Cocrystallization of Binuclear Iron(III) Porphyrins with C60: Bending of μ-O{FeIII(Octaethylporphyrin)} and the First Structure of the Iron(III) Octaethyloxophlorin Dimer
Lee, Hon Man; Olmstead, Marilyn M.; Gross, Garrett G.; Balch, Alan L.; Crystal Growth & Design 3 (2003) 691–; doi:10.1021/cg030013z

data_4505675
_publ_section_title
;
 Cocrystallization of Binuclear Iron(III) Porphyrins with C60:&#x2009;
 Bending of \m-O{FeIII(Octaethylporphyrin)} and the First Structure of the
 Iron(III) Octaethyloxophlorin Dimer
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              691
_journal_paper_doi               10.1021/cg030013z
_journal_volume                  3
_journal_year                    2003
_chemical_formula_sum            'C138 H94 Fe2 N8 O'
_chemical_formula_weight         1991.92
_chemical_name_common            C60^.^\m-O[Fe(OEP)]~2~^.^benzene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 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                 102.1940(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1533(6)
_cell_length_b                   24.0768(9)
_cell_length_c                   23.5407(9)
_cell_measurement_reflns_used    7973
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.1
_cell_measurement_theta_min      2.4
_cell_volume                     9502.9(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SHELXS-97 (Sheldrick, 1990)'
_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 8.3
_diffrn_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.955
_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  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            129730
_diffrn_reflns_theta_full        31.49
_diffrn_reflns_theta_max         31.49
_diffrn_reflns_theta_min         0.85
_exptl_absorpt_coefficient_mu    0.371
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.814
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4152
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2684
_refine_ls_number_reflns         58098
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0636P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                43647
_reflns_number_total             58098
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg030013z_s1.cif
_cod_data_source_block           hml65
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4505675