#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:50:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179131 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/93/4309385.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_4309385
loop_
_publ_author_name
'Vojtech Jancik'
'Herbert W. Roesky'
_publ_contact_author_address
;Institut für Anorganische Chemie, 
Georg-August-Universität Göttingen, 
Tammannstrasse 4, D 37077 Göttingen, Germany
;
_publ_contact_author_email       vjancik@centrum.cz
_publ_contact_author_fax         +49-551-393373
_publ_contact_author_name        'Vojtech Jancik'
_publ_contact_author_phone       +49-551-393010
_publ_section_title
;
Unusual Anions [LAl(SH)(S)]- and [LAl(S)2]2- Stabilized by Weakly
Coordinating Imidazolium Cations. Synthesis of LAl(SSiMe2)2O (L =
HC[C(Me)N(Ar)]2, Ar = 2,6-iPr2C6H3)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5556
_journal_page_last               5558
_journal_paper_doi               10.1021/ic050693q
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C33 H53 Al N2 O S2 Si2'
_chemical_formula_weight         641.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 104.29(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.749(3)
_cell_length_b                   18.857(4)
_cell_length_c                   15.726(3)
_cell_measurement_reflns_used    5253
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.05
_cell_measurement_theta_min      3.73
_cell_volume                     3663.7(14)
_computing_cell_refinement       'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_data_collection       'Proteum (v 1.40, Bruker 2002)'
_computing_data_reduction        'Bruker AXS SAINT (v 7.01A, Bruker 2003)'
_computing_molecular_graphics    'Bruker AXS SHELXTL (v 6.12)'
_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 5.602
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker three circle diffractometer'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'mirror system'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23505
_diffrn_reflns_theta_full        59.05
_diffrn_reflns_theta_max         59.05
_diffrn_reflns_theta_min         3.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.375
_exptl_absorpt_correction_T_max  0.9322
_exptl_absorpt_correction_T_min  0.8327
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         5253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0310P)²+2.0630P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                5055
_reflns_number_total             5253
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050693qsi20050620_094637.cif
_cod_data_source_block           Compound7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3664(1)
_cod_database_code               4309385
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
N1 N 0.71486(10) 0.17709(7) 0.80500(8) 0.0160(3) Uani 1 1 d . . .
S1 S 0.96687(3) 0.11996(2) 0.80666(2) 0.01879(11) Uani 1 1 d . . .
O1 O 0.96936(9) 0.05343(6) 0.62519(7) 0.0219(3) Uani 1 1 d . . .
Al1 Al 0.80758(3) 0.16062(2) 0.72853(3) 0.01504(12) Uani 1 1 d . . .
C1 C 0.66321(14) 0.24890(9) 0.92097(11) 0.0249(4) Uani 1 1 d . . .
H1A H 0.6054 0.2137 0.9152 0.037 Uiso 1 1 calc R . .
H1B H 0.6322 0.2967 0.9177 0.037 Uiso 1 1 calc R . .
H1C H 0.7157 0.2427 0.9776 0.037 Uiso 1 1 calc R . .
Si1 Si 1.01150(3) 0.03712(2) 0.73062(3) 0.01868(12) Uani 1 1 d . . .
S2 S 0.72911(3) 0.08918(2) 0.61883(3) 0.01993(11) Uani 1 1 d . . .
N2 N 0.81949(10) 0.25686(7) 0.69647(8) 0.0159(3) Uani 1 1 d . . .
Si2 Si 0.85160(3) 0.05950(2) 0.55414(3) 0.02020(12) Uani 1 1 d . . .
C2 C 0.71927(12) 0.23909(8) 0.84769(10) 0.0176(3) Uani 1 1 d . . .
C3 C 0.77339(12) 0.29853(9) 0.82714(11) 0.0184(3) Uani 1 1 d . . .
H3A H 0.7729(14) 0.3381(10) 0.8638(12) 0.022 Uiso 1 1 d . . .
C4 C 0.81073(12) 0.30957(8) 0.75198(10) 0.0171(3) Uani 1 1 d . . .
C5 C 0.83607(14) 0.38495(8) 0.73266(11) 0.0221(4) Uani 1 1 d . . .
H5A H 0.8164 0.3927 0.6691 0.033 Uiso 0.38(2) 1 calc PR A 1
H5B H 0.9136 0.3938 0.7557 0.033 Uiso 0.38(2) 1 calc PR A 1
H5C H 0.7947 0.4174 0.7606 0.033 Uiso 0.38(2) 1 calc PR A 1
H5D H 0.9024 0.3860 0.7118 0.033 Uiso 0.62(2) 1 d PR A 2
H5E H 0.8463 0.4135 0.7862 0.033 Uiso 0.62(2) 1 d PR A 2
H5F H 0.7760 0.4045 0.6874 0.033 Uiso 0.62(2) 1 d PR A 2
C6 C 0.84494(12) 0.27902(8) 0.61507(10) 0.0169(3) Uani 1 1 d . . .
C7 C 0.95249(13) 0.29530(8) 0.61472(10) 0.0183(3) Uani 1 1 d . . .
C8 C 0.97079(13) 0.32551(8) 0.53872(11) 0.0216(4) Uani 1 1 d . . .
H8A H 1.0424 0.3383 0.5374 0.026 Uiso 1 1 calc R . .
C9 C 0.88753(14) 0.33724(9) 0.46538(11) 0.0241(4) Uani 1 1 d . . .
H9A H 0.9018 0.3591 0.4150 0.029 Uiso 1 1 calc R . .
C10 C 0.78308(14) 0.31710(9) 0.46526(11) 0.0226(4) Uani 1 1 d . . .
H10A H 0.7266 0.3238 0.4138 0.027 Uiso 1 1 calc R . .
C11 C 0.75943(13) 0.28713(8) 0.53941(10) 0.0187(3) Uani 1 1 d . . .
C12 C 0.64419(12) 0.26497(8) 0.53757(11) 0.0196(4) Uani 1 1 d . . .
H12A H 0.6483 0.2313 0.5874 0.024 Uiso 1 1 calc R . .
C13 C 0.58959(14) 0.22551(9) 0.45302(11) 0.0258(4) Uani 1 1 d . . .
H13A H 0.6334 0.1842 0.4461 0.039 Uiso 1 1 calc R . .
H13B H 0.5831 0.2573 0.4027 0.039 Uiso 1 1 calc R . .
H13C H 0.5174 0.2098 0.4562 0.039 Uiso 1 1 calc R . .
C14 C 0.57534(14) 0.32811(9) 0.55240(12) 0.0261(4) Uani 1 1 d . . .
H14A H 0.6092 0.3507 0.6086 0.039 Uiso 1 1 calc R . .
H14B H 0.5027 0.3115 0.5533 0.039 Uiso 1 1 calc R . .
H14C H 0.5700 0.3625 0.5048 0.039 Uiso 1 1 calc R . .
C15 C 1.04835(13) 0.27812(9) 0.69148(11) 0.0214(4) Uani 1 1 d . . .
H15A H 1.0190 0.2592 0.7404 0.026 Uiso 1 1 calc R . .
C16 C 1.11683(14) 0.21965(9) 0.66430(12) 0.0275(4) Uani 1 1 d . . .
H16A H 1.0702 0.1796 0.6397 0.041 Uiso 1 1 calc R . .
H16B H 1.1722 0.2038 0.7158 0.041 Uiso 1 1 calc R . .
H16C H 1.1519 0.2382 0.6200 0.041 Uiso 1 1 calc R . .
C17 C 1.12111(14) 0.34156(9) 0.72707(11) 0.0261(4) Uani 1 1 d . . .
H17A H 1.0787 0.3778 0.7483 0.039 Uiso 1 1 calc R . .
H17B H 1.1504 0.3615 0.6802 0.039 Uiso 1 1 calc R . .
H17C H 1.1808 0.3259 0.7755 0.039 Uiso 1 1 calc R . .
C18 C 0.64101(12) 0.12270(8) 0.82146(10) 0.0177(3) Uani 1 1 d . . .
C19 C 0.67335(13) 0.07630(8) 0.89290(11) 0.0186(3) Uani 1 1 d . . .
C20 C 0.59902(13) 0.02513(8) 0.90545(12) 0.0242(4) Uani 1 1 d . . .
H20A H 0.6189 -0.0067 0.9535 0.029 Uiso 1 1 calc R . .
C21 C 0.49753(14) 0.02013(9) 0.84931(12) 0.0265(4) Uani 1 1 d . . .
H21A H 0.4484 -0.0151 0.8587 0.032 Uiso 1 1 calc R . .
C22 C 0.46704(13) 0.06630(9) 0.77934(12) 0.0256(4) Uani 1 1 d . . .
H22A H 0.3971 0.0621 0.7408 0.031 Uiso 1 1 calc R . .
C23 C 0.53712(13) 0.11902(9) 0.76425(11) 0.0215(4) Uani 1 1 d . . .
C24 C 0.49789(13) 0.17364(10) 0.69208(12) 0.0286(4) Uani 1 1 d . . .
H24A H 0.5632 0.1942 0.6767 0.034 Uiso 1 1 calc R . .
C25 C 0.42571(16) 0.14245(13) 0.60851(13) 0.0457(5) Uani 1 1 d . . .
H25A H 0.4623 0.1019 0.5894 0.069 Uiso 1 1 calc R . .
H25B H 0.4112 0.1786 0.5624 0.069 Uiso 1 1 calc R . .
H25C H 0.3572 0.1267 0.6200 0.069 Uiso 1 1 calc R . .
C26 C 0.43889(16) 0.23438(11) 0.72579(14) 0.0400(5) Uani 1 1 d . . .
H26A H 0.4103 0.2677 0.6778 0.060 Uiso 1 1 calc R . .
H26B H 0.4896 0.2592 0.7735 0.060 Uiso 1 1 calc R . .
H26C H 0.3791 0.2151 0.7476 0.060 Uiso 1 1 calc R . .
C27 C 0.78346(13) 0.07971(9) 0.95806(11) 0.0218(4) Uani 1 1 d . . .
H27A H 0.8269 0.1180 0.9389 0.026 Uiso 1 1 calc R . .
C28 C 0.77299(14) 0.09738(10) 1.05083(12) 0.0294(4) Uani 1 1 d . . .
H28A H 0.7379 0.1436 1.0504 0.044 Uiso 1 1 calc R . .
H28B H 0.8451 0.0989 1.0911 0.044 Uiso 1 1 calc R . .
H28C H 0.7293 0.0609 1.0702 0.044 Uiso 1 1 calc R . .
C29 C 0.84435(14) 0.00969(10) 0.96022(13) 0.0310(4) Uani 1 1 d . . .
H29A H 0.8543 -0.0006 0.9016 0.046 Uiso 1 1 calc R . .
H29B H 0.8026 -0.0286 0.9783 0.046 Uiso 1 1 calc R . .
H29C H 0.9152 0.0133 1.0021 0.046 Uiso 1 1 calc R . .
C30 C 0.95557(14) -0.04960(9) 0.75414(12) 0.0269(4) Uani 1 1 d . . .
H30A H 0.9797 -0.0869 0.7199 0.040 Uiso 1 1 calc R . .
H30B H 0.8763 -0.0474 0.7381 0.040 Uiso 1 1 calc R . .
H30C H 0.9812 -0.0603 0.8168 0.040 Uiso 1 1 calc R . .
C31 C 1.16187(13) 0.03368(9) 0.75689(12) 0.0263(4) Uani 1 1 d . . .
H31A H 1.1848 -0.0099 0.7327 0.039 Uiso 1 1 calc R . .
H31B H 1.1908 0.0343 0.8207 0.039 Uiso 1 1 calc R . .
H31C H 1.1892 0.0749 0.7311 0.039 Uiso 1 1 calc R . .
C32 C 0.81150(16) -0.02851(10) 0.50386(13) 0.0346(4) Uani 1 1 d . . .
H32A H 0.8655 -0.0446 0.4733 0.052 Uiso 1 1 calc R . .
H32B H 0.7408 -0.0248 0.4619 0.052 Uiso 1 1 calc R . .
H32C H 0.8071 -0.0627 0.5498 0.052 Uiso 1 1 calc R . .
C33 C 0.86936(15) 0.12240(10) 0.46824(11) 0.0294(4) Uani 1 1 d . . .
H33A H 0.9265 0.1051 0.4418 0.044 Uiso 1 1 calc R . .
H33B H 0.8896 0.1691 0.4946 0.044 Uiso 1 1 calc R . .
H33C H 0.8013 0.1263 0.4229 0.044 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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
C2 N1 C18 118.23(12) . . ?
C2 N1 Al1 120.06(10) . . ?
C18 N1 Al1 121.66(10) . . ?
Si1 S1 Al1 106.00(3) . . ?
Si2 O1 Si1 135.90(7) . . ?
N2 Al1 N1 96.56(6) . . ?
N2 Al1 S2 115.03(5) . . ?
N1 Al1 S2 110.96(5) . . ?
N2 Al1 S1 110.64(4) . . ?
N1 Al1 S1 109.25(5) . . ?
S2 Al1 S1 113.13(3) . . ?
O1 Si1 C30 108.68(7) . . ?
O1 Si1 C31 107.06(8) . . ?
C30 Si1 C31 110.51(8) . . ?
O1 Si1 S1 111.34(5) . . ?
C30 Si1 S1 111.43(6) . . ?
C31 Si1 S1 107.74(6) . . ?
Si2 S2 Al1 106.64(3) . . ?
C4 N2 C6 115.49(13) . . ?
C4 N2 Al1 120.57(10) . . ?
C6 N2 Al1 123.83(10) . . ?
O1 Si2 C33 106.59(7) . . ?
O1 Si2 C32 109.74(8) . . ?
C33 Si2 C32 109.42(9) . . ?
O1 Si2 S2 110.33(5) . . ?
C33 Si2 S2 114.47(6) . . ?
C32 Si2 S2 106.27(6) . . ?
N1 C2 C3 123.08(14) . . ?
N1 C2 C1 121.28(14) . . ?
C3 C2 C1 115.63(14) . . ?
C4 C3 C2 127.44(15) . . ?
N2 C4 C3 122.69(14) . . ?
N2 C4 C5 120.68(14) . . ?
C3 C4 C5 116.56(14) . . ?
C7 C6 C11 121.64(14) . . ?
C7 C6 N2 119.65(14) . . ?
C11 C6 N2 118.62(13) . . ?
C8 C7 C6 117.51(15) . . ?
C8 C7 C15 119.61(14) . . ?
C6 C7 C15 122.81(14) . . ?
C9 C8 C7 121.68(15) . . ?
C8 C9 C10 119.92(15) . . ?
C9 C10 C11 121.11(16) . . ?
C10 C11 C6 117.91(15) . . ?
C10 C11 C12 120.18(14) . . ?
C6 C11 C12 121.90(14) . . ?
C11 C12 C14 111.78(13) . . ?
C11 C12 C13 112.31(13) . . ?
C14 C12 C13 110.80(13) . . ?
C7 C15 C16 109.43(14) . . ?
C7 C15 C17 114.69(14) . . ?
C16 C15 C17 109.18(13) . . ?
C19 C18 C23 121.69(14) . . ?
C19 C18 N1 120.38(14) . . ?
C23 C18 N1 117.92(14) . . ?
C20 C19 C18 117.86(15) . . ?
C20 C19 C27 118.57(15) . . ?
C18 C19 C27 123.56(14) . . ?
C21 C20 C19 121.20(16) . . ?
C20 C21 C22 120.15(16) . . ?
C21 C22 C23 121.22(16) . . ?
C22 C23 C18 117.86(16) . . ?
C22 C23 C24 120.16(15) . . ?
C18 C23 C24 121.83(14) . . ?
C23 C24 C25 113.52(16) . . ?
C23 C24 C26 110.25(15) . . ?
C25 C24 C26 110.04(16) . . ?
C19 C27 C29 110.96(14) . . ?
C19 C27 C28 111.55(13) . . ?
C29 C27 C28 109.25(14) . . ?
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
N1 C2 1.342(2) . ?
N1 C18 1.458(2) . ?
N1 Al1 1.9084(14) . ?
S1 Si1 2.1283(7) . ?
S1 Al1 2.2338(9) . ?
O1 Si2 1.6394(13) . ?
O1 Si1 1.6408(12) . ?
Al1 N2 1.8998(14) . ?
Al1 S2 2.2225(8) . ?
C1 C2 1.510(2) . ?
Si1 C30 1.8574(17) . ?
Si1 C31 1.8599(17) . ?
S2 Si2 2.1380(8) . ?
N2 C4 1.346(2) . ?
N2 C6 1.457(2) . ?
Si2 C33 1.8530(18) . ?
Si2 C32 1.8551(18) . ?
C2 C3 1.395(2) . ?
C3 C4 1.394(2) . ?
C4 C5 1.505(2) . ?
C6 C7 1.407(2) . ?
C6 C11 1.410(2) . ?
C7 C8 1.395(2) . ?
C7 C15 1.526(2) . ?
C8 C9 1.379(2) . ?
C9 C10 1.384(2) . ?
C10 C11 1.394(2) . ?
C11 C12 1.521(2) . ?
C12 C14 1.531(2) . ?
C12 C13 1.533(2) . ?
C15 C16 1.531(2) . ?
C15 C17 1.533(2) . ?
C18 C19 1.403(2) . ?
C18 C23 1.407(2) . ?
C19 C20 1.400(2) . ?
C19 C27 1.522(2) . ?
C20 C21 1.378(3) . ?
C21 C22 1.382(3) . ?
C22 C23 1.396(2) . ?
C23 C24 1.523(2) . ?
C24 C25 1.524(3) . ?
C24 C26 1.535(3) . ?
C27 C29 1.528(2) . ?
C27 C28 1.534(2) . ?
