3-Methyl-4,5,6,7,8,9-hexahydrocycloocteno-1,2,3-selenadiazolium iodide‒trichloromethane (4/1)
Schollmeyer, Dieter; Detert, Heiner; IUCrData 2 (2017) x170167–; doi:10.1107/S2414314617001675

data_1545485
_publ_section_title
;
 3-Methyl-4,5,6,7,8,9-hexahydrocycloocteno-1,2,3-selenadiazolium
 iodide--trichloromethane (4/1)
;
_journal_issue                   2
_journal_name_full               IUCrData
_journal_page_first              x170167
_journal_paper_doi               10.1107/S2414314617001675
_journal_volume                  2
_journal_year                    2017
_chemical_formula_iupac          'C9 H15 N2 Se +, I -, 0.25(CH Cl3)'
_chemical_formula_moiety         'C9 H15 N2 Se +, I -, 0.25(C H Cl3)'
_chemical_formula_sum            'C9.25 H15.25 Cl0.75 I N2 Se'
_chemical_formula_weight         386.93
_chemical_name_systematic
'3-Methyl-4,5,6,7,8,9-hexahydrocycloocteno-1,2,3-selenadiazolium iodide--trichloromethane (4/1)'
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                71.141(8)
_cell_angle_beta                 89.472(9)
_cell_angle_gamma                76.460(6)
_cell_formula_units_Z            8
_cell_length_a                   10.5250(9)
_cell_length_b                   13.4368(9)
_cell_length_c                   20.112(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      38
_cell_measurement_theta_min      24
_cell_volume                     2610.0(4)
_computing_cell_refinement
;
CAD-4 Software (Enraf--Nonius, 1989)
;
_computing_data_collection
;
CAD-4 Software (Enraf--Nonius, 1989)
;
_computing_data_reduction
;
<i>CORINC</i> (Dr\"ager & Gattow, 1971)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR2004 (Burla <i>et al.</i>,  2005)
;
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            11193
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.991
_diffrn_reflns_theta_min         2.327
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    23.623
_exptl_absorpt_correction_T_max  0.202
_exptl_absorpt_correction_T_min  0.006
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(PLATON; Spek, 2009)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_description       plate
_exptl_crystal_F_000             1476
_exptl_crystal_size_max          0.556
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.118
_refine_diff_density_max         1.837
_refine_diff_density_min         -1.185
_refine_ls_extinction_coef       0.00067(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2014 (Sheldrick, 2008)
;
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         10589
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1024P)^2^+1.7825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1748
_refine_ls_wR_factor_ref         0.1967
_reflns_number_gt                7331
_reflns_number_total             10589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            bt4038sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;

2019-07-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C37 H61 Cl3 I4 N8 Se4'
_cod_original_formula_weight         1547.73
_cod_original_formula_moiety         '4(C9 H15 N2 Se +), 4(I -), CH Cl3'
_cod_original_formula_iupac          '4C9 H15 N2 Se +, 4I -, CH Cl3'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        2609.9(4)
_cod_database_code               1545485
_shelx_estimated_absorpt_t_min   0.027
_shelx_estimated_absorpt_t_max   0.167
_shelx_hkl_checksum              24017
_shelx_res_checksum              59133
_cod_database_fobs_code 1545485