Trospium Chloride: Unusual Example of Polymorphism Based on Structure Disorder
Skořepová, Eliška; Čejka, Jan; Hušák, Michal; Eigner, Václav; Rohlíček, Jan; Šturc, Antonín; Kratochvíl, Bohumil; Crystal Growth & Design 13 (2013) 5193–; doi:10.1021/cg4007394

data_4508402
_publ_section_title
;
 Trospium Chloride: Unusual Example of Polymorphism Based on Structure
 Disorder
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              5193
_journal_paper_doi               10.1021/cg4007394
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         'C25.00 H30 Cl1.00 N1.00 O3.00'
_chemical_formula_sum            'C25 H30 Cl N O3'
_chemical_formula_weight         427.97
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 100.685(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9483(3)
_cell_length_b                   10.9241(3)
_cell_length_c                   18.0149(5)
_cell_measurement_reflns_used    10999
_cell_measurement_temperature    150
_cell_measurement_theta_max      77
_cell_measurement_theta_min      4
_cell_volume                     2117.23(10)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.036
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23949
_diffrn_reflns_theta_full        74.605
_diffrn_reflns_theta_max         77.713
_diffrn_reflns_theta_min         4.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.812
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.68429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912.000
_exptl_crystal_size_max          0.491
_exptl_crystal_size_mid          0.377
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.71
_refine_ls_extinction_coef       11.8(7)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4459
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.0003739
_refine_ls_shift/su_mean         0.0000202
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Quasi-Unit weights 
 W = 1.0 or 1./2F 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1006
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1006
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                3253
_reflns_number_total             4459
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.91
_oxford_diffrn_Wilson_scale      0.06
_oxford_refine_ls_r_factor_ref   0.0680
_oxford_refine_ls_scale          4.04(5)
_oxford_reflns_number_all        4459
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            cg4007394_si_002.cif
_cod_data_source_block           1
_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 2.4.2 from
2011-04-26.

'_atom_sites_solution_primary' value 'Direct' changed to
'direct' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/c 1 '
_cod_original_formula_sum        'C25.00 H30 Cl1.00 N1.00 O3.00'
_cod_database_code               4508402
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE FIRST(X'S, U'S, OCC) UNTIL C(25) 
CONT EXTPARAM 
EQUIVALENCE CL(1,OCC) UNTIL H(252) CL(31,OCC) UNTIL H(552) 
WEIGHT -1 CL(31,OCC) UNTIL H(552) 
LINK CL(1,U'S) UNTIL C(25) AND CL(31,U'S) UNTIL C(55) 
RIDE CL(1,X'S) CL(31,X'S) 
RIDE O(1,X'S) O(31,X'S) H(1,X'S) H(301,X'S) 
RIDE O(2,X'S) O(32,X'S) 
RIDE O(3,X'S) O(33,X'S) 
RIDE N(1,X'S) N(31,X'S) 
RIDE C(1,X'S) C(31,X'S) 
RIDE C(2,X'S) C(32,X'S) 
RIDE C(3,X'S) C(33,X'S) 
RIDE C(4,X'S) H(41,X'S) C(34,X'S) H(341,X'S) 
RIDE C(5,X'S) H(51,X'S) C(35,X'S) H(351,X'S) 
RIDE C(6,X'S) H(61,X'S) C(36,X'S) H(361,X'S) 
RIDE C(7,X'S) H(71,X'S) C(37,X'S) H(371,X'S) 
RIDE C(8,X'S) H(81,X'S) C(38,X'S) H(381,X'S) 
RIDE C(9,X'S) C(39,X'S) 
RIDE C(10,X'S) H(101,X'S) C(40,X'S) H(401,X'S) 
RIDE C(11,X'S) H(111,X'S) C(41,X'S) H(411,X'S) 
RIDE C(12,X'S) H(121,X'S) C(42,X'S) H(421,X'S) 
RIDE C(13,X'S) H(131,X'S) C(43,X'S) H(431,X'S) 
RIDE C(14,X'S) H(141,X'S) C(44,X'S) H(441,X'S) 
RIDE C(15,X'S) H(151,X'S) C(45,X'S) H(451,X'S) 
RIDE C(16,X'S) H(161,X'S) H(162,X'S) 
CONT C(46,X'S) H(461,X'S) H(462,X'S) 
RIDE C(17,X'S) H(171,X'S) C(47,X'S) H(471,X'S) 
RIDE C(18,X'S) H(182,X'S) H(181,X'S) 
CONT C(48,X'S) H(482,X'S) H(481,X'S) 
RIDE C(19,X'S) H(191,X'S) H(192,X'S) 
CONT C(49,X'S) H(491,X'S) H(492,X'S) 
RIDE C(20,X'S) H(201,X'S) C(50,X'S) H(501,X'S) 
RIDE C(21,X'S) H(212,X'S) H(211,X'S) 
CONT C(51,X'S) H(512,X'S) H(511,X'S) 
RIDE C(22,X'S) H(221,X'S) H(222,X'S) 
CONT C(52,X'S) H(521,X'S) H(522,X'S) 
RIDE C(23,X'S) H(232,X'S) H(231,X'S) 
CONT C(53,X'S) H(532,X'S) H(531,X'S) 
RIDE C(24,X'S) H(242,X'S) H(241,X'S) 
CONT C(54,X'S) H(542,X'S) H(541,X'S) 
RIDE C(25,X'S) H(251,X'S) H(252,X'S) 
CONT C(55,X'S) H(551,X'S) H(552,X'S) 
WEIGHT -1 CL(31,Y) UNTIL LAST 
WEIGHT -1 CL(31,U[12]) UNTIL C(55) 
WEIGHT -1 CL(31,U[23]) UNTIL C(55) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;