#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:28:50 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179921 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/16/7021664.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_7021664
loop_
_publ_author_name
'Lorber, Christian'
'Vendier, Laure'
_publ_section_title
;
 Novel aspects of the transamination reaction between Ti(NMe2)4 and
 primary amines.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12203
_journal_page_last               12219
_journal_paper_doi               10.1039/c3dt50840d
_journal_volume                  42
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C44 H54 N6 Si2 Ti2'
_chemical_formula_sum            'C44 H54 N6 Si2 Ti2'
_chemical_formula_weight         818.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 108.955(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8129(18)
_cell_length_b                   15.846(3)
_cell_length_c                   11.4001(17)
_cell_measurement_reflns_used    2400
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_measurement_wavelength     0.71073
_cell_volume                     2189.1(6)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       φ
_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  0.2704
_diffrn_reflns_av_unetI/netI     0.3163
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14897
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_time  4
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
        (See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.777
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.777
_refine_ls_R_factor_all          0.2369
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1539
_reflns_number_gt                1084
_reflns_number_total             3712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50840d.txt
_cod_data_source_block           3
_cod_database_code               7021664
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.8037(7) -0.0333(6) 0.5192(7) 0.053(2) Uani 1 1 d .
C2 C 0.7950(9) -0.1213(6) 0.5213(9) 0.058(3) Uani 1 1 d .
H2 H 0.7606 -0.1468 0.5725 0.07 Uiso 1 1 calc R
C3 C 0.8385(10) -0.1714(7) 0.4457(9) 0.069(3) Uani 1 1 d .
H3 H 0.8322 -0.2298 0.4475 0.083 Uiso 1 1 calc R
C4 C 0.8891(9) -0.1358(8) 0.3710(9) 0.069(3) Uani 1 1 d .
H4 H 0.9195 -0.1698 0.3239 0.082 Uiso 1 1 calc R
C5 C 0.8958(9) -0.0500(9) 0.3645(8) 0.071(3) Uani 1 1 d .
H5 H 0.9281 -0.026 0.3102 0.086 Uiso 1 1 calc R
C6 C 0.8542(8) 0.0029(6) 0.4392(8) 0.058(2) Uani 1 1 d .
H6 H 0.8604 0.0613 0.4352 0.07 Uiso 1 1 calc R
C7 C 0.7908(8) 0.1434(6) 0.6289(8) 0.056(2) Uani 1 1 d .
C8 C 0.7577(9) 0.1983(6) 0.5261(8) 0.063(3) Uani 1 1 d .
H8 H 0.7156 0.1773 0.4491 0.075 Uiso 1 1 calc R
C9 C 0.7873(10) 0.2842(6) 0.5379(11) 0.074(3) Uani 1 1 d .
H9 H 0.7618 0.3195 0.4694 0.088 Uiso 1 1 calc R
C10 C 0.8533(9) 0.3169(7) 0.6492(10) 0.065(3) Uani 1 1 d .
H10 H 0.8741 0.3734 0.6562 0.078 Uiso 1 1 calc R
C11 C 0.8871(10) 0.2647(7) 0.7478(10) 0.067(3) Uani 1 1 d .
H11 H 0.9316 0.2859 0.8236 0.081 Uiso 1 1 calc R
C12 C 0.8570(8) 0.1796(6) 0.7393(9) 0.058(3) Uani 1 1 d .
H12 H 0.8821 0.146 0.8098 0.07 Uiso 1 1 calc R
C13 C 0.7912(7) -0.0146(6) 0.7792(7) 0.049(2) Uani 1 1 d .
C14 C 0.7346(8) 0.0043(6) 0.8639(8) 0.057(2) Uani 1 1 d .
H14 H 0.6742 0.0405 0.8399 0.068 Uiso 1 1 calc R
C15 C 0.7678(9) -0.0305(6) 0.9827(7) 0.062(3) Uani 1 1 d .
H15 H 0.727 -0.0192 1.0351 0.074 Uiso 1 1 calc R
C16 C 0.8600(9) -0.0812(6) 1.0240(7) 0.064(3) Uani 1 1 d .
H16 H 0.8825 -0.1032 1.104 0.077 Uiso 1 1 calc R
C17 C 0.9182(9) -0.0987(6) 0.9437(7) 0.061(3) Uani 1 1 d .
H17 H 0.9803 -0.1331 0.9694 0.073 Uiso 1 1 calc R
C18 C 0.8838(7) -0.0650(6) 0.8245(7) 0.056(2) Uani 1 1 d .
H18 H 0.9251 -0.0769 0.7728 0.067 Uiso 1 1 calc R
C19 C 0.5793(10) 0.0882(6) 0.1872(9) 0.070(3) Uani 1 1 d .
H19A H 0.5356 0.074 0.1039 0.105 Uiso 1 1 calc R
H19B H 0.6562 0.0838 0.1959 0.105 Uiso 1 1 calc R
H19C H 0.5631 0.145 0.2051 0.105 Uiso 1 1 calc R
C20 C 0.5731(8) -0.0575(6) 0.2459(7) 0.059(2) Uani 1 1 d .
H20A H 0.6494 -0.0646 0.2537 0.088 Uiso 1 1 calc R
H20B H 0.528 -0.0708 0.1627 0.088 Uiso 1 1 calc R
H20C H 0.5545 -0.0944 0.3028 0.088 Uiso 1 1 calc R
C21 C 0.3795(8) 0.2066(6) 0.2782(8) 0.056(2) Uani 1 1 d .
H21A H 0.417 0.2516 0.2522 0.084 Uiso 1 1 calc R
H21B H 0.3137 0.228 0.2903 0.084 Uiso 1 1 calc R
H21C H 0.3604 0.1634 0.2158 0.084 Uiso 1 1 calc R
C22 C 0.4769(10) 0.2347(6) 0.4937(8) 0.065(3) Uani 1 1 d .
H22A H 0.4101 0.2504 0.5089 0.097 Uiso 1 1 calc R
H22B H 0.5087 0.2835 0.4687 0.097 Uiso 1 1 calc R
H22C H 0.5282 0.2117 0.5681 0.097 Uiso 1 1 calc R
N1 N 0.5998(6) 0.0274(4) 0.5624(5) 0.0464(17) Uani 1 1 d .
N2 N 0.5535(6) 0.0302(4) 0.2740(6) 0.0487(18) Uani 1 1 d .
N3 N 0.4520(6) 0.1710(4) 0.3949(6) 0.0508(19) Uani 1 1 d .
Si1 Si 0.7421(2) 0.03131(15) 0.6188(2) 0.0474(6) Uani 1 1 d .
Ti1 Ti 0.49811(14) 0.05709(10) 0.40428(13) 0.0450(4) Uani 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 0 '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
C2 C1 C6 118.4(9) . .
C2 C1 Si1 118.7(8) . .
C6 C1 Si1 122.9(7) . .
C1 C2 C3 120.0(10) . .
C4 C3 C2 121.0(10) . .
C3 C4 C5 120.1(11) . .
C4 C5 C6 120.9(10) . .
C1 C6 C5 119.5(10) . .
C12 C7 C8 115.3(9) . .
C12 C7 Si1 122.6(7) . .
C8 C7 Si1 122.0(7) . .
C9 C8 C7 121.2(9) . .
C10 C9 C8 121.1(10) . .
C11 C10 C9 118.2(9) . .
C10 C11 C12 121.8(9) . .
C7 C12 C11 122.3(9) . .
C18 C13 C14 115.7(7) . .
C18 C13 Si1 124.3(7) . .
C14 C13 Si1 120.0(7) . .
C15 C14 C13 121.2(9) . .
C16 C15 C14 121.3(9) . .
C15 C16 C17 118.5(8) . .
C16 C17 C18 120.1(9) . .
C13 C18 C17 123.2(9) . .
Si1 N1 Ti1 131.1(4) . .
Si1 N1 Ti1 128.3(4) . 3_656
Ti1 N1 Ti1 93.9(3) . 3_656
C20 N2 C19 110.8(7) . .
C20 N2 Ti1 121.3(5) . .
C19 N2 Ti1 127.8(6) . .
C21 N3 C22 110.4(7) . .
C21 N3 Ti1 120.8(5) . .
C22 N3 Ti1 128.7(6) . .
N1 Si1 C7 110.3(4) . .
N1 Si1 C13 109.2(4) . .
C7 Si1 C13 108.0(4) . .
N1 Si1 C1 110.7(3) . .
C7 Si1 C1 110.9(4) . .
C13 Si1 C1 107.7(4) . .
N2 Ti1 N3 111.1(3) . .
N2 Ti1 N1 111.8(3) . .
N3 Ti1 N1 113.2(3) . .
N2 Ti1 N1 115.3(3) . 3_656
N3 Ti1 N1 117.1(3) . 3_656
N1 Ti1 N1 86.1(3) . 3_656
N2 Ti1 Ti1 123.1(2) . 3_656
N3 Ti1 Ti1 125.6(2) . 3_656
N1 Ti1 Ti1 43.7(2) . 3_656
N1 Ti1 Ti1 42.41(17) 3_656 3_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.400(14) .
C1 C6 1.401(13) .
C1 Si1 1.883(10) .
C2 C3 1.413(14) .
C3 C4 1.350(16) .
C4 C5 1.366(16) .
C5 C6 1.417(14) .
C7 C12 1.393(13) .
C7 C8 1.409(13) .
C7 Si1 1.873(10) .
C8 C9 1.409(13) .
C9 C10 1.377(14) .
C10 C11 1.349(14) .
C11 C12 1.396(14) .
C13 C18 1.384(12) .
C13 C14 1.414(13) .
C13 Si1 1.876(8) .
C14 C15 1.395(11) .
C15 C16 1.378(13) .
C16 C17 1.384(13) .
C17 C18 1.392(11) .
C19 N2 1.465(11) .
C20 N2 1.465(11) .
C21 N3 1.465(10) .
C22 N3 1.467(11) .
N1 Si1 1.726(7) .
N1 Ti1 1.908(6) .
N1 Ti1 1.954(7) 3_656
N2 Ti1 1.892(7) .
N3 Ti1 1.892(7) .
Ti1 N1 1.954(7) 3_656
Ti1 Ti1 2.823(3) 3_656
