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_4347806
_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         'C90.50 H9 Cl2 N2 O4 S Sc3'
_chemical_formula_sum            'C90.5 H9 Cl2 N2 O4 S Sc3'
_chemical_formula_weight         1425.84
_chemical_name_common            Sc3N@C80PNO
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.9451(10)
_cell_length_b                   24.9451(10)
_cell_length_c                   15.7646(7)
_cell_measurement_reflns_used    9572
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.5095
_cell_measurement_theta_min      2.654
_cell_volume                     9809.6(7)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'Apex2 (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXTL XT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 CMOS detector'
_diffrn_measurement_method       '\f/\w scans'
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            99942
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         30.647
_diffrn_reflns_theta_min         1.780
_diffrn_source                   'ALS, Beamline 11.3.1'
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.7486
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_description       block
_exptl_crystal_F_000             5688
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         4.666
_refine_diff_density_min         -2.225
_refine_diff_density_rms         0.246
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.367
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1693
_refine_ls_number_reflns         11716
_refine_ls_number_restraints     8671
_refine_ls_restrained_S_all      2.560
_refine_ls_R_factor_all          0.2010
_refine_ls_R_factor_gt           0.1928
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.003
_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          0.5896
_refine_ls_wR_factor_ref         0.5993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10561
_reflns_number_total             11716
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00631_si_002.cif
_cod_data_source_block           Sc3N@C80PNO
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        9809.6(9)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_original_formula_sum        'C90.50 H9 Cl2 N2 O4 S Sc3'
_cod_database_code               4347806
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.925
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              29534
_shelx_hkl_checksum              88433