3-Methyl-4,5,6,7,8,9-hexahydrocycloocta[<i>d</i>][1,2,3]selenadiazol]-3-ium iodide triiodide (3/2/1)
Schollmeyer, Dieter; Detert, Heiner; IUCrData 1 (2016) x161950–; doi:10.1107/S2414314616019507

data_1544768
_publ_section_title
;
 3-Methyl-4,5,6,7,8,9-hexahydrocycloocta[<i>d</i>][1,2,3]selenadiazol]-3-ium
 iodide triiodide (3/2/1)
;
_journal_issue                   12
_journal_name_full               IUCrData
_journal_page_first              x161950
_journal_paper_doi               10.1107/S2414314616019507
_journal_volume                  1
_journal_year                    2016
_chemical_formula_iupac          '3C9 H15 N2 Se +, I3 -, 2I -'
_chemical_formula_moiety         '3(C9 H15 N2 Se +), I3 -, 2(I -)'
_chemical_formula_sum            'C27 H45 I5 N6 Se3'
_chemical_formula_weight         1325.07
_chemical_melting_point          444
_chemical_name_systematic
;
3-Methyl-4,5,6,7,8,9-hexahydrocycloocta[d][1,2,3]selenadiazol]-3-ium iodide
triiodide (3/2/1)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2016/6
_cell_angle_alpha                81.913(2)
_cell_angle_beta                 86.409(2)
_cell_angle_gamma                78.801(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2438(4)
_cell_length_b                   13.9980(8)
_cell_length_c                   20.1035(11)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.4
_cell_volume                     1978.46(19)
_computing_cell_refinement
;
SAINT (Bruker (1997)
;
_computing_data_collection
;
SMART (Bruker (1997)
;
_computing_data_reduction
;
SAINT (Bruker (1997)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL2016 (Sheldrick, 2015) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Altomare <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2'
_diffrn_measurement_method       'CCD scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            64010
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.933
_diffrn_reflns_theta_min         1.024
_exptl_absorpt_coefficient_mu    6.716
_exptl_absorpt_correction_T_max  0.8099
_exptl_absorpt_correction_T_min  0.0951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 1997)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.224
_exptl_crystal_description       plate
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.740
_exptl_crystal_size_mid          0.338
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.412
_refine_diff_density_min         -2.665
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         9472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0374P)^2^+36.6012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                8038
_reflns_number_total             9472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su4106sup1.cif
_cod_data_source_block           I
_cod_database_code               1544768
_cod_database_fobs_code          1544768
_shelx_estimated_absorpt_t_min   0.083
_shelx_estimated_absorpt_t_max   0.730
_shelx_hkl_checksum              68804
_shelx_res_checksum              73710