#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/05/4110595.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_4110595
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            'C17.5 H23 O0.5 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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.0570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2729(8)
_cell_length_b                   12.0720(5)
_cell_length_c                   14.6636(6)
_cell_measurement_reflns_used    3838
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      2.26
_cell_volume                     3183.8(2)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0382
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18171
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  0.9908
_exptl_absorpt_correction_T_min  0.8662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                3544
_reflns_number_total             4819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja061213crom20060220_113527.cif
_cod_data_source_block           th24
_cod_original_formula_sum        'C17.50 H23 O0.50 Si Ti0.50'
_cod_database_code               4110595
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 0.32122(3) 0.2500 0.01929(9) Uani 1 2 d S
Si1 Si 0.16162(2) 0.20382(3) 0.20612(3) 0.02407(10) Uani 1 1 d .
O1 O 0.0000 0.06200(12) 0.2500 0.0399(4) Uani 1 2 d S
C1 C 0.07823(7) 0.29653(10) 0.16441(9) 0.0210(3) Uani 1 1 d .
C2 C 0.08091(7) 0.41235(10) 0.19137(9) 0.0208(2) Uani 1 1 d .
C3 C 0.01053(7) 0.46105(10) 0.14000(9) 0.0226(3) Uani 1 1 d .
C4 C -0.03705(7) 0.37737(11) 0.08349(9) 0.0231(3) Uani 1 1 d .
C5 C 0.00310(7) 0.27664(11) 0.09604(9) 0.0225(3) Uani 1 1 d .
C6 C 0.14925(8) 0.47307(12) 0.25423(11) 0.0266(3) Uani 1 1 d .
H6C H 0.1760(9) 0.4886(13) 0.2133(12) 0.035(4) Uiso 1 1 d .
H6B H 0.1825(10) 0.4270(15) 0.3086(13) 0.046(5) Uiso 1 1 d .
H6A H 0.1382(10) 0.5448(16) 0.2820(13) 0.050(5) Uiso 1 1 d .
C7 C -0.00858(9) 0.58215(12) 0.13312(12) 0.0299(3) Uani 1 1 d .
H7C H 0.0294(10) 0.6238(15) 0.1833(14) 0.046(5) Uiso 1 1 d .
H7B H -0.0540(10) 0.5958(14) 0.1437(12) 0.040(5) Uiso 1 1 d .
H7A H -0.0137(9) 0.6060(14) 0.0680(14) 0.042(5) Uiso 1 1 d .
C8 C -0.11588(8) 0.39585(15) 0.01546(12) 0.0334(3) Uani 1 1 d .
H8C H -0.1163(10) 0.4213(15) -0.0459(14) 0.048(5) Uiso 1 1 d .
H8B H -0.1422(12) 0.4491(19) 0.0429(16) 0.073(7) Uiso 1 1 d .
H8A H -0.1455(14) 0.3228(19) 0.0053(17) 0.072(7) Uiso 1 1 d .
C9 C -0.02560(9) 0.17561(13) 0.03429(11) 0.0312(3) Uani 1 1 d .
H9C H -0.0096(10) 0.1049(16) 0.0700(13) 0.047(5) Uiso 1 1 d .
H9B H -0.0804(11) 0.1732(14) 0.0065(14) 0.049(5) Uiso 1 1 d .
H9A H -0.0092(11) 0.1804(15) -0.0221(16) 0.054(6) Uiso 1 1 d .
C10 C 0.0000 0.15732(16) 0.2500 0.0237(4) Uani 1 2 d S
C11 C 0.14272(9) 0.06748(12) 0.14217(13) 0.0348(3) Uani 1 1 d .
H11C H 0.1041(9) 0.0241(14) 0.1606(12) 0.041(5) Uiso 1 1 d .
H11B H 0.1235(9) 0.0758(14) 0.0677(13) 0.035(4) Uiso 1 1 d .
H11A H 0.1907(12) 0.0258(16) 0.1605(15) 0.059(6) Uiso 1 1 d .
C12 C 0.19629(9) 0.17827(15) 0.34060(12) 0.0356(4) Uani 1 1 d .
H12C H 0.2118(11) 0.2451(18) 0.3746(14) 0.052(6) Uiso 1 1 d .
H12B H 0.2368(11) 0.1205(16) 0.3595(14) 0.052(5) Uiso 1 1 d .
H12A H 0.1569(11) 0.1484(16) 0.3581(14) 0.052(5) Uiso 1 1 d .
C13 C 0.23737(8) 0.27558(11) 0.17554(11) 0.0264(3) Uani 1 1 d .
C14 C 0.31190(8) 0.27312(13) 0.23784(12) 0.0324(3) Uani 1 1 d .
H14 H 0.3253(9) 0.2388(15) 0.3030(13) 0.044(5) Uiso 1 1 d .
C15 C 0.36705(9) 0.32478(13) 0.21267(14) 0.0380(4) Uani 1 1 d .
H15 H 0.4214(11) 0.3249(14) 0.2615(14) 0.050(5) Uiso 1 1 d .
C16 C 0.34899(9) 0.38036(13) 0.12530(14) 0.0391(4) Uani 1 1 d .
H16 H 0.3868(11) 0.4179(16) 0.1061(15) 0.061(6) Uiso 1 1 d .
C17 C 0.27585(10) 0.38436(14) 0.06245(13) 0.0392(4) Uani 1 1 d .
H17 H 0.2613(10) 0.4231(16) -0.0019(14) 0.052(5) Uiso 1 1 d .
C18 C 0.22091(9) 0.33247(13) 0.08736(12) 0.0335(3) Uani 1 1 d .
H18 H 0.1704(11) 0.3351(15) 0.0428(15) 0.049(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'
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'
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
C10 Ti1 C1 82.56(3) . 2
C10 Ti1 C1 82.56(3) . .
C1 Ti1 C1 165.12(6) 2 .
C10 Ti1 C2 118.42(3) . 2
C1 Ti1 C2 36.61(4) 2 2
C1 Ti1 C2 157.82(5) . 2
C10 Ti1 C2 118.42(3) . .
C1 Ti1 C2 157.82(5) 2 .
C1 Ti1 C2 36.61(4) . .
C2 Ti1 C2 123.17(6) 2 .
C10 Ti1 C5 76.72(3) . .
C1 Ti1 C5 138.11(4) 2 .
C1 Ti1 C5 36.50(4) . .
C2 Ti1 C5 136.21(4) 2 .
C2 Ti1 C5 59.78(4) . .
C10 Ti1 C5 76.72(3) . 2
C1 Ti1 C5 36.50(4) 2 2
C1 Ti1 C5 138.11(4) . 2
C2 Ti1 C5 59.78(4) 2 2
C2 Ti1 C5 136.21(4) . 2
C5 Ti1 C5 153.43(7) . 2
C10 Ti1 C4 106.53(3) . 2
C1 Ti1 C4 59.47(4) 2 2
C1 Ti1 C4 125.57(4) . 2
C2 Ti1 C4 58.50(4) 2 2
C2 Ti1 C4 104.58(4) . 2
C5 Ti1 C4 161.97(4) . 2
C5 Ti1 C4 34.90(4) 2 2
C10 Ti1 C4 106.53(3) . .
C1 Ti1 C4 125.57(4) 2 .
C1 Ti1 C4 59.46(4) . .
C2 Ti1 C4 104.58(4) 2 .
C2 Ti1 C4 58.49(4) . .
C5 Ti1 C4 34.90(4) . .
C5 Ti1 C4 161.97(4) 2 .
C4 Ti1 C4 146.94(7) 2 .
C10 Ti1 C3 134.86(3) . 2
C1 Ti1 C3 59.54(4) 2 2
C1 Ti1 C3 133.60(4) . 2
C2 Ti1 C3 35.10(4) 2 2
C2 Ti1 C3 98.44(4) . 2
C5 Ti1 C3 148.14(5) . 2
C5 Ti1 C3 58.32(4) 2 2
C4 Ti1 C3 34.46(4) 2 2
C4 Ti1 C3 115.03(5) . 2
C10 Ti1 C3 134.86(3) . .
C1 Ti1 C3 133.60(4) 2 .
C1 Ti1 C3 59.53(4) . .
C2 Ti1 C3 98.45(4) 2 .
C2 Ti1 C3 35.10(4) . .
C5 Ti1 C3 58.32(4) . .
C5 Ti1 C3 148.14(5) 2 .
C4 Ti1 C3 115.03(5) 2 .
C4 Ti1 C3 34.46(4) . .
C3 Ti1 C3 90.28(6) 2 .
C11 Si1 C12 108.46(8) . .
C11 Si1 C1 111.96(7) . .
C12 Si1 C1 112.55(7) . .
C11 Si1 C13 108.31(7) . .
C12 Si1 C13 108.26(7) . .
C1 Si1 C13 107.16(6) . .
C2 C1 C5 106.05(11) . .
C2 C1 Si1 123.06(10) . .
C5 C1 Si1 130.67(10) . .
C2 C1 Ti1 72.09(7) . .
C5 C1 Ti1 73.28(7) . .
Si1 C1 Ti1 123.58(6) . .
C3 C2 C1 108.72(11) . .
C3 C2 C6 125.72(12) . .
C1 C2 C6 125.23(12) . .
C3 C2 Ti1 75.58(7) . .
C1 C2 Ti1 71.31(7) . .
C6 C2 Ti1 124.39(9) . .
C4 C3 C2 108.03(11) . .
C4 C3 C7 124.32(12) . .
C2 C3 C7 127.06(12) . .
C4 C3 Ti1 72.37(7) . .
C2 C3 Ti1 69.32(7) . .
C7 C3 Ti1 130.81(9) . .
C3 C4 C5 109.13(11) . .
C3 C4 C8 124.75(13) . .
C5 C4 C8 125.97(13) . .
C3 C4 Ti1 73.17(7) . .
C5 C4 Ti1 70.99(7) . .
C8 C4 Ti1 125.52(10) . .
C4 C5 C1 108.04(11) . .
C4 C5 C9 123.58(12) . .
C1 C5 C9 127.56(12) . .
C4 C5 Ti1 74.11(7) . .
C1 C5 Ti1 70.22(7) . .
C9 C5 Ti1 129.53(10) . .
O1 C10 Ti1 180.0 . .
C18 C13 C14 116.98(13) . .
C18 C13 Si1 120.57(11) . .
C14 C13 Si1 122.44(11) . .
C15 C14 C13 121.35(16) . .
C16 C15 C14 120.24(16) . .
C15 C16 C17 119.67(15) . .
C16 C17 C18 120.09(16) . .
C17 C18 C13 121.67(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 C10 1.9786(19) .
Ti1 C1 2.3014(12) 2
Ti1 C1 2.3015(12) .
Ti1 C2 2.3118(12) 2
Ti1 C2 2.3119(12) .
Ti1 C5 2.3424(13) .
Ti1 C5 2.3424(13) 2
Ti1 C4 2.3828(13) 2
Ti1 C4 2.3829(13) .
Ti1 C3 2.3932(12) 2
Ti1 C3 2.3933(12) .
Si1 C11 1.8642(16) .
Si1 C12 1.8665(17) .
Si1 C1 1.8717(13) .
Si1 C13 1.8851(14) .
O1 C10 1.151(2) .
C1 C2 1.4488(17) .
C1 C5 1.4547(18) .
C2 C3 1.4209(17) .
C2 C6 1.4998(18) .
C3 C4 1.4149(18) .
C3 C7 1.5021(19) .
C4 C5 1.4175(18) .
C4 C8 1.5047(19) .
C5 C9 1.5012(19) .
C13 C18 1.396(2) .
C13 C14 1.399(2) .
C14 C15 1.392(2) .
C15 C16 1.376(3) .
C16 C17 1.380(2) .
C17 C18 1.387(2) .
