Solid‒Solid Transition between Hydrated Racemic Compound and Anhydrous Conglomerate in Na-Ibuprofen: A Combined X-ray Diffraction, Solid-State NMR, Calorimetric, and Computational Study
Rossi, Patrizia; Macedi, Eleonora; Paoli, Paola; Bernazzani, Luca; Carignani, Elisa; Borsacchi, Silvia; Geppi, Marco; Crystal Growth & Design 14 (2014) 2441–; doi:10.1021/cg500161e

data_4510388
_publ_section_title
;
 Solid--Solid Transition between Hydrated Racemic Compound and Anhydrous
 Conglomerate in Na-Ibuprofen: A Combined X-ray Diffraction, Solid-State
 NMR, Calorimetric, and Computational Study
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2441
_journal_paper_doi               10.1021/cg500161e
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         '(C13 H17 O2)-, Na +, (H2 O) 2'
_chemical_formula_sum            'C13 H21 Na O4'
_chemical_formula_weight         264.29
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.309(8)
_cell_angle_beta                 90.212(8)
_cell_angle_gamma                117.137(9)
_cell_formula_units_Z            2
_cell_length_a                   5.7808(5)
_cell_length_b                   6.0812(5)
_cell_length_c                   23.998(2)
_cell_measurement_reflns_used    1163
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.5880
_cell_measurement_theta_min      4.1589
_cell_volume                     746.54(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'ORTEP-3 (Farruggia, 1997)'
_computing_publication_material  'PARST97 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.826
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_av_sigmaI/netI    0.2128
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8188
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.65
_diffrn_reflns_theta_min         4.17
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2602
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.2339
_refine_ls_R_factor_gt           0.0987
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.2379
_reflns_number_gt                1038
_reflns_number_total             2602
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg500161e_si_001.cif
_cod_data_source_block           RS-Hrt
_cod_depositor_comments
'Adding full bibliography for 4510385--4510388.cif.'
_cod_original_cell_volume        746.54(11)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4510388