#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:09:30 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179882 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/78/7017855.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_7017855
loop_
_publ_author_name
'Colquhoun, Victoria P.'
'Strohmann, Carsten'
_publ_section_title
;
 Structural influence of steric factors and donor functions on lithium
 silylamides in non-coordinating solvents.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1897
_journal_page_last               1902
_journal_paper_doi               10.1039/c1dt11550b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C22 H50 Li2 N4 Si2'
_chemical_formula_weight         440.72
_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_date             2011-06-29T15:22:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 122.498(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.239(4)
_cell_length_b                   8.340(2)
_cell_length_c                   17.941(4)
_cell_measurement_reflns_used    13062
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.17
_cell_volume                     2806.5(12)
_computing_cell_refinement       'Cell in IPDS (Stoe & Cie, 1999)'
_computing_data_collection       'Expose in IPDS (Stoe & Cie, 1999)'
_computing_data_reduction        'Integrate in IPDS (Stoe & Cie, 1999)'
_computing_molecular_graphics
;
Ortep-3 (Farrugia, 1997) and Schakal 92 (Keller
1992)
;
_computing_publication_material  'wingx (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13062
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.9590
_exptl_absorpt_correction_T_min  0.9459
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT in IPDS (Stoe & Cie, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.5
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1351P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.162
_refine_ls_wR_factor_ref         0.1705
_reflns_number_gt                2257
_reflns_number_total             2757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11550b.txt
_cod_data_source_block           vc060408
_cod_original_cell_volume        2806.8(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7017855
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.33552(10) 0.1109(3) 0.51980(14) 0.0341(5) Uani 1 1 d .
H1A H 0.3383 0.0455 0.5669 0.051 Uiso 1 1 calc R
H1B H 0.3309 0.0407 0.4732 0.051 Uiso 1 1 calc R
H1C H 0.2939 0.1817 0.495 0.051 Uiso 1 1 calc R
C2 C 0.41062(11) 0.3202(3) 0.46327(13) 0.0356(5) Uani 1 1 d .
H2A H 0.3657 0.3796 0.4291 0.053 Uiso 1 1 calc R
H2B H 0.4111 0.2323 0.4273 0.053 Uiso 1 1 calc R
H2C H 0.4507 0.3925 0.48 0.053 Uiso 1 1 calc R
C3 C 0.39100(10) 0.5200(2) 0.61094(12) 0.0295(4) Uani 1 1 d .
H3 H 0.3501 0.4965 0.5497 0.035 Uiso 1 1 calc R
C4 C 0.43161(13) 0.6642(2) 0.60593(17) 0.0432(5) Uani 1 1 d .
H4A H 0.4709 0.6928 0.6656 0.065 Uiso 1 1 calc R
H4B H 0.3991 0.7555 0.5794 0.065 Uiso 1 1 calc R
H4C H 0.4508 0.6363 0.5696 0.065 Uiso 1 1 calc R
C5 C 0.36048(12) 0.5647(3) 0.66673(17) 0.0430(5) Uani 1 1 d .
H5A H 0.3307 0.4767 0.6654 0.064 Uiso 1 1 calc R
H5B H 0.3315 0.662 0.6427 0.064 Uiso 1 1 calc R
H5C H 0.3996 0.5842 0.7278 0.064 Uiso 1 1 calc R
C6 C 0.49493(9) 0.0844(2) 0.62537(12) 0.0257(4) Uani 1 1 d .
H6A H 0.4876 0.0212 0.6665 0.031 Uiso 1 1 calc R
H6B H 0.4918 0.0092 0.5807 0.031 Uiso 1 1 calc R
C7 C 0.58964(10) 0.2006(2) 0.61404(13) 0.0305(4) Uani 1 1 d .
H7A H 0.5558 0.2822 0.5727 0.037 Uiso 1 1 calc R
H7B H 0.5866 0.1059 0.5789 0.037 Uiso 1 1 calc R
C8 C 0.66496(11) 0.2683(3) 0.66120(15) 0.0371(5) Uani 1 1 d .
H8A H 0.667 0.369 0.6917 0.044 Uiso 1 1 calc R
H8B H 0.6774 0.2937 0.6172 0.044 Uiso 1 1 calc R
C9 C 0.71912(11) 0.1486(3) 0.72873(15) 0.0426(5) Uani 1 1 d .
H9A H 0.7224 0.0541 0.6977 0.051 Uiso 1 1 calc R
H9B H 0.7668 0.1993 0.7631 0.051 Uiso 1 1 calc R
C10 C 0.69585(10) 0.0959(3) 0.79093(14) 0.0360(5) Uani 1 1 d .
H10A H 0.6986 0.1881 0.8274 0.043 Uiso 1 1 calc R
H10B H 0.7285 0.0115 0.8312 0.043 Uiso 1 1 calc R
C11 C 0.61965(9) 0.0311(2) 0.73879(12) 0.0297(4) Uani 1 1 d .
H11A H 0.6177 -0.0652 0.7053 0.036 Uiso 1 1 calc R
H11B H 0.6055 -0.0012 0.7804 0.036 Uiso 1 1 calc R
Li Li 0.45604(16) 0.3458(4) 0.7677(2) 0.0289(7) Uani 1 1 d .
N2 N 0.56853(7) 0.15316(17) 0.67626(10) 0.0233(4) Uani 1 1 d .
N1 N 0.43619(8) 0.37458(17) 0.64463(10) 0.0247(4) Uani 1 1 d .
Si Si 0.41913(2) 0.23560(6) 0.56645(3) 0.0238(2) Uani 1 1 d .
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'
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
N1 C3 C5 112.07(16) . .
N1 C3 C4 111.95(16) . .
C5 C3 C4 109.24(17) . .
N2 C6 Si 115.88(11) . .
N2 C6 Li 50.83(10) . 2_656
Si C6 Li 76.13(9) . 2_656
N2 C7 C8 112.36(16) . .
C7 C8 C9 111.15(17) . .
C10 C9 C8 109.57(17) . .
C9 C10 C11 110.76(17) . .
N2 C11 C10 111.50(16) . .
N1 Li N1 107.61(15) . 2_656
N1 Li N2 130.43(17) . 2_656
N1 Li N2 102.58(14) 2_656 2_656
N1 Li Li 55.33(14) . 2_656
N1 Li Li 53.95(13) 2_656 2_656
N2 Li Li 126.22(11) 2_656 2_656
N1 Li C6 129.52(15) . 2_656
N1 Li C6 72.11(10) 2_656 2_656
N2 Li C6 33.21(7) 2_656 2_656
Li Li C6 96.55(12) 2_656 2_656
N1 Li Si 132.91(14) . 2_656
N1 Li Si 34.70(7) 2_656 2_656
N2 Li Si 67.91(9) 2_656 2_656
Li Li Si 78.63(14) 2_656 2_656
C6 Li Si 39.33(6) 2_656 2_656
C7 N2 C11 109.15(14) . .
C7 N2 C6 109.21(14) . .
C11 N2 C6 109.88(13) . .
C7 N2 Li 115.03(14) . 2_656
C11 N2 Li 116.66(14) . 2_656
C6 N2 Li 95.97(13) . 2_656
C3 N1 Si 114.86(12) . .
C3 N1 Li 104.19(14) . .
Si N1 Li 129.98(12) . .
C3 N1 Li 131.64(15) . 2_656
Si N1 Li 101.74(11) . 2_656
Li N1 Li 70.72(15) . 2_656
N1 Si C1 118.15(9) . .
N1 Si C2 114.45(9) . .
C1 Si C2 102.39(10) . .
N1 Si C6 104.77(8) . .
C1 Si C6 104.36(9) . .
C2 Si C6 112.52(9) . .
N1 Si Li 43.56(8) . 2_656
C1 Si Li 142.70(10) . 2_656
C2 Si Li 114.82(9) . 2_656
C6 Si Li 64.53(8) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 Si 1.889(2) .
C2 Si 1.893(2) .
C3 N1 1.481(2) .
C3 C5 1.527(3) .
C3 C4 1.536(3) .
C6 N2 1.495(2) .
C6 Si 1.9065(18) .
C6 Li 2.716(3) 2_656
C7 N2 1.479(2) .
C7 C8 1.522(3) .
C8 C9 1.532(3) .
C9 C10 1.526(3) .
C10 C11 1.528(3) .
C11 N2 1.489(2) .
Li N1 2.021(4) .
Li N1 2.055(3) 2_656
Li N2 2.117(3) 2_656
Li Li 2.359(6) 2_656
Li C6 2.716(3) 2_656
Li Si 2.920(3) 2_656
N2 Li 2.117(3) 2_656
N1 Si 1.6981(15) .
N1 Li 2.055(4) 2_656
Si Li 2.920(3) 2_656
