#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:29:14 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178567 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/76/4067697.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_4067697
loop_
_publ_author_name
'Forret, Robert'
'Kennedy, Alan R.'
'Klett, Jan'
'Mulvey, Robert E.'
'Robertson, Stuart D.'
_publ_section_title
;
 Multistep Self-Assembly of Heteroleptic Magnesium and
 Sodium−Magnesium Benzamidinate Complexes
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1436
_journal_paper_doi               10.1021/om9010824
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C15 H27 Mg N Si2'
_chemical_formula_sum            'C15 H27 Mg N Si2'
_chemical_formula_weight         301.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                63.035(6)
_cell_angle_beta                 70.686(7)
_cell_angle_gamma                89.924(6)
_cell_formula_units_Z            2
_cell_length_a                   10.0894(8)
_cell_length_b                   10.2655(6)
_cell_length_c                   11.1908(7)
_cell_measurement_reflns_used    5571
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      29.5869
_cell_measurement_theta_min      2.7631
_cell_volume                     959.57(14)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.782
_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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9464
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.74
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    0.207
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         4281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0567P)²+0.0105P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                3416
_reflns_number_total             4281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9010824_si_001.cif
_cod_data_source_block           5a
_cod_database_code               4067697
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
Si2 Si 0.78553(4) 0.50151(5) 0.22644(4) 0.02347(11) Uani 1 1 d .
Mg1 Mg 0.49698(5) 0.35801(5) 0.51073(5) 0.01985(12) Uani 1 1 d .
N1 N 0.58654(14) 0.24609(15) 0.67382(14) 0.0295(3) Uani 1 1 d .
C1 C 0.62007(15) 0.19921(17) 0.77070(16) 0.0249(3) Uani 1 1 d .
C2 C 0.65880(14) 0.14254(16) 0.89514(15) 0.0203(3) Uani 1 1 d .
C3 C 0.75672(16) 0.04741(17) 0.90909(16) 0.0274(3) Uani 1 1 d .
H3A H 0.7993 0.0196 0.8366 0.033 Uiso 1 1 calc R
C4 C 0.79119(18) -0.00621(19) 1.03043(19) 0.0361(4) Uani 1 1 d .
H4A H 0.8589 -0.0709 1.0412 0.043 Uiso 1 1 calc R
C5 C 0.72900(19) 0.0327(2) 1.13526(18) 0.0372(4) Uani 1 1 d .
H5A H 0.7535 -0.0054 1.2184 0.045 Uiso 1 1 calc R
C6 C 0.6312(2) 0.1267(2) 1.12129(17) 0.0379(4) Uani 1 1 d .
H6A H 0.5876 0.1527 1.1949 0.045 Uiso 1 1 calc R
C7 C 0.59673(17) 0.18279(18) 1.00038(17) 0.0298(3) Uani 1 1 d .
H7A H 0.5304 0.2490 0.9893 0.036 Uiso 1 1 calc R
C10 C 0.41589(15) 0.21201(17) 0.45474(16) 0.0242(3) Uani 1 1 d .
H10A H 0.4903 0.2215 0.3659 0.029 Uiso 1 1 calc R
H10B H 0.4050 0.1096 0.5322 0.029 Uiso 1 1 calc R
C11 C 0.09013(16) 0.1627(2) 0.59631(18) 0.0361(4) Uani 1 1 d .
H11A H 0.1032 0.2129 0.6492 0.054 Uiso 1 1 calc R
H11B H 0.0803 0.0553 0.6556 0.054 Uiso 1 1 calc R
H11C H 0.0039 0.1851 0.5743 0.054 Uiso 1 1 calc R
C12 C 0.21599(18) 0.1236(2) 0.33382(19) 0.0378(4) Uani 1 1 d .
H12A H 0.2922 0.1609 0.2387 0.057 Uiso 1 1 calc R
H12B H 0.1239 0.1368 0.3224 0.057 Uiso 1 1 calc R
H12C H 0.2149 0.0179 0.3931 0.057 Uiso 1 1 calc R
C13 C 0.24574(19) 0.42711(19) 0.3042(2) 0.0387(4) Uani 1 1 d .
H13A H 0.3271 0.4649 0.2125 0.058 Uiso 1 1 calc R
H13B H 0.2519 0.4864 0.3510 0.058 Uiso 1 1 calc R
H13C H 0.1568 0.4339 0.2859 0.058 Uiso 1 1 calc R
C20 C 0.67377(15) 0.55345(17) 0.36113(15) 0.0250(3) Uani 1 1 d .
H20A H 0.6361 0.6446 0.3145 0.030 Uiso 1 1 calc R
H20B H 0.7288 0.5698 0.4132 0.030 Uiso 1 1 calc R
Si1 Si 0.24851(4) 0.22942(5) 0.42422(4) 0.02325(11) Uani 1 1 d .
C21 C 0.81878(17) 0.30738(18) 0.31436(18) 0.0334(4) Uani 1 1 d .
H21A H 0.8782 0.2838 0.2402 0.050 Uiso 1 1 calc R
H21B H 0.7276 0.2383 0.3697 0.050 Uiso 1 1 calc R
H21C H 0.8680 0.2983 0.3793 0.050 Uiso 1 1 calc R
C22 C 0.96518(17) 0.6235(2) 0.1175(2) 0.0407(4) Uani 1 1 d .
H22A H 1.0265 0.5824 0.0597 0.061 Uiso 1 1 calc R
H22B H 1.0083 0.6285 0.1823 0.061 Uiso 1 1 calc R
H22C H 0.9549 0.7234 0.0533 0.061 Uiso 1 1 calc R
C23 C 0.69739(18) 0.5248(2) 0.09711(17) 0.0365(4) Uani 1 1 d .
H23A H 0.7529 0.4908 0.0298 0.055 Uiso 1 1 calc R
H23B H 0.6922 0.6298 0.0431 0.055 Uiso 1 1 calc R
H23C H 0.6008 0.4660 0.1505 0.055 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'
Mg Mg 0.0486 0.0363 '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
C20 Si2 C23 109.30(7) . .
C20 Si2 C21 111.67(8) . .
C23 Si2 C21 110.71(9) . .
C20 Si2 C22 111.96(8) . .
C23 Si2 C22 106.83(9) . .
C21 Si2 C22 106.23(8) . .
C20 Si2 Mg1 42.32(5) . .
C23 Si2 Mg1 95.71(6) . .
C21 Si2 Mg1 80.72(7) . .
C22 Si2 Mg1 151.61(7) . .
C10 Mg1 N1 112.56(6) . .
C10 Mg1 C20 125.76(6) . .
N1 Mg1 C20 97.65(6) . .
C10 Mg1 C20 115.38(6) . 2_666
N1 Mg1 C20 96.72(6) . 2_666
C20 Mg1 C20 103.80(5) . 2_666
C10 Mg1 Mg1 144.90(5) . 2_666
N1 Mg1 Mg1 101.67(5) . 2_666
C20 Mg1 Mg1 53.28(5) . 2_666
C20 Mg1 Mg1 50.51(5) 2_666 2_666
C10 Mg1 Si2 95.06(5) . .
N1 Mg1 Si2 99.84(5) . .
C20 Mg1 Si2 33.89(4) . .
C20 Mg1 Si2 136.10(5) 2_666 .
Mg1 Mg1 Si2 86.28(5) 2_666 .
C1 N1 Mg1 168.49(13) . .
N1 C1 C2 177.98(16) . .
C7 C2 C3 120.76(14) . .
C7 C2 C1 119.37(13) . .
C3 C2 C1 119.87(14) . .
C4 C3 C2 118.60(15) . .
C4 C3 H3A 120.7 . .
C2 C3 H3A 120.7 . .
C5 C4 C3 120.69(15) . .
C5 C4 H4A 119.7 . .
C3 C4 H4A 119.7 . .
C4 C5 C6 120.51(15) . .
C4 C5 H5A 119.7 . .
C6 C5 H5A 119.7 . .
C7 C6 C5 119.69(15) . .
C7 C6 H6A 120.2 . .
C5 C6 H6A 120.2 . .
C6 C7 C2 119.74(15) . .
C6 C7 H7A 120.1 . .
C2 C7 H7A 120.1 . .
Si1 C10 Mg1 120.34(8) . .
Si1 C10 H10A 107.2 . .
Mg1 C10 H10A 107.2 . .
Si1 C10 H10B 107.2 . .
Mg1 C10 H10B 107.2 . .
H10A C10 H10B 106.9 . .
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 . .
Si1 C12 H12A 109.5 . .
Si1 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
Si1 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
Si1 C13 H13A 109.5 . .
Si1 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
Si1 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
Si2 C20 Mg1 103.79(7) . .
Si2 C20 H20A 111.0 . .
Mg1 C20 H20A 111.0 . .
Si2 C20 H20B 111.0 . .
Mg1 C20 H20B 111.0 . .
H20A C20 H20B 109.0 . .
C10 Si1 C13 110.57(8) . .
C10 Si1 C11 112.14(8) . .
C13 Si1 C11 107.62(9) . .
C10 Si1 C12 114.05(7) . .
C13 Si1 C12 105.75(8) . .
C11 Si1 C12 106.29(8) . .
Si2 C21 H21A 109.5 . .
Si2 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
Si2 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
Si2 C22 H22A 109.5 . .
Si2 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
Si2 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
Si2 C23 H23A 109.5 . .
Si2 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
Si2 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si2 C20 1.8521(15) .
Si2 C23 1.8654(17) .
Si2 C21 1.8686(17) .
Si2 C22 1.871(2) .
Si2 Mg1 3.2256(19) .
Mg1 C10 2.1217(15) .
Mg1 N1 2.1575(15) .
Mg1 C20 2.236(2) .
Mg1 C20 2.3224(16) 2_666
Mg1 Mg1 2.8136(11) 2_666
N1 C1 1.1361(19) .
C1 C2 1.434(2) .
C2 C7 1.379(2) .
C2 C3 1.384(2) .
C3 C4 1.379(2) .
C3 H3A 0.9500 .
C4 C5 1.366(2) .
C4 H4A 0.9500 .
C5 C6 1.376(2) .
C5 H5A 0.9500 .
C6 C7 1.374(2) .
C6 H6A 0.9500 .
C7 H7A 0.9500 .
C10 Si1 1.8237(15) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 Si1 1.8716(19) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 Si1 1.8783(16) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 Si1 1.8648(19) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C20 Si2 Mg1 C10 156.96(8) . .
C23 Si2 Mg1 C10 44.39(7) . .
C21 Si2 Mg1 C10 -65.72(7) . .
C22 Si2 Mg1 C10 -172.78(13) . .
C20 Si2 Mg1 N1 -89.07(8) . .
C23 Si2 Mg1 N1 158.36(7) . .
C21 Si2 Mg1 N1 48.25(7) . .
C22 Si2 Mg1 N1 -58.81(13) . .
C23 Si2 Mg1 C20 -112.56(9) . .
C21 Si2 Mg1 C20 137.32(9) . .
C22 Si2 Mg1 C20 30.27(14) . .
C20 Si2 Mg1 C20 21.51(12) . 2_666
C23 Si2 Mg1 C20 -91.05(9) . 2_666
C21 Si2 Mg1 C20 158.83(8) . 2_666
C22 Si2 Mg1 C20 51.78(14) . 2_666
C20 Si2 Mg1 Mg1 12.14(7) . 2_666
C23 Si2 Mg1 Mg1 -100.43(7) . 2_666
C21 Si2 Mg1 Mg1 149.46(6) . 2_666
C22 Si2 Mg1 Mg1 42.41(13) . 2_666
C10 Mg1 N1 C1 -131.1(6) . .
C20 Mg1 N1 C1 94.9(6) . .
C20 Mg1 N1 C1 -10.0(6) 2_666 .
Mg1 Mg1 N1 C1 41.0(6) 2_666 .
Si2 Mg1 N1 C1 129.2(6) . .
Mg1 N1 C1 C2 6(5) . .
N1 C1 C2 C7 -4(5) . .
N1 C1 C2 C3 176(5) . .
C7 C2 C3 C4 -0.1(2) . .
C1 C2 C3 C4 -179.54(14) . .
C2 C3 C4 C5 0.6(2) . .
C3 C4 C5 C6 -0.3(3) . .
C4 C5 C6 C7 -0.6(3) . .
C5 C6 C7 C2 1.0(3) . .
C3 C2 C7 C6 -0.7(2) . .
C1 C2 C7 C6 178.75(15) . .
N1 Mg1 C10 Si1 139.51(8) . .
C20 Mg1 C10 Si1 -102.02(10) . .
C20 Mg1 C10 Si1 29.80(11) 2_666 .
Mg1 Mg1 C10 Si1 -26.90(14) 2_666 .
Si2 Mg1 C10 Si1 -117.62(8) . .
C23 Si2 C20 Mg1 76.81(9) . .
C21 Si2 C20 Mg1 -46.04(9) . .
C22 Si2 C20 Mg1 -165.02(7) . .
C10 Mg1 C20 Si2 -28.72(10) . .
N1 Mg1 C20 Si2 96.29(7) . .
C20 Mg1 C20 Si2 -164.82(9) 2_666 .
Mg1 Mg1 C20 Si2 -164.82(9) 2_666 .
Mg1 C10 Si1 C13 47.12(11) . .
Mg1 C10 Si1 C11 -72.99(11) . .
Mg1 C10 Si1 C12 166.13(8) . .
