4-(4-Chlorophenyl)-4-hydroxy-<i>N</i>,<i>N</i>-dimethyl-α,α-diphenyl-1-piperidinebutanamide <i>N</i>-Oxide Hydrate (Loperamide <i>N</i>-Oxide Hydrate)
Peeters, O. M.; Blaton, N. M.; De Ranter, C. J.; Acta Crystallographica Section C 52 (1996) 2100–2102; doi:10.1107/S0108270196005884

data_2005287
_publ_section_title
;4-(4-Chlorophenyl)-4-hydroxy-<i>N</i>,<i>N</i>-dimethyl-\a,\a-diphenyl-1-piperidinebutanamide
 <i>N</i>-Oxide Hydrate (Loperamide <i>N</i>-Oxide Hydrate)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2100
_journal_page_last               2102
_journal_paper_doi               10.1107/S0108270196005884
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          'C29 H33 Cl1 N2 O3, 2.25H2 O'
_chemical_formula_moiety         'C29 H33 Cl1 N2 O3, 2.25H2 O'
_chemical_formula_sum            'C29 H37.5 Cl N2 O5.25'
_chemical_formula_weight         533.58
_chemical_name_systematic
;
4-(4-Chlorophenyl)-4-hydroxy-N,N-dimethyl-\a,\a-diphenyl-
1-piperidinebutanamide-N-oxide
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 96.813(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0543(7)
_cell_length_b                   9.6959(6)
_cell_length_c                   35.025(2)
_cell_measurement_radiation      'Cu K\a'
_cell_measurement_reflns_used    41
_cell_measurement_temperature    293
_cell_measurement_theta_max      27
_cell_measurement_theta_min      11
_cell_measurement_wavelength     1.54184
_cell_volume                     5750.7(5)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1994)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'ORTEX2.1 (McArdle, 1994)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Siemens P4 four-circle diffractometer   '
_diffrn_measurement_method       '\w/2\q scan                             '
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  .0225
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            5226
_diffrn_reflns_theta_max         56.74
_diffrn_standards_decay_%        3.5
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.500
_exptl_absorpt_correction_T_max  .464
_exptl_absorpt_correction_T_min  .337
_exptl_absorpt_correction_type
;
empirical via \y scans (XEMP; Siemens, 1989)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_density_meas      1.232
_exptl_crystal_density_method    'flotation in n-heptane/CCl~4~'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2276
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .10
_refine_diff_density_max         .33
_refine_diff_density_min         -.18
_refine_ls_extinction_coef       .00057(6)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.054
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         3850
_refine_ls_R_factor_all          .0637
_refine_ls_R_factor_obs          .0489
_refine_ls_shift/esd_max         -.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+ 4.9738P]  where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .1407
_refine_ls_wR_factor_obs         .1403
_reflns_number_observed          3030
_reflns_number_total             3851
_reflns_observed_criterion       '> 2.0 sigma(I)'
_cod_data_source_file            na1244.cif
_cod_data_source_block           Y
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+ 4.9738P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+ 4.9738P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5750.8(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C29 H37.5 Cl1 N2 O5.25'
_cod_database_code               2005287