Exceptional Chemical Properties of Sc@C2v(9)-C82 Probed with Adamantylidene Carbene
Makoto Hachiya; Hidefumi Nikawa; Naomi Mizorogi; Takahiro Tsuchiya; Xing Lu; Takeshi Akasaka; Journal of the American Chemical Society 134 (2012) 15550–15555; doi:10.1021/ja306890x

data_4118647
_publ_contact_author_address
;Aspect of Creation of New Materials
Center for Tsukuba Advanced Research Alliance
University of Tsukuba
Tsukuba, Ibaraki 305-8577, Japan 
;
_publ_contact_author_email       akasaka@tara.tsukuba.ac.jp
_publ_contact_author_fax         +81-298-53-6409
_publ_contact_author_name        'Takeshi AKASAKA'
_publ_contact_author_phone       +81-298-53-6409
_publ_section_title
;
 Exceptional Chemical Properties of Sc@C2v(9)-C82 Probed with
 Adamantylidene Carbene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15550
_journal_page_last               15555
_journal_paper_doi               10.1021/ja306890x
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'Sc C92 H14, 2.5(C1 S2)'
_chemical_formula_sum            'C94.5 H14 S5 Sc'
_chemical_formula_weight         1354.32
_chemical_name_common            Sc@C82Ad-A
_chemical_name_systematic        Sc@C82Ad-A
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 101.644(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.332(3)
_cell_length_b                   21.875(5)
_cell_length_c                   20.992(4)
_cell_measurement_temperature    110(2)
_cell_volume                     5097(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        Yadokari-XG
_computing_molecular_graphics    Yadokari-XG
_computing_publication_material  Yadokari-XG
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51727
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    0.417
_exptl_absorpt_correction_T_max  0.9595
_exptl_absorpt_correction_T_min  0.8851
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_description       Block
_exptl_crystal_F_000             2728
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1264
_refine_ls_number_reflns         12903
_refine_ls_number_restraints     1542
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1076
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1029P)^2^+10.3496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2234
_reflns_number_gt                9013
_reflns_number_total             12903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja306890x_si_002.cif
_cod_data_source_block           sc@c82ad_110k
_cod_original_cell_volume        5096.6(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C94.50 H14 S5 Sc'
_cod_database_code               4118647