#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:20:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179811 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/07/7010780.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_7010780
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Layh, Marcus'
_publ_section_title
;
 The reactions of lithium trimethysilylmethyls with isocyanides;
 structures and reactions of the derived lithium 1-azaallyls,
 β-diketiminates and a 1-azabuta-1,3-dienyl-3-amide
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2409
_journal_paper_doi               10.1039/b103553n
_journal_year                    2001
_chemical_formula_structural     '[(tmeda)Li{PhCHC(SiMe3)NC6H3Me2}]'
_chemical_formula_sum            'C25 H40 Li N3 Si'
_chemical_formula_weight         417.63
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.77(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.900(7)
_cell_length_b                   8.553(2)
_cell_length_c                   19.852(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     5112(2)
_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  0.0522
_diffrn_reflns_av_sigmaI/netI    0.1624
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4567
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.011
_refine_ls_goodness_of_fit_obs   1.134
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_restrained_S_obs      1.134
_refine_ls_R_factor_all          0.1941
_refine_ls_R_factor_obs          0.0884
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0581P)²+17.3952P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2225
_refine_ls_wR_factor_obs         0.1695
_reflns_number_observed          2174
_reflns_number_total             4494
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b103553n.txt
_cod_data_source_block           mfl-6b-(jan1698)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+17.3952P] 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^)+(0.0581P)^2^+17.3952P] 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        5112.4(21)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7010780
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Li Li 0.3731(3) 0.5161(11) 0.0560(5) 0.036(2) Uani 1 d . .
Si Si 0.40053(5) 0.1999(2) 0.25119(8) 0.0298(4) Uani 1 d . .
N1 N 0.35600(14) 0.3764(5) 0.1174(2) 0.0277(10) Uani 1 d . .
N2 N 0.3371(2) 0.6907(6) -0.0205(3) 0.061(2) Uani 1 d . .
N3 N 0.4307(2) 0.6384(6) 0.0717(4) 0.064(2) Uani 1 d . .
C1 C 0.3860(2) 0.2616(6) 0.1517(2) 0.0246(12) Uani 1 d . .
C2 C 0.4130(2) 0.1969(6) 0.1213(2) 0.0285(12) Uani 1 d . .
H2 H 0.4365(2) 0.1339(6) 0.1538(2) 0.034 Uiso 1 calc R .
C3 C 0.4112(2) 0.2098(5) 0.0470(3) 0.0239(11) Uani 1 d . .
C4 C 0.4484(2) 0.1577(6) 0.0345(3) 0.0289(13) Uani 1 d . .
H4 H 0.4738(2) 0.1200(6) 0.0747(3) 0.035 Uiso 1 calc R .
C5 C 0.4486(2) 0.1604(6) -0.0349(3) 0.0331(14) Uani 1 d . .
H5 H 0.4740(2) 0.1239(6) -0.0417(3) 0.040 Uiso 1 calc R .
C6 C 0.4122(2) 0.2158(6) -0.0949(3) 0.0339(13) Uani 1 d . .
H6 H 0.4128(2) 0.2211(6) -0.1422(3) 0.041 Uiso 1 calc R .
C7 C 0.3753(2) 0.2626(6) -0.0846(3) 0.0357(14) Uani 1 d . .
H7 H 0.3498(2) 0.2967(6) -0.1256(3) 0.043 Uiso 1 calc R .
C8 C 0.3745(2) 0.2612(6) -0.0146(3) 0.0283(13) Uani 1 d . .
H8 H 0.3487(2) 0.2957(6) -0.0088(3) 0.034 Uiso 1 calc R .
C9 C 0.4236(2) 0.3694(8) 0.3141(3) 0.059(2) Uani 1 d . .
H9C H 0.3992(3) 0.4381(26) 0.3120(17) 0.088 Uiso 1 calc R .
H9B H 0.4441(11) 0.4277(29) 0.2989(14) 0.088 Uiso 1 calc R .
H9A H 0.4395(12) 0.3315(8) 0.3646(5) 0.088 Uiso 1 calc R .
C10 C 0.4443(2) 0.0446(8) 0.2796(3) 0.046(2) Uani 1 d . .
H10C H 0.4517(9) 0.0152(31) 0.3309(7) 0.069 Uiso 1 calc R .
H10B H 0.4710(4) 0.0846(15) 0.2749(19) 0.069 Uiso 1 calc R .
H10A H 0.4332(5) -0.0472(17) 0.2479(13) 0.069 Uiso 1 calc R .
C11 C 0.3540(2) 0.1185(7) 0.2715(3) 0.042(2) Uani 1 d . .
H11C H 0.3656(3) 0.0808(38) 0.3224(7) 0.063 Uiso 1 calc R .
H11B H 0.3402(8) 0.0315(27) 0.2379(13) 0.063 Uiso 1 calc R .
H11A H 0.3319(6) 0.2003(13) 0.2647(19) 0.063 Uiso 1 calc R .
C12 C 0.3213(2) 0.4031(6) 0.1412(3) 0.0302(13) Uani 1 d . .
C13 C 0.3195(2) 0.5423(7) 0.1777(3) 0.040(2) Uani 1 d . .
C14 C 0.2841(3) 0.5648(9) 0.1986(3) 0.059(2) Uani 1 d . .
H14 H 0.2827(3) 0.6587(9) 0.2231(3) 0.071 Uiso 1 calc R .
C15 C 0.2513(2) 0.4538(10) 0.1845(4) 0.062(2) Uani 1 d . .
H15 H 0.2283(2) 0.4683(10) 0.2012(4) 0.074 Uiso 1 calc R .
C16 C 0.2525(2) 0.3221(9) 0.1460(3) 0.054(2) Uani 1 d . .
H16 H 0.2291(2) 0.2483(9) 0.1339(3) 0.065 Uiso 1 calc R .
C17 C 0.2866(2) 0.2932(7) 0.1241(3) 0.0366(14) Uani 1 d . .
C18 C 0.3548(2) 0.6652(7) 0.1936(3) 0.057(2) Uani 1 d . .
H18C H 0.3514(8) 0.7439(26) 0.2268(18) 0.086 Uiso 1 calc R .
H18B H 0.3519(9) 0.7152(33) 0.1474(4) 0.086 Uiso 1 calc R .
H18A H 0.3842(2) 0.6164(10) 0.2168(20) 0.086 Uiso 1 calc R .
C19 C 0.2860(2) 0.1476(7) 0.0808(3) 0.048(2) Uani 1 d . .
H19C H 0.2558(3) 0.1051(26) 0.0592(17) 0.072 Uiso 1 calc R .
H19B H 0.3062(10) 0.0696(18) 0.1136(5) 0.072 Uiso 1 calc R .
H19A H 0.2957(12) 0.1736(11) 0.0414(13) 0.072 Uiso 1 calc R .
C20 C 0.3725(5) 0.8000(11) -0.0139(4) 0.148(6) Uani 1 d . .
H20B H 0.3680(5) 0.8303(11) -0.0646(4) 0.178 Uiso 1 calc R .
H20A H 0.3675(5) 0.8953(11) 0.0100(4) 0.178 Uiso 1 calc R .
C21 C 0.4124(5) 0.7655(12) 0.0188(13) 0.255(13) Uani 1 d . .
H21B H 0.4272(5) 0.8618(12) 0.0448(13) 0.306 Uiso 1 calc R .
H21A H 0.4234(5) 0.7475(12) -0.0201(13) 0.306 Uiso 1 calc R .
C22 C 0.3012(4) 0.7613(13) -0.0047(5) 0.165(6) Uani 1 d . .
H22C H 0.2813(20) 0.8196(100) -0.0479(20) 0.248 Uiso 1 calc R .
H22B H 0.3139(5) 0.8326(86) 0.0373(35) 0.248 Uiso 1 calc R .
H22A H 0.2844(20) 0.6787(14) 0.0070(53) 0.248 Uiso 1 calc R .
C23 C 0.3165(2) 0.6334(7) -0.0965(3) 0.055(2) Uani 1 d . .
H23C H 0.3031(12) 0.7212(10) -0.1298(4) 0.083 Uiso 1 calc R .
H23B H 0.2935(10) 0.5565(36) -0.1007(6) 0.083 Uiso 1 calc R .
H23A H 0.3392(3) 0.5842(42) -0.1098(8) 0.083 Uiso 1 calc R .
C24 C 0.4544(4) 0.6907(19) 0.1461(8) 0.224(10) Uani 1 d . .
H24C H 0.4801(29) 0.7533(145) 0.1493(18) 0.336 Uiso 1 calc R .
H24B H 0.4646(41) 0.5999(19) 0.1788(14) 0.336 Uiso 1 calc R .
H24A H 0.4347(16) 0.7545(141) 0.1610(28) 0.336 Uiso 1 calc R .
C25 C 0.4625(2) 0.5538(8) 0.0513(4) 0.059(2) Uani 1 d . .
H25C H 0.4470(3) 0.5073(41) 0.0024(10) 0.088 Uiso 1 calc R .
H25B H 0.4764(10) 0.4710(32) 0.0873(13) 0.088 Uiso 1 calc R .
H25A H 0.4853(8) 0.6262(12) 0.0503(23) 0.088 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'
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
N1 Li N3 133.9(5) . . ?
N1 Li N2 131.5(5) . . ?
N3 Li N2 88.0(4) . . ?
N1 Li C8 84.0(4) . . ?
N3 Li C8 106.8(4) . . ?
N2 Li C8 109.3(4) . . ?
N1 Li C21 158.8(7) . . ?
N3 Li C21 31.6(4) . . ?
N2 Li C21 56.4(4) . . ?
C8 Li C21 113.2(5) . . ?
C9 Si C11 107.0(3) . . ?
C9 Si C10 107.1(3) . . ?
C11 Si C10 105.6(3) . . ?
C9 Si C1 110.1(3) . . ?
C11 Si C1 116.1(2) . . ?
C10 Si C1 110.5(2) . . ?
C1 N1 C12 117.8(4) . . ?
C1 N1 Li 115.0(4) . . ?
C12 N1 Li 125.8(4) . . ?
C20 N2 C23 109.1(5) . . ?
C20 N2 C22 113.6(9) . . ?
C23 N2 C22 106.2(7) . . ?
C20 N2 Li 101.1(6) . . ?
C23 N2 Li 113.2(5) . . ?
C22 N2 Li 113.7(5) . . ?
C24 N3 C25 106.8(7) . . ?
C24 N3 C21 113.8(10) . . ?
C25 N3 C21 107.8(8) . . ?
C24 N3 Li 113.3(6) . . ?
C25 N3 Li 114.9(5) . . ?
C21 N3 Li 100.3(7) . . ?
N1 C1 C2 122.4(4) . . ?
N1 C1 Si 123.0(3) . . ?
C2 C1 Si 113.9(4) . . ?
C1 C2 C3 130.2(5) . . ?
C8 C3 C4 116.6(4) . . ?
C8 C3 C2 125.2(4) . . ?
C4 C3 C2 118.0(4) . . ?
C5 C4 C3 121.5(5) . . ?
C4 C5 C6 120.8(5) . . ?
C7 C6 C5 118.8(5) . . ?
C6 C7 C8 121.2(5) . . ?
C3 C8 C7 121.1(5) . . ?
C3 C8 Li 89.4(4) . . ?
C7 C8 Li 122.6(4) . . ?
C13 C12 C17 119.4(5) . . ?
C13 C12 N1 120.9(5) . . ?
C17 C12 N1 119.6(5) . . ?
C14 C13 C12 118.9(6) . . ?
C14 C13 C18 120.5(6) . . ?
C12 C13 C18 120.7(5) . . ?
C15 C14 C13 121.4(6) . . ?
C16 C15 C14 118.8(6) . . ?
C15 C16 C17 122.3(7) . . ?
C16 C17 C12 119.1(6) . . ?
C16 C17 C19 120.1(6) . . ?
C12 C17 C19 120.7(5) . . ?
C21 C20 N2 122.1(9) . . ?
C20 C21 N3 126.6(9) . . ?
C20 C21 Li 79.3(7) . . ?
N3 C21 Li 48.1(4) . . ?
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 N1 1.946(10) . ?
Li N3 2.075(11) . ?
Li N2 2.119(10) . ?
Li C8 2.602(10) . ?
Li C21 2.743(13) . ?
Si C9 1.864(6) . ?
Si C11 1.867(5) . ?
Si C10 1.871(6) . ?
Si C1 1.909(5) . ?
N1 C1 1.363(6) . ?
N1 C12 1.420(6) . ?
N2 C20 1.458(11) . ?
N2 C23 1.467(8) . ?
N2 C22 1.469(10) . ?
N3 C24 1.436(12) . ?
N3 C25 1.456(7) . ?
N3 C21 1.46(2) . ?
C1 C2 1.376(6) . ?
C2 C3 1.457(6) . ?
C3 C8 1.398(7) . ?
C3 C4 1.414(7) . ?
C4 C5 1.380(7) . ?
C5 C6 1.390(7) . ?
C6 C7 1.369(7) . ?
C7 C8 1.400(7) . ?
C12 C13 1.408(7) . ?
C12 C17 1.409(7) . ?
C13 C14 1.396(8) . ?
C13 C18 1.503(8) . ?
C14 C15 1.379(10) . ?
C15 C16 1.371(10) . ?
C16 C17 1.378(7) . ?
C17 C19 1.509(8) . ?
C20 C21 1.241(15) . ?
