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

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Norbert Mitzel'
'Beate Neumann'
'Hans-Georg Stammler'
'Alexander Willner'

_publ_contact_author_name        'Norbert Mitzel'
_publ_contact_author_email       MITZEL@UNI-BIELEFELD.DE

_publ_section_title              
;
Transformation of hydroxylamide into hydra-zide
units in the coordination spheres of group 4 metals
;

# Attachment 'compounds_2_3.CIF'

data_compound2
_database_code_depnum_ccdc_archive 'CCDC 729348'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H33 N3 O Si Ti'
_chemical_formula_sum            'C16 H33 N3 O Si Ti'
_chemical_formula_weight         359.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'C m c a'

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

_cell_length_a                   14.9808(7)
_cell_length_b                   10.0118(4)
_cell_length_c                   26.2621(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3938.9(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    31490
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      30.034

_exptl_crystal_description       fragment
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1552
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8643
_exptl_absorpt_correction_T_max  0.8643
_exptl_absorpt_process_details   
'Denzo and Scalepack (Otwinowski & Minor, 1997)'

_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  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17269
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         29.96
_reflns_number_total             2929
_reflns_number_gt                2169
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
Disorder of N(1) to C(11) on the mirror plane. Therefore this ligands were

refined with a part -1.

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^)+(0.0566P)^2^+2.5670P] 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         2929
_refine_ls_number_parameters     150
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0429
_refine_ls_wR_factor_ref         0.1157
_refine_ls_wR_factor_gt          0.1058
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 1.0000 0.19121(4) 0.107848(15) 0.02792(13) Uani 1 2 d S . .
Si1 Si 1.0000 -0.06737(6) 0.15532(2) 0.02847(17) Uani 1 2 d S . .
O1 O 1.0000 0.00009(19) 0.09926(7) 0.0649(8) Uani 1 2 d S A .
C1 C 1.0000 0.0956(2) 0.18988(8) 0.0220(4) Uani 1 2 d S . .
C2 C 1.07627(11) 0.18124(17) 0.18799(6) 0.0274(3) Uani 1 1 d . A .
C3 C 1.04679(14) 0.31533(17) 0.18497(6) 0.0353(4) Uani 1 1 d . . .
C4 C 1.17284(12) 0.1389(3) 0.19048(8) 0.0488(5) Uani 1 1 d . . .
H4A H 1.1907 0.1009 0.1576 0.073 Uiso 1 1 calc R A .
H4B H 1.1803 0.0717 0.2173 0.073 Uiso 1 1 calc R . .
H4C H 1.2102 0.2167 0.1981 0.073 Uiso 1 1 calc R . .
C5 C 1.1031(2) 0.4397(2) 0.18621(9) 0.0680(8) Uani 1 1 d . . .
H5A H 1.0916 0.4885 0.2179 0.102 Uiso 1 1 calc R A .
H5B H 1.0880 0.4964 0.1570 0.102 Uiso 1 1 calc R . .
H5C H 1.1663 0.4151 0.1845 0.102 Uiso 1 1 calc R . .
C6 C 1.09841(18) -0.1764(2) 0.16603(12) 0.0725(8) Uani 1 1 d . A .
H6A H 1.0962 -0.2523 0.1425 0.109 Uiso 1 1 calc R . .
H6B H 1.0978 -0.2093 0.2012 0.109 Uiso 1 1 calc R . .
H6C H 1.1532 -0.1253 0.1601 0.109 Uiso 1 1 calc R . .
N1 N 1.0907(9) 0.2624(19) 0.0740(7) 0.039(2) Uani 0.50 1 d P A -1
N2 N 1.0634(2) 0.1830(3) 0.03394(10) 0.0339(6) Uani 0.50 1 d P A -1
N3 N 0.8877(8) 0.2737(17) 0.0763(6) 0.0314(17) Uani 0.50 1 d P A -1
C7 C 1.1764(3) 0.3327(6) 0.07049(17) 0.0548(12) Uani 0.50 1 d P A -1
H7A H 1.2244 0.2678 0.0649 0.082 Uiso 0.50 1 calc PR A -1
H7B H 1.1876 0.3813 0.1023 0.082 Uiso 0.50 1 calc PR A -1
H7C H 1.1746 0.3959 0.0420 0.082 Uiso 0.50 1 calc PR A -1
C8 C 1.1220(3) 0.0707(5) 0.02262(16) 0.0505(11) Uani 0.50 1 d P A -1
H8A H 1.0921 0.0098 -0.0011 0.076 Uiso 0.50 1 calc PR A -1
H8B H 1.1361 0.0230 0.0542 0.076 Uiso 0.50 1 calc PR A -1
H8C H 1.1773 0.1037 0.0071 0.076 Uiso 0.50 1 calc PR A -1
C9 C 1.0388(3) 0.2559(5) -0.01242(13) 0.0499(11) Uani 0.50 1 d P A -1
H9A H 1.0929 0.2890 -0.0292 0.075 Uiso 0.50 1 calc PR A -1
H9B H 1.0003 0.3315 -0.0035 0.075 Uiso 1 2 calc SR A -1
H9C H 1.0067 0.1960 -0.0356 0.075 Uiso 0.50 1 calc PR A -1
C10 C 0.8072(3) 0.1940(5) 0.06598(18) 0.0563(12) Uani 0.50 1 d P A -1
H10A H 0.7564 0.2322 0.0845 0.084 Uiso 0.50 1 calc PR A -1
H10B H 0.8169 0.1018 0.0772 0.084 Uiso 0.50 1 calc PR A -1
H10C H 0.7946 0.1949 0.0294 0.084 Uiso 0.50 1 calc PR A -1
C11 C 0.8753(4) 0.4099(5) 0.0606(2) 0.0686(16) Uani 0.50 1 d P A -1
H11A H 0.8621 0.4126 0.0241 0.103 Uiso 0.50 1 calc PR A -1
H11B H 0.9298 0.4608 0.0675 0.103 Uiso 0.50 1 calc PR A -1
H11C H 0.8254 0.4491 0.0796 0.103 Uiso 0.50 1 calc PR A -1

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
Ti1 0.0442(3) 0.0223(2) 0.01727(19) 0.00102(14) 0.000 0.000
Si1 0.0372(4) 0.0221(3) 0.0262(3) 0.0019(2) 0.000 0.000
O1 0.150(2) 0.0193(9) 0.0251(9) -0.0022(7) 0.000 0.000
C1 0.0225(10) 0.0266(10) 0.0168(9) 0.0033(7) 0.000 0.000
C2 0.0251(8) 0.0348(8) 0.0223(7) 0.0008(6) -0.0031(6) -0.0063(7)
C3 0.0562(11) 0.0276(8) 0.0220(7) -0.0024(6) 0.0004(7) -0.0104(8)
C4 0.0238(9) 0.0741(15) 0.0485(12) 0.0031(10) -0.0047(8) -0.0088(10)
C5 0.113(2) 0.0470(13) 0.0443(12) -0.0110(10) 0.0085(13) -0.0438(14)
C6 0.0700(17) 0.0467(13) 0.101(2) -0.0245(14) -0.0152(16) 0.0270(12)
N1 0.038(6) 0.047(4) 0.031(2) -0.004(2) -0.003(4) -0.023(4)
N2 0.0427(17) 0.0391(16) 0.0199(12) -0.0022(11) 0.0054(12) -0.0062(14)
N3 0.034(5) 0.037(3) 0.024(3) 0.000(2) -0.007(3) 0.019(3)
C7 0.051(3) 0.077(4) 0.037(2) -0.005(2) 0.011(2) -0.027(3)
C8 0.046(2) 0.063(3) 0.042(2) -0.0075(19) 0.0203(18) -0.004(2)
C9 0.073(3) 0.056(2) 0.0204(16) 0.0058(15) 0.0042(17) -0.023(2)
C10 0.036(2) 0.086(4) 0.047(2) -0.005(2) -0.0152(19) 0.008(2)
C11 0.089(4) 0.055(3) 0.061(3) 0.013(2) -0.022(3) 0.031(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 N1 1.773(15) 11_755 ?
Ti1 N1 1.773(15) . ?
Ti1 O1 1.927(2) . ?
Ti1 N3 2.049(12) . ?
Ti1 N3 2.049(12) 11_755 ?
Ti1 N2 2.163(3) . ?
Ti1 N2 2.163(3) 11_755 ?
Ti1 C1 2.357(2) . ?
Ti1 C2 2.3969(16) . ?
Ti1 C2 2.3970(16) 11_755 ?
Ti1 C3 2.4775(17) . ?
Ti1 C3 2.4775(17) 11_755 ?
Si1 O1 1.6196(19) . ?
Si1 C6 1.856(2) . ?
Si1 C6 1.856(2) 11_755 ?
Si1 C1 1.867(2) . ?
C1 C2 1.429(2) 11_755 ?
C1 C2 1.429(2) . ?
C2 C3 1.415(2) . ?
C2 C4 1.509(3) . ?
C3 C3 1.402(4) 11_755 ?
C3 C5 1.504(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
N1 N2 1.380(16) . ?
N1 C7 1.468(11) . ?
N2 C8 1.458(5) . ?
N2 C9 1.467(5) . ?
N3 C11 1.436(17) . ?
N3 C10 1.472(17) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 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 Ti1 N1 100.1(12) 11_755 . ?
N1 Ti1 O1 109.9(6) 11_755 . ?
N1 Ti1 O1 109.9(6) . . ?
N1 Ti1 N3 6.4(9) 11_755 . ?
N1 Ti1 N3 105.4(2) . . ?
O1 Ti1 N3 110.7(5) . . ?
N1 Ti1 N3 105.4(2) 11_755 11_755 ?
N1 Ti1 N3 6.4(9) . 11_755 ?
O1 Ti1 N3 110.7(5) . 11_755 ?
N3 Ti1 N3 110.4(9) . 11_755 ?
N1 Ti1 N2 84.4(5) 11_755 . ?
N1 Ti1 N2 39.5(5) . . ?
O1 Ti1 N2 81.80(9) . . ?
N3 Ti1 N2 90.8(4) . . ?
N3 Ti1 N2 44.9(4) 11_755 . ?
N1 Ti1 N2 39.5(5) 11_755 11_755 ?
N1 Ti1 N2 84.4(5) . 11_755 ?
O1 Ti1 N2 81.80(9) . 11_755 ?
N3 Ti1 N2 44.9(4) . 11_755 ?
N3 Ti1 N2 90.8(4) 11_755 11_755 ?
N2 Ti1 N2 52.13(17) . 11_755 ?
N1 Ti1 C1 128.4(5) 11_755 . ?
N1 Ti1 C1 128.4(5) . . ?
O1 Ti1 C1 72.76(8) . . ?
N3 Ti1 C1 122.2(4) . . ?
N3 Ti1 C1 122.2(4) 11_755 . ?
N2 Ti1 C1 143.59(9) . . ?
N2 Ti1 C1 143.59(9) 11_755 . ?
N1 Ti1 C2 145.3(5) 11_755 . ?
N1 Ti1 C2 95.2(5) . . ?
O1 Ti1 C2 93.52(6) . . ?
N3 Ti1 C2 139.7(4) . . ?
N3 Ti1 C2 88.9(4) 11_755 . ?
N2 Ti1 C2 125.24(9) . . ?
N2 Ti1 C2 174.85(9) 11_755 . ?
C1 Ti1 C2 34.98(5) . . ?
N1 Ti1 C2 95.2(5) 11_755 11_755 ?
N1 Ti1 C2 145.3(5) . 11_755 ?
O1 Ti1 C2 93.52(6) . 11_755 ?
N3 Ti1 C2 88.9(4) . 11_755 ?
N3 Ti1 C2 139.7(4) 11_755 11_755 ?
N2 Ti1 C2 174.85(9) . 11_755 ?
N2 Ti1 C2 125.24(9) 11_755 11_755 ?
C1 Ti1 C2 34.98(5) . 11_755 ?
C2 Ti1 C2 56.94(8) . 11_755 ?
N1 Ti1 C3 115.2(6) 11_755 . ?
N1 Ti1 C3 89.5(5) . . ?
O1 Ti1 C3 126.43(7) . . ?
N3 Ti1 C3 111.1(4) . . ?
N3 Ti1 C3 84.0(4) 11_755 . ?
N2 Ti1 C3 128.93(9) . . ?
N2 Ti1 C3 151.29(9) 11_755 . ?
C1 Ti1 C3 57.09(6) . . ?
C2 Ti1 C3 33.71(6) . . ?
C2 Ti1 C3 55.80(6) 11_755 . ?
N1 Ti1 C3 89.5(5) 11_755 11_755 ?
N1 Ti1 C3 115.2(6) . 11_755 ?
O1 Ti1 C3 126.42(7) . 11_755 ?
N3 Ti1 C3 84.0(4) . 11_755 ?
N3 Ti1 C3 111.1(4) 11_755 11_755 ?
N2 Ti1 C3 151.29(9) . 11_755 ?
N2 Ti1 C3 128.93(9) 11_755 11_755 ?
C1 Ti1 C3 57.08(6) . 11_755 ?
C2 Ti1 C3 55.80(6) . 11_755 ?
C2 Ti1 C3 33.71(6) 11_755 11_755 ?
C3 Ti1 C3 32.87(10) . 11_755 ?
O1 Si1 C6 112.53(11) . . ?
O1 Si1 C6 112.53(11) . 11_755 ?
C6 Si1 C6 105.18(19) . 11_755 ?
O1 Si1 C1 94.44(10) . . ?
C6 Si1 C1 116.13(9) . . ?
C6 Si1 C1 116.13(9) 11_755 . ?
O1 Si1 Ti1 39.64(7) . . ?
C6 Si1 Ti1 126.57(10) . . ?
C6 Si1 Ti1 126.57(10) 11_755 . ?
C1 Si1 Ti1 54.80(6) . . ?
Si1 O1 Ti1 107.93(10) . . ?
C2 C1 C2 106.1(2) 11_755 . ?
C2 C1 Si1 120.49(11) 11_755 . ?
C2 C1 Si1 120.49(11) . . ?
C2 C1 Ti1 74.02(10) 11_755 . ?
C2 C1 Ti1 74.02(10) . . ?
Si1 C1 Ti1 84.87(8) . . ?
C3 C2 C1 108.76(16) . . ?
C3 C2 C4 124.60(17) . . ?
C1 C2 C4 126.61(17) . . ?
C3 C2 Ti1 76.27(10) . . ?
C1 C2 Ti1 71.00(10) . . ?
C4 C2 Ti1 120.45(12) . . ?
C3 C3 C2 108.18(11) 11_755 . ?
C3 C3 C5 124.11(15) 11_755 . ?
C2 C3 C5 127.5(2) . . ?
C3 C3 Ti1 73.57(5) 11_755 . ?
C2 C3 Ti1 70.02(9) . . ?
C5 C3 Ti1 126.26(13) . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1 C6 H6A 109.5 . . ?
Si1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N2 N1 C7 119.1(13) . . ?
N2 N1 Ti1 85.6(6) . . ?
C7 N1 Ti1 153.5(12) . . ?
N1 N2 C8 114.9(8) . . ?
N1 N2 C9 114.9(9) . . ?
C8 N2 C9 111.5(3) . . ?
N1 N2 Ti1 54.8(6) . . ?
C8 N2 Ti1 118.5(2) . . ?
C9 N2 Ti1 128.0(3) . . ?
C11 N3 C10 110.8(8) . . ?
C11 N3 Ti1 127.2(10) . . ?
C10 N3 Ti1 121.9(10) . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        29.96
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.054

#==============================================================================

data_compound3
_database_code_depnum_ccdc_archive 'CCDC 729349'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H66 N6 O2 Si2 Zr2'
_chemical_formula_sum            'C32 H66 N6 O2 Si2 Zr2'
_chemical_formula_weight         805.53

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

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

_cell_length_a                   10.2455(2)
_cell_length_b                   14.0552(3)
_cell_length_c                   13.9038(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.2933(14)
_cell_angle_gamma                90.00
_cell_volume                     1998.88(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    38546
_cell_measurement_theta_min      2.910
_cell_measurement_theta_max      27.485

_exptl_crystal_description       fragment
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             848
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8369
_exptl_absorpt_correction_T_max  0.9410
_exptl_absorpt_process_details   
'Denzo and Scalepack (Otwinowski & Minor, 1997)'

_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  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            40492
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         27.45
_reflns_number_total             4569
_reflns_number_gt                3902
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect, Bruker AXS, 2004'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-PLUS (1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0415P)^2^+1.2628P] 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         4569
_refine_ls_number_parameters     210
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0295
_refine_ls_wR_factor_ref         0.0801
_refine_ls_wR_factor_gt          0.0760
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.496899(18) 0.393593(13) 0.680550(12) 0.02043(7) Uani 1 1 d . . .
Si1 Si 0.28051(5) 0.55218(4) 0.50107(4) 0.02136(12) Uani 1 1 d . . .
O1 O 0.40186(14) 0.57338(10) 0.43393(10) 0.0251(3) Uani 1 1 d . . .
N1 N 0.4000(2) 0.26722(14) 0.68445(16) 0.0404(5) Uani 1 1 d . . .
N2 N 0.5076(2) 0.23031(15) 0.63707(16) 0.0421(5) Uani 1 1 d . . .
N3 N 0.6399(2) 0.37173(14) 0.79115(13) 0.0326(4) Uani 1 1 d . . .
C1 C 0.33290(19) 0.52230(14) 0.62913(14) 0.0221(4) Uani 1 1 d . . .
C2 C 0.4360(2) 0.56804(14) 0.68601(14) 0.0237(4) Uani 1 1 d . . .
C3 C 0.4328(2) 0.53780(15) 0.78273(14) 0.0270(4) Uani 1 1 d . . .
C4 C 0.3279(2) 0.47244(16) 0.78818(14) 0.0284(4) Uani 1 1 d . . .
C5 C 0.26545(19) 0.46383(15) 0.69488(14) 0.0252(4) Uani 1 1 d . . .
C6 C 0.5276(2) 0.64206(15) 0.65099(16) 0.0288(4) Uani 1 1 d . . .
H6A H 0.4891 0.7053 0.6580 0.043 Uiso 1 1 calc R . .
H6B H 0.5426 0.6305 0.5830 0.043 Uiso 1 1 calc R . .
H6C H 0.6110 0.6387 0.6891 0.043 Uiso 1 1 calc R . .
C7 C 0.5185(2) 0.57468(18) 0.86586(16) 0.0360(5) Uani 1 1 d . . .
H7A H 0.6069 0.5856 0.8448 0.054 Uiso 1 1 calc R . .
H7B H 0.5219 0.5279 0.9182 0.054 Uiso 1 1 calc R . .
H7C H 0.4826 0.6346 0.8888 0.054 Uiso 1 1 calc R . .
C8 C 0.2826(3) 0.4281(2) 0.87918(16) 0.0403(6) Uani 1 1 d . . .
H8A H 0.2132 0.4673 0.9044 0.060 Uiso 1 1 calc R . .
H8B H 0.3562 0.4242 0.9272 0.060 Uiso 1 1 calc R . .
H8C H 0.2489 0.3641 0.8651 0.060 Uiso 1 1 calc R . .
C9 C 0.1394(2) 0.41052(19) 0.67376(18) 0.0375(5) Uani 1 1 d . . .
H9A H 0.1157 0.3764 0.7317 0.056 Uiso 1 1 calc R . .
H9B H 0.1506 0.3649 0.6216 0.056 Uiso 1 1 calc R . .
H9C H 0.0699 0.4556 0.6543 0.056 Uiso 1 1 calc R . .
C10 C 0.1772(2) 0.66224(16) 0.50483(16) 0.0326(5) Uani 1 1 d . . .
H10A H 0.2306 0.7154 0.5302 0.049 Uiso 1 1 calc R . .
H10B H 0.1048 0.6512 0.5466 0.049 Uiso 1 1 calc R . .
H10C H 0.1420 0.6776 0.4396 0.049 Uiso 1 1 calc R . .
C11 C 0.1789(2) 0.45276(16) 0.44700(15) 0.0312(5) Uani 1 1 d . . .
H11A H 0.1693 0.4609 0.3769 0.047 Uiso 1 1 calc R . .
H11B H 0.0924 0.4536 0.4736 0.047 Uiso 1 1 calc R . .
H11C H 0.2218 0.3918 0.4621 0.047 Uiso 1 1 calc R . .
C12 C 0.2993(3) 0.1993(2) 0.7055(2) 0.0576(8) Uani 1 1 d . . .
H12A H 0.2532 0.1791 0.6452 0.086 Uiso 1 1 calc R . .
H12B H 0.2372 0.2290 0.7473 0.086 Uiso 1 1 calc R . .
H12C H 0.3394 0.1438 0.7381 0.086 Uiso 1 1 calc R . .
C13 C 0.4719(4) 0.1930(2) 0.5425(2) 0.0685(10) Uani 1 1 d . . .
H13A H 0.4312 0.1304 0.5487 0.103 Uiso 1 1 calc R . .
H13B H 0.5503 0.1870 0.5058 0.103 Uiso 1 1 calc R . .
H13C H 0.4099 0.2364 0.5088 0.103 Uiso 1 1 calc R . .
C14 C 0.5871(4) 0.1617(2) 0.6932(3) 0.0840(13) Uani 1 1 d . . .
H14A H 0.6124 0.1889 0.7565 0.126 Uiso 1 1 calc R . .
H14B H 0.6659 0.1469 0.6593 0.126 Uiso 1 1 calc R . .
H14C H 0.5366 0.1034 0.7015 0.126 Uiso 1 1 calc R . .
C15 C 0.7708(3) 0.4062(3) 0.7923(3) 0.0826(14) Uani 1 1 d . . .
H15A H 0.7861 0.4503 0.8464 0.124 Uiso 1 1 calc R . .
H15B H 0.7845 0.4394 0.7317 0.124 Uiso 1 1 calc R . .
H15C H 0.8317 0.3526 0.7996 0.124 Uiso 1 1 calc R . .
C16 C 0.6222(3) 0.3268(3) 0.8839(2) 0.0760(12) Uani 1 1 d . . .
H16A H 0.6897 0.2782 0.8961 0.114 Uiso 1 1 calc R . .
H16B H 0.5356 0.2970 0.8831 0.114 Uiso 1 1 calc R . .
H16C H 0.6293 0.3750 0.9349 0.114 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 0.02098(11) 0.02089(11) 0.01952(11) 0.00266(7) 0.00211(7) -0.00059(7)
Si1 0.0213(3) 0.0227(3) 0.0202(2) 0.0009(2) 0.0028(2) 0.0034(2)
O1 0.0264(7) 0.0270(7) 0.0222(7) 0.0038(6) 0.0055(6) 0.0047(6)
N1 0.0423(12) 0.0271(10) 0.0520(12) 0.0037(9) 0.0027(10) -0.0076(9)
N2 0.0408(12) 0.0354(11) 0.0504(12) 0.0059(10) 0.0041(10) -0.0006(9)
N3 0.0368(11) 0.0328(10) 0.0273(9) 0.0056(8) -0.0059(8) 0.0021(8)
C1 0.0196(9) 0.0238(10) 0.0231(9) 0.0007(8) 0.0041(7) 0.0025(8)
C2 0.0234(10) 0.0231(10) 0.0250(10) -0.0017(8) 0.0035(8) 0.0036(8)
C3 0.0276(11) 0.0299(11) 0.0235(9) -0.0026(8) 0.0029(8) 0.0051(9)
C4 0.0251(10) 0.0379(12) 0.0227(10) 0.0031(9) 0.0057(8) 0.0047(9)
C5 0.0206(10) 0.0317(11) 0.0238(9) 0.0026(8) 0.0044(8) 0.0020(8)
C6 0.0303(11) 0.0244(10) 0.0319(11) -0.0017(9) 0.0035(9) -0.0007(9)
C7 0.0393(13) 0.0432(13) 0.0252(11) -0.0074(10) -0.0006(9) 0.0003(11)
C8 0.0416(14) 0.0535(15) 0.0269(11) 0.0043(11) 0.0110(10) -0.0018(12)
C9 0.0243(11) 0.0516(15) 0.0368(12) 0.0110(11) 0.0031(9) -0.0067(10)
C10 0.0329(12) 0.0309(11) 0.0343(11) 0.0005(9) 0.0040(9) 0.0104(9)
C11 0.0285(11) 0.0363(12) 0.0288(10) -0.0057(9) 0.0015(9) 0.0006(9)
C12 0.0592(19) 0.0443(16) 0.071(2) 0.0034(14) 0.0184(15) -0.0141(14)
C13 0.114(3) 0.0371(15) 0.0565(18) -0.0036(14) 0.0248(19) -0.0132(17)
C14 0.081(3) 0.0351(17) 0.131(3) 0.0084(19) -0.032(2) 0.0059(16)
C15 0.0399(17) 0.149(4) 0.058(2) 0.054(2) -0.0072(15) -0.012(2)
C16 0.0512(18) 0.118(3) 0.0572(18) 0.046(2) -0.0161(15) -0.025(2)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zr1 O1 2.0036(13) 3_666 ?
Zr1 N1 2.0369(19) . ?
Zr1 N3 2.0848(18) . ?
Zr1 N2 2.377(2) . ?
Zr1 C2 2.532(2) . ?
Zr1 C1 2.5435(19) . ?
Zr1 C3 2.582(2) . ?
Zr1 C5 2.587(2) . ?
Zr1 C4 2.600(2) . ?
Si1 O1 1.6246(14) . ?
Si1 C11 1.874(2) . ?
Si1 C10 1.877(2) . ?
Si1 C1 1.878(2) . ?
O1 Zr1 2.0036(13) 3_666 ?
N1 N2 1.415(3) . ?
N1 C12 1.448(3) . ?
N2 C13 1.443(4) . ?
N2 C14 1.459(4) . ?
N3 C15 1.425(4) . ?
N3 C16 1.457(3) . ?
C1 C2 1.435(3) . ?
C1 C5 1.436(3) . ?
C2 C3 1.413(3) . ?
C2 C6 1.501(3) . ?
C3 C4 1.419(3) . ?
C3 C7 1.503(3) . ?
C4 C5 1.418(3) . ?
C4 C8 1.507(3) . ?
C5 C9 1.507(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 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
O1 Zr1 N1 119.90(7) 3_666 . ?
O1 Zr1 N3 104.25(7) 3_666 . ?
N1 Zr1 N3 100.06(8) . . ?
O1 Zr1 N2 89.32(7) 3_666 . ?
N1 Zr1 N2 36.35(8) . . ?
N3 Zr1 N2 90.27(8) . . ?
O1 Zr1 C2 86.51(6) 3_666 . ?
N1 Zr1 C2 136.24(8) . . ?
N3 Zr1 C2 106.53(7) . . ?
N2 Zr1 C2 163.20(7) . . ?
O1 Zr1 C1 88.61(6) 3_666 . ?
N1 Zr1 C1 108.22(8) . . ?
N3 Zr1 C1 137.48(7) . . ?
N2 Zr1 C1 130.88(7) . . ?
C2 Zr1 C1 32.84(6) . . ?
O1 Zr1 C3 114.52(6) 3_666 . ?
N1 Zr1 C3 122.01(8) . . ?
N3 Zr1 C3 84.26(7) . . ?
N2 Zr1 C3 156.16(7) . . ?
C2 Zr1 C3 32.05(6) . . ?
C1 Zr1 C3 53.94(6) . . ?
O1 Zr1 C5 119.44(6) 3_666 . ?
N1 Zr1 C5 83.13(8) . . ?
N3 Zr1 C5 127.43(7) . . ?
N2 Zr1 C5 116.34(7) . . ?
C2 Zr1 C5 53.11(7) . . ?
C1 Zr1 C5 32.49(6) . . ?
C3 Zr1 C5 52.75(7) . . ?
O1 Zr1 C4 138.64(6) 3_666 . ?
N1 Zr1 C4 90.85(8) . . ?
N3 Zr1 C4 95.80(7) . . ?
N2 Zr1 C4 126.84(7) . . ?
C2 Zr1 C4 52.90(7) . . ?
C1 Zr1 C4 53.68(6) . . ?
C3 Zr1 C4 31.78(7) . . ?
C5 Zr1 C4 31.74(6) . . ?
O1 Si1 C11 109.41(9) . . ?
O1 Si1 C10 108.45(9) . . ?
C11 Si1 C10 108.92(11) . . ?
O1 Si1 C1 113.54(8) . . ?
C11 Si1 C1 109.61(10) . . ?
C10 Si1 C1 106.79(9) . . ?
Si1 O1 Zr1 161.29(9) . 3_666 ?
N2 N1 C12 115.8(2) . . ?
N2 N1 Zr1 85.04(13) . . ?
C12 N1 Zr1 159.14(19) . . ?
N1 N2 C13 113.2(2) . . ?
N1 N2 C14 114.8(3) . . ?
C13 N2 C14 110.6(3) . . ?
N1 N2 Zr1 58.60(11) . . ?
C13 N2 Zr1 124.72(18) . . ?
C14 N2 Zr1 122.3(2) . . ?
C15 N3 C16 107.6(2) . . ?
C15 N3 Zr1 125.40(17) . . ?
C16 N3 Zr1 126.79(18) . . ?
C2 C1 C5 105.76(17) . . ?
C2 C1 Si1 125.72(15) . . ?
C5 C1 Si1 127.59(15) . . ?
C2 C1 Zr1 73.15(11) . . ?
C5 C1 Zr1 75.42(11) . . ?
Si1 C1 Zr1 125.02(9) . . ?
C3 C2 C1 109.46(18) . . ?
C3 C2 C6 124.51(19) . . ?
C1 C2 C6 125.88(18) . . ?
C3 C2 Zr1 75.90(12) . . ?
C1 C2 Zr1 74.01(11) . . ?
C6 C2 Zr1 120.11(14) . . ?
C2 C3 C4 107.75(18) . . ?
C2 C3 C7 125.7(2) . . ?
C4 C3 C7 126.36(19) . . ?
C2 C3 Zr1 72.05(11) . . ?
C4 C3 Zr1 74.84(12) . . ?
C7 C3 Zr1 122.55(15) . . ?
C5 C4 C3 108.04(18) . . ?
C5 C4 C8 126.0(2) . . ?
C3 C4 C8 125.7(2) . . ?
C5 C4 Zr1 73.60(11) . . ?
C3 C4 Zr1 73.39(11) . . ?
C8 C4 Zr1 123.67(16) . . ?
C4 C5 C1 108.97(18) . . ?
C4 C5 C9 123.86(19) . . ?
C1 C5 C9 126.79(19) . . ?
C4 C5 Zr1 74.66(12) . . ?
C1 C5 Zr1 72.10(11) . . ?
C9 C5 Zr1 125.05(15) . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N2 C13 H13A 109.5 . . ?
N2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C14 H14A 109.5 . . ?
N2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N3 C15 H15A 109.5 . . ?
N3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N3 C16 H16A 109.5 . . ?
N3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.069

#===END