#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/04/7010493.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_7010493
loop_
_publ_author_name
'Bezombes, Jean Philippe'
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Merle, Philippe G.'
_publ_section_title
;
 Synthesis and structures of lithium N-trimethylsilyl- and
 -neopentyl-anilides and their Et2O and tmen adducts; crystal
 structures of [(Li{μ-N(Ph)R}-trans)2(μ-tmen)]∞
 (R = SiMe3 1 or CH2But 2) and
 [Li{μ-N(Ph)CH2But}(OEt2)]2 †
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              816
_journal_paper_doi               10.1039/b009724l
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C30 H52 Li2 N2 O2'
_chemical_formula_structural     'C30 H52 LI2 N2 O2'
_chemical_formula_sum            'C30 H52 Li2 N2 O2'
_chemical_formula_weight         486.62
_chemical_name_common            '[{Li(OEt2)(PhNCH2tBu)}2]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             1999-11-09T15:43:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.7960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9810(2)
_cell_length_b                   16.1914(4)
_cell_length_c                   19.2524(4)
_cell_measurement_reflns_used    14770
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      4.246
_cell_measurement_wavelength     0.71073
_cell_volume                     3095.40(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25409
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         4.33
_exptl_absorpt_coefficient_mu    0.063
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.044
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0897P)²+1.3997P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1795
_reflns_number_gt                5366
_reflns_number_total             7257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009724l.txt
_cod_data_source_block           nov1399
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010493
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_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
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 1.0439(2) 0.58555(18) 0.19470(14) 0.0368(6) Uani 1 1 d . A .
Li2 Li 0.9554(2) 0.64271(18) 0.30203(13) 0.0361(6) Uani 1 1 d . A .
O1 O 1.14403(11) 0.50840(7) 0.13884(6) 0.0402(3) Uani 1 1 d . . .
O2 O 0.85138(11) 0.71632(8) 0.35587(6) 0.0450(3) Uani 1 1 d . . .
N1 N 0.84995(11) 0.59386(8) 0.21366(6) 0.0292(3) Uani 1 1 d . . .
N2 N 1.14995(11) 0.63424(8) 0.28298(6) 0.0296(3) Uani 1 1 d . . .
C1 C 0.79091(13) 0.53541(9) 0.25231(7) 0.0280(3) Uani 1 1 d . A .
C2 C 0.65055(14) 0.52244(10) 0.25600(8) 0.0319(3) Uani 1 1 d . . .
H2 H 0.5875 0.5544 0.2271 0.038 Uiso 1 1 calc R A .
C3 C 0.60374(15) 0.46451(11) 0.30062(8) 0.0364(4) Uani 1 1 d . A .
H3 H 0.5094 0.4581 0.3017 0.044 Uiso 1 1 calc R . .
C4 C 0.69042(16) 0.41567(11) 0.34381(8) 0.0392(4) Uani 1 1 d . . .
H4 H 0.6569 0.3766 0.3745 0.047 Uiso 1 1 calc R A .
C5 C 0.82818(16) 0.42571(11) 0.34080(8) 0.0376(4) Uani 1 1 d . A .
H5 H 0.8897 0.3927 0.3697 0.045 Uiso 1 1 calc R . .
C6 C 0.87677(14) 0.48304(10) 0.29638(7) 0.0323(3) Uani 1 1 d . . .
H6 H 0.9714 0.4877 0.2952 0.039 Uiso 1 1 calc R A .
C7 C 0.76122(14) 0.65147(10) 0.17285(7) 0.0306(3) Uani 1 1 d . A .
H7A H 0.802 0.7072 0.1777 0.037 Uiso 1 1 calc R . .
H7B H 0.6747 0.6536 0.1938 0.037 Uiso 1 1 calc R . .
C8 C 0.73015(14) 0.63292(11) 0.09400(8) 0.0342(3) Uani 1 1 d . . .
C9 C 0.64117(17) 0.70280(12) 0.06211(9) 0.0445(4) Uani 1 1 d . A .
H9A H 0.6882 0.7556 0.0701 0.067 Uiso 1 1 calc R . .
H9B H 0.5567 0.7041 0.084 0.067 Uiso 1 1 calc R . .
H9C H 0.6215 0.6935 0.0118 0.067 Uiso 1 1 calc R . .
C10 C 0.86159(17) 0.63040(13) 0.05932(9) 0.0472(4) Uani 1 1 d . A .
H10A H 0.9187 0.5857 0.0798 0.071 Uiso 1 1 calc R . .
H10B H 0.9089 0.6832 0.0668 0.071 Uiso 1 1 calc R . .
H10C H 0.8413 0.6207 0.0091 0.071 Uiso 1 1 calc R . .
C11 C 0.65711(17) 0.55020(12) 0.08225(9) 0.0426(4) Uani 1 1 d . A .
H11A H 0.7145 0.5057 0.103 0.064 Uiso 1 1 calc R . .
H11B H 0.6373 0.5404 0.032 0.064 Uiso 1 1 calc R . .
H11C H 0.5727 0.5516 0.1042 0.064 Uiso 1 1 calc R . .
C12 C 1.13870(17) 0.42332(12) 0.15934(10) 0.0466(4) Uani 1 1 d . . .
H12A H 1.1638 0.4183 0.2102 0.056 Uiso 1 1 calc R . .
H12B H 1.2036 0.3907 0.135 0.056 Uiso 1 1 calc R . .
C13 C 1.00010(18) 0.39066(12) 0.14136(10) 0.0473(4) Uani 1 1 d . . .
H13A H 0.9968 0.3326 0.1554 0.071 Uiso 1 1 calc R . .
H13B H 0.976 0.3951 0.0909 0.071 Uiso 1 1 calc R . .
H13C H 0.9363 0.4227 0.1659 0.071 Uiso 1 1 calc R . .
C14 C 1.27031(18) 0.53382(13) 0.11789(11) 0.0500(5) Uani 1 1 d . . .
H14A H 1.3117 0.4876 0.094 0.06 Uiso 1 1 calc R . .
H14B H 1.3317 0.5491 0.1595 0.06 Uiso 1 1 calc R . .
C15 C 1.25120(18) 0.60603(12) 0.06982(10) 0.0480(4) Uani 1 1 d . . .
H15A H 1.3386 0.6234 0.0559 0.072 Uiso 1 1 calc R . .
H15B H 1.2107 0.6517 0.0937 0.072 Uiso 1 1 calc R . .
H15C H 1.1917 0.5904 0.0283 0.072 Uiso 1 1 calc R . .
C16 C 1.20915(13) 0.69429(9) 0.24617(7) 0.0285(3) Uani 1 1 d . A .
C17 C 1.34970(14) 0.70897(10) 0.24424(8) 0.0334(3) Uani 1 1 d . . .
H17 H 1.4126 0.6767 0.273 0.04 Uiso 1 1 calc R A .
C18 C 1.39674(15) 0.76895(11) 0.20164(8) 0.0373(4) Uani 1 1 d . A .
H18 H 1.4912 0.7764 0.2017 0.045 Uiso 1 1 calc R . .
C19 C 1.31030(17) 0.81865(11) 0.15879(9) 0.0404(4) Uani 1 1 d . . .
H19 H 1.3441 0.8593 0.1295 0.048 Uiso 1 1 calc R A .
C20 C 1.17262(16) 0.80691(10) 0.16016(8) 0.0372(4) Uani 1 1 d . A .
H20 H 1.1112 0.8403 0.1316 0.045 Uiso 1 1 calc R . .
C21 C 1.12378(14) 0.74744(10) 0.20243(8) 0.0324(3) Uani 1 1 d . . .
H21 H 1.029 0.7417 0.2023 0.039 Uiso 1 1 calc R A .
C22 C 1.23916(14) 0.57811(10) 0.32563(7) 0.0297(3) Uani 1 1 d . A .
H22A H 1.3275 0.5774 0.3064 0.036 Uiso 1 1 calc R . .
H22B H 1.2012 0.5217 0.3204 0.036 Uiso 1 1 calc R . .
C23 C 1.26378(14) 0.59784(10) 0.40466(8) 0.0320(3) Uani 1 1 d . . .
C24 C 1.13058(17) 0.59559(13) 0.43764(9) 0.0447(4) Uani 1 1 d . A .
H24A H 1.0884 0.5413 0.4296 0.067 Uiso 1 1 calc R . .
H24B H 1.0702 0.6384 0.4164 0.067 Uiso 1 1 calc R . .
H24C H 1.1478 0.6056 0.488 0.067 Uiso 1 1 calc R . .
C25 C 1.35736(19) 0.53148(12) 0.43844(9) 0.0487(5) Uani 1 1 d . A .
H25A H 1.3158 0.4771 0.4302 0.073 Uiso 1 1 calc R . .
H25B H 1.373 0.5416 0.4888 0.073 Uiso 1 1 calc R . .
H25C H 1.4434 0.5331 0.418 0.073 Uiso 1 1 calc R . .
C26 C 1.32855(18) 0.68244(12) 0.41730(9) 0.0435(4) Uani 1 1 d . A .
H26A H 1.414 0.6842 0.3963 0.065 Uiso 1 1 calc R . .
H26B H 1.3454 0.6924 0.4676 0.065 Uiso 1 1 calc R . .
H26C H 1.268 0.7251 0.3961 0.065 Uiso 1 1 calc R . .
C27 C 0.8531(2) 0.80264(15) 0.34026(18) 0.0812(8) Uani 1 1 d . A .
H27A H 0.7885 0.8313 0.3678 0.097 Uiso 1 1 calc R . .
H27B H 0.8224 0.8107 0.2902 0.097 Uiso 1 1 calc R . .
C28 C 0.9848(2) 0.83994(14) 0.35523(12) 0.0591(5) Uani 1 1 d . . .
H28A H 0.9794 0.8989 0.344 0.089 Uiso 1 1 calc R A .
H28B H 1.0487 0.8131 0.327 0.089 Uiso 1 1 calc R . .
H28C H 1.0155 0.833 0.4049 0.089 Uiso 1 1 calc R . .
C29 C 0.7377(4) 0.6771(3) 0.3837(3) 0.0492(14) Uani 0.572(8) 1 d P A 1
H29A H 0.7369 0.6177 0.3716 0.059 Uiso 0.572(8) 1 calc PR A 1
H29B H 0.6533 0.7019 0.3615 0.059 Uiso 0.572(8) 1 calc PR A 1
C30 C 0.7423(5) 0.6863(4) 0.4623(2) 0.084(2) Uani 0.572(8) 1 d P A 1
H30A H 0.665 0.6578 0.4788 0.125 Uiso 0.572(8) 1 calc PR A 1
H30B H 0.739 0.745 0.4743 0.125 Uiso 0.572(8) 1 calc PR A 1
H30C H 0.8259 0.6621 0.4844 0.125 Uiso 0.572(8) 1 calc PR A 1
C29A C 0.7643(15) 0.7086(8) 0.4054(7) 0.149(6) Uani 0.428(8) 1 d P A 2
H29C H 0.7916 0.7482 0.4434 0.179 Uiso 0.428(8) 1 calc PR A 2
H29D H 0.6737 0.7253 0.3844 0.179 Uiso 0.428(8) 1 calc PR A 2
C30A C 0.7537(5) 0.6316(4) 0.4347(3) 0.0545(18) Uani 0.428(8) 1 d P A 2
H30D H 0.6827 0.6324 0.4663 0.082 Uiso 0.428(8) 1 calc PR A 2
H30E H 0.8396 0.6168 0.4609 0.082 Uiso 0.428(8) 1 calc PR A 2
H30F H 0.7312 0.5909 0.3977 0.082 Uiso 0.428(8) 1 calc PR A 2
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 0 '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'
O O 0.0106 0.006 '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
O1 Li1 N1 133.45(15) . . ?
O1 Li1 N2 116.27(13) . . ?
N1 Li1 N2 104.34(12) . . ?
O2 Li2 N2 135.52(15) . . ?
O2 Li2 N1 114.72(13) . . ?
N2 Li2 N1 104.13(12) . . ?
C14 O1 C12 114.46(13) . . ?
C14 O1 Li1 118.74(13) . . ?
C12 O1 Li1 114.88(13) . . ?
C29A O2 C27 105.0(5) . . ?
C29A O2 C29 28.4(8) . . ?
C27 O2 C29 122.2(3) . . ?
C29A O2 Li2 136.9(6) . . ?
C27 O2 Li2 117.91(17) . . ?
C29 O2 Li2 114.1(2) . . ?
C1 N1 C7 117.50(11) . . ?
C1 N1 Li1 121.74(12) . . ?
C7 N1 Li1 119.21(12) . . ?
C1 N1 Li2 91.63(11) . . ?
C7 N1 Li2 115.45(12) . . ?
Li1 N1 Li2 75.83(11) . . ?
C16 N2 C22 117.40(11) . . ?
C16 N2 Li2 121.24(12) . . ?
C22 N2 Li2 118.83(12) . . ?
C16 N2 Li1 93.27(11) . . ?
C22 N2 Li1 117.15(12) . . ?
Li2 N2 Li1 75.70(11) . . ?
N1 C1 C6 117.91(12) . . ?
N1 C1 C2 127.33(13) . . ?
C6 C1 C2 114.71(13) . . ?
C3 C2 C1 121.71(14) . . ?
C2 C3 C4 121.97(14) . . ?
C3 C4 C5 117.91(15) . . ?
C6 C5 C4 120.92(15) . . ?
C5 C6 C1 122.74(13) . . ?
N1 C7 C8 117.04(13) . . ?
C9 C8 C11 109.85(13) . . ?
C9 C8 C10 109.46(14) . . ?
C11 C8 C10 109.17(14) . . ?
C9 C8 C7 107.53(13) . . ?
C11 C8 C7 111.09(13) . . ?
C10 C8 C7 109.70(12) . . ?
O1 C12 C13 109.65(14) . . ?
O1 C14 C15 109.95(15) . . ?
N2 C16 C21 118.06(12) . . ?
N2 C16 C17 127.40(13) . . ?
C21 C16 C17 114.50(13) . . ?
C18 C17 C16 121.72(14) . . ?
C17 C18 C19 122.09(14) . . ?
C18 C19 C20 117.75(15) . . ?
C21 C20 C19 120.99(15) . . ?
C20 C21 C16 122.94(14) . . ?
N2 C22 C23 116.72(12) . . ?
C25 C23 C26 109.49(14) . . ?
C25 C23 C24 109.06(14) . . ?
C26 C23 C24 109.12(14) . . ?
C25 C23 C22 107.63(13) . . ?
C26 C23 C22 111.39(13) . . ?
C24 C23 C22 110.12(12) . . ?
O2 C27 C28 113.27(18) . . ?
O2 C29 C30 112.3(3) . . ?
C30A C29A O2 116.8(8) . . ?
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
Li1 O1 1.983(3) . ?
Li1 N1 2.011(3) . ?
Li1 N2 2.065(3) . ?
Li2 O2 1.947(3) . ?
Li2 N2 2.017(3) . ?
Li2 N1 2.065(3) . ?
O1 C14 1.422(2) . ?
O1 C12 1.436(2) . ?
O2 C29A 1.360(8) . ?
O2 C27 1.430(3) . ?
O2 C29 1.448(5) . ?
N1 C1 1.3730(19) . ?
N1 C7 1.4598(18) . ?
N2 C16 1.3717(19) . ?
N2 C22 1.4646(18) . ?
C1 C6 1.424(2) . ?
C1 C2 1.4254(19) . ?
C2 C3 1.385(2) . ?
C3 C4 1.386(2) . ?
C4 C5 1.391(2) . ?
C5 C6 1.383(2) . ?
C7 C8 1.548(2) . ?
C8 C9 1.528(2) . ?
C8 C11 1.531(2) . ?
C8 C10 1.532(2) . ?
C12 C13 1.489(2) . ?
C14 C15 1.491(3) . ?
C16 C21 1.425(2) . ?
C16 C17 1.4271(19) . ?
C17 C18 1.383(2) . ?
C18 C19 1.389(2) . ?
C19 C20 1.390(2) . ?
C20 C21 1.381(2) . ?
C22 C23 1.550(2) . ?
C23 C25 1.526(2) . ?
C23 C26 1.524(2) . ?
C23 C24 1.530(2) . ?
C27 C28 1.449(3) . ?
C29 C30 1.517(7) . ?
C29A C30A 1.376(13) . ?
