Application and Comparison of Cocrystallization Techniques on Trospium Chloride Cocrystals
Sládková, Veronika; Cibulková, Jana; Eigner, Václav; Šturc, Antonín; Kratochvíl, Bohumil; Rohlíček, Jan; Crystal Growth & Design 14 (2014) 2931–; doi:10.1021/cg500226z

data_4510822
_publ_section_title
;
 Application and Comparison of Cocrystallization Techniques on Trospium
 Chloride Cocrystals
;
_journal_issue                   6
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2931
_journal_paper_doi               10.1021/cg500226z
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         '2(C25 H30 N O3), C2 H2 O4, 2Cl'
_chemical_formula_sum            'C52 H62 Cl2 N2 O10'
_chemical_formula_weight         945.98
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 99.7909(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.4462(7)
_cell_length_b                   6.61949(10)
_cell_length_c                   16.5083(2)
_cell_measurement_reflns_used    16642
_cell_measurement_temperature    190
_cell_measurement_theta_max      77
_cell_measurement_theta_min      5
_cell_volume                     4678.50(12)
_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_pressure         101
_diffrn_ambient_temperature      190
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -54
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30810
_diffrn_reflns_theta_full        75.704
_diffrn_reflns_theta_max         77.249
_diffrn_reflns_theta_min         5.439
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.760
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plane
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.533
_exptl_crystal_size_mid          0.407
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.29
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4939
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.0014079
_refine_ls_shift/su_mean         0.0000612
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.10P)^2^ + 1.58P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1221
_refine_ls_wR_factor_gt          0.1174
_refine_ls_wR_factor_ref         0.1221
_reflns_limit_h_max              53
_reflns_limit_h_min              -54
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              0
_reflns_number_gt                4512
_reflns_number_total             4939
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.36
_oxford_diffrn_Wilson_scale      0.07
_oxford_refine_ls_r_factor_ref   0.0428
_oxford_refine_ls_scale          2.22(2)
_oxford_reflns_number_all        4939
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            cg500226z_si_001.cif
_cod_data_source_block           VS_TCl_Stav
_cod_depositor_comments
'Adding full bibliography for 4510821--4510824.cif.'
_cod_original_cell_volume        4678.51(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4510822
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) H   ( 162,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 182,X'S) H   ( 181,X'S) 
RIDE C   (  19,X'S) H   ( 192,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) 
RIDE C   (  21,X'S) H   ( 212,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) H   ( 222,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) H   ( 232,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) H   ( 242,X'S) 
RIDE C   (  25,X'S) H   ( 252,X'S) H   ( 251,X'S) 
RIDE O   (  31,X'S) H   ( 311,X'S) 
RIDE O   (   3,X'S) H   (  31,X'S) 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;