Single Crystal Structures and Theoretical Calculations of Uranium Endohedral Metallofullerenes (U@C2n, 2n=74, 82) Show Cage Isomer Dependent Oxidation States for U
Cai, Wenting; Morales-Martínez, Roser; Zhang, Xingxing; Najera, Daniel; Romero, Elkin; Metta Magana, Alejandro Jose; Rodriguez-Fortea, Antonio; Fortier, Skye; Chen, Ning; Poblet, Josep M.; Echegoyen, Luis; Chem. Sci.  (2017) –; doi:10.1039/C7SC01711A

data_1546092
_publ_section_title
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 Single Crystal Structures and Theoretical Calculations of Uranium
 Endohedral Metallofullerenes (U@C2n, 2n=74, 82) Show Cage Isomer
 Dependent Oxidation States for U
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_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC01711A
_journal_year                    2017
_chemical_formula_sum            'C128 H53 N4 Ni S2 U'
_chemical_formula_weight         2007.60
_chemical_name_systematic
;
 ?
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_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-12-13 deposited with the CCDC.
2017-05-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.3760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7846(5)
_cell_length_b                   17.2807(5)
_cell_length_c                   26.6533(7)
_cell_measurement_reflns_used    28272
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      136.643
_cell_measurement_theta_min      6.177
_cell_volume                     7817.6(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            94768
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.394
_diffrn_reflns_theta_min         1.200
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.431
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4004
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.882
_refine_diff_density_min         -1.483
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.737
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2045
_refine_ls_number_reflns         14336
_refine_ls_number_restraints     15663
_refine_ls_restrained_S_all      2.286
_refine_ls_R_factor_all          0.1324
_refine_ls_R_factor_gt           0.0987
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2627
_refine_ls_wR_factor_ref         0.2849
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9344
_reflns_number_total             14336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc01711a2.cif
_cod_data_source_block           6666
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
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_cod_database_code               1546092
_shelxl_version_number           2013-2
_shelx_res_checksum              86366