Reactions between N-Heterocyclic Carbene and Lutetium-Metallofullerenes: High Regioselectivity Directed by Electronic Effect in Addition to Steric Hindrance.
Shen, Wangqiang; Yang, Le; Wu, Yongbo; Bao, Lipiao; Li, Ying; Jin, Peng; Fang, Hongyun; Xie, Yunpeng; Lu, Xing; The Journal of organic chemistry 84 (2019) 606–612; doi:10.1021/acs.joc.8b02423

data_4035948
_publ_section_title
;
 Reactions between N-Heterocyclic Carbene and Lutetium-Metallofullerenes:
 High Regioselectivity Directed by Electronic Effect in Addition to Steric
 Hindrance.
;
_journal_issue                   2
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              606
_journal_page_last               612
_journal_paper_doi               10.1021/acs.joc.8b02423
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         'C103 H24 Lu2 N2, 3(C S2)'
_chemical_formula_sum            'C106 H24 Lu2 N2 S6'
_chemical_formula_weight         1867.57
_chemical_name_common            'Lu2@C2v-C82 NHC'
_chemical_name_systematic        'Lu2@C3v-C82 NHC'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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            4
_cell_length_a                   21.244(3)
_cell_length_b                   19.830(3)
_cell_length_c                   14.957(2)
_cell_measurement_reflns_used    9815
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.342
_cell_measurement_theta_min      3.061
_cell_volume                     6300.9(16)
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0589
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            62938
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.422
_diffrn_reflns_theta_min         2.888
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.381
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5378
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.459
_refine_diff_density_min         -1.659
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         5968
_refine_ls_number_restraints     1098
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1712
_refine_ls_R_factor_gt           0.1581
_refine_ls_shift/su_max          0.070
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1397P)^2^+131.4110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3720
_refine_ls_wR_factor_ref         0.3810
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5123
_reflns_number_total             5968
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b02423_si_003.cif
_cod_data_source_block           Lu2C3v_C82
_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/data/users/saulius/crontab/automatic-downloads/current/ACS/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        6301.0(15)
_cod_database_code               4035948
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.551
_shelx_estimated_absorpt_t_max   0.729
_shelx_res_checksum              87223
_shelx_hkl_checksum              92647