Anti-Inflammatory Drugs. III. Salts of Diclofenac with <i>N</i>-(2-Hydroxyethyl)piperidine, <i>N</i>-(2-Hydroxyethyl)morpholine and <i>N</i>-(2-Hydroxyethyl)piperazine
Castellari, C.; Sabatino, P.; Acta Crystallographica Section C 52 (1996) 1708–1712; doi:10.1107/S0108270196000571

data_2005092
_publ_section_title
;
 Anti-Inflammatory Drugs. III. Salts of Diclofenac with
 <i>N</i>-(2-Hydroxyethyl)piperidine,
 <i>N</i>-(2-Hydroxyethyl)morpholine and
 <i>N</i>-(2-Hydroxyethyl)piperazine
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1708
_journal_page_last               1712
_journal_paper_doi               10.1107/S0108270196000571
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          'C6 H14 N O2 1+, C14 H10 Cl2 N O2 1-'
_chemical_formula_moiety         'C6 H14 N O2 1+, C14 H10 Cl2 N O2 1-'
_chemical_formula_sum            'C20 H24 Cl2 N2 O4'
_chemical_formula_weight         427.31
_chemical_name_systematic
;
N-(2-hydroxyethyl)morpholinium[2-[(2,6-dichlorophenyl)amino]phenyl]acetate
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.81(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.525(2)
_cell_length_b                   12.962(4)
_cell_length_c                   16.579(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      9.87
_cell_measurement_theta_min      6.6
_cell_volume                     2045.9(12)
_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)'
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3711
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.65
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.346
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_density_meas      1.37(2)
_exptl_crystal_density_method
'flotation in a 1-bromo-2-chloroethane/p-xylene mixture'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.035
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_hydrogen_treatment
'H atoms riding except for H1, H11 and H24 for which all parameters refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_obs          0.0428
_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^) + (0.047P)^2^ + 1.27P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1208
_refine_ls_wR_factor_obs         0.1006
_reflns_number_observed          2316
_reflns_number_total             3581
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bm1046.cif
_cod_data_source_block           2
_cod_original_cell_volume        2045.9(11)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2005092