Dibrucinium sulfate heptahydrate
Agata Białońska; Zbigniew Ciunik; Acta Crystallographica Section E 61 (2005) o4222–o4224; doi:10.1107/S1600536805037451

data_2207635
_publ_section_title
;
 Dibrucinium sulfate heptahydrate
;
_journal_coeditor_code           SG6038
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4222
_journal_page_last               o4224
_journal_paper_doi               10.1107/S1600536805037451
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '2C23 H27 N2 O4 + , S1 O4 2- , 7H2 O'
_chemical_formula_moiety         '2C23 H27 N2 O4 + , O4 S1 2- , 7H2 O'
_chemical_formula_sum            'C46 H68 N4 O19 S'
_chemical_formula_weight         1013.10
_chemical_name_systematic
;
Dibrucinium sulfate heptahydrate
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 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                   12.1765(9)
_cell_length_b                   14.2518(10)
_cell_length_c                   26.6488(18)
_cell_measurement_reflns_used    5256
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.45
_cell_measurement_theta_min      3.67
_cell_volume                     4624.6(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, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Kuma KM4 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  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15405
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.67
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.22
_refine_diff_density_min         -0.27
_refine_ls_abs_structure_details 'Toda <i>et al.</i> (1985) and Flack (1983)'
_refine_ls_abs_structure_Flack   -0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.056
_refine_ls_R_factor_gt           0.047
_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^)+(0.043P)^2^+1.9728P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.091
_refine_ls_wR_factor_ref         0.094
_reflns_number_gt                4393
_reflns_number_total             4939
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg6038.cif
_cod_data_source_block           I
_cod_database_code               2207635
_cod_database_fobs_code          2207635