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_2300358
_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_absolute_configuration unk
_chemical_formula_sum            'C6 H24 N8 Ni O6'
_chemical_formula_weight         363.04
_space_group_IT_number           182
_symmetry_space_group_name_Hall  'P 6c 2c'
_symmetry_space_group_name_H-M   'P 63 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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             2011-03-11T15:48:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   8.8647(3)
_cell_length_b                   8.8647(3)
_cell_length_c                   11.3595(4)
_cell_measurement_temperature    293(2)
_cell_volume                     773.07(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16770
_diffrn_reflns_theta_full        32.76
_diffrn_reflns_theta_max         32.76
_diffrn_reflns_theta_min         3.2
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85267
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_coef       0.060(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.03
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                838
_reflns_number_total             935
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            he5530.cif
_cod_data_source_block           IB
_cod_database_code               2300358