Tetraaza Analogues of Lithium and Sodium Alums: Synthesis and X-ray Structures of the Single Strand Polymer [Li(THF)2{Al[SO2(NtBu)2]2}]∞and the Contact Ion Pairs [Na(15-crown-5)][Al{SO2(NtBu)2}2] and {[Na(15-crown-5)][O2S(μ-NBn)2Al(μ-NBnSO2NBn)]}2
Pierre Blais; Justin K. Brask; Tristram Chivers; Gabriele Schatte; Inorganic Chemistry 40 (2001) 384–388; doi:10.1021/ic0006549

data_4319170
_publ_contact_author_address
; Department of Chemistry
  University of Calgary
  Calgary Alberta T2N 1N4
  Canada
;
_publ_contact_author_email       chivers@ucalgary.ca
_publ_contact_author_fax         '001 403 289 9488'
_publ_contact_author_name        'Dr Tristram Chivers'
_publ_contact_author_phone       '001 403 220 5741'
_publ_section_title
;
 Tetraaza Analogues of Lithium and Sodium Alums: Synthesis and X-ray
 Structures of the Single Strand Polymer
 [Li(THF)2{Al[SO2(NtBu)2]2}]\\infty and the Contact Ion Pairs
 [Na(15-crown-5)][Al{SO2(NtBu)2}2] and
 {[Na(15-crown-5)][O2S(\m-NBn)2Al(\m-NBnSO2NBn)]}2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              384
_journal_page_last               388
_journal_paper_doi               10.1021/ic0006549
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         'C24 H52 Al Li N4 O6 S2'
_chemical_formula_sum            'C24 H52 Al Li N4 O6 S2'
_chemical_formula_weight         590.74
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.159(5)
_cell_length_b                   10.354(3)
_cell_length_c                   15.833(4)
_cell_measurement_reflns_used    2614
_cell_measurement_temperature    193(2)
_cell_volume                     3304.8(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP-3 (1.06) in WinGX-1.63'
_computing_publication_material  WinGX-1.63
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.912
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10379
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.227
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.9066
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;SADABS, V 2.01, Software for Area-Detector Absorption
  Corrections; Bruker AXS Inc., Madison, WI, 2000.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.09(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         4791
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0540
_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/[\s^2^(Fo^2^)+(0.0937P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1493
_reflns_number_gt                3641
_reflns_number_total             4791
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0006549_3.cif
_cod_data_source_block           1
_cod_original_cell_volume        3304.7(15)
_cod_database_code               4319170