#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/36/4123687.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_4123687
loop_
_publ_author_name
'Tymonko, Steven A.'
'Smith, Russell C.'
'Ambrosi, Andrea'
'Denmark, Scott E.'
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Mechanistic significance of the si-o-pd bond in the palladium-catalyzed
 cross-coupling reactions of alkenylsilanolates.
;
_journal_issue                   19
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6192
_journal_page_last               6199
_journal_paper_doi               10.1021/jacs.5b02515
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C53 H50 O P2 Pd Si, 0.5(C6 H6)'
_chemical_formula_sum            'C56 H53 O P2 Pd Si'
_chemical_formula_weight         938.41
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
; 
2008-01-03   text and data added, srw 
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.315(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9632(11)
_cell_length_b                   11.8061(6)
_cell_length_c                   21.5367(12)
_cell_measurement_reflns_used    8266
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      2.38
_cell_volume                     4728.7(5)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.0-1 (Bruker, 2004)'
_computing_data_reduction
; 
SAINT V7.23A, XPREP V2005/2, SADABS V2007/4, (Bruker, 2005 & 2007) 
;
_computing_molecular_graphics    'SHELXTL V6.12 (Bruker, 2005)'
_computing_publication_material  'XCIF V6.12 (Bruker, 2005)'
_computing_structure_refinement  'SHELXTL V6.12 (Bruker, 2005)'
_computing_structure_solution    'SHELXTL V6.12 (Bruker, 2005)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  ga45xas
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61435
_diffrn_reflns_theta_full        26.78
_diffrn_reflns_theta_max         26.78
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.9460
_exptl_absorpt_correction_T_min  0.7940
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2005/2 (Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1948
_exptl_crystal_id                ga45xas
_exptl_crystal_preparation
; 
The data crystal was mounted using epoxy to a 0.3 mm cryo-loop 
(Hampton Research) with the (-4 -2 3) scattering planes roughly 
normal to the spindle axis. 
;
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.124
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         10045
_refine_ls_number_restraints     595
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0405P)²+4.7706P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                7724
_reflns_number_total             10045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b02515_si_004.cif
_cod_data_source_block           ga45xasd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4123686--4123687.cif.
;
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n  '
_cod_database_code               4123687
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.88280(15) 0.3529(2) 0.03625(14) 0.0303(6) Uani 1 1 d . . .
C2 C 0.88595(17) 0.2386(3) 0.05075(17) 0.0445(8) Uani 1 1 d . . .
H2 H 0.8428 0.1975 0.0432 0.053 Uiso 1 1 calc R . .
C3 C 0.9516(2) 0.1836(3) 0.07618(19) 0.0559(9) Uani 1 1 d . . .
H3 H 0.9534 0.1050 0.0862 0.067 Uiso 1 1 calc R . .
C4 C 1.01410(19) 0.2428(3) 0.08693(18) 0.0519(9) Uani 1 1 d . . .
H4 H 1.0592 0.2054 0.1052 0.062 Uiso 1 1 calc R . .
C5 C 1.01147(17) 0.3551(3) 0.07150(18) 0.0483(8) Uani 1 1 d . . .
H5 H 1.0548 0.3951 0.0780 0.058 Uiso 1 1 calc R . .
C6 C 0.94626(16) 0.4112(3) 0.04639(16) 0.0389(7) Uani 1 1 d . . .
H6 H 0.9449 0.4896 0.0361 0.047 Uiso 1 1 calc R . .
C7 C 0.73766(14) 0.3561(2) 0.03728(14) 0.0282(6) Uani 1 1 d . . .
C8 C 0.73141(16) 0.4011(2) 0.09449(15) 0.0363(7) Uani 1 1 d . . .
H8 H 0.7582 0.4665 0.1146 0.044 Uiso 1 1 calc R . .
C9 C 0.68618(18) 0.3509(3) 0.12247(17) 0.0441(8) Uani 1 1 d . . .
H9 H 0.6827 0.3813 0.1620 0.053 Uiso 1 1 calc R . .
C10 C 0.64619(17) 0.2568(3) 0.09287(17) 0.0460(8) Uani 1 1 d . . .
H10 H 0.6141 0.2240 0.1113 0.055 Uiso 1 1 calc R . .
C11 C 0.65278(17) 0.2105(3) 0.03669(17) 0.0418(7) Uani 1 1 d . . .
H11 H 0.6259 0.1449 0.0169 0.050 Uiso 1 1 calc R . .
C12 C 0.69851(16) 0.2594(2) 0.00893(15) 0.0361(7) Uani 1 1 d . . .
H12 H 0.7032 0.2269 -0.0296 0.043 Uiso 1 1 calc R . .
C13 C 0.76276(16) 0.3923(2) -0.08556(14) 0.0321(6) Uani 1 1 d . . .
C14 C 0.68926(17) 0.3969(2) -0.12207(15) 0.0383(7) Uani 1 1 d . . .
H14 H 0.6568 0.4147 -0.1004 0.046 Uiso 1 1 calc R . .
C15 C 0.6632(2) 0.3757(3) -0.18991(17) 0.0507(9) Uani 1 1 d . . .
H15 H 0.6129 0.3772 -0.2144 0.061 Uiso 1 1 calc R . .
C16 C 0.7099(2) 0.3525(4) -0.22183(18) 0.0626(11) Uani 1 1 d . . .
H16 H 0.6919 0.3390 -0.2685 0.075 Uiso 1 1 calc R . .
C17 C 0.7830(2) 0.3486(4) -0.18645(18) 0.0610(10) Uani 1 1 d . . .
H17 H 0.8151 0.3329 -0.2089 0.073 Uiso 1 1 calc R . .
C18 C 0.80981(18) 0.3676(3) -0.11823(16) 0.0435(7) Uani 1 1 d . . .
H18 H 0.8601 0.3639 -0.0938 0.052 Uiso 1 1 calc R . .
C19 C 0.77642(14) 0.9115(2) -0.01550(13) 0.0264(6) Uani 1 1 d . . .
C20 C 0.70198(15) 0.9210(2) -0.04390(15) 0.0339(6) Uani 1 1 d . . .
H20 H 0.6729 0.8790 -0.0257 0.041 Uiso 1 1 calc R . .
C21 C 0.66966(16) 0.9905(3) -0.09820(16) 0.0402(7) Uani 1 1 d . . .
H21 H 0.6187 0.9955 -0.1171 0.048 Uiso 1 1 calc R . .
C22 C 0.71068(18) 1.0523(3) -0.12501(16) 0.0443(8) Uani 1 1 d . . .
H22 H 0.6884 1.0995 -0.1626 0.053 Uiso 1 1 calc R . .
C23 C 0.78413(18) 1.0452(3) -0.09707(17) 0.0488(8) Uani 1 1 d . . .
H23 H 0.8128 1.0888 -0.1150 0.059 Uiso 1 1 calc R . .
C24 C 0.81720(16) 0.9749(3) -0.04262(15) 0.0383(7) Uani 1 1 d . . .
H24 H 0.8682 0.9704 -0.0240 0.046 Uiso 1 1 calc R . .
C25 C 0.90770(14) 0.8554(2) 0.09414(14) 0.0281(6) Uani 1 1 d . . .
C26 C 0.93235(15) 0.9122(2) 0.15464(15) 0.0344(6) Uani 1 1 d . . .
H26 H 0.8998 0.9319 0.1759 0.041 Uiso 1 1 calc R . .
C27 C 1.00454(17) 0.9402(3) 0.18411(17) 0.0453(8) Uani 1 1 d . . .
H27 H 1.0214 0.9778 0.2260 0.054 Uiso 1 1 calc R . .
C28 C 1.05152(16) 0.9143(3) 0.15341(18) 0.0481(8) Uani 1 1 d . . .
H28 H 1.1006 0.9354 0.1735 0.058 Uiso 1 1 calc R . .
C29 C 1.02808(16) 0.8579(3) 0.09347(18) 0.0460(8) Uani 1 1 d . . .
H29 H 1.0609 0.8405 0.0721 0.055 Uiso 1 1 calc R . .
C30 C 0.95657(15) 0.8263(3) 0.06419(16) 0.0377(7) Uani 1 1 d . . .
H30 H 0.9408 0.7847 0.0236 0.045 Uiso 1 1 calc R . .
C31 C 0.77019(14) 0.8509(2) 0.11064(14) 0.0306(6) Uani 1 1 d . . .
C32 C 0.75173(18) 0.7660(3) 0.14562(17) 0.0464(8) Uani 1 1 d . . .
H32 H 0.7615 0.6891 0.1389 0.056 Uiso 1 1 calc R . .
C33 C 0.7190(2) 0.7929(4) 0.1905(2) 0.0631(11) Uani 1 1 d . . .
H33 H 0.7065 0.7343 0.2146 0.076 Uiso 1 1 calc R . .
C34 C 0.70468(19) 0.9027(4) 0.20044(18) 0.0579(10) Uani 1 1 d . . .
H34 H 0.6822 0.9203 0.2312 0.070 Uiso 1 1 calc R . .
C35 C 0.72269(18) 0.9881(3) 0.16603(17) 0.0504(9) Uani 1 1 d . . .
H35 H 0.7130 1.0646 0.1734 0.061 Uiso 1 1 calc R . .
C36 C 0.75495(16) 0.9628(3) 0.12051(15) 0.0379(7) Uani 1 1 d . . .
H36 H 0.7666 1.0218 0.0962 0.046 Uiso 1 1 calc R . .
O1 O 0.89575(17) 0.5951(3) 0.11660(16) 0.0573(10) Uani 0.836(3) 1 d PDU A 1
Si1 Si 0.94165(10) 0.56338(14) 0.18902(8) 0.0400(4) Uani 0.836(3) 1 d PDU A 1
C37 C 0.93312(18) 0.4132(3) 0.21283(17) 0.0345(8) Uani 0.836(3) 1 d PDU A 1
H37 H 0.8922 0.3726 0.1848 0.041 Uiso 0.836(3) 1 calc PR A 1
C38 C 0.97808(19) 0.3572(3) 0.26475(18) 0.0388(8) Uani 0.836(3) 1 d PDU A 1
H38 H 1.0227 0.3945 0.2862 0.047 Uiso 0.836(3) 1 calc PR A 1
C39 C 0.97161(17) 0.2487(2) 0.29502(14) 0.0400(9) Uani 0.836(3) 1 d PGDU A 1
C40 C 0.91842(19) 0.1730(3) 0.25883(13) 0.0446(9) Uani 0.836(3) 1 d PGDU A 1
H40 H 0.8898 0.1889 0.2137 0.054 Uiso 0.836(3) 1 calc PR A 1
C41 C 0.9071(2) 0.0741(3) 0.28867(17) 0.0523(11) Uani 0.836(3) 1 d PGU A 1
H41 H 0.8708 0.0224 0.2639 0.063 Uiso 0.836(3) 1 calc PR A 1
C42 C 0.9491(3) 0.0509(3) 0.35469(18) 0.0568(12) Uani 0.836(3) 1 d PGU A 1
H42 H 0.9413 -0.0167 0.3751 0.068 Uiso 0.836(3) 1 calc PR A 1
C43 C 1.0022(2) 0.1266(3) 0.39088(14) 0.0633(13) Uani 0.836(3) 1 d PGU A 1
H43 H 1.0309 0.1107 0.4360 0.076 Uiso 0.836(3) 1 calc PR A 1
C44 C 1.01352(18) 0.2255(2) 0.36105(15) 0.0561(12) Uani 0.836(3) 1 d PGDU A 1
H44 H 1.0499 0.2772 0.3858 0.067 Uiso 0.836(3) 1 calc PR A 1
C45 C 0.9180(3) 0.6454(4) 0.2533(2) 0.0570(12) Uani 0.836(3) 1 d PDU A 1
H45A H 0.9201 0.7268 0.2452 0.085 Uiso 0.836(3) 1 calc PR A 1
H45B H 0.9523 0.6269 0.2979 0.085 Uiso 0.836(3) 1 calc PR A 1
H45C H 0.8693 0.6252 0.2503 0.085 Uiso 0.836(3) 1 calc PR A 1
C46 C 1.0398(2) 0.5881(5) 0.2067(3) 0.0529(13) Uani 0.836(3) 1 d PDU A 1
H46A H 1.0471 0.6667 0.1960 0.079 Uiso 0.836(3) 1 calc PR A 1
H46B H 1.0562 0.5368 0.1794 0.079 Uiso 0.836(3) 1 calc PR A 1
H46C H 1.0673 0.5737 0.2540 0.079 Uiso 0.836(3) 1 calc PR A 1
C47 C 0.71438(11) 0.6444(3) -0.04464(12) 0.0387(9) Uani 0.836(3) 1 d PGDU A 1
C48 C 0.70876(14) 0.6710(3) -0.10922(13) 0.0529(10) Uani 0.836(3) 1 d PGDU A 1
C49 C 0.64150(17) 0.6883(3) -0.15840(11) 0.0757(14) Uani 0.836(3) 1 d PGDU A 1
H49 H 0.6377 0.7065 -0.2025 0.091 Uiso 0.836(3) 1 calc PR A 1
C50 C 0.57988(13) 0.6790(3) -0.14300(16) 0.0855(17) Uani 0.836(3) 1 d PGU A 1
H50 H 0.5339 0.6908 -0.1766 0.103 Uiso 0.836(3) 1 calc PR A 1
C51 C 0.58551(11) 0.6524(3) -0.07843(18) 0.0737(14) Uani 0.836(3) 1 d PGU A 1
H51 H 0.5434 0.6460 -0.0679 0.088 Uiso 0.836(3) 1 calc PR A 1
C52 C 0.65276(14) 0.6351(3) -0.02924(13) 0.0537(12) Uani 0.836(3) 1 d PGU A 1
H52 H 0.6566 0.6169 0.0149 0.064 Uiso 0.836(3) 1 calc PR A 1
C53 C 0.7736(3) 0.6816(4) -0.1269(2) 0.0615(12) Uani 0.836(3) 1 d PDU A 1
H53A H 0.8167 0.6684 -0.0871 0.092 Uiso 0.836(3) 1 calc PR A 1
H53B H 0.7756 0.7579 -0.1441 0.092 Uiso 0.836(3) 1 calc PR A 1
H53C H 0.7715 0.6255 -0.1611 0.092 Uiso 0.836(3) 1 calc PR A 1
P1 P 0.79743(4) 0.42866(6) 0.00311(4) 0.02671(15) Uani 1 1 d . A .
P2 P 0.81443(3) 0.81169(6) 0.05329(3) 0.02462(15) Uani 1 1 d . A .
Pd1 Pd 0.807277(10) 0.618842(16) 0.031267(10) 0.02554(7) Uani 1 1 d D . .
C54 C 0.45528(19) 1.0902(3) -0.0263(2) 0.0567(10) Uani 1 1 d . . .
H54 H 0.4243 1.1526 -0.0447 0.085 Uiso 1 1 calc R . .
C55 C 0.47291(18) 1.0163(3) -0.0679(2) 0.0548(9) Uani 1 1 d . . .
H55 H 0.4541 1.0278 -0.1148 0.066 Uiso 1 1 calc R . .
C56 C 0.51767(18) 0.9264(3) -0.0412(2) 0.0533(9) Uani 1 1 d . . .
H56 H 0.5299 0.8757 -0.0696 0.080 Uiso 1 1 calc R . .
C57 C 0.7312(5) 0.6467(15) -0.0583(4) 0.039(3) Uani 0.164(3) 1 d PGDU A 2
C58 C 0.6581(6) 0.6500(14) -0.0695(5) 0.052(2) Uani 0.164(3) 1 d PGDU A 2
C59 C 0.6087(5) 0.6720(16) -0.1330(6) 0.070(3) Uani 0.164(3) 1 d PGDU A 2
H59 H 0.5588 0.6743 -0.1407 0.084 Uiso 0.164(3) 1 calc PR A 2
C60 C 0.6324(7) 0.6906(16) -0.1854(4) 0.074(3) Uani 0.164(3) 1 d PGU A 2
H60 H 0.5986 0.7057 -0.2288 0.089 Uiso 0.164(3) 1 calc PR A 2
C61 C 0.7054(8) 0.6873(14) -0.1742(4) 0.061(3) Uani 0.164(3) 1 d PGU A 2
H61 H 0.7216 0.7000 -0.2100 0.074 Uiso 0.164(3) 1 calc PR A 2
C62 C 0.7548(6) 0.6653(15) -0.1107(5) 0.051(3) Uani 0.164(3) 1 d PGU A 2
H62 H 0.8048 0.6630 -0.1030 0.061 Uiso 0.164(3) 1 calc PR A 2
C63 C 0.6321(9) 0.627(2) -0.0144(8) 0.054(3) Uani 0.164(3) 1 d PDU A 2
H63A H 0.5795 0.6312 -0.0313 0.081 Uiso 0.164(3) 1 calc PR A 2
H63B H 0.6521 0.6838 0.0208 0.081 Uiso 0.164(3) 1 calc PR A 2
H63C H 0.6476 0.5514 0.0037 0.081 Uiso 0.164(3) 1 calc PR A 2
O2 O 0.8723(6) 0.5763(12) 0.1277(4) 0.040(3) Uani 0.164(3) 1 d PDU A 2
Si2 Si 0.9356(5) 0.5755(8) 0.1952(4) 0.0400(4) Uani 0.164(3) 1 d PDU A 2
C64 C 0.9556(9) 0.4416(10) 0.2438(6) 0.053(3) Uani 0.164(3) 1 d PDU A 2
H64 H 0.9883 0.4528 0.2882 0.063 Uiso 0.164(3) 1 calc PR A 2
C65 C 0.9357(10) 0.3356(10) 0.2321(7) 0.049(3) Uani 0.164(3) 1 d PDU A 2
H65 H 0.9046 0.3206 0.1876 0.059 Uiso 0.164(3) 1 calc PR A 2
C66 C 0.9530(10) 0.2359(10) 0.2758(7) 0.048(3) Uani 0.164(3) 1 d PGDU A 2
C67 C 1.0009(10) 0.2467(12) 0.3411(8) 0.057(3) Uani 0.164(3) 1 d PGDU A 2
H67 H 1.0304 0.3120 0.3543 0.069 Uiso 0.164(3) 1 calc PR A 2
C68 C 1.0055(14) 0.1618(17) 0.3873(8) 0.062(3) Uani 0.164(3) 1 d PGU A 2
H68 H 1.0382 0.1691 0.4319 0.075 Uiso 0.164(3) 1 calc PR A 2
C69 C 0.9622(15) 0.0662(17) 0.3680(10) 0.058(3) Uani 0.164(3) 1 d PGU A 2
H69 H 0.9654 0.0081 0.3995 0.070 Uiso 0.164(3) 1 calc PR A 2
C70 C 0.9143(14) 0.0554(14) 0.3027(11) 0.053(3) Uani 0.164(3) 1 d PGU A 2
H70 H 0.8847 -0.0099 0.2896 0.063 Uiso 0.164(3) 1 calc PR A 2
C71 C 0.9097(12) 0.1403(11) 0.2566(8) 0.050(3) Uani 0.164(3) 1 d PGDU A 2
H71 H 0.8769 0.1329 0.2119 0.060 Uiso 0.164(3) 1 calc PR A 2
C72 C 0.9224(15) 0.6811(15) 0.2555(8) 0.064(5) Uani 0.164(3) 1 d PDU A 2
H72A H 0.9248 0.7581 0.2395 0.096 Uiso 0.164(3) 1 calc PR A 2
H72B H 0.9602 0.6710 0.2995 0.096 Uiso 0.164(3) 1 calc PR A 2
H72C H 0.8752 0.6691 0.2589 0.096 Uiso 0.164(3) 1 calc PR A 2
C73 C 1.0243(6) 0.612(2) 0.1876(11) 0.051(4) Uani 0.164(3) 1 d PDU A 2
H73A H 1.0248 0.6928 0.1770 0.077 Uiso 0.164(3) 1 calc PR A 2
H73B H 1.0305 0.5668 0.1520 0.077 Uiso 0.164(3) 1 calc PR A 2
H73C H 1.0635 0.5959 0.2298 0.077 Uiso 0.164(3) 1 calc PR A 2
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'
Si Si 0.0817 0.0704 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 0.00 0.3000
-1.00 0.00 1.00 0.0900
1.00 0.00 0.00 0.0800
1.00 0.00 1.00 0.0600
0.00 0.00 1.00 0.0700
1.00 0.00 -1.00 0.0900
-1.00 0.00 -1.00 0.0600
0.00 -1.00 0.00 0.2600
-1.00 0.00 0.00 0.0800
0.00 0.00 -1.00 0.0700
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
C2 C1 C6 119.0(3) .
C2 C1 P1 121.8(2) .
C6 C1 P1 119.2(2) .
C1 C2 C3 120.4(3) .
C1 C2 H2 119.8 .
C3 C2 H2 119.8 .
C4 C3 C2 119.9(3) .
C4 C3 H3 120.0 .
C2 C3 H3 120.0 .
C5 C4 C3 120.1(3) .
C5 C4 H4 120.0 .
C3 C4 H4 120.0 .
C4 C5 C6 120.5(3) .
C4 C5 H5 119.7 .
C6 C5 H5 119.7 .
C5 C6 C1 120.0(3) .
C5 C6 H6 120.0 .
C1 C6 H6 120.0 .
C8 C7 C12 119.1(3) .
C8 C7 P1 117.4(2) .
C12 C7 P1 123.5(2) .
C9 C8 C7 120.3(3) .
C9 C8 H8 119.8 .
C7 C8 H8 119.8 .
C10 C9 C8 120.1(3) .
C10 C9 H9 120.0 .
C8 C9 H9 120.0 .
C11 C10 C9 120.1(3) .
C11 C10 H10 120.0 .
C9 C10 H10 120.0 .
C10 C11 C12 120.1(3) .
C10 C11 H11 119.9 .
C12 C11 H11 119.9 .
C11 C12 C7 120.3(3) .
C11 C12 H12 119.8 .
C7 C12 H12 119.8 .
C14 C13 C18 119.3(3) .
C14 C13 P1 120.1(2) .
C18 C13 P1 120.5(2) .
C15 C14 C13 120.2(3) .
C15 C14 H14 119.9 .
C13 C14 H14 119.9 .
C16 C15 C14 120.2(3) .
C16 C15 H15 119.9 .
C14 C15 H15 119.9 .
C15 C16 C17 120.3(3) .
C15 C16 H16 119.9 .
C17 C16 H16 119.9 .
C16 C17 C18 120.2(3) .
C16 C17 H17 119.9 .
C18 C17 H17 119.9 .
C17 C18 C13 119.8(3) .
C17 C18 H18 120.1 .
C13 C18 H18 120.1 .
C24 C19 C20 118.0(3) .
C24 C19 P2 123.8(2) .
C20 C19 P2 118.1(2) .
C21 C20 C19 121.0(3) .
C21 C20 H20 119.5 .
C19 C20 H20 119.5 .
C22 C21 C20 120.4(3) .
C22 C21 H21 119.8 .
C20 C21 H21 119.8 .
C21 C22 C23 119.4(3) .
C21 C22 H22 120.3 .
C23 C22 H22 120.3 .
C22 C23 C24 120.7(3) .
C22 C23 H23 119.7 .
C24 C23 H23 119.7 .
C19 C24 C23 120.5(3) .
C19 C24 H24 119.8 .
C23 C24 H24 119.8 .
C26 C25 C30 119.0(3) .
C26 C25 P2 122.8(2) .
C30 C25 P2 118.1(2) .
C25 C26 C27 120.0(3) .
C25 C26 H26 120.0 .
C27 C26 H26 120.0 .
C28 C27 C26 120.5(3) .
C28 C27 H27 119.8 .
C26 C27 H27 119.8 .
C27 C28 C29 120.3(3) .
C27 C28 H28 119.8 .
C29 C28 H28 119.9 .
C28 C29 C30 120.0(3) .
C28 C29 H29 120.0 .
C30 C29 H29 120.0 .
C29 C30 C25 120.1(3) .
C29 C30 H30 119.9 .
C25 C30 H30 119.9 .
C32 C31 C36 119.4(3) .
C32 C31 P2 118.4(2) .
C36 C31 P2 122.2(2) .
C31 C32 C33 120.0(3) .
C31 C32 H32 120.0 .
C33 C32 H32 120.0 .
C34 C33 C32 120.5(3) .
C34 C33 H33 119.8 .
C32 C33 H33 119.8 .
C33 C34 C35 120.2(3) .
C33 C34 H34 119.9 .
C35 C34 H34 119.9 .
C34 C35 C36 120.2(3) .
C34 C35 H35 119.9 .
C36 C35 H35 119.9 .
C35 C36 C31 119.8(3) .
C35 C36 H36 120.1 .
C31 C36 H36 120.1 .
Si1 O1 Pd1 160.2(3) .
O1 Si1 C37 115.32(18) .
O1 Si1 C46 111.1(2) .
C37 Si1 C46 106.49(18) .
O1 Si1 C45 113.78(19) .
C37 Si1 C45 102.34(19) .
C46 Si1 C45 107.0(2) .
C38 C37 Si1 127.0(3) .
C38 C37 H37 116.5 .
Si1 C37 H37 116.5 .
C37 C38 C39 131.9(3) .
C37 C38 H38 114.0 .
C39 C38 H38 114.0 .
C40 C39 C44 120.0 .
C40 C39 C38 119.1(2) .
C44 C39 C38 120.7(2) .
C41 C40 C39 120.0 .
C41 C40 H40 120.0 .
C39 C40 H40 120.0 .
C40 C41 C42 120.0 .
C40 C41 H41 120.0 .
C42 C41 H41 120.0 .
C41 C42 C43 120.0 .
C41 C42 H42 120.0 .
C43 C42 H42 120.0 .
C44 C43 C42 120.0 .
C44 C43 H43 120.0 .
C42 C43 H43 120.0 .
C43 C44 C39 120.0 .
C43 C44 H44 120.0 .
C39 C44 H44 120.0 .
Si1 C45 H45A 109.5 .
Si1 C45 H45B 109.5 .
H45A C45 H45B 109.5 .
Si1 C45 H45C 109.5 .
H45A C45 H45C 109.5 .
H45B C45 H45C 109.5 .
Si1 C46 H46A 109.5 .
Si1 C46 H46B 109.5 .
H46A C46 H46B 109.5 .
Si1 C46 H46C 109.5 .
H46A C46 H46C 109.5 .
H46B C46 H46C 109.5 .
C48 C47 C52 120.0 .
C48 C47 Pd1 124.46(14) .
C52 C47 Pd1 115.54(14) .
C47 C48 C49 120.0 .
C47 C48 C53 121.0(2) .
C49 C48 C53 119.0(2) .
C48 C49 C50 120.0 .
C48 C49 H49 120.0 .
C50 C49 H49 120.0 .
C51 C50 C49 120.0 .
C51 C50 H50 120.0 .
C49 C50 H50 120.0 .
C52 C51 C50 120.0 .
C52 C51 H51 120.0 .
C50 C51 H51 120.0 .
C51 C52 C47 120.0 .
C51 C52 H52 120.0 .
C47 C52 H52 120.0 .
C48 C53 H53A 109.5 .
C48 C53 H53B 109.5 .
H53A C53 H53B 109.5 .
C48 C53 H53C 109.5 .
H53A C53 H53C 109.5 .
H53B C53 H53C 109.5 .
C1 P1 C7 105.46(12) .
C1 P1 C13 103.80(13) .
C7 P1 C13 104.82(13) .
C1 P1 Pd1 113.23(9) .
C7 P1 Pd1 110.79(9) .
C13 P1 Pd1 117.68(9) .
C31 P2 C25 105.26(13) .
C31 P2 C19 103.00(12) .
C25 P2 C19 105.02(12) .
C31 P2 Pd1 112.32(9) .
C25 P2 Pd1 110.67(9) .
C19 P2 Pd1 119.36(9) .
C47 Pd1 O1 173.09(14) .
C57 Pd1 O2 170.2(5) .
C47 Pd1 P1 88.11(10) .
C57 Pd1 P1 86.8(5) .
O1 Pd1 P1 93.75(9) .
O2 Pd1 P1 89.4(4) .
C47 Pd1 P2 89.36(10) .
C57 Pd1 P2 90.3(5) .
O1 Pd1 P2 88.98(9) .
O2 Pd1 P2 93.6(4) .
P1 Pd1 P2 176.86(3) .
C56 C54 C55 120.1(4) 3_675
C56 C54 H54 119.9 3_675
C55 C54 H54 119.9 .
C56 C55 C54 119.8(4) .
C56 C55 H55 120.1 .
C54 C55 H55 120.1 .
C54 C56 C55 120.1(4) 3_675
C54 C56 H56 119.9 3_675
C55 C56 H56 119.9 .
C58 C57 C62 120.0 .
C58 C57 Pd1 123.6(6) .
C62 C57 Pd1 116.4(6) .
C57 C58 C59 120.0 .
C57 C58 C63 120.5(4) .
C59 C58 C63 119.5(4) .
C58 C59 C60 120.0 .
C58 C59 H59 120.0 .
C60 C59 H59 120.0 .
C61 C60 C59 120.0 .
C61 C60 H60 120.0 .
C59 C60 H60 120.0 .
C60 C61 C62 120.0 .
C60 C61 H61 120.0 .
C62 C61 H61 120.0 .
C61 C62 C57 120.0 .
C61 C62 H62 120.0 .
C57 C62 H62 120.0 .
C58 C63 H63A 109.5 .
C58 C63 H63B 109.5 .
H63A C63 H63B 109.5 .
C58 C63 H63C 109.5 .
H63A C63 H63C 109.5 .
H63B C63 H63C 109.5 .
Si2 O2 Pd1 161.4(7) .
O2 Si2 C64 118.1(5) .
O2 Si2 C73 113.0(5) .
C64 Si2 C73 103.2(4) .
O2 Si2 C72 111.9(5) .
C64 Si2 C72 103.2(4) .
C73 Si2 C72 106.2(5) .
C65 C64 Si2 135.8(8) .
C65 C64 H64 112.1 .
Si2 C64 H64 112.1 .
C64 C65 C66 131.2(8) .
C64 C65 H65 114.4 .
C66 C65 H65 114.4 .
C67 C66 C71 120.0 .
C67 C66 C65 119.4(4) .
C71 C66 C65 119.0(5) .
C68 C67 C66 120.0 .
C68 C67 H67 120.0 .
C66 C67 H67 120.0 .
C67 C68 C69 120.0 .
C67 C68 H68 120.0 .
C69 C68 H68 120.0 .
C68 C69 C70 120.0 .
C68 C69 H69 120.0 .
C70 C69 H69 120.0 .
C71 C70 C69 120.0 .
C71 C70 H70 120.0 .
C69 C70 H70 120.0 .
C70 C71 C66 120.0 .
C70 C71 H71 120.0 .
C66 C71 H71 120.0 .
Si2 C72 H72A 109.5 .
Si2 C72 H72B 109.5 .
H72A C72 H72B 109.5 .
Si2 C72 H72C 109.5 .
H72A C72 H72C 109.5 .
H72B C72 H72C 109.5 .
Si2 C73 H73A 109.5 .
Si2 C73 H73B 109.5 .
H73A C73 H73B 109.5 .
Si2 C73 H73C 109.5 .
H73A C73 H73C 109.5 .
H73B C73 H73C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.381(4) .
C1 C6 1.387(4) .
C1 P1 1.825(3) .
C2 C3 1.385(4) .
C2 H2 0.9500 .
C3 C4 1.374(5) .
C3 H3 0.9500 .
C4 C5 1.363(5) .
C4 H4 0.9500 .
C5 C6 1.383(4) .
C5 H5 0.9500 .
C6 H6 0.9500 .
C7 C8 1.388(4) .
C7 C12 1.392(4) .
C7 P1 1.827(3) .
C8 C9 1.387(4) .
C8 H8 0.9500 .
C9 C10 1.381(5) .
C9 H9 0.9500 .
C10 C11 1.377(5) .
C10 H10 0.9500 .
C11 C12 1.386(4) .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.391(4) .
C13 C18 1.394(4) .
C13 P1 1.830(3) .
C14 C15 1.384(4) .
C14 H14 0.9500 .
C15 C16 1.372(5) .
C15 H15 0.9500 .
C16 C17 1.379(5) .
C16 H16 0.9500 .
C17 C18 1.387(5) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C19 C24 1.382(4) .
C19 C20 1.391(4) .
C19 P2 1.828(3) .
C20 C21 1.382(4) .
C20 H20 0.9500 .
C21 C22 1.371(4) .
C21 H21 0.9500 .
C22 C23 1.370(5) .
C22 H22 0.9500 .
C23 C24 1.392(4) .
C23 H23 0.9500 .
C24 H24 0.9500 .
C25 C26 1.387(4) .
C25 C30 1.394(4) .
C25 P2 1.821(3) .
C26 C27 1.387(4) .
C26 H26 0.9500 .
C27 C28 1.364(5) .
C27 H27 0.9500 .
C28 C29 1.375(5) .
C28 H28 0.9500 .
C29 C30 1.386(4) .
C29 H29 0.9500 .
C30 H30 0.9500 .
C31 C32 1.383(4) .
C31 C36 1.388(4) .
C31 P2 1.820(3) .
C32 C33 1.387(5) .
C32 H32 0.9500 .
C33 C34 1.360(5) .
C33 H33 0.9500 .
C34 C35 1.374(5) .
C34 H34 0.9500 .
C35 C36 1.387(4) .
C35 H35 0.9500 .
C36 H36 0.9500 .
O1 Si1 1.541(3) .
O1 Pd1 2.053(3) .
Si1 C37 1.871(4) .
Si1 C46 1.878(3) .
Si1 C45 1.885(4) .
C37 C38 1.328(5) .
C37 H37 0.9500 .
C38 C39 1.464(4) .
C38 H38 0.9500 .
C39 C40 1.3900 .
C39 C44 1.3900 .
C40 C41 1.3900 .
C40 H40 0.9500 .
C41 C42 1.3900 .
C41 H41 0.9500 .
C42 C43 1.3900 .
C42 H42 0.9500 .
C43 C44 1.3900 .
C43 H43 0.9500 .
C44 H44 0.9500 .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
C46 H46A 0.9800 .
C46 H46B 0.9800 .
C46 H46C 0.9800 .
C47 C48 1.3900 .
C47 C52 1.3900 .
C47 Pd1 1.9997(17) .
C48 C49 1.3900 .
C48 C53 1.481(6) .
C49 C50 1.3900 .
C49 H49 0.9500 .
C50 C51 1.3900 .
C50 H50 0.9500 .
C51 C52 1.3900 .
C51 H51 0.9500 .
C52 H52 0.9500 .
C53 H53A 0.9800 .
C53 H53B 0.9800 .
C53 H53C 0.9800 .
P1 Pd1 2.3154(7) .
P2 Pd1 2.3195(7) .
Pd1 C57 2.002(5) .
Pd1 O2 2.072(5) .
C54 C56 1.369(5) 3_675
C54 C55 1.384(5) .
C54 H54 0.9500 .
C55 C56 1.371(5) .
C55 H55 0.9500 .
C56 C54 1.369(5) 3_675
C56 H56 0.9500 .
C57 C58 1.3900 .
C57 C62 1.3900 .
C58 C59 1.3900 .
C58 C63 1.481(8) .
C59 C60 1.3900 .
C59 H59 0.9500 .
C60 C61 1.3900 .
C60 H60 0.9500 .
C61 C62 1.3900 .
C61 H61 0.9500 .
C62 H62 0.9500 .
C63 H63A 0.9800 .
C63 H63B 0.9800 .
C63 H63C 0.9800 .
O2 Si2 1.540(5) .
Si2 C64 1.858(6) .
Si2 C73 1.886(5) .
Si2 C72 1.888(5) .
C64 C65 1.309(6) .
C64 H64 0.9500 .
C65 C66 1.467(6) .
C65 H65 0.9500 .
C66 C67 1.3900 .
C66 C71 1.3900 .
C67 C68 1.3900 .
C67 H67 0.9500 .
C68 C69 1.3900 .
C68 H68 0.9500 .
C69 C70 1.3900 .
C69 H69 0.9500 .
C70 C71 1.3900 .
C70 H70 0.9500 .
C71 H71 0.9500 .
C72 H72A 0.9800 .
C72 H72B 0.9800 .
C72 H72C 0.9800 .
C73 H73A 0.9800 .
C73 H73B 0.9800 .
C73 H73C 0.9800 .
