#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:38:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179800 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/96/7009625.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_7009625
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Layh, Marcus'
'Liu, Dian-Sheng'
'Sablong, Rafael'
'Shun, Tian'
_publ_section_title
;
 Reactions of LiCHR2 and related lithium alkyls with α-H free nitriles
 and the crystal structures of eleven representative lithium
 1,3-diazaallyls, 1-azaallyls and β-diketiminates
;
_journal_issue                   14
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2301
_journal_paper_doi               10.1039/b002376k
_journal_year                    2000
_chemical_formula_structural     '[{Li(thf)(Me3SiNCPhNCPhCHNSiMe3)}2]'
_chemical_formula_sum            'C50 H74 Li2 N4 O2 Si4'
_chemical_formula_weight         889.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                94.22(7)
_cell_angle_beta                 93.81(7)
_cell_angle_gamma                110.94(8)
_cell_formula_units_Z            1
_cell_length_a                   11.075
_cell_length_b                   11.440(5)
_cell_length_c                   11.514(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     1352.0(12)
_computing_cell_refinement       'Enraf-Nonius CAD4'
_computing_data_collection       'Enraf-Nonius CAD4'
_computing_molecular_graphics    'CAMERON (Watkin and Pearce,1993)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       ' Enraf-Nonius CAD4'
_diffrn_measurement_method       ω--2θ
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0970
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3289
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.991
_refine_ls_goodness_of_fit_obs   1.048
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.1281
_refine_ls_R_factor_obs          0.0793
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1451P)²+0.7252P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2341
_refine_ls_wR_factor_obs         0.1946
_reflns_number_observed          2096
_reflns_number_total             3289
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b002376k.txt
_cod_data_source_block           oct797
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+0.7252P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+0.7252P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1352.0(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009625
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
Li Li 0.1049(10) 0.0160(10) 0.0649(9) 0.038(3) Uani 1 d . .
Si1 Si 0.3499(2) 0.2267(2) -0.05137(15) 0.0320(5) Uani 1 d . .
Si2 Si -0.2575(2) -0.3350(2) -0.3818(2) 0.0354(6) Uani 1 d . .
O O 0.1474(4) -0.1027(4) 0.1483(4) 0.0452(12) Uani 1 d . .
N1 N 0.2106(4) 0.0956(4) -0.0609(4) 0.0284(12) Uani 1 d . .
N2 N 0.0264(4) -0.0680(4) -0.1407(4) 0.0281(12) Uani 1 d . .
C1 C 0.1528(5) 0.0071(5) -0.1457(5) 0.0258(14) Uani 1 d . .
C2 C -0.0316(5) -0.1751(5) -0.2219(5) 0.0234(14) Uani 1 d . .
C3 C -0.1469(5) -0.1962(5) -0.2840(5) 0.0281(15) Uani 1 d . .
H3 H -0.1765(5) -0.1279(5) -0.2762(5) 0.034 Uiso 1 calc R .
C4 C 0.4791(6) 0.2012(7) 0.0456(7) 0.058(2) Uani 1 d . .
H4C H 0.5007(6) 0.1319(7) 0.0092(7) 0.088 Uiso 1 calc R .
H4B H 0.4474(6) 0.1802(7) 0.1217(7) 0.088 Uiso 1 calc R .
H4A H 0.5569(6) 0.2782(7) 0.0567(7) 0.088 Uiso 1 calc R .
C5 C 0.4146(7) 0.2769(7) -0.1909(6) 0.054(2) Uani 1 d . .
H5C H 0.4367(7) 0.2099(7) -0.2313(6) 0.081 Uiso 1 calc R .
H5B H 0.4927(7) 0.3533(7) -0.1749(6) 0.081 Uiso 1 calc R .
H5A H 0.3489(7) 0.2942(7) -0.2404(6) 0.081 Uiso 1 calc R .
C6 C 0.3112(7) 0.3572(6) 0.0188(7) 0.053(2) Uani 1 d . .
H6C H 0.2764(7) 0.3344(6) 0.0935(7) 0.079 Uiso 1 calc R .
H6B H 0.2463(7) 0.3738(6) -0.0326(7) 0.079 Uiso 1 calc R .
H6A H 0.3902(7) 0.4329(6) 0.0329(7) 0.079 Uiso 1 calc R .
C7 C -0.2152(8) -0.3290(7) -0.5339(6) 0.059(2) Uani 1 d . .
H7C H -0.2754(8) -0.4036(7) -0.5825(6) 0.089 Uiso 1 calc R .
H7B H -0.1262(8) -0.3270(7) -0.5363(6) 0.089 Uiso 1 calc R .
H7A H -0.2215(8) -0.2531(7) -0.5637(6) 0.089 Uiso 1 calc R .
C8 C -0.2653(6) -0.4890(6) -0.3333(6) 0.043(2) Uani 1 d . .
H8C H -0.2876(6) -0.4932(6) -0.2523(6) 0.065 Uiso 1 calc R .
H8B H -0.1807(6) -0.4974(6) -0.3378(6) 0.065 Uiso 1 calc R .
H8A H -0.3317(6) -0.5574(6) -0.3841(6) 0.065 Uiso 1 calc R .
C9 C -0.4234(7) -0.3247(8) -0.3824(8) 0.067(3) Uani 1 d . .
H9C H -0.4495(7) -0.3276(8) -0.3026(8) 0.101 Uiso 1 calc R .
H9B H -0.4862(7) -0.3957(8) -0.4335(8) 0.101 Uiso 1 calc R .
H9A H -0.4210(7) -0.2455(8) -0.4113(8) 0.101 Uiso 1 calc R .
C10 C 0.2174(5) -0.0131(5) -0.2505(5) 0.0275(15) Uani 1 d . .
C11 C 0.3251(6) -0.0482(6) -0.2385(6) 0.038(2) Uani 1 d . .
H11 H 0.3583(6) -0.0582(6) -0.1632(6) 0.045 Uiso 1 calc R .
C12 C 0.3837(6) -0.0686(7) -0.3362(7) 0.052(2) Uani 1 d . .
H12 H 0.4543(6) -0.0971(7) -0.3285(7) 0.063 Uiso 1 calc R .
C13 C 0.3404(7) -0.0478(8) -0.4440(7) 0.057(2) Uani 1 d . .
H13 H 0.3829(7) -0.0601(8) -0.5103(7) 0.068 Uiso 1 calc R .
C14 C 0.2359(7) -0.0093(7) -0.4580(6) 0.046(2) Uani 1 d . .
H14 H 0.2072(7) 0.0061(7) -0.5330(6) 0.056 Uiso 1 calc R .
C15 C 0.1741(6) 0.0065(6) -0.3614(5) 0.035(2) Uani 1 d . .
H15 H 0.1009(6) 0.0310(6) -0.3703(5) 0.041 Uiso 1 calc R .
C16 C 0.0341(6) -0.2692(5) -0.2265(5) 0.0300(15) Uani 1 d . .
C17 C 0.0679(6) -0.3109(6) -0.3308(6) 0.043(2) Uani 1 d . .
H17 H 0.0471(6) -0.2817(6) -0.4017(6) 0.051 Uiso 1 calc R .
C18 C 0.1328(7) -0.3964(6) -0.3322(7) 0.052(2) Uani 1 d . .
H18 H 0.1563(7) -0.4242(6) -0.4041(7) 0.062 Uiso 1 calc R .
C19 C 0.1622(7) -0.4398(7) -0.2308(8) 0.055(2) Uani 1 d . .
H19 H 0.2059(7) -0.4976(7) -0.2322(8) 0.065 Uiso 1 calc R .
C20 C 0.1286(7) -0.3997(7) -0.1270(7) 0.058(2) Uani 1 d . .
H20 H 0.1487(7) -0.4299(7) -0.0564(7) 0.069 Uiso 1 calc R .
C21 C 0.0652(6) -0.3152(6) -0.1256(6) 0.041(2) Uani 1 d . .
H21 H 0.0425(6) -0.2879(6) -0.0531(6) 0.049 Uiso 1 calc R .
C22 C 0.2660(7) -0.1274(8) 0.1528(9) 0.074(3) Uani 1 d . .
H22B H 0.3383(7) -0.0541(8) 0.1939(9) 0.089 Uiso 1 calc R .
H22A H 0.2878(7) -0.1431(8) 0.0726(9) 0.089 Uiso 1 calc R .
C23 C 0.2470(9) -0.2384(10) 0.2156(9) 0.092(3) Uani 1 d . .
H23B H 0.2431(9) -0.3108(10) 0.1609(9) 0.111 Uiso 1 calc R .
H23A H 0.3199(9) -0.2214(10) 0.2770(9) 0.111 Uiso 1 calc R .
C24 C 0.1264(8) -0.2656(8) 0.2677(9) 0.078(3) Uani 1 d . .
H24B H 0.1434(8) -0.2462(8) 0.3538(9) 0.094 Uiso 1 calc R .
H24A H 0.0715(8) -0.3557(8) 0.2495(9) 0.094 Uiso 1 calc R .
C25 C 0.0601(7) -0.1858(7) 0.2178(6) 0.050(2) Uani 1 d . .
H25B H -0.0206(7) -0.2390(7) 0.1690(6) 0.060 Uiso 1 calc R .
H25A H 0.0371(7) -0.1369(7) 0.2814(6) 0.060 Uiso 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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
O Li N2 111.1(5) . 2 ?
O Li N1 120.3(5) . . ?
N2 Li N1 127.5(6) 2 . ?
N1 Si1 C6 106.4(3) . . ?
N1 Si1 C5 116.7(3) . . ?
C6 Si1 C5 106.8(4) . . ?
N1 Si1 C4 108.9(3) . . ?
C6 Si1 C4 108.7(4) . . ?
C5 Si1 C4 109.1(4) . . ?
C7 Si2 C3 111.9(3) . . ?
C7 Si2 C8 108.7(3) . . ?
C3 Si2 C8 114.1(3) . . ?
C7 Si2 C9 107.0(4) . . ?
C3 Si2 C9 105.8(3) . . ?
C8 Si2 C9 109.0(4) . . ?
C25 O C22 108.7(5) . . ?
C25 O Li 123.3(5) . . ?
C22 O Li 128.1(5) . . ?
C1 N1 Si1 131.9(4) . . ?
C1 N1 Li 97.7(5) . . ?
Si1 N1 Li 129.6(4) . . ?
C1 N2 C2 119.7(5) . . ?
C1 N2 Li 125.4(5) . 2 ?
C2 N2 Li 112.0(5) . 2 ?
N1 C1 N2 119.0(5) . . ?
N1 C1 C10 122.8(5) . . ?
N2 C1 C10 118.2(5) . . ?
C3 C2 N2 121.0(5) . . ?
C3 C2 C16 122.4(5) . . ?
N2 C2 C16 116.4(5) . . ?
C2 C3 Si2 131.4(5) . . ?
C11 C10 C15 118.9(6) . . ?
C11 C10 C1 120.1(5) . . ?
C15 C10 C1 121.0(5) . . ?
C12 C11 C10 119.9(6) . . ?
C13 C12 C11 120.2(7) . . ?
C12 C13 C14 121.1(7) . . ?
C15 C14 C13 118.8(7) . . ?
C14 C15 C10 121.0(6) . . ?
C21 C16 C17 117.8(6) . . ?
C21 C16 C2 120.8(5) . . ?
C17 C16 C2 121.3(6) . . ?
C16 C17 C18 120.3(7) . . ?
C19 C18 C17 120.3(7) . . ?
C18 C19 C20 120.0(7) . . ?
C19 C20 C21 119.7(7) . . ?
C16 C21 C20 121.9(7) . . ?
O C22 C23 108.1(6) . . ?
C24 C23 C22 107.3(7) . . ?
C23 C24 C25 107.1(7) . . ?
O C25 C24 107.7(6) . . ?
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
Li O 1.891(11) . ?
Li N2 1.985(11) 2 ?
Li N1 1.989(11) . ?
Si1 N1 1.715(5) . ?
Si1 C6 1.843(7) . ?
Si1 C5 1.849(7) . ?
Si1 C4 1.874(7) . ?
Si2 C7 1.842(8) . ?
Si2 C3 1.858(6) . ?
Si2 C8 1.861(6) . ?
Si2 C9 1.883(7) . ?
O C25 1.427(8) . ?
O C22 1.438(8) . ?
N1 C1 1.302(7) . ?
N2 C1 1.364(7) . ?
N2 C2 1.406(7) . ?
N2 Li 1.985(11) 2 ?
C1 C10 1.487(8) . ?
C2 C3 1.353(8) . ?
C2 C16 1.500(8) . ?
C10 C11 1.390(8) . ?
C10 C15 1.395(8) . ?
C11 C12 1.381(9) . ?
C12 C13 1.369(10) . ?
C13 C14 1.382(10) . ?
C14 C15 1.378(9) . ?
C16 C21 1.383(9) . ?
C16 C17 1.383(9) . ?
C17 C18 1.406(9) . ?
C18 C19 1.366(10) . ?
C19 C20 1.369(10) . ?
C20 C21 1.382(9) . ?
C22 C23 1.464(11) . ?
C23 C24 1.441(11) . ?
C24 C25 1.485(10) . ?
