Interaction of Curved and Flat Molecular Surfaces. The Structures of Crystalline Compounds Composed of Fullerene (C60, C60O, C70, and C120O) and Metal Octaethylporphyrin Units
Marilyn M. Olmstead; David A. Costa; Kalyani Maitra; Bruce C. Noll; Shane L. Phillips; Pamela M. Van Calcar; Alan L. Balch; Journal of the American Chemical Society 121 (1999) 7090–7097; doi:10.1021/ja990618c

data_4116474
_publ_contact_author
; Dr. Alan L. Balch
  Department of Chemistry
  University of California
  Davis, CA 95616
  USA
;
_publ_contact_author_email       balch@indigo.ucdavis.edu
_publ_contact_author_fax         530-752-8995
_publ_contact_author_phone       530-752-0941
_publ_section_title
;
 Interaction of Curved and Flat Molecular Surfaces. The Structures of
 Crystalline Compounds Composed of Fullerene (C60, C60O, C70, and C120O)
 and Metal Octaethylporphyrin Units
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7090
_journal_page_last               7097
_journal_paper_doi               10.1021/ja990618c
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C97 H45 Cl4 Fe N4'
_chemical_formula_weight         1464.02
_chemical_name_common            C~60~^.^ClFe(OEP)^.^CHCl~3~
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.951(4)
_cell_length_b                   20.784(4)
_cell_length_c                   15.810(3)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.6
_cell_measurement_theta_min      4.2
_cell_volume                     6227(2)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97-2 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.747
_diffrn_measured_fraction_theta_max 0.747
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       2\q-\w
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Siemens rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.045
_diffrn_reflns_av_sigmaI/netI    0.042
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2119
_diffrn_reflns_theta_full        56.06
_diffrn_reflns_theta_max         56.06
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        1.0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    4.008
_exptl_absorpt_correction_T_max  0.7398
_exptl_absorpt_correction_T_min  0.5011
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;XABS2: an empirical absorption correction program. Parkin, S.; Moezzi,
 B.; Hope, H. J. Appl. Cryst. 1995, 28, 53-56.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       obelisk
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         1643
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1440
_refine_ls_R_factor_gt           0.1258
_refine_ls_shift/su_max          0.902
_refine_ls_shift/su_mean         0.027
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1702P)^2^+177.1206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3252
_refine_ls_wR_factor_ref         0.3435
_reflns_number_gt                1347
_reflns_number_total             1643
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja990618c_6.cif
_cod_data_source_block           mn675
_cod_database_code               4116474