#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:21:33 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180134 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/32/7103212.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_7103212
loop_
_publ_author_name
'Solomon, Sophia A'
'Muryn, Christopher A'
'Layfield, Richard A'
_publ_section_title
;
 s-Block metal complexes of a bulky, donor-functionalized allyl ligand.
;
_journal_issue                   27
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3142
_journal_page_last               3144
_journal_paper_doi               10.1039/b803364a
_journal_year                    2008
_chemical_formula_sum            'C28 H58 Mg O2 Si4'
_chemical_formula_weight         563.41
_chemical_name_systematic
;
?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.0480(10)
_cell_length_b                   15.1550(10)
_cell_length_c                   19.4280(10)
_cell_measurement_reflns_used    2176
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.6568
_cell_measurement_theta_min      2.6866
_cell_volume                     3547.3(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
;
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Oxford Diffraction XCalibur 2'
_diffrn_measurement_method       'phi and omega'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_av_sigmaI/netI    0.1451
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11765
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         4.20
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  0.9797
_exptl_absorpt_correction_T_min  0.8524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET)
(compiled Apr 27 2007,17:53:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            White
_exptl_crystal_density_diffrn    1.055
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         3120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1348
_refine_ls_R_factor_gt           0.0572
_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)+(0.0360P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.1075
_reflns_number_gt                1655
_reflns_number_total             3120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b803364a.txt
_cod_data_source_block           compound3
_cod_database_code               7103212
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'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
Mg1 Mg 0.7500 0.2500 0.45240(7) 0.0197(4) Uani 1 2 d S . .
O1 O 0.71838(18) 0.34424(16) 0.52649(10) 0.0212(6) Uani 1 1 d . . .
Si1 Si 0.99062(8) 0.22890(7) 0.35472(5) 0.0234(3) Uani 1 1 d . . .
Si2 Si 0.79788(8) 0.55615(7) 0.37476(5) 0.0215(3) Uani 1 1 d . . .
C1 C 0.9087(3) 0.2961(2) 0.41318(18) 0.0211(10) Uani 1 1 d . . .
C2 C 0.8701(3) 0.3818(3) 0.38860(18) 0.0184(9) Uani 1 1 d . . .
C3 C 0.8442(3) 0.4573(2) 0.42163(16) 0.0178(9) Uani 1 1 d . . .
C4 C 0.8547(3) 0.4602(2) 0.49959(16) 0.0215(9) Uani 1 1 d . . .
H4A H 0.9150 0.4196 0.5136 0.026 Uiso 1 1 calc R . .
H4B H 0.8770 0.5205 0.5133 0.026 Uiso 1 1 calc R . .
C5 C 0.7515(3) 0.4358(2) 0.53856(15) 0.0203(9) Uani 1 1 d . . .
H5 H 0.6897 0.4754 0.5235 0.024 Uiso 1 1 calc R . .
C6 C 0.7600(3) 0.4392(2) 0.61630(15) 0.0223(9) Uani 1 1 d . . .
H6A H 0.7493 0.5002 0.6334 0.027 Uiso 1 1 calc R . .
H6B H 0.8330 0.4173 0.6321 0.027 Uiso 1 1 calc R . .
C7 C 0.6666(3) 0.3790(3) 0.64087(17) 0.0297(10) Uani 1 1 d . . .
H7A H 0.6926 0.3401 0.6785 0.036 Uiso 1 1 calc R . .
H7B H 0.6027 0.4141 0.6576 0.036 Uiso 1 1 calc R . .
C8 C 0.6346(3) 0.3251(3) 0.57812(17) 0.0308(11) Uani 1 1 d . . .
H8A H 0.6338 0.2614 0.5893 0.037 Uiso 1 1 calc R . .
H8B H 0.5600 0.3424 0.5614 0.037 Uiso 1 1 calc R . .
C9 C 0.9030(3) 0.1793(3) 0.28540(17) 0.0347(11) Uani 1 1 d . . .
H9A H 0.8516 0.1364 0.3057 0.052 Uiso 1 1 calc R . .
H9B H 0.9507 0.1495 0.2518 0.052 Uiso 1 1 calc R . .
H9C H 0.8606 0.2259 0.2623 0.052 Uiso 1 1 calc R . .
C10 C 1.1000(3) 0.2957(3) 0.31003(19) 0.0385(11) Uani 1 1 d . . .
H10A H 1.0653 0.3459 0.2867 0.058 Uiso 1 1 calc R . .
H10B H 1.1382 0.2587 0.2761 0.058 Uiso 1 1 calc R . .
H10C H 1.1537 0.3173 0.3439 0.058 Uiso 1 1 calc R . .
C11 C 1.0582(3) 0.1380(3) 0.40355(19) 0.0346(11) Uani 1 1 d . . .
H11A H 1.1138 0.1627 0.4349 0.052 Uiso 1 1 calc R . .
H11B H 1.0944 0.0974 0.3713 0.052 Uiso 1 1 calc R . .
H11C H 1.0021 0.1060 0.4301 0.052 Uiso 1 1 calc R . .
C12 C 0.8167(3) 0.5415(2) 0.28037(17) 0.0332(11) Uani 1 1 d . . .
H12A H 0.8937 0.5249 0.2708 0.050 Uiso 1 1 calc R . .
H12B H 0.7994 0.5970 0.2568 0.050 Uiso 1 1 calc R . .
H12C H 0.7668 0.4950 0.2639 0.050 Uiso 1 1 calc R . .
C13 C 0.8789(3) 0.6549(3) 0.4016(2) 0.0397(11) Uani 1 1 d . . .
H13A H 0.8707 0.6637 0.4513 0.060 Uiso 1 1 calc R . .
H13B H 0.8512 0.7070 0.3771 0.060 Uiso 1 1 calc R . .
H13C H 0.9574 0.6460 0.3905 0.060 Uiso 1 1 calc R . .
C14 C 0.6480(3) 0.5813(3) 0.38999(18) 0.0345(11) Uani 1 1 d . . .
H14A H 0.6031 0.5297 0.3779 0.052 Uiso 1 1 calc R . .
H14B H 0.6258 0.6316 0.3615 0.052 Uiso 1 1 calc R . .
H14C H 0.6367 0.5958 0.4386 0.052 Uiso 1 1 calc R . .
H1 H 0.943(3) 0.303(2) 0.4557(17) 0.041 Uiso 1 1 d . . .
H2 H 0.859(3) 0.381(2) 0.3405(17) 0.041 Uiso 1 1 d . . .
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'
O O 0.0106 0.0060 '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
_geom_angle_publ_flag
O1 Mg1 O1 91.52(13) . 2_655 ?
O1 Mg1 C1 100.65(12) . . ?
O1 Mg1 C1 107.73(11) 2_655 . ?
O1 Mg1 C1 107.73(11) . 2_655 ?
O1 Mg1 C1 100.65(12) 2_655 2_655 ?
C1 Mg1 C1 138.9(2) . 2_655 ?
O1 Mg1 C2 135.84(10) . 2_655 ?
O1 Mg1 C2 84.78(10) 2_655 2_655 ?
C1 Mg1 C2 122.42(13) . 2_655 ?
C1 Mg1 C2 31.69(11) 2_655 2_655 ?
C8 O1 C5 105.5(2) . . ?
C8 O1 Mg1 118.2(2) . . ?
C5 O1 Mg1 135.92(19) . . ?
C1 Si1 C11 109.51(17) . . ?
C1 Si1 C9 111.64(16) . . ?
C11 Si1 C9 108.47(18) . . ?
C1 Si1 C10 111.67(18) . . ?
C11 Si1 C10 109.15(18) . . ?
C9 Si1 C10 106.28(17) . . ?
C3 Si2 C12 110.73(16) . . ?
C3 Si2 C13 110.90(17) . . ?
C12 Si2 C13 107.93(17) . . ?
C3 Si2 C14 112.40(17) . . ?
C12 Si2 C14 107.33(17) . . ?
C13 Si2 C14 107.34(19) . . ?
C2 C1 Si1 117.8(3) . . ?
C2 C1 Mg1 96.9(2) . . ?
Si1 C1 Mg1 121.16(19) . . ?
C2 C1 H1 110(2) . . ?
Si1 C1 H1 112(2) . . ?
Mg1 C1 H1 97(2) . . ?
C3 C2 C1 132.3(3) . . ?
C3 C2 H2 116(2) . . ?
C1 C2 H2 111(2) . . ?
C2 C3 C4 118.6(3) . . ?
C2 C3 Si2 121.7(3) . . ?
C4 C3 Si2 119.7(3) . . ?
C5 C4 C3 115.3(3) . . ?
C5 C4 H4A 108.5 . . ?
C3 C4 H4A 108.5 . . ?
C5 C4 H4B 108.5 . . ?
C3 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
O1 C5 C4 112.2(3) . . ?
O1 C5 C6 102.2(3) . . ?
C4 C5 C6 116.0(3) . . ?
O1 C5 H5 108.7 . . ?
C4 C5 H5 108.7 . . ?
C6 C5 H5 108.7 . . ?
C5 C6 C7 104.0(3) . . ?
C5 C6 H6A 111.0 . . ?
C7 C6 H6A 111.0 . . ?
C5 C6 H6B 111.0 . . ?
C7 C6 H6B 111.0 . . ?
H6A C6 H6B 109.0 . . ?
C8 C7 C6 105.0(3) . . ?
C8 C7 H7A 110.8 . . ?
C6 C7 H7A 110.8 . . ?
C8 C7 H7B 110.8 . . ?
C6 C7 H7B 110.8 . . ?
H7A C7 H7B 108.8 . . ?
O1 C8 C7 105.7(3) . . ?
O1 C8 H8A 110.6 . . ?
C7 C8 H8A 110.6 . . ?
O1 C8 H8B 110.6 . . ?
C7 C8 H8B 110.6 . . ?
H8A C8 H8B 108.7 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
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 . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si2 C14 H14A 109.5 . . ?
Si2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
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
Mg1 O1 2.063(2) . ?
Mg1 O1 2.063(2) 2_655 ?
Mg1 C1 2.173(4) . ?
Mg1 C1 2.173(4) 2_655 ?
Mg1 C2 2.761(4) 2_655 ?
O1 C8 1.452(4) . ?
O1 C5 1.462(4) . ?
Si1 C1 1.817(4) . ?
Si1 C11 1.860(4) . ?
Si1 C9 1.869(3) . ?
Si1 C10 1.875(4) . ?
Si2 C3 1.840(4) . ?
Si2 C12 1.861(3) . ?
Si2 C13 1.861(4) . ?
Si2 C14 1.869(4) . ?
C1 C2 1.461(5) . ?
C1 H1 0.93(3) . ?
C2 C3 1.348(5) . ?
C2 H2 0.94(3) . ?
C3 C4 1.520(4) . ?
C4 C5 1.502(5) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.515(4) . ?
C5 H5 1.0000 . ?
C6 C7 1.525(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.517(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Mg1 O1 C8 -55.1(2) 2_655 . . . ?
C1 Mg1 O1 C8 -163.5(2) . . . . ?
C1 Mg1 O1 C8 46.6(2) 2_655 . . . ?
C2 Mg1 O1 C8 29.0(3) 2_655 . . . ?
O1 Mg1 O1 C5 133.1(3) 2_655 . . . ?
C1 Mg1 O1 C5 24.8(3) . . . . ?
C1 Mg1 O1 C5 -125.2(3) 2_655 . . . ?
C2 Mg1 O1 C5 -142.8(3) 2_655 . . . ?
C11 Si1 C1 C2 166.1(3) . . . . ?
C9 Si1 C1 C2 -73.8(3) . . . . ?
C10 Si1 C1 C2 45.1(3) . . . . ?
C11 Si1 C1 Mg1 -75.3(2) . . . . ?
C9 Si1 C1 Mg1 44.8(3) . . . . ?
C10 Si1 C1 Mg1 163.65(19) . . . . ?
O1 Mg1 C1 C2 -61.3(2) . . . . ?
O1 Mg1 C1 C2 -156.3(2) 2_655 . . . ?
C1 Mg1 C1 C2 72.2(2) 2_655 . . . ?
C2 Mg1 C1 C2 108.5(3) 2_655 . . . ?
O1 Mg1 C1 Si1 170.18(19) . . . . ?
O1 Mg1 C1 Si1 75.1(2) 2_655 . . . ?
C1 Mg1 C1 Si1 -56.38(18) 2_655 . . . ?
C2 Mg1 C1 Si1 -20.1(3) 2_655 . . . ?
Si1 C1 C2 C3 -153.3(3) . . . . ?
Mg1 C1 C2 C3 75.9(4) . . . . ?
C1 C2 C3 C4 0.0(6) . . . . ?
C1 C2 C3 Si2 179.7(3) . . . . ?
C12 Si2 C3 C2 -9.8(4) . . . . ?
C13 Si2 C3 C2 -129.6(3) . . . . ?
C14 Si2 C3 C2 110.2(3) . . . . ?
C12 Si2 C3 C4 169.8(3) . . . . ?
C13 Si2 C3 C4 50.0(3) . . . . ?
C14 Si2 C3 C4 -70.2(3) . . . . ?
C2 C3 C4 C5 -91.3(4) . . . . ?
Si2 C3 C4 C5 89.1(4) . . . . ?
C8 O1 C5 C4 167.7(3) . . . . ?
Mg1 O1 C5 C4 -19.8(4) . . . . ?
C8 O1 C5 C6 42.8(3) . . . . ?
Mg1 O1 C5 C6 -144.8(2) . . . . ?
C3 C4 C5 O1 63.7(4) . . . . ?
C3 C4 C5 C6 -179.3(3) . . . . ?
O1 C5 C6 C7 -35.8(3) . . . . ?
C4 C5 C6 C7 -158.2(3) . . . . ?
C5 C6 C7 C8 16.4(4) . . . . ?
C5 O1 C8 C7 -32.6(3) . . . . ?
Mg1 O1 C8 C7 153.3(2) . . . . ?
C6 C7 C8 O1 9.2(4) . . . . ?
