Charge-density analysis of 1-nitroindoline: refinement quality using free <i>R</i> factors and restraints
Zarychta, Bartosz; Zaleski, Jacek; Kyzioł, Janusz; Daszkiewicz, Zdzisław; Jelsch, Christian; Acta Crystallographica Section B 67 (2011) 250–262; doi:10.1107/S0108768111013140

data_2104966
_publ_section_title
;
 Charge-density analysis of 1-nitroindoline: refinement quality using
 free <i>R</i> factors and restraints
;
_journal_coeditor_code           PI5008
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              250
_journal_page_last               262
_journal_paper_doi               10.1107/S0108768111013140
_journal_volume                  67
_journal_year                    2011
_chemical_formula_moiety         'C8 H8 N2 O2'
_chemical_formula_sum            'C8 H8 N2 O2'
_chemical_formula_weight         164.154
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           MoPro
_cell_angle_alpha                116.823(8)
_cell_angle_beta                 104.589(9)
_cell_angle_gamma                91.602(5)
_cell_formula_units_Z            2
_cell_length_a                   5.7913(3)
_cell_length_b                   8.2458(6)
_cell_length_c                   8.9223(10)
_cell_measurement_reflns_used    29060
_cell_measurement_temperature    90.00(10)
_cell_measurement_theta_max      70.78
_cell_measurement_theta_min      2.81
_cell_volume                     362.99(6)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'MoPro (Guillot et al., 2001; Jelsch et al., 2005)'
_computing_structure_refinement  'MoPro (J. Appl. Cryst. 2005, 38, 38-54)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.00(10)
_diffrn_detector_area_resol_mean 10.4508
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.621
_diffrn_measurement_device       '4-circle kappa geometry goniometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur System'
_diffrn_measurement_method       \w--scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.02828
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29060
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         70.19
_diffrn_reflns_theta_min         2.81
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.111
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.923
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlis RED (Oxford Diffraction, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             172
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.6
_refine_diff_density_max         0.23
_refine_diff_density_min         -0.20
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         8768
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      1.435
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'calc w =1/[1.1712*\s^2^(Fo^2^)+0.0007*Yo^2]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0230
_refine_ls_wR_factor_ref         0.0237
_reflns_number_gt                7946
_reflns_number_total             8768
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            pi5008.cif
_cod_data_source_block           I
_cod_original_cell_volume        362.99(5)
_cod_database_code               2104966
_cod_database_fobs_code          2104966