The binary adduct of 3,6,9,16,19,22-hexaazatricyclo[22.2.2.2^11,14^]triaconta-11,13,24,26(1),27,29-hexaene and benzene-1,2,4,5-tetracarboxylic acid
Zhu, Long-Gen; Ellern, Arkady M.; Kostić, Nenad M.; Acta Crystallographica Section C 58 (2002) o129–o130; doi:10.1107/S0108270101020777

data_2012603
_publ_section_title
;The binary adduct of
 3,6,9,16,19,22-hexaazatricyclo[22.2.2.2^11,14^]triaconta-11,13,24,26(1),27,29-hexaene
 and benzene-1,2,4,5-tetracarboxylic acid
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o129
_journal_page_last               o130
_journal_paper_doi               10.1107/S0108270101020777
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C24 H42 N6 4+ , C10 H2 O8 4- , 6H2 O'
_chemical_formula_sum            'C34 H56 N6 O14'
_chemical_formula_weight         772.85
_chemical_name_systematic
;
6,21-diaza-3,9,18,24-tetraazoniatricyclo[22.2.2.2^11,14^]triaconta-
11,13,24,26(1),27,29-hexaene benzene-1,2,4,5-tetracarboxylate hexahydrate
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                87.686(3)
_cell_angle_beta                 79.635(3)
_cell_angle_gamma                79.498(3)
_cell_formula_units_Z            1
_cell_length_a                   7.0983(11)
_cell_length_b                   9.3947(15)
_cell_length_c                   13.880(2)
_cell_measurement_reflns_used    3621
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21
_cell_measurement_theta_min      7
_cell_volume                     895.2(2)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full .987
_diffrn_measured_fraction_theta_max .987
_diffrn_measurement_device_type  'Bruker SMART Query CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .034
_diffrn_reflns_av_sigmaI/netI    .107
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4531
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 1085
_diffrn_standards_number         50
_exptl_absorpt_coefficient_mu    .112
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             414
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .1
_refine_diff_density_max         .22
_refine_diff_density_min         -.22
_refine_ls_extinction_coef       .010(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   .899
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         3011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .899
_refine_ls_R_factor_all          .099
_refine_ls_R_factor_gt           .047
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.039P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .093
_refine_ls_wR_factor_ref         .104
_reflns_number_gt                1669
_reflns_number_total             3011
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1508.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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2012603
_cod_database_fobs_code          2012603