#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:58:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179272 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/92/4319274.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4319274
loop_
_publ_author_name
'Alexander J. Blake'
'Philip E. Collier'
'Lutz H. Gade'
'Philip Mountford'
'Julian Lloyd'
'Stephen M. Pugh'
'Martin Schubart'
'Michael E. G. Skinner'
'Dominique J. M. Trösch'
_publ_contact_author
;
 Professor L H Gade
 Laboratoire de Chimie Organometallique et de Catalyse
 Institut Le Bel
 Universite Louis Pasteur
 4 rue Blaise Pascal
 67070 Strasbourg Cedex
 FRANCE
;
_publ_contact_author_email       Gade@chimie.u-strasbg.fr
_publ_section_title
;
 Group 4 Imido Complexes Stabilized by a Tridentate Diamido-Donor Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              870
_journal_page_last               877
_journal_paper_doi               10.1021/ic0005644
_journal_volume                  40
_journal_year                    2001
_chemical_formula_structural
;

 [{MeC(2-C5H4N)(CH2NSiMe3)2}Ti(NBu-t)(py)]

;
_chemical_formula_sum            'C24 H43 N5 Si2 Ti'
_chemical_formula_weight         505.71
_chemical_name_common
;

 [{(2-C5H4N)CMe(CH2NSiMe3)2}Ti(Nt-Bu)(py)]

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'initially placed geometrically'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.63(3)
_cell_angle_beta                 106.61(3)
_cell_angle_gamma                105.40(2)
_cell_formula_units_Z            2
_cell_length_a                   9.535(3)
_cell_length_b                   10.125(3)
_cell_length_c                   15.948(3)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      35.5
_cell_measurement_theta_min      27.9
_cell_volume                     1416.1(7)
_computing_cell_refinement       'STADI-4 version 1.06a (Stoe & Cie, 1996a)'
_computing_data_collection       'STADI-4 version 1.06a (Stoe & Cie, 1996a)'
_computing_data_reduction        'X-RED version 1.08 (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'SHELXTL/PC version 5.03 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.0(2)
_diffrn_measurement_device       'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       omega/theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7218
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        'variation +/-5'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.909
_exptl_absorpt_correction_type   'numerical integration'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'trigonal prism'
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.30
_refine_diff_density_rms         0.06
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.025
_refine_ls_goodness_of_fit_obs   1.033
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_restrained_S_obs      1.033
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_obs          0.0416
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.049)²+1.615P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1084
_refine_ls_wR_factor_obs         0.1011
_reflns_number_observed          4308
_reflns_number_total             4983
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0005644_2.cif
_cod_data_source_block           COMPOUND_3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_angle_publ_flag' value 'Yes' changed to 'yes' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (10 times).

'_geom_bond_publ_flag' value 'Yes'
changed to 'yes' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (6
times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.049)^2^+1.615P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.049)^2^+1.615P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4319274
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Ti Ti 0.13822(4) 0.28739(4) 0.24212(2) 0.01769(12) Uani 1 d . .
N1 N 0.2231(2) 0.2119(2) 0.33173(12) 0.0236(4) Uani 1 d . .
C10 C 0.3073(3) 0.1542(3) 0.40642(15) 0.0275(5) Uani 1 d . .
C11 C 0.3324(4) 0.0220(3) 0.37408(19) 0.0426(7) Uani 1 d . .
H11A H 0.3902 0.0428 0.3317 0.064 Uiso 1 calc R .
H11B H 0.2335 -0.0447 0.3458 0.064 Uiso 1 calc R .
H11C H 0.3895 -0.0169 0.4241 0.064 Uiso 1 calc R .
C12 C 0.2165(3) 0.1211(3) 0.47302(18) 0.0416(7) Uani 1 d . .
H12A H 0.1169 0.0559 0.4443 0.062 Uiso 1 calc R .
H12B H 0.2021 0.2060 0.4947 0.062 Uiso 1 calc R .
H12C H 0.2728 0.0805 0.5224 0.062 Uiso 1 calc R .
C13 C 0.4628(3) 0.2563(3) 0.45161(18) 0.0390(6) Uani 1 d . .
H13A H 0.5210 0.2776 0.4094 0.059 Uiso 1 calc R .
H13B H 0.5188 0.2155 0.5010 0.059 Uiso 1 calc R .
H13C H 0.4481 0.3410 0.4733 0.059 Uiso 1 calc R .
Si1 Si 0.40498(8) 0.56936(7) 0.21317(4) 0.02674(17) Uani 1 d . .
C21 C 0.4147(5) 0.7211(3) 0.2857(2) 0.0625(11) Uani 1 d . .
H21A H 0.3890 0.6892 0.3387 0.094 Uiso 1 calc R .
H21B H 0.3421 0.7694 0.2538 0.094 Uiso 1 calc R .
H21C H 0.5181 0.7840 0.3024 0.094 Uiso 1 calc R .
C22 C 0.4556(3) 0.6413(3) 0.11441(18) 0.0369(6) Uani 1 d . .
H22A H 0.4524 0.5661 0.0741 0.055 Uiso 1 calc R .
H22B H 0.5585 0.7051 0.1331 0.055 Uiso 1 calc R .
H22C H 0.3825 0.6904 0.0845 0.055 Uiso 1 calc R .
C23 C 0.5470(4) 0.4815(4) 0.2704(3) 0.0787(14) Uani 1 d . .
H23A H 0.5410 0.4026 0.2320 0.118 Uiso 1 calc R .
H23B H 0.5260 0.4495 0.3245 0.118 Uiso 1 calc R .
H23C H 0.6494 0.5458 0.2850 0.118 Uiso 1 calc R .
N2 N 0.2282(2) 0.45402(18) 0.18558(12) 0.0209(4) Uani 1 d . .
C3 C 0.1007(3) 0.5026(3) 0.13505(16) 0.0277(5) Uani 1 d . .
H3A H 0.0653 0.4567 0.0746 0.033 Uiso 1 calc R .
H3B H 0.1402 0.6024 0.1310 0.033 Uiso 1 calc R .
C4 C -0.0425(3) 0.4806(2) 0.16954(15) 0.0214(5) Uani 1 d . .
C4M C -0.1408(3) 0.5666(3) 0.11583(17) 0.0298(5) Uani 1 d . .
H4MA H -0.2318 0.5564 0.1349 0.045 Uiso 1 calc R .
H4MB H -0.1715 0.5347 0.0533 0.045 Uiso 1 calc R .
H4MC H -0.0817 0.6637 0.1250 0.045 Uiso 1 calc R .
C5 C -0.1453(3) 0.3282(2) 0.14940(15) 0.0253(5) Uani 1 d . .
H5A H -0.2430 0.3259 0.1604 0.030 Uiso 1 calc R .
H5B H -0.1689 0.3021 0.0858 0.030 Uiso 1 calc R .
N6 N -0.0874(2) 0.22119(18) 0.19749(12) 0.0195(4) Uani 1 d . .
Si2 Si -0.20817(7) 0.10935(6) 0.24382(4) 0.02144(16) Uani 1 d . .
C31 C -0.2078(3) 0.1875(3) 0.35093(17) 0.0346(6) Uani 1 d . .
H31A H -0.1038 0.2142 0.3913 0.052 Uiso 1 calc R .
H31B H -0.2743 0.1201 0.3767 0.052 Uiso 1 calc R .
H31C H -0.2453 0.2690 0.3409 0.052 Uiso 1 calc R .
C32 C -0.1481(3) -0.0516(2) 0.26306(17) 0.0284(5) Uani 1 d . .
H32A H -0.0426 -0.0288 0.3013 0.043 Uiso 1 calc R .
H32B H -0.1552 -0.0968 0.2067 0.043 Uiso 1 calc R .
H32C H -0.2150 -0.1137 0.2912 0.043 Uiso 1 calc R .
C33 C -0.4102(3) 0.0610(3) 0.17044(18) 0.0345(6) Uani 1 d . .
H33A H -0.4151 0.0196 0.1135 0.052 Uiso 1 calc R .
H33B H -0.4460 0.1435 0.1618 0.052 Uiso 1 calc R .
H33C H -0.4750 -0.0052 0.1977 0.052 Uiso 1 calc R .
N41 N 0.0951(2) 0.44913(19) 0.31655(12) 0.0212(4) Uani 1 d . .
C42 C 0.1511(3) 0.4815(2) 0.40368(15) 0.0260(5) Uani 1 d . .
H42A H 0.2101 0.4280 0.4381 0.031 Uiso 1 calc R .
C43 C 0.1265(3) 0.5895(3) 0.44537(17) 0.0329(6) Uani 1 d . .
H43A H 0.1683 0.6104 0.5072 0.040 Uiso 1 calc R .
C44 C 0.0398(3) 0.6665(3) 0.39542(18) 0.0350(6) Uani 1 d . .
H44A H 0.0210 0.7414 0.4224 0.042 Uiso 1 calc R .
C45 C -0.0190(3) 0.6330(2) 0.30568(17) 0.0299(5) Uani 1 d . .
H45A H -0.0795 0.6846 0.2705 0.036 Uiso 1 calc R .
C46 C 0.0102(3) 0.5241(2) 0.26692(15) 0.0220(5) Uani 1 d . .
N51 N 0.1780(2) 0.15653(19) 0.13878(12) 0.0213(4) Uani 1 d . .
C52 C 0.1440(3) 0.0191(2) 0.14006(16) 0.0262(5) Uani 1 d . .
H52A H 0.1100 -0.0207 0.1869 0.031 Uiso 1 calc R .
C53 C 0.1563(3) -0.0669(3) 0.07641(17) 0.0309(6) Uani 1 d . .
H53A H 0.1302 -0.1636 0.0798 0.037 Uiso 1 calc R .
C54 C 0.2063(3) -0.0122(3) 0.00806(17) 0.0308(6) Uani 1 d . .
H54A H 0.2137 -0.0698 -0.0370 0.037 Uiso 1 calc R .
C55 C 0.2456(3) 0.1293(3) 0.00702(16) 0.0308(6) Uani 1 d . .
H55A H 0.2834 0.1711 -0.0381 0.037 Uiso 1 calc R .
C56 C 0.2291(3) 0.2093(2) 0.07265(15) 0.0259(5) Uani 1 d . .
H56A H 0.2553 0.3063 0.0708 0.031 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 Ti N2 130.09(9) . . yes
N1 Ti N6 115.84(9) . . yes
N1 Ti N41 96.73(8) . . yes
N1 Ti N51 96.45(8) . . yes
N2 Ti N6 113.33(8) . . yes
N2 Ti N41 80.34(7) . . yes
N2 Ti N51 87.19(7) . . yes
N6 Ti N41 83.79(8) . . yes
N6 Ti N51 95.12(8) . . yes
N41 Ti N51 165.83(7) . . yes
C10 N1 Ti 175.10(17) . . ?
N1 C10 C11 109.2(2) . . ?
N1 C10 C13 110.4(2) . . ?
C11 C10 C13 108.7(2) . . ?
N1 C10 C12 110.0(2) . . ?
C11 C10 C12 109.3(2) . . ?
C13 C10 C12 109.2(2) . . ?
N2 Si1 C23 108.62(14) . . ?
N2 Si1 C22 112.21(11) . . ?
C23 Si1 C22 108.83(16) . . ?
N2 Si1 C21 111.02(14) . . ?
C23 Si1 C21 110.1(2) . . ?
C22 Si1 C21 106.01(14) . . ?
C3 N2 Si1 116.75(15) . . ?
C3 N2 Ti 106.71(14) . . ?
Si1 N2 Ti 132.29(11) . . ?
N2 C3 C4 118.09(18) . . ?
C46 C4 C4M 112.74(19) . . ?
C46 C4 C5 110.84(18) . . ?
C4M C4 C5 105.57(19) . . ?
C46 C4 C3 109.31(19) . . ?
C4M C4 C3 106.31(18) . . ?
C5 C4 C3 111.99(19) . . ?
N6 C5 C4 118.65(18) . . ?
C5 N6 Si2 116.93(15) . . ?
C5 N6 Ti 108.97(14) . . ?
Si2 N6 Ti 127.41(10) . . ?
N6 Si2 C32 109.70(10) . . ?
N6 Si2 C31 111.49(11) . . ?
C32 Si2 C31 108.92(12) . . ?
N6 Si2 C33 111.60(11) . . ?
C32 Si2 C33 108.02(12) . . ?
C31 Si2 C33 106.98(13) . . ?
C42 N41 C46 119.3(2) . . ?
C42 N41 Ti 125.72(16) . . ?
C46 N41 Ti 114.94(15) . . ?
N41 C42 C43 122.6(2) . . ?
C42 C43 C44 118.6(2) . . ?
C43 C44 C45 119.0(2) . . ?
C44 C45 C46 120.0(2) . . ?
N41 C46 C45 120.4(2) . . ?
N41 C46 C4 114.43(19) . . ?
C45 C46 C4 125.1(2) . . ?
C56 N51 C52 116.8(2) . . ?
C56 N51 Ti 123.11(15) . . ?
C52 N51 Ti 120.06(15) . . ?
N51 C52 C53 123.0(2) . . ?
C54 C53 C52 119.8(2) . . ?
C53 C54 C55 117.9(2) . . ?
C54 C55 C56 119.2(2) . . ?
N51 C56 C55 123.3(2) . . ?
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
Ti N1 1.724(2) . yes
Ti N2 2.025(2) . yes
Ti N6 1.983(2) . yes
Ti N41 2.203(2) . yes
Ti N51 2.278(2) . yes
N1 C10 1.457(3) . yes
C10 C11 1.531(4) . ?
C10 C13 1.531(4) . ?
C10 C12 1.539(4) . ?
Si1 N2 1.709(2) . ?
Si1 C23 1.846(3) . ?
Si1 C22 1.876(3) . ?
Si1 C21 1.879(3) . ?
N2 C3 1.461(3) . ?
C3 C4 1.578(3) . ?
C4 C46 1.510(3) . ?
C4 C4M 1.537(3) . ?
C4 C5 1.566(3) . ?
C5 N6 1.470(3) . ?
N6 Si2 1.722(2) . ?
Si2 C32 1.867(2) . ?
Si2 C31 1.873(3) . ?
Si2 C33 1.875(3) . ?
N41 C42 1.340(3) . ?
N41 C46 1.353(3) . ?
C42 C43 1.379(4) . ?
C43 C44 1.380(4) . ?
C44 C45 1.381(4) . ?
C45 C46 1.387(3) . ?
N51 C56 1.343(3) . ?
N51 C52 1.344(3) . ?
C52 C53 1.380(3) . ?
C53 C54 1.376(4) . ?
C54 C55 1.383(4) . ?
C55 C56 1.385(3) . ?
