#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:06:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179313 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/10/4321085.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_4321085
loop_
_publ_author_name
'Larry R. Falvello'
'Susana Fernández'
'Rafael Navarro'
'Esteban P. Urriolabeitia'
_publ_section_title
;
 Reactivity of Pd(0) Complexes with the Phosphino Ylide
 [Ph2PCH2PPh2C(H)C(O)Me]. Molecular Structure of
 [Pd(PPh2CHPPh2C(H)C(O)Me)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2957
_journal_page_last               2960
_journal_paper_doi               10.1021/ic990923z
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C56 H50 O2 P4 Pd'
_chemical_formula_weight         985.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.236(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.443(3)
_cell_length_b                   17.7206(17)
_cell_length_c                   16.871(3)
_cell_measurement_temperature    223(2)
_cell_volume                     4669.0(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.483
_diffrn_measured_fraction_theta_max 0.483
_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  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5533
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.9499
_exptl_absorpt_correction_T_min  0.7306
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.296
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0396P)²+2.0298P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                4448
_reflns_number_total             5351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990923z.cif
_cod_data_source_block           cad4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+2.0298P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+2.0298P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4669.0(13)
_cod_database_code               4321085
loop_
_symmetry_equiv_pos_as_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_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.5000 0.278628(13) 0.7500 0.02152(7) Uani 1 d S . .
P1 P 0.56257(4) 0.22470(3) 0.59725(4) 0.02576(13) Uani 1 d . . .
P2 P 0.47477(4) 0.36434(3) 0.84441(4) 0.02467(13) Uani 1 d . . .
C1 C 0.67767(15) 0.21923(14) 0.65181(16) 0.0308(5) Uani 1 d . . .
C2 C 0.71572(17) 0.17873(17) 0.72359(18) 0.0430(6) Uani 1 d . . .
H2A H 0.6818 0.1491 0.7471 0.052 Uiso 1 calc R . .
C3 C 0.80414(19) 0.1814(2) 0.7616(2) 0.0549(8) Uani 1 d . . .
H3A H 0.8297 0.1535 0.8105 0.066 Uiso 1 calc R . .
C4 C 0.85351(19) 0.22442(18) 0.7278(2) 0.0551(9) Uani 1 d . . .
H4A H 0.9131 0.2262 0.7536 0.066 Uiso 1 calc R . .
C5 C 0.8169(2) 0.26527(19) 0.6562(2) 0.0575(9) Uani 1 d . . .
H5A H 0.8514 0.2946 0.6329 0.069 Uiso 1 calc R . .
C6 C 0.72917(18) 0.26292(17) 0.6185(2) 0.0455(7) Uani 1 d . . .
H6A H 0.7041 0.2912 0.5698 0.055 Uiso 1 calc R . .
C7 C 0.54966(15) 0.16289(14) 0.50856(15) 0.0301(5) Uani 1 d . . .
C8 C 0.59049(18) 0.09345(16) 0.52106(17) 0.0409(6) Uani 1 d . . .
H8A H 0.6260 0.0801 0.5746 0.049 Uiso 1 calc R . .
C9 C 0.57940(19) 0.04365(17) 0.4553(2) 0.0504(8) Uani 1 d . . .
H9A H 0.6063 -0.0038 0.4646 0.060 Uiso 1 calc R . .
C10 C 0.52918(19) 0.06343(17) 0.37653(18) 0.0448(7) Uani 1 d . . .
H10A H 0.5230 0.0301 0.3316 0.054 Uiso 1 calc R . .
C11 C 0.48813(19) 0.13158(17) 0.36339(18) 0.0434(7) Uani 1 d . . .
H11A H 0.4529 0.1445 0.3096 0.052 Uiso 1 calc R . .
C12 C 0.49803(17) 0.18202(15) 0.42900(16) 0.0369(6) Uani 1 d . . .
H12A H 0.4698 0.2289 0.4194 0.044 Uiso 1 calc R . .
C13 C 0.52487(16) 0.31291(14) 0.56735(15) 0.0295(5) Uani 1 d . . .
H13 H 0.5400(17) 0.3362(15) 0.5263(17) 0.034(7) Uiso 1 d . . .
C14 C 0.54722(17) 0.44327(14) 0.88306(16) 0.0337(6) Uani 1 d . . .
C15 C 0.62661(19) 0.42893(19) 0.94168(19) 0.0488(7) Uani 1 d . . .
H15A H 0.6396 0.3803 0.9643 0.059 Uiso 1 calc R . .
C16 C 0.6868(2) 0.4864(2) 0.9668(2) 0.0678(11) Uani 1 d . . .
H16A H 0.7409 0.4759 1.0050 0.081 Uiso 1 calc R . .
C17 C 0.6680(3) 0.5575(2) 0.9365(3) 0.0756(13) Uani 1 d . . .
H17A H 0.7092 0.5960 0.9535 0.091 Uiso 1 calc R . .
C18 C 0.5890(3) 0.57304(19) 0.8812(3) 0.0696(11) Uani 1 d . . .
H18A H 0.5753 0.6226 0.8618 0.084 Uiso 1 calc R . .
C19 C 0.5292(2) 0.51612(16) 0.8538(2) 0.0489(7) Uani 1 d . . .
H19A H 0.4757 0.5272 0.8148 0.059 Uiso 1 calc R . .
C20 C 0.37005(15) 0.40841(13) 0.79959(15) 0.0295(5) Uani 1 d . . .
C21 C 0.33961(18) 0.46073(16) 0.84560(19) 0.0415(6) Uani 1 d . . .
H21A H 0.3755 0.4769 0.8979 0.050 Uiso 1 calc R . .
C22 C 0.2573(2) 0.48885(18) 0.8148(2) 0.0519(8) Uani 1 d . . .
H22A H 0.2376 0.5241 0.8462 0.062 Uiso 1 calc R . .
C23 C 0.2043(2) 0.46560(19) 0.7389(2) 0.0533(8) Uani 1 d . . .
H23A H 0.1484 0.4850 0.7180 0.064 Uiso 1 calc R . .
C24 C 0.23320(19) 0.4138(2) 0.6932(2) 0.0512(8) Uani 1 d . . .
H24A H 0.1968 0.3978 0.6410 0.061 Uiso 1 calc R . .
C25 C 0.31549(17) 0.38480(16) 0.72346(17) 0.0376(6) Uani 1 d . . .
H25A H 0.3342 0.3489 0.6920 0.045 Uiso 1 calc R . .
C26 C 0.51024(15) 0.18820(13) 0.66684(15) 0.0267(5) Uani 1 d . . .
H26A H 0.5460 0.1475 0.7005 0.032 Uiso 1 calc R . .
C27 C 0.42131(16) 0.15978(14) 0.63083(16) 0.0332(6) Uani 1 d . . .
O1 O 0.39915(13) 0.10150(10) 0.65730(13) 0.0443(5) Uani 1 d . . .
C28 C 0.35536(18) 0.20252(18) 0.5637(2) 0.0482(7) Uani 1 d . . .
H28A H 0.3222 0.1674 0.5218 0.072 Uiso 1 calc R . .
H28B H 0.3838 0.2384 0.5378 0.072 Uiso 1 calc R . .
H28C H 0.3175 0.2293 0.5880 0.072 Uiso 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C26 Pd1 C26 84.85(12) 2_656 . y
C26 Pd1 P2 171.64(6) 2_656 2_656 y
C26 Pd1 P2 88.45(6) . 2_656 y
C26 Pd1 P2 88.45(6) 2_656 . y
C26 Pd1 P2 171.63(6) . . y
P2 Pd1 P2 98.64(3) 2_656 . y
C13 P1 C26 108.87(11) . . y
C13 P1 C7 111.92(12) . . y
C26 P1 C7 111.66(11) . . y
C13 P1 C1 114.96(12) . . y
C26 P1 C1 106.64(12) . . y
C7 P1 C1 102.63(11) . . y
C13 P2 C14 105.58(12) 2_656 . y
C13 P2 C20 109.15(11) 2_656 . y
C14 P2 C20 104.27(12) . . y
C13 P2 Pd1 106.81(8) 2_656 . y
C14 P2 Pd1 120.60(8) . . y
C20 P2 Pd1 110.02(8) . . y
C2 C1 C6 118.6(3) . . ?
C2 C1 P1 125.7(2) . . ?
C6 C1 P1 115.6(2) . . ?
C1 C2 C3 120.5(3) . . ?
C1 C2 H2A 119.7 . . ?
C3 C2 H2A 119.7 . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3A 120.1 . . ?
C2 C3 H3A 120.1 . . ?
C3 C4 C5 120.6(3) . . ?
C3 C4 H4A 119.7 . . ?
C5 C4 H4A 119.7 . . ?
C4 C5 C6 119.6(3) . . ?
C4 C5 H5A 120.2 . . ?
C6 C5 H5A 120.2 . . ?
C5 C6 C1 120.7(3) . . ?
C5 C6 H6A 119.6 . . ?
C1 C6 H6A 119.6 . . ?
C8 C7 C12 119.0(2) . . ?
C8 C7 P1 119.0(2) . . ?
C12 C7 P1 121.96(19) . . ?
C9 C8 C7 120.5(3) . . ?
C9 C8 H8A 119.7 . . ?
C7 C8 H8A 119.7 . . ?
C10 C9 C8 120.1(3) . . ?
C10 C9 H9A 119.9 . . ?
C8 C9 H9A 120.0 . . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C10 C11 C12 120.6(3) . . ?
C10 C11 H11A 119.7 . . ?
C12 C11 H11A 119.7 . . ?
C7 C12 C11 119.8(3) . . ?
C7 C12 H12A 120.1 . . ?
C11 C12 H12A 120.1 . . ?
P1 C13 P2 108.89(13) . 2_656 y
P1 C13 H13 119.0(17) . . y
P2 C13 H13 119.1(17) 2_656 . y
C19 C14 C15 118.2(3) . . ?
C19 C14 P2 123.2(2) . . ?
C15 C14 P2 118.5(2) . . ?
C16 C15 C14 120.2(3) . . ?
C16 C15 H15A 119.9 . . ?
C14 C15 H15A 119.9 . . ?
C17 C16 C15 120.6(4) . . ?
C17 C16 H16A 119.7 . . ?
C15 C16 H16A 119.7 . . ?
C16 C17 C18 119.8(3) . . ?
C16 C17 H17A 120.1 . . ?
C18 C17 H17A 120.1 . . ?
C17 C18 C19 120.3(4) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C14 C19 C18 120.8(3) . . ?
C14 C19 H19A 119.6 . . ?
C18 C19 H19A 119.6 . . ?
C25 C20 C21 118.4(2) . . ?
C25 C20 P2 120.63(19) . . ?
C21 C20 P2 120.6(2) . . ?
C22 C21 C20 120.6(3) . . ?
C22 C21 H21A 119.7 . . ?
C20 C21 H21A 119.7 . . ?
C23 C22 C21 120.3(3) . . ?
C23 C22 H22A 119.8 . . ?
C21 C22 H22A 119.8 . . ?
C22 C23 C24 119.7(3) . . ?
C22 C23 H23A 120.2 . . ?
C24 C23 H23A 120.2 . . ?
C23 C24 C25 120.6(3) . . ?
C23 C24 H24A 119.7 . . ?
C25 C24 H24A 119.7 . . ?
C20 C25 C24 120.3(3) . . ?
C20 C25 H25A 119.8 . . ?
C24 C25 H25A 119.8 . . ?
C27 C26 P1 118.08(18) . . y
C27 C26 Pd1 104.43(14) . . y
P1 C26 Pd1 108.02(11) . . y
C27 C26 H26A 108.7 . . ?
P1 C26 H26A 108.7 . . ?
Pd1 C26 H26A 108.7 . . ?
O1 C27 C26 120.3(3) . . y
O1 C27 C28 118.2(2) . . y
C26 C27 C28 121.5(2) . . y
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C26 2.171(2) 2_656 ?
Pd1 C26 2.171(2) . y
Pd1 P2 2.3301(6) 2_656 ?
Pd1 P2 2.3301(6) . y
P1 C13 1.699(3) . y
P1 C26 1.780(2) . y
P1 C7 1.812(2) . y
P1 C1 1.830(3) . y
P2 C13 1.744(2) 2_656 y
P2 C14 1.821(3) . y
P2 C20 1.825(2) . y
C1 C2 1.378(4) . ?
C1 C6 1.389(4) . ?
C2 C3 1.394(4) . ?
C2 H2A 0.9400 . ?
C3 C4 1.363(5) . ?
C3 H3A 0.9400 . ?
C4 C5 1.375(5) . ?
C4 H4A 0.9400 . ?
C5 C6 1.383(4) . ?
C5 H5A 0.9400 . ?
C6 H6A 0.9400 . ?
C7 C8 1.386(4) . ?
C7 C12 1.387(4) . ?
C8 C9 1.384(4) . ?
C8 H8A 0.9400 . ?
C9 C10 1.373(4) . ?
C9 H9A 0.9400 . ?
C10 C11 1.367(4) . ?
C10 H10A 0.9400 . ?
C11 C12 1.392(4) . ?
C11 H11A 0.9400 . ?
C12 H12A 0.9400 . ?
C13 P2 1.744(2) 2_656 ?
C13 H13 0.91(3) . y
C14 C19 1.381(4) . ?
C14 C15 1.392(4) . ?
C15 C16 1.390(4) . ?
C15 H15A 0.9400 . ?
C16 C17 1.359(6) . ?
C16 H16A 0.9400 . ?
C17 C18 1.370(6) . ?
C17 H17A 0.9400 . ?
C18 C19 1.383(4) . ?
C18 H18A 0.9400 . ?
C19 H19A 0.9400 . ?
C20 C25 1.381(4) . ?
C20 C21 1.398(3) . ?
C21 C22 1.382(4) . ?
C21 H21A 0.9400 . ?
C22 C23 1.368(5) . ?
C22 H22A 0.9400 . ?
C23 C24 1.375(5) . ?
C23 H23A 0.9400 . ?
C24 C25 1.386(4) . ?
C24 H24A 0.9400 . ?
C25 H25A 0.9400 . ?
C26 C27 1.485(3) . y
C26 H26A 0.9900 . ?
C27 O1 1.225(3) . y
C27 C28 1.505(4) . y
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C28 H28C 0.9700 . ?
