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)
Vojtech Jancik; Herbert W. Roesky; Inorganic Chemistry 44 (2005) 5556–5558; doi:10.1021/ic050693q

data_4309383
_publ_contact_author_address
;Institut f\"ur Anorganische Chemie, 
Georg-August-Universit\"at G\"ottingen, 
Tammannstrasse 4, D 37077 G\"ottingen, 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            'C44 H71 Al N4 O S2'
_chemical_formula_weight         763.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   12.402(3)
_cell_length_b                   14.274(4)
_cell_length_c                   25.362(3)
_cell_measurement_reflns_used    7146
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.72
_cell_measurement_theta_min      3.49
_cell_volume                     4489.7(17)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0489
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20999
_diffrn_reflns_theta_full        58.91
_diffrn_reflns_theta_max         58.91
_diffrn_reflns_theta_min         3.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.529
_exptl_absorpt_correction_T_max  0.7497
_exptl_absorpt_correction_T_min  0.6570
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.163
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         6314
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0350
_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/[\s^2^(Fo^2^)+(0.0452P)^2^+0.1133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                5455
_reflns_number_total             6314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050693qsi20050620_094544.cif
_cod_data_source_block           Compound4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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        4490(2)
_cod_database_code               4309383