Brucinium 3,5-dinitrobenzoate methanol solvate, methanol disolvate and trihydrate
Agata Białońska; Zbigniew Ciunik; Acta Crystallographica Section C 62 (2006) o450–o453; doi:10.1107/S0108270106021068

data_2015491
_publ_section_title
;
 Brucinium 3,5-dinitrobenzoate methanol solvate, methanol disolvate and
 trihydrate
;
_journal_coeditor_code           GG3018
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o450
_journal_page_last               o453
_journal_paper_doi               10.1107/S0108270106021068
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C23 H27 N2 O4 +, C7 H3 N2 O6 -, 3H2 O'
_chemical_formula_moiety         'C23 H27 N2 O4 +, C7 H3 N2 O6 -, 3H2 O'
_chemical_formula_sum            'C30 H36 N4 O13'
_chemical_formula_weight         660.63
_chemical_name_systematic
;
brucinium 3,5-dinitrobenzoate trihydrate
;
_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                   8.2499(8)
_cell_length_b                   12.5379(12)
_cell_length_c                   29.109(3)
_cell_measurement_reflns_used    18822
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.54
_cell_measurement_theta_min      3.54
_cell_volume                     3010.9(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0695
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            20148
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.247
_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   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         3700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0633P)^2^+0.1372P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1266
_reflns_number_gt                3036
_reflns_number_total             3700
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3018.cif
_cod_data_source_block           III
_cod_database_code               2015491