Neutral Acyclic Anion Receptor with Thiadiazole Spacer: Halide Binding Study and Halide-Directed Self-Assembly in the Solid State
Arghya Basu; Gopal Das; Inorganic Chemistry 51 (2012) 882–889; doi:10.1021/ic201656y

data_4327972
_publ_section_title
;
 Neutral Acyclic Anion Receptor with Thiadiazole Spacer: Halide Binding
 Study and Halide-Directed Self-Assembly in the Solid State
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              882
_journal_page_last               889
_journal_paper_doi               10.1021/ic201656y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C46 H84 Br2 N8 O5 S'
_chemical_formula_weight         1021.08
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   31.372(7)
_cell_length_b                   8.1971(19)
_cell_length_c                   21.581(5)
_cell_measurement_reflns_used    3900
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.98
_cell_measurement_theta_min      3.99
_cell_volume                     5550(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 'phi and omega scans'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_sigmaI/netI    0.1016
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24379
_diffrn_reflns_theta_full        24.29
_diffrn_reflns_theta_max         24.29
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_description       block
_exptl_crystal_F_000             2168.0
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         7656
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.1097
_reflns_number_gt                4548
_reflns_number_total             4604
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201656y_si_002_2.cif
_cod_data_source_block           Br-complex
_cod_database_code               4327972