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_2019632
_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 H27 F2 N2 , C6 H4 N O2'
_chemical_formula_moiety         'C26 H27 F2 N2, C6 H4 N O2'
_chemical_formula_sum            'C32 H31 F2 N3 O2'
_chemical_formula_weight         527.60
_chemical_name_common
;
Flunarizinium nicotinate
;
_chemical_name_systematic
'4-Bis[(4-fluorophenyl)methyl]-1-[(2<i>E</i>)-3-phenylprop-2-en-1-yl]piperazin-1-ium pyridine-3-carboxylate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL2014
_cell_angle_alpha                90
_cell_angle_beta                 92.717(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8536(4)
_cell_length_b                   10.8103(4)
_cell_length_c                   11.3901(4)
_cell_measurement_reflns_used    6092
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      1.88
_cell_volume                     1334.91(8)
_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 0.996
_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  0.0269
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23278
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.349
_diffrn_reflns_theta_min         1.878
_exptl_absorpt_coefficient_mu    0.092
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       plate
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.539
_exptl_crystal_size_mid          0.494
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.181
_refine_ls_abs_structure_details
;
Flack <i>x</i> parameter (Flack, 1983) determined using 2539 quotients
[(I+)-(I-)]/[(I+)+(I-)] (Parsons <i>et al.</i>, 2013)
;
_refine_ls_abs_structure_Flack   0.10(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6092
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.1632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0807
_reflns_number_gt                5770
_reflns_number_total             6092
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3553sup1.cif
_cod_data_source_block           I
_cod_database_code               2019632
_cod_database_fobs_code          2019632
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.988
_shelx_hkl_checksum              82726
_shelx_res_checksum              41167
_shelxl_version_number           2.014