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_2300490
_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                   8.442(2)
_cell_length_b                   10.569(2)
_cell_length_c                   13.816(3)
_cell_measurement_reflns_used    9598
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.0475
_cell_measurement_theta_min      3.4215
_cell_volume                     1232.7(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 0.995
_diffrn_measurement_device_type  'Bruker Smart APEX II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            80496
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         54.046
_diffrn_reflns_theta_min         2.949
_diffrn_source                   'INCOATEC Microsource'
_exptl_absorpt_coefficient_mu    18.839
_exptl_absorpt_correction_T_max  0.5800
_exptl_absorpt_correction_T_min  0.4162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_density_diffrn    3.555
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.109
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.032
_refine_diff_density_max         2.643
_refine_diff_density_min         -2.702
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       0.00164(4)
_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   1.175
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         7584
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0172
_refine_ls_R_factor_gt           0.0150
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0103P)^2^+1.1388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0321
_refine_ls_wR_factor_ref         0.0326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7024
_reflns_number_total             7584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            aj5242sup1.cif
_cod_data_source_block           3-(Mo)
_cod_database_code               2300490
_cod_database_fobs_code          2300490
_shelx_estimated_absorpt_t_min   0.233
_shelx_estimated_absorpt_t_max   0.584
_shelxl_version_number           2014-3
_shelx_res_checksum              80690
_shelx_hkl_checksum              32166