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_4117203
_publ_contact_author
; 
        Daniel J. Nurco 
        Chemistry Department 
        University of California 
        Davis, CA 
        95616 
        USA 
;
_publ_contact_author_email       nurco@chem.ucdavis.edu
_publ_section_title
;
 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 H60 N4 Ni, 5.84(C6 H12), 0.85(C H Cl3)'
_chemical_formula_sum            'C127.9 H130.9 Cl2.6 N4 Ni'
_chemical_formula_weight         1875.06
_chemical_name_common            'Ni(II) DPP'
_chemical_name_systematic
; 
 Ni(II) 2,3,5,7,8,10,12,13,15,17,18,20-dodecaphenylporphyrin
;
_space_group_IT_number           219
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F -4a 2 3'
_symmetry_space_group_name_H-M   'F -4 3 c'
_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            24
_cell_length_a                   40.950(5)
_cell_length_b                   40.950(5)
_cell_length_c                   40.950(5)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      44.21
_cell_measurement_theta_min      8.94
_cell_volume                     68669(15)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  'Siemens XCIF'
_computing_structure_refinement  'Siemens SHELXTL V. 5.03'
_computing_structure_solution    'Siemens SHELXTL V. 5.03'
_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  0.070
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            19913
_diffrn_reflns_theta_max         57.07
_diffrn_reflns_theta_min         2.16
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.162
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_correction_T_min  0.54
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'translucent red'
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             23964
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.64
_exptl_crystal_size_min          0.64
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.365
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.05(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.041
_refine_ls_hydrogen_treatment
;
Hydrogens on the porphyrin were treated as riding.  Solvent cyclohexanes 
and chloroform were not assigned hydrogens.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3088
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.279
_refine_ls_restrained_S_obs      1.058
_refine_ls_R_factor_all          0.1102
_refine_ls_R_factor_obs          0.0891
_refine_ls_shift/esd_max         -0.085
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+763.3912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2883
_refine_ls_wR_factor_obs         0.2250
_reflns_number_observed          2739
_reflns_number_total             3151
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja962164e_4.cif
_cod_data_source_block           djn95w
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+763.3912P] 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^)+(0.1451P)^2^+763.3912P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        68669.2(137)
_cod_database_code               4117203