#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/52/2205279.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2205279
loop_
_publ_author_name
'Xia Chen'
'Li Wang'
'Jian-Ping Guo'
'Shu-Ping Huang'
'Dian-Sheng Liu'
_publ_section_title
catena-Poly[lithium(I)-μ-1-tert-butyl-3-(3-pyridyl)-N,N'-bis(trimethylsilyl)propane-1,3-diiminato]
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m574
_journal_page_last               m576
_journal_paper_doi               10.1107/S1600536805005210
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Li (C18 H32 N3 Si2)]'
_chemical_formula_moiety         'C18 H32 Li N3 Si2'
_chemical_formula_sum            'C18 H32 Li N3 Si2'
_chemical_formula_weight         353.59
_chemical_name_systematic
;
catena-Poly[lithium(I)-μ-1-tert-butyl-3-(3-pyridyl)-N,N'-bis(trimethylsilyl)
propane-1,3-diiminato]
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 115.690(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.398(4)
_cell_length_b                   18.283(6)
_cell_length_c                   11.659(4)
_cell_measurement_reflns_used    1413
_cell_measurement_temperature    190(2)
_cell_measurement_theta_max      27.448
_cell_measurement_theta_min      2.440
_cell_volume                     2189.5(13)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      190(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SMART CCD area-detector'
_diffrn_measurement_method       ω
_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  0.0675
_diffrn_reflns_av_sigmaI/netI    0.1460
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8928
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.09
_diffrn_standards_decay_%        2.02
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  0.9676
_exptl_absorpt_correction_T_min  0.9519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2000)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.838
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0545
_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)+(0.0002P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0654
_reflns_number_gt                1749
_reflns_number_total             3845
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg6142.cif
_cod_data_source_block           I
_cod_original_cell_volume        2189.3(13)
_cod_original_sg_symbol_Hall     '-p 2yn'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2205279
_cod_database_fobs_code          2205279
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_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Li1 0.2564(5) 0.1267(3) 0.1526(5) 0.0459(15) Uani d . 1 Li
N1 0.4210(2) 0.17438(14) 0.2474(2) 0.0377(7) Uani d . 1 N
N2 0.1504(2) 0.16677(14) 0.2309(2) 0.0353(7) Uani d . 1 N
N3 0.6729(2) 0.36768(14) 0.4593(2) 0.0385(7) Uani d . 1 N
Si1 0.56233(9) 0.12539(6) 0.29166(9) 0.0467(3) Uani d . 1 Si
Si2 0.07108(9) 0.09181(5) 0.24724(8) 0.0430(3) Uani d . 1 Si
C1 0.1662(3) 0.23808(18) 0.2450(3) 0.0350(8) Uani d . 1 C
C2 0.0588(3) 0.28644(17) 0.2567(3) 0.0417(9) Uani d . 1 C
C3 0.0292(3) 0.25756(18) 0.3642(3) 0.0653(11) Uani d . 1 C
H3A 0.1076 0.2573 0.4422 0.098 Uiso calc R 1 H
H3B -0.0045 0.2087 0.3445 0.098 Uiso calc R 1 H
H3C -0.0342 0.2885 0.3734 0.098 Uiso calc R 1 H
C4 -0.0645(3) 0.28363(17) 0.1307(3) 0.0651(12) Uani d . 1 C
H4A -0.1332 0.3098 0.1394 0.098 Uiso calc R 1 H
H4B -0.0903 0.2336 0.1089 0.098 Uiso calc R 1 H
H4C -0.0475 0.3057 0.0647 0.098 Uiso calc R 1 H
C5 0.0958(3) 0.36687(17) 0.2870(3) 0.0638(11) Uani d . 1 C
H5A 0.1748 0.3704 0.3642 0.096 Uiso calc R 1 H
H5B 0.0272 0.3921 0.2975 0.096 Uiso calc R 1 H
H5C 0.1086 0.3887 0.2184 0.096 Uiso calc R 1 H
C6 0.2771(3) 0.27347(16) 0.2483(3) 0.0356(9) Uani d . 1 C
H6 0.2715 0.3242 0.2414 0.043 Uiso calc R 1 H
C7 0.3946(3) 0.24312(19) 0.2606(3) 0.0365(9) Uani d . 1 C
C8 0.5032(3) 0.29881(17) 0.2925(3) 0.0346(8) Uani d . 1 C
C9 0.5437(3) 0.32449(18) 0.2059(3) 0.0499(10) Uani d . 1 C
H9 0.5012 0.3101 0.1212 0.060 Uiso calc R 1 H
C10 0.6478(3) 0.3719(2) 0.2444(3) 0.0545(11) Uani d . 1 C
H10 0.6760 0.3907 0.1865 0.065 Uiso calc R 1 H
C11 0.7090(3) 0.39061(17) 0.3714(3) 0.0438(9) Uani d . 1 C
H11 0.7807 0.4215 0.3974 0.053 Uiso calc R 1 H
C12 0.5688(3) 0.32324(16) 0.4169(3) 0.0370(9) Uani d . 1 C
H12 0.5386 0.3077 0.4752 0.044 Uiso calc R 1 H
C13 0.7211(3) 0.17301(18) 0.3567(3) 0.0918(14) Uani d . 1 C
H13A 0.7247 0.2051 0.2932 0.138 Uiso calc R 1 H
H13B 0.7899 0.1376 0.3806 0.138 Uiso calc R 1 H
H13C 0.7311 0.2010 0.4301 0.138 Uiso calc R 1 H
C14 0.5697(3) 0.0622(2) 0.4179(3) 0.1032(16) Uani d . 1 C
H14A 0.5802 0.0897 0.4918 0.155 Uiso calc R 1 H
H14B 0.6422 0.0296 0.4393 0.155 Uiso calc R 1 H
H14C 0.4906 0.0344 0.3881 0.155 Uiso calc R 1 H
C15 0.5462(3) 0.07068(18) 0.1524(3) 0.0810(13) Uani d . 1 C
H15A 0.4673 0.0426 0.1222 0.121 Uiso calc R 1 H
H15B 0.6193 0.0383 0.1766 0.121 Uiso calc R 1 H
H15C 0.5435 0.1027 0.0861 0.121 Uiso calc R 1 H
C16 0.1064(3) 0.07107(17) 0.4155(2) 0.0702(12) Uani d . 1 C
H16A 0.1973 0.0789 0.4690 0.105 Uiso calc R 1 H
H16B 0.0846 0.0210 0.4221 0.105 Uiso calc R 1 H
H16C 0.0556 0.1026 0.4422 0.105 Uiso calc R 1 H
C17 -0.1079(3) 0.08788(17) 0.1460(3) 0.0677(11) Uani d . 1 C
H17A -0.1506 0.1235 0.1753 0.101 Uiso calc R 1 H
H17B -0.1396 0.0399 0.1513 0.101 Uiso calc R 1 H
H17C -0.1257 0.0982 0.0593 0.101 Uiso calc R 1 H
C18 0.1420(3) 0.01364(16) 0.1940(3) 0.0605(11) Uani d . 1 C
H18A 0.1253 0.0207 0.1067 0.091 Uiso calc R 1 H
H18B 0.1027 -0.0313 0.2022 0.091 Uiso calc R 1 H
H18C 0.2342 0.0115 0.2460 0.091 Uiso calc R 1 H
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'
Li Li -0.0003 0.0001 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Li1 N2 . 102.1(3) yes
N1 Li1 N3 4_565 119.0(3) yes
N2 Li1 N3 4_565 114.4(3) yes
C7 N1 Si1 . 134.1(2) yes
C7 N1 Li1 . 106.5(3) yes
Si1 N1 Li1 . 119.4(2) yes
C1 N2 Si2 . 146.7(2) yes
C1 N2 Li1 . 110.6(3) yes
Si2 N2 Li1 . 102.6(2) yes
C11 N3 C12 . 115.3(3) ?
C11 N3 Li1 4_666 133.4(3) ?
C12 N3 Li1 4_666 110.6(3) ?
N1 Si1 C14 . 106.22(14) ?
N1 Si1 C15 . 107.20(13) ?
C14 Si1 C15 . 108.34(17) ?
N1 Si1 C13 . 120.14(14) ?
C14 Si1 C13 . 105.65(16) ?
C15 Si1 C13 . 108.82(15) ?
N2 Si2 C16 . 113.59(14) ?
N2 Si2 C17 . 116.73(13) ?
C16 Si2 C17 . 109.69(14) ?
N2 Si2 C18 . 104.55(13) ?
C16 Si2 C18 . 105.42(14) ?
C17 Si2 C18 . 105.76(14) ?
N2 C1 C6 . 122.1(3) yes
N2 C1 C2 . 120.1(3) ?
C6 C1 C2 . 117.8(3) ?
C3 C2 C5 . 106.2(3) ?
C3 C2 C4 . 109.7(3) ?
C5 C2 C4 . 107.5(3) ?
C3 C2 C1 . 109.6(3) ?
C5 C2 C1 . 114.7(3) ?
C4 C2 C1 . 109.0(2) ?
C2 C3 H3A . 109.5 ?
C2 C3 H3B . 109.5 ?
H3A C3 H3B . 109.5 ?
C2 C3 H3C . 109.5 ?
H3A C3 H3C . 109.5 ?
H3B C3 H3C . 109.5 ?
C2 C4 H4A . 109.5 ?
C2 C4 H4B . 109.5 ?
H4A C4 H4B . 109.5 ?
C2 C4 H4C . 109.5 ?
H4A C4 H4C . 109.5 ?
H4B C4 H4C . 109.5 ?
C2 C5 H5A . 109.5 ?
C2 C5 H5B . 109.5 ?
H5A C5 H5B . 109.5 ?
C2 C5 H5C . 109.5 ?
H5A C5 H5C . 109.5 ?
H5B C5 H5C . 109.5 ?
C7 C6 C1 . 129.1(3) yes
C7 C6 H6 . 115.5 ?
C1 C6 H6 . 115.5 ?
N1 C7 C6 . 128.6(3) yes
N1 C7 C8 . 117.7(3) ?
C6 C7 C8 . 113.7(3) ?
C9 C8 C12 . 117.5(3) ?
C9 C8 C7 . 123.4(3) ?
C12 C8 C7 . 119.0(3) ?
C8 C9 C10 . 119.7(3) ?
C8 C9 H9 . 120.2 ?
C10 C9 H9 . 120.2 ?
C9 C10 C11 . 118.0(3) ?
C9 C10 H10 . 121.0 ?
C11 C10 H10 . 121.0 ?
N3 C11 C10 . 124.7(3) ?
N3 C11 H11 . 117.7 ?
C10 C11 H11 . 117.7 ?
N3 C12 C8 . 124.7(3) ?
N3 C12 H12 . 117.6 ?
C8 C12 H12 . 117.6 ?
Si1 C13 H13A . 109.5 ?
Si1 C13 H13B . 109.5 ?
H13A C13 H13B . 109.5 ?
Si1 C13 H13C . 109.5 ?
H13A C13 H13C . 109.5 ?
H13B C13 H13C . 109.5 ?
Si1 C14 H14A . 109.5 ?
Si1 C14 H14B . 109.5 ?
H14A C14 H14B . 109.5 ?
Si1 C14 H14C . 109.5 ?
H14A C14 H14C . 109.5 ?
H14B C14 H14C . 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 ?
Si2 C16 H16A . 109.5 ?
Si2 C16 H16B . 109.5 ?
H16A C16 H16B . 109.5 ?
Si2 C16 H16C . 109.5 ?
H16A C16 H16C . 109.5 ?
H16B C16 H16C . 109.5 ?
Si2 C17 H17A . 109.5 ?
Si2 C17 H17B . 109.5 ?
H17A C17 H17B . 109.5 ?
Si2 C17 H17C . 109.5 ?
H17A C17 H17C . 109.5 ?
H17B C17 H17C . 109.5 ?
Si2 C18 H18A . 109.5 ?
Si2 C18 H18B . 109.5 ?
H18A C18 H18B . 109.5 ?
Si2 C18 H18C . 109.5 ?
H18A C18 H18C . 109.5 ?
H18B C18 H18C . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Li1 N1 . 1.924(5) yes
Li1 N2 . 1.946(5) yes
Li1 N3 4_565 2.033(6) yes
N1 C7 . 1.317(4) yes
N1 Si1 . 1.716(2) yes
N2 C1 . 1.317(3) yes
N2 Si2 . 1.697(3) yes
N3 C11 . 1.326(3) ?
N3 C12 . 1.343(3) ?
N3 Li1 4_666 2.033(6) ?
Si1 C14 . 1.844(3) ?
Si1 C15 . 1.847(3) ?
Si1 C13 . 1.849(3) ?
Si2 C16 . 1.863(3) ?
Si2 C17 . 1.863(3) ?
Si2 C18 . 1.875(3) ?
C1 C6 . 1.405(4) yes
C1 C2 . 1.562(4) ?
C2 C3 . 1.527(4) ?
C2 C5 . 1.528(4) ?
C2 C4 . 1.532(3) ?
C3 H3A . 0.9600 ?
C3 H3B . 0.9600 ?
C3 H3C . 0.9600 ?
C4 H4A . 0.9600 ?
C4 H4B . 0.9600 ?
C4 H4C . 0.9600 ?
C5 H5A . 0.9600 ?
C5 H5B . 0.9600 ?
C5 H5C . 0.9600 ?
C6 C7 . 1.399(4) yes
C6 H6 . 0.9300 ?
C7 C8 . 1.519(4) ?
C8 C9 . 1.363(4) ?
C8 C12 . 1.386(3) ?
C9 C10 . 1.378(4) ?
C9 H9 . 0.9300 ?
C10 C11 . 1.378(3) ?
C10 H10 . 0.9300 ?
C11 H11 . 0.9300 ?
C12 H12 . 0.9300 ?
C13 H13A . 0.9600 ?
C13 H13B . 0.9600 ?
C13 H13C . 0.9600 ?
C14 H14A . 0.9600 ?
C14 H14B . 0.9600 ?
C14 H14C . 0.9600 ?
C15 H15A . 0.9600 ?
C15 H15B . 0.9600 ?
C15 H15C . 0.9600 ?
C16 H16A . 0.9600 ?
C16 H16B . 0.9600 ?
C16 H16C . 0.9600 ?
C17 H17A . 0.9600 ?
C17 H17B . 0.9600 ?
C17 H17C . 0.9600 ?
C18 H18A . 0.9600 ?
C18 H18B . 0.9600 ?
C18 H18C . 0.9600 ?
