Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination
Krause, Lennard; Herbst-Irmer, Regine; Sheldrick, George M.; Stalke, Dietmar; Journal of Applied Crystallography 48 (2015) –; doi:10.1107/S1600576714022985

data_2300489
_publ_section_title
;
 Comparison of silver and molybdenum microfocus X-ray sources for
 single-crystal structure determination
;
_journal_coeditor_code           aj5242
_journal_issue                   1
_journal_name_full               'Journal of Applied Crystallography'
_journal_paper_doi               10.1107/S1600576714022985
_journal_volume                  48
_journal_year                    2015
_chemical_formula_moiety         'O4 W, 2(H2 O), 2(Na)'
_chemical_formula_sum            'H4 Na2 O6 W'
_chemical_formula_weight         329.86
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.439(2)
_cell_length_b                   10.559(2)
_cell_length_c                   13.807(3)
_cell_measurement_reflns_used    9695
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.434
_cell_measurement_theta_min      2.328
_cell_volume                     1230.3(5)
_computing_cell_refinement       'SAINT V8.30C'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.30C'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56086
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            146508
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         44.498
_diffrn_reflns_theta_min         2.328
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    10.164
_exptl_absorpt_correction_T_max  0.7343
_exptl_absorpt_correction_T_min  0.5666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_density_diffrn    3.562
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.812
_refine_diff_density_min         -3.035
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       0.00107(3)
_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   1.156
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         10047
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0136
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0046P)^2^+0.8512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0239
_refine_ls_wR_factor_ref         0.0248
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8783
_reflns_number_total             10047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aj5242sup1.cif
_cod_data_source_block           3-(Ag)
_cod_database_code               2300489
_cod_database_fobs_code          2300489
_shelx_estimated_absorpt_t_min   0.430
_shelx_estimated_absorpt_t_max   0.743
_shelxl_version_number           2014-3
_shelx_res_checksum              97713
_shelx_hkl_checksum              35886