Ammonium 2,5,8,11,21,24,27-octaoxatricyclo[26.4.0.0^12,17^]dotriaconta-1(32),12(17),13,15,28,30-hexaene hexafluorophosphate
Fallon, Gary D.; Lau, Vei-Lin; Langford, Steven J.; Acta Crystallographica Section E 58 (2002) o321–o323; doi:10.1107/S1600536802003100

data_2200996
_publ_section_title
;Ammonium
 2,5,8,11,21,24,27-octaoxatricyclo[26.4.0.0^12,17^]dotriaconta-1(32),12(17),13,15,28,30-hexaene
 hexafluorophosphate
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o321
_journal_page_last               o323
_journal_paper_doi               10.1107/S1600536802003100
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'N1 H4 1+, C24 H32 O8, P1 F6 1-'
_chemical_formula_moiety         'N1 H4 1+, C24 H32 O8, P1 F6 1-'
_chemical_formula_sum            'C24 H36 F6 N O8 P'
_chemical_formula_weight         611.51
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                69.3710(10)
_cell_angle_beta                 71.5360(10)
_cell_angle_gamma                89.6700(10)
_cell_formula_units_Z            2
_cell_length_a                   10.1950(2)
_cell_length_b                   10.6379(2)
_cell_length_c                   14.5447(3)
_cell_measurement_reflns_used    16366
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      .4
_cell_volume                     1390.30(5)
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2000)'
_computing_data_reduction
'HKL DENZO and SCALEPACK (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full .992
_diffrn_measured_fraction_theta_max .97
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method
'CCD rotation images, thick slices [scan type available ?]'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0437
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16366
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    .187
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             640
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .08
_refine_diff_density_max         .635
_refine_diff_density_min         -.551
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .974
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .974
_refine_ls_R_factor_gt           .0508
_refine_ls_shift/su_max          .009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0619P)^2^] where  P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1325
_reflns_number_gt                3813
_reflns_number_total             6721
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ww6007.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C24 H36 F6 N1 O8 P1'
_cod_database_code               2200996
_cod_database_fobs_code          2200996