CB-TE2A^+^·Cl^{-^}·3H~2~O: a short intermolecular hydrogen bond between zwitterionic bicyclo[6.6.2]tetraamine macrocycles
Jurek, Paul; Reibenspies, Joseph H.; Kiefer, Garry E.; Acta Crystallographica Section C 72 (2016) 139–142; doi:10.1107/S2053229616000358

data_2020400
_publ_section_title
;
 CB-TE2A^+^&#x00B7;Cl^{-^}&#x00B7;3H~2~O: a short intermolecular hydrogen
 bond between zwitterionic bicyclo[6.6.2]tetraamine macrocycles
;
_journal_coeditor_code           SK3611
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              139
_journal_page_last               142
_journal_paper_doi               10.1107/S2053229616000358
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          'C16 H31 N4 O4 +, Cl -, 3H2 O'
_chemical_formula_moiety         'C16 H31 N4 O4 +, Cl -, 3(H2 O)'
_chemical_formula_sum            'C16 H37 Cl N4 O7'
_chemical_formula_weight         432.94
_chemical_name_systematic
;
11-Carboxymethyl-1,8-tetraaza-4,11-diazoniabicyclo[6.6.2]hexadecane-4-acetate
chloride trihydrate
;
_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   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                106.332(4)
_cell_angle_beta                 90.296(5)
_cell_angle_gamma                93.842(5)
_cell_formula_units_Z            2
_cell_length_a                   8.3119(7)
_cell_length_b                   10.7358(8)
_cell_length_c                   12.2031(10)
_cell_measurement_reflns_used    3363
_cell_measurement_temperature    110
_cell_measurement_theta_max      64.01
_cell_measurement_theta_min      3.78
_cell_volume                     1042.33(15)
_computing_cell_refinement
;
FRAMBO (Bruker, 2004)
;
_computing_data_collection
;
FRAMBO (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2004)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009) and
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      110
_diffrn_detector_area_resol_mean 4
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker GADDS'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10728
_diffrn_reflns_theta_full        64.003
_diffrn_reflns_theta_max         64.003
_diffrn_reflns_theta_min         3.776
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_T_max  0.9058
_exptl_absorpt_correction_T_min  0.8236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2009)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_description       needle
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         3289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                2674
_reflns_number_total             3289
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            sk3611sup1.cif
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2020400.cif.'
_cod_database_code               2020400
_cod_database_fobs_code          2020400
_shelx_estimated_absorpt_t_min   0.824
_shelx_estimated_absorpt_t_max   0.906
_shelx_hkl_checksum              39964
_shelx_res_checksum              8662