#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:22:13 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178896 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/25/4112538.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4112538
loop_
_publ_author_name
'James W. Raebiger'
'Alex Miedaner'
'Calvin J. Curtis'
'Susie M. Miller'
'Oren P. Anderson'
'Daniel L. DuBois'
_publ_section_title
;
 Using Ligand Bite Angles To Control the Hydricity of Palladium
 Diphosphine Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5502
_journal_page_last               5514
_journal_paper_doi               10.1021/ja0395240
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C32 H56 P4 Pd'
_chemical_formula_weight         671.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.890(9)
_cell_angle_beta                 79.214(9)
_cell_angle_gamma                66.363(8)
_cell_formula_units_Z            2
_cell_length_a                   10.035(5)
_cell_length_b                   10.316(5)
_cell_length_c                   18.247(9)
_cell_measurement_reflns_used    968
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.23
_cell_measurement_theta_min      3.77
_cell_volume                     1692.6(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10659
_diffrn_reflns_theta_full        23.31
_diffrn_reflns_theta_max         23.31
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_meas      0
_exptl_crystal_description       rods
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.997
_refine_diff_density_min         -0.778
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.054(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4817
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0443P)²+0.1283P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                4211
_reflns_number_total             4817
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0395240si20031117_031625.cif
_cod_data_source_block           Pd(depx)2
_cod_original_cell_volume        1692.6(15)
_cod_database_code               4112538
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pd1 Pd 0.57782(3) 0.72355(3) 0.241294(14) 0.01550(15) Uani 1 1 d .
P1 P 0.77336(10) 0.52430(9) 0.28297(5) 0.0189(2) Uani 1 1 d .
P2 P 0.51499(10) 0.70155(9) 0.12830(5) 0.0184(2) Uani 1 1 d .
P3 P 0.63466(10) 0.92723(9) 0.21594(5) 0.0187(2) Uani 1 1 d .
P4 P 0.38864(10) 0.74276(10) 0.34090(5) 0.0209(2) Uani 1 1 d .
C1 C 0.7577(4) 0.4652(4) 0.3853(2) 0.0259(9) Uani 1 1 d .
H1A H 0.6827 0.4226 0.3976 0.031 Uiso 1 1 calc R
H1B H 0.8527 0.3905 0.3965 0.031 Uiso 1 1 calc R
C2 C 0.7165(4) 0.5837(4) 0.4344(2) 0.0254(9) Uani 1 1 d .
C3 C 0.8263(5) 0.6049(4) 0.4602(2) 0.0342(10) Uani 1 1 d .
H3A H 0.9255 0.5434 0.4470 0.041 Uiso 1 1 calc R
C4 C 0.7965(6) 0.7126(5) 0.5046(2) 0.0432(12) Uani 1 1 d .
H4A H 0.8744 0.7254 0.5212 0.052 Uiso 1 1 calc R
C5 C 0.6532(6) 0.8012(5) 0.5245(2) 0.0456(12) Uani 1 1 d .
H5A H 0.6313 0.8761 0.5548 0.055 Uiso 1 1 calc R
C6 C 0.5408(5) 0.7805(4) 0.5002(2) 0.0363(10) Uani 1 1 d .
H6A H 0.4420 0.8415 0.5145 0.044 Uiso 1 1 calc R
C7 C 0.5691(4) 0.6735(4) 0.45578(19) 0.0249(9) Uani 1 1 d .
C8 C 0.4432(4) 0.6513(4) 0.4331(2) 0.0282(9) Uani 1 1 d .
H8A H 0.3570 0.6850 0.4721 0.034 Uiso 1 1 calc R
H8B H 0.4704 0.5481 0.4320 0.034 Uiso 1 1 calc R
C9 C 0.5577(4) 0.8170(4) 0.0462(2) 0.0231(8) Uani 1 1 d .
H9A H 0.5334 0.7937 0.0012 0.028 Uiso 1 1 calc R
H9B H 0.4937 0.9172 0.0540 0.028 Uiso 1 1 calc R
C10 C 0.7147(4) 0.8039(4) 0.03161(19) 0.0212(8) Uani 1 1 d .
C11 C 0.8167(4) 0.7060(4) -0.0164(2) 0.0287(9) Uani 1 1 d .
H11A H 0.7852 0.6483 -0.0390 0.034 Uiso 1 1 calc R
C12 C 0.9615(5) 0.6907(5) -0.0318(2) 0.0356(10) Uani 1 1 d .
H12A H 1.0289 0.6223 -0.0641 0.043 Uiso 1 1 calc R
C13 C 1.0086(5) 0.7753(5) -0.0002(2) 0.0383(11) Uani 1 1 d .
H13A H 1.1083 0.7658 -0.0107 0.046 Uiso 1 1 calc R
C14 C 0.9094(5) 0.8737(4) 0.0470(2) 0.0318(10) Uani 1 1 d .
H14A H 0.9423 0.9320 0.0683 0.038 Uiso 1 1 calc R
C15 C 0.7623(4) 0.8902(4) 0.06436(19) 0.0232(9) Uani 1 1 d .
C16 C 0.6603(4) 0.9984(4) 0.1164(2) 0.0247(9) Uani 1 1 d .
H16A H 0.5632 1.0426 0.0984 0.030 Uiso 1 1 calc R
H16B H 0.6984 1.0741 0.1139 0.030 Uiso 1 1 calc R
C17 C 0.8132(4) 0.3521(4) 0.2475(2) 0.0257(9) Uani 1 1 d .
H17A H 0.7247 0.3289 0.2629 0.031 Uiso 1 1 calc R
H17B H 0.8270 0.3661 0.1920 0.031 Uiso 1 1 calc R
C18 C 0.9449(5) 0.2219(4) 0.2711(3) 0.0445(12) Uani 1 1 d .
H18A H 0.9523 0.1395 0.2478 0.067 Uiso 1 1 calc R
H18B H 0.9318 0.2025 0.3257 0.067 Uiso 1 1 calc R
H18C H 1.0349 0.2405 0.2548 0.067 Uiso 1 1 calc R
C19 C 0.9584(4) 0.5287(4) 0.2696(2) 0.0253(9) Uani 1 1 d .
H19A H 0.9538 0.6108 0.2931 0.030 Uiso 1 1 calc R
H19B H 1.0252 0.4411 0.2952 0.030 Uiso 1 1 calc R
C20 C 1.0207(5) 0.5402(5) 0.1869(2) 0.0362(10) Uani 1 1 d .
H20A H 1.1190 0.5415 0.1824 0.054 Uiso 1 1 calc R
H20B H 0.9563 0.6281 0.1617 0.054 Uiso 1 1 calc R
H20C H 1.0266 0.4585 0.1635 0.054 Uiso 1 1 calc R
C21 C 0.3185(4) 0.7538(4) 0.1205(2) 0.0297(9) Uani 1 1 d .
H21A H 0.3091 0.7479 0.0682 0.036 Uiso 1 1 calc R
H21B H 0.2822 0.6852 0.1531 0.036 Uiso 1 1 calc R
C22 C 0.2222(4) 0.9023(4) 0.1421(2) 0.0361(10) Uani 1 1 d .
H22A H 0.1201 0.9227 0.1368 0.054 Uiso 1 1 calc R
H22B H 0.2554 0.9715 0.1092 0.054 Uiso 1 1 calc R
H22C H 0.2288 0.9088 0.1942 0.054 Uiso 1 1 calc R
C23 C 0.5917(5) 0.5338(4) 0.0823(2) 0.0292(9) Uani 1 1 d .
H23A H 0.5660 0.5558 0.0307 0.035 Uiso 1 1 calc R
H23B H 0.7001 0.4964 0.0783 0.035 Uiso 1 1 calc R
C24 C 0.5396(5) 0.4179(4) 0.1218(2) 0.0388(11) Uani 1 1 d .
H24A H 0.5856 0.3338 0.0937 0.058 Uiso 1 1 calc R
H24B H 0.4326 0.4523 0.1247 0.058 Uiso 1 1 calc R
H24C H 0.5669 0.3929 0.1725 0.058 Uiso 1 1 calc R
C25 C 0.8055(4) 0.9213(4) 0.2433(2) 0.0255(9) Uani 1 1 d .
H25A H 0.8893 0.8382 0.2233 0.031 Uiso 1 1 calc R
H25B H 0.8226 1.0080 0.2204 0.031 Uiso 1 1 calc R
C26 C 0.8001(5) 0.9112(5) 0.3282(2) 0.0402(11) Uani 1 1 d .
H26A H 0.8931 0.9077 0.3398 0.060 Uiso 1 1 calc R
H26B H 0.7846 0.8249 0.3511 0.060 Uiso 1 1 calc R
H26C H 0.7192 0.9946 0.3482 0.060 Uiso 1 1 calc R
C27 C 0.5090(4) 1.0984(4) 0.2528(2) 0.0283(9) Uani 1 1 d .
H27A H 0.4877 1.0821 0.3079 0.034 Uiso 1 1 calc R
H27B H 0.5603 1.1650 0.2422 0.034 Uiso 1 1 calc R
C28 C 0.3644(5) 1.1687(4) 0.2212(3) 0.0382(11) Uani 1 1 d .
H28A H 0.3055 1.2581 0.2437 0.057 Uiso 1 1 calc R
H28B H 0.3106 1.1053 0.2327 0.057 Uiso 1 1 calc R
H28C H 0.3835 1.1882 0.1667 0.057 Uiso 1 1 calc R
C29 C 0.2500(4) 0.6689(4) 0.3366(2) 0.0329(10) Uani 1 1 d .
H29A H 0.1833 0.6796 0.3846 0.040 Uiso 1 1 calc R
H29B H 0.1904 0.7246 0.2964 0.040 Uiso 1 1 calc R
C30 C 0.3167(5) 0.5146(5) 0.3218(3) 0.0411(11) Uani 1 1 d .
H30A H 0.2384 0.4817 0.3200 0.062 Uiso 1 1 calc R
H30B H 0.3738 0.4582 0.3621 0.062 Uiso 1 1 calc R
H30C H 0.3813 0.5034 0.2738 0.062 Uiso 1 1 calc R
C31 C 0.2687(4) 0.9235(4) 0.3664(2) 0.0328(10) Uani 1 1 d .
H31A H 0.3328 0.9685 0.3769 0.039 Uiso 1 1 calc R
H31B H 0.2239 0.9778 0.3214 0.039 Uiso 1 1 calc R
C32 C 0.1443(5) 0.9452(5) 0.4321(2) 0.0436(11) Uani 1 1 d .
H32A H 0.0921 1.0470 0.4378 0.065 Uiso 1 1 calc R
H32B H 0.1853 0.8965 0.4782 0.065 Uiso 1 1 calc R
H32C H 0.0757 0.9060 0.4224 0.065 Uiso 1 1 calc R
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'
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
P2 Pd1 P4 112.45(5)
P2 Pd1 P1 113.74(4)
P4 Pd1 P1 102.66(5)
P2 Pd1 P3 103.73(4)
P4 Pd1 P3 112.64(4)
P1 Pd1 P3 111.94(5)
C19 P1 C17 101.41(17)
C19 P1 C1 98.99(18)
C17 P1 C1 97.94(17)
C19 P1 Pd1 119.55(13)
C17 P1 Pd1 117.92(12)
C1 P1 Pd1 117.16(12)
C21 P2 C23 99.08(18)
C21 P2 C9 97.57(17)
C23 P2 C9 97.24(18)
C21 P2 Pd1 118.52(13)
C23 P2 Pd1 123.70(13)
C9 P2 Pd1 115.73(13)
C27 P3 C25 97.70(18)
C27 P3 C16 96.79(17)
C25 P3 C16 98.28(17)
C27 P3 Pd1 121.87(13)
C25 P3 Pd1 119.31(12)
C16 P3 Pd1 117.85(12)
C31 P4 C29 100.8(2)
C31 P4 C8 101.34(18)
C29 P4 C8 97.59(18)
C31 P4 Pd1 117.02(13)
C29 P4 Pd1 119.73(14)
C8 P4 Pd1 116.89(13)
C2 C1 P1 113.5(3)
C3 C2 C7 118.6(4)
C3 C2 C1 119.0(4)
C7 C2 C1 122.4(3)
C2 C3 C4 122.0(4)
C5 C4 C3 119.4(4)
C4 C5 C6 119.6(4)
C7 C6 C5 121.6(4)
C6 C7 C2 118.8(4)
C6 C7 C8 119.8(4)
C2 C7 C8 121.4(3)
C7 C8 P4 115.0(3)
C10 C9 P2 114.6(2)
C11 C10 C15 118.6(3)
C11 C10 C9 119.7(3)
C15 C10 C9 121.6(3)
C12 C11 C10 121.8(4)
C11 C12 C13 119.8(4)
C14 C13 C12 119.4(4)
C13 C14 C15 122.0(4)
C14 C15 C10 118.3(3)
C14 C15 C16 119.5(3)
C10 C15 C16 122.2(3)
C15 C16 P3 114.8(2)
C18 C17 P1 118.8(3)
C20 C19 P1 112.2(3)
C22 C21 P2 113.9(3)
C24 C23 P2 115.2(3)
C26 C25 P3 112.6(3)
C28 C27 P3 115.2(3)
C30 C29 P4 113.2(3)
C32 C31 P4 120.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 P2 2.3345(14)
Pd1 P4 2.3384(13)
Pd1 P1 2.3415(12)
Pd1 P3 2.3470(14)
P1 C19 1.845(4)
P1 C17 1.853(4)
P1 C1 1.867(4)
P2 C21 1.851(4)
P2 C23 1.855(4)
P2 C9 1.857(4)
P3 C27 1.853(4)
P3 C25 1.849(4)
P3 C16 1.860(4)
P4 C31 1.846(4)
P4 C29 1.852(4)
P4 C8 1.857(4)
C1 C2 1.508(5)
C2 C3 1.380(5)
C2 C7 1.413(5)
C3 C4 1.382(6)
C4 C5 1.375(7)
C5 C6 1.388(6)
C6 C7 1.379(6)
C7 C8 1.509(5)
C9 C10 1.501(5)
C10 C11 1.397(5)
C10 C15 1.412(5)
C11 C12 1.376(6)
C12 C13 1.382(6)
C13 C14 1.382(6)
C14 C15 1.396(5)
C15 C16 1.500(5)
C17 C18 1.531(6)
C19 C20 1.527(5)
C21 C22 1.515(6)
C23 C24 1.521(6)
C25 C26 1.529(6)
C27 C28 1.517(6)
C29 C30 1.506(6)
C31 C32 1.533(5)
