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_4130765
_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
'C54 H123 Ge18 Pd3 Sn6, C18 H36 K N2 O6, C18 H34 K N2 O6, C6 H14 O'
_chemical_formula_sum            'C96 H212 Ge18 K2 N4 O13 Pd3 Sn6'
_chemical_formula_weight         4046.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.851(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.3152(9)
_cell_length_b                   31.1602(17)
_cell_length_c                   26.1732(13)
_cell_measurement_reflns_used    9480
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.90
_cell_measurement_theta_min      2.37
_cell_volume                     14020.8(13)
_computing_cell_refinement       'Bruker SAINT v8.34A'
_computing_data_collection       'Bruker APEX-II v2013-10.0'
_computing_data_reduction        'Bruker SAINT v8.34A'
_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      120.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            245922
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.519
_diffrn_reflns_theta_min         1.020
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.318
_exptl_absorpt_correction_T_max  0.4144
_exptl_absorpt_correction_T_min  0.3080
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0819 before and 0.0534 after correction.
The Ratio of minimum to maximum transmission is 0.7432.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_description       block
_exptl_crystal_F_000             7888
_exptl_crystal_size_max          0.481
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.269
_refine_diff_density_max         4.970
_refine_diff_density_min         -2.954
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1318
_refine_ls_number_reflns         29056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+81.3530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21155
_reflns_number_total             29056
_reflns_threshold_expression     'I > 2\s(I)'
_olex2_submission_special_instructions 'No special instructions were received'
_cod_data_source_file            ja6b06545_si_002.cif
_cod_data_source_block           ge18pd3r6
_cod_database_code               4130765
_shelx_estimated_absorpt_t_max   0.329
_shelx_estimated_absorpt_t_min   0.184
_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.a Ternary CH refined with riding coordinates:
 C41(H41), C11(H11), C14(H14), C44(H44), C35(H35), C17(H17), C53(H53),
 C20(H20), C38(H38), C26(H26), C23(H23), C95(H95), C50(H50), C8(H8), C29(H29),
 C32(H32), C92(H92), C47(H47)
2.b Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C82(H82A,H82B), C68(H68A,H68B), C58(H58A,H58B), C60(H60A,
 H60B), C59(H59A,H59B), C65(H65A,H65B), C69(H69A,H69B), C57(H57A,H57B),
 C63(H63A,H63B), C62(H62A,H62B), C56(H56A,H56B), C86(H86A,H86B), C55(H55A,H55B),
  C66(H66A,H66B), C64(H64A,H64B), C67(H67A,H67B), C79(H79A,H79B), C84(H84A,
 H84B), C75(H75A,H75B), C74(H74A,H74B), C70(H70A,H70B), C80(H80A,H80B),
 C61(H61A,H61B), C72(H72A,H72B), C71(H71A,H71B), C90(H90A,H90B), C73(H73A,H73B),
  C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B), C76(H76A,H76B), C77(H77A,
 H77B), C85(H85A,H85B), C78(H78A,H78B)
2.c X=CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C7(H7A,H7B,H7C), C18(H18A,
 H18B,H18C), C30(H30A,H30B,H30C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C),
 C3(H3A,H3B,H3C), C19(H19A,H19B,H19C), C34(H34A,H34B,H34C), C24(H24A,H24B,H24C),
  C40(H40A,H40B,H40C), C94(H94A,H94B,H94C), C52(H52A,H52B,H52C), C96(H96A,H96B,
 H96C), C36(H36A,H36B,H36C), C27(H27A,H27B,H27C), C9(H9A,H9B,H9C), C21(H21A,
 H21B,H21C), C37(H37A,H37B,H37C), C48(H48A,H48B,H48C), C16(H16A,H16B,H16C),
 C39(H39A,H39B,H39C), C4(H4A,H4B,H4C), C25(H25A,H25B,H25C), C54(H54A,H54B,H54C),
  C91(H91A,H91B,H91C), C46(H46A,H46B,H46C), C93(H93A,H93B,H93C), C28(H28A,H28B,
 H28C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C6(H6A,H6B,H6C), C31(H31A,
 H31B,H31C), C33(H33A,H33B,H33C)
;
_shelx_shelxl_version_number     2014/7