Internal and External Factors in the Structural Organization in Cocrystals of the Mixed-Metal Endohedrals (GdSc2N@Ih-C80, Gd2ScN@Ih-C80, and TbSc2N@Ih-C80) and Nickel(II) Octaethylporphyrin
Steven Stevenson; Christopher J. Chancellor; Hon Man Lee; Marilyn M. Olmstead; Alan L. Balch; Inorganic Chemistry 47 (2008) 1420–1427; doi:10.1021/ic701824q

data_4304338
_publ_section_title
;
Internal and External Factors in the Structural Organization in Cocrystals
of the Mixed-Metal Endohedrals (GdSc2N@Ih-C80, Gd2ScN@Ih-C80, and
TbSc2N@Ih-C80) and Nickel(II) Octaethylporphyrin
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1420
_journal_page_last               1427
_journal_paper_doi               10.1021/ic701824q
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C80 Sc2 Tb N, C36 H44 N4, 2(C6 H6)'
_chemical_formula_sum            'C128 H56 N5 Ni Sc2 Tb'
_chemical_formula_weight         1971.33
_chemical_name_common            Sc2TbN@C80.NiOEP.2benzene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 94.791(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.180(2)
_cell_length_b                   15.0633(13)
_cell_length_c                   19.650(2)
_cell_measurement_temperature    100(2)
_cell_volume                     7427.1(12)
_computing_cell_refinement       'Mosflm (Leslie, A.G.W., 1992)'
_computing_data_collection       'MarControl (marUSA Inc, Evanston, IL)'
_computing_data_reduction        Mosflm
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Huber goniometer, 345mm MAR Detector'
_diffrn_measurement_method       \p
_diffrn_radiation_monochromator
'Cylindrically bent cubed root Si(311), asymmetric cut, horizontal focus'
_diffrn_radiation_source
'synchrotron, 16 pole 1.9T wiggler, SSRL BL9-1'
_diffrn_radiation_type           '16,039 eV'
_diffrn_radiation_wavelength     0.75100
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8157
_diffrn_reflns_theta_full        22.18
_diffrn_reflns_theta_max         22.18
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    1.438
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             3976
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         4101
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1215P)^2^+168.4573P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2288
_refine_ls_wR_factor_ref         0.2303
_reflns_number_gt                3918
_reflns_number_total             4101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701824q-file002.cif
_cod_data_source_block           hml41
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4304338