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_7238613
_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         '3(C22 H28 O7),3(C5 H8 N2),6(Cl O4),5(H2 O)'
_chemical_formula_sum            'C81 H118 Cl6 N6 O50'
_chemical_formula_weight         2188.51
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                85.190(1)
_cell_angle_beta                 89.215(1)
_cell_angle_gamma                89.297(1)
_cell_formula_units_Z            2
_cell_length_a                   11.9802(8)
_cell_length_b                   12.7041(9)
_cell_length_c                   34.277(2)
_cell_measurement_reflns_used    6067
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.30
_cell_volume                     5197.7(6)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            43314
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_correction_T_min  0.9024
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1332
_refine_ls_number_reflns         18210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0659
_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^)+(0.0683P)^2^+11.0448P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1668
_reflns_number_gt                14548
_reflns_number_total             18210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra20109g.txt
_cod_data_source_block           3AP-DB21C7
_cod_database_code               7238613