Diffuse scattering and short-range order in uranium iodine phthalocyanine [U~1{-~<i>x</i>}Pc~2~]I~2{-~<i>y</i>} and the X-ray structure analysis of crystals with diffuse superstructure reflections
Krawczyk, J.; Pietraszko, A.; Kubiak, R.; Łukaszewicz, K.; Acta Crystallographica Section B 59 (2003) 384–392; doi:10.1107/S0108768103004804

data_2103884
_publ_section_title
;
 Diffuse scattering and short-range order in uranium iodine
 phthalocyanine [U~1{-~<i>x</i>}Pc~2~]I~2{-~<i>y</i>} and the X-ray
 structure analysis of crystals with diffuse superstructure reflections
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              384
_journal_page_last               392
_journal_paper_doi               10.1107/S0108768103004804
_journal_volume                  59
_journal_year                    2003
_chemical_formula_sum            'C64 H32 I1.74 N16 U0.96'
_chemical_formula_weight         1474.37
_chemical_name_common            'iodine-doped uranium pthalocyianine'
_space_group_IT_number           124
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2c'
_symmetry_space_group_name_H-M   'P 4/m c c'
_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            1
_cell_length_a                   13.997(2)
_cell_length_b                   13.997(2)
_cell_length_c                   6.5230(10)
_cell_measurement_temperature    293(2)
_cell_volume                     1278.0(3)
_computing_cell_refinement       'CrysAlis 189'
_computing_data_collection       'CrysAlis 189'
_computing_data_reduction        'CrysAlis 189'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KM4-CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            15699
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    4.163
_exptl_absorpt_correction_T_max  0.734
_exptl_absorpt_correction_T_min  0.438
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             709
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.504
_refine_ls_extinction_coef       0.0000(8)
_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   1.199
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     78
_refine_ls_number_reflns         980
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          2.708
_refine_ls_shift/su_mean         0.035
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.9211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                867
_reflns_number_total             980
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ck0017.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Removing duplicate rows from the ATOM_TYPE loop.

 Antanas Vaitkus,
 2018-08-07

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.9211P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+0.9211P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P4/mcc
_cod_original_formula_sum        'C64 H32 H0 I1.74 N16 U0.96'
_cod_database_code               2103884
_cod_database_fobs_code          2103884