Tris(2-benzamidoethyl)ammonium tetrafluoroborate
Pilate, Marcy L.; Blount, Henry; Fronczek, Frank R.; Hossain, Md. Alamgir; Acta Crystallographica Section E 66 (2010) o1833–o1834; doi:10.1107/S1600536810024323

data_2226645
_publ_section_title
;
 Tris(2-benzamidoethyl)ammonium tetrafluoroborate
;
_journal_coeditor_code           RK2214
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1833
_journal_page_last               o1834
_journal_paper_doi               10.1107/S1600536810024323
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C27 H31 N4 O3 +, B F4 -'
_chemical_formula_moiety         'C27 H31 N4 O3 +, B F4 -'
_chemical_formula_sum            'C27 H31 B F4 N4 O3'
_chemical_formula_weight         546.37
_chemical_melting_point          423
_chemical_name_systematic
;
Tris(2-benzamidoethyl)ammonium tetrafluoroborate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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
_cell_angle_beta                 94.546(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.325(2)
_cell_length_b                   9.572(2)
_cell_length_c                   21.118(3)
_cell_measurement_reflns_used    6170
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.5
_cell_volume                     2685.1(8)
_computing_cell_refinement
;
<i>DENZO</i> and <i>SCALEPACK</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection       '<i>COLLECT</i> (Nonius, 1999)'
_computing_data_reduction
'<i>DENZO</i> and <i>SCALEPACK</i> (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    '<i>ORTEP-3</i> (Farrugia, 1997)'
_computing_publication_material  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_refinement  '<i>SHELXL97</i> (Sheldrick, 2008)'
_computing_structure_solution    '<i>SIR97</i> (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
'Nonius KappaCCD diffractometer with Oxford Cryostream'
_diffrn_measurement_method       ' \w--scans with \k--offsets'
_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  0.068
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31844
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         27.1
_diffrn_reflns_theta_min         2.6
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.266
_refine_ls_extinction_coef       0.0047(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '<i>SHELXL97</i> (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5914
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.117
_refine_ls_R_factor_gt           0.048
_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^)+(0.0492P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.093
_refine_ls_wR_factor_ref         0.114
_reflns_number_gt                3310
_reflns_number_total             5914
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2214.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2226645
_cod_database_fobs_code          2226645