#------------------------------------------------------------------------------
#$Date: 2016-03-26 03:03:07 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180166 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/62/7106281.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_7106281
loop_
_publ_author_name
'Benjamin M. Day'
'Natalie E. Mansfield'
'Martyn P. Coles'
'Peter B. Hitchcock'
_publ_section_title
;
 Bicyclic guanidinate compounds of magnesium and their activity as
 pre-catalysts in the Tishchenko reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              4995
_journal_paper_doi               10.1039/c0cc04789a
_journal_volume                  47
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C26 H60 Mg2 N8 Si4'
_chemical_formula_sum            'C26 H60 Mg2 N8 Si4'
_chemical_formula_weight         645.8
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-06-19T13:40:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3450(2)
_cell_length_b                   16.7408(3)
_cell_length_c                   18.0363(4)
_cell_measurement_reflns_used    16889
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3727.48(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.765528E-1
_diffrn_orient_matrix_UB_12      0.84448E-2
_diffrn_orient_matrix_UB_13      -0.163446E-1
_diffrn_orient_matrix_UB_21      0.214967E-1
_diffrn_orient_matrix_UB_22      0.116458E-1
_diffrn_orient_matrix_UB_23      0.523515E-1
_diffrn_orient_matrix_UB_31      0.154687E-1
_diffrn_orient_matrix_UB_32      -0.579763E-1
_diffrn_orient_matrix_UB_33      0.81352E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.028
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30490
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         3.52
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.221
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.043
_refine_ls_R_factor_gt           0.033
_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)+(0.0341P)²+2.0133P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                3095
_reflns_number_total             3652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc04789a.txt
_cod_data_source_block           (3)-jun1506
_cod_database_code               7106281
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'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
Si1 Si 0.46241(4) 0.59657(2) 0.70769(3) 0.02293(12) Uani 1 1 d . A .
Si2 Si 0.39155(4) 0.42687(3) 0.73467(3) 0.02539(13) Uani 1 1 d . A .
Mg Mg 0.48267(4) 0.47428(3) 0.57668(3) 0.02145(14) Uani 1 1 d . . .
N1 N 0.62645(10) 0.49202(8) 0.50894(8) 0.0224(3) Uani 1 1 d . . .
N2 N 0.55754(11) 0.37120(8) 0.53874(8) 0.0278(3) Uani 1 1 d . . .
N3 N 0.74357(11) 0.37833(9) 0.50816(8) 0.0307(3) Uani 1 1 d . . .
N4 N 0.44220(11) 0.50058(7) 0.68006(7) 0.0217(3) Uani 1 1 d . . .
C1 C 0.64486(13) 0.41144(10) 0.51821(9) 0.0240(4) Uani 1 1 d . A .
C2 C 0.72415(13) 0.54239(11) 0.50607(10) 0.0306(4) Uani 1 1 d . A .
H2A H 0.7545 0.5484 0.5566 0.037 Uiso 1 1 calc R . .
H2B H 0.7049 0.5962 0.4874 0.037 Uiso 1 1 calc R . .
C3 C 0.80840(15) 0.50495(12) 0.45543(11) 0.0387(5) Uani 1 1 d . . .
H3A H 0.7786 0.4991 0.4048 0.046 Uiso 1 1 calc R A .
H3B H 0.8733 0.5396 0.4528 0.046 Uiso 1 1 calc R . .
C4 C 0.83907(15) 0.42386(13) 0.48595(12) 0.0419(5) Uani 1 1 d . A .
H4A H 0.8795 0.3936 0.4477 0.05 Uiso 1 1 calc R . .
H4B H 0.8873 0.4309 0.5293 0.05 Uiso 1 1 calc R . .
C8 C 0.33753(16) 0.65968(11) 0.69973(13) 0.0424(5) Uani 1 1 d . . .
H8A H 0.2798 0.6366 0.7303 0.064 Uiso 1 1 calc R A .
H8B H 0.314 0.6614 0.6478 0.064 Uiso 1 1 calc R . .
H8C H 0.3535 0.714 0.7169 0.064 Uiso 1 1 calc R . .
C9 C 0.51113(17) 0.60657(11) 0.80586(11) 0.0378(4) Uani 1 1 d . . .
H9A H 0.4583 0.5822 0.8395 0.057 Uiso 1 1 calc R A .
H9B H 0.5195 0.6633 0.8181 0.057 Uiso 1 1 calc R . .
H9C H 0.5811 0.5795 0.8112 0.057 Uiso 1 1 calc R . .
C10 C 0.56848(15) 0.64470(10) 0.64798(11) 0.0345(4) Uani 1 1 d . . .
H10A H 0.6356 0.6135 0.6506 0.052 Uiso 1 1 calc R A .
H10B H 0.5822 0.6991 0.6656 0.052 Uiso 1 1 calc R . .
H10C H 0.543 0.6466 0.5965 0.052 Uiso 1 1 calc R . .
C11 C 0.49529(18) 0.38383(13) 0.79913(14) 0.0512(6) Uani 1 1 d . . .
H11A H 0.5245 0.4263 0.8307 0.077 Uiso 1 1 calc R A .
H11B H 0.5541 0.3599 0.7702 0.077 Uiso 1 1 calc R . .
H11C H 0.4615 0.3428 0.8302 0.077 Uiso 1 1 calc R . .
C12 C 0.27452(17) 0.45993(13) 0.79345(12) 0.0439(5) Uani 1 1 d . . .
H12A H 0.2974 0.5043 0.8253 0.066 Uiso 1 1 calc R A .
H12B H 0.25 0.4153 0.8243 0.066 Uiso 1 1 calc R . .
H12C H 0.215 0.4776 0.7614 0.066 Uiso 1 1 calc R . .
C13 C 0.33991(18) 0.34230(11) 0.67658(12) 0.0451(5) Uani 1 1 d . . .
H13A H 0.2851 0.3623 0.642 0.068 Uiso 1 1 calc R A .
H13B H 0.3076 0.3016 0.7087 0.068 Uiso 1 1 calc R . .
H13C H 0.4001 0.3188 0.6486 0.068 Uiso 1 1 calc R . .
C5 C 0.76366(16) 0.29433(12) 0.52629(12) 0.0438(5) Uani 0.829(6) 1 d P A 1
H5A H 0.8329 0.2899 0.5537 0.053 Uiso 0.829(6) 1 calc PR A 1
H5B H 0.7707 0.2633 0.4798 0.053 Uiso 0.829(6) 1 calc PR A 1
C6 C 0.6737(2) 0.25930(14) 0.57264(15) 0.0433(8) Uani 0.829(6) 1 d P A 1
H6A H 0.6791 0.2003 0.5725 0.052 Uiso 0.829(6) 1 calc PR A 1
H6B H 0.6807 0.278 0.6245 0.052 Uiso 0.829(6) 1 calc PR A 1
C7 C 0.56650(17) 0.28411(10) 0.54220(13) 0.0432(5) Uani 0.829(6) 1 d P A 1
H7A H 0.5574 0.2615 0.4918 0.052 Uiso 0.829(6) 1 calc PR A 1
H7B H 0.508 0.2626 0.574 0.052 Uiso 0.829(6) 1 calc PR A 1
C5A C 0.76366(16) 0.29433(12) 0.52629(12) 0.0438(5) Uani 0.171(6) 1 d P A 2
H5A1 H 0.7852 0.2887 0.5789 0.053 Uiso 0.171(6) 1 calc PR A 2
H5A2 H 0.8221 0.2724 0.4947 0.053 Uiso 0.171(6) 1 calc PR A 2
C6A C 0.6524(9) 0.2487(7) 0.5110(7) 0.040(4) Uiso 0.171(6) 1 d P A 2
H6A1 H 0.6407 0.2454 0.4568 0.048 Uiso 0.171(6) 1 calc PR A 2
H6A2 H 0.6583 0.1935 0.5303 0.048 Uiso 0.171(6) 1 calc PR A 2
C7A C 0.56650(17) 0.28411(10) 0.54220(13) 0.0432(5) Uani 0.171(6) 1 d P A 2
H7A1 H 0.5651 0.2685 0.5951 0.052 Uiso 0.171(6) 1 calc PR A 2
H7A2 H 0.5007 0.2614 0.519 0.052 Uiso 0.171(6) 1 calc PR A 2
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'
Mg Mg 0.0486 0.0363 '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
N4 Si1 C8 112.91(8) . . ?
N4 Si1 C10 109.87(7) . . ?
C8 Si1 C10 106.73(9) . . ?
N4 Si1 C9 114.05(8) . . ?
C8 Si1 C9 106.58(10) . . ?
C10 Si1 C9 106.22(9) . . ?
N4 Si2 C13 110.49(8) . . ?
N4 Si2 C11 112.81(8) . . ?
C13 Si2 C11 106.80(11) . . ?
N4 Si2 C12 113.39(8) . . ?
C13 Si2 C12 106.09(10) . . ?
C11 Si2 C12 106.81(11) . . ?
N4 Mg N2 127.47(6) . . ?
N4 Mg N1 117.73(6) . 5_666 ?
N2 Mg N1 105.28(6) . 5_666 ?
N4 Mg N1 134.79(6) . . ?
N2 Mg N1 64.19(5) . . ?
N1 Mg N1 94.17(5) 5_666 . ?
C1 N1 C2 115.45(13) . . ?
C1 N1 Mg 116.90(10) . 5_666 ?
C2 N1 Mg 109.97(10) . 5_666 ?
C1 N1 Mg 86.15(9) . . ?
C2 N1 Mg 140.02(11) . . ?
Mg N1 Mg 85.83(5) 5_666 . ?
C1 N2 C7 117.21(14) . . ?
C1 N2 Mg 91.82(10) . . ?
C7 N2 Mg 148.06(13) . . ?
C1 N3 C4 123.44(15) . . ?
C1 N3 C5 121.11(15) . . ?
C4 N3 C5 115.19(14) . . ?
Si2 N4 Si1 124.79(8) . . ?
Si2 N4 Mg 118.52(7) . . ?
Si1 N4 Mg 116.68(7) . . ?
N2 C1 N3 124.27(15) . . ?
N2 C1 N1 113.43(14) . . ?
N3 C1 N1 122.29(15) . . ?
N1 C2 C3 110.22(15) . . ?
N1 C2 H2A 109.6 . . ?
C3 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 C2 108.83(15) . . ?
C4 C3 H3A 109.9 . . ?
C2 C3 H3A 109.9 . . ?
C4 C3 H3B 109.9 . . ?
C2 C3 H3B 109.9 . . ?
H3A C3 H3B 108.3 . . ?
N3 C4 C3 111.48(15) . . ?
N3 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
N3 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
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 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si2 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 . . ?
N3 C5 C6 111.86(16) . . ?
N3 C5 H5A 109.2 . . ?
C6 C5 H5A 109.2 . . ?
N3 C5 H5B 109.2 . . ?
C6 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
C7 C6 C5 109.93(19) . . ?
C7 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C7 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
N2 C7 C6 111.10(17) . . ?
N2 C7 H7A 109.4 . . ?
C6 C7 H7A 109.4 . . ?
N2 C7 H7B 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108 . . ?
H6A1 C6A H6A2 107.7 . . ?
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 N4 1.7009(13) . ?
Si1 C8 1.8745(19) . ?
Si1 C10 1.8770(18) . ?
Si1 C9 1.8774(19) . ?
Si2 N4 1.6983(13) . ?
Si2 C13 1.873(2) . ?
Si2 C11 1.874(2) . ?
Si2 C12 1.876(2) . ?
Mg N4 1.9798(14) . ?
Mg N2 2.0738(14) . ?
Mg N1 2.1255(14) 5_666 ?
Mg N1 2.1752(14) . ?
N1 C1 1.378(2) . ?
N1 C2 1.473(2) . ?
N1 Mg 2.1255(14) 5_666 ?
N2 C1 1.324(2) . ?
N2 C7 1.464(2) . ?
N3 C1 1.351(2) . ?
N3 C4 1.460(2) . ?
N3 C5 1.465(2) . ?
C2 C3 1.520(2) . ?
C2 H2A 0.99 . ?
C2 H2B 0.99 . ?
C3 C4 1.513(3) . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C5 C6 1.508(3) . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 C7 1.492(3) . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C6A H6A1 0.99 . ?
C6A H6A2 0.99 . ?
