Exohedral Cuprofullerene: Sequentially Expanding Metal Olefin Up to a C<sub>60</sub>@Cu<sub>24</sub> Rhombicuboctahedron.
Zhan, Shun-Ze; Zhang, Guo-Hui; Li, Jing-Hong; Liu, Jia-Li; Zhu, Si-Hui; Lu, Weigang; Zheng, Ji; Ng, Seik Weng; Li, Dan; Journal of the American Chemical Society 142 (2020) 5943–5947; doi:10.1021/jacs.0c00090

data_4134518
_publ_section_title
;
 Exohedral Cuprofullerene: Sequentially Expanding Metal Olefin Up to a
 C<sub>60</sub>@Cu<sub>24</sub> Rhombicuboctahedron.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5943
_journal_page_last               5947
_journal_paper_doi               10.1021/jacs.0c00090
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C84 H12 Cu6 F42 O18'
_chemical_formula_sum            'C84 H12 Cu6 F42 O18'
_chemical_formula_weight         2488.18
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.22334(8)
_cell_length_b                   14.22334(8)
_cell_length_c                   37.3147(2)
_cell_measurement_reflns_used    13744
_cell_measurement_temperature    100.01(15)
_cell_measurement_theta_max      73.9980
_cell_measurement_theta_min      3.7520
_cell_volume                     6537.53(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(15)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -89.00 -43.00   0.50    1.18    --    0.00 -58.00 119.00   92
  2  \w    -18.00   9.00   0.50    1.18    --    0.00  19.00  30.00   54
  3  \w    -16.00  32.00   0.50    1.18    --    0.00  38.00 120.00   96
  4  \w     42.00  87.00   0.50    1.18    --    0.00  19.00  30.00   90
  5  \w    -26.00   1.00   0.50    1.18    --    0.00 -58.00 119.00   54
  6  \w     35.00  75.00   0.50    1.18    --    0.00  38.00 120.00   80
  7  \w     14.00  44.00   0.50    4.71    --   95.80 -82.00   0.00   60
  8  \w      9.00 100.00   0.50    4.71    --   95.80 -30.00 120.00  182
  9  \w     72.00 185.00   0.50    4.71    --   95.80  15.00 -60.00  226
 10  \w     58.00 120.00   0.50    4.71    --   95.80 -82.00 -90.00  124
 11  \w     72.00 105.00   0.50    4.71    --   95.80 -82.00  60.00   66
 12  \w     81.00 134.00   0.50    4.71    --   95.80  45.00  90.00  106
 13  \w    149.00 175.00   0.50    4.71    --   95.80  45.00  90.00   52
 14  \w     53.00 122.00   0.50    4.71    --   95.80 -77.00 120.00  138
 15  \w     80.00 106.00   0.50    4.71    --   95.80  30.00   0.00   52
 16  \w     17.00  43.00   0.50    4.71    --   95.80 -77.00 120.00   52
 17  \w     67.00 115.00   0.50    4.71    --   95.80 -61.00-180.00   96
 18  \w    130.00 181.00   0.50    4.71    --   95.80  30.00   0.00  102
 19  \w     52.00 103.00   0.50    4.71    --   95.80 -82.00   0.00  102
 20  \w     11.00  37.00   0.50    4.71    --   95.80 -82.00 -90.00   52
 21  \w      7.00  97.00   0.50    4.71    --   95.80 -61.00   0.00  180
 22  \w     59.00 116.00   0.50    4.71    --   95.80 -82.00-150.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0909474000
_diffrn_orient_matrix_UB_12      0.0280851000
_diffrn_orient_matrix_UB_13      0.0041116000
_diffrn_orient_matrix_UB_21      0.0299354000
_diffrn_orient_matrix_UB_22      0.0271689000
_diffrn_orient_matrix_UB_23      0.0398199000
_diffrn_orient_matrix_UB_31      0.0804343000
_diffrn_orient_matrix_UB_32      0.1188011000
_diffrn_orient_matrix_UB_33      -0.0100979000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0104
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            17729
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.250
_diffrn_reflns_theta_min         3.553
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    3.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_description       block
_exptl_crystal_F_000             3636
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.526
_refine_diff_density_min         -1.290
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         1675
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1183
_refine_ls_R_factor_gt           0.1171
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+200.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3200
_refine_ls_wR_factor_ref         0.3211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1626
_reflns_number_total             1675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00090_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4134518--4134521.cif.'
_cod_original_cell_volume        6537.54(8)
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4134518
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H N F Cu'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C8-C9
 1.5 with sigma of 0.02
 C8-C7
 1.5 with sigma of 0.02
 F3-C9
 2.33 with sigma of 0.02
 C10-C9
 1.5 with sigma of 0.02
 F4-C10
 1.35 with sigma of 0.02
 F1-C8
 1.35 with sigma of 0.02
 C10-F1'
 2.33 with sigma of 0.02
 F1'-F2'
 2.33 with sigma of 0.02
 F2'-F3'
 2.33 with sigma of 0.02
 F4'-C10
 1.5 with sigma of 0.02
 C8'-C7
 1.5 with sigma of 0.02
 C8'-F2'
 2.1 with sigma of 0.02
 C9'-C8
 1.5 with sigma of 0.02
 C8-C9'
 1.2 with sigma of 0.02
 C9'-C7
 2.33 with sigma of 0.02
 F2'-C9'
 1.35 with sigma of 0.02
 C9'-F5'
 2.33 with sigma of 0.02
 C9'-C8'
 1.5 with sigma of 0.02
 C8'-C9'
 1.5 with sigma of 0.02
 F4'-C10'
 1.35 with sigma of 0.02
 F5'-C10'
 1.35 with sigma of 0.02
 C10'-C9'
 1.5 with sigma of 0.02
 F4'-F5'
 2.1 with sigma of 0.02
 F4'-F4'_$1
 2.1 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C10 \\sim C10': within 3.8A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F1') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F2') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F4') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F5') \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
Uanis(C8) \\sim Ueq, Uanis(C8') \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C9') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C10') \\sim Ueq, Uanis(C9') \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(F1) = Uanis(F1')
Uanis(F4') = Uanis(F3)
Uanis(C8) = Uanis(C8')
Uanis(C9) = Uanis(C9')
Uanis(C10) = Uanis(C10')
4. Others
 Fixed Sof: F1(0.5) F1'(0.5) F2(0.5) F2'(0.25) F3(0.25) F3'(0.25) F4(0.5)
 F4'(0.5) F5'(0.25) C8(0.25) C8'(0.25) C9(0.25) C9'(0.25) C10(0.25) C10'(0.25)
5.a Tetrahedral OH refined with riding coordinates:
 O1W(H1W)
;
_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 2.368
_oxdiff_exptl_absorpt_empirical_full_min 0.529