[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_4135122
_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 Sn18, 4(C18 H36 K N2 O6), 4(C3 H7 N O)'
_chemical_formula_sum            'C84 H172 Cu4 K4 N12 O28 Sn18'
_chemical_formula_weight         4345.31
_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             2019-12-26
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                107.945(2)
_cell_angle_beta                 96.8800(10)
_cell_angle_gamma                112.688(2)
_cell_formula_units_Z            1
_cell_length_a                   15.6801(3)
_cell_length_b                   15.8817(3)
_cell_length_c                   16.6035(3)
_cell_measurement_reflns_used    19694
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.1790
_cell_measurement_theta_min      3.2630
_cell_volume                     3492.49(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.965
_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     21.00  89.00   0.50    0.65    --    0.00  82.00  90.00  136
  2  \w     26.00  87.00   0.50    0.65    --    0.00  57.00-180.00  122
  3  \w    -36.00 -10.00   0.50    0.65    --    0.00  57.00-180.00   52
  4  \w      6.00  60.00   0.50    0.65    --    0.00  77.00 -30.00  108
  5  \w    -42.00  17.00   0.50    0.65    --    0.00  82.00  90.00  118
  6  \w    -49.00  37.00   0.50    0.65    --    0.00 -77.00  30.00  172
  7  \w     22.00  95.00   0.50    2.61    --   98.20 -61.00 120.00  146
  8  \w     86.00 112.00   0.50    2.61    --   98.20 -82.00 120.00   52
  9  \w     31.00 105.00   0.50    2.61    --   98.20  15.00  60.00  148
 10  \w     44.00 186.00   0.50    2.61    --   98.20  30.00-120.00  284
 11  \w      9.00 140.00   0.50    2.61    --   98.20 -82.00  30.00  262
 12  \w     10.00 134.00   0.50    2.61    --   98.20 -61.00-150.00  248
 13  \w     11.00 123.00   0.50    2.61    --   98.20 -61.00  30.00  224
 14  \w     14.00 139.00   0.50    2.61    --   98.20 -82.00-150.00  250
 15  \w     33.00  58.00   0.50    2.61    --   98.20 -82.00 120.00   50
 16  \w     57.00 138.00   0.50    2.61    --   98.20  82.00   0.00  162
 17  \w     84.00 162.00   0.50    2.61    --   98.20  45.00 -90.00  156
 18  \w     34.00  60.00   0.50    2.61    --   98.20 -45.00 -60.00   52
 19  \w     84.00 111.00   0.50    2.61    --   98.20 -82.00 -30.00   54
 20  \w    101.00 178.00   0.50    2.61    --   98.20  45.00 -60.00  154
 21  \w     73.00  98.00   0.50    2.61    --   98.20 -82.00-120.00   50
 22  \w     75.00 103.00   0.50    2.61    --   98.20 -82.00 150.00   56
 23  \w     88.00 120.00   0.50    2.61    --   98.20 -82.00 -90.00   64
 24  \w     69.00  94.00   0.50    2.61    --   98.20 -82.00   0.00   50
 25  \w     81.00 106.00   0.50    2.61    --   98.20 -82.00  60.00   50
 26  \w    136.00 179.00   0.50    2.61    --   98.20  15.00  60.00   86
;
_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      0.0151194000
_diffrn_orient_matrix_UB_12      0.0957915000
_diffrn_orient_matrix_UB_13      0.0737073000
_diffrn_orient_matrix_UB_21      0.0744725000
_diffrn_orient_matrix_UB_22      -0.0096152000
_diffrn_orient_matrix_UB_23      0.0613619000
_diffrn_orient_matrix_UB_31      0.0804386000
_diffrn_orient_matrix_UB_32      0.0610776000
_diffrn_orient_matrix_UB_33      -0.0327607000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.965
_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       -20
_diffrn_reflns_number            38396
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.669
_diffrn_reflns_theta_min         2.907
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    27.274
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic grayish black'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_description       plate
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.242
_refine_diff_density_min         -1.371
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         13636
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0790P)^2^+5.1673P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1317
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11670
_reflns_number_total             13636
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c04815_si_002.cif
_cod_data_source_block           ql
_cod_original_cell_volume        3492.49(13)
_cod_database_code               4135122
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.078
_shelx_estimated_absorpt_t_min   0.051
_reflns_odcompleteness_completeness 99.45
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9-C10
 1.5 with sigma of 0.02
3. Others
 Sof(H7bc)=Sof(H7bd)=Sof(H10c)=Sof(H10d)=Sof(C9A)=Sof(H9Ab)=Sof(H9Aa)=Sof(C8A)=
 Sof(H8Aa)=Sof(H8Ab)=1-FVAR(1)
 Sof(H7aa)=Sof(H7ab)=Sof(H10a)=Sof(H10b)=Sof(C8)=Sof(H8a)=Sof(H8b)=Sof(C9)=
 Sof(H9a)=Sof(H9b)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C32(H32a,H32b), C22(H22a,H22b), C34(H34a,H34b), C33(H33a,H33b), C35(H35a,
 H35b), C36(H36a,H36b), C21(H21a,H21b), C20(H20a,H20b), C14(H14a,H14b),
 C28(H28a,H28b), C30(H30a,H30b), C5(H5a,H5b), C13(H13a,H13b), C6(H6a,H6b),
 C12(H12a,H12b), C19(H19a,H19b), C17(H17a,H17b), C25(H25a,H25b), C24(H24a,H24b),
  C3(H3a,H3b), C16(H16a,H16b), C4(H4a,H4b), C29(H29a,H29b), C18(H18a,H18b),
 C23(H23a,H23b), C26(H26a,H26b), C15(H15a,H15b), C11(H11a,H11b), C31(H31a,H31b),
  C2(H2a,H2b), C1(H1a,H1b), C7(H7aa,H7ab), C7(H7bc,H7bd), C27(H27a,H27b),
 C10(H10a,H10b), C10(H10c,H10d), C8(H8a,H8b), C9(H9a,H9b), C9A(H9Ab,H9Aa),
 C8A(H8Aa,H8Ab)
4.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C42(H42)
4.c Idealised Me refined as rotating group:
 C38(H38a,H38b,H38c), C37(H37a,H37b,H37c), C40(H40a,H40b,H40c), C41(H41a,H41b,
 H41c)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              94186
_shelx_hkl_checksum              48506
_shelx_fab_checksum              46638
_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 3.470
_oxdiff_exptl_absorpt_empirical_full_min 0.629