#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/70/2237005.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_2237005
loop_
_publ_author_name
'Chen, Juan'
'Yuan, Li'
_publ_section_title
;
 Bis[μ-N-(tert-butyldimethylsilyl)quinolin-8-aminato-1:2κ²N¹,N⁸:N⁸](N,N,N',N'-tetramethylethane-1,2-diamine-1κ²N,N')lithiumsodium
;
_journal_coeditor_code           RK2385
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1474
_journal_paper_doi               10.1107/S160053681204576X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Li Na (C15 H21 N2 Si)2 (C6 H16 N2)]'
_chemical_formula_moiety         'C36 H58 Li N6 Na Si2'
_chemical_formula_sum            'C36 H58 Li N6 Na Si2'
_chemical_formula_weight         660.99
_chemical_name_systematic
;
Bis[μ-N-(tert-butyldimethylsilyl)quinolin-8-aminato-
1:2κ²N¹,N⁸:N⁸](N,N,N',
N'-tetramethylethane-1,2-diamine-1κ²N,N')lithiumsodium
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.794(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.653(2)
_cell_length_b                   18.542(3)
_cell_length_c                   18.296(3)
_cell_measurement_reflns_used    3078
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.486
_cell_measurement_theta_min      2.237
_cell_volume                     4063.6(11)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0780
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11843
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.9747
_exptl_absorpt_correction_T_min  0.9624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.264
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         4001
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1027P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1953
_reflns_number_gt                2128
_reflns_number_total             4001
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            rk2385.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2237005
_cod_database_fobs_code          2237005
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_type_symbol
_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_symmetry_multiplicity
Si Si1 0.79825(8) 0.03304(5) 0.11244(5) 0.0488(3) Uani d . 1 1
Na Na1 1.0000 -0.04676(9) 0.2500 0.0575(5) Uani d S 1 2
Li Li1 1.0000 0.1121(4) 0.2500 0.0521(19) Uani d S 1 2
N N1 0.9134(3) 0.16649(16) 0.30734(17) 0.0624(8) Uani d . 1 1
N N2 0.8563(2) 0.05043(13) 0.20820(14) 0.0464(7) Uani d . 1 1
N N3 1.0507(4) -0.15746(18) 0.1852(2) 0.0823(11) Uani d . 1 1
C C1 0.9395(4) 0.2245(2) 0.3513(2) 0.0823(13) Uani d . 1 1
H H1A 0.9985 0.2530 0.3483 0.099 Uiso calc R 1 1
C C2 0.8829(5) 0.2453(3) 0.4023(3) 0.110(2) Uani d . 1 1
H H2A 0.9042 0.2862 0.4329 0.132 Uiso calc R 1 1
C C3 0.7970(5) 0.2042(4) 0.4057(3) 0.108(2) Uani d . 1 1
H H3A 0.7591 0.2170 0.4397 0.130 Uiso calc R 1 1
C C4 0.7628(4) 0.1428(3) 0.3595(2) 0.0729(12) Uani d . 1 1
C C5 0.6742(4) 0.1006(4) 0.3607(3) 0.1021(18) Uani d . 1 1
H H5 0.6337 0.1117 0.3936 0.122 Uiso calc R 1 1
C C6 0.6462(4) 0.0414(3) 0.3125(3) 0.0976(17) Uani d . 1 1
H H6 0.5867 0.0124 0.3134 0.117 Uiso calc R 1 1
C C7 0.7050(3) 0.0245(2) 0.2627(2) 0.0748(12) Uani d . 1 1
H H7 0.6828 -0.0158 0.2311 0.090 Uiso calc R 1 1
C C8 0.7963(3) 0.06445(18) 0.25710(18) 0.0504(8) Uani d . 1 1
C C9 0.8254(3) 0.1260(2) 0.30898(18) 0.0545(9) Uani d . 1 1
C C10 0.9163(3) 0.0301(2) 0.0717(2) 0.0705(11) Uani d . 1 1
H H10A 0.8932 0.0517 0.0214 0.106 Uiso calc R 1 1
H H10B 0.9374 -0.0192 0.0679 0.106 Uiso calc R 1 1
H H10C 0.9789 0.0561 0.1050 0.106 Uiso calc R 1 1
C C11 0.7207(4) -0.05573(19) 0.0867(2) 0.0783(13) Uani d . 1 1
H H11A 0.6527 -0.0483 0.0447 0.117 Uiso calc R 1 1
H H11B 0.7035 -0.0738 0.1307 0.117 Uiso calc R 1 1
H H11C 0.7666 -0.0900 0.0715 0.117 Uiso calc R 1 1
C C12 0.6967(3) 0.10601(18) 0.05847(19) 0.0565(9) Uani d . 1 1
C C13 0.7530(4) 0.1797(2) 0.0801(3) 0.0890(14) Uani d . 1 1
H H13A 0.7026 0.2170 0.0534 0.134 Uiso calc R 1 1
H H13B 0.8195 0.1814 0.0657 0.134 Uiso calc R 1 1
H H13C 0.7721 0.1869 0.1348 0.134 Uiso calc R 1 1
C C14 0.5904(3) 0.1066(2) 0.0806(2) 0.0827(13) Uani d . 1 1
H H14A 0.5416 0.1439 0.0525 0.124 Uiso calc R 1 1
H H14B 0.6091 0.1154 0.1350 0.124 Uiso calc R 1 1
H H14C 0.5537 0.0607 0.0683 0.124 Uiso calc R 1 1
C C15 0.6644(4) 0.0951(3) -0.0291(2) 0.0963(16) Uani d . 1 1
H H15A 0.6132 0.1323 -0.0551 0.144 Uiso calc R 1 1
H H15B 0.6295 0.0489 -0.0426 0.144 Uiso calc R 1 1
H H15C 0.7301 0.0974 -0.0443 0.144 Uiso calc R 1 1
C C16 1.1708(6) -0.1574(4) 0.2048(4) 0.154(3) Uani d . 1 1
H H16A 1.1936 -0.1983 0.1814 0.231 Uiso calc R 1 1
H H16B 1.2042 -0.1601 0.2598 0.231 Uiso calc R 1 1
H H16C 1.1942 -0.1139 0.1861 0.231 Uiso calc R 1 1
C C17 1.0020(6) -0.1651(3) 0.1025(3) 0.142(3) Uani d . 1 1
H H17A 1.0289 -0.2087 0.0862 0.213 Uiso calc R 1 1
H H17B 1.0226 -0.1246 0.0774 0.213 Uiso calc R 1 1
H H17C 0.9222 -0.1673 0.0889 0.213 Uiso calc R 1 1
C C18 1.0183(8) -0.2176(3) 0.2183(4) 0.168(3) Uani d D 1 1
H H18A 0.9594 -0.2404 0.1771 0.201 Uiso calc R 1 1
H H18B 1.0813 -0.2504 0.2310 0.201 Uiso calc R 1 1
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'
Na Na 0.0362 0.0249 '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_1
_geom_angle_site_symmetry_3
_geom_angle
N2 Si1 C10 . . 106.28(15)
N2 Si1 C11 . . 116.03(15)
C10 Si1 C11 . . 106.90(18)
N2 Si1 C12 . . 113.25(14)
C10 Si1 C12 . . 107.79(17)
C11 Si1 C12 . . 106.18(17)
N2 Si1 Na1 . . 47.72(9)
C10 Si1 Na1 . . 76.71(12)
C11 Si1 Na1 . . 90.67(12)
C12 Si1 Na1 . . 159.86(11)
N2 Na1 N2 2_755 . 87.66(13)
N2 Na1 N3 2_755 . 117.08(11)
N2 Na1 N3 . . 134.80(10)
N2 Na1 N3 2_755 2_755 134.80(10)
N2 Na1 N3 . 2_755 117.08(11)
N3 Na1 N3 . 2_755 72.99(19)
N2 Na1 Li1 2_755 . 43.83(6)
N2 Na1 Li1 . . 43.83(6)
N3 Na1 Li1 . . 143.51(9)
N3 Na1 Li1 2_755 . 143.51(9)
N2 Na1 Si1 2_755 2_755 30.20(6)
N2 Na1 Si1 . 2_755 102.57(8)
N3 Na1 Si1 . 2_755 117.78(10)
N3 Na1 Si1 2_755 2_755 104.74(9)
Li1 Na1 Si1 . 2_755 63.38(3)
N2 Na1 Si1 2_755 . 102.57(8)
N2 Na1 Si1 . . 30.20(6)
N3 Na1 Si1 . . 104.74(9)
N3 Na1 Si1 2_755 . 117.78(10)
Li1 Na1 Si1 . . 63.38(3)
Si1 Na1 Si1 2_755 . 126.75(6)
N1 Li1 N1 2_755 . 119.9(4)
N1 Li1 N2 2_755 . 130.03(11)
N1 Li1 N2 . . 84.77(12)
N1 Li1 N2 2_755 2_755 84.77(12)
N1 Li1 N2 . 2_755 130.03(11)
N2 Li1 N2 . 2_755 113.1(4)
N1 Li1 C9 2_755 2_755 27.53(11)
N1 Li1 C9 . 2_755 142.5(3)
N2 Li1 C9 . 2_755 128.53(19)
N2 Li1 C9 2_755 2_755 58.66(11)
N1 Li1 C9 2_755 . 142.5(3)
N1 Li1 C9 . . 27.53(11)
N2 Li1 C9 . . 58.66(11)
N2 Li1 C9 2_755 . 128.53(19)
C9 Li1 C9 2_755 . 169.3(3)
N1 Li1 C8 2_755 . 148.81(15)
N1 Li1 C8 . . 57.60(12)
N2 Li1 C8 . . 28.62(10)
N2 Li1 C8 2_755 . 121.7(3)
C9 Li1 C8 2_755 . 157.1(2)
C9 Li1 C8 . . 30.47(10)
N1 Li1 C8 2_755 2_755 57.60(12)
N1 Li1 C8 . 2_755 148.81(15)
N2 Li1 C8 . 2_755 121.7(3)
N2 Li1 C8 2_755 2_755 28.62(10)
C9 Li1 C8 2_755 2_755 30.47(10)
C9 Li1 C8 . 2_755 157.1(2)
C8 Li1 C8 . 2_755 142.7(3)
N1 Li1 Na1 2_755 . 120.0(2)
N1 Li1 Na1 . . 120.0(2)
N2 Li1 Na1 . . 56.53(18)
N2 Li1 Na1 2_755 . 56.53(18)
C9 Li1 Na1 2_755 . 95.34(17)
C9 Li1 Na1 . . 95.34(17)
C8 Li1 Na1 . . 71.37(16)
C8 Li1 Na1 2_755 . 71.37(16)
C1 N1 C9 . . 119.0(4)
C1 N1 Li1 . . 130.8(3)
C9 N1 Li1 . . 108.9(3)
C8 N2 Si1 . . 124.2(2)
C8 N2 Li1 . . 105.0(2)
Si1 N2 Li1 . . 121.45(14)
C8 N2 Na1 . . 115.99(18)
Si1 N2 Na1 . . 102.07(12)
Li1 N2 Na1 . . 79.64(19)
C18 N3 C16 . . 109.0(6)
C18 N3 C17 . . 106.9(5)
C16 N3 C17 . . 108.6(5)
C18 N3 Na1 . . 106.8(3)
C16 N3 Na1 . . 106.6(3)
C17 N3 Na1 . . 118.6(3)
N1 C1 C2 . . 123.3(5)
N1 C1 H1A . . 118.4
C2 C1 H1A . . 118.4
C3 C2 C1 . . 118.0(5)
C3 C2 H2A . . 121.0
C1 C2 H2A . . 121.0
C2 C3 C4 . . 121.9(5)
C2 C3 H3A . . 119.0
C4 C3 H3A . . 119.0
C5 C4 C3 . . 123.3(5)
C5 C4 C9 . . 120.7(4)
C3 C4 C9 . . 116.0(5)
C4 C5 C6 . . 119.0(4)
C4 C5 H5 . . 120.5
C6 C5 H5 . . 120.5
C5 C6 C7 . . 121.3(5)
C5 C6 H6 . . 119.4
C7 C6 H6 . . 119.4
C6 C7 C8 . . 123.8(4)
C6 C7 H7 . . 118.1
C8 C7 H7 . . 118.1
N2 C8 C7 . . 126.1(3)
N2 C8 C9 . . 119.8(3)
C7 C8 C9 . . 114.1(3)
N2 C8 Li1 . . 46.37(17)
C7 C8 Li1 . . 166.6(3)
C9 C8 Li1 . . 74.7(2)
N1 C9 C4 . . 121.6(4)
N1 C9 C8 . . 117.3(3)
C4 C9 C8 . . 121.0(4)
N1 C9 Li1 . . 43.6(2)
C4 C9 Li1 . . 161.7(3)
C8 C9 Li1 . . 74.8(2)
Si1 C10 H10A . . 109.5
Si1 C10 H10B . . 109.5
H10A C10 H10B . . 109.5
Si1 C10 H10C . . 109.5
H10A C10 H10C . . 109.5
H10B C10 H10C . . 109.5
Si1 C11 H11A . . 109.5
Si1 C11 H11B . . 109.5
H11A C11 H11B . . 109.5
Si1 C11 H11C . . 109.5
H11A C11 H11C . . 109.5
H11B C11 H11C . . 109.5
C14 C12 C15 . . 108.5(3)
C14 C12 C13 . . 107.5(3)
C15 C12 C13 . . 109.4(3)
C14 C12 Si1 . . 111.8(2)
C15 C12 Si1 . . 110.8(3)
C13 C12 Si1 . . 108.6(3)
C12 C13 H13A . . 109.5
C12 C13 H13B . . 109.5
H13A C13 H13B . . 109.5
C12 C13 H13C . . 109.5
H13A C13 H13C . . 109.5
H13B C13 H13C . . 109.5
C12 C14 H14A . . 109.5
C12 C14 H14B . . 109.5
H14A C14 H14B . . 109.5
C12 C14 H14C . . 109.5
H14A C14 H14C . . 109.5
H14B C14 H14C . . 109.5
C12 C15 H15A . . 109.5
C12 C15 H15B . . 109.5
H15A C15 H15B . . 109.5
C12 C15 H15C . . 109.5
H15A C15 H15C . . 109.5
H15B C15 H15C . . 109.5
N3 C16 H16A . . 109.5
N3 C16 H16B . . 109.5
H16A C16 H16B . . 109.5
N3 C16 H16C . . 109.5
H16A C16 H16C . . 109.5
H16B C16 H16C . . 109.5
N3 C17 H17A . . 109.5
N3 C17 H17B . . 109.5
H17A C17 H17B . . 109.5
N3 C17 H17C . . 109.5
H17A C17 H17C . . 109.5
H17B C17 H17C . . 109.5
C18 C18 N3 2_755 . 126.3(3)
C18 C18 H18A 2_755 . 105.8
N3 C18 H18A . . 105.8
C18 C18 H18B 2_755 . 105.8
N3 C18 H18B . . 105.8
H18A C18 H18B . . 106.2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Si1 N2 . 1.698(3)
Si1 C10 . 1.873(4)
Si1 C11 . 1.896(4)
Si1 C12 . 1.908(3)
Si1 Na1 . 3.3014(12)
Na1 N2 2_755 2.498(3)
Na1 N2 . 2.498(3)
Na1 N3 . 2.553(4)
Na1 N3 2_755 2.553(4)
Na1 Li1 . 2.946(7)
Na1 Si1 2_755 3.3014(12)
Li1 N1 2_755 2.015(5)
Li1 N1 . 2.015(5)
Li1 N2 . 2.074(5)
Li1 N2 2_755 2.074(5)
Li1 C9 2_755 2.765(4)
Li1 C9 . 2.765(4)
Li1 C8 . 2.768(4)
Li1 C8 2_755 2.768(4)
N1 C1 . 1.321(4)
N1 C9 . 1.351(5)
N2 C8 . 1.373(4)
N3 C18 . 1.392(6)
N3 C16 . 1.444(7)
N3 C17 . 1.446(5)
C1 C2 . 1.400(7)
C1 H1A . 0.9300
C2 C3 . 1.345(8)
C2 H2A . 0.9300
C3 C4 . 1.401(7)
C3 H3A . 0.9300
C4 C5 . 1.373(7)
C4 C9 . 1.432(5)
C5 C6 . 1.381(7)
C5 H5 . 0.9300
C6 C7 . 1.386(6)
C6 H6 . 0.9300
C7 C8 . 1.403(5)
C7 H7 . 0.9300
C8 C9 . 1.454(5)
C10 H10A . 0.9600
C10 H10B . 0.9600
C10 H10C . 0.9600
C11 H11A . 0.9600
C11 H11B . 0.9600
C11 H11C . 0.9600
C12 C14 . 1.524(5)
C12 C15 . 1.533(5)
C12 C13 . 1.533(5)
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 C18 2_755 1.379(10)
C18 H18A . 0.9700
C18 H18B . 0.9700
