On the precision and accuracy of structural analysis of light-induced metastable states
Legrand, Vincent; Pillet, Sébastien; Weber, Hans-Peter; Souhassou, Mohamed; Létard, Jean-François; Guionneau, Philippe; Lecomte, Claude; Journal of Applied Crystallography 40 (2007) 1076–1088; doi:10.1107/S0021889807040149

data_2300188
_publ_section_title
;
 On the precision and accuracy of structural analysis of light-induced
 metastable states
;
_journal_issue                   6
_journal_name_full               'Journal of Applied Crystallography'
_journal_page_first              1076
_journal_page_last               1088
_journal_paper_doi               10.1107/S0021889807040149
_journal_volume                  40
_journal_year                    2007
_chemical_formula_moiety         'C26 H16 Fe N6 S2'
_chemical_formula_sum            'C26 H16 Fe N6 S2'
_chemical_formula_weight         532.42
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.7620(10)
_cell_length_b                   10.0240(10)
_cell_length_c                   17.0900(10)
_cell_measurement_reflns_used    23007
_cell_measurement_temperature    15(2)
_cell_measurement_theta_max      45.31
_cell_measurement_theta_min      3.99
_cell_volume                     2186.3(3)
_computing_cell_refinement       'CRYSALIS Oxford Diffraction (2004)'
_computing_data_collection       'CRYSALIS Oxford Diffraction (2004)'
_computing_data_reduction        'CRYSALIS Oxford Diffraction (2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      15(2)
_diffrn_measured_fraction_theta_full 0.776
_diffrn_measured_fraction_theta_max 0.776
_diffrn_measurement_device_type  'KUMA KM6'
_diffrn_measurement_method       'phi scans'
_diffrn_radiation_monochromator  Si
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23007
_diffrn_reflns_theta_full        45.31
_diffrn_reflns_theta_max         45.31
_diffrn_reflns_theta_min         3.99
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Absorption correction were performed using CRYSALIS Oxford Diffraction (2004)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.656
_refine_diff_density_min         -0.725
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         7122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1061P)^2^+0.2257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1364
_refine_ls_wR_factor_ref         0.1482
_reflns_number_gt                5377
_reflns_number_total             7122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            db5028.cif
_cod_data_source_block           ls_15k
_cod_original_cell_volume        2186.2(3)
_cod_original_sg_symbol_H-M      'P bcn'
_cod_database_code               2300188
_cod_database_fobs_code          2300188