#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/05/4110596.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_4110596
loop_
_publ_author_name
'Tamara E. Hanna'
'Emil Lobkovsky'
'Paul J. Chirik'
_publ_section_title
;
 Mono(dinitrogen) and Carbon Monoxide Adducts of Bis(cyclopentadienyl)
 Titanium Sandwiches
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6018
_journal_page_last               6019
_journal_paper_doi               10.1021/ja061213c
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C17 H23 N Si Ti0.5'
_chemical_formula_weight         293.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.937(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2468(6)
_cell_length_b                   12.0669(4)
_cell_length_c                   14.6246(5)
_cell_measurement_reflns_used    6747
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.27
_cell_volume                     3172.29(18)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT+'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi  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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0304
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19466
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  0.9817
_exptl_absorpt_correction_T_min  0.8659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       rod
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         3990
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0548P)²+0.6946P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0891
_reflns_number_gt                3243
_reflns_number_total             3990
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja061213crom20060220_113547.cif
_cod_data_source_block           th18
_cod_original_formula_sum        'C17 H23 N Si Ti0.50'
_cod_database_code               4110596
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Ti1 Ti 0.0000 0.32025(2) 0.2500 0.01535(9) Uani 1 2 d S
Si1 Si 0.16057(2) 0.20397(3) 0.20589(3) 0.02004(10) Uani 1 1 d .
N1 N 0.0000 0.15317(13) 0.2500 0.0206(3) Uani 1 2 d S
N2 N 0.0000 0.06047(14) 0.2500 0.0297(4) Uani 1 2 d S
C1 C 0.07761(7) 0.29664(10) 0.16402(10) 0.0181(3) Uani 1 1 d .
C2 C 0.08011(7) 0.41260(10) 0.19124(9) 0.0181(3) Uani 1 1 d .
C3 C 0.00973(7) 0.46119(10) 0.13970(9) 0.0196(3) Uani 1 1 d .
C4 C -0.03774(7) 0.37780(11) 0.08253(9) 0.0202(3) Uani 1 1 d .
C5 C 0.00249(7) 0.27720(11) 0.09492(9) 0.0194(3) Uani 1 1 d .
C6 C 0.14857(8) 0.47327(11) 0.25415(11) 0.0230(3) Uani 1 1 d .
H6C H 0.1388(10) 0.5443(16) 0.2836(13) 0.045(5) Uiso 1 1 d .
H6B H 0.1808(10) 0.4295(15) 0.3094(14) 0.043(5) Uiso 1 1 d .
H6A H 0.1787(9) 0.4899(14) 0.2152(13) 0.039(5) Uiso 1 1 d .
C7 C -0.00955(8) 0.58235(11) 0.13293(12) 0.0258(3) Uani 1 1 d .
H7C H 0.0287(10) 0.6267(15) 0.1828(14) 0.042(5) Uiso 1 1 d .
H7B H -0.0119(9) 0.6096(14) 0.0704(14) 0.036(4) Uiso 1 1 d .
H7A H -0.0553(9) 0.5973(13) 0.1445(12) 0.032(4) Uiso 1 1 d .
C8 C -0.11625(8) 0.39671(14) 0.01433(11) 0.0285(3) Uani 1 1 d .
H8C H -0.1464(14) 0.3263(19) 0.0059(18) 0.071(7) Uiso 1 1 d .
H8B H -0.1412(11) 0.4485(17) 0.0407(15) 0.051(5) Uiso 1 1 d .
H8A H -0.1165(10) 0.4231(16) -0.0476(15) 0.049(5) Uiso 1 1 d .
C9 C -0.02644(9) 0.17575(12) 0.03382(11) 0.0267(3) Uani 1 1 d .
H9C H -0.0105(9) 0.1052(16) 0.0693(13) 0.040(5) Uiso 1 1 d .
H9B H -0.0796(11) 0.1741(14) 0.0049(14) 0.043(5) Uiso 1 1 d .
H9A H -0.0104(11) 0.1773(15) -0.0200(16) 0.047(5) Uiso 1 1 d .
C10 C 0.19426(9) 0.17794(14) 0.34061(12) 0.0301(3) Uani 1 1 d .
H10C H 0.2113(10) 0.2435(16) 0.3759(14) 0.039(5) Uiso 1 1 d .
H10B H 0.2340(11) 0.1243(16) 0.3593(14) 0.048(5) Uiso 1 1 d .
H10A H 0.1562(10) 0.1450(15) 0.3572(14) 0.040(5) Uiso 1 1 d .
C11 C 0.14215(9) 0.06743(12) 0.14158(13) 0.0295(3) Uani 1 1 d .
H11B H 0.1055(9) 0.0259(14) 0.1589(12) 0.036(5) Uiso 1 1 d .
H11A H 0.1242(9) 0.0755(14) 0.0696(14) 0.037(5) Uiso 1 1 d .
H11C H 0.1882(10) 0.0244(14) 0.1622(13) 0.041(5) Uiso 1 1 d .
C12 C 0.23695(7) 0.27535(10) 0.17600(11) 0.0228(3) Uani 1 1 d .
C13 C 0.31128(8) 0.27237(12) 0.23853(12) 0.0284(3) Uani 1 1 d .
H13 H 0.3241(9) 0.2362(14) 0.3017(13) 0.032(4) Uiso 1 1 d .
C14 C 0.36700(9) 0.32320(12) 0.21350(14) 0.0333(4) Uani 1 1 d .
H14 H 0.4201(11) 0.3220(13) 0.2600(14) 0.037(5) Uiso 1 1 d .
C15 C 0.34908(9) 0.37878(12) 0.12566(13) 0.0339(4) Uani 1 1 d .
H15 H 0.3859(10) 0.4165(14) 0.1055(14) 0.044(5) Uiso 1 1 d .
C16 C 0.27594(9) 0.38331(13) 0.06253(13) 0.0345(4) Uani 1 1 d .
H16 H 0.2627(10) 0.4223(15) 0.0017(14) 0.044(5) Uiso 1 1 d .
C17 C 0.22079(9) 0.33211(12) 0.08772(12) 0.0296(3) Uani 1 1 d .
H17 H 0.1714(10) 0.3363(14) 0.0440(14) 0.038(5) Uiso 1 1 d .
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
N1 Ti1 C1 82.85(3) . 2
N1 Ti1 C1 82.85(3) . .
C1 Ti1 C1 165.70(6) 2 .
N1 Ti1 C2 118.94(3) . 2
C1 Ti1 C2 36.84(4) 2 2
C1 Ti1 C2 157.04(5) . 2
N1 Ti1 C2 118.94(3) . .
C1 Ti1 C2 157.04(5) 2 .
C1 Ti1 C2 36.84(4) . .
C2 Ti1 C2 122.12(6) 2 .
N1 Ti1 C5 77.20(3) . 2
C1 Ti1 C5 36.64(5) 2 2
C1 Ti1 C5 138.35(5) . 2
C2 Ti1 C5 59.89(4) 2 2
C2 Ti1 C5 135.74(5) . 2
N1 Ti1 C5 77.20(3) . .
C1 Ti1 C5 138.35(5) 2 .
C1 Ti1 C5 36.64(5) . .
C2 Ti1 C5 135.74(5) 2 .
C2 Ti1 C5 59.89(4) . .
C5 Ti1 C5 154.39(6) 2 .
N1 Ti1 C4 106.85(3) . .
C1 Ti1 C4 125.38(4) 2 .
C1 Ti1 C4 59.55(4) . .
C2 Ti1 C4 104.03(4) 2 .
C2 Ti1 C4 58.47(4) . .
C5 Ti1 C4 161.82(4) 2 .
C5 Ti1 C4 34.76(4) . .
N1 Ti1 C4 106.85(3) . 2
C1 Ti1 C4 59.55(4) 2 2
C1 Ti1 C4 125.38(4) . 2
C2 Ti1 C4 58.47(4) 2 2
C2 Ti1 C4 104.03(4) . 2
C5 Ti1 C4 34.76(4) 2 2
C5 Ti1 C4 161.82(4) . 2
C4 Ti1 C4 146.29(6) . 2
N1 Ti1 C3 135.20(3) . 2
C1 Ti1 C3 59.68(4) 2 2
C1 Ti1 C3 132.96(4) . 2
C2 Ti1 C3 35.10(4) 2 2
C2 Ti1 C3 97.55(4) . 2
C5 Ti1 C3 58.16(4) 2 2
C5 Ti1 C3 147.35(5) . 2
C4 Ti1 C3 114.48(5) . 2
C4 Ti1 C3 34.33(4) 2 2
N1 Ti1 C3 135.20(3) . .
C1 Ti1 C3 132.96(4) 2 .
C1 Ti1 C3 59.68(4) . .
C2 Ti1 C3 97.55(4) 2 .
C2 Ti1 C3 35.10(4) . .
C5 Ti1 C3 147.35(5) 2 .
C5 Ti1 C3 58.17(4) . .
C4 Ti1 C3 34.33(4) . .
C4 Ti1 C3 114.48(5) 2 .
C3 Ti1 C3 89.61(6) 2 .
C1 Si1 C10 112.40(7) . .
C1 Si1 C11 112.19(7) . .
C10 Si1 C11 108.35(8) . .
C1 Si1 C12 107.29(6) . .
C10 Si1 C12 108.42(7) . .
C11 Si1 C12 108.05(6) . .
N2 N1 Ti1 180.0 . .
C2 C1 C5 105.85(10) . .
C2 C1 Si1 123.22(9) . .
C5 C1 Si1 130.72(9) . .
C2 C1 Ti1 72.14(7) . .
C5 C1 Ti1 73.76(7) . .
Si1 C1 Ti1 123.01(6) . .
C3 C2 C1 108.71(11) . .
C3 C2 C6 125.87(11) . .
C1 C2 C6 125.06(11) . .
C3 C2 Ti1 76.06(7) . .
C1 C2 Ti1 71.02(7) . .
C6 C2 Ti1 124.43(9) . .
C4 C3 C2 108.19(11) . .
C4 C3 C7 124.13(12) . .
C2 C3 C7 127.07(12) . .
C4 C3 Ti1 72.76(7) . .
C2 C3 Ti1 68.84(7) . .
C7 C3 Ti1 131.13(9) . .
C5 C4 C3 109.03(11) . .
C5 C4 C8 126.15(12) . .
C3 C4 C8 124.67(12) . .
C5 C4 Ti1 70.64(7) . .
C3 C4 Ti1 72.90(7) . .
C8 C4 Ti1 126.08(9) . .
C4 C5 C1 108.20(11) . .
C4 C5 C9 123.60(12) . .
C1 C5 C9 127.57(12) . .
C4 C5 Ti1 74.61(7) . .
C1 C5 Ti1 69.60(7) . .
C9 C5 Ti1 128.72(9) . .
C17 C12 C13 117.14(13) . .
C17 C12 Si1 120.31(11) . .
C13 C12 Si1 122.54(11) . .
C14 C13 C12 121.42(15) . .
C15 C14 C13 119.94(15) . .
C14 C15 C16 119.85(14) . .
C15 C16 C17 119.91(15) . .
C16 C17 C12 121.74(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N1 2.0161(16) .
Ti1 C1 2.2881(12) 2
Ti1 C1 2.2881(12) .
Ti1 C2 2.3031(12) 2
Ti1 C2 2.3032(12) .
Ti1 C5 2.3439(13) 2
Ti1 C5 2.3439(13) .
Ti1 C4 2.3952(13) .
Ti1 C4 2.3952(13) 2
Ti1 C3 2.3970(12) 2
Ti1 C3 2.3970(12) .
Si1 C1 1.8645(13) .
Si1 C10 1.8676(17) .
Si1 C11 1.8673(15) .
Si1 C12 1.8849(13) .
N1 N2 1.119(2) .
C1 C2 1.4508(17) .
C1 C5 1.4568(18) .
C2 C3 1.4202(17) .
C2 C6 1.5007(18) .
C3 C4 1.4144(18) .
C3 C7 1.5029(18) .
C4 C5 1.4163(18) .
C4 C8 1.5010(19) .
C5 C9 1.5005(19) .
C12 C17 1.395(2) .
C12 C13 1.396(2) .
C13 C14 1.393(2) .
C14 C15 1.379(2) .
C15 C16 1.381(2) .
C16 C17 1.387(2) .
