Reductive Activation of C70 Equatorial Carbons and Structurally Characterized C70 δ-Adduct with Closed [5,6]-Ring Fusion.
Yang, Wei-Wei; Li, Zong-Jun; Li, Shu-Hui; Wu, Sheng-Li; Shi, Zujin; Gao, Xiang; The Journal of organic chemistry 82 (2017) 9253–9257; doi:10.1021/acs.joc.7b01756

data_4032707
_publ_section_title
;
 Reductive Activation of C70 Equatorial Carbons and Structurally
 Characterized C70 \d-Adduct with Closed [5,6]-Ring Fusion.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              9253
_journal_page_last               9257
_journal_paper_doi               10.1021/acs.joc.7b01756
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C78 H8, C S2'
_chemical_formula_sum            'C79 H8 S2'
_chemical_formula_weight         1020.97
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_Hall           '-I 4'
_space_group_name_H-M_alt        'I 4/m'
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.3119(7)
_cell_length_b                   24.3119(7)
_cell_length_c                   13.9782(8)
_cell_measurement_reflns_used    4260
_cell_measurement_temperature    187(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.68
_cell_volume                     8262.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      187.65
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22735
_diffrn_reflns_theta_full        26.05
_diffrn_reflns_theta_max         26.05
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.9830
_exptl_absorpt_correction_T_min  0.9609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;

;
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         4260
_refine_ls_number_restraints     1544
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1036
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0628P)^2^+15.9756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1707
_reflns_number_gt                2914
_reflns_number_total             4260
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo7b01756_si_003.cif
_cod_data_source_block           x203
_cod_database_code               4032707
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C4B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C30A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C1B(0.4) C9A(0.6) C14A(0.6) C13A(0.6) C12A(0.6) C30A(0.6)
 C14B(0.4) C26A(0.6) C32A(0.3) C31A(0.3) C29A(0.6) C28A(0.6) C16A(0.6)
 C15A(0.6) C7A(0.6) C7B(0.4) C8B(0.4) C17B(0.4) C18B(0.4) C6B(0.4) C3A(0.6)
 C4A(0.6) C5A(0.6) C6A(0.6) C18A(0.6) C19A(0.6) C20A(0.6) C21A(0.6) C22A(0.6)
 C23A(0.6) C17A(0.6) C33B(0.4) C32B(0.4) C37A(0.6) C35A(0.6) C33A(0.6)
 C34A(0.6) C25A(0.6) C24A(0.6) C36A(0.6) C2A(0.3) C1A(0.3) C27A(0.6) C25B(0.4)
 C29B(0.4) C30B(0.4) C3B(0.2) C28B(0.4) C27B(0.4) C15B(0.4) C16B(0.4) C26B(0.4)
 C9B(0.4) C8A(0.6) C11B(0.4) C10B(0.4) C12B(0.4) C19B(0.4) C35B(0.2) C23B(0.4)
 C34B(0.2) C24B(0.4) C20B(0.4) C22B(0.4) C2B(0.4) C4B(0.2) C5B(0.4) C21B(0.4)
 C13B(0.4) C31B(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B)
5.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C41(H41)
;
_olex2_submission_special_instructions 'No special instructions were received'