data_global 
 
_audit_creation_method            SHELXL-97 
 
# PROCESSING SUMMARY ( IUCr Office Use Only) 
 
_journal_date_recd_electronic      2020-12-10
_journal_date_to_coeditor        ?
_journal_date_from_coeditor       ? 
_journal_date_accepted     2021-02-02
_journal_date_printers_first        ?
_journal_date_printers_final        ?
_journal_date_proofs_out        ?
_journal_date_proofs_in        ?
_journal_coeditor_name        ?
_journal_coeditor_code      XK5078SUP1
_journal_coeditor_notes
;

;
_journal_paper_category      FA
_journal_techeditor_code      B210125
_iucr_compatibility_tag          ACTA95
_journal_techeditor_notes
;

;
_journal_coden_ASTM        ?
_journal_name_full        ?
_journal_year        ?
_journal_volume        ?
_journal_issue        ?
_journal_page_first        ?
_journal_page_last        ?
_journal_suppl_publ_number        ?
_journal_suppl_publ_pages        ?
 
# SUBMISSION DETAILS 
 
_publ_contact_author_name         'Bartosz Zarychta' 
_publ_contact_author_address 
; Faculty of Chemistry 
  University of Opole 
  Oleska 48 
  45-052 Opole 
  Poland 
; 
 
_publ_contact_author_email         bzarychta@uni.opole.pl 
_publ_contact_letter 
; Please consider this CIF submission for publication in
 Acta Cryst. B
; 
_publ_requested_journal              
' ' 
_publ_requested_category             '' 
_publ_requested_coeditor             ? 
 
 
# TITLE AND AUTHOR LIST 
 
_publ_section_title 
;

;  
 
loop_ 
_publ_author_name 
_publ_author_address
 
 'Zarychta, Bartosz' 
; Institute of Chemistry 
  University of Opole 
  Oleska 48 
  45-052 Opole 
  Poland   
; 

 'Czapla, Zbigniew' 
; Department of  Physics 
  Opole University of Technology
  75 Ozimska 
  45-370 Opole 
  Poland 
; 

 'Przesławski, Janusz' 
; Institute of Experimental Physics 
  University of Wrocław
  M. Borna 9 
  50-204 Wrocław 
  Poland   
; 

 'Szkarz, Przemysła' 
; Faculty of Chemistry University of Wrocław
  14 F. Joliot - Curie
  50-383 Wrocław 
  Poland 
; 

############################################################################# 

 
data_I_non-standard_setting

 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C3 H17 Al N2 O14 S2' 
_chemical_formula_weight          396.29

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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            13
_space_group_name_H-M_alt         'P 2/a'
_space_group_name_Hall            '-P 2ya'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, y, -z'
 '-x, -y, -z'
 'x-1/2, -y, z'
 
_cell_length_a                    12.0026(10)
_cell_length_b                    6.7859(6)
_cell_length_c                    9.1005(11)
_cell_angle_alpha                 90
_cell_angle_beta                  88.835(9)
_cell_angle_gamma                 90
_cell_volume                      741.07(13)
_cell_formula_units_Z             2
_cell_measurement_temperature     290.0(1)
_cell_measurement_reflns_used     4395 
_cell_measurement_theta_min       3.002 
_cell_measurement_theta_max       25.998 
 
_exptl_crystal_description        'irregular' 
_exptl_crystal_colour             'colorless' 
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.776          
_exptl_crystal_F_000              412
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.125 
_exptl_absorpt_coefficient_mu     0.495
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       290.0(1)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator   'graphite'
_diffrn_measurement_device_type     'Oxford Diffraction Xcalibur System'
_diffrn_measurement_device        '4-circle kappa geometry goniometer'
_diffrn_measurement_method        'ω--scan' 
_diffrn_detector_area_resol_mean  10.4508
_diffrn_standards_number             0 
_diffrn_standards_interval_count     0 
_diffrn_standards_interval_time      0 
_diffrn_standards_decay_%            0
_diffrn_reflns_number             4395
_diffrn_reflns_av_unetI/netI      0.0539
_diffrn_reflns_av_R_equivalents   0.0622
_diffrn_reflns_limit_h_min        -14
_diffrn_reflns_limit_h_max        14
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          3.002
_diffrn_reflns_theta_max          25.998
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.979
_diffrn_measured_fraction_theta_full  0.979
_diffrn_reflns_Laue_measured_fraction_max    0.979
_diffrn_reflns_Laue_measured_fraction_full   0.979
_diffrn_reflns_point_group_measured_fraction_max   0.979
_diffrn_reflns_point_group_measured_fraction_full  0.979
_reflns_number_total              1431
_reflns_number_gt                 1082
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection     'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement     'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction     'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution  'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement   'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics        'Mercury (Macrae, 2020)' 
_computing_publication_material   ?
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0750P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          1431
_refine_ls_number_parameters      125
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0673
_refine_ls_R_factor_gt            0.0498
_refine_ls_wR_factor_ref          0.1214
_refine_ls_wR_factor_gt           0.1154
_refine_ls_goodness_of_fit_ref    0.972
_refine_ls_restrained_S_all       0.972
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Al1 Al 0.2500 0.26554(15) 0.0000 0.0198(3) Uani 1 2 d S T P . .
O1 O 0.31352(19) 0.4649(3) 0.1142(2) 0.0280(5) Uani 1 1 d . . . . .
H1A H 0.275(3) 0.568(6) 0.155(4) 0.050(11) Uiso 1 1 d . . . . .
H1B H 0.365(3) 0.460(6) 0.145(4) 0.049(13) Uiso 1 1 d . . . . .
O1A O 0.1197(2) 0.2657(3) 0.1153(3) 0.0289(6) Uani 1 1 d . . . . .
H1AA H 0.093(3) 0.348(5) 0.147(4) 0.032(11) Uiso 1 1 d . . . . .
H1AB H 0.091(3) 0.169(5) 0.139(4) 0.034(10) Uiso 1 1 d . . . . .
O1B O 0.18848(19) 0.0682(3) -0.1164(2) 0.0289(5) Uani 1 1 d . . . . .
H1BA H 0.130(3) 0.061(5) -0.139(4) 0.040(11) Uiso 1 1 d . . . . .
H1BB H 0.228(3) -0.044(6) -0.153(4) 0.053(11) Uiso 1 1 d . . . . .
S1 S 0.57521(6) 0.23069(9) 0.26261(8) 0.0227(3) Uani 1 1 d . . . . .
O2 O 0.52020(15) 0.4138(3) 0.2171(2) 0.0304(5) Uani 1 1 d . . . . .
O2A O 0.52129(16) 0.0634(3) 0.1882(2) 0.0365(6) Uani 1 1 d . . . . .
O2B O 0.69411(17) 0.2363(2) 0.2168(3) 0.0297(5) Uani 1 1 d . . . . .
O3 O 0.56481(19) 0.2052(3) 0.4211(3) 0.0390(6) Uani 1 1 d . . . . .
N1 N 0.6636(2) 0.7997(5) 0.5045(3) 0.0448(8) Uani 1 1 d . . . . .
H1 H 0.5957 0.8402 0.5078 0.054 Uiso 1 1 calc R U . . .
C2 C 0.7500 0.9107(7) 0.5000 0.0416(12) Uani 1 2 d S T P . .
H2 H 0.7500 1.0478 0.5000 0.050 Uiso 1 2 calc R U P . .
C2A C 0.6956(3) 0.6120(6) 0.5030(4) 0.0533(10) Uani 1 1 d . . . . .
H2A H 0.6494 0.5019 0.5058 0.064 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
Al1 O1A 1.866(2) 2 ?
Al1 O1A 1.866(2) . ?
Al1 O1B 1.869(2) . ?
Al1 O1B 1.869(2) 2 ?
Al1 O1 1.877(2) . ?
Al1 O1 1.877(2) 2 ?
O1 H1A 0.91(4) . ?
O1 H1B 0.69(4) . ?
O1A H1AA 0.70(3) . ?
O1A H1AB 0.77(3) . ?
O1B H1BA 0.74(4) . ?
O1B H1BB 0.95(4) . ?
S1 O3 1.455(2) . ?
S1 O2 1.4706(19) . ?
S1 O2A 1.478(2) . ?
S1 O2B 1.479(2) . ?
N1 C2 1.282(4) . ?
N1 C2A 1.331(5) . ?
N1 H1 0.8600 . ?
C2 N1 1.282(4) 2_656 ?
C2 H2 0.9300 . ?
C2A C2A 1.307(7) 2_656 ?
C2A H2A 0.9300 . ?
 
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
O1A Al1 O1A 179.92(14) 2 . ?
O1A Al1 O1B 91.03(10) 2 . ?
O1A Al1 O1B 89.03(10) . . ?
O1A Al1 O1B 89.03(10) 2 2 ?
O1A Al1 O1B 91.03(10) . 2 ?
O1B Al1 O1B 88.46(14) . 2 ?
O1A Al1 O1 88.03(10) 2 . ?
O1A Al1 O1 91.91(11) . . ?
O1B Al1 O1 178.99(9) . . ?
O1B Al1 O1 91.90(11) 2 . ?
O1A Al1 O1 91.91(11) 2 2 ?
O1A Al1 O1 88.02(10) . 2 ?
O1B Al1 O1 91.90(11) . 2 ?
O1B Al1 O1 178.99(9) 2 2 ?
O1 Al1 O1 87.77(15) . 2 ?
Al1 O1 H1A 125(2) . . ?
Al1 O1 H1B 125(3) . . ?
H1A O1 H1B 109(4) . . ?
Al1 O1A H1AA 127(3) . . ?
Al1 O1A H1AB 121(2) . . ?
H1AA O1A H1AB 111(4) . . ?
Al1 O1B H1BA 126(3) . . ?
Al1 O1B H1BB 125(2) . . ?
H1BA O1B H1BB 109(4) . . ?
O3 S1 O2 110.46(12) . . ?
O3 S1 O2A 109.45(13) . . ?
O2 S1 O2A 108.48(13) . . ?
O3 S1 O2B 110.19(14) . . ?
O2 S1 O2B 109.58(11) . . ?
O2A S1 O2B 108.64(12) . . ?
C2 N1 C2A 109.2(3) . . ?
C2 N1 H1 125.4 . . ?
C2A N1 H1 125.4 . . ?
N1 C2 N1 108.0(4) 2_656 . ?
N1 C2 H2 126.0 2_656 . ?
N1 C2 H2 126.0 . . ?
C2A C2A N1 106.77(19) 2_656 . ?
C2A C2A H2A 126.6 2_656 . ?
N1 C2A H2A 126.6 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C2A N1 C2 N1 0.09(17) . . . 2_656 ?
C2 N1 C2A C2A -0.2(5) . . . 2_656 ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
O1 H1A S1  0.91(4) 2.91(4) 3.757(2) 155(3) 4_565
O1 H1A O2B  0.91(4) 1.73(4) 2.643(3) 174(3) 4_565
O1 H1B O2  0.69(4) 2.01(4) 2.692(3) 172(4) .
O1A H1AA O2  0.70(3) 1.94(3) 2.640(3) 175(4) 4_565
O1A H1AB S1  0.77(3) 2.94(3) 3.661(2) 157(3) 4
O1A H1AB O2A  0.77(3) 1.84(3) 2.606(3) 178(4) 4
O1B H1BA S1  0.74(4) 2.96(4) 3.630(2) 152(4) 2
O1B H1BA O2A  0.74(4) 1.87(4) 2.614(3) 175(4) 2
O1B H1BB S1  0.95(4) 2.84(4) 3.711(2) 152(3) 3_655
O1B H1BB O2B  0.95(4) 1.70(4) 2.653(3) 177(3) 3_655
N1 H1 S1  0.86 2.94 3.536(3) 128.4 3_666
N1 H1 O3  0.86 2.04 2.811(4) 148.2 3_666
C2 H2 O3  0.93 2.58 3.084(4) 114.4 1_565
C2 H2 O3  0.93 2.58 3.084(4) 114.4 2_666
C2A H2A O3  0.93 2.39 3.269(4) 157.6 .
 
_refine_diff_density_max    0.521
_refine_diff_density_min   -0.479
_refine_diff_density_rms    0.097

_shelxl_version_number 2013-4




#############################################################################
 
data_II
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             
  'Imidazolium hexa-aqua-aluminium disulphate'
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C3 H17 Al N2 O14 S2'
_chemical_formula_sum
 'C3 H17 Al N2 O14 S2' 
_chemical_formula_weight          396.29

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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            164
_space_group_name_H-M_alt         'P -3 m 1'
_space_group_name_Hall            '-P 3 2"'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -z'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z'
 '-x+y, y, z'
 'x, x-y, z'
 
_cell_length_a                    6.8748(5)
_cell_length_b                    6.8748(5)
_cell_length_c                    9.1550(12)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      374.72(7)
_cell_formula_units_Z             1
_cell_measurement_temperature     345.0(1)
_cell_measurement_reflns_used     2491 
_cell_measurement_theta_min       3.422 
_cell_measurement_theta_max       5.935 
 
_exptl_crystal_description        'irregular' 
_exptl_crystal_colour             'colorless'
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.756          
_exptl_crystal_F_000              206
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.25 
_exptl_crystal_size_mid           0.20 
_exptl_crystal_size_min           0.125 
_exptl_absorpt_coefficient_mu     0.489
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       345.0(1)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator   'graphite'
_diffrn_measurement_device_type     'Oxford Diffraction Xcalibur System'
_diffrn_measurement_device        '4-circle kappa geometry goniometer'
_diffrn_measurement_method        'ω--scan' 
_diffrn_detector_area_resol_mean  10.4508
_diffrn_standards_number             0 
_diffrn_standards_interval_count     0 
_diffrn_standards_interval_time      0 
_diffrn_standards_decay_%            0
_diffrn_reflns_number             2491
_diffrn_reflns_av_unetI/netI      0.0151
_diffrn_reflns_av_R_equivalents   0.0335
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        8
_diffrn_reflns_limit_l_min        -8
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          3.422
_diffrn_reflns_theta_max          25.935
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.978
_diffrn_measured_fraction_theta_full  0.976
_diffrn_reflns_Laue_measured_fraction_max    0.978
_diffrn_reflns_Laue_measured_fraction_full   0.976
_diffrn_reflns_point_group_measured_fraction_max   0.978
_diffrn_reflns_point_group_measured_fraction_full  0.976
_reflns_number_total              311
_reflns_number_gt                 274
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection     'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement     'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction     'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution  'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics        'SHELXTL (Sheldrick, 2008)' 
_computing_publication_material   ?

 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0268P)²+0.3072P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          311
_refine_ls_number_parameters      32
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0396
_refine_ls_R_factor_gt            0.0339
_refine_ls_wR_factor_ref          0.0793
_refine_ls_wR_factor_gt           0.0779
_refine_ls_goodness_of_fit_ref    1.120
_refine_ls_restrained_S_all       1.120
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Al1 Al 1.0000 1.0000 1.0000 0.0312(5) Uani 1 12 d S T P . .
O1 O 0.86995(17) 0.7399(3) 0.8850(2) 0.0418(6) Uani 1 2 d S T P . .
H1A H 0.9349 0.6587 0.8545 0.050 Uiso 1 1 d R U . . .
S1 S 0.3333 0.6667 0.73910(15) 0.0374(4) Uani 1 6 d S T P . .
O2 O 0.44987(18) 0.55013(18) 0.7935(3) 0.0485(6) Uani 1 2 d S T P . .
O3 O 0.3333 0.6667 0.5807(5) 0.0757(15) Uani 1 6 d S T P . .
N1 N 0.085(3) 0.170(6) 0.506(3) 0.056(7) Uani 0.3333 2 d S T P . .
H1 H 0.1521 0.3042 0.5020 0.067 Uiso 0.3333 2 d R U P . .
C2 C 0.176(4) 0.176(4) 0.5000 0.056(7) Uani 0.5 2 d S T P . .
H2 H 0.3007 0.3007 0.5000 0.068 Uiso 0.5 2 d R U P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
Al1 O1 1.8728(19) . ?
Al1 O1 1.8728(19) 7_777 ?
Al1 O1 1.8728(19) 9_657 ?
Al1 O1 1.8728(19) 3_675 ?
Al1 O1 1.873(2) 2_765 ?
Al1 O1 1.8728(19) 8_567 ?
O1 H1A 0.9154 . ?
S1 O3 1.450(5) . ?
S1 O2 1.474(2) 2_665 ?
S1 O2 1.474(2) 3_565 ?
S1 O2 1.474(2) . ?
N1 C2 0.607(15) . ?
N1 C2 0.607(15) 9_556 ?
N1 N1 1.02(4) 8_556 ?
N1 N1 1.02(4) 9_556 ?
N1 C2 1.575(11) 8_556 ?
N1 C2 1.575(11) 2 ?
N1 N1 1.75(7) 3 ?
N1 N1 1.75(7) 2 ?
N1 H1 0.8023 . ?
N1 H2 1.2967 . ?
C2 N1 0.607(15) 8_556 ?
C2 C2 1.21(3) 9_556 ?
C2 C2 1.21(3) 8_556 ?
C2 N1 1.575(11) 9_556 ?
C2 N1 1.575(11) 3 ?
C2 H1 0.9749 . ?
C2 H2 0.8600 . ?
 
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
O1 Al1 O1 180.0 . 7_777 ?
O1 Al1 O1 88.53(9) . 9_657 ?
O1 Al1 O1 91.47(9) 7_777 9_657 ?
O1 Al1 O1 91.47(9) . 3_675 ?
O1 Al1 O1 88.53(9) 7_777 3_675 ?
O1 Al1 O1 180.0 9_657 3_675 ?
O1 Al1 O1 91.47(9) . 2_765 ?
O1 Al1 O1 88.53(9) 7_777 2_765 ?
O1 Al1 O1 88.53(9) 9_657 2_765 ?
O1 Al1 O1 91.47(9) 3_675 2_765 ?
O1 Al1 O1 88.53(9) . 8_567 ?
O1 Al1 O1 91.47(9) 7_777 8_567 ?
O1 Al1 O1 91.47(9) 9_657 8_567 ?
O1 Al1 O1 88.53(9) 3_675 8_567 ?
O1 Al1 O1 180.0 2_765 8_567 ?
Al1 O1 H1A 127.5 . . ?
O3 S1 O2 109.73(10) . 2_665 ?
O3 S1 O2 109.73(10) . 3_565 ?
O2 S1 O2 109.21(10) 2_665 3_565 ?
O3 S1 O2 109.73(10) . . ?
O2 S1 O2 109.21(11) 2_665 . ?
O2 S1 O2 109.21(10) 3_565 . ?
C2 N1 C2 167(5) . 9_556 ?
C2 N1 N1 33(5) . 8_556 ?
C2 N1 N1 151(6) 9_556 8_556 ?
C2 N1 N1 151(6) . 9_556 ?
C2 N1 N1 33(6) 9_556 9_556 ?
N1 N1 N1 118.8(11) 8_556 9_556 ?
C2 N1 C2 43(4) . 8_556 ?
C2 N1 C2 143(7) 9_556 8_556 ?
N1 N1 C2 10.8(19) 8_556 8_556 ?
N1 N1 C2 109.7(18) 9_556 8_556 ?
C2 N1 C2 143(7) . 2 ?
C2 N1 C2 43(4) 9_556 2 ?
N1 N1 C2 109.7(18) 8_556 2 ?
N1 N1 C2 10.8(19) 9_556 2 ?
C2 N1 C2 100(3) 8_556 2 ?
C2 N1 N1 64(5) . 3 ?
C2 N1 N1 123(5) 9_556 3 ?
N1 N1 N1 30.6(6) 8_556 3 ?
N1 N1 N1 89.999(5) 9_556 3 ?
C2 N1 N1 20.2(15) 8_556 3 ?
C2 N1 N1 80.1(16) 2 3 ?
C2 N1 N1 123(5) . 2 ?
C2 N1 N1 64(5) 9_556 2 ?
N1 N1 N1 89.999(18) 8_556 2 ?
N1 N1 N1 30.6(5) 9_556 2 ?
C2 N1 N1 80.1(16) 8_556 2 ?
C2 N1 N1 20.2(15) 2 2 ?
N1 N1 N1 60.000(6) 3 2 ?
C2 N1 H1 86.3 . . ?
C2 N1 H1 86.3 9_556 . ?
N1 N1 H1 119.4 8_556 . ?
N1 N1 H1 119.4 9_556 . ?
C2 N1 H1 129.7 8_556 . ?
C2 N1 H1 129.7 2 . ?
N1 N1 H1 149.9 3 . ?
N1 N1 H1 149.9 2 . ?
C2 N1 H2 33.7 . . ?
C2 N1 H2 138.8 9_556 . ?
N1 N1 H2 66.9 8_556 . ?
N1 N1 H2 168.6 9_556 . ?
C2 N1 H2 76.9 8_556 . ?
C2 N1 H2 174.6 2 . ?
N1 N1 H2 97.1 3 . ?
N1 N1 H2 156.9 2 . ?
H1 N1 H2 52.9 . . ?
N1 C2 N1 113(10) . 8_556 ?
N1 C2 C2 6(3) . 9_556 ?
N1 C2 C2 116(5) 8_556 9_556 ?
N1 C2 C2 116(5) . 8_556 ?
N1 C2 C2 6(3) 8_556 8_556 ?
C2 C2 C2 120.001(14) 9_556 8_556 ?
N1 C2 N1 18(4) . 9_556 ?
N1 C2 N1 96(7) 8_556 9_556 ?
C2 C2 N1 20.2(16) 9_556 9_556 ?
C2 C2 N1 99.9(16) 8_556 9_556 ?
N1 C2 N1 96(7) . 3 ?
N1 C2 N1 18(4) 8_556 3 ?
C2 C2 N1 99.9(16) 9_556 3 ?
C2 C2 N1 20.2(16) 8_556 3 ?
N1 C2 N1 80(3) 9_556 3 ?
N1 C2 H1 55.2 . . ?
N1 C2 H1 167.6 8_556 . ?
C2 C2 H1 51.7 9_556 . ?
C2 C2 H1 171.7 8_556 . ?
N1 C2 H1 71.9 9_556 . ?
N1 C2 H1 151.5 3 . ?
N1 C2 H2 123.3 . . ?
N1 C2 H2 123.3 8_556 . ?
C2 C2 H2 120.0 9_556 . ?
C2 C2 H2 120.0 8_556 . ?
N1 C2 H2 140.1 9_556 . ?
N1 C2 H2 140.1 3 . ?
H1 C2 H2 68.3 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C2 N1 C2 N1 -119(50) 9_556 . . 8_556 ?
N1 N1 C2 N1 -20(7) 9_556 . . 8_556 ?
C2 N1 C2 N1 6(3) 8_556 . . 8_556 ?
C2 N1 C2 N1 -7(3) 2 . . 8_556 ?
N1 N1 C2 N1 6(3) 3 . . 8_556 ?
N1 N1 C2 N1 0.001(2) 2 . . 8_556 ?
N1 N1 C2 C2 119(50) 8_556 . . 9_556 ?
N1 N1 C2 C2 99(52) 9_556 . . 9_556 ?
C2 N1 C2 C2 125(48) 8_556 . . 9_556 ?
C2 N1 C2 C2 112(51) 2 . . 9_556 ?
N1 N1 C2 C2 125(48) 3 . . 9_556 ?
N1 N1 C2 C2 119(50) 2 . . 9_556 ?
C2 N1 C2 C2 -125(48) 9_556 . . 8_556 ?
N1 N1 C2 C2 -6(3) 8_556 . . 8_556 ?
N1 N1 C2 C2 -26(10) 9_556 . . 8_556 ?
C2 N1 C2 C2 -13(5) 2 . . 8_556 ?
N1 N1 C2 C2 0.000(1) 3 . . 8_556 ?
N1 N1 C2 C2 -6(3) 2 . . 8_556 ?
C2 N1 C2 N1 -99(53) 9_556 . . 9_556 ?
N1 N1 C2 N1 20(7) 8_556 . . 9_556 ?
C2 N1 C2 N1 26(10) 8_556 . . 9_556 ?
C2 N1 C2 N1 13(4) 2 . . 9_556 ?
N1 N1 C2 N1 26(10) 3 . . 9_556 ?
N1 N1 C2 N1 20(7) 2 . . 9_556 ?
C2 N1 C2 N1 -125(48) 9_556 . . 3 ?
N1 N1 C2 N1 -6(3) 8_556 . . 3 ?
N1 N1 C2 N1 -26(10) 9_556 . . 3 ?
C2 N1 C2 N1 0.000(1) 8_556 . . 3 ?
C2 N1 C2 N1 -13(5) 2 . . 3 ?
N1 N1 C2 N1 -6(3) 2 . . 3 ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
O1 H1A S1  0.92 2.91 3.7134(9) 147.2 1_655
O1 H1A O2  0.92 1.74 2.6413(17) 170.0 3_665
N1 H1 S1  0.80 3.06 3.65(4) 132.1 .
N1 H1 O3  0.80 2.28 3.04(4) 158.8 .
C2 H1 S1  0.97 3.06 3.702(15) 124.5 .
C2 H1 O3  0.97 2.28 3.075(18) 138.6 .
N1 H2 O3  1.30 2.52 3.661(9) 145.0 7_666
C2 H1 O3  0.97 2.28 3.075(18) 138.6 .
C2 H2 O3  0.86 2.52 3.075(18) 122.9 7_666
 
_refine_diff_density_max    0.246
_refine_diff_density_min   -0.281
_refine_diff_density_rms    0.050

_shelxl_version_number 2013-4





############################################################################# 

 
data_III
 
_audit_creation_method            SHELXL-2013
_chemical_name_systematic
;
 ?
;
_chemical_name_common             
 'Imidazolium hexa-aqua-aluminium disulphate'
_chemical_melting_point           ?
_chemical_formula_moiety          
 'C3 H17 Al N2 O14 S2' 
_chemical_formula_sum
 'C3 H17 Al N2 O14 S2' 
_chemical_formula_weight          396.29

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'
 'S'  'S'   0.1246   0.1234
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       trigonal
_space_group_IT_number            164
_space_group_name_H-M_alt         'P -3 m 1'
_space_group_name_Hall            '-P 3 2"'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-y, x-y, z'
 '-x+y, -x, z'
 'y, x, -z'
 'x-y, -y, -z'
 '-x, -x+y, -z'
 '-x, -y, -z'
 'y, -x+y, -z'
 'x-y, x, -z'
 '-y, -x, z'
 '-x+y, y, z'
 'x, x-y, z'
 
_cell_length_a                    6.8680(4)
_cell_length_b                    6.8680(4)
_cell_length_c                    9.1617(10)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 120
_cell_volume                      374.25(6)
_cell_formula_units_Z             1
_cell_measurement_temperature     350.0(1)
_cell_measurement_reflns_used     2563 
_cell_measurement_theta_min       3.425 
_cell_measurement_theta_max       25.962 
 
_exptl_crystal_description        'irregular' 
_exptl_crystal_colour             'colorless' 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ?              
_exptl_crystal_density_diffrn     1.758          
_exptl_crystal_F_000              206
_exptl_transmission_factor_min    ?                                             
_exptl_transmission_factor_max    ?                                             
_exptl_crystal_size_max           0.4 
_exptl_crystal_size_mid           0.36 
_exptl_crystal_size_min           0.34 
_exptl_absorpt_coefficient_mu     0.490
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    none 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
_exptl_absorpt_process_details    ? 
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       350.0(1)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source 'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator   'graphite'
_diffrn_measurement_device_type     'Oxford Diffraction Xcalibur System'
_diffrn_measurement_device        '4-circle kappa geometry goniometer'
_diffrn_measurement_method        'ω--scan' 
_diffrn_detector_area_resol_mean  10.4508
_diffrn_standards_number             0 
_diffrn_standards_interval_count     0 
_diffrn_standards_interval_time      0 
_diffrn_standards_decay_%            0
_diffrn_reflns_number             2563
_diffrn_reflns_av_unetI/netI      0.0124
_diffrn_reflns_av_R_equivalents   0.0222
_diffrn_reflns_limit_h_min        -8
_diffrn_reflns_limit_h_max        8
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        8
_diffrn_reflns_limit_l_min        -7
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          3.425
_diffrn_reflns_theta_max          25.962
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.997
_diffrn_measured_fraction_theta_full  0.997
_diffrn_reflns_Laue_measured_fraction_max    0.997
_diffrn_reflns_Laue_measured_fraction_full   0.997
_diffrn_reflns_point_group_measured_fraction_max   0.997
_diffrn_reflns_point_group_measured_fraction_full  0.997
_reflns_number_total              317
_reflns_number_gt                 279
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection     'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement     'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction     'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution  'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement   'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics        'SHELXTL (Sheldrick, 2008)' 
 
_refine_special_details
;
 ?
;
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0346P)²+0.2265P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          317
_refine_ls_number_parameters      32
_refine_ls_number_restraints      7
_refine_ls_R_factor_all           0.0365
_refine_ls_R_factor_gt            0.0300
_refine_ls_wR_factor_ref          0.0800
_refine_ls_wR_factor_gt           0.0777
_refine_ls_goodness_of_fit_ref    1.114
_refine_ls_restrained_S_all       1.101
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Al1 Al 1.0000 1.0000 1.0000 0.0299(5) Uani 1 12 d S T P . .
O1 O 0.86970(15) 0.7394(3) 0.88502(18) 0.0404(5) Uani 1 2 d S T P . .
H1A H 0.9346 0.6587 0.8545 0.048 Uiso 1 1 d R U . . .
S1 S 0.3333 0.6667 0.73902(13) 0.0352(3) Uani 1 6 d S T P . .
O2 O 0.44965(15) 0.55035(15) 0.7932(2) 0.0470(5) Uani 1 2 d S T P . .
O3 O 0.3333 0.6667 0.5813(4) 0.0726(13) Uani 1 6 d S T P . .
N1 N 0.171(6) 0.085(3) 0.493(2) 0.052(5) Uani 0.3333 2 d S TU P . .
H1 H 0.3289 0.1644 0.5055 0.062 Uiso 0.3333 2 d R U P . .
C2 C 0.176(3) 0.176(3) 0.5000 0.054(6) Uani 0.5 2 d S TU P . .
H2 H 0.3006 0.2801 0.5000 0.065 Uiso 0.25 1 d R U P . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
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
Al1 O1 1.8741(17) . ?
Al1 O1 1.8741(17) 7_777 ?
Al1 O1 1.8741(17) 9_657 ?
Al1 O1 1.8741(17) 3_675 ?
Al1 O1 1.8741(17) 2_765 ?
Al1 O1 1.8741(17) 8_567 ?
O1 H1A 0.9117 . ?
S1 O3 1.445(4) . ?
S1 O2 1.4702(19) 2_665 ?
S1 O2 1.4702(19) 3_565 ?
S1 O2 1.4702(19) . ?
N1 C2 0.607(12) . ?
N1 C2 0.607(12) 8_556 ?
N1 N1 1.02(4) 9_556 ?
N1 N1 1.02(4) 8_556 ?
N1 C2 1.577(10) 9_556 ?
N1 C2 1.577(10) 3 ?
N1 N1 1.76(6) 3 ?
N1 N1 1.76(6) 2 ?
N1 H1 0.9480 . ?
N1 H2 1.1819 . ?
C2 N1 0.607(12) 9_556 ?
C2 C2 1.21(2) 9_556 ?
C2 C2 1.21(2) 8_556 ?
C2 N1 1.577(11) 2 ?
C2 N1 1.577(11) 8_556 ?
C2 H1 1.0944 . ?
C2 H2 0.7982 . ?
 
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
O1 Al1 O1 180.0 . 7_777 ?
O1 Al1 O1 88.51(7) . 9_657 ?
O1 Al1 O1 91.49(7) 7_777 9_657 ?
O1 Al1 O1 91.49(7) . 3_675 ?
O1 Al1 O1 88.51(7) 7_777 3_675 ?
O1 Al1 O1 180.0 9_657 3_675 ?
O1 Al1 O1 91.49(7) . 2_765 ?
O1 Al1 O1 88.51(7) 7_777 2_765 ?
O1 Al1 O1 88.51(8) 9_657 2_765 ?
O1 Al1 O1 91.49(7) 3_675 2_765 ?
O1 Al1 O1 88.51(7) . 8_567 ?
O1 Al1 O1 91.49(7) 7_777 8_567 ?
O1 Al1 O1 91.49(7) 9_657 8_567 ?
O1 Al1 O1 88.51(8) 3_675 8_567 ?
O1 Al1 O1 180.0 2_765 8_567 ?
Al1 O1 H1A 127.4 . . ?
O3 S1 O2 109.75(9) . 2_665 ?
O3 S1 O2 109.75(9) . 3_565 ?
O2 S1 O2 109.19(9) 2_665 3_565 ?
O3 S1 O2 109.75(9) . . ?
O2 S1 O2 109.19(9) 2_665 . ?
O2 S1 O2 109.19(9) 3_565 . ?
C2 N1 C2 167(4) . 8_556 ?
C2 N1 N1 33(5) . 9_556 ?
C2 N1 N1 150(5) 8_556 9_556 ?
C2 N1 N1 150(5) . 8_556 ?
C2 N1 N1 33(5) 8_556 8_556 ?
N1 N1 N1 118.5(10) 9_556 8_556 ?
C2 N1 C2 43(3) . 9_556 ?
C2 N1 C2 142(6) 8_556 9_556 ?
N1 N1 C2 11.2(16) 9_556 9_556 ?
N1 N1 C2 109.4(16) 8_556 9_556 ?
C2 N1 C2 142(6) . 3 ?
C2 N1 C2 43(3) 8_556 3 ?
N1 N1 C2 109.4(16) 9_556 3 ?
N1 N1 C2 11.2(16) 8_556 3 ?
C2 N1 C2 100(3) 9_556 3 ?
C2 N1 N1 123(5) . 3 ?
C2 N1 N1 63(5) 8_556 3 ?
N1 N1 N1 90.00(2) 9_556 3 ?
N1 N1 N1 30.8(5) 8_556 3 ?
C2 N1 N1 79.9(14) 9_556 3 ?
C2 N1 N1 20.0(14) 3 3 ?
C2 N1 N1 63(5) . 2 ?
C2 N1 N1 123(5) 8_556 2 ?
N1 N1 N1 30.8(5) 9_556 2 ?
N1 N1 N1 90.002(8) 8_556 2 ?
C2 N1 N1 20.0(14) 9_556 2 ?
C2 N1 N1 79.9(14) 3 2 ?
N1 N1 N1 59.999(4) 3 2 ?
C2 N1 H1 86.6 . . ?
C2 N1 H1 86.6 8_556 . ?
N1 N1 H1 118.5 9_556 . ?
N1 N1 H1 118.5 8_556 . ?
C2 N1 H1 129.3 9_556 . ?
C2 N1 H1 129.3 3 . ?
N1 N1 H1 149.3 3 . ?
N1 N1 H1 149.3 2 . ?
C2 N1 H2 38.2 . . ?
C2 N1 H2 135.4 8_556 . ?
N1 N1 H2 70.7 9_556 . ?
N1 N1 H2 165.0 8_556 . ?
C2 N1 H2 80.9 9_556 . ?
C2 N1 H2 174.5 3 . ?
N1 N1 H2 160.7 3 . ?
N1 N1 H2 100.9 2 . ?
H1 N1 H2 49.0 . . ?
N1 C2 N1 115(10) 9_556 . ?
N1 C2 C2 7(2) 9_556 9_556 ?
N1 C2 C2 117(5) . 9_556 ?
N1 C2 C2 117(5) 9_556 8_556 ?
N1 C2 C2 7(2) . 8_556 ?
C2 C2 C2 120.000(11) 9_556 8_556 ?
N1 C2 N1 19(4) 9_556 2 ?
N1 C2 N1 97(6) . 2 ?
C2 C2 N1 20.0(14) 9_556 2 ?
C2 C2 N1 100.1(14) 8_556 2 ?
N1 C2 N1 97(6) 9_556 8_556 ?
N1 C2 N1 19(4) . 8_556 ?
C2 C2 N1 100.1(14) 9_556 8_556 ?
C2 C2 N1 20.0(14) 8_556 8_556 ?
N1 C2 N1 80(3) 2 8_556 ?
N1 C2 H1 169.3 9_556 . ?
N1 C2 H1 59.8 . . ?
C2 C2 H1 175.6 9_556 . ?
C2 C2 H1 56.6 8_556 . ?
N1 C2 H1 156.7 2 . ?
N1 C2 H1 76.4 8_556 . ?
N1 C2 H2 131.2 9_556 . ?
N1 C2 H2 113.8 . . ?
C2 C2 H2 128.8 9_556 . ?
C2 C2 H2 111.2 8_556 . ?
N1 C2 H2 148.6 2 . ?
N1 C2 H2 131.1 8_556 . ?
H1 C2 H2 54.7 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C2 N1 C2 N1 -111(43) 8_556 . . 9_556 ?
N1 N1 C2 N1 -22(6) 8_556 . . 9_556 ?
C2 N1 C2 N1 7(2) 9_556 . . 9_556 ?
C2 N1 C2 N1 -8(2) 3 . . 9_556 ?
N1 N1 C2 N1 -0.001(2) 3 . . 9_556 ?
N1 N1 C2 N1 7(2) 2 . . 9_556 ?
C2 N1 C2 C2 -118(42) 8_556 . . 9_556 ?
N1 N1 C2 C2 -7(2) 9_556 . . 9_556 ?
N1 N1 C2 C2 -29(8) 8_556 . . 9_556 ?
C2 N1 C2 C2 -15(5) 3 . . 9_556 ?
N1 N1 C2 C2 -7(2) 3 . . 9_556 ?
N1 N1 C2 C2 0.000(2) 2 . . 9_556 ?
N1 N1 C2 C2 111(43) 9_556 . . 8_556 ?
N1 N1 C2 C2 89(44) 8_556 . . 8_556 ?
C2 N1 C2 C2 118(41) 9_556 . . 8_556 ?
C2 N1 C2 C2 103(43) 3 . . 8_556 ?
N1 N1 C2 C2 111(43) 3 . . 8_556 ?
N1 N1 C2 C2 118(41) 2 . . 8_556 ?
C2 N1 C2 N1 -118(42) 8_556 . . 2 ?
N1 N1 C2 N1 -7(2) 9_556 . . 2 ?
N1 N1 C2 N1 -29(8) 8_556 . . 2 ?
C2 N1 C2 N1 0.000(1) 9_556 . . 2 ?
C2 N1 C2 N1 -15(5) 3 . . 2 ?
N1 N1 C2 N1 -7(2) 3 . . 2 ?
C2 N1 C2 N1 -89(44) 8_556 . . 8_556 ?
N1 N1 C2 N1 22(6) 9_556 . . 8_556 ?
C2 N1 C2 N1 29(8) 9_556 . . 8_556 ?
C2 N1 C2 N1 14(3) 3 . . 8_556 ?
N1 N1 C2 N1 22(6) 3 . . 8_556 ?
N1 N1 C2 N1 29(8) 2 . . 8_556 ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
O1 H1A S1  0.91 2.91 3.7106(8) 147.3 1_655
O1 H1A O2  0.91 1.74 2.6400(15) 170.0 3_665
N1 H1 S1  0.95 3.01 3.64(4) 125.0 7_666
N1 H1 O3  0.95 2.16 3.03(4) 151.5 7_666
C2 H2 S1  0.80 3.21 3.700(13) 122.1 7_666
C2 H2 O3  0.80 2.47 3.074(15) 133.8 7_666
N1 H2 O3  1.18 2.66 3.658(8) 141.7 .
C2 H2 O3  0.80 2.66 3.074(15) 114.5 .
C2 H2 O3  0.80 2.47 3.074(15) 133.8 7_666
 
_refine_diff_density_max    0.316
_refine_diff_density_min   -0.290
_refine_diff_density_rms    0.048

_shelxl_version_number 2013-4







