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_2015793
_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_moiety         'C23 H27 N2 O4, C7 H4 N O4, 2.6(H2 O)'
_chemical_formula_sum            'C30 H36.2 N3 O10.6'
_chemical_formula_weight         608.42
_chemical_name_systematic
;
brucinium 4-nitrobenzoate 2.6 hydrate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.075(2)
_cell_length_b                   12.464(2)
_cell_length_c                   29.994(3)
_cell_measurement_reflns_used    15622
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      3.30
_cell_volume                     3018.8(9)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Kuma KM-4 CCD'
_diffrn_measurement_method       '\w scan'
_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  0.0760
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            20212
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.30
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.289
_refine_ls_abs_structure_details
;
Toda, F., Tanaka, K., Ueda, H. and Oshima, T. (1985).
Isr. J. Chem., 25, 338-345.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         3716
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0882
_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^)+(0.1818P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2387
_refine_ls_wR_factor_ref         0.2613
_reflns_number_gt                2840
_reflns_number_total             3716
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            gd3069.cif
_cod_data_source_block           supplement
_cod_original_formula_sum        'C30 H36.20 N3 O10.60'
_cod_database_code               2015793
_cod_database_fobs_code          2015793