#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:13:34 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179804 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/00/7010091.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_7010091
loop_
_publ_author_name
'David Doyle'
'Yurii K. Gun'ko'
'Peter B. Hitchcock'
'Michael F. Lappert'
_publ_section_title
;
 Synthesis and structures of lithium, aluminium, gallium and lanthanide
 amidinates containing a γ-pendant amine functionality
;
_journal_issue                   22
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              4093
_journal_page_last               4097
_journal_paper_doi               10.1039/b005824f
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C15 H26 Al1 Cl2 N3 Si1'
_chemical_formula_structural     'C15 H26 AL CL2 N3 SI'
_chemical_formula_sum            'C15 H26 Al Cl2 N3 Si'
_chemical_formula_weight         374.36
_chemical_name_common            '[AlCl2{Me3SiNC(Ph)N(CH2)3NMe2}]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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             1999-12-21T10:41:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.373(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.8881(3)
_cell_length_b                   11.4278(5)
_cell_length_c                   10.3472(5)
_cell_measurement_reflns_used    4777
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      4.246
_cell_measurement_wavelength     0.71073
_cell_volume                     991.47(7)
_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 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8799
_diffrn_reflns_theta_full        30
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         4.32
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.8813
_exptl_absorpt_correction_T_min  0.8813
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4202
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0304P)²+0.2161P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0736
_refine_ls_wR_factor_ref         0.0753
_reflns_number_gt                3972
_reflns_number_total             4202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005824f.txt
_cod_data_source_block           gunko-2
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7010091
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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
Al Al 0.21673(6) 0.13591(5) 0.84595(5) 0.02081(11) Uani 1 1 d . . .
Cl1 Cl 0.44982(5) 0.05273(5) 0.89837(5) 0.03164(11) Uani 1 1 d . . .
Cl2 Cl 0.23747(7) 0.30754(5) 0.93792(6) 0.04133(13) Uani 1 1 d . . .
Si Si 0.31116(6) 0.21494(5) 0.55461(5) 0.02503(11) Uani 1 1 d . . .
N1 N 0.19085(17) 0.17184(15) 0.64877(15) 0.0251(3) Uani 1 1 d . . .
N2 N 0.00317(17) 0.11425(17) 0.72689(16) 0.0296(4) Uani 1 1 d . . .
N3 N 0.15689(17) 0.04162(16) 0.99538(15) 0.0247(3) Uani 1 1 d . . .
C1 C 0.03621(19) 0.15240(18) 0.61873(17) 0.0235(3) Uani 1 1 d . . .
C2 C -0.08982(19) 0.17248(18) 0.48284(18) 0.0246(4) Uani 1 1 d . . .
C3 C -0.1744(2) 0.2765(2) 0.4584(2) 0.0346(5) Uani 1 1 d . . .
H3 H -0.1522 0.3346 0.5279 0.042 Uiso 1 1 calc R . .
C4 C -0.2915(3) 0.2961(2) 0.3328(2) 0.0417(5) Uani 1 1 d . . .
H4 H -0.3481 0.3681 0.316 0.05 Uiso 1 1 calc R . .
C5 C -0.3258(2) 0.2113(2) 0.2324(2) 0.0385(5) Uani 1 1 d . . .
H5 H -0.4065 0.2249 0.1467 0.046 Uiso 1 1 calc R . .
C6 C -0.2434(3) 0.1067(2) 0.2560(2) 0.0367(5) Uani 1 1 d . . .
H6 H -0.2674 0.0482 0.1868 0.044 Uiso 1 1 calc R . .
C7 C -0.1247(2) 0.0874(2) 0.3818(2) 0.0318(4) Uani 1 1 d . . .
H7 H -0.0676 0.0156 0.3982 0.038 Uiso 1 1 calc R . .
C8 C 0.1998(3) 0.2945(2) 0.3938(2) 0.0391(5) Uani 1 1 d . . .
H8A H 0.1182 0.2429 0.3339 0.059 Uiso 1 1 calc R . .
H8B H 0.2741 0.3184 0.3468 0.059 Uiso 1 1 calc R . .
H8C H 0.1487 0.3639 0.4163 0.059 Uiso 1 1 calc R . .
C9 C 0.4071(2) 0.0829(2) 0.5109(2) 0.0342(4) Uani 1 1 d . . .
H9A H 0.3249 0.0315 0.4513 0.051 Uiso 1 1 calc R . .
H9B H 0.466 0.0409 0.5951 0.051 Uiso 1 1 calc R . .
H9C H 0.4809 0.1067 0.4634 0.051 Uiso 1 1 calc R . .
C10 C 0.4657(3) 0.3134(2) 0.6671(2) 0.0392(5) Uani 1 1 d . . .
H10A H 0.4144 0.3827 0.6897 0.059 Uiso 1 1 calc R . .
H10B H 0.5392 0.3376 0.6194 0.059 Uiso 1 1 calc R . .
H10C H 0.5251 0.2719 0.7515 0.059 Uiso 1 1 calc R . .
C11 C -0.1540(2) 0.1082(2) 0.7403(2) 0.0374(5) Uani 1 1 d . . .
H11A H -0.2299 0.0713 0.6577 0.045 Uiso 1 1 calc R . .
H11B H -0.1928 0.1881 0.7489 0.045 Uiso 1 1 calc R . .
C12 C -0.1446(2) 0.0369(2) 0.8660(2) 0.0368(5) Uani 1 1 d . . .
H12A H -0.132 -0.0466 0.8466 0.044 Uiso 1 1 calc R . .
H12B H -0.2465 0.0452 0.8845 0.044 Uiso 1 1 calc R . .
C13 C -0.0082(2) 0.0724(2) 0.9939(2) 0.0323(4) Uani 1 1 d . . .
H13A H -0.0132 0.1582 1.0054 0.039 Uiso 1 1 calc R . .
H13B H -0.0255 0.0352 1.0742 0.039 Uiso 1 1 calc R . .
C14 C 0.1650(3) -0.0866(2) 0.9708(2) 0.0362(5) Uani 1 1 d . . .
H14A H 0.0933 -0.1058 0.8786 0.054 Uiso 1 1 calc R . .
H14B H 0.1326 -0.1301 1.0388 0.054 Uiso 1 1 calc R . .
H14C H 0.2745 -0.108 0.9787 0.054 Uiso 1 1 calc R . .
C15 C 0.2672(3) 0.0654(3) 1.13593(19) 0.0389(5) Uani 1 1 d . . .
H15A H 0.2653 0.1491 1.1559 0.058 Uiso 1 1 calc R . .
H15B H 0.3756 0.0423 1.1425 0.058 Uiso 1 1 calc R . .
H15C H 0.2333 0.0204 1.2022 0.058 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'
Cl Cl 0.1484 0.1585 '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
N2 Al N1 67.53(6) . . ?
N2 Al N3 88.17(7) . . ?
N1 Al N3 151.64(7) . . ?
N2 Al Cl2 108.90(6) . . ?
N1 Al Cl2 103.00(6) . . ?
N3 Al Cl2 98.48(5) . . ?
N2 Al Cl1 139.95(7) . . ?
N1 Al Cl1 96.92(5) . . ?
N3 Al Cl1 92.59(5) . . ?
Cl2 Al Cl1 110.56(3) . . ?
N2 Al C1 33.78(6) . . ?
N1 Al C1 33.86(6) . . ?
N3 Al C1 121.24(6) . . ?
Cl2 Al C1 107.16(6) . . ?
Cl1 Al C1 123.77(5) . . ?
N1 Si C10 106.55(9) . . ?
N1 Si C9 108.83(10) . . ?
C10 Si C9 109.90(11) . . ?
N1 Si C8 113.24(9) . . ?
C10 Si C8 109.08(12) . . ?
C9 Si C8 109.19(11) . . ?
C1 N1 Si 134.38(13) . . ?
C1 N1 Al 87.96(11) . . ?
Si N1 Al 137.62(8) . . ?
C1 N2 C11 126.01(15) . . ?
C1 N2 Al 92.93(11) . . ?
C11 N2 Al 136.80(14) . . ?
C15 N3 C14 107.03(18) . . ?
C15 N3 C13 106.99(15) . . ?
C14 N3 C13 109.29(16) . . ?
C15 N3 Al 112.50(13) . . ?
C14 N3 Al 109.92(12) . . ?
C13 N3 Al 110.97(12) . . ?
N2 C1 N1 111.20(15) . . ?
N2 C1 C2 122.61(15) . . ?
N1 C1 C2 126.18(16) . . ?
N2 C1 Al 53.28(9) . . ?
N1 C1 Al 58.17(9) . . ?
C2 C1 Al 172.80(14) . . ?
C3 C2 C7 119.51(17) . . ?
C3 C2 C1 119.68(17) . . ?
C7 C2 C1 120.80(17) . . ?
C2 C3 C4 120.2(2) . . ?
C5 C4 C3 120.1(2) . . ?
C4 C5 C6 120.23(18) . . ?
C5 C6 C7 119.6(2) . . ?
C2 C7 C6 120.3(2) . . ?
N2 C11 C12 109.10(16) . . ?
C11 C12 C13 113.84(19) . . ?
N3 C13 C12 116.07(17) . . ?
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
Al N2 1.9053(15) . ?
Al N1 2.0182(16) . ?
Al N3 2.0929(16) . ?
Al Cl2 2.1610(8) . ?
Al Cl1 2.1782(6) . ?
Al C1 2.3738(17) . ?
Si N1 1.7396(16) . ?
Si C10 1.856(2) . ?
Si C9 1.861(2) . ?
Si C8 1.866(2) . ?
N1 C1 1.324(2) . ?
N2 C1 1.322(2) . ?
N2 C11 1.451(2) . ?
N3 C15 1.484(2) . ?
N3 C14 1.493(3) . ?
N3 C13 1.504(2) . ?
C1 C2 1.496(2) . ?
C2 C3 1.384(3) . ?
C2 C7 1.386(3) . ?
C3 C4 1.387(3) . ?
C4 C5 1.379(4) . ?
C5 C6 1.381(4) . ?
C6 C7 1.394(3) . ?
C11 C12 1.514(3) . ?
C12 C13 1.524(3) . ?
