Influence of the Ammonium Cation and 18-Crown-6 Guest on the Supramolecular Networks of 1,3,5-Cyclohexanetricarboxylic Acid
Bhogala, Balakrishna R.; Nangia, Ashwini; Crystal Growth & Design 6 (2006) 32–35; doi:10.1021/cg050396w

data_4504651
_publ_section_title
;
 Influence of the Ammonium Cation and 18-Crown-6 Guest on the
 Supramolecular Networks of 1,3,5-Cyclohexanetricarboxylic Acid
;
_journal_coden_ASTM              CGDEFU
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              32
_journal_page_last               35
_journal_paper_doi               10.1021/cg050396w
_journal_volume                  6
_journal_year                    2006
_chemical_formula_moiety         'C9 H11 O6-,N H4+,C12 H24 O6,H2 O'
_chemical_formula_sum            'C21 H41 N O13'
_chemical_formula_weight         515.55
_chemical_melting_point          458
_chemical_name_systematic
; 
  Ammonium Cyclohexane-3cis,5cis-dicarboxylic acid-1-carboxylate 
- 18-Crown-6 - Hydrate 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.4695(14)
_cell_length_b                   20.8784(12)
_cell_length_c                   9.6872(5)
_cell_measurement_reflns_used    7534
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.32
_cell_volume                     5151.3(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT Plus'
_computing_molecular_graphics    'PLUTON (Spek, 1992)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            33229
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_T_max  0.9858
_exptl_absorpt_correction_T_min  0.9490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS - Bruker Nonius area detector scaling and absorption correction - V2.10'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.5(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         5578
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0546P)^2^+0.9590P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                5224
_reflns_number_total             5578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg050396wsi20050809_043928.cif
_cod_data_source_block           1
_cod_depositor_comments
;
 Updated the moiety chemical formula to make it consistent with
 the summary chemical formula.

 Antanas Vaitkus,
 2020-09-30
;
_cod_original_sg_symbol_Hall     'P2c -2n'
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               4504651