Validation of experimental charge-density refinement strategies: when do we overfit?
Krause, Lennard; Niepötter, Benedikt; Schürmann, Christian J.; Stalke, Dietmar; Herbst-Irmer, Regine; IUCrJ 4 (2017) –; doi:10.1107/S2052252517005103

data_1546116
_publ_section_title
;
 Validation of experimental charge-density refinement strategies: when do
 we overfit?
;
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052252517005103
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C20 H23 P S'
_chemical_formula_sum            'C20 H23 P S'
_chemical_formula_weight         326.41
_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   geom
_audit_creation_method           XD2016rev.2016.01
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.932(2)
_cell_length_b                   14.570(2)
_cell_length_c                   21.091(3)
_cell_measurement_reflns_used    9781
_cell_measurement_temperature    99(2)
_cell_measurement_theta_max      52.1495
_cell_measurement_theta_min      2.6835
_cell_volume                     3359.4(9)
_computing_cell_refinement       'SAINT V8.37A'
_computing_data_collection       'APEX2 v2012.2'
_computing_data_reduction        'SAINT V8.37A'
_computing_molecular_graphics    'XP Version 5.1'
_computing_publication_material  'XP Version 5.1'
_computing_structure_refinement  'Volkov et al, (2006)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      99(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            222190
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         52.228
_diffrn_reflns_theta_min         1.931
_diffrn_source                   'BRUKER Rotating Anode'
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  0.9285
_exptl_absorpt_correction_T_min  0.8845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2016/2
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.204
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         18435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.204
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0183
_refine_ls_R_Fsqd_factor         0.0117
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0.000
_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         0.0157
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15462
_reflns_number_total             19329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lc5072.cif
_cod_data_source_block           2_xd
_cod_database_code               1546116