#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:27:31 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179791 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/87/7008733.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_7008733
loop_
_publ_author_name
'Gehrhus, Barbara'
'Hitchcock, Peter B.'
'Parruci, Massimo'
_publ_section_title
;
 Reaction of the stable silylene Si[(NCH2But)2C6H4-1,2] with lithium
 amides
;
_journal_issue                   16
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2720
_journal_page_last               2725
_journal_paper_doi               10.1039/b506610g
_journal_year                    2005
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C35 H60 Li N3 O2 Si2'
_chemical_formula_sum            'C35 H60 Li N3 O2 Si2'
_chemical_formula_weight         617.98
_chemical_name_common
;
[C6H4(NCH2tBu)2Si(Li(thf)2}{N(SiMe3)(C6H3Me2)}]
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2000-10-17T09:52:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.2629(10)
_cell_length_b                   19.5814(7)
_cell_length_c                   21.4761(11)
_cell_measurement_reflns_used    14679
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     7680.1(6)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0781
_diffrn_reflns_av_unetI/netI     0.059
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20489
_diffrn_reflns_theta_full        22.98
_diffrn_reflns_theta_max         22.98
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.05
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.01
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         5293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.01
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.062
_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)+(0.0922P)²+7.2912P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                3844
_reflns_number_total             5293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b506610g.txt
_cod_data_source_block           (3)-oct2400
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7008733
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
Li Li 0.4185(5) 0.0344(3) 0.7265(3) 0.066(2) Uani 1 1 d . . .
Si1 Si 0.42786(5) 0.14762(4) 0.66142(4) 0.0320(3) Uani 1 1 d . . .
Si2 Si 0.56527(6) 0.20109(5) 0.57872(4) 0.0393(3) Uani 1 1 d . . .
O1 O 0.38639(17) -0.05544(13) 0.70448(17) 0.0752(10) Uani 1 1 d . . .
O2 O 0.4434(2) 0.02194(16) 0.81429(15) 0.0816(10) Uani 1 1 d . . .
N1 N 0.41076(15) 0.22811(13) 0.69931(12) 0.0333(7) Uani 1 1 d . . .
N2 N 0.37531(15) 0.18175(13) 0.59778(12) 0.0350(7) Uani 1 1 d . . .
N3 N 0.52173(15) 0.14792(13) 0.63214(12) 0.0346(7) Uani 1 1 d . . .
C1 C 0.38819(18) 0.27948(16) 0.65884(16) 0.0354(8) Uani 1 1 d . . .
C2 C 0.36711(18) 0.25275(17) 0.60002(15) 0.0357(8) Uani 1 1 d . . .
C3 C 0.3430(2) 0.2971(2) 0.55381(17) 0.0476(10) Uani 1 1 d . . .
H3 H 0.3277 0.2796 0.5146 0.057 Uiso 1 1 calc R . .
C4 C 0.3411(2) 0.3673(2) 0.5649(2) 0.0591(12) Uani 1 1 d . . .
H4 H 0.3252 0.3975 0.533 0.071 Uiso 1 1 calc R . .
C5 C 0.3620(2) 0.3931(2) 0.6214(2) 0.0556(11) Uani 1 1 d . . .
H5 H 0.3604 0.4409 0.6285 0.067 Uiso 1 1 calc R . .
C6 C 0.3858(2) 0.34949(18) 0.66869(18) 0.0451(9) Uani 1 1 d . . .
H6 H 0.4003 0.3678 0.7077 0.054 Uiso 1 1 calc R . .
C7 C 0.42224(19) 0.24185(18) 0.76492(15) 0.0379(8) Uani 1 1 d . . .
H7A H 0.4425 0.2886 0.769 0.045 Uiso 1 1 calc R . .
H7B H 0.4598 0.2097 0.7806 0.045 Uiso 1 1 calc R . .
C8 C 0.3545(2) 0.23631(18) 0.80735(15) 0.0405(9) Uani 1 1 d . . .
C9 C 0.3220(2) 0.16475(19) 0.80285(18) 0.0517(10) Uani 1 1 d . . .
H9A H 0.305 0.1565 0.7602 0.078 Uiso 1 1 calc R . .
H9B H 0.2807 0.1607 0.8317 0.078 Uiso 1 1 calc R . .
H9C H 0.3595 0.131 0.8137 0.078 Uiso 1 1 calc R . .
C10 C 0.3806(3) 0.2492(3) 0.87406(18) 0.0743(14) Uani 1 1 d . . .
H10A H 0.4016 0.2952 0.877 0.111 Uiso 1 1 calc R . .
H10B H 0.4178 0.2154 0.8852 0.111 Uiso 1 1 calc R . .
H10C H 0.339 0.2454 0.9027 0.111 Uiso 1 1 calc R . .
C11 C 0.2957(2) 0.2887(2) 0.7909(2) 0.0548(11) Uani 1 1 d . . .
H11A H 0.278 0.2802 0.7486 0.082 Uiso 1 1 calc R . .
H11B H 0.3165 0.3348 0.7934 0.082 Uiso 1 1 calc R . .
H11C H 0.2549 0.2848 0.8203 0.082 Uiso 1 1 calc R . .
C12 C 0.3514(2) 0.14368(19) 0.54286(16) 0.0445(9) Uani 1 1 d . . .
H12A H 0.3852 0.1047 0.5367 0.053 Uiso 1 1 calc R . .
H12B H 0.3561 0.1738 0.5061 0.053 Uiso 1 1 calc R . .
C13 C 0.2721(2) 0.1157(2) 0.54474(19) 0.0575(11) Uani 1 1 d . . .
C14 C 0.2167(3) 0.1712(3) 0.5562(4) 0.118(2) Uani 1 1 d . . .
H14A H 0.2204 0.2056 0.5232 0.177 Uiso 1 1 calc R . .
H14B H 0.2263 0.1925 0.5966 0.177 Uiso 1 1 calc R . .
H14C H 0.1674 0.1514 0.5561 0.177 Uiso 1 1 calc R . .
C15 C 0.2668(3) 0.0622(3) 0.5941(3) 0.105(2) Uani 1 1 d . . .
H15A H 0.3028 0.0262 0.5859 0.158 Uiso 1 1 calc R . .
H15B H 0.2175 0.0424 0.5939 0.158 Uiso 1 1 calc R . .
H15C H 0.2766 0.0828 0.6348 0.158 Uiso 1 1 calc R . .
C16 C 0.2588(4) 0.0831(5) 0.4816(3) 0.150(3) Uani 1 1 d . . .
H16A H 0.2613 0.1181 0.4491 0.225 Uiso 1 1 calc R . .
H16B H 0.2103 0.0617 0.4811 0.225 Uiso 1 1 calc R . .
H16C H 0.2963 0.0483 0.4738 0.225 Uiso 1 1 calc R . .
C17 C 0.6588(2) 0.1667(2) 0.5621(2) 0.0583(11) Uani 1 1 d . . .
H17A H 0.6863 0.1628 0.6011 0.087 Uiso 1 1 calc R . .
H17B H 0.6845 0.1978 0.5338 0.087 Uiso 1 1 calc R . .
H17C H 0.6545 0.1216 0.5427 0.087 Uiso 1 1 calc R . .
C18 C 0.5175(2) 0.2066(2) 0.50240(17) 0.0563(11) Uani 1 1 d . . .
H18A H 0.5112 0.1606 0.4853 0.084 Uiso 1 1 calc R . .
H18B H 0.5468 0.2342 0.4736 0.084 Uiso 1 1 calc R . .
H18C H 0.4695 0.228 0.5082 0.084 Uiso 1 1 calc R . .
C19 C 0.5743(3) 0.29088(19) 0.6069(2) 0.0614(12) Uani 1 1 d . . .
H19A H 0.5992 0.2912 0.6473 0.092 Uiso 1 1 calc R . .
H19B H 0.5256 0.3112 0.6112 0.092 Uiso 1 1 calc R . .
H19C H 0.603 0.3174 0.5768 0.092 Uiso 1 1 calc R . .
C20 C 0.56658(19) 0.09514(18) 0.65973(15) 0.0383(8) Uani 1 1 d . . .
C21 C 0.5665(2) 0.02891(19) 0.63460(18) 0.0494(10) Uani 1 1 d . . .
C22 C 0.6101(3) -0.0211(2) 0.6611(2) 0.0642(12) Uani 1 1 d . . .
H22 H 0.6095 -0.0659 0.644 0.077 Uiso 1 1 calc R . .
C23 C 0.6538(3) -0.0079(2) 0.7111(2) 0.0689(13) Uani 1 1 d . . .
H23 H 0.6837 -0.0427 0.7284 0.083 Uiso 1 1 calc R . .
C24 C 0.6540(2) 0.0564(2) 0.7359(2) 0.0598(11) Uani 1 1 d . . .
H24 H 0.6843 0.0658 0.7708 0.072 Uiso 1 1 calc R . .
C25 C 0.6107(2) 0.10885(19) 0.71130(16) 0.0441(9) Uani 1 1 d . . .
C26 C 0.5218(3) 0.0124(2) 0.5779(2) 0.0648(12) Uani 1 1 d . . .
H26A H 0.5324 -0.0344 0.5645 0.097 Uiso 1 1 calc R . .
H26B H 0.5341 0.0443 0.5444 0.097 Uiso 1 1 calc R . .
H26C H 0.4696 0.0164 0.588 0.097 Uiso 1 1 calc R . .
C27 C 0.6143(2) 0.1788(2) 0.73967(18) 0.0511(10) Uani 1 1 d . . .
H27A H 0.6531 0.2052 0.7194 0.077 Uiso 1 1 calc R . .
H27B H 0.6249 0.1748 0.7843 0.077 Uiso 1 1 calc R . .
H27C H 0.5672 0.202 0.7339 0.077 Uiso 1 1 calc R . .
C28 C 0.3186(3) -0.0832(3) 0.6848(4) 0.109(2) Uani 1 1 d . . .
H28A H 0.2899 -0.0488 0.6615 0.131 Uiso 1 1 calc R . .
H28B H 0.2896 -0.0989 0.721 0.131 Uiso 1 1 calc R . .
C29 C 0.3379(3) -0.1418(3) 0.6437(3) 0.1015(19) Uani 1 1 d . . .
H29A H 0.303 -0.18 0.6495 0.122 Uiso 1 1 calc R . .
H29B H 0.3376 -0.1279 0.5994 0.122 Uiso 1 1 calc R . .
C30 C 0.4114(4) -0.1616(3) 0.6634(3) 0.102(2) Uani 1 1 d . . .
H30A H 0.4103 -0.2071 0.6835 0.122 Uiso 1 1 calc R . .
H30B H 0.4446 -0.1638 0.627 0.122 Uiso 1 1 calc R . .
C31 C 0.4361(3) -0.1118(2) 0.7061(3) 0.097(2) Uani 1 1 d . . .
H31A H 0.4859 -0.0964 0.6946 0.117 Uiso 1 1 calc R . .
H31B H 0.438 -0.1313 0.7486 0.117 Uiso 1 1 calc R . .
C32 C 0.4011(5) -0.0165(3) 0.8577(3) 0.137(3) Uani 1 1 d . . .
H32A H 0.4024 -0.0658 0.8476 0.165 Uiso 1 1 calc R . .
H32B H 0.3496 -0.0008 0.8582 0.165 Uiso 1 1 calc R . .
C33 C 0.4378(8) -0.0026(6) 0.9186(4) 0.227(7) Uani 1 1 d . . .
H33A H 0.4004 0.0111 0.9496 0.273 Uiso 1 1 calc R . .
H33B H 0.4614 -0.045 0.9337 0.273 Uiso 1 1 calc R . .
C34 C 0.4922(5) 0.0504(5) 0.9139(3) 0.138(3) Uani 1 1 d . . .
H34A H 0.5374 0.0375 0.9366 0.165 Uiso 1 1 calc R . .
H34B H 0.4735 0.094 0.9312 0.165 Uiso 1 1 calc R . .
C35 C 0.5062(4) 0.0566(4) 0.8481(3) 0.127(3) Uani 1 1 d . . .
H35A H 0.5532 0.0344 0.8373 0.152 Uiso 1 1 calc R . .
H35B H 0.509 0.1054 0.8361 0.152 Uiso 1 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 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Li O2 101.2(3) . . ?
O1 Li Si1 131.6(4) . . ?
O2 Li Si1 127.2(4) . . ?
N2 Si1 N1 85.73(12) . . ?
N2 Si1 N3 103.77(13) . . ?
N1 Si1 N3 108.39(13) . . ?
N2 Si1 Li 133.1(2) . . ?
N1 Si1 Li 119.13(19) . . ?
N3 Si1 Li 104.3(2) . . ?
N3 Si2 C18 113.68(17) . . ?
N3 Si2 C19 112.97(17) . . ?
C18 Si2 C19 105.8(2) . . ?
N3 Si2 C17 109.14(16) . . ?
C18 Si2 C17 106.30(19) . . ?
C19 Si2 C17 108.6(2) . . ?
C28 O1 C31 105.4(4) . . ?
C28 O1 Li 134.0(4) . . ?
C31 O1 Li 120.6(4) . . ?
C32 O2 C35 109.4(4) . . ?
C32 O2 Li 124.8(5) . . ?
C35 O2 Li 125.5(4) . . ?
C1 N1 C7 121.0(3) . . ?
C1 N1 Si1 113.7(2) . . ?
C7 N1 Si1 125.2(2) . . ?
C2 N2 C12 120.1(3) . . ?
C2 N2 Si1 113.6(2) . . ?
C12 N2 Si1 125.7(2) . . ?
C20 N3 Si2 116.0(2) . . ?
C20 N3 Si1 112.9(2) . . ?
Si2 N3 Si1 131.11(16) . . ?
C6 C1 N1 128.9(3) . . ?
C6 C1 C2 119.4(3) . . ?
N1 C1 C2 111.7(3) . . ?
C3 C2 N2 129.1(3) . . ?
C3 C2 C1 119.4(3) . . ?
N2 C2 C1 111.6(3) . . ?
C2 C3 C4 120.1(4) . . ?
C5 C4 C3 120.5(4) . . ?
C4 C5 C6 120.5(4) . . ?
C5 C6 C1 120.2(4) . . ?
N1 C7 C8 116.5(3) . . ?
C9 C8 C10 109.4(3) . . ?
C9 C8 C11 109.3(3) . . ?
C10 C8 C11 108.9(3) . . ?
C9 C8 C7 109.9(3) . . ?
C10 C8 C7 107.0(3) . . ?
C11 C8 C7 112.4(3) . . ?
N2 C12 C13 116.1(3) . . ?
C15 C13 C14 110.3(5) . . ?
C15 C13 C16 109.2(5) . . ?
C14 C13 C16 110.0(5) . . ?
C15 C13 C12 109.1(4) . . ?
C14 C13 C12 112.1(4) . . ?
C16 C13 C12 105.9(4) . . ?
C25 C20 C21 118.9(3) . . ?
C25 C20 N3 121.0(3) . . ?
C21 C20 N3 120.1(3) . . ?
C22 C21 C20 119.7(4) . . ?
C22 C21 C26 119.6(4) . . ?
C20 C21 C26 120.7(3) . . ?
C23 C22 C21 121.7(4) . . ?
C22 C23 C24 119.0(4) . . ?
C23 C24 C25 121.8(4) . . ?
C24 C25 C20 119.0(4) . . ?
C24 C25 C27 119.5(3) . . ?
C20 C25 C27 121.5(3) . . ?
O1 C28 C29 105.5(5) . . ?
C30 C29 C28 104.5(5) . . ?
C31 C30 C29 107.3(5) . . ?
C30 C31 O1 108.4(5) . . ?
O2 C32 C33 103.5(6) . . ?
C34 C33 C32 112.3(7) . . ?
C33 C34 C35 104.5(7) . . ?
C34 C35 O2 107.3(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 O1 1.914(8) . ?
Li O2 1.954(8) . ?
Li Si1 2.626(7) . ?
Si1 N2 1.799(3) . ?
Si1 N1 1.801(3) . ?
Si1 N3 1.826(3) . ?
Si2 N3 1.741(3) . ?
Si2 C18 1.860(4) . ?
Si2 C19 1.867(4) . ?
Si2 C17 1.870(4) . ?
O1 C28 1.417(6) . ?
O1 C31 1.429(5) . ?
O2 C32 1.425(7) . ?
O2 C35 1.518(8) . ?
N1 C1 1.392(4) . ?
N1 C7 1.450(4) . ?
N2 C2 1.399(4) . ?
N2 C12 1.462(4) . ?
N3 C20 1.446(4) . ?
C1 C6 1.388(5) . ?
C1 C2 1.421(5) . ?
C2 C3 1.391(5) . ?
C3 C4 1.396(6) . ?
C4 C5 1.368(6) . ?
C5 C6 1.396(5) . ?
C7 C8 1.540(5) . ?
C8 C9 1.524(5) . ?
C8 C10 1.531(5) . ?
C8 C11 1.526(5) . ?
C12 C13 1.549(5) . ?
C13 C15 1.493(6) . ?
C13 C14 1.505(7) . ?
C13 C16 1.519(7) . ?
C20 C25 1.396(5) . ?
C20 C21 1.405(5) . ?
C21 C22 1.385(6) . ?
C21 C26 1.501(6) . ?
C22 C23 1.362(6) . ?
C23 C24 1.367(6) . ?
C24 C25 1.399(5) . ?
C25 C27 1.500(5) . ?
C28 C29 1.488(8) . ?
C29 C30 1.460(8) . ?
C30 C31 1.412(7) . ?
C32 C33 1.495(10) . ?
C33 C34 1.440(11) . ?
C34 C35 1.442(9) . ?
