Poly[[μ-(1-ammonioethane-1,1-diyl)bis(hydrogenphosphonato)]diaquachloridodisodium]: a powder X-ray diffraction study
Rukiah, Mwaffak; Assaad, Thaer; Acta Crystallographica Section E 68 (2012) m699–m700; doi:10.1107/S1600536812018077

data_2234837
_publ_section_title
;
 Poly[[\m-(1-ammonioethane-1,1-diyl)bis(hydrogenphosphonato)]diaquachloridodisodium]:
 a powder X-ray diffraction study
;
_journal_coeditor_code           WM2620
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m699
_journal_page_last               m700
_journal_paper_doi               10.1107/S1600536812018077
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Na2 (C2 H8 N O6 P2) Cl (H2 O)2]'
_chemical_formula_moiety         'C2 H12 Cl N Na2 O8 P2'
_chemical_formula_sum            'C2 H12 Cl N Na2 O8 P2'
_chemical_formula_weight         321.50
_chemical_melting_point          623
_chemical_name_systematic
;
Poly[[\m-(1-ammonioethane-1,1-
diyl)bis(hydrogenphosphonato)]diaquachloridodisodium]
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 104.0764(7)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   5.53806(4)
_cell_length_b                   10.50365(8)
_cell_length_c                   10.20960(10)
_cell_measurement_temperature    298
_cell_volume                     576.058(8)
_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, 1997)'
_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 Transmission STADI P'
_diffrn_radiation_monochromator  'curved Ge(111)'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.5406
_exptl_absorpt_coefficient_mu    6.622
_exptl_absorpt_correction_T_max  0.4509
_exptl_absorpt_correction_T_min  0.3180
_exptl_absorpt_correction_type   cylinder
_exptl_absorpt_process_details
;
Absorption/surface roughness correction: function number 4
in GSAS (Larson & Von Dreele, 2004).
Flat plate transmission absorption correction,
terms =     0.51550         0.0000,
correction is not refined.
;
_exptl_crystal_density_diffrn    1.854
_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
 P.O.Box 6091
 Syrian Arab Republic
;
_pd_meas_2theta_range_inc        0.02
_pd_meas_2theta_range_max        91.98
_pd_meas_2theta_range_min        7.00
_pd_meas_number_of_points        4250
_pd_meas_scan_method             step
_pd_phase_name                   EHDP2-1
_pd_prep_pressure                101.3
_pd_prep_temperature             298
_pd_proc_2theta_range_inc        0.02
_pd_proc_2theta_range_max        91.98
_pd_proc_2theta_range_min        7.00
_pd_proc_info_data_reduction     none
_pd_proc_info_datetime           2012-02-01T10:47:00
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 20 terms.
 Shifted Chebyshev function of 1st kind
      1:    914.240     2:   -1034.48     3:    577.328     4:   -206.578
      5:    31.4580     6:    15.1650     7:   -17.0889     8:   0.311333
      9:    15.3490    10:   -12.5113    11:    3.19417    12:    9.78413
     13:   -11.5493    14:    7.63897    15:  -0.448352    16:   -4.70971
     17:    6.05628    18:   -4.89696    19:    6.60474    20:   -2.48023
;
_pd_proc_ls_peak_cutoff          0.00100
_pd_proc_ls_pref_orient_corr
;
March-Dollase
AXIS  1 Ratio=   1.12753  h= 0.000  k= 0.000  l= 1.000
Prefered orientation correction range: Min=   0.69761, Max=   1.19727
;
_pd_proc_ls_profile_function
;
CW Profile function number 4 with 21 terms
Pseudovoigt profile coefficients as parameterized in Thompson <i>et al.</i>
(1987)
Asymmetry correction of Finger <i>et al.</i> (1994).
Microstrain broadening by Stephens (1999).
Peak tails are ignored  where the intensity is below 0.0010 times the peak
  Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0286
_pd_proc_ls_prof_wR_expected     0.0293
_pd_proc_ls_prof_wR_factor       0.0383
_pd_proc_number_of_points        4250
_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
_pd_spec_size_thick              0.1
_refine_diff_density_max         0.177
_refine_diff_density_min         -0.162
_refine_ls_goodness_of_fit_all   1.33
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     109
_refine_ls_number_restraints     10
_refine_ls_shift/su_max          0.08
_refine_ls_shift/su_mean         0.00
_reflns_number_total             525
_cod_data_source_file            wm2620.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2234837