3,10-<i>C</i>-<i>meso</i>-2,5,5,7,9,12,12,14-Octamethyl-1,8-diaza-4,11-diazoniacyclotetradecane bis(thiocyanate)
Benson, Ronald E.; Roy, Tapashi G.; Hazari, Saroj K. S.; Barua, Kanak K.; Tiekink, Edward R. T.; Acta Crystallographica Section E 62 (2006) o1968–o1970; doi:10.1107/S1600536806013869

data_2208794
_publ_section_title
;3,10-<i>C</i>-<i>meso</i>-2,5,5,7,9,12,12,14-Octamethyl-1,8-diaza-4,11-diazoniacyclotetradecane
 bis(thiocyanate)
;
_journal_coeditor_code           BI2006
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1968
_journal_page_last               o1970
_journal_paper_doi               10.1107/S1600536806013869
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C18 H42 N4 2+ , 2N C S -'
_chemical_formula_moiety         'C18 H42 N4 2+ , 2N C S -'
_chemical_formula_sum            'C20 H42 N6 S2'
_chemical_formula_weight         430.72
_chemical_name_systematic
;
3,10-C-meso-2,5,5,7,9,12,12,14-Octamethyl-1,8-diaza-4,11-diazonia-
cyclotetradecane bis(thiocyanate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 107.74(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.804(4)
_cell_length_b                   14.490(5)
_cell_length_c                   11.057(6)
_cell_measurement_reflns_used    1066
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      3.0
_cell_volume                     1190.9(10)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and DIAMOND (Crystal Impact, 2006)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution
'PATTY in DIRDIF92 (Beurskens <i>et al.</i>,  1992)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_sigmaI/netI    0.029
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6518
_diffrn_reflns_theta_full        26.0
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         3.1
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.241
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.882
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Katayama, 1986; Paturle & Coppens, 1988)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         2330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.11
_refine_ls_R_factor_all          0.050
_refine_ls_R_factor_gt           0.043
_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^)+(0.0736P)^2^+0.6204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.125
_refine_ls_wR_factor_ref         0.131
_reflns_number_gt                1986
_reflns_number_total             2330
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2006.cif
_cod_data_source_block           I
_cod_original_cell_volume        1190.8(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2208794
_cod_database_fobs_code          2208794