A copper-promoted synthesis of epoxy-bridged [60]fullerene-fused lactones and further derivatization.
Lu, Wen-Qiang; Zhou, Dian-Bing; Yin, Zheng-Chun; Liu, Qing-Song; Wang, Guan-Wu; Chemical communications (Cambridge, England) 57 (2021) 7043–7046; doi:10.1039/d1cc02669k

data_7128513
_publ_section_title
;
 A copper-promoted synthesis of epoxy-bridged [60]fullerene-fused lactones
 and further derivatization.
;
_journal_issue                   57
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7043
_journal_page_last               7046
_journal_paper_doi               10.1039/d1cc02669k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '2(C S2), C75 H13 O2'
_chemical_formula_sum            'C77 H13 O2 S4'
_chemical_formula_weight         1098.11
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-02-25
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-02-25 deposited with the CCDC.	2021-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.49560(18)
_cell_length_b                   21.1248(5)
_cell_length_c                   16.7633(3)
_cell_measurement_reflns_used    5217
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.6660
_cell_measurement_theta_min      4.8860
_cell_volume                     4424.96(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 97-2 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2169
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -113.00 -21.00   1.00    5.00    --  -41.05 -57.00 120.00   92
  2  \w      3.00  32.00   1.00    5.00    --   41.05 -99.00-150.00   29
  3  \w    -21.00   8.00   1.00    5.00    --   41.05 -77.00  30.00   29
  4  \w    114.00 173.00   1.00   12.00    --   99.68 125.00 -30.00   59
  5  \w    111.00 175.00   1.00   12.00    --   99.68 104.00 -84.00   64
  6  \w     99.00 171.00   1.00   12.00    --   99.68  45.00-180.00   72
  7  \w    101.00 172.00   1.00   12.00    --   99.68  45.00  90.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0610343000
_diffrn_orient_matrix_UB_12      0.0398195000
_diffrn_orient_matrix_UB_13      -0.0620496000
_diffrn_orient_matrix_UB_21      -0.0198341000
_diffrn_orient_matrix_UB_22      -0.0514778000
_diffrn_orient_matrix_UB_23      -0.0633933000
_diffrn_orient_matrix_UB_31      -0.1052577000
_diffrn_orient_matrix_UB_32      0.0328874000
_diffrn_orient_matrix_UB_33      -0.0240861000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10959
_diffrn_reflns_theta_full        70.09
_diffrn_reflns_theta_max         70.09
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.479
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2220
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         4222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0659
_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^)+(0.0636P)^2^+4.0408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1622
_refine_ls_wR_factor_ref         0.1692
_reflns_number_gt                3597
_reflns_number_total             4222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1cc02669k2.cif
_cod_data_source_block           lwqet3sihp2
_cod_depositor_comments
'Adding full bibliography for 7128512--7128513.cif.'
_cod_original_cell_volume        4424.97(15)
_cod_database_code               7128513
_chemical_oxdiff_formula         C75H14O3
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: O2(0.5) C33(0.5) H33A(0.5) H33B(0.5) H3(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B)
3.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C37(H37), C38(H38), C40(H40), C39(H39)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.610
_oxdiff_exptl_absorpt_empirical_full_min 0.700