#------------------------------------------------------------------------------
#$Date: 2025-08-23 01:36:08 +0200 (Sat 23 de Aug de 2025) $
#$Revision: 301880 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/04/8100439.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_8100439
loop_
_publ_author_name
'Kempe, Rhett'
_publ_section_title
;
Crystal structure of dimethylamido-hexahydro-2-azepinato-bis
[2-(trimethylsilylamino)-4-methyl-pyridinato]-titanium(IV), 
C₂₆H₄₆N₆OSi₂Ti
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              467
_journal_page_last               468
_journal_volume                  218
_journal_year                    2003
_chemical_formula_sum            'C26 H46 N6 O Si2 Ti'
_chemical_formula_weight         562.77
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                91.820(14)
_cell_angle_beta                 102.600(15)
_cell_angle_gamma                112.81(2)
_cell_formula_units_Z            2
_cell_length_a                   10.178(2)
_cell_length_b                   10.906(2)
_cell_length_c                   16.254(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1609.4(5)
_diffrn_ambient_temperature      293(2)
_exptl_crystal_density_diffrn    1.161
_refine_ls_R_factor_obs          0.0457
_refine_ls_wR_factor_obs         0.1157
_cod_database_code               8100439
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
C1 C 0.2389(5) -0.3951(4) 0.8844(2) 0.0779(12) Uani 1 d . .
H1A H 0.2168(5) -0.4880(4) 0.8691(2) 0.117 Uiso 1 calc R .
H1B H 0.1701(5) -0.3880(4) 0.9144(2) 0.117 Uiso 1 calc R .
H1C H 0.3370(5) -0.3520(4) 0.9202(2) 0.117 Uiso 1 calc R .
C2 C 0.2682(4) -0.1324(3) 0.8162(2) 0.0663(10) Uani 1 d . .
H2A H 0.2613(4) -0.0894(3) 0.7657(2) 0.099 Uiso 1 calc R .
H2B H 0.3662(4) -0.0895(3) 0.8521(2) 0.099 Uiso 1 calc R .
H2C H 0.1993(4) -0.1253(3) 0.8461(2) 0.099 Uiso 1 calc R .
C3 C 0.0312(4) -0.3961(4) 0.7203(2) 0.0639(10) Uani 1 d . .
H3A H 0.0083(4) -0.4891(4) 0.7047(2) 0.096 Uiso 1 calc R .
H3B H 0.0206(4) -0.3537(4) 0.6698(2) 0.096 Uiso 1 calc R .
H3C H -0.0348(4) -0.3887(4) 0.7523(2) 0.096 Uiso 1 calc R .
C4 C 0.8948(4) 0.1784(4) 0.9446(3) 0.0884(13) Uani 1 d . .
H4A H 0.9662(4) 0.1451(4) 0.9364(3) 0.133 Uiso 1 calc R .
H4B H 0.8605(4) 0.1456(4) 0.9935(3) 0.133 Uiso 1 calc R .
H4C H 0.9392(4) 0.2746(4) 0.9534(3) 0.133 Uiso 1 calc R .
C5 C 0.8092(5) 0.1971(4) 0.7588(3) 0.0874(13) Uani 1 d . .
H5A H 0.8793(5) 0.1640(4) 0.7480(3) 0.131 Uiso 1 calc R .
H5B H 0.8563(5) 0.2928(4) 0.7733(3) 0.131 Uiso 1 calc R .
H5C H 0.7296(5) 0.1746(4) 0.7089(3) 0.131 Uiso 1 calc R .
C6 C 0.6015(5) 0.1860(4) 0.8675(3) 0.103(2) Uani 1 d . .
H6A H 0.5622(5) 0.1469(4) 0.9136(3) 0.154 Uiso 1 calc R .
H6B H 0.5229(5) 0.1638(4) 0.8171(3) 0.154 Uiso 1 calc R .
H6C H 0.6496(5) 0.2817(4) 0.8817(3) 0.154 Uiso 1 calc R .
C7 C 0.4250(3) -0.0986(3) 0.6006(2) 0.0452(8) Uani 1 d . .
C8 C 0.3226(4) -0.0500(3) 0.5434(2) 0.0557(9) Uani 1 d . .
H8A H 0.3442(4) -0.0437(3) 0.4880(2) 0.067 Uiso 1 calc R .
H8B H 0.3391(4) 0.0391(3) 0.5671(2) 0.067 Uiso 1 calc R .
C9 C 0.1627(4) -0.1429(4) 0.5329(2) 0.0642(10) Uani 1 d . .
H9A H 0.1020(4) -0.0954(4) 0.5112(2) 0.077 Uiso 1 calc R .
H9B H 0.1478(4) -0.1648(4) 0.5885(2) 0.077 Uiso 1 calc R .
C10 C 0.1103(4) -0.2728(4) 0.4741(2) 0.0699(11) Uani 1 d . .
H10A H 0.1217(4) -0.2509(4) 0.4180(2) 0.084 Uiso 1 calc R .
H10B H 0.0061(4) -0.3228(4) 0.4693(2) 0.084 Uiso 1 calc R .
C11 C 0.1904(4) -0.3632(4) 0.5021(2) 0.0686(11) Uani 1 d . .
H11A H 0.1447(4) -0.4453(4) 0.4627(2) 0.082 Uiso 1 calc R .
H11B H 0.1769(4) -0.3870(4) 0.5576(2) 0.082 Uiso 1 calc R .
C12 C 0.3553(4) -0.3018(4) 0.5072(2) 0.0640(10) Uani 1 d . .
H12A H 0.3890(4) -0.3735(4) 0.5052(2) 0.077 Uiso 1 calc R .
H12B H 0.3710(4) -0.2560(4) 0.4578(2) 0.077 Uiso 1 calc R .
C13 C 0.3612(3) -0.4326(3) 0.7047(2) 0.0398(7) Uani 1 d . .
C14 C 0.2633(3) -0.5684(3) 0.7001(2) 0.0444(8) Uani 1 d . .
H14 H 0.1758(3) -0.5890(3) 0.7164(2) 0.053 Uiso 1 calc R .
C15 C 0.2976(4) -0.6699(3) 0.6716(2) 0.0503(8) Uani 1 d . .
C16 C 0.4294(4) -0.6358(3) 0.6475(2) 0.0599(9) Uani 1 d . .
H16 H 0.4560(4) -0.7025(3) 0.6292(2) 0.072 Uiso 1 calc R .
C17 C 0.5192(4) -0.5038(3) 0.6511(2) 0.0553(9) Uani 1 d . .
H17 H 0.6065(4) -0.4822(3) 0.6345(2) 0.066 Uiso 1 calc R .
C18 C 0.6695(3) -0.1469(3) 0.8779(2) 0.0481(8) Uani 1 d . .
C19 C 0.6933(4) -0.1386(4) 0.9671(2) 0.0553(9) Uani 1 d . .
H19 H 0.7080(4) -0.0600(4) 0.9990(2) 0.066 Uiso 1 calc R .
C20 C 0.6944(4) -0.2494(4) 1.0068(2) 0.0594(9) Uani 1 d . .
C21 C 0.6688(4) -0.3651(4) 0.9570(2) 0.0673(10) Uani 1 d . .
H21 H 0.6700(4) -0.4401(4) 0.9823(2) 0.081 Uiso 1 calc R .
C22 C 0.6416(4) -0.3697(4) 0.8701(2) 0.0598(9) Uani 1 d . .
H22 H 0.6211(4) -0.4494(4) 0.8372(2) 0.072 Uiso 1 calc R .
C23 C 0.7540(4) -0.1998(4) 0.5962(2) 0.0784(12) Uani 1 d . .
H23A H 0.6589(4) -0.2327(4) 0.5568(2) 0.118 Uiso 1 calc R .
H23B H 0.7876(4) -0.2708(4) 0.6025(2) 0.118 Uiso 1 calc R .
H23C H 0.8223(4) -0.1272(4) 0.5752(2) 0.118 Uiso 1 calc R .
C24 C 0.8896(4) -0.1021(4) 0.7381(3) 0.0851(13) Uani 1 d . .
H24A H 0.8832(4) -0.0705(4) 0.7923(3) 0.128 Uiso 1 calc R .
H24B H 0.9577(4) -0.0297(4) 0.7168(3) 0.128 Uiso 1 calc R .
H24C H 0.9233(4) -0.1730(4) 0.7445(3) 0.128 Uiso 1 calc R .
C25 C 0.1951(4) -0.8155(3) 0.6666(2) 0.0677(10) Uani 1 d . .
H25A H 0.2365(4) -0.8718(3) 0.6455(2) 0.102 Uiso 1 calc R .
H25B H 0.1014(4) -0.8321(3) 0.6289(2) 0.102 Uiso 1 calc R .
H25C H 0.1823(4) -0.8351(3) 0.7222(2) 0.102 Uiso 1 calc R .
C26 C 0.7231(5) -0.2425(5) 1.1019(2) 0.0863(14) Uani 1 d . .
H26A H 0.7383(5) -0.1550(5) 1.1259(2) 0.129 Uiso 1 calc R .
H26B H 0.8093(5) -0.2592(5) 1.1240(2) 0.129 Uiso 1 calc R .
H26C H 0.6400(5) -0.3089(5) 1.1167(2) 0.129 Uiso 1 calc R .
N1 N 0.3519(3) -0.3191(2) 0.73312(14) 0.0410(6) Uani 1 d . .
N2 N 0.4861(3) -0.4040(2) 0.67764(15) 0.0440(6) Uani 1 d . .
N3 N 0.6613(3) -0.0535(3) 0.8251(2) 0.0464(6) Uani 1 d . .
N4 N 0.6439(3) -0.2627(3) 0.8317(2) 0.0499(7) Uani 1 d . .
N5 N 0.4443(3) -0.2068(3) 0.58398(15) 0.0474(7) Uani 1 d . .
N6 N 0.7436(3) -0.1528(3) 0.6781(2) 0.0545(7) Uani 1 d . .
O1 O 0.4977(2) -0.0349(2) 0.67562(13) 0.0512(6) Uani 1 d . .
Si1 Si 0.22513(10) -0.31194(9) 0.78646(5) 0.0439(2) Uani 1 d . .
Si2 Si 0.73619(11) 0.11950(10) 0.84857(6) 0.0552(3) Uani 1 d . .
Ti1 Ti 0.56550(6) -0.18936(5) 0.71353(3) 0.0408(2) Uani 1 d . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 Si1 1.863(4) . ?
C2 Si1 1.856(3) . ?
C3 Si1 1.872(4) . ?
C4 Si2 1.868(4) . ?
C5 Si2 1.860(4) . ?
C6 Si2 1.855(4) . ?
C7 O1 1.292(4) . ?
C7 N5 1.299(4) . ?
C7 C8 1.508(4) . ?
C7 Ti1 2.541(3) . ?
C8 C9 1.514(5) . ?
C9 C10 1.520(5) . ?
C10 C11 1.527(5) . ?
C11 C12 1.528(5) . ?
C12 N5 1.465(4) . ?
C13 N1 1.352(3) . ?
C13 N2 1.361(3) . ?
C13 C14 1.417(4) . ?
C13 Ti1 2.636(3) . ?
C14 C15 1.379(4) . ?
C15 C16 1.394(4) . ?
C15 C25 1.513(5) . ?
C16 C17 1.364(5) . ?
C17 N2 1.342(4) . ?
C18 N4 1.352(4) . ?
C18 N3 1.369(4) . ?
C18 C19 1.410(4) . ?
C18 Ti1 2.605(3) . ?
C19 C20 1.391(5) . ?
C20 C21 1.379(5) . ?
C20 C26 1.504(4) . ?
C21 C22 1.375(5) . ?
C22 N4 1.336(4) . ?
C23 N6 1.451(4) . ?
C24 N6 1.471(4) . ?
N1 Si1 1.727(2) . ?
N1 Ti1 2.185(2) . ?
N2 Ti1 2.171(3) . ?
N3 Si2 1.732(3) . ?
N3 Ti1 2.091(3) . ?
N4 Ti1 2.211(3) . ?
N5 Ti1 2.157(3) . ?
N6 Ti1 1.920(3) . ?
O1 Ti1 2.115(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139206114
