Double-Sandwich Pentalene Complexes M2(pent†)2(M = Rh, Pd; pent†= 1,4-Bis(triisopropylsilyl)pentalene): Synthesis, Structure, and Bonding
Summerscales, Owen T.; Rivers, Christopher J.; Taylor, Morgan J.; Hitchcock, Peter B.; Green, Jennifer C.; Cloke, F. Geoffrey N.; Organometallics 31 (2012) 8613–; doi:10.1021/om3010004

data_4079728
_publ_section_title
;
 Double-Sandwich Pentalene Complexes M2(pent&#x2020;)2(M = Rh, Pd;
 pent&#x2020;= 1,4-Bis(triisopropylsilyl)pentalene): Synthesis, Structure,
 and Bonding
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              8613
_journal_paper_doi               10.1021/om3010004
_journal_volume                  31
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C52 H92 Pd2 Si4'
_chemical_formula_structural     'C52 H92 Pd2 Si4'
_chemical_formula_sum            'C52 H92 Pd2 Si4'
_chemical_formula_weight         1042.42
_chemical_name_common            '[Pd2(pentalene(SiiPr3)2)2]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-03-13T16:10:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.549(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3740(12)
_cell_length_b                   13.3834(8)
_cell_length_c                   21.1553(12)
_cell_measurement_reflns_used    188782
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      4.529
_cell_measurement_wavelength     0.71073
_cell_volume                     6012.1(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15822
_diffrn_reflns_theta_full        23.05
_diffrn_reflns_theta_max         23.05
_diffrn_reflns_theta_min         4.55
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.7528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.176
_refine_diff_density_min         -1.457
_refine_diff_density_rms         0.173
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.43(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7174
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1155
_refine_ls_R_factor_gt           0.1087
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1585P)^2^+114.8349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2962
_refine_ls_wR_factor_ref         0.3021
_reflns_number_gt                6603
_reflns_number_total             7174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3010004_si_001.cif
_cod_data_source_block           mar1500
_cod_original_sg_symbol_H-M      C2
_cod_database_code               4079728