#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:20:08 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179372 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/69/4326999.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_4326999
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            'C44 H54 N6 Si2 Ti2'
_chemical_formula_weight         818.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 133.6060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.0630(2)
_cell_length_b                   12.8160(2)
_cell_length_c                   18.0421(3)
_cell_measurement_reflns_used    41005
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.2
_cell_measurement_theta_min      3.78
_cell_volume                     2187.16(7)
_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 0.934
_diffrn_measured_fraction_theta_max 0.934
_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  0.0990
_diffrn_reflns_av_sigmaI/netI    0.0947
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            41005
_diffrn_reflns_theta_full        30.20
_diffrn_reflns_theta_max         30.20
_diffrn_reflns_theta_min         3.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.9142
_exptl_absorpt_correction_T_min  0.8943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         6078
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1244
_refine_ls_R_factor_gt           0.0527
_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)+(0.0692P)²+0.0352P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                3593
_reflns_number_total             6078
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2015644_si_003_01.cif
_cod_data_source_block           1
_cod_original_cell_volume        2187.16(6)
_cod_database_code               4326999
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
Ti1 Ti 0.47949(4) 0.03457(3) 0.06292(3) 0.02173(13) Uani 1 1 d .
Si1 Si 0.75455(6) 0.14331(5) 0.12378(4) 0.02347(16) Uani 1 1 d .
N1 N 0.38312(19) 0.16069(15) 0.03826(14) 0.0293(4) Uani 1 1 d .
N2 N 0.53695(19) -0.03376(14) 0.17935(13) 0.0265(4) Uani 1 1 d .
N3 N 0.62116(18) 0.05138(13) 0.05854(12) 0.0228(4) Uani 1 1 d .
C1 C 0.3111(3) 0.2217(2) -0.05481(19) 0.0413(6) Uani 1 1 d .
H1A H 0.2119 0.2315 -0.0903 0.062 Uiso 1 1 calc R
H1B H 0.3161 0.1846 -0.0997 0.062 Uiso 1 1 calc R
H1C H 0.3570 0.2899 -0.0367 0.062 Uiso 1 1 calc R
C2 C 0.3639(3) 0.2073(2) 0.10168(19) 0.0427(6) Uani 1 1 d .
H2A H 0.3921 0.2809 0.1142 0.064 Uiso 1 1 calc R
H2B H 0.4224 0.1702 0.1671 0.064 Uiso 1 1 calc R
H2C H 0.2642 0.2023 0.0664 0.064 Uiso 1 1 calc R
C3 C 0.4260(3) -0.0627(2) 0.17543(18) 0.0380(6) Uani 1 1 d .
H3A H 0.4264 -0.1385 0.1827 0.057 Uiso 1 1 calc R
H3B H 0.3342 -0.0410 0.1097 0.057 Uiso 1 1 calc R
H3C H 0.4423 -0.0282 0.2313 0.057 Uiso 1 1 calc R
C4 C 0.6745(3) -0.0676(2) 0.27380(19) 0.0444(7) Uani 1 1 d .
H4A H 0.6946 -0.0353 0.3320 0.067 Uiso 1 1 calc R
H4B H 0.7468 -0.0466 0.2741 0.067 Uiso 1 1 calc R
H4C H 0.6750 -0.1437 0.2793 0.067 Uiso 1 1 calc R
C11 C 0.6889(2) 0.27513(17) 0.06165(16) 0.0254(5) Uani 1 1 d .
C12 C 0.5797(3) 0.28483(19) -0.04478(17) 0.0339(6) Uani 1 1 d .
H12 H 0.5352 0.2238 -0.0856 0.041 Uiso 1 1 calc R
C13 C 0.5354(3) 0.3816(2) -0.0917(2) 0.0443(7) Uani 1 1 d .
H13 H 0.4615 0.3864 -0.1641 0.053 Uiso 1 1 calc R
C14 C 0.5983(3) 0.4714(2) -0.0337(2) 0.0435(7) Uani 1 1 d .
H14 H 0.5680 0.5378 -0.0660 0.052 Uiso 1 1 calc R
C15 C 0.7050(3) 0.46411(19) 0.0711(2) 0.0421(6) Uani 1 1 d .
H15 H 0.7483 0.5256 0.1114 0.050 Uiso 1 1 calc R
C16 C 0.7493(2) 0.36690(19) 0.11795(18) 0.0355(6) Uani 1 1 d .
H16 H 0.8228 0.3630 0.1904 0.043 Uiso 1 1 calc R
C21 C 0.8370(2) 0.15432(18) 0.25970(15) 0.0268(5) Uani 1 1 d .
C22 C 0.7685(3) 0.20343(19) 0.28424(18) 0.0366(6) Uani 1 1 d .
H22 H 0.6813 0.2381 0.2322 0.044 Uiso 1 1 calc R
C23 C 0.8262(3) 0.2025(2) 0.3842(2) 0.0470(7) Uani 1 1 d .
H23 H 0.7780 0.2361 0.3996 0.056 Uiso 1 1 calc R
C24 C 0.9530(3) 0.1527(2) 0.46052(19) 0.0476(7) Uani 1 1 d .
H24 H 0.9923 0.1520 0.5286 0.057 Uiso 1 1 calc R
C25 C 1.0222(3) 0.1043(2) 0.43781(18) 0.0464(7) Uani 1 1 d .
H25 H 1.1097 0.0701 0.4904 0.056 Uiso 1 1 calc R
C26 C 0.9657(2) 0.1048(2) 0.33905(17) 0.0362(6) Uani 1 1 d .
H26 H 1.0152 0.0710 0.3247 0.043 Uiso 1 1 calc R
C31 C 0.8986(2) 0.10378(19) 0.12990(16) 0.0287(5) Uani 1 1 d .
C32 C 0.9999(3) 0.1765(2) 0.1581(2) 0.0509(8) Uani 1 1 d .
H32 H 0.9932 0.2464 0.1718 0.061 Uiso 1 1 calc R
C33 C 1.1097(3) 0.1487(3) 0.1664(3) 0.0682(10) Uani 1 1 d .
H33 H 1.1780 0.1993 0.1865 0.082 Uiso 1 1 calc R
C34 C 1.1206(3) 0.0487(3) 0.1459(2) 0.0625(10) Uani 1 1 d .
H34 H 1.1957 0.0304 0.1510 0.075 Uiso 1 1 calc R
C35 C 1.0233(3) -0.0250(3) 0.1180(2) 0.0522(8) Uani 1 1 d .
H35 H 1.0302 -0.0943 0.1032 0.063 Uiso 1 1 calc R
C36 C 0.9135(2) 0.0027(2) 0.11152(18) 0.0411(6) Uani 1 1 d .
H36 H 0.8479 -0.0491 0.0941 0.049 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
N2 Ti1 N1 110.19(8) . .
N2 Ti1 N3 116.31(8) . .
N1 Ti1 N3 113.35(8) . .
N2 Ti1 N3 115.63(8) . 3_655
N1 Ti1 N3 113.21(7) . 3_655
N3 Ti1 N3 86.49(7) . 3_655
N2 Ti1 Ti1 126.95(6) . 3_655
N1 Ti1 Ti1 122.85(6) . 3_655
N3 Ti1 Ti1 43.57(5) . 3_655
N3 Ti1 Ti1 42.92(5) 3_655 3_655
N3 Si1 C11 112.12(9) . .
N3 Si1 C31 110.82(10) . .
C11 Si1 C31 107.74(10) . .
N3 Si1 C21 109.91(9) . .
C11 Si1 C21 109.00(10) . .
C31 Si1 C21 107.09(10) . .
C2 N1 C1 111.05(19) . .
C2 N1 Ti1 127.50(16) . .
C1 N1 Ti1 121.39(15) . .
C4 N2 C3 111.60(18) . .
C4 N2 Ti1 131.79(16) . .
C3 N2 Ti1 116.56(14) . .
Si1 N3 Ti1 126.68(10) . .
Si1 N3 Ti1 137.40(11) . 3_655
Ti1 N3 Ti1 93.51(7) . 3_655
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 . .
C16 C11 C12 117.1(2) . .
C16 C11 Si1 122.01(16) . .
C12 C11 Si1 120.87(17) . .
C13 C12 C11 121.3(2) . .
C13 C12 H12 119.4 . .
C11 C12 H12 119.4 . .
C14 C13 C12 120.3(2) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
C15 C14 C13 119.7(2) . .
C15 C14 H14 120.2 . .
C13 C14 H14 120.2 . .
C14 C15 C16 120.0(2) . .
C14 C15 H15 120.0 . .
C16 C15 H15 120.0 . .
C15 C16 C11 121.7(2) . .
C15 C16 H16 119.1 . .
C11 C16 H16 119.1 . .
C22 C21 C26 117.5(2) . .
C22 C21 Si1 122.14(17) . .
C26 C21 Si1 120.15(18) . .
C21 C22 C23 121.0(2) . .
C21 C22 H22 119.5 . .
C23 C22 H22 119.5 . .
C24 C23 C22 120.1(3) . .
C24 C23 H23 120.0 . .
C22 C23 H23 120.0 . .
C25 C24 C23 119.7(2) . .
C25 C24 H24 120.1 . .
C23 C24 H24 120.1 . .
C24 C25 C26 120.5(2) . .
C24 C25 H25 119.7 . .
C26 C25 H25 119.7 . .
C25 C26 C21 121.2(2) . .
C25 C26 H26 119.4 . .
C21 C26 H26 119.4 . .
C36 C31 C32 117.2(2) . .
C36 C31 Si1 122.64(18) . .
C32 C31 Si1 120.09(19) . .
C33 C32 C31 121.3(3) . .
C33 C32 H32 119.3 . .
C31 C32 H32 119.3 . .
C34 C33 C32 120.4(3) . .
C34 C33 H33 119.8 . .
C32 C33 H33 119.8 . .
C33 C34 C35 120.1(3) . .
C33 C34 H34 119.9 . .
C35 C34 H34 119.9 . .
C34 C35 C36 119.5(3) . .
C34 C35 H35 120.2 . .
C36 C35 H35 120.2 . .
C31 C36 C35 121.4(3) . .
C31 C36 H36 119.3 . .
C35 C36 H36 119.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N2 1.8889(18) .
Ti1 N1 1.9034(19) .
Ti1 N3 1.9182(18) .
Ti1 N3 1.9416(17) 3_655
Ti1 Ti1 2.8115(7) 3_655
Si1 N3 1.7265(18) .
Si1 C11 1.876(2) .
Si1 C31 1.878(2) .
Si1 C21 1.884(2) .
N1 C2 1.458(3) .
N1 C1 1.462(3) .
N2 C4 1.448(3) .
N2 C3 1.450(3) .
N3 Ti1 1.9416(17) 3_655
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 .
C11 C16 1.390(3) .
C11 C12 1.400(3) .
C12 C13 1.384(3) .
C12 H12 0.9500 .
C13 C14 1.381(4) .
C13 H13 0.9500 .
C14 C15 1.375(4) .
C14 H14 0.9500 .
C15 C16 1.388(3) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C21 C22 1.392(3) .
C21 C26 1.400(3) .
C22 C23 1.395(3) .
C22 H22 0.9500 .
C23 C24 1.378(4) .
C23 H23 0.9500 .
C24 C25 1.371(4) .
C24 H24 0.9500 .
C25 C26 1.381(3) .
C25 H25 0.9500 .
C26 H26 0.9500 .
C31 C36 1.384(4) .
C31 C32 1.396(3) .
C32 C33 1.382(4) .
C32 H32 0.9500 .
C33 C34 1.368(5) .
C33 H33 0.9500 .
C34 C35 1.371(4) .
C34 H34 0.9500 .
C35 C36 1.402(4) .
C35 H35 0.9500 .
C36 H36 0.9500 .
