<i>rac</i>-4-[4-Cyano-2-(hydroxymethyl)phenyl]-4-(4-fluorophenyl)-4-hydroxy-<i>N</i>,<i>N</i>-dimethylbutanaminium hemifumarate
Wang, En-Ju; Chen, Guang-Ying; Acta Crystallographica Section E 67 (2011) o284–; doi:10.1107/S1600536810054346

data_2229270
_publ_section_title
;
 <i>rac</i>-4-[4-Cyano-2-(hydroxymethyl)phenyl]-4-(4-fluorophenyl)-4-hydroxy-<i>N</i>,<i>N</i>-dimethylbutanaminium
 hemifumarate
;
_journal_coeditor_code           XU5099
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o284
_journal_paper_doi               10.1107/S1600536810054346
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'C20 H24 F N2 O2 +, 0.5C4 H2 O4 2-'
_chemical_formula_moiety         'C20 H24 F N2 O2 +, 0.5(C4 H2 O4 2-)'
_chemical_formula_sum            'C22 H25 F N2 O4'
_chemical_formula_weight         400.44
_chemical_name_systematic
;
<i>rac</i>-4-[4-Cyano-2-(hydroxymethyl)phenyl]-4-(4-fluorophenyl)-4-hydroxy-
<i>N</i>,<i>N</i>-dimethylbutanaminium hemifumarate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.2360(10)
_cell_angle_beta                 102.681(2)
_cell_angle_gamma                107.508(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3312(9)
_cell_length_b                   8.8372(11)
_cell_length_c                   15.0396(13)
_cell_measurement_reflns_used    5256
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1.5
_cell_volume                     1023.64(19)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7766
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.47
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0681P)^2^+0.4116P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1386
_refine_ls_wR_factor_ref         0.1575
_reflns_number_gt                3071
_reflns_number_total             4381
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            xu5099.cif
_cod_data_source_block           I
_cod_database_code               2229270
_cod_database_fobs_code          2229270