Conformational Flexibility in Dodecasubstituted Porphyrins
Daniel J. Nurco; Craig J. Medforth; Timothy P. Forsyth; Marilyn M. Olmstead; Kevin M. Smith; Journal of the American Chemical Society 118 (1996) 10918–10919; doi:10.1021/ja962164e

data_4117200
_publ_contact_author
;
Dan Nurco, Chemistry Department, University of California, Davis, 95616 USA
;
_publ_contact_author_email       nurco@chem.ucdavis.edu
_publ_section_title
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 Conformational Flexibility in Dodecasubstituted Porphyrins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10918
_journal_page_last               10919
_journal_paper_doi               10.1021/ja962164e
_journal_volume                  118
_journal_year                    1996
_chemical_compound_source        synthetic
_chemical_formula_moiety         'C92 H42 N4 F20, 4(C H2 Cl2)'
_chemical_formula_sum            'C96 H50 Cl8 F20 N4'
_chemical_formula_weight         1923.00
_chemical_name_common            H~2~F~20~DPP
_chemical_name_systematic
; 
 5,10,15,20-tetrakis-(pentafluorophenyl)-2,3,7,8,12,13,17,18-octaphenyl-
 porphyrin
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.605(2)
_cell_length_b                   28.605(2)
_cell_length_c                   9.9690(10)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      45.75
_cell_measurement_theta_min      3.60
_cell_volume                     8157.1(11)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        XDISK
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'Siemens SHELXTL Plus, V. 5.02'
_computing_structure_solution    'Siemens SHELXTL Plus, V. 5.02'
_diffrn_ambient_temperature      130(2)
_diffrn_measurement_device       'Syntex P2~1~'
_diffrn_measurement_method       '\q - 2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3066
_diffrn_reflns_theta_max         56.98
_diffrn_reflns_theta_min         3.09
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.395
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   XABS2
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       needle
_exptl_crystal_F_000             3880
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.727
_refine_ls_goodness_of_fit_obs   0.741
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         2737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.727
_refine_ls_restrained_S_obs      0.741
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_obs          0.0396
_refine_ls_shift/esd_max         0.604
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0954P)^2^+24.3478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1169
_refine_ls_wR_factor_obs         0.1088
_reflns_number_observed          2321
_reflns_number_total             2737
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja962164e_1.cif
_cod_data_source_block           01xc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0954P)^2^+24.3478P] 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^)+(0.0954P)^2^+24.3478P] 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      'I 41/a'
_cod_database_code               4117200