5,7,7,12,14,14-Hexamethyl-4,11-diaza-1,8-diazoniacyclotetradeca-4,11-diene bis(methanesulfonate)
Spendel, Katherine; Nazarenko, Alexander Y.; IUCrData 1 (2016) x161033–; doi:10.1107/S2414314616010336

data_1543575
_publ_section_title
;
 5,7,7,12,14,14-Hexamethyl-4,11-diaza-1,8-diazoniacyclotetradeca-4,11-diene
 bis(methanesulfonate)
;
_journal_coeditor_code           HB4059
_journal_issue                   6
_journal_name_full               IUCrData
_journal_page_first              x161033
_journal_paper_doi               10.1107/S2414314616010336
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          'C16 H34 N4 2+, 2C H3 O3 S -'
_chemical_formula_moiety         'C16 H34 N4 2+, 2(C H3 O3 S -)'
_chemical_formula_sum            'C18 H40 N4 O6 S2'
_chemical_formula_weight         472.66
_chemical_name_systematic
;
5,7,7,12,14,14-Hexamethyl-4,11-diaza-1,8-diazoniacyclotetradeca-4,11-diene
bis(methanesulfonate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.003(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7931(12)
_cell_length_b                   8.6816(11)
_cell_length_c                   14.1098(17)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      33.79
_cell_measurement_theta_min      3.14
_cell_volume                     1196.7(3)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62436
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         34.967
_diffrn_reflns_theta_min         2.894
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.9522
_exptl_absorpt_correction_T_min  0.8930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.585
_exptl_crystal_size_mid          0.418
_exptl_crystal_size_min          0.216
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.381
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         5245
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+0.2818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                3974
_reflns_number_total             5245
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb4059sup1.cif
_cod_data_source_block           I
_cod_database_code               1543575
_cod_database_fobs_code          1543575
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.946
_shelx_hkl_checksum              3362
_shelx_res_checksum              74104