Anti-Inflammatory Drugs. V. [Tris-(2-hydroxymethyl)methyl]ammonium 2-[(2,6-Dichlorophenyl)amino]phenylacetate (TRISH. D)
Castellari, C.; Ottani, S.; Acta Crystallographica Section C 53 (1997) 482–486; doi:10.1107/S0108270196013649

data_2006074
_publ_section_title
;
 Anti-Inflammatory Drugs. V. [Tris-(2-hydroxymethyl)methyl]ammonium
 2-[(2,6-Dichlorophenyl)amino]phenylacetate (TRISH. D)
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              482
_journal_page_last               486
_journal_paper_doi               10.1107/S0108270196013649
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C4 H12 N O3 1+, C14 H10 Cl2 N O2 1-'
_chemical_formula_sum            'C18 H22 Cl2 N2 O5'
_chemical_formula_weight         417.28
_chemical_name_systematic
;
 Tris(2-hydroxymethyl)methylammonium (2,6-dichlorophenyl)amino-phenylacetate
 (HTRIS.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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.12(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.152(3)
_cell_length_b                   9.407(3)
_cell_length_c                   19.448(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      5
_cell_volume                     1857.3(11)
_computing_cell_refinement       'CAD4 software'
_computing_data_collection       'CAD4 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      298(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0849
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6488
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  160
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.49
_exptl_crystal_density_meas      1.48
_exptl_crystal_density_method
;
flotation in a mixture of 1-bromo-2-chloroethane and p-xylene
;
_exptl_crystal_description       plate
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.211
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.996
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_hydrogen_treatment
;H atoms riding except H1, H11, H12, H13, H20, H21 and H22 for which all
 parameters were refined
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         3251
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.008
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.1153
_refine_ls_R_factor_obs          0.0403
_refine_ls_shift/esd_max         -0.069
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.0058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0866
_refine_ls_wR_factor_obs         0.0670
_reflns_number_observed          1804
_reflns_number_total             3258
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            na1262.cif
_cod_data_source_block           TRISH.D
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.0058P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.0058P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               2006074