#------------------------------------------------------------------------------
#$Date: 2019-12-28 00:26:57 +0200 (Sat, 28 Dec 2019) $
#$Revision: 246259 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/72/4517271.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_4517271
loop_
_publ_author_name
'Scharf, Lennart T.'
'Rodstein, Ilja'
'Schmidt, Michelle'
'Scherpf, Thorsten'
'Gessner, Viktoria H.'
_publ_section_title
;
 Unraveling the High Activity of Ylide-Functionalized Phosphines in
 Palladium-Catalyzed Amination Reactions: A Comparative Study with
 CyJohnPhos and PtBu3
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              999
_journal_paper_doi               10.1021/acscatal.9b04666
_journal_year                    2019
_chemical_formula_moiety         'C39 H65 Cl P2 Pd, 2.5(C4 H8 O)'
_chemical_formula_sum            'C49 H85 Cl O2.5 P2 Pd'
_chemical_formula_weight         917.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                116.403(2)
_cell_angle_beta                 99.017(2)
_cell_angle_gamma                106.380(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8057(3)
_cell_length_b                   15.6134(3)
_cell_length_c                   15.6605(4)
_cell_measurement_reflns_used    17531
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      76.0410
_cell_measurement_theta_min      4.1010
_cell_volume                     2343.10(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4409
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34788
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.073
_diffrn_reflns_theta_min         3.336
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.645
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.078
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.882
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         8891
_refine_ls_number_restraints     256
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0273
_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)+(0.0402P)²+0.9924P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0707
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8258
_reflns_number_total             8891
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs9b04666_si_002.cif
_cod_data_source_block           ST144
_cod_original_cell_volume        2343.10(11)
_cod_original_formula_sum        'C49 H85 Cl O2.50 P2 Pd'
_cod_database_code               4517271
_shelx_shelxl_version_number     2018/1
_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.
;
_shelx_estimated_absorpt_t_min   0.556
_shelx_estimated_absorpt_t_max   0.885
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.41664(2) 0.36299(2) 0.44910(2) 0.01526(5) Uani 1 1 d . . . . .
Cl1 Cl 0.42734(4) 0.48675(3) 0.39502(3) 0.01998(9) Uani 1 1 d . . . . .
P1 P 0.69695(4) 0.27082(3) 0.51295(3) 0.01612(9) Uani 1 1 d . . . . .
P2 P 0.41299(4) 0.23816(3) 0.48910(3) 0.01487(9) Uani 1 1 d . . . . .
C1 C 0.55218(17) 0.22191(14) 0.52196(14) 0.0182(4) Uani 1 1 d . . . . .
C2 C 0.54353(18) 0.15094(15) 0.56633(16) 0.0239(4) Uani 1 1 d . . . . .
H2A H 0.474253 0.083169 0.519438 0.036 Uiso 1 1 calc R U . . .
H2B H 0.528912 0.183230 0.631035 0.036 Uiso 1 1 calc R U . . .
H2C H 0.621914 0.141195 0.576780 0.036 Uiso 1 1 calc R U . . .
C3 C 0.82737(17) 0.36527(14) 0.63509(14) 0.0190(4) Uani 1 1 d . . . . .
H3 H 0.905535 0.384657 0.618405 0.023 Uiso 1 1 calc R U . . .
C4 C 0.84983(19) 0.32104(15) 0.70328(15) 0.0225(4) Uani 1 1 d . . . . .
H4A H 0.773786 0.300539 0.720990 0.027 Uiso 1 1 calc R U . . .
H4B H 0.866210 0.257907 0.666169 0.027 Uiso 1 1 calc R U . . .
C5 C 0.9609(2) 0.40113(16) 0.80016(15) 0.0279(4) Uani 1 1 d . . . . .
H5A H 1.038273 0.416459 0.782734 0.033 Uiso 1 1 calc R U . . .
H5B H 0.970546 0.371369 0.843663 0.033 Uiso 1 1 calc R U . . .
C6 C 0.9430(2) 0.50260(16) 0.85850(15) 0.0280(4) Uani 1 1 d . . . . .
H6A H 0.870980 0.489082 0.882597 0.034 Uiso 1 1 calc R U . . .
H6B H 1.018490 0.554287 0.918085 0.034 Uiso 1 1 calc R U . . .
C7 C 0.9200(2) 0.54603(15) 0.79044(15) 0.0255(4) Uani 1 1 d . . . . .
H7A H 0.995513 0.565732 0.771837 0.031 Uiso 1 1 calc R U . . .
H7B H 0.904456 0.609571 0.827666 0.031 Uiso 1 1 calc R U . . .
C8 C 0.80796(18) 0.46598(14) 0.69441(15) 0.0222(4) Uani 1 1 d . . . . .
H8A H 0.796273 0.495899 0.651328 0.027 Uiso 1 1 calc R U . . .
H8B H 0.731423 0.449750 0.712750 0.027 Uiso 1 1 calc R U . . .
C9 C 0.75071(17) 0.16306(14) 0.45556(14) 0.0187(4) Uani 1 1 d . . . . .
H9 H 0.769748 0.144538 0.508052 0.022 Uiso 1 1 calc R U . . .
C10 C 0.87227(18) 0.19162(15) 0.43153(15) 0.0227(4) Uani 1 1 d . . . . .
H10A H 0.859134 0.209520 0.378576 0.027 Uiso 1 1 calc R U . . .
H10B H 0.938769 0.253398 0.492726 0.027 Uiso 1 1 calc R U . . .
C11 C 0.91335(18) 0.10009(15) 0.39509(16) 0.0248(4) Uani 1 1 d . . . . .
H11A H 0.989619 0.118613 0.377024 0.030 Uiso 1 1 calc R U . . .
H11B H 0.933991 0.086650 0.450469 0.030 Uiso 1 1 calc R U . . .
C12 C 0.8109(2) 0.00154(16) 0.30364(16) 0.0269(4) Uani 1 1 d . . . . .
H12A H 0.795903 0.012692 0.246112 0.032 Uiso 1 1 calc R U . . .
H12B H 0.838471 -0.056791 0.283966 0.032 Uiso 1 1 calc R U . . .
C13 C 0.69007(19) -0.02678(15) 0.32680(15) 0.0247(4) Uani 1 1 d . . . . .
H13A H 0.702772 -0.045652 0.379062 0.030 Uiso 1 1 calc R U . . .
H13B H 0.624046 -0.088371 0.265143 0.030 Uiso 1 1 calc R U . . .
C14 C 0.64702(18) 0.06322(14) 0.36394(15) 0.0223(4) Uani 1 1 d . . . . .
H14A H 0.571834 0.043823 0.382974 0.027 Uiso 1 1 calc R U . . .
H14B H 0.624163 0.076465 0.308746 0.027 Uiso 1 1 calc R U . . .
C15 C 0.70029(18) 0.33888(14) 0.44244(14) 0.0188(4) Uani 1 1 d . . . . .
H15 H 0.650181 0.381506 0.465813 0.023 Uiso 1 1 calc R U . . .
C16 C 0.63411(18) 0.26432(15) 0.32774(14) 0.0216(4) Uani 1 1 d . . . . .
H16A H 0.682376 0.222497 0.299335 0.026 Uiso 1 1 calc R U . . .
H16B H 0.549867 0.215878 0.314979 0.026 Uiso 1 1 calc R U . . .
C17 C 0.62249(19) 0.32584(16) 0.27586(15) 0.0245(4) Uani 1 1 d . . . . .
H17A H 0.568088 0.362770 0.300153 0.029 Uiso 1 1 calc R U . . .
H17B H 0.582761 0.277022 0.202125 0.029 Uiso 1 1 calc R U . . .
C18 C 0.7503(2) 0.40503(17) 0.29713(16) 0.0284(4) Uani 1 1 d . . . . .
H18A H 0.802394 0.368033 0.267402 0.034 Uiso 1 1 calc R U . . .
H18B H 0.739599 0.446126 0.265570 0.034 Uiso 1 1 calc R U . . .
C19 C 0.8153(2) 0.47783(16) 0.41073(16) 0.0268(4) Uani 1 1 d . . . . .
H19A H 0.765637 0.518136 0.439413 0.032 Uiso 1 1 calc R U . . .
H19B H 0.898565 0.527790 0.423744 0.032 Uiso 1 1 calc R U . . .
C20 C 0.83054(18) 0.41684(15) 0.46291(15) 0.0223(4) Uani 1 1 d . . . . .
H20A H 0.872260 0.465578 0.536480 0.027 Uiso 1 1 calc R U . . .
H20B H 0.883188 0.378729 0.436697 0.027 Uiso 1 1 calc R U . . .
C21 C 0.35558(17) 0.26304(13) 0.59834(14) 0.0173(3) Uani 1 1 d . . . . .
H21 H 0.337164 0.198732 0.602545 0.021 Uiso 1 1 calc R U . . .
C22 C 0.23210(18) 0.27705(15) 0.58259(15) 0.0221(4) Uani 1 1 d . . . . .
H22A H 0.246600 0.343304 0.583883 0.027 Uiso 1 1 calc R U . . .
H22B H 0.171734 0.219294 0.515804 0.027 Uiso 1 1 calc R U . . .
C23 C 0.1779(2) 0.27825(17) 0.66545(16) 0.0274(4) Uani 1 1 d . . . . .
H23A H 0.100199 0.290348 0.655995 0.033 Uiso 1 1 calc R U . . .
H23B H 0.156423 0.209539 0.659943 0.033 Uiso 1 1 calc R U . . .
C24 C 0.2705(2) 0.36309(16) 0.77030(16) 0.0278(4) Uani 1 1 d . . . . .
H24A H 0.236051 0.357285 0.822114 0.033 Uiso 1 1 calc R U . . .
H24B H 0.282335 0.432377 0.779536 0.033 Uiso 1 1 calc R U . . .
C25 C 0.3969(2) 0.35387(16) 0.78478(15) 0.0246(4) Uani 1 1 d . . . . .
H25A H 0.387026 0.288787 0.784844 0.030 Uiso 1 1 calc R U . . .
H25B H 0.456818 0.413176 0.851038 0.030 Uiso 1 1 calc R U . . .
C26 C 0.44968(18) 0.35319(15) 0.70102(14) 0.0214(4) Uani 1 1 d . . . . .
H26A H 0.465491 0.420131 0.703522 0.026 Uiso 1 1 calc R U . . .
H26B H 0.529887 0.344796 0.711011 0.026 Uiso 1 1 calc R U . . .
C27 C 0.28445(17) 0.10796(14) 0.38873(14) 0.0191(4) Uani 1 1 d . . . . .
H27 H 0.215531 0.124948 0.363718 0.023 Uiso 1 1 calc R U . . .
C28 C 0.22278(19) 0.02805(14) 0.41747(15) 0.0224(4) Uani 1 1 d . . . . .
H28A H 0.284564 0.003323 0.438000 0.027 Uiso 1 1 calc R U . . .
H28B H 0.194361 0.061566 0.475331 0.027 Uiso 1 1 calc R U . . .
C29 C 0.11112(19) -0.06457(15) 0.32747(16) 0.0261(4) Uani 1 1 d . . . . .
H29A H 0.074249 -0.116357 0.346134 0.031 Uiso 1 1 calc R U . . .
H29B H 0.046533 -0.040218 0.311161 0.031 Uiso 1 1 calc R U . . .
C30 C 0.1483(2) -0.11676(15) 0.23432(16) 0.0273(4) Uani 1 1 d . . . . .
H30A H 0.072961 -0.173226 0.176807 0.033 Uiso 1 1 calc R U . . .
H30B H 0.205915 -0.148072 0.247758 0.033 Uiso 1 1 calc R U . . .
C31 C 0.2122(2) -0.03703(15) 0.20731(15) 0.0270(4) Uani 1 1 d . . . . .
H31A H 0.151712 -0.011208 0.186923 0.032 Uiso 1 1 calc R U . . .
H31B H 0.240662 -0.070748 0.149533 0.032 Uiso 1 1 calc R U . . .
C32 C 0.32429(18) 0.05466(14) 0.29755(14) 0.0208(4) Uani 1 1 d . . . . .
H32A H 0.386866 0.029236 0.315344 0.025 Uiso 1 1 calc R U . . .
H32B H 0.363932 0.105755 0.278910 0.025 Uiso 1 1 calc R U . . .
C33 C 0.26840(18) 0.26721(14) 0.32454(14) 0.0200(4) Uani 1 1 d . . . . .
C34 C 0.27615(19) 0.21924(15) 0.22795(15) 0.0238(4) Uani 1 1 d . . . . .
H34 H 0.354303 0.219636 0.219738 0.029 Uiso 1 1 calc R U . . .
C35 C 0.1709(2) 0.17057(16) 0.14300(16) 0.0282(4) Uani 1 1 d . . . . .
H35 H 0.178414 0.137468 0.077796 0.034 Uiso 1 1 calc R U . . .
C36 C 0.0552(2) 0.16943(16) 0.15166(17) 0.0305(5) Uani 1 1 d . . . . .
C37 C 0.0471(2) 0.21777(17) 0.24785(17) 0.0290(4) Uani 1 1 d . . . . .
H37 H -0.031067 0.218062 0.255590 0.035 Uiso 1 1 calc R U . . .
C38 C 0.15159(19) 0.26601(15) 0.33350(15) 0.0240(4) Uani 1 1 d . . . . .
H38 H 0.143596 0.298404 0.398598 0.029 Uiso 1 1 calc R U . . .
C39 C -0.0580(2) 0.1195(2) 0.0592(2) 0.0451(6) Uani 1 1 d . . . . .
H39A H -0.038826 0.079419 -0.001346 0.068 Uiso 0.70(4) 1 calc R U P . .
H39B H -0.079788 0.173795 0.054788 0.068 Uiso 0.70(4) 1 calc R U P . .
H39C H -0.128533 0.072830 0.064252 0.068 Uiso 0.70(4) 1 calc R U P . .
H39D H -0.125939 0.137944 0.079809 0.068 Uiso 0.30(4) 1 calc R U P . .
H39E H -0.084977 0.043568 0.023675 0.068 Uiso 0.30(4) 1 calc R U P . .
H39F H -0.036232 0.144533 0.014211 0.068 Uiso 0.30(4) 1 calc R U P . .
O1_1 O 0.72871(19) 0.38232(14) 0.07270(13) 0.0437(4) Uani 1 1 d D . . . .
C1_1 C 0.6924(3) 0.2721(2) 0.0224(2) 0.0507(7) Uani 1 1 d D . . . .
H1A_1 H 0.642631 0.242675 0.055482 0.061 Uiso 1 1 calc R U . . .
H1B_1 H 0.767029 0.255077 0.024134 0.061 Uiso 1 1 calc R U . . .
C2_1 C 0.6149(3) 0.2280(2) -0.0854(2) 0.0498(7) Uani 1 1 d D . . . .
H2A_1 H 0.620753 0.162482 -0.132396 0.060 Uiso 1 1 calc R U . . .
H2B_1 H 0.526003 0.215575 -0.092402 0.060 Uiso 1 1 calc R U . . .
C3_1 C 0.6771(3) 0.3153(2) -0.10221(19) 0.0460(6) Uani 1 1 d D . . . .
H3A_1 H 0.619926 0.313431 -0.157101 0.055 Uiso 1 1 calc R U . . .
H3B_1 H 0.754171 0.312225 -0.118359 0.055 Uiso 1 1 calc R U . . .
C4_1 C 0.7064(3) 0.4108(2) -0.00128(19) 0.0426(6) Uani 1 1 d D . . . .
H4A_1 H 0.781234 0.469335 0.011748 0.051 Uiso 1 1 calc R U . . .
H4B_1 H 0.635161 0.432359 0.000120 0.051 Uiso 1 1 calc R U . . .
O1_2 O 0.3753(5) 0.2464(3) 0.0275(4) 0.0473(12) Uani 0.647(10) 1 d D U P A 1
C1_2 C 0.2652(8) 0.2149(5) -0.0527(4) 0.050(2) Uani 0.647(10) 1 d D U P A 1
H1A_2 H 0.204167 0.144944 -0.073968 0.060 Uiso 0.647(10) 1 calc R U P A 1
H1B_2 H 0.287652 0.212529 -0.111756 0.060 Uiso 0.647(10) 1 calc R U P A 1
C2_2 C 0.2103(7) 0.2955(7) -0.0104(6) 0.0430(17) Uani 0.647(10) 1 d D U P A 1
H2A_2 H 0.157201 0.281115 0.028605 0.052 Uiso 0.647(10) 1 calc R U P A 1
H2B_2 H 0.161651 0.300817 -0.064109 0.052 Uiso 0.647(10) 1 calc R U P A 1
C3_2 C 0.3313(4) 0.3929(3) 0.0576(4) 0.0362(11) Uani 0.647(10) 1 d D U P A 1
H3A_2 H 0.369227 0.420599 0.018353 0.043 Uiso 0.647(10) 1 calc R U P A 1
H3B_2 H 0.316331 0.448138 0.111988 0.043 Uiso 0.647(10) 1 calc R U P A 1
C4_2 C 0.4126(5) 0.3529(4) 0.0998(4) 0.0363(11) Uani 0.647(10) 1 d D U P A 1
H4A_2 H 0.501550 0.392166 0.112800 0.044 Uiso 0.647(10) 1 calc R U P A 1
H4B_2 H 0.402108 0.361067 0.164167 0.044 Uiso 0.647(10) 1 calc R U P A 1
O1_3 O 0.3339(10) 0.2316(7) -0.0165(9) 0.061(3) Uani 0.353(10) 1 d D U P A 2
C1_3 C 0.2152(12) 0.2191(10) -0.0695(9) 0.043(2) Uani 0.353(10) 1 d D U P A 2
H1A_3 H 0.150447 0.150989 -0.090017 0.052 Uiso 0.353(10) 1 calc R U P A 2
H1B_3 H 0.218148 0.222453 -0.130867 0.052 Uiso 0.353(10) 1 calc R U P A 2
C2_3 C 0.1856(11) 0.3070(12) 0.0017(11) 0.039(3) Uani 0.353(10) 1 d D U P A 2
H2A_3 H 0.115431 0.279795 0.022417 0.047 Uiso 0.353(10) 1 calc R U P A 2
H2B_3 H 0.162233 0.343821 -0.031145 0.047 Uiso 0.353(10) 1 calc R U P A 2
C3_3 C 0.3048(7) 0.3808(5) 0.0934(6) 0.0308(18) Uani 0.353(10) 1 d D U P A 2
H3A_3 H 0.326522 0.454048 0.111371 0.037 Uiso 0.353(10) 1 calc R U P A 2
H3B_3 H 0.295789 0.374985 0.152658 0.037 Uiso 0.353(10) 1 calc R U P A 2
C4_3 C 0.4015(9) 0.3419(9) 0.0563(10) 0.058(3) Uani 0.353(10) 1 d D U P A 2
H4A_3 H 0.441561 0.378464 0.024133 0.070 Uiso 0.353(10) 1 calc R U P A 2
H4B_3 H 0.467028 0.353556 0.112906 0.070 Uiso 0.353(10) 1 calc R U P A 2
O1_4 O 0.5068(5) -0.0121(5) -0.1029(4) 0.0760(14) Uani 0.5 1 d D . P B -1
C1_4 C 0.5801(13) -0.0362(13) -0.0421(9) 0.052(3) Uani 0.5 1 d D . P B -1
H1A_4 H 0.667547 -0.014410 -0.041683 0.063 Uiso 0.5 1 calc R U P B -1
H1B_4 H 0.545196 -0.111856 -0.067608 0.063 Uiso 0.5 1 calc R U P B -1
C2_4 C 0.5735(11) 0.0244(11) 0.0619(8) 0.056(3) Uani 0.5 1 d D . P B -1
H2A_4 H 0.636474 0.097089 0.098874 0.067 Uiso 0.5 1 calc R U P B -1
H2B_4 H 0.586886 -0.008789 0.101546 0.067 Uiso 0.5 1 calc R U P B -1
C3_4 C 0.4412(13) 0.0208(15) 0.0412(10) 0.052(3) Uani 0.5 1 d D . P B -1
H3A_4 H 0.383641 -0.035597 0.046008 0.062 Uiso 0.5 1 calc R U P B -1
H3B_4 H 0.439299 0.088014 0.088643 0.062 Uiso 0.5 1 calc R U P B -1
C4_4 C 0.4081(12) -0.0007(12) -0.0652(9) 0.060(3) Uani 0.5 1 d D . P B -1
H4A_4 H 0.331339 -0.065214 -0.108557 0.072 Uiso 0.5 1 calc R U P B -1
H4B_4 H 0.391366 0.057508 -0.066316 0.072 Uiso 0.5 1 calc R U P B -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 '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_3
C33 Pd1 P2 94.12(5) .
C33 Pd1 Cl1 84.41(5) .
P2 Pd1 Cl1 174.885(15) .
C33 Pd1 Cl1 164.58(6) 2_666
P2 Pd1 Cl1 98.095(16) 2_666
Cl1 Pd1 Cl1 84.197(16) 2_666
Pd1 Cl1 Pd1 95.803(15) 2_666
C1 P1 C15 113.31(9) .
C1 P1 C9 109.20(9) .
C15 P1 C9 110.98(8) .
C1 P1 C3 116.01(9) .
C15 P1 C3 104.96(8) .
C9 P1 C3 101.75(8) .
C1 P2 C21 104.87(9) .
C1 P2 C27 109.94(8) .
C21 P2 C27 100.06(8) .
C1 P2 Pd1 119.75(6) .
C21 P2 Pd1 109.61(6) .
C27 P2 Pd1 110.65(6) .
C2 C1 P1 113.54(13) .
C2 C1 P2 114.80(13) .
P1 C1 P2 131.66(11) .
C1 C2 H2A 109.5 .
C1 C2 H2B 109.5 .
H2A C2 H2B 109.5 .
C1 C2 H2C 109.5 .
H2A C2 H2C 109.5 .
H2B C2 H2C 109.5 .
C4 C3 C8 109.27(15) .
C4 C3 P1 114.11(13) .
C8 C3 P1 111.54(13) .
C4 C3 H3 107.2 .
C8 C3 H3 107.2 .
P1 C3 H3 107.2 .
C5 C4 C3 111.32(16) .
C5 C4 H4A 109.4 .
C3 C4 H4A 109.4 .
C5 C4 H4B 109.4 .
C3 C4 H4B 109.4 .
H4A C4 H4B 108.0 .
C4 C5 C6 111.61(17) .
C4 C5 H5A 109.3 .
C6 C5 H5A 109.3 .
C4 C5 H5B 109.3 .
C6 C5 H5B 109.3 .
H5A C5 H5B 108.0 .
C7 C6 C5 109.96(17) .
C7 C6 H6A 109.7 .
C5 C6 H6A 109.7 .
C7 C6 H6B 109.7 .
C5 C6 H6B 109.7 .
H6A C6 H6B 108.2 .
C6 C7 C8 111.28(17) .
C6 C7 H7A 109.4 .
C8 C7 H7A 109.4 .
C6 C7 H7B 109.4 .
C8 C7 H7B 109.4 .
H7A C7 H7B 108.0 .
C7 C8 C3 111.10(16) .
C7 C8 H8A 109.4 .
C3 C8 H8A 109.4 .
C7 C8 H8B 109.4 .
C3 C8 H8B 109.4 .
H8A C8 H8B 108.0 .
C10 C9 C14 111.15(15) .
C10 C9 P1 115.57(13) .
C14 C9 P1 112.68(13) .
C10 C9 H9 105.5 .
C14 C9 H9 105.5 .
P1 C9 H9 105.5 .
C11 C10 C9 110.41(16) .
C11 C10 H10A 109.6 .
C9 C10 H10A 109.6 .
C11 C10 H10B 109.6 .
C9 C10 H10B 109.6 .
H10A C10 H10B 108.1 .
C12 C11 C10 111.33(17) .
C12 C11 H11A 109.4 .
C10 C11 H11A 109.4 .
C12 C11 H11B 109.4 .
C10 C11 H11B 109.4 .
H11A C11 H11B 108.0 .
C13 C12 C11 111.02(16) .
C13 C12 H12A 109.4 .
C11 C12 H12A 109.4 .
C13 C12 H12B 109.4 .
C11 C12 H12B 109.4 .
H12A C12 H12B 108.0 .
C12 C13 C14 111.78(16) .
C12 C13 H13A 109.3 .
C14 C13 H13A 109.3 .
C12 C13 H13B 109.3 .
C14 C13 H13B 109.3 .
H13A C13 H13B 107.9 .
C13 C14 C9 111.00(16) .
C13 C14 H14A 109.4 .
C9 C14 H14A 109.4 .
C13 C14 H14B 109.4 .
C9 C14 H14B 109.4 .
H14A C14 H14B 108.0 .
C16 C15 C20 109.87(15) .
C16 C15 P1 113.15(13) .
C20 C15 P1 115.75(13) .
C16 C15 H15 105.7 .
C20 C15 H15 105.7 .
P1 C15 H15 105.7 .
C17 C16 C15 110.45(16) .
C17 C16 H16A 109.6 .
C15 C16 H16A 109.6 .
C17 C16 H16B 109.6 .
C15 C16 H16B 109.6 .
H16A C16 H16B 108.1 .
C16 C17 C18 111.40(17) .
C16 C17 H17A 109.3 .
C18 C17 H17A 109.3 .
C16 C17 H17B 109.3 .
C18 C17 H17B 109.3 .
H17A C17 H17B 108.0 .
C19 C18 C17 109.98(16) .
C19 C18 H18A 109.7 .
C17 C18 H18A 109.7 .
C19 C18 H18B 109.7 .
C17 C18 H18B 109.7 .
H18A C18 H18B 108.2 .
C18 C19 C20 111.30(17) .
C18 C19 H19A 109.4 .
C20 C19 H19A 109.4 .
C18 C19 H19B 109.4 .
C20 C19 H19B 109.4 .
H19A C19 H19B 108.0 .
C19 C20 C15 109.24(16) .
C19 C20 H20A 109.8 .
C15 C20 H20A 109.8 .
C19 C20 H20B 109.8 .
C15 C20 H20B 109.8 .
H20A C20 H20B 108.3 .
C26 C21 C22 109.66(15) .
C26 C21 P2 115.29(13) .
C22 C21 P2 112.56(13) .
C26 C21 H21 106.2 .
C22 C21 H21 106.2 .
P2 C21 H21 106.2 .
C23 C22 C21 110.24(16) .
C23 C22 H22A 109.6 .
C21 C22 H22A 109.6 .
C23 C22 H22B 109.6 .
C21 C22 H22B 109.6 .
H22A C22 H22B 108.1 .
C24 C23 C22 111.46(17) .
C24 C23 H23A 109.3 .
C22 C23 H23A 109.3 .
C24 C23 H23B 109.3 .
C22 C23 H23B 109.3 .
H23A C23 H23B 108.0 .
C23 C24 C25 111.27(16) .
C23 C24 H24A 109.4 .
C25 C24 H24A 109.4 .
C23 C24 H24B 109.4 .
C25 C24 H24B 109.4 .
H24A C24 H24B 108.0 .
C24 C25 C26 111.60(17) .
C24 C25 H25A 109.3 .
C26 C25 H25A 109.3 .
C24 C25 H25B 109.3 .
C26 C25 H25B 109.3 .
H25A C25 H25B 108.0 .
C21 C26 C25 109.29(15) .
C21 C26 H26A 109.8 .
C25 C26 H26A 109.8 .
C21 C26 H26B 109.8 .
C25 C26 H26B 109.8 .
H26A C26 H26B 108.3 .
C32 C27 C28 109.20(15) .
C32 C27 P2 111.12(12) .
C28 C27 P2 119.69(14) .
C32 C27 H27 105.2 .
C28 C27 H27 105.2 .
P2 C27 H27 105.2 .
C29 C28 C27 110.02(16) .
C29 C28 H28A 109.7 .
C27 C28 H28A 109.7 .
C29 C28 H28B 109.7 .
C27 C28 H28B 109.7 .
H28A C28 H28B 108.2 .
C30 C29 C28 112.07(16) .
C30 C29 H29A 109.2 .
C28 C29 H29A 109.2 .
C30 C29 H29B 109.2 .
C28 C29 H29B 109.2 .
H29A C29 H29B 107.9 .
C29 C30 C31 110.29(16) .
C29 C30 H30A 109.6 .
C31 C30 H30A 109.6 .
C29 C30 H30B 109.6 .
C31 C30 H30B 109.6 .
H30A C30 H30B 108.1 .
C30 C31 C32 110.54(17) .
C30 C31 H31A 109.5 .
C32 C31 H31A 109.5 .
C30 C31 H31B 109.5 .
C32 C31 H31B 109.5 .
H31A C31 H31B 108.1 .
C27 C32 C31 111.14(16) .
C27 C32 H32A 109.4 .
C31 C32 H32A 109.4 .
C27 C32 H32B 109.4 .
C31 C32 H32B 109.4 .
H32A C32 H32B 108.0 .
C34 C33 C38 117.80(18) .
C34 C33 Pd1 123.74(15) .
C38 C33 Pd1 117.05(14) .
C33 C34 C35 120.9(2) .
C33 C34 H34 119.5 .
C35 C34 H34 119.5 .
C36 C35 C34 121.4(2) .
C36 C35 H35 119.3 .
C34 C35 H35 119.3 .
C37 C36 C35 117.9(2) .
C37 C36 C39 120.9(2) .
C35 C36 C39 121.2(2) .
C36 C37 C38 121.2(2) .
C36 C37 H37 119.4 .
C38 C37 H37 119.4 .
C37 C38 C33 120.74(19) .
C37 C38 H38 119.6 .
C33 C38 H38 119.6 .
C36 C39 H39A 109.5 .
C36 C39 H39B 109.5 .
H39A C39 H39B 109.5 .
C36 C39 H39C 109.5 .
H39A C39 H39C 109.5 .
H39B C39 H39C 109.5 .
C36 C39 H39D 109.5 .
H39A C39 H39D 141.1 .
H39B C39 H39D 56.3 .
H39C C39 H39D 56.3 .
C36 C39 H39E 109.5 .
H39A C39 H39E 56.3 .
H39B C39 H39E 141.1 .
H39C C39 H39E 56.3 .
H39D C39 H39E 109.5 .
C36 C39 H39F 109.5 .
H39A C39 H39F 56.3 .
H39B C39 H39F 56.3 .
H39C C39 H39F 141.1 .
H39D C39 H39F 109.5 .
H39E C39 H39F 109.5 .
C1_1 O1_1 C4_1 108.71(19) .
O1_1 C1_1 C2_1 106.7(2) .
O1_1 C1_1 H1A_1 110.4 .
C2_1 C1_1 H1A_1 110.4 .
O1_1 C1_1 H1B_1 110.4 .
C2_1 C1_1 H1B_1 110.4 .
H1A_1 C1_1 H1B_1 108.6 .
C3_1 C2_1 C1_1 100.8(2) .
C3_1 C2_1 H2A_1 111.6 .
C1_1 C2_1 H2A_1 111.6 .
C3_1 C2_1 H2B_1 111.6 .
C1_1 C2_1 H2B_1 111.6 .
H2A_1 C2_1 H2B_1 109.4 .
C2_1 C3_1 C4_1 102.1(2) .
C2_1 C3_1 H3A_1 111.4 .
C4_1 C3_1 H3A_1 111.4 .
C2_1 C3_1 H3B_1 111.4 .
C4_1 C3_1 H3B_1 111.4 .
H3A_1 C3_1 H3B_1 109.2 .
O1_1 C4_1 C3_1 106.4(2) .
O1_1 C4_1 H4A_1 110.5 .
C3_1 C4_1 H4A_1 110.5 .
O1_1 C4_1 H4B_1 110.5 .
C3_1 C4_1 H4B_1 110.5 .
H4A_1 C4_1 H4B_1 108.6 .
C4_2 O1_2 C1_2 108.5(4) .
O1_2 C1_2 C2_2 106.4(4) .
O1_2 C1_2 H1A_2 110.4 .
C2_2 C1_2 H1A_2 110.4 .
O1_2 C1_2 H1B_2 110.4 .
C2_2 C1_2 H1B_2 110.4 .
H1A_2 C1_2 H1B_2 108.6 .
C1_2 C2_2 C3_2 99.4(5) .
C1_2 C2_2 H2A_2 111.9 .
C3_2 C2_2 H2A_2 111.9 .
C1_2 C2_2 H2B_2 111.9 .
C3_2 C2_2 H2B_2 111.9 .
H2A_2 C2_2 H2B_2 109.6 .
C4_2 C3_2 C2_2 102.8(5) .
C4_2 C3_2 H3A_2 111.2 .
C2_2 C3_2 H3A_2 111.2 .
C4_2 C3_2 H3B_2 111.2 .
C2_2 C3_2 H3B_2 111.2 .
H3A_2 C3_2 H3B_2 109.1 .
O1_2 C4_2 C3_2 107.3(4) .
O1_2 C4_2 H4A_2 110.3 .
C3_2 C4_2 H4A_2 110.3 .
O1_2 C4_2 H4B_2 110.3 .
C3_2 C4_2 H4B_2 110.3 .
H4A_2 C4_2 H4B_2 108.5 .
C1_3 O1_3 C4_3 106.6(8) .
O1_3 C1_3 C2_3 106.8(9) .
O1_3 C1_3 H1A_3 110.4 .
C2_3 C1_3 H1A_3 110.4 .
O1_3 C1_3 H1B_3 110.4 .
C2_3 C1_3 H1B_3 110.4 .
H1A_3 C1_3 H1B_3 108.6 .
C1_3 C2_3 C3_3 106.2(8) .
C1_3 C2_3 H2A_3 110.5 .
C3_3 C2_3 H2A_3 110.5 .
C1_3 C2_3 H2B_3 110.5 .
C3_3 C2_3 H2B_3 110.5 .
H2A_3 C2_3 H2B_3 108.7 .
C4_3 C3_3 C2_3 102.4(7) .
C4_3 C3_3 H3A_3 111.3 .
C2_3 C3_3 H3A_3 111.3 .
C4_3 C3_3 H3B_3 111.3 .
C2_3 C3_3 H3B_3 111.3 .
H3A_3 C3_3 H3B_3 109.2 .
O1_3 C4_3 C3_3 105.6(7) .
O1_3 C4_3 H4A_3 110.6 .
C3_3 C4_3 H4A_3 110.6 .
O1_3 C4_3 H4B_3 110.6 .
C3_3 C4_3 H4B_3 110.6 .
H4A_3 C4_3 H4B_3 108.7 .
C4_4 O1_4 C1_4 106.3(8) .
O1_4 C1_4 C2_4 104.9(8) .
O1_4 C1_4 H1A_4 110.8 .
C2_4 C1_4 H1A_4 110.8 .
O1_4 C1_4 H1B_4 110.8 .
C2_4 C1_4 H1B_4 110.8 .
H1A_4 C1_4 H1B_4 108.8 .
C1_4 C2_4 C3_4 103.2(9) .
C1_4 C2_4 H2A_4 111.1 .
C3_4 C2_4 H2A_4 111.1 .
C1_4 C2_4 H2B_4 111.1 .
C3_4 C2_4 H2B_4 111.1 .
H2A_4 C2_4 H2B_4 109.1 .
C4_4 C3_4 C2_4 102.6(8) .
C4_4 C3_4 H3A_4 111.3 .
C2_4 C3_4 H3A_4 111.3 .
C4_4 C3_4 H3B_4 111.3 .
C2_4 C3_4 H3B_4 111.3 .
H3A_4 C3_4 H3B_4 109.2 .
O1_4 C4_4 C3_4 110.0(8) .
O1_4 C4_4 H4A_4 109.7 .
C3_4 C4_4 H4A_4 109.7 .
O1_4 C4_4 H4B_4 109.7 .
C3_4 C4_4 H4B_4 109.7 .
H4A_4 C4_4 H4B_4 108.2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 C33 1.9909(19) .
Pd1 P2 2.2891(4) .
Pd1 Cl1 2.4122(4) .
Pd1 Cl1 2.4322(5) 2_666
P1 C1 1.7204(18) .
P1 C15 1.8394(19) .
P1 C9 1.8649(18) .
P1 C3 1.8686(19) .
P2 C1 1.7650(19) .
P2 C21 1.8595(18) .
P2 C27 1.8913(19) .
C1 C2 1.538(3) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 C4 1.536(3) .
C3 C8 1.536(2) .
C3 H3 1.0000 .
C4 C5 1.532(3) .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.533(3) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C7 1.525(3) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.532(3) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
C9 C10 1.535(3) .
C9 C14 1.540(3) .
C9 H9 1.0000 .
C10 C11 1.535(3) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.526(3) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 C13 1.520(3) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C13 C14 1.530(3) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.543(3) .
C15 C20 1.547(3) .
C15 H15 1.0000 .
C16 C17 1.528(3) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 C18 1.530(3) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 C19 1.526(3) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C20 1.533(3) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 C26 1.532(3) .
C21 C22 1.533(3) .
C21 H21 1.0000 .
C22 C23 1.529(3) .
C22 H22A 0.9900 .
C22 H22B 0.9900 .
C23 C24 1.527(3) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 C25 1.531(3) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25 C26 1.535(3) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C27 C32 1.526(2) .
C27 C28 1.542(2) .
C27 H27 1.0000 .
C28 C29 1.531(3) .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C29 C30 1.526(3) .
C29 H29A 0.9900 .
C29 H29B 0.9900 .
C30 C31 1.528(3) .
C30 H30A 0.9900 .
C30 H30B 0.9900 .
C31 C32 1.531(3) .
C31 H31A 0.9900 .
C31 H31B 0.9900 .
C32 H32A 0.9900 .
C32 H32B 0.9900 .
C33 C34 1.390(3) .
C33 C38 1.404(3) .
C34 C35 1.393(3) .
C34 H34 0.9500 .
C35 C36 1.390(3) .
C35 H35 0.9500 .
C36 C37 1.387(3) .
C36 C39 1.513(3) .
C37 C38 1.396(3) .
C37 H37 0.9500 .
C38 H38 0.9500 .
C39 H39A 0.9800 .
C39 H39B 0.9800 .
C39 H39C 0.9800 .
C39 H39D 0.9800 .
C39 H39E 0.9800 .
C39 H39F 0.9800 .
O1_1 C1_1 1.427(3) .
O1_1 C4_1 1.427(3) .
C1_1 C2_1 1.513(4) .
C1_1 H1A_1 0.9900 .
C1_1 H1B_1 0.9900 .
C2_1 C3_1 1.510(4) .
C2_1 H2A_1 0.9900 .
C2_1 H2B_1 0.9900 .
C3_1 C4_1 1.511(3) .
C3_1 H3A_1 0.9900 .
C3_1 H3B_1 0.9900 .
C4_1 H4A_1 0.9900 .
C4_1 H4B_1 0.9900 .
O1_2 C4_2 1.413(6) .
O1_2 C1_2 1.445(7) .
C1_2 C2_2 1.515(8) .
C1_2 H1A_2 0.9900 .
C1_2 H1B_2 0.9900 .
C2_2 C3_2 1.531(7) .
C2_2 H2A_2 0.9900 .
C2_2 H2B_2 0.9900 .
C3_2 C4_2 1.501(6) .
C3_2 H3A_2 0.9900 .
C3_2 H3B_2 0.9900 .
C4_2 H4A_2 0.9900 .
C4_2 H4B_2 0.9900 .
O1_3 C1_3 1.425(10) .
O1_3 C4_3 1.447(10) .
C1_3 C2_3 1.509(10) .
C1_3 H1A_3 0.9900 .
C1_3 H1B_3 0.9900 .
C2_3 C3_3 1.533(12) .
C2_3 H2A_3 0.9900 .
C2_3 H2B_3 0.9900 .
C3_3 C4_3 1.515(10) .
C3_3 H3A_3 0.9900 .
C3_3 H3B_3 0.9900 .
C4_3 H4A_3 0.9900 .
C4_3 H4B_3 0.9900 .
O1_4 C4_4 1.406(10) .
O1_4 C1_4 1.427(10) .
C1_4 C2_4 1.505(11) .
C1_4 H1A_4 0.9900 .
C1_4 H1B_4 0.9900 .
C2_4 C3_4 1.524(13) .
C2_4 H2A_4 0.9900 .
C2_4 H2B_4 0.9900 .
C3_4 C4_4 1.505(11) .
C3_4 H3A_4 0.9900 .
C3_4 H3B_4 0.9900 .
C4_4 H4A_4 0.9900 .
C4_4 H4B_4 0.9900 .
