4-Benzyl-4-ethylmorpholin-1-ium hexafluorophosphate
Yang, Fang; Zang, Hongjun; Cheng, Bowen; Xu, Xianlin; Ren, Yuanlin; Acta Crystallographica Section E 68 (2012) o840–; doi:10.1107/S1600536812001006

data_2233978
_publ_section_title
;
 4-Benzyl-4-ethylmorpholin-1-ium hexafluorophosphate
;
_journal_coeditor_code           RZ2692
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o840
_journal_paper_doi               10.1107/S1600536812001006
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C13 H20 N O +, P F6 -'
_chemical_formula_moiety         'C13 H20 N O +, F6 P -'
_chemical_formula_sum            'C13 H20 F6 N O P'
_chemical_formula_weight         351.27
_chemical_name_systematic
;
4-Benzyl-4-ethylmorpholin-1-ium hexafluorophosphate
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            32
_cell_length_a                   26.054(3)
_cell_length_b                   28.528(3)
_cell_length_c                   16.2950(15)
_cell_measurement_reflns_used    11300
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      29.1
_cell_measurement_theta_min      2.1
_cell_volume                     12112(2)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure (Rigaku, 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39690
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.247
_exptl_absorpt_correction_T_max  0.9570
_exptl_absorpt_correction_T_min  0.9478
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku/MSC, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5824
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.235
_refine_ls_abs_structure_details 'Flack (1983), 3877 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.06(5)
_refine_ls_extinction_coef       0.00044(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         8072
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0336P)^2^+3.6844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                7799
_reflns_number_total             8072
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rz2692.cif
_cod_data_source_block           I
_cod_original_cell_volume        12111(2)
_cod_database_code               2233978
_cod_database_fobs_code          2233978