Regioselective Synthesis and Crystallographic Characterization of Isoxazoline-Ring-Fused Derivatives of Sc3N@Ih-C80 and C60.
Bao, Lipiao; Chen, Muqing; Shen, Wangqiang; Pan, Changwang; Ghiassi, Kamran B.; Olmstead, Marilyn M.; Balch, Alan L.; Akasaka, Takeshi; Lu, Xing; Inorganic chemistry 55 (2016) 4075–4077; doi:10.1021/acs.inorgchem.6b00631

data_4347805
_publ_section_title
;
 Regioselective Synthesis and Crystallographic Characterization of
 Isoxazoline-Ring-Fused Derivatives of Sc3N@Ih-C80 and C60.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4075
_journal_page_last               4077
_journal_paper_doi               10.1021/acs.inorgchem.6b00631
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C70 H9 Cl2 N O4'
_chemical_formula_sum            'C70 H9 Cl2 N O4'
_chemical_formula_weight         998.68
_chemical_name_common            C60PNO
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.938(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8893(13)
_cell_length_b                   13.0757(18)
_cell_length_c                   29.424(4)
_cell_measurement_reflns_used    9697
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.5145
_cell_measurement_theta_min      2.914
_cell_volume                     3804.3(9)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'Apex 2 v2014.09 (Bruker,2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker D8 quest'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            54163
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.519
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.244
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         7873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1114P)^2^+8.2639P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.1876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7577
_reflns_number_total             7873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00631_si_003.cif
_cod_data_source_block           lb04
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347805
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              9904
_shelx_hkl_checksum              87377