# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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_lsg2-110
_database_code_depnum_ccdc_archive 'CCDC 1037603'
_audit_update_record             
;
2014-12-04 deposited with the CCDC.
2015-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C76 H92 N8 O8 P4 Pd4, 2(C H2 Cl2)'
_chemical_formula_sum            'C78 H96 Cl4 N8 O8 P4 Pd4'
_chemical_formula_weight         1964.91

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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I-4   '
_symmetry_space_group_name_Hall  'I -4 '

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

_cell_length_a                   15.1307(6)
_cell_length_b                   15.1307(6)
_cell_length_c                   19.1938(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4394.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    6455
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      28.30

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1992
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6371
_exptl_absorpt_correction_T_max  0.8664
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16059
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.90
_diffrn_reflns_theta_max         28.30
_reflns_number_total             5359
_reflns_number_gt                4433
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0277P)²+0.6340P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_number_reflns         5359
_refine_ls_number_parameters     240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0213
_refine_ls_wR_factor_ref         0.0561
_refine_ls_wR_factor_gt          0.0472
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.003
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.763174(11) 0.027583(11) 0.934587(9) 0.03287(6) Uani 1 1 d . . .
Cl1 Cl 0.48267(16) -0.09286(13) 1.06206(18) 0.1937(10) Uani 1 1 d . . .
P1 P 0.70118(5) 0.10847(5) 0.84866(4) 0.04686(17) Uani 1 1 d . . .
O1 O 0.69524(15) -0.09434(14) 0.83229(11) 0.0590(6) Uani 1 1 d . . .
O2 O 0.85548(12) -0.20854(11) 1.00853(10) 0.0440(4) Uani 1 1 d . . .
N2 N 0.82265(14) -0.05845(13) 1.00309(11) 0.0345(4) Uani 1 1 d . . .
N1 N 0.77365(13) -0.15433(13) 0.91977(11) 0.0374(5) Uani 1 1 d . . .
C1 C 0.58597(19) 0.0888(2) 0.83073(18) 0.0585(8) Uani 1 1 d . . .
H1A H 0.5765 0.0255 0.8228 0.088 Uiso 1 1 calc R . .
H1B H 0.5684 0.1219 0.7891 0.088 Uiso 1 1 calc R . .
H1C H 0.5504 0.1081 0.8706 0.088 Uiso 1 1 calc R . .
C2 C 0.7561(2) 0.0916(3) 0.76542(18) 0.0774(11) Uani 1 1 d . . .
H2A H 0.7564 0.0284 0.7541 0.116 Uiso 1 1 calc R . .
H2B H 0.8171 0.1131 0.7683 0.116 Uiso 1 1 calc R . .
H2C H 0.7245 0.1240 0.7290 0.116 Uiso 1 1 calc R . .
C3 C 0.7057(3) 0.2265(2) 0.8613(3) 0.0906(14) Uani 1 1 d . . .
H3A H 0.7665 0.2441 0.8719 0.136 Uiso 1 1 calc R . .
H3B H 0.6670 0.2430 0.9001 0.136 Uiso 1 1 calc R . .
H3C H 0.6860 0.2564 0.8188 0.136 Uiso 1 1 calc R . .
C4 C 0.73630(17) -0.08254(17) 0.88616(13) 0.0390(6) Uani 1 1 d . . .
C5 C 0.76610(18) -0.24319(18) 0.89005(16) 0.0448(6) Uani 1 1 d . . .
H5A H 0.8159 -0.2796 0.9073 0.054 Uiso 1 1 calc R . .
H5B H 0.7717 -0.2390 0.8388 0.054 Uiso 1 1 calc R . .
C6 C 0.6811(2) -0.28919(17) 0.90714(15) 0.0451(6) Uani 1 1 d . . .
C7 C 0.6626(3) -0.3679(2) 0.87393(18) 0.0618(9) Uani 1 1 d . . .
H7 H 0.7046 -0.3922 0.8425 0.074 Uiso 1 1 calc R . .
C8 C 0.5849(3) -0.4115(3) 0.8855(2) 0.0856(13) Uani 1 1 d . . .
H8 H 0.5737 -0.4658 0.8624 0.103 Uiso 1 1 calc R . .
C9 C 0.5232(3) -0.3775(3) 0.9302(3) 0.0900(13) Uani 1 1 d . . .
H9 H 0.4690 -0.4078 0.9376 0.108 Uiso 1 1 calc R . .
C10 C 0.5396(3) -0.2998(3) 0.9644(2) 0.0830(12) Uani 1 1 d . . .
H10 H 0.4974 -0.2761 0.9959 0.100 Uiso 1 1 calc R . .
C11 C 0.6191(2) -0.2558(2) 0.9523(2) 0.0642(10) Uani 1 1 d . . .
H11 H 0.6306 -0.2018 0.9758 0.077 Uiso 1 1 calc R . .
C12 C 0.82134(15) -0.14123(16) 0.98190(13) 0.0352(5) Uani 1 1 d . . .
C13 C 0.87339(15) -0.03474(16) 1.06453(15) 0.0382(5) Uani 1 1 d . . .
H13A H 0.9134 0.0146 1.0522 0.046 Uiso 1 1 calc R . .
H13B H 0.9107 -0.0858 1.0776 0.046 Uiso 1 1 calc R . .
C14 C 0.8200(2) -0.00779(18) 1.12711(14) 0.0449(6) Uani 1 1 d . . .
C15 C 0.7323(2) -0.0271(2) 1.13460(19) 0.0640(9) Uani 1 1 d . . .
H15 H 0.7018 -0.0571 1.0984 0.077 Uiso 1 1 calc R . .
C16 C 0.6865(3) -0.0027(3) 1.1957(3) 0.0937(14) Uani 1 1 d . . .
H16 H 0.6258 -0.0168 1.2014 0.112 Uiso 1 1 calc R . .
C17 C 0.7328(5) 0.0430(4) 1.2479(2) 0.105(2) Uani 1 1 d . . .
H17 H 0.7028 0.0610 1.2890 0.126 Uiso 1 1 calc R . .
C18 C 0.8181(4) 0.0612(3) 1.2403(2) 0.0892(15) Uani 1 1 d . . .
H18 H 0.8485 0.0912 1.2766 0.107 Uiso 1 1 calc R . .
C19 C 0.8637(3) 0.0372(2) 1.18043(16) 0.0640(9) Uani 1 1 d . . .
H19 H 0.9246 0.0514 1.1758 0.077 Uiso 1 1 calc R . .
C20 C 0.5000 0.0000 1.0107(5) 0.151(4) Uani 1 2 d S . .
H20A H 0.4479 0.0097 0.9804 0.181 Uiso 0.50 1 calc PR . .
H20B H 0.5521 -0.0097 0.9804 0.181 Uiso 0.50 1 calc PR . .


_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 C4 1.951(3) . ?
Pd1 N2 2.0575(19) . ?
Pd1 O2 2.1227(17) 3_667 ?
Pd1 P1 2.2579(7) . ?
Cl1 C20 1.736(6) . ?
P1 C1 1.802(3) . ?
P1 C3 1.803(4) . ?
P1 C2 1.819(4) . ?
O1 C4 1.219(3) . ?
O2 C12 1.251(3) . ?
O2 Pd1 2.1227(17) 4_647 ?
N2 C12 1.317(3) . ?
N2 C13 1.452(3) . ?
N1 C4 1.384(3) . ?
N1 C12 1.408(3) . ?
N1 C5 1.465(3) . ?
C5 C6 1.498(4) . ?
C6 C11 1.374(4) . ?
C6 C7 1.379(4) . ?
C7 C8 1.366(5) . ?
C8 C9 1.369(6) . ?
C9 C10 1.369(6) . ?
C10 C11 1.393(5) . ?
C13 C14 1.504(4) . ?
C14 C15 1.367(5) . ?
C14 C19 1.396(4) . ?
C15 C16 1.411(6) . ?
C16 C17 1.404(8) . ?
C17 C18 1.328(8) . ?
C18 C19 1.389(6) . ?
C20 Cl1 1.736(6) 2_655 ?

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
C4 Pd1 N2 81.67(9) . . ?
C4 Pd1 O2 177.49(10) . 3_667 ?
N2 Pd1 O2 96.34(8) . 3_667 ?
C4 Pd1 P1 91.63(8) . . ?
N2 Pd1 P1 172.51(6) . . ?
O2 Pd1 P1 90.44(6) 3_667 . ?
C1 P1 C3 103.07(19) . . ?
C1 P1 C2 104.55(17) . . ?
C3 P1 C2 103.9(2) . . ?
C1 P1 Pd1 116.86(11) . . ?
C3 P1 Pd1 115.00(15) . . ?
C2 P1 Pd1 112.05(12) . . ?
C12 O2 Pd1 135.92(16) . 4_647 ?
C12 N2 C13 119.6(2) . . ?
C12 N2 Pd1 113.43(16) . . ?
C13 N2 Pd1 126.43(15) . . ?
C4 N1 C12 119.6(2) . . ?
C4 N1 C5 120.5(2) . . ?
C12 N1 C5 119.9(2) . . ?
O1 C4 N1 119.2(2) . . ?
O1 C4 Pd1 129.4(2) . . ?
N1 C4 Pd1 111.30(16) . . ?
N1 C5 C6 114.1(2) . . ?
C11 C6 C7 118.0(3) . . ?
C11 C6 C5 123.6(3) . . ?
C7 C6 C5 118.3(3) . . ?
C8 C7 C6 121.1(4) . . ?
C7 C8 C9 120.5(3) . . ?
C8 C9 C10 119.9(3) . . ?
C9 C10 C11 119.2(4) . . ?
C6 C11 C10 121.3(3) . . ?
O2 C12 N2 129.9(2) . . ?
O2 C12 N1 116.3(2) . . ?
N2 C12 N1 113.8(2) . . ?
N2 C13 C14 115.6(2) . . ?
C15 C14 C19 119.1(3) . . ?
C15 C14 C13 123.2(3) . . ?
C19 C14 C13 117.6(3) . . ?
C14 C15 C16 120.5(4) . . ?
C17 C16 C15 118.5(4) . . ?
C18 C17 C16 120.6(4) . . ?
C17 C18 C19 121.3(4) . . ?
C18 C19 C14 119.9(4) . . ?
Cl1 C20 Cl1 110.8(5) . 2_655 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.081
####################################################################### 
# 
# 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_lsg231
_database_code_depnum_ccdc_archive 'CCDC 1037604'
_audit_update_record             
;
2014-12-04 deposited with the CCDC.
2015-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C26 H38 N2 O2 P2 Pd '
_chemical_formula_sum            'C26 H38 N2 O2 P2 Pd'
_chemical_formula_weight         578.92

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n  '
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   19.3654(8)
_cell_length_b                   14.0152(6)
_cell_length_c                   21.2584(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.4220(10)
_cell_angle_gamma                90.00
_cell_volume                     5407.1(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    8788
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      28.25

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2400
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8132
_exptl_absorpt_correction_T_max  0.9676
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            38568
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.04
_diffrn_reflns_theta_max         28.29
_reflns_number_total             13151
_reflns_number_gt                8462
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0791P)²+2.6524P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13151
_refine_ls_number_parameters     595
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0483
_refine_ls_wR_factor_ref         0.1621
_refine_ls_wR_factor_gt          0.1272
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.466113(16) 0.17359(2) 0.905391(15) 0.04850(11) Uani 1 1 d . . .
Pd2 Pd 0.472910(16) 0.20142(2) 0.432992(16) 0.05171(11) Uani 1 1 d . . .
P1 P 0.56003(6) 0.19187(9) 1.01033(6) 0.0568(3) Uani 1 1 d . . .
P2 P 0.55790(6) 0.17354(10) 0.86368(7) 0.0658(3) Uani 1 1 d . . .
P3 P 0.57114(6) 0.22983(10) 0.40235(7) 0.0616(3) Uani 1 1 d . . .
P4 P 0.55906(7) 0.20278(15) 0.54208(7) 0.0904(5) Uani 1 1 d . . .
O1 O 0.39566(17) 0.1552(3) 0.75781(15) 0.0653(8) Uani 1 1 d . . .
O2 O 0.24676(16) 0.1794(2) 0.88149(17) 0.0669(8) Uani 1 1 d . . .
O3 O 0.41418(18) 0.2082(3) 0.28355(16) 0.0717(9) Uani 1 1 d . . .
O4 O 0.25031(15) 0.1808(2) 0.39210(16) 0.0628(8) Uani 1 1 d . . .
N1 N 0.31859(18) 0.1728(2) 0.81547(17) 0.0508(8) Uani 1 1 d . . .
N2 N 0.37275(18) 0.1744(3) 0.93080(17) 0.0525(8) Uani 1 1 d . . .
N3 N 0.32991(18) 0.1990(2) 0.33427(16) 0.0500(8) Uani 1 1 d . . .
N4 N 0.37548(18) 0.1817(3) 0.44915(17) 0.0533(8) Uani 1 1 d . . .
C1 C 0.3874(2) 0.1641(3) 0.8121(2) 0.0484(8) Uani 1 1 d . . .
C2 C 0.3094(2) 0.1755(3) 0.8796(2) 0.0534(9) Uani 1 1 d . . .
C3 C 0.2531(2) 0.1841(3) 0.7549(2) 0.0578(10) Uani 1 1 d . . .
H3A H 0.2684 0.2119 0.7190 0.069 Uiso 1 1 calc R . .
H3B H 0.2193 0.2301 0.7646 0.069 Uiso 1 1 calc R . .
C4 C 0.2115(2) 0.0929(3) 0.72919(19) 0.0548(10) Uani 1 1 d . . .
C5 C 0.1390(3) 0.0851(4) 0.7226(3) 0.0714(13) Uani 1 1 d . . .
H5 H 0.1154 0.1364 0.7363 0.086 Uiso 1 1 calc R . .
C6 C 0.0992(3) 0.0022(5) 0.6958(3) 0.0863(16) Uani 1 1 d . . .
H6 H 0.0486 -0.0024 0.6907 0.104 Uiso 1 1 calc R . .
C7 C 0.1336(4) -0.0724(4) 0.6769(3) 0.0867(16) Uani 1 1 d . . .
H7 H 0.1064 -0.1281 0.6576 0.104 Uiso 1 1 calc R . .
C8 C 0.2054(3) -0.0668(4) 0.6855(3) 0.0874(17) Uani 1 1 d . . .
H8 H 0.2296 -0.1201 0.6748 0.105 Uiso 1 1 calc R . .
C9 C 0.2448(3) 0.0164(4) 0.7101(3) 0.0751(13) Uani 1 1 d . . .
H9 H 0.2950 0.0207 0.7137 0.090 Uiso 1 1 calc R . .
C10 C 0.3662(3) 0.1712(4) 0.9970(2) 0.0614(11) Uani 1 1 d . . .
H10A H 0.4108 0.1397 1.0282 0.074 Uiso 1 1 calc R . .
H10B H 0.3235 0.1305 0.9942 0.074 Uiso 1 1 calc R . .
C11 C 0.3571(3) 0.2662(4) 1.0270(2) 0.0698(13) Uani 1 1 d . . .
C12 C 0.3692(4) 0.2710(6) 1.0961(3) 0.0960(19) Uani 1 1 d . . .
H12 H 0.3863 0.2165 1.1236 0.115 Uiso 1 1 calc R . .
C13 C 0.3563(5) 0.3552(8) 1.1238(4) 0.132(3) Uani 1 1 d . . .
H13 H 0.3640 0.3577 1.1704 0.158 Uiso 1 1 calc R . .
C14 C 0.3327(5) 0.4352(7) 1.0853(5) 0.134(3) Uani 1 1 d . . .
H14 H 0.3237 0.4924 1.1051 0.161 Uiso 1 1 calc R . .
C15 C 0.3219(4) 0.4323(5) 1.0167(4) 0.106(2) Uani 1 1 d . . .
H15 H 0.3058 0.4874 0.9894 0.127 Uiso 1 1 calc R . .
C16 C 0.3351(3) 0.3475(4) 0.9896(3) 0.0783(14) Uani 1 1 d . . .
H16 H 0.3286 0.3456 0.9432 0.094 Uiso 1 1 calc R . .
C17 C 0.6460(3) 0.2165(4) 0.9945(3) 0.0732(14) Uani 1 1 d . . .
H17A H 0.6502 0.2857 0.9874 0.088 Uiso 1 1 calc R . .
H17B H 0.6889 0.1969 1.0340 0.088 Uiso 1 1 calc R . .
C18 C 0.6462(2) 0.1614(4) 0.9325(3) 0.0695(13) Uani 1 1 d . . .
H18A H 0.6559 0.0931 0.9440 0.083 Uiso 1 1 calc R . .
H18B H 0.6862 0.1858 0.9179 0.083 Uiso 1 1 calc R . .
C19 C 0.5804(3) 0.0849(4) 1.0624(2) 0.0700(12) Uani 1 1 d . . .
H19A H 0.5335 0.0608 1.0652 0.084 Uiso 1 1 calc R . .
H19B H 0.5991 0.0356 1.0390 0.084 Uiso 1 1 calc R . .
C20 C 0.6359(3) 0.0945(4) 1.1342(3) 0.0868(16) Uani 1 1 d . . .
H20A H 0.6423 0.0324 1.1567 0.130 Uiso 1 1 calc R . .
H20B H 0.6175 0.1409 1.1590 0.130 Uiso 1 1 calc R . .
H20C H 0.6834 0.1163 1.1326 0.130 Uiso 1 1 calc R . .
C21 C 0.5535(3) 0.2890(4) 1.0649(3) 0.0753(14) Uani 1 1 d . . .
H21A H 0.5164 0.2725 1.0855 0.090 Uiso 1 1 calc R . .
H21B H 0.6016 0.2969 1.1016 0.090 Uiso 1 1 calc R . .
C22 C 0.5319(3) 0.3829(4) 1.0271(3) 0.0945(18) Uani 1 1 d . . .
H22A H 0.5288 0.4330 1.0581 0.142 Uiso 1 1 calc R . .
H22B H 0.4840 0.3757 0.9912 0.142 Uiso 1 1 calc R . .
H22C H 0.5692 0.4004 1.0076 0.142 Uiso 1 1 calc R . .
C23 C 0.5703(4) 0.3242(11) 0.8385(4) 0.206(9) Uani 1 1 d . . .
H23A H 0.5427 0.3705 0.8559 0.247 Uiso 1 1 calc R . .
H23B H 0.6218 0.3449 0.8479 0.247 Uiso 1 1 calc R . .
C24 C 0.5403(8) 0.3000(13) 0.7850(9) 0.279(11) Uani 1 1 d . . .
H24A H 0.5342 0.3543 0.7544 0.418 Uiso 1 1 calc R . .
H24B H 0.4918 0.2748 0.7810 0.418 Uiso 1 1 calc R . .
H24C H 0.5690 0.2500 0.7732 0.418 Uiso 1 1 calc R . .
C25 C 0.5601(3) 0.0825(5) 0.8051(3) 0.093(2) Uani 1 1 d . . .
H25A H 0.5206 0.0955 0.7616 0.111 Uiso 1 1 calc R . .
H25B H 0.6078 0.0862 0.7979 0.111 Uiso 1 1 calc R . .
C26 C 0.5504(4) -0.0179(5) 0.8271(3) 0.103(2) Uani 1 1 d . . .
H26A H 0.5516 -0.0633 0.7925 0.155 Uiso 1 1 calc R . .
H26B H 0.5029 -0.0227 0.8339 0.155 Uiso 1 1 calc R . .
H26C H 0.5903 -0.0325 0.8693 0.155 Uiso 1 1 calc R . .
C27 C 0.4012(2) 0.2028(3) 0.3361(2) 0.0540(9) Uani 1 1 d . . .
C28 C 0.3152(2) 0.1862(3) 0.3947(2) 0.0516(9) Uani 1 1 d . . .
C29 C 0.2681(2) 0.2095(3) 0.2707(2) 0.0569(10) Uani 1 1 d . . .
H29A H 0.2827 0.2542 0.2415 0.068 Uiso 1 1 calc R . .
H29B H 0.2260 0.2383 0.2800 0.068 Uiso 1 1 calc R . .
C30 C 0.2433(2) 0.1168(3) 0.23343(19) 0.0517(9) Uani 1 1 d . . .
C31 C 0.2012(3) 0.0518(4) 0.2535(2) 0.0644(11) Uani 1 1 d . . .
H31 H 0.1878 0.0657 0.2914 0.077 Uiso 1 1 calc R . .
C32 C 0.1788(3) -0.0317(4) 0.2197(2) 0.0754(14) Uani 1 1 d . . .
H32 H 0.1504 -0.0755 0.2347 0.090 Uiso 1 1 calc R . .
C33 C 0.1968(3) -0.0533(4) 0.1644(3) 0.0776(14) Uani 1 1 d . . .
H33 H 0.1809 -0.1115 0.1409 0.093 Uiso 1 1 calc R . .
C34 C 0.2382(3) 0.0107(4) 0.1433(2) 0.0723(13) Uani 1 1 d . . .
H34 H 0.2508 -0.0033 0.1049 0.087 Uiso 1 1 calc R . .
C35 C 0.2615(2) 0.0954(4) 0.1779(2) 0.0615(11) Uani 1 1 d . . .
H35 H 0.2903 0.1390 0.1632 0.074 Uiso 1 1 calc R . .
C36 C 0.3622(2) 0.1691(3) 0.5120(2) 0.0567(10) Uani 1 1 d . . .
H36A H 0.4045 0.1339 0.5436 0.068 Uiso 1 1 calc R . .
H36B H 0.3179 0.1285 0.5032 0.068 Uiso 1 1 calc R . .
C37 C 0.3512(2) 0.2592(3) 0.5459(2) 0.0538(10) Uani 1 1 d . . .
C38 C 0.3364(2) 0.3465(3) 0.5134(2) 0.0581(10) Uani 1 1 d . . .
H38 H 0.3358 0.3512 0.4686 0.070 Uiso 1 1 calc R . .
C39 C 0.3225(3) 0.4269(4) 0.5446(2) 0.0659(12) Uani 1 1 d . . .
H39 H 0.3113 0.4856 0.5209 0.079 Uiso 1 1 calc R . .
C40 C 0.3249(3) 0.4223(4) 0.6102(2) 0.0713(13) Uani 1 1 d . . .
H40 H 0.3154 0.4774 0.6319 0.086 Uiso 1 1 calc R . .
C41 C 0.3413(3) 0.3365(4) 0.6437(2) 0.0711(13) Uani 1 1 d . . .
H41 H 0.3439 0.3330 0.6891 0.085 Uiso 1 1 calc R . .
C42 C 0.3539(2) 0.2558(4) 0.6124(2) 0.0644(11) Uani 1 1 d . . .
H42 H 0.3645 0.1972 0.6363 0.077 Uiso 1 1 calc R . .
C43 C 0.6534(3) 0.2262(10) 0.4732(4) 0.204(6) Uani 1 1 d . . .
H43A H 0.6783 0.1649 0.4718 0.245 Uiso 1 1 calc R . .
H43B H 0.6860 0.2777 0.4679 0.245 Uiso 1 1 calc R . .
C44 C 0.6491(3) 0.2350(6) 0.5366(3) 0.099(2) Uani 1 1 d . . .
H44A H 0.6604 0.3019 0.5517 0.119 Uiso 1 1 calc R . .
H44B H 0.6875 0.1941 0.5680 0.119 Uiso 1 1 calc R . .
C45 C 0.5749(5) 0.3444(7) 0.3691(7) 0.200(6) Uani 1 1 d . . .
H45A H 0.6050 0.3832 0.4079 0.240 Uiso 1 1 calc R . .
H45B H 0.6051 0.3364 0.3403 0.240 Uiso 1 1 calc R . .
C46 C 0.5200(3) 0.4009(5) 0.3346(4) 0.119(3) Uani 1 1 d . . .
H46A H 0.5399 0.4611 0.3249 0.179 Uiso 1 1 calc R . .
H46B H 0.4884 0.4136 0.3611 0.179 Uiso 1 1 calc R . .
H46C H 0.4910 0.3697 0.2924 0.179 Uiso 1 1 calc R . .
C47 C 0.5874(4) 0.1568(5) 0.3396(5) 0.125(3) Uani 1 1 d . . .
H47A H 0.5517 0.1752 0.2952 0.150 Uiso 1 1 calc R . .
H47B H 0.6374 0.1712 0.3393 0.150 Uiso 1 1 calc R . .
C48 C 0.5819(5) 0.0536(5) 0.3478(5) 0.136(3) Uani 1 1 d . . .
H48A H 0.5903 0.0203 0.3106 0.204 Uiso 1 1 calc R . .
H48B H 0.5326 0.0380 0.3480 0.204 Uiso 1 1 calc R . .
H48C H 0.6190 0.0335 0.3904 0.204 Uiso 1 1 calc R . .
C49 C 0.5762(4) 0.0754(6) 0.5823(4) 0.121(3) Uani 1 1 d . . .
H49A H 0.5299 0.0536 0.5876 0.145 Uiso 1 1 calc R . .
H49B H 0.5865 0.0315 0.5501 0.145 Uiso 1 1 calc R . .
C50 C 0.6338(5) 0.0657(7) 0.6451(5) 0.164(4) Uani 1 1 d . . .
H50A H 0.6375 -0.0011 0.6595 0.246 Uiso 1 1 calc R . .
H50B H 0.6233 0.1059 0.6784 0.246 Uiso 1 1 calc R . .
H50C H 0.6804 0.0857 0.6408 0.246 Uiso 1 1 calc R . .
C51 C 0.5499(5) 0.2838(13) 0.6015(5) 0.241(10) Uani 1 1 d . . .
H51A H 0.5092 0.2628 0.6163 0.289 Uiso 1 1 calc R . .
H51B H 0.5958 0.2838 0.6412 0.289 Uiso 1 1 calc R . .
C52 C 0.5343(6) 0.3853(10) 0.5737(9) 0.266(11) Uani 1 1 d . . .
H52A H 0.5297 0.4279 0.6086 0.399 Uiso 1 1 calc R . .
H52B H 0.4883 0.3860 0.5350 0.399 Uiso 1 1 calc R . .
H52C H 0.5749 0.4069 0.5598 0.399 Uiso 1 1 calc R . .


_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 2.042(4) . ?
Pd1 N2 2.060(3) . ?
Pd1 P2 2.2462(12) . ?
Pd1 P1 2.3492(12) . ?
Pd2 C27 2.043(4) . ?
Pd2 N4 2.051(3) . ?
Pd2 P3 2.2508(11) . ?
Pd2 P4 2.3371(14) . ?
P1 C21 1.823(6) . ?
P1 C19 1.823(5) . ?
P1 C17 1.843(5) . ?
P2 C25 1.793(6) . ?
P2 C18 1.829(5) . ?
P2 C23 2.212(14) . ?
P3 C45 1.767(8) . ?
P3 C43 1.771(7) . ?
P3 C47 1.795(7) . ?
P4 C51 1.753(10) . ?
P4 C44 1.845(5) . ?
P4 C49 1.957(8) . ?
O1 C1 1.225(5) . ?
O2 C2 1.229(5) . ?
O3 C27 1.231(5) . ?
O4 C28 1.240(5) . ?
N1 C1 1.365(5) . ?
N1 C2 1.435(5) . ?
N1 C3 1.467(5) . ?
N2 C2 1.327(5) . ?
N2 C10 1.457(5) . ?
N3 C27 1.368(5) . ?
N3 C28 1.422(5) . ?
N3 C29 1.466(5) . ?
N4 C28 1.328(5) . ?
N4 C36 1.458(5) . ?
C3 C4 1.509(6) . ?
C4 C5 1.365(6) . ?
C4 C9 1.383(6) . ?
C5 C6 1.402(7) . ?
C6 C7 1.374(8) . ?
C7 C8 1.339(8) . ?
C8 C9 1.392(7) . ?
C10 C11 1.513(7) . ?
C11 C16 1.370(8) . ?
C11 C12 1.406(7) . ?
C12 C13 1.380(11) . ?
C13 C14 1.369(12) . ?
C14 C15 1.400(11) . ?
C15 C16 1.383(8) . ?
C17 C18 1.529(8) . ?
C19 C20 1.535(7) . ?
C21 C22 1.523(8) . ?
C23 C24 1.134(15) . ?
C25 C26 1.515(9) . ?
C29 C30 1.510(6) . ?
C30 C35 1.379(6) . ?
C30 C31 1.385(6) . ?
C31 C32 1.363(7) . ?
C32 C33 1.372(7) . ?
C33 C34 1.379(7) . ?
C34 C35 1.387(7) . ?
C36 C37 1.506(6) . ?
C37 C38 1.385(6) . ?
C37 C42 1.398(6) . ?
C38 C39 1.380(7) . ?
C39 C40 1.382(7) . ?
C40 C41 1.376(7) . ?
C41 C42 1.377(7) . ?
C43 C44 1.385(9) . ?
C45 C46 1.322(9) . ?
C47 C48 1.465(10) . ?
C49 C50 1.417(10) . ?
C51 C52 1.53(2) . ?

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 N2 80.16(15) . . ?
C1 Pd1 P2 92.39(12) . . ?
N2 Pd1 P2 172.51(10) . . ?
C1 Pd1 P1 176.55(12) . . ?
N2 Pd1 P1 102.13(10) . . ?
P2 Pd1 P1 85.28(5) . . ?
C27 Pd2 N4 80.12(15) . . ?
C27 Pd2 P3 93.02(12) . . ?
N4 Pd2 P3 172.78(10) . . ?
C27 Pd2 P4 177.39(12) . . ?
N4 Pd2 P4 102.41(10) . . ?
P3 Pd2 P4 84.43(5) . . ?
C21 P1 C19 106.0(3) . . ?
C21 P1 C17 104.2(3) . . ?
C19 P1 C17 104.3(2) . . ?
C21 P1 Pd1 118.91(18) . . ?
C19 P1 Pd1 114.75(16) . . ?
C17 P1 Pd1 107.28(18) . . ?
C25 P2 C18 104.3(3) . . ?
C25 P2 C23 118.7(4) . . ?
C18 P2 C23 97.6(3) . . ?
C25 P2 Pd1 119.2(2) . . ?
C18 P2 Pd1 109.37(17) . . ?
C23 P2 Pd1 105.2(3) . . ?
C45 P3 C43 102.5(6) . . ?
C45 P3 C47 100.3(5) . . ?
C43 P3 C47 106.0(5) . . ?
C45 P3 Pd2 115.7(3) . . ?
C43 P3 Pd2 110.5(2) . . ?
C47 P3 Pd2 120.0(2) . . ?
C51 P4 C44 102.9(4) . . ?
C51 P4 C49 108.7(7) . . ?
C44 P4 C49 103.4(3) . . ?
C51 P4 Pd2 120.2(4) . . ?
C44 P4 Pd2 107.6(2) . . ?
C49 P4 Pd2 112.3(2) . . ?
C1 N1 C2 120.0(3) . . ?
C1 N1 C3 121.6(4) . . ?
C2 N1 C3 118.3(3) . . ?
C2 N2 C10 115.2(3) . . ?
C2 N2 Pd1 115.5(3) . . ?
C10 N2 Pd1 129.3(3) . . ?
C27 N3 C28 119.8(3) . . ?
C27 N3 C29 120.9(4) . . ?
C28 N3 C29 119.2(3) . . ?
C28 N4 C36 114.9(3) . . ?
C28 N4 Pd2 115.4(3) . . ?
C36 N4 Pd2 129.6(3) . . ?
O1 C1 N1 120.7(4) . . ?
O1 C1 Pd1 128.5(3) . . ?
N1 C1 Pd1 110.7(3) . . ?
O2 C2 N2 127.9(4) . . ?
O2 C2 N1 118.9(4) . . ?
N2 C2 N1 113.2(3) . . ?
N1 C3 C4 114.5(3) . . ?
C5 C4 C9 118.5(4) . . ?
C5 C4 C3 120.3(4) . . ?
C9 C4 C3 121.2(4) . . ?
C4 C5 C6 120.5(5) . . ?
C7 C6 C5 119.7(5) . . ?
C8 C7 C6 120.1(6) . . ?
C7 C8 C9 120.5(6) . . ?
C4 C9 C8 120.6(5) . . ?
N2 C10 C11 116.3(4) . . ?
C16 C11 C12 118.1(6) . . ?
C16 C11 C10 123.1(4) . . ?
C12 C11 C10 118.8(6) . . ?
C13 C12 C11 119.9(8) . . ?
C14 C13 C12 121.1(7) . . ?
C13 C14 C15 119.8(7) . . ?
C16 C15 C14 118.5(8) . . ?
C11 C16 C15 122.6(6) . . ?
C18 C17 P1 109.7(3) . . ?
C17 C18 P2 111.1(3) . . ?
C20 C19 P1 117.4(4) . . ?
C22 C21 P1 112.1(4) . . ?
C24 C23 P2 84.1(16) . . ?
C26 C25 P2 114.3(4) . . ?
O3 C27 N3 120.0(4) . . ?
O3 C27 Pd2 129.3(3) . . ?
N3 C27 Pd2 110.7(3) . . ?
O4 C28 N4 127.3(4) . . ?
O4 C28 N3 119.1(4) . . ?
N4 C28 N3 113.6(3) . . ?
N3 C29 C30 113.9(3) . . ?
C35 C30 C31 118.3(4) . . ?
C35 C30 C29 120.5(4) . . ?
C31 C30 C29 121.2(4) . . ?
C32 C31 C30 121.1(4) . . ?
C31 C32 C33 120.8(5) . . ?
C32 C33 C34 119.1(5) . . ?
C33 C34 C35 120.2(5) . . ?
C30 C35 C34 120.5(4) . . ?
N4 C36 C37 115.8(4) . . ?
C38 C37 C42 117.6(4) . . ?
C38 C37 C36 122.9(4) . . ?
C42 C37 C36 119.5(4) . . ?
C39 C38 C37 121.5(4) . . ?
C38 C39 C40 120.3(5) . . ?
C41 C40 C39 118.9(5) . . ?
C40 C41 C42 121.0(4) . . ?
C41 C42 C37 120.7(5) . . ?
C44 C43 P3 118.9(5) . . ?
C43 C44 P4 114.8(5) . . ?
C46 C45 P3 128.9(6) . . ?
C48 C47 P3 115.8(6) . . ?
C50 C49 P4 117.1(6) . . ?
C52 C51 P4 112.4(10) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        28.29
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.792
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.096
####################################################################### 
# 
# 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_lsg278
_database_code_depnum_ccdc_archive 'CCDC 1037605'
_audit_update_record             
;
2014-12-04 deposited with the CCDC.
2015-02-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H32 Cl2 N2 O2 P2 Pd, C H2 Cl2'
_chemical_formula_sum            'C25 H34 Cl4 N2 O2 P2 Pd'
_chemical_formula_weight         704.68

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n  '
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   13.1299(9)
_cell_length_b                   11.2538(8)
_cell_length_c                   20.6433(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.048(2)
_cell_angle_gamma                90.00
_cell_volume                     3012.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    5283
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      28.29

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7404
_exptl_absorpt_correction_T_max  0.8790
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21550
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.99
_diffrn_reflns_theta_max         28.30
_reflns_number_total             7352
_reflns_number_gt                5087
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0325P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7352
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0807
_refine_ls_wR_factor_gt          0.0647
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_restrained_S_all      1.002
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.715852(15) 0.286927(19) 0.837488(9) 0.02623(7) Uani 1 1 d . . .
Cl1 Cl 1.31530(6) 0.59412(8) 0.81808(4) 0.0507(2) Uani 1 1 d . . .
Cl2 Cl 0.78555(7) -0.05513(9) 1.14553(4) 0.0588(2) Uani 1 1 d . . .
Cl3 Cl 0.78819(7) 0.52149(8) 0.95993(4) 0.0559(2) Uani 1 1 d . . .
Cl4 Cl 0.69053(7) 0.75285(8) 0.96254(4) 0.0589(2) Uani 1 1 d . . .
P1 P 0.60961(5) 0.34245(7) 0.74645(3) 0.03165(17) Uani 1 1 d . . .
P2 P 0.57394(5) 0.17918(7) 0.86340(3) 0.02831(16) Uani 1 1 d . . .
O1 O 0.84182(15) 0.4387(2) 0.76220(9) 0.0500(6) Uani 1 1 d . . .
O2 O 1.00525(14) 0.25818(18) 0.94587(9) 0.0407(5) Uani 1 1 d . . .
N1 N 0.92862(16) 0.3444(2) 0.85038(10) 0.0289(5) Uani 1 1 d . . .
N2 N 0.82939(16) 0.24137(19) 0.91378(10) 0.0277(5) Uani 1 1 d . . .
C1 C 0.8374(2) 0.3724(3) 0.80842(12) 0.0312(6) Uani 1 1 d . . .
C2 C 0.9249(2) 0.2766(2) 0.90774(12) 0.0287(6) Uani 1 1 d . . .
C3 C 1.0240(2) 0.4025(2) 0.84307(12) 0.0298(6) Uani 1 1 d . . .
C4 C 1.0867(2) 0.3562(3) 0.80150(14) 0.0377(7) Uani 1 1 d . . .
H4A H 1.0679 0.2848 0.7781 0.045 Uiso 1 1 calc R . .
C5 C 1.1775(2) 0.4144(3) 0.79408(14) 0.0407(7) Uani 1 1 d . . .
H5A H 1.2213 0.3832 0.7657 0.049 Uiso 1 1 calc R . .
C6 C 1.2032(2) 0.5177(3) 0.82825(13) 0.0323(6) Uani 1 1 d . . .
C7 C 1.1413(2) 0.5639(3) 0.87003(13) 0.0361(7) Uani 1 1 d . . .
H7A H 1.1598 0.6354 0.8934 0.043 Uiso 1 1 calc R . .
C8 C 1.0517(2) 0.5044(3) 0.87740(13) 0.0344(6) Uani 1 1 d . . .
H8A H 1.0089 0.5347 0.9066 0.041 Uiso 1 1 calc R . .
C9 C 0.81937(19) 0.1705(2) 0.96933(12) 0.0260(6) Uani 1 1 d . . .
C10 C 0.8701(2) 0.0633(2) 0.98016(13) 0.0319(6) Uani 1 1 d . . .
H10A H 0.9135 0.0375 0.9502 0.038 Uiso 1 1 calc R . .
C11 C 0.8594(2) -0.0078(3) 1.03355(14) 0.0377(7) Uani 1 1 d . . .
H11A H 0.8944 -0.0818 1.0400 0.045 Uiso 1 1 calc R . .
C12 C 0.7969(2) 0.0313(3) 1.07704(13) 0.0356(7) Uani 1 1 d . . .
C13 C 0.7452(2) 0.1376(3) 1.06759(13) 0.0339(6) Uani 1 1 d . . .
H13A H 0.7018 0.1631 1.0976 0.041 Uiso 1 1 calc R . .
C14 C 0.7570(2) 0.2076(2) 1.01352(12) 0.0296(6) Uani 1 1 d . . .
H14A H 0.7218 0.2815 1.0070 0.036 Uiso 1 1 calc R . .
C15 C 0.4770(2) 0.3024(3) 0.75488(13) 0.0348(7) Uani 1 1 d . . .
H15A H 0.4476 0.3638 0.7809 0.042 Uiso 1 1 calc R . .
H15B H 0.4340 0.2985 0.7110 0.042 Uiso 1 1 calc R . .
C16 C 0.4764(2) 0.1822(3) 0.78888(13) 0.0357(7) Uani 1 1 d . . .
H16A H 0.4913 0.1186 0.7586 0.043 Uiso 1 1 calc R . .
H16B H 0.4073 0.1672 0.8007 0.043 Uiso 1 1 calc R . .
C17 C 0.6059(2) 0.4995(3) 0.72439(14) 0.0441(8) Uani 1 1 d . . .
H17A H 0.6682 0.5192 0.7051 0.053 Uiso 1 1 calc R . .
H17B H 0.5449 0.5143 0.6905 0.053 Uiso 1 1 calc R . .
C18 C 0.6008(3) 0.5807(3) 0.78244(17) 0.0571(9) Uani 1 1 d . . .
H18A H 0.5991 0.6637 0.7679 0.086 Uiso 1 1 calc R . .
H18B H 0.6616 0.5678 0.8158 0.086 Uiso 1 1 calc R . .
H18C H 0.5383 0.5632 0.8012 0.086 Uiso 1 1 calc R . .
C19 C 0.6358(2) 0.2621(3) 0.67459(13) 0.0430(8) Uani 1 1 d . . .
H19A H 0.7076 0.2794 0.6684 0.052 Uiso 1 1 calc R . .
H19B H 0.6316 0.1759 0.6834 0.052 Uiso 1 1 calc R . .
C20 C 0.5646(3) 0.2898(3) 0.61073(14) 0.0475(8) Uani 1 1 d . . .
H20A H 0.5846 0.2415 0.5752 0.071 Uiso 1 1 calc R . .
H20B H 0.5701 0.3742 0.6002 0.071 Uiso 1 1 calc R . .
H20C H 0.4933 0.2714 0.6157 0.071 Uiso 1 1 calc R . .
C21 C 0.5947(2) 0.0220(3) 0.88167(14) 0.0366(7) Uani 1 1 d . . .
H21A H 0.6274 -0.0142 0.8464 0.044 Uiso 1 1 calc R . .
H21B H 0.6440 0.0147 0.9230 0.044 Uiso 1 1 calc R . .
C22 C 0.4978(2) -0.0496(3) 0.88862(16) 0.0525(9) Uani 1 1 d . . .
H22A H 0.5168 -0.1325 0.8986 0.079 Uiso 1 1 calc R . .
H22B H 0.4492 -0.0458 0.8474 0.079 Uiso 1 1 calc R . .
H22C H 0.4654 -0.0161 0.9242 0.079 Uiso 1 1 calc R . .
C23 C 0.5068(2) 0.2346(3) 0.92885(14) 0.0387(7) Uani 1 1 d . . .
H23A H 0.4364 0.2005 0.9225 0.046 Uiso 1 1 calc R . .
H23B H 0.5435 0.2052 0.9714 0.046 Uiso 1 1 calc R . .
C24 C 0.4983(3) 0.3681(3) 0.93250(17) 0.0580(10) Uani 1 1 d . . .
H24A H 0.4613 0.3896 0.9685 0.087 Uiso 1 1 calc R . .
H24B H 0.4606 0.3983 0.8910 0.087 Uiso 1 1 calc R . .
H24C H 0.5675 0.4030 0.9404 0.087 Uiso 1 1 calc R . .
C25 C 0.7696(2) 0.6465(3) 1.00814(14) 0.0417(7) Uani 1 1 d . . .
H25A H 0.7374 0.6211 1.0461 0.050 Uiso 1 1 calc R . .
H25B H 0.8373 0.6826 1.0251 0.050 Uiso 1 1 calc R . .


_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 2.032(3) . ?
Pd1 N2 2.056(2) . ?
Pd1 P1 2.2458(7) . ?
Pd1 P2 2.3541(7) . ?
Cl1 C6 1.746(3) . ?
Cl2 C12 1.742(3) . ?
Cl3 C25 1.762(3) . ?
Cl4 C25 1.758(3) . ?
P1 C19 1.816(3) . ?
P1 C17 1.824(3) . ?
P1 C15 1.833(3) . ?
P2 C21 1.820(3) . ?
P2 C23 1.835(3) . ?
P2 C16 1.840(3) . ?
O1 C1 1.220(3) . ?
O2 C2 1.230(3) . ?
N1 C1 1.400(3) . ?
N1 C2 1.416(3) . ?
N1 C3 1.442(3) . ?
N2 C2 1.340(3) . ?
N2 C9 1.420(3) . ?
C3 C8 1.367(4) . ?
C3 C4 1.382(4) . ?
C4 C5 1.390(4) . ?
C5 C6 1.374(4) . ?
C6 C7 1.378(4) . ?
C7 C8 1.382(4) . ?
C9 C10 1.379(4) . ?
C9 C14 1.383(4) . ?
C10 C11 1.387(4) . ?
C11 C12 1.380(4) . ?
C12 C13 1.374(4) . ?
C13 C14 1.395(4) . ?
C15 C16 1.525(4) . ?
C17 C18 1.517(4) . ?
C19 C20 1.524(4) . ?
C21 C22 1.531(4) . ?
C23 C24 1.509(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pd1 N2 80.55(10) . . ?
C1 Pd1 P1 91.97(8) . . ?
N2 Pd1 P1 172.10(6) . . ?
C1 Pd1 P2 175.45(8) . . ?
N2 Pd1 P2 101.65(6) . . ?
P1 Pd1 P2 85.63(3) . . ?
C19 P1 C17 106.26(15) . . ?
C19 P1 C15 105.08(14) . . ?
C17 P1 C15 105.84(14) . . ?
C19 P1 Pd1 111.86(10) . . ?
C17 P1 Pd1 117.86(10) . . ?
C15 P1 Pd1 109.06(9) . . ?
C21 P2 C23 104.56(13) . . ?
C21 P2 C16 104.65(14) . . ?
C23 P2 C16 104.94(14) . . ?
C21 P2 Pd1 116.72(10) . . ?
C23 P2 Pd1 118.77(10) . . ?
C16 P2 Pd1 105.78(9) . . ?
C1 N1 C2 120.0(2) . . ?
C1 N1 C3 120.4(2) . . ?
C2 N1 C3 118.5(2) . . ?
C2 N2 C9 116.6(2) . . ?
C2 N2 Pd1 115.56(17) . . ?
C9 N2 Pd1 127.63(16) . . ?
O1 C1 N1 118.7(2) . . ?
O1 C1 Pd1 131.1(2) . . ?
N1 C1 Pd1 110.26(18) . . ?
O2 C2 N2 127.7(2) . . ?
O2 C2 N1 119.2(2) . . ?
N2 C2 N1 113.1(2) . . ?
C8 C3 C4 120.2(3) . . ?
C8 C3 N1 119.4(2) . . ?
C4 C3 N1 120.4(3) . . ?
C3 C4 C5 119.7(3) . . ?
C6 C5 C4 119.2(3) . . ?
C5 C6 C7 121.3(3) . . ?
C5 C6 Cl1 119.9(2) . . ?
C7 C6 Cl1 118.8(2) . . ?
C6 C7 C8 118.8(3) . . ?
C3 C8 C7 120.7(3) . . ?
C10 C9 C14 118.6(2) . . ?
C10 C9 N2 121.2(2) . . ?
C14 C9 N2 120.2(2) . . ?
C9 C10 C11 121.8(3) . . ?
C12 C11 C10 118.6(3) . . ?
C13 C12 C11 121.1(3) . . ?
C13 C12 Cl2 119.8(2) . . ?
C11 C12 Cl2 119.1(2) . . ?
C12 C13 C14 119.4(3) . . ?
C9 C14 C13 120.6(3) . . ?
C16 C15 P1 109.57(19) . . ?
C15 C16 P2 110.37(19) . . ?
C18 C17 P1 112.9(2) . . ?
C20 C19 P1 115.8(2) . . ?
C22 C21 P2 115.5(2) . . ?
C24 C23 P2 115.0(2) . . ?
Cl4 C25 Cl3 111.34(16) . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        28.30
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         0.794
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.109
