#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:52:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179940 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/35/7023503.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_7023503
loop_
_publ_author_name
'Li, Yan'
'Wang, Jinjin'
'Wu, Yile'
'Zhu, Hongping'
'Samuel, Prinson P.'
'Roesky, Herbert W.'
_publ_section_title
;
 Synthesis of metallasiloxanes of group 13-15 and their application in
 catalysis.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13715
_journal_page_last               13722
_journal_paper_doi               10.1039/c3dt51408k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C42 H80 Al2 N2 O6 Si4'
_chemical_formula_weight         875.40
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.36(3)
_cell_angle_beta                 97.64(3)
_cell_angle_gamma                114.32(3)
_cell_formula_units_Z            1
_cell_length_a                   10.273(2)
_cell_length_b                   11.090(2)
_cell_length_c                   12.605(3)
_cell_measurement_reflns_used    3916
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.75
_cell_measurement_theta_min      6.08
_cell_volume                     1270.1(6)
_computing_cell_refinement       'rapid auto (rigaku 2004)'
_computing_data_collection       'rapid auto (rigaku 2004)'
_computing_data_reduction        'rapid auto (rigaku 2004)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'rigaku raxis rapid IP area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1024
_diffrn_reflns_av_unetI/netI     0.1285
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10419
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.9641
_exptl_absorpt_correction_T_min  0.9441
_exptl_absorpt_correction_type   'empirical absorption correction'
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment
'refined in a riding mode to the carrier atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1312
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0638P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1565
_reflns_number_gt                2818
_reflns_number_total             4893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51408k.txt
_cod_data_source_block           compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1270.1(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7023503
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
Si1 Si 0.33542(10) 0.77403(10) 0.42551(7) 0.0318(3) Uani 1 1 d .
Si2 Si 0.03886(10) 0.61267(11) 0.26554(8) 0.0370(3) Uani 1 1 d .
Al1 Al 0.67993(11) 0.94733(11) 0.47456(8) 0.0321(3) Uani 1 1 d .
O1 O 0.5043(2) 0.8300(2) 0.41643(17) 0.0353(6) Uani 1 1 d .
O2 O 0.2970(2) 0.8923(2) 0.47718(17) 0.0360(6) Uani 1 1 d .
O3 O 0.7585(2) 0.9735(2) 0.34795(17) 0.0373(6) Uani 1 1 d .
N1 N 0.2297(3) 0.6977(3) 0.2936(2) 0.0290(7) Uani 1 1 d .
C1 C 0.7981(4) 0.8811(4) 0.5610(3) 0.0488(11) Uani 1 1 d .
H1A H 0.7590 0.8585 0.6264 0.073 Uiso 1 1 calc R
H1B H 0.8990 0.9513 0.5829 0.073 Uiso 1 1 calc R
H1C H 0.7958 0.8003 0.5173 0.073 Uiso 1 1 calc R
C2 C 0.2912(4) 0.6447(4) 0.5130(3) 0.0437(10) Uani 1 1 d .
H2B H 0.3450 0.6878 0.5883 0.066 Uiso 1 1 calc R
H2C H 0.3194 0.5743 0.4852 0.066 Uiso 1 1 calc R
H2D H 0.1862 0.6042 0.5116 0.066 Uiso 1 1 calc R
C3 C -0.0392(4) 0.6312(5) 0.1295(3) 0.0589(13) Uani 1 1 d .
H3A H -0.0206 0.7257 0.1322 0.088 Uiso 1 1 calc R
H3B H -0.1446 0.5737 0.1111 0.088 Uiso 1 1 calc R
H3C H 0.0068 0.6039 0.0737 0.088 Uiso 1 1 calc R
C4 C -0.0344(4) 0.6811(4) 0.3725(3) 0.0495(11) Uani 1 1 d .
H4A H 0.0034 0.6686 0.4437 0.074 Uiso 1 1 calc R
H4B H -0.1412 0.6333 0.3557 0.074 Uiso 1 1 calc R
H4C H -0.0040 0.7777 0.3744 0.074 Uiso 1 1 calc R
C5 C -0.0309(4) 0.4277(4) 0.2606(4) 0.0596(12) Uani 1 1 d .
H5A H 0.0139 0.4125 0.3281 0.089 Uiso 1 1 calc R
H5B H -0.0061 0.3860 0.1979 0.089 Uiso 1 1 calc R
H5C H -0.1371 0.3872 0.2532 0.089 Uiso 1 1 calc R
C6 C 0.7289(4) 0.8609(4) 0.2592(3) 0.0439(10) Uani 1 1 d .
H6A H 0.6256 0.8196 0.2204 0.053 Uiso 1 1 calc R
H6B H 0.7509 0.7907 0.2875 0.053 Uiso 1 1 calc R
C7 C 0.8296(4) 0.9248(4) 0.1848(3) 0.0545(11) Uani 1 1 d .
H7A H 0.7889 0.8746 0.1082 0.065 Uiso 1 1 calc R
H7B H 0.9273 0.9285 0.2084 0.065 Uiso 1 1 calc R
C8 C 0.8371(5) 1.0649(4) 0.1972(3) 0.0614(13) Uani 1 1 d .
H8A H 0.9273 1.1285 0.1780 0.074 Uiso 1 1 calc R
H8B H 0.7517 1.0641 0.1497 0.074 Uiso 1 1 calc R
C9 C 0.8366(4) 1.1040(4) 0.3154(3) 0.0403(9) Uani 1 1 d .
H9A H 0.9374 1.1534 0.3592 0.048 Uiso 1 1 calc R
H9B H 0.7849 1.1615 0.3249 0.048 Uiso 1 1 calc R
C11 C 0.2995(3) 0.7030(4) 0.2007(3) 0.0320(8) Uani 1 1 d .
C12 C 0.3397(4) 0.6004(4) 0.1644(3) 0.0380(9) Uani 1 1 d .
C13 C 0.4005(4) 0.6056(4) 0.0710(3) 0.0460(10) Uani 1 1 d .
H13A H 0.4274 0.5364 0.0458 0.055 Uiso 1 1 calc R
C14 C 0.4223(4) 0.7086(4) 0.0150(3) 0.0464(10) Uani 1 1 d .
H14A H 0.4613 0.7093 -0.0493 0.056 Uiso 1 1 calc R
C15 C 0.3866(4) 0.8113(4) 0.0533(3) 0.0434(10) Uani 1 1 d .
H15A H 0.4037 0.8835 0.0156 0.052 Uiso 1 1 calc R
C16 C 0.3265(3) 0.8114(3) 0.1456(3) 0.0327(9) Uani 1 1 d .
C121 C 0.3250(4) 0.4871(4) 0.2252(3) 0.0413(9) Uani 1 1 d .
H12A H 0.2631 0.4890 0.2797 0.050 Uiso 1 1 calc R
C122 C 0.4730(4) 0.5080(4) 0.2884(3) 0.0594(12) Uani 1 1 d .
H12B H 0.5154 0.5924 0.3432 0.089 Uiso 1 1 calc R
H12C H 0.5386 0.5129 0.2376 0.089 Uiso 1 1 calc R
H12D H 0.4599 0.4322 0.3250 0.089 Uiso 1 1 calc R
C123 C 0.2489(5) 0.3466(4) 0.1495(3) 0.0604(12) Uani 1 1 d .
H12E H 0.1554 0.3346 0.1077 0.091 Uiso 1 1 calc R
H12F H 0.2318 0.2769 0.1935 0.091 Uiso 1 1 calc R
H12G H 0.3112 0.3388 0.0990 0.091 Uiso 1 1 calc R
C161 C 0.2950(4) 0.9294(3) 0.1862(3) 0.0349(9) Uani 1 1 d .
H16A H 0.2301 0.9022 0.2399 0.042 Uiso 1 1 calc R
C162 C 0.4385(4) 1.0532(4) 0.2466(3) 0.0476(10) Uani 1 1 d .
H16B H 0.4852 1.0288 0.3078 0.071 Uiso 1 1 calc R
H16C H 0.4165 1.1278 0.2744 0.071 Uiso 1 1 calc R
H16D H 0.5046 1.0812 0.1958 0.071 Uiso 1 1 calc R
C163 C 0.2181(4) 0.9719(4) 0.0959(3) 0.0505(11) Uani 1 1 d .
H16E H 0.1316 0.8926 0.0532 0.076 Uiso 1 1 calc R
H16F H 0.2850 1.0110 0.0478 0.076 Uiso 1 1 calc R
H16G H 0.1886 1.0391 0.1288 0.076 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'
O O 0.0106 0.0060 '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'
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
O2 Si1 O1 112.08(13) . .
O2 Si1 N1 109.95(13) . .
O1 Si1 N1 107.57(13) . .
O2 Si1 C2 108.28(16) . .
O1 Si1 C2 110.09(16) . .
N1 Si1 C2 108.83(15) . .
N1 Si2 C4 110.11(15) . .
N1 Si2 C5 113.03(16) . .
C4 Si2 C5 107.4(2) . .
N1 Si2 C3 110.72(16) . .
C4 Si2 C3 109.1(2) . .
C5 Si2 C3 106.3(2) . .
O2 Al1 O1 116.31(13) 2_676 .
O2 Al1 O3 99.94(12) 2_676 .
O1 Al1 O3 99.94(11) . .
O2 Al1 C1 116.69(15) 2_676 .
O1 Al1 C1 115.40(16) . .
O3 Al1 C1 104.59(15) . .
Si1 O1 Al1 145.51(15) . .
Si1 O2 Al1 158.62(16) . 2_676
C6 O3 C9 110.4(3) . .
C6 O3 Al1 122.2(2) . .
C9 O3 Al1 126.8(2) . .
C11 N1 Si1 120.09(19) . .
C11 N1 Si2 116.50(19) . .
Si1 N1 Si2 123.41(16) . .
Al1 C1 H1A 109.5 . .
Al1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Al1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Si1 C2 H2B 109.5 . .
Si1 C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
Si1 C2 H2D 109.5 . .
H2B C2 H2D 109.5 . .
H2C C2 H2D 109.5 . .
Si2 C3 H3A 109.5 . .
Si2 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
Si2 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
Si2 C4 H4A 109.5 . .
Si2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
Si2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
Si2 C5 H5A 109.5 . .
Si2 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
Si2 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
O3 C6 C7 104.1(3) . .
O3 C6 H6A 110.9 . .
C7 C6 H6A 110.9 . .
O3 C6 H6B 110.9 . .
C7 C6 H6B 110.9 . .
H6A C6 H6B 108.9 . .
C6 C7 C8 102.9(3) . .
C6 C7 H7A 111.2 . .
C8 C7 H7A 111.2 . .
C6 C7 H7B 111.2 . .
C8 C7 H7B 111.2 . .
H7A C7 H7B 109.1 . .
C9 C8 C7 104.7(3) . .
C9 C8 H8A 110.8 . .
C7 C8 H8A 110.8 . .
C9 C8 H8B 110.8 . .
C7 C8 H8B 110.8 . .
H8A C8 H8B 108.9 . .
O3 C9 C8 104.1(3) . .
O3 C9 H9A 110.9 . .
C8 C9 H9A 110.9 . .
O3 C9 H9B 110.9 . .
C8 C9 H9B 110.9 . .
H9A C9 H9B 109.0 . .
C12 C11 C16 119.8(3) . .
C12 C11 N1 120.5(3) . .
C16 C11 N1 119.8(3) . .
C13 C12 C11 118.8(4) . .
C13 C12 C121 118.8(3) . .
C11 C12 C121 122.4(3) . .
C14 C13 C12 121.6(4) . .
C14 C13 H13A 119.2 . .
C12 C13 H13A 119.2 . .
C13 C14 C15 119.2(4) . .
C13 C14 H14A 120.4 . .
C15 C14 H14A 120.4 . .
C14 C15 C16 121.6(4) . .
C14 C15 H15A 119.2 . .
C16 C15 H15A 119.2 . .
C15 C16 C11 119.0(3) . .
C15 C16 C161 119.2(3) . .
C11 C16 C161 121.8(3) . .
C12 C121 C122 111.6(3) . .
C12 C121 C123 112.7(3) . .
C122 C121 C123 109.7(3) . .
C12 C121 H12A 107.5 . .
C122 C121 H12A 107.5 . .
C123 C121 H12A 107.5 . .
C121 C122 H12B 109.5 . .
C121 C122 H12C 109.5 . .
H12B C122 H12C 109.5 . .
C121 C122 H12D 109.5 . .
H12B C122 H12D 109.5 . .
H12C C122 H12D 109.5 . .
C121 C123 H12E 109.5 . .
C121 C123 H12F 109.5 . .
H12E C123 H12F 109.5 . .
C121 C123 H12G 109.5 . .
H12E C123 H12G 109.5 . .
H12F C123 H12G 109.5 . .
C16 C161 C163 113.9(3) . .
C16 C161 C162 110.2(3) . .
C163 C161 C162 108.8(3) . .
C16 C161 H16A 107.9 . .
C163 C161 H16A 107.9 . .
C162 C161 H16A 107.9 . .
C161 C162 H16B 109.5 . .
C161 C162 H16C 109.5 . .
H16B C162 H16C 109.5 . .
C161 C162 H16D 109.5 . .
H16B C162 H16D 109.5 . .
H16C C162 H16D 109.5 . .
C161 C163 H16E 109.5 . .
C161 C163 H16F 109.5 . .
H16E C163 H16F 109.5 . .
C161 C163 H16G 109.5 . .
H16E C163 H16G 109.5 . .
H16F C163 H16G 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 O2 1.605(2) .
Si1 O1 1.611(2) .
Si1 N1 1.750(3) .
Si1 C2 1.866(4) .
Si2 N1 1.751(3) .
Si2 C4 1.854(4) .
Si2 C5 1.863(4) .
Si2 C3 1.867(4) .
Al1 O2 1.711(3) 2_676
Al1 O1 1.719(2) .
Al1 O3 1.884(2) .
Al1 C1 1.947(4) .
O2 Al1 1.711(3) 2_676
O3 C6 1.464(4) .
O3 C9 1.479(4) .
N1 C11 1.448(4) .
C1 H1A 0.9800 .
C1 H1B 0.9800 .
C1 H1C 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C2 H2D 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 C7 1.509(5) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.511(6) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C9 1.500(5) .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C11 C12 1.406(5) .
C11 C16 1.412(5) .
C12 C13 1.400(5) .
C12 C121 1.519(5) .
C13 C14 1.375(5) .
C13 H13A 0.9500 .
C14 C15 1.383(5) .
C14 H14A 0.9500 .
C15 C16 1.388(5) .
C15 H15A 0.9500 .
C16 C161 1.518(5) .
C121 C122 1.531(5) .
C121 C123 1.539(5) .
C121 H12A 1.0000 .
C122 H12B 0.9800 .
C122 H12C 0.9800 .
C122 H12D 0.9800 .
C123 H12E 0.9800 .
C123 H12F 0.9800 .
C123 H12G 0.9800 .
C161 C163 1.532(5) .
C161 C162 1.551(4) .
C161 H16A 1.0000 .
C162 H16B 0.9800 .
C162 H16C 0.9800 .
C162 H16D 0.9800 .
C163 H16E 0.9800 .
C163 H16F 0.9800 .
C163 H16G 0.9800 .
