#------------------------------------------------------------------------------
#$Date: 2016-01-14 05:25:27 +0200 (Thu, 14 Jan 2016) $
#$Revision: 174443 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/14/2241459.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241459
loop_
_publ_author_name
'Robeyns, Koen'
'Willocq, Christopher'
'Tinant, Bernard'
'Devillers, Michel'
'Hermans, Sophie'
_publ_section_title
;
 Crystal structure of a Pd₄ carbonyl triphenylphosphane cluster
 [Pd₄(CO)₅(PPh₃)₄]·2C₄H₈O, 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(μ-carbonyl-κ²C:C)tetrakis(triphenylphosphane-κP)tetrapalladium(5 Pd---Pd) 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
;
marHKL (Klein & Bartels, 2000)
;
_computing_data_collection
;
mar345 (Klein, 1998)
;
_computing_data_reduction
;
marHKL (Klein & Bartels, 2000)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2008)
;
_computing_publication_material
;
Mercury (Macrae et al.,  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, ΔΦ 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/[σ²(Fo²)+(0.0201P)²+36.9627P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_data_source_file            lh5801sup1.cif
_cod_data_source_block           I
_cod_database_code               2241459
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Pd Pd1 0.00088(2) 0.70651(2) 0.16201(2) 0.01857(13) Uani d 1
Pd Pd2 -0.05342(2) 0.59762(2) 0.22629(2) 0.01713(13) Uani d 1
C C1 0.0757(2) 0.6757(3) 0.1897(3) 0.0248(13) Uani d 1
O O1 0.11225(15) 0.6829(2) 0.1692(2) 0.0345(9) Uani d 1
C C2 -0.0735(2) 0.6741(3) 0.1236(3) 0.0239(12) Uani d 1
O O2 -0.10823(14) 0.6805(2) 0.0691(2) 0.0333(9) Uani d 1
C C3 0.0000 0.5003(5) 0.2500 0.0231(17) Uani d 1
O O3 0.0000 0.4268(3) 0.2500 0.0320(13) Uani d 1
P P3 -0.00131(5) 0.82666(8) 0.09097(7) 0.0185(3) Uani d 1
C C4 0.06148(19) 0.8732(3) 0.1019(3) 0.0180(11) Uani d 1
C C5 0.0797(2) 0.8963(3) 0.0400(3) 0.0235(12) Uani d 1
H H5 0.0579 0.8915 -0.0113 0.028 Uiso calc 1
C C6 0.1284(2) 0.9258(3) 0.0510(3) 0.0275(13) Uani d 1
H H6 0.1405 0.9401 0.0078 0.033 Uiso calc 1
C C7 0.1599(2) 0.9346(4) 0.1258(3) 0.0328(14) Uani d 1
H H7 0.1937 0.9548 0.1340 0.039 Uiso calc 1
C C8 0.1422(2) 0.9140(4) 0.1878(3) 0.0365(15) Uani d 1
H H8 0.1636 0.9211 0.2390 0.044 Uiso calc 1
C C9 0.0937(2) 0.8833(3) 0.1764(3) 0.0281(13) Uani d 1
H H9 0.0819 0.8686 0.2199 0.034 Uiso calc 1
C C10 -0.02718(19) 0.8146(3) -0.0143(3) 0.0208(12) Uani d 1
C C11 -0.0615(2) 0.8691(3) -0.0601(3) 0.0262(13) Uani d 1
H H11 -0.0741 0.9150 -0.0372 0.031 Uiso calc 1
C C12 -0.0777(2) 0.8572(4) -0.1398(3) 0.0346(15) Uani d 1
H H12 -0.1024 0.8936 -0.1714 0.041 Uiso calc 1
C C13 -0.0577(2) 0.7919(4) -0.1732(3) 0.0373(15) Uani d 1
H H13 -0.0678 0.7850 -0.2279 0.045 Uiso calc 1
C C14 -0.0234(2) 0.7371(4) -0.1274(3) 0.0373(15) Uani d 1
H H14 -0.0100 0.6924 -0.1506 0.045 Uiso calc 1
C C15 -0.0085(2) 0.7470(3) -0.0478(3) 0.0280(13) Uani d 1
H H15 0.0143 0.7082 -0.0161 0.034 Uiso calc 1
C C16 -0.03973(19) 0.9103(3) 0.1160(3) 0.0199(12) Uani d 1
C C17 -0.0907(2) 0.8940(3) 0.1112(3) 0.0253(13) Uani d 1
H H17 -0.1050 0.8410 0.0939 0.030 Uiso calc 1
C C18 -0.1208(2) 0.9551(4) 0.1318(3) 0.0317(14) Uani d 1
H H18 -0.1556 0.9436 0.1275 0.038 Uiso calc 1
C C19 -0.1010(2) 1.0321(3) 0.1581(3) 0.0327(15) Uani d 1
H H19 -0.1216 1.0734 0.1728 0.039 Uiso calc 1
C C20 -0.0505(2) 1.0477(4) 0.1628(3) 0.0309(14) Uani d 1
H H20 -0.0364 1.1008 0.1802 0.037 Uiso calc 1
C C21 -0.0199(2) 0.9878(3) 0.1425(3) 0.0258(13) Uani d 1
H H21 0.0149 0.9998 0.1468 0.031 Uiso calc 1
P P4 -0.12826(5) 0.52022(8) 0.19235(7) 0.0191(3) Uani d 1
C C22 -0.12432(19) 0.4330(3) 0.1291(3) 0.0233(12) Uani d 1
C C23 -0.1279(2) 0.3498(3) 0.1471(3) 0.0314(14) Uani d 1
H H23 -0.1329 0.3344 0.1956 0.038 Uiso calc 1
C C24 -0.1241(2) 0.2883(4) 0.0939(4) 0.0433(16) Uani d 1
H H24 -0.1259 0.2312 0.1072 0.052 Uiso calc 1
C C25 -0.1178(2) 0.3084(4) 0.0231(4) 0.0373(15) Uani d 1
H H25 -0.1160 0.2660 -0.0131 0.045 Uiso calc 1
C C26 -0.1141(3) 0.3903(4) 0.0058(4) 0.0475(17) Uani d 1
H H26 -0.1096 0.4052 -0.0431 0.057 Uiso calc 1
C C27 -0.1170(2) 0.4521(4) 0.0578(3) 0.0419(16) Uani d 1
H H27 -0.1139 0.5088 0.0444 0.050 Uiso calc 1
C C28 -0.14892(18) 0.4741(3) 0.2725(3) 0.0195(12) Uani d 1
C C29 -0.1977(2) 0.4841(4) 0.2804(3) 0.0312(14) Uani d 1
H H29 -0.2223 0.5150 0.2426 0.037 Uiso calc 1
C C30 -0.2109(2) 0.4494(4) 0.3431(3) 0.0359(15) Uani d 1
H H30 -0.2441 0.4583 0.3491 0.043 Uiso calc 1
C C31 -0.1761(2) 0.4022(3) 0.3967(3) 0.0323(14) Uani d 1
H H31 -0.1856 0.3765 0.4384 0.039 Uiso calc 1
C C32 -0.1277(2) 0.3926(4) 0.3896(3) 0.0411(16) Uani d 1
H H32 -0.1034 0.3604 0.4266 0.049 Uiso calc 1
C C33 -0.1139(2) 0.4299(4) 0.3281(3) 0.0349(15) Uani d 1
H H33 -0.0798 0.4247 0.3246 0.042 Uiso calc 1
C C34 -0.18558(19) 0.5748(3) 0.1361(3) 0.0232(12) Uani d 1
C C35 -0.1923(2) 0.6592(4) 0.1488(3) 0.0359(15) Uani d 1
H H35 -0.1663 0.6881 0.1861 0.043 Uiso calc 1
C C36 -0.2352(2) 0.7020(4) 0.1092(4) 0.0501(18) Uani d 1
H H36 -0.2390 0.7594 0.1197 0.060 Uiso calc 1
C C37 -0.2727(3) 0.6609(5) 0.0542(4) 0.057(2) Uani d 1
H H37 -0.3024 0.6902 0.0263 0.069 Uiso calc 1
C C38 -0.2673(2) 0.5785(5) 0.0398(4) 0.053(2) Uani d 1
H H38 -0.2933 0.5506 0.0016 0.064 Uiso calc 1
C C39 -0.2241(2) 0.5345(4) 0.0806(3) 0.0374(15) Uani d 1
H H39 -0.2209 0.4769 0.0704 0.045 Uiso calc 1
O O100 0.2944(2) 0.6292(4) 0.1655(3) 0.0822(18) Uani d 1
C C101 0.2603(3) 0.6561(5) 0.0954(5) 0.079(3) Uani d 1
H H10A 0.2303 0.6185 0.0805 0.095 Uiso calc 1
H H10B 0.2773 0.6562 0.0533 0.095 Uiso calc 1
C C102 0.2439(3) 0.7435(5) 0.1096(4) 0.063(2) Uani d 1
H H10C 0.2675 0.7859 0.0989 0.076 Uiso calc 1
H H10D 0.2088 0.7555 0.0777 0.076 Uiso calc 1
C C103 0.2467(3) 0.7403(5) 0.1944(4) 0.069(2) Uani d 1
H H10E 0.2541 0.7962 0.2185 0.082 Uiso calc 1
H H10F 0.2143 0.7194 0.2024 0.082 Uiso calc 1
C C104 0.2894(3) 0.6812(5) 0.2274(4) 0.063(2) Uani d 1
H H10G 0.3215 0.7123 0.2497 0.076 Uiso calc 1
H H10H 0.2818 0.6471 0.2689 0.076 Uiso calc 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C2 Pd1 C1 . . 150.4(2)
C2 Pd1 P3 . . 98.89(15)
C1 Pd1 P3 . . 102.22(16)
C2 Pd1 Pd2 . . 51.16(15)
C1 Pd1 Pd2 . . 111.46(15)
P3 Pd1 Pd2 . . 146.24(4)
C2 Pd1 Pd2 . 2 111.07(15)
C1 Pd1 Pd2 . 2 51.44(15)
P3 Pd1 Pd2 . 2 149.92(4)
Pd2 Pd1 Pd2 . 2 61.43(3)
C2 Pd1 Pd1 . 2 92.97(15)
C1 Pd1 Pd1 . 2 92.60(15)
P3 Pd1 Pd1 . 2 123.13(4)
Pd2 Pd1 Pd1 . 2 54.768(18)
Pd2 Pd1 Pd1 2 2 54.58(2)
C3 Pd2 C2 . . 126.58(14)
C3 Pd2 C1 . 2 126.77(14)
C2 Pd2 C1 . 2 102.29(19)
C3 Pd2 P4 . . 99.66(15)
C2 Pd2 P4 . . 94.64(15)
C1 Pd2 P4 2 . 95.57(15)
C3 Pd2 Pd1 . . 97.67(12)
C2 Pd2 Pd1 . . 46.94(15)
C1 Pd2 Pd1 2 . 102.24(15)
P4 Pd2 Pd1 . . 140.12(4)
C3 Pd2 Pd1 . 2 97.47(12)
C2 Pd2 Pd1 . 2 102.83(14)
C1 Pd2 Pd1 2 2 46.81(15)
P4 Pd2 Pd1 . 2 140.88(4)
Pd1 Pd2 Pd1 . 2 70.66(3)
C3 Pd2 Pd2 . 2 48.05(15)
C2 Pd2 Pd2 . 2 104.98(15)
C1 Pd2 Pd2 2 2 104.73(15)
P4 Pd2 Pd2 . 2 147.71(4)
Pd1 Pd2 Pd2 . 2 59.40(2)
Pd1 Pd2 Pd2 2 2 59.171(19)
O1 C1 Pd1 . . 142.6(4)
O1 C1 Pd2 . 2 135.0(4)
Pd1 C1 Pd2 . 2 81.7(2)
O2 C2 Pd1 . . 140.6(4)
O2 C2 Pd2 . . 136.5(4)
Pd1 C2 Pd2 . . 81.9(2)
O3 C3 Pd2 . . 138.05(15)
O3 C3 Pd2 . 2 138.05(15)
Pd2 C3 Pd2 . 2 83.9(3)
C4 P3 C16 . . 104.9(2)
C4 P3 C10 . . 103.7(2)
C16 P3 C10 . . 104.2(2)
C4 P3 Pd1 . . 113.63(16)
C16 P3 Pd1 . . 113.95(16)
C10 P3 Pd1 . . 115.24(17)
C5 C4 C9 . . 118.0(5)
C5 C4 P3 . . 123.6(4)
C9 C4 P3 . . 118.4(4)
C6 C5 C4 . . 121.4(5)
C6 C5 H5 . . 119.3
C4 C5 H5 . . 119.3
C5 C6 C7 . . 119.4(5)
C5 C6 H6 . . 120.3
C7 C6 H6 . . 120.3
C8 C7 C6 . . 120.0(5)
C8 C7 H7 . . 120.0
C6 C7 H7 . . 120.0
C7 C8 C9 . . 120.4(5)
C7 C8 H8 . . 119.8
C9 C8 H8 . . 119.8
C8 C9 C4 . . 120.8(5)
C8 C9 H9 . . 119.6
C4 C9 H9 . . 119.6
C11 C10 C15 . . 120.1(5)
C11 C10 P3 . . 123.7(4)
C15 C10 P3 . . 116.1(4)
C10 C11 C12 . . 120.1(5)
C10 C11 H11 . . 120.0
C12 C11 H11 . . 120.0
C13 C12 C11 . . 119.7(5)
C13 C12 H12 . . 120.1
C11 C12 H12 . . 120.1
C14 C13 C12 . . 120.3(5)
C14 C13 H13 . . 119.8
C12 C13 H13 . . 119.8
C13 C14 C15 . . 120.1(6)
C13 C14 H14 . . 119.9
C15 C14 H14 . . 119.9
C14 C15 C10 . . 119.6(5)
C14 C15 H15 . . 120.2
C10 C15 H15 . . 120.2
C21 C16 C17 . . 118.4(5)
C21 C16 P3 . . 123.0(4)
C17 C16 P3 . . 118.5(4)
C18 C17 C16 . . 120.2(5)
C18 C17 H17 . . 119.9
C16 C17 H17 . . 119.9
C19 C18 C17 . . 121.2(5)
C19 C18 H18 . . 119.4
C17 C18 H18 . . 119.4
C18 C19 C20 . . 118.3(5)
C18 C19 H19 . . 120.9
C20 C19 H19 . . 120.9
C19 C20 C21 . . 121.4(5)
C19 C20 H20 . . 119.3
C21 C20 H20 . . 119.3
C20 C21 C16 . . 120.4(5)
C20 C21 H21 . . 119.8
C16 C21 H21 . . 119.8
C22 P4 C34 . . 102.1(2)
C22 P4 C28 . . 105.2(2)
C34 P4 C28 . . 103.0(2)
C22 P4 Pd2 . . 112.06(17)
C34 P4 Pd2 . . 116.44(17)
C28 P4 Pd2 . . 116.45(16)
C23 C22 C27 . . 117.8(5)
C23 C22 P4 . . 125.1(4)
C27 C22 P4 . . 117.0(4)
C22 C23 C24 . . 120.0(6)
C22 C23 H23 . . 120.0
C24 C23 H23 . . 120.0
C25 C24 C23 . . 121.4(6)
C25 C24 H24 . . 119.3
C23 C24 H24 . . 119.3
C26 C25 C24 . . 118.5(6)
C26 C25 H25 . . 120.8
C24 C25 H25 . . 120.8
C25 C26 C27 . . 121.2(6)
C25 C26 H26 . . 119.4
C27 C26 H26 . . 119.4
C26 C27 C22 . . 121.2(6)
C26 C27 H27 . . 119.4
C22 C27 H27 . . 119.4
C33 C28 C29 . . 118.8(5)
C33 C28 P4 . . 118.3(4)
C29 C28 P4 . . 122.8(4)
C28 C29 C30 . . 120.4(5)
C28 C29 H29 . . 119.8
C30 C29 H29 . . 119.8
C31 C30 C29 . . 120.2(5)
C31 C30 H30 . . 119.9
C29 C30 H30 . . 119.9
C32 C31 C30 . . 119.6(5)
C32 C31 H31 . . 120.2
C30 C31 H31 . . 120.2
C31 C32 C33 . . 120.1(5)
C31 C32 H32 . . 119.9
C33 C32 H32 . . 119.9
C28 C33 C32 . . 120.7(5)
C28 C33 H33 . . 119.6
C32 C33 H33 . . 119.6
C35 C34 C39 . . 117.4(5)
C35 C34 P4 . . 120.2(4)
C39 C34 P4 . . 122.4(4)
C36 C35 C34 . . 122.1(6)
C36 C35 H35 . . 119.0
C34 C35 H35 . . 119.0
C35 C36 C37 . . 119.5(7)
C35 C36 H36 . . 120.3
C37 C36 H36 . . 120.3
C38 C37 C36 . . 120.2(6)
C38 C37 H37 . . 119.9
C36 C37 H37 . . 119.9
C37 C38 C39 . . 120.6(6)
C37 C38 H38 . . 119.7
C39 C38 H38 . . 119.7
C34 C39 C38 . . 120.3(6)
C34 C39 H39 . . 119.8
C38 C39 H39 . . 119.8
C101 O100 C104 . . 109.6(6)
O100 C101 C102 . . 106.6(7)
O100 C101 H10A . . 110.4
C102 C101 H10A . . 110.4
O100 C101 H10B . . 110.4
C102 C101 H10B . . 110.4
H10A C101 H10B . . 108.6
C103 C102 C101 . . 101.7(6)
C103 C102 H10C . . 111.4
C101 C102 H10C . . 111.4
C103 C102 H10D . . 111.4
C101 C102 H10D . . 111.4
H10C C102 H10D . . 109.3
C104 C103 C102 . . 104.0(6)
C104 C103 H10E . . 111.0
C102 C103 H10E . . 111.0
C104 C103 H10F . . 111.0
C102 C103 H10F . . 111.0
H10E C103 H10F . . 109.0
O100 C104 C103 . . 107.0(6)
O100 C104 H10G . . 110.3
C103 C104 H10G . . 110.3
O100 C104 H10H . . 110.3
C103 C104 H10H . . 110.3
H10G C104 H10H . . 108.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 C2 . 2.021(6) ?
Pd1 C1 . 2.022(6) ?
Pd1 P3 . 2.2998(15) ?
Pd1 Pd2 . 2.7381(8) y
Pd1 Pd2 2 2.7446(9) y
Pd1 Pd1 2 3.1704(14) y
Pd2 C3 . 2.095(6) ?
Pd2 C2 . 2.154(5) ?
Pd2 C1 2 2.169(6) ?
Pd2 P4 . 2.3208(15) y
Pd2 Pd1 2 2.7446(9) y
Pd2 Pd2 2 2.8006(12) y
C1 O1 . 1.159(6) ?
C1 Pd2 2 2.169(6) ?
C2 O2 . 1.164(6) ?
C3 O3 . 1.178(9) ?
C3 Pd2 2 2.095(6) ?
P3 C4 . 1.827(5) ?
P3 C16 . 1.830(5) ?
P3 C10 . 1.836(5) ?
C4 C5 . 1.385(7) ?
C4 C9 . 1.392(7) ?
C5 C6 . 1.373(7) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.387(7) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.368(8) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.372(8) ?
C8 H8 . 0.9500 ?
C9 H9 . 0.9500 ?
C10 C11 . 1.374(7) ?
C10 C15 . 1.401(7) ?
C11 C12 . 1.390(7) ?
C11 H11 . 0.9500 ?
C12 C13 . 1.388(8) ?
C12 H12 . 0.9500 ?
C13 C14 . 1.379(8) ?
C13 H13 . 0.9500 ?
C14 C15 . 1.382(7) ?
C14 H14 . 0.9500 ?
C15 H15 . 0.9500 ?
C16 C21 . 1.385(7) ?
C16 C17 . 1.394(7) ?
C17 C18 . 1.389(8) ?
C17 H17 . 0.9500 ?
C18 C19 . 1.376(8) ?
C18 H18 . 0.9500 ?
C19 C20 . 1.379(8) ?
C19 H19 . 0.9500 ?
C20 C21 . 1.384(7) ?
C20 H20 . 0.9500 ?
C21 H21 . 0.9500 ?
P4 C22 . 1.821(5) ?
P4 C34 . 1.832(5) ?
P4 C28 . 1.837(5) ?
C22 C23 . 1.380(8) ?
C22 C27 . 1.383(7) ?
C23 C24 . 1.395(8) ?
C23 H23 . 0.9500 ?
C24 C25 . 1.365(9) ?
C24 H24 . 0.9500 ?
C25 C26 . 1.358(8) ?
C25 H25 . 0.9500 ?
C26 C27 . 1.377(8) ?
C26 H26 . 0.9500 ?
C27 H27 . 0.9500 ?
C28 C33 . 1.373(7) ?
C28 C29 . 1.384(7) ?
C29 C30 . 1.388(8) ?
C29 H29 . 0.9500 ?
C30 C31 . 1.377(8) ?
C30 H30 . 0.9500 ?
C31 C32 . 1.369(8) ?
C31 H31 . 0.9500 ?
C32 C33 . 1.394(8) ?
C32 H32 . 0.9500 ?
C33 H33 . 0.9500 ?
C34 C35 . 1.391(8) ?
C34 C39 . 1.391(7) ?
C35 C36 . 1.375(8) ?
C35 H35 . 0.9500 ?
C36 C37 . 1.377(10) ?
C36 H36 . 0.9500 ?
C37 C38 . 1.361(10) ?
C37 H37 . 0.9500 ?
C38 C39 . 1.395(9) ?
C38 H38 . 0.9500 ?
C39 H39 . 0.9500 ?
O100 C101 . 1.410(9) ?
O100 C104 . 1.425(9) ?
C101 C102 . 1.512(11) ?
C101 H10A . 0.9900 ?
C101 H10B . 0.9900 ?
C102 C103 . 1.503(10) ?
C102 H10C . 0.9900 ?
C102 H10D . 0.9900 ?
C103 C104 . 1.490(10) ?
C103 H10E . 0.9900 ?
C103 H10F . 0.9900 ?
C104 H10G . 0.9900 ?
C104 H10H . 0.9900 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C19 H19 O100 3_455 0.95 2.43 3.282(8) 149 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C16 P3 C4 C5 -105.5(4)
C10 P3 C4 C5 3.6(5)
Pd1 P3 C4 C5 129.5(4)
C16 P3 C4 C9 77.1(4)
C10 P3 C4 C9 -173.9(4)
Pd1 P3 C4 C9 -48.0(4)
C9 C4 C5 C6 1.9(8)
P3 C4 C5 C6 -175.5(4)
C4 C5 C6 C7 -1.5(8)
C5 C6 C7 C8 -0.1(9)
C6 C7 C8 C9 1.2(9)
C7 C8 C9 C4 -0.7(9)
C5 C4 C9 C8 -0.8(8)
P3 C4 C9 C8 176.7(4)
C4 P3 C10 C11 -99.7(5)
C16 P3 C10 C11 9.8(5)
Pd1 P3 C10 C11 135.4(4)
C4 P3 C10 C15 77.9(4)
C16 P3 C10 C15 -172.5(4)
Pd1 P3 C10 C15 -46.9(4)
C15 C10 C11 C12 0.0(8)
P3 C10 C11 C12 177.5(4)
C10 C11 C12 C13 -2.3(8)
C11 C12 C13 C14 2.5(8)
C12 C13 C14 C15 -0.3(8)
C13 C14 C15 C10 -2.1(8)
C11 C10 C15 C14 2.2(8)
P3 C10 C15 C14 -175.5(4)
C4 P3 C16 C21 -4.3(5)
C10 P3 C16 C21 -113.0(4)
Pd1 P3 C16 C21 120.6(4)
C4 P3 C16 C17 178.4(4)
C10 P3 C16 C17 69.7(4)
Pd1 P3 C16 C17 -56.7(4)
C21 C16 C17 C18 0.9(7)
P3 C16 C17 C18 178.3(4)
C16 C17 C18 C19 -0.9(7)
C17 C18 C19 C20 0.9(7)
C18 C19 C20 C21 -0.8(7)
C19 C20 C21 C16 0.8(7)
C17 C16 C21 C20 -0.8(7)
P3 C16 C21 C20 -178.1(4)
C34 P4 C22 C23 -117.1(5)
C28 P4 C22 C23 -9.8(5)
Pd2 P4 C22 C23 117.6(4)
C34 P4 C22 C27 63.2(5)
C28 P4 C22 C27 170.4(4)
Pd2 P4 C22 C27 -62.1(5)
C27 C22 C23 C24 0.0(8)
P4 C22 C23 C24 -179.8(4)
C22 C23 C24 C25 -1.2(9)
C23 C24 C25 C26 1.3(9)
C24 C25 C26 C27 -0.3(10)
C25 C26 C27 C22 -0.9(10)
C23 C22 C27 C26 1.0(9)
P4 C22 C27 C26 -179.2(5)
C22 P4 C28 C33 75.3(5)
C34 P4 C28 C33 -178.1(4)
Pd2 P4 C28 C33 -49.4(5)
C22 P4 C28 C29 -106.7(5)
C34 P4 C28 C29 -0.1(5)
Pd2 P4 C28 C29 128.6(4)
C33 C28 C29 C30 -0.5(8)
P4 C28 C29 C30 -178.6(4)
C28 C29 C30 C31 -2.3(9)
C29 C30 C31 C32 2.7(9)
C30 C31 C32 C33 -0.4(9)
C29 C28 C33 C32 2.8(9)
P4 C28 C33 C32 -179.1(5)
C31 C32 C33 C28 -2.4(10)
C22 P4 C34 C35 -156.5(4)
C28 P4 C34 C35 94.6(4)
Pd2 P4 C34 C35 -34.1(5)
C22 P4 C34 C39 24.4(5)
C28 P4 C34 C39 -84.5(5)
Pd2 P4 C34 C39 146.8(4)
C39 C34 C35 C36 0.7(8)
P4 C34 C35 C36 -178.5(5)
C34 C35 C36 C37 -1.0(9)
C35 C36 C37 C38 0.5(10)
C36 C37 C38 C39 0.3(10)
C35 C34 C39 C38 0.2(8)
P4 C34 C39 C38 179.3(4)
C37 C38 C39 C34 -0.6(9)
C104 O100 C101 C102 16.7(9)
O100 C101 C102 C103 -30.5(8)
C101 C102 C103 C104 32.2(8)
C101 O100 C104 C103 4.4(9)
C102 C103 C104 O100 -23.6(8)

_cod_database_fobs_code 2241459
