Polysulfonylamines. CX. Hydroxylammonium di(methanesulfonyl)amidate 1,4,7,10,13,16-hexaoxacyclooctadecane (1/1/1) and 2-aminopyridinium di(methanesulfonyl)amidate 1,4,7,10,13,16-hexaoxacyclooctadecane (1/1/1)
Henschel, Dagmar; Wijaya, Karna; Jones, Peter G.; Blaschette, Armand; Acta Crystallographica Section C 55 (1999) 664–668; doi:10.1107/S0108270199001274

data_2008326
_publ_section_title
;
 Polysulfonylamines. CX. Hydroxylammonium di(methanesulfonyl)amidate
 1,4,7,10,13,16-hexaoxacyclooctadecane (1/1/1) and 2-aminopyridinium
 di(methanesulfonyl)amidate 1,4,7,10,13,16-hexaoxacyclooctadecane
 (1/1/1)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              664
_journal_page_last               668
_journal_paper_doi               10.1107/S0108270199001274
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C5 H7 N2 +, C2 H6 N O4 S2 -, C12 H24 O6'
_chemical_formula_sum            'C19 H37 N3 O10 S2'
_chemical_formula_weight         531.64
_chemical_name_systematic
;
 2-Aminopyridinium Di(methanesulfonyl)amidate
 1,4,7,1O,13,16-Hexaoxacyclooctadecane (1/1/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.74(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.670(3)
_cell_length_b                   15.623(5)
_cell_length_c                   14.528(4)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      10
_cell_volume                     2508.3(13)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992b)'
_computing_molecular_graphics    'XP (Siemens, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe Stadi-4'
_diffrn_measurement_method       \w/\q
_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  0.022
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4790
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.269
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.33
_refine_diff_density_min         -0.40
_refine_ls_extinction_coef       0.0115(6)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4431
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.049
_refine_ls_R_factor_gt           0.038
_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^)+(0.0392P)^2^+1.2421P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.094
_reflns_number_gt                3668
_reflns_number_total             4431
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bm1316.cif
_cod_data_source_block           IV
_cod_original_cell_volume        2508.2(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2008326