Tris(2-ethylammonio)amine–4-nitrobenzoate–water (1/3/2)
Daniel E. Lynch; Acta Crystallographica Section E 59 (2003) o1157–o1158; doi:10.1107/S1600536803015538

data_2202791
_publ_section_title
;
 Tris(2-ethylammonio)amine--4-nitrobenzoate--water (1/3/2)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1157
_journal_page_last               o1158
_journal_paper_doi               10.1107/S1600536803015538
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C6 H21 N4 3+, 3C7 H4 N O4 1-, 2H2 O'
_chemical_formula_moiety         'C6 H21 N4 3+, 3C7 H4 N O4 1-, 2H2 O'
_chemical_formula_sum            'C27 H37 N7 O14'
_chemical_formula_weight         683.64
_chemical_melting_point          457
_chemical_name_systematic
;
Tris(2-ethylammonio)amine--4-nitrobenzoate--water (2/6/4)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.758(5)
_cell_angle_beta                 99.715(6)
_cell_angle_gamma                105.898(7)
_cell_formula_units_Z            4
_cell_length_a                   14.0950(10)
_cell_length_b                   14.6970(10)
_cell_length_c                   17.1308(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      6
_cell_volume                     3209.5(4)
_computing_cell_refinement       MolEN
_computing_data_collection       'MolEN (Fair, 1990)'
_computing_data_reduction        'Xtal3.2 (Hall et al., 1992)'
_computing_molecular_graphics    'PLATON97 (Spek, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       2\q/\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  0.0106
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11786
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        15
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(Xtal3.2; Hall et al., 1992)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.333
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     922
_refine_ls_number_reflns         11286
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.1212
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1205P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.2056
_reflns_number_gt                5646
_reflns_number_total             11286
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6271.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-08-09

 Marking atoms 'O41W' and 'O42W' as belonging to disorder groups
 '1' and '2' of disorder assembly 'A' after consulting the original
 publication.

 Antanas Vaitkus,
 2017-08-09

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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:

'_chemical_melting_point' value '457 K' was changed to '457' - the
value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '457 K' was changed to '457' - the
value should be numeric and without a unit
designator.

'_symmetry_cell_setting' value 'Triclinic' changed to
'triclinic' 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        3209.5(3)
_cod_database_code               2202791
_cod_database_fobs_code          2202791