Acemetacin cocrystals and salts: structure solution from powder X-ray data and form selection of the piperazine salt
Sanphui, Palash; Bolla, Geetha; Nangia, Ashwini; Chernyshev, Vladimir; IUCrJ 1 (2014) 136–150; doi:10.1107/S2052252514004229

data_1542843
_publ_section_title
;
 Acemetacin cocrystals and salts: structure solution from powder X-ray
 data and form selection of the piperazine salt
;
_journal_issue                   2
_journal_name_full               IUCrJ
_journal_page_first              136
_journal_page_last               150
_journal_paper_doi               10.1107/S2052252514004229
_journal_volume                  1
_journal_year                    2014
_chemical_formula_moiety         'C21 H18 Cl N O6, C6 H6 N2 O'
_chemical_formula_sum            'C27 H24 Cl N3 O7'
_chemical_formula_weight         537.94
_chemical_melting_point          384
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_method           'MRIA, SHELXL-97, manual'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.954(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.7202(15)
_cell_length_b                   5.0077(14)
_cell_length_c                   11.8457(17)
_cell_measurement_reflns_used    915
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      39.982
_cell_measurement_theta_min      2.040
_cell_volume                     1285.4(4)
_computing_cell_refinement       'MRIA (Zlokazov & Chernyshev, 1992)'
_computing_data_collection       'DataCollector (PANalytical, 2010)'
_computing_data_reduction        DataCollector
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'MRIA, SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  MRIA
_computing_structure_solution    'simulated annealing (Zhukov et al., 2001)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_type            Xcelerator
_diffrn_measurement_device       'EMPYREAN (PANanalytical)'
_diffrn_radiation_monochromator  Ni-filter
_diffrn_radiation_source         'line-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_source                   'Fine focus X-ray tube'
_diffrn_source_target            Cu
_exptl_absorpt_coefficient_mu    1.763
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560
_pd_block_diffractogram_id       PAM
_pd_char_colour                  colorless
_pd_char_particle_morphology     needle
_pd_instr_location
;
 A. N. Frumkin Institute of Physical Chemistry and Electrochemistry RAS,
 Leninsky prospect, 31,
 Moscow 119071, 
 Russian Federation
;
_pd_meas_2theta_range_inc        0.017
_pd_meas_2theta_range_max        80.011
_pd_meas_2theta_range_min        3.001
_pd_meas_number_of_points        4531
_pd_meas_scan_method             cont
_pd_prep_pressure                101
_pd_prep_temperature             298(2)
_pd_proc_2theta_range_inc        0.017
_pd_proc_2theta_range_max        80.011
_pd_proc_2theta_range_min        3.001
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function  'Chebyshev polynomial up to the 5th order'
_pd_proc_ls_pref_orient_corr
;
spherical harmonics expansion up to the 6th order 
(Ahtee et al.,  1989; Jarvinen, 1993)
;
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_prof_R_factor        0.0312
_pd_proc_ls_prof_wR_expected     0.0232
_pd_proc_ls_prof_wR_factor       0.0465
_pd_proc_wavelength              1.5418
_pd_spec_mounting
; 
thin layer on the non-diffracting silicon plate
;
_pd_spec_mount_mode              reflection
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              15
_pd_spec_size_equat              1
_pd_spec_size_thick              1
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.38
_refine_diff_density_rms         0.29
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.0013
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    36
_refine_ls_number_parameters     185
_refine_ls_number_restraints     125
_refine_ls_R_I_factor            0.0607
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_publcif_datablock.id            {e093e25f-2a36-48ef-9bd1-f4dc1f006a1a}
_cod_data_source_file            bi5031.cif
_cod_data_source_block           ACM-PAM
_cod_depositor_comments          'Adding Fobs data.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1542843
_cod_database_fobs_code          1542843