Chiral drug timolol maleate as a continuous solid solution: Thermochemical and single crystal X-ray evidence
Bredikhin, Alexander A.; Bredikhina, Zemfira A.; Zakharychev, Dmitry V.; Gubaidullin, Aidar T.; Fayzullin, Robert R.; CrystEngComm 14 (2012) 648–; doi:10.1039/c1ce05850a

data_7207042
_publ_section_title
;
 Chiral drug timolol maleate as a continuous solid solution:
 Thermochemical and single crystal X-ray evidence
;
_journal_issue                   2
_journal_name_full               CrystEngComm
_journal_page_first              648
_journal_paper_doi               10.1039/c1ce05850a
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C13 H25 N4 O3 S, C4 H3 O4'
_chemical_formula_sum            'C17 H28 N4 O7 S'
_chemical_formula_weight         432.49
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                72.634(6)
_cell_angle_beta                 74.208(5)
_cell_angle_gamma                62.075(5)
_cell_formula_units_Z            2
_cell_length_a                   9.545(4)
_cell_length_b                   10.223(3)
_cell_length_c                   13.408(6)
_cell_measurement_reflns_used    1064
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.20
_cell_measurement_theta_min      2.30
_cell_volume                     1089.6(7)
_computing_cell_refinement       'APEX2 v2008.6-1 (Bruker AXS)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT V7.34A (Bruker AXS, 2006)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_sigmaI/netI    0.1096
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8906
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_T_max  0.9962
_exptl_absorpt_correction_T_min  0.9426
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
G.M. Sheldrick (1998a). SADABS v.2.01, Bruker.
Siemens Area Detector Absorption Correction Program.
Bruker AXS. Madison. Wisconsin. USA
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       0.0045(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         3752
_refine_ls_number_restraints     368
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1652
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0825
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                1493
_reflns_number_total             3752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05850a.txt
_cod_data_source_block           rac_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        1089.5(7)
_cod_database_code               7207042