#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:48:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179765 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/61/7006199.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_7006199
loop_
_publ_author_name
'Bertolasi, Valerio'
'Boaretto, Rita'
'Chierotti, Michele R.'
'Gobetto, Roberto'
'Sostero, Silvana'
_publ_section_title
;
 Synthesis, characterization and reactivity of new complexes of
 titanium and zirconium containing a potential tridentate
 amidinato-cyclopentadienyl ligand.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5179
_journal_page_last               5189
_journal_paper_doi               10.1039/b709923a
_journal_year                    2007
_chemical_formula_moiety         'C18 H32 N4 S Si Ti'
_chemical_formula_sum            'C18 H32 N4 S Si Ti'
_chemical_formula_weight         412.53
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.870(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8186(2)
_cell_length_b                   17.3817(4)
_cell_length_c                   12.8635(3)
_cell_measurement_reflns_used    36023
_cell_measurement_temperature    150
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.40
_cell_volume                     2155.95(8)
_computing_cell_refinement       'Denzo SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        'Denzo SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP III (Burnett & Johnson, 1996)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'φ scans and ω scans'
_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  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34166
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.788
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SORTAV (R. H. Blessing, Acta Crystallogr., 1995, A51, 33)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         6260
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0421P)²+0.6772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                4268
_reflns_number_total             6260
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b709923a.txt
_cod_data_source_block           (2d)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7006199
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'
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 0.52352(3) 0.680455(19) 0.74738(2) 0.01866(9) Uani 1 1 d . . .
S1 S 0.26217(6) 0.82833(3) 0.75560(4) 0.03032(13) Uani 1 1 d . . .
Si1 Si 0.27713(5) 0.57835(3) 0.71509(4) 0.02006(12) Uani 1 1 d . . .
N1 N 0.31483(16) 0.67675(9) 0.72456(12) 0.0202(3) Uani 1 1 d . . .
N2 N 0.08885(17) 0.71558(10) 0.74316(13) 0.0269(4) Uani 1 1 d . . .
N3 N 0.56301(18) 0.70093(10) 0.89522(13) 0.0280(4) Uani 1 1 d . . .
N4 N 0.57220(17) 0.77792(10) 0.69214(13) 0.0272(4) Uani 1 1 d . . .
C1 C 0.45700(19) 0.55581(10) 0.69420(14) 0.0194(4) Uani 1 1 d . . .
C2 C 0.57809(19) 0.54669(11) 0.77606(14) 0.0214(4) Uani 1 1 d . . .
C3 C 0.69305(19) 0.57728(11) 0.73973(15) 0.0228(4) Uani 1 1 d . . .
C4 C 0.6482(2) 0.60349(11) 0.63304(15) 0.0231(4) Uani 1 1 d . . .
C5 C 0.50507(19) 0.58929(11) 0.60449(14) 0.0213(4) Uani 1 1 d . . .
C6 C 0.5860(2) 0.50833(12) 0.88202(16) 0.0279(4) Uani 1 1 d . . .
H61 H 0.6537 0.4679 0.8897 0.034 Uiso 1 1 calc R . .
H62 H 0.4970 0.4871 0.8866 0.034 Uiso 1 1 calc R . .
H63 H 0.6122 0.5455 0.9373 0.034 Uiso 1 1 calc R . .
C7 C 0.8424(2) 0.57333(13) 0.79519(18) 0.0318(5) Uani 1 1 d . . .
H71 H 0.8466 0.5685 0.8701 0.038 Uiso 1 1 calc R . .
H72 H 0.8896 0.6194 0.7809 0.038 Uiso 1 1 calc R . .
H73 H 0.8861 0.5296 0.7699 0.038 Uiso 1 1 calc R . .
C8 C 0.7448(2) 0.63184(14) 0.56440(17) 0.0328(5) Uani 1 1 d . . .
H81 H 0.7956 0.5892 0.5433 0.039 Uiso 1 1 calc R . .
H82 H 0.8084 0.6682 0.6032 0.039 Uiso 1 1 calc R . .
H83 H 0.6923 0.6562 0.5026 0.039 Uiso 1 1 calc R . .
C9 C 0.4178(2) 0.60316(12) 0.49656(15) 0.0280(4) Uani 1 1 d . . .
H91 H 0.4706 0.6318 0.4541 0.034 Uiso 1 1 calc R . .
H92 H 0.3365 0.6318 0.5037 0.034 Uiso 1 1 calc R . .
H93 H 0.3908 0.5547 0.4631 0.034 Uiso 1 1 calc R . .
C10 C 0.2331(2) 0.54089(12) 0.84032(16) 0.0285(4) Uani 1 1 d . . .
H101 H 0.3011 0.5583 0.8993 0.034 Uiso 1 1 calc R . .
H102 H 0.2323 0.4857 0.8387 0.034 Uiso 1 1 calc R . .
H103 H 0.1432 0.5594 0.8475 0.034 Uiso 1 1 calc R . .
C11 C 0.1345(2) 0.55015(13) 0.60506(17) 0.0318(5) Uani 1 1 d . . .
H111 H 0.0478 0.5687 0.6194 0.038 Uiso 1 1 calc R . .
H112 H 0.1312 0.4951 0.5990 0.038 Uiso 1 1 calc R . .
H113 H 0.1508 0.5721 0.5400 0.038 Uiso 1 1 calc R . .
C12 C 0.2188(2) 0.73036(11) 0.73878(14) 0.0216(4) Uani 1 1 d . . .
C13 C 0.0939(2) 0.84786(13) 0.76864(16) 0.0328(5) Uani 1 1 d . . .
H13 H 0.0595 0.8963 0.7803 0.039 Uiso 1 1 calc R . .
C14 C 0.0203(2) 0.78228(13) 0.75942(16) 0.0316(5) Uani 1 1 d . . .
H14 H -0.0731 0.7820 0.7638 0.038 Uiso 1 1 calc R . .
C15 C 0.4703(2) 0.70407(14) 0.97127(16) 0.0373(5) Uani 1 1 d . . .
H151 H 0.4888 0.6613 1.0190 0.045 Uiso 1 1 calc R . .
H152 H 0.3758 0.7017 0.9343 0.045 Uiso 1 1 calc R . .
H153 H 0.4851 0.7513 1.0106 0.045 Uiso 1 1 calc R . .
C16 C 0.7071(2) 0.70458(15) 0.94962(18) 0.0416(6) Uani 1 1 d . . .
H161 H 0.7201 0.7488 0.9952 0.050 Uiso 1 1 calc R . .
H162 H 0.7664 0.7085 0.8984 0.050 Uiso 1 1 calc R . .
H163 H 0.7298 0.6588 0.9911 0.050 Uiso 1 1 calc R . .
C17 C 0.5674(3) 0.79657(14) 0.58071(18) 0.0412(6) Uani 1 1 d . . .
H171 H 0.5091 0.8406 0.5618 0.049 Uiso 1 1 calc R . .
H172 H 0.5306 0.7536 0.5376 0.049 Uiso 1 1 calc R . .
H173 H 0.6593 0.8078 0.5696 0.049 Uiso 1 1 calc R . .
C18 C 0.6164(2) 0.84608(13) 0.75578(19) 0.0401(5) Uani 1 1 d . . .
H181 H 0.7077 0.8608 0.7467 0.048 Uiso 1 1 calc R . .
H182 H 0.6178 0.8349 0.8290 0.048 Uiso 1 1 calc R . .
H183 H 0.5529 0.8875 0.7335 0.048 Uiso 1 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'
S S 0.1246 0.1234 '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
N3 Ti1 N4 100.71(7) . . ?
N3 Ti1 N1 99.30(7) . . ?
N4 Ti1 N1 106.84(7) . . ?
N3 Ti1 C1 117.46(7) . . ?
N4 Ti1 C1 141.55(7) . . ?
N1 Ti1 C1 72.92(6) . . ?
N3 Ti1 C2 91.72(7) . . ?
N4 Ti1 C2 147.45(7) . . ?
N1 Ti1 C2 100.54(6) . . ?
C1 Ti1 C2 35.45(6) . . ?
N3 Ti1 C5 149.15(7) . . ?
N4 Ti1 C5 106.53(7) . . ?
N1 Ti1 C5 86.54(6) . . ?
C1 Ti1 C5 35.58(6) . . ?
C2 Ti1 C5 57.45(6) . . ?
N3 Ti1 C3 99.47(7) . . ?
N4 Ti1 C3 114.09(7) . . ?
N1 Ti1 C3 130.35(6) . . ?
C1 Ti1 C3 57.63(6) . . ?
C2 Ti1 C3 33.57(6) . . ?
C5 Ti1 C3 56.22(6) . . ?
N3 Ti1 C4 131.67(7) . . ?
N4 Ti1 C4 94.06(7) . . ?
N1 Ti1 C4 119.95(6) . . ?
C1 Ti1 C4 57.69(6) . . ?
C2 Ti1 C4 56.40(6) . . ?
C5 Ti1 C4 33.42(6) . . ?
C3 Ti1 C4 33.77(6) . . ?
N3 Ti1 Si1 105.02(5) . . ?
N4 Ti1 Si1 136.48(5) . . ?
N1 Ti1 Si1 34.96(4) . . ?
C1 Ti1 Si1 39.26(5) . . ?
C2 Ti1 Si1 66.06(5) . . ?
C5 Ti1 Si1 63.72(5) . . ?
C3 Ti1 Si1 95.64(5) . . ?
C4 Ti1 Si1 94.31(5) . . ?
C13 S1 C12 89.35(10) . . ?
N1 Si1 C11 115.46(9) . . ?
N1 Si1 C10 111.24(9) . . ?
C11 Si1 C10 107.56(10) . . ?
N1 Si1 C1 91.24(8) . . ?
C11 Si1 C1 115.47(9) . . ?
C10 Si1 C1 115.41(9) . . ?
N1 Si1 Ti1 41.31(5) . . ?
C11 Si1 Ti1 137.89(8) . . ?
C10 Si1 Ti1 113.86(7) . . ?
C1 Si1 Ti1 51.71(6) . . ?
C12 N1 Si1 122.39(13) . . ?
C12 N1 Ti1 131.98(13) . . ?
Si1 N1 Ti1 103.73(8) . . ?
C12 N2 C14 110.41(18) . . ?
C16 N3 C15 110.42(16) . . ?
C16 N3 Ti1 119.02(14) . . ?
C15 N3 Ti1 130.00(14) . . ?
C18 N4 C17 108.74(17) . . ?
C18 N4 Ti1 125.02(14) . . ?
C17 N4 Ti1 126.21(14) . . ?
C2 C1 C5 106.17(15) . . ?
C2 C1 Si1 125.97(14) . . ?
C5 C1 Si1 119.14(13) . . ?
C2 C1 Ti1 74.96(10) . . ?
C5 C1 Ti1 75.21(10) . . ?
Si1 C1 Ti1 89.03(7) . . ?
C3 C2 C1 108.62(16) . . ?
C3 C2 C6 124.13(17) . . ?
C1 C2 C6 127.20(17) . . ?
C3 C2 Ti1 75.66(11) . . ?
C1 C2 Ti1 69.59(10) . . ?
C6 C2 Ti1 122.69(13) . . ?
C2 C3 C4 108.53(16) . . ?
C2 C3 C7 126.62(17) . . ?
C4 C3 C7 124.28(18) . . ?
C2 C3 Ti1 70.77(11) . . ?
C4 C3 Ti1 73.68(11) . . ?
C7 C3 Ti1 128.27(14) . . ?
C5 C4 C3 107.78(16) . . ?
C5 C4 C8 128.12(17) . . ?
C3 C4 C8 123.74(17) . . ?
C5 C4 Ti1 70.61(10) . . ?
C3 C4 Ti1 72.55(11) . . ?
C8 C4 Ti1 127.75(14) . . ?
C4 C5 C1 108.80(16) . . ?
C4 C5 C9 125.40(17) . . ?
C1 C5 C9 125.74(17) . . ?
C4 C5 Ti1 75.97(11) . . ?
C1 C5 Ti1 69.21(10) . . ?
C9 C5 Ti1 123.09(13) . . ?
C2 C6 H61 109.5 . . ?
C2 C6 H62 109.5 . . ?
H61 C6 H62 109.5 . . ?
C2 C6 H63 109.5 . . ?
H61 C6 H63 109.5 . . ?
H62 C6 H63 109.5 . . ?
C3 C7 H71 109.5 . . ?
C3 C7 H72 109.5 . . ?
H71 C7 H72 109.5 . . ?
C3 C7 H73 109.5 . . ?
H71 C7 H73 109.5 . . ?
H72 C7 H73 109.5 . . ?
C4 C8 H81 109.5 . . ?
C4 C8 H82 109.5 . . ?
H81 C8 H82 109.5 . . ?
C4 C8 H83 109.5 . . ?
H81 C8 H83 109.5 . . ?
H82 C8 H83 109.5 . . ?
C5 C9 H91 109.5 . . ?
C5 C9 H92 109.5 . . ?
H91 C9 H92 109.5 . . ?
C5 C9 H93 109.5 . . ?
H91 C9 H93 109.5 . . ?
H92 C9 H93 109.5 . . ?
Si1 C10 H101 109.5 . . ?
Si1 C10 H102 109.5 . . ?
H101 C10 H102 109.5 . . ?
Si1 C10 H103 109.5 . . ?
H101 C10 H103 109.5 . . ?
H102 C10 H103 109.5 . . ?
Si1 C11 H111 109.5 . . ?
Si1 C11 H112 109.5 . . ?
H111 C11 H112 109.5 . . ?
Si1 C11 H113 109.5 . . ?
H111 C11 H113 109.5 . . ?
H112 C11 H113 109.5 . . ?
N2 C12 N1 125.07(18) . . ?
N2 C12 S1 113.49(14) . . ?
N1 C12 S1 121.44(14) . . ?
C14 C13 S1 109.50(16) . . ?
C14 C13 H13 125.3 . . ?
S1 C13 H13 125.3 . . ?
C13 C14 N2 117.25(19) . . ?
C13 C14 H14 121.4 . . ?
N2 C14 H14 121.4 . . ?
N3 C15 H151 109.5 . . ?
N3 C15 H152 109.5 . . ?
H151 C15 H152 109.5 . . ?
N3 C15 H153 109.5 . . ?
H151 C15 H153 109.5 . . ?
H152 C15 H153 109.5 . . ?
N3 C16 H161 109.5 . . ?
N3 C16 H162 109.5 . . ?
H161 C16 H162 109.5 . . ?
N3 C16 H163 109.5 . . ?
H161 C16 H163 109.5 . . ?
H162 C16 H163 109.5 . . ?
N4 C17 H171 109.5 . . ?
N4 C17 H172 109.5 . . ?
H171 C17 H172 109.5 . . ?
N4 C17 H173 109.5 . . ?
H171 C17 H173 109.5 . . ?
H172 C17 H173 109.5 . . ?
N4 C18 H181 109.5 . . ?
N4 C18 H182 109.5 . . ?
H181 C18 H182 109.5 . . ?
N4 C18 H183 109.5 . . ?
H181 C18 H183 109.5 . . ?
H182 C18 H183 109.5 . . ?
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 N3 1.9014(16) . ?
Ti1 N4 1.9317(17) . ?
Ti1 N1 2.0154(16) . ?
Ti1 C1 2.3280(18) . ?
Ti1 C2 2.3989(19) . ?
Ti1 C5 2.4077(18) . ?
Ti1 C3 2.4614(19) . ?
Ti1 C4 2.4763(19) . ?
Ti1 Si1 2.9657(6) . ?
S1 C13 1.725(2) . ?
S1 C12 1.759(2) . ?
Si1 N1 1.7493(16) . ?
Si1 C11 1.860(2) . ?
Si1 C10 1.862(2) . ?
Si1 C1 1.8771(19) . ?
N1 C12 1.362(2) . ?
N2 C12 1.314(2) . ?
N2 C14 1.376(3) . ?
N3 C16 1.457(3) . ?
N3 C15 1.458(3) . ?
N4 C18 1.459(3) . ?
N4 C17 1.462(3) . ?
C1 C2 1.441(3) . ?
C1 C5 1.449(3) . ?
C2 C3 1.405(3) . ?
C2 C6 1.506(3) . ?
C3 C4 1.434(3) . ?
C3 C7 1.506(3) . ?
C4 C5 1.406(3) . ?
C4 C8 1.495(3) . ?
C5 C9 1.507(3) . ?
C6 H61 0.9600 . ?
C6 H62 0.9600 . ?
C6 H63 0.9600 . ?
C7 H71 0.9600 . ?
C7 H72 0.9600 . ?
C7 H73 0.9600 . ?
C8 H81 0.9600 . ?
C8 H82 0.9600 . ?
C8 H83 0.9600 . ?
C9 H91 0.9600 . ?
C9 H92 0.9600 . ?
C9 H93 0.9600 . ?
C10 H101 0.9600 . ?
C10 H102 0.9600 . ?
C10 H103 0.9600 . ?
C11 H111 0.9600 . ?
C11 H112 0.9600 . ?
C11 H113 0.9600 . ?
C13 C14 1.343(3) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C15 H151 0.9600 . ?
C15 H152 0.9600 . ?
C15 H153 0.9600 . ?
C16 H161 0.9600 . ?
C16 H162 0.9600 . ?
C16 H163 0.9600 . ?
C17 H171 0.9600 . ?
C17 H172 0.9600 . ?
C17 H173 0.9600 . ?
C18 H181 0.9600 . ?
C18 H182 0.9600 . ?
C18 H183 0.9600 . ?
