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_4319168
_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         'C66 H96 Al2 N8 Na2 O18 S4, 3(C4H8O)'
_chemical_formula_sum            'C88 H120 Al2 N8 Na2 O21 S4'
_chemical_formula_weight         1854.10
_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
_cell_angle_alpha                110.3505(16)
_cell_angle_beta                 111.538(2)
_cell_angle_gamma                97.3496(17)
_cell_formula_units_Z            1
_cell_length_a                   12.7237(11)
_cell_length_b                   14.0108(13)
_cell_length_c                   16.2050(14)
_cell_measurement_reflns_used    4944
_cell_measurement_temperature    193(2)
_cell_volume                     2408.8(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ORTEP-3 (1.05) in WinGX-1.62'
_computing_publication_material  WinGX-1.62
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10008
_diffrn_reflns_theta_full        21.97
_diffrn_reflns_theta_max         21.97
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.9561
_exptl_absorpt_correction_T_min  0.9149
_exptl_absorpt_correction_type   'Gaussian integration'
_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    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         5857
_refine_ls_number_restraints     751
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0868P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1482
_reflns_number_gt                3949
_reflns_number_total             5857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0006549_1.cif
_cod_data_source_block           3
_cod_database_code               4319168