Crystal structure of a Pd~4~ carbonyl triphenylphosphane cluster [Pd~4~(CO)~5~(PPh~3~)~4~]·2C~4~H~8~O, comparing solvates
Robeyns, Koen; Willocq, Christopher; Tinant, Bernard; Devillers, Michel; Hermans, Sophie; Acta Crystallographica Section E 72 (2016) 120–123; doi:10.1107/S205698901502441X

data_2241459
_publ_section_title
;
 Crystal structure of a Pd~4~ carbonyl triphenylphosphane cluster
 [Pd~4~(CO)~5~(PPh~3~)~4~]&#x00B7;2C~4~H~8~O, comparing solvates
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              120
_journal_page_last               123
_journal_paper_doi               10.1107/S205698901502441X
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Pd4 (C O)5 (C18 H15 P)4], 2C4 H8 O'
_chemical_formula_moiety         'C77 H60 O5 P4 Pd4, 2(C4 H8 O)'
_chemical_formula_sum            'C85 H76 O7 P4 Pd4'
_chemical_formula_weight         1758.93
_chemical_name_systematic
'Pentakis(\m-carbonyl-\k^2^<i>C</i>:<i>C</i>)tetrakis(triphenylphosphane-\k<i>P</i>)tetrapalladium(5 <i>Pd</i>---<i>Pd</i>) tetrahydrofuran disolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.92(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.254(9)
_cell_length_b                   16.016(6)
_cell_length_c                   17.938(7)
_cell_measurement_reflns_used    4740
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      22.2
_cell_measurement_theta_min      2.6
_cell_volume                     7530(5)
_computing_cell_refinement
;
<i>marHKL</i> (Klein & Bartels, 2000)
;
_computing_data_collection
;
<i>mar345</i> (Klein, 1998)
;
_computing_data_reduction
;
<i>marHKL</i> (Klein & Bartels, 2000)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
Mercury (Macrae <i>et al.</i>,  2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '111 images, \D\F 2\%'
_diffrn_radiation_monochromator  'Zr filter'
_diffrn_radiation_source         'Rigaku UltraX 18 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9236
_diffrn_reflns_theta_full        22.224
_diffrn_reflns_theta_max         22.224
_diffrn_reflns_theta_min         2.543
_exptl_absorpt_coefficient_mu    1.080
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       platelets
_exptl_crystal_F_000             3544
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.529
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         4739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0201P)^2^+36.9627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                3938
_reflns_number_total             4739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lh5801sup1.cif
_cod_data_source_block           I
_cod_database_code               2241459
_cod_database_fobs_code          2241459
_shelx_hkl_checksum              94539
_shelx_res_checksum              31367
_shelx_fab_checksum              54039