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_4508401
_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_absolute_configuration ad
_chemical_formula_moiety         'C25 H30.00 Cl1 N1 O3'
_chemical_formula_sum            'C25 H30 Cl N O3'
_chemical_formula_weight         427.97
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 101.042(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1551(10)
_cell_length_b                   10.9184(13)
_cell_length_c                   11.0126(12)
_cell_measurement_reflns_used    3016
_cell_measurement_temperature    150
_cell_measurement_theta_max      78
_cell_measurement_theta_min      4
_cell_volume                     1080.4(2)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'XRED (Stoe & Cie 1996)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13800
_diffrn_reflns_theta_full        74.714
_diffrn_reflns_theta_max         78.646
_diffrn_reflns_theta_min         4.090
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.776
_exptl_absorpt_correction_T_max  0.66
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456.001
_exptl_crystal_size_max          0.430
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.29
_refine_ls_abs_structure_details 'Flack (1983), 2046 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.35(7)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         4446
_refine_ls_number_restraints     337
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.0001167
_refine_ls_shift/su_mean         0.0000119
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.182E+04 0.301E+04 0.176E+04 688. 160. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1600
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1600
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                2272
_reflns_number_total             4446
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.50
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0895
_oxford_refine_ls_scale          8.0(2)
_oxford_reflns_number_all        4446
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            cg4007394_si_002.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C25 H30.00 Cl1 N1 O3'
_cod_database_code               4508401
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE ENANTIO FIRST(X'S, U'S, OCC) UNTIL C(25) 
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) 
RIDE O(2,X'S) O(32,X'S) 
RIDE O(3,X'S) O(33,X'S) H(31,X'S) H(331,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) 
DELU 0.01 C(1) C(2) C(3) C(4) 
CONT C(5) C(6) C(7) C(8) AND 
CONT C(31) C(32) C(33) C(34) 
CONT C(35) C(36) C(37) C(38) 
SIMU 0.01 C(1) C(2) C(3) C(4) 
CONT C(5) C(6) C(7) C(8) AND 
CONT C(31) C(32) C(33) C(34) 
CONT C(35) C(36) C(37) C(38) 
DELU 0.01 C(9) C(10) C(11) C(12) C(13) C(14) AND 
CONT C(39) C(40) C(41) C(42) C(43) C(44) 
SIMU 0.01 C(9) C(10) C(11) C(12) C(13) C(14) AND 
CONT C(39) C(40) C(41) C(42) C(43) C(44) 
DELU 0.01 N(1) C(16) C(17) C(18) C(19) 
CONT C(22) C(23) C(24) C(25) AND 
CONT N(31) C(46) C(47) C(48) C(49) 
CONT C(52) C(53) C(54) C(55) 
SIMU 0.01 N(1) C(16) C(17) C(18) C(19) 
CONT C(22) C(23) C(24) C(25) AND 
CONT N(31) C(46) C(47) C(48) C(49) 
CONT C(52) C(53) C(54) C(55) 
REM DISTANCE 0.100000 , 0.030000 = C(9) TO C(39) 
DISTANCE 0.140000 , 0.030000 = N(1) TO N(31) 
DISTANCE 1.440000 , 0.030000 = C(13) TO C(14) 
DISTANCE 1.540000 , 0.003000 = N(1) TO C(25) 
DISTANCE 1.540000 , 0.003000 = C(22) TO C(23) 
DISTANCE 1.540000 , 0.003000 = C(23) TO C(24) 
DISTANCE 1.540000 , 0.003000 = C(24) TO C(25) 
DISTANCE 1.540000 , 0.030000 = C(17) TO C(18) 
DISTANCE 1.350000 , 0.03000 = C(2) TO O(3) 
REM DISTANCE 0.050000 , 0.030000 = C(2) TO C(32) 
PLANAR 0.010000  C(9) C(10) C(11) C(12) C(13) C(14) 
REM   SHIFTLIMIT   START (DO NOT REMOVE THIS LINE) 
REM   SHIFTLIMIT   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;