2,3,7,8,12,13,17,18-Octafluoro-5,10,15,20-tetrakis(pentafluorophenyl)porphyrin
Leroy, Jacques; Bondon, Arnaud; Toupet, Loic; Acta Crystallographica Section C 55 (1999) 464–466; doi:10.1107/S0108270198014000

data_2008276
_publ_section_title
2,3,7,8,12,13,17,18-Octafluoro-5,10,15,20-tetrakis(pentafluorophenyl)porphyrin
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              464
_journal_page_last               466
_journal_paper_doi               10.1107/S0108270198014000
_journal_volume                  55
_journal_year                    1999
_chemical_formula_moiety         'C44 H2 F28 N4'
_chemical_formula_sum            'C44 H2 F28 N4'
_chemical_formula_weight         1118.5
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.00(3)
_cell_angle_beta                 92.46(3)
_cell_angle_gamma                101.74(2)
_cell_formula_units_Z            1
_cell_length_a                   6.1818(10)
_cell_length_b                   13.008(3)
_cell_length_c                   13.605(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      9.0
_cell_volume                     1029.3(8)
_computing_cell_refinement       CAD4_Software
_computing_data_collection       CAD4_Software(Enraf-Nonius,_1977)
_computing_data_reduction        MolEN_(Fair,_1990)
_computing_molecular_graphics    ORTEPII_(Johnson,_1976)
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997b)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  Enraf_Nonius_CAD4
_diffrn_measurement_method       \w
_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  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4909
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.00
_exptl_absorpt_correction_T_min  0.00
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             546
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.219
_refine_ls_extinction_coef       0.010(2)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997a)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         4481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0644P)^2^+0.2708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                2901
_reflns_number_total             4481
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ln1059.cif
_cod_data_source_block           noyau
_cod_depositor_comments
;
Automatic conversion scripts had previously changed 
'_atom_site_refinement_flags' tag values 'd' into 'D' as recommended by 
'cif_core.dic' version 2.4.1. However, manual inspection revealed that the 
underlying problem was actually related to a bad tag order inside the 
atom site loop. The following changes were performed to resolve the problem:

* '_atom_site_refinement_flags' tag was changed into '_atom_site_calc_flag'.
  '_atom_site_calc_flag' was already present with all values set to '1' so 
  these values were removed (possible placeholder values for occupancies).
* there were two disordered hydrogen atoms with 'atom_site_disorder_assembly' 
  values 'PR'. The name of the disorder assembly also corresponded to 
  '_atom_site_refinement_flags_occupancy' and '_atom_site_refinement_flags_posn'
  tag values 'P' and 'R' so these tags were added into the loop.

For all changes the original paper was consulted.
;
_cod_original_cell_volume        1029.3(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2008276