# 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_rhopa
_database_code_depnum_ccdc_archive 'CCDC 1423102'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-11-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H29 Cl N2 P Rh'
_chemical_formula_weight         514.82

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'
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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.1441(6)
_cell_length_b                   9.8885(6)
_cell_length_c                   13.5572(8)
_cell_angle_alpha                83.875(2)
_cell_angle_beta                 81.588(2)
_cell_angle_gamma                67.831(3)
_cell_volume                     1121.25(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9491
_cell_measurement_theta_min      2.23
_cell_measurement_theta_max      31.02

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             528
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6940
_exptl_absorpt_correction_T_max  0.8304
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX II 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            61697
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_sigmaI/netI    0.0153
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         31.06
_reflns_number_total             7166
_reflns_number_gt                6891
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker APEX2'
_computing_data_reduction        'Bruker APEX2'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97

_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.

 Hydrogens at coordinated C=C were refined freely using the distance
 restraint SADI for the C-H bond lengths; methyls were refined as idealized
 rigid groups allowed to rotate but not tip; other hydrogens were included
 using a riding model starting from calculated positions.
;

_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)+(0.0166P)²+0.5733P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7166
_refine_ls_number_parameters     281
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0166
_refine_ls_wR_factor_ref         0.0429
_refine_ls_wR_factor_gt          0.0422
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.038
_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
Rh Rh 0.287508(9) 0.476923(8) 0.238290(5) 0.01350(2) Uani 1 1 d . . .
Cl Cl 0.00784(3) 0.58180(3) 0.25632(2) 0.02438(6) Uani 1 1 d . . .
N1 N 0.42098(10) 0.02257(9) 0.35575(6) 0.01480(15) Uani 1 1 d . . .
C2 C 0.29561(11) 0.14048(10) 0.35594(7) 0.01375(16) Uani 1 1 d . . .
P3 P 0.27925(3) 0.24960(3) 0.233541(18) 0.01159(4) Uani 1 1 d . . .
C3A C 0.45731(11) 0.10385(10) 0.18418(7) 0.01189(15) Uani 1 1 d . . .
N4 N 0.52529(10) 0.09714(9) 0.09002(6) 0.01377(14) Uani 1 1 d . . .
C5 C 0.65659(11) -0.02260(11) 0.07041(7) 0.01500(17) Uani 1 1 d . . .
H5 H 0.7064 -0.0335 0.0036 0.018 Uiso 1 1 calc R . .
C6 C 0.72353(12) -0.13131(11) 0.14258(8) 0.01601(17) Uani 1 1 d . . .
H6 H 0.8178 -0.2123 0.1247 0.019 Uiso 1 1 calc R . .
C7 C 0.65224(12) -0.12096(11) 0.24063(8) 0.01521(17) Uani 1 1 d . . .
H7 H 0.6968 -0.1926 0.2914 0.018 Uiso 1 1 calc R . .
C7A C 0.51312(11) -0.00141(10) 0.26128(7) 0.01276(16) Uani 1 1 d . . .
C11 C 0.12719(11) 0.22003(10) 0.17580(7) 0.01408(16) Uani 1 1 d . . .
C12 C 0.08708(13) 0.09694(11) 0.20294(8) 0.01911(19) Uani 1 1 d . . .
H12 H 0.1335 0.0308 0.2559 0.023 Uiso 1 1 calc R . .
C13 C -0.02082(14) 0.07138(13) 0.15237(10) 0.0234(2) Uani 1 1 d . . .
H13 H -0.0499 -0.0111 0.1717 0.028 Uiso 1 1 calc R . .
C14 C -0.08627(13) 0.16645(13) 0.07342(9) 0.0223(2) Uani 1 1 d . . .
H14 H -0.1594 0.1483 0.0386 0.027 Uiso 1 1 calc R . .
C15 C -0.04517(13) 0.28754(12) 0.04536(8) 0.02040(19) Uani 1 1 d . . .
H15 H -0.0890 0.3515 -0.0091 0.024 Uiso 1 1 calc R . .
C16 C 0.06048(12) 0.31555(11) 0.09705(8) 0.01728(18) Uani 1 1 d . . .
H16 H 0.0870 0.3996 0.0786 0.021 Uiso 1 1 calc R . .
C17 C 0.18601(12) 0.19129(11) 0.45080(8) 0.01763(18) Uani 1 1 d . . .
C18 C 0.20451(14) 0.06141(13) 0.52723(8) 0.0238(2) Uani 1 1 d . . .
H18A H 0.1775 -0.0124 0.4993 0.029 Uiso 1 1 calc R . .
H18B H 0.1332 0.0952 0.5884 0.029 Uiso 1 1 calc R . .
H18C H 0.3147 0.0185 0.5428 0.029 Uiso 1 1 calc R . .
C19 C 0.23701(16) 0.30380(13) 0.49220(9) 0.0257(2) Uani 1 1 d . . .
H19A H 0.3474 0.2570 0.5070 0.031 Uiso 1 1 calc R . .
H19B H 0.1679 0.3408 0.5535 0.031 Uiso 1 1 calc R . .
H19C H 0.2282 0.3852 0.4425 0.031 Uiso 1 1 calc R . .
C20 C 0.01205(13) 0.26393(14) 0.42959(9) 0.0260(2) Uani 1 1 d . . .
H20A H 0.0021 0.3437 0.3784 0.031 Uiso 1 1 calc R . .
H20B H -0.0552 0.3031 0.4910 0.031 Uiso 1 1 calc R . .
H20C H -0.0218 0.1913 0.4059 0.031 Uiso 1 1 calc R . .
C21 C 0.28868(15) 0.69912(11) 0.19905(9) 0.0226(2) Uani 1 1 d D . .
H21 H 0.1856(16) 0.7483(17) 0.1821(12) 0.029(4) Uiso 1 1 d D . .
C22 C 0.30620(19) 0.66843(13) 0.29924(9) 0.0292(3) Uani 1 1 d D . .
H22 H 0.2135(17) 0.6960(18) 0.3441(12) 0.034(4) Uiso 1 1 d D . .
C23 C 0.4623(2) 0.62745(17) 0.34095(11) 0.0406(4) Uani 1 1 d . . .
H23A H 0.4423 0.6698 0.4068 0.049 Uiso 1 1 calc R . .
H23B H 0.5306 0.6707 0.2960 0.049 Uiso 1 1 calc R . .
C24 C 0.5511(2) 0.46165(17) 0.35314(11) 0.0378(3) Uani 1 1 d . . .
H24A H 0.6663 0.4411 0.3506 0.045 Uiso 1 1 calc R . .
H24B H 0.5151 0.4258 0.4196 0.045 Uiso 1 1 calc R . .
C25 C 0.52562(14) 0.37886(13) 0.27376(10) 0.0239(2) Uani 1 1 d D . .
H25 H 0.5482(19) 0.2798(14) 0.2928(12) 0.028(4) Uiso 1 1 d D . .
C26 C 0.52800(13) 0.41882(12) 0.17132(9) 0.0207(2) Uani 1 1 d D . .
H26 H 0.5497(18) 0.3441(15) 0.1290(11) 0.026(4) Uiso 1 1 d D . .
C27 C 0.56781(15) 0.54923(13) 0.12319(10) 0.0263(2) Uani 1 1 d . . .
H27A H 0.6232 0.5257 0.0552 0.032 Uiso 1 1 calc R . .
H27B H 0.6415 0.5664 0.1627 0.032 Uiso 1 1 calc R . .
C28 C 0.42028(15) 0.68965(13) 0.11622(9) 0.0244(2) Uani 1 1 d . . .
H28A H 0.4518 0.7749 0.1172 0.029 Uiso 1 1 calc R . .
H28B H 0.3795 0.6956 0.0515 0.029 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
Rh C25 2.1274(11) . ?
Rh C26 2.1364(11) . ?
Rh C21 2.2085(11) . ?
Rh C22 2.2176(11) . ?
Rh P3 2.2855(3) . ?
Rh Cl 2.3547(3) . ?
N1 C2 1.2902(13) . ?
N1 C7A 1.4159(12) . ?
C2 C17 1.5137(14) . ?
C2 P3 1.8733(10) . ?
P3 C3A 1.8144(10) . ?
P3 C11 1.8181(10) . ?
C3A N4 1.3323(12) . ?
C3A C7A 1.3998(13) . ?
N4 C5 1.3473(13) . ?
C5 C6 1.3934(14) . ?
C6 C7 1.3884(14) . ?
C7 C7A 1.3877(13) . ?
C11 C16 1.3945(14) . ?
C11 C12 1.3976(14) . ?
C12 C13 1.3895(15) . ?
C13 C14 1.3913(17) . ?
C14 C15 1.3858(16) . ?
C15 C16 1.3937(14) . ?
C17 C18 1.5346(15) . ?
C17 C20 1.5351(16) . ?
C17 C19 1.5400(16) . ?
C21 C22 1.3791(17) . ?
C21 C28 1.5033(17) . ?
C22 C23 1.507(2) . ?
C23 C24 1.533(2) . ?
C24 C25 1.5128(18) . ?
C25 C26 1.4022(17) . ?
C26 C27 1.5253(16) . ?
C27 C28 1.5338(17) . ?

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
C25 Rh C26 38.40(5) . . ?
C25 Rh C21 96.88(5) . . ?
C26 Rh C21 81.32(4) . . ?
C25 Rh C22 81.30(5) . . ?
C26 Rh C22 89.02(5) . . ?
C21 Rh C22 36.31(4) . . ?
C25 Rh P3 89.64(3) . . ?
C26 Rh P3 95.34(3) . . ?
C21 Rh P3 164.30(3) . . ?
C22 Rh P3 159.39(3) . . ?
C25 Rh Cl 161.21(4) . . ?
C26 Rh Cl 159.88(3) . . ?
C21 Rh Cl 87.76(3) . . ?
C22 Rh Cl 92.13(4) . . ?
P3 Rh Cl 90.624(10) . . ?
C2 N1 C7A 113.10(8) . . ?
N1 C2 C17 121.62(9) . . ?
N1 C2 P3 113.53(7) . . ?
C17 C2 P3 124.45(7) . . ?
C3A P3 C11 101.39(4) . . ?
C3A P3 C2 87.53(4) . . ?
C11 P3 C2 106.34(4) . . ?
C3A P3 Rh 118.56(3) . . ?
C11 P3 Rh 122.16(3) . . ?
C2 P3 Rh 114.88(3) . . ?
N4 C3A C7A 125.04(9) . . ?
N4 C3A P3 125.95(7) . . ?
C7A C3A P3 109.00(7) . . ?
C3A N4 C5 115.44(8) . . ?
N4 C5 C6 123.72(9) . . ?
C7 C6 C5 119.87(9) . . ?
C7A C7 C6 117.15(9) . . ?
C7 C7A C3A 118.69(9) . . ?
C7 C7A N1 124.64(9) . . ?
C3A C7A N1 116.67(8) . . ?
C16 C11 C12 119.81(9) . . ?
C16 C11 P3 118.79(7) . . ?
C12 C11 P3 121.15(8) . . ?
C13 C12 C11 119.91(10) . . ?
C12 C13 C14 120.06(10) . . ?
C15 C14 C13 120.22(10) . . ?
C14 C15 C16 120.04(10) . . ?
C15 C16 C11 119.93(10) . . ?
C2 C17 C18 110.00(9) . . ?
C2 C17 C20 111.14(9) . . ?
C18 C17 C20 109.91(9) . . ?
C2 C17 C19 106.68(9) . . ?
C18 C17 C19 109.60(9) . . ?
C20 C17 C19 109.44(10) . . ?
C22 C21 C28 125.78(12) . . ?
C22 C21 Rh 72.21(6) . . ?
C28 C21 Rh 108.41(7) . . ?
C21 C22 C23 123.64(13) . . ?
C21 C22 Rh 71.49(7) . . ?
C23 C22 Rh 111.09(9) . . ?
C22 C23 C24 113.06(10) . . ?
C25 C24 C23 113.06(10) . . ?
C26 C25 C24 125.92(10) . . ?
C26 C25 Rh 71.15(6) . . ?
C24 C25 Rh 110.15(10) . . ?
C25 C26 C27 123.93(10) . . ?
C25 C26 Rh 70.45(7) . . ?
C27 C26 Rh 113.51(8) . . ?
C26 C27 C28 112.88(10) . . ?
C21 C28 C27 113.77(9) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C20 H20A Cl 0.98 2.74 3.7094(13) 169.1 .
C6 H6 Cl 0.95 2.79 3.4435(10) 126.3 1_645
C7 H7 Cl 0.95 2.89 3.4805(10) 121.6 1_645
C19 H19B Cl 0.98 2.85 3.8204(12) 173.1 2_566

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.053


####################################################################### 
# 
# 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_gstaab
_database_code_depnum_ccdc_archive 'CCDC 1423103'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-11-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H78 Cl4 N4 O4.50 P2 Pd2'
_chemical_formula_weight         1175.66

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'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'C 2/c'

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

_cell_length_a                   27.727(3)
_cell_length_b                   16.625(2)
_cell_length_c                   23.302(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.891(6)
_cell_angle_gamma                90.00
_cell_volume                     10739(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9734
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      30.47

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4864
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7322
_exptl_absorpt_correction_T_max  0.8679
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX2 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            153859
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         30.03
_reflns_number_total             15352
_reflns_number_gt                11085
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97

_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.

 O151-C155 and O161-C165 represent alternative positions of the disordered THF.
;

_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)+(0.0185P)²+64.0719P] 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         15352
_refine_ls_number_parameters     585
_refine_ls_number_restraints     511
_refine_ls_R_factor_all          0.0782
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_ref         0.0982
_refine_ls_wR_factor_gt          0.0803
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_restrained_S_all      1.185
_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 0.534739(9) 0.634164(15) 0.418459(10) 0.01537(6) Uani 1 1 d . . .
Pd2 Pd 0.556095(9) 0.870272(15) 0.439133(10) 0.01585(6) Uani 1 1 d . . .
Cl1 Cl 0.54591(3) 0.61348(6) 0.32318(3) 0.02817(19) Uani 1 1 d . . .
Cl2 Cl 0.59454(3) 0.54028(5) 0.44263(3) 0.02124(16) Uani 1 1 d . . .
Cl3 Cl 0.63030(3) 0.89847(6) 0.40453(4) 0.02860(19) Uani 1 1 d . . .
Cl4 Cl 0.51990(3) 0.96176(5) 0.37582(3) 0.02129(16) Uani 1 1 d . . .
N1 N 0.39032(10) 0.70726(17) 0.44820(12) 0.0203(6) Uani 1 1 d . . .
C2 C 0.41345(12) 0.67361(19) 0.40738(14) 0.0183(6) Uani 1 1 d . . .
P3 P 0.47425(3) 0.71797(5) 0.39532(3) 0.01533(15) Uani 1 1 d . . .
C3A C 0.46124(11) 0.78913(18) 0.45166(13) 0.0159(6) Uani 1 1 d . . .
N4 N 0.49019(10) 0.84719(15) 0.47295(11) 0.0154(5) Uani 1 1 d . . .
C5 C 0.47392(12) 0.89071(19) 0.51780(13) 0.0190(6) Uani 1 1 d . . .
H5 H 0.4939 0.9319 0.5335 0.023 Uiso 1 1 calc R . .
C6 C 0.42878(12) 0.8772(2) 0.54177(14) 0.0196(6) Uani 1 1 d . . .
H6 H 0.4180 0.9100 0.5724 0.024 Uiso 1 1 calc R . .
C7 C 0.39982(13) 0.8159(2) 0.52081(14) 0.0221(7) Uani 1 1 d . . .
H7 H 0.3695 0.8045 0.5375 0.026 Uiso 1 1 calc R . .
C7A C 0.41636(12) 0.77151(19) 0.47460(13) 0.0180(6) Uani 1 1 d . . .
C8 C 0.39358(12) 0.6016(2) 0.37515(14) 0.0212(7) Uani 1 1 d . . .
C9 C 0.40706(15) 0.6047(2) 0.31169(14) 0.0286(8) Uani 1 1 d . . .
H9A H 0.3938 0.5575 0.2918 0.043 Uiso 1 1 calc R . .
H9B H 0.4423 0.6048 0.3084 0.043 Uiso 1 1 calc R . .
H9C H 0.3938 0.6537 0.2942 0.043 Uiso 1 1 calc R . .
C10 C 0.41618(16) 0.5260(2) 0.40210(17) 0.0329(9) Uani 1 1 d . . .
H10A H 0.4040 0.4781 0.3820 0.049 Uiso 1 1 calc R . .
H10B H 0.4076 0.5230 0.4427 0.049 Uiso 1 1 calc R . .
H10C H 0.4513 0.5285 0.3988 0.049 Uiso 1 1 calc R . .
C11 C 0.33885(14) 0.5990(3) 0.38049(18) 0.0376(10) Uani 1 1 d . . .
H11A H 0.3261 0.5524 0.3595 0.056 Uiso 1 1 calc R . .
H11B H 0.3249 0.6484 0.3643 0.056 Uiso 1 1 calc R . .
H11C H 0.3304 0.5947 0.4211 0.056 Uiso 1 1 calc R . .
C12 C 0.47181(12) 0.7734(2) 0.32795(13) 0.0189(6) Uani 1 1 d . . .
H12A H 0.5006 0.8085 0.3258 0.023 Uiso 1 1 calc R . .
H12B H 0.4732 0.7347 0.2957 0.023 Uiso 1 1 calc R . .
C13 C 0.42671(12) 0.8248(2) 0.32073(14) 0.0205(7) Uani 1 1 d . . .
H13A H 0.4273 0.8683 0.3497 0.025 Uiso 1 1 calc R . .
H13B H 0.3978 0.7912 0.3274 0.025 Uiso 1 1 calc R . .
C14 C 0.42322(14) 0.8617(2) 0.26079(14) 0.0259(7) Uani 1 1 d . . .
H14A H 0.4527 0.8937 0.2537 0.031 Uiso 1 1 calc R . .
H14B H 0.4216 0.8181 0.2319 0.031 Uiso 1 1 calc R . .
C15 C 0.37937(15) 0.9153(2) 0.25353(16) 0.0318(9) Uani 1 1 d . . .
H15A H 0.3786 0.9378 0.2146 0.048 Uiso 1 1 calc R . .
H15B H 0.3811 0.9592 0.2816 0.048 Uiso 1 1 calc R . .
H15C H 0.3501 0.8837 0.2597 0.048 Uiso 1 1 calc R . .
N1' N 0.57271(10) 0.79400(17) 0.61239(11) 0.0193(6) Uani 1 1 d . . .
C2' C 0.59967(12) 0.82757(19) 0.57482(14) 0.0183(6) Uani 1 1 d . . .
P3' P 0.59118(3) 0.78486(5) 0.50128(3) 0.01521(15) Uani 1 1 d . . .
C3A' C 0.54942(11) 0.71346(18) 0.53161(13) 0.0149(6) Uani 1 1 d . . .
N4' N 0.52441(9) 0.65551(15) 0.50394(11) 0.0149(5) Uani 1 1 d . . .
C5' C 0.49372(12) 0.61116(19) 0.53487(14) 0.0187(6) Uani 1 1 d . . .
H5' H 0.4761 0.5695 0.5161 0.022 Uiso 1 1 calc R . .
C6' C 0.48663(12) 0.6238(2) 0.59361(13) 0.0194(6) Uani 1 1 d . . .
H6' H 0.4647 0.5910 0.6141 0.023 Uiso 1 1 calc R . .
C7' C 0.51202(12) 0.6849(2) 0.62170(14) 0.0200(7) Uani 1 1 d . . .
H7' H 0.5076 0.6953 0.6614 0.024 Uiso 1 1 calc R . .
C7A' C 0.54397(11) 0.73010(19) 0.58959(13) 0.0167(6) Uani 1 1 d . . .
C8' C 0.63180(12) 0.8987(2) 0.58930(14) 0.0203(6) Uani 1 1 d . . .
C9' C 0.67859(13) 0.8963(2) 0.55496(16) 0.0287(8) Uani 1 1 d . . .
H9'1 H 0.6986 0.9428 0.5652 0.043 Uiso 1 1 calc R . .
H9'2 H 0.6708 0.8979 0.5138 0.043 Uiso 1 1 calc R . .
H9'3 H 0.6962 0.8466 0.5639 0.043 Uiso 1 1 calc R . .
C10' C 0.60379(15) 0.9754(2) 0.57398(18) 0.0321(9) Uani 1 1 d . . .
H10D H 0.6237 1.0225 0.5831 0.048 Uiso 1 1 calc R . .
H10E H 0.5741 0.9775 0.5962 0.048 Uiso 1 1 calc R . .
H10F H 0.5957 0.9752 0.5329 0.048 Uiso 1 1 calc R . .
C11' C 0.64465(14) 0.8973(2) 0.65306(15) 0.0280(8) Uani 1 1 d . . .
H11D H 0.6654 0.9433 0.6625 0.042 Uiso 1 1 calc R . .
H11E H 0.6618 0.8472 0.6623 0.042 Uiso 1 1 calc R . .
H11F H 0.6151 0.9003 0.6754 0.042 Uiso 1 1 calc R . .
C12' C 0.64505(12) 0.7286(2) 0.48358(14) 0.0202(6) Uani 1 1 d . . .
H12C H 0.6376 0.6924 0.4508 0.024 Uiso 1 1 calc R . .
H12D H 0.6703 0.7666 0.4712 0.024 Uiso 1 1 calc R . .
C13' C 0.66483(12) 0.6783(2) 0.53361(15) 0.0229(7) Uani 1 1 d . . .
H13C H 0.6694 0.7132 0.5677 0.028 Uiso 1 1 calc R . .
H13D H 0.6411 0.6362 0.5434 0.028 Uiso 1 1 calc R . .
C14' C 0.71229(14) 0.6391(2) 0.51907(17) 0.0321(8) Uani 1 1 d . . .
H14C H 0.7071 0.6017 0.4865 0.038 Uiso 1 1 calc R . .
H14D H 0.7352 0.6811 0.5067 0.038 Uiso 1 1 calc R . .
C15' C 0.73420(15) 0.5934(3) 0.5688(2) 0.0415(11) Uani 1 1 d . . .
H15D H 0.7647 0.5690 0.5571 0.062 Uiso 1 1 calc R . .
H15E H 0.7119 0.5510 0.5808 0.062 Uiso 1 1 calc R . .
H15F H 0.7402 0.6303 0.6009 0.062 Uiso 1 1 calc R . .
O111 O 0.5000 0.7711(2) 0.7500 0.0251(7) Uani 1 2 d SU . .
C112 C 0.54131(13) 0.8213(2) 0.76048(16) 0.0272(8) Uani 1 1 d U . .
H11G H 0.5689 0.8029 0.7374 0.033 Uiso 1 1 calc R . .
H11H H 0.5509 0.8196 0.8016 0.033 Uiso 1 1 calc R . .
C113 C 0.52658(13) 0.9056(2) 0.74321(17) 0.0296(8) Uani 1 1 d U . .
H11I H 0.5443 0.9466 0.7660 0.036 Uiso 1 1 calc R . .
H11J H 0.5319 0.9153 0.7019 0.036 Uiso 1 1 calc R . .
O121 O 0.68883(12) 1.1734(2) 0.39690(14) 0.0471(8) Uani 1 1 d DU . .
C122 C 0.70500(15) 1.0918(3) 0.40063(17) 0.0357(9) Uani 1 1 d DU . .
H12E H 0.6832 1.0602 0.4252 0.043 Uiso 1 1 calc R . .
H12F H 0.7379 1.0896 0.4176 0.043 Uiso 1 1 calc R . .
C123 C 0.70492(14) 1.0580(3) 0.34094(17) 0.0363(9) Uani 1 1 d DU . .
H12G H 0.6986 0.9994 0.3407 0.044 Uiso 1 1 calc R . .
H12H H 0.7355 1.0692 0.3212 0.044 Uiso 1 1 calc R . .
C124 C 0.66244(19) 1.1059(3) 0.3145(2) 0.0517(12) Uani 1 1 d DU . .
H12I H 0.6646 1.1088 0.2722 0.062 Uiso 1 1 calc R . .
H12J H 0.6310 1.0821 0.3249 0.062 Uiso 1 1 calc R . .
C125 C 0.6695(2) 1.1868(3) 0.3416(2) 0.0531(13) Uani 1 1 d DU . .
H12K H 0.6920 1.2197 0.3187 0.064 Uiso 1 1 calc R . .
H12L H 0.6384 1.2156 0.3439 0.064 Uiso 1 1 calc R . .
O131 O 0.59785(13) 0.6287(2) 0.70218(16) 0.0610(10) Uani 1 1 d DU . .
C132 C 0.64589(17) 0.6539(3) 0.7130(2) 0.0479(12) Uani 1 1 d DU . .
H13E H 0.6467 0.7108 0.7255 0.057 Uiso 1 1 calc R . .
H13F H 0.6655 0.6482 0.6781 0.057 Uiso 1 1 calc R . .
C133 C 0.66434(18) 0.5997(3) 0.7598(2) 0.0533(13) Uani 1 1 d DU . .
H13G H 0.6909 0.6253 0.7820 0.064 Uiso 1 1 calc R . .
H13H H 0.6756 0.5477 0.7442 0.064 Uiso 1 1 calc R . .
C134 C 0.61967(19) 0.5889(3) 0.7962(2) 0.0601(14) Uani 1 1 d DU . .
H13I H 0.6185 0.5340 0.8126 0.072 Uiso 1 1 calc R . .
H13J H 0.6193 0.6285 0.8279 0.072 Uiso 1 1 calc R . .
C135 C 0.57810(19) 0.6027(3) 0.7553(2) 0.0548(13) Uani 1 1 d DU . .
H13K H 0.5596 0.5523 0.7496 0.066 Uiso 1 1 calc R . .
H13L H 0.5562 0.6442 0.7706 0.066 Uiso 1 1 calc R . .
O141 O 0.73993(16) 1.0706(2) 0.6213(2) 0.0780(13) Uani 1 1 d DU . .
C142 C 0.71559(19) 1.1447(3) 0.6127(2) 0.0540(13) Uani 1 1 d DU . .
H14E H 0.7238 1.1829 0.6440 0.065 Uiso 1 1 calc R . .
H14F H 0.6802 1.1363 0.6120 0.065 Uiso 1 1 calc R . .
C143 C 0.7317(2) 1.1761(5) 0.5572(3) 0.085(2) Uani 1 1 d DU . .
H14G H 0.7332 1.2356 0.5574 0.102 Uiso 1 1 calc R . .
H14H H 0.7102 1.1582 0.5254 0.102 Uiso 1 1 calc R . .
C144 C 0.7817(3) 1.1397(5) 0.5521(3) 0.098(2) Uani 1 1 d DU . .
H14I H 0.7894 1.1294 0.5114 0.117 Uiso 1 1 calc R . .
H14J H 0.8065 1.1758 0.5689 0.117 Uiso 1 1 calc R . .
C145 C 0.7791(2) 1.0677(4) 0.5829(3) 0.088(2) Uani 1 1 d DU . .
H14K H 0.8096 1.0591 0.6047 0.105 Uiso 1 1 calc R . .
H14L H 0.7747 1.0221 0.5560 0.105 Uiso 1 1 calc R . .
O151 O 0.7489(2) 0.6769(3) 0.2729(3) 0.0668(19) Uani 0.652(6) 1 d PDU A 1
C152 C 0.7222(3) 0.6108(4) 0.2934(3) 0.0435(17) Uani 0.652(6) 1 d PDU A 1
H15G H 0.7442 0.5683 0.3081 0.052 Uiso 0.652(6) 1 calc PR A 1
H15H H 0.7018 0.5878 0.2622 0.052 Uiso 0.652(6) 1 calc PR A 1
C153 C 0.6916(3) 0.6425(4) 0.3404(4) 0.050(2) Uani 0.652(6) 1 d PDU A 1
H15I H 0.7097 0.6447 0.3774 0.060 Uiso 0.652(6) 1 calc PR A 1
H15J H 0.6622 0.6095 0.3452 0.060 Uiso 0.652(6) 1 calc PR A 1
C154 C 0.6794(3) 0.7262(5) 0.3187(4) 0.060(2) Uani 0.652(6) 1 d PDU A 1
H15K H 0.6479 0.7266 0.2981 0.071 Uiso 0.652(6) 1 calc PR A 1
H15L H 0.6784 0.7653 0.3507 0.071 Uiso 0.652(6) 1 calc PR A 1
C155 C 0.7201(4) 0.7449(5) 0.2787(5) 0.068(3) Uani 0.652(6) 1 d PDU A 1
H15M H 0.7068 0.7611 0.2407 0.082 Uiso 0.652(6) 1 calc PR A 1
H15N H 0.7396 0.7900 0.2942 0.082 Uiso 0.652(6) 1 calc PR A 1
O161 O 0.7404(5) 0.7117(9) 0.3523(6) 0.103(5) Uiso 0.348(6) 1 d PDU A 2
C162 C 0.7183(6) 0.6360(9) 0.3501(7) 0.059(4) Uiso 0.348(6) 1 d PDU A 2
H16A H 0.6998 0.6266 0.3855 0.071 Uiso 0.348(6) 1 calc PR A 2
H16B H 0.7430 0.5933 0.3470 0.071 Uiso 0.348(6) 1 calc PR A 2
C163 C 0.6860(6) 0.6340(9) 0.3000(8) 0.068(5) Uiso 0.348(6) 1 d PDU A 2
H16C H 0.6548 0.6088 0.3095 0.081 Uiso 0.348(6) 1 calc PR A 2
H16D H 0.7007 0.6038 0.2681 0.081 Uiso 0.348(6) 1 calc PR A 2
C164 C 0.6792(7) 0.7224(10) 0.2840(9) 0.079(5) Uiso 0.348(6) 1 d PDU A 2
H16E H 0.6790 0.7298 0.2419 0.094 Uiso 0.348(6) 1 calc PR A 2
H16F H 0.6487 0.7438 0.2996 0.094 Uiso 0.348(6) 1 calc PR A 2
C165 C 0.7214(7) 0.7621(10) 0.3110(9) 0.079(5) Uiso 0.348(6) 1 d PDU A 2
H16G H 0.7459 0.7736 0.2816 0.094 Uiso 0.348(6) 1 calc PR A 2
H16H H 0.7116 0.8136 0.3286 0.094 Uiso 0.348(6) 1 calc PR A 2


_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 N4' 2.048(3) . ?
Pd1 P3 2.2397(9) . ?
Pd1 Cl1 2.2725(9) . ?
Pd1 Cl2 2.3396(8) . ?
Pd2 N4 2.038(3) . ?
Pd2 P3' 2.2396(9) . ?
Pd2 Cl3 2.2704(9) . ?
Pd2 Cl4 2.3346(8) . ?
N1 C2 1.284(4) . ?
N1 C7A 1.424(4) . ?
C2 C8 1.513(5) . ?
C2 P3 1.865(3) . ?
P3 C3A 1.808(3) . ?
P3 C12 1.821(3) . ?
C3A N4 1.345(4) . ?
C3A C7A 1.393(4) . ?
N4 C5 1.354(4) . ?
C5 C6 1.397(4) . ?
C6 C7 1.381(5) . ?
C7 C7A 1.389(4) . ?
C8 C11 1.525(5) . ?
C8 C9 1.532(5) . ?
C8 C10 1.535(5) . ?
C12 C13 1.522(5) . ?
C13 C14 1.527(4) . ?
C14 C15 1.515(5) . ?
N1' C2' 1.287(4) . ?
N1' C7A' 1.426(4) . ?
C2' C8' 1.515(5) . ?
C2' P3' 1.866(3) . ?
P3' C3A' 1.810(3) . ?
P3' C12' 1.816(3) . ?
C3A' N4' 1.346(4) . ?
C3A' C7A' 1.390(4) . ?
N4' C5' 1.344(4) . ?
C5' C6' 1.402(4) . ?
C6' C7' 1.393(5) . ?
C7' C7A' 1.389(4) . ?
C8' C11' 1.523(5) . ?
C8' C10' 1.533(5) . ?
C8' C9' 1.535(5) . ?
C12' C13' 1.529(5) . ?
C13' C14' 1.512(5) . ?
C14' C15' 1.506(5) . ?
O111 C112 1.435(4) . ?
O111 C112 1.435(4) 2_656 ?
C112 C113 1.513(5) . ?
C113 C113 1.512(7) 2_656 ?
O121 C125 1.405(5) . ?
O121 C122 1.432(5) . ?
C122 C123 1.500(5) . ?
C123 C124 1.542(6) . ?
C124 C125 1.498(6) . ?
O131 C132 1.415(6) . ?
O131 C135 1.427(6) . ?
C132 C133 1.499(6) . ?
C133 C134 1.522(7) . ?
C134 C135 1.502(7) . ?
O141 C142 1.418(6) . ?
O141 C145 1.418(6) . ?
C142 C143 1.471(7) . ?
C143 C144 1.518(7) . ?
C144 C145 1.399(7) . ?
O151 C155 1.392(8) . ?
O151 C152 1.412(7) . ?
C152 C153 1.493(8) . ?
C153 C154 1.517(9) . ?
C154 C155 1.508(9) . ?
O161 C165 1.375(12) . ?
O161 C162 1.401(12) . ?
C162 C163 1.462(13) . ?
C163 C164 1.526(13) . ?
C164 C165 1.476(13) . ?

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
N4' Pd1 P3 90.62(8) . . ?
N4' Pd1 Cl1 178.70(8) . . ?
P3 Pd1 Cl1 88.39(3) . . ?
N4' Pd1 Cl2 89.47(8) . . ?
P3 Pd1 Cl2 176.55(3) . . ?
Cl1 Pd1 Cl2 91.57(3) . . ?
N4 Pd2 P3' 90.78(7) . . ?
N4 Pd2 Cl3 177.85(8) . . ?
P3' Pd2 Cl3 88.49(3) . . ?
N4 Pd2 Cl4 89.30(7) . . ?
P3' Pd2 Cl4 178.67(3) . . ?
Cl3 Pd2 Cl4 91.38(3) . . ?
C2 N1 C7A 113.0(3) . . ?
N1 C2 C8 122.0(3) . . ?
N1 C2 P3 113.7(2) . . ?
C8 C2 P3 124.1(2) . . ?
C3A P3 C12 106.86(15) . . ?
C3A P3 C2 87.61(15) . . ?
C12 P3 C2 107.96(15) . . ?
C3A P3 Pd1 112.92(10) . . ?
C12 P3 Pd1 122.68(11) . . ?
C2 P3 Pd1 113.13(11) . . ?
N4 C3A C7A 122.7(3) . . ?
N4 C3A P3 127.8(2) . . ?
C7A C3A P3 109.3(2) . . ?
C3A N4 C5 117.6(3) . . ?
C3A N4 Pd2 121.7(2) . . ?
C5 N4 Pd2 120.6(2) . . ?
N4 C5 C6 122.3(3) . . ?
C7 C6 C5 119.8(3) . . ?
C6 C7 C7A 117.9(3) . . ?
C7 C7A C3A 119.6(3) . . ?
C7 C7A N1 124.2(3) . . ?
C3A C7A N1 116.2(3) . . ?
C2 C8 C11 109.7(3) . . ?
C2 C8 C9 111.1(3) . . ?
C11 C8 C9 109.7(3) . . ?
C2 C8 C10 107.6(3) . . ?
C11 C8 C10 110.2(3) . . ?
C9 C8 C10 108.6(3) . . ?
C13 C12 P3 113.5(2) . . ?
C12 C13 C14 111.5(3) . . ?
C15 C14 C13 112.2(3) . . ?
C2' N1' C7A' 113.4(3) . . ?
N1' C2' C8' 122.2(3) . . ?
N1' C2' P3' 113.2(2) . . ?
C8' C2' P3' 124.5(2) . . ?
C3A' P3' C12' 106.51(15) . . ?
C3A' P3' C2' 87.90(14) . . ?
C12' P3' C2' 108.20(15) . . ?
C3A' P3' Pd2 113.22(10) . . ?
C12' P3' Pd2 122.04(11) . . ?
C2' P3' Pd2 113.56(11) . . ?
N4' C3A' C7A' 123.0(3) . . ?
N4' C3A' P3' 127.6(2) . . ?
C7A' C3A' P3' 109.2(2) . . ?
C5' N4' C3A' 117.5(3) . . ?
C5' N4' Pd1 121.7(2) . . ?
C3A' N4' Pd1 120.8(2) . . ?
N4' C5' C6' 122.7(3) . . ?
C7' C6' C5' 119.4(3) . . ?
C7A' C7' C6' 117.6(3) . . ?
C7' C7A' C3A' 119.7(3) . . ?
C7' C7A' N1' 124.0(3) . . ?
C3A' C7A' N1' 116.2(3) . . ?
C2' C8' C11' 109.5(3) . . ?
C2' C8' C10' 107.7(3) . . ?
C11' C8' C10' 110.5(3) . . ?
C2' C8' C9' 111.2(3) . . ?
C11' C8' C9' 108.8(3) . . ?
C10' C8' C9' 109.2(3) . . ?
C13' C12' P3' 113.3(2) . . ?
C14' C13' C12' 111.6(3) . . ?
C15' C14' C13' 112.8(3) . . ?
C112 O111 C112 108.9(4) . 2_656 ?
O111 C112 C113 106.4(3) . . ?
C113 C113 C112 101.8(2) 2_656 . ?
C125 O121 C122 108.7(3) . . ?
O121 C122 C123 107.6(3) . . ?
C122 C123 C124 99.6(3) . . ?
C125 C124 C123 101.6(4) . . ?
O121 C125 C124 106.8(4) . . ?
C132 O131 C135 108.0(4) . . ?
O131 C132 C133 105.1(4) . . ?
C132 C133 C134 101.8(4) . . ?
C135 C134 C133 104.5(4) . . ?
O131 C135 C134 107.2(4) . . ?
C142 O141 C145 108.0(4) . . ?
O141 C142 C143 106.4(4) . . ?
C142 C143 C144 102.6(5) . . ?
C145 C144 C143 104.3(5) . . ?
C144 C145 O141 109.9(5) . . ?
C155 O151 C152 107.2(5) . . ?
O151 C152 C153 106.2(5) . . ?
C152 C153 C154 101.9(6) . . ?
C155 C154 C153 103.3(6) . . ?
O151 C155 C154 109.2(6) . . ?
C165 O161 C162 111.1(11) . . ?
O161 C162 C163 108.1(11) . . ?
C162 C163 C164 104.2(10) . . ?
C165 C164 C163 103.5(10) . . ?
O161 C165 C164 108.5(12) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_full 0.977
_refine_diff_density_max         1.331
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.124

####################################################################### 
# 
# 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_shaker
_database_code_depnum_ccdc_archive 'CCDC 1423104'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-11-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C34 H42 D12 Cl4 N4 O2 P2 Pd2'
_chemical_formula_weight         979.43

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'
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'
O O 0.0106 0.0060 '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/c'

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

_cell_length_a                   11.9584(4)
_cell_length_b                   29.4872(8)
_cell_length_c                   13.0738(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.816(5)
_cell_angle_gamma                90.00
_cell_volume                     4150.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    18418
_cell_measurement_theta_min      2.6899
_cell_measurement_theta_max      30.6071

_exptl_crystal_description       tablet
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1968
_exptl_absorpt_coefficient_mu    1.236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.95193
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 16.1057
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            76588
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.0888
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         28.28
_reflns_number_total             10287
_reflns_number_gt                6543
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.13 (release 29-11-2007 CrysAlis171 .NET)
(compiled Nov 29 2007,17:23:28)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97

_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)+(0.0199P)²] 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         10287
_refine_ls_number_parameters     445
_refine_ls_number_restraints     266
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0516
_refine_ls_wR_factor_gt          0.0481
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_restrained_S_all      0.814
_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 0.62989(2) 0.553425(6) 0.722982(17) 0.01308(5) Uani 1 1 d . . .
Pd2 Pd 0.72132(2) 0.684537(6) 0.783648(17) 0.01424(5) Uani 1 1 d . . .
Cl1 Cl 0.71747(7) 0.52005(2) 0.89757(6) 0.02232(16) Uani 1 1 d . . .
Cl2 Cl 0.43245(6) 0.52735(2) 0.68910(6) 0.01865(15) Uani 1 1 d . . .
Cl3 Cl 0.65007(7) 0.70402(2) 0.91329(6) 0.02451(17) Uani 1 1 d . . .
Cl4 Cl 0.91924(7) 0.71281(2) 0.89728(6) 0.02461(17) Uani 1 1 d . . .
N1 N 0.8879(2) 0.56146(7) 0.58516(18) 0.0154(5) Uani 1 1 d U . .
C2 C 0.8820(2) 0.54007(8) 0.6686(2) 0.0152(6) Uani 1 1 d U . .
P3 P 0.82034(7) 0.57551(2) 0.75036(6) 0.01394(15) Uani 1 1 d . . .
C3A C 0.8172(2) 0.62272(8) 0.6607(2) 0.0119(6) Uani 1 1 d U . .
N4 N 0.77961(19) 0.66557(7) 0.66453(17) 0.0130(5) Uani 1 1 d U . .
C5 C 0.7800(2) 0.69463(8) 0.5851(2) 0.0161(6) Uani 1 1 d U . .
H5 H 0.7563 0.7252 0.5873 0.019 Uiso 1 1 calc R . .
C6 C 0.8136(2) 0.68182(9) 0.5010(2) 0.0174(6) Uani 1 1 d U . .
H6 H 0.8119 0.7034 0.4464 0.021 Uiso 1 1 calc R . .
C7 C 0.8497(2) 0.63765(8) 0.4954(2) 0.0175(6) Uani 1 1 d U . .
H7 H 0.8719 0.6282 0.4372 0.021 Uiso 1 1 calc R . .
C7A C 0.8521(2) 0.60785(8) 0.5782(2) 0.0141(6) Uani 1 1 d U . .
C8 C 0.9126(3) 0.48990(8) 0.6882(2) 0.0167(6) Uani 1 1 d U . .
C9 C 0.9858(3) 0.48043(9) 0.8152(2) 0.0263(7) Uani 1 1 d U . .
H9A H 1.0613 0.4990 0.8460 0.039 Uiso 1 1 calc R . .
H9B H 1.0085 0.4483 0.8267 0.039 Uiso 1 1 calc R . .
H9C H 0.9345 0.4879 0.8543 0.039 Uiso 1 1 calc R . .
C10 C 0.7895(3) 0.46375(9) 0.6432(2) 0.0259(7) Uani 1 1 d U . .
H10A H 0.7414 0.4737 0.6835 0.039 Uiso 1 1 calc R . .
H10B H 0.8066 0.4312 0.6555 0.039 Uiso 1 1 calc R . .
H10C H 0.7420 0.4696 0.5617 0.039 Uiso 1 1 calc R . .
C11 C 0.9868(3) 0.47473(9) 0.6252(3) 0.0329(8) Uani 1 1 d U . .
H11A H 0.9384 0.4803 0.5436 0.049 Uiso 1 1 calc R . .
H11B H 1.0051 0.4423 0.6381 0.049 Uiso 1 1 calc R . .
H11C H 1.0648 0.4918 0.6530 0.049 Uiso 1 1 calc R . .
C12 C 0.9398(2) 0.58710(8) 0.8924(2) 0.0162(6) Uani 1 1 d U . .
H12A H 0.9092 0.6112 0.9265 0.019 Uiso 1 1 calc R . .
H12B H 0.9522 0.5594 0.9391 0.019 Uiso 1 1 calc R . .
C13 C 1.0644(3) 0.60166(10) 0.8998(2) 0.0254(7) Uani 1 1 d U . .
H13A H 1.0575 0.6329 0.8702 0.031 Uiso 1 1 calc R . .
H13B H 1.0870 0.5816 0.8511 0.031 Uiso 1 1 calc R . .
C14 C 1.1673(3) 0.60008(10) 1.0209(3) 0.0321(8) Uani 1 1 d U . .
H14A H 1.2466 0.6093 1.0204 0.039 Uiso 1 1 calc R . .
H14B H 1.1768 0.5685 1.0493 0.039 Uiso 1 1 calc R . .
C15 C 1.1408(3) 0.63139(11) 1.1027(3) 0.0405(9) Uani 1 1 d U . .
H15A H 1.1320 0.6627 1.0753 0.061 Uiso 1 1 calc R . .
H15B H 1.2098 0.6295 1.1788 0.061 Uiso 1 1 calc R . .
H15C H 1.0638 0.6218 1.1056 0.061 Uiso 1 1 calc R . .
N1' N 0.4368(2) 0.69644(6) 0.45577(17) 0.0152(5) Uani 1 1 d U . .
C2' C 0.4548(2) 0.70986(8) 0.5548(2) 0.0146(6) Uani 1 1 d U . .
P3' P 0.52584(7) 0.66545(2) 0.66683(6) 0.01368(15) Uani 1 1 d . . .
C3A' C 0.5161(2) 0.62732(8) 0.5558(2) 0.0124(6) Uani 1 1 d U . .
N4' N 0.55470(19) 0.58370(6) 0.56762(17) 0.0123(5) Uani 1 1 d U . .
C5' C 0.5446(2) 0.56195(8) 0.4730(2) 0.0152(6) Uani 1 1 d U . .
H5' H 0.5702 0.5312 0.4790 0.018 Uiso 1 1 calc R . .
C6' C 0.4987(2) 0.58274(8) 0.3681(2) 0.0178(6) Uani 1 1 d U . .
H6' H 0.4920 0.5661 0.3035 0.021 Uiso 1 1 calc R . .
C7' C 0.4622(3) 0.62800(9) 0.3567(2) 0.0189(6) Uani 1 1 d U . .
H7' H 0.4330 0.6431 0.2856 0.023 Uiso 1 1 calc R . .
C7A' C 0.4702(2) 0.65014(8) 0.4529(2) 0.0144(6) Uani 1 1 d U . .
C8' C 0.4311(3) 0.75827(8) 0.5798(2) 0.0174(6) Uani 1 1 d U . .
C9' C 0.3606(3) 0.75932(9) 0.6529(2) 0.0254(7) Uani 1 1 d U . .
H9'1 H 0.2838 0.7417 0.6158 0.038 Uiso 1 1 calc R . .
H9'2 H 0.3401 0.7908 0.6622 0.038 Uiso 1 1 calc R . .
H9'3 H 0.4124 0.7462 0.7276 0.038 Uiso 1 1 calc R . .
C10' C 0.5574(3) 0.78209(8) 0.6444(2) 0.0230(7) Uani 1 1 d U . .
H10D H 0.6074 0.7652 0.7140 0.034 Uiso 1 1 calc R . .
H10E H 0.5438 0.8130 0.6641 0.034 Uiso 1 1 calc R . .
H10F H 0.6012 0.7832 0.5962 0.034 Uiso 1 1 calc R . .
C11' C 0.3573(3) 0.78349(9) 0.4685(2) 0.0252(7) Uani 1 1 d U . .
H11D H 0.4036 0.7830 0.4224 0.038 Uiso 1 1 calc R . .
H11E H 0.3443 0.8150 0.4849 0.038 Uiso 1 1 calc R . .
H11F H 0.2767 0.7686 0.4268 0.038 Uiso 1 1 calc R . .
C12' C 0.4108(2) 0.64629(8) 0.7131(2) 0.0161(6) Uani 1 1 d U . .
H12C H 0.4433 0.6192 0.7621 0.019 Uiso 1 1 calc R . .
H12D H 0.3977 0.6704 0.7595 0.019 Uiso 1 1 calc R . .
C13' C 0.2855(2) 0.63437(9) 0.6139(2) 0.0183(6) Uani 1 1 d U . .
H13C H 0.2602 0.6593 0.5575 0.022 Uiso 1 1 calc R . .
H13D H 0.2952 0.6066 0.5760 0.022 Uiso 1 1 calc R . .
C14' C 0.1844(3) 0.62680(9) 0.6525(2) 0.0258(7) Uani 1 1 d U . .
H14C H 0.2162 0.6062 0.7190 0.031 Uiso 1 1 calc R . .
H14D H 0.1129 0.6117 0.5907 0.031 Uiso 1 1 calc R . .
C15' C 0.1403(3) 0.67046(9) 0.6843(2) 0.0272(7) Uani 1 1 d U . .
H15D H 0.2109 0.6859 0.7445 0.041 Uiso 1 1 calc R . .
H15E H 0.0777 0.6635 0.7115 0.041 Uiso 1 1 calc R . .
H15F H 0.1037 0.6902 0.6175 0.041 Uiso 1 1 calc R . .
O1 O 0.5013(3) 0.89124(8) 0.6371(2) 0.0565(8) Uani 1 1 d U . .
C94 C 0.4556(4) 0.93875(13) 0.4790(3) 0.0634(12) Uani 1 1 d U . .
H94A H 0.4229 0.9683 0.4870 0.095 Uiso 1 1 calc R . .
H94B H 0.3866 0.9177 0.4406 0.095 Uiso 1 1 calc R . .
H94C H 0.5027 0.9421 0.4341 0.095 Uiso 1 1 calc R . .
C95 C 0.5393(4) 0.92057(11) 0.5944(3) 0.0427(9) Uani 1 1 d U . .
C96 C 0.6654(3) 0.94134(11) 0.6568(3) 0.0511(10) Uani 1 1 d U . .
H96A H 0.7081 0.9272 0.7318 0.077 Uiso 1 1 calc R . .
H96B H 0.6568 0.9740 0.6658 0.077 Uiso 1 1 calc R . .
H96C H 0.7139 0.9364 0.6136 0.077 Uiso 1 1 calc R . .
O2 O 0.9513(3) 0.35508(8) 0.6500(2) 0.0632(8) Uani 1 1 d U . .
C97 C 0.9251(3) 0.28838(11) 0.7391(3) 0.0573(11) Uani 1 1 d U . .
H97A H 0.8362 0.2953 0.7002 0.086 Uiso 1 1 calc R . .
H97B H 0.9501 0.2853 0.8208 0.086 Uiso 1 1 calc R . .
H97C H 0.9416 0.2599 0.7094 0.086 Uiso 1 1 calc R . .
C98 C 0.9964(3) 0.32535(11) 0.7194(3) 0.0388(9) Uani 1 1 d U . .
C99 C 1.1324(3) 0.32294(12) 0.7878(3) 0.0507(10) Uani 1 1 d U . .
H99A H 1.1712 0.3498 0.7729 0.076 Uiso 1 1 calc R . .
H99B H 1.1645 0.2956 0.7673 0.076 Uiso 1 1 calc R . .
H99C H 1.1515 0.3218 0.8687 0.076 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 N4' 2.035(2) . ?
Pd1 P3 2.2427(8) . ?
Pd1 Cl1 2.2789(7) . ?
Pd1 Cl2 2.3347(7) . ?
Pd2 N4 2.042(2) . ?
Pd2 P3' 2.2370(8) . ?
Pd2 Cl3 2.2774(7) . ?
Pd2 Cl4 2.3327(7) . ?
N1 C2 1.288(3) . ?
N1 C7A 1.424(3) . ?
C2 C8 1.519(3) . ?
C2 P3 1.862(3) . ?
P3 C3A 1.809(2) . ?
P3 C12 1.816(3) . ?
C3A N4 1.349(3) . ?
C3A C7A 1.387(3) . ?
N4 C5 1.348(3) . ?
C5 C6 1.378(3) . ?
C6 C7 1.384(3) . ?
C7 C7A 1.384(3) . ?
C8 C11 1.518(4) . ?
C8 C9 1.528(3) . ?
C8 C10 1.534(4) . ?
C12 C13 1.513(4) . ?
C13 C14 1.525(4) . ?
C14 C15 1.546(4) . ?
N1' C2' 1.279(3) . ?
N1' C7A' 1.428(3) . ?
C2' C8' 1.518(3) . ?
C2' P3' 1.871(3) . ?
P3' C3A' 1.799(3) . ?
P3' C12' 1.817(3) . ?
C3A' N4' 1.353(3) . ?
C3A' C7A' 1.386(3) . ?
N4' C5' 1.351(3) . ?
C5' C6' 1.379(3) . ?
C6' C7' 1.392(3) . ?
C7' C7A' 1.383(3) . ?
C8' C9' 1.525(4) . ?
C8' C11' 1.527(3) . ?
C8' C10' 1.541(4) . ?
C12' C13' 1.536(3) . ?
C13' C14' 1.516(4) . ?
C14' C15' 1.517(4) . ?
O1 C95 1.220(4) . ?
C94 C95 1.500(5) . ?
C95 C96 1.498(5) . ?
O2 C98 1.207(3) . ?
C97 C98 1.474(5) . ?
C98 C99 1.477(5) . ?

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
N4' Pd1 P3 90.48(6) . . ?
N4' Pd1 Cl1 178.97(7) . . ?
P3 Pd1 Cl1 88.50(3) . . ?
N4' Pd1 Cl2 89.11(6) . . ?
P3 Pd1 Cl2 177.11(3) . . ?
Cl1 Pd1 Cl2 91.92(3) . . ?
N4 Pd2 P3' 90.73(6) . . ?
N4 Pd2 Cl3 177.89(6) . . ?
P3' Pd2 Cl3 87.32(3) . . ?
N4 Pd2 Cl4 89.71(6) . . ?
P3' Pd2 Cl4 173.46(3) . . ?
Cl3 Pd2 Cl4 92.32(3) . . ?
C2 N1 C7A 113.5(2) . . ?
N1 C2 C8 121.5(2) . . ?
N1 C2 P3 113.12(19) . . ?
C8 C2 P3 125.21(19) . . ?
C3A P3 C12 107.63(11) . . ?
C3A P3 C2 87.82(12) . . ?
C12 P3 C2 111.18(12) . . ?
C3A P3 Pd1 112.75(9) . . ?
C12 P3 Pd1 120.66(9) . . ?
C2 P3 Pd1 111.95(9) . . ?
N4 C3A C7A 122.8(2) . . ?
N4 C3A P3 127.6(2) . . ?
C7A C3A P3 109.41(18) . . ?
C5 N4 C3A 117.0(2) . . ?
C5 N4 Pd2 122.02(17) . . ?
C3A N4 Pd2 120.94(17) . . ?
N4 C5 C6 122.7(2) . . ?
C5 C6 C7 120.4(2) . . ?
C6 C7 C7A 117.2(2) . . ?
C7 C7A C3A 119.8(2) . . ?
C7 C7A N1 124.3(2) . . ?
C3A C7A N1 115.9(2) . . ?
C11 C8 C2 110.5(2) . . ?
C11 C8 C9 110.0(2) . . ?
C2 C8 C9 110.1(2) . . ?
C11 C8 C10 109.5(2) . . ?
C2 C8 C10 107.7(2) . . ?
C9 C8 C10 109.0(2) . . ?
C13 C12 P3 115.66(19) . . ?
C12 C13 C14 112.6(2) . . ?
C13 C14 C15 112.6(2) . . ?
C2' N1' C7A' 113.4(2) . . ?
N1' C2' C8' 123.0(2) . . ?
N1' C2' P3' 113.26(18) . . ?
C8' C2' P3' 123.57(18) . . ?
C3A' P3' C12' 106.36(12) . . ?
C3A' P3' C2' 87.59(11) . . ?
C12' P3' C2' 109.09(12) . . ?
C3A' P3' Pd2 112.93(9) . . ?
C12' P3' Pd2 124.62(9) . . ?
C2' P3' Pd2 109.99(9) . . ?
N4' C3A' C7A' 122.9(2) . . ?
N4' C3A' P3' 127.12(19) . . ?
C7A' C3A' P3' 109.81(18) . . ?
C5' N4' C3A' 117.2(2) . . ?
C5' N4' Pd1 122.00(17) . . ?
C3A' N4' Pd1 120.76(16) . . ?
N4' C5' C6' 122.5(2) . . ?
C5' C6' C7' 120.2(2) . . ?
C7A' C7' C6' 117.4(2) . . ?
C7' C7A' C3A' 119.7(2) . . ?
C7' C7A' N1' 124.5(2) . . ?
C3A' C7A' N1' 115.8(2) . . ?
C2' C8' C9' 111.1(2) . . ?
C2' C8' C11' 109.7(2) . . ?
C9' C8' C11' 109.8(2) . . ?
C2' C8' C10' 108.4(2) . . ?
C9' C8' C10' 108.9(2) . . ?
C11' C8' C10' 108.8(2) . . ?
C13' C12' P3' 113.02(18) . . ?
C14' C13' C12' 112.2(2) . . ?
C13' C14' C15' 112.9(2) . . ?
O1 C95 C96 121.9(3) . . ?
O1 C95 C94 119.7(4) . . ?
C96 C95 C94 118.3(3) . . ?
O2 C98 C97 124.5(4) . . ?
O2 C98 C99 120.2(3) . . ?
C97 C98 C99 115.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.474
_refine_diff_density_rms         0.092


# start Validation Reply Form
_vrf_CHEMS01_shaker              
;
PROBLEM: The sum formula contains elements in the wrong order.
RESPONSE: The refinement progrm does not interpret D (= deuterium)
correctly!
;
_vrf_PLAT043_shaker              
;
PROBLEM: Calculated and Reported Mol. Weight Differ by .. 12.08 Check
RESPONSE: see above
;
####################################################################### 
# 
# 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_effri
_database_code_depnum_ccdc_archive 'CCDC 1423105'
_audit_update_record             
;
2015-09-08 deposited with the CCDC.
2015-11-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H54 Cl10 N4 P2 Pd3'
_chemical_formula_weight         1278.47

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'
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           Triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.5594(7)
_cell_length_b                   9.6780(8)
_cell_length_c                   16.4206(13)
_cell_angle_alpha                101.959(4)
_cell_angle_beta                 92.199(4)
_cell_angle_gamma                109.528(4)
_cell_volume                     1245.60(18)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9974
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      30.6

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_absorpt_coefficient_mu    1.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8080
_exptl_absorpt_correction_T_max  0.9507
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX2 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            38910
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0247
_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       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         30.58
_reflns_number_total             7630
_reflns_number_gt                6560
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97

_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.

 The hydrogen atoms of the allyl group were refined freely; other hydrogens
 were included using a riding model starting from calculated positions.
;

_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)+(0.0232P)²+1.7489P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7630
_refine_ls_number_parameters     274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0248
_refine_ls_wR_factor_ref         0.0612
_refine_ls_wR_factor_gt          0.0572
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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 0.566573(18) 0.140529(16) 0.856527(9) 0.01373(4) Uani 1 1 d . . .
Cl1 Cl 0.27524(6) 0.03495(6) 0.85481(3) 0.02193(10) Uani 1 1 d . . .
Pd2 Pd 0.5000 0.5000 1.0000 0.01116(4) Uani 1 2 d S . .
Cl2 Cl 0.65679(6) 0.37760(6) 1.05057(3) 0.01936(9) Uani 1 1 d . . .
N1 N 0.80247(19) 0.48648(18) 0.72467(10) 0.0131(3) Uani 1 1 d . . .
C2 C 0.6767(2) 0.3622(2) 0.70925(11) 0.0124(3) Uani 1 1 d . . .
P3 P 0.55508(6) 0.33098(5) 0.79874(3) 0.01095(9) Uani 1 1 d . . .
C3A C 0.6906(2) 0.51571(19) 0.85546(11) 0.0110(3) Uani 1 1 d . . .
N4 N 0.68534(19) 0.58801(17) 0.93353(10) 0.0121(3) Uani 1 1 d . . .
C5 C 0.8066(2) 0.7217(2) 0.96668(12) 0.0156(3) Uani 1 1 d . . .
H5 H 0.8029 0.7750 1.0217 0.019 Uiso 1 1 calc R . .
C6 C 0.9369(2) 0.7835(2) 0.92226(12) 0.0173(4) Uani 1 1 d . . .
H6 H 1.0221 0.8769 0.9477 0.021 Uiso 1 1 calc R . .
C7 C 0.9437(2) 0.7101(2) 0.84107(12) 0.0158(4) Uani 1 1 d . . .
H7 H 1.0322 0.7512 0.8102 0.019 Uiso 1 1 calc R . .
C7A C 0.8162(2) 0.5745(2) 0.80694(11) 0.0124(3) Uani 1 1 d . . .
C8 C 0.6447(2) 0.2448(2) 0.62727(12) 0.0152(3) Uani 1 1 d . . .
C9 C 0.7509(3) 0.1476(2) 0.63677(13) 0.0213(4) Uani 1 1 d . . .
H9A H 0.8683 0.2125 0.6522 0.032 Uiso 1 1 calc R . .
H9B H 0.7394 0.0749 0.5835 0.032 Uiso 1 1 calc R . .
H9C H 0.7128 0.0933 0.6806 0.032 Uiso 1 1 calc R . .
C10 C 0.6977(3) 0.3231(3) 0.55571(13) 0.0245(4) Uani 1 1 d . . .
H10A H 0.6316 0.3869 0.5506 0.037 Uiso 1 1 calc R . .
H10B H 0.6790 0.2470 0.5031 0.037 Uiso 1 1 calc R . .
H10C H 0.8163 0.3855 0.5675 0.037 Uiso 1 1 calc R . .
C11 C 0.4607(3) 0.1433(3) 0.60875(14) 0.0252(5) Uani 1 1 d . . .
H11A H 0.4277 0.0955 0.6555 0.038 Uiso 1 1 calc R . .
H11B H 0.4447 0.0653 0.5573 0.038 Uiso 1 1 calc R . .
H11C H 0.3920 0.2041 0.6016 0.038 Uiso 1 1 calc R . .
C12 C 0.3559(2) 0.3521(2) 0.77214(12) 0.0147(3) Uani 1 1 d . . .
H12A H 0.2814 0.2572 0.7341 0.018 Uiso 1 1 calc R . .
H12B H 0.3025 0.3681 0.8240 0.018 Uiso 1 1 calc R . .
C13 C 0.3726(2) 0.4822(2) 0.73033(13) 0.0172(4) Uani 1 1 d . . .
H13A H 0.4536 0.5761 0.7663 0.021 Uiso 1 1 calc R . .
H13B H 0.4173 0.4625 0.6761 0.021 Uiso 1 1 calc R . .
C14 C 0.2074(3) 0.5044(3) 0.71517(14) 0.0228(4) Uani 1 1 d . . .
H14A H 0.1622 0.5233 0.7693 0.027 Uiso 1 1 calc R . .
H14B H 0.1267 0.4109 0.6787 0.027 Uiso 1 1 calc R . .
C15 C 0.2256(3) 0.6353(3) 0.67424(17) 0.0330(6) Uani 1 1 d . . .
H15A H 0.2999 0.7291 0.7117 0.050 Uiso 1 1 calc R . .
H15B H 0.1158 0.6430 0.6633 0.050 Uiso 1 1 calc R . .
H15C H 0.2729 0.6182 0.6212 0.050 Uiso 1 1 calc R . .
C16 C 0.6470(3) -0.0072(3) 0.92001(18) 0.0317(5) Uani 1 1 d . . .
H16A H 0.582(4) -0.106(4) 0.905(2) 0.038(8) Uiso 1 1 d . . .
H16B H 0.662(4) 0.061(3) 0.977(2) 0.034(8) Uiso 1 1 d . . .
C17 C 0.7616(3) 0.0482(3) 0.86699(17) 0.0304(5) Uani 1 1 d . . .
H17 H 0.767(3) -0.022(3) 0.8129(18) 0.027(7) Uiso 1 1 d . . .
C18 C 0.8304(3) 0.2037(3) 0.87476(15) 0.0237(4) Uani 1 1 d . . .
H18A H 0.856(4) 0.269(3) 0.9279(19) 0.034(8) Uiso 1 1 d . . .
H18B H 0.896(3) 0.245(3) 0.8357(18) 0.027(7) Uiso 1 1 d . . .
C99 C 0.8527(3) 0.7495(3) 0.60772(15) 0.0255(4) Uani 1 1 d . . .
H99 H 0.8671 0.6614 0.6257 0.031 Uiso 1 1 calc R . .
Cl3 Cl 0.64749(7) 0.74110(7) 0.61951(5) 0.03518(14) Uani 1 1 d . . .
Cl4 Cl 0.99626(8) 0.91344(7) 0.67272(5) 0.03601(14) Uani 1 1 d . . .
Cl5 Cl 0.88653(13) 0.73198(14) 0.50305(5) 0.0679(3) 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 C18 2.125(2) . ?
Pd1 C17 2.157(2) . ?
Pd1 C16 2.197(2) . ?
Pd1 P3 2.2685(5) . ?
Pd1 Cl1 2.3542(5) . ?
Pd2 N4 2.0120(15) 2_667 ?
Pd2 N4 2.0121(15) . ?
Pd2 Cl2 2.2976(5) 2_667 ?
Pd2 Cl2 2.2976(5) . ?
N1 C2 1.288(2) . ?
N1 C7A 1.417(2) . ?
C2 C8 1.519(3) . ?
C2 P3 1.8506(19) . ?
P3 C3A 1.8027(18) . ?
P3 C12 1.8305(19) . ?
C3A N4 1.337(2) . ?
C3A C7A 1.400(2) . ?
N4 C5 1.347(2) . ?
C5 C6 1.390(3) . ?
C6 C7 1.388(3) . ?
C7 C7A 1.385(3) . ?
C8 C10 1.530(3) . ?
C8 C11 1.531(3) . ?
C8 C9 1.536(3) . ?
C12 C13 1.524(3) . ?
C13 C14 1.519(3) . ?
C14 C15 1.520(3) . ?
C16 C17 1.384(4) . ?
C17 C18 1.396(4) . ?
C99 Cl5 1.737(3) . ?
C99 Cl4 1.750(2) . ?
C99 Cl3 1.751(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
C18 Pd1 C17 38.05(10) . . ?
C18 Pd1 C16 67.44(10) . . ?
C17 Pd1 C16 37.05(10) . . ?
C18 Pd1 P3 97.89(7) . . ?
C17 Pd1 P3 131.02(7) . . ?
C16 Pd1 P3 165.00(8) . . ?
C18 Pd1 Cl1 167.66(7) . . ?
C17 Pd1 Cl1 131.73(8) . . ?
C16 Pd1 Cl1 100.35(7) . . ?
P3 Pd1 Cl1 94.182(19) . . ?
N4 Pd2 N4 180.0 2_667 . ?
N4 Pd2 Cl2 89.37(5) 2_667 2_667 ?
N4 Pd2 Cl2 90.63(5) . 2_667 ?
N4 Pd2 Cl2 90.63(5) 2_667 . ?
N4 Pd2 Cl2 89.37(5) . . ?
Cl2 Pd2 Cl2 180.0 2_667 . ?
C2 N1 C7A 112.59(16) . . ?
N1 C2 C8 121.76(17) . . ?
N1 C2 P3 114.44(14) . . ?
C8 C2 P3 123.46(14) . . ?
C3A P3 C12 105.39(9) . . ?
C3A P3 C2 87.36(8) . . ?
C12 P3 C2 106.44(9) . . ?
C3A P3 Pd1 114.31(6) . . ?
C12 P3 Pd1 121.33(6) . . ?
C2 P3 Pd1 116.46(6) . . ?
N4 C3A C7A 122.45(16) . . ?
N4 C3A P3 127.97(14) . . ?
C7A C3A P3 109.47(13) . . ?
C3A N4 C5 118.54(16) . . ?
C3A N4 Pd2 120.86(12) . . ?
C5 N4 Pd2 120.59(13) . . ?
N4 C5 C6 121.50(17) . . ?
C7 C6 C5 120.60(18) . . ?
C7A C7 C6 117.37(17) . . ?
C7 C7A C3A 119.50(17) . . ?
C7 C7A N1 124.65(17) . . ?
C3A C7A N1 115.85(16) . . ?
C2 C8 C10 109.74(16) . . ?
C2 C8 C11 111.13(16) . . ?
C10 C8 C11 110.25(18) . . ?
C2 C8 C9 107.25(16) . . ?
C10 C8 C9 109.57(17) . . ?
C11 C8 C9 108.84(17) . . ?
C13 C12 P3 113.70(13) . . ?
C14 C13 C12 112.44(16) . . ?
C13 C14 C15 112.05(18) . . ?
C17 C16 Pd1 69.92(14) . . ?
C16 C17 C18 119.4(2) . . ?
C16 C17 Pd1 73.03(14) . . ?
C18 C17 Pd1 69.71(13) . . ?
C17 C18 Pd1 72.25(14) . . ?
Cl5 C99 Cl4 112.42(14) . . ?
Cl5 C99 Cl3 110.38(13) . . ?
Cl4 C99 Cl3 111.01(13) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         2.527
_refine_diff_density_min         -1.593
_refine_diff_density_rms         0.096



#=============================================================================
# end of cif data for "effri"
#=============================================================================

#=============================================================================
# end of cif file
#=============================================================================

