# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       m.tamm@tu-bs.de
_publ_contact_author_name        'Tamm, Matthias'

loop_
_publ_author_name
'Tamm, Matthias'
'Glockner, Andreas'
'Daniliuc, Constantin'
'Freytag, Matthias'
'Jones, P.'

data_andyg60
_database_code_depnum_ccdc_archive 'CCDC 879002'
#TrackingRef '- andyg60.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H25 N Si2 Zr'
_chemical_formula_weight         342.74

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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   15.8898(6)
_cell_length_b                   7.1098(2)
_cell_length_c                   28.0195(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.564(4)
_cell_angle_gamma                90.00
_cell_volume                     3121.5(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    17267
_cell_measurement_theta_min      2.2077
_cell_measurement_theta_max      29.2681

_exptl_crystal_description       needle
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87662
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.1419
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            47045
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0194
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         25.68
_reflns_number_total             2962
_reflns_number_gt                2817
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER XP'
_computing_publication_material  SHELXL-97

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

The hydrogens of the seven-membered ring were refined freely but with a
C-H distance restraint. The methyls were refined as idealized rigid groups
allowed to rotate but not tip.

The largest difference peak of ca. 2.4 e/A3 is related to the Zr
coordinates (the x and z coordinates both sum to 0.5) and may arise from
a minor twinning component, which however was not identified.
;

_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^)+(0.0201P)^2^+27.7220P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2962
_refine_ls_number_parameters     187
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.0942
_refine_ls_wR_factor_gt          0.0934
_refine_ls_goodness_of_fit_ref   1.291
_refine_ls_restrained_S_all      1.287
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.23849(2) 0.57230(5) 0.193700(13) 0.00989(12) Uani 1 1 d . . .
Si1 Si 0.31291(7) 0.39982(15) 0.09976(4) 0.0110(2) Uani 1 1 d . . .
Si2 Si 0.11949(6) 0.40227(15) 0.09484(4) 0.0106(2) Uani 1 1 d . . .
N N 0.22261(19) 0.4236(5) 0.12670(11) 0.0117(6) Uani 1 1 d . . .
C1 C 0.2317(2) 0.8755(5) 0.15613(14) 0.0124(8) Uani 1 1 d D . .
H1 H 0.223(3) 0.889(7) 0.1225(8) 0.019 Uiso 1 1 d D . .
C2 C 0.1548(2) 0.8463(6) 0.17405(14) 0.0143(8) Uani 1 1 d D . .
H2 H 0.1035(18) 0.855(6) 0.1518(12) 0.003(9) Uiso 1 1 d D . .
C3 C 0.1433(3) 0.7849(6) 0.22112(14) 0.0144(8) Uani 1 1 d D . .
H3 H 0.0864(17) 0.765(7) 0.2258(16) 0.024(13) Uiso 1 1 d D . .
C4 C 0.2073(3) 0.7553(6) 0.26241(14) 0.0147(8) Uani 1 1 d D . .
H4 H 0.194(3) 0.699(6) 0.2907(11) 0.019(12) Uiso 1 1 d D . .
C5 C 0.2988(3) 0.7551(6) 0.26511(14) 0.0148(8) Uani 1 1 d D . .
H5 H 0.327(3) 0.697(6) 0.2938(11) 0.023(13) Uiso 1 1 d D . .
C6 C 0.3474(2) 0.7835(6) 0.22720(14) 0.0145(8) Uani 1 1 d D . .
H6 H 0.4071(15) 0.766(7) 0.2352(15) 0.015(11) Uiso 1 1 d D . .
C7 C 0.3165(3) 0.8440(6) 0.17886(14) 0.0149(8) Uani 1 1 d D . .
H7 H 0.360(2) 0.853(7) 0.1596(15) 0.023(13) Uiso 1 1 d D . .
C8 C 0.3197(3) 0.1751(6) 0.06596(15) 0.0168(9) Uani 1 1 d . . .
H8A H 0.3161 0.0683 0.0876 0.025 Uiso 1 1 calc R . .
H8B H 0.3741 0.1703 0.0539 0.025 Uiso 1 1 calc R . .
H8C H 0.2725 0.1689 0.0386 0.025 Uiso 1 1 calc R . .
C9 C 0.3235(3) 0.5963(6) 0.05636(15) 0.0196(9) Uani 1 1 d . . .
H9A H 0.2752 0.5929 0.0296 0.029 Uiso 1 1 calc R . .
H9B H 0.3769 0.5814 0.0435 0.029 Uiso 1 1 calc R . .
H9C H 0.3240 0.7170 0.0733 0.029 Uiso 1 1 calc R . .
C10 C 0.4125(2) 0.3984(6) 0.14686(15) 0.0188(9) Uani 1 1 d . . .
H10A H 0.4105 0.5031 0.1694 0.028 Uiso 1 1 calc R . .
H10B H 0.4627 0.4120 0.1310 0.028 Uiso 1 1 calc R . .
H10C H 0.4161 0.2793 0.1647 0.028 Uiso 1 1 calc R . .
C11 C 0.0982(3) 0.1809(6) 0.05865(15) 0.0174(9) Uani 1 1 d . . .
H11A H 0.1344 0.1777 0.0335 0.026 Uiso 1 1 calc R . .
H11B H 0.0381 0.1771 0.0435 0.026 Uiso 1 1 calc R . .
H11C H 0.1111 0.0719 0.0800 0.026 Uiso 1 1 calc R . .
C12 C 0.0905(3) 0.6034(6) 0.05173(15) 0.0187(9) Uani 1 1 d . . .
H12A H 0.1025 0.7227 0.0690 0.028 Uiso 1 1 calc R . .
H12B H 0.0296 0.5967 0.0382 0.028 Uiso 1 1 calc R . .
H12C H 0.1241 0.5957 0.0255 0.028 Uiso 1 1 calc R . .
C13 C 0.0396(2) 0.3973(6) 0.13740(15) 0.0178(9) Uani 1 1 d . . .
H13A H 0.0458 0.2798 0.1559 0.027 Uiso 1 1 calc R . .
H13B H -0.0182 0.4052 0.1188 0.027 Uiso 1 1 calc R . .
H13C H 0.0497 0.5044 0.1596 0.027 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
Zr 0.01024(19) 0.00825(19) 0.01112(19) -0.00063(14) 0.00165(13) -0.00012(15)
Si1 0.0098(5) 0.0103(5) 0.0134(5) -0.0001(4) 0.0037(4) 0.0007(4)
Si2 0.0091(5) 0.0097(5) 0.0126(5) -0.0001(4) 0.0005(4) -0.0006(4)
N 0.0094(15) 0.0145(16) 0.0114(15) -0.0021(13) 0.0019(12) 0.0003(14)
C1 0.0159(19) 0.0099(19) 0.0115(18) 0.0009(15) 0.0024(15) -0.0005(15)
C2 0.0093(18) 0.014(2) 0.018(2) 0.0009(16) -0.0013(15) 0.0024(16)
C3 0.0133(19) 0.0114(19) 0.020(2) -0.0055(16) 0.0070(16) -0.0003(16)
C4 0.023(2) 0.0086(19) 0.0140(19) -0.0012(15) 0.0071(16) -0.0031(16)
C5 0.019(2) 0.0099(19) 0.0138(19) -0.0009(16) -0.0025(16) 0.0013(16)
C6 0.0116(19) 0.0112(19) 0.019(2) -0.0027(16) -0.0011(16) -0.0017(16)
C7 0.0135(19) 0.015(2) 0.017(2) -0.0001(16) 0.0063(16) -0.0022(16)
C8 0.018(2) 0.016(2) 0.018(2) -0.0008(17) 0.0081(16) 0.0012(17)
C9 0.022(2) 0.018(2) 0.022(2) 0.0001(18) 0.0107(17) 0.0017(18)
C10 0.0103(19) 0.022(2) 0.024(2) -0.0030(18) 0.0046(16) 0.0008(17)
C11 0.017(2) 0.015(2) 0.019(2) -0.0032(17) -0.0016(16) -0.0007(17)
C12 0.018(2) 0.016(2) 0.019(2) 0.0015(17) -0.0037(16) -0.0017(17)
C13 0.0118(19) 0.020(2) 0.022(2) -0.0010(17) 0.0045(16) -0.0028(16)

_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
Zr N 2.133(3) . ?
Zr C3 2.356(4) . ?
Zr C6 2.364(4) . ?
Zr C7 2.369(4) . ?
Zr C2 2.371(4) . ?
Zr C1 2.394(4) . ?
Zr C4 2.442(4) . ?
Zr C5 2.444(4) . ?
Zr C4 2.642(4) 4_545 ?
Zr C5 2.645(4) 4_545 ?
Si1 N 1.737(3) . ?
Si1 C8 1.870(4) . ?
Si1 C9 1.878(4) . ?
Si1 C10 1.885(4) . ?
Si2 N 1.737(3) . ?
Si2 C11 1.873(4) . ?
Si2 C12 1.879(4) . ?
Si2 C13 1.880(4) . ?
C1 C7 1.410(6) . ?
C1 C2 1.410(6) . ?
C2 C3 1.430(6) . ?
C3 C4 1.423(6) . ?
C4 C5 1.443(6) . ?
C4 Zr 2.642(4) 4 ?
C5 C6 1.427(6) . ?
C5 Zr 2.645(4) 4 ?
C6 C7 1.428(6) . ?

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
N Zr C3 128.08(13) . . ?
N Zr C6 129.49(13) . . ?
C3 Zr C6 86.01(14) . . ?
N Zr C7 103.79(13) . . ?
C3 Zr C7 85.24(14) . . ?
C6 Zr C7 35.13(14) . . ?
N Zr C2 102.89(13) . . ?
C3 Zr C2 35.21(14) . . ?
C6 Zr C2 85.16(14) . . ?
C7 Zr C2 65.08(14) . . ?
N Zr C1 93.96(13) . . ?
C3 Zr C1 65.22(14) . . ?
C6 Zr C1 65.13(13) . . ?
C7 Zr C1 34.43(13) . . ?
C2 Zr C1 34.43(13) . . ?
N Zr C4 161.52(13) . . ?
C3 Zr C4 34.46(14) . . ?
C6 Zr C4 65.14(14) . . ?
C7 Zr C4 83.36(13) . . ?
C2 Zr C4 64.27(14) . . ?
C1 Zr C4 82.33(13) . . ?
N Zr C5 163.15(13) . . ?
C3 Zr C5 65.01(14) . . ?
C6 Zr C5 34.48(14) . . ?
C7 Zr C5 64.18(14) . . ?
C2 Zr C5 83.20(14) . . ?
C1 Zr C5 82.18(13) . . ?
C4 Zr C5 34.37(13) . . ?
N Zr C4 88.21(12) . 4_545 ?
C3 Zr C4 124.94(13) . 4_545 ?
C6 Zr C4 101.33(13) . 4_545 ?
C7 Zr C4 129.63(14) . 4_545 ?
C2 Zr C4 159.34(13) . 4_545 ?
C1 Zr C4 163.82(13) . 4_545 ?
C4 Zr C4 100.41(6) . 4_545 ?
C5 Zr C4 91.12(13) . 4_545 ?
N Zr C5 87.67(12) . 4_545 ?
C3 Zr C5 101.65(13) . 4_545 ?
C6 Zr C5 124.79(13) . 4_545 ?
C7 Zr C5 159.00(13) . 4_545 ?
C2 Zr C5 130.09(13) . 4_545 ?
C1 Zr C5 164.29(13) . 4_545 ?
C4 Zr C5 91.18(13) . 4_545 ?
C5 Zr C5 100.50(6) . 4_545 ?
C4 Zr C5 31.69(12) 4_545 4_545 ?
N Si1 C8 115.15(18) . . ?
N Si1 C9 112.24(18) . . ?
C8 Si1 C9 106.77(18) . . ?
N Si1 C10 110.75(17) . . ?
C8 Si1 C10 103.75(19) . . ?
C9 Si1 C10 107.6(2) . . ?
N Si2 C11 114.94(18) . . ?
N Si2 C12 111.93(18) . . ?
C11 Si2 C12 106.78(19) . . ?
N Si2 C13 110.73(17) . . ?
C11 Si2 C13 104.33(19) . . ?
C12 Si2 C13 107.60(19) . . ?
Si1 N Si2 123.02(18) . . ?
Si1 N Zr 116.45(16) . . ?
Si2 N Zr 117.33(16) . . ?
C7 C1 C2 129.4(4) . . ?
C7 C1 Zr 71.8(2) . . ?
C2 C1 Zr 71.9(2) . . ?
C1 C2 C3 128.6(4) . . ?
C1 C2 Zr 73.7(2) . . ?
C3 C2 Zr 71.8(2) . . ?
C4 C3 C2 127.7(4) . . ?
C4 C3 Zr 76.1(2) . . ?
C2 C3 Zr 73.0(2) . . ?
C3 C4 C5 128.3(4) . . ?
C3 C4 Zr 69.5(2) . . ?
C5 C4 Zr 72.9(2) . . ?
C3 C4 Zr 112.7(3) . 4 ?
C5 C4 Zr 74.3(2) . 4 ?
Zr C4 Zr 136.76(17) . 4 ?
C6 C5 C4 128.7(4) . . ?
C6 C5 Zr 69.7(2) . . ?
C4 C5 Zr 72.7(2) . . ?
C6 C5 Zr 113.1(3) . 4 ?
C4 C5 Zr 74.0(2) . 4 ?
Zr C5 Zr 136.44(16) . 4 ?
C5 C6 C7 127.2(4) . . ?
C5 C6 Zr 75.8(2) . . ?
C7 C6 Zr 72.6(2) . . ?
C1 C7 C6 129.0(4) . . ?
C1 C7 Zr 73.8(2) . . ?
C6 C7 Zr 72.3(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C8 Si1 N Si2 -54.8(3) . . . . ?
C9 Si1 N Si2 67.6(3) . . . . ?
C10 Si1 N Si2 -172.1(2) . . . . ?
C8 Si1 N Zr 146.00(19) . . . . ?
C9 Si1 N Zr -91.6(2) . . . . ?
C10 Si1 N Zr 28.7(2) . . . . ?
C11 Si2 N Si1 52.8(3) . . . . ?
C12 Si2 N Si1 -69.2(3) . . . . ?
C13 Si2 N Si1 170.7(2) . . . . ?
C11 Si2 N Zr -148.12(19) . . . . ?
C12 Si2 N Zr 89.8(2) . . . . ?
C13 Si2 N Zr -30.2(2) . . . . ?
C3 Zr N Si1 141.44(18) . . . . ?
C6 Zr N Si1 19.4(3) . . . . ?
C7 Zr N Si1 46.6(2) . . . . ?
C2 Zr N Si1 113.75(19) . . . . ?
C1 Zr N Si1 80.1(2) . . . . ?
C4 Zr N Si1 157.7(3) . . . . ?
C5 Zr N Si1 4.1(6) . . . . ?
C4 Zr N Si1 -83.86(19) 4_545 . . . ?
C5 Zr N Si1 -115.56(19) 4_545 . . . ?
C3 Zr N Si2 -19.0(3) . . . . ?
C6 Zr N Si2 -141.04(18) . . . . ?
C7 Zr N Si2 -113.78(19) . . . . ?
C2 Zr N Si2 -46.7(2) . . . . ?
C1 Zr N Si2 -80.3(2) . . . . ?
C4 Zr N Si2 -2.7(5) . . . . ?
C5 Zr N Si2 -156.3(4) . . . . ?
C4 Zr N Si2 115.7(2) 4_545 . . . ?
C5 Zr N Si2 84.02(19) 4_545 . . . ?
N Zr C1 C7 -108.8(2) . . . . ?
C3 Zr C1 C7 120.8(3) . . . . ?
C6 Zr C1 C7 23.3(2) . . . . ?
C2 Zr C1 C7 144.1(4) . . . . ?
C4 Zr C1 C7 89.4(2) . . . . ?
C5 Zr C1 C7 54.8(2) . . . . ?
C4 Zr C1 C7 -11.5(6) 4_545 . . . ?
C5 Zr C1 C7 155.8(4) 4_545 . . . ?
N Zr C1 C2 107.1(2) . . . . ?
C3 Zr C1 C2 -23.3(2) . . . . ?
C6 Zr C1 C2 -120.8(3) . . . . ?
C7 Zr C1 C2 -144.1(4) . . . . ?
C4 Zr C1 C2 -54.7(2) . . . . ?
C5 Zr C1 C2 -89.4(2) . . . . ?
C4 Zr C1 C2 -155.6(4) 4_545 . . . ?
C5 Zr C1 C2 11.6(6) 4_545 . . . ?
C7 C1 C2 C3 3.3(7) . . . . ?
Zr C1 C2 C3 49.4(4) . . . . ?
C7 C1 C2 Zr -46.1(4) . . . . ?
N Zr C2 C1 -78.0(2) . . . . ?
C3 Zr C2 C1 141.4(4) . . . . ?
C6 Zr C2 C1 51.5(2) . . . . ?
C7 Zr C2 C1 21.4(2) . . . . ?
C4 Zr C2 C1 116.2(3) . . . . ?
C5 Zr C2 C1 86.1(2) . . . . ?
C4 Zr C2 C1 161.0(3) 4_545 . . . ?
C5 Zr C2 C1 -175.9(2) 4_545 . . . ?
N Zr C2 C3 140.6(2) . . . . ?
C6 Zr C2 C3 -89.9(2) . . . . ?
C7 Zr C2 C3 -120.0(3) . . . . ?
C1 Zr C2 C3 -141.4(4) . . . . ?
C4 Zr C2 C3 -25.2(2) . . . . ?
C5 Zr C2 C3 -55.3(2) . . . . ?
C4 Zr C2 C3 19.6(5) 4_545 . . . ?
C5 Zr C2 C3 42.7(3) 4_545 . . . ?
C1 C2 C3 C4 6.3(7) . . . . ?
Zr C2 C3 C4 56.4(4) . . . . ?
C1 C2 C3 Zr -50.0(4) . . . . ?
N Zr C3 C4 171.0(2) . . . . ?
C6 Zr C3 C4 -50.0(2) . . . . ?
C7 Zr C3 C4 -85.2(2) . . . . ?
C2 Zr C3 C4 -137.2(4) . . . . ?
C1 Zr C3 C4 -114.4(3) . . . . ?
C5 Zr C3 C4 -21.5(2) . . . . ?
C4 Zr C3 C4 51.1(3) 4_545 . . . ?
C5 Zr C3 C4 74.7(2) 4_545 . . . ?
N Zr C3 C2 -51.8(3) . . . . ?
C6 Zr C3 C2 87.3(2) . . . . ?
C7 Zr C3 C2 52.0(2) . . . . ?
C1 Zr C3 C2 22.9(2) . . . . ?
C4 Zr C3 C2 137.2(4) . . . . ?
C5 Zr C3 C2 115.7(3) . . . . ?
C4 Zr C3 C2 -171.7(2) 4_545 . . . ?
C5 Zr C3 C2 -148.0(2) 4_545 . . . ?
C2 C3 C4 C5 -9.2(7) . . . . ?
Zr C3 C4 C5 45.9(4) . . . . ?
C2 C3 C4 Zr -55.1(4) . . . . ?
C2 C3 C4 Zr 78.2(5) . . . 4 ?
Zr C3 C4 Zr 133.4(2) . . . 4 ?
N Zr C4 C3 -22.9(5) . . . . ?
C6 Zr C4 C3 122.6(3) . . . . ?
C7 Zr C4 C3 91.3(2) . . . . ?
C2 Zr C4 C3 25.8(2) . . . . ?
C1 Zr C4 C3 56.6(2) . . . . ?
C5 Zr C4 C3 143.9(4) . . . . ?
C4 Zr C4 C3 -139.6(2) 4_545 . . . ?
C5 Zr C4 C3 -109.1(2) 4_545 . . . ?
N Zr C4 C5 -166.8(4) . . . . ?
C3 Zr C4 C5 -143.9(4) . . . . ?
C6 Zr C4 C5 -21.3(2) . . . . ?
C7 Zr C4 C5 -52.7(2) . . . . ?
C2 Zr C4 C5 -118.2(3) . . . . ?
C1 Zr C4 C5 -87.4(2) . . . . ?
C4 Zr C4 C5 76.5(3) 4_545 . . . ?
C5 Zr C4 C5 107.0(2) 4_545 . . . ?
N Zr C4 Zr -124.6(4) . . . 4 ?
C3 Zr C4 Zr -101.7(3) . . . 4 ?
C6 Zr C4 Zr 20.9(2) . . . 4 ?
C7 Zr C4 Zr -10.5(2) . . . 4 ?
C2 Zr C4 Zr -75.9(3) . . . 4 ?
C1 Zr C4 Zr -45.1(2) . . . 4 ?
C5 Zr C4 Zr 42.2(2) . . . 4 ?
C4 Zr C4 Zr 118.7(3) 4_545 . . 4 ?
C5 Zr C4 Zr 149.2(3) 4_545 . . 4 ?
C3 C4 C5 C6 -0.4(7) . . . . ?
Zr C4 C5 C6 44.3(4) . . . . ?
Zr C4 C5 C6 -107.1(4) 4 . . . ?
C3 C4 C5 Zr -44.7(4) . . . . ?
Zr C4 C5 Zr -151.44(13) 4 . . . ?
C3 C4 C5 Zr 106.7(4) . . . 4 ?
Zr C4 C5 Zr 151.44(13) . . . 4 ?
N Zr C5 C6 21.1(6) . . . . ?
C3 Zr C5 C6 -122.9(3) . . . . ?
C7 Zr C5 C6 -25.8(2) . . . . ?
C2 Zr C5 C6 -91.3(2) . . . . ?
C1 Zr C5 C6 -56.6(2) . . . . ?
C4 Zr C5 C6 -144.5(4) . . . . ?
C4 Zr C5 C6 108.6(2) 4_545 . . . ?
C5 Zr C5 C6 139.0(2) 4_545 . . . ?
N Zr C5 C4 165.5(4) . . . . ?
C3 Zr C5 C4 21.6(2) . . . . ?
C6 Zr C5 C4 144.5(4) . . . . ?
C7 Zr C5 C4 118.7(3) . . . . ?
C2 Zr C5 C4 53.1(2) . . . . ?
C1 Zr C5 C4 87.8(2) . . . . ?
C4 Zr C5 C4 -107.0(2) 4_545 . . . ?
C5 Zr C5 C4 -76.5(3) 4_545 . . . ?
N Zr C5 Zr 123.7(4) . . . 4 ?
C3 Zr C5 Zr -20.3(2) . . . 4 ?
C6 Zr C5 Zr 102.6(3) . . . 4 ?
C7 Zr C5 Zr 76.8(3) . . . 4 ?
C2 Zr C5 Zr 11.3(2) . . . 4 ?
C1 Zr C5 Zr 46.0(2) . . . 4 ?
C4 Zr C5 Zr -41.8(2) . . . 4 ?
C4 Zr C5 Zr -148.8(2) 4_545 . . 4 ?
C5 Zr C5 Zr -118.3(3) 4_545 . . 4 ?
C4 C5 C6 C7 9.3(7) . . . . ?
Zr C5 C6 C7 54.6(4) . . . . ?
Zr C5 C6 C7 -78.4(5) 4 . . . ?
C4 C5 C6 Zr -45.3(4) . . . . ?
Zr C5 C6 Zr -133.01(19) 4 . . . ?
N Zr C6 C5 -172.2(2) . . . . ?
C3 Zr C6 C5 49.7(2) . . . . ?
C7 Zr C6 C5 137.1(4) . . . . ?
C2 Zr C6 C5 85.0(2) . . . . ?
C1 Zr C6 C5 114.2(3) . . . . ?
C4 Zr C6 C5 21.2(2) . . . . ?
C4 Zr C6 C5 -75.1(2) 4_545 . . . ?
C5 Zr C6 C5 -51.7(3) 4_545 . . . ?
N Zr C6 C7 50.6(3) . . . . ?
C3 Zr C6 C7 -87.4(2) . . . . ?
C2 Zr C6 C7 -52.1(2) . . . . ?
C1 Zr C6 C7 -22.9(2) . . . . ?
C4 Zr C6 C7 -115.9(3) . . . . ?
C5 Zr C6 C7 -137.1(4) . . . . ?
C4 Zr C6 C7 147.7(2) 4_545 . . . ?
C5 Zr C6 C7 171.2(2) 4_545 . . . ?
C2 C1 C7 C6 -3.8(7) . . . . ?
Zr C1 C7 C6 -49.9(4) . . . . ?
C2 C1 C7 Zr 46.1(4) . . . . ?
C5 C6 C7 C1 -5.4(7) . . . . ?
Zr C6 C7 C1 50.5(4) . . . . ?
C5 C6 C7 Zr -55.9(4) . . . . ?
N Zr C7 C1 76.6(2) . . . . ?
C3 Zr C7 C1 -51.5(2) . . . . ?
C6 Zr C7 C1 -141.3(4) . . . . ?
C2 Zr C7 C1 -21.4(2) . . . . ?
C4 Zr C7 C1 -86.1(2) . . . . ?
C5 Zr C7 C1 -116.0(3) . . . . ?
C4 Zr C7 C1 175.9(2) 4_545 . . . ?
C5 Zr C7 C1 -161.9(3) 4_545 . . . ?
N Zr C7 C6 -142.1(2) . . . . ?
C3 Zr C7 C6 89.8(2) . . . . ?
C2 Zr C7 C6 119.9(3) . . . . ?
C1 Zr C7 C6 141.3(4) . . . . ?
C4 Zr C7 C6 55.2(2) . . . . ?
C5 Zr C7 C6 25.3(2) . . . . ?
C4 Zr C7 C6 -42.8(3) 4_545 . . . ?
C5 Zr C7 C6 -20.6(5) 4_545 . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.68
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.375
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.100
_iucr_refine_instructions_details 
;
TITL andyg60 in C2/c
CELL 0.71073 15.8898 7.1098 28.0195 90.000 99.564 90.000
ZERR 8.00 0.0006 0.0002 0.0012 0.000 0.004 0.000
LATT 7
SYMM - X, Y, 1/2 - Z
SFAC C H N ZR SI
UNIT 104 200 8 8 16
SIZE 0.22 0.10 0.03
TEMP -173
SHEL 999 0.82
ACTA
CONF

FMAP 2
PLAN 10
L.S. 8

OMIT -5 7 5
OMIT -1 1 23
OMIT -5 1 5
OMIT 5 1 3
OMIT -3 7 5
OMIT 4 4 0
OMIT -5 1 7
OMIT 5 7 3

SADI C1 H1 C2 H2 c3 h3 C4 H4 C5 H5 C6 H6 C7 H7

WGHT 0.020100 27.722002
FVAR 1.04848
ZR 4 0.238494 0.572297 0.193700 11.00000 0.01024 0.00825 =
0.01112 -0.00063 0.00165 -0.00012
SI1 5 0.312908 0.399817 0.099761 11.00000 0.00984 0.01026 =
0.01343 -0.00014 0.00372 0.00066
SI2 5 0.119489 0.402266 0.094842 11.00000 0.00908 0.00974 =
0.01261 -0.00010 0.00048 -0.00058
N 3 0.222611 0.423635 0.126696 11.00000 0.00935 0.01447 =
0.01137 -0.00211 0.00191 0.00035
C1 1 0.231655 0.875536 0.156126 11.00000 0.01590 0.00991 =
0.01152 0.00093 0.00243 -0.00048
H1 2 0.222723 0.889402 0.122535 11.00000 -1.50000
C2 1 0.154835 0.846340 0.174047 11.00000 0.00932 0.01421 =
0.01817 0.00089 -0.00128 0.00240
H2 2 0.103480 0.855487 0.151807 11.00000 0.00345
C3 1 0.143314 0.784900 0.221122 11.00000 0.01327 0.01142 =
0.01980 -0.00553 0.00695 -0.00029
H3 2 0.086361 0.764807 0.225802 11.00000 0.02387
C4 1 0.207334 0.755311 0.262409 11.00000 0.02290 0.00856 =
0.01404 -0.00118 0.00710 -0.00311
H4 2 0.193807 0.699253 0.290671 11.00000 0.01898
C5 1 0.298843 0.755147 0.265106 11.00000 0.01888 0.00993 =
0.01377 -0.00093 -0.00250 0.00133
H5 2 0.326678 0.697344 0.293767 11.00000 0.02349
C6 1 0.347405 0.783453 0.227196 11.00000 0.01161 0.01124 =
0.01949 -0.00270 -0.00106 -0.00166
H6 2 0.407097 0.765956 0.235214 11.00000 0.01541
C7 1 0.316482 0.843963 0.178856 11.00000 0.01354 0.01524 =
0.01719 -0.00007 0.00632 -0.00218
H7 2 0.359754 0.853476 0.159604 11.00000 0.02329
C8 1 0.319719 0.175090 0.065957 11.00000 0.01844 0.01578 =
0.01800 -0.00080 0.00812 0.00119
AFIX 137
H8A 2 0.316070 0.068339 0.087645 11.00000 -1.50000
H8B 2 0.374139 0.170268 0.053890 11.00000 -1.50000
H8C 2 0.272517 0.168873 0.038617 11.00000 -1.50000
AFIX 0
C9 1 0.323525 0.596254 0.056360 11.00000 0.02154 0.01767 =
0.02202 0.00014 0.01069 0.00166
AFIX 137
H9A 2 0.275189 0.592855 0.029626 11.00000 -1.50000
H9B 2 0.376895 0.581385 0.043547 11.00000 -1.50000
H9C 2 0.324032 0.717041 0.073255 11.00000 -1.50000
AFIX 0
C10 1 0.412487 0.398391 0.146862 11.00000 0.01028 0.02245 =
0.02417 -0.00297 0.00455 0.00077
AFIX 137
H10A 2 0.410472 0.503133 0.169380 11.00000 -1.50000
H10B 2 0.462657 0.411974 0.130991 11.00000 -1.50000
H10C 2 0.416115 0.279326 0.164708 11.00000 -1.50000
AFIX 0
C11 1 0.098215 0.180856 0.058653 11.00000 0.01673 0.01500 =
0.01897 -0.00322 -0.00157 -0.00075
AFIX 137
H11A 2 0.134369 0.177741 0.033530 11.00000 -1.50000
H11B 2 0.038057 0.177105 0.043464 11.00000 -1.50000
H11C 2 0.111087 0.071851 0.080026 11.00000 -1.50000
AFIX 0
C12 1 0.090454 0.603398 0.051731 11.00000 0.01840 0.01646 =
0.01885 0.00148 -0.00367 -0.00174
AFIX 137
H12A 2 0.102533 0.722676 0.069044 11.00000 -1.50000
H12B 2 0.029568 0.596715 0.038176 11.00000 -1.50000
H12C 2 0.124120 0.595688 0.025492 11.00000 -1.50000
AFIX 0
C13 1 0.039637 0.397325 0.137397 11.00000 0.01182 0.01977 =
0.02237 -0.00100 0.00452 -0.00281
AFIX 137
H13A 2 0.045821 0.279835 0.155940 11.00000 -1.50000
H13B 2 -0.018197 0.405187 0.118783 11.00000 -1.50000
H13C 2 0.049670 0.504377 0.159649 11.00000 -1.50000

HKLF 4
;

# Attachment '- neu_andyg51.cif'

data_temp_andyg51
_database_code_depnum_ccdc_archive 'CCDC 879003'
#TrackingRef '- neu_andyg51.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H33 N O Si2 Zr'
_chemical_formula_weight         414.84

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/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                   10.2102(2)
_cell_length_b                   10.7387(2)
_cell_length_c                   19.2391(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.648(2)
_cell_angle_gamma                90.00
_cell_volume                     2079.62(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19007
_cell_measurement_theta_min      4.1133
_cell_measurement_theta_max      75.7899

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             872
_exptl_absorpt_coefficient_mu    5.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.73269
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
?
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Atlas, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22020
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         4.39
_diffrn_reflns_theta_max         75.98
_reflns_number_total             4301
_reflns_number_gt                4248
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
?
;
_computing_cell_refinement       
;
?
;
_computing_data_reduction        
;
?
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'BRUKER XP'
_computing_publication_material  SHELXL-97

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

The hydrogens of the seven-membered ring were refined freely.
The methyls were refined as idealized rigid groups allowed to
rotate but not tip. Other H atoms were refined using a riding model,
starting from calculated positions.

;

_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^)+(0.0300P)^2^+1.0255P] 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    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00114(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         4301
_refine_ls_number_parameters     234
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0203
_refine_ls_wR_factor_ref         0.0518
_refine_ls_wR_factor_gt          0.0516
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr Zr 0.665240(10) 0.264200(10) 0.158295(6) 0.01462(6) Uani 1 1 d . . .
Si1 Si 0.77916(4) 0.17681(3) 0.014353(19) 0.01694(9) Uani 1 1 d . . .
Si2 Si 0.97843(4) 0.27953(3) 0.13636(2) 0.01684(9) Uani 1 1 d . . .
O O 0.67431(10) 0.47694(9) 0.13417(5) 0.0198(2) Uani 1 1 d . . .
N N 0.81839(12) 0.24973(10) 0.09493(6) 0.0156(2) Uani 1 1 d . . .
C1 C 0.68960(17) 0.11224(16) 0.24635(9) 0.0305(3) Uani 1 1 d . . .
H1 H 0.767(2) 0.073(2) 0.2663(12) 0.042(6) Uiso 1 1 d . . .
C2 C 0.62194(17) 0.05553(14) 0.18433(9) 0.0302(3) Uani 1 1 d . . .
H2 H 0.664(2) -0.015(2) 0.1677(11) 0.037(6) Uiso 1 1 d . . .
C3 C 0.51362(16) 0.10216(15) 0.13558(9) 0.0287(3) Uani 1 1 d . . .
H3 H 0.492(2) 0.056(2) 0.0943(12) 0.038(6) Uiso 1 1 d . . .
C4 C 0.43967(15) 0.21419(16) 0.13928(9) 0.0274(3) Uani 1 1 d . . .
H4 H 0.376(2) 0.2337(19) 0.0993(12) 0.034(6) Uiso 1 1 d . . .
C5 C 0.45460(15) 0.30386(15) 0.19461(9) 0.0258(3) Uani 1 1 d . . .
H5 H 0.401(2) 0.371(2) 0.1871(10) 0.031(5) Uiso 1 1 d . . .
C6 C 0.55343(16) 0.31037(15) 0.25505(8) 0.0257(3) Uani 1 1 d . . .
H6 H 0.5548(19) 0.3806(19) 0.2797(10) 0.028(5) Uiso 1 1 d . . .
C7 C 0.66159(18) 0.22760(16) 0.27743(9) 0.0281(3) Uani 1 1 d . . .
H7 H 0.727(2) 0.2531(18) 0.3180(12) 0.029(5) Uiso 1 1 d . . .
C8 C 0.61333(16) 0.23350(16) -0.03192(9) 0.0270(3) Uani 1 1 d . . .
H8A H 0.5475 0.2247 -0.0005 0.040 Uiso 1 1 calc R . .
H8B H 0.5856 0.1841 -0.0747 0.040 Uiso 1 1 calc R . .
H8C H 0.6203 0.3213 -0.0447 0.040 Uiso 1 1 calc R . .
C9 C 0.76915(16) 0.00286(14) 0.02287(9) 0.0267(3) Uani 1 1 d . . .
H9A H 0.8502 -0.0280 0.0524 0.040 Uiso 1 1 calc R . .
H9B H 0.7600 -0.0353 -0.0240 0.040 Uiso 1 1 calc R . .
H9C H 0.6920 -0.0189 0.0446 0.040 Uiso 1 1 calc R . .
C10 C 0.90236(16) 0.20929(16) -0.04565(8) 0.0252(3) Uani 1 1 d . . .
H10A H 0.9002 0.2981 -0.0576 0.038 Uiso 1 1 calc R . .
H10B H 0.8795 0.1601 -0.0889 0.038 Uiso 1 1 calc R . .
H10C H 0.9917 0.1866 -0.0218 0.038 Uiso 1 1 calc R . .
C11 C 1.08105(14) 0.13471(14) 0.14833(8) 0.0243(3) Uani 1 1 d . . .
H11A H 1.0423 0.0762 0.1783 0.036 Uiso 1 1 calc R . .
H11B H 1.1718 0.1556 0.1707 0.036 Uiso 1 1 calc R . .
H11C H 1.0829 0.0964 0.1023 0.036 Uiso 1 1 calc R . .
C12 C 1.06901(16) 0.39697(16) 0.08961(9) 0.0306(3) Uani 1 1 d . . .
H12A H 1.0838 0.3626 0.0444 0.046 Uiso 1 1 calc R . .
H12B H 1.1547 0.4165 0.1188 0.046 Uiso 1 1 calc R . .
H12C H 1.0157 0.4731 0.0813 0.046 Uiso 1 1 calc R . .
C13 C 0.97319(16) 0.34806(18) 0.22559(9) 0.0319(4) Uani 1 1 d . . .
H13A H 0.9148 0.4211 0.2205 0.048 Uiso 1 1 calc R . .
H13B H 1.0629 0.3730 0.2475 0.048 Uiso 1 1 calc R . .
H13C H 0.9391 0.2859 0.2553 0.048 Uiso 1 1 calc R . .
C14 C 0.70271(17) 0.53646(14) 0.07084(8) 0.0280(3) Uani 1 1 d . . .
H14A H 0.6199 0.5527 0.0372 0.034 Uiso 1 1 calc R . .
H14B H 0.7622 0.4841 0.0474 0.034 Uiso 1 1 calc R . .
C15 C 0.7700(2) 0.65686(16) 0.09694(12) 0.0444(5) Uani 1 1 d . . .
H15A H 0.7571 0.7212 0.0595 0.053 Uiso 1 1 calc R . .
H15B H 0.8664 0.6441 0.1128 0.053 Uiso 1 1 calc R . .
C16 C 0.70200(17) 0.69397(15) 0.15807(9) 0.0292(3) Uani 1 1 d . . .
H16A H 0.6328 0.7576 0.1431 0.035 Uiso 1 1 calc R . .
H16B H 0.7672 0.7282 0.1973 0.035 Uiso 1 1 calc R . .
C17 C 0.64022(16) 0.57517(14) 0.18056(9) 0.0268(3) Uani 1 1 d . . .
H17A H 0.6763 0.5556 0.2304 0.032 Uiso 1 1 calc R . .
H17B H 0.5426 0.5842 0.1755 0.032 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
Zr 0.01515(8) 0.01266(7) 0.01719(8) -0.00063(4) 0.00603(5) -0.00080(4)
Si1 0.01608(17) 0.01800(18) 0.01718(17) -0.00209(13) 0.00409(13) 0.00179(13)
Si2 0.01441(17) 0.01639(18) 0.01986(18) -0.00056(14) 0.00327(14) 0.00034(13)
O 0.0246(5) 0.0136(5) 0.0234(5) -0.0001(4) 0.0103(4) 0.0013(4)
N 0.0149(5) 0.0148(5) 0.0179(6) -0.0008(4) 0.0049(5) 0.0006(4)
C1 0.0338(8) 0.0287(8) 0.0322(8) 0.0141(7) 0.0151(7) 0.0071(7)
C2 0.0403(9) 0.0136(7) 0.0427(9) 0.0031(6) 0.0245(7) -0.0018(6)
C3 0.0316(8) 0.0232(7) 0.0348(8) -0.0088(6) 0.0162(7) -0.0145(6)
C4 0.0184(7) 0.0335(8) 0.0314(8) 0.0004(7) 0.0071(6) -0.0083(6)
C5 0.0208(7) 0.0234(7) 0.0371(8) 0.0012(6) 0.0163(6) 0.0013(6)
C6 0.0321(8) 0.0222(7) 0.0275(7) -0.0053(6) 0.0183(6) -0.0038(6)
C7 0.0319(8) 0.0344(9) 0.0197(7) 0.0026(6) 0.0090(6) -0.0040(7)
C8 0.0216(7) 0.0361(9) 0.0226(8) -0.0021(6) 0.0016(6) 0.0041(6)
C9 0.0301(8) 0.0201(7) 0.0313(8) -0.0072(6) 0.0092(6) -0.0009(6)
C10 0.0246(7) 0.0308(8) 0.0219(7) 0.0007(6) 0.0085(6) 0.0037(6)
C11 0.0206(7) 0.0244(7) 0.0278(7) 0.0039(6) 0.0038(5) 0.0050(6)
C12 0.0231(7) 0.0270(8) 0.0411(9) 0.0074(7) 0.0036(6) -0.0067(6)
C13 0.0231(7) 0.0421(9) 0.0295(8) -0.0152(7) 0.0011(6) 0.0016(7)
C14 0.0401(9) 0.0200(7) 0.0272(8) 0.0066(6) 0.0156(7) 0.0080(6)
C15 0.0555(11) 0.0177(8) 0.0706(14) 0.0005(8) 0.0415(11) -0.0042(8)
C16 0.0350(8) 0.0187(7) 0.0340(8) -0.0027(6) 0.0064(7) -0.0058(7)
C17 0.0331(8) 0.0170(7) 0.0338(8) -0.0060(6) 0.0154(6) 0.0000(6)

_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
Zr N 2.1436(12) . ?
Zr C3 2.3214(15) . ?
Zr C7 2.3320(16) . ?
Zr C4 2.3333(15) . ?
Zr C1 2.3352(16) . ?
Zr O 2.3361(10) . ?
Zr C2 2.3542(15) . ?
Zr C6 2.3930(14) . ?
Zr C5 2.4080(14) . ?
Si1 N 1.7229(12) . ?
Si1 C10 1.8771(16) . ?
Si1 C8 1.8774(16) . ?
Si1 C9 1.8795(16) . ?
Si2 N 1.7238(12) . ?
Si2 C11 1.8678(15) . ?
Si2 C13 1.8768(16) . ?
Si2 C12 1.8798(16) . ?
O C14 1.4476(17) . ?
O C17 1.4610(17) . ?
C1 C2 1.413(3) . ?
C1 C7 1.425(2) . ?
C2 C3 1.416(3) . ?
C3 C4 1.428(2) . ?
C4 C5 1.424(2) . ?
C5 C6 1.408(2) . ?
C6 C7 1.427(2) . ?
C14 C15 1.510(2) . ?
C15 C16 1.516(2) . ?
C16 C17 1.518(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N Zr C3 111.45(5) . . ?
N Zr C7 132.86(5) . . ?
C3 Zr C7 86.48(6) . . ?
N Zr C4 133.56(5) . . ?
C3 Zr C4 35.74(6) . . ?
C7 Zr C4 86.41(6) . . ?
N Zr C1 111.27(5) . . ?
C3 Zr C1 66.38(6) . . ?
C7 Zr C1 35.56(6) . . ?
C4 Zr C1 86.29(6) . . ?
N Zr O 84.31(4) . . ?
C3 Zr O 137.99(5) . . ?
C7 Zr O 111.58(5) . . ?
C4 Zr O 105.36(5) . . ?
C1 Zr O 145.54(5) . . ?
N Zr C2 103.47(5) . . ?
C3 Zr C2 35.26(6) . . ?
C7 Zr C2 66.17(6) . . ?
C4 Zr C2 66.34(6) . . ?
C1 Zr C2 35.06(7) . . ?
O Zr C2 171.20(5) . . ?
N Zr C6 161.09(5) . . ?
C3 Zr C6 84.94(5) . . ?
C7 Zr C6 35.12(6) . . ?
C4 Zr C6 65.33(6) . . ?
C1 Zr C6 65.62(6) . . ?
O Zr C6 89.54(5) . . ?
C2 Zr C6 84.30(6) . . ?
N Zr C5 161.80(5) . . ?
C3 Zr C5 65.63(6) . . ?
C7 Zr C5 65.32(6) . . ?
C4 Zr C5 34.92(6) . . ?
C1 Zr C5 84.54(6) . . ?
O Zr C5 87.23(5) . . ?
C2 Zr C5 84.14(6) . . ?
C6 Zr C5 34.10(6) . . ?
N Si1 C10 112.97(7) . . ?
N Si1 C8 109.54(7) . . ?
C10 Si1 C8 106.99(7) . . ?
N Si1 C9 112.40(6) . . ?
C10 Si1 C9 106.87(7) . . ?
C8 Si1 C9 107.80(7) . . ?
N Si2 C11 111.78(6) . . ?
N Si2 C13 109.01(7) . . ?
C11 Si2 C13 108.37(8) . . ?
N Si2 C12 114.05(7) . . ?
C11 Si2 C12 107.87(7) . . ?
C13 Si2 C12 105.45(8) . . ?
C14 O C17 107.29(11) . . ?
C14 O Zr 128.26(8) . . ?
C17 O Zr 124.28(9) . . ?
Si1 N Si2 124.05(7) . . ?
Si1 N Zr 117.58(6) . . ?
Si2 N Zr 116.67(6) . . ?
C2 C1 C7 128.69(16) . . ?
C2 C1 Zr 73.20(9) . . ?
C7 C1 Zr 72.10(9) . . ?
C1 C2 C3 128.60(15) . . ?
C1 C2 Zr 71.74(9) . . ?
C3 C2 Zr 71.11(9) . . ?
C2 C3 C4 128.71(15) . . ?
C2 C3 Zr 73.64(9) . . ?
C4 C3 Zr 72.58(9) . . ?
C5 C4 C3 127.97(16) . . ?
C5 C4 Zr 75.41(9) . . ?
C3 C4 Zr 71.67(9) . . ?
C6 C5 C4 128.53(15) . . ?
C6 C5 Zr 72.36(8) . . ?
C4 C5 Zr 69.67(8) . . ?
C5 C6 C7 129.03(15) . . ?
C5 C6 Zr 73.53(9) . . ?
C7 C6 Zr 70.10(9) . . ?
C1 C7 C6 127.91(16) . . ?
C1 C7 Zr 72.34(9) . . ?
C6 C7 Zr 74.77(9) . . ?
O C14 C15 104.03(13) . . ?
C14 C15 C16 103.94(13) . . ?
C15 C16 C17 105.46(13) . . ?
O C17 C16 106.25(12) . . ?

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
N Zr O C14 33.25(12) . . . . ?
C3 Zr O C14 -82.76(13) . . . . ?
C7 Zr O C14 167.33(12) . . . . ?
C4 Zr O C14 -100.45(12) . . . . ?
C1 Zr O C14 153.19(12) . . . . ?
C2 Zr O C14 -119.3(3) . . . . ?
C6 Zr O C14 -164.66(12) . . . . ?
C5 Zr O C14 -130.62(12) . . . . ?
N Zr O C17 -152.12(11) . . . . ?
C3 Zr O C17 91.87(12) . . . . ?
C7 Zr O C17 -18.04(12) . . . . ?
C4 Zr O C17 74.18(12) . . . . ?
C1 Zr O C17 -32.17(15) . . . . ?
C2 Zr O C17 55.4(4) . . . . ?
C6 Zr O C17 9.97(11) . . . . ?
C5 Zr O C17 44.02(11) . . . . ?
C10 Si1 N Si2 -31.63(10) . . . . ?
C8 Si1 N Si2 -150.79(8) . . . . ?
C9 Si1 N Si2 89.41(9) . . . . ?
C10 Si1 N Zr 163.78(7) . . . . ?
C8 Si1 N Zr 44.62(9) . . . . ?
C9 Si1 N Zr -75.19(8) . . . . ?
C11 Si2 N Si1 -55.64(10) . . . . ?
C13 Si2 N Si1 -175.41(9) . . . . ?
C12 Si2 N Si1 67.06(10) . . . . ?
C11 Si2 N Zr 109.09(7) . . . . ?
C13 Si2 N Zr -10.69(9) . . . . ?
C12 Si2 N Zr -128.22(8) . . . . ?
C3 Zr N Si1 28.30(8) . . . . ?
C7 Zr N Si1 134.23(7) . . . . ?
C4 Zr N Si1 -5.62(10) . . . . ?
C1 Zr N Si1 100.30(8) . . . . ?
O Zr N Si1 -111.45(6) . . . . ?
C2 Zr N Si1 64.39(8) . . . . ?
C6 Zr N Si1 176.96(13) . . . . ?
C5 Zr N Si1 -48.71(18) . . . . ?
C3 Zr N Si2 -137.45(7) . . . . ?
C7 Zr N Si2 -31.51(10) . . . . ?
C4 Zr N Si2 -171.36(7) . . . . ?
C1 Zr N Si2 -65.45(8) . . . . ?
O Zr N Si2 82.81(6) . . . . ?
C2 Zr N Si2 -101.35(7) . . . . ?
C6 Zr N Si2 11.22(19) . . . . ?
C5 Zr N Si2 145.55(14) . . . . ?
N Zr C1 C2 -83.13(10) . . . . ?
C3 Zr C1 C2 21.82(9) . . . . ?
C7 Zr C1 C2 141.60(15) . . . . ?
C4 Zr C1 C2 52.58(10) . . . . ?
O Zr C1 C2 164.58(8) . . . . ?
C6 Zr C1 C2 117.12(11) . . . . ?
C5 Zr C1 C2 87.58(10) . . . . ?
N Zr C1 C7 135.27(10) . . . . ?
C3 Zr C1 C7 -119.78(11) . . . . ?
C4 Zr C1 C7 -89.02(11) . . . . ?
O Zr C1 C7 22.98(15) . . . . ?
C2 Zr C1 C7 -141.60(15) . . . . ?
C6 Zr C1 C7 -24.47(10) . . . . ?
C5 Zr C1 C7 -54.02(10) . . . . ?
C7 C1 C2 C3 3.6(3) . . . . ?
Zr C1 C2 C3 -45.59(16) . . . . ?
C7 C1 C2 Zr 49.22(16) . . . . ?
N Zr C2 C1 107.95(10) . . . . ?
C3 Zr C2 C1 -143.84(14) . . . . ?
C7 Zr C2 C1 -23.26(9) . . . . ?
C4 Zr C2 C1 -120.09(11) . . . . ?
O Zr C2 C1 -100.3(3) . . . . ?
C6 Zr C2 C1 -54.56(10) . . . . ?
C5 Zr C2 C1 -88.84(10) . . . . ?
N Zr C2 C3 -108.21(9) . . . . ?
C7 Zr C2 C3 120.58(11) . . . . ?
C4 Zr C2 C3 23.76(9) . . . . ?
C1 Zr C2 C3 143.84(14) . . . . ?
O Zr C2 C3 43.6(4) . . . . ?
C6 Zr C2 C3 89.29(10) . . . . ?
C5 Zr C2 C3 55.00(10) . . . . ?
C1 C2 C3 C4 -4.8(3) . . . . ?
Zr C2 C3 C4 -50.57(15) . . . . ?
C1 C2 C3 Zr 45.80(16) . . . . ?
N Zr C3 C2 82.98(10) . . . . ?
C7 Zr C3 C2 -52.09(10) . . . . ?
C4 Zr C3 C2 -140.83(15) . . . . ?
C1 Zr C3 C2 -21.71(9) . . . . ?
O Zr C3 C2 -170.94(8) . . . . ?
C6 Zr C3 C2 -87.28(10) . . . . ?
C5 Zr C3 C2 -116.54(11) . . . . ?
N Zr C3 C4 -136.19(9) . . . . ?
C7 Zr C3 C4 88.74(10) . . . . ?
C1 Zr C3 C4 119.12(11) . . . . ?
O Zr C3 C4 -30.11(13) . . . . ?
C2 Zr C3 C4 140.83(15) . . . . ?
C6 Zr C3 C4 53.55(10) . . . . ?
C5 Zr C3 C4 24.29(10) . . . . ?
C2 C3 C4 C5 -2.5(3) . . . . ?
Zr C3 C4 C5 -53.47(15) . . . . ?
C2 C3 C4 Zr 50.96(15) . . . . ?
N Zr C4 C5 -158.12(9) . . . . ?
C3 Zr C4 C5 139.11(15) . . . . ?
C7 Zr C4 C5 50.14(10) . . . . ?
C1 Zr C4 C5 85.78(10) . . . . ?
O Zr C4 C5 -61.26(10) . . . . ?
C2 Zr C4 C5 115.65(11) . . . . ?
C6 Zr C4 C5 20.96(9) . . . . ?
N Zr C4 C3 62.77(12) . . . . ?
C7 Zr C4 C3 -88.97(10) . . . . ?
C1 Zr C4 C3 -53.33(10) . . . . ?
O Zr C4 C3 159.63(9) . . . . ?
C2 Zr C4 C3 -23.46(10) . . . . ?
C6 Zr C4 C3 -118.16(11) . . . . ?
C5 Zr C4 C3 -139.11(15) . . . . ?
C3 C4 C5 C6 7.1(3) . . . . ?
Zr C4 C5 C6 -44.92(16) . . . . ?
C3 C4 C5 Zr 52.02(15) . . . . ?
N Zr C5 C6 -155.58(14) . . . . ?
C3 Zr C5 C6 119.75(11) . . . . ?
C7 Zr C5 C6 22.05(9) . . . . ?
C4 Zr C5 C6 144.57(15) . . . . ?
C1 Zr C5 C6 53.24(10) . . . . ?
O Zr C5 C6 -93.26(9) . . . . ?
C2 Zr C5 C6 88.48(10) . . . . ?
N Zr C5 C4 59.85(19) . . . . ?
C3 Zr C5 C4 -24.82(10) . . . . ?
C7 Zr C5 C4 -122.53(11) . . . . ?
C1 Zr C5 C4 -91.33(11) . . . . ?
O Zr C5 C4 122.17(10) . . . . ?
C2 Zr C5 C4 -56.09(11) . . . . ?
C6 Zr C5 C4 -144.57(15) . . . . ?
C4 C5 C6 C7 -1.8(3) . . . . ?
Zr C5 C6 C7 -45.86(16) . . . . ?
C4 C5 C6 Zr 44.01(15) . . . . ?
N Zr C6 C5 156.52(13) . . . . ?
C3 Zr C6 C5 -52.55(10) . . . . ?
C7 Zr C6 C5 -143.64(15) . . . . ?
C4 Zr C6 C5 -21.42(9) . . . . ?
C1 Zr C6 C5 -118.88(11) . . . . ?
O Zr C6 C5 85.75(9) . . . . ?
C2 Zr C6 C5 -87.97(10) . . . . ?
N Zr C6 C7 -59.84(19) . . . . ?
C3 Zr C6 C7 91.09(10) . . . . ?
C4 Zr C6 C7 122.22(11) . . . . ?
C1 Zr C6 C7 24.76(10) . . . . ?
O Zr C6 C7 -130.61(10) . . . . ?
C2 Zr C6 C7 55.68(10) . . . . ?
C5 Zr C6 C7 143.64(15) . . . . ?
C2 C1 C7 C6 3.7(3) . . . . ?
Zr C1 C7 C6 53.33(16) . . . . ?
C2 C1 C7 Zr -49.63(16) . . . . ?
C5 C6 C7 C1 -5.3(3) . . . . ?
Zr C6 C7 C1 -52.38(16) . . . . ?
C5 C6 C7 Zr 47.04(16) . . . . ?
N Zr C7 C1 -63.45(12) . . . . ?
C3 Zr C7 C1 52.82(11) . . . . ?
C4 Zr C7 C1 88.64(11) . . . . ?
O Zr C7 C1 -166.26(9) . . . . ?
C2 Zr C7 C1 22.96(10) . . . . ?
C6 Zr C7 C1 139.02(15) . . . . ?
C5 Zr C7 C1 117.56(11) . . . . ?
N Zr C7 C6 157.53(8) . . . . ?
C3 Zr C7 C6 -86.19(10) . . . . ?
C4 Zr C7 C6 -50.38(10) . . . . ?
C1 Zr C7 C6 -139.02(15) . . . . ?
O Zr C7 C6 54.73(10) . . . . ?
C2 Zr C7 C6 -116.05(11) . . . . ?
C5 Zr C7 C6 -21.46(9) . . . . ?
C17 O C14 C15 35.77(16) . . . . ?
Zr O C14 C15 -148.88(11) . . . . ?
O C14 C15 C16 -34.30(18) . . . . ?
C14 C15 C16 C17 20.4(2) . . . . ?
C14 O C17 C16 -22.72(16) . . . . ?
Zr O C17 C16 161.69(9) . . . . ?
C15 C16 C17 O 0.60(19) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        72.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.059
_iucr_refine_instructions_details 
;
TITL andyg51 in P2(1)/c
CELL 1.54184 10.2102 10.7387 19.2391 90.000 99.648 90.000
ZERR 4.00 0.0002 0.0002 0.0004 0.000 0.002 0.000
LATT 1
SYMM - X, 1/2 + Y, 1/2 - Z
SFAC C H O SI ZR N
UNIT 68 132 4 8 4 4
SIZE 0.13 0.09 0.05
TEMP -173
ACTA 145
CONF

FMAP 2
PLAN 10
L.S. 8

OMIT -6 11 10
OMIT 12 0 4
OMIT -4 12 9
OMIT -8 7 16
OMIT 8 9 7
OMIT 10 7 5
OMIT 7 10 7
OMIT 1 12 10
OMIT 8 1 16
OMIT -10 5 15
OMIT 8 3 15
OMIT -2 5 22
OMIT -4 12 8
OMIT 7 10 6
OMIT 7 4 16

WGHT 0.030000 1.025500
EXTI 0.001142
FVAR 4.64751
ZR 5 0.665240 0.264200 0.158295 11.00000 0.01515 0.01266 =
0.01719 -0.00063 0.00603 -0.00080
SI1 4 0.779163 0.176814 0.014353 11.00000 0.01608 0.01800 =
0.01718 -0.00209 0.00409 0.00179
SI2 4 0.978435 0.279528 0.136362 11.00000 0.01441 0.01639 =
0.01986 -0.00056 0.00327 0.00034
O 3 0.674307 0.476939 0.134171 11.00000 0.02456 0.01357 =
0.02336 -0.00012 0.01033 0.00127
N 6 0.818394 0.249726 0.094925 11.00000 0.01489 0.01481 =
0.01792 -0.00079 0.00495 0.00064
C1 1 0.689605 0.112243 0.246346 11.00000 0.03378 0.02868 =
0.03223 0.01406 0.01510 0.00710
H1 2 0.767375 0.072684 0.266290 11.00000 0.04201
C2 1 0.621944 0.055525 0.184328 11.00000 0.04032 0.01356 =
0.04267 0.00307 0.02449 -0.00180
H2 2 0.664330 -0.014661 0.167665 11.00000 0.03742
C3 1 0.513622 0.102158 0.135581 11.00000 0.03156 0.02325 =
0.03482 -0.00880 0.01617 -0.01445
H3 2 0.491966 0.056000 0.094308 11.00000 0.03789
C4 1 0.439668 0.214186 0.139281 11.00000 0.01837 0.03353 =
0.03141 0.00040 0.00705 -0.00835
H4 2 0.375839 0.233731 0.099297 11.00000 0.03440
C5 1 0.454597 0.303856 0.194609 11.00000 0.02085 0.02339 =
0.03705 0.00124 0.01633 0.00128
H5 2 0.400954 0.370951 0.187142 11.00000 0.03097
C6 1 0.553431 0.310368 0.255050 11.00000 0.03208 0.02220 =
0.02746 -0.00527 0.01834 -0.00377
H6 2 0.554823 0.380580 0.279711 11.00000 0.02796
C7 1 0.661593 0.227596 0.277434 11.00000 0.03190 0.03441 =
0.01973 0.00256 0.00901 -0.00405
H7 2 0.727242 0.253140 0.318039 11.00000 0.02949
C8 1 0.613327 0.233500 -0.031916 11.00000 0.02156 0.03611 =
0.02258 -0.00213 0.00160 0.00413
AFIX 137
H8A 2 0.547548 0.224683 -0.000537 11.00000 -1.50000
H8B 2 0.585585 0.184098 -0.074677 11.00000 -1.50000
H8C 2 0.620285 0.321309 -0.044684 11.00000 -1.50000
AFIX 0
C9 1 0.769146 0.002861 0.022871 11.00000 0.03009 0.02012 =
0.03128 -0.00720 0.00917 -0.00086
AFIX 137
H9A 2 0.850234 -0.027971 0.052413 11.00000 -1.50000
H9B 2 0.759983 -0.035272 -0.023972 11.00000 -1.50000
H9C 2 0.691997 -0.018875 0.044614 11.00000 -1.50000
AFIX 0
C10 1 0.902364 0.209291 -0.045653 11.00000 0.02459 0.03078 =
0.02189 0.00073 0.00845 0.00367
AFIX 137
H10A 2 0.900211 0.298084 -0.057551 11.00000 -1.50000
H10B 2 0.879532 0.160102 -0.088892 11.00000 -1.50000
H10C 2 0.991669 0.186644 -0.021844 11.00000 -1.50000
AFIX 0
C11 1 1.081053 0.134705 0.148326 11.00000 0.02057 0.02440 =
0.02778 0.00387 0.00381 0.00498
AFIX 137
H11A 2 1.042307 0.076150 0.178279 11.00000 -1.50000
H11B 2 1.171799 0.155567 0.170713 11.00000 -1.50000
H11C 2 1.082896 0.096412 0.102263 11.00000 -1.50000
AFIX 0
C12 1 1.069006 0.396973 0.089608 11.00000 0.02308 0.02703 =
0.04114 0.00740 0.00357 -0.00672
AFIX 137
H12A 2 1.083800 0.362575 0.044383 11.00000 -1.50000
H12B 2 1.154732 0.416502 0.118779 11.00000 -1.50000
H12C 2 1.015703 0.473070 0.081290 11.00000 -1.50000
AFIX 0
C13 1 0.973186 0.348058 0.225591 11.00000 0.02307 0.04207 =
0.02948 -0.01524 0.00108 0.00165
AFIX 137
H13A 2 0.914779 0.421070 0.220547 11.00000 -1.50000
H13B 2 1.062948 0.373033 0.247533 11.00000 -1.50000
H13C 2 0.939092 0.285856 0.255285 11.00000 -1.50000
AFIX 0
C14 1 0.702707 0.536458 0.070840 11.00000 0.04011 0.01996 =
0.02723 0.00664 0.01560 0.00798
AFIX 23
H14A 2 0.619881 0.552693 0.037245 11.00000 -1.20000
H14B 2 0.762222 0.484135 0.047404 11.00000 -1.20000
AFIX 0
C15 1 0.770004 0.656863 0.096936 11.00000 0.05546 0.01769 =
0.07063 0.00046 0.04147 -0.00417
AFIX 23
H15A 2 0.757073 0.721173 0.059543 11.00000 -1.20000
H15B 2 0.866409 0.644136 0.112815 11.00000 -1.20000
AFIX 0
C16 1 0.702000 0.693966 0.158075 11.00000 0.03503 0.01870 =
0.03398 -0.00273 0.00641 -0.00575
AFIX 23
H16A 2 0.632839 0.757579 0.143100 11.00000 -1.20000
H16B 2 0.767202 0.728158 0.197339 11.00000 -1.20000
AFIX 0
C17 1 0.640219 0.575169 0.180562 11.00000 0.03308 0.01703 =
0.03382 -0.00600 0.01540 -0.00001
AFIX 23
H17A 2 0.676257 0.555562 0.230379 11.00000 -1.20000
H17B 2 0.542587 0.584167 0.175541 11.00000 -1.20000
HKLF 4
;