Hydrogen Bonding in Two Forms of Bis(diethylenetriammonium) Trioxalate Tetrahydrate
Barnes, John C.; Weakley, Timothy J.R.; Acta Crystallographica Section C 54 (1998) IUC9800025–; doi:10.1107/S0108270198099612

data_2007372
_publ_section_title
;
 Hydrogen Bonding in Two Forms of Bis(diethylenetriammonium) Trioxalate
 Tetrahydrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9800025
_journal_paper_doi               10.1107/S0108270198099612
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         '2(C4 H16 N3 3+), 3(C2 O4 2-), 4(H2 O)'
_chemical_formula_sum            'C14 H40 N6 O16'
_chemical_formula_weight         548.52
_chemical_name_systematic
;
 Diethylenetriammonium oxalate hydrate (2:3:4)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                66.011(9)
_cell_angle_beta                 72.016(9)
_cell_angle_gamma                86.618(10)
_cell_formula_units_Z            1
_cell_length_a                   8.5553(11)
_cell_length_b                   9.2494(11)
_cell_length_c                   9.3431(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      14
_cell_volume                     640.58(14)
_computing_cell_refinement       'CAD4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Woclado, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(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       \w--2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0085
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2405
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             294
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0604P)^2^+0.2535P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                1733
_reflns_number_total             2242
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            qb0014.cif
_cod_data_source_block           jcb14bI
_cod_depositor_comments
;

2019-10-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        640.58(12)
_cod_original_formula_moiety     'C4 H16 N3 3+, 1.5C2 O4 2-, 2H2 O'
_cod_original_formula_sum        'C7 H20 N3 O8'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     274.26
_cod_database_code               2007372