4-(9,10-Dihydro-4<i>H</i>-benzo[4,5]cyclohepta[1,2-<i>b</i>]thien-4-ylidene)-1-methylpiperidinium Hydrogen Malate
Peeters, O. M.; Blaton, N. M.; De Ranter, C. J.; Acta Crystallographica Section C 51 (1995) 1435–1438; doi:10.1107/S0108270194015088

data_2003713
_publ_section_title
;4-(9,10-Dihydro-4<i>H</i>-benzo[4,5]cyclohepta[1,2-<i>b</i>]thien-4-ylidene)-1-methylpiperidinium
 Hydrogen Malate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1435
_journal_page_last               1438
_journal_paper_doi               10.1107/S0108270194015088
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source
'Janssen Research Foundation, Beerse, Belgium'
_chemical_formula_moiety         'C19 H22 N1 S1 1+, C4 H5 O5 1-'
_chemical_formula_sum            'C23 H27 N O5 S'
_chemical_formula_weight         429.52
_chemical_name_systematic
;
4-(9,10-Dihydro-4H-benzo[4,5]cyclohepta[1,2-b]thien-4-ylidene)-
1-methylpiperidinium hydrogen malate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2bc 2ac'
_symmetry_space_group_name_H-M   'P c a b'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.973(1)
_cell_length_b                   17.101(2)
_cell_length_c                   25.496(3)
_cell_measurement_radiation      CuK\a
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_measurement_wavelength     1.54184
_cell_volume                     4348.3(8)
_computing_cell_refinement       'XRAY76 (Stewart et al., 1976)'
_computing_data_collection       'Y290 (Hilger & Watts, 1969)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992)'
_computing_molecular_graphics    'ORTEX2.1 (McArdle, 1994)'
_computing_publication_material  'PARST (Nardelli, 1983a)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1992)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device
'Hilger & Watts four-circle diffractometer   '
_diffrn_measurement_method       '\w/2\q scan                             '
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  .0743
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            5220
_diffrn_reflns_theta_max         56.99
_diffrn_standards_decay_%        <3.0
_diffrn_standards_interval_count 50
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    1.610
_exptl_absorpt_correction_T_max  .968
_exptl_absorpt_correction_T_min  .757
_exptl_absorpt_correction_type   'empirical (North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      1.306
_exptl_crystal_density_method    'flotation in n-heptane/CCl~4~'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          .47
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .05
_refine_diff_density_max         .17
_refine_diff_density_min         -.20
_refine_ls_extinction_coef       .00021(3)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.136
_refine_ls_goodness_of_fit_obs   1.415
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         2773
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          .1952
_refine_ls_R_factor_obs          .0561
_refine_ls_shift/esd_max         .085
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.044P)^2^]  where P = (Fo^2^ + 2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .1411
_refine_ls_wR_factor_obs         .0909
_reflns_number_observed          985
_reflns_number_total             2773
_reflns_observed_criterion       '> 3.0 sigma(F^2^)'
_cod_data_source_file            na1139.cif
_cod_data_source_block           Y
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '
w = 1/[\s^2^(Fo^2^) + (0.044P)^2^] where P = (Fo^2^ + 2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^) +
(0.044P)^2^] where P = (Fo^2^ + 2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4348.4(8)
_cod_original_sg_symbol_Hall     '-P 2bc -2ac'
_cod_original_formula_sum        'C23 H27 N1 O5 S1 '
_cod_database_code               2003713