A Stannyl-Decorated Zintl Ion [Ge18Pd3(Sn(i)Pr3)6](2-): Twinned Icosahedron with a Common Pd3-Face or 18-Vertex Hypho-Deltahedron with a Pd3-Triangle Inside.
Perla, Luis G.; Sevov, Slavi C.; Journal of the American Chemical Society 138 (2016) 9795–9798; doi:10.1021/jacs.6b06545

data_4130764
_publ_section_title
;
 A Stannyl-Decorated Zintl Ion [Ge18Pd3(Sn(i)Pr3)6](2-): Twinned
 Icosahedron with a Common Pd3-Face or 18-Vertex Hypho-Deltahedron with a
 Pd3-Triangle Inside.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9795
_journal_page_last               9798
_journal_paper_doi               10.1021/jacs.6b06545
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C63 H147 Ge18 Pd3 Sn7, C56 H48 Cu N P3'
_chemical_formula_sum            'C119 H195 Cu Ge18 N P3 Pd3 Sn7'
_chemical_formula_weight         4252.85
_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
_audit_creation_date             2016-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                79.329(3)
_cell_angle_beta                 75.196(2)
_cell_angle_gamma                80.078(3)
_cell_formula_units_Z            2
_cell_length_a                   14.6690(11)
_cell_length_b                   22.4404(18)
_cell_length_c                   23.8287(19)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.41
_cell_volume                     7387.6(10)
_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_temperature      120.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_unetI/netI     0.0713
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            98657
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.607
_diffrn_reflns_theta_min         0.894
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.323
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.3134
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0962 before and 0.0689 after correction.
The Ratio of minimum to maximum transmission is 0.4204.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_description       block
_exptl_crystal_F_000             4108
_exptl_crystal_size_max          0.401
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.292
_refine_diff_density_max         1.527
_refine_diff_density_min         -1.833
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1427
_refine_ls_number_reflns         30450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0552P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1027
_refine_ls_wR_factor_ref         0.1112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22943
_reflns_number_total             30450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b06545_si_003.cif
_cod_data_source_block           ge18r7pd3
_cod_database_code               4130764
_shelx_estimated_absorpt_t_max   0.306
_shelx_estimated_absorpt_t_min   0.224
_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. Others
 Sof(C44B)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C46B)=Sof(H46D)=Sof(H46E)=
 Sof(H46F)=Sof(C45B)=Sof(H45B)=1-FVAR(1)
 Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C45A)=Sof(H45A)=Sof(C44A)=
 Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C23(H23), C54(H54), C51(H51), C11(H11), C0AA(H0AA), C5(H5), C32(H32),
 C60(H60), C48(H48), C8(H8), C17(H17), C20(H20), C14(H14), C29(H29), C63(H63),
 C26(H26), C39(H39), C42(H42), C57(H57), C35(H35), C45A(H45A), C45B(H45B)
3.b Aromatic/amide H refined with riding coordinates:
 C90(H90), C106(H106), C108(H108), C94(H94), C88(H88), C102(H102), C75(H75),
 C103(H103), C70(H70), C76(H76), C100(H100), C78(H78), C82(H82), C96(H96),
 C81(H81), C114(H114), C87(H87), C104(H104), C93(H93), C84(H84), C105(H105),
 C92(H92), C66(H66), C91(H91), C85(H85), C99(H99), C72(H72), C109(H109),
 C80(H80), C86(H86), C98(H98), C97(H97), C115(H115), C112(H112), C79(H79),
 C74(H74), C118(H118), C69(H69), C73(H73), C116(H116), C68(H68), C67(H67),
 C117(H117), C110(H110), C111(H111)
3.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C49(H49A,H49B,
 H49C), C58(H58A,H58B,H58C), C120(H12D,H12E,H12F), C25(H25A,H25B,H25C), C1(H1A,
 H1B,H1C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C30(H30A,H30B,H30C),
 C28(H28A,H28B,H28C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C59(H59A,H59B,
 H59C), C43(H43A,H43B,H43C), C6(H6A,H6B,H6C), C33(H33A,H33B,H33C), C22(H22A,
 H22B,H22C), C56(H56A,H56B,H56C), C1AA(H1AA,H1AB,H1AC), C47(H47A,H47B,H47C),
 C19(H19A,H19B,H19C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C), C50(H50A,H50B,
 H50C), C61(H61A,H61B,H61C), C31(H31A,H31B,H31C), C13(H13A,H13B,H13C), C4(H4A,
 H4B,H4C), C52(H52A,H52B,H52C), C27(H27A,H27B,H27C), C18(H18A,H18B,H18C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C7(H7A,H7B,H7C), C41(H41A,H41B,H41C),
  C16(H16A,H16B,H16C), C40(H40A,H40B,H40C), C34(H34A,H34B,H34C), C9(H9A,H9B,
 H9C), C46A(H46A,H46B,H46C), C44A(H44A,H44B,H44C), C44B(H44D,H44E,H44F),
 C46B(H46D,H46E,H46F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'