Low-energy contamination of Mo microsource X-ray radiation: analysis and solution of the problem
Macchi, Piero; Bürgi, Hans-Beat; Chimpri, Abita S.; Hauser, Jürg; Gál, Zoltán; Journal of Applied Crystallography 44 (2011) 763–771; doi:10.1107/S0021889811016232

data_2300364
_publ_section_title
;
 Low-energy contamination of Mo microsource X-ray radiation: analysis
 and solution of the problem
;
_journal_coeditor_code           HE5530
_journal_issue                   4
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              763
_journal_page_last               771
_journal_paper_doi               10.1107/S0021889811016232
_journal_volume                  44
_journal_year                    2011
_chemical_formula_sum            'C8 H14 N2 O8'
_chemical_formula_weight         266.22
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-03-11T09:37:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.3321(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.82035(12)
_cell_length_b                   5.68088(3)
_cell_length_c                   12.09343(8)
_cell_measurement_reflns_used    20347
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.2959
_cell_measurement_theta_min      3.5234
_cell_volume                     1037.528(13)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
        (compiled Sep 13 2010,14:28:38)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
        (compiled Sep 13 2010,14:28:38)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
        (compiled Sep 13 2010,14:28:38)
;
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2413
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0162572
_diffrn_orient_matrix_UB_12      -0.010493
_diffrn_orient_matrix_UB_13      -0.0485009
_diffrn_orient_matrix_UB_21      -0.0073981
_diffrn_orient_matrix_UB_22      0.1219477
_diffrn_orient_matrix_UB_23      -0.0114676
_diffrn_orient_matrix_UB_31      0.0434064
_diffrn_orient_matrix_UB_32      0.0247517
_diffrn_orient_matrix_UB_33      0.0359588
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15647
_diffrn_reflns_theta_full        45.36
_diffrn_reflns_theta_max         45.36
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  1.034
_exptl_absorpt_correction_T_min  0.967
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.41 (release 13-09-2010 CrysAlis171 .NET)
        (compiled Sep 13 2010,14:28:38)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
;
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.1318
_exptl_crystal_size_min          0.1116
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.206
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.028
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         4302
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.022
_refine_ls_R_factor_gt           0.021
_refine_ls_shift/su_max          0.0005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
        calc w1 = 1/[s^2^(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.013
_reflns_number_gt                3729
_reflns_number_total             4172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            he5530.cif
_cod_data_source_block           IIC
_cod_original_cell_volume        1037.528(11)
_cod_database_code               2300364