# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_ljy075a
_database_code_depnum_ccdc_archive 'CCDC 1477475'
_audit_update_record             
;
2016-05-21 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C28 H24 F N2 O3 P Pd, C4 H8 O'
_chemical_formula_sum            'C32 H32 F N2 O4 P Pd'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         664.96
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0



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'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.723(2)
_cell_length_b                   12.725(3)
_cell_length_c                   22.555(5)
_cell_angle_alpha                76.391(6)
_cell_angle_beta                 79.537(6)
_cell_angle_gamma                86.496(6)
_cell_volume                     2940.7(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3577
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      20.3
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_F_000             1360
_exptl_transmission_factor_min   0.924
_exptl_transmission_factor_max   0.943
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.732
_shelx_estimated_absorpt_T_min   0.917
_shelx_estimated_absorpt_T_max   0.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36736
_diffrn_reflns_av_unetI/netI     0.1084
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         0.943
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12813
_reflns_number_gt                7195
_reflns_threshold_expression     I>2σ
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'DIAMOND (Brandenburg, 2006)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0426P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12813
_refine_ls_number_parameters     739
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1100
_refine_ls_wR_factor_gt          0.1004
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      0.954
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000

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
C1 C 0.3647(6) 0.0679(5) 0.3172(2) 0.082(2) Uani 1 1 d . . . . .
H1 H 0.4281 0.0766 0.2811 0.099 Uiso 1 1 calc R U . . .
C2 C 0.2993(6) -0.0270(5) 0.3388(3) 0.0721(18) Uani 1 1 d . . . . .
H2 H 0.3174 -0.0835 0.3173 0.087 Uiso 1 1 calc R U . . .
C3 C 0.2102(6) -0.0409(4) 0.3900(3) 0.0740(17) Uani 1 1 d . . . . .
H3 H 0.1661 -0.1071 0.4044 0.089 Uiso 1 1 calc R U . . .
C4 C 0.1820(5) 0.0407(4) 0.4219(3) 0.0587(14) Uani 1 1 d . . . . .
H4 H 0.1188 0.0301 0.4581 0.070 Uiso 1 1 calc R U . . .
C5 C 0.2455(4) 0.1377(3) 0.4012(2) 0.0408(11) Uani 1 1 d . . . . .
C6 C 0.3382(6) 0.1500(4) 0.3479(2) 0.0649(16) Uani 1 1 d . . . . .
H6 H 0.3833 0.2157 0.3328 0.078 Uiso 1 1 calc R U . . .
C7 C 0.3476(4) 0.2413(3) 0.48162(19) 0.0377(11) Uani 1 1 d . . . . .
C8 C 0.3985(5) 0.1423(4) 0.5084(2) 0.0481(12) Uani 1 1 d . . . . .
H8 H 0.3686 0.0773 0.5027 0.058 Uiso 1 1 calc R U . . .
C9 C 0.4926(4) 0.1382(4) 0.5435(2) 0.0487(12) Uani 1 1 d . . . . .
H9 H 0.5277 0.0702 0.5612 0.058 Uiso 1 1 calc R U . . .
C10 C 0.5360(4) 0.2311(4) 0.5530(2) 0.0483(12) Uani 1 1 d . . . . .
H10 H 0.5999 0.2276 0.5776 0.058 Uiso 1 1 calc R U . . .
C11 C 0.4857(4) 0.3295(4) 0.5264(2) 0.0496(13) Uani 1 1 d . . . . .
H11 H 0.5154 0.3941 0.5328 0.060 Uiso 1 1 calc R U . . .
C12 C 0.3929(4) 0.3353(4) 0.4907(2) 0.0423(11) Uani 1 1 d . . . . .
H12 H 0.3598 0.4037 0.4723 0.051 Uiso 1 1 calc R U . . .
C13 C 0.0810(4) 0.2163(3) 0.5007(2) 0.0433(11) Uani 1 1 d . . . . .
H13A H 0.0145 0.1838 0.4858 0.052 Uiso 1 1 calc R U . . .
H13B H 0.1076 0.1625 0.5358 0.052 Uiso 1 1 calc R U . . .
C14 C 0.0281(4) 0.3184(4) 0.52197(19) 0.0438(12) Uani 1 1 d . . . . .
H14A H -0.0265 0.2977 0.5631 0.053 Uiso 1 1 calc R U . . .
H14B H 0.0990 0.3610 0.5261 0.053 Uiso 1 1 calc R U . . .
C15 C -0.1760(4) 0.3979(4) 0.4905(2) 0.0460(12) Uani 1 1 d . . . . .
H15 H -0.2302 0.3725 0.5290 0.055 Uiso 1 1 calc R U . . .
C16 C -0.2109(4) 0.4539(4) 0.4372(2) 0.0495(12) Uani 1 1 d . . . . .
H16 H -0.2948 0.4751 0.4307 0.059 Uiso 1 1 calc R U . . .
C17 C 0.0036(4) 0.4328(3) 0.41771(19) 0.0379(11) Uani 1 1 d . . . . .
C18 C -0.1009(5) 0.5350(4) 0.3291(2) 0.0484(12) Uani 1 1 d . . . . .
H18A H -0.1601 0.5006 0.3108 0.058 Uiso 1 1 calc R U . . .
H18B H -0.0149 0.5307 0.3047 0.058 Uiso 1 1 calc R U . . .
C19 C -0.1393(5) 0.6518(4) 0.32463(19) 0.0452(12) Uani 1 1 d . . . . .
C20 C -0.2650(5) 0.6849(5) 0.3274(2) 0.0638(15) Uani 1 1 d . . . . .
H20 H -0.3282 0.6327 0.3328 0.077 Uiso 1 1 calc R U . . .
C21 C -0.3005(7) 0.7926(6) 0.3223(3) 0.092(2) Uani 1 1 d . . . . .
H21 H -0.3867 0.8158 0.3233 0.110 Uiso 1 1 calc R U . . .
C22 C -0.2053(11) 0.8649(6) 0.3159(3) 0.103(3) Uani 1 1 d . . . . .
C23 C -0.0814(9) 0.8362(6) 0.3128(3) 0.100(2) Uani 1 1 d . . . . .
H23 H -0.0187 0.8885 0.3081 0.120 Uiso 1 1 calc R U . . .
C24 C -0.0487(6) 0.7288(5) 0.3166(2) 0.0656(15) Uani 1 1 d . . . . .
H24 H 0.0382 0.7072 0.3136 0.079 Uiso 1 1 calc R U . . .
C25 C 0.4455(5) 0.4939(4) 0.3418(2) 0.0532(13) Uani 1 1 d . . . . .
C26 C 0.3547(4) 0.4648(4) 0.3092(2) 0.0432(11) Uani 1 1 d . . . . .
H26 H 0.3819 0.4258 0.2752 0.052 Uiso 1 1 calc R U . . .
C27 C 0.2622(4) 0.5523(3) 0.3030(2) 0.0432(11) Uani 1 1 d . . . . .
H27 H 0.2234 0.5759 0.2647 0.052 Uiso 1 1 calc R U . . .
C28 C 0.2964(5) 0.6295(4) 0.3344(2) 0.0484(12) Uani 1 1 d . . . . .
C29 C 0.1850(6) -0.1632(4) 0.1642(3) 0.0740(18) Uani 1 1 d . . . . .
H29 H 0.1866 -0.2370 0.1855 0.089 Uiso 1 1 calc R U . . .
C30 C 0.2385(8) -0.0870(5) 0.1845(3) 0.104(3) Uani 1 1 d . . . . .
H30 H 0.2796 -0.1080 0.2195 0.125 Uiso 1 1 calc R U . . .
C31 C 0.2332(6) 0.0214(4) 0.1543(3) 0.080(2) Uani 1 1 d . . . . .
H31 H 0.2704 0.0739 0.1690 0.096 Uiso 1 1 calc R U . . .
C32 C 0.1745(4) 0.0539(3) 0.1030(2) 0.0398(11) Uani 1 1 d . . . . .
C33 C 0.1254(5) -0.0257(4) 0.0828(2) 0.0566(14) Uani 1 1 d . . . . .
H33 H 0.0875 -0.0063 0.0467 0.068 Uiso 1 1 calc R U . . .
C34 C 0.1294(5) -0.1328(4) 0.1131(3) 0.0683(16) Uani 1 1 d . . . . .
H34 H 0.0930 -0.1858 0.0983 0.082 Uiso 1 1 calc R U . . .
C35 C 0.4013(5) 0.1496(4) -0.0063(2) 0.0498(12) Uani 1 1 d . . . . .
H35 H 0.3683 0.0796 -0.0007 0.060 Uiso 1 1 calc R U . . .
C36 C 0.5178(5) 0.1748(4) -0.0429(2) 0.0545(13) Uani 1 1 d . . . . .
H36 H 0.5645 0.1221 -0.0619 0.065 Uiso 1 1 calc R U . . .
C37 C 0.5673(5) 0.2757(4) -0.0520(2) 0.0517(13) Uani 1 1 d . . . . .
H37 H 0.6470 0.2934 -0.0779 0.062 Uiso 1 1 calc R U . . .
C38 C 0.4992(4) 0.3515(4) -0.0229(2) 0.0514(13) Uani 1 1 d . . . . .
H38 H 0.5331 0.4211 -0.0285 0.062 Uiso 1 1 calc R U . . .
C39 C 0.3830(4) 0.3260(4) 0.0139(2) 0.0446(12) Uani 1 1 d . . . . .
H39 H 0.3374 0.3782 0.0338 0.054 Uiso 1 1 calc R U . . .
C40 C 0.3313(4) 0.2245(3) 0.02238(19) 0.0377(10) Uani 1 1 d . . . . .
C41 C 0.0785(4) 0.2106(4) 0.0048(2) 0.0443(12) Uani 1 1 d . . . . .
H41A H 0.1288 0.1822 -0.0297 0.053 Uiso 1 1 calc R U . . .
H41B H 0.0005 0.1678 0.0205 0.053 Uiso 1 1 calc R U . . .
C42 C 0.0430(4) 0.3306(3) -0.01895(19) 0.0434(11) Uani 1 1 d . . . . .
H42A H 0.1185 0.3755 -0.0249 0.052 Uiso 1 1 calc R U . . .
H42B H 0.0155 0.3404 -0.0595 0.052 Uiso 1 1 calc R U . . .
C43 C -0.2502(5) 0.4152(4) 0.0628(2) 0.0532(13) Uani 1 1 d . . . . .
H43 H -0.3374 0.4360 0.0682 0.064 Uiso 1 1 calc R U . . .
C44 C -0.1789(5) 0.3959(4) 0.0115(2) 0.0465(12) Uani 1 1 d . . . . .
H44 H -0.2054 0.4014 -0.0271 0.056 Uiso 1 1 calc R U . . .
C45 C -0.0530(4) 0.3673(3) 0.08410(19) 0.0364(10) Uani 1 1 d . . . . .
C46 C -0.2179(5) 0.4074(4) 0.1713(2) 0.0553(14) Uani 1 1 d . . . . .
H46A H -0.1479 0.3881 0.1954 0.066 Uiso 1 1 calc R U . . .
H46B H -0.2867 0.3551 0.1903 0.066 Uiso 1 1 calc R U . . .
C47 C -0.2675(5) 0.5209(4) 0.17498(19) 0.0443(12) Uani 1 1 d . . . . .
C48 C -0.3968(5) 0.5428(4) 0.1810(2) 0.0551(14) Uani 1 1 d . . . . .
H48 H -0.4534 0.4872 0.1827 0.066 Uiso 1 1 calc R U . . .
C49 C -0.4440(5) 0.6455(5) 0.1847(2) 0.0648(15) Uani 1 1 d . . . . .
H49 H -0.5325 0.6617 0.1894 0.078 Uiso 1 1 calc R U . . .
C50 C -0.3579(7) 0.7224(5) 0.1813(3) 0.0741(18) Uani 1 1 d . . . . .
C51 C -0.2303(6) 0.7038(5) 0.1752(2) 0.0691(16) Uani 1 1 d . . . . .
H51 H -0.1738 0.7601 0.1725 0.083 Uiso 1 1 calc R U . . .
C52 C -0.1864(5) 0.6015(5) 0.1730(2) 0.0576(14) Uani 1 1 d . . . . .
H52 H -0.0980 0.5859 0.1700 0.069 Uiso 1 1 calc R U . . .
C53 C 0.3288(6) 0.3606(5) 0.1660(3) 0.0605(15) Uani 1 1 d . . . . .
C54 C 0.2118(5) 0.3093(4) 0.1980(2) 0.0518(13) Uani 1 1 d . . . . .
H54 H 0.2114 0.2444 0.2331 0.062 Uiso 1 1 calc R U . . .
C55 C 0.1162(4) 0.3934(4) 0.2008(2) 0.0436(12) Uani 1 1 d . . . . .
H55 H 0.0478 0.3902 0.2378 0.052 Uiso 1 1 calc R U . . .
C56 C 0.1764(5) 0.4935(4) 0.1668(2) 0.0481(12) Uani 1 1 d . . . . .
C57 C 0.8131(7) 0.0651(7) 0.1564(3) 0.121(3) Uani 1 1 d . . . . .
H57A H 0.8707 0.1198 0.1606 0.145 Uiso 1 1 calc R U . . .
H57B H 0.8342 -0.0060 0.1820 0.145 Uiso 1 1 calc R U . . .
C58 C 0.6784(9) 0.0959(7) 0.1752(4) 0.126(3) Uani 1 1 d . . . . .
H58A H 0.6369 0.0404 0.2106 0.152 Uiso 1 1 calc R U . . .
H58B H 0.6726 0.1661 0.1875 0.152 Uiso 1 1 calc R U . . .
C59 C 0.6179(7) 0.1042(7) 0.1216(4) 0.121(3) Uani 1 1 d . . . . .
H59A H 0.5511 0.0495 0.1305 0.145 Uiso 1 1 calc R U . . .
H59B H 0.5792 0.1770 0.1096 0.145 Uiso 1 1 calc R U . . .
C60 C 0.7169(9) 0.0851(7) 0.0737(4) 0.117(3) Uani 1 1 d . . . . .
H60A H 0.6925 0.0256 0.0569 0.140 Uiso 1 1 calc R U . . .
H60B H 0.7277 0.1508 0.0396 0.140 Uiso 1 1 calc R U . . .
C61 C 0.9265(8) 0.1939(7) 0.3434(5) 0.135(3) Uani 1 1 d . . . . .
H61A H 1.0004 0.2311 0.3490 0.162 Uiso 1 1 calc R U . . .
H61B H 0.9579 0.1400 0.3185 0.162 Uiso 1 1 calc R U . . .
C62 C 0.8560(11) 0.1395(8) 0.4039(4) 0.143(4) Uani 1 1 d . . . . .
H62A H 0.8784 0.1681 0.4378 0.171 Uiso 1 1 calc R U . . .
H62B H 0.8717 0.0604 0.4124 0.171 Uiso 1 1 calc R U . . .
C63 C 0.7137(13) 0.1692(10) 0.3954(5) 0.206(8) Uani 1 1 d . . . . .
H63A H 0.6640 0.1033 0.4014 0.247 Uiso 1 1 calc R U . . .
H63B H 0.6721 0.2129 0.4247 0.247 Uiso 1 1 calc R U . . .
C64 C 0.7270(10) 0.2277(10) 0.3356(8) 0.196(7) Uani 1 1 d . . . . .
H64A H 0.6638 0.2880 0.3331 0.235 Uiso 1 1 calc R U . . .
H64B H 0.7080 0.1808 0.3091 0.235 Uiso 1 1 calc R U . . .
F1 F -0.4061(4) 0.8233(3) 0.18519(18) 0.1164(14) Uani 1 1 d . . . . .
F2 F -0.2420(6) 0.9715(3) 0.31266(19) 0.168(2) Uani 1 1 d . . . . .
N1 N -0.1713(4) 0.3986(3) 0.10661(16) 0.0440(10) Uani 1 1 d . . . . .
N2 N -0.0589(3) 0.3665(3) 0.02486(16) 0.0386(9) Uani 1 1 d . . . . .
N3 N -0.0457(3) 0.3848(3) 0.47786(15) 0.0354(8) Uani 1 1 d . . . . .
N4 N -0.1010(3) 0.4743(3) 0.39391(16) 0.0406(9) Uani 1 1 d . . . . .
O1 O 0.5446(3) 0.4532(3) 0.35496(17) 0.0720(11) Uani 1 1 d . . . . .
O2 O 0.4043(3) 0.5903(3) 0.36055(14) 0.0557(9) Uani 1 1 d . . . . .
O3 O 0.2509(4) 0.7169(3) 0.34163(17) 0.0696(11) Uani 1 1 d . . . . .
O4 O 0.4378(4) 0.3292(3) 0.1577(2) 0.0910(14) Uani 1 1 d . . . . .
O5 O 0.3021(3) 0.4727(3) 0.14403(16) 0.0587(9) Uani 1 1 d . . . . .
O6 O 0.1374(3) 0.5872(3) 0.15695(17) 0.0691(11) Uani 1 1 d . . . . .
O8 O 0.8450(8) 0.2691(7) 0.3126(3) 0.178(3) Uani 1 1 d . . . . .
O7 O 0.8230(5) 0.0602(6) 0.0931(3) 0.171(3) Uani 1 1 d . . . . .
P2 P 0.21764(11) 0.25205(9) 0.43789(5) 0.0366(3) Uani 1 1 d . . . . .
P1 P 0.17170(11) 0.19734(9) 0.06724(5) 0.0374(3) Uani 1 1 d . . . . .
Pd1 Pd 0.09935(3) 0.31593(3) 0.12893(2) 0.03737(11) Uani 1 1 d . . . . .
Pd2 Pd 0.18909(3) 0.41936(3) 0.37567(2) 0.03552(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 C2 1.375(8) . ?
C1 C6 1.373(7) . ?
C1 H1 0.9500 . ?
C2 C3 1.341(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.386(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(6) . ?
C4 H4 0.9500 . ?
C5 C6 1.398(6) . ?
C5 P2 1.821(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.389(6) . ?
C7 C12 1.389(6) . ?
C7 P2 1.829(4) . ?
C8 C9 1.382(6) . ?
C8 H8 0.9500 . ?
C9 C10 1.371(6) . ?
C9 H9 0.9500 . ?
C10 C11 1.378(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.377(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.532(6) . ?
C13 P2 1.840(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 N3 1.462(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.349(6) . ?
C15 N3 1.382(5) . ?
C15 H15 0.9500 . ?
C16 N4 1.383(5) . ?
C16 H16 0.9500 . ?
C17 N4 1.356(5) . ?
C17 N3 1.372(5) . ?
C17 Pd2 2.057(4) . ?
C18 N4 1.484(5) . ?
C18 C19 1.503(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C20 1.382(6) . ?
C19 C24 1.380(7) . ?
C20 C21 1.384(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.381(10) . ?
C21 H21 0.9500 . ?
C22 C23 1.350(10) . ?
C22 F2 1.378(7) . ?
C23 C24 1.377(8) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 O1 1.209(6) . ?
C25 O2 1.411(6) . ?
C25 C26 1.434(7) . ?
C26 C27 1.444(6) . ?
C26 Pd2 2.117(4) . ?
C26 H26 1.0000 . ?
C27 C28 1.438(6) . ?
C27 Pd2 2.134(4) . ?
C27 H27 1.0000 . ?
C28 O3 1.221(5) . ?
C28 O2 1.405(5) . ?
C29 C34 1.357(7) . ?
C29 C30 1.361(8) . ?
C29 H29 0.9500 . ?
C30 C31 1.391(7) . ?
C30 H30 0.9500 . ?
C31 C32 1.382(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.371(6) . ?
C32 P1 1.815(4) . ?
C33 C34 1.376(7) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C36 1.376(6) . ?
C35 C40 1.385(6) . ?
C35 H35 0.9500 . ?
C36 C37 1.375(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.389(6) . ?
C37 H37 0.9500 . ?
C38 C39 1.377(6) . ?
C38 H38 0.9500 . ?
C39 C40 1.394(6) . ?
C39 H39 0.9500 . ?
C40 P1 1.830(4) . ?
C41 C42 1.544(6) . ?
C41 P1 1.842(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 N2 1.462(5) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.332(6) . ?
C43 N1 1.386(5) . ?
C43 H43 0.9500 . ?
C44 N2 1.383(5) . ?
C44 H44 0.9500 . ?
C45 N1 1.351(5) . ?
C45 N2 1.351(5) . ?
C45 Pd1 2.068(4) . ?
C46 N1 1.482(5) . ?
C46 C47 1.524(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C52 1.372(7) . ?
C47 C48 1.386(6) . ?
C48 C49 1.389(7) . ?
C48 H48 0.9500 . ?
C49 C50 1.365(8) . ?
C49 H49 0.9500 . ?
C50 F1 1.371(6) . ?
C50 C51 1.361(8) . ?
C51 C52 1.366(7) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 O4 1.208(6) . ?
C53 O5 1.425(6) . ?
C53 C54 1.439(7) . ?
C54 C55 1.439(6) . ?
C54 Pd1 2.121(5) . ?
C54 H54 1.0000 . ?
C55 C56 1.445(6) . ?
C55 Pd1 2.124(4) . ?
C55 H55 1.0000 . ?
C56 O6 1.222(5) . ?
C56 O5 1.385(5) . ?
C57 O7 1.429(8) . ?
C57 C58 1.486(9) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 C59 1.452(9) . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C59 C60 1.424(9) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 O7 1.288(8) . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C61 O8 1.403(8) . ?
C61 C62 1.470(11) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C62 C63 1.584(14) . ?
C62 H62A 0.9900 . ?
C62 H62B 0.9900 . ?
C63 C64 1.367(16) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C64 O8 1.365(11) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
P2 Pd2 2.2947(12) . ?
P1 Pd1 2.2952(12) . ?

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
C2 C1 C6 119.9(6) . . ?
C2 C1 H1 120.1 . . ?
C6 C1 H1 120.1 . . ?
C3 C2 C1 120.8(5) . . ?
C3 C2 H2 119.6 . . ?
C1 C2 H2 119.6 . . ?
C2 C3 C4 120.5(5) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C5 C4 C3 120.3(5) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 118.2(4) . . ?
C4 C5 P2 125.1(4) . . ?
C6 C5 P2 116.7(3) . . ?
C1 C6 C5 120.4(5) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
C8 C7 C12 118.8(4) . . ?
C8 C7 P2 122.3(3) . . ?
C12 C7 P2 118.8(3) . . ?
C7 C8 C9 120.1(4) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
C10 C9 C8 120.8(5) . . ?
C10 C9 H9 119.6 . . ?
C8 C9 H9 119.6 . . ?
C9 C10 C11 119.2(5) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C10 C11 C12 120.8(4) . . ?
C10 C11 H11 119.6 . . ?
C12 C11 H11 119.6 . . ?
C11 C12 C7 120.2(4) . . ?
C11 C12 H12 119.9 . . ?
C7 C12 H12 119.9 . . ?
C14 C13 P2 109.2(3) . . ?
C14 C13 H13A 109.8 . . ?
P2 C13 H13A 109.8 . . ?
C14 C13 H13B 109.8 . . ?
P2 C13 H13B 109.8 . . ?
H13A C13 H13B 108.3 . . ?
N3 C14 C13 110.9(4) . . ?
N3 C14 H14A 109.4 . . ?
C13 C14 H14A 109.4 . . ?
N3 C14 H14B 109.4 . . ?
C13 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 N3 106.2(4) . . ?
C16 C15 H15 126.9 . . ?
N3 C15 H15 126.9 . . ?
C15 C16 N4 106.7(4) . . ?
C15 C16 H16 126.7 . . ?
N4 C16 H16 126.7 . . ?
N4 C17 N3 102.8(4) . . ?
N4 C17 Pd2 131.1(3) . . ?
N3 C17 Pd2 125.5(3) . . ?
N4 C18 C19 112.5(4) . . ?
N4 C18 H18A 109.1 . . ?
C19 C18 H18A 109.1 . . ?
N4 C18 H18B 109.1 . . ?
C19 C18 H18B 109.1 . . ?
H18A C18 H18B 107.8 . . ?
C20 C19 C24 118.5(5) . . ?
C20 C19 C18 121.1(5) . . ?
C24 C19 C18 120.3(5) . . ?
C19 C20 C21 121.3(6) . . ?
C19 C20 H20 119.3 . . ?
C21 C20 H20 119.3 . . ?
C22 C21 C20 117.0(6) . . ?
C22 C21 H21 121.5 . . ?
C20 C21 H21 121.5 . . ?
C23 C22 C21 123.6(7) . . ?
C23 C22 F2 119.7(9) . . ?
C21 C22 F2 116.6(9) . . ?
C22 C23 C24 117.9(7) . . ?
C22 C23 H23 121.0 . . ?
C24 C23 H23 121.0 . . ?
C19 C24 C23 121.5(6) . . ?
C19 C24 H24 119.3 . . ?
C23 C24 H24 119.3 . . ?
O1 C25 O2 117.7(5) . . ?
O1 C25 C26 133.2(5) . . ?
O2 C25 C26 109.1(4) . . ?
C25 C26 C27 106.6(4) . . ?
C25 C26 Pd2 106.5(3) . . ?
C27 C26 Pd2 70.8(2) . . ?
C25 C26 H26 120.7 . . ?
C27 C26 H26 120.7 . . ?
Pd2 C26 H26 120.7 . . ?
C28 C27 C26 107.1(4) . . ?
C28 C27 Pd2 104.5(3) . . ?
C26 C27 Pd2 69.5(2) . . ?
C28 C27 H27 121.3 . . ?
C26 C27 H27 121.3 . . ?
Pd2 C27 H27 121.3 . . ?
O3 C28 O2 118.3(4) . . ?
O3 C28 C27 132.9(5) . . ?
O2 C28 C27 108.8(4) . . ?
C34 C29 C30 119.4(5) . . ?
C34 C29 H29 120.3 . . ?
C30 C29 H29 120.3 . . ?
C29 C30 C31 120.3(6) . . ?
C29 C30 H30 119.8 . . ?
C31 C30 H30 119.8 . . ?
C32 C31 C30 120.9(5) . . ?
C32 C31 H31 119.5 . . ?
C30 C31 H31 119.5 . . ?
C33 C32 C31 117.0(4) . . ?
C33 C32 P1 125.6(4) . . ?
C31 C32 P1 117.5(4) . . ?
C32 C33 C34 122.1(5) . . ?
C32 C33 H33 119.0 . . ?
C34 C33 H33 119.0 . . ?
C29 C34 C33 120.3(5) . . ?
C29 C34 H34 119.9 . . ?
C33 C34 H34 119.9 . . ?
C36 C35 C40 121.1(4) . . ?
C36 C35 H35 119.5 . . ?
C40 C35 H35 119.5 . . ?
C37 C36 C35 120.6(5) . . ?
C37 C36 H36 119.7 . . ?
C35 C36 H36 119.7 . . ?
C36 C37 C38 119.2(4) . . ?
C36 C37 H37 120.4 . . ?
C38 C37 H37 120.4 . . ?
C37 C38 C39 120.2(4) . . ?
C37 C38 H38 119.9 . . ?
C39 C38 H38 119.9 . . ?
C38 C39 C40 120.9(4) . . ?
C38 C39 H39 119.6 . . ?
C40 C39 H39 119.6 . . ?
C35 C40 C39 118.1(4) . . ?
C35 C40 P1 122.5(3) . . ?
C39 C40 P1 119.4(3) . . ?
C42 C41 P1 109.8(3) . . ?
C42 C41 H41A 109.7 . . ?
P1 C41 H41A 109.7 . . ?
C42 C41 H41B 109.7 . . ?
P1 C41 H41B 109.7 . . ?
H41A C41 H41B 108.2 . . ?
N2 C42 C41 111.0(3) . . ?
N2 C42 H42A 109.4 . . ?
C41 C42 H42A 109.4 . . ?
N2 C42 H42B 109.4 . . ?
C41 C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?
C44 C43 N1 106.0(4) . . ?
C44 C43 H43 127.0 . . ?
N1 C43 H43 127.0 . . ?
C43 C44 N2 107.2(4) . . ?
C43 C44 H44 126.4 . . ?
N2 C44 H44 126.4 . . ?
N1 C45 N2 103.5(4) . . ?
N1 C45 Pd1 130.0(3) . . ?
N2 C45 Pd1 126.2(3) . . ?
N1 C46 C47 112.1(4) . . ?
N1 C46 H46A 109.2 . . ?
C47 C46 H46A 109.2 . . ?
N1 C46 H46B 109.2 . . ?
C47 C46 H46B 109.2 . . ?
H46A C46 H46B 107.9 . . ?
C52 C47 C48 119.4(5) . . ?
C52 C47 C46 121.2(5) . . ?
C48 C47 C46 119.4(5) . . ?
C49 C48 C47 120.4(5) . . ?
C49 C48 H48 119.8 . . ?
C47 C48 H48 119.8 . . ?
C50 C49 C48 117.2(5) . . ?
C50 C49 H49 121.4 . . ?
C48 C49 H49 121.4 . . ?
F1 C50 C49 116.4(6) . . ?
F1 C50 C51 119.5(7) . . ?
C49 C50 C51 124.0(6) . . ?
C52 C51 C50 117.7(6) . . ?
C52 C51 H51 121.1 . . ?
C50 C51 H51 121.1 . . ?
C51 C52 C47 121.3(5) . . ?
C51 C52 H52 119.3 . . ?
C47 C52 H52 119.3 . . ?
O4 C53 O5 118.2(6) . . ?
O4 C53 C54 133.7(6) . . ?
O5 C53 C54 108.0(4) . . ?
C55 C54 C53 107.3(4) . . ?
C55 C54 Pd1 70.3(2) . . ?
C53 C54 Pd1 105.7(3) . . ?
C55 C54 H54 120.9 . . ?
C53 C54 H54 120.9 . . ?
Pd1 C54 H54 120.9 . . ?
C54 C55 C56 106.5(4) . . ?
C54 C55 Pd1 70.1(2) . . ?
C56 C55 Pd1 102.3(3) . . ?
C54 C55 H55 121.9 . . ?
C56 C55 H55 121.9 . . ?
Pd1 C55 H55 121.9 . . ?
O6 C56 O5 118.4(5) . . ?
O6 C56 C55 132.1(5) . . ?
O5 C56 C55 109.4(4) . . ?
O7 C57 C58 104.5(6) . . ?
O7 C57 H57A 110.9 . . ?
C58 C57 H57A 110.9 . . ?
O7 C57 H57B 110.9 . . ?
C58 C57 H57B 110.9 . . ?
H57A C57 H57B 108.9 . . ?
C59 C58 C57 106.3(6) . . ?
C59 C58 H58A 110.5 . . ?
C57 C58 H58A 110.5 . . ?
C59 C58 H58B 110.5 . . ?
C57 C58 H58B 110.5 . . ?
H58A C58 H58B 108.7 . . ?
C60 C59 C58 105.3(7) . . ?
C60 C59 H59A 110.7 . . ?
C58 C59 H59A 110.7 . . ?
C60 C59 H59B 110.7 . . ?
C58 C59 H59B 110.7 . . ?
H59A C59 H59B 108.8 . . ?
O7 C60 C59 112.1(7) . . ?
O7 C60 H60A 109.2 . . ?
C59 C60 H60A 109.2 . . ?
O7 C60 H60B 109.2 . . ?
C59 C60 H60B 109.2 . . ?
H60A C60 H60B 107.9 . . ?
O8 C61 C62 108.6(8) . . ?
O8 C61 H61A 110.0 . . ?
C62 C61 H61A 110.0 . . ?
O8 C61 H61B 110.0 . . ?
C62 C61 H61B 110.0 . . ?
H61A C61 H61B 108.4 . . ?
C61 C62 C63 101.8(7) . . ?
C61 C62 H62A 111.4 . . ?
C63 C62 H62A 111.4 . . ?
C61 C62 H62B 111.4 . . ?
C63 C62 H62B 111.4 . . ?
H62A C62 H62B 109.3 . . ?
C64 C63 C62 102.6(8) . . ?
C64 C63 H63A 111.2 . . ?
C62 C63 H63A 111.2 . . ?
C64 C63 H63B 111.2 . . ?
C62 C63 H63B 111.2 . . ?
H63A C63 H63B 109.2 . . ?
C63 C64 O8 113.7(12) . . ?
C63 C64 H64A 108.8 . . ?
O8 C64 H64A 108.8 . . ?
C63 C64 H64B 108.8 . . ?
O8 C64 H64B 108.8 . . ?
H64A C64 H64B 107.7 . . ?
C45 N1 C43 112.0(4) . . ?
C45 N1 C46 125.6(4) . . ?
C43 N1 C46 122.3(4) . . ?
C45 N2 C44 111.3(4) . . ?
C45 N2 C42 125.5(4) . . ?
C44 N2 C42 123.0(4) . . ?
C17 N3 C15 112.1(4) . . ?
C17 N3 C14 124.3(4) . . ?
C15 N3 C14 123.3(4) . . ?
C17 N4 C16 112.3(4) . . ?
C17 N4 C18 125.1(4) . . ?
C16 N4 C18 122.6(4) . . ?
C25 O2 C28 107.9(4) . . ?
C56 O5 C53 108.4(4) . . ?
C64 O8 C61 104.4(9) . . ?
C60 O7 C57 111.6(6) . . ?
C5 P2 C7 103.83(19) . . ?
C5 P2 C13 106.0(2) . . ?
C7 P2 C13 101.4(2) . . ?
C5 P2 Pd2 117.44(15) . . ?
C7 P2 Pd2 115.21(14) . . ?
C13 P2 Pd2 111.33(14) . . ?
C32 P1 C40 104.67(19) . . ?
C32 P1 C41 105.2(2) . . ?
C40 P1 C41 100.9(2) . . ?
C32 P1 Pd1 118.44(14) . . ?
C40 P1 Pd1 114.52(14) . . ?
C41 P1 Pd1 111.24(14) . . ?
C45 Pd1 C54 154.79(18) . . ?
C45 Pd1 C55 115.37(17) . . ?
C54 Pd1 C55 39.64(16) . . ?
C45 Pd1 P1 93.01(12) . . ?
C54 Pd1 P1 112.12(13) . . ?
C55 Pd1 P1 151.58(13) . . ?
C17 Pd2 C26 156.29(17) . . ?
C17 Pd2 C27 116.84(17) . . ?
C26 Pd2 C27 39.71(16) . . ?
C17 Pd2 P2 93.07(12) . . ?
C26 Pd2 P2 110.48(12) . . ?
C27 Pd2 P2 150.08(13) . . ?

_refine_diff_density_max         1.221
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.090

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ljy083
_database_code_depnum_ccdc_archive 'CCDC 1477476'
_audit_update_record             
;
2016-05-21 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C29 H27 N2 O4 P Pd'
_chemical_formula_sum            'C29 H27 N2 O4 P Pd'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         604.89
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.1522(5)
_cell_length_b                   25.9604(14)
_cell_length_c                   10.9541(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.829(3)
_cell_angle_gamma                90
_cell_volume                     2596.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    18429
_cell_measurement_theta_min      2.4
_cell_measurement_theta_max      33.6
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   0.848
_exptl_transmission_factor_max   0.854
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            33576
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.569
_diffrn_reflns_theta_max         28.699
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6708
_reflns_number_gt                6064
_reflns_threshold_expression     I>2σ
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'DIAMOND (Brandenburg, 2006)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0295P)²+9.7706P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6708
_refine_ls_number_parameters     335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1048
_refine_ls_wR_factor_gt          0.1019
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.37724(3) 0.60083(2) 0.36152(2) 0.02320(7) Uani 1 1 d . . . . .
P1 P 0.60253(8) 0.63606(3) 0.34579(7) 0.02195(16) Uani 1 1 d . . . . .
O1 O 0.0805(3) 0.50400(12) 0.2744(3) 0.0499(8) Uani 1 1 d . . . . .
O2 O 0.2149(3) 0.54147(10) 0.1351(2) 0.0373(6) Uani 1 1 d . . . . .
O3 O 0.3178(4) 0.59994(14) 0.0149(3) 0.0534(8) Uani 1 1 d . . . . .
O4 O 0.1170(4) 0.75639(11) 0.5494(3) 0.0544(8) Uani 1 1 d . . . . .
N1 N 0.3459(3) 0.56591(10) 0.6287(2) 0.0272(6) Uani 1 1 d . . . . .
N2 N 0.5699(3) 0.56228(11) 0.5847(2) 0.0273(6) Uani 1 1 d . . . . .
C1 C 0.1538(4) 0.59406(14) 0.2946(3) 0.0302(7) Uani 1 1 d . . . . .
H1 H 0.1163 0.6053 0.3689 0.036 Uiso 1 1 calc R U . . .
C2 C 0.1409(4) 0.54311(14) 0.2431(3) 0.0335(7) Uani 1 1 d . . . . .
C3 C 0.2639(4) 0.59142(15) 0.1101(3) 0.0343(7) Uani 1 1 d . . . . .
C4 C 0.2340(4) 0.62474(13) 0.2127(3) 0.0284(6) Uani 1 1 d . . . . .
H4 H 0.2620 0.6598 0.2233 0.034 Uiso 1 1 calc R U . . .
C5 C 0.4328(3) 0.57063(12) 0.5334(3) 0.0249(6) Uani 1 1 d . . . . .
C6 C 0.1860(4) 0.56797(14) 0.6176(3) 0.0317(7) Uani 1 1 d . . . . .
H6A H 0.1478 0.5421 0.6737 0.038 Uiso 1 1 calc R U . . .
H6B H 0.1522 0.5580 0.5332 0.038 Uiso 1 1 calc R U . . .
C7 C 0.1201(4) 0.61979(14) 0.6454(3) 0.0295(7) Uani 1 1 d . . . . .
C8 C 0.1560(4) 0.66414(14) 0.5811(3) 0.0320(7) Uani 1 1 d . . . . .
H8 H 0.2265 0.6624 0.5214 0.038 Uiso 1 1 calc R U . . .
C9 C 0.0886(4) 0.71061(15) 0.6045(4) 0.0389(8) Uani 1 1 d . . . . .
C10 C -0.0171(5) 0.71234(18) 0.6908(4) 0.0478(10) Uani 1 1 d . . . . .
H10 H -0.0655 0.7439 0.7059 0.057 Uiso 1 1 calc R U . . .
C11 C -0.0513(5) 0.66891(19) 0.7536(4) 0.0485(10) Uani 1 1 d . . . . .
H11 H -0.1227 0.6706 0.8126 0.058 Uiso 1 1 calc R U . . .
C12 C 0.0168(4) 0.62263(17) 0.7323(3) 0.0384(8) Uani 1 1 d . . . . .
H12 H -0.0070 0.5928 0.7770 0.046 Uiso 1 1 calc R U . . .
C13 C 0.2175(5) 0.75623(19) 0.4561(5) 0.0550(12) Uani 1 1 d . . . . .
H13A H 0.3141 0.7453 0.4907 0.083 Uiso 1 1 calc R U . . .
H13B H 0.2245 0.7910 0.4220 0.083 Uiso 1 1 calc R U . . .
H13C H 0.1833 0.7323 0.3912 0.083 Uiso 1 1 calc R U . . .
C14 C 0.4284(4) 0.55600(14) 0.7367(3) 0.0341(8) Uani 1 1 d . . . . .
H14 H 0.3924 0.5520 0.8155 0.041 Uiso 1 1 calc R U . . .
C15 C 0.5685(4) 0.55309(14) 0.7092(3) 0.0338(7) Uani 1 1 d . . . . .
H15 H 0.6507 0.5461 0.7642 0.041 Uiso 1 1 calc R U . . .
C16 C 0.7039(4) 0.56490(14) 0.5182(3) 0.0299(7) Uani 1 1 d . . . . .
H16A H 0.6943 0.5418 0.4463 0.036 Uiso 1 1 calc R U . . .
H16B H 0.7883 0.5530 0.5722 0.036 Uiso 1 1 calc R U . . .
C17 C 0.7320(4) 0.61999(14) 0.4759(3) 0.0289(7) Uani 1 1 d . . . . .
H17A H 0.8337 0.6231 0.4511 0.035 Uiso 1 1 calc R U . . .
H17B H 0.7196 0.6443 0.5439 0.035 Uiso 1 1 calc R U . . .
C18 C 0.6017(3) 0.70578(13) 0.3355(3) 0.0268(6) Uani 1 1 d . . . . .
C19 C 0.5258(5) 0.72818(16) 0.2343(4) 0.0471(10) Uani 1 1 d . . . . .
H19 H 0.4888 0.7069 0.1688 0.056 Uiso 1 1 calc R U . . .
C20 C 0.5034(5) 0.78096(18) 0.2278(5) 0.0583(13) Uani 1 1 d . . . . .
H20 H 0.4538 0.7957 0.1573 0.070 Uiso 1 1 calc R U . . .
C21 C 0.5531(6) 0.81177(17) 0.3233(5) 0.0560(12) Uani 1 1 d . . . . .
H21 H 0.5339 0.8477 0.3207 0.067 Uiso 1 1 calc R U . . .
C22 C 0.6291(7) 0.79118(18) 0.4207(5) 0.0624(14) Uani 1 1 d . . . . .
H22 H 0.6650 0.8129 0.4858 0.075 Uiso 1 1 calc R U . . .
C23 C 0.6560(5) 0.73809(17) 0.4275(4) 0.0489(11) Uani 1 1 d . . . . .
H23 H 0.7120 0.7243 0.4959 0.059 Uiso 1 1 calc R U . . .
C24 C 0.6962(3) 0.61303(12) 0.2148(3) 0.0243(6) Uani 1 1 d . . . . .
C25 C 0.8191(4) 0.63711(14) 0.1731(3) 0.0309(7) Uani 1 1 d . . . . .
H25 H 0.8561 0.6675 0.2122 0.037 Uiso 1 1 calc R U . . .
C26 C 0.8883(4) 0.61694(17) 0.0745(3) 0.0380(8) Uani 1 1 d . . . . .
H26 H 0.9704 0.6341 0.0448 0.046 Uiso 1 1 calc R U . . .
C27 C 0.8372(4) 0.57167(16) 0.0196(3) 0.0397(9) Uani 1 1 d . . . . .
H27 H 0.8870 0.5571 -0.0454 0.048 Uiso 1 1 calc R U . . .
C28 C 0.7143(5) 0.54776(17) 0.0593(4) 0.0453(10) Uani 1 1 d . . . . .
H28 H 0.6785 0.5171 0.0206 0.054 Uiso 1 1 calc R U . . .
C29 C 0.6429(4) 0.56860(14) 0.1561(3) 0.0351(8) Uani 1 1 d . . . . .
H29 H 0.5573 0.5524 0.1822 0.042 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C5 2.071(3) . ?
Pd1 C4 2.116(3) . ?
Pd1 C1 2.133(3) . ?
Pd1 P1 2.2727(8) . ?
P1 C18 1.813(3) . ?
P1 C24 1.821(3) . ?
P1 C17 1.839(3) . ?
O1 C2 1.216(4) . ?
O2 C2 1.403(5) . ?
O2 C3 1.405(5) . ?
O3 C3 1.204(4) . ?
O4 C9 1.366(5) . ?
O4 C13 1.420(6) . ?
N1 C5 1.360(4) . ?
N1 C14 1.385(4) . ?
N1 C6 1.461(4) . ?
N2 C5 1.358(4) . ?
N2 C15 1.386(4) . ?
N2 C16 1.469(4) . ?
C1 C4 1.438(5) . ?
C1 C2 1.440(5) . ?
C1 H1 0.9500 . ?
C3 C4 1.458(5) . ?
C4 H4 0.9500 . ?
C6 C7 1.513(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C12 1.388(5) . ?
C7 C8 1.400(5) . ?
C8 C9 1.387(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.398(6) . ?
C10 C11 1.368(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.381(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.339(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.530(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C23 1.378(5) . ?
C18 C19 1.395(5) . ?
C19 C20 1.387(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.371(7) . ?
C20 H20 0.9500 . ?
C21 C22 1.345(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.401(7) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C24 C29 1.393(5) . ?
C24 C25 1.391(4) . ?
C25 C26 1.390(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.387(6) . ?
C26 H26 0.9500 . ?
C27 C28 1.380(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.391(5) . ?
C28 H28 0.9500 . ?
C29 H29 0.9500 . ?

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
C5 Pd1 C4 155.96(13) . . ?
C5 Pd1 C1 116.90(13) . . ?
C4 Pd1 C1 39.55(13) . . ?
C5 Pd1 P1 93.01(9) . . ?
C4 Pd1 P1 110.01(9) . . ?
C1 Pd1 P1 149.43(10) . . ?
C18 P1 C24 106.20(14) . . ?
C18 P1 C17 105.95(16) . . ?
C24 P1 C17 102.89(15) . . ?
C18 P1 Pd1 113.96(11) . . ?
C24 P1 Pd1 113.88(11) . . ?
C17 P1 Pd1 113.00(11) . . ?
C2 O2 C3 108.3(3) . . ?
C9 O4 C13 117.9(3) . . ?
C5 N1 C14 111.0(3) . . ?
C5 N1 C6 124.5(3) . . ?
C14 N1 C6 124.3(3) . . ?
C5 N2 C15 111.4(3) . . ?
C5 N2 C16 124.5(3) . . ?
C15 N2 C16 124.0(3) . . ?
C4 C1 C2 107.2(3) . . ?
C4 C1 Pd1 69.57(19) . . ?
C2 C1 Pd1 105.2(2) . . ?
C4 C1 H1 126.4 . . ?
C2 C1 H1 126.4 . . ?
Pd1 C1 H1 94.2 . . ?
O1 C2 O2 117.8(4) . . ?
O1 C2 C1 133.1(4) . . ?
O2 C2 C1 109.1(3) . . ?
O3 C3 O2 119.5(4) . . ?
O3 C3 C4 131.9(4) . . ?
O2 C3 C4 108.6(3) . . ?
C1 C4 C3 106.4(3) . . ?
C1 C4 Pd1 70.88(19) . . ?
C3 C4 Pd1 106.3(2) . . ?
C1 C4 H4 126.8 . . ?
C3 C4 H4 126.8 . . ?
Pd1 C4 H4 92.2 . . ?
N1 C5 N2 103.9(3) . . ?
N1 C5 Pd1 127.7(2) . . ?
N2 C5 Pd1 126.9(2) . . ?
N1 C6 C7 115.2(3) . . ?
N1 C6 H6A 108.5 . . ?
C7 C6 H6A 108.5 . . ?
N1 C6 H6B 108.5 . . ?
C7 C6 H6B 108.5 . . ?
H6A C6 H6B 107.5 . . ?
C12 C7 C8 119.7(3) . . ?
C12 C7 C6 118.9(3) . . ?
C8 C7 C6 121.3(3) . . ?
C9 C8 C7 120.0(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
O4 C9 C8 125.1(4) . . ?
O4 C9 C10 115.6(4) . . ?
C8 C9 C10 119.3(4) . . ?
C11 C10 C9 120.4(4) . . ?
C11 C10 H10 119.8 . . ?
C9 C10 H10 119.8 . . ?
C10 C11 C12 120.7(4) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 119.9(4) . . ?
C11 C12 H12 120.1 . . ?
C7 C12 H12 120.1 . . ?
O4 C13 H13A 109.5 . . ?
O4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
O4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N1 107.1(3) . . ?
C15 C14 H14 126.4 . . ?
N1 C14 H14 126.4 . . ?
C14 C15 N2 106.5(3) . . ?
C14 C15 H15 126.7 . . ?
N2 C15 H15 126.7 . . ?
N2 C16 C17 110.9(3) . . ?
N2 C16 H16A 109.5 . . ?
C17 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
C17 C16 H16B 109.5 . . ?
H16A C16 H16B 108.1 . . ?
C16 C17 P1 109.5(2) . . ?
C16 C17 H17A 109.8 . . ?
P1 C17 H17A 109.8 . . ?
C16 C17 H17B 109.8 . . ?
P1 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
C23 C18 C19 117.6(4) . . ?
C23 C18 P1 124.2(3) . . ?
C19 C18 P1 117.7(3) . . ?
C20 C19 C18 121.1(4) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
C21 C20 C19 119.8(5) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C22 C21 C20 120.1(4) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C21 C22 C23 120.8(4) . . ?
C21 C22 H22 119.6 . . ?
C23 C22 H22 119.6 . . ?
C18 C23 C22 120.4(4) . . ?
C18 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C29 C24 C25 119.1(3) . . ?
C29 C24 P1 117.9(2) . . ?
C25 C24 P1 123.0(3) . . ?
C26 C25 C24 120.4(3) . . ?
C26 C25 H25 119.8 . . ?
C24 C25 H25 119.8 . . ?
C27 C26 C25 119.9(3) . . ?
C27 C26 H26 120.1 . . ?
C25 C26 H26 120.1 . . ?
C28 C27 C26 120.2(3) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 119.9(4) . . ?
C27 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C28 C29 C24 120.4(3) . . ?
C28 C29 H29 119.8 . . ?
C24 C29 H29 119.8 . . ?

_refine_diff_density_max         4.091
_refine_diff_density_min         -1.602
_refine_diff_density_rms         0.100

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ymj088
_database_code_depnum_ccdc_archive 'CCDC 1477477'
_audit_update_record             
;
2016-05-21 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '2(C28 H25 N2 O3 P Pd), C4 H8 O'
_chemical_formula_sum            'C60 H58 N4 O7 P2 Pd2'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         1221.84
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?


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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6104(6)
_cell_length_b                   11.6829(6)
_cell_length_c                   12.5519(6)
_cell_angle_alpha                95.426(3)
_cell_angle_beta                 93.106(3)
_cell_angle_gamma                110.644(3)
_cell_volume                     1443.09(13)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6101
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      28.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_F_000             624
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.733
_shelx_estimated_absorpt_T_min   0.867
_shelx_estimated_absorpt_T_max   0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14625
_diffrn_reflns_av_unetI/netI     0.0904
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.637
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measured_fraction_theta_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_point_group_measured_fraction_full 0.954
_reflns_number_total             5871
_reflns_number_gt                4377
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'DIAMOND (Brandenburg, 2006)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1156P)²+9.6858P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5871
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0871
_refine_ls_wR_factor_ref         0.2466
_refine_ls_wR_factor_gt          0.2308
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.74292(7) 0.75117(6) 0.15723(5) 0.0268(2) Uani 1 1 d . . . . .
P1 P 0.7427(2) 0.6273(2) 0.28789(17) 0.0261(5) Uani 1 1 d . . . . .
O1 O 0.9679(7) 0.7768(6) -0.0031(5) 0.0389(16) Uani 1 1 d . . . . .
O2 O 0.8190(8) 0.8023(7) -0.1218(5) 0.0457(18) Uani 1 1 d . . . . .
O3 O 1.1145(7) 0.7994(8) 0.1422(7) 0.056(2) Uani 1 1 d . . . . .
N1 N 0.4638(7) 0.5449(6) 0.1254(5) 0.0235(14) Uani 1 1 d . . . . .
N2 N 0.4423(7) 0.7122(6) 0.0868(6) 0.0272(15) Uani 1 1 d . . . . .
C1 C 0.5361(8) 0.6637(8) 0.1151(6) 0.0245(17) Uani 1 1 d . . . . .
C2 C 0.3124(9) 0.6235(9) 0.0805(8) 0.034(2) Uani 1 1 d . . . . .
H2 H 0.2317 0.6343 0.0617 0.041 Uiso 1 1 calc R U . . .
C3 C 0.3263(9) 0.5193(8) 0.1068(7) 0.0297(19) Uani 1 1 d . . . . .
H3 H 0.2572 0.4447 0.1115 0.036 Uiso 1 1 calc R U . . .
C4 C 0.5179(8) 0.4551(8) 0.1655(7) 0.0252(17) Uani 1 1 d . . . . .
H4A H 0.5872 0.4468 0.1214 0.030 Uiso 1 1 calc R U . . .
H4B H 0.4460 0.3752 0.1612 0.030 Uiso 1 1 calc R U . . .
C5 C 0.5780(8) 0.4990(8) 0.2824(7) 0.0278(18) Uani 1 1 d . . . . .
H5A H 0.5905 0.4312 0.3150 0.033 Uiso 1 1 calc R U . . .
H5B H 0.5162 0.5262 0.3227 0.033 Uiso 1 1 calc R U . . .
C6 C 0.7815(11) 0.6963(9) 0.4268(7) 0.039(2) Uani 1 1 d . . . . .
C7 C 0.7084(10) 0.6532(10) 0.5092(8) 0.043(2) Uani 1 1 d . . . . .
H7 H 0.6323 0.5813 0.4967 0.051 Uiso 1 1 calc R U . . .
C8 C 0.7468(11) 0.7165(12) 0.6130(8) 0.047(3) Uani 1 1 d . . . . .
H8 H 0.6923 0.6907 0.6682 0.056 Uiso 1 1 calc R U . . .
C9 C 0.8626(19) 0.8144(12) 0.6328(10) 0.081(5) Uani 1 1 d . . . . .
H9 H 0.8842 0.8591 0.7009 0.097 Uiso 1 1 calc R U . . .
C10 C 0.953(2) 0.8515(16) 0.5529(11) 0.117(8) Uani 1 1 d . . . . .
H10 H 1.0392 0.9105 0.5686 0.140 Uiso 1 1 calc R U . . .
C11 C 0.904(2) 0.7940(16) 0.4496(12) 0.135(10) Uani 1 1 d . . . . .
H11 H 0.9546 0.8222 0.3931 0.161 Uiso 1 1 calc R U . . .
C12 C 0.8577(9) 0.5432(9) 0.2715(7) 0.032(2) Uani 1 1 d . . . . .
C13 C 0.8967(9) 0.5229(9) 0.1692(7) 0.033(2) Uani 1 1 d . . . . .
H13 H 0.8695 0.5569 0.1122 0.039 Uiso 1 1 calc R U . . .
C14 C 0.9761(10) 0.4518(9) 0.1528(8) 0.038(2) Uani 1 1 d . . . . .
H14 H 1.0041 0.4403 0.0850 0.045 Uiso 1 1 calc R U . . .
C15 C 1.0139(10) 0.3983(10) 0.2350(8) 0.041(2) Uani 1 1 d . . . . .
H15 H 1.0663 0.3500 0.2227 0.049 Uiso 1 1 calc R U . . .
C16 C 0.9746(11) 0.4158(11) 0.3354(8) 0.048(3) Uani 1 1 d . . . . .
H16 H 1.0013 0.3804 0.3916 0.058 Uiso 1 1 calc R U . . .
C17 C 0.8945(10) 0.4867(10) 0.3534(8) 0.042(2) Uani 1 1 d . . . . .
H17 H 0.8655 0.4960 0.4211 0.051 Uiso 1 1 calc R U . . .
C18 C 0.4696(10) 0.8394(8) 0.0647(7) 0.034(2) Uani 1 1 d . . . . .
H18A H 0.5646 0.8877 0.0844 0.041 Uiso 1 1 calc R U . . .
H18B H 0.4171 0.8749 0.1088 0.041 Uiso 1 1 calc R U . . .
C19 C 0.4348(9) 0.8468(8) -0.0525(7) 0.0301(19) Uani 1 1 d . . . . .
C20 C 0.3090(10) 0.8457(8) -0.0875(8) 0.037(2) Uani 1 1 d . . . . .
H20 H 0.2446 0.8393 -0.0387 0.044 Uiso 1 1 calc R U . . .
C21 C 0.2773(14) 0.8538(11) -0.1933(10) 0.059(3) Uani 1 1 d . . . . .
H21 H 0.1921 0.8532 -0.2160 0.071 Uiso 1 1 calc R U . . .
C22 C 0.3732(16) 0.8629(11) -0.2663(9) 0.060(3) Uani 1 1 d . . . . .
H22 H 0.3524 0.8686 -0.3380 0.072 Uiso 1 1 calc R U . . .
C23 C 0.4990(16) 0.8636(10) -0.2324(10) 0.061(4) Uani 1 1 d . . . . .
H23 H 0.5626 0.8683 -0.2816 0.074 Uiso 1 1 calc R U . . .
C24 C 0.5307(12) 0.8572(9) -0.1260(8) 0.042(2) Uani 1 1 d . . . . .
H24 H 0.6166 0.8600 -0.1031 0.051 Uiso 1 1 calc R U . . .
C25 C 0.9378(10) 0.8870(9) 0.1515(7) 0.034(2) Uani 1 1 d . . . . .
H25 H 0.9430 0.9188 0.2231 0.041 Uiso 1 1 calc R U . . .
C26 C 0.8472(9) 0.8940(8) 0.0640(7) 0.0311(19) Uani 1 1 d . . . . .
H26 H 0.7871 0.9357 0.0667 0.037 Uiso 1 1 calc R U . . .
C27 C 0.8699(9) 0.8222(9) -0.0289(8) 0.035(2) Uani 1 1 d . . . . .
C28 C 1.0189(10) 0.8208(10) 0.1059(8) 0.041(2) Uani 1 1 d . . . . .
C302 C 0.376(2) 0.8736(18) 0.3801(19) 0.077(8) Uani 0.5 1 d G . P . .
H30A H 0.3529 0.8700 0.3037 0.092 Uiso 0.5 1 calc R U P . .
H30B H 0.4086 0.9588 0.4124 0.092 Uiso 0.5 1 calc R U P . .
C301 C 0.4783(14) 0.8148(16) 0.4006(16) 0.054(6) Uani 0.5 1 d G . P . .
H30C H 0.5439 0.8326 0.3478 0.065 Uiso 0.5 1 calc R U P . .
H30D H 0.5258 0.8449 0.4717 0.065 Uiso 0.5 1 calc R U P . .
O11 O 0.404(3) 0.6870(14) 0.3923(18) 0.146(14) Uani 0.5 1 d G . P . .
C305 C 0.269(2) 0.670(2) 0.417(2) 0.24(5) Uani 0.5 1 d G . P . .
H30E H 0.2495 0.6297 0.4813 0.289 Uiso 0.5 1 calc R U P . .
H30F H 0.2043 0.6190 0.3582 0.289 Uiso 0.5 1 calc R U P . .
C300 C 0.2566(18) 0.795(3) 0.434(2) 0.17(3) Uani 0.5 1 d G . P . .
H30G H 0.2638 0.8241 0.5097 0.202 Uiso 0.5 1 calc R U P . .
H30H H 0.1718 0.7938 0.3998 0.202 Uiso 0.5 1 calc R U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C1 2.081(8) . ?
Pd1 C25 2.127(10) . ?
Pd1 C26 2.142(8) . ?
Pd1 P1 2.287(2) . ?
P1 C6 1.811(10) . ?
P1 C12 1.825(9) . ?
P1 C5 1.851(9) . ?
O1 C27 1.362(11) . ?
O1 C28 1.420(13) . ?
O2 C27 1.224(12) . ?
O3 C28 1.204(12) . ?
N1 C1 1.351(11) . ?
N1 C3 1.384(11) . ?
N1 C4 1.475(9) . ?
N2 C1 1.355(10) . ?
N2 C2 1.395(12) . ?
N2 C18 1.467(11) . ?
C2 C3 1.346(12) . ?
C2 H2 0.9300 . ?
C3 H3 0.9300 . ?
C4 C5 1.533(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.354(13) . ?
C6 C11 1.38(2) . ?
C7 C8 1.399(15) . ?
C7 H7 0.9300 . ?
C8 C9 1.343(19) . ?
C8 H8 0.9300 . ?
C9 C10 1.42(2) . ?
C9 H9 0.9300 . ?
C10 C11 1.39(2) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C17 1.383(13) . ?
C12 C13 1.395(12) . ?
C13 C14 1.387(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.367(14) . ?
C14 H14 0.9300 . ?
C15 C16 1.368(14) . ?
C15 H15 0.9300 . ?
C16 C17 1.392(14) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
C18 C19 1.515(12) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.378(13) . ?
C19 C24 1.392(13) . ?
C20 C21 1.373(15) . ?
C20 H20 0.9300 . ?
C21 C22 1.389(18) . ?
C21 H21 0.9300 . ?
C22 C23 1.375(19) . ?
C22 H22 0.9300 . ?
C23 C24 1.375(16) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?
C25 C26 1.447(13) . ?
C25 C28 1.451(13) . ?
C25 H25 0.9300 . ?
C26 C27 1.452(12) . ?
C26 H26 0.9300 . ?
C302 C301 1.4990 . ?
C302 C300 1.5143 . ?
C302 H30A 0.9700 . ?
C302 H30B 0.9700 . ?
C301 O11 1.4123 . ?
C301 H30C 0.9700 . ?
C301 H30D 0.9700 . ?
O11 C305 1.4321 . ?
C305 C300 1.5058 . ?
C305 H30E 0.9700 . ?
C305 H30F 0.9700 . ?
C300 H30G 0.9700 . ?
C300 H30H 0.9700 . ?

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
C1 Pd1 C25 155.4(3) . . ?
C1 Pd1 C26 116.1(3) . . ?
C25 Pd1 C26 39.6(4) . . ?
C1 Pd1 P1 92.7(2) . . ?
C25 Pd1 P1 111.8(3) . . ?
C26 Pd1 P1 151.1(3) . . ?
C6 P1 C12 103.7(4) . . ?
C6 P1 C5 105.8(4) . . ?
C12 P1 C5 101.2(4) . . ?
C6 P1 Pd1 118.6(3) . . ?
C12 P1 Pd1 114.3(3) . . ?
C5 P1 Pd1 111.4(3) . . ?
C27 O1 C28 108.4(7) . . ?
C1 N1 C3 111.5(7) . . ?
C1 N1 C4 126.1(7) . . ?
C3 N1 C4 122.0(7) . . ?
C1 N2 C2 110.5(7) . . ?
C1 N2 C18 126.1(7) . . ?
C2 N2 C18 123.3(7) . . ?
N1 C1 N2 104.7(7) . . ?
N1 C1 Pd1 125.2(6) . . ?
N2 C1 Pd1 129.6(6) . . ?
C3 C2 N2 106.8(8) . . ?
C3 C2 H2 126.6 . . ?
N2 C2 H2 126.6 . . ?
C2 C3 N1 106.5(8) . . ?
C2 C3 H3 126.8 . . ?
N1 C3 H3 126.8 . . ?
N1 C4 C5 109.6(7) . . ?
N1 C4 H4A 109.8 . . ?
C5 C4 H4A 109.8 . . ?
N1 C4 H4B 109.8 . . ?
C5 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
C4 C5 P1 110.2(5) . . ?
C4 C5 H5A 109.6 . . ?
P1 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
P1 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C7 C6 C11 118.7(10) . . ?
C7 C6 P1 125.6(8) . . ?
C11 C6 P1 115.5(8) . . ?
C6 C7 C8 120.3(10) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C9 C8 C7 119.9(10) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 121.7(12) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 H9 119.1 . . ?
C11 C10 C9 115.5(17) . . ?
C11 C10 H10 122.2 . . ?
C9 C10 H10 122.2 . . ?
C6 C11 C10 122.8(14) . . ?
C6 C11 H11 118.6 . . ?
C10 C11 H11 118.6 . . ?
C17 C12 C13 118.6(8) . . ?
C17 C12 P1 122.4(7) . . ?
C13 C12 P1 118.5(7) . . ?
C14 C13 C12 119.7(8) . . ?
C14 C13 H13 120.1 . . ?
C12 C13 H13 120.1 . . ?
C15 C14 C13 120.9(9) . . ?
C15 C14 H14 119.5 . . ?
C13 C14 H14 119.5 . . ?
C14 C15 C16 120.0(9) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 C17 119.9(9) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C12 C17 C16 120.7(9) . . ?
C12 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
N2 C18 C19 112.2(7) . . ?
N2 C18 H18A 109.2 . . ?
C19 C18 H18A 109.2 . . ?
N2 C18 H18B 109.2 . . ?
C19 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C20 C19 C24 119.0(9) . . ?
C20 C19 C18 120.6(8) . . ?
C24 C19 C18 120.3(9) . . ?
C21 C20 C19 120.9(10) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C20 C21 C22 119.6(12) . . ?
C20 C21 H21 120.2 . . ?
C22 C21 H21 120.2 . . ?
C23 C22 C21 120.0(11) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C24 C23 C22 120.1(11) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C19 120.3(11) . . ?
C23 C24 H24 119.8 . . ?
C19 C24 H24 119.8 . . ?
C26 C25 C28 106.7(8) . . ?
C26 C25 Pd1 70.7(5) . . ?
C28 C25 Pd1 105.5(6) . . ?
C26 C25 H25 126.7 . . ?
C28 C25 H25 126.7 . . ?
Pd1 C25 H25 93.0 . . ?
C25 C26 C27 105.6(8) . . ?
C25 C26 Pd1 69.6(5) . . ?
C27 C26 Pd1 101.0(6) . . ?
C25 C26 H26 127.2 . . ?
C27 C26 H26 127.2 . . ?
Pd1 C26 H26 97.5 . . ?
O2 C27 O1 119.0(8) . . ?
O2 C27 C26 130.2(9) . . ?
O1 C27 C26 110.7(8) . . ?
O3 C28 O1 118.9(9) . . ?
O3 C28 C25 132.9(10) . . ?
O1 C28 C25 108.2(8) . . ?
C301 C302 C300 102.3 . . ?
C301 C302 H30A 111.3 . . ?
C300 C302 H30A 111.3 . . ?
C301 C302 H30B 111.3 . . ?
C300 C302 H30B 111.3 . . ?
H30A C302 H30B 109.2 . . ?
O11 C301 C302 105.6 . . ?
O11 C301 H30C 110.6 . . ?
C302 C301 H30C 110.6 . . ?
O11 C301 H30D 110.6 . . ?
C302 C301 H30D 110.6 . . ?
H30C C301 H30D 108.8 . . ?
C301 O11 C305 108.2 . . ?
O11 C305 C300 108.1 . . ?
O11 C305 H30E 110.1 . . ?
C300 C305 H30E 110.1 . . ?
O11 C305 H30F 110.1 . . ?
C300 C305 H30F 110.1 . . ?
H30E C305 H30F 108.4 . . ?
C305 C300 C302 102.1 . . ?
C305 C300 H30G 111.3 . . ?
C302 C300 H30G 111.3 . . ?
C305 C300 H30H 111.3 . . ?
C302 C300 H30H 111.3 . . ?
H30G C300 H30H 109.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 N1 C1 N2 -1.6(9) . . . . ?
C4 N1 C1 N2 -173.6(7) . . . . ?
C3 N1 C1 Pd1 170.5(6) . . . . ?
C4 N1 C1 Pd1 -1.5(11) . . . . ?
C2 N2 C1 N1 0.5(9) . . . . ?
C18 N2 C1 N1 -179.3(7) . . . . ?
C2 N2 C1 Pd1 -171.2(6) . . . . ?
C18 N2 C1 Pd1 9.1(12) . . . . ?
C1 N2 C2 C3 0.9(10) . . . . ?
C18 N2 C2 C3 -179.4(8) . . . . ?
N2 C2 C3 N1 -1.8(10) . . . . ?
C1 N1 C3 C2 2.2(10) . . . . ?
C4 N1 C3 C2 174.6(7) . . . . ?
C1 N1 C4 C5 62.5(10) . . . . ?
C3 N1 C4 C5 -108.7(8) . . . . ?
N1 C4 C5 P1 -75.0(7) . . . . ?
C6 P1 C5 C4 165.6(6) . . . . ?
C12 P1 C5 C4 -86.5(6) . . . . ?
Pd1 P1 C5 C4 35.4(6) . . . . ?
C12 P1 C6 C7 -100.8(10) . . . . ?
C5 P1 C6 C7 5.3(11) . . . . ?
Pd1 P1 C6 C7 131.2(9) . . . . ?
C12 P1 C6 C11 72.7(14) . . . . ?
C5 P1 C6 C11 178.8(13) . . . . ?
Pd1 P1 C6 C11 -55.3(14) . . . . ?
C11 C6 C7 C8 8(2) . . . . ?
P1 C6 C7 C8 -178.4(8) . . . . ?
C6 C7 C8 C9 -5.5(18) . . . . ?
C7 C8 C9 C10 -4(2) . . . . ?
C8 C9 C10 C11 10(3) . . . . ?
C7 C6 C11 C10 -2(3) . . . . ?
P1 C6 C11 C10 -175(2) . . . . ?
C9 C10 C11 C6 -8(3) . . . . ?
C6 P1 C12 C17 34.4(10) . . . . ?
C5 P1 C12 C17 -75.2(9) . . . . ?
Pd1 P1 C12 C17 165.0(8) . . . . ?
C6 P1 C12 C13 -153.5(8) . . . . ?
C5 P1 C12 C13 97.0(8) . . . . ?
Pd1 P1 C12 C13 -22.9(9) . . . . ?
C17 C12 C13 C14 -2.9(14) . . . . ?
P1 C12 C13 C14 -175.4(7) . . . . ?
C12 C13 C14 C15 1.8(15) . . . . ?
C13 C14 C15 C16 -0.7(16) . . . . ?
C14 C15 C16 C17 0.9(18) . . . . ?
C13 C12 C17 C16 3.1(16) . . . . ?
P1 C12 C17 C16 175.3(9) . . . . ?
C15 C16 C17 C12 -2.1(18) . . . . ?
C1 N2 C18 C19 112.2(9) . . . . ?
C2 N2 C18 C19 -67.4(11) . . . . ?
N2 C18 C19 C20 92.7(10) . . . . ?
N2 C18 C19 C24 -88.6(10) . . . . ?
C24 C19 C20 C21 0.5(14) . . . . ?
C18 C19 C20 C21 179.2(9) . . . . ?
C19 C20 C21 C22 0.2(16) . . . . ?
C20 C21 C22 C23 0.1(18) . . . . ?
C21 C22 C23 C24 -1.1(18) . . . . ?
C22 C23 C24 C19 1.8(16) . . . . ?
C20 C19 C24 C23 -1.5(14) . . . . ?
C18 C19 C24 C23 179.8(9) . . . . ?
C28 C25 C26 C27 4.8(10) . . . . ?
Pd1 C25 C26 C27 -96.2(6) . . . . ?
C28 C25 C26 Pd1 101.0(7) . . . . ?
C28 O1 C27 O2 174.9(8) . . . . ?
C28 O1 C27 C26 -2.7(10) . . . . ?
C25 C26 C27 O2 -178.7(10) . . . . ?
Pd1 C26 C27 O2 109.6(10) . . . . ?
C25 C26 C27 O1 -1.4(10) . . . . ?
Pd1 C26 C27 O1 -73.1(7) . . . . ?
C27 O1 C28 O3 -174.0(9) . . . . ?
C27 O1 C28 C25 5.8(10) . . . . ?
C26 C25 C28 O3 173.2(11) . . . . ?
Pd1 C25 C28 O3 -112.7(12) . . . . ?
C26 C25 C28 O1 -6.6(10) . . . . ?
Pd1 C25 C28 O1 67.5(8) . . . . ?
C300 C302 C301 O11 37.0 . . . . ?
C302 C301 O11 C305 -25.9 . . . . ?
C301 O11 C305 C300 4.1 . . . . ?
O11 C305 C300 C302 18.7 . . . . ?
C301 C302 C300 C305 -32.9 . . . . ?

_refine_diff_density_max         3.144
_refine_diff_density_min         -1.309
_refine_diff_density_rms         0.193

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_yhh080
_database_code_depnum_ccdc_archive 'CCDC 1477478'
_audit_update_record             
;
2016-05-21 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         '2(C30 H29 N2 O3 P Pd), H2 O'
_chemical_formula_sum            'C60 H60 N4 O7 P2 Pd2'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         1223.86
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?


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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8121(3)
_cell_length_b                   10.9909(3)
_cell_length_c                   12.7110(3)
_cell_angle_alpha                84.157(2)
_cell_angle_beta                 69.851(2)
_cell_angle_gamma                71.348(2)
_cell_volume                     1343.53(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8342
_cell_measurement_theta_min      3.1140
_cell_measurement_theta_max      29.2077
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_F_000             626
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.787
_shelx_estimated_absorpt_T_min   0.891
_shelx_estimated_absorpt_T_max   0.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.91123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 16.0690
_diffrn_reflns_number            11796
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.120
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5780
_reflns_number_gt                4845
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.46 (release 27-08-2009 CrysAlis171 .NET)
(compiled Aug 27 2009,17:19:36)
;
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'DIAMOND (Brandenburg, 2006)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0613P)²+0.7340P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5780
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0255
_refine_ls_wR_factor_ref         0.0669
_refine_ls_wR_factor_gt          0.0643
_refine_ls_goodness_of_fit_ref   0.693
_refine_ls_restrained_S_all      0.693
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
C1 C 0.6268(2) 0.5435(2) 0.30119(17) 0.0155(4) Uani 1 1 d . . . . .
C2 C 0.7338(2) 0.6051(2) 0.40153(19) 0.0201(5) Uani 1 1 d . . . . .
H2 H 0.7470 0.6463 0.4572 0.024 Uiso 1 1 calc R U . . .
C3 C 0.8332(2) 0.5283(2) 0.31816(19) 0.0203(5) Uani 1 1 d . . . . .
H3 H 0.9301 0.5044 0.3036 0.024 Uiso 1 1 calc R U . . .
C4 C 0.8338(2) 0.4114(2) 0.15750(17) 0.0146(4) Uani 1 1 d . . . . .
C5 C 0.8359(2) 0.4700(2) 0.05446(18) 0.0159(4) Uani 1 1 d . . . . .
C6 C 0.8975(2) 0.3914(2) -0.04072(18) 0.0184(4) Uani 1 1 d . . . . .
H6 H 0.8996 0.4290 -0.1117 0.022 Uiso 1 1 calc R U . . .
C7 C 0.9560(2) 0.2598(2) -0.03481(19) 0.0202(5) Uani 1 1 d . . . . .
C8 C 0.9518(2) 0.2056(2) 0.06939(19) 0.0205(5) Uani 1 1 d . . . . .
H8 H 0.9918 0.1155 0.0741 0.025 Uiso 1 1 calc R U . . .
C9 C 0.8905(2) 0.2796(2) 0.16721(18) 0.0177(4) Uani 1 1 d . . . . .
C10 C 0.8850(3) 0.2174(2) 0.2794(2) 0.0270(5) Uani 1 1 d . . . . .
H10A H 0.9494 0.2388 0.3075 0.040 Uiso 1 1 calc R U . . .
H10B H 0.9111 0.1240 0.2712 0.040 Uiso 1 1 calc R U . . .
H10C H 0.7909 0.2489 0.3326 0.040 Uiso 1 1 calc R U . . .
C11 C 0.7759(2) 0.6122(2) 0.04417(19) 0.0206(5) Uani 1 1 d . . . . .
H11A H 0.8212 0.6392 -0.0314 0.031 Uiso 1 1 calc R U . . .
H11B H 0.7910 0.6569 0.0994 0.031 Uiso 1 1 calc R U . . .
H11C H 0.6765 0.6336 0.0577 0.031 Uiso 1 1 calc R U . . .
C12 C 1.0259(3) 0.1775(2) -0.1401(2) 0.0290(5) Uani 1 1 d . . . . .
H12A H 1.1144 0.1178 -0.1378 0.044 Uiso 1 1 calc R U . . .
H12B H 1.0423 0.2326 -0.2059 0.044 Uiso 1 1 calc R U . . .
H12C H 0.9663 0.1287 -0.1448 0.044 Uiso 1 1 calc R U . . .
C13 C 0.4736(2) 0.6958(2) 0.45864(18) 0.0209(5) Uani 1 1 d . . . . .
H13A H 0.4842 0.7328 0.5217 0.025 Uiso 1 1 calc R U . . .
H13B H 0.4090 0.6445 0.4903 0.025 Uiso 1 1 calc R U . . .
C14 C 0.4139(2) 0.8042(2) 0.38765(18) 0.0193(5) Uani 1 1 d . . . . .
H14A H 0.4862 0.8439 0.3437 0.023 Uiso 1 1 calc R U . . .
H14B H 0.3365 0.8711 0.4376 0.023 Uiso 1 1 calc R U . . .
C15 C 0.3446(2) 0.8674(2) 0.18407(17) 0.0148(4) Uani 1 1 d . . . . .
C16 C 0.3445(2) 0.9914(2) 0.19777(19) 0.0221(5) Uani 1 1 d . . . . .
H16 H 0.3550 1.0138 0.2637 0.027 Uiso 1 1 calc R U . . .
C17 C 0.3290(3) 1.0825(2) 0.1152(2) 0.0265(5) Uani 1 1 d . . . . .
H17 H 0.3289 1.1671 0.1249 0.032 Uiso 1 1 calc R U . . .
C18 C 0.3138(2) 1.0506(2) 0.0192(2) 0.0236(5) Uani 1 1 d . . . . .
H18 H 0.3030 1.1132 -0.0369 0.028 Uiso 1 1 calc R U . . .
C19 C 0.3143(2) 0.9272(2) 0.00468(19) 0.0237(5) Uani 1 1 d . . . . .
H19 H 0.3037 0.9053 -0.0614 0.028 Uiso 1 1 calc R U . . .
C20 C 0.3302(2) 0.8355(2) 0.08667(18) 0.0201(5) Uani 1 1 d . . . . .
H20 H 0.3313 0.7508 0.0762 0.024 Uiso 1 1 calc R U . . .
C21 C 0.1690(2) 0.7692(2) 0.37137(17) 0.0152(4) Uani 1 1 d . . . . .
C22 C 0.0690(2) 0.8875(2) 0.37572(19) 0.0216(5) Uani 1 1 d . . . . .
H22 H 0.0948 0.9580 0.3350 0.026 Uiso 1 1 calc R U . . .
C23 C -0.0683(2) 0.9030(2) 0.4395(2) 0.0257(5) Uani 1 1 d . . . . .
H23 H -0.1365 0.9834 0.4406 0.031 Uiso 1 1 calc R U . . .
C24 C -0.1065(2) 0.8021(2) 0.50116(18) 0.0230(5) Uani 1 1 d . . . . .
H24 H -0.2001 0.8137 0.5462 0.028 Uiso 1 1 calc R U . . .
C25 C -0.0083(2) 0.6844(2) 0.49726(19) 0.0247(5) Uani 1 1 d . . . . .
H25 H -0.0344 0.6149 0.5397 0.030 Uiso 1 1 calc R U . . .
C26 C 0.1287(2) 0.6671(2) 0.43142(18) 0.0216(5) Uani 1 1 d . . . . .
H26 H 0.1953 0.5852 0.4273 0.026 Uiso 1 1 calc R U . . .
C27 C 0.4029(2) 0.4385(2) 0.15078(17) 0.0169(4) Uani 1 1 d . . . . .
H27 H 0.3942 0.4683 0.0759 0.020 Uiso 1 1 calc R U . . .
C28 C 0.5324(2) 0.3571(2) 0.16157(18) 0.0184(4) Uani 1 1 d . . . . .
H28 H 0.6168 0.3281 0.0941 0.022 Uiso 1 1 calc R U . . .
C30 C 0.2939(2) 0.4000(2) 0.23739(18) 0.0197(5) Uani 1 1 d . . . . .
C31 C 0.4993(2) 0.2702(2) 0.2539(2) 0.0236(5) Uani 1 1 d . . . . .
N1 N 0.60832(18) 0.61246(17) 0.39056(15) 0.0171(4) Uani 1 1 d . . . . .
N2 N 0.76628(18) 0.49080(17) 0.25734(14) 0.0154(4) Uani 1 1 d . . . . .
O1 O 0.35414(17) 0.30413(16) 0.30289(13) 0.0234(3) Uani 1 1 d . . . . .
O2 O 0.17020(16) 0.43340(18) 0.26018(13) 0.0276(4) Uani 1 1 d . . . . .
O3 O 0.5702(2) 0.18097(17) 0.29100(16) 0.0368(5) Uani 1 1 d . . . . .
P1 P 0.35131(5) 0.74444(5) 0.29120(4) 0.01381(11) Uani 1 1 d . . . . .
Pd1 Pd 0.47859(2) 0.53617(2) 0.23862(2) 0.01332(6) Uani 1 1 d . . . . .
O4 O 0.6066(10) 0.9618(7) 0.4242(13) 0.214(7) Uani 0.5 1 d . . P . .
H4A H 0.6451 0.9380 0.3621 0.256 Uiso 0.5 1 d . U P . .
H4B H 0.5799 0.9213 0.5024 0.256 Uiso 0.5 1 d . U P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 N1 1.351(3) . ?
C1 N2 1.359(3) . ?
C1 Pd1 2.0450(19) . ?
C2 C3 1.344(3) . ?
C2 N1 1.388(3) . ?
C2 H2 0.9500 . ?
C3 N2 1.390(3) . ?
C3 H3 0.9500 . ?
C4 C9 1.391(3) . ?
C4 C5 1.396(3) . ?
C4 N2 1.444(3) . ?
C5 C6 1.394(3) . ?
C5 C11 1.500(3) . ?
C6 C7 1.386(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.388(3) . ?
C7 C12 1.515(3) . ?
C8 C9 1.393(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.508(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 N1 1.466(3) . ?
C13 C14 1.529(3) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 P1 1.847(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.390(3) . ?
C15 C20 1.391(3) . ?
C15 P1 1.821(2) . ?
C16 C17 1.390(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.378(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.385(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.389(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.392(3) . ?
C21 C26 1.392(3) . ?
C21 P1 1.824(2) . ?
C22 C23 1.389(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.381(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.378(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.389(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.445(3) . ?
C27 C30 1.452(3) . ?
C27 Pd1 2.122(2) . ?
C27 H27 1.0000 . ?
C28 C31 1.455(3) . ?
C28 Pd1 2.107(2) . ?
C28 H28 1.0000 . ?
C30 O2 1.204(3) . ?
C30 O1 1.408(3) . ?
C31 O3 1.202(3) . ?
C31 O1 1.411(3) . ?
P1 Pd1 2.2897(6) . ?
O4 H4A 0.7812 . ?
O4 H4B 1.0317 . ?

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
N1 C1 N2 104.29(17) . . ?
N1 C1 Pd1 127.18(15) . . ?
N2 C1 Pd1 128.28(15) . . ?
C3 C2 N1 106.73(18) . . ?
C3 C2 H2 126.6 . . ?
N1 C2 H2 126.6 . . ?
C2 C3 N2 106.57(18) . . ?
C2 C3 H3 126.7 . . ?
N2 C3 H3 126.7 . . ?
C9 C4 C5 122.4(2) . . ?
C9 C4 N2 119.35(19) . . ?
C5 C4 N2 118.26(19) . . ?
C6 C5 C4 117.5(2) . . ?
C6 C5 C11 120.24(19) . . ?
C4 C5 C11 122.2(2) . . ?
C7 C6 C5 121.9(2) . . ?
C7 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C6 C7 C8 118.6(2) . . ?
C6 C7 C12 120.7(2) . . ?
C8 C7 C12 120.7(2) . . ?
C7 C8 C9 121.8(2) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
C4 C9 C8 117.8(2) . . ?
C4 C9 C10 121.7(2) . . ?
C8 C9 C10 120.5(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C5 C11 H11A 109.5 . . ?
C5 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C5 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C7 C12 H12A 109.5 . . ?
C7 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C7 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N1 C13 C14 110.54(18) . . ?
N1 C13 H13A 109.5 . . ?
C14 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 108.1 . . ?
C13 C14 P1 111.43(15) . . ?
C13 C14 H14A 109.3 . . ?
P1 C14 H14A 109.3 . . ?
C13 C14 H14B 109.3 . . ?
P1 C14 H14B 109.3 . . ?
H14A C14 H14B 108.0 . . ?
C16 C15 C20 119.3(2) . . ?
C16 C15 P1 123.65(16) . . ?
C20 C15 P1 116.90(16) . . ?
C15 C16 C17 120.1(2) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C18 C17 C16 120.3(2) . . ?
C18 C17 H17 119.9 . . ?
C16 C17 H17 119.9 . . ?
C17 C18 C19 120.0(2) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 120.1(2) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C19 C20 C15 120.2(2) . . ?
C19 C20 H20 119.9 . . ?
C15 C20 H20 119.9 . . ?
C22 C21 C26 118.9(2) . . ?
C22 C21 P1 122.00(16) . . ?
C26 C21 P1 119.09(17) . . ?
C23 C22 C21 120.2(2) . . ?
C23 C22 H22 119.9 . . ?
C21 C22 H22 119.9 . . ?
C24 C23 C22 120.4(2) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C25 C24 C23 119.9(2) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 120.1(2) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C21 120.5(2) . . ?
C25 C26 H26 119.8 . . ?
C21 C26 H26 119.8 . . ?
C28 C27 C30 106.69(19) . . ?
C28 C27 Pd1 69.47(11) . . ?
C30 C27 Pd1 104.57(13) . . ?
C28 C27 H27 121.4 . . ?
C30 C27 H27 121.4 . . ?
Pd1 C27 H27 121.4 . . ?
C27 C28 C31 107.11(19) . . ?
C27 C28 Pd1 70.59(12) . . ?
C31 C28 Pd1 104.83(14) . . ?
C27 C28 H28 121.1 . . ?
C31 C28 H28 121.1 . . ?
Pd1 C28 H28 121.1 . . ?
O2 C30 O1 118.5(2) . . ?
O2 C30 C27 132.7(2) . . ?
O1 C30 C27 108.82(18) . . ?
O3 C31 O1 119.2(2) . . ?
O3 C31 C28 132.5(2) . . ?
O1 C31 C28 108.32(19) . . ?
C1 N1 C2 111.34(18) . . ?
C1 N1 C13 123.72(17) . . ?
C2 N1 C13 124.59(17) . . ?
C1 N2 C3 111.07(18) . . ?
C1 N2 C4 123.47(16) . . ?
C3 N2 C4 125.40(17) . . ?
C30 O1 C31 108.66(17) . . ?
C15 P1 C21 102.76(9) . . ?
C15 P1 C14 104.19(10) . . ?
C21 P1 C14 102.95(10) . . ?
C15 P1 Pd1 119.28(7) . . ?
C21 P1 Pd1 115.10(7) . . ?
C14 P1 Pd1 110.80(7) . . ?
C1 Pd1 C28 111.05(8) . . ?
C1 Pd1 C27 150.97(9) . . ?
C28 Pd1 C27 39.94(8) . . ?
C1 Pd1 P1 92.06(6) . . ?
C28 Pd1 P1 156.74(6) . . ?
C27 Pd1 P1 116.86(6) . . ?
H4A O4 H4B 137.4 . . ?

_refine_diff_density_max         0.480
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.074

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jss458a
_database_code_depnum_ccdc_archive 'CCDC 1477479'
_audit_update_record             
;
2016-05-21 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C27 H23 N2 O3 P Pd, 2(C H Cl3)'
_chemical_formula_sum            'C29 H25 Cl6 N2 O3 P Pd'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         799.58
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4095(18)
_cell_length_b                   14.834(3)
_cell_length_c                   22.083(4)
_cell_angle_alpha                87.766(12)
_cell_angle_beta                 88.760(11)
_cell_angle_gamma                76.094(11)
_cell_volume                     3307.2(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    3749
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      20.5
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_F_000             1600
_exptl_transmission_factor_min   0.816
_exptl_transmission_factor_max   0.873
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    1.128
_shelx_estimated_absorpt_T_min   0.806
_shelx_estimated_absorpt_T_max   0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39141
_diffrn_reflns_av_unetI/netI     0.1475
_diffrn_reflns_av_R_equivalents  0.1363
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.016
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12981
_reflns_number_gt                6875
_reflns_threshold_expression     I>2σ
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'DIAMOND (Brandenburg, 2006)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1601P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12981
_refine_ls_number_parameters     759
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1716
_refine_ls_R_factor_gt           0.0966
_refine_ls_wR_factor_ref         0.2863
_refine_ls_wR_factor_gt          0.2361
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001

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
Pd2 Pd 0.57483(7) 1.07400(5) 0.12688(3) 0.0469(2) Uani 1 1 d . . . . .
P2 P 0.6615(2) 0.92715(16) 0.16790(10) 0.0438(5) Uani 1 1 d . . . . .
Pd1 Pd 0.95459(7) 0.37027(5) 0.38981(3) 0.0555(3) Uani 1 1 d . . . . .
P1 P 0.8762(2) 0.49967(17) 0.32747(11) 0.0477(6) Uani 1 1 d . . . . .
C4 C 1.1120(10) 0.4090(8) 0.4283(4) 0.061(3) Uani 1 1 d . . . . .
C11 C 0.9833(8) 0.5787(7) 0.3130(4) 0.047(2) Uani 1 1 d . . . . .
C6 C 1.0397(9) 0.6121(7) 0.3623(4) 0.055(3) Uani 1 1 d . . . . .
C10 C 1.0111(9) 0.6078(8) 0.2550(5) 0.063(3) Uani 1 1 d . . . . .
H10 H 0.9747 0.5859 0.2211 0.076 Uiso 1 1 calc R U . . .
C5 C 1.0179(8) 0.5795(7) 0.4269(4) 0.054(2) Uani 1 1 d . . . . .
H5A H 1.0225 0.6291 0.4549 0.065 Uiso 1 1 calc R U . . .
H5B H 0.9285 0.5675 0.4308 0.065 Uiso 1 1 calc R U . . .
C9 C 1.0930(10) 0.6694(9) 0.2465(5) 0.072(3) Uani 1 1 d . . . . .
H9 H 1.1124 0.6888 0.2065 0.086 Uiso 1 1 calc R U . . .
C8 C 1.1449(10) 0.7018(9) 0.2941(5) 0.073(3) Uani 1 1 d . . . . .
H8 H 1.1999 0.7439 0.2874 0.088 Uiso 1 1 calc R U . . .
C3 C 1.2316(11) 0.4972(11) 0.4717(5) 0.075(3) Uani 1 1 d . . . . .
H3 H 1.2568 0.5502 0.4857 0.090 Uiso 1 1 calc R U . . .
C1 C 1.2679(13) 0.2554(9) 0.4470(7) 0.100(5) Uani 1 1 d . . . . .
H1A H 1.2207 0.2274 0.4785 0.149 Uiso 1 1 calc R U . . .
H1B H 1.3634 0.2354 0.4539 0.149 Uiso 1 1 calc R U . . .
H1C H 1.2479 0.2357 0.4072 0.149 Uiso 1 1 calc R U . . .
C2 C 1.3002(11) 0.4100(12) 0.4753(5) 0.084(4) Uani 1 1 d . . . . .
H2 H 1.3853 0.3888 0.4927 0.101 Uiso 1 1 calc R U . . .
C7 C 1.1183(9) 0.6739(8) 0.3529(5) 0.061(3) Uani 1 1 d . . . . .
H7 H 1.1542 0.6974 0.3864 0.073 Uiso 1 1 calc R U . . .
N2 N 1.1166(7) 0.4953(6) 0.4437(3) 0.054(2) Uani 1 1 d . . . . .
N1 N 1.2271(9) 0.3534(8) 0.4490(4) 0.074(3) Uani 1 1 d . . . . .
C19 C 0.7052(9) 0.6695(7) 0.3601(4) 0.055(2) Uani 1 1 d . . . . .
H19 H 0.7766 0.6973 0.3503 0.066 Uiso 1 1 calc R U . . .
C18 C 0.7211(8) 0.5763(7) 0.3521(4) 0.050(2) Uani 1 1 d . . . . .
C20 C 0.5873(10) 0.7244(8) 0.3820(5) 0.066(3) Uani 1 1 d . . . . .
H20 H 0.5772 0.7889 0.3879 0.079 Uiso 1 1 calc R U . . .
C23 C 0.6157(9) 0.5368(8) 0.3667(4) 0.060(3) Uani 1 1 d . . . . .
H23 H 0.6273 0.4717 0.3631 0.073 Uiso 1 1 calc R U . . .
C22 C 0.4960(9) 0.5884(8) 0.3862(5) 0.072(3) Uani 1 1 d . . . . .
H22 H 0.4237 0.5605 0.3932 0.086 Uiso 1 1 calc R U . . .
C21 C 0.4822(9) 0.6803(8) 0.3955(5) 0.063(3) Uani 1 1 d . . . . .
H21 H 0.4008 0.7158 0.4112 0.075 Uiso 1 1 calc R U . . .
C12 C 0.8427(9) 0.4680(7) 0.2518(4) 0.054(2) Uani 1 1 d . . . . .
C13 C 0.9126(12) 0.3841(8) 0.2306(5) 0.071(3) Uani 1 1 d . . . . .
H13 H 0.9747 0.3433 0.2561 0.086 Uiso 1 1 calc R U . . .
C17 C 0.7486(12) 0.5239(9) 0.2151(5) 0.071(3) Uani 1 1 d . . . . .
H17 H 0.6961 0.5807 0.2295 0.086 Uiso 1 1 calc R U . . .
C15 C 0.8011(15) 0.4136(11) 0.1376(6) 0.089(4) Uani 1 1 d . . . . .
H15 H 0.7846 0.3940 0.0987 0.107 Uiso 1 1 calc R U . . .
C14 C 0.8935(16) 0.3586(10) 0.1726(6) 0.090(4) Uani 1 1 d . . . . .
H14 H 0.9458 0.3021 0.1576 0.108 Uiso 1 1 calc R U . . .
C16 C 0.7307(14) 0.4969(11) 0.1571(5) 0.089(4) Uani 1 1 d . . . . .
H16 H 0.6692 0.5369 0.1309 0.107 Uiso 1 1 calc R U . . .
C24 C 0.9517(13) 0.2303(8) 0.4132(5) 0.074(3) Uani 1 1 d . . . . .
H24 H 1.0375 0.2061 0.3967 0.089 Uiso 1 1 calc R U . . .
C25 C 0.8367(11) 0.2719(8) 0.3804(5) 0.068(3) Uani 1 1 d . . . . .
H25 H 0.8295 0.2827 0.3377 0.082 Uiso 1 1 calc R U . . .
C26 C 0.7313(15) 0.2946(9) 0.4257(7) 0.086(4) Uani 1 1 d . . . . .
C27 C 0.9151(15) 0.2314(8) 0.4765(6) 0.081(4) Uani 1 1 d . . . . .
O1 O 0.7831(10) 0.2756(6) 0.4824(4) 0.089(3) Uani 1 1 d . . . . .
O2 O 0.6115(10) 0.3275(7) 0.4211(5) 0.108(3) Uani 1 1 d . . . . .
O3 O 0.9779(11) 0.2001(7) 0.5210(5) 0.110(3) Uani 1 1 d . . . . .
C31 C 0.4121(8) 1.0517(6) 0.0833(4) 0.051(2) Uani 1 1 d . . . . .
C38 C 0.5551(8) 0.8446(6) 0.1689(4) 0.047(2) Uani 1 1 d . . . . .
C37 C 0.5368(8) 0.7930(6) 0.2222(4) 0.049(2) Uani 1 1 d . . . . .
H37 H 0.5769 0.8030 0.2588 0.059 Uiso 1 1 calc R U . . .
C33 C 0.4936(8) 0.8300(6) 0.1162(4) 0.046(2) Uani 1 1 d . . . . .
C36 C 0.4622(10) 0.7292(8) 0.2216(5) 0.065(3) Uani 1 1 d . . . . .
H36 H 0.4507 0.6950 0.2578 0.078 Uiso 1 1 calc R U . . .
C32 C 0.5049(9) 0.8862(6) 0.0584(4) 0.048(2) Uani 1 1 d . . . . .
H32A H 0.5931 0.9003 0.0562 0.058 Uiso 1 1 calc R U . . .
H32B H 0.4966 0.8491 0.0230 0.058 Uiso 1 1 calc R U . . .
C30 C 0.2813(9) 0.9833(8) 0.0287(5) 0.060(3) Uani 1 1 d . . . . .
H30 H 0.2526 0.9381 0.0068 0.072 Uiso 1 1 calc R U . . .
C34 C 0.4195(9) 0.7648(7) 0.1169(4) 0.056(2) Uani 1 1 d . . . . .
H34 H 0.3781 0.7541 0.0809 0.067 Uiso 1 1 calc R U . . .
C29 C 0.2133(10) 1.0683(8) 0.0392(5) 0.064(3) Uani 1 1 d . . . . .
H29 H 0.1259 1.0962 0.0262 0.077 Uiso 1 1 calc R U . . .
C35 C 0.4044(10) 0.7143(8) 0.1700(5) 0.067(3) Uani 1 1 d . . . . .
H35 H 0.3532 0.6692 0.1699 0.080 Uiso 1 1 calc R U . . .
C28 C 0.2544(11) 1.2061(8) 0.0904(7) 0.085(4) Uani 1 1 d . . . . .
H28A H 0.2906 1.2115 0.1303 0.127 Uiso 1 1 calc R U . . .
H28B H 0.1577 1.2266 0.0922 0.127 Uiso 1 1 calc R U . . .
H28C H 0.2892 1.2450 0.0605 0.127 Uiso 1 1 calc R U . . .
N4 N 0.4026(7) 0.9728(5) 0.0559(3) 0.0478(18) Uani 1 1 d . . . . .
N3 N 0.2930(8) 1.1091(6) 0.0726(4) 0.058(2) Uani 1 1 d . . . . .
C39 C 0.8135(8) 0.8586(6) 0.1337(4) 0.048(2) Uani 1 1 d . . . . .
C44 C 0.9140(9) 0.9026(7) 0.1226(5) 0.065(3) Uani 1 1 d . . . . .
H44 H 0.9040 0.9648 0.1344 0.078 Uiso 1 1 calc R U . . .
C40 C 0.8311(9) 0.7686(7) 0.1171(5) 0.063(3) Uani 1 1 d . . . . .
H40 H 0.7643 0.7363 0.1263 0.076 Uiso 1 1 calc R U . . .
C42 C 1.0451(10) 0.7687(10) 0.0748(5) 0.077(3) Uani 1 1 d . . . . .
H42 H 1.1229 0.7388 0.0534 0.092 Uiso 1 1 calc R U . . .
C41 C 0.9461(10) 0.7237(8) 0.0866(6) 0.074(3) Uani 1 1 d . . . . .
H41 H 0.9559 0.6619 0.0741 0.089 Uiso 1 1 calc R U . . .
C46 C 0.8075(11) 0.8746(8) 0.2746(5) 0.063(3) Uani 1 1 d . . . . .
H46 H 0.8663 0.8289 0.2517 0.076 Uiso 1 1 calc R U . . .
C45 C 0.7018(9) 0.9327(7) 0.2464(4) 0.052(2) Uani 1 1 d . . . . .
C50 C 0.6213(14) 0.9992(10) 0.2817(6) 0.096(4) Uani 1 1 d . . . . .
H50 H 0.5449 1.0397 0.2646 0.115 Uiso 1 1 calc R U . . .
C47 C 0.8308(13) 0.8809(10) 0.3357(5) 0.081(3) Uani 1 1 d . . . . .
H47 H 0.9012 0.8372 0.3551 0.098 Uiso 1 1 calc R U . . .
C49 C 0.651(2) 1.0073(14) 0.3415(8) 0.136(7) Uani 1 1 d . . . . .
H49 H 0.5971 1.0553 0.3645 0.163 Uiso 1 1 calc R U . . .
C51 C 0.5744(10) 1.2164(7) 0.1303(5) 0.055(2) Uani 1 1 d . . . . .
H51 H 0.4907 1.2321 0.1504 0.066 Uiso 1 1 calc R U . . .
C54 C 0.6024(11) 1.2437(7) 0.0702(5) 0.063(3) Uani 1 1 d . . . . .
C52 C 0.6928(10) 1.1618(7) 0.1550(5) 0.061(3) Uani 1 1 d . . . . .
H52 H 0.7120 1.1650 0.1989 0.073 Uiso 1 1 calc R U . . .
C53 C 0.7949(12) 1.1612(8) 0.1099(6) 0.069(3) Uani 1 1 d . . . . .
O4 O 0.7361(7) 1.2046(5) 0.0562(3) 0.068(2) Uani 1 1 d . . . . .
C48 C 0.7535(16) 0.9488(13) 0.3673(6) 0.105(5) Uani 1 1 d . . . . .
H48 H 0.7723 0.9552 0.4086 0.125 Uiso 1 1 calc R U . . .
C43 C 1.0308(10) 0.8564(9) 0.0939(6) 0.076(3) Uani 1 1 d . . . . .
H43 H 1.1009 0.8867 0.0878 0.091 Uiso 1 1 calc R U . . .
O6 O 0.5356(9) 1.2921(5) 0.0309(4) 0.083(2) Uani 1 1 d . . . . .
O5 O 0.9142(7) 1.1298(6) 0.1100(4) 0.084(3) Uani 1 1 d . . . . .
C56 C 0.4381(14) 0.3506(10) 0.3028(6) 0.095(4) Uani 1 1 d . . . . .
H56 H 0.4719 0.3507 0.3449 0.113 Uiso 1 1 calc R U . . .
Cl4 Cl 0.5524(5) 0.3760(5) 0.2524(2) 0.162(3) Uani 1 1 d . . . . .
Cl5 Cl 0.2933(7) 0.4297(7) 0.2967(3) 0.255(5) Uani 1 1 d . . . . .
Cl7 Cl 0.1768(8) 0.1459(5) 0.2545(4) 0.187(3) Uani 1 1 d . . . . .
Cl3 Cl 0.2570(10) 0.4597(5) 0.1341(3) 0.233(4) Uani 1 1 d . . . . .
Cl10 Cl 0.5987(8) 0.0911(6) 0.5128(4) 0.233(4) Uani 1 1 d . . . . .
Cl1 Cl 0.3429(5) 0.5609(3) 0.0351(2) 0.1250(15) Uani 1 1 d . . . . .
Cl11 Cl 0.6997(10) 0.0632(8) 0.6310(3) 0.284(6) Uani 1 1 d . . . . .
C57 C 0.1050(13) 0.0614(11) 0.2252(8) 0.102(4) Uani 1 1 d . . . . .
H57 H 0.0642 0.0867 0.1856 0.122 Uiso 1 1 calc R U . . .
Cl9 Cl 0.2201(6) -0.0356(5) 0.2114(3) 0.177(3) Uani 1 1 d . . . . .
Cl12 Cl 0.8525(7) -0.0125(5) 0.5312(4) 0.191(3) Uani 1 1 d . . . . .
Cl6 Cl 0.4199(12) 0.2445(6) 0.2895(4) 0.301(7) Uani 1 1 d . . . . .
Cl8 Cl -0.0175(5) 0.0520(6) 0.2730(3) 0.186(3) Uani 1 1 d . . . . .
C55 C 0.3000(14) 0.4600(9) 0.0572(7) 0.096(4) Uani 1 1 d . . . . .
H55 H 0.3742 0.4051 0.0485 0.116 Uiso 1 1 calc R U . . .
Cl2 Cl 0.1636(8) 0.4556(5) 0.0176(4) 0.236(4) Uani 1 1 d . . . . .
C62 C 0.743(2) 0.0740(14) 0.5575(11) 0.180(11) Uani 1 1 d . . . . .
H62 H 0.7785 0.1309 0.5524 0.216 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Pd2 C31 2.067(10) . ?
Pd2 C52 2.111(10) . ?
Pd2 C51 2.116(9) . ?
Pd2 P2 2.306(2) . ?
P2 C45 1.803(10) . ?
P2 C39 1.828(8) . ?
P2 C38 1.838(9) . ?
Pd1 C4 2.071(11) . ?
Pd1 C24 2.127(12) . ?
Pd1 C25 2.139(11) . ?
Pd1 P1 2.310(3) . ?
P1 C12 1.817(10) . ?
P1 C11 1.818(9) . ?
P1 C18 1.822(9) . ?
C4 N2 1.349(14) . ?
C4 N1 1.358(14) . ?
C11 C10 1.382(12) . ?
C11 C6 1.410(13) . ?
C6 C7 1.375(12) . ?
C6 C5 1.517(12) . ?
C10 C9 1.398(14) . ?
C10 H10 0.9500 . ?
C5 N2 1.455(13) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C9 C8 1.347(16) . ?
C9 H9 0.9500 . ?
C8 C7 1.390(15) . ?
C8 H8 0.9500 . ?
C3 C2 1.320(18) . ?
C3 N2 1.366(14) . ?
C3 H3 0.9500 . ?
C1 N1 1.415(16) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 N1 1.409(17) . ?
C2 H2 0.9500 . ?
C7 H7 0.9500 . ?
C19 C18 1.371(13) . ?
C19 C20 1.388(13) . ?
C19 H19 0.9500 . ?
C18 C23 1.389(12) . ?
C20 C21 1.425(13) . ?
C20 H20 0.9500 . ?
C23 C22 1.367(14) . ?
C23 H23 0.9500 . ?
C22 C21 1.358(15) . ?
C22 H22 0.9500 . ?
C21 H21 0.9500 . ?
C12 C13 1.375(14) . ?
C12 C17 1.376(16) . ?
C13 C14 1.381(18) . ?
C13 H13 0.9500 . ?
C17 C16 1.388(16) . ?
C17 H17 0.9500 . ?
C15 C14 1.34(2) . ?
C15 C16 1.357(19) . ?
C15 H15 0.9500 . ?
C14 H14 0.9500 . ?
C16 H16 0.9500 . ?
C24 C25 1.409(17) . ?
C24 C27 1.441(16) . ?
C24 H24 0.9500 . ?
C25 C26 1.456(16) . ?
C25 H25 0.9500 . ?
C26 O2 1.230(16) . ?
C26 O1 1.366(17) . ?
C27 O3 1.206(16) . ?
C27 O1 1.378(16) . ?
C31 N3 1.344(12) . ?
C31 N4 1.363(12) . ?
C38 C33 1.389(13) . ?
C38 C37 1.414(11) . ?
C37 C36 1.362(13) . ?
C37 H37 0.9500 . ?
C33 C34 1.374(12) . ?
C33 C32 1.515(12) . ?
C36 C35 1.350(15) . ?
C36 H36 0.9500 . ?
C32 N4 1.459(11) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C30 C29 1.315(14) . ?
C30 N4 1.383(13) . ?
C30 H30 0.9500 . ?
C34 C35 1.393(13) . ?
C34 H34 0.9500 . ?
C29 N3 1.379(14) . ?
C29 H29 0.9500 . ?
C35 H35 0.9500 . ?
C28 N3 1.464(14) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C39 C40 1.368(13) . ?
C39 C44 1.373(12) . ?
C44 C43 1.395(13) . ?
C44 H44 0.9500 . ?
C40 C41 1.395(13) . ?
C40 H40 0.9500 . ?
C42 C43 1.357(16) . ?
C42 C41 1.371(15) . ?
C42 H42 0.9500 . ?
C41 H41 0.9500 . ?
C46 C45 1.368(15) . ?
C46 C47 1.388(16) . ?
C46 H46 0.9500 . ?
C45 C50 1.385(14) . ?
C50 C49 1.38(2) . ?
C50 H50 0.9500 . ?
C47 C48 1.338(19) . ?
C47 H47 0.9500 . ?
C49 C48 1.33(2) . ?
C49 H49 0.9500 . ?
C51 C52 1.410(15) . ?
C51 C54 1.417(15) . ?
C51 H51 0.9500 . ?
C54 O6 1.220(14) . ?
C54 O4 1.406(13) . ?
C52 C53 1.439(14) . ?
C52 H52 1.0000 . ?
C53 O5 1.217(13) . ?
C53 O4 1.406(15) . ?
C48 H48 0.9500 . ?
C43 H43 0.9500 . ?
C56 Cl6 1.667(15) . ?
C56 Cl5 1.678(16) . ?
C56 Cl4 1.710(12) . ?
C56 H56 1.0000 . ?
Cl7 C57 1.755(16) . ?
Cl3 C55 1.745(17) . ?
Cl10 C62 1.78(3) . ?
Cl1 C55 1.713(14) . ?
Cl11 C62 1.69(2) . ?
C57 Cl8 1.666(14) . ?
C57 Cl9 1.671(16) . ?
C57 H57 1.0000 . ?
Cl12 C62 1.615(18) . ?
C55 Cl2 1.701(15) . ?
C55 H55 1.0000 . ?
C62 H62 1.0000 . ?

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
C31 Pd2 C52 151.7(4) . . ?
C31 Pd2 C51 113.0(4) . . ?
C52 Pd2 C51 39.0(4) . . ?
C31 Pd2 P2 100.2(3) . . ?
C52 Pd2 P2 107.9(3) . . ?
C51 Pd2 P2 145.2(3) . . ?
C45 P2 C39 104.4(4) . . ?
C45 P2 C38 103.9(4) . . ?
C39 P2 C38 101.4(4) . . ?
C45 P2 Pd2 110.6(3) . . ?
C39 P2 Pd2 117.6(3) . . ?
C38 P2 Pd2 117.2(3) . . ?
C4 Pd1 C24 112.2(5) . . ?
C4 Pd1 C25 150.5(5) . . ?
C24 Pd1 C25 38.6(4) . . ?
C4 Pd1 P1 99.5(3) . . ?
C24 Pd1 P1 147.3(4) . . ?
C25 Pd1 P1 110.0(3) . . ?
C12 P1 C11 102.9(4) . . ?
C12 P1 C18 104.4(5) . . ?
C11 P1 C18 103.2(4) . . ?
C12 P1 Pd1 111.7(3) . . ?
C11 P1 Pd1 117.7(3) . . ?
C18 P1 Pd1 115.4(3) . . ?
N2 C4 N1 104.6(10) . . ?
N2 C4 Pd1 126.9(8) . . ?
N1 C4 Pd1 128.2(10) . . ?
C10 C11 C6 118.5(8) . . ?
C10 C11 P1 122.2(8) . . ?
C6 C11 P1 119.3(6) . . ?
C7 C6 C11 120.6(9) . . ?
C7 C6 C5 118.3(9) . . ?
C11 C6 C5 121.1(8) . . ?
C11 C10 C9 119.9(11) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
N2 C5 C6 111.3(7) . . ?
N2 C5 H5A 109.4 . . ?
C6 C5 H5A 109.4 . . ?
N2 C5 H5B 109.4 . . ?
C6 C5 H5B 109.4 . . ?
H5A C5 H5B 108.0 . . ?
C8 C9 C10 120.9(10) . . ?
C8 C9 H9 119.5 . . ?
C10 C9 H9 119.5 . . ?
C9 C8 C7 120.4(9) . . ?
C9 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C2 C3 N2 105.4(12) . . ?
C2 C3 H3 127.3 . . ?
N2 C3 H3 127.3 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 N1 109.0(11) . . ?
C3 C2 H2 125.5 . . ?
N1 C2 H2 125.5 . . ?
C6 C7 C8 119.6(10) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C4 N2 C3 112.8(10) . . ?
C4 N2 C5 124.5(8) . . ?
C3 N2 C5 122.4(10) . . ?
C4 N1 C2 108.1(11) . . ?
C4 N1 C1 127.3(12) . . ?
C2 N1 C1 124.6(12) . . ?
C18 C19 C20 121.7(8) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C19 C18 C23 118.4(8) . . ?
C19 C18 P1 123.6(6) . . ?
C23 C18 P1 117.9(8) . . ?
C19 C20 C21 117.4(10) . . ?
C19 C20 H20 121.3 . . ?
C21 C20 H20 121.3 . . ?
C22 C23 C18 122.2(10) . . ?
C22 C23 H23 118.9 . . ?
C18 C23 H23 118.9 . . ?
C21 C22 C23 119.0(9) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C22 C21 C20 121.3(9) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C13 C12 C17 118.6(10) . . ?
C13 C12 P1 118.8(9) . . ?
C17 C12 P1 122.6(8) . . ?
C12 C13 C14 120.7(13) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C12 C17 C16 119.8(12) . . ?
C12 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C14 C15 C16 120.8(13) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C15 C14 C13 119.9(13) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C15 C16 C17 120.1(14) . . ?
C15 C16 H16 120.0 . . ?
C17 C16 H16 120.0 . . ?
C25 C24 C27 107.4(11) . . ?
C25 C24 Pd1 71.2(7) . . ?
C27 C24 Pd1 104.6(7) . . ?
C25 C24 H24 126.3 . . ?
C27 C24 H24 126.3 . . ?
Pd1 C24 H24 93.4 . . ?
C24 C25 C26 105.3(11) . . ?
C24 C25 Pd1 70.2(7) . . ?
C26 C25 Pd1 105.8(8) . . ?
C24 C25 H25 127.4 . . ?
C26 C25 H25 127.4 . . ?
Pd1 C25 H25 93.1 . . ?
O2 C26 O1 118.4(13) . . ?
O2 C26 C25 131.8(15) . . ?
O1 C26 C25 109.8(12) . . ?
O3 C27 O1 119.7(12) . . ?
O3 C27 C24 131.4(14) . . ?
O1 C27 C24 108.9(13) . . ?
C26 O1 C27 108.3(10) . . ?
N3 C31 N4 102.5(9) . . ?
N3 C31 Pd2 130.5(8) . . ?
N4 C31 Pd2 127.0(6) . . ?
C33 C38 C37 118.7(8) . . ?
C33 C38 P2 120.0(6) . . ?
C37 C38 P2 121.3(8) . . ?
C36 C37 C38 120.6(10) . . ?
C36 C37 H37 119.7 . . ?
C38 C37 H37 119.7 . . ?
C34 C33 C38 119.4(8) . . ?
C34 C33 C32 119.6(9) . . ?
C38 C33 C32 121.0(7) . . ?
C35 C36 C37 120.4(9) . . ?
C35 C36 H36 119.8 . . ?
C37 C36 H36 119.8 . . ?
N4 C32 C33 111.3(6) . . ?
N4 C32 H32A 109.4 . . ?
C33 C32 H32A 109.4 . . ?
N4 C32 H32B 109.4 . . ?
C33 C32 H32B 109.4 . . ?
H32A C32 H32B 108.0 . . ?
C29 C30 N4 106.5(10) . . ?
C29 C30 H30 126.7 . . ?
N4 C30 H30 126.7 . . ?
C33 C34 C35 120.6(10) . . ?
C33 C34 H34 119.7 . . ?
C35 C34 H34 119.7 . . ?
C30 C29 N3 107.0(10) . . ?
C30 C29 H29 126.5 . . ?
N3 C29 H29 126.5 . . ?
C36 C35 C34 120.3(10) . . ?
C36 C35 H35 119.9 . . ?
C34 C35 H35 119.9 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C31 N4 C30 111.7(8) . . ?
C31 N4 C32 124.0(8) . . ?
C30 N4 C32 124.2(8) . . ?
C31 N3 C29 112.3(9) . . ?
C31 N3 C28 124.3(9) . . ?
C29 N3 C28 123.3(9) . . ?
C40 C39 C44 118.7(8) . . ?
C40 C39 P2 124.4(6) . . ?
C44 C39 P2 116.9(7) . . ?
C39 C44 C43 120.4(10) . . ?
C39 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C39 C40 C41 120.7(9) . . ?
C39 C40 H40 119.6 . . ?
C41 C40 H40 119.6 . . ?
C43 C42 C41 119.3(9) . . ?
C43 C42 H42 120.4 . . ?
C41 C42 H42 120.4 . . ?
C42 C41 C40 120.1(10) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C45 C46 C47 121.5(11) . . ?
C45 C46 H46 119.3 . . ?
C47 C46 H46 119.3 . . ?
C46 C45 C50 116.6(10) . . ?
C46 C45 P2 124.4(8) . . ?
C50 C45 P2 119.0(9) . . ?
C49 C50 C45 120.7(14) . . ?
C49 C50 H50 119.7 . . ?
C45 C50 H50 119.7 . . ?
C48 C47 C46 119.6(13) . . ?
C48 C47 H47 120.2 . . ?
C46 C47 H47 120.2 . . ?
C48 C49 C50 120.8(14) . . ?
C48 C49 H49 119.6 . . ?
C50 C49 H49 119.6 . . ?
C52 C51 C54 107.8(9) . . ?
C52 C51 Pd2 70.3(6) . . ?
C54 C51 Pd2 105.4(6) . . ?
C52 C51 H51 126.1 . . ?
C54 C51 H51 126.1 . . ?
Pd2 C51 H51 93.5 . . ?
O6 C54 O4 117.4(9) . . ?
O6 C54 C51 133.2(10) . . ?
O4 C54 C51 109.3(10) . . ?
C51 C52 C53 106.7(10) . . ?
C51 C52 Pd2 70.7(6) . . ?
C53 C52 Pd2 108.1(7) . . ?
C51 C52 H52 120.3 . . ?
C53 C52 H52 120.3 . . ?
Pd2 C52 H52 120.3 . . ?
O5 C53 O4 118.4(11) . . ?
O5 C53 C52 132.9(13) . . ?
O4 C53 C52 108.7(10) . . ?
C54 O4 C53 106.8(8) . . ?
C49 C48 C47 120.6(14) . . ?
C49 C48 H48 119.7 . . ?
C47 C48 H48 119.7 . . ?
C42 C43 C44 120.7(10) . . ?
C42 C43 H43 119.7 . . ?
C44 C43 H43 119.7 . . ?
Cl6 C56 Cl5 110.9(10) . . ?
Cl6 C56 Cl4 108.3(7) . . ?
Cl5 C56 Cl4 110.8(10) . . ?
Cl6 C56 H56 108.9 . . ?
Cl5 C56 H56 108.9 . . ?
Cl4 C56 H56 108.9 . . ?
Cl8 C57 Cl9 117.1(10) . . ?
Cl8 C57 Cl7 106.1(9) . . ?
Cl9 C57 Cl7 110.9(9) . . ?
Cl8 C57 H57 107.4 . . ?
Cl9 C57 H57 107.4 . . ?
Cl7 C57 H57 107.4 . . ?
Cl2 C55 Cl1 107.3(9) . . ?
Cl2 C55 Cl3 107.4(9) . . ?
Cl1 C55 Cl3 111.1(8) . . ?
Cl2 C55 H55 110.3 . . ?
Cl1 C55 H55 110.3 . . ?
Cl3 C55 H55 110.3 . . ?
Cl12 C62 Cl11 115.8(14) . . ?
Cl12 C62 Cl10 108.1(15) . . ?
Cl11 C62 Cl10 108.6(14) . . ?
Cl12 C62 H62 108.0 . . ?
Cl11 C62 H62 108.0 . . ?
Cl10 C62 H62 108.0 . . ?

_refine_diff_density_max         1.679
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.153

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jss480
_database_code_depnum_ccdc_archive 'CCDC 1477480'
_audit_update_record             
;
2016-05-23 deposited with the CCDC.
2016-05-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H35 N2 O3 P Pd'
_chemical_formula_sum            'C27 H35 N2 O3 P Pd'
_chemical_formula_weight         572.94

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.2416(16)
_cell_length_b                   9.8555(18)
_cell_length_c                   14.849(3)
_cell_angle_alpha                79.479(14)
_cell_angle_beta                 82.978(13)
_cell_angle_gamma                86.719(13)
_cell_volume                     1318.9(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1958
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      20.0

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_F_000             592
_exptl_transmission_factor_min   0.853
_exptl_transmission_factor_max   0.867
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.794
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8573
_exptl_absorpt_correction_T_max  0.8702
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19020
_diffrn_reflns_av_unetI/netI     0.1001
_diffrn_reflns_av_R_equivalents  0.0802
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.404
_diffrn_reflns_theta_max         28.765
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6809
_reflns_number_gt                4384
_reflns_threshold_expression     I>2σ
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'DIAMOND (Brandenburg, 2006)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6809
_refine_ls_number_parameters     308
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1695
_refine_ls_wR_factor_gt          0.1374
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_restrained_S_all      0.900
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.54243(4) 0.32432(4) 0.20056(3) 0.03581(14) Uani 1 1 d . . . . .
P1 P 0.28922(13) 0.34673(11) 0.21705(8) 0.0314(3) Uani 1 1 d . . . . .
C3 C 0.5672(6) 0.4668(5) 0.2816(3) 0.0405(11) Uani 1 1 d . . . . .
C4 C 0.5425(7) 0.6732(6) 0.3273(4) 0.0535(14) Uani 1 1 d . . . . .
H4 H 0.5176 0.7680 0.3277 0.064 Uiso 1 1 calc R U . . .
C2 C 0.6064(7) 0.5858(7) 0.3914(4) 0.0579(16) Uani 1 1 d . . . . .
H2 H 0.6354 0.6063 0.4465 0.069 Uiso 1 1 calc R U . . .
C11 C 0.1999(5) 0.5172(5) 0.2266(3) 0.0354(10) Uani 1 1 d . . . . .
C5 C 0.4376(6) 0.6475(5) 0.1813(3) 0.0391(11) Uani 1 1 d . . . . .
H5A H 0.4664 0.5902 0.1334 0.047 Uiso 1 1 calc R U . . .
H5B H 0.4622 0.7441 0.1545 0.047 Uiso 1 1 calc R U . . .
C10 C 0.0490(6) 0.5225(5) 0.2516(3) 0.0436(12) Uani 1 1 d . . . . .
H10 H -0.0032 0.4398 0.2623 0.052 Uiso 1 1 calc R U . . .
C6 C 0.2745(6) 0.6402(5) 0.2093(3) 0.0409(11) Uani 1 1 d . . . . .
C9 C -0.0254(6) 0.6451(6) 0.2610(4) 0.0515(14) Uani 1 1 d . . . . .
H9 H -0.1280 0.6466 0.2773 0.062 Uiso 1 1 calc R U . . .
C7 C 0.1984(7) 0.7642(5) 0.2193(4) 0.0553(15) Uani 1 1 d . . . . .
H7 H 0.2490 0.8481 0.2071 0.066 Uiso 1 1 calc R U . . .
C8 C 0.0492(8) 0.7656(7) 0.2469(5) 0.0617(17) Uani 1 1 d . . . . .
H8 H -0.0014 0.8495 0.2560 0.074 Uiso 1 1 calc R U . . .
C12 C 0.1906(5) 0.3024(5) 0.1248(3) 0.0353(10) Uani 1 1 d . . . . .
H12 H 0.0848 0.3265 0.1394 0.042 Uiso 1 1 calc R U . . .
C17 C 0.2038(6) 0.1495(5) 0.1191(3) 0.0436(12) Uani 1 1 d . . . . .
H17A H 0.3084 0.1206 0.1120 0.052 Uiso 1 1 calc R U . . .
H17B H 0.1578 0.0957 0.1774 0.052 Uiso 1 1 calc R U . . .
C13 C 0.2448(7) 0.3929(6) 0.0327(3) 0.0476(13) Uani 1 1 d . . . . .
H13A H 0.2249 0.4913 0.0373 0.057 Uiso 1 1 calc R U . . .
H13B H 0.3516 0.3782 0.0197 0.057 Uiso 1 1 calc R U . . .
C16 C 0.1326(7) 0.1170(6) 0.0394(4) 0.0527(14) Uani 1 1 d . . . . .
H16A H 0.0255 0.1313 0.0514 0.063 Uiso 1 1 calc R U . . .
H16B H 0.1532 0.0188 0.0345 0.063 Uiso 1 1 calc R U . . .
C14 C 0.1712(8) 0.3598(6) -0.0458(4) 0.0606(16) Uani 1 1 d . . . . .
H14A H 0.2147 0.4142 -0.1047 0.073 Uiso 1 1 calc R U . . .
H14B H 0.0662 0.3867 -0.0372 0.073 Uiso 1 1 calc R U . . .
C15 C 0.1877(8) 0.2073(7) -0.0508(4) 0.0623(17) Uani 1 1 d . . . . .
H15A H 0.1330 0.1884 -0.1002 0.075 Uiso 1 1 calc R U . . .
H15B H 0.2919 0.1832 -0.0670 0.075 Uiso 1 1 calc R U . . .
C18 C 0.2147(6) 0.2356(5) 0.3263(3) 0.0404(11) Uani 1 1 d . . . . .
H18 H 0.1119 0.2148 0.3206 0.049 Uiso 1 1 calc R U . . .
C23 C 0.2144(7) 0.3031(6) 0.4109(3) 0.0527(14) Uani 1 1 d . . . . .
H23A H 0.1551 0.3904 0.4033 0.063 Uiso 1 1 calc R U . . .
H23B H 0.3153 0.3249 0.4179 0.063 Uiso 1 1 calc R U . . .
C19 C 0.3039(7) 0.0984(6) 0.3410(4) 0.0522(14) Uani 1 1 d . . . . .
H19A H 0.3040 0.0536 0.2865 0.063 Uiso 1 1 calc R U . . .
H19B H 0.4061 0.1174 0.3467 0.063 Uiso 1 1 calc R U . . .
C22 C 0.1510(9) 0.2046(8) 0.4970(4) 0.077(2) Uani 1 1 d . . . . .
H22A H 0.1524 0.2484 0.5518 0.092 Uiso 1 1 calc R U . . .
H22B H 0.0481 0.1882 0.4912 0.092 Uiso 1 1 calc R U . . .
C20 C 0.2429(10) 0.0005(7) 0.4266(5) 0.086(3) Uani 1 1 d . . . . .
H20A H 0.1439 -0.0256 0.4189 0.104 Uiso 1 1 calc R U . . .
H20B H 0.3057 -0.0847 0.4350 0.104 Uiso 1 1 calc R U . . .
C21 C 0.2359(10) 0.0673(9) 0.5109(5) 0.095(3) Uani 1 1 d . . . . .
H21A H 0.3360 0.0822 0.5234 0.114 Uiso 1 1 calc R U . . .
H21B H 0.1882 0.0050 0.5650 0.114 Uiso 1 1 calc R U . . .
C1 C 0.6906(8) 0.3354(7) 0.4119(5) 0.0676(18) Uani 1 1 d . . . . .
H1A H 0.6164 0.2831 0.4551 0.101 Uiso 1 1 calc R U . . .
H1B H 0.7660 0.3612 0.4460 0.101 Uiso 1 1 calc R U . . .
H1C H 0.7350 0.2784 0.3675 0.101 Uiso 1 1 calc R U . . .
N2 N 0.5196(5) 0.5991(4) 0.2600(3) 0.0409(9) Uani 1 1 d . . . . .
N1 N 0.6225(5) 0.4604(5) 0.3626(3) 0.0494(11) Uani 1 1 d . . . . .
C25 C 0.6267(6) 0.1862(6) 0.1109(4) 0.0454(12) Uani 1 1 d . . . . .
H25 H 0.5737 0.2284 0.0616 0.055 Uiso 1 1 calc R U . . .
C26 C 0.7442(6) 0.2450(5) 0.1443(4) 0.0458(12) Uani 1 1 d . . . . .
H26 H 0.7833 0.3335 0.1216 0.055 Uiso 1 1 calc R U . . .
C27 C 0.7917(6) 0.1428(6) 0.2197(4) 0.0510(14) Uani 1 1 d . . . . .
C24 C 0.6045(7) 0.0520(6) 0.1660(5) 0.0566(16) Uani 1 1 d . . . . .
O2 O 0.7013(5) 0.0311(4) 0.2346(3) 0.0607(11) Uani 1 1 d . . . . .
O3 O 0.8886(5) 0.1404(5) 0.2673(3) 0.0714(13) Uani 1 1 d . . . . .
O1 O 0.5228(5) -0.0371(4) 0.1637(4) 0.0822(16) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 C3 2.048(5) . ?
Pd1 C26 2.116(5) . ?
Pd1 C25 2.125(5) . ?
Pd1 P1 2.3249(13) . ?
P1 C11 1.851(5) . ?
P1 C12 1.862(5) . ?
P1 C18 1.863(5) . ?
C3 N2 1.347(6) . ?
C3 N1 1.353(7) . ?
C4 C2 1.333(9) . ?
C4 N2 1.383(7) . ?
C2 N1 1.375(7) . ?
C11 C6 1.396(7) . ?
C11 C10 1.399(7) . ?
C5 N2 1.462(7) . ?
C5 C6 1.516(7) . ?
C10 C9 1.377(7) . ?
C6 C7 1.397(7) . ?
C9 C8 1.377(9) . ?
C7 C8 1.390(9) . ?
C12 C17 1.522(7) . ?
C12 C13 1.535(7) . ?
C17 C16 1.513(7) . ?
C13 C14 1.512(8) . ?
C16 C15 1.515(8) . ?
C14 C15 1.517(9) . ?
C18 C23 1.525(7) . ?
C18 C19 1.537(7) . ?
C23 C22 1.532(8) . ?
C19 C20 1.518(8) . ?
C22 C21 1.519(11) . ?
C20 C21 1.509(11) . ?
C1 N1 1.464(7) . ?
C25 C24 1.434(8) . ?
C25 C26 1.439(8) . ?
C26 C27 1.455(8) . ?
C27 O3 1.204(7) . ?
C27 O2 1.389(7) . ?
C24 O1 1.198(7) . ?
C24 O2 1.416(8) . ?

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
C3 Pd1 C26 112.7(2) . . ?
C3 Pd1 C25 152.3(2) . . ?
C26 Pd1 C25 39.7(2) . . ?
C3 Pd1 P1 94.12(15) . . ?
C26 Pd1 P1 153.10(17) . . ?
C25 Pd1 P1 113.46(16) . . ?
C11 P1 C12 99.2(2) . . ?
C11 P1 C18 102.8(2) . . ?
C12 P1 C18 106.1(2) . . ?
C11 P1 Pd1 119.49(17) . . ?
C12 P1 Pd1 118.08(16) . . ?
C18 P1 Pd1 109.37(18) . . ?
N2 C3 N1 104.2(4) . . ?
N2 C3 Pd1 121.9(4) . . ?
N1 C3 Pd1 133.9(4) . . ?
C2 C4 N2 106.6(5) . . ?
C4 C2 N1 107.0(5) . . ?
C6 C11 C10 118.5(4) . . ?
C6 C11 P1 123.6(4) . . ?
C10 C11 P1 117.8(4) . . ?
N2 C5 C6 111.5(4) . . ?
C9 C10 C11 121.4(5) . . ?
C11 C6 C7 119.8(5) . . ?
C11 C6 C5 123.3(4) . . ?
C7 C6 C5 116.9(5) . . ?
C10 C9 C8 119.9(5) . . ?
C8 C7 C6 120.3(6) . . ?
C9 C8 C7 119.9(5) . . ?
C17 C12 C13 111.8(4) . . ?
C17 C12 P1 113.1(3) . . ?
C13 C12 P1 108.8(3) . . ?
C16 C17 C12 112.4(4) . . ?
C14 C13 C12 111.6(5) . . ?
C17 C16 C15 111.5(5) . . ?
C13 C14 C15 111.4(5) . . ?
C16 C15 C14 112.3(5) . . ?
C23 C18 C19 108.7(5) . . ?
C23 C18 P1 113.3(4) . . ?
C19 C18 P1 109.8(4) . . ?
C18 C23 C22 109.6(5) . . ?
C20 C19 C18 112.1(5) . . ?
C21 C22 C23 112.1(6) . . ?
C21 C20 C19 110.7(6) . . ?
C20 C21 C22 110.8(6) . . ?
C3 N2 C4 111.1(5) . . ?
C3 N2 C5 122.1(4) . . ?
C4 N2 C5 126.3(5) . . ?
C3 N1 C2 111.1(5) . . ?
C3 N1 C1 123.8(5) . . ?
C2 N1 C1 125.2(5) . . ?
C24 C25 C26 107.2(5) . . ?
C24 C25 Pd1 104.0(4) . . ?
C26 C25 Pd1 69.8(3) . . ?
C25 C26 C27 106.7(5) . . ?
C25 C26 Pd1 70.5(3) . . ?
C27 C26 Pd1 104.0(3) . . ?
O3 C27 O2 119.0(5) . . ?
O3 C27 C26 132.4(6) . . ?
O2 C27 C26 108.6(5) . . ?
O1 C24 O2 119.1(6) . . ?
O1 C24 C25 132.4(7) . . ?
O2 C24 C25 108.5(5) . . ?
C27 O2 C24 108.8(4) . . ?

_refine_diff_density_max         1.810
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.108

_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0

