Diethylenetriammonium oxonium naphthalene-1,6-disulfonate 3.5-hydrate
Zhi-Min Jin; Li Li; Li-Zhao Chen; Ling-Su Li; Mao-Lin Hu; Acta Crystallographica Section E 61 (2005) o4325–o4327; doi:10.1107/S1600536805038766

data_2207434
_publ_section_title
;
 Diethylenetriammonium oxonium naphthalene-1,6-disulfonate 3.5-hydrate
;
_journal_coeditor_code           BD6015
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4325
_journal_page_last               o4327
_journal_paper_doi               10.1107/S1600536805038766
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'C4 H16 N3 3+, H3 O +, 2C10 H6 O6 S2 2-, 3.5H2 O'
_chemical_formula_moiety
'C4 H16 N3 3+, H3 O +, 2C10 H6 O6 S2 2-, 3.5H2 O'
_chemical_formula_sum            'C24 H38 N3 O16.5 S4'
_chemical_formula_weight         760.85
_chemical_name_systematic
;
Diethylenetriammonium oxonium naphthalene-1,6-disulfonate 3.5-hydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 96.011(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.392(2)
_cell_length_b                   13.1747(11)
_cell_length_c                   19.5144(16)
_cell_measurement_reflns_used    1109
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      18.06
_cell_measurement_theta_min      2.15
_cell_volume                     6492.3(9)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0302
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16963
_diffrn_reflns_theta_full        25.21
_diffrn_reflns_theta_max         25.21
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3192
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.814
_refine_diff_density_min         -0.556
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     464
_refine_ls_number_reflns         5848
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0722P)^2^+13.0061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1470
_reflns_number_gt                4933
_reflns_number_total             5848
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bd6015.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6492.2(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2207434
_cod_database_fobs_code          2207434