#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:05:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179740 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/36/7003692.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_7003692
loop_
_publ_author_name
'Bourget-Merle, Laurence'
'Hitchcock, Peter B.'
'Lappert, Michael F.'
'Merle, Philippe G.'
_publ_section_title
;
 Synthesis and structures of crystalline Li, Al and Sn(ii) 1-azaallyls
 and β-diketiminates derived from [Li{μ,η3-N(SiMe3)C(Ad)C(H)SiMe3}]2
 (Ad = 1-adamantyl)
;
_journal_issue                   26
_journal_name_full               'Dalton Transactions'
_journal_page_first              3493
_journal_page_last               3501
_journal_paper_doi               10.1039/b718728a
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C27 H45 Al1 N2 Si2'
_chemical_formula_sum            'C27 H45 Al N2 Si2'
_chemical_formula_weight         480.81
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2000-09-06T10:30:25-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                97.866(2)
_cell_angle_beta                 93.585(2)
_cell_angle_gamma                98.304(2)
_cell_formula_units_Z            2
_cell_length_a                   6.5294(2)
_cell_length_b                   12.4764(4)
_cell_length_c                   17.8535(7)
_cell_measurement_reflns_used    8065
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     1420.58(8)
_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 0.97
_diffrn_measured_fraction_theta_max 0.97
_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  0.0367
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12549
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         8060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0435
_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)+(0.0441P)²+0.7313P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                6885
_reflns_number_total             8060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718728a.txt
_cod_data_source_block           (4)-sep700
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7003692
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Si1 Si 0.54820(6) 0.52811(3) 0.34282(2) 0.02217(9) Uani 1 1 d . . .
Si2 Si 0.53479(6) 0.72452(3) 0.08727(2) 0.01971(9) Uani 1 1 d . . .
Al Al 0.81882(6) 0.64967(3) 0.22012(2) 0.01871(9) Uani 1 1 d . . .
N1 N 0.65385(18) 0.64837(9) 0.30687(6) 0.0193(2) Uani 1 1 d . . .
N2 N 0.69166(17) 0.75709(9) 0.17405(6) 0.0173(2) Uani 1 1 d . . .
C1 C 0.6577(2) 0.75158(10) 0.33955(7) 0.0194(2) Uani 1 1 d . . .
C2 C 0.7081(2) 0.84459(10) 0.30332(7) 0.0210(3) Uani 1 1 d . . .
H2 H 0.74 0.9127 0.3359 0.025 Uiso 1 1 calc R . .
C3 C 0.71719(19) 0.84958(10) 0.22562(7) 0.0167(2) Uani 1 1 d . . .
C4 C 0.6277(2) 0.77775(11) 0.42229(7) 0.0233(3) Uani 1 1 d . . .
C5 C 0.7700(3) 0.75044(14) 0.47531(9) 0.0317(3) Uani 1 1 d . . .
H5 H 0.8813 0.7145 0.4587 0.038 Uiso 1 1 calc R . .
C6 C 0.7490(3) 0.77592(16) 0.55266(9) 0.0428(4) Uani 1 1 d . . .
H6 H 0.8466 0.7579 0.5888 0.051 Uiso 1 1 calc R . .
C7 C 0.5862(4) 0.82733(17) 0.57665(10) 0.0491(5) Uani 1 1 d . . .
H7 H 0.5699 0.8429 0.6293 0.059 Uiso 1 1 calc R . .
C8 C 0.4466(3) 0.85622(16) 0.52444(10) 0.0446(4) Uani 1 1 d . . .
H8 H 0.3356 0.8923 0.5413 0.053 Uiso 1 1 calc R . .
C9 C 0.4685(3) 0.83251(13) 0.44699(9) 0.0322(3) Uani 1 1 d . . .
H9 H 0.3744 0.8539 0.4112 0.039 Uiso 1 1 calc R . .
C10 C 0.7689(3) 0.46308(14) 0.37750(10) 0.0341(3) Uani 1 1 d . . .
H10A H 0.8624 0.4527 0.3372 0.051 Uiso 1 1 calc R . .
H10B H 0.715 0.3919 0.3918 0.051 Uiso 1 1 calc R . .
H10C H 0.8451 0.5105 0.4218 0.051 Uiso 1 1 calc R . .
C11 C 0.3929(3) 0.43328(13) 0.26289(10) 0.0385(4) Uani 1 1 d . . .
H11A H 0.4809 0.419 0.2213 0.058 Uiso 1 1 calc R . .
H11B H 0.2757 0.4668 0.245 0.058 Uiso 1 1 calc R . .
H11C H 0.3403 0.3642 0.2804 0.058 Uiso 1 1 calc R . .
C12 C 0.3663(2) 0.54924(13) 0.41807(9) 0.0308(3) Uani 1 1 d . . .
H12A H 0.4397 0.5988 0.4619 0.046 Uiso 1 1 calc R . .
H12B H 0.314 0.4787 0.4336 0.046 Uiso 1 1 calc R . .
H12C H 0.2495 0.5813 0.3982 0.046 Uiso 1 1 calc R . .
C13 C 0.77359(19) 0.96611(10) 0.20488(7) 0.0170(2) Uani 1 1 d . . .
C14 C 0.9793(2) 1.02166(11) 0.25246(8) 0.0224(3) Uani 1 1 d . . .
H14A H 0.9602 1.0236 0.3072 0.027 Uiso 1 1 calc R . .
H14B H 1.0913 0.9782 0.2402 0.027 Uiso 1 1 calc R . .
C15 C 0.6029(2) 1.03673(11) 0.22398(8) 0.0226(3) Uani 1 1 d . . .
H15A H 0.4715 1.0034 0.1936 0.027 Uiso 1 1 calc R . .
H15B H 0.5787 1.0393 0.2783 0.027 Uiso 1 1 calc R . .
C16 C 0.8176(2) 0.96601(10) 0.12117(7) 0.0201(2) Uani 1 1 d . . .
H16A H 0.9313 0.9233 0.1097 0.024 Uiso 1 1 calc R . .
H16B H 0.6921 0.9301 0.0882 0.024 Uiso 1 1 calc R . .
C17 C 1.0422(2) 1.13898(12) 0.23557(9) 0.0266(3) Uani 1 1 d . . .
H17 H 1.1728 1.1734 0.2674 0.032 Uiso 1 1 calc R . .
C18 C 0.8694(3) 1.20599(12) 0.25492(9) 0.0314(3) Uani 1 1 d . . .
H18A H 0.91 1.2819 0.2449 0.038 Uiso 1 1 calc R . .
H18B H 0.847 1.2087 0.3094 0.038 Uiso 1 1 calc R . .
C19 C 0.6682(2) 1.15365(11) 0.20668(9) 0.0279(3) Uani 1 1 d . . .
H19 H 0.556 1.1983 0.219 0.033 Uiso 1 1 calc R . .
C20 C 0.7044(2) 1.15004(12) 0.12234(9) 0.0283(3) Uani 1 1 d . . .
H20A H 0.5753 1.1159 0.0908 0.034 Uiso 1 1 calc R . .
H20B H 0.7428 1.2254 0.1108 0.034 Uiso 1 1 calc R . .
C21 C 0.8791(2) 1.08341(11) 0.10400(8) 0.0233(3) Uani 1 1 d . . .
H21 H 0.9023 1.0808 0.049 0.028 Uiso 1 1 calc R . .
C22 C 1.0791(2) 1.13738(12) 0.15171(9) 0.0269(3) Uani 1 1 d . . .
H22A H 1.1187 1.2131 0.141 0.032 Uiso 1 1 calc R . .
H22B H 1.1934 1.0957 0.139 0.032 Uiso 1 1 calc R . .
C23 C 0.3277(2) 0.81368(14) 0.08014(9) 0.0310(3) Uani 1 1 d . . .
H23A H 0.3929 0.8898 0.0815 0.047 Uiso 1 1 calc R . .
H23B H 0.2414 0.8085 0.1229 0.047 Uiso 1 1 calc R . .
H23C H 0.2409 0.7892 0.0324 0.047 Uiso 1 1 calc R . .
C24 C 0.6929(3) 0.72004(13) 0.00349(8) 0.0299(3) Uani 1 1 d . . .
H24A H 0.7754 0.7922 0.0035 0.045 Uiso 1 1 calc R . .
H24B H 0.6004 0.7001 -0.0433 0.045 Uiso 1 1 calc R . .
H24C H 0.7859 0.6654 0.0063 0.045 Uiso 1 1 calc R . .
C25 C 0.3822(3) 0.58525(13) 0.08363(9) 0.0320(3) Uani 1 1 d . . .
H25A H 0.2971 0.5845 0.1269 0.048 Uiso 1 1 calc R . .
H25B H 0.4774 0.5316 0.0858 0.048 Uiso 1 1 calc R . .
H25C H 0.292 0.5665 0.0363 0.048 Uiso 1 1 calc R . .
C26 C 0.8245(3) 0.50795(12) 0.15625(9) 0.0315(3) Uani 1 1 d . . .
H26A H 0.8928 0.4605 0.1858 0.047 Uiso 1 1 calc R . .
H26B H 0.9015 0.5203 0.112 0.047 Uiso 1 1 calc R . .
H26C H 0.682 0.4728 0.1392 0.047 Uiso 1 1 calc R . .
C27 C 1.1041(2) 0.71356(13) 0.26406(9) 0.0268(3) Uani 1 1 d . . .
H27A H 1.1678 0.6583 0.2874 0.04 Uiso 1 1 calc R . .
H27B H 1.098 0.7766 0.3027 0.04 Uiso 1 1 calc R . .
H27C H 1.1876 0.7373 0.2238 0.04 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'
Al Al 0.0645 0.0514 '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'
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 Si1 C11 107.77(7) . . ?
N1 Si1 C12 115.24(6) . . ?
C11 Si1 C12 105.69(8) . . ?
N1 Si1 C10 107.90(7) . . ?
C11 Si1 C10 109.27(9) . . ?
C12 Si1 C10 110.80(8) . . ?
N2 Si2 C25 108.38(6) . . ?
N2 Si2 C24 112.12(6) . . ?
C25 Si2 C24 107.16(7) . . ?
N2 Si2 C23 113.13(6) . . ?
C25 Si2 C23 103.04(8) . . ?
C24 Si2 C23 112.35(8) . . ?
N2 Al N1 97.01(5) . . ?
N2 Al C26 117.08(6) . . ?
N1 Al C26 117.33(6) . . ?
N2 Al C27 110.01(6) . . ?
N1 Al C27 104.59(6) . . ?
C26 Al C27 109.66(7) . . ?
C1 N1 Si1 126.48(9) . . ?
C1 N1 Al 108.46(9) . . ?
Si1 N1 Al 124.52(6) . . ?
C3 N2 Si2 129.16(9) . . ?
C3 N2 Al 107.26(8) . . ?
Si2 N2 Al 122.66(6) . . ?
N1 C1 C2 124.59(12) . . ?
N1 C1 C4 120.98(11) . . ?
C2 C1 C4 114.17(11) . . ?
C3 C2 C1 128.51(12) . . ?
N2 C3 C2 121.17(11) . . ?
N2 C3 C13 123.52(11) . . ?
C2 C3 C13 115.16(10) . . ?
C9 C4 C5 119.64(14) . . ?
C9 C4 C1 121.64(13) . . ?
C5 C4 C1 118.66(14) . . ?
C6 C5 C4 120.02(16) . . ?
C7 C6 C5 119.91(17) . . ?
C6 C7 C8 120.35(16) . . ?
C7 C8 C9 120.07(18) . . ?
C4 C9 C8 119.97(16) . . ?
C16 C13 C15 109.60(11) . . ?
C16 C13 C3 113.11(10) . . ?
C15 C13 C3 111.47(10) . . ?
C16 C13 C14 105.99(10) . . ?
C15 C13 C14 108.40(10) . . ?
C3 C13 C14 108.01(10) . . ?
C17 C14 C13 110.69(11) . . ?
C19 C15 C13 110.29(11) . . ?
C21 C16 C13 111.12(10) . . ?
C18 C17 C22 109.41(13) . . ?
C18 C17 C14 109.38(12) . . ?
C22 C17 C14 110.24(12) . . ?
C17 C18 C19 109.66(12) . . ?
C18 C19 C20 109.34(13) . . ?
C18 C19 C15 109.53(12) . . ?
C20 C19 C15 109.73(12) . . ?
C21 C20 C19 109.24(12) . . ?
C22 C21 C20 109.73(12) . . ?
C22 C21 C16 109.78(11) . . ?
C20 C21 C16 109.59(11) . . ?
C21 C22 C17 108.59(12) . . ?
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
Si1 N1 1.7773(11) . ?
Si1 C11 1.8641(17) . ?
Si1 C12 1.8652(16) . ?
Si1 C10 1.8659(17) . ?
Si2 N2 1.7674(11) . ?
Si2 C25 1.8646(16) . ?
Si2 C24 1.8692(15) . ?
Si2 C23 1.8798(16) . ?
Al N2 1.9235(11) . ?
Al N1 1.9417(12) . ?
Al C26 1.9749(15) . ?
Al C27 1.9846(15) . ?
N1 C1 1.3350(16) . ?
N2 C3 1.3569(15) . ?
C1 C2 1.4124(18) . ?
C1 C4 1.5000(18) . ?
C2 C3 1.4018(17) . ?
C3 C13 1.5479(17) . ?
C4 C9 1.386(2) . ?
C4 C5 1.395(2) . ?
C5 C6 1.394(2) . ?
C6 C7 1.380(3) . ?
C7 C8 1.382(3) . ?
C8 C9 1.395(2) . ?
C13 C16 1.5393(17) . ?
C13 C15 1.5440(18) . ?
C13 C14 1.5598(18) . ?
C14 C17 1.5379(19) . ?
C15 C19 1.5379(19) . ?
C16 C21 1.5393(18) . ?
C17 C18 1.528(2) . ?
C17 C22 1.529(2) . ?
C18 C19 1.533(2) . ?
C19 C20 1.534(2) . ?
C20 C21 1.532(2) . ?
C21 C22 1.528(2) . ?
