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_4116476
_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            'C113 H50 Cl3 Cu N4'
_chemical_formula_weight         1633.46
_chemical_name_common            C~70~^.^Cu(OEP)^.^CHCl~3~^.^benzene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.088(10)
_cell_angle_beta                 87.450(14)
_cell_angle_gamma                61.380(7)
_cell_formula_units_Z            2
_cell_length_a                   14.402(6)
_cell_length_b                   14.654(7)
_cell_length_c                   18.836(11)
_cell_measurement_reflns_used    3000
_cell_measurement_temperature    156(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1.08
_cell_volume                     3485(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'SHELXTL 5.03, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'by isostructural comparison'
_diffrn_ambient_temperature      156(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Siemens SMART'
_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  0.1398
_diffrn_reflns_av_sigmaI/netI    0.1824
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24975
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.08
_diffrn_standards_decay_%        <0.1
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.9709
_exptl_absorpt_correction_T_min  0.8266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
' Blessing, R. H., Acta Cryst. (1995). A51, 33-38.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_description       needle
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.429
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         9080
_refine_ls_number_restraints     1993
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.2197
_refine_ls_R_factor_gt           0.1262
_refine_ls_shift/su_max          0.772
_refine_ls_shift/su_mean         0.030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3233
_refine_ls_wR_factor_ref         0.3829
_reflns_number_gt                4462
_reflns_number_total             9080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja990618c_8.cif
_cod_data_source_block           bc241
_cod_database_code               4116476