Formation of new polymorphs without any nucleation step. Desolvation of the rimonabant monohydrate: directional crystallisation concomitant to smooth dehydration.
Fours, Baptiste; Cartigny, Yohann; Petit, Samuel; Coquerel, Gérard; Faraday discussions 179 (2015) 475–488; doi:10.1039/c4fd00222a

data_1518537
_publ_section_title
;
 Formation of new polymorphs without any nucleation step. Desolvation of
 the rimonabant monohydrate: directional crystallisation concomitant to
 smooth dehydration.
;
_journal_name_full               'Faraday discussions'
_journal_page_first              475
_journal_page_last               488
_journal_paper_doi               10.1039/c4fd00222a
_journal_volume                  179
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H23 Cl3 N4 O2'
_chemical_formula_sum            'C22 H23 Cl3 N4 O2'
_chemical_formula_weight         481.79
_chemical_name_systematic        'rimonaban monohydrate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2014-11-12T10:25:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                96.8980(10)
_cell_angle_beta                 96.1770(10)
_cell_angle_gamma                90.6640(10)
_cell_formula_units_Z            4
_cell_length_a                   7.4245(5)
_cell_length_b                   13.2237(8)
_cell_length_c                   24.7183(16)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    569(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     2394.5(3)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      569(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            19375
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.408
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         9674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.095
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                4953
_reflns_number_total             9674
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4fd00222a2.cif
_cod_data_source_block           spsr141m
_cod_depositor_comments          'Adding full bibliography for 1518537.cif.'
_cod_database_code               1518537