#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:16:44 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178600 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/11/4071194.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_4071194
loop_
_publ_author_name
'Bai, Tao'
'Xue, Liqin'
'Xue, Peng'
'Zhu, Jun'
'Sung, Herman Ho-Yung'
'Ma, Shengming'
'Wiliams, Ian Duncan'
'Lin, Zhenyang'
'Jia, Guochen'
_publ_section_title
;
 Insertion Reactions of Allenes with Palladium Aryl Complexes
 [PdI(Ph)(PPh3)]2and PdI(Ph)(dppe)
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2614
_journal_paper_doi               10.1021/om800030a
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C31 H32 I P Pd'
_chemical_formula_weight         668.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 95.5750(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8326(11)
_cell_length_b                   10.1125(7)
_cell_length_c                   18.9106(14)
_cell_measurement_reflns_used    5187
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.67
_cell_volume                     2823.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            15844
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         5514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0197
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0264P)²+1.2505P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0494
_reflns_number_gt                5072
_reflns_number_total             5514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800030a-file002.cif
_cod_data_source_block           peng46-trans-5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4071194
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.223258(10) 0.512308(14) 0.304426(7) 0.01486(5) Uani 1 1 d .
I1 I 0.181491(9) 0.579383(13) 0.169764(7) 0.02188(5) Uani 1 1 d .
P1 P 0.27588(3) 0.29658(5) 0.29984(3) 0.01550(10) Uani 1 1 d .
C1 C 0.23856(15) 0.5134(2) 0.41830(10) 0.0204(4) Uani 1 1 d .
H1A H 0.1839 0.4919 0.4422 0.025 Uiso 1 1 calc R
H1B H 0.2946 0.4729 0.4415 0.025 Uiso 1 1 calc R
C2 C 0.24581(14) 0.6454(2) 0.39396(10) 0.0186(4) Uani 1 1 d .
C3 C 0.17370(14) 0.7010(2) 0.34869(11) 0.0201(4) Uani 1 1 d .
H3A H 0.1919 0.7813 0.3227 0.024 Uiso 1 1 calc R
C4 C 0.07086(14) 0.6945(2) 0.35602(12) 0.0255(5) Uani 1 1 d .
C5 C 0.05459(17) 0.7368(3) 0.43188(14) 0.0389(6) Uani 1 1 d .
H5A H 0.0826 0.6724 0.4659 0.058 Uiso 1 1 calc R
H5B H -0.0107 0.7409 0.4361 0.058 Uiso 1 1 calc R
H5C H 0.0815 0.8241 0.4419 0.058 Uiso 1 1 calc R
C6 C 0.02587(17) 0.7965(3) 0.30346(15) 0.0454(7) Uani 1 1 d .
H6A H 0.0358 0.7709 0.2548 0.068 Uiso 1 1 calc R
H6B H 0.0524 0.8839 0.3139 0.068 Uiso 1 1 calc R
H6C H -0.0393 0.7997 0.3081 0.068 Uiso 1 1 calc R
C7 C 0.02546(17) 0.5598(3) 0.34011(17) 0.0441(7) Uani 1 1 d .
H7A H 0.0531 0.4935 0.3733 0.066 Uiso 1 1 calc R
H7B H 0.0338 0.5334 0.2913 0.066 Uiso 1 1 calc R
H7C H -0.0394 0.5666 0.3456 0.066 Uiso 1 1 calc R
C8 C 0.33660(14) 0.7119(2) 0.40244(11) 0.0197(4) Uani 1 1 d .
C9 C 0.37566(14) 0.7695(2) 0.34553(11) 0.0208(4) Uani 1 1 d .
H9A H 0.3435 0.7692 0.2996 0.025 Uiso 1 1 calc R
C10 C 0.46088(15) 0.8272(2) 0.35551(11) 0.0247(4) Uani 1 1 d .
H10A H 0.4871 0.8645 0.3162 0.030 Uiso 1 1 calc R
C11 C 0.50802(16) 0.8307(3) 0.42268(13) 0.0354(6) Uani 1 1 d .
H11A H 0.5661 0.8710 0.4295 0.042 Uiso 1 1 calc R
C12 C 0.46968(19) 0.7748(3) 0.47969(13) 0.0466(7) Uani 1 1 d .
H12A H 0.5014 0.7773 0.5258 0.056 Uiso 1 1 calc R
C13 C 0.38462(16) 0.7148(3) 0.46962(12) 0.0335(6) Uani 1 1 d .
H13A H 0.3592 0.6756 0.5088 0.040 Uiso 1 1 calc R
C21 C 0.25183(13) 0.18569(19) 0.22360(10) 0.0177(4) Uani 1 1 d .
C22 C 0.22453(14) 0.0550(2) 0.23197(11) 0.0199(4) Uani 1 1 d .
H22A H 0.2160 0.0227 0.2780 0.024 Uiso 1 1 calc R
C23 C 0.20964(14) -0.0283(2) 0.17354(11) 0.0221(4) Uani 1 1 d .
H23A H 0.1908 -0.1169 0.1798 0.027 Uiso 1 1 calc R
C24 C 0.22216(15) 0.0177(2) 0.10609(12) 0.0246(5) Uani 1 1 d .
H24A H 0.2122 -0.0395 0.0662 0.030 Uiso 1 1 calc R
C25 C 0.24941(17) 0.1477(2) 0.09706(11) 0.0290(5) Uani 1 1 d .
H25A H 0.2579 0.1794 0.0509 0.035 Uiso 1 1 calc R
C26 C 0.26426(15) 0.2317(2) 0.15538(11) 0.0248(5) Uani 1 1 d .
H26A H 0.2829 0.3204 0.1489 0.030 Uiso 1 1 calc R
C31 C 0.39953(13) 0.2896(2) 0.31509(10) 0.0176(4) Uani 1 1 d .
C32 C 0.44749(14) 0.1721(2) 0.30662(11) 0.0212(4) Uani 1 1 d .
H32A H 0.4155 0.0937 0.2923 0.025 Uiso 1 1 calc R
C33 C 0.54117(14) 0.1695(2) 0.31891(11) 0.0227(4) Uani 1 1 d .
H33A H 0.5730 0.0891 0.3138 0.027 Uiso 1 1 calc R
C34 C 0.58863(14) 0.2847(2) 0.33883(10) 0.0218(4) Uani 1 1 d .
H34A H 0.6528 0.2825 0.3475 0.026 Uiso 1 1 calc R
C35 C 0.54227(14) 0.4028(2) 0.34611(11) 0.0231(4) Uani 1 1 d .
H35A H 0.5747 0.4816 0.3589 0.028 Uiso 1 1 calc R
C36 C 0.44806(14) 0.4051(2) 0.33459(11) 0.0201(4) Uani 1 1 d .
H36A H 0.4164 0.4856 0.3400 0.024 Uiso 1 1 calc R
C41 C 0.23218(14) 0.20233(19) 0.37189(10) 0.0179(4) Uani 1 1 d .
C42 C 0.13815(15) 0.2085(2) 0.37548(11) 0.0234(4) Uani 1 1 d .
H42A H 0.1016 0.2579 0.3409 0.028 Uiso 1 1 calc R
C43 C 0.09778(16) 0.1431(2) 0.42892(11) 0.0273(5) Uani 1 1 d .
H43A H 0.0341 0.1475 0.4307 0.033 Uiso 1 1 calc R
C44 C 0.15130(17) 0.0710(2) 0.47980(11) 0.0284(5) Uani 1 1 d .
H44A H 0.1244 0.0279 0.5171 0.034 Uiso 1 1 calc R
C45 C 0.24428(17) 0.0623(2) 0.47595(11) 0.0282(5) Uani 1 1 d .
H45A H 0.2804 0.0116 0.5102 0.034 Uiso 1 1 calc R
C46 C 0.28502(15) 0.1275(2) 0.42208(11) 0.0228(4) Uani 1 1 d .
H46A H 0.3485 0.1208 0.4197 0.027 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'
I I -0.4742 1.8119 '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
C1 Pd1 C2 38.50(8)
C1 Pd1 C3 68.06(8)
C2 Pd1 C3 37.60(7)
C1 Pd1 P1 92.23(6)
C2 Pd1 P1 125.94(6)
C3 Pd1 P1 160.00(5)
C1 Pd1 I1 163.00(6)
C2 Pd1 I1 126.64(5)
C3 Pd1 I1 94.97(5)
P1 Pd1 I1 104.640(13)
C31 P1 C41 106.52(9)
C31 P1 C21 102.45(9)
C41 P1 C21 102.16(9)
C31 P1 Pd1 111.46(7)
C41 P1 Pd1 108.46(6)
C21 P1 Pd1 124.30(7)
C2 C1 Pd1 71.52(11)
C3 C2 C1 119.44(18)
C3 C2 C8 120.21(18)
C1 C2 C8 118.84(18)
C3 C2 Pd1 73.99(11)
C1 C2 Pd1 69.99(11)
C8 C2 Pd1 115.56(13)
C2 C3 C4 128.41(19)
C2 C3 Pd1 68.42(11)
C4 C3 Pd1 111.12(13)
C7 C4 C5 108.9(2)
C7 C4 C6 108.3(2)
C5 C4 C6 108.6(2)
C7 C4 C3 115.94(18)
C5 C4 C3 108.50(18)
C6 C4 C3 106.46(19)
C13 C8 C9 118.63(19)
C13 C8 C2 118.72(18)
C9 C8 C2 122.65(18)
C10 C9 C8 120.69(19)
C9 C10 C11 120.4(2)
C12 C11 C10 119.5(2)
C11 C12 C13 120.3(2)
C8 C13 C12 120.5(2)
C22 C21 C26 118.98(18)
C22 C21 P1 121.74(15)
C26 C21 P1 119.24(15)
C23 C22 C21 120.61(19)
C24 C23 C22 120.20(19)
C23 C24 C25 119.7(2)
C24 C25 C26 120.3(2)
C25 C26 C21 120.2(2)
C32 C31 C36 118.85(18)
C32 C31 P1 121.78(15)
C36 C31 P1 119.36(15)
C33 C32 C31 120.56(19)
C32 C33 C34 120.1(2)
C35 C34 C33 120.16(19)
C34 C35 C36 119.76(19)
C35 C36 C31 120.58(19)
C46 C41 C42 119.10(19)
C46 C41 P1 124.93(16)
C42 C41 P1 115.97(15)
C43 C42 C41 120.9(2)
C42 C43 C44 119.6(2)
C45 C44 C43 119.9(2)
C44 C45 C46 120.6(2)
C41 C46 C45 119.8(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 C1 2.143(2)
Pd1 C2 2.1634(19)
Pd1 C3 2.2363(19)
Pd1 P1 2.3214(5)
Pd1 I1 2.6500(3)
P1 C31 1.830(2)
P1 C41 1.832(2)
P1 C21 1.834(2)
C1 C2 1.420(3)
C2 C3 1.419(3)
C2 C8 1.500(3)
C3 C4 1.546(3)
C4 C7 1.536(3)
C4 C5 1.538(3)
C4 C6 1.539(3)
C8 C13 1.395(3)
C8 C9 1.398(3)
C9 C10 1.388(3)
C10 C11 1.390(3)
C11 C12 1.387(3)
C12 C13 1.396(3)
C21 C22 1.395(3)
C21 C26 1.400(3)
C22 C23 1.390(3)
C23 C24 1.387(3)
C24 C25 1.391(3)
C25 C26 1.392(3)
C31 C32 1.402(3)
C31 C36 1.402(3)
C32 C33 1.387(3)
C33 C34 1.394(3)
C34 C35 1.392(3)
C35 C36 1.393(3)
C41 C46 1.394(3)
C41 C42 1.404(3)
C42 C43 1.391(3)
C43 C44 1.392(3)
C44 C45 1.391(3)
C45 C46 1.399(3)
