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_1542840
_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 H11 N O'
_chemical_formula_sum            'C27 H29 Cl N2 O7'
_chemical_formula_weight         528.97
_chemical_melting_point          365
_chemical_name_common            ACM-CPR
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'MRIA, SHELXL-97, manual'
_cell_angle_alpha                92.373(15)
_cell_angle_beta                 93.003(16)
_cell_angle_gamma                85.308(17)
_cell_formula_units_Z            2
_cell_length_a                   11.9406(16)
_cell_length_b                   21.3081(19)
_cell_length_c                   5.1030(14)
_cell_measurement_reflns_used    1572
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      39.989
_cell_measurement_theta_min      2.071
_cell_volume                     1291.3(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    1.728
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             556
_pd_block_diffractogram_id       CPR
_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        0.008
_pd_meas_2theta_range_max        80.000
_pd_meas_2theta_range_min        3.000
_pd_meas_number_of_points        9626
_pd_meas_scan_method             cont
_pd_prep_pressure                101
_pd_prep_temperature             298(2)
_pd_proc_2theta_range_inc        0.008
_pd_proc_2theta_range_max        80.000
_pd_proc_2theta_range_min        3.000
_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 4th order 
(Ahtee et al., 1989; Jarvinen, 1993)
;
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_prof_R_factor        0.0429
_pd_proc_ls_prof_wR_expected     0.0428
_pd_proc_ls_prof_wR_factor       0.0503
_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         0.44
_refine_diff_density_min         -0.32
_refine_diff_density_rms         0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.1753
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    0
_refine_ls_number_parameters     183
_refine_ls_number_restraints     123
_refine_ls_R_I_factor            0.0784
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_publcif_datablock.id            {9a9228c2-4b53-46ea-94d1-4b03e2b0fcb9}
_cod_data_source_file            bi5031.cif
_cod_data_source_block           ACM-CPR
_cod_depositor_comments          'Adding Fobs data.'
_cod_database_code               1542840
_cod_database_fobs_code          1542840