[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_4130492
_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         'C8 H24 Cl8 Pd2 Sb4'
_chemical_formula_sum            'C8 H24 Cl8 Pd2 Sb4'
_chemical_formula_weight         1103.74
_chemical_name_systematic
bis(dimethylchlorostibine)dichloridoplalladium(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2016-03-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.761(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6504(4)
_cell_length_b                   10.0441(3)
_cell_length_c                   13.2924(5)
_cell_measurement_reflns_used    4566
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.6720
_cell_measurement_theta_min      2.1870
_cell_volume                     1251.44(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -107.00  31.00   1.00    5.00    --  -17.00 -24.00 120.00  138
  2  \w    -71.00  -2.00   1.00    5.00    --  -17.00 -72.00 -30.00   69
  3  \w    -25.00  14.00   1.00    5.00    --  -17.00 -72.00 120.00   39
  4  \w   -107.00 -56.00   1.00    5.00    --  -17.00 -72.00-180.00   51
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support MiTeGen
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0463946000
_diffrn_orient_matrix_UB_12      0.0518683000
_diffrn_orient_matrix_UB_13      0.0235680000
_diffrn_orient_matrix_UB_21      -0.0414197000
_diffrn_orient_matrix_UB_22      0.0466483000
_diffrn_orient_matrix_UB_23      -0.0345713000
_diffrn_orient_matrix_UB_31      -0.0431169000
_diffrn_orient_matrix_UB_32      0.0109485000
_diffrn_orient_matrix_UB_33      0.0356078000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8204
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.972
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           0.0
_exptl_absorpt_coefficient_mu    6.509
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.929
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.129
_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     104
_refine_ls_number_reflns         2866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0181
_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^)+(0.0160P)^2^+0.9670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0370
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2545
_reflns_number_total             2866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b04060_si_002.cif
_cod_data_source_block           2014slbr393b
_cod_database_code               4130492
_chemical_oxdiff_formula         ' C4 H12 Cl4 Pd1 Sb2'
_reflns_odcompleteness_completeness 90.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.75
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              6251
_shelx_hkl_checksum              19954
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method MiTeGen
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.830
_oxdiff_exptl_absorpt_empirical_full_min 0.717