#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:21:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179373 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/70/4327003.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_4327003
loop_
_publ_author_name
'Samuel D. Cosham'
'Andrew L. Johnson'
'Kieran C. Molloy'
'Andrew J. Kingsley'
_publ_contact_author_address
;
Department of Chemistry,
University of Bath.
Claverton Down.
Bath.
BA2 7AY
United Kingdon
;
_publ_contact_author_email       a.l.johnson@bath.ac.uk
_publ_contact_author_fax         '+44 (0) 1225 386231'
_publ_contact_author_name
;
Dr. Andrew L. Johnson and Prof. Kieran C. Molloy
;
_publ_contact_author_phone       '+44 (0) 1225 384467'
_publ_section_title
;
 Synthesis, Characterization, and Materials Chemistry of Group 4
 Silylimides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12053
_journal_page_last               12063
_journal_paper_doi               10.1021/ic2015644
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C20 H54 N6 Si2 Ti2'
_chemical_formula_weight         530.67
_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                 91.0290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.9270(2)
_cell_length_b                   13.3320(3)
_cell_length_c                   11.6030(3)
_cell_measurement_reflns_used    32777
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      7.86
_cell_volume                     1535.37(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Kappa CCD'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP 3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker Kappa CCD Diffractometer'
_diffrn_measurement_method       'omega and 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  0.0926
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            32777
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         7.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.9411
_exptl_absorpt_correction_T_min  0.9134
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         4571
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0412P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                3103
_reflns_number_total             4571
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2015644_si_003_05.cif
_cod_data_source_block           7
_cod_database_code               4327003
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
Ti1 Ti 0.09663(3) -0.008993(19) 0.08890(2) 0.02307(9) Uani 1 1 d .
Si1 Si 0.15533(4) 0.18246(3) -0.07680(3) 0.02346(11) Uani 1 1 d .
N3 N 0.05151(12) 0.08782(9) -0.02669(10) 0.0234(3) Uani 1 1 d .
N1 N 0.08342(14) 0.03812(9) 0.24268(11) 0.0298(3) Uani 1 1 d .
N2 N 0.26755(13) -0.07150(9) 0.06803(11) 0.0301(3) Uani 1 1 d .
C1 C 0.0455(2) 0.13629(14) 0.28513(16) 0.0445(4) Uani 1 1 d .
H1A H -0.0386 0.1309 0.3277 0.067 Uiso 1 1 calc R
H1B H 0.0324 0.1822 0.2199 0.067 Uiso 1 1 calc R
H1C H 0.1169 0.1621 0.3364 0.067 Uiso 1 1 calc R
C2 C 0.1076(3) -0.03146(15) 0.33774(16) 0.0525(5) Uani 1 1 d .
H2A H 0.1790 -0.0049 0.3886 0.079 Uiso 1 1 calc R
H2B H 0.1354 -0.0966 0.3071 0.079 Uiso 1 1 calc R
H2C H 0.0247 -0.0396 0.3814 0.079 Uiso 1 1 calc R
C3 C 0.38217(18) -0.07320(14) 0.14748(17) 0.0442(4) Uani 1 1 d .
H3A H 0.4069 -0.1429 0.1645 0.066 Uiso 1 1 calc R
H3B H 0.3584 -0.0390 0.2191 0.066 Uiso 1 1 calc R
H3C H 0.4586 -0.0388 0.1125 0.066 Uiso 1 1 calc R
C4 C 0.29762(18) -0.12390(15) -0.03854(16) 0.0434(4) Uani 1 1 d .
H4A H 0.3748 -0.0919 -0.0752 0.065 Uiso 1 1 calc R
H4B H 0.2191 -0.1209 -0.0908 0.065 Uiso 1 1 calc R
H4C H 0.3192 -0.1941 -0.0214 0.065 Uiso 1 1 calc R
C15 C 0.29824(17) 0.20307(13) 0.02768(15) 0.0369(4) Uani 1 1 d .
H15A H 0.2628 0.2251 0.1018 0.055 Uiso 1 1 calc R
H15B H 0.3586 0.2546 -0.0024 0.055 Uiso 1 1 calc R
H15C H 0.3482 0.1403 0.0384 0.055 Uiso 1 1 calc R
C16 C 0.22780(18) 0.14689(14) -0.21860(15) 0.0387(4) Uani 1 1 d .
H16A H 0.2741 0.0822 -0.2112 0.058 Uiso 1 1 calc R
H16B H 0.2921 0.1983 -0.2424 0.058 Uiso 1 1 calc R
H16C H 0.1552 0.1414 -0.2766 0.058 Uiso 1 1 calc R
C11 C 0.05610(16) 0.30372(11) -0.09149(13) 0.0280(3) Uani 1 1 d .
C13 C 0.14940(19) 0.38904(12) -0.12992(15) 0.0388(4) Uani 1 1 d .
H13A H 0.0968 0.4507 -0.1404 0.058 Uiso 1 1 calc R
H13B H 0.1912 0.3708 -0.2029 0.058 Uiso 1 1 calc R
H13C H 0.2197 0.4000 -0.0709 0.058 Uiso 1 1 calc R
C12 C -0.05708(19) 0.29179(13) -0.18211(16) 0.0395(4) Uani 1 1 d .
H12A H -0.1183 0.2382 -0.1584 0.059 Uiso 1 1 calc R
H12B H -0.0182 0.2746 -0.2566 0.059 Uiso 1 1 calc R
H12C H -0.1072 0.3549 -0.1893 0.059 Uiso 1 1 calc R
C14 C -0.0062(2) 0.33273(13) 0.02333(16) 0.0420(4) Uani 1 1 d .
H14A H -0.0572 0.3953 0.0138 0.063 Uiso 1 1 calc R
H14B H 0.0654 0.3423 0.0815 0.063 Uiso 1 1 calc R
H14C H -0.0669 0.2793 0.0482 0.063 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'
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 N3 114.67(5) . .
N1 Ti1 N2 109.88(6) . .
N3 Ti1 N2 113.81(5) . .
N1 Ti1 N3 117.72(5) . 3
N3 Ti1 N3 86.45(5) . 3
N2 Ti1 N3 112.73(5) . 3
N1 Ti1 Ti1 127.28(4) . 3
N3 Ti1 Ti1 43.61(4) . 3
N2 Ti1 Ti1 122.82(4) . 3
N3 Ti1 Ti1 42.84(4) 3 3
N3 Si1 C16 110.53(7) . .
N3 Si1 C15 109.74(7) . .
C16 Si1 C15 107.97(8) . .
N3 Si1 C11 109.80(6) . .
C16 Si1 C11 110.14(8) . .
C15 Si1 C11 108.63(8) . .
Si1 N3 Ti1 126.41(7) . .
Si1 N3 Ti1 136.14(7) . 3
Ti1 N3 Ti1 93.55(5) . 3
C1 N1 C2 110.95(14) . .
C1 N1 Ti1 129.82(11) . .
C2 N1 Ti1 119.17(11) . .
C3 N2 C4 111.20(14) . .
C3 N2 Ti1 127.90(11) . .
C4 N2 Ti1 120.89(10) . .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
N2 C3 H3A 109.5 . .
N2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
N2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
N2 C4 H4A 109.5 . .
N2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
N2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Si1 C15 H15A 109.5 . .
Si1 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
Si1 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
Si1 C16 H16A 109.5 . .
Si1 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
Si1 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C14 C11 C12 108.71(14) . .
C14 C11 C13 108.71(13) . .
C12 C11 C13 108.40(13) . .
C14 C11 Si1 110.76(11) . .
C12 C11 Si1 110.23(10) . .
C13 C11 Si1 109.97(11) . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C14 H14A 109.5 . .
C11 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C11 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N1 1.8984(13) .
Ti1 N3 1.9089(12) .
Ti1 N2 1.9096(13) .
Ti1 N3 1.9365(12) 3
Ti1 Ti1 2.8022(5) 3
Si1 N3 1.7360(12) .
Si1 C16 1.8687(17) .
Si1 C15 1.8698(16) .
Si1 C11 1.8992(16) .
N3 Ti1 1.9365(12) 3
N1 C1 1.451(2) .
N1 C2 1.458(2) .
N2 C3 1.452(2) .
N2 C4 1.456(2) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C11 C14 1.529(2) .
C11 C12 1.533(2) .
C11 C13 1.538(2) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
