.0126(11) 0.0075(13)
C20 0.070(2) 0.0225(10) 0.0358(12) 0.0097(9) 0.0146(12) 0.0012(11)
C21 0.0338(14) 0.0408(12) 0.0354(11) 0.0075(10) 0.0109(10) -0.0051(10)
C22 0.0264(11) 0.0265(9) 0.0175(9) 0.0014(7) -0.0044(8) -0.0068(8)
C23 0.0475(16) 0.0342(11) 0.0190(9) -0.0070(8) 0.0025(10) -0.0136(10)
C24 0.0329(13) 0.0427(12) 0.0371(11) 0.0098(10) -0.0122(11) -0.0075(10)
C25 0.0415(13) 0.0319(11) 0.0183(9) 0.0037(7) -0.0038(8) -0.0130(9)
C26 0.0367(14) 0.0236(9) 0.0220(9) 0.0016(7) 0.0097(9) -0.0083(9)
C27 0.0168(11) 0.0273(9) 0.031(1) -0.0046(8) -0.0040(8) -0.0038(8)
C28 0.0225(11) 0.0136(8) 0.0239(9) -0.0034(7) -0.0006(8) 0.0017(7)
C29 0.0398(15) 0.0289(10) 0.0269(10) -0.0126(9) -0.005(1) 0.0088(10)
C30 0.0231(12) 0.0212(9) 0.0414(11) 0.0002(8) -0.0014(9) 0.0065(8)
C31 0.0310(13) 0.0170(9) 0.0444(12) 0.0048(8) 0.0014(10) -0.0013(8)
_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 N1 2.0346(15) . ?
Zr1 C1 2.3862(18) . ?
Zr1 Cl1 2.3935(6) . ?
Zr1 Cl2 2.3969(5) . ?
Zr1 C2 2.4803(18) . ?
Zr1 C17 2.5181(18) . ?
Zr1 C11 2.5977(18) . ?
Zr1 C12 2.6193(17) . ?
Zr1 Si1 2.9971(7) . ?
Si1 N1 1.7487(16) . ?
Si1 C27 1.862(2) . ?
Si1 C26 1.8629(18) . ?
Si1 C1 1.8689(18) . ?
N1 C28 1.487(2) . ?
C1 C17 1.448(2) . ?
C1 C2 1.458(2) . ?
C2 C3 1.407(2) . ?
C2 C11 1.427(3) . ?
C3 C4 1.383(2) . ?
C3 H3 0.9500 . ?
C4 C9 1.428(3) . ?
C4 C5 1.531(2) . ?
C5 C19 1.526(3) . ?
C5 C18 1.532(3) . ?
C5 C6 1.543(3) . ?
C6 C7 1.482(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.532(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C21 1.529(3) . ?
C8 C9 1.531(2) . ?
C8 C20 1.537(3) . ?
C9 C10 1.382(3) . ?
C10 C11 1.408(2) . ?
C10 H10 0.9500 . ?
C11 C12 1.447(2) . ?
C12 C13 1.412(2) . ?
C12 C17 1.429(2) . ?
C13 C14 1.361(2) . ?
C13 H13 0.9500 . ?
C14 C15 1.428(3) . ?
C14 H14 0.9500 . ?
C15 C16 1.371(2) . ?
C15 C22 1.530(2) . ?
C16 C17 1.422(2) . ?
C16 H16 0.9500 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C25 1.527(3) . ?
C22 C23 1.536(3) . ?
C22 C24 1.539(3) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.524(3) . ?
C28 C29 1.527(3) . ?
C28 C31 1.528(3) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 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
N1 Zr1 C1 72.77(6) . . ?
N1 Zr1 Cl1 108.93(4) . . ?
C1 Zr1 Cl1 124.12(4) . . ?
N1 Zr1 Cl2 107.81(4) . . ?
C1 Zr1 Cl2 129.14(4) . . ?
Cl1 Zr1 Cl2 104.26(2) . . ?
N1 Zr1 C2 91.12(6) . . ?
C1 Zr1 C2 34.79(5) . . ?
Cl1 Zr1 C2 145.13(4) . . ?
Cl2 Zr1 C2 95.82(4) . . ?
N1 Zr1 C17 96.83(6) . . ?
C1 Zr1 C17 34.21(6) . . ?
Cl1 Zr1 C17 93.74(4) . . ?
Cl2 Zr1 C17 142.30(4) . . ?
C2 Zr1 C17 54.75(6) . . ?
N1 Zr1 C11 123.46(6) . . ?
C1 Zr1 C11 56.48(6) . . ?
Cl1 Zr1 C11 118.92(4) . . ?
Cl2 Zr1 C11 88.52(4) . . ?
C2 Zr1 C11 32.54(6) . . ?
C17 Zr1 C11 53.86(5) . . ?
N1 Zr1 C12 127.38(6) . . ?
C1 Zr1 C12 56.05(6) . . ?
Cl1 Zr1 C12 91.71(4) . . ?
Cl2 Zr1 C12 113.13(4) . . ?
C2 Zr1 C12 53.90(6) . . ?
C17 Zr1 C12 32.22(5) . . ?
C11 Zr1 C12 32.20(5) . . ?
N1 Zr1 Si1 34.39(4) . . ?
C1 Zr1 Si1 38.57(4) . . ?
Cl1 Zr1 Si1 120.137(19) . . ?
Cl2 Zr1 Si1 127.455(17) . . ?
C2 Zr1 Si1 63.46(4) . . ?
C17 Zr1 Si1 64.53(4) . . ?
C11 Zr1 Si1 92.94(5) . . ?
C12 Zr1 Si1 93.27(5) . . ?
N1 Si1 C27 115.39(8) . . ?
N1 Si1 C26 114.39(9) . . ?
C27 Si1 C26 107.35(10) . . ?
N1 Si1 C1 93.56(8) . . ?
C27 Si1 C1 113.73(8) . . ?
C26 Si1 C1 112.15(8) . . ?
N1 Si1 Zr1 41.08(5) . . ?
C27 Si1 Zr1 131.23(7) . . ?
C26 Si1 Zr1 121.23(8) . . ?
C1 Si1 Zr1 52.75(6) . . ?
C28 N1 Si1 127.32(12) . . ?
C28 N1 Zr1 128.01(12) . . ?
Si1 N1 Zr1 104.53(7) . . ?
C17 C1 C2 104.56(15) . . ?
C17 C1 Si1 126.81(13) . . ?
C2 C1 Si1 121.83(12) . . ?
C17 C1 Zr1 77.89(10) . . ?
C2 C1 Zr1 76.14(10) . . ?
Si1 C1 Zr1 88.69(7) . . ?
C3 C2 C11 118.37(16) . . ?
C3 C2 C1 131.25(16) . . ?
C11 C2 C1 110.17(15) . . ?
C3 C2 Zr1 115.71(12) . . ?
C11 C2 Zr1 78.26(11) . . ?
C1 C2 Zr1 69.07(10) . . ?
C4 C3 C2 121.30(17) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C3 C4 C9 120.07(16) . . ?
C3 C4 C5 117.14(17) . . ?
C9 C4 C5 122.76(16) . . ?
C19 C5 C4 108.96(17) . . ?
C19 C5 C18 109.42(19) . . ?
C4 C5 C18 110.67(16) . . ?
C19 C5 C6 111.49(19) . . ?
C4 C5 C6 110.10(17) . . ?
C18 C5 C6 106.18(18) . . ?
C7 C6 C5 113.46(19) . . ?
C7 C6 H6A 108.9 . . ?
C5 C6 H6A 108.9 . . ?
C7 C6 H6B 108.9 . . ?
C5 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C6 C7 C8 113.16(18) . . ?
C6 C7 H7A 108.9 . . ?
C8 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
C8 C7 H7B 108.9 . . ?
H7A C7 H7B 107.8 . . ?
C21 C8 C9 108.67(17) . . ?
C21 C8 C7 111.33(18) . . ?
C9 C8 C7 110.19(18) . . ?
C21 C8 C20 107.65(19) . . ?
C9 C8 C20 111.70(16) . . ?
C7 C8 C20 107.29(19) . . ?
C10 C9 C4 119.40(16) . . ?
C10 C9 C8 118.13(17) . . ?
C4 C9 C8 122.40(16) . . ?
C9 C10 C11 120.83(18) . . ?
C9 C10 H10 119.6 . . ?
C11 C10 H10 119.6 . . ?
C10 C11 C2 119.97(16) . . ?
C10 C11 C12 132.74(18) . . ?
C2 C11 C12 107.28(15) . . ?
C10 C11 Zr1 121.94(12) . . ?
C2 C11 Zr1 69.2(1) . . ?
C12 C11 Zr1 74.72(10) . . ?
C13 C12 C17 120.54(16) . . ?
C13 C12 C11 131.96(17) . . ?
C17 C12 C11 107.42(16) . . ?
C13 C12 Zr1 124.34(13) . . ?
C17 C12 Zr1 69.99(9) . . ?
C11 C12 Zr1 73.07(10) . . ?
C14 C13 C12 118.82(16) . . ?
C14 C13 H13 120.6 . . ?
C12 C13 H13 120.6 . . ?
C13 C14 C15 122.13(17) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C16 C15 C14 119.44(16) . . ?
C16 C15 C22 122.49(16) . . ?
C14 C15 C22 118.04(16) . . ?
C15 C16 C17 120.51(16) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C16 C17 C12 118.51(16) . . ?
C16 C17 C1 131.12(16) . . ?
C12 C17 C1 110.30(15) . . ?
C16 C17 Zr1 119.05(12) . . ?
C12 C17 Zr1 77.79(10) . . ?
C1 C17 Zr1 67.90(9) . . ?
C5 C18 H18A 109.5 . . ?
C5 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C5 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C5 C19 H19A 109.5 . . ?
C5 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C5 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C8 C20 H20A 109.5 . . ?
C8 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C8 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C21 H21A 109.5 . . ?
C8 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C8 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C25 C22 C15 112.17(16) . . ?
C25 C22 C23 108.84(17) . . ?
C15 C22 C23 110.05(16) . . ?
C25 C22 C24 108.31(17) . . ?
C15 C22 C24 107.81(17) . . ?
C23 C22 C24 109.62(18) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si1 C26 H26A 109.5 . . ?
Si1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si1 C27 H27A 109.5 . . ?
Si1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
Si1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N1 C28 C30 109.45(16) . . ?
N1 C28 C29 108.29(15) . . ?
C30 C28 C29 109.32(18) . . ?
N1 C28 C31 110.33(16) . . ?
C30 C28 C31 109.49(17) . . ?
C29 C28 C31 109.94(17) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C28 C31 H31A 109.5 . . ?
C28 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C28 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.051


data_jfc2_complex6
_database_code_depnum_ccdc_archive 'CCDC 919742'
#TrackingRef '16854_web_deposit_cif_file_2_StephenA.Miller_1358192858.complex6.cif'
_audit_update_record             
;
2009-06-11 # Formatted by publCIF
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H43 N Si Zr'
_chemical_formula_weight         524.95
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'
Si Si 0.0817 0.0704 '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           Triclinic
_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   11.1665(8)
_cell_length_b                   11.7337(8)
_cell_length_c                   11.9069(8)
_cell_angle_alpha                89.864(1)
_cell_angle_beta                 65.186(1)
_cell_angle_gamma                77.355(1)
_cell_volume                     1374.64(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    295
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      28.0
_exptl_crystal_description       plates
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.082
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             556
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6767
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   
'based on measured indexed crystal faces, Bruker SHELXTL v6.12 (Bruker 1998)'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(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       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10006
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         27.50
_reflns_number_total             5991
_reflns_number_gt                5704
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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.
;
_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^)+(0.0273P)^2^+0.7537P] 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_number_reflns         5991
_refine_ls_number_parameters     300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0604
_refine_ls_wR_factor_gt          0.0595
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.003
_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 0.261585(12) 0.325025(10) 0.158296(11) 0.01205(5) Uani 1 1 d . . .
Si1 Si 0.25460(4) 0.07937(3) 0.22677(3) 0.01341(8) Uani 1 1 d . . .
C1 C 0.39263(13) 0.12598(11) 0.09282(12) 0.0133(2) Uani 1 1 d . . .
C17 C 0.37812(13) 0.16486(11) -0.01781(12) 0.0129(2) Uani 1 1 d . . .
C2 C 0.49121(13) 0.18390(11) 0.10144(12) 0.0142(2) Uani 1 1 d . . .
C14 C 0.18287(15) 0.17781(13) -0.21803(14) 0.0195(3) Uani 1 1 d . . .
C15 C 0.28780(13) 0.19839(11) -0.17316(13) 0.0149(3) Uani 1 1 d . . .
C10 C 0.37838(14) 0.27290(11) -0.23228(12) 0.0151(3) Uani 1 1 d . . .
C8 C 0.45662(13) 0.24945(11) -0.06965(12) 0.0138(2) Uani 1 1 d . . .
C9 C 0.45833(13) 0.29921(12) -0.17757(12) 0.0151(3) Uani 1 1 d . . .
H9A H 0.5150 0.3516 -0.2136 0.018 Uiso 1 1 calc R . .
C3 C 0.54904(14) 0.18019(13) 0.18807(13) 0.0180(3) Uani 1 1 d . . .
H3A H 0.5258 0.1310 0.2536 0.022 Uiso 1 1 calc R . .
C7 C 0.52643(13) 0.26309(12) 0.00634(12) 0.0144(3) Uani 1 1 d . . .
C11 C 0.38988(15) 0.32543(12) -0.35354(13) 0.0186(3) Uani 1 1 d . . .
C6 C 0.61810(14) 0.33314(12) -0.00268(13) 0.0178(3) Uani 1 1 d . . .
H6A H 0.6409 0.3849 -0.0658 0.021 Uiso 1 1 calc R . .
C5 C 0.67349(14) 0.32489(13) 0.08153(14) 0.0209(3) Uani 1 1 d . . .
H5A H 0.7355 0.3709 0.0762 0.025 Uiso 1 1 calc R . .
C16 C 0.29104(13) 0.14460(11) -0.07061(13) 0.0147(3) Uani 1 1 d . . .
H16A H 0.2336 0.0929 -0.0347 0.018 Uiso 1 1 calc R . .
C4 C 0.63887(15) 0.24839(14) 0.17607(14) 0.0214(3) Uani 1 1 d . . .
H4A H 0.6788 0.2440 0.2329 0.026 Uiso 1 1 calc R . .
C19 C 0.53970(17) 0.30026(15) -0.44956(14) 0.0273(3) Uani 1 1 d . . .
H19A H 0.5897 0.3412 -0.4192 0.041 Uiso 1 1 calc R . .
H19B H 0.5448 0.3280 -0.5288 0.041 Uiso 1 1 calc R . .
H19C H 0.5799 0.2156 -0.4618 0.041 Uiso 1 1 calc R . .
C18 C 0.33285(17) 0.45935(13) -0.32756(15) 0.0251(3) Uani 1 1 d . . .
H18A H 0.3868 0.4941 -0.2965 0.038 Uiso 1 1 calc R . .
H18B H 0.2381 0.4770 -0.2651 0.038 Uiso 1 1 calc R . .
H18C H 0.3374 0.4922 -0.4046 0.038 Uiso 1 1 calc R . .
N1 N 0.14691(11) 0.21953(10) 0.27258(11) 0.0140(2) Uani 1 1 d . . .
C26 C 0.00210(14) 0.25642(12) 0.36294(13) 0.0166(3) Uani 1 1 d . . .
C25 C 0.31376(16) 0.01703(13) 0.34484(14) 0.0221(3) Uani 1 1 d . . .
H25A H 0.2436 -0.0165 0.4066 0.033 Uiso 1 1 calc R . .
H25B H 0.3309 0.0795 0.3863 0.033 Uiso 1 1 calc R . .
H25C H 0.3977 -0.0445 0.3033 0.033 Uiso 1 1 calc R . .
C29 C -0.08895(14) 0.24066(13) 0.29977(14) 0.0216(3) Uani 1 1 d . . .
H29A H -0.0711 0.2873 0.2286 0.032 Uiso 1 1 calc R . .
H29B H -0.1846 0.2671 0.3594 0.032 Uiso 1 1 calc R . .
H29C H -0.0693 0.1576 0.2709 0.032 Uiso 1 1 calc R . .
C24 C 0.18199(15) -0.03319(12) 0.18244(14) 0.0212(3) Uani 1 1 d . . .
H24A H 0.1158 -0.0568 0.2578 0.032 Uiso 1 1 calc R . .
H24B H 0.2553 -0.1019 0.1357 0.032 Uiso 1 1 calc R . .
H24C H 0.1370 0.0003 0.1306 0.032 Uiso 1 1 calc R . .
C27 C -0.02912(16) 0.38625(13) 0.40858(16) 0.0256(3) Uani 1 1 d . . .
H27A H -0.0097 0.4330 0.3375 0.038 Uiso 1 1 calc R . .
H27B H 0.0276 0.3960 0.4505 0.038 Uiso 1 1 calc R . .
H27C H -0.1252 0.4128 0.4670 0.038 Uiso 1 1 calc R . .
C21 C 0.04123(15) 0.19961(15) -0.10751(16) 0.0265(3) Uani 1 1 d . . .
H21A H 0.0186 0.2776 -0.0640 0.040 Uiso 1 1 calc R . .
H21B H 0.0417 0.1398 -0.0500 0.040 Uiso 1 1 calc R . .
H21C H -0.0266 0.1953 -0.1382 0.040 Uiso 1 1 calc R . .
C28 C -0.02757(16) 0.18434(15) 0.47500(15) 0.0263(3) Uani 1 1 d . . .
H28A H 0.0333 0.1911 0.5133 0.039 Uiso 1 1 calc R . .
H28B H -0.0128 0.1018 0.4474 0.039 Uiso 1 1 calc R . .
H28C H -0.1221 0.2141 0.5360 0.039 Uiso 1 1 calc R . .
C20 C 0.22325(17) 0.05035(14) -0.27709(16) 0.0263(3) Uani 1 1 d . . .
H20A H 0.3140 0.0351 -0.3465 0.039 Uiso 1 1 calc R . .
H20B H 0.1574 0.0388 -0.3078 0.039 Uiso 1 1 calc R . .
H20C H 0.2240 -0.0039 -0.2145 0.039 Uiso 1 1 calc R . .
C22 C 0.14044(15) 0.43915(12) 0.07098(14) 0.0199(3) Uani 1 1 d . . .
H22A H 0.1278 0.5219 0.0963 0.030 Uiso 1 1 calc R . .
H22B H 0.0515 0.4208 0.0984 0.030 Uiso 1 1 calc R . .
H22C H 0.1893 0.4243 -0.0198 0.030 Uiso 1 1 calc R . .
C23 C 0.30491(15) 0.45146(13) 0.27207(14) 0.0199(3) Uani 1 1 d . . .
H23A H 0.2439 0.5291 0.2844 0.030 Uiso 1 1 calc R . .
H23B H 0.3994 0.4573 0.2279 0.030 Uiso 1 1 calc R . .
H23C H 0.2902 0.4227 0.3531 0.030 Uiso 1 1 calc R . .
C12 C 0.31229(19) 0.27070(15) -0.41016(15) 0.0285(3) Uani 1 1 d . . .
H12A H 0.3016 0.3181 -0.4757 0.034 Uiso 1 1 calc R . .
H12B H 0.3657 0.1906 -0.4495 0.034 Uiso 1 1 calc R . .
C13 C 0.17301(18) 0.26426(15) -0.31270(17) 0.0288(4) Uani 1 1 d . . .
H13A H 0.1213 0.2393 -0.3544 0.035 Uiso 1 1 calc R . .
H13B H 0.1226 0.3433 -0.2684 0.035 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 0.01255(7) 0.01135(7) 0.01207(7) 0.00108(4) -0.00483(5) -0.00348(5)
Si1 0.01477(17) 0.01249(16) 0.01333(18) 0.00245(13) -0.00588(14) -0.00430(13)
C1 0.0131(6) 0.0134(6) 0.0129(6) 0.0004(5) -0.0058(5) -0.0020(5)
C17 0.0123(6) 0.0127(6) 0.0117(6) -0.0003(4) -0.0036(5) -0.0021(5)
C2 0.0120(6) 0.0149(6) 0.0138(6) -0.0003(5) -0.0048(5) -0.0013(5)
C14 0.0232(7) 0.0199(7) 0.0229(7) 0.0040(5) -0.0157(6) -0.0078(5)
C15 0.0158(6) 0.0146(6) 0.0157(6) -0.0002(5) -0.0082(5) -0.0031(5)
C10 0.0175(6) 0.0146(6) 0.0122(6) 0.0011(5) -0.0060(5) -0.0028(5)
C8 0.0126(6) 0.0154(6) 0.0123(6) -0.0003(5) -0.0044(5) -0.0031(5)
C9 0.0145(6) 0.0157(6) 0.0138(6) 0.0020(5) -0.0041(5) -0.0056(5)
C3 0.0170(6) 0.0220(7) 0.0159(7) 0.0032(5) -0.0083(5) -0.0040(5)
C7 0.0123(6) 0.0176(6) 0.0122(6) 0.0006(5) -0.0041(5) -0.0036(5)
C11 0.0243(7) 0.0190(7) 0.0159(7) 0.0051(5) -0.0112(6) -0.0067(5)
C6 0.0160(6) 0.0212(7) 0.0163(7) 0.0018(5) -0.0059(5) -0.0069(5)
C5 0.0167(6) 0.0267(7) 0.0216(7) -0.0001(6) -0.0083(6) -0.0096(6)
C16 0.0147(6) 0.0148(6) 0.0154(6) 0.0011(5) -0.0064(5) -0.0052(5)
C4 0.0191(7) 0.0288(8) 0.0202(7) 0.0016(6) -0.0121(6) -0.0062(6)
C19 0.0305(8) 0.0326(8) 0.0151(7) 0.0067(6) -0.0068(6) -0.0064(7)
C18 0.0334(8) 0.0193(7) 0.0267(8) 0.0077(6) -0.0165(7) -0.0066(6)
N1 0.0130(5) 0.0144(5) 0.0137(5) 0.0006(4) -0.0045(4) -0.0038(4)
C26 0.0139(6) 0.0190(6) 0.0147(6) 0.0000(5) -0.0034(5) -0.0050(5)
C25 0.0249(7) 0.0229(7) 0.0203(7) 0.0085(6) -0.0111(6) -0.0066(6)
C29 0.0160(6) 0.0260(7) 0.0226(7) 0.0006(6) -0.0080(6) -0.0054(6)
C24 0.0223(7) 0.0173(6) 0.0231(7) 0.0005(5) -0.0070(6) -0.0086(5)
C27 0.0200(7) 0.0215(7) 0.0270(8) -0.0078(6) -0.0032(6) -0.0027(6)
C21 0.0197(7) 0.0327(8) 0.0328(9) 0.0033(7) -0.0157(7) -0.0081(6)
C28 0.0223(7) 0.0352(8) 0.0176(7) 0.0066(6) -0.0038(6) -0.0092(6)
C20 0.0352(8) 0.0228(7) 0.0309(8) 0.0014(6) -0.0221(7) -0.0104(6)
C22 0.0210(7) 0.0181(6) 0.0200(7) 0.0033(5) -0.0091(6) -0.0027(5)
C23 0.0224(7) 0.0194(7) 0.0184(7) -0.0003(5) -0.0081(6) -0.0072(5)
C12 0.0470(10) 0.0317(8) 0.0221(8) 0.0112(6) -0.0244(8) -0.0193(7)
C13 0.0378(9) 0.0305(8) 0.0378(9) 0.0141(7) -0.0313(8) -0.0156(7)
_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 N1 2.0609(11) . ?
Zr1 C22 2.2549(14) . ?
Zr1 C23 2.2681(14) . ?
Zr1 C1 2.3997(13) . ?
Zr1 C17 2.5059(13) . ?
Zr1 C2 2.5425(13) . ?
Zr1 C8 2.6647(13) . ?
Zr1 C7 2.6687(13) . ?
Zr1 Si1 3.0022(4) . ?
Si1 N1 1.7424(12) . ?
Si1 C25 1.8738(15) . ?
Si1 C24 1.8740(14) . ?
Si1 C1 1.8762(14) . ?
C1 C2 1.4514(18) . ?
C1 C17 1.4538(18) . ?
C17 C16 1.4186(17) . ?
C17 C8 1.4348(18) . ?
C2 C3 1.4246(19) . ?
C2 C7 1.4429(19) . ?
C14 C13 1.537(2) . ?
C14 C15 1.5382(18) . ?
C14 C21 1.541(2) . ?
C14 C20 1.542(2) . ?
C15 C16 1.3835(19) . ?
C15 C10 1.4386(19) . ?
C10 C9 1.3880(18) . ?
C10 C11 1.5348(19) . ?
C8 C9 1.4047(19) . ?
C8 C7 1.4489(18) . ?
C9 H9A 0.9500 . ?
C3 C4 1.378(2) . ?
C3 H3A 0.9500 . ?
C7 C6 1.4179(19) . ?
C11 C12 1.534(2) . ?
C11 C18 1.539(2) . ?
C11 C19 1.540(2) . ?
C6 C5 1.375(2) . ?
C6 H6A 0.9500 . ?
C5 C4 1.416(2) . ?
C5 H5A 0.9500 . ?
C16 H16A 0.9500 . ?
C4 H4A 0.9500 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
N1 C26 1.4816(17) . ?
C26 C27 1.5330(19) . ?
C26 C28 1.534(2) . ?
C26 C29 1.5357(19) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C12 C13 1.519(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Zr1 C22 109.55(5) . . ?
N1 Zr1 C23 110.15(5) . . ?
C22 Zr1 C23 105.35(5) . . ?
N1 Zr1 C1 72.78(4) . . ?
C22 Zr1 C1 128.50(5) . . ?
C23 Zr1 C1 122.47(5) . . ?
N1 Zr1 C17 91.65(4) . . ?
C22 Zr1 C17 95.47(5) . . ?
C23 Zr1 C17 141.94(5) . . ?
C1 Zr1 C17 34.39(4) . . ?
N1 Zr1 C2 96.14(4) . . ?
C22 Zr1 C2 141.27(5) . . ?
C23 Zr1 C2 91.62(5) . . ?
C1 Zr1 C2 34.00(4) . . ?
C17 Zr1 C2 54.20(4) . . ?
N1 Zr1 C8 123.35(4) . . ?
C22 Zr1 C8 88.35(5) . . ?
C23 Zr1 C8 116.01(5) . . ?
C1 Zr1 C8 55.59(4) . . ?
C17 Zr1 C8 32.03(4) . . ?
C2 Zr1 C8 53.02(4) . . ?
N1 Zr1 C7 126.65(4) . . ?
C22 Zr1 C7 112.24(5) . . ?
C23 Zr1 C7 89.14(5) . . ?
C1 Zr1 C7 55.54(4) . . ?
C17 Zr1 C7 53.21(4) . . ?
C2 Zr1 C7 32.03(4) . . ?
C8 Zr1 C7 31.53(4) . . ?
N1 Zr1 Si1 34.28(3) . . ?
C22 Zr1 Si1 128.24(4) . . ?
C23 Zr1 Si1 120.20(4) . . ?
C1 Zr1 Si1 38.66(3) . . ?
C17 Zr1 Si1 63.63(3) . . ?
C2 Zr1 Si1 64.11(3) . . ?
C8 Zr1 Si1 92.40(3) . . ?
C7 Zr1 Si1 92.74(3) . . ?
N1 Si1 C25 114.50(6) . . ?
N1 Si1 C24 114.46(6) . . ?
C25 Si1 C24 106.56(7) . . ?
N1 Si1 C1 94.58(6) . . ?
C25 Si1 C1 112.05(6) . . ?
C24 Si1 C1 114.67(6) . . ?
N1 Si1 Zr1 41.78(4) . . ?
C25 Si1 Zr1 121.84(5) . . ?
C24 Si1 Zr1 131.32(5) . . ?
C1 Si1 Zr1 53.03(4) . . ?
C2 C1 C17 104.70(11) . . ?
C2 C1 Si1 125.80(10) . . ?
C17 C1 Si1 123.06(9) . . ?
C2 C1 Zr1 78.40(7) . . ?
C17 C1 Zr1 76.81(7) . . ?
Si1 C1 Zr1 88.31(5) . . ?
C16 C17 C8 117.43(12) . . ?
C16 C17 C1 131.59(12) . . ?
C8 C17 C1 110.48(11) . . ?
C16 C17 Zr1 112.29(8) . . ?
C8 C17 Zr1 80.09(7) . . ?
C1 C17 Zr1 68.80(7) . . ?
C3 C2 C7 117.88(12) . . ?
C3 C2 C1 131.82(13) . . ?
C7 C2 C1 110.19(11) . . ?
C3 C2 Zr1 117.88(9) . . ?
C7 C2 Zr1 78.81(7) . . ?
C1 C2 Zr1 67.60(7) . . ?
C13 C14 C15 110.05(11) . . ?
C13 C14 C21 107.62(13) . . ?
C15 C14 C21 110.05(12) . . ?
C13 C14 C20 110.15(13) . . ?
C15 C14 C20 110.10(12) . . ?
C21 C14 C20 108.83(13) . . ?
C16 C15 C10 120.04(12) . . ?
C16 C15 C14 117.75(12) . . ?
C10 C15 C14 122.20(12) . . ?
C9 C10 C15 118.97(12) . . ?
C9 C10 C11 118.37(12) . . ?
C15 C10 C11 122.65(12) . . ?
C9 C8 C17 120.54(12) . . ?
C9 C8 C7 132.17(13) . . ?
C17 C8 C7 107.25(12) . . ?
C9 C8 Zr1 123.92(9) . . ?
C17 C8 Zr1 67.88(7) . . ?
C7 C8 Zr1 74.39(7) . . ?
C10 C9 C8 120.88(12) . . ?
C10 C9 H9A 119.6 . . ?
C8 C9 H9A 119.6 . . ?
C4 C3 C2 119.51(14) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C6 C7 C2 121.22(12) . . ?
C6 C7 C8 131.59(13) . . ?
C2 C7 C8 107.15(11) . . ?
C6 C7 Zr1 123.34(9) . . ?
C2 C7 Zr1 69.16(7) . . ?
C8 C7 Zr1 74.08(7) . . ?
C12 C11 C10 110.41(12) . . ?
C12 C11 C18 110.05(12) . . ?
C10 C11 C18 109.69(12) . . ?
C12 C11 C19 107.83(13) . . ?
C10 C11 C19 110.43(12) . . ?
C18 C11 C19 108.39(12) . . ?
C5 C6 C7 118.83(14) . . ?
C5 C6 H6A 120.6 . . ?
C7 C6 H6A 120.6 . . ?
C6 C5 C4 120.58(13) . . ?
C6 C5 H5A 119.7 . . ?
C4 C5 H5A 119.7 . . ?
C15 C16 C17 121.59(12) . . ?
C15 C16 H16A 119.2 . . ?
C17 C16 H16A 119.2 . . ?
C3 C4 C5 121.96(13) . . ?
C3 C4 H4A 119.0 . . ?
C5 C4 H4A 119.0 . . ?
C11 C19 H19A 109.5 . . ?
C11 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C11 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C11 C18 H18A 109.5 . . ?
C11 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C11 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C26 N1 Si1 129.41(9) . . ?
C26 N1 Zr1 126.41(9) . . ?
Si1 N1 Zr1 103.94(5) . . ?
N1 C26 C27 108.32(11) . . ?
N1 C26 C28 111.08(12) . . ?
C27 C26 C28 108.88(13) . . ?
N1 C26 C29 109.89(11) . . ?
C27 C26 C29 109.50(12) . . ?
C28 C26 C29 109.15(12) . . ?
Si1 C25 H25A 109.5 . . ?
Si1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si1 C24 H24A 109.5 . . ?
Si1 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si1 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C14 C21 H21A 109.5 . . ?
C14 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C14 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C14 C20 H20A 109.5 . . ?
C14 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C14 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Zr1 C22 H22A 109.5 . . ?
Zr1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Zr1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Zr1 C23 H23A 109.5 . . ?
Zr1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Zr1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C13 C12 C11 111.74(13) . . ?
C13 C12 H12A 109.3 . . ?
C11 C12 H12A 109.3 . . ?
C13 C12 H12B 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 107.9 . . ?
C12 C13 C14 111.93(13) . . ?
C12 C13 H13A 109.2 . . ?
C14 C13 H13A 109.2 . . ?
C12 C13 H13B 109.2 . . ?
C14 C13 H13B 109.2 . . ?
H13A C13 H13B 107.9 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C22 Zr1 Si1 N1 -66.45(7) . . . . ?
C23 Zr1 Si1 N1 81.60(7) . . . . ?
C1 Zr1 Si1 N1 -172.93(8) . . . . ?
C17 Zr1 Si1 N1 -141.66(7) . . . . ?
C2 Zr1 Si1 N1 157.36(7) . . . . ?
C8 Zr1 Si1 N1 -156.24(6) . . . . ?
C7 Zr1 Si1 N1 172.21(6) . . . . ?
N1 Zr1 Si1 C25 -92.15(8) . . . . ?
C22 Zr1 Si1 C25 -158.61(8) . . . . ?
C23 Zr1 Si1 C25 -10.55(7) . . . . ?
C1 Zr1 Si1 C25 94.92(8) . . . . ?
C17 Zr1 Si1 C25 126.19(7) . . . . ?
C2 Zr1 Si1 C25 65.21(7) . . . . ?
C8 Zr1 Si1 C25 111.61(7) . . . . ?
C7 Zr1 Si1 C25 80.05(7) . . . . ?
N1 Zr1 Si1 C24 80.99(8) . . . . ?
C22 Zr1 Si1 C24 14.54(8) . . . . ?
C23 Zr1 Si1 C24 162.60(8) . . . . ?
C1 Zr1 Si1 C24 -91.93(8) . . . . ?
C17 Zr1 Si1 C24 -60.66(7) . . . . ?
C2 Zr1 Si1 C24 -121.65(7) . . . . ?
C8 Zr1 Si1 C24 -75.24(7) . . . . ?
C7 Zr1 Si1 C24 -106.80(7) . . . . ?
N1 Zr1 Si1 C1 172.93(8) . . . . ?
C22 Zr1 Si1 C1 106.48(7) . . . . ?
C23 Zr1 Si1 C1 -105.47(7) . . . . ?
C17 Zr1 Si1 C1 31.27(6) . . . . ?
C2 Zr1 Si1 C1 -29.71(6) . . . . ?
C8 Zr1 Si1 C1 16.69(6) . . . . ?
C7 Zr1 Si1 C1 -14.86(6) . . . . ?
N1 Si1 C1 C2 79.10(12) . . . . ?
C25 Si1 C1 C2 -39.68(13) . . . . ?
C24 Si1 C1 C2 -161.31(11) . . . . ?
Zr1 Si1 C1 C2 74.38(11) . . . . ?
N1 Si1 C1 C17 -68.32(11) . . . . ?
C25 Si1 C1 C17 172.91(10) . . . . ?
C24 Si1 C1 C17 51.27(12) . . . . ?
Zr1 Si1 C1 C17 -73.04(10) . . . . ?
N1 Si1 C1 Zr1 4.72(5) . . . . ?
C25 Si1 C1 Zr1 -114.05(6) . . . . ?
C24 Si1 C1 Zr1 124.32(6) . . . . ?
N1 Zr1 C1 C2 -131.28(9) . . . . ?
C22 Zr1 C1 C2 127.11(8) . . . . ?
C23 Zr1 C1 C2 -27.96(10) . . . . ?
C17 Zr1 C1 C2 108.31(11) . . . . ?
C8 Zr1 C1 C2 73.24(8) . . . . ?
C7 Zr1 C1 C2 34.78(7) . . . . ?
Si1 Zr1 C1 C2 -127.12(10) . . . . ?
N1 Zr1 C1 C17 120.41(8) . . . . ?
C22 Zr1 C1 C17 18.80(10) . . . . ?
C23 Zr1 C1 C17 -136.27(8) . . . . ?
C2 Zr1 C1 C17 -108.31(11) . . . . ?
C8 Zr1 C1 C17 -35.07(7) . . . . ?
C7 Zr1 C1 C17 -73.53(8) . . . . ?
Si1 Zr1 C1 C17 124.58(9) . . . . ?
N1 Zr1 C1 Si1 -4.16(4) . . . . ?
C22 Zr1 C1 Si1 -105.77(6) . . . . ?
C23 Zr1 C1 Si1 99.15(6) . . . . ?
C17 Zr1 C1 Si1 -124.58(9) . . . . ?
C2 Zr1 C1 Si1 127.12(10) . . . . ?
C8 Zr1 C1 Si1 -159.64(7) . . . . ?
C7 Zr1 C1 Si1 161.90(7) . . . . ?
C2 C1 C17 C16 -175.56(13) . . . . ?
Si1 C1 C17 C16 -22.4(2) . . . . ?
Zr1 C1 C17 C16 -101.52(14) . . . . ?
C2 C1 C17 C8 -4.03(14) . . . . ?
Si1 C1 C17 C8 149.13(10) . . . . ?
Zr1 C1 C17 C8 70.01(9) . . . . ?
C2 C1 C17 Zr1 -74.04(8) . . . . ?
Si1 C1 C17 Zr1 79.12(9) . . . . ?
N1 Zr1 C17 C16 72.13(10) . . . . ?
C22 Zr1 C17 C16 -37.69(10) . . . . ?
C23 Zr1 C17 C16 -161.29(9) . . . . ?
C1 Zr1 C17 C16 127.63(13) . . . . ?
C2 Zr1 C17 C16 168.51(12) . . . . ?
C8 Zr1 C17 C16 -115.71(13) . . . . ?
C7 Zr1 C17 C16 -151.47(11) . . . . ?
Si1 Zr1 C17 C16 92.59(9) . . . . ?
N1 Zr1 C17 C8 -172.16(8) . . . . ?
C22 Zr1 C17 C8 78.02(8) . . . . ?
C23 Zr1 C17 C8 -45.58(11) . . . . ?
C1 Zr1 C17 C8 -116.66(11) . . . . ?
C2 Zr1 C17 C8 -75.78(8) . . . . ?
C7 Zr1 C17 C8 -35.76(7) . . . . ?
Si1 Zr1 C17 C8 -151.70(8) . . . . ?
N1 Zr1 C17 C1 -55.50(8) . . . . ?
C22 Zr1 C17 C1 -165.32(8) . . . . ?
C23 Zr1 C17 C1 71.08(11) . . . . ?
C2 Zr1 C17 C1 40.88(7) . . . . ?
C8 Zr1 C17 C1 116.66(11) . . . . ?
C7 Zr1 C17 C1 80.90(8) . . . . ?
Si1 Zr1 C17 C1 -35.04(6) . . . . ?
C17 C1 C2 C3 -179.09(14) . . . . ?
Si1 C1 C2 C3 28.7(2) . . . . ?
Zr1 C1 C2 C3 108.05(15) . . . . ?
C17 C1 C2 C7 4.90(14) . . . . ?
Si1 C1 C2 C7 -147.29(10) . . . . ?
Zr1 C1 C2 C7 -67.96(9) . . . . ?
C17 C1 C2 Zr1 72.86(8) . . . . ?
Si1 C1 C2 Zr1 -79.33(9) . . . . ?
N1 Zr1 C2 C3 -80.50(11) . . . . ?
C22 Zr1 C2 C3 147.26(10) . . . . ?
C23 Zr1 C2 C3 29.97(11) . . . . ?
C1 Zr1 C2 C3 -126.72(15) . . . . ?
C17 Zr1 C2 C3 -168.10(13) . . . . ?
C8 Zr1 C2 C3 151.83(13) . . . . ?
C7 Zr1 C2 C3 115.76(14) . . . . ?
Si1 Zr1 C2 C3 -93.10(11) . . . . ?
N1 Zr1 C2 C7 163.74(8) . . . . ?
C22 Zr1 C2 C7 31.50(11) . . . . ?
C23 Zr1 C2 C7 -85.79(8) . . . . ?
C1 Zr1 C2 C7 117.52(11) . . . . ?
C17 Zr1 C2 C7 76.14(8) . . . . ?
C8 Zr1 C2 C7 36.08(7) . . . . ?
Si1 Zr1 C2 C7 151.14(8) . . . . ?
N1 Zr1 C2 C1 46.22(8) . . . . ?
C22 Zr1 C2 C1 -86.02(10) . . . . ?
C23 Zr1 C2 C1 156.69(8) . . . . ?
C17 Zr1 C2 C1 -41.39(7) . . . . ?
C8 Zr1 C2 C1 -81.45(8) . . . . ?
C7 Zr1 C2 C1 -117.52(11) . . . . ?
Si1 Zr1 C2 C1 33.62(7) . . . . ?
C13 C14 C15 C16 167.69(13) . . . . ?
C21 C14 C15 C16 49.25(16) . . . . ?
C20 C14 C15 C16 -70.71(16) . . . . ?
C13 C14 C15 C10 -10.81(18) . . . . ?
C21 C14 C15 C10 -129.25(14) . . . . ?
C20 C14 C15 C10 110.79(15) . . . . ?
C16 C15 C10 C9 -6.51(19) . . . . ?
C14 C15 C10 C9 171.96(12) . . . . ?
C16 C15 C10 C11 173.86(12) . . . . ?
C14 C15 C10 C11 -7.67(19) . . . . ?
C16 C17 C8 C9 -7.29(18) . . . . ?
C1 C17 C8 C9 179.84(12) . . . . ?
Zr1 C17 C8 C9 -117.36(12) . . . . ?
C16 C17 C8 C7 174.58(11) . . . . ?
C1 C17 C8 C7 1.71(14) . . . . ?
Zr1 C17 C8 C7 64.51(9) . . . . ?
C16 C17 C8 Zr1 110.07(11) . . . . ?
C1 C17 C8 Zr1 -62.80(9) . . . . ?
N1 Zr1 C8 C9 122.20(11) . . . . ?
C22 Zr1 C8 C9 9.76(11) . . . . ?
C23 Zr1 C8 C9 -96.53(11) . . . . ?
C1 Zr1 C8 C9 150.53(12) . . . . ?
C17 Zr1 C8 C9 112.81(14) . . . . ?
C2 Zr1 C8 C9 -167.38(13) . . . . ?
C7 Zr1 C8 C9 -130.70(15) . . . . ?
Si1 Zr1 C8 C9 137.97(11) . . . . ?
N1 Zr1 C8 C17 9.39(9) . . . . ?
C22 Zr1 C8 C17 -103.05(8) . . . . ?
C23 Zr1 C8 C17 150.66(8) . . . . ?
C1 Zr1 C8 C17 37.72(7) . . . . ?
C2 Zr1 C8 C17 79.81(8) . . . . ?
C7 Zr1 C8 C17 116.49(11) . . . . ?
Si1 Zr1 C8 C17 25.16(7) . . . . ?
N1 Zr1 C8 C7 -107.09(8) . . . . ?
C22 Zr1 C8 C7 140.46(8) . . . . ?
C23 Zr1 C8 C7 34.17(9) . . . . ?
C1 Zr1 C8 C7 -78.76(8) . . . . ?
C17 Zr1 C8 C7 -116.49(11) . . . . ?
C2 Zr1 C8 C7 -36.68(7) . . . . ?
Si1 Zr1 C8 C7 -91.33(7) . . . . ?
C15 C10 C9 C8 3.24(19) . . . . ?
C11 C10 C9 C8 -177.11(12) . . . . ?
C17 C8 C9 C10 3.70(19) . . . . ?
C7 C8 C9 C10 -178.70(13) . . . . ?
Zr1 C8 C9 C10 -78.82(15) . . . . ?
C7 C2 C3 C4 -2.09(19) . . . . ?
C1 C2 C3 C4 -177.86(14) . . . . ?
Zr1 C2 C3 C4 -93.89(14) . . . . ?
C3 C2 C7 C6 1.43(19) . . . . ?
C1 C2 C7 C6 178.07(12) . . . . ?
Zr1 C2 C7 C6 117.19(12) . . . . ?
C3 C2 C7 C8 179.36(11) . . . . ?
C1 C2 C7 C8 -4.00(14) . . . . ?
Zr1 C2 C7 C8 -64.88(9) . . . . ?
C3 C2 C7 Zr1 -115.76(12) . . . . ?
C1 C2 C7 Zr1 60.88(9) . . . . ?
C9 C8 C7 C6 1.2(2) . . . . ?
C17 C8 C7 C6 179.02(14) . . . . ?
Zr1 C8 C7 C6 -120.73(15) . . . . ?
C9 C8 C7 C2 -176.45(14) . . . . ?
C17 C8 C7 C2 1.38(14) . . . . ?
Zr1 C8 C7 C2 61.63(9) . . . . ?
C9 C8 C7 Zr1 121.92(15) . . . . ?
C17 C8 C7 Zr1 -60.25(9) . . . . ?
N1 Zr1 C7 C6 -134.72(11) . . . . ?
C22 Zr1 C7 C6 86.26(12) . . . . ?
C23 Zr1 C7 C6 -19.99(12) . . . . ?
C1 Zr1 C7 C6 -151.39(13) . . . . ?
C17 Zr1 C7 C6 166.05(13) . . . . ?
C2 Zr1 C7 C6 -114.42(14) . . . . ?
C8 Zr1 C7 C6 129.69(15) . . . . ?
Si1 Zr1 C7 C6 -140.18(11) . . . . ?
N1 Zr1 C7 C2 -20.30(9) . . . . ?
C22 Zr1 C7 C2 -159.32(8) . . . . ?
C23 Zr1 C7 C2 94.43(8) . . . . ?
C1 Zr1 C7 C2 -36.97(7) . . . . ?
C17 Zr1 C7 C2 -79.53(8) . . . . ?
C8 Zr1 C7 C2 -115.89(11) . . . . ?
Si1 Zr1 C7 C2 -25.76(7) . . . . ?
N1 Zr1 C7 C8 95.59(8) . . . . ?
C22 Zr1 C7 C8 -43.43(9) . . . . ?
C23 Zr1 C7 C8 -149.68(8) . . . . ?
C1 Zr1 C7 C8 78.92(8) . . . . ?
C17 Zr1 C7 C8 36.36(7) . . . . ?
C2 Zr1 C7 C8 115.89(11) . . . . ?
Si1 Zr1 C7 C8 90.12(7) . . . . ?
C9 C10 C11 C12 170.75(13) . . . . ?
C15 C10 C11 C12 -9.61(18) . . . . ?
C9 C10 C11 C18 -67.80(16) . . . . ?
C15 C10 C11 C18 111.83(14) . . . . ?
C9 C10 C11 C19 51.60(17) . . . . ?
C15 C10 C11 C19 -128.77(14) . . . . ?
C2 C7 C6 C5 -0.2(2) . . . . ?
C8 C7 C6 C5 -177.54(14) . . . . ?
Zr1 C7 C6 C5 84.12(15) . . . . ?
C7 C6 C5 C4 -0.4(2) . . . . ?
C10 C15 C16 C17 2.8(2) . . . . ?
C14 C15 C16 C17 -175.75(12) . . . . ?
C8 C17 C16 C15 4.02(19) . . . . ?
C1 C17 C16 C15 175.08(13) . . . . ?
Zr1 C17 C16 C15 94.20(13) . . . . ?
C2 C3 C4 C5 1.6(2) . . . . ?
C6 C5 C4 C3 -0.3(2) . . . . ?
C25 Si1 N1 C26 -74.43(13) . . . . ?
C24 Si1 N1 C26 49.04(13) . . . . ?
C1 Si1 N1 C26 168.80(12) . . . . ?
Zr1 Si1 N1 C26 174.46(15) . . . . ?
C25 Si1 N1 Zr1 111.11(7) . . . . ?
C24 Si1 N1 Zr1 -125.42(6) . . . . ?
C1 Si1 N1 Zr1 -5.66(6) . . . . ?
C22 Zr1 N1 C26 -44.51(11) . . . . ?
C23 Zr1 N1 C26 70.93(11) . . . . ?
C1 Zr1 N1 C26 -170.07(11) . . . . ?
C17 Zr1 N1 C26 -140.90(10) . . . . ?
C2 Zr1 N1 C26 164.93(10) . . . . ?
C8 Zr1 N1 C26 -145.87(10) . . . . ?
C7 Zr1 N1 C26 175.60(9) . . . . ?
Si1 Zr1 N1 C26 -174.68(14) . . . . ?
C22 Zr1 N1 Si1 130.18(6) . . . . ?
C23 Zr1 N1 Si1 -114.39(6) . . . . ?
C1 Zr1 N1 Si1 4.62(5) . . . . ?
C17 Zr1 N1 Si1 33.78(6) . . . . ?
C2 Zr1 N1 Si1 -20.38(6) . . . . ?
C8 Zr1 N1 Si1 28.81(7) . . . . ?
C7 Zr1 N1 Si1 -9.72(8) . . . . ?
Si1 N1 C26 C27 157.61(11) . . . . ?
Zr1 N1 C26 C27 -29.08(16) . . . . ?
Si1 N1 C26 C28 38.07(16) . . . . ?
Zr1 N1 C26 C28 -148.62(10) . . . . ?
Si1 N1 C26 C29 -82.82(14) . . . . ?
Zr1 N1 C26 C29 90.50(12) . . . . ?
C10 C11 C12 C13 45.28(17) . . . . ?
C18 C11 C12 C13 -75.95(16) . . . . ?
C19 C11 C12 C13 166.00(13) . . . . ?
C11 C12 C13 C14 -66.98(17) . . . . ?
C15 C14 C13 C12 46.61(17) . . . . ?
C21 C14 C13 C12 166.53(13) . . . . ?
C20 C14 C13 C12 -74.96(16) . . . . ?
_diffrn_measured_fraction_theta_max 0.947
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.947
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.060


data_jfc4_complex7
_database_code_depnum_ccdc_archive 'CCDC 919743'
#TrackingRef '16855_web_deposit_cif_file_3_StephenA.Miller_1358192858.complex7.cif'
_audit_update_record             
;
2013-01-09 # Formatted by publCIF
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C45 H55 Cl2 N Si Zr'
_chemical_formula_weight         800.11
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a                   15.5695(14)
_cell_length_b                   15.1100(13)
_cell_length_c                   18.8408(19)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.982(3)
_cell_angle_gamma                90.00
_cell_volume                     4080.6(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9984
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      27.89
_exptl_crystal_description       prisms
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1680
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.9113
_exptl_absorpt_correction_T_max  0.9424
_exptl_absorpt_process_details   
'based on measured indexed crystal faces, Bruker SHELXTL v6.14 (Bruker 2008)'
_exptl_special_details           ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'Bruker Triumph'
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38165
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         27.50
_reflns_number_total             9379
_reflns_number_gt                6953
_reflns_threshold_expression     I>2\s(I)
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_structure_solution    'Bruker SHELXTL (Bruker, 2008)'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
All H atoms were positioned geometrically ( C---H = 0.93/1.00 \%A) and allowed
to ride with <i>U</i>~iso~(H)= 1.2/1.5<i>U</i>~eq~(C).
Methyl ones were allowed to rotate around the corresponding C---C.
One end of the ligand is disordered whereby atoms C15, C16 of the ring and
consequently the ring's methyl groups (C22-C25) are disordered. They were
refined in two parts and their site occupation factors dependently refined. The
latter refined to 50% but was fixed at this value for the final refinement
model. All of the disordered atoms were refined with isotropic displacement
parameters.
;
_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^)+(0.0469P)^2^] 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_number_reflns         9379
_refine_ls_number_parameters     442
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0897
_refine_ls_wR_factor_gt          0.0841
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.004
_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 0.309144(13) 0.244048(13) 0.482485(12) 0.02048(6) Uani 1 1 d . . .
Si1 Si 0.11839(4) 0.16703(4) 0.41647(3) 0.02099(13) Uani 1 1 d . . .
Cl1 Cl 0.43779(4) 0.14433(4) 0.51738(3) 0.03562(15) Uani 1 1 d . . .
Cl2 Cl 0.36924(4) 0.37086(4) 0.56275(4) 0.03669(14) Uani 1 1 d . . .
N1 N 0.20478(11) 0.18632(11) 0.50728(10) 0.0222(4) Uani 1 1 d . . .
C1 C 0.17881(13) 0.23038(13) 0.36395(12) 0.0202(4) Uani 1 1 d . . .
C2 C 0.19533(14) 0.32563(13) 0.37335(12) 0.0228(4) Uani 1 1 d . . .
C3 C 0.14989(15) 0.39367(14) 0.39678(13) 0.0277(5) Uani 1 1 d . . .
H3A H 0.0959 0.3798 0.4063 0.033 Uiso 1 1 calc R . .
C4 C 0.18203(16) 0.47989(14) 0.40615(14) 0.0313(5) Uani 1 1 d . A .
C5 C 0.26546(16) 0.50179(14) 0.39476(14) 0.0303(5) Uani 1 1 d . A .
C6 C 0.31287(15) 0.43544(14) 0.37489(13) 0.0278(5) Uani 1 1 d . . .
H6A H 0.3685 0.4493 0.3677 0.033 Uiso 1 1 calc R . .
C7 C 0.28023(14) 0.34771(13) 0.36508(13) 0.0221(4) Uani 1 1 d . . .
C8 C 0.31839(14) 0.26654(12) 0.34830(12) 0.0202(4) Uani 1 1 d . . .
C9 C 0.40162(13) 0.24836(13) 0.33853(12) 0.0213(4) Uani 1 1 d . . .
H9A H 0.4441 0.2951 0.3426 0.026 Uiso 1 1 calc R . .
C10 C 0.42270(13) 0.16392(13) 0.32311(12) 0.0193(4) Uani 1 1 d . . .
C11 C 0.35656(13) 0.09409(13) 0.31387(12) 0.0194(4) Uani 1 1 d . . .
C12 C 0.27515(13) 0.11132(13) 0.32459(12) 0.0199(4) Uani 1 1 d . . .
H12A H 0.2325 0.0644 0.3194 0.024 Uiso 1 1 calc R . .
C13 C 0.25382(13) 0.19693(13) 0.34308(12) 0.0192(4) Uani 1 1 d . . .
C14 C 0.12613(19) 0.54932(15) 0.43032(16) 0.0401(6) Uani 1 1 d . . .
C15 C 0.1455(3) 0.6394(3) 0.4134(3) 0.0324(5) Uiso 0.50 1 d P A 1
H15A H 0.1168 0.6824 0.4373 0.039 Uiso 0.50 1 calc PR A 1
H15B H 0.1192 0.6495 0.3570 0.039 Uiso 0.50 1 calc PR A 1
C16 C 0.2502(3) 0.6515(3) 0.4458(3) 0.0324(5) Uiso 0.50 1 d P A 1
H16A H 0.2748 0.6360 0.5013 0.039 Uiso 0.50 1 calc PR A 1
H16B H 0.2635 0.7150 0.4422 0.039 Uiso 0.50 1 calc PR A 1
C15' C 0.1954(3) 0.6388(3) 0.4632(3) 0.0324(5) Uiso 0.50 1 d P A 2
H15C H 0.1579 0.6890 0.4691 0.039 Uiso 0.50 1 calc PR A 2
H15D H 0.2444 0.6255 0.5145 0.039 Uiso 0.50 1 calc PR A 2
C16' C 0.2404(3) 0.6644(3) 0.4083(3) 0.0324(5) Uiso 0.50 1 d P A 2
H16C H 0.1917 0.6724 0.3559 0.039 Uiso 0.50 1 calc PR A 2
H16D H 0.2738 0.7213 0.4248 0.039 Uiso 0.50 1 calc PR A 2
C17 C 0.30638(19) 0.59600(15) 0.40643(17) 0.0427(7) Uani 1 1 d . . .
C18 C 0.51847(13) 0.14633(13) 0.32008(13) 0.0234(5) Uani 1 1 d . . .
C19 C 0.51546(14) 0.06077(14) 0.27483(14) 0.0278(5) Uani 1 1 d . . .
H19A H 0.4787 0.0715 0.2193 0.033 Uiso 1 1 calc R . .
H19B H 0.5797 0.0448 0.2811 0.033 Uiso 1 1 calc R . .
C20 C 0.47321(15) -0.01528(14) 0.30130(14) 0.0301(5) Uani 1 1 d . . .
H20A H 0.5100 -0.0257 0.3568 0.036 Uiso 1 1 calc R . .
H20B H 0.4772 -0.0693 0.2731 0.036 Uiso 1 1 calc R . .
C21 C 0.37071(13) 0.00056(13) 0.28870(12) 0.0224(4) Uani 1 1 d . . .
C22 C 0.1252(8) 0.5299(6) 0.5062(7) 0.0361(4) Uiso 0.50 1 d P A 1
H22A H 0.1884 0.5361 0.5458 0.054 Uiso 0.50 1 calc PR A 1
H22B H 0.1031 0.4693 0.5067 0.054 Uiso 0.50 1 calc PR A 1
H22C H 0.0834 0.5715 0.5169 0.054 Uiso 0.50 1 calc PR A 1
C23 C 0.0097(3) 0.5358(3) 0.3705(3) 0.0361(4) Uiso 0.50 1 d P A 1
H23A H -0.0082 0.4739 0.3716 0.054 Uiso 0.50 1 calc PR A 1
H23B H 0.0004 0.5522 0.3177 0.054 Uiso 0.50 1 calc PR A 1
H23C H -0.0288 0.5738 0.3884 0.054 Uiso 0.50 1 calc PR A 1
C24 C 0.2791(3) 0.6342(3) 0.3229(3) 0.0361(4) Uiso 0.50 1 d P A 1
H24A H 0.2145 0.6178 0.2910 0.054 Uiso 0.50 1 calc PR A 1
H24B H 0.3208 0.6097 0.3001 0.054 Uiso 0.50 1 calc PR A 1
H24C H 0.2849 0.6988 0.3254 0.054 Uiso 0.50 1 calc PR A 1
C25 C 0.3987(3) 0.5975(3) 0.4540(3) 0.0361(4) Uiso 0.50 1 d P A 1
H25A H 0.4366 0.5966 0.4230 0.054 Uiso 0.50 1 calc PR A 1
H25B H 0.4134 0.5455 0.4878 0.054 Uiso 0.50 1 calc PR A 1
H25C H 0.4122 0.6514 0.4854 0.054 Uiso 0.50 1 calc PR A 1
C22' C 0.1210(8) 0.5177(6) 0.5072(7) 0.0361(4) Uiso 0.50 1 d P A 2
H22D H 0.1830 0.5222 0.5489 0.054 Uiso 0.50 1 calc PR A 2
H22E H 0.1001 0.4560 0.5018 0.054 Uiso 0.50 1 calc PR A 2
H22F H 0.0769 0.5549 0.5192 0.054 Uiso 0.50 1 calc PR A 2
C23' C 0.0449(3) 0.5733(3) 0.3717(3) 0.0361(4) Uiso 0.50 1 d P A 2
H23D H 0.0549 0.6279 0.3478 0.054 Uiso 0.50 1 calc PR A 2
H23E H -0.0034 0.5832 0.3920 0.054 Uiso 0.50 1 calc PR A 2
H23F H 0.0250 0.5261 0.3330 0.054 Uiso 0.50 1 calc PR A 2
C24' C 0.3451(3) 0.6232(3) 0.3442(3) 0.0361(4) Uiso 0.50 1 d P A 2
H24D H 0.2938 0.6246 0.2933 0.054 Uiso 0.50 1 calc PR A 2
H24E H 0.3920 0.5801 0.3440 0.054 Uiso 0.50 1 calc PR A 2
H24F H 0.3737 0.6820 0.3565 0.054 Uiso 0.50 1 calc PR A 2
C25' C 0.4045(3) 0.5980(3) 0.4903(3) 0.0361(4) Uiso 0.50 1 d P A 2
H25D H 0.4548 0.5655 0.4829 0.054 Uiso 0.50 1 calc PR A 2
H25E H 0.3908 0.5703 0.5317 0.054 Uiso 0.50 1 calc PR A 2
H25F H 0.4239 0.6595 0.5041 0.054 Uiso 0.50 1 calc PR A 2
C26 C 0.54797(16) 0.22099(15) 0.27921(16) 0.0347(6) Uani 1 1 d . . .
H26A H 0.4983 0.2316 0.2285 0.052 Uiso 1 1 calc R . .
H26B H 0.6053 0.2040 0.2729 0.052 Uiso 1 1 calc R . .
H26C H 0.5591 0.2751 0.3102 0.052 Uiso 1 1 calc R . .
C27 C 0.59062(15) 0.13787(17) 0.40278(15) 0.0382(6) Uani 1 1 d . . .
H27A H 0.6517 0.1238 0.4020 0.057 Uiso 1 1 calc R . .
H27B H 0.5718 0.0905 0.4293 0.057 Uiso 1 1 calc R . .
H27C H 0.5946 0.1939 0.4301 0.057 Uiso 1 1 calc R . .
C28 C 0.34447(15) -0.07027(13) 0.33524(13) 0.0269(5) Uani 1 1 d . . .
H28A H 0.3591 -0.1291 0.3210 0.040 Uiso 1 1 calc R . .
H28B H 0.2776 -0.0665 0.3240 0.040 Uiso 1 1 calc R . .
H28C H 0.3800 -0.0604 0.3904 0.040 Uiso 1 1 calc R . .
C29 C 0.30728(16) -0.00911(15) 0.20316(13) 0.0308(5) Uani 1 1 d . . .
H29A H 0.3227 0.0368 0.1734 0.046 Uiso 1 1 calc R . .
H29B H 0.2420 -0.0027 0.1966 0.046 Uiso 1 1 calc R . .
H29C H 0.3166 -0.0676 0.1848 0.046 Uiso 1 1 calc R . .
C30 C -0.00250(13) 0.21028(14) 0.39310(13) 0.0245(5) Uani 1 1 d . . .
C31 C -0.04291(15) 0.26589(15) 0.33018(15) 0.0348(6) Uani 1 1 d . . .
H31A H -0.0070 0.2849 0.3022 0.042 Uiso 1 1 calc R . .
C32 C -0.13496(16) 0.29458(17) 0.30702(17) 0.0436(7) Uani 1 1 d . . .
H32A H -0.1611 0.3331 0.2640 0.052 Uiso 1 1 calc R . .
C33 C -0.18787(16) 0.26675(15) 0.34686(17) 0.0412(7) Uani 1 1 d . . .
H33A H -0.2506 0.2863 0.3315 0.049 Uiso 1 1 calc R . .
C34 C -0.14982(15) 0.21058(16) 0.40907(16) 0.0364(6) Uani 1 1 d . . .
H34A H -0.1865 0.1911 0.4362 0.044 Uiso 1 1 calc R . .
C35 C -0.05805(14) 0.18245(14) 0.43202(14) 0.0302(5) Uani 1 1 d . . .
H35A H -0.0325 0.1437 0.4749 0.036 Uiso 1 1 calc R . .
C36 C 0.10406(14) 0.04618(14) 0.39261(13) 0.0239(5) Uani 1 1 d . . .
C37 C 0.17641(15) -0.01444(14) 0.42763(14) 0.0298(5) Uani 1 1 d . . .
H37A H 0.2350 0.0064 0.4632 0.036 Uiso 1 1 calc R . .
C38 C 0.16447(18) -0.10381(15) 0.41164(16) 0.0381(6) Uani 1 1 d . . .
H38A H 0.2144 -0.1437 0.4365 0.046 Uiso 1 1 calc R . .
C39 C 0.07989(19) -0.13546(16) 0.35949(16) 0.0419(6) Uani 1 1 d . . .
H39A H 0.0715 -0.1970 0.3489 0.050 Uiso 1 1 calc R . .
C40 C 0.00728(17) -0.07679(16) 0.32274(15) 0.0374(6) Uani 1 1 d . . .
H40A H -0.0506 -0.0978 0.2862 0.045 Uiso 1 1 calc R . .
C41 C 0.01991(15) 0.01254(15) 0.33985(13) 0.0290(5) Uani 1 1 d . . .
H41A H -0.0302 0.0522 0.3149 0.035 Uiso 1 1 calc R . .
C42 C 0.20750(15) 0.16767(15) 0.58584(13) 0.0282(5) Uani 1 1 d . . .
C43 C 0.30905(16) 0.16549(18) 0.64326(14) 0.0403(6) Uani 1 1 d . . .
H43A H 0.3427 0.1191 0.6283 0.060 Uiso 1 1 calc R . .
H43B H 0.3113 0.1530 0.6950 0.060 Uiso 1 1 calc R . .
H43C H 0.3383 0.2229 0.6433 0.060 Uiso 1 1 calc R . .
C44 C 0.15575(18) 0.24171(15) 0.60849(16) 0.0366(6) Uani 1 1 d . . .
H44A H 0.0909 0.2440 0.5713 0.055 Uiso 1 1 calc R . .
H44B H 0.1862 0.2985 0.6086 0.055 Uiso 1 1 calc R . .
H44C H 0.1571 0.2300 0.6601 0.055 Uiso 1 1 calc R . .
C45 C 0.16398(16) 0.07789(15) 0.58952(14) 0.0344(6) Uani 1 1 d . . .
H45A H 0.2002 0.0307 0.5784 0.052 Uiso 1 1 calc R . .
H45B H 0.0996 0.0762 0.5513 0.052 Uiso 1 1 calc R . .
H45C H 0.1643 0.0692 0.6412 0.052 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 0.01852(10) 0.02267(11) 0.02136(12) 0.00215(8) 0.00900(8) 0.00178(7)
Si1 0.0173(3) 0.0219(3) 0.0254(3) 0.0059(2) 0.0101(2) 0.0041(2)
Cl1 0.0280(3) 0.0514(4) 0.0282(3) 0.0118(3) 0.0119(2) 0.0185(2)
Cl2 0.0431(3) 0.0343(3) 0.0329(4) -0.0078(3) 0.0151(3) -0.0058(2)
N1 0.0224(8) 0.0243(10) 0.0222(10) 0.0058(7) 0.0113(8) 0.0048(7)
C1 0.0184(9) 0.0207(11) 0.0217(12) 0.0057(8) 0.0080(8) 0.0050(7)
C2 0.025(1) 0.0231(11) 0.0228(12) 0.0091(9) 0.0118(9) 0.0063(8)
C3 0.0313(11) 0.0282(12) 0.0300(14) 0.0112(10) 0.0189(10) 0.0107(9)
C4 0.0460(13) 0.0249(12) 0.0351(15) 0.0103(10) 0.0291(12) 0.0135(10)
C5 0.0433(13) 0.0193(11) 0.0363(15) 0.0071(10) 0.0244(12) 0.0062(9)
C6 0.0366(12) 0.0220(11) 0.0336(14) 0.0044(9) 0.0233(11) 0.0021(9)
C7 0.0261(10) 0.0201(11) 0.0246(12) 0.0045(9) 0.0149(9) 0.0044(8)
C8 0.0233(10) 0.0186(10) 0.0204(11) 0.0029(8) 0.0104(9) 0.0021(7)
C9 0.0209(9) 0.0198(10) 0.0248(12) 0.0001(9) 0.0108(9) -0.0021(8)
C10 0.0166(9) 0.0221(11) 0.0188(11) 0.0008(8) 0.0066(8) 0.0020(7)
C11 0.0185(9) 0.0195(10) 0.0174(11) 0.0005(8) 0.0039(8) 0.0018(7)
C12 0.0178(9) 0.0203(11) 0.0198(12) 0.0007(8) 0.0055(8) -0.0018(7)
C13 0.0165(9) 0.0220(11) 0.0177(11) 0.0039(8) 0.0051(8) 0.0023(7)
C14 0.0631(17) 0.0279(13) 0.0505(17) 0.0096(11) 0.0451(15) 0.0158(11)
C17 0.0655(17) 0.0182(12) 0.062(2) 0.0014(11) 0.0443(16) 0.0050(11)
C18 0.0180(9) 0.0223(11) 0.0312(13) -0.0034(9) 0.0109(9) 0.0008(8)
C19 0.0245(11) 0.0252(12) 0.0373(15) -0.0036(10) 0.0159(10) 0.0014(8)
C20 0.0295(11) 0.0237(12) 0.0403(15) -0.005(1) 0.0173(11) 0.0038(9)
C21 0.0221(10) 0.0195(10) 0.0260(13) -0.0028(9) 0.0097(9) -0.0014(8)
C26 0.0284(12) 0.0298(13) 0.0549(18) -0.0011(11) 0.0262(12) -0.0012(9)
C27 0.0218(11) 0.0521(16) 0.0364(15) -0.0108(12) 0.0066(10) 0.0027(10)
C28 0.0288(11) 0.0204(11) 0.0308(14) 0.0015(9) 0.0108(10) 0.0024(8)
C29 0.0389(13) 0.0264(12) 0.0254(13) -0.0039(10) 0.0106(10) -0.0068(9)
C30 0.0194(10) 0.0223(11) 0.0321(13) 0.0014(9) 0.0105(9) 0.0025(8)
C31 0.0221(11) 0.0373(14) 0.0441(16) 0.0149(11) 0.0120(11) 0.0042(9)
C32 0.0242(12) 0.0379(15) 0.061(2) 0.0184(13) 0.0081(12) 0.0085(10)
C33 0.0181(10) 0.0318(14) 0.070(2) 0.0023(12) 0.0134(12) 0.0053(9)
C34 0.0240(11) 0.0348(13) 0.0562(18) -0.0021(12) 0.0218(12) -0.0028(9)
C35 0.0237(11) 0.0284(12) 0.0398(15) 0.0046(10) 0.0138(10) 0.0009(9)
C36 0.0237(10) 0.0254(11) 0.0273(13) 0.0048(9) 0.0152(9) 0.0014(8)
C37 0.0309(12) 0.0273(12) 0.0337(14) 0.0067(10) 0.0155(11) 0.0048(9)
C38 0.0500(15) 0.0262(13) 0.0477(17) 0.0092(11) 0.0297(14) 0.0085(11)
C39 0.0639(18) 0.0258(13) 0.0505(18) -0.0039(12) 0.0381(15) -0.0029(12)
C40 0.0416(14) 0.0379(14) 0.0393(16) -0.0101(11) 0.0231(12) -0.0092(11)
C41 0.0308(11) 0.0310(13) 0.0298(14) 0.0002(10) 0.017(1) 0.0005(9)
C42 0.0287(11) 0.0344(13) 0.0261(13) 0.0069(10) 0.016(1) 0.0028(9)
C43 0.0343(13) 0.0634(18) 0.0238(14) 0.0089(12) 0.0120(11) 0.0019(11)
C44 0.0432(14) 0.0399(15) 0.0351(15) -0.0012(11) 0.0243(12) 0.0019(11)
C45 0.0376(13) 0.0366(14) 0.0346(15) 0.0112(11) 0.0201(12) 0.005(1)
_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 N1 2.0523(16) . ?
Zr1 C1 2.368(2) . ?
Zr1 Cl1 2.3845(6) . ?
Zr1 Cl2 2.3935(6) . ?
Zr1 C2 2.458(2) . ?
Zr1 C13 2.526(2) . ?
Zr1 C7 2.602(2) . ?
Zr1 C8 2.610(2) . ?
Zr1 Si1 2.9728(6) . ?
Si1 N1 1.7392(19) . ?
Si1 C1 1.873(2) . ?
Si1 C36 1.873(2) . ?
Si1 C30 1.875(2) . ?
N1 C42 1.491(3) . ?
C1 C13 1.460(2) . ?
C1 C2 1.461(3) . ?
C2 C3 1.413(3) . ?
C2 C7 1.430(3) . ?
C3 C4 1.382(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.436(3) . ?
C4 C14 1.541(3) . ?
C5 C6 1.381(3) . ?
C5 C17 1.540(3) . ?
C6 C7 1.406(3) . ?
C6 H6A 0.9500 . ?
C7 C8 1.450(3) . ?
C8 C9 1.405(2) . ?
C8 C13 1.432(3) . ?
C9 C10 1.376(3) . ?
C9 H9A 0.9500 . ?
C10 C11 1.437(3) . ?
C10 C18 1.537(2) . ?
C11 C12 1.384(3) . ?
C11 C21 1.534(3) . ?
C12 C13 1.412(3) . ?
C12 H12A 0.9500 . ?
C14 C23' 1.364(5) . ?
C14 C15 1.457(5) . ?
C14 C22 1.465(11) . ?
C14 C22' 1.556(11) . ?
C14 C15' 1.689(5) . ?
C14 C23 1.732(6) . ?
C15 C16 1.511(6) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.590(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C15' C16' 1.509(7) . ?
C15' H15C 0.9900 . ?
C15' H15D 0.9900 . ?
C16' C17 1.467(5) . ?
C16' H16C 0.9900 . ?
C16' H16D 0.9900 . ?
C17 C25 1.365(6) . ?
C17 C24' 1.568(5) . ?
C17 C24 1.572(6) . ?
C17 C25' 1.716(6) . ?
C18 C27 1.530(3) . ?
C18 C26 1.534(3) . ?
C18 C19 1.539(3) . ?
C19 C20 1.503(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.538(3) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C29 1.533(3) . ?
C21 C28 1.536(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C22' H22D 0.9800 . ?
C22' H22E 0.9800 . ?
C22' H22F 0.9800 . ?
C23' H23D 0.9800 . ?
C23' H23E 0.9800 . ?
C23' H23F 0.9800 . ?
C24' H24D 0.9800 . ?
C24' H24E 0.9800 . ?
C24' H24F 0.9800 . ?
C25' H25D 0.9800 . ?
C25' H25E 0.9800 . ?
C25' H25F 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.387(3) . ?
C30 C35 1.399(3) . ?
C31 C32 1.394(3) . ?
C31 H31A 0.9500 . ?
C32 C33 1.379(3) . ?
C32 H32A 0.9500 . ?
C33 C34 1.379(4) . ?
C33 H33A 0.9500 . ?
C34 C35 1.388(3) . ?
C34 H34A 0.9500 . ?
C35 H35A 0.9500 . ?
C36 C41 1.395(3) . ?
C36 C37 1.401(3) . ?
C37 C38 1.380(3) . ?
C37 H37A 0.9500 . ?
C38 C39 1.385(4) . ?
C38 H38A 0.9500 . ?
C39 C40 1.390(4) . ?
C39 H39A 0.9500 . ?
C40 C41 1.384(3) . ?
C40 H40A 0.9500 . ?
C41 H41A 0.9500 . ?
C42 C43 1.528(3) . ?
C42 C45 1.530(3) . ?
C42 C44 1.533(3) . ?
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 . ?
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
N1 Zr1 C1 73.42(7) . . ?
N1 Zr1 Cl1 108.86(5) . . ?
C1 Zr1 Cl1 121.54(5) . . ?
N1 Zr1 Cl2 110.20(5) . . ?
C1 Zr1 Cl2 130.18(5) . . ?
Cl1 Zr1 Cl2 104.63(2) . . ?
N1 Zr1 C2 91.57(7) . . ?
C1 Zr1 C2 35.17(7) . . ?
Cl1 Zr1 C2 143.24(5) . . ?
Cl2 Zr1 C2 95.93(5) . . ?
N1 Zr1 C13 97.94(6) . . ?
C1 Zr1 C13 34.53(6) . . ?
Cl1 Zr1 C13 90.99(4) . . ?
Cl2 Zr1 C13 140.63(5) . . ?
C2 Zr1 C13 55.24(7) . . ?
N1 Zr1 C7 124.04(6) . . ?
C1 Zr1 C7 56.68(6) . . ?
Cl1 Zr1 C7 117.56(4) . . ?
Cl2 Zr1 C7 87.16(5) . . ?
C2 Zr1 C7 32.66(6) . . ?
C13 Zr1 C7 53.86(6) . . ?
N1 Zr1 C8 128.60(7) . . ?
C1 Zr1 C8 56.56(6) . . ?
Cl1 Zr1 C8 89.50(4) . . ?
Cl2 Zr1 C8 110.61(5) . . ?
C2 Zr1 C8 54.47(6) . . ?
C13 Zr1 C8 32.32(6) . . ?
C7 Zr1 C8 32.31(6) . . ?
N1 Zr1 Si1 34.76(5) . . ?
C1 Zr1 Si1 39.02(5) . . ?
Cl1 Zr1 Si1 117.54(2) . . ?
Cl2 Zr1 Si1 131.144(19) . . ?
C2 Zr1 Si1 64.54(5) . . ?
C13 Zr1 Si1 64.87(4) . . ?
C7 Zr1 Si1 93.84(5) . . ?
C8 Zr1 Si1 93.99(5) . . ?
N1 Si1 C1 94.53(9) . . ?
N1 Si1 C36 111.93(9) . . ?
C1 Si1 C36 114.13(9) . . ?
N1 Si1 C30 119.50(9) . . ?
C1 Si1 C30 111.29(9) . . ?
C36 Si1 C30 105.60(9) . . ?
N1 Si1 Zr1 42.28(5) . . ?
C1 Si1 Zr1 52.78(7) . . ?
C36 Si1 Zr1 119.21(6) . . ?
C30 Si1 Zr1 135.15(7) . . ?
C42 N1 Si1 131.01(13) . . ?
C42 N1 Zr1 126.03(13) . . ?
Si1 N1 Zr1 102.96(8) . . ?
C13 C1 C2 104.61(16) . . ?
C13 C1 Si1 125.80(14) . . ?
C2 C1 Si1 122.72(14) . . ?
C13 C1 Zr1 78.65(11) . . ?
C2 C1 Zr1 75.77(12) . . ?
Si1 C1 Zr1 88.20(8) . . ?
C3 C2 C7 117.48(19) . . ?
C3 C2 C1 131.98(18) . . ?
C7 C2 C1 110.07(16) . . ?
C3 C2 Zr1 112.89(15) . . ?
C7 C2 Zr1 79.22(12) . . ?
C1 C2 Zr1 69.06(11) . . ?
C4 C3 C2 121.69(19) . . ?
C4 C3 H3A 119.2 . . ?
C2 C3 H3A 119.2 . . ?
C3 C4 C5 120.12(18) . . ?
C3 C4 C14 117.48(19) . . ?
C5 C4 C14 122.4(2) . . ?
C6 C5 C4 118.9(2) . . ?
C6 C5 C17 118.35(19) . . ?
C4 C5 C17 122.67(18) . . ?
C5 C6 C7 121.09(19) . . ?
C5 C6 H6A 119.5 . . ?
C7 C6 H6A 119.5 . . ?
C6 C7 C2 120.52(17) . . ?
C6 C7 C8 131.93(18) . . ?
C2 C7 C8 107.54(17) . . ?
C6 C7 Zr1 121.48(15) . . ?
C2 C7 Zr1 68.12(11) . . ?
C8 C7 Zr1 74.14(11) . . ?
C9 C8 C13 120.40(17) . . ?
C9 C8 C7 132.15(18) . . ?
C13 C8 C7 107.45(16) . . ?
C9 C8 Zr1 120.26(14) . . ?
C13 C8 Zr1 70.61(11) . . ?
C7 C8 Zr1 73.55(11) . . ?
C10 C9 C8 121.13(17) . . ?
C10 C9 H9A 119.4 . . ?
C8 C9 H9A 119.4 . . ?
C9 C10 C11 119.19(16) . . ?
C9 C10 C18 118.87(17) . . ?
C11 C10 C18 121.88(17) . . ?
C12 C11 C10 119.88(17) . . ?
C12 C11 C21 117.96(17) . . ?
C10 C11 C21 122.11(16) . . ?
C11 C12 C13 121.68(17) . . ?
C11 C12 H12A 119.2 . . ?
C13 C12 H12A 119.2 . . ?
C12 C13 C8 117.61(17) . . ?
C12 C13 C1 132.30(17) . . ?
C8 C13 C1 109.95(17) . . ?
C12 C13 Zr1 119.80(14) . . ?
C8 C13 Zr1 77.07(12) . . ?
C1 C13 Zr1 66.82(11) . . ?
C23' C14 C15 77.3(3) . . ?
C23' C14 C22 119.0(5) . . ?
C15 C14 C22 118.8(4) . . ?
C23' C14 C4 113.2(3) . . ?
C15 C14 C4 112.5(2) . . ?
C22 C14 C4 112.0(5) . . ?
C23' C14 C22' 117.9(5) . . ?
C15 C14 C22' 125.5(4) . . ?
C22 C14 C22' 6.7(7) . . ?
C4 C14 C22' 107.8(4) . . ?
C23' C14 C15' 110.0(3) . . ?
C15 C14 C15' 34.4(2) . . ?
C22 C14 C15' 92.9(4) . . ?
C4 C14 C15' 107.4(2) . . ?
C22' C14 C15' 99.3(4) . . ?
C23' C14 C23 26.0(3) . . ?
C15 C14 C23 102.8(3) . . ?
C22 C14 C23 101.8(5) . . ?
C4 C14 C23 107.2(2) . . ?
C22' C14 C23 98.6(4) . . ?
C15' C14 C23 133.5(3) . . ?
C14 C15 C16 107.9(4) . . ?
C14 C15 H15A 110.1 . . ?
C16 C15 H15A 110.1 . . ?
C14 C15 H15B 110.1 . . ?
C16 C15 H15B 110.1 . . ?
H15A C15 H15B 108.4 . . ?
C15 C16 C17 116.8(4) . . ?
C15 C16 H16A 108.1 . . ?
C17 C16 H16A 108.1 . . ?
C15 C16 H16B 108.1 . . ?
C17 C16 H16B 108.1 . . ?
H16A C16 H16B 107.3 . . ?
C16' C15' C14 110.8(4) . . ?
C16' C15' H15C 109.5 . . ?
C14 C15' H15C 109.5 . . ?
C16' C15' H15D 109.5 . . ?
C14 C15' H15D 109.5 . . ?
H15C C15' H15D 108.1 . . ?
C17 C16' C15' 110.7(4) . . ?
C17 C16' H16C 109.5 . . ?
C15' C16' H16C 109.5 . . ?
C17 C16' H16D 109.5 . . ?
C15' C16' H16D 109.5 . . ?
H16C C16' H16D 108.1 . . ?
C25 C17 C16' 122.7(4) . . ?
C25 C17 C5 112.3(3) . . ?
C16' C17 C5 113.6(3) . . ?
C25 C17 C24' 82.7(3) . . ?
C16' C17 C24' 108.1(3) . . ?
C5 C17 C24' 113.2(3) . . ?
C25 C17 C24 117.1(3) . . ?
C16' C17 C24 81.2(3) . . ?
C5 C17 C24 105.1(3) . . ?
C24' C17 C24 35.6(2) . . ?
C25 C17 C16 108.3(3) . . ?
C16' C17 C16 25.7(2) . . ?
C5 C17 C16 106.4(2) . . ?
C24' C17 C16 130.8(3) . . ?
C24 C17 C16 107.0(3) . . ?
C25 C17 C25' 20.7(3) . . ?
C16' C17 C25' 110.2(3) . . ?
C5 C17 C25' 108.5(2) . . ?
C24' C17 C25' 102.7(3) . . ?
C24 C17 C25' 135.3(3) . . ?
C16 C17 C25' 90.9(3) . . ?
C27 C18 C26 109.15(18) . . ?
C27 C18 C10 108.29(17) . . ?
C26 C18 C10 112.10(16) . . ?
C27 C18 C19 110.21(18) . . ?
C26 C18 C19 106.86(18) . . ?
C10 C18 C19 110.22(16) . . ?
C20 C19 C18 112.39(18) . . ?
C20 C19 H19A 109.1 . . ?
C18 C19 H19A 109.1 . . ?
C20 C19 H19B 109.1 . . ?
C18 C19 H19B 109.1 . . ?
H19A C19 H19B 107.9 . . ?
C19 C20 C21 113.10(18) . . ?
C19 C20 H20A 109.0 . . ?
C21 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
C21 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C29 C21 C11 107.54(17) . . ?
C29 C21 C28 109.14(17) . . ?
C11 C21 C28 111.29(17) . . ?
C29 C21 C20 110.55(17) . . ?
C11 C21 C20 111.18(16) . . ?
C28 C21 C20 107.14(17) . . ?
C14 C22 H22A 109.5 . . ?
C14 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C14 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C14 C23 H23A 109.5 . . ?
C14 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C14 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C17 C24 H24A 109.5 . . ?
C17 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C17 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C17 C25 H25A 109.5 . . ?
C17 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C17 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C14 C22' H22D 109.5 . . ?
C14 C22' H22E 109.5 . . ?
H22D C22' H22E 109.5 . . ?
C14 C22' H22F 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 109.5 . . ?
C14 C23' H23D 109.5 . . ?
C14 C23' H23E 109.5 . . ?
H23D C23' H23E 109.5 . . ?
C14 C23' H23F 109.5 . . ?
H23D C23' H23F 109.5 . . ?
H23E C23' H23F 109.5 . . ?
C17 C24' H24D 109.5 . . ?
C17 C24' H24E 109.5 . . ?
H24D C24' H24E 109.5 . . ?
C17 C24' H24F 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 109.5 . . ?
C17 C25' H25D 109.5 . . ?
C17 C25' H25E 109.5 . . ?
H25D C25' H25E 109.5 . . ?
C17 C25' H25F 109.5 . . ?
H25D C25' H25F 109.5 . . ?
H25E C25' H25F 109.5 . . ?
C18 C26 H26A 109.5 . . ?
C18 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C18 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C18 C27 H27A 109.5 . . ?
C18 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C18 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C21 C28 H28A 109.5 . . ?
C21 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C21 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C21 C29 H29A 109.5 . . ?
C21 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C21 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C35 117.58(19) . . ?
C31 C30 Si1 119.37(16) . . ?
C35 C30 Si1 122.78(17) . . ?
C30 C31 C32 121.6(2) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
C33 C32 C31 119.6(2) . . ?
C33 C32 H32A 120.2 . . ?
C31 C32 H32A 120.2 . . ?
C32 C33 C34 120.0(2) . . ?
C32 C33 H33A 120.0 . . ?
C34 C33 H33A 120.0 . . ?
C33 C34 C35 120.1(2) . . ?
C33 C34 H34A 120.0 . . ?
C35 C34 H34A 120.0 . . ?
C34 C35 C30 121.1(2) . . ?
C34 C35 H35A 119.5 . . ?
C30 C35 H35A 119.5 . . ?
C41 C36 C37 117.1(2) . . ?
C41 C36 Si1 121.13(16) . . ?
C37 C36 Si1 121.73(17) . . ?
C38 C37 C36 121.5(2) . . ?
C38 C37 H37A 119.3 . . ?
C36 C37 H37A 119.3 . . ?
C37 C38 C39 120.2(2) . . ?
C37 C38 H38A 119.9 . . ?
C39 C38 H38A 119.9 . . ?
C38 C39 C40 119.8(2) . . ?
C38 C39 H39A 120.1 . . ?
C40 C39 H39A 120.1 . . ?
C41 C40 C39 119.5(2) . . ?
C41 C40 H40A 120.3 . . ?
C39 C40 H40A 120.3 . . ?
C40 C41 C36 122.0(2) . . ?
C40 C41 H41A 119.0 . . ?
C36 C41 H41A 119.0 . . ?
N1 C42 C43 109.11(16) . . ?
N1 C42 C45 111.79(19) . . ?
C43 C42 C45 107.63(19) . . ?
N1 C42 C44 108.90(18) . . ?
C43 C42 C44 109.2(2) . . ?
C45 C42 C44 110.13(17) . . ?
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 . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.061