1-[(4-Chlorobenzoyl)methyl]-4-(<i>N</i>,<i>N</i>-dimethylamino)pyridinium bromide sesquihydrate and 1-[(4-bromobenzoyl)methyl]-4-(<i>N</i>,<i>N</i>-dimethylamino)pyridinium bromide sesquihydrate
Sundar, T.V.; Parthasarathi, V.; Sarkunam, K.; Nallu, M.; Walfort, B.; Lang, H.; Acta Crystallographica Section C 60 (2004) o464–o466; doi:10.1107/S0108270104010923

data_2014223
_publ_section_title
;
 1-[(4-Chlorobenzoyl)methyl]-4-(<i>N</i>,<i>N</i>-dimethylamino)pyridinium
 bromide sesquihydrate and
 1-[(4-bromobenzoyl)methyl]-4-(<i>N</i>,<i>N</i>-dimethylamino)pyridinium
 bromide sesquihydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o464
_journal_page_last               o466
_journal_paper_doi               10.1107/S0108270104010923
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C15 H16 Br N2 O +, Br -, 1.5H2 O'
_chemical_formula_moiety         'C15 H16 Br N2 O +, Br -, 1.5H2 O'
_chemical_formula_sum            'C15 H19 Br2 N2 O2.5'
_chemical_formula_weight         427.14
_chemical_melting_point          512.5
_chemical_name_systematic
;
1-[(4-Bromobenzoyl)methyl]-4-(N,N-dimethylamino)pyridinium bromide
sesquihydrate
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.182(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.403(6)
_cell_length_b                   10.022(3)
_cell_length_c                   17.386(4)
_cell_measurement_reflns_used    873
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.38
_cell_measurement_theta_min      2.26
_cell_volume                     3499.1(17)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
'WinGX (Farrugia, 1999) and PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Smart 1K CCD'
_diffrn_measurement_method       '\w 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  0.0453
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            20471
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.642
_exptl_absorpt_correction_T_max  0.3365
_exptl_absorpt_correction_T_min  0.2582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Siemens, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.579
_refine_diff_density_min         -0.794
_refine_ls_extinction_coef       0.00162(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+3.7037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                2391
_reflns_number_total             3587
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1711.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '512.5 K' was changed to '512.5' -
the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '512.5 K' was changed to '512.5' -
the value should be numeric and without a unit
designator.

'_symmetry_cell_setting' value 'Monoclinic' changed to
'monoclinic' 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        3499.0(17)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C15 H19 Br2 N2 O2.50'
_cod_database_code               2014223
_cod_database_fobs_code          2014223