Isolation and Crystallographic Identification of Four Isomers of Sm@C90
Hua Yang; Hongxiao Jin; Hongyu Zhen; Zhimin Wang; Ziyang Liu; Christine M. Beavers; Brandon Q. Mercado; Marilyn M. Olmstead; Alan L. Balch; Journal of the American Chemical Society 133 (2011) 6299–6306; doi:10.1021/ja111465n

data_4106025
_publ_section_title
;
 Isolation and Crystallographic Identification of Four Isomers of Sm@C90
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6299
_journal_page_last               6306
_journal_paper_doi               10.1021/ja111465n
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C90 Sm, C36 H44 N4 Ni, 2(C7 H8)'
_chemical_formula_sum            'C140 H60 N4 Ni Sm'
_chemical_formula_weight         2006.98
_chemical_name_common            Sm@C90(90:46)NiOEP.2toluene
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 95.150(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.5939(13)
_cell_length_b                   15.2087(6)
_cell_length_c                   41.538(2)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      32.9
_cell_measurement_theta_min      2.7
_cell_volume                     16103.4(13)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART ApexII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            127285
_diffrn_reflns_theta_full        30.99
_diffrn_reflns_theta_max         30.99
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.028
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             8144
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.647
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1437
_refine_ls_number_reflns         25610
_refine_ls_number_restraints     4329
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0775
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1288P)^2^+90.2884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2176
_refine_ls_wR_factor_ref         0.2336
_reflns_number_gt                21012
_reflns_number_total             25610
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja111465n_si_003.cif
_cod_data_source_block           mn1916
_cod_original_cell_volume        16103.3(14)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4106025