Ammonium‒crown ether based host‒guest systems: N‒H⋯O hydrogen bond directed guest inclusion featuring N‒H donor functionalities in angular geometry
Sarma, Monima; Chatterjee, Tanmay; Das, Samar K.; RSC Advances 2 (2012) 3920–; doi:10.1039/c2ra20109g

data_7238612
_publ_section_title
;
 Ammonium--crown ether based host--guest systems: N--H&#x22EF;O hydrogen
 bond directed guest inclusion featuring N--H donor functionalities in
 angular geometry
;
_journal_issue                   9
_journal_name_full               'RSC Advances'
_journal_page_first              3920
_journal_paper_doi               10.1039/c2ra20109g
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety
'2(C14 H20 O5),2(C5 H8 N2), 4(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C38 H60 Cl4 N4 O28'
_chemical_formula_weight         1162.70
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 112.756(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7353(14)
_cell_length_b                   15.4444(12)
_cell_length_c                   19.7642(16)
_cell_measurement_reflns_used    7692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.48
_cell_volume                     4992.2(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47292
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.334
_exptl_absorpt_correction_T_max  0.9547
_exptl_absorpt_correction_T_min  0.9065
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.252
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         8790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0647
_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^)+(0.0575P)^2^+13.4466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1559
_reflns_number_gt                7709
_reflns_number_total             8790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra20109g.txt
_cod_data_source_block           3AP-B15C5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7238612