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_4032392
_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         '2(C107 H36 Lu3 N3), 5(C S2)'
_chemical_formula_sum            'C219 H72 Lu6 N6 O0 S10'
_chemical_formula_weight         4157.24
_chemical_name_common            'Lu3N@IhC80 NHC'
_chemical_name_systematic        'Lu3N@IhC80 NHC'
_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                99.143(5)
_cell_angle_beta                 106.102(5)
_cell_angle_gamma                106.977(5)
_cell_formula_units_Z            1
_cell_length_a                   11.028(5)
_cell_length_b                   17.708(5)
_cell_length_c                   19.684(5)
_cell_measurement_reflns_used    9381
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.355
_cell_measurement_theta_min      2.609
_cell_volume                     3410(2)
_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      173(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            40568
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         28.368
_diffrn_reflns_theta_min         2.608
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.528
_exptl_absorpt_correction_T_max  0.7434
_exptl_absorpt_correction_T_min  0.6744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_description       block
_exptl_crystal_F_000             2014
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.461
_refine_diff_density_min         -2.854
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1158
_refine_ls_number_reflns         16488
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0405P)^2^+23.1051P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13848
_reflns_number_total             16488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b03004_si_001.cif
_cod_data_source_block           Lu3N@IhC80
_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/ACS/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 

 Adding full bibliography for 4032391--4032392.cif.
;
_cod_database_code               4032392
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.587
_shelx_estimated_absorpt_t_max   0.636
_shelx_res_checksum              5599
_shelx_hkl_checksum              32514