1,4,10,13-Tetraoxa-7,16-diazoniacyclooctadecane bis(1<i>H</i>-pyrrole-2-carboxylate)
Zeng, Fanglei; Yin, Zhenming; Acta Crystallographica Section E 69 (2013) o1108–; doi:10.1107/S1600536813016176

data_2238150
_publ_section_title
;
 1,4,10,13-Tetraoxa-7,16-diazoniacyclooctadecane
 bis(1<i>H</i>-pyrrole-2-carboxylate)
;
_journal_coeditor_code           FF2108
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1108
_journal_paper_doi               10.1107/S1600536813016176
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C12 H28 N2 O4 2+, 2C5 H4 N O2 -'
_chemical_formula_moiety         'C12 H28 N2 O4 2+, 2(C5 H4 N O2 -)'
_chemical_formula_sum            'C22 H36 N4 O8'
_chemical_formula_weight         484.55
_chemical_name_systematic
;
1,4,10,13-Tetraoxa-7,16-diazoniacyclooctadecane
bis(1<i>H</i>-pyrrole-2-carboxylate)
;
_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                73.028(4)
_cell_angle_beta                 76.547(4)
_cell_angle_gamma                77.824(4)
_cell_formula_units_Z            1
_cell_length_a                   7.8963(19)
_cell_length_b                   9.164(2)
_cell_length_c                   9.244(2)
_cell_measurement_reflns_used    1288
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.61
_cell_measurement_theta_min      2.68
_cell_volume                     614.8(2)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3484
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.140
_refine_diff_density_min         -0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0587P)^2^+0.0353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1129
_reflns_number_gt                1695
_reflns_number_total             2471
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ff2108.cif
_cod_data_source_block           I
_cod_original_cell_volume        614.8(3)
_cod_database_code               2238150
_cod_database_fobs_code          2238150