5,7,7,12,14,14-Hexamethyl-4,8-diaza-1,11-diazoniocyclotetradeca-4,11-diene diiodide dihydrate
Kennedy, Alan R.; Lutta, Samwel T.; Morrison, Catriona A.; Okoth, Maurice O.; Orang'o, Daniel M.; Acta Crystallographica Section E 67 (2011) o682–o683; doi:10.1107/S1600536811005848

data_2229488
_publ_section_title
;
 5,7,7,12,14,14-Hexamethyl-4,8-diaza-1,11-diazoniocyclotetradeca-4,11-diene
 diiodide dihydrate
;
_journal_coeditor_code           RK2263
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o682
_journal_page_last               o683
_journal_paper_doi               10.1107/S1600536811005848
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C16 H34 N4 2+, 2I -, 2H2 O'
_chemical_formula_moiety         'C16 H34 N4 2+, 2(I -), 2(H2 O)'
_chemical_formula_sum            'C16 H38 I2 N4 O2'
_chemical_formula_weight         572.30
_chemical_name_systematic
;
5,7,7,12,14,14-Hexamethyl-4,8-diaza-1,11-diazoniocyclotetradeca-4,11-diene
diiodide dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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           SHELXL97
_cell_angle_alpha                74.673(2)
_cell_angle_beta                 66.2670(10)
_cell_angle_gamma                75.809(2)
_cell_formula_units_Z            1
_cell_length_a                   8.4098(3)
_cell_length_b                   8.7252(2)
_cell_length_c                   8.7724(3)
_cell_measurement_reflns_used    10421
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     561.24(3)
_computing_cell_refinement
'<i>DENZO</i> (Otwinowski & Minor, 1997) and <i>COLLECT</i> (Hooft, 1988)'
_computing_data_collection       '<i>COLLECT</i> (Hooft, 1988)'
_computing_data_reduction
'<i>DENZO</i> (Otwinowski & Minor, 1997) and <i>COLLECT</i> (Hooft, 1988)'
_computing_molecular_graphics    '<i>ORTEP-3</i> (Farrugia, 1997)'
_computing_publication_material  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SIR2004</i> (Burla <i>et al.</i>, 2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker--Nonius Roper CCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker--Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0276
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12010
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.21
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.817
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Sheldrick, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.985
_refine_diff_density_min         -0.750
_refine_ls_extinction_coef       0.0243(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2563
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0194
_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^)+(0.0124P)^2^+0.33P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0464
_reflns_number_gt                2478
_reflns_number_total             2563
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2263.cif
_cod_data_source_block           I
_cod_database_code               2229488
_cod_database_fobs_code          2229488