Synthesis of Selenenium Ions: Isolation of Highly Conjugated, pH-Sensitive 4,4′-Bis(methylimino)-1,1′-binaphthylene-5-diselenenium(II) Triflate
Rakesh, Prakul; Singh, Harkesh B.; Butcher, Ray J.; Organometallics 32 (2013) 7275–; doi:10.1021/om400460z

data_4082069
_publ_section_title
;
 Synthesis of Selenenium Ions: Isolation of Highly Conjugated,
 pH-Sensitive
 4,4&#x2032;-Bis(methylimino)-1,1&#x2032;-binaphthylene-5-diselenenium(II)
 Triflate
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7275
_journal_paper_doi               10.1021/om400460z
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C13 H12 N2 Se'
_chemical_formula_sum            'C13 H12 N2 Se'
_chemical_formula_weight         275.21
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.1305(5)
_cell_length_b                   13.9195(8)
_cell_length_c                   19.2955(11)
_cell_measurement_reflns_used    2270
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      34.9650
_cell_measurement_theta_min      5.0307
_cell_volume                     2452.3(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics    'SHELXLTL (Sheldrick, 2008)'
_computing_publication_material  SHELXLTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_sigmaI/netI    0.1357
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14443
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         35.05
_diffrn_reflns_theta_min         5.04
_exptl_absorpt_coefficient_mu    3.036
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle plate'
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.663
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         5014
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.663
_refine_ls_R_factor_all          0.1808
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0207P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0460
_refine_ls_wR_factor_ref         0.0574
_reflns_number_gt                1490
_reflns_number_total             5014
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om400460z_si_002.cif
_cod_data_source_block           20
_cod_database_code               4082069