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_4106023
_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(C6 H5 Cl)'
_chemical_formula_sum            'C138 H54 Cl2 N4 Ni Sm'
_chemical_formula_weight         2047.81
_chemical_name_common            Sm@C2(40)-C90.Ni(OEP).2chlorobenzene
_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                 94.899(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.283(2)
_cell_length_b                   15.3956(12)
_cell_length_c                   20.7739(17)
_cell_measurement_reflns_used    9692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.1
_cell_measurement_theta_min      8.9
_cell_volume                     8056.6(11)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'Apex2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(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  silicon(111)
_diffrn_radiation_source         'Beamline 11.3.1, ALS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            129476
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             4136
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.208
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1175
_refine_ls_number_reflns         10693
_refine_ls_number_restraints     3169
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1010P)^2^+25.5180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1809
_refine_ls_wR_factor_ref         0.1824
_reflns_number_gt                10255
_reflns_number_total             10693
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja111465n_si_001.cif
_cod_data_source_block           cb120
_cod_original_cell_volume        8056.7(11)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4106023