Unusual Aryl-Porphyrin Rotational Barriers in Peripherally Crowded Porphyrins
Craig J. Medforth; Raid E. Haddad; Cinzia M. Muzzi; Neal R. Dooley; Laurent Jaquinod; David C. Shyr; Daniel J. Nurco; Marilyn M. Olmstead; Kevin M. Smith; Jian-Guo Ma; John A. Shelnutt; Inorganic Chemistry 42 (2003) 2227–2241; doi:10.1021/ic010958a

data_4313417
_publ_section_title
;
 Unusual Aryl-Porphyrin Rotational Barriers in Peripherally Crowded
 Porphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2227
_journal_page_last               2241
_journal_paper_doi               10.1021/ic010958a
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C108.5 H69 Cl9 F8 N10 O14'
_chemical_formula_weight         2207.79
_chemical_name_systematic
;
dication 5,10,15,20-tetra-(4-fluorophenyl)porphyrin, 2(picrate)-,
4.5dichloromethane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 103.130(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.708(2)
_cell_length_b                   24.506(3)
_cell_length_c                   29.129(4)
_cell_measurement_reflns_used    5728
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.1
_cell_measurement_theta_min      2.4
_cell_volume                     10225(2)
_computing_cell_refinement       'Bruker, SAINT'
_computing_data_collection       'Bruker, SMART'
_computing_data_reduction        'Bruker, SAINT'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.063
_diffrn_reflns_av_sigmaI/netI    0.058
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            102945
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.10
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count
;
Measured at the beginning and end of the data collection.
;
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.344
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS 2.0 (Sheldrick, 2000)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4561
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.616
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1444
_refine_ls_number_reflns         23472
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.150
_refine_ls_R_factor_gt           0.099
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1986P)^2^+17.7353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.297
_refine_ls_wR_factor_ref         0.337
_reflns_number_gt                13877
_reflns_number_total             23472
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic010958a_3.cif
_cod_data_source_block           mn938
_cod_original_cell_volume        10224.8(15)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4313417