Eclipsed- and Staggered-[Ge18Pd3{E(i)Pr3}6](2-) (E = Si, Sn): Positional Isomerism in Deltahedral Zintl Clusters.
Perla, Luis G.; Muñoz-Castro, Alvaro; Sevov, Slavi C.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08562

data_4126600
_publ_section_title
;
 Eclipsed- and Staggered-[Ge18Pd3{E(i)Pr3}6](2-) (E = Si, Sn): Positional
 Isomerism in Deltahedral Zintl Clusters.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08562
_journal_year                    2017
_chemical_formula_moiety
'C108 H198 Ge18 Pd3 Sn6, C18 H36 K N2 O6, C18 H35 K N2 O6, 2(C4 H8 O)'
_chemical_formula_sum            'C156 H294 Ge18 K2 N4 O15 Pd3 Sn6'
_chemical_formula_weight         4882.09
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-27
_audit_creation_method
;
Olex2 1.2
(compiled Jul 19 2017 14:18:06 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                95.902(3)
_cell_angle_beta                 90.310(3)
_cell_angle_gamma                113.358(3)
_cell_formula_units_Z            2
_cell_length_a                   16.848(4)
_cell_length_b                   19.140(5)
_cell_length_c                   32.176(8)
_cell_measurement_reflns_used    9151
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.17
_cell_volume                     9463(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      120.52
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.848
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.923
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            187718
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.442
_diffrn_reflns_theta_min         0.637
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.957
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4911
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1308 before and 0.0521 after correction.
The Ratio of minimum to maximum transmission is 0.6586.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             4860
_exptl_crystal_size_max          0.645
_exptl_crystal_size_mid          0.384
_exptl_crystal_size_min          0.384
_refine_diff_density_max         1.847
_refine_diff_density_min         -1.312
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1742
_refine_ls_number_reflns         44513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0329P)^2^+79.0464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1010
_reflns_Friedel_coverage         0.000
_reflns_number_gt                37801
_reflns_number_total             44513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08562_si_003.cif
_cod_data_source_block           ge18pd3(sncy3)6
_cod_database_code               4126600
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.312
_shelx_estimated_absorpt_t_min   0.185
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C67(H67), C79(H79), C103(H103), C91(H91), C7(H7), C61(H61), C55(H55),
 C85(H85), C97(H97), C19(H19), C73(H73), C49(H49), C1(H1), C37(H37), C31(H31),
 C13(H13), C43(H43), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C8(H8A,H8B), C92(H92A,H92B), C10(H10A,H10B), C108(H10C,H10D),
 C84(H84A,H84B), C82(H82A,H82B), C104(H10E,H10F), C96(H96A,H96B), C59(H59A,
 H59B), C60(H60A,H60B), C107(H10G,H10H), C83(H83A,H83B), C78(H78A,H78B),
 C11(H11A,H11B), C106(H10I,H10J), C93(H93A,H93B), C68(H68A,H68B), C69(H69A,
 H69B), C101(H10K,H10L), C12(H12A,H12B), C81(H81A,H81B), C63(H63A,H63B),
 C54(H54A,H54B), C71(H71A,H71B), C80(H80A,H80B), C72(H72A,H72B), C64(H64A,H64B),
  C126(H12C,H12D), C102(H10M,H10N), C62(H62A,H62B), C118(H11C,H11D), C56(H56A,
 H56B), C70(H70A,H70B), C65(H65A,H65B), C66(H66A,H66B), C94(H94A,H94B),
 C119(H11E,H11F), C42(H42A,H42B), C2(H2A,H2B), C5(H5A,H5B), C38(H38A,H38B),
 C57(H57A,H57B), C32(H32A,H32B), C143(H14C,H14D), C117(H11G,H11H), C105(H10O,
 H10P), C95(H95A,H95B), C48(H48A,H48B), C115(H11I,H11J), C6(H6A,H6B), C100(H10Q,
 H10R), C120(H12E,H12F), C14(H14A,H14B), C98(H98A,H98B), C58(H58A,H58B),
 C39(H39A,H39B), C51(H51A,H51B), C144(H14E,H14F), C129(H12Q,H12R), C40(H40A,
 H40B), C50(H50A,H50B), C74(H74A,H74B), C20(H20A,H20B), C53(H53A,H53B),
 C109(H10S,H10T), C77(H77A,H77B), C86(H86A,H86B), C110(H11K,H11L), C125(H12G,
 H12H), C52(H52A,H52B), C18(H18A,H18B), C24(H24A,H24B), C130(H13A,H13B),
 C22(H22A,H22B), C121(H12I,H12J), C75(H75A,H75B), C131(H13C,H13D), C116(H11M,
 H11N), C34(H34A,H34B), C142(H14G,H14H), C41(H41A,H41B), C123(H12K,H12L),
 C135(H13E,H13F), C76(H76A,H76B), C114(H11O,H11P), C30(H30A,H30B), C21(H21A,
 H21B), C33(H33A,H33B), C122(H12M,H12N), C15(H15A,H15B), C99(H99A,H99B),
 C124(H12O,H12P), C133(H13G,H13H), C111(H11Q,H11R), C4(H4A,H4B), C16(H16A,H16B),
  C112(H11S,H11T), C113(H11U,H11V), C156(H15C,H15D), C36(H36A,H36B), C87(H87A,
 H87B), C23(H23A,H23B), C88(H88A,H88B), C47(H47A,H47B), C26(H26A,H26B),
 C27(H27A,H27B), C132(H13I,H13J), C128(H12S,H12T), C35(H35A,H35B), C141(H14I,
 H14J), C17(H17A,H17B), C29(H29A,H29B), C89(H89A,H89B), C28(H28A,H28B),
 C90(H90A,H90B), C3(H3A,H3B), C137(H13K,H13L), C127(H12U,H12V), C44(H44A,H44B),
 C138(H13M,H13N), C46(H46A,H46B), C139(H13O,H13P), C136(H13Q,H13R), C45(H45A,
 H45B), C154(H15E,H15F), C140(H14K,H14L), C153(H15G,H15H), C155(H15I,H15J),
 C146(H14M,H14N), C145(H14O,H14P), C148(H14Q,H14R), C147(H14S,H14T)
2.c Aromatic/amide H refined with riding coordinates:
 C134(H134)
;
_shelx_res_checksum              43022
_shelx_hkl_checksum              35920
_shelx_fab_checksum              11985
_olex2_submission_special_instructions 'No special instructions were received'