#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/30/7013051.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_7013051
loop_
_publ_author_name
'Cole, Marcus L.'
'Junk, Peter C.'
_publ_section_title
;
 Pyridyl donor induced 1,3-silyl migration in metal complexes of the
 guanidine CyHNC{N(SiMe3)Py}NCy, Py = 2-(6-MeC5H3N)
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              2109
_journal_paper_doi               10.1039/b303772j
_journal_year                    2003
_chemical_formula_sum            'C22 H37 Al Cl2 N4 Si'
_chemical_formula_weight         483.53
_chemical_name_common            '[AlCl2(AMPTMSDCC)]'
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 125.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.997(6)
_cell_length_b                   9.1761(18)
_cell_length_c                   21.752(4)
_cell_measurement_temperature    123(2)
_cell_volume                     5179(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'X -Seed'
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega 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  0.0730
_diffrn_reflns_av_sigmaI/netI    0.0610
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16593
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         3.07
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.9661
_exptl_absorpt_correction_T_min  0.9337
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'performed as part of the DENZO-SMN package'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.932
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         6305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[σ²(Fo²)+(0.0864P)²+0.0000P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1397
_reflns_number_gt                4860
_reflns_number_total             6305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303772j.txt
_cod_data_source_block           Compound_4
_cod_original_cell_volume        5178.4(18)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7013051
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl2 Cl 0.166020(19) 0.16240(5) 0.09649(3) 0.02386(13) Uani 1 1 d . . .
Si1 Si 0.13716(2) 0.60235(5) 0.33678(3) 0.01863(14) Uani 1 1 d . . .
Cl1 Cl 0.06393(2) 0.06838(5) 0.10766(3) 0.02940(15) Uani 1 1 d . . .
Al1 Al 0.11757(2) 0.23359(5) 0.12776(3) 0.01517(14) Uani 1 1 d . . .
N4 N 0.13787(6) 0.42064(14) 0.30887(8) 0.0147(3) Uani 1 1 d . . .
N2 N 0.09833(6) 0.50804(15) 0.18854(9) 0.0161(3) Uani 1 1 d . . .
N1 N 0.08148(6) 0.40775(15) 0.07395(8) 0.0152(3) Uani 1 1 d . . .
N3 N 0.15321(6) 0.30336(15) 0.22521(8) 0.0142(3) Uani 1 1 d . . .
C9 C 0.20756(7) 0.08218(18) 0.29279(11) 0.0179(4) Uani 1 1 d . . .
H9A H 0.2040 0.0460 0.2470 0.022 Uiso 1 1 calc R . .
H9B H 0.1793 0.0401 0.2934 0.022 Uiso 1 1 calc R . .
C1 C 0.08483(7) 0.52317(18) 0.11696(10) 0.0145(3) Uani 1 1 d . . .
C4 C 0.04183(7) 0.5625(2) -0.03515(11) 0.0222(4) Uani 1 1 d . . .
H4 H 0.0257 0.5742 -0.0879 0.027 Uiso 1 1 calc R . .
C5 C 0.05824(7) 0.4274(2) -0.00226(11) 0.0189(4) Uani 1 1 d . . .
C13 C 0.24777(7) 0.31678(18) 0.29068(11) 0.0176(4) Uani 1 1 d . . .
H13A H 0.2449 0.2862 0.2447 0.021 Uiso 1 1 calc R . .
H13B H 0.2450 0.4243 0.2900 0.021 Uiso 1 1 calc R . .
C11 C 0.30469(7) 0.10308(19) 0.36805(11) 0.0207(4) Uani 1 1 d . . .
H11A H 0.3057 0.0636 0.3266 0.025 Uiso 1 1 calc R . .
H11B H 0.3374 0.0764 0.4168 0.025 Uiso 1 1 calc R . .
C8 C 0.20394(7) 0.24843(17) 0.29041(10) 0.0142(4) Uani 1 1 d . . .
H8 H 0.2083 0.2807 0.3378 0.017 Uiso 1 1 calc R . .
C7 C 0.12942(7) 0.40836(17) 0.23860(10) 0.0140(4) Uani 1 1 d . . .
C12 C 0.30003(8) 0.26904(19) 0.36137(11) 0.0211(4) Uani 1 1 d . . .
H12A H 0.3279 0.3087 0.3591 0.025 Uiso 1 1 calc R . .
H12B H 0.3044 0.3096 0.4070 0.025 Uiso 1 1 calc R . .
C19 C 0.17123(8) 0.24335(19) 0.41963(11) 0.0208(4) Uani 1 1 d . . .
H19A H 0.1729 0.3164 0.4545 0.025 Uiso 1 1 calc R . .
H19B H 0.2051 0.2414 0.4278 0.025 Uiso 1 1 calc R . .
C14 C 0.12901(7) 0.28535(18) 0.33746(10) 0.0168(4) Uani 1 1 d . . .
H14 H 0.1272 0.2040 0.3054 0.020 Uiso 1 1 calc R . .
C2 C 0.06923(7) 0.66293(18) 0.08400(11) 0.0188(4) Uani 1 1 d . . .
H2 H 0.0729 0.7438 0.1141 0.023 Uiso 1 1 calc R . .
C10 C 0.25968(7) 0.03505(19) 0.36395(11) 0.0207(4) Uani 1 1 d . . .
H10A H 0.2616 0.0638 0.4094 0.025 Uiso 1 1 calc R . .
H10B H 0.2625 -0.0724 0.3642 0.025 Uiso 1 1 calc R . .
C3 C 0.04906(7) 0.6830(2) 0.00976(12) 0.0225(4) Uani 1 1 d . . .
H3 H 0.0399 0.7779 -0.0117 0.027 Uiso 1 1 calc R . .
C6 C 0.05038(8) 0.2954(2) -0.04908(11) 0.0247(4) Uani 1 1 d . . .
H6A H 0.0826 0.2721 -0.0426 0.037 Uiso 1 1 calc R . .
H6B H 0.0234 0.3158 -0.1026 0.037 Uiso 1 1 calc R . .
H6C H 0.0400 0.2125 -0.0325 0.037 Uiso 1 1 calc R . .
C16 C 0.06441(9) 0.1407(2) 0.34396(13) 0.0312(5) Uani 1 1 d . . .
H16A H 0.0318 0.1482 0.3394 0.037 Uiso 1 1 calc R . .
H16B H 0.0596 0.0665 0.3072 0.037 Uiso 1 1 calc R . .
C15 C 0.07659(8) 0.2890(2) 0.32455(11) 0.0221(4) Uani 1 1 d . . .
H15A H 0.0494 0.3133 0.2709 0.026 Uiso 1 1 calc R . .
H15B H 0.0768 0.3658 0.3567 0.026 Uiso 1 1 calc R . .
C22 C 0.16755(9) 0.6047(2) 0.44056(12) 0.0307(5) Uani 1 1 d . . .
H22A H 0.1465 0.5475 0.4510 0.046 Uiso 1 1 calc R . .
H22B H 0.1699 0.7054 0.4573 0.046 Uiso 1 1 calc R . .
H22C H 0.2022 0.5624 0.4679 0.046 Uiso 1 1 calc R . .
C20 C 0.17965(9) 0.7126(2) 0.32264(13) 0.0316(5) Uani 1 1 d . . .
H20A H 0.2111 0.6576 0.3406 0.047 Uiso 1 1 calc R . .
H20B H 0.1888 0.8038 0.3513 0.047 Uiso 1 1 calc R . .
H20C H 0.1615 0.7347 0.2686 0.047 Uiso 1 1 calc R . .
C17 C 0.10753(9) 0.0923(2) 0.42399(13) 0.0316(5) Uani 1 1 d . . .
H17A H 0.1089 0.1586 0.4611 0.038 Uiso 1 1 calc R . .
H17B H 0.1001 -0.0071 0.4329 0.038 Uiso 1 1 calc R . .
C18 C 0.15933(9) 0.0926(2) 0.43630(12) 0.0274(5) Uani 1 1 d . . .
H18A H 0.1591 0.0194 0.4027 0.033 Uiso 1 1 calc R . .
H18B H 0.1867 0.0652 0.4894 0.033 Uiso 1 1 calc R . .
C21 C 0.07209(9) 0.6858(2) 0.28873(13) 0.0320(5) Uani 1 1 d . . .
H21A H 0.0568 0.6992 0.2348 0.048 Uiso 1 1 calc R . .
H21B H 0.0752 0.7805 0.3119 0.048 Uiso 1 1 calc R . .
H21C H 0.0500 0.6215 0.2943 0.048 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 0.0000 0.0000 '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'
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'
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
N4 Si1 C20 107.28(8) . . ?
N4 Si1 C21 115.30(9) . . ?
C20 Si1 C21 111.66(11) . . ?
N4 Si1 C22 108.80(8) . . ?
C20 Si1 C22 106.29(11) . . ?
C21 Si1 C22 107.13(11) . . ?
N3 Al1 N1 99.16(7) . . ?
N3 Al1 Cl2 113.55(6) . . ?
N1 Al1 Cl2 110.61(5) . . ?
N3 Al1 Cl1 111.44(6) . . ?
N1 Al1 Cl1 110.00(6) . . ?
Cl2 Al1 Cl1 111.44(3) . . ?
C7 N4 C14 115.41(13) . . ?
C7 N4 Si1 114.67(11) . . ?
C14 N4 Si1 126.56(11) . . ?
C7 N2 C1 126.67(15) . . ?
C1 N1 C5 119.42(15) . . ?
C1 N1 Al1 116.58(12) . . ?
C5 N1 Al1 123.54(12) . . ?
C7 N3 C8 118.14(14) . . ?
C7 N3 Al1 116.52(12) . . ?
C8 N3 Al1 125.24(11) . . ?
C8 C9 C10 109.41(15) . . ?
N2 C1 N1 123.18(14) . . ?
N2 C1 C2 117.16(15) . . ?
N1 C1 C2 119.41(16) . . ?
C5 C4 C3 119.49(18) . . ?
C4 C5 N1 121.23(17) . . ?
C4 C5 C6 120.81(17) . . ?
N1 C5 C6 117.96(16) . . ?
C12 C13 C8 110.23(15) . . ?
C10 C11 C12 111.50(16) . . ?
N3 C8 C9 112.94(14) . . ?
N3 C8 C13 110.53(13) . . ?
C9 C8 C13 110.93(14) . . ?
N2 C7 N3 124.03(16) . . ?
N2 C7 N4 114.70(14) . . ?
N3 C7 N4 121.24(15) . . ?
C11 C12 C13 111.65(15) . . ?
C14 C19 C18 109.37(16) . . ?
N4 C14 C19 116.37(15) . . ?
N4 C14 C15 111.20(14) . . ?
C19 C14 C15 110.08(16) . . ?
C3 C2 C1 120.60(17) . . ?
C11 C10 C9 112.12(15) . . ?
C2 C3 C4 119.48(17) . . ?
C17 C16 C15 111.43(18) . . ?
C14 C15 C16 110.87(16) . . ?
C18 C17 C16 111.50(17) . . ?
C17 C18 C19 110.93(16) . . ?
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
Cl2 Al1 2.1275(8) . ?
Si1 N4 1.7791(15) . ?
Si1 C20 1.859(2) . ?
Si1 C21 1.862(2) . ?
Si1 C22 1.864(2) . ?
Cl1 Al1 2.1348(8) . ?
Al1 N3 1.8369(17) . ?
Al1 N1 1.9172(16) . ?
N4 C7 1.392(2) . ?
N4 C14 1.488(2) . ?
N2 C7 1.321(2) . ?
N2 C1 1.357(2) . ?
N1 C1 1.375(2) . ?
N1 C5 1.375(2) . ?
N3 C7 1.361(2) . ?
N3 C8 1.485(2) . ?
C9 C8 1.528(2) . ?
C9 C10 1.531(3) . ?
C1 C2 1.410(2) . ?
C4 C5 1.373(3) . ?
C4 C3 1.402(3) . ?
C5 C6 1.505(3) . ?
C13 C12 1.531(3) . ?
C13 C8 1.533(2) . ?
C11 C10 1.524(3) . ?
C11 C12 1.529(2) . ?
C19 C14 1.530(3) . ?
C19 C18 1.533(3) . ?
C14 C15 1.530(3) . ?
C2 C3 1.356(3) . ?
C16 C17 1.523(3) . ?
C16 C15 1.541(3) . ?
C17 C18 1.516(3) . ?
