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_4126599
_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         'C54 H126 Ge18 Pd3 Si6, 2(C18 H36 K N2 O6)'
_chemical_formula_sum            'C90 H198 Ge18 K2 N4 O12 Pd3 Si6'
_chemical_formula_weight         3401.07
_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
_atom_sites_solution_primary     dual
_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                95.184(2)
_cell_angle_beta                 91.202(3)
_cell_angle_gamma                117.634(2)
_cell_formula_units_Z            2
_cell_length_a                   16.1039(6)
_cell_length_b                   17.0961(6)
_cell_length_c                   27.6983(10)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      71.69
_cell_measurement_theta_min      2.94
_cell_volume                     6711.1(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      120.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            146165
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         71.881
_diffrn_reflns_theta_min         2.936
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.006
_exptl_absorpt_correction_T_max  0.2619
_exptl_absorpt_correction_T_min  0.1271
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1127 before and 0.0855 after correction.
The Ratio of minimum to maximum transmission is 0.4853.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       plate
_exptl_crystal_F_000             3396
_refine_diff_density_max         1.361
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1299
_refine_ls_number_reflns         24986
_refine_ls_number_restraints     321
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0678P)^2^+22.8532P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1661
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18451
_reflns_number_total             24986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08562_si_002.cif
_cod_data_source_block           ge18pd3si6
_cod_database_code               4126599
_shelx_shelxl_version_number     2016
_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, All C(H,H,H,H,H,H) groups
2. Rigid bond restraints
 C49, C46, C47, C48, C52, C53, C54, C51, C50
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C10, C11, C12, C16, C17, C18, C13, C14, C15
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C43, C44, C45, O12, C39, C40, C38, C41, C37, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1B, C2B, C4B, C5B, C7B, C8B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1A, C2A, C4A, C5A, C7A, C8A, C6, C9, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32, C33, C30, C28, C31, C29, C35, C36, C34
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Rigid body (RIGU) restrains
 C79, C80, C81, C82, C83, C84, N3, N4, O9, O10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C73, C74, C75, C76, C77, C78, O7, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C85, C86, C87, C88, C89, C90, O11, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C46, C47, C48, C52, C53, C54, C51, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C11, C12, C16, C17, C18, C13, C14, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C43, C44, C45, C39, C40, C38, C41, C37, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1B, C2B, C4B, C5B, C7B, C8B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C2A, C4A, C5A, C7A, C8A, C6, C9, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C33, C30, C28, C31, C29, C35, C36, C34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C1B)=Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=Sof(C2B)=Sof(H2B)=Sof(C4B)=Sof(H4BA)=
 Sof(H4BB)=Sof(H4BC)=Sof(C5B)=Sof(H5B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=
 Sof(C8B)=Sof(H8B)=Sof(H6BD)=Sof(H6BE)=Sof(H6BF)=Sof(H9BD)=Sof(H9BE)=Sof(H9BF)=
 Sof(H3BD)=Sof(H3BE)=Sof(H3BF)=1-FVAR(1)
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2A)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(H4AC)=Sof(C5A)=Sof(H5A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=
 Sof(C8A)=Sof(H8A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=
 Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C2A(H2A), C5A(H5A), C8A(H8A), C2B(H2B), C5B(H5B), C8B(H8B), C32(H32),
 C11(H11), C17(H17), C20(H20), C23(H23), C26(H26), C44(H44), C47(H47), C53(H53),
  C14(H14), C38(H38), C41(H41), C50(H50), C29(H29), C35(H35)
5.b Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,
 H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B),
  C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,
 H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B),
 C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B),
  C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,
 H87B), C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B)
5.c Me refined with riding coordinates:
 C1A(H1AA,H1AB,H1AC), C4A(H4AA,H4AB,H4AC), C7A(H7AA,H7AB,H7AC), C1B(H1BA,H1BB,
 H1BC), C4B(H4BA,H4BB,H4BC), C7B(H7BA,H7BB,H7BC), C6(H6AA,H6AB,H6AC), C6(H6BD,
 H6BE,H6BF), C9(H9AA,H9AB,H9AC), C9(H9BD,H9BE,H9BF), C3(H3AA,H3AB,H3AC),
 C3(H3BD,H3BE,H3BF), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C)
5.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C49(H49A,H49B,H49C), C10(H10A,H10B,H10C), C12(H12A,H12B,
 H12C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,
 H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C),
 C27(H27A,H27B,H27C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C13(H13A,
 H13B,H13C), C15(H15A,H15B,H15C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C51(H51A,H51B,H51C), C42(H42A,H42B,H42C), C28(H28A,H28B,H28C), C31(H31A,H31B,
 H31C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              26619
_shelx_hkl_checksum              62282
_shelx_fab_checksum              57450
_olex2_submission_special_instructions 'No special instructions were received'