#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/23/4332357.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_4332357
loop_
_publ_author_name
'Aizawa, Sen-ichi'
'Saito, Kenji'
'Kawamoto, Tatsuya'
'Matsumoto, Emi'
_publ_section_title
;
 Stereoselective Preparation, Structures, and Reactivities of
 Phosphine-Bridged Mixed-Metal Trinuclear and Pentanuclear Complexes with
 Tris[2-(diphenylphosphino)ethyl]phosphine
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4859
_journal_page_last               4866
_journal_paper_doi               10.1021/ic060277l
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C85 H87 B2 Cl7 F8 O P8 Pd2 Pt '
_chemical_formula_sum            'C85 H87 B2 Cl7 F8 O P8 Pd2 Pt'
_chemical_formula_weight         2202.08
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.276(4)
_cell_length_b                   23.610(4)
_cell_length_c                   13.933(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.8
_cell_volume                     9302(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure Ver. 3.5.1'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SHELXS97
_diffrn_measured_fraction_theta_full 0.9959
_diffrn_measured_fraction_theta_max 0.9959
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            23234
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_standards_decay_%        -17.23
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.275
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.492
_exptl_absorpt_correction_type   psi-scans
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4384.00
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.37
_refine_diff_density_min         -2.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.953
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     529
_refine_ls_number_reflns         4824
_refine_ls_R_factor_gt           0.0750
_refine_ls_shift/su_max          0.9970
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 1/σ²(Fo²)'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                4817
_reflns_number_total             10684
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic060277lsup1.cif
_cod_data_source_block           '_7a(BF4)2'
_cod_original_cell_volume        9301(2)
_cod_original_sg_symbol_Hall     'P 21/B 21/C 21/A '
_cod_original_sg_symbol_H-M      'P 21/b 21/c 21/a'
_cod_original_formula_sum        'C85 H87 B2 Cl7 F8 O P8 Pd2 Pt '
_cod_database_code               4332357
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,z
x+1/2,-y+1/2,-z
x,-y+1/2,z+1/2
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pt(1) Pt 0.0000 0.5000 0.5000 0.0483(2) Uani 1.00 1 d .
Pd(1) Pd 0.08282(4) 0.35826(5) 0.90373(8) 0.0491(4) Uani 1.00 1 d .
Cl(1) Cl 0.0419(1) 0.3225(2) 1.0386(3) 0.070(1) Uani 1.00 1 d .
Cl(2) Cl 0.0064(1) 0.4044(2) 0.5220(3) 0.064(1) Uani 1.00 1 d .
Cl(3) Cl 0.2455(8) 0.7031(9) 0.458(1) 0.256(9) Uiso 0.50 1 d P
Cl(4) Cl 0.1752(5) 0.7615(7) 0.431(1) 0.177(6) Uiso 0.50 1 d P
Cl(5) Cl 0.2334(5) 0.7166(6) 0.3014(9) 0.148(5) Uiso 0.50 1 d P
P(1) P 0.1198(1) 0.3875(2) 0.7730(3) 0.049(1) Uani 1.00 1 d .
P(2) P 0.1225(1) 0.4332(2) 0.9783(3) 0.056(1) Uani 1.00 1 d .
P(3) P 0.0592(2) 0.2840(2) 0.8065(3) 0.056(1) Uani 1.00 1 d .
P(4) P 0.0772(1) 0.5148(2) 0.5525(3) 0.050(1) Uani 1.00 1 d .
F(1) F 0.2005(5) 0.8985(6) 0.581(1) 0.198(6) Uiso 1.00 1 d .
F(2) F 0.2688(5) 0.9314(7) 0.593(1) 0.218(7) Uiso 1.00 1 d .
F(3) F 0.2406(6) 0.9054(7) 0.465(1) 0.228(7) Uiso 1.00 1 d .
F(4) F 0.2561(6) 0.8478(7) 0.565(1) 0.278(9) Uiso 1.00 1 d .
O(1) O 0.191(1) 0.685(1) 0.484(2) 0.13(1) Uiso 0.50 1 d P
C(1) C 0.1732(5) 0.4255(7) 0.810(1) 0.068(6) Uani 1.00 1 d .
C(2) C 0.1588(5) 0.4681(7) 0.887(1) 0.070(6) Uani 1.00 1 d .
C(3) C 0.1261(6) 0.3270(7) 0.695(1) 0.078(7) Uani 1.00 1 d .
C(4) C 0.0798(6) 0.2963(7) 0.684(1) 0.069(6) Uani 1.00 1 d .
C(5) C 0.0851(5) 0.4376(6) 0.7063(9) 0.047(5) Uani 1.00 1 d .
C(6) C 0.1052(5) 0.4531(6) 0.6076(9) 0.055(5) Uani 1.00 1 d .
C(7) C 0.1652(7) 0.4128(9) 1.069(1) 0.069(7) Uani 1.00 1 d .
C(8) C 0.1652(6) 0.357(1) 1.094(1) 0.099(8) Uani 1.00 1 d .
C(9) C 0.2028(9) 0.342(1) 1.173(2) 0.14(1) Uani 1.00 1 d .
C(10) C 0.2273(8) 0.390(2) 1.204(2) 0.17(1) Uani 1.00 1 d .
C(11) C 0.229(1) 0.441(2) 1.179(3) 0.27(2) Uani 1.00 1 d .
C(12) C 0.1948(6) 0.450(1) 1.110(1) 0.112(9) Uani 1.00 1 d .
C(13) C 0.0885(6) 0.4883(7) 1.033(1) 0.053(5) Uani 1.00 1 d .
C(14) C 0.0969(7) 0.5442(8) 1.021(1) 0.078(7) Uani 1.00 1 d .
C(15) C 0.0677(8) 0.5856(8) 1.062(1) 0.089(8) Uani 1.00 1 d .
C(16) C 0.0308(8) 0.569(1) 1.117(2) 0.094(9) Uani 1.00 1 d .
C(17) C 0.0233(7) 0.515(1) 1.127(1) 0.102(9) Uani 1.00 1 d .
C(18) C 0.0494(7) 0.4715(8) 1.087(1) 0.092(8) Uani 1.00 1 d .
C(19) C 0.0848(7) 0.2189(8) 0.840(1) 0.062(6) Uani 1.00 1 d .
C(20) C 0.0739(6) 0.1688(8) 0.799(1) 0.076(7) Uani 1.00 1 d .
C(21) C 0.0977(8) 0.119(1) 0.816(1) 0.097(9) Uani 1.00 1 d .
C(22) C 0.1357(9) 0.1177(9) 0.876(2) 0.10(1) Uani 1.00 1 d .
C(23) C 0.1486(7) 0.166(1) 0.920(1) 0.084(8) Uani 1.00 1 d .
C(24) C 0.1226(7) 0.2158(8) 0.902(1) 0.078(7) Uani 1.00 1 d .
C(25) C -0.0012(7) 0.2715(7) 0.801(1) 0.069(6) Uani 1.00 1 d .
C(26) C -0.0213(7) 0.241(1) 0.877(2) 0.103(9) Uani 1.00 1 d .
C(27) C -0.069(1) 0.238(1) 0.888(2) 0.15(1) Uani 1.00 1 d .
C(28) C -0.0961(8) 0.263(1) 0.817(2) 0.13(1) Uani 1.00 1 d .
C(29) C -0.076(1) 0.292(1) 0.740(2) 0.13(1) Uani 1.00 1 d .
C(30) C -0.0286(7) 0.2955(9) 0.730(2) 0.11(1) Uani 1.00 1 d .
C(31) C 0.0824(6) 0.5680(7) 0.648(1) 0.053(5) Uani 1.00 1 d .
C(32) C 0.1267(6) 0.5856(8) 0.678(1) 0.086(7) Uani 1.00 1 d .
C(33) C 0.1292(8) 0.6202(9) 0.763(2) 0.11(1) Uani 1.00 1 d .
C(34) C 0.0904(8) 0.6340(9) 0.810(1) 0.096(8) Uani 1.00 1 d .
C(35) C 0.0476(7) 0.6166(9) 0.782(1) 0.083(8) Uani 1.00 1 d .
C(36) C 0.0449(6) 0.5838(7) 0.703(1) 0.067(6) Uani 1.00 1 d .
C(37) C 0.1193(5) 0.5335(7) 0.457(1) 0.054(5) Uani 1.00 1 d .
C(38) C 0.1678(6) 0.5254(9) 0.465(1) 0.092(7) Uani 1.00 1 d .
C(39) C 0.1983(7) 0.540(1) 0.394(1) 0.13(1) Uani 1.00 1 d .
C(40) C 0.1812(7) 0.5555(9) 0.311(1) 0.098(9) Uani 1.00 1 d .
C(41) C 0.1340(8) 0.5611(9) 0.297(1) 0.110(9) Uani 1.00 1 d .
C(42) C 0.1015(6) 0.5502(8) 0.370(1) 0.082(7) Uani 1.00 1 d .
C(43) C 0.223(1) 0.754(2) 0.395(3) 0.10(1) Uiso 0.50 1 d P
B(1) B 0.2464(5) 0.8933(4) 0.5609(8) 0.8270 Uiso 1.00 1 d .
H(8) H 0.1433(6) 0.332(1) 1.063(1) 0.118(8) Uiso 1.00 1 c .
H(9) H 0.2074(9) 0.303(1) 1.189(2) 0.17(1) Uiso 1.00 1 c .
H(10) H 0.2455(8) 0.380(2) 1.260(2) 0.21(2) Uiso 1.00 1 c .
H(11) H 0.256(1) 0.463(2) 1.195(3) 0.32(3) Uiso 1.00 1 c .
H(12) H 0.1947(6) 0.489(1) 1.089(1) 0.13(1) Uiso 1.00 1 c .
H(14) H 0.1233(7) 0.5560(8) 0.983(1) 0.093(7) Uiso 1.00 1 c .
H(15) H 0.0740(8) 0.6253(8) 1.053(1) 0.106(8) Uiso 1.00 1 c .
H(16) H 0.0105(8) 0.597(1) 1.147(2) 0.113(9) Uiso 1.00 1 c .
H(17) H -0.0031(7) 0.504(1) 1.167(1) 0.122(9) Uiso 1.00 1 c .
H(18) H 0.0421(7) 0.4322(8) 1.096(1) 0.111(8) Uiso 1.00 1 c .
H(20) H 0.0479(6) 0.1686(8) 0.754(1) 0.091(7) Uiso 1.00 1 c .
H(21) H 0.0872(8) 0.084(1) 0.789(1) 0.116(9) Uiso 1.00 1 c .
H(22) H 0.1541(9) 0.0841(9) 0.886(2) 0.12(1) Uiso 1.00 1 c .
H(23) H 0.1744(7) 0.166(1) 0.964(1) 0.101(8) Uiso 1.00 1 c .
H(24) H 0.1322(7) 0.2503(8) 0.933(1) 0.094(7) Uiso 1.00 1 c .
H(26) H -0.0015(7) 0.222(1) 0.923(2) 0.12(1) Uiso 1.00 1 c .
H(27) H -0.084(1) 0.219(1) 0.940(2) 0.18(1) Uiso 1.00 1 c .
H(28) H -0.1300(8) 0.260(1) 0.818(2) 0.16(2) Uiso 1.00 1 c .
H(29) H -0.096(1) 0.312(1) 0.695(2) 0.15(1) Uiso 1.00 1 c .
H(30) H -0.0136(7) 0.3130(9) 0.676(2) 0.14(1) Uiso 1.00 1 c .
H(32) H 0.1543(6) 0.5747(8) 0.642(1) 0.103(8) Uiso 1.00 1 c .
H(33) H 0.1592(8) 0.6339(9) 0.786(2) 0.14(1) Uiso 1.00 1 c .
H(34) H 0.0928(8) 0.6576(9) 0.866(1) 0.115(9) Uiso 1.00 1 c .
H(35) H 0.0200(7) 0.6270(9) 0.818(1) 0.100(8) Uiso 1.00 1 c .
H(36) H 0.0143(6) 0.5705(7) 0.683(1) 0.081(6) Uiso 1.00 1 c .
H(38) H 0.1799(6) 0.5087(9) 0.523(1) 0.111(8) Uiso 1.00 1 c .
H(39) H 0.2319(7) 0.537(1) 0.402(1) 0.16(1) Uiso 1.00 1 c .
H(40) H 0.2027(7) 0.5649(9) 0.260(1) 0.117(9) Uiso 1.00 1 c .
H(41) H 0.1221(8) 0.5731(9) 0.236(1) 0.13(1) Uiso 1.00 1 c .
H(42) H 0.0680(6) 0.5540(8) 0.362(1) 0.098(8) Uiso 1.00 1 c .
H(101) H 0.1958(5) 0.3995(7) 0.836(1) 0.081(6) Uiso 1.00 1 c .
H(102) H 0.1867(5) 0.4442(7) 0.755(1) 0.081(6) Uiso 1.00 1 c .
H(201) H 0.1406(5) 0.4978(7) 0.857(1) 0.084(6) Uiso 1.00 1 c .
H(202) H 0.1866(5) 0.4839(7) 0.916(1) 0.084(6) Uiso 1.00 1 c .
H(301) H 0.1375(6) 0.3394(7) 0.633(1) 0.093(7) Uiso 1.00 1 c .
H(302) H 0.1486(6) 0.3014(7) 0.723(1) 0.093(7) Uiso 1.00 1 c .
H(401) H 0.0580(6) 0.3198(7) 0.649(1) 0.083(6) Uiso 1.00 1 c .
H(402) H 0.0837(6) 0.2610(7) 0.650(1) 0.083(6) Uiso 1.00 1 c .
H(501) H 0.0540(5) 0.4223(6) 0.6975(9) 0.056(5) Uiso 1.00 1 c .
H(502) H 0.0831(5) 0.4722(6) 0.7423(9) 0.056(5) Uiso 1.00 1 c .
H(601) H 0.1005(5) 0.4211(6) 0.5661(9) 0.066(5) Uiso 1.00 1 c .
H(602) H 0.1384(5) 0.4600(6) 0.6149(9) 0.066(5) Uiso 1.00 1 c .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
; 
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) 
;
H H 0.000 0.000
; 
International Tables for Crystallography 
(1992, Vol. C, Table 6.1.1.4) 
;
B B 0.001 0.001
; 
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) 
;
Cl Cl 0.148 0.159
; 
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) 
;
F F 0.017 0.010
; 
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) 
;
P P 0.102 0.094
; 
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) 
;
Pd Pd -0.999 1.007
; 
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) 
;
Pt Pt -1.703 8.390
; 
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) 
;
O O 0.011 0.006
; 
International Tables for Crystallography 
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pt(1) Cl(2) 2.286(4) yes
Pt(1) P(4) 2.329(4) yes
Pd(1) Cl(1) 2.363(4) yes
Pd(1) P(1) 2.210(4) yes
Pd(1) P(2) 2.340(5) yes
Pd(1) P(3) 2.314(5) yes
Cl(3) Cl(5) 2.23(2) yes
Cl(3) O(1) 1.65(3) yes
Cl(3) C(43) 1.61(5) yes
Cl(4) O(1) 2.01(3) yes
Cl(4) C(43) 1.46(4) yes
Cl(5) C(43) 1.60(4) yes
P(1) C(1) 1.83(2) yes
P(1) C(3) 1.81(2) yes
P(1) C(5) 1.79(1) yes
P(2) C(2) 1.83(2) yes
P(2) C(7) 1.81(2) yes
P(2) C(13) 1.79(2) yes
P(3) C(4) 1.83(2) yes
P(3) C(19) 1.76(2) yes
P(3) C(25) 1.73(2) yes
P(4) C(6) 1.83(1) yes
P(4) C(31) 1.84(2) yes
P(4) C(37) 1.84(1) yes
F(1) B(1) 1.33(2) yes
F(2) B(1) 1.19(2) yes
F(3) B(1) 1.38(2) yes
F(4) B(1) 1.11(2) yes
C(1) C(2) 1.52(2) yes
C(1) H(101) 0.96(2) no
C(1) H(102) 0.96(2) no
C(2) H(201) 0.96(2) no
C(2) H(202) 0.96(2) no
C(3) C(4) 1.51(2) yes
C(3) H(301) 0.96(2) no
C(3) H(302) 0.96(2) no
C(4) H(401) 0.96(2) no
C(4) H(402) 0.96(2) no
C(5) C(6) 1.53(2) yes
C(5) H(501) 0.96(2) no
C(5) H(502) 0.96(2) no
C(6) H(601) 0.96(2) no
C(6) H(602) 0.96(2) no
C(7) C(8) 1.36(3) yes
C(7) C(12) 1.34(3) yes
C(8) C(9) 1.57(3) yes
C(8) H(8) 0.96(3) no
C(9) C(10) 1.38(4) yes
C(9) H(9) 0.96(4) no
C(10) C(11) 1.26(5) yes
C(10) H(10) 0.96(4) no
C(11) C(12) 1.37(5) yes
C(11) H(11) 0.96(5) no
C(12) H(12) 0.96(3) no
C(13) C(14) 1.35(3) yes
C(13) C(18) 1.39(2) yes
C(14) C(15) 1.40(3) yes
C(14) H(14) 0.96(3) no
C(15) C(16) 1.35(3) yes
C(15) H(15) 0.96(3) no
C(16) C(17) 1.32(3) yes
C(16) H(16) 0.96(3) no
C(17) C(18) 1.38(3) yes
C(17) H(17) 0.96(3) no
C(18) H(18) 0.96(3) no
C(19) C(20) 1.35(3) yes
C(19) C(24) 1.38(3) yes
C(20) C(21) 1.38(3) yes
C(20) H(20) 0.96(2) no
C(21) C(22) 1.36(3) yes
C(21) H(21) 0.96(3) no
C(22) C(23) 1.34(3) yes
C(22) H(22) 0.96(3) no
C(23) C(24) 1.41(3) yes
C(23) H(23) 0.96(3) no
C(24) H(24) 0.96(3) no
C(25) C(26) 1.40(3) yes
C(25) C(30) 1.37(3) yes
C(26) C(27) 1.36(3) yes
C(26) H(26) 0.96(3) no
C(27) C(28) 1.39(4) yes
C(27) H(27) 0.96(4) no
C(28) C(29) 1.39(4) yes
C(28) H(28) 0.96(3) no
C(29) C(30) 1.36(3) yes
C(29) H(29) 0.96(4) no
C(30) H(30) 0.96(3) no
C(31) C(32) 1.38(2) yes
C(31) C(36) 1.36(2) yes
C(32) C(33) 1.44(3) yes
C(32) H(32) 0.96(3) no
C(33) C(34) 1.32(3) yes
C(33) H(33) 0.96(3) no
C(34) C(35) 1.34(3) yes
C(34) H(34) 0.96(3) no
C(35) C(36) 1.35(2) yes
C(35) H(35) 0.96(3) no
C(36) H(36) 0.96(2) no
C(37) C(38) 1.39(2) yes
C(37) C(42) 1.37(2) yes
C(38) C(39) 1.36(3) yes
C(38) H(38) 0.96(2) no
C(39) C(40) 1.31(3) yes
C(39) H(39) 0.96(3) no
C(40) C(41) 1.36(3) yes
C(40) H(40) 0.96(3) no
C(41) C(42) 1.40(3) yes
C(41) H(41) 0.96(3) no
C(42) H(42) 0.96(2) no
