Stabilizing Three-Center Single-Electron Metal-Metal Bond in a Fullerene Cage
Yang, Shangfeng; Jin, Fei; Xin, Jinpeng; Guan, Runnan; Xie, Xiao-Ming; Chen, Muqing; Zhang, Qianyan; Popov, Alexey A.; Xie, Su-Yuan; Chemical Science  (2021) –; doi:10.1039/D1SC00965F

data_1561472
_publ_section_title
;
 Stabilizing Three-Center Single-Electron Metal-Metal Bond in a Fullerene
 Cage
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC00965F
_journal_year                    2021
_chemical_formula_moiety
'C2 Dy1.41, Dy1.59, 2(C60 H40 N10), C80, 3(C7 H8)'
_chemical_formula_sum            'C223 H104 Dy3 N20'
_chemical_formula_weight         3550.76
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-20 deposited with the CCDC.	2021-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.88
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.761
_cell_length_b                   32.102
_cell_length_c                   32.240
_cell_measurement_reflns_used    25501
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.712
_cell_measurement_theta_min      1.438
_cell_volume                     14949.947
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD MX300-HE'
_diffrn_measurement_method       ??phi_scans??
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_number            25480
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.712
_diffrn_reflns_theta_max         24.712
_diffrn_reflns_theta_min         1.438
_diffrn_source                   'SSRF, Beamline BL17B'
_exptl_absorpt_coefficient_mu    1.558
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_description       block
_exptl_crystal_F_000             7120
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.958
_refine_diff_density_min         -1.804
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2396
_refine_ls_number_reflns         25480
_refine_ls_number_restraints     1198
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0907
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1586P)^2^+56.2572P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2494
_refine_ls_wR_factor_ref         0.2709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20088
_reflns_number_total             25480
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00965f2.cif
_cod_data_source_block           Dy3C2@Ih(7)-C80
_cod_original_cell_volume        14949.9
_cod_database_code               1561472
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.652
_shelx_estimated_absorpt_t_min   0.652
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C306-C307
 1.54 with sigma of 0.02
 C106-C104 \\sim C105-C103 \\sim C104-C102 \\sim C103-C101 \\sim C102-C106
\\sim C101-C105
 with sigma of 0.05
 C106-C103 \\sim C105-C102 \\sim C104-C101
 with sigma of 0.05
 C706-C704 \\sim C705-C703 \\sim C704-C702 \\sim C703-C701 \\sim C702-C706
\\sim C701-C705
 with sigma of 0.05
 C706-C703 \\sim C705-C702 \\sim C704-C701
 with sigma of 0.05
3. Uiso/Uaniso restraints and constraints
C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim
C301 \\sim C302 \\sim C303 \\sim C304 \\sim C305 \\sim C306 \\sim C307: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.04
C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim
C701 \\sim C702 \\sim C703 \\sim C704 \\sim C705 \\sim C706 \\sim C707: within
2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Dy1 \\sim Dy2 \\sim Dy3 \\sim C81 \\sim C82 \\sim Dy4 \\sim Dy5 \\sim Dy6 \\sim
Dy7 \\sim Dy8 \\sim Dy9 \\sim Dy10 \\sim Dy11 \\sim Dy12 \\sim Dy13 \\sim Dy14
\\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim
C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim
C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim
C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim
C57 \\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim
C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim
C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim
C81 \\sim C82: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Others
 1*[Sof(Dy3)]+1*[Sof(Dy13)]+1*[Sof(Dy7)]+1*[Sof(Dy14)]+1*[Sof(Dy12)]=1 with
 esd of 0.0001
 1*[Sof(Dy1)]+1*[Sof(Dy5)]+1*[Sof(Dy4)]+1*[Sof(Dy6)]=1 with esd of 0.0001
 1*[Sof(Dy9)]+1*[Sof(Dy11)]+1*[Sof(Dy8)]+1*[Sof(Dy10)]+1*[Sof(Dy2)]=1 with esd
 of 0.0001
 Sof(C101)=Sof(H101)=Sof(C102)=Sof(H102)=Sof(C103)=Sof(H103)=Sof(C104)=
 Sof(H104)=Sof(C105)=Sof(H105)=Sof(C106)=Sof(C107)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=1-FVAR(14)
 Sof(C701)=Sof(H701)=Sof(C702)=Sof(H702)=Sof(C703)=Sof(H703)=Sof(C704)=
 Sof(H704)=Sof(C705)=Sof(H705)=Sof(C706)=Sof(C707)=Sof(H70A)=Sof(H70B)=
 Sof(H70C)=FVAR(14)
5.a Aromatic/amide H refined with riding coordinates:
 C521(H521), C522(H522), C523(H523), C524(H524), C525(H525), C526(H526),
 C527(H527), C528(H528), C529(H529), C530(H530), C531(H531), C532(H532),
 C533(H533), C534(H534), C535(H535), C536(H536), C537(H537), C538(H538),
 C539(H539), C540(H540), C541(H541), C542(H542), C543(H543), C544(H544),
 C545(H545), C546(H546), C547(H547), C548(H548), C549(H549), C550(H550),
 C551(H551), C552(H552), C553(H553), C554(H554), C555(H555), C556(H556),
 C557(H557), C558(H558), C559(H559), C560(H560), C621(H621), C622(H622),
 C623(H623), C624(H624), C625(H625), C626(H626), C627(H627), C628(H628),
 C629(H629), C630(H630), C631(H631), C632(H632), C633(H633), C634(H634),
 C635(H635), C636(H636), C637(H637), C638(H638), C639(H639), C640(H640),
 C641(H641), C642(H642), C643(H643), C644(H644), C645(H645), C646(H646),
 C647(H647), C648(H648), C649(H649), C650(H650), C651(H651), C652(H652),
 C653(H653), C654(H654), C655(H655), C656(H656), C657(H657), C658(H658),
 C659(H659), C660(H660), C101(H101), C102(H102), C103(H103), C104(H104),
 C105(H105), C201(H201), C202(H202), C203(H203), C204(H204), C205(H205),
 C301(H301), C302(H302), C303(H303), C304(H304), C305(H305), C701(H701),
 C702(H702), C703(H703), C704(H704), C705(H705)
5.b Idealised Me refined as rotating group:
 C107(H10A,H10B,H10C), C207(H20A,H20B,H20C), C307(H30A,H30B,H30C), C707(H70A,
 H70B,H70C)
;
_shelx_res_checksum              83919
_shelx_hkl_checksum              58490
_shelx_fab_checksum              37203
_olex2_submission_special_instructions 'No special instructions were received'