Influence of the cavity dimension on encapsulation of halides within the capsular assembly and side-cleft recognition of a sulfate‒water cluster assisted by polyammonium tripodal receptors
Manna, Utsab; Nayak, Biswajit; Hoque, Md. Najbul; Das, Gopal; CrystEngComm 18 (2016) 5036–; doi:10.1039/C6CE00220J

data_7225334
_publ_section_title
;
 Influence of the cavity dimension on encapsulation of halides within the
 capsular assembly and side-cleft recognition of a sulfate--water cluster
 assisted by polyammonium tripodal receptors
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              5036
_journal_paper_doi               10.1039/C6CE00220J
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety
'2(C27 H36 Br3 N4), 3(O4 S), 4(C3 H7 N O), 0.5(H4O2), 7(H2O)'
_chemical_formula_sum            'C66 H116 Br6 N12 O24 S3'
_chemical_formula_weight         2030.92
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1kn86p
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-05-19 deposited with the CCDC.
2016-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                83.354(6)
_cell_angle_beta                 72.763(6)
_cell_angle_gamma                62.704(6)
_cell_formula_units_Z            2
_cell_length_a                   15.3545(17)
_cell_length_b                   15.5993(18)
_cell_length_c                   21.362(2)
_cell_measurement_reflns_used    4500
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      13.17
_cell_measurement_theta_min      2.45
_cell_volume                     4341.4(9)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.829
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.2498
_diffrn_reflns_Laue_measured_fraction_full 0.857
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38150
_diffrn_reflns_point_group_measured_fraction_full 0.857
_diffrn_reflns_point_group_measured_fraction_max 0.829
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.553
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       block
_exptl_crystal_F_000             1996.0
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   0.592
_exptl_transmission_factor_min   0.452
_platon_squeeze_details
;
Three highly disordered C~3~H~7~NO molecules were accounted for using the Platon SQUEEZE function.
A total of 255 electrons was removed from the unit-cell contents by SQUEEZE, which implies  
that 255/2 = 128 of the squeezed-out electrons associated with the formula unit in this 2b complex 
in triclinic space group P-1 with Z = 2. As one DMF molecule contains 40 electrons, this 
implies the contributions of 128/40 = 3 DMF molecules were removed from the Formula unit
by the SQUEEZE process.
;
_refine_diff_density_max         0.844
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.837
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         14721
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.837
_refine_ls_R_factor_all          0.2168
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1020P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2171
_refine_ls_wR_factor_ref         0.2540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4507
_reflns_number_total             14721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce00220j2.cif
_cod_data_source_block           2L2H6_3SO4_8H2O_4DMF
_cod_depositor_comments
'Adding full bibliography for 7225330--7225335.cif.'
_cod_database_code               7225334
_shelx_estimated_absorpt_t_min   0.486
_shelx_estimated_absorpt_t_max   0.622
_shelxl_version_number           2013-4
_shelx_res_checksum              55494