Selective Synthesis, Isolation, and Crystallographic Characterization of LaSc2N@Ih-C80
Steven Stevenson; Coralie B. Rose; Juliya S. Maslenikova; Jimmy R. Villarreal; Mary A. Mackey; Brandon Q. Mercado; Kelly Chen; Marilyn M. Olmstead; Alan L. Balch; Inorganic Chemistry 51 (2012) 13096–13102; doi:10.1021/ic300888e

data_4331260
_publ_section_title
;
 Selective Synthesis, Isolation, and Crystallographic Characterization of
 LaSc2N@Ih-C80
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13096
_journal_page_last               13102
_journal_paper_doi               10.1021/ic300888e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C80 La N Sc2, C36 H44 N4 Ni, 2(C6 H6)'
_chemical_formula_sum            'C128 H56 La N5 Ni Sc2'
_chemical_formula_weight         1951.32
_chemical_name_common            LaSc2N@Ih(7)-C80.Ni(OEP).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                 95.385(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.3518(8)
_cell_length_b                   14.9702(8)
_cell_length_c                   19.6995(8)
_cell_measurement_reflns_used    9969
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      2.5
_cell_volume                     7443.4(6)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'Apex2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0521
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            47355
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    1.058
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       block
_exptl_crystal_F_000             3944
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.604
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1010
_refine_ls_number_reflns         10382
_refine_ls_number_restraints     480
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0554P)^2^+15.5628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                8246
_reflns_number_total             10382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300888e_si_001_1.cif
_cod_data_source_block           bqm15
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4331260