data_2105811
_chemical_formula_moiety         'C29 H34 Cl N2 O2 +, Cl -'
_chemical_formula_sum            'C29 H34 Cl2 N2 O2'
_chemical_formula_weight         513.48
_chemical_melting_point          ?
_chemical_name_common            'loperamide hydrochloride anhydrate'
_chemical_name_systematic
;
4-(p-Chlorophenyl)-4-hydroxy-N,N-dimethyl-\a,\a-diphenyl-1-piperidinebutyramide
 hydrochloride
;
_space_group_crystal_system      monoclinic
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_update_record
;
2013-08-27 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 101.6420(29)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.70954(81)
_cell_length_b                   12.37731(46)
_cell_length_c                   13.21351(47)
_cell_measurement_temperature    298(2)
_cell_volume                     2676.59(19)
_computing_cell_refinement       '<i>TOPAS Academic</i> (Coelho, 2007)'
_computing_data_collection       '<i>STOE WinXPOW</i> (STOE & Cie GmbH, 2006)'
_computing_data_reduction        '<i>TOPAS Academic</i> (Coelho, 2007)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_computing_structure_refinement  '<i>TOPAS Academic</i> (Coelho, 2007)'
_computing_structure_solution    'FIDEL (Habermehl et al., 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector
;
linear position sensitive detector
;
_diffrn_measurement_device_type
;
STOE Stadi-P
;
_diffrn_radiation_monochromator
;
primary focussing Ge 111
;
_diffrn_radiation_type
;
Cu K\a~1~
;
_diffrn_radiation_wavelength     1.54056
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    2.401
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       powder
_exptl_crystal_F_000             1088.0
_pd_char_colour                  colourless
_pd_char_particle_morphology     ?
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        100.190
_pd_meas_2theta_range_min        2.000
_pd_meas_number_of_points        9820
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        100.190
_pd_proc_2theta_range_min        2.000
_pd_proc_info_excluded_regions   ?
_pd_proc_ls_background_function  'Chebyshev with 20 terms'
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function
' modified Thompson-Cox-Hastings pseudo-Voigt'
_pd_proc_ls_prof_R_factor        0.043
_pd_proc_ls_prof_wR_expected     0.027
_pd_proc_ls_prof_wR_factor       0.060
_pd_proc_wavelength              1.54056
_pd_spec_mounting                'glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder
_pd_spec_size_axial              10
_pd_spec_size_equat              1
_pd_spec_size_thick              1
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.254
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    0
_refine_ls_number_parameters     259
_refine_ls_number_restraints     201
_refine_ls_R_factor_all          ?
_refine_ls_R_Fsqd_factor         ?
_refine_ls_R_I_factor            0.030
_refine_ls_shift/su_max          0.001
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            og5067Isup2.rtv
_cod_data_source_block           I
loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_B_iso_or_equiv
_atom_site_U_iso_or_equiv
Cl1 Cl 0.53266(31) 0.07952(34) 0.88473(29) 1 0 4.32(20) 0.05469
C2 C 0.31872(24) 0.39660(32) 0.49174(34) 1 0 3.86(13) 0.04888
C3 C 0.34070(24) 0.28451(32) 0.45621(34) 1 0 3.86(13) 0.04888
H4 H 0.35642(90) 0.4541(10) 0.47646(97) 1 0 4.63(16) 0.05866
H5 H 0.3207(10) 0.3970(11) 0.56715(92) 1 0 4.63(16) 0.05866
C6 C 0.23052(25) 0.41698(26) 0.42898(27) 1 0 3.86(13) 0.04888
N7 N 0.42813(26) 0.26286(33) 0.50122(30) 1 0 3.86(13) 0.04888
H8 H 0.30509(99) 0.22825(98) 0.4777(10) 1 0 4.63(16) 0.05866
H9 H 0.3307(11) 0.28300(99) 0.37907(88) 1 0 4.63(16) 0.05866
C10 C 0.18025(38) 0.30354(41) 0.41201(33) 1 0 3.86(13) 0.04888
C11 C 0.19112(24) 0.51241(31) 0.47310(25) 1 0 3.86(13) 0.04888
C12 C 0.23580(26) 0.45787(24) 0.31975(31) 1 0 3.86(13) 0.04888
H13 H 0.4584(11) 0.3179(10) 0.4753(11) 1 0 4.63(16) 0.05866
C14 C 0.44954(24) 0.26136(35) 0.61718(30) 1 0 3.86(13) 0.04888
C15 C 0.45931(24) 0.15756(33) 0.46662(34) 1 0 3.86(13) 0.04888
O16 O 0.15539(56) 0.26718(57) 0.32227(45) 1 0 3.86(13) 0.04888
N17 N 0.14343(31) 0.26224(45) 0.48944(32) 1 0 3.86(13) 0.04888
C18 C 0.10051(24) 0.52566(31) 0.44546(26) 1 0 3.86(13) 0.04888
C19 C 0.24535(23) 0.58438(30) 0.53920(24) 1 0 3.86(13) 0.04888
C20 C 0.15913(25) 0.48292(25) 0.24182(30) 1 0 3.86(13) 0.04888
C21 C 0.31434(25) 0.47035(25) 0.29648(29) 1 0 3.86(13) 0.04888
C22 C 0.54552(26) 0.26654(33) 0.65291(32) 1 0 3.86(13) 0.04888
H23 H 0.42760(91) 0.1923(10) 0.64111(93) 1 0 4.63(16) 0.05866
H24 H 0.42075(97) 0.3228(10) 0.64382(91) 1 0 4.63(16) 0.05866
H25 H 0.4434(11) 0.1531(11) 0.39159(92) 1 0 4.63(16) 0.05866
H26 H 0.43240(90) 0.09644(99) 0.49608(99) 1 0 4.63(16) 0.05866
C27 C 0.55446(27) 0.15347(35) 0.50399(30) 1 0 3.86(13) 0.04888
C28 C 0.17287(25) 0.29505(32) 0.59901(29) 1 0 3.86(13) 0.04888
C29 C 0.06518(25) 0.19376(34) 0.46064(30) 1 0 3.86(13) 0.04888
H30 H 0.06579(90) 0.4753(11) 0.40029(96) 1 0 4.63(16) 0.05866
C31 C 0.06263(24) 0.61124(30) 0.48392(25) 1 0 3.86(13) 0.04888
C32 C 0.20477(24) 0.66790(31) 0.57548(26) 1 0 3.86(13) 0.04888
H33 H 0.30629(96) 0.5766(11) 0.55800(93) 1 0 4.63(16) 0.05866
H34 H 0.10119(91) 0.4767(11) 0.25320(93) 1 0 4.63(16) 0.05866
C35 C 0.16917(25) 0.51792(23) 0.14859(30) 1 0 3.86(13) 0.04888
C36 C 0.32058(24) 0.50431(24) 0.20399(29) 1 0 3.86(13) 0.04888
H37 H 0.36441(89) 0.4556(10) 0.34534(86) 1 0 4.63(16) 0.05866
C38 C 0.58543(27) 0.15856(33) 0.62397(27) 1 0 3.86(13) 0.04888
H39 H 0.56016(98) 0.2768(10) 0.72857(98) 1 0 4.63(16) 0.05866
H40 H 0.56909(97) 0.3300(10) 0.62143(94) 1 0 4.63(16) 0.05866
H41 H 0.57490(89) 0.0854(11) 0.47918(94) 1 0 4.63(16) 0.05866
H42 H 0.58049(91) 0.21431(96) 0.4729(10) 1 0 4.63(16) 0.05866
H43 H 0.18794(92) 0.23155(98) 0.6424(10) 1 0 4.63(16) 0.05866
H44 H 0.22313(96) 0.3397(11) 0.60525(96) 1 0 4.63(16) 0.05866
H45 H 0.12755(97) 0.3361(11) 0.6207(10) 1 0 4.63(16) 0.05866
H46 H 0.0515(12) 0.1831(10) 0.3844(11) 1 0 4.63(16) 0.05866
H47 H 0.0159(12) 0.23014(99) 0.4805(12) 1 0 4.63(16) 0.05866
H48 H 0.07361(99) 0.1218(10) 0.4938(11) 1 0 4.63(16) 0.05866
H49 H 0.0032(12) 0.62190(98) 0.4675(10) 1 0 4.63(16) 0.05866
C50 C 0.11530(24) 0.68205(32) 0.54869(26) 1 0 3.86(13) 0.04888
H51 H 0.23833(97) 0.7161(10) 0.61894(91) 1 0 4.63(16) 0.05866
H52 H 0.12027(85) 0.5341(12) 0.09664(93) 1 0 4.63(16) 0.05866
C53 C 0.25111(25) 0.52831(22) 0.13004(31) 1 0 3.86(13) 0.04888
H54 H 0.37337(88) 0.5102(11) 0.19025(93) 1 0 4.63(16) 0.05866
O55 O 0.55119(42) 0.06436(44) 0.65873(38) 1 0 3.86(13) 0.04888
C56 C 0.67675(24) 0.13973(33) 0.64654(22) 1 0 3.86(13) 0.04888
H57 H 0.08869(96) 0.7408(10) 0.5742(11) 1 0 4.63(16) 0.05866
H58 H 0.25823(83) 0.5519(11) 0.06395(93) 1 0 4.63(16) 0.05866
H59 H 0.5553(11) 0.0696(11) 0.72500(83) 1 0 4.63(16) 0.05866
C60 C 0.73285(24) 0.21718(33) 0.64579(22) 1 0 3.86(13) 0.04888
C61 C 0.70704(25) 0.03952(31) 0.66633(20) 1 0 3.86(13) 0.04888
H62 H 0.7126(10) 0.2888(10) 0.63178(88) 1 0 4.63(16) 0.05866
C63 C 0.81815(24) 0.19667(32) 0.66470(22) 1 0 3.86(13) 0.04888
C64 C 0.79080(24) 0.01528(33) 0.68515(21) 1 0 3.86(13) 0.04888
H65 H 0.67000(95) -0.01663(96) 0.66741(88) 1 0 4.63(16) 0.05866
H66 H 0.85628(93) 0.2547(10) 0.6644(10) 1 0 4.63(16) 0.05866
C67 C 0.85025(24) 0.09524(35) 0.68481(22) 1 0 3.86(13) 0.04888
H68 H 0.80684(97) -0.0569(11) 0.69820(99) 1 0 4.63(16) 0.05866
Cl69 Cl 0.96051(27) 0.07468(36) 0.70607(27) 1 0 7.53(24) 0.09537
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_source
C C 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C38 O55 H59 108.2(11) . . . no
C3 N7 C15 114.0(3) . . . no
C14 N7 C15 105.8(3) . . . no
C3 N7 C14 115.0(4) . . . no
C10 N17 C28 120.3(4) . . . no
C28 N17 C29 119.3(4) . . . no
C10 N17 C29 120.0(4) . . . no
C14 N7 H13 110.0(9) . . . no
C3 N7 H13 106.2(11) . . . no
C15 N7 H13 105.5(10) . . . no
C3 C2 C6 104.1(3) . . . no
N7 C3 C2 108.5(3) . . . no
C10 C6 C11 118.1(4) . . . no
C11 C6 C12 102.3(3) . . . no
C2 C6 C11 110.9(3) . . . no
C10 C6 C12 106.2(3) . . . no
C2 C6 C10 109.8(3) . . . no
C2 C6 C12 108.8(4) . . . no
O16 C10 N17 116.7(6) . . . no
O16 C10 C6 120.1(5) . . . no
N17 C10 C6 120.5(4) . . . no
C6 C11 C18 119.2(3) . . . no
C18 C11 C19 124.4(3) . . . no
C6 C11 C19 116.4(3) . . . no
C6 C12 C20 120.3(4) . . . no
C6 C12 C21 117.9(4) . . . no
C20 C12 C21 121.8(4) . . . no
N7 C14 C22 108.8(3) . . . no
N7 C15 C27 108.9(3) . . . no
C11 C18 C31 120.8(3) . . . no
C11 C19 C32 112.5(3) . . . no
C12 C20 C35 116.4(4) . . . no
C12 C21 C36 119.2(4) . . . no
C14 C22 C38 110.4(3) . . . no
C15 C27 C38 115.1(4) . . . no
C18 C31 C50 115.1(3) . . . no
C19 C32 C50 123.6(3) . . . no
C20 C35 C53 118.8(4) . . . no
C21 C36 C53 120.6(4) . . . no
O55 C38 C27 102.9(4) . . . no
O55 C38 C56 105.5(4) . . . no
O55 C38 C22 113.7(4) . . . no
C27 C38 C56 107.8(3) . . . no
C22 C38 C27 102.2(3) . . . no
C22 C38 C56 122.9(3) . . . no
C31 C50 C32 123.5(3) . . . no
C35 C53 C36 123.2(3) . . . no
C38 C56 C61 120.3(4) . . . no
C60 C56 C61 115.2(4) . . . no
C38 C56 C60 124.5(3) . . . no
C56 C60 C63 123.3(3) . . . no
C56 C61 C64 123.6(4) . . . no
C60 C63 C67 122.5(3) . . . no
C61 C64 C67 122.1(3) . . . no
Cl69 C67 C64 126.6(3) . . . no
C63 C67 C64 113.4(3) . . . no
Cl69 C67 C63 120.1(3) . . . no
C3 C2 H4 112.6(8) . . . no
C3 C2 H5 110.6(9) . . . no
C6 C2 H4 110.2(9) . . . no
C6 C2 H5 111.7(10) . . . no
H4 C2 H5 107.7(12) . . . no
N7 C3 H8 110.9(9) . . . no
N7 C3 H9 110.7(11) . . . no
C2 C3 H8 110.6(9) . . . no
C2 C3 H9 109.1(8) . . . no
H8 C3 H9 107.0(12) . . . no
N7 C14 H23 107.7(7) . . . no
N7 C14 H24 108.5(8) . . . no
C22 C14 H23 110.6(9) . . . no
C22 C14 H24 113.3(9) . . . no
H23 C14 H24 107.8(12) . . . no
N7 C15 H25 108.5(9) . . . no
N7 C15 H26 109.1(9) . . . no
C27 C15 H25 111.7(11) . . . no
C27 C15 H26 111.1(9) . . . no
H25 C15 H26 107.6(12) . . . no
C11 C18 H30 122.0(9) . . . no
C31 C18 H30 117.2(9) . . . no
C11 C19 H33 125.2(8) . . . no
C32 C19 H33 122.3(8) . . . no
C12 C20 H34 126.2(8) . . . no
C35 C20 H34 117.4(8) . . . no
C12 C21 H37 123.4(9) . . . no
C36 C21 H37 117.4(9) . . . no
C14 C22 H39 109.7(11) . . . no
C14 C22 H40 111.5(9) . . . no
C38 C22 H39 108.9(9) . . . no
C38 C22 H40 110.0(9) . . . no
H39 C22 H40 106.2(11) . . . no
C15 C27 H41 108.6(9) . . . no
C15 C27 H42 110.1(9) . . . no
C38 C27 H41 107.7(8) . . . no
C38 C27 H42 107.7(8) . . . no
H41 C27 H42 107.4(12) . . . no
N17 C28 H43 110.3(8) . . . no
N17 C28 H44 110.0(8) . . . no
N17 C28 H45 107.2(9) . . . no
H43 C28 H44 106.6(13) . . . no
H43 C28 H45 111.1(12) . . . no
H44 C28 H45 111.7(12) . . . no
N17 C29 H46 109.5(11) . . . no
N17 C29 H47 112.6(9) . . . no
N17 C29 H48 110.4(10) . . . no
H46 C29 H47 106.7(15) . . . no
H46 C29 H48 108.1(11) . . . no
H47 C29 H48 109.4(13) . . . no
C18 C31 H49 122.7(8) . . . no
C50 C31 H49 122.1(8) . . . no
C19 C32 H51 114.7(10) . . . no
C50 C32 H51 121.7(10) . . . no
C20 C35 H52 117.9(9) . . . no
C53 C35 H52 123.3(9) . . . no
C21 C36 H54 117.3(8) . . . no
C53 C36 H54 122.1(8) . . . no
C31 C50 H57 114.5(10) . . . no
C32 C50 H57 122.1(10) . . . no
C35 C53 H58 118.8(9) . . . no
C36 C53 H58 118.0(9) . . . no
C56 C60 H62 116.4(10) . . . no
C63 C60 H62 120.4(10) . . . no
C56 C61 H65 117.8(10) . . . no
C64 C61 H65 118.6(10) . . . no
C60 C63 H66 120.6(9) . . . no
C67 C63 H66 116.9(9) . . . no
C61 C64 H68 118.2(11) . . . no
C67 C64 H68 119.7(11) . . . no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl69 C67 1.824(6) . . no
O16 C10 1.257(7) . . no
O55 C38 1.415(7) . . no
O55 H59 0.867(12) . . no
N7 C14 1.502(5) . . no
N7 C15 1.509(5) . . no
N7 C3 1.486(6) . . no
N17 C28 1.489(6) . . no
N17 C29 1.539(7) . . no
N17 C10 1.394(7) . . no
N7 H13 0.952(16) . . no
C2 C6 1.559(6) . . no
C2 C3 1.533(5) . . no
C6 C10 1.628(7) . . no
C6 C11 1.524(6) . . no
C6 C12 1.548(6) . . no
C11 C18 1.493(5) . . no
C11 C19 1.435(5) . . no
C12 C21 1.415(7) . . no
C12 C20 1.506(6) . . no
C14 C22 1.579(6) . . no
C15 C27 1.568(6) . . no
C18 C31 1.381(5) . . no
C19 C32 1.375(5) . . no
C20 C35 1.348(6) . . no
C21 C36 1.316(5) . . no
C22 C38 1.574(6) . . no
C27 C38 1.567(6) . . no
C31 C50 1.405(5) . . no
C32 C50 1.476(5) . . no
C35 C53 1.444(7) . . no
C36 C53 1.391(6) . . no
C38 C56 1.514(6) . . no
C56 C61 1.345(5) . . no
C56 C60 1.343(5) . . no
C60 C63 1.419(5) . . no
C61 C64 1.404(6) . . no
C63 C67 1.371(5) . . no
C64 C67 1.403(5) . . no
C2 H4 0.997(14) . . no
C2 H5 0.991(12) . . no
C3 H8 0.993(15) . . no
C3 H9 0.999(12) . . no
C14 H23 1.006(13) . . no
C14 H24 1.000(14) . . no
C15 H25 0.974(12) . . no
C15 H26 0.999(14) . . no
C18 H30 0.971(14) . . no
C19 H33 1.002(17) . . no
C20 H34 1.012(16) . . no
C21 H37 0.966(14) . . no
C22 H39 0.989(14) . . no
C22 H40 1.006(14) . . no
C27 H41 0.990(14) . . no
C27 H42 0.998(14) . . no
C28 H43 0.975(13) . . no
C28 H44 0.994(17) . . no
C28 H45 1.000(17) . . no
C29 H46 0.995(15) . . no
C29 H47 1.018(19) . . no
C29 H48 0.991(13) . . no
C31 H49 0.98(2) . . no
C32 H51 0.932(14) . . no
C35 H52 0.976(14) . . no
C36 H54 0.939(15) . . no
C50 H57 0.948(15) . . no
C53 H58 0.950(13) . . no
C60 H62 0.954(13) . . no
C61 H65 0.932(15) . . no
C63 H66 0.960(14) . . no
C64 H68 0.939(14) . . no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N7 H13 Cl1 0.952(16) 2.278(16) 3.212(6) 166.7(12) . no
O55 H59 Cl1 0.867(12) 2.221(12) 3.069(7) 165.9(17) . no
loop_
_pd_proc_2theta_corrected
_pd_proc_intensity_net
_pd_calc_intensity_net
_pd_proc_ls_weight
2.00000 1303.00000 1348.89964 0.00077
2.01000 1399.00000 1354.82341 0.00071
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