Brucinium hydrogen <i>N</i>-(4-nitrobenzoyl)-<small>L</small>-aspartate dihydrate
Agata Białońska; Zbigniew Ciunik; Acta Crystallographica Section E 63 (2007) o2002–o2004; doi:10.1107/S1600536807013244

data_2212920
_publ_section_title
;
 Brucinium hydrogen
 <i>N</i>-(4-nitrobenzoyl)-<small>L</small>-aspartate dihydrate
;
_journal_coeditor_code           HG2210
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2002
_journal_page_last               o2004
_journal_paper_doi               10.1107/S1600536807013244
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C23 H27 N2 O4 + , C11 H9 N2 O7 - , 2H2 O'
_chemical_formula_moiety         'C23 H27 N2 O4 + , C11 H9 N2 O7 - , 2H2 O'
_chemical_formula_sum            'C34 H40 N4 O13'
_chemical_formula_weight         712.70
_chemical_melting_point          .446E-305
_chemical_name_systematic
;
Brucinium hydrogen N-(4-nitrobenzoyl)-L-aspartate dihydrate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.435(2)
_cell_length_b                   12.168(3)
_cell_length_c                   35.664(4)
_cell_measurement_reflns_used    12256
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      3.40
_cell_volume                     3226.5(12)
_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) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Kuma KM-4 CCD area-detector'
_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  0.1172
_diffrn_reflns_av_sigmaI/netI    0.0921
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            20076
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         3.40
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.275
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         3595
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1242
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0915P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1702
_refine_ls_wR_factor_ref         0.1932
_reflns_number_gt                2569
_reflns_number_total             3595
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2210.cif
_cod_data_source_block           I
_cod_database_code               2212920
_cod_database_fobs_code          2212920