Isomorphous brucinium 4-nitrobenzoate methanol solvate and brucinium 4-nitrobenzoate dihydrate
Agata Białońska; Zbigniew Ciunik; Acta Crystallographica Section C 63 (2007) o120–o122; doi:10.1107/S010827010605517X

data_2015792
_publ_section_title
;
 Isomorphous brucinium 4-nitrobenzoate methanol solvate and brucinium
 4-nitrobenzoate dihydrate
;
_journal_coeditor_code           GD3069
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o120
_journal_page_last               o122
_journal_paper_doi               10.1107/S010827010605517X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C23 H27 N2 O4 +, C7 H4 N O4 -, 2H2 O'
_chemical_formula_moiety         'C23 H27 N2 O4 +, C7 H4 N O4 -, 2(H2 O)'
_chemical_formula_sum            'C30 H35 N3 O10'
_chemical_formula_weight         597.61
_chemical_name_systematic
;
brucinium 4-nitrobenzoate dihydrate
;
_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                 108.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.085(2)
_cell_length_b                   12.338(3)
_cell_length_c                   11.615(3)
_cell_measurement_reflns_used    7856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      3.63
_cell_volume                     1369.7(6)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9184
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.63
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.110
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.199
_refine_ls_abs_structure_details
;
Toda <i>et al.</i> (1985)
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         3110
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0521P)^2^+0.1159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0781
_reflns_number_gt                2925
_reflns_number_total             3110
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gd3069.cif
_cod_data_source_block           II
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2015792
_cod_database_fobs_code          2015792