Accurate atomic displacement parameters from time-of-flight neutron-diffraction data at TOPAZ
Jørgensen, Mads R. V.; Hathwar, Venkatesha R.; Sist, Mattia; Wang, Xiaoping; Hoffmann, Christina M.; Briseno, Alejandro L.; Overgaard, Jacob; Iversen, Bo B.; Acta Crystallographica Section A Foundations and Advances 70 (2014) 679–; doi:10.1107/S2053273314015599

data_2312013
_publ_section_title
;
 Accurate atomic displacement parameters from time-of-flight
 neutron-diffraction data at TOPAZ
;
_journal_coeditor_code           PC5039
_journal_issue                   6
_journal_name_full
'Acta Crystallographica Section A Foundations and Advances'
_journal_page_first              679
_journal_paper_doi               10.1107/S2053273314015599
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety         '2(C6 H2 N3 O7), C5 H11 N O2, 2(C3 H5 N2)'
_chemical_formula_structural     '2(C6 H2 N3 O7), C5 H11 N O2, 2(C3 H5 N2)'
_chemical_formula_sum            'C23 H25 N11 O16'
_chemical_formula_weight         711.51
_chemical_name_common            'Betaine, Imidazole and Picric acid'
_chemical_name_systematic
'cocrystal between picric acid, imidazole and betaine'
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_creation_date
;
'Mon Jul 01 15:34:14 2013'
;
_audit_creation_method
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_audit_update_record
' 2014-01-21T11:07  Initial CIF as created by GSAS2CIF'
_cell_angle_alpha                90.0
_cell_angle_beta                 114.7162(17)
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   33.5939(5)
_cell_length_b                   7.66580(8)
_cell_length_c                   25.1324(3)
_cell_measurement_reflns_used    37970
_cell_measurement_temperature    99.98(19)
_cell_measurement_theta_max      57.9410
_cell_measurement_theta_min      2.7860
_cell_volume                     5879.28(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_refinement  'Volkov et al, (2006)'
_diffrn_ambient_temperature      99.98(19)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.9976
_diffrn_measured_fraction_theta_max 0.9836
_diffrn_measurement_details
;
  1 omega   35.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.6250 -178.0000   30.0000 52

  2 omega  -60.00   -1.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.6250  -77.0000  120.0000 59

  3 omega   77.00  121.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       75.4353  125.0000  150.0000 44

  4 omega   13.00  107.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       75.4353  -77.0000    0.0000 94

  5 omega   46.00  138.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       75.4353   61.0000  150.0000 92

  6 omega    1.00   34.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       75.4353  -45.0000   30.0000 33

  7 omega    0.00   43.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       75.4353  -30.0000 -150.0000 43

  8 omega   66.00  139.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       75.4353   61.0000   90.0000 73

  9 omega   34.00   88.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.6250 -178.0000   90.0000 54

 10 omega  -77.00   26.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.6250  -38.0000 -180.0000 103

 11 omega   48.00  150.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       75.4353   45.0000  -30.0000 102

 12 omega   -3.00  109.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       75.4353  -77.0000 -150.0000 112

 13 omega   48.00  150.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       75.4353   45.0000   60.0000 102

 14 omega    1.00   23.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       75.4353  -45.0000   90.0000 22

;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0077022000
_diffrn_orient_matrix_UB_12      -0.0320502000
_diffrn_orient_matrix_UB_13      0.0290725000
_diffrn_orient_matrix_UB_21      0.0049278000
_diffrn_orient_matrix_UB_22      -0.0813559000
_diffrn_orient_matrix_UB_23      -0.0092931000
_diffrn_orient_matrix_UB_31      0.0213681000
_diffrn_orient_matrix_UB_32      0.0303058000
_diffrn_orient_matrix_UB_33      0.0058012000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       79
_diffrn_reflns_limit_h_min       -73
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            165808
_diffrn_reflns_theta_full        47.6339
_diffrn_reflns_theta_max         58.5631
_diffrn_reflns_theta_min         2.4354
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.982
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.62
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.2874
_exptl_crystal_size_mid          0.2068
_exptl_crystal_size_min          0.1611
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.26
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1306
_refine_ls_number_reflns         21277
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.066
_refine_ls_R_factor_gt           0.03
_refine_ls_R_Fsqd_factor         0.03
_refine_ls_shift/su_max          0.00909
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w2 = 1/[s^2^(Fo^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.072
_reflns_number_gt                21277
_reflns_number_total             27262
_reflns_threshold_expression     >3sigma(I)
_cod_data_source_file            pc5039sup1.cif
_cod_data_source_block           BIPa_X_MM_Shade
_cod_original_cell_volume        5879.29(13)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2312013
_cod_duplicate_entry 2312012