Hierarchy of hydrogen bonding in bis(1,4,7-trioxa-10-azoniacyclododecane) bis(4-aminobenzoate) trihydrate
Basok, Stepan S.; Bocelli, Gabriele; Fonari, Marina S.; Ganin, Eduard V.; Simonov, Yurii A.; Acta Crystallographica Section C 62 (2006) o50–o52; doi:10.1107/S0108270105040667

data_2014333
_publ_section_title
;
 Hierarchy of hydrogen bonding in
 bis(1,4,7-trioxa-10-azoniacyclododecane) bis(4-aminobenzoate)
 trihydrate
;
_journal_coeditor_code           FG3002
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o50
_journal_page_last               o52
_journal_paper_doi               10.1107/S0108270105040667
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '2C8 H18 N O3 + , 2C7 H6 N O2 - , 3H2 O'
_chemical_formula_moiety         '2C8 H18 N O3 + , 2C7 H6 N O2 - , 3H2 O'
_chemical_formula_sum            'C30 H54 N4 O13'
_chemical_formula_weight         678.77
_chemical_melting_point          114.5(5)
_chemical_name_common
;
Bis(azonia-12-crown-4) bis(4-aminobenzoate) trihydrate
;
_chemical_name_systematic
;
bis(1,4,7-trioxa-10-azoniacyclododecane)
bis(4-aminobenzoate) trihydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.91(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.541(3)
_cell_length_b                   9.5315(19)
_cell_length_c                   15.989(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      5.0
_cell_volume                     1785.4(7)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       \w/2\q
_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  0.0305
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17540
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74523
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.118
_refine_diff_density_min         -0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         3714
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0314P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                2856
_reflns_number_total             3714
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg3002.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '114--115' was changed to '114.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '114--115' was changed to '114.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1785.4(6)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               2014333