# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005


data_global
_audit_creation_method           CRYSTALS

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Philip Mountford'
'Andrew R. Cowley'
'Robert G. Howe'
'Sally C. Lawrence'
'Suparabhorn Subongkoj'
'Cara S. Tredget'

_publ_contact_author_name        'Philip Mountford'
_publ_contact_author_address     
;
Chemistry Research Laboratory
Oxford University
Mansfield Road
Oxford
OX1 3TA
UNITED KINGDOM
;

_publ_contact_author_phone       '+44 1865 285140'
_publ_contact_author_fax         '+44 1865 285141'
_publ_contact_author_email       Philip.Mountford@chem.ox.ac.uk

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
A Novel Transformation of a Zirconium Imido Compound
and the Development of a New Class of N3 Donor Heteroscorpionate Ligand
;

data_Compound_1.THF
_database_code_depnum_ccdc_archive 'CCDC 285656'

#Local code arc1148

#=============================================================
# Diffractometer details
#=============================================================
_diffrn_measurement_device_type  
;
Nonius KappaCCD
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction        
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement       
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
#=============================================================
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'

_chemical_name_systematic        
;
[Zr{(Me2pz)2SiMe(NAr)}Cl3].THF
;
_chemical_melting_point          ?
_exptl_crystal_thermal_history   
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_special_details          
;
Geometric restraints were applied to the disordered solvent O1-C17.
The O-C distances were restrained to 1.44(2) \%A, the C-C distances
to 1.54(2) \%A and the C-O-C, O-C-C and C-C-C angles to 106(2) \%.
Similarity restraints were applied to the displacement parameters of
the O and C atoms.

All hydrogen atoms were positioned geometrically, the preferred
orientation of the methyl groups having been previously identified by
examination of a difference Fourier map.
;

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

_cell_length_a                   20.1923(7)
_cell_angle_alpha                90
_cell_length_b                   17.1332(6)
_cell_angle_beta                 90
_cell_length_c                   9.1763(3)
_cell_angle_gamma                90
_cell_volume                     3174.62(19)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P n m a '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z+1/2
x+1/2,-y+1/2,-z+1/2
x,-y+1/2,z
-x,y+1/2,-z
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 International_Tables_Vol_IV_Table_2.2B
'Si ' 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937
1.1407 International_Tables_Vol_IV_Table_2.2B
'Zr ' -2.9673 0.5597 17.8765 1.2762 10.9480 11.9160 5.4173 0.1176 3.6572
87.6627 2.0693 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            4
_chemical_formula_sum            ' C27 H42 Cl3 N5 O Si Zr '
_chemical_formula_moiety         ' C23 H34 Cl3 N5 Si Zr, C4 H8 O '
_chemical_compound_source        
;
synthesis as described
;
_chemical_formula_weight         678.33

_cell_measurement_reflns_used    18858
_cell_measurement_theta_min      5
_cell_measurement_theta_max      28
_cell_measurement_temperature    150

_exptl_crystal_description       ' fragment '
_exptl_crystal_colour            ' colourless '
_exptl_crystal_size_min          0.06
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_max          0.14

_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    0.665

_diffrn_measurement_method       \w

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_T_max  0.96

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      150
_diffrn_reflns_number            18858
_reflns_number_total             3724
#4056 unique reflections including absences
_diffrn_reflns_av_R_equivalents  0.068

_diffrn_reflns_theta_min         5.141
_diffrn_reflns_theta_max         27.476
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        27.476
_diffrn_measured_fraction_theta_full 0.999

_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_reflns_limit_h_min              0
_reflns_limit_h_max              26
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              11

_refine_diff_density_min         -0.67
_refine_diff_density_max         0.89

_refine_ls_number_reflns         2287
_refine_ls_number_restraints     20
_refine_ls_number_parameters     205

#_refine_ls_R_factor_ref 0.0400
_refine_ls_wR_factor_ref         0.0471
_refine_ls_goodness_of_fit_ref   1.1053

#_reflns_number_all 3724
_refine_ls_R_factor_all          0.0789
_refine_ls_wR_factor_all         0.0617

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                2287
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_gt          0.0471

_refine_ls_shift/su_max          0.015575
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.00 0.349 0.731
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_disorder_assembly
_atom_site_refinement_disorder_group
Zr1 Zr 0.55885(2) 0.2500 0.00905(5) 0.0300 1.0000 Uani S T . . .
Cl1 Cl 0.61234(5) 0.14417(6) -0.11607(10) 0.0435 1.0000 Uani . . . . .
Cl2 Cl 0.45975(7) 0.2500 -0.14251(14) 0.0411 1.0000 Uani S T . . .
N1 N 0.49871(13) 0.16012(18) 0.1542(3) 0.0320 1.0000 Uani . . . . .
N2 N 0.50609(13) 0.16928(17) 0.3048(3) 0.0313 1.0000 Uani . . . . .
Si1 Si 0.55767(6) 0.2500 0.34910(13) 0.0286 1.0000 Uani S T . . .
N3 N 0.61136(18) 0.2500 0.2085(4) 0.0296 1.0000 Uani S T . . .
C1 C 0.45784(16) 0.0990(2) 0.1360(4) 0.0360 1.0000 Uani . . . . .
C2 C 0.43984(18) 0.0689(2) 0.2703(4) 0.0415 1.0000 Uani . . . . .
C3 C 0.47014(17) 0.1134(2) 0.3753(4) 0.0374 1.0000 Uani . . . . .
C4 C 0.4374(2) 0.0705(2) -0.0117(4) 0.0475 1.0000 Uani . . . . .
C5 C 0.4677(2) 0.1071(3) 0.5376(5) 0.0501 1.0000 Uani . . . . .
C6 C 0.5863(3) 0.2500 0.5379(6) 0.0427 1.0000 Uani S T . . .
C7 C 0.6820(2) 0.2500 0.2391(5) 0.0292 1.0000 Uani S T . . .
C8 C 0.71550(17) 0.1786(2) 0.2560(4) 0.0330 1.0000 Uani . . . . .
C9 C 0.78275(17) 0.1809(2) 0.2921(4) 0.0382 1.0000 Uani . . . . .
C10 C 0.8161(2) 0.2500 0.3111(6) 0.0423 1.0000 Uani S T . . .
C11 C 0.68202(18) 0.0999(2) 0.2377(5) 0.0427 1.0000 Uani . . . . .
C12 C 0.7213(2) 0.0457(3) 0.1385(6) 0.0577 1.0000 Uani . . . . .
C13 C 0.6703(2) 0.0606(3) 0.3854(6) 0.0638 1.0000 Uani . . . . .
O1 O 0.8016(8) 0.3132(8) 0.8094(14) 0.0871 0.5000 Uani D U . 1 -1
C14 C 0.7601(5) 0.2690(6) 0.7008(10) 0.0668 0.5000 Uani D U . 1 -1
C15 C 0.7819(6) 0.1829(7) 0.7001(16) 0.0759 0.5000 Uani D U . 1 -1
C16 C 0.8157(13) 0.1725(13) 0.845(3) 0.1012 0.5000 Uani D U . 1 -1
C17 C 0.8093(5) 0.2537(14) 0.9174(9) 0.1023 0.5000 Uani D U . 1 -1
H21 H 0.4102 0.0230 0.2876 0.0499 1.0000 Uiso . . . . .
H41 H 0.4071 0.0247 -0.0008 0.0570 1.0000 Uiso . . . . .
H42 H 0.4776 0.0544 -0.0679 0.0570 1.0000 Uiso . . . . .
H43 H 0.4140 0.1132 -0.0650 0.0570 1.0000 Uiso . . . . .
H51 H 0.4386 0.0623 0.5659 0.0601 1.0000 Uiso . . . . .
H52 H 0.5134 0.0981 0.5761 0.0601 1.0000 Uiso . . . . .
H53 H 0.4495 0.1565 0.5795 0.0601 1.0000 Uiso . . . . .
H61 H 0.5472 0.2500 0.6049 0.0512 1.0000 Uiso . . . . .
H62 H 0.6137 0.2977 0.5561 0.0512 1.0000 Uiso . . . . .
H91 H 0.8073 0.1306 0.3044 0.0459 1.0000 Uiso . . . . .
H101 H 0.8640 0.2500 0.3384 0.0508 1.0000 Uiso . . . . .
H111 H 0.6383 0.1101 0.1904 0.0513 1.0000 Uiso . . . . .
H121 H 0.6976 -0.0053 0.1294 0.0692 1.0000 Uiso . . . . .
H122 H 0.7663 0.0367 0.1811 0.0692 1.0000 Uiso . . . . .
H123 H 0.7258 0.0701 0.0400 0.0692 1.0000 Uiso . . . . .
H131 H 0.6483 0.0090 0.3702 0.0766 1.0000 Uiso . . . . .
H132 H 0.7137 0.0526 0.4357 0.0766 1.0000 Uiso . . . . .
H133 H 0.6413 0.0946 0.4468 0.0766 1.0000 Uiso . . . . .
H141 H 0.7663 0.2918 0.6015 0.0802 0.5000 Uiso . . . 1 -1
H142 H 0.7124 0.2725 0.7290 0.0802 0.5000 Uiso . . . 1 -1
H151 H 0.8133 0.1725 0.6181 0.0910 0.5000 Uiso . . . 1 -1
H152 H 0.7428 0.1475 0.6914 0.0910 0.5000 Uiso . . . 1 -1
H161 H 0.8633 0.1579 0.8320 0.1214 0.5000 Uiso . . . 1 -1
H162 H 0.7929 0.1317 0.9047 0.1214 0.5000 Uiso . . . 1 -1
H171 H 0.8501 0.2646 0.9757 0.1227 0.5000 Uiso . . . 1 -1
H172 H 0.7699 0.2540 0.9832 0.1227 0.5000 Uiso . . . 1 -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
Zr1 0.0276(2) 0.0379(2) 0.0245(2) 0.0000 -0.00116(19) 0.0000
Cl1 0.0443(5) 0.0483(5) 0.0378(4) -0.0054(4) 0.0044(4) 0.0050(4)
Cl2 0.0382(6) 0.0512(8) 0.0338(6) 0.0000 -0.0096(5) 0.0000
N1 0.0270(13) 0.0380(15) 0.0308(15) 0.0015(12) -0.0036(10) 0.0001(12)
N2 0.0272(13) 0.0377(15) 0.0290(14) 0.0033(12) 0.0016(11) -0.0002(12)
Si1 0.0233(6) 0.0372(7) 0.0254(6) 0.0000 0.0004(5) 0.0000
N3 0.0215(18) 0.039(2) 0.0280(19) 0.0000 -0.0021(15) 0.0000
C1 0.0246(15) 0.0327(17) 0.051(2) 0.0003(16) -0.0055(14) -0.0005(13)
C2 0.0310(16) 0.0375(18) 0.056(2) 0.0049(17) 0.0023(17) -0.0024(17)
C3 0.0308(17) 0.0402(19) 0.0413(18) 0.0046(17) 0.0080(15) -0.0007(15)
C4 0.046(2) 0.043(2) 0.054(2) 0.0003(19) -0.0153(19) -0.0072(18)
C5 0.056(2) 0.051(2) 0.043(2) 0.0092(19) 0.0157(18) -0.009(2)
C6 0.041(3) 0.056(3) 0.032(2) 0.0000 -0.003(2) 0.0000
C7 0.025(2) 0.039(3) 0.024(2) 0.0000 0.0039(17) 0.0000
C8 0.0272(16) 0.041(2) 0.0304(16) 0.0001(15) -0.0002(13) 0.0017(14)
C9 0.0267(17) 0.043(2) 0.045(2) 0.0006(16) -0.0029(15) 0.0063(15)
C10 0.026(2) 0.055(3) 0.047(3) 0.0000 -0.001(2) 0.0000
C11 0.0326(18) 0.039(2) 0.057(2) 0.0043(18) -0.0081(17) 0.0020(15)
C12 0.049(2) 0.045(2) 0.080(3) -0.015(2) -0.008(2) 0.0081(19)
C13 0.059(3) 0.051(3) 0.082(3) 0.015(2) -0.001(3) -0.002(2)
O1 0.095(11) 0.081(6) 0.086(7) -0.014(5) 0.016(6) 0.007(6)
C14 0.071(6) 0.082(9) 0.047(4) 0.006(4) 0.009(4) 0.036(6)
C15 0.062(7) 0.076(8) 0.089(7) -0.016(6) 0.003(6) 0.023(5)
C16 0.064(9) 0.104(7) 0.136(14) 0.072(8) -0.023(9) 0.000(8)
C17 0.095(8) 0.164(7) 0.047(4) 0.018(6) -0.006(4) -0.066(13)
_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zr1 . Cl1 . 2.4026(10) yes
Zr1 . Cl1 5_555 2.4026(10) yes
Zr1 . Cl2 . 2.4370(13) yes
Zr1 . N1 . 2.371(3) yes
Zr1 . N1 5_555 2.371(3) yes
Zr1 . N3 . 2.115(4) yes
N1 . N2 . 1.399(4) yes
N1 . C1 . 1.344(5) yes
N2 . Si1 . 1.778(3) yes
N2 . C3 . 1.364(5) yes
Si1 . N3 . 1.685(4) yes
Si1 . C6 . 1.826(5) yes
N3 . C7 . 1.454(6) yes
C1 . C2 . 1.384(5) yes
C1 . C4 . 1.499(5) yes
C2 . C3 . 1.374(6) yes
C2 . H21 . 1.000 no
C3 . C5 . 1.494(5) yes
C4 . H41 . 1.000 no
C4 . H42 . 1.000 no
C4 . H43 . 1.000 no
C5 . H51 . 1.000 no
C5 . H52 . 1.000 no
C5 . H53 . 1.000 no
C6 . H61 . 1.000 no
C6 . H62 . 1.000 no
C6 . H62 5_555 1.000 no
C7 . C8 . 1.406(4) yes
C7 . C8 5_555 1.406(4) yes
C8 . C9 . 1.398(5) yes
C8 . C11 . 1.518(5) yes
C9 . C10 . 1.373(5) yes
C9 . H91 . 1.000 no
C10 . H101 . 1.000 no
C11 . C12 . 1.522(6) yes
C11 . C13 . 1.532(7) yes
C11 . H111 . 1.000 no
C12 . H121 . 1.000 no
C12 . H122 . 1.000 no
C12 . H123 . 1.000 no
C13 . H131 . 1.000 no
C13 . H132 . 1.000 no
C13 . H133 . 1.000 no
O1 . C14 . 1.506(12) yes
O1 . C17 . 1.431(14) yes
C14 . C15 . 1.538(13) yes
C14 . H141 . 1.000 no
C14 . H142 . 1.000 no
C15 . C16 . 1.507(15) yes
C15 . H151 . 1.000 no
C15 . H152 . 1.000 no
C16 . C17 . 1.547(17) yes
C16 . H161 . 1.000 no
C16 . H162 . 1.000 no
C17 . H171 . 1.000 no
C17 . H172 . 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Zr1 . Cl1 5_555 98.00(5) yes
Cl1 . Zr1 . Cl2 . 95.53(3) yes
Cl1 5_555 Zr1 . Cl2 . 95.53(3) yes
Cl1 . Zr1 . N1 . 90.49(8) yes
Cl1 5_555 Zr1 . N1 . 171.49(8) yes
Cl2 . Zr1 . N1 . 84.26(7) yes
Cl1 . Zr1 . N1 5_555 171.49(8) yes
Cl1 5_555 Zr1 . N1 5_555 90.49(8) yes
Cl2 . Zr1 . N1 5_555 84.26(7) yes
N1 . Zr1 . N1 5_555 81.02(14) yes
Cl1 . Zr1 . N3 . 100.85(7) yes
Cl1 5_555 Zr1 . N3 . 100.85(7) yes
Cl2 . Zr1 . N3 . 154.89(11) yes
N1 . Zr1 . N3 . 76.75(10) yes
N1 5_555 Zr1 . N3 . 76.75(10) yes
Si1 . Zr1 . N3 . 30.52(10) yes
Zr1 . N1 . N2 . 115.3(2) yes
Zr1 . N1 . C1 . 138.7(2) yes
N2 . N1 . C1 . 106.0(3) yes
N1 . N2 . Si1 . 112.0(2) yes
N1 . N2 . C3 . 109.5(3) yes
Si1 . N2 . C3 . 138.5(3) yes
N2 . Si1 . N2 5_555 102.09(19) yes
N2 . Si1 . N3 . 101.65(13) yes
N2 5_555 Si1 . N3 . 101.65(13) yes
N2 . Si1 . C6 . 113.71(14) yes
N2 5_555 Si1 . C6 . 113.71(14) yes
N3 . Si1 . C6 . 121.5(2) yes
Zr1 . N3 . Si1 . 109.87(19) yes
Zr1 . N3 . C7 . 131.2(3) yes
Si1 . N3 . C7 . 118.9(3) yes
N1 . C1 . C2 . 110.0(3) yes
N1 . C1 . C4 . 122.4(3) yes
C2 . C1 . C4 . 127.7(3) yes
C1 . C2 . C3 . 107.5(3) yes
C1 . C2 . H21 . 126.259 no
C3 . C2 . H21 . 126.260 no
N2 . C3 . C2 . 107.1(3) yes
N2 . C3 . C5 . 122.8(4) yes
C2 . C3 . C5 . 130.1(4) yes
C1 . C4 . H41 . 109.467 no
C1 . C4 . H42 . 109.466 no
H41 . C4 . H42 . 109.475 no
C1 . C4 . H43 . 109.467 no
H41 . C4 . H43 . 109.476 no
H42 . C4 . H43 . 109.476 no
C3 . C5 . H51 . 109.467 no
C3 . C5 . H52 . 109.467 no
H51 . C5 . H52 . 109.475 no
C3 . C5 . H53 . 109.467 no
H51 . C5 . H53 . 109.476 no
H52 . C5 . H53 . 109.476 no
Si1 . C6 . H61 . 109.467 no
Si1 . C6 . H62 . 109.467 no
H61 . C6 . H62 . 109.476 no
Si1 . C6 . H62 5_555 109.467 no
H61 . C6 . H62 5_555 109.476 no
H62 . C6 . H62 5_555 109.476 no
N3 . C7 . C8 . 119.5(2) yes
N3 . C7 . C8 5_555 119.5(2) yes
C8 . C7 . C8 5_555 120.9(4) yes
C7 . C8 . C9 . 118.0(3) yes
C7 . C8 . C11 . 123.1(3) yes
C9 . C8 . C11 . 118.9(3) yes
C8 . C9 . C10 . 122.0(3) yes
C8 . C9 . H91 . 119.009 no
C10 . C9 . H91 . 119.010 no
C9 . C10 . C9 5_555 119.2(5) yes
C9 . C10 . H101 . 120.393 no
C9 5_555 C10 . H101 . 120.393 no
C8 . C11 . C12 . 112.1(3) yes
C8 . C11 . C13 . 111.1(3) yes
C12 . C11 . C13 . 110.0(4) yes
C8 . C11 . H111 . 106.664 no
C12 . C11 . H111 . 107.899 no
C13 . C11 . H111 . 108.935 no
C11 . C12 . H121 . 109.467 no
C11 . C12 . H122 . 109.467 no
H121 . C12 . H122 . 109.476 no
C11 . C12 . H123 . 109.466 no
H121 . C12 . H123 . 109.476 no
H122 . C12 . H123 . 109.475 no
C11 . C13 . H131 . 109.466 no
C11 . C13 . H132 . 109.467 no
H131 . C13 . H132 . 109.476 no
C11 . C13 . H133 . 109.466 no
H131 . C13 . H133 . 109.476 no
H132 . C13 . H133 . 109.477 no
C14 . O1 . C17 . 99.2(7) yes
O1 . C14 . C15 . 109.0(8) yes
O1 . C14 . H141 . 109.586 no
C15 . C14 . H141 . 109.576 no
O1 . C14 . H142 . 109.583 no
C15 . C14 . H142 . 109.585 no
H141 . C14 . H142 . 109.464 no
C14 . C15 . C16 . 103.8(9) yes
C14 . C15 . H151 . 110.868 no
C16 . C15 . H151 . 110.855 no
C14 . C15 . H152 . 110.861 no
C16 . C15 . H152 . 110.850 no
H151 . C15 . H152 . 109.478 no
C15 . C16 . C17 . 103.6(8) yes
C15 . C16 . H161 . 110.943 no
C17 . C16 . H161 . 110.919 no
C15 . C16 . H162 . 110.944 no
C17 . C16 . H162 . 110.914 no
H161 . C16 . H162 . 109.468 no
O1 . C17 . C16 . 110.7(8) yes
O1 . C17 . H171 . 109.159 no
C16 . C17 . H171 . 109.178 no
O1 . C17 . H172 . 109.155 no
C16 . C17 . H172 . 109.178 no
H171 . C17 . H172 . 109.462 no

##end

data_Compound_xx
_database_code_depnum_ccdc_archive 'CCDC 285657'

#=============================================================
# Diffractometer details
#=============================================================
_diffrn_measurement_device_type  
;
Nonius KappaCCD
;
_diffrn_radiation_monochromator  graphite
_computing_data_collection       
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction        
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_cell_refinement       
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
#=============================================================
# General computing
#=============================================================
_computing_structure_refinement  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_publication_material  
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'

_chemical_name_systematic        
;
[Sc{(Me2pz)2CHSiMe2NiPr}(CH2SiMe3)3]
;
_chemical_melting_point          ?
_exptl_crystal_thermal_history   
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_ls_matrix_type           full
_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_special_details          
;
The hydrogen atoms attached to the coordinated alkyl carbon atoms
were located in a difference Fourier map and their coordinates and
isotropic thermal parameters subsequently refined. Other hydrogen
atoms were positioned geometrically, the preferred orientations of
the methyl substituents of the pyrazolyl groups having been
previously identified in the difference Fourier map.
;
#=============================================================

_cell_length_a                   10.4827(2)
_cell_angle_alpha                82.0937(10)
_cell_length_b                   10.9399(3)
_cell_angle_beta                 89.6905(11)
_cell_length_c                   14.6107(4)
_cell_angle_gamma                72.2736(12)
_cell_volume                     1579.64(7)

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
'Sc ' 0.2519 0.3716 9.1890 9.0213 7.3679 0.5729 1.6409 136.1080 1.4680 51.3531
1.3329 International_Tables_Vol_IV_Table_2.2B
'Si ' 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937
1.1407 International_Tables_Vol_IV_Table_2.2B

_cell_formula_units_Z            2
_chemical_formula_sum            ' C24 H50 N5 Sc1 Si3 '
_chemical_formula_moiety         ' C24 H50 N5 Sc1 Si3 '
_chemical_compound_source        
;
synthesis as described
;
_chemical_formula_weight         537.91

_cell_measurement_reflns_used    27522
_cell_measurement_theta_min      5
_cell_measurement_theta_max      28
_cell_measurement_temperature    150

_exptl_crystal_description       ' block '
_exptl_crystal_colour            ' colourless '
_exptl_crystal_size_min          0.14
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_max          0.18

_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_meas      ?
# Non-dispersive F(000):
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    0.367

_diffrn_measurement_method       \w

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  0.95

_diffrn_standards_interval_time  0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_diffrn_standards_decay_%        0.00

_diffrn_ambient_temperature      150
_diffrn_reflns_number            27522
_reflns_number_total             7134
_diffrn_reflns_av_R_equivalents  0.047

_diffrn_reflns_theta_min         5.129
_diffrn_reflns_theta_max         27.436
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        27.436
_diffrn_measured_fraction_theta_full 0.999

_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18

_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              -13
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              18

_refine_diff_density_min         -0.40
_refine_diff_density_max         0.42

_refine_ls_number_reflns         4738
_refine_ls_number_restraints     0
_refine_ls_number_parameters     314

#_refine_ls_R_factor_ref 0.0385
_refine_ls_wR_factor_ref         0.0444
_refine_ls_goodness_of_fit_ref   1.0856

#_reflns_number_all 7134
_refine_ls_R_factor_all          0.0671
_refine_ls_wR_factor_all         0.0639

# The I/u(I) cutoff below was used for refinement as
# well as the _gt R-factors:
_reflns_threshold_expression     I>3.00u(I)
_reflns_number_gt                4738
_refine_ls_R_factor_gt           0.0385
_refine_ls_wR_factor_gt          0.0444

_refine_ls_shift/su_max          0.008087
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.692 0.291 0.411
;
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073

# Uequiv = arithmetic mean of Ui
# i.e. Ueqiv = (U1+U2+U3)/3

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_occupancy
_atom_site_adp_type
Sc1 Sc 0.01487(4) 0.27873(4) 0.27033(3) 0.0230 1.0000 Uani
N1 N 0.06869(17) 0.30741(17) 0.11342(12) 0.0259 1.0000 Uani
N2 N 0.20341(17) 0.26269(17) 0.09778(12) 0.0258 1.0000 Uani
C1 C 0.0077(2) 0.3299(2) 0.02946(15) 0.0289 1.0000 Uani
C2 C 0.1015(2) 0.2981(2) -0.03793(15) 0.0331 1.0000 Uani
C3 C 0.2259(2) 0.2567(2) 0.00682(15) 0.0304 1.0000 Uani
C4 C -0.1412(2) 0.3855(2) 0.01552(17) 0.0366 1.0000 Uani
C5 C 0.3631(3) 0.2125(3) -0.02980(16) 0.0393 1.0000 Uani
N3 N 0.15972(18) 0.41519(17) 0.25854(13) 0.0276 1.0000 Uani
N4 N 0.27156(18) 0.37364(17) 0.20778(12) 0.0263 1.0000 Uani
C6 C 0.1619(2) 0.5303(2) 0.27957(16) 0.0319 1.0000 Uani
C7 C 0.2733(2) 0.5611(2) 0.24229(18) 0.0352 1.0000 Uani
C8 C 0.3417(2) 0.4606(2) 0.19641(16) 0.0323 1.0000 Uani
C9 C 0.0578(3) 0.6095(2) 0.3359(2) 0.0452 1.0000 Uani
C10 C 0.4651(3) 0.4405(3) 0.1424(2) 0.0456 1.0000 Uani
C11 C 0.2991(2) 0.2495(2) 0.17431(14) 0.0258 1.0000 Uani
Si1 Si 0.32368(6) 0.10369(5) 0.27147(4) 0.0251 1.0000 Uani
N5 N 0.17181(18) 0.11719(17) 0.31593(12) 0.0257 1.0000 Uani
C12 C 0.4558(2) 0.1234(3) 0.34855(17) 0.0396 1.0000 Uani
C13 C 0.4012(3) -0.0371(2) 0.20782(18) 0.0390 1.0000 Uani
C14 C 0.1443(2) 0.0289(2) 0.39430(16) 0.0333 1.0000 Uani
C15 C 0.1890(3) 0.0520(3) 0.48665(18) 0.0503 1.0000 Uani
C16 C 0.2024(4) -0.1136(3) 0.3834(2) 0.0559 1.0000 Uani
C17 C -0.0889(2) 0.3681(2) 0.39191(17) 0.0335 1.0000 Uani
Si2 Si -0.25693(6) 0.48927(6) 0.38033(4) 0.0321 1.0000 Uani
C18 C -0.3911(3) 0.4090(3) 0.4021(2) 0.0439 1.0000 Uani
C19 C -0.2848(3) 0.6173(3) 0.4586(2) 0.0507 1.0000 Uani
C20 C -0.2921(3) 0.5831(3) 0.26012(19) 0.0431 1.0000 Uani
C21 C -0.1566(2) 0.2060(2) 0.23229(18) 0.0334 1.0000 Uani
Si3 Si -0.14613(6) 0.06357(6) 0.17456(4) 0.0298 1.0000 Uani
C22 C -0.1794(3) -0.0692(3) 0.2569(2) 0.0472 1.0000 Uani
C23 C -0.2748(3) 0.0985(3) 0.07673(19) 0.0438 1.0000 Uani
C24 C 0.0221(2) -0.0075(3) 0.12594(19) 0.0418 1.0000 Uani
H1 H -0.100(3) 0.286(3) 0.430(2) 0.048(8) 1.0000 Uiso
H2 H -0.033(4) 0.397(4) 0.418(3) 0.077(12) 1.0000 Uiso
H3 H -0.221(3) 0.280(3) 0.206(2) 0.061(10) 1.0000 Uiso
H4 H -0.190(4) 0.190(3) 0.289(3) 0.063(10) 1.0000 Uiso
H21 H 0.0825 0.3041 -0.1057 0.0397 1.0000 Uiso
H41 H -0.1826 0.3983 0.0767 0.0429 1.0000 Uiso
H42 H -0.1636 0.4709 -0.0255 0.0429 1.0000 Uiso
H43 H -0.1767 0.3246 -0.0139 0.0429 1.0000 Uiso
H51 H 0.3562 0.2158 -0.0984 0.0469 1.0000 Uiso
H52 H 0.4152 0.2705 -0.0148 0.0469 1.0000 Uiso
H53 H 0.4098 0.1215 -0.0007 0.0469 1.0000 Uiso
H71 H 0.2984 0.6410 0.2479 0.0432 1.0000 Uiso
H91 H -0.0100 0.5637 0.3532 0.0556 1.0000 Uiso
H92 H 0.1011 0.6220 0.3932 0.0556 1.0000 Uiso
H93 H 0.0124 0.6959 0.2989 0.0556 1.0000 Uiso
H101 H 0.5001 0.5159 0.1430 0.0580 1.0000 Uiso
H102 H 0.5345 0.3592 0.1707 0.0580 1.0000 Uiso
H103 H 0.4438 0.4330 0.0772 0.0580 1.0000 Uiso
H111 H 0.3899 0.2251 0.1475 0.0306 1.0000 Uiso
H121 H 0.5404 0.1133 0.3143 0.0470 1.0000 Uiso
H122 H 0.4249 0.2115 0.3681 0.0470 1.0000 Uiso
H123 H 0.4727 0.0559 0.4045 0.0470 1.0000 Uiso
H131 H 0.4904 -0.0331 0.1854 0.0454 1.0000 Uiso
H132 H 0.4134 -0.1200 0.2503 0.0454 1.0000 Uiso
H133 H 0.3413 -0.0334 0.1538 0.0454 1.0000 Uiso
H141 H 0.0444 0.0505 0.3930 0.0398 1.0000 Uiso
H151 H 0.1680 -0.0100 0.5369 0.0617 1.0000 Uiso
H152 H 0.1408 0.1430 0.4967 0.0617 1.0000 Uiso
H153 H 0.2877 0.0384 0.4875 0.0617 1.0000 Uiso
H161 H 0.1806 -0.1682 0.4383 0.0671 1.0000 Uiso
H162 H 0.3018 -0.1362 0.3789 0.0671 1.0000 Uiso
H163 H 0.1628 -0.1301 0.3260 0.0671 1.0000 Uiso
H181 H -0.4810 0.4764 0.3954 0.0530 1.0000 Uiso
H182 H -0.3781 0.3600 0.4661 0.0530 1.0000 Uiso
H183 H -0.3857 0.3477 0.3563 0.0530 1.0000 Uiso
H191 H -0.3780 0.6782 0.4475 0.0606 1.0000 Uiso
H192 H -0.2724 0.5752 0.5245 0.0606 1.0000 Uiso
H193 H -0.2190 0.6665 0.4453 0.0606 1.0000 Uiso
H201 H -0.3837 0.6476 0.2563 0.0513 1.0000 Uiso
H202 H -0.2240 0.6294 0.2460 0.0513 1.0000 Uiso
H203 H -0.2874 0.5219 0.2143 0.0513 1.0000 Uiso
H221 H -0.1732 -0.1450 0.2241 0.0554 1.0000 Uiso
H222 H -0.2713 -0.0373 0.2811 0.0554 1.0000 Uiso
H223 H -0.1116 -0.0961 0.3096 0.0554 1.0000 Uiso
H231 H -0.2639 0.0178 0.0485 0.0534 1.0000 Uiso
H232 H -0.3668 0.1282 0.1011 0.0534 1.0000 Uiso
H233 H -0.2618 0.1678 0.0288 0.0534 1.0000 Uiso
H241 H 0.0213 -0.0840 0.0958 0.0515 1.0000 Uiso
H242 H 0.0925 -0.0357 0.1770 0.0515 1.0000 Uiso
H243 H 0.0422 0.0593 0.0792 0.0515 1.0000 Uiso
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
Sc1 0.02238(19) 0.02306(19) 0.02312(19) -0.00560(14) 0.00032(14) -0.00517(14)
N1 0.0252(9) 0.0269(9) 0.0254(9) -0.0031(7) -0.0017(7) -0.0079(7)
N2 0.0274(9) 0.0271(9) 0.0221(8) -0.0030(7) 0.0001(7) -0.0075(7)
C1 0.0358(12) 0.0264(10) 0.0246(10) 0.0004(8) -0.0048(8) -0.0116(9)
C2 0.0435(13) 0.0321(11) 0.0237(11) -0.0019(8) -0.0048(9) -0.0123(10)
C3 0.0413(12) 0.0269(10) 0.0247(10) -0.0054(8) 0.0037(9) -0.0122(9)
C4 0.0350(12) 0.0367(12) 0.0355(12) 0.0021(10) -0.0098(10) -0.0102(10)
C5 0.0433(14) 0.0440(14) 0.0299(12) -0.0080(10) 0.0075(10) -0.0116(11)
N3 0.0260(9) 0.0255(9) 0.0308(9) -0.0073(7) -0.0008(7) -0.0055(7)
N4 0.0277(9) 0.0244(8) 0.0277(9) -0.0043(7) -0.0010(7) -0.0093(7)
C6 0.0336(11) 0.0256(10) 0.0376(12) -0.0079(9) -0.0061(9) -0.0090(9)
C7 0.0369(12) 0.0255(11) 0.0457(13) -0.0055(9) -0.0076(10) -0.0127(9)
C8 0.0307(11) 0.0338(11) 0.0347(12) 0.0005(9) -0.0066(9) -0.0154(9)
C9 0.0379(13) 0.0347(13) 0.0665(18) -0.0242(12) 0.0031(12) -0.0091(10)
C10 0.0396(14) 0.0497(15) 0.0557(16) -0.0086(12) 0.0071(12) -0.0252(12)
C11 0.0235(10) 0.0284(10) 0.0246(10) -0.0045(8) 0.0004(8) -0.0064(8)
Si1 0.0235(3) 0.0239(3) 0.0252(3) -0.0026(2) -0.0010(2) -0.0037(2)
N5 0.0269(9) 0.0249(8) 0.0244(9) -0.0019(7) 0.0005(7) -0.0073(7)
C12 0.0305(12) 0.0507(15) 0.0361(13) -0.0046(11) -0.0060(10) -0.0110(11)
C13 0.0371(13) 0.0320(12) 0.0443(14) -0.0091(10) 0.0075(10) -0.0038(10)
C14 0.0358(12) 0.0325(11) 0.0311(11) 0.0036(9) 0.0010(9) -0.0134(9)
C15 0.0659(18) 0.0616(17) 0.0268(12) -0.0005(11) 0.0016(12) -0.0272(15)
C16 0.090(2) 0.0338(14) 0.0444(16) 0.0035(11) 0.0038(15) -0.0232(14)
C17 0.0315(12) 0.0377(13) 0.0319(12) -0.0107(10) 0.0004(9) -0.0087(10)
Si2 0.0317(3) 0.0343(3) 0.0308(3) -0.0083(2) 0.0035(2) -0.0093(3)
C18 0.0353(13) 0.0489(15) 0.0484(15) -0.0091(12) 0.0108(11) -0.0135(11)
C19 0.0502(16) 0.0499(16) 0.0514(16) -0.0253(13) 0.0053(12) -0.0069(13)
C20 0.0479(15) 0.0385(13) 0.0417(14) 0.0007(11) -0.0041(11) -0.0141(11)
C21 0.0284(11) 0.0362(12) 0.0370(13) -0.0144(10) 0.0027(9) -0.0078(10)
Si3 0.0283(3) 0.0311(3) 0.0312(3) -0.0098(2) -0.0006(2) -0.0086(2)
C22 0.0582(17) 0.0356(13) 0.0446(15) -0.0058(11) 0.0093(12) -0.0099(12)
C23 0.0425(14) 0.0438(14) 0.0472(15) -0.0097(11) -0.0093(11) -0.0146(11)
C24 0.0332(12) 0.0494(15) 0.0461(14) -0.0241(12) 0.0044(10) -0.0100(11)
_refine_ls_extinction_method     None
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sc1 . N1 . 2.3597(18) yes
Sc1 . N3 . 2.4230(18) yes
Sc1 . N5 . 2.0472(18) yes
Sc1 . C17 . 2.259(2) yes
Sc1 . C21 . 2.275(2) yes
N1 . N2 . 1.376(2) yes
N1 . C1 . 1.343(3) yes
N2 . C3 . 1.355(3) yes
N2 . C11 . 1.469(3) yes
C1 . C2 . 1.390(3) yes
C1 . C4 . 1.496(3) yes
C2 . C3 . 1.378(3) yes
C2 . H21 . 1.000 no
C3 . C5 . 1.493(3) yes
C4 . H41 . 1.000 no
C4 . H42 . 1.000 no
C4 . H43 . 1.000 no
C5 . H51 . 1.000 no
C5 . H52 . 1.000 no
C5 . H53 . 1.000 no
N3 . N4 . 1.375(2) yes
N3 . C6 . 1.343(3) yes
N4 . C8 . 1.362(3) yes
N4 . C11 . 1.452(3) yes
C6 . C7 . 1.399(3) yes
C6 . C9 . 1.494(3) yes
C7 . C8 . 1.375(3) yes
C7 . H71 . 1.000 no
C8 . C10 . 1.485(4) yes
C9 . H91 . 1.000 no
C9 . H92 . 1.000 no
C9 . H93 . 1.000 no
C10 . H101 . 1.000 no
C10 . H102 . 1.000 no
C10 . H103 . 1.000 no
C11 . Si1 . 1.938(2) yes
C11 . H111 . 1.000 no
Si1 . N5 . 1.6883(18) yes
Si1 . C12 . 1.870(2) yes
Si1 . C13 . 1.877(2) yes
N5 . C14 . 1.479(3) yes
C12 . H121 . 1.000 no
C12 . H122 . 1.000 no
C12 . H123 . 1.000 no
C13 . H131 . 1.000 no
C13 . H132 . 1.000 no
C13 . H133 . 1.000 no
C14 . C15 . 1.509(4) yes
C14 . C16 . 1.522(4) yes
C14 . H141 . 1.000 no
C15 . H151 . 1.000 no
C15 . H152 . 1.000 no
C15 . H153 . 1.000 no
C16 . H161 . 1.000 no
C16 . H162 . 1.000 no
C16 . H163 . 1.000 no
C17 . Si2 . 1.846(2) yes
C17 . H1 . 1.02(3) no
C17 . H2 . 0.86(4) no
Si2 . C18 . 1.877(3) yes
Si2 . C19 . 1.882(3) yes
Si2 . C20 . 1.885(3) yes
C18 . H181 . 1.000 no
C18 . H182 . 1.000 no
C18 . H183 . 1.000 no
C19 . H191 . 1.000 no
C19 . H192 . 1.000 no
C19 . H193 . 1.000 no
C20 . H201 . 1.000 no
C20 . H202 . 1.000 no
C20 . H203 . 1.000 no
C21 . Si3 . 1.846(2) yes
C21 . H3 . 0.92(4) no
C21 . H4 . 0.91(4) no
Si3 . C22 . 1.871(3) yes
Si3 . C23 . 1.888(3) yes
Si3 . C24 . 1.877(3) yes
C22 . H221 . 1.000 no
C22 . H222 . 1.000 no
C22 . H223 . 1.000 no
C23 . H231 . 1.000 no
C23 . H232 . 1.000 no
C23 . H233 . 1.000 no
C24 . H241 . 1.000 no
C24 . H242 . 1.000 no
C24 . H243 . 1.000 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . Sc1 . N3 . 73.50(6) yes
N1 . Sc1 . N5 . 98.72(7) yes
N3 . Sc1 . N5 . 91.63(7) yes
N1 . Sc1 . C17 . 148.14(8) yes
N3 . Sc1 . C17 . 91.91(8) yes
N5 . Sc1 . C17 . 110.09(8) yes
N1 . Sc1 . C21 . 90.54(8) yes
N3 . Sc1 . C21 . 157.81(8) yes
N5 . Sc1 . C21 . 106.24(8) yes
C17 . Sc1 . C21 . 94.07(9) yes
Sc1 . N1 . N2 . 114.47(12) yes
Sc1 . N1 . C1 . 138.79(15) yes
N2 . N1 . C1 . 104.91(17) yes
N1 . N2 . C3 . 111.59(17) yes
N1 . N2 . C11 . 118.27(16) yes
C3 . N2 . C11 . 129.27(18) yes
N1 . C1 . C2 . 110.61(19) yes
N1 . C1 . C4 . 121.9(2) yes
C2 . C1 . C4 . 127.4(2) yes
C1 . C2 . C3 . 106.63(19) yes
C1 . C2 . H21 . 126.685 no
C3 . C2 . H21 . 126.685 no
N2 . C3 . C2 . 106.2(2) yes
N2 . C3 . C5 . 122.9(2) yes
C2 . C3 . C5 . 130.8(2) yes
C1 . C4 . H41 . 109.467 no
C1 . C4 . H42 . 109.467 no
H41 . C4 . H42 . 109.476 no
C1 . C4 . H43 . 109.467 no
H41 . C4 . H43 . 109.476 no
H42 . C4 . H43 . 109.476 no
C3 . C5 . H51 . 109.467 no
C3 . C5 . H52 . 109.467 no
H51 . C5 . H52 . 109.476 no
C3 . C5 . H53 . 109.467 no
H51 . C5 . H53 . 109.476 no
H52 . C5 . H53 . 109.476 no
Sc1 . N3 . N4 . 114.92(12) yes
Sc1 . N3 . C6 . 139.92(15) yes
N4 . N3 . C6 . 104.83(17) yes
N3 . N4 . C8 . 111.96(18) yes
N3 . N4 . C11 . 118.70(16) yes
C8 . N4 . C11 . 129.34(19) yes
N3 . C6 . C7 . 110.4(2) yes
N3 . C6 . C9 . 122.7(2) yes
C7 . C6 . C9 . 126.9(2) yes
C6 . C7 . C8 . 106.91(19) yes
C6 . C7 . H71 . 126.546 no
C8 . C7 . H71 . 126.546 no
N4 . C8 . C7 . 105.9(2) yes
N4 . C8 . C10 . 122.8(2) yes
C7 . C8 . C10 . 131.3(2) yes
C6 . C9 . H91 . 109.467 no
C6 . C9 . H92 . 109.466 no
H91 . C9 . H92 . 109.476 no
C6 . C9 . H93 . 109.467 no
H91 . C9 . H93 . 109.476 no
H92 . C9 . H93 . 109.476 no
C8 . C10 . H101 . 109.467 no
C8 . C10 . H102 . 109.467 no
H101 . C10 . H102 . 109.475 no
C8 . C10 . H103 . 109.467 no
H101 . C10 . H103 . 109.476 no
H102 . C10 . H103 . 109.476 no
N2 . C11 . N4 . 108.84(16) yes
N2 . C11 . Si1 . 117.45(14) yes
N4 . C11 . Si1 . 113.97(14) yes
N2 . C11 . H111 . 105.927 no
N4 . C11 . H111 . 110.123 no
Si1 . C11 . H111 . 99.709 no
C11 . Si1 . N5 . 106.63(9) yes
C11 . Si1 . C12 . 102.14(10) yes
N5 . Si1 . C12 . 117.26(10) yes
C11 . Si1 . C13 . 101.73(10) yes
N5 . Si1 . C13 . 118.01(10) yes
C12 . Si1 . C13 . 108.57(12) yes
Sc1 . N5 . Si1 . 118.73(9) yes
Sc1 . N5 . C14 . 115.59(14) yes
Si1 . N5 . C14 . 125.26(15) yes
Si1 . C12 . H121 . 109.467 no
Si1 . C12 . H122 . 109.467 no
H121 . C12 . H122 . 109.476 no
Si1 . C12 . H123 . 109.466 no
H121 . C12 . H123 . 109.476 no
H122 . C12 . H123 . 109.476 no
Si1 . C13 . H131 . 109.467 no
Si1 . C13 . H132 . 109.466 no
H131 . C13 . H132 . 109.476 no
Si1 . C13 . H133 . 109.467 no
H131 . C13 . H133 . 109.476 no
H132 . C13 . H133 . 109.476 no
N5 . C14 . C15 . 112.86(19) yes
N5 . C14 . C16 . 113.2(2) yes
C15 . C14 . C16 . 110.1(2) yes
N5 . C14 . H141 . 104.601 no
C15 . C14 . H141 . 108.025 no
C16 . C14 . H141 . 107.683 no
C14 . C15 . H151 . 109.466 no
C14 . C15 . H152 . 109.467 no
H151 . C15 . H152 . 109.476 no
C14 . C15 . H153 . 109.467 no
H151 . C15 . H153 . 109.476 no
H152 . C15 . H153 . 109.476 no
C14 . C16 . H161 . 109.466 no
C14 . C16 . H162 . 109.467 no
H161 . C16 . H162 . 109.476 no
C14 . C16 . H163 . 109.466 no
H161 . C16 . H163 . 109.475 no
H162 . C16 . H163 . 109.476 no
Sc1 . C17 . Si2 . 122.37(12) yes
Sc1 . C17 . H1 . 98.8(17) no
Si2 . C17 . H1 . 106.3(17) no
Sc1 . C17 . H2 . 106(3) no
Si2 . C17 . H2 . 110(3) no
H1 . C17 . H2 . 112(3) no
C17 . Si2 . C18 . 110.97(12) yes
C17 . Si2 . C19 . 115.10(12) yes
C18 . Si2 . C19 . 107.51(13) yes
C17 . Si2 . C20 . 111.59(12) yes
C18 . Si2 . C20 . 106.62(13) yes
C19 . Si2 . C20 . 104.50(13) yes
Si2 . C18 . H181 . 109.467 no
Si2 . C18 . H182 . 109.467 no
H181 . C18 . H182 . 109.476 no
Si2 . C18 . H183 . 109.467 no
H181 . C18 . H183 . 109.476 no
H182 . C18 . H183 . 109.476 no
Si2 . C19 . H191 . 109.467 no
Si2 . C19 . H192 . 109.467 no
H191 . C19 . H192 . 109.476 no
Si2 . C19 . H193 . 109.466 no
H191 . C19 . H193 . 109.475 no
H192 . C19 . H193 . 109.476 no
Si2 . C20 . H201 . 109.467 no
Si2 . C20 . H202 . 109.466 no
H201 . C20 . H202 . 109.475 no
Si2 . C20 . H203 . 109.467 no
H201 . C20 . H203 . 109.476 no
H202 . C20 . H203 . 109.476 no
Sc1 . C21 . Si3 . 127.48(12) yes
Sc1 . C21 . H3 . 104(2) no
Si3 . C21 . H3 . 113(2) no
Sc1 . C21 . H4 . 101(2) no
Si3 . C21 . H4 . 106(2) no
H3 . C21 . H4 . 102(3) no
C21 . Si3 . C22 . 111.03(12) yes
C21 . Si3 . C23 . 113.37(12) yes
C22 . Si3 . C23 . 104.85(13) yes
C21 . Si3 . C24 . 113.40(11) yes
C22 . Si3 . C24 . 106.75(13) yes
C23 . Si3 . C24 . 106.87(12) yes
Si3 . C22 . H221 . 109.467 no
Si3 . C22 . H222 . 109.467 no
H221 . C22 . H222 . 109.476 no
Si3 . C22 . H223 . 109.466 no
H221 . C22 . H223 . 109.476 no
H222 . C22 . H223 . 109.476 no
Si3 . C23 . H231 . 109.467 no
Si3 . C23 . H232 . 109.466 no
H231 . C23 . H232 . 109.476 no
Si3 . C23 . H233 . 109.467 no
H231 . C23 . H233 . 109.476 no
H232 . C23 . H233 . 109.476 no
Si3 . C24 . H241 . 109.466 no
Si3 . C24 . H242 . 109.466 no
H241 . C24 . H242 . 109.476 no
Si3 . C24 . H243 . 109.467 no
H241 . C24 . H243 . 109.476 no
H242 . C24 . H243 . 109.476 no

##end