On the crystal structures and phase transitions of hydrates in the binary dimethyl sulfoxide–water system
Fortes, A. D.; Ponsonby, J.; Kirichek, O.; García-Sakai, V.; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620008999

data_2108651
_publ_section_title
;
 On the crystal structures and phase transitions of hydrates in the binary
 dimethyl sulfoxide--water system
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620008999
_journal_volume                  76
_journal_year                    2020
_chemical_formula_moiety         'C2 D6 O S, 3(D2 O)'
_chemical_formula_sum            'C2 D12 O4 S'
_chemical_formula_weight         144.25
_chemical_melting_point          211
_chemical_name_common            'dimethyl sulfoxide trihydrate'
_chemical_name_systematic        'hexadeutero-dimethyl sulfoxide trideuterate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_audit_creation_date             2020-04-28T15:03
_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_update_record
' 2020-04-28T15:03  Initial CIF as created by GSAS2CIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 101.50300(20)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   10.266194(30)
_cell_length_b                   7.011130(21)
_cell_length_c                   10.068968(29)
_cell_measurement_temperature    195
_cell_volume                     710.183(4)
_computing_data_collection       'HRPD DAE3, IBEX'
_computing_data_reduction
'Mantid (Arnold <i>et al</i>., 2014: Mantid, 2013)'
_computing_molecular_graphics    'Diamond (Putz & Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  GSAS
_computing_structure_solution    'FOX Free Objects for Crystallography'
_diffrn_ambient_pressure         10
_diffrn_ambient_temperature      195
_diffrn_measurement_device_type
'HRPD, High Resolution Neutron Powder Diffractometer'
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           'white beam'
_diffrn_radiation_wavelength     0.5-8.2
_diffrn_source                   'spallation source'
_diffrn_source_type              'ISIS TS1 beamline HRPD'
_exptl_absorpt_correction_T_max  0.83333
_exptl_absorpt_correction_T_min  0.51486
_exptl_absorpt_process_details
;   GSAS Absorption/surface roughness correction: function number 1
 Linear absorption correction
Term =     0.12743    
Correction is refined.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.3491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_recrystallization_method
'Devitrification of LN2-quenched amorphous solid'
_pd_block_id                     2020-04-28T15:03|DMSO_TRIHYDRATE|Fortes|HRPD
_pd_calc_method                  'Rietveld Refinement'
_pd_char_colour                  colourless
_pd_char_particle_morphology     'fine powder'
_pd_instr_dist_spec/detc         965
_pd_instr_dist_src/spec          95000
_pd_instr_location
;
High Resolution Powder Diffractometer, ISIS neutron spallation source,
 Rutherford Appleton Laboratory, Oxfordshire, U.K.
;
_pd_meas_2theta_fixed            168.33
_pd_meas_number_of_points        4610
_pd_meas_scan_method             tof
_pd_phase_name                   'DMSO-d6 trideuterate'
_pd_prep_pressure                100
_pd_prep_temperature             80
_pd_proc_info_data_reduction
'Incident-beam normalisation and instrumental efficiency correction'
_pd_proc_info_datetime           2020-04-28T15:03:10
_pd_proc_info_excluded_regions
;
Between 39.884 and 40.088 ms to remove a small prompt-pulse artefact. Between
 102.815 and 103.309 ms to remove a small isolated vanadium peak due to the CCR
 tail.
;
_pd_proc_ls_background_function
;   GSAS Background function number 1 with 12 terms.
 Shifted Chebyshev function of 1st kind
      1:    4.23683     2:  -9.935880E-02 3:  -5.649680E-02 4:  -0.135816    
      5:  -0.203796     6:   7.670750E-02 7:  -5.766730E-02 8:   3.895410E-02
      9:  -5.290950E-0210:   2.903560E-0211:  -1.609620E-0212:  -2.338790E-02
;
_pd_proc_ls_peak_cutoff          0.00050
_pd_proc_ls_profile_function
;
 TOF Profile function number 3 with  21 terms
 Profile coefficients for exponential pseudovoigt
  convolution Von Dreele, 1990 (unpublished)
 (\a) = 0.2466, (\b~0~) = 0.026586, (\b~1~) = 0.007428,
 (\s~0~) = 0, (\s~1~) = 270.3, (\s~2~) = 3.8,
 (\g~0~) = 0, (\g~1~) = 0, (\g~2~) = 0,
 (\g~2s~) = 0, (\g~1e~) = 0, (\g~2e~) = 0,
 (\e~i~) = 0, (\e~a~) = 0, (\e~A~) = 0,
 (\g~11~) = 0.162, (\g~22~) = 0.260, (\g~33~) = 0.139,
 (\g~12~) = -0.075, (\g~13~) = -0.015, (\g~23~) = 0.012.
 Peak tails are ignored  where the intensity is below 0.0005 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_prof_R_factor        0.0140
_pd_proc_ls_prof_wR_expected     0.0102
_pd_proc_ls_prof_wR_factor       0.0137
_pd_proc_number_of_points        4610
_pd_spec_mounting
;
Aluminium-framed slab can with vanadium windows, shielded with Gd foil
;
_pd_spec_mount_mode              reflection
_pd_spec_size_axial              18
_pd_spec_size_equat              23
_pd_spec_size_thick              15
_refine_ls_goodness_of_fit_all   1.39
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_restraints     0
_refine_ls_R_Fsqd_factor         0.08240
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0.00
_reflns_d_resolution_high        0.722
_reflns_d_resolution_low         2.547
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              -14
_reflns_number_total             1903
_cod_data_source_file            bm5129sup1.cif
_cod_data_source_block           DMSO_TRIHYDRATE
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_geom_angle_publ_flag' value 'N' was changed to 'n' in
accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (18 times).

data item '_geom_bond_publ_flag' value 'N' was changed to 'n' in
accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/IUCr/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26 (72 times).

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        710.1830(30)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2108651