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_4134519
_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
'C117 H14 Cu12 F99 O34, C8 H8 Cu F14 O8, 2(C6 H5 Cl)'
_chemical_formula_sum            'C137 H32 Cl2 Cu13 F113 O42'
_chemical_formula_weight         5393.54
_chemical_name_common            7F-12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                107.6850(10)
_cell_angle_beta                 108.6850(10)
_cell_angle_gamma                95.6440(10)
_cell_formula_units_Z            1
_cell_length_a                   13.5207(2)
_cell_length_b                   18.2853(3)
_cell_length_c                   18.8367(2)
_cell_measurement_reflns_used    25767
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.9360
_cell_measurement_theta_min      2.9630
_cell_volume                     4103.10(11)
_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      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_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    -85.00 -58.00   0.50    0.50    --    0.00 -19.00  60.00   54
  2  \w    -88.00 -58.00   0.50    0.50    --    0.00 -38.00 -30.00   60
  3  \w     55.00  82.00   0.50    0.50    --    0.00  38.00-120.00   54
  4  \w    -12.00  18.00   0.50    0.50    --    0.00 -19.00  60.00   60
  5  \w    -33.00  16.00   0.50    0.50    --    0.00 -38.00 -30.00   98
  6  \w     30.00  87.00   0.50    0.50    --    0.00  38.00-150.00  114
  7  \w    -39.00   1.00   0.50    0.50    --    0.00 -38.00-120.00   80
  8  \w    -88.00 -12.00   0.50    0.50    --    0.00 -77.00 150.00  152
  9  \w     35.00 126.00   0.50    2.00    --   95.80 -82.00-120.00  182
 10  \w     65.00 100.00   0.50    2.00    --   95.80 -82.00  30.00   70
 11  \w     74.00 101.00   0.50    2.00    --   95.80 -82.00 -60.00   54
 12  \w     80.00 184.00   0.50    2.00    --   95.80  30.00 120.00  208
 13  \w     12.00 116.00   0.50    2.00    --   95.80 -61.00-120.00  208
 14  \w      8.00 127.00   0.50    2.00    --   95.80 -82.00  60.00  238
 15  \w     46.00 110.00   0.50    2.00    --   95.80 -82.00 150.00  128
 16  \w    134.00 184.00   0.50    2.00    --   95.80  77.00 150.00  100
 17  \w     58.00 124.00   0.50    2.00    --   95.80 -82.00  90.00  132
 18  \w     10.00  39.00   0.50    2.00    --   95.80 -30.00  30.00   58
 19  \w     64.00 104.00   0.50    2.00    --   95.80 -30.00  30.00   80
 20  \w     10.00 111.00   0.50    2.00    --   95.80 -30.00 120.00  202
 21  \w     79.00 184.00   0.50    2.00    --   95.80  30.00  90.00  210
 22  \w     15.00  59.00   0.50    2.00    --   95.80 -82.00 -60.00   88
 23  \w     10.00 100.00   0.50    2.00    --   95.80 -15.00 120.00  180
 24  \w     94.00 124.00   0.50    2.00    --   95.80 -82.00 -50.03   60
 25  \w     14.00 113.00   0.50    2.00    --   95.80 -82.00   6.77  198
;
_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      -0.0047895000
_diffrn_orient_matrix_UB_12      -0.0833590000
_diffrn_orient_matrix_UB_13      -0.0547255000
_diffrn_orient_matrix_UB_21      0.0440112000
_diffrn_orient_matrix_UB_22      -0.0234826000
_diffrn_orient_matrix_UB_23      0.0741872000
_diffrn_orient_matrix_UB_31      -0.1149827000
_diffrn_orient_matrix_UB_32      -0.0265612000
_diffrn_orient_matrix_UB_33      -0.0058908000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45555
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.429
_diffrn_reflns_theta_min         2.979
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    4.021
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76264
_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    2.183
_exptl_crystal_description       needle
_exptl_crystal_F_000             2618
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.002
_refine_diff_density_max         2.076
_refine_diff_density_min         -1.503
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1521
_refine_ls_number_reflns         16148
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0898
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1717P)^2^+20.8055P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2559
_refine_ls_wR_factor_ref         0.2629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14261
_reflns_number_total             16148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00090_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4134518--4134521.cif.'
_cod_original_cell_volume        4103.09(11)
_cod_database_code               4134519
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H O F Cu'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H2Wa,H2Wb} of O2W
 At 1.5 times of:
  All O(H) groups, {H3Wa,H3Wb} of O3W, {H5Wa,H5Wb} of O5W, {H4Wa,H4Wb} of O4W,
   {H1Wa,H1Wb} of O1W
2. Restrained distances
 C53-C54
 1.5 with sigma of 0.02
 C53'-C52
 1.5 with sigma of 0.02
 F7'-C34'
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C58) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C34) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C53) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F39') \\sim Ueq, Uanis(F42) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(F5') \\sim Ueq, Uanis(F6') \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(F7') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F55) \\sim Ueq, Uanis(F54) \\sim Ueq, Uanis(F38) \\sim Ueq, Uanis(F49)
\\sim Ueq, Uanis(F47) \\sim Ueq, Uanis(F48) \\sim Ueq, Uanis(F5') \\sim Ueq,
Uanis(F7) \\sim Ueq, Uanis(F21') \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C53') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C34') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C58) = Uanis(C38)
Uanis(C53) = Uanis(C53')
Uanis(C42) = Uanis(C41')
4. Others
 Fixed Sof: F4(0.5) F4'(0.5) F5(0.5) F5'(0.5) F6(0.5) F6'(0.5) F7(0.5)
 F7'(0.5) F17(0.5) F17'(0.5) F18(0.5) F18'(0.5) F19(0.5) F19'(0.5) F20(0.5)
 F20'(0.5) F21(0.5) F21'(0.5) F38'(0.5) F39(0.5) F39'(0.5) F40(0.5) F40'(0.5)
 F41(0.5) F41'(0.5) F42(0.5) F42'(0.5) C34(0.5) C34'(0.5) C41(0.5) C41'(0.5)
 C42(0.5) C42'(0.5) C53'(0.5) C54(0.5) C54'(0.5)
5.a Rotating group:
 O1W(H1Wa,H1Wb), O3W(H3Wa,H3Wb), O4W(H4Wa,H4Wb), O5W(H5Wa,H5Wb)
5.b Secondary CH2 refined with riding coordinates:
 O2W(H2Wa,H2Wb)
5.c Aromatic/amide H refined with riding coordinates:
 C65(H65), C64(H64), C68(H68), C67(H67), C66(H66)
5.d Fitted hexagon refined as free rotating group:
 C65(C64,C63,C68,C67,C66)
5.e Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_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 1.828
_oxdiff_exptl_absorpt_empirical_full_min 0.500