Evidence of Oxygen Activation in the Reaction between an N-Heterocyclic Carbene and M3N@Ih(7)-C80: An Unexpected Method of Steric Hindrance Release.
Chen, Muqing; Shen, Wangqiang; Peng, Ping; Bao, Lipiao; Zhao, Shasha; Xie, Yunpeng; Jin, Peng; Fang, Hongyun; Li, Fang-Fang; Lu, Xing; The Journal of organic chemistry 82 (2017) 3500–3505; doi:10.1021/acs.joc.6b03004

data_4032391
_publ_section_title
;
 Evidence of Oxygen Activation in the Reaction between an N-Heterocyclic
 Carbene and M3N@Ih(7)-C80: An Unexpected Method of Steric Hindrance
 Release.
;
_journal_issue                   7
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              3500
_journal_page_last               3505
_journal_paper_doi               10.1021/acs.joc.6b03004
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C107 H36 N3 Sc3, 2.5(C S2)'
_chemical_formula_sum            'C109.5 H36 N3 S5 Sc3'
_chemical_formula_weight         1688.59
_chemical_name_common            Sc3N@C80-NHC-2a
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                99.562(3)
_cell_angle_beta                 105.779(3)
_cell_angle_gamma                107.217(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9903(19)
_cell_length_b                   17.558(3)
_cell_length_c                   19.758(4)
_cell_measurement_reflns_used    3267
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      21.886
_cell_measurement_theta_min      2.224
_cell_volume                     3376.1(11)
_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    'SHELXTL XT-2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12355
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.426
_diffrn_reflns_theta_min         1.260
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             1714
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.924
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.0077(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         12355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0784
_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^)+(0.1185P)^2^+5.6752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2050
_refine_ls_wR_factor_ref         0.2401
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7675
_reflns_number_total             12355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b03004_si_003.cif
_cod_data_source_block           Sc3N@C80-NHC
_cod_depositor_comments
;
Adding full bibliography for 4032391--4032392.cif.

2020-12-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C219 H72 N6 S10 Sc6'
_cod_original_formula_weight         3377.18
_cod_original_formula_moiety         '2(C107 H36 N3 Sc3), 5(C S2)'
_cod_original_formula_units_Z            1
_cod_original_cell_volume        3376.2(10)
_cod_database_code               4032391
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.980
_shelx_estimated_absorpt_t_max   0.992
_shelx_res_checksum              2550
_shelx_hkl_checksum              8585