Three-dimensional hydrogen-bonded framework structures in flunarizinium nicotinate and flunarizinediium bis(4-toluenesulfonate) dihydrate
Kavitha, Channappa N.; Yathirajan, Hemmige S.; Kaur, Manpreet; Hosten, Eric C.; Betz, Richard; Glidewell, Christopher; Acta Crystallographica Section C 70 (2014) –; doi:10.1107/S2053229614016532

data_2019633
_publ_section_title
;
 Three-dimensional hydrogen-bonded framework structures in flunarizinium
 nicotinate and flunarizinediium bis(4-toluenesulfonate) dihydrate
;
_journal_coeditor_code           SK3553
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229614016532
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C26 H28 F2 N2 2+ , 2C7 H7 O3 S - , 2H2 O'
_chemical_formula_moiety         'C26 H28 F2 N2 2+, 2(C7 H7 O3 S -), 2H2 O'
_chemical_formula_sum            'C40 H46 F2 N2 O8 S2'
_chemical_formula_weight         784.91
_chemical_name_common
;
Flunarizinediium bis(4-toluenesulfonate) dihydrate
;
_chemical_name_systematic
;
1-[Bis(4-fluorophenyl)methyl]-4-[(2<i>E</i>)-3-phenylprop-2-en-1-\
yl]piperazine-1,4-diium  bis(4-methylbenzenesulfonate) dihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL2014
_cell_angle_alpha                90
_cell_angle_beta                 106.497(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0546(5)
_cell_length_b                   14.8338(6)
_cell_length_c                   26.9437(12)
_cell_measurement_reflns_used    9580
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      1.58
_cell_volume                     3853.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2010)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2010)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2014) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            45646
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.550
_diffrn_reflns_theta_min         2.091
_exptl_absorpt_coefficient_mu    0.203
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.592
_exptl_crystal_size_mid          0.432
_exptl_crystal_size_min          0.237
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.604
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         7212
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0731P)^2^+8.0533P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1952
_refine_ls_wR_factor_ref         0.2019
_reflns_number_gt                6219
_reflns_number_total             7212
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3553sup1.cif
_cod_data_source_block           II
_cod_database_code               2019633
_cod_database_fobs_code          2019633
_shelx_estimated_absorpt_t_min   0.889
_shelx_estimated_absorpt_t_max   0.953
_shelx_hkl_checksum              45455
_shelx_res_checksum              24616
_shelxl_version_number           2.014