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_4134521
_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         'C150 H120 Cu24 O72, 3(C20 H14 Cl2)'
_chemical_formula_sum            'C210 H162 Cl6 Cu24 O72'
_chemical_formula_weight         5575.05
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-01
_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                   25.6664(6)
_cell_length_b                   25.6664(6)
_cell_length_c                   24.6267(9)
_cell_measurement_reflns_used    9249
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      73.7100
_cell_measurement_theta_min      3.4250
_cell_volume                     14049.7(7)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_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    -48.00  15.00   0.50   10.00    --    0.00 -38.00  60.00  126
  2  \w    -84.00 -59.00   0.50   10.00    --    0.00 -38.00  60.00   50
  3  \w     33.00  58.00   0.50   10.00    --    0.00  27.00 -91.00   50
  4  \w     14.00 112.00   0.50   60.00    --   95.80 -30.00 -90.00  196
  5  \w    139.00 179.00   0.50   60.00    --   95.80  15.00 -30.00   80
  6  \w     72.00 102.00   0.50   60.00    --   95.80  15.00 -30.00   60
  7  \w      9.00 111.00   0.50   60.00    --   95.80 -27.00 106.00  204
  8  \w    150.00 176.00   0.50   60.00    --   95.80  15.00  90.00   52
  9  \w     85.00 130.00   0.50   60.00    --   95.80  15.00  90.00   90
;
_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      -0.0672352000
_diffrn_orient_matrix_UB_12      -0.0247037000
_diffrn_orient_matrix_UB_13      -0.0119109000
_diffrn_orient_matrix_UB_21      0.0117125000
_diffrn_orient_matrix_UB_22      -0.0030851000
_diffrn_orient_matrix_UB_23      -0.0609534000
_diffrn_orient_matrix_UB_31      -0.0120483000
_diffrn_orient_matrix_UB_32      -0.0647104000
_diffrn_orient_matrix_UB_33      0.0075112000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15603
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.216
_diffrn_reflns_theta_min         3.444
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.475
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_description       block
_exptl_crystal_F_000             8388
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.032
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         6122
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0904P)^2^+135.6152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1539
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5451
_reflns_number_total             6122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00090_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4134518--4134521.cif.'
_cod_original_cell_volume        14049.7(8)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4134521
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C H O Cu'
_reflns_odcompleteness_completeness 99.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C19-C20
 1.3 with sigma of 0.02
 O8'-O7
 2.2 with sigma of 0.02
 O8'-C20
 1.2 with sigma of 0.02
 Cl1'-C29
 1.5 with sigma of 0.02
 C28-Cl1'
 2.6 with sigma of 0.02
 C30-Cl1'
 2.6 with sigma of 0.02
3. Rigid bond restraints
 C26, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C28, C29
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C29, C30
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C30, C35
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C19) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C19') \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O8') \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Cl1') \\sim Ueq, Uanis(Cl1') \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Others
 Fixed Sof: O6(0.6) H6(0.6) O6'(0.4) H6'(0.4) O8(0.6) H8(0.6) O8'(0.4)
 H8'(0.4) C16(0.6) C16'(0.4) C17(0.6) H17A(0.6) H17B(0.6) C17'(0.4) H17C(0.4)
 H17D(0.4) C18(0.6) H18A(0.6) H18B(0.6) C18'(0.4) H18C(0.4) H18D(0.4) C19(0.6)
 H19A(0.6) H19B(0.6) C19'(0.4) H19C(0.4) H19D(0.4) Cl1(0.5) Cl1'(0.5) H26(0.5)
 H29(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C17'(H17C,
 H17D), C18(H18A,H18B), C18'(H18C,H18D), C19(H19A,H19B), C19'(H19C,H19D),
 C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
6.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C29(H29), C28(H28), C27(H27), C31(H31), C32(H32), C33(H33), C34(H34)
6.c Fitted hexagon refined as free rotating group:
 C26(C35,C30,C29,C28,C27)
6.d Idealised tetrahedral OH refined as rotating group:
 O6(H6), O6'(H6'), O8(H8), O8'(H8')
;
_shelx_res_checksum              51610
_shelx_hkl_checksum              84049
_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 5.732
_oxdiff_exptl_absorpt_empirical_full_min 0.635