[Pd4(μ3-SbMe3)4(SbMe3)4]: A Pd(0) Tetrahedron with μ3-Bridging Trimethylantimony Ligands.
Benjamin, Sophie L.; Krämer, Tobias; Levason, William; Light, Mark E.; Macgregor, Stuart A.; Reid, Gillian; Journal of the American Chemical Society 138 (2016) 6964–6967; doi:10.1021/jacs.6b04060

data_4130491
_publ_section_title
;
 [Pd4(\m3-SbMe3)4(SbMe3)4]: A Pd(0) Tetrahedron with \m3-Bridging
 Trimethylantimony Ligands.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6964
_journal_page_last               6967
_journal_paper_doi               10.1021/jacs.6b04060
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C24 H72 Pd4 Sb8'
_chemical_formula_sum            'C24 H72 Pd4 Sb8'
_chemical_formula_weight         1760.41
_chemical_name_systematic        octakis(trimethylstibine)tetrapalladium(0)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4966(4)
_cell_length_b                   13.0377(3)
_cell_length_c                   19.9791(5)
_cell_measurement_reflns_used    9049
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3590
_cell_measurement_theta_min      1.8850
_cell_volume                     4818.02(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega -103.00   73.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0000    0.0000 -180.0000 176

  2 omega  -11.00   -1.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.0000  -72.0000 -180.0000 10
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0232504000
_diffrn_orient_matrix_UB_12      -0.0389797000
_diffrn_orient_matrix_UB_13      0.0122599000
_diffrn_orient_matrix_UB_21      -0.0271116000
_diffrn_orient_matrix_UB_22      -0.0155779000
_diffrn_orient_matrix_UB_23      0.0229655000
_diffrn_orient_matrix_UB_31      -0.0139661000
_diffrn_orient_matrix_UB_32      -0.0346108000
_diffrn_orient_matrix_UB_33      -0.0241344000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10419
_diffrn_reflns_point_group_measured_fraction_full 0.826
_diffrn_reflns_point_group_measured_fraction_max 0.805
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.002
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.871
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.427
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Flack x determined using 1508 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         4573
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0246
_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^)+(0.0209P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0474
_reflns_Friedel_coverage         0.573
_reflns_Friedel_fraction_full    0.642
_reflns_Friedel_fraction_max     0.604
_reflns_number_gt                4359
_reflns_number_total             4573
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04060_si_003.cif
_cod_data_source_block           2014slbk412_ml
_cod_original_cell_volume        4818.0(2)
_cod_database_code               4130491
_reflns_odcompleteness_completeness 91.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.41
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C1B) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(C1A) = Uanis(C2A) = Uanis(C1B)
4. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H7C(0.5) H12A(0.5) H12B(0.5) H12C(0.5) H14A(0.5)
 H14B(0.5) H14C(0.5) C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C1A(0.5) H1AA(0.5)
 H1AB(0.5) H1AC(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) H2AC(0.5)
5.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C1B(H1BA,
 H1BB,H1BC), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC)
;
_shelx_res_checksum              2425
_shelx_hkl_checksum              9938
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'