Synthesis, characterization and electronic properties of an endohedral plumbaspherene [Au@Pb12]3−
Li, Lei-Jiao; Pan, Fu-Xing; Li, Feng-Yu; Chen, Zhong-Fang; Sun, Zhong-Ming; Inorganic Chemistry Frontiers 4 (2017) 1393–; doi:10.1039/C7QI00209B

data_4349710
_publ_section_title
;
 Synthesis, characterization and electronic properties of an endohedral
 plumbaspherene [Au@Pb12]3&#x2212;
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1393
_journal_paper_doi               10.1039/C7QI00209B
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety
'2(Au0.5 Pb6), C16 H30 K N2 O6, C18 H36 K N2 O6, C18 H34 K N2 O6, 2(C5 H5 N)'
_chemical_formula_sum            'C63 H112 Au K3 N8 O18 Pb12'
_chemical_formula_weight         4070.15
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-08-18
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-06-27 deposited with the CCDC.
2017-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                95.424(2)
_cell_angle_beta                 93.193(2)
_cell_angle_gamma                109.314(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4831(14)
_cell_length_b                   14.7999(15)
_cell_length_c                   27.189(3)
_cell_measurement_reflns_used    3066
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.225
_cell_measurement_theta_min      2.223
_cell_volume                     5451.8(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.1407
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31502
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.47
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    19.956
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1163 before and 0.0478 after correction.
The Ratio of minimum to maximum transmission is 0.6475.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            DARK
_exptl_crystal_density_diffrn    2.479
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3620
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.172
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         19097
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1447
_refine_ls_R_factor_gt           0.0677
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1715
_refine_ls_wR_factor_ref         0.2043
_reflns_number_gt                9821
_reflns_number_total             19097
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7qi00209b2.cif
_cod_data_source_block           20151012p_0m
_cod_original_cell_volume        5451.7(9)
_cod_database_code               4349710
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 H38A-H71B
 2 with sigma of 0.01
 H24A-H37B
 2 with sigma of 0.01
 C40B-C39B
 1.35 with sigma of 0.01
 C70-C71
 1.35 with sigma of 0.01
 C21-C46C
 1.35 with sigma of 0.01
 C47-C48
 1.35 with sigma of 0.01
3. Rigid bond restraints
 O14, C72
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21, C46C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N4, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N3, C42B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O8, C39B
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C72) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C90) \\sim Ueq,
Uanis(C91) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.002 and sigma for
terminal atoms of 0.001
5. Others
 Sof(Pb1)=1-FVAR(1)
 Sof(Pb11)=FVAR(1)
 Sof(Pb16)=1-FVAR(2)
 Sof(Pb14)=FVAR(2)
 Sof(Pb17)=1-FVAR(3)
 Sof(Pb15)=FVAR(3)
 Sof(Pb18)=1-FVAR(4)
 Sof(Pb10)=FVAR(4)
 Sof(Pb)=1-FVAR(5)
 Sof(Pb13)=FVAR(5)
 Fixed Sof: C71(0.5) H71A(0.5) H71B(0.5) C70(0.5) H70A(0.5) H70B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2AA(H2AA,H2AB), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,
 H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
  C3AA(H3AA,H3AB), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,
 H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C24(H24A,H24B), C28A(H28A,H28B), C29A(H29A,H29B), C30A(H30A,
 H30B), C31A(H31A,H31B), C32A(H32A,H32B), C33A(H33A,H33B), C35B(H35A,H35B),
 C36B(H36A,H36B), C37B(H37A,H37B), C38B(H38A,H38B), C39B(H39A,H39B), C40B(H40A,
 H40B), C41B(H41A,H41B), C43B(H43A,H43B), C44B(H44A,H44B), C45C(H45A,H45B),
 C46C(H46A,H46B), C47(H47A,H47B), C51C(H51A,H51B), C53C(H53A,H53B), C2(H2A,H2B),
  C71(H71A,H71B), C70(H70A,H70B), C72(H72A,H72B), C48(H48A,H48B), C1AA(H1AA,
 H1AB), C7AA(H7AA,H7AB), C0AA(H0AA,H0AB), C6AA(H6AA,H6AB)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C57D(H57D), C58D(H58D), C59D(H59D), C62D(H62D), C64(H64), C65(H65),
 C63(H63), C91(H91), C90(H90)
;
_olex2_submission_special_instructions 'No special instructions were received'