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_7109165
_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 Cl N7 O13'
_chemical_formula_weight         924.31
_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                69.237(3)
_cell_angle_beta                 75.363(3)
_cell_angle_gamma                83.377(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3971(5)
_cell_length_b                   14.8204(7)
_cell_length_c                   17.5829(9)
_cell_measurement_reflns_used    5824
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.10
_cell_measurement_theta_min      2.54
_cell_volume                     2214.5(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_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27999
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.861
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         9512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.1339
_refine_ls_R_factor_gt           0.0568
_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^)+(0.1000P)^2^+0.9550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1856
_reflns_number_gt                4793
_reflns_number_total             10812
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc40955d.txt
_cod_data_source_block           1
_cod_original_cell_volume        2214.51(19)
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7109165