Encapsulation of a discrete cyclic halide water tetramer [X2(H2O)2]2-, X = Cl-/Br- within a dimeric capsular assembly of a tripodal amide receptor
Arghya Basu; Gopal Das; Chem.Commun. 49 (2013) 3997–; doi:10.1039/c3cc40955d

data_7109166
_publ_section_title
;
 Encapsulation of a discrete cyclic halide water tetramer [X2(H2O)2]2-, X
 = Cl-/Br- within a dimeric capsular assembly of a tripodal amide receptor
;
_journal_name_full               Chem.Commun.
_journal_page_first              3997
_journal_paper_doi               10.1039/c3cc40955d
_journal_volume                  49
_journal_year                    2013
_chemical_formula_sum            'C45 H42 Br N7 O13'
_chemical_formula_weight         968.76
_chemical_name_systematic
;
?
;
_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           SHELXL-97
_cell_angle_alpha                68.839(8)
_cell_angle_beta                 74.960(9)
_cell_angle_gamma                83.360(8)
_cell_formula_units_Z            2
_cell_length_a                   9.4231(11)
_cell_length_b                   14.9240(12)
_cell_length_c                   17.6464(15)
_cell_measurement_reflns_used    4822
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      21.10
_cell_measurement_theta_min      1.84
_cell_volume                     2234.3(4)
_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_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0770
_diffrn_reflns_av_unetI/netI     0.1203
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18093
_diffrn_reflns_theta_full        28.77
_diffrn_reflns_theta_max         28.77
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.788
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000.0
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         9981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1618
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1303P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2079
_refine_ls_wR_factor_ref         0.2748
_reflns_number_gt                4794
_reflns_number_total             11412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40955d.txt
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7109166