Redetermination of loperamide monohydrate
Jasinski, Jerry P.; Guild, Curtis J.; Dayananda, A. S.; Yathirajan, H. S.; Ramesha, A. R.; Acta Crystallographica Section E 68 (2012) o539–o540; doi:10.1107/S1600536812003091

data_2233572
_publ_section_title
;
 Redetermination of loperamide monohydrate
;
_journal_coeditor_code           LX2225
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o539
_journal_page_last               o540
_journal_paper_doi               10.1107/S1600536812003091
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C29 H33 Cl N2 O2, H2 O'
_chemical_formula_moiety         'C29 H33 Cl N2 O2, H2 O'
_chemical_formula_sum            'C29 H35 Cl N2 O3'
_chemical_formula_weight         495.04
_chemical_name_common            'loperamide monohydrate'
_chemical_name_systematic
;
4-[4-(4-chlorophenyl)-4-hydroxypiperidin-1-yl]-<i>N</i>,<i>N</i>-dimethyl-
2,2-diphenylbutanamide monohydrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.7869(4)
_cell_length_b                   15.1506(6)
_cell_length_c                   20.6617(6)
_cell_measurement_reflns_used    15584
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      32.3408
_cell_measurement_theta_min      3.1043
_cell_volume                     5254.9(3)
_computing_cell_refinement
'<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)'
_computing_data_collection
'<i>CrysAlis PRO</i> (Oxford Diffraction, 2010)'
_computing_data_reduction
'<i>CrysAlis RED</i> (Oxford Diffraction, 2010)'
_computing_molecular_graphics
'<i>SHELXTL</i> (Sheldrick, 2008) and <i>DIAMOND</i> (Brandenburg, 1998)'
_computing_publication_material  '<i>SHELXTL</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SHELXS97</i> (Sheldrick, 2008)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 16.1500
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur Eos Gemini'
_diffrn_measurement_method       '\w scans'
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            48373
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis RED</i>; Oxford Diffraction, 2010)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6247
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+2.2656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                5231
_reflns_number_total             6247
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lx2225.cif
_cod_data_source_block           I
_cod_database_code               2233572
_cod_database_fobs_code          2233572