[Cu4@E18]4- (E=Sn, Pb): Fused Derivatives of Endohedral Stannaspherene and Plumbaspherene.
Lei, Qiao; Zhang, Chao; Shu, Cong-Cong; Morgan, Harry; McGrady, John E.; Sun, Zhong-Ming; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c04815

data_4135121
_publ_section_title
;
 [Cu4@E18]4- (E=Sn, Pb): Fused Derivatives of Endohedral Stannaspherene
 and Plumbaspherene.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c04815
_journal_year                    2020
_chemical_formula_moiety
'Cu4 Pb18, 4.032(C17.714 H35.428 K N2 O6), 4(C3 H7 N O)'
_chemical_formula_sum            'C84 H172 Cu4 K4 N12 O28 Pb18'
_chemical_formula_weight         5938.31
_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     dual
_audit_creation_date             2020-01-13
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                107.799(2)
_cell_angle_beta                 96.824(2)
_cell_angle_gamma                112.746(2)
_cell_formula_units_Z            1
_cell_length_a                   15.7192(4)
_cell_length_b                   15.9825(4)
_cell_length_c                   16.7031(3)
_cell_measurement_reflns_used    25916
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.3160
_cell_measurement_theta_min      2.8750
_cell_volume                     3547.99(17)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0506
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            41638
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.552
_diffrn_reflns_theta_min         2.886
_exptl_absorpt_coefficient_mu    42.676
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.09290
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'metallic dark black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.779
_exptl_crystal_description       plate
_exptl_crystal_F_000             2652
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.790
_refine_diff_density_min         -4.384
_refine_diff_density_rms         0.574
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         13878
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0520
_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^)+(0.1063P)^2^+13.4574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12630
_reflns_number_total             13878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04815_si_003.cif
_cod_data_source_block           12
_cod_original_cell_volume        3547.99(16)
_cod_database_code               4135121
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.040
_shelx_estimated_absorpt_t_min   0.031
_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 C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C25) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Others
 Sof(C28A)=Sof(H28A)=Sof(H28B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C22(H22A,H22B), C15(H15A,H15B), C25(H25A,H25B), C10(H10A,
 H10B), C35(H35A,H35B), C21(H21A,H21B), C9(H9A,H9B), C30(H30A,H30B), C17(H17A,
 H17B), C24(H24A,H24B), C13(H13A,H13B), C16(H16A,H16B), C20(H20A,H20B),
 C36(H36A,H36B), C26(H26A,H26B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,
 H6B), C12(H12A,H12B), C14(H14A,H14B), C8(H8A,H8B), C19(H19A,H19B), C1(H1A,H1B),
  C23(H23A,H23B), C7(H7A,H7B), C2(H2A,H2B), C27(H27A,H27B), C29(H29A,H29B),
 C18(H18A,H18B), C34(H34A,H34B), C33(H33A,H33B), C31(H31A,H31B), C32(H32A,H32B),
  C28A(H28A,H28B)
4.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C39(H39)
4.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C41(H41A,H41B,H41C), C40(H40A,H40B,H40C), C38(H38A,H38B,
 H38C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              86985
_shelx_hkl_checksum              67784
_shelx_fab_checksum              36552
_olex2_submission_special_instructions 'No special instructions were received'