Complexation of Sc3N@C80 Endohedral Fullerene with Cyclic Zn-Bisporphyrins: Solid State and Solution Studies
Laura P. Hernández-Eguía; Eduardo C. Escudero-Adán; Julio R. Pinzón; Luis Echegoyen; Pablo Ballester; Journal of Organic Chemistry 76 (2011) 3258–3265; doi:10.1021/jo200154d

data_4026246
_publ_section_title
;
 Complexation of Sc3N@C80 Endohedral Fullerene with Cyclic
 Zn-Bisporphyrins: Solid State and Solution Studies
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3258
_journal_page_last               3265
_journal_paper_doi               10.1021/jo200154d
_journal_volume                  76
_journal_year                    2011
_chemical_formula_sum            'C170 H122.5 N8.5 O4 Sc1.5 Zn2'
_chemical_formula_weight         2546.45
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 110.573(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   34.2052(14)
_cell_length_b                   24.7010(12)
_cell_length_c                   31.3815(14)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.24
_cell_measurement_theta_min      2.24
_cell_volume                     24823(2)
_computing_cell_refinement       'Bruker APEX2 v2009.1-0'
_computing_data_collection       'Bruker APEX2 v2009.1-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'ESRF BM-16'
_diffrn_measurement_method
;
 Fullsphere data collection, phi scans
;
_diffrn_radiation_monochromator  Si111
_diffrn_radiation_source         Synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.73780
_diffrn_reflns_av_R_equivalents  0.1252
_diffrn_reflns_av_sigmaI/netI    0.1246
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            54250
_diffrn_reflns_theta_full        24.24
_diffrn_reflns_theta_max         24.24
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_description       Needle
_exptl_crystal_F_000             10604
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.608
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.806
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1832
_refine_ls_number_reflns         17620
_refine_ls_number_restraints     1773
_refine_ls_restrained_S_all      1.763
_refine_ls_R_factor_all          0.1867
_refine_ls_R_factor_gt           0.1325
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3027
_refine_ls_wR_factor_ref         0.3232
_reflns_number_gt                11620
_reflns_number_total             17620
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo200154d_si_002.cif
_cod_data_source_block           lph005c801eqb_0m
_cod_original_cell_volume        24823.4(19)
_cod_original_formula_sum        'C170 H122.50 N8.50 O4 Sc1.50 Zn2'
_cod_database_code               4026246