Poly[[μ-(1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonato)]sodium]: a powder X-ray diffraction study
Rukiah, Mwaffak; Assaad, Thaer; Acta Crystallographica Section C 69 (2013) 815–818; doi:10.1107/S0108270113016491

data_2019096
_publ_section_title
;
 Poly[[\m-(1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonato)]sodium]: a
 powder X-ray diffraction study
;
_journal_coeditor_code           SK3495
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              815
_journal_page_last               818
_journal_paper_doi               10.1107/S0108270113016491
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Na (C2 H8 N O6 P2)]'
_chemical_formula_moiety         'C2 H8 N Na O6 P2'
_chemical_formula_sum            'C2 H8 N Na O6 P2'
_chemical_formula_weight         227.02
_chemical_melting_point          551
_chemical_name_systematic
;
Poly[[\m-(1-azaniumylethane-1,1-diyl)bis(hydrogen phosphonato)]sodium]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                98.086(2)
_cell_angle_beta                 102.0847(16)
_cell_angle_gamma                101.4987(19)
_cell_formula_units_Z            2
_cell_length_a                   5.53651(11)
_cell_length_b                   8.1058(3)
_cell_length_c                   9.1108(2)
_cell_measurement_temperature    298
_cell_volume                     384.624(19)
_computing_cell_refinement       'GSAS (Larson & Von Dreele, 2004)'
_computing_data_collection       'WinXPOW (Stoe & Cie, 1999)'
_computing_data_reduction        'WinXPOW (Stoe & Cie, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'publCIF  (Westrip, 2010)'
_computing_structure_refinement  'GSAS (Larson & Von Dreele, 2004)'
_computing_structure_solution    'EXPO2009 (Altomare <i>et al.</i>, 2009)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Stoe STADI P'
_diffrn_radiation_monochromator  'Ge (111)'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.5406
_exptl_absorpt_coefficient_mu    5.763
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
[GSAS absorption/surface roughness correction (Larson & Von Dreele,
2004):
function number 4; flat plate in transmission mode, absorbtion correction
term (\m.d) not refined]
;
_exptl_crystal_density_diffrn    1.96
_exptl_crystal_F_000             232
_pd_calc_method                  'Rietveld refinement'
_pd_char_colour                  white
_pd_char_particle_morphology     'Fine powder'
_pd_instr_dist_mono/spec         130
_pd_instr_dist_spec/detc         173
_pd_instr_dist_src/mono          260
_pd_instr_location
;
Chemistry Department
Atomic Energy Commission
Damascus
PO Box 6091
Syrian Arab Republic
;
_pd_meas_2theta_range_inc        0.02
_pd_meas_2theta_range_max        84.98
_pd_meas_2theta_range_min        5.0
_pd_meas_number_of_points        4000
_pd_meas_scan_method             step
_pd_phase_name                   EHDP2-Na
_pd_prep_pressure                101.3
_pd_prep_temperature             298
_pd_proc_2theta_range_inc        0.02
_pd_proc_2theta_range_max        85
_pd_proc_2theta_range_min        5.0
_pd_proc_info_data_reduction     none
_pd_proc_info_datetime           2013-03-17T12:06:51
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function
'shifted Chebyshev polynomial with 20 coefficients.'
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_ls_pref_orient_corr     'spherical harmonics correction'
_pd_proc_ls_profile_function
;
pseudo-Voigt function of the peak shape for angle-dependent asymmetry with
axial divergence
;
_pd_proc_ls_prof_R_factor        0.0227
_pd_proc_ls_prof_wR_expected     0.0223
_pd_proc_ls_prof_wR_factor       0.0304
_pd_proc_number_of_points        4000
_pd_spec_mounting                'powder loaded between two Mylar foils'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              8
_pd_spec_size_equat              8
_refine_diff_density_max         0.149
_refine_diff_density_min         -0.137
_refine_ls_goodness_of_fit_all   1.38
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    3
_refine_ls_number_parameters     112
_refine_ls_number_restraints     2
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.00
_reflns_number_total             542
_cod_data_source_file            sk3495.cif
_cod_data_source_block           I
_cod_original_cell_volume        384.622(19)
_cod_database_code               2019096