3,6,9,16,19,22-Hexaazatricyclo[22.2.2.2^11,14^]triaconta-1(27),11(30),12,14(29),24(28),25-hexaene hexakis(<i>p</i>-toluenesulfonate) dihydrate
Saeed, Musabbir A.; Thompson, Jameskia J.; Fronczek, Frank R.; Hossain, Md. Alamgir; Acta Crystallographica Section E 65 (2009) o2405–o2406; doi:10.1107/S1600536809035648

data_2223332
_publ_section_title
;3,6,9,16,19,22-Hexaazatricyclo[22.2.2.2^11,14^]triaconta-1(27),11(30),12,14(29),24(28),25-hexaene
 hexakis(<i>p</i>-toluenesulfonate) dihydrate
;
_journal_coeditor_code           CI2898
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2405
_journal_page_last               o2406
_journal_paper_doi               10.1107/S1600536809035648
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C24 H44 N6 6+, 6C7 H7 O3 S -, 2H2 O'
_chemical_formula_moiety         'C24 H44 N6 6+, 6(C7 H7 O3 S -), 2(H2 O)'
_chemical_formula_sum            'C66 H90 N6 O20 S6'
_chemical_formula_weight         1479.80
_chemical_name_systematic
;
3,6,9,16,19,22-Hexaazatricyclo[22.2.2.2^11,14^]triaconta-
1(27),11(30),12,14(29),24(28),25-hexaene hexakis(<i>p</i>-toluenesulfonate)
dihydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.578(16)
_cell_angle_beta                 71.88(2)
_cell_angle_gamma                89.30(2)
_cell_formula_units_Z            1
_cell_length_a                   11.513(3)
_cell_length_b                   12.639(5)
_cell_length_c                   13.556(6)
_cell_measurement_reflns_used    6760
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      2.5
_cell_volume                     1835.0(12)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device
;
Nonius KappaCCD diffractometer with an Oxford Cryosystems Cryostream cooler
;
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.145
_diffrn_reflns_av_sigmaI/netI    0.232
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            27691
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         26.3
_diffrn_reflns_theta_min         2.7
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.39
_refine_diff_density_min         -0.33
_refine_ls_extinction_coef       0.0019(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         7213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.219
_refine_ls_R_factor_gt           0.072
_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^)+(0.0515P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.116
_refine_ls_wR_factor_ref         0.156
_reflns_number_gt                2920
_reflns_number_total             7213
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci2898.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2223332
_cod_database_fobs_code          2223332