Diclofenac Salts. IV. Tris(2-hydroxyethyl)ammonium 2-(2,6-Dichlorophenylamino)phenylacetate
Castellari, C.; Ottani, S.; Acta Crystallographica Section C 52 (1996) 2619–2622; doi:10.1107/S0108270196006300

data_2005442
_publ_section_title
;
 Diclofenac Salts. IV. Tris(2-hydroxyethyl)ammonium
 2-(2,6-Dichlorophenylamino)phenylacetate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2619
_journal_page_last               2622
_journal_paper_doi               10.1107/S0108270196006300
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C6 H16 N O3 1+, C14 H10 Cl2 N O2 1-'
_chemical_formula_sum            'C20 H26 Cl2 N2 O5'
_chemical_formula_weight         445.33
_chemical_melting_point          406
_chemical_name_systematic
;
Tris(2-hydroxyethyl)ammonium (2,6-dichlorophenyl)amino-phenylacetate (HTEA.D)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_cell_angle_alpha                90.00(2)
_cell_angle_beta                 93.24(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   10.589(3)
_cell_length_b                   9.396(2)
_cell_length_c                   21.132(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      6
_cell_volume                     2099.2(9)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'MolEN (Fair, 1990)'
_computing_molecular_graphics
'SCHAKAL92 (Keller, 1992), ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       'profile data from \w'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1050
_diffrn_reflns_av_sigmaI/netI    0.1524
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10213
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.90
_diffrn_standards_decay_%        'intensity variation: none'
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.40
_exptl_crystal_density_meas      1.41
_exptl_crystal_description       prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.955
_refine_ls_goodness_of_fit_obs   1.133
_refine_ls_hydrogen_treatment
;
H atoms riding except for H1, H11, H16, H21 and H26, for which all
parameters were refined
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5051
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      0.959
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.1955
_refine_ls_R_factor_obs          0.0464
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0344P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1006
_refine_ls_wR_factor_obs         0.0698
_reflns_number_observed          1936
_reflns_number_total             5053
_reflns_observed_criterion       >2\s(I)
_cod_data_source_file            ab1345.cif
_cod_data_source_block           team
_cod_original_cell_volume        2099.3(9)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2005442
_cod_database_fobs_code          2005442