Pergolide mesylate form II
Jegorov, Alexandr; Horák, Zdeněk; Čejka, Jan; Kratochvíl, Bohumil; Císařová, Ivana; Acta Crystallographica Section C 59 (2003) o575–o576; doi:10.1107/S0108270103017499

data_2013672
_publ_section_title
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 Pergolide mesylate form II
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o575
_journal_page_last               o576
_journal_paper_doi               10.1107/S0108270103017499
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C19 H27 N2 S 1+, C H3 O3 S 1-'
_chemical_formula_moiety         'C19 H27 N2 S 1+, C H3 O3 S 1-'
_chemical_formula_sum            'C20 H30 N2 O3 S2'
_chemical_formula_weight         410.60
_chemical_name_common            'Pergolide mesylate'
_chemical_name_systematic
;
8\b-[(methylsulfanyl)methyl]-6-propylergolinium methanesulfonate
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   8.8510(2)
_cell_length_b                   8.8510(2)
_cell_length_c                   44.8860(8)
_cell_measurement_reflns_used    4009
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      1.02
_cell_volume                     3045.27(11)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        DENZO/SCALEPACK
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement  'CRYSTALS (Watkin et al., 2001)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            7908
_diffrn_reflns_theta_full        26.019
_diffrn_reflns_theta_max         26.019
_diffrn_reflns_theta_min         1.361
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  1.00
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.23
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1514
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         1937
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.000375
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Prince modified Chebychev polynomial (Watkin, 1994);
W = [weight][1-(\dF/6\sF)^2]^2, with 0.551, 0.377 and 0.369
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0413
_refine_ls_wR_factor_gt          0.0343
_refine_ls_wR_factor_ref         0.0343
_reflns_number_gt                1937
_reflns_number_total             2389
_reflns_threshold_expression     I>1.96\s(I)
_cod_data_source_file            sk1650.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               2013672
_cod_database_fobs_code          2013672