Sc2O@C(3v)(8)-C82: A Missing Isomer of Sc2O@C82.
Tang, Qiangqiang; Abella, Laura; Hao, Yajuan; Li, Xiaohong; Wan, Yingbo; Rodríguez-Fortea, Antonio; Poblet, Josep M.; Feng, Lai; Chen, Ning; Inorganic chemistry 55 (2016) 1926–1933; doi:10.1021/acs.inorgchem.5b02901

data_4347227
_publ_section_title
;
 Sc2O@C(3v)(8)-C82: A Missing Isomer of Sc2O@C82.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1926
_journal_page_last               1933
_journal_paper_doi               10.1021/acs.inorgchem.5b02901
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'Sc2O C82, Ni N4 C36 H44, 0.90(bz), 0.10(CF)'
_chemical_formula_sum            'C123.5 H49.5 Cl0.25 N4 Ni O Sc2'
_chemical_formula_weight         1762.66
_chemical_name_common            Sc2O@C82/NiOEP/0.90(bz)0.10(CF)
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 95.0798(34)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.3629(30)
_cell_length_b                   15.1841(16)
_cell_length_c                   19.8128(25)
_cell_measurement_temperature    120(2)
_cell_volume                     7600.2(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            108901
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         2.504
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.9521
_exptl_absorpt_correction_T_min  0.9160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick 1996)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_description       block
_exptl_crystal_F_000             3603
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.586
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.669
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1288
_refine_ls_number_reflns         11134
_refine_ls_number_restraints     5600
_refine_ls_restrained_S_all      1.721
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.1065
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3397
_refine_ls_wR_factor_ref         0.3505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9632
_reflns_number_total             11134
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02901_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        7599.9(24)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C123.50 H49.50 Cl0.25 N4 Ni O Sc2'
_cod_database_code               4347227
_shelx_estimated_absorpt_t_min   0.916
_shelx_estimated_absorpt_t_max   0.952
_shelxl_version_number           2013-2
_shelx_res_checksum              33312
_shelx_hkl_checksum              96564