Strychninium <i>N</i>-phthaloyl-β-alaninate <i>N</i>-phthaloyl-β-alanine and brucinium <i>N</i>-phthaloyl-β-alaninate 5.67-hydrate
Agata Białońska; Zbigniew Ciunik; Acta Crystallographica Section C 62 (2006) o182–o185; doi:10.1107/S0108270106005555

data_2015243
_publ_section_title
;
 Strychninium <i>N</i>-phthaloyl-\b-alaninate
 <i>N</i>-phthaloyl-\b-alanine and brucinium
 <i>N</i>-phthaloyl-\b-alaninate 5.67-hydrate
;
_journal_coeditor_code           GD1431
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o182
_journal_page_last               o185
_journal_paper_doi               10.1107/S0108270106005555
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C23 H27 N2 O4 +, C11 H8 N O4 -, 5.67H2 O'
_chemical_formula_moiety         'C23 H27 N2 O4 +, C11 H8 N O4 -, 5.67H2 O'
_chemical_formula_sum            'C34 H46.34 N3 O13.67'
_chemical_formula_weight         715.80
_chemical_name_systematic
;
brucinium N-phthaloyl-\b-alaninate 5.67-hydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.832(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.527(2)
_cell_length_b                   7.6690(13)
_cell_length_c                   19.500(3)
_cell_measurement_reflns_used    10253
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      3.31
_cell_volume                     1717.7(5)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2001)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2001)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'SHELXTL-NT (Bruker, 1999)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       \w
_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  0.1135
_diffrn_reflns_av_sigmaI/netI    0.1661
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11409
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.31
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             761.4
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.276
_refine_ls_abs_structure_details
'from known structure (Toda <i>et al.</i>,  1985)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         3937
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.0776
_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^)+(0.0298P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.1143
_reflns_number_gt                2391
_reflns_number_total             3937
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd1431.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2015243
_cod_database_fobs_code          2015243