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_4134520
_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         'C120 H24 Cu24 F72 O60, 4(C7 H8), 18(H2 O)'
_chemical_formula_sum            'C148 H92 Cu24 F72 O78'
_chemical_formula_weight         6011.17
_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   difmap
_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                63.110(3)
_cell_angle_beta                 88.8395(17)
_cell_angle_gamma                86.946(2)
_cell_formula_units_Z            1
_cell_length_a                   17.7170(3)
_cell_length_b                   17.7627(6)
_cell_length_c                   17.8073(4)
_cell_measurement_reflns_used    31800
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      73.7610
_cell_measurement_theta_min      2.7700
_cell_volume                     4990.9(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.968
_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    -29.00  30.00   0.50    0.80    --    0.00  78.00 -33.00  118
  2  \w    -21.00   5.00   0.50    0.80    --    0.00  77.00-180.00   52
  3  \w    -26.00  89.00   0.50    0.80    --    0.00  82.00  90.00  230
  4  \w    -24.00  33.00   0.50    0.80    --    0.00  -8.00-166.44  114
  5  \w     31.00  57.00   0.50    0.80    --    0.00  57.00-150.00   52
  6  \w     36.00  69.00   0.50    0.80    --    0.00  77.00-180.00   66
  7  \w    -89.00 -36.00   0.50    0.80    --    0.00  -8.00-166.44  106
  8  \w     81.00 185.00   0.50    6.00    --   95.80  15.00 -90.00  208
  9  \w     12.00  94.00   0.50    6.00    --   95.80 -61.00 -60.00  164
 10  \w     14.00 105.00   0.50    6.00    --   95.80 -82.00  60.00  182
 11  \w     24.00 126.00   0.50    6.00    --   95.80 -82.00 -60.00  204
 12  \w     20.00  86.00   0.50    6.00    --   95.80 -61.00 150.00  132
 13  \w     14.00  58.00   0.50    6.00    --   95.80 -45.00   0.00   88
 14  \w     75.00 115.00   0.50    6.00    --   95.80 -45.00   0.00   80
 15  \w     83.00 109.00   0.50    6.00    --   95.80 -82.00  90.00   52
 16  \w     82.00 127.00   0.50    6.00    --   95.80  30.00 120.00   90
 17  \w     22.00 127.00   0.50    6.00    --   95.80 -82.00 150.00  210
 18  \w     63.00  97.00   0.50    6.00    --   95.80 -82.00 -90.00   68
 19  \w     79.00 126.00   0.50    6.00    --   95.80 -82.00   0.00   94
 20  \w     15.00 100.00   0.50    6.00    --   95.80 -61.00   0.00  170
 21  \w     74.00 178.00   0.50    6.00    --   95.80  15.00   0.00  208
 22  \w     98.00 123.00   0.50    6.00    --   95.80  30.00 -60.00   50
 23  \w    147.00 180.00   0.50    6.00    --   95.80  30.00 -60.00   66
 24  \w     79.00 124.00   0.50    6.00    --   95.80 -82.00-180.00   90
 25  \w     99.00 124.00   0.50    6.00    --   95.80 -82.00 120.00   50
 26  \w      6.00 109.00   0.50    6.00    --   95.80 -30.00 150.00  206
;
_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      -0.0067517000
_diffrn_orient_matrix_UB_12      0.0693322000
_diffrn_orient_matrix_UB_13      0.0294855000
_diffrn_orient_matrix_UB_21      -0.0734906000
_diffrn_orient_matrix_UB_22      0.0359160000
_diffrn_orient_matrix_UB_23      -0.0514730000
_diffrn_orient_matrix_UB_31      -0.0462186000
_diffrn_orient_matrix_UB_32      -0.0581619000
_diffrn_orient_matrix_UB_33      0.0767497000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            59746
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.211
_diffrn_reflns_theta_min         2.782
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    4.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92438
_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            red
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_description       block
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.859
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1429
_refine_ls_number_reflns         19675
_refine_ls_number_restraints     120
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0997P)^2^+19.9186P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17242
_reflns_number_total             19675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00090_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4134518--4134521.cif.'
_cod_original_cell_volume        4990.9(2)
_cod_database_code               4134520
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H O F Cu'
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H6Wa,H6Wb} of O6W, {H5Wa,H5Wb} of O5W, {H3Wa,H3Wb} of O3W,
   {H4Wa,H4Wb} of O4W, {H1Wa,H1Wb} of O1W, {H2Wa,H2Wb} of O2W, {H12a,H12b} of
  O12W, {H10a,H10b} of O10W, {H14a,H14b} of O14W, {H8Wa,H8Wb} of O8W, {H7Wa,
  H7Wb} of O7W, {H13a,H13b} of O13W, {H9Wa,H9Wb} of O9W, {H11a,H11b} of O11W
 At 1.5 times of:
  All C(H,H,H) groups, {H15a,H15b} of O15W, {H16a,H16b} of O16W
2. Uiso/Uaniso restraints and constraints
Uanis(C74) \\sim Ueq, Uanis(C73) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C71)
\\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C68) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C65) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C67) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C66)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C63) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O5W) \\sim Ueq, Uanis(O7W) \\sim Ueq, Uanis(O6W) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O3W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O8W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O15W) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: O15W(0.55) H15a(0.55) H15b(0.55) O16W(0.45) H16a(0.45) H16b(0.45)
4.a Riding coordinates:
 O1W(H1Wa,H1Wb), O2W(H2Wa,H2Wb), O3W(H3Wa,H3Wb), O4W(H4Wa,H4Wb), O5W(H5Wa,
 H5Wb), O6W(H6Wa,H6Wb), C53(C69,C70,H70,C71,H71,C72,H72,C73,H73,C74,H74),
 O7W(H7Wa,H7Wb), O8W(H8Wa,H8Wb), O9W(H9Wa,H9Wb), O10W(H10a,H10b), O11W(H11a,
 H11b), O12W(H12a,H12b), O13W(H13a,H13b), O14W(H14a,H14b), C61(H61a,H61b,H61c),
 C68(C62,C63,H63,C64,H64,C65,H65,C66,H66,C67,H67,H68a,H68b,H68c)
4.b Free rotating group:
 O15W(H15a,H15b), O16W(H16a,H16b)
;
_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 1.132
_oxdiff_exptl_absorpt_empirical_full_min 0.725