# 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_1
_audit_block_doi                 10.5517/cc13wwgb
_database_code_depnum_ccdc_archive 'CCDC 1039692'
_audit_update_record             
;
2014-12-16 deposited with the CCDC.
2015-07-30 downloaded from the CCDC.
;

_cell_length_a                   8.2299(2)
_cell_length_b                   16.7796(3)
_cell_length_c                   9.6743(2)
_cell_angle_alpha                90
_cell_angle_beta                 103.9540(10)
_cell_angle_gamma                90
_cell_volume                     1296.54(5)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21 1 '
_symmetry_space_group_name_Hall  'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

_chemical_formula_sum            'C22 H39 Cl2 N2 O1 P1 Pd1'
_chemical_formula_moiety         'C22 H39 Cl2 N2 O1 P1 Pd1'
_chemical_compound_source        synthesis
_chemical_formula_weight         555.84


_cell_measurement_reflns_used    9914
_cell_measurement_theta_min      2
_cell_measurement_theta_max      27
_cell_measurement_temperature    123

_exptl_crystal_description       brick
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.420
_exptl_crystal_size_mid          0.430
_exptl_crystal_size_max          0.580

_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             576
_exptl_absorpt_coefficient_mu    0.999

_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_T_max  0.66
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω/2θ

_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      123
_diffrn_reflns_number            15750
_reflns_number_total             5091
_diffrn_reflns_av_R_equivalents  0.026

_diffrn_reflns_theta_min         2.169
_diffrn_reflns_theta_max         26.629
_diffrn_measured_fraction_theta_max 0.993

_diffrn_reflns_theta_full        26.096
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              -19
_reflns_limit_k_max              21
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   1.17
_oxford_diffrn_Wilson_scale      4.42

_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.45
_refine_diff_density_max         0.31

_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         4950
_refine_ls_number_restraints     1
_refine_ls_number_parameters     263
_oxford_refine_ls_R_factor_ref   0.0164
_refine_ls_wR_factor_ref         0.0169
_refine_ls_goodness_of_fit_ref   1.1025
_refine_ls_shift/su_max          0.0461381
_refine_ls_shift/su_mean         0.0032966


_oxford_reflns_number_all        5071
_refine_ls_R_factor_all          0.0171
_refine_ls_wR_factor_all         0.0170

_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                5001
_refine_ls_R_factor_gt           0.0166
_refine_ls_wR_factor_gt          0.0169

_refine_ls_abs_structure_Flack   0.019(12)
_refine_ls_abs_structure_details 'Flack (1983), 2285 Friedel-pairs'
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 1.26 -0.440 1.32 -0.128 0.412 
;

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Pd1 Pd 0.645601(14) 0.27965(4) 0.452679(11) 0.0124 1.0000 Uani . . . . . .
Cl1 Cl 0.52519(6) 0.32663(5) 0.22706(5) 0.0211 1.0000 Uani . . . . . .
Cl2 Cl 0.43111(5) 0.18537(5) 0.43654(5) 0.0213 1.0000 Uani . . . . . .
P1 P 0.86271(5) 0.36195(5) 0.51253(4) 0.0119 1.0000 Uani . . . . . .
O1 O 0.62505(19) 0.05646(9) 1.06428(15) 0.0246 1.0000 Uani . . . . . .
N1 N 0.78735(18) 0.25013(9) 0.64927(15) 0.0137 1.0000 Uani . . . . . .
N2 N 1.07278(15) 0.28292(13) 0.76652(12) 0.0133 1.0000 Uani . . . . . .
C1 C 0.9259(2) 0.29233(11) 0.66876(17) 0.0123 1.0000 Uani . . . . . .
C2 C 0.7084(3) 0.11991(13) 0.7300(2) 0.0171 1.0000 Uani . . . . . .
C3 C 0.6699(2) 0.07289(11) 0.8358(2) 0.0182 1.0000 Uani . . . . . .
C4 C 0.6636(2) 0.10706(12) 0.96663(19) 0.0170 1.0000 Uani . . . . . .
C5 C 0.6931(2) 0.18807(12) 0.98944(18) 0.0162 1.0000 Uani . . . . . .
C6 C 0.7338(2) 0.23422(11) 0.88344(18) 0.0155 1.0000 Uani . . . . . .
C7 C 0.7446(2) 0.20044(11) 0.75537(18) 0.0148 1.0000 Uani . . . . . .
C8 C 1.0140(2) 0.36051(13) 0.39687(18) 0.0193 1.0000 Uani . . . . . .
C9 C 1.1932(2) 0.38523(14) 0.4705(2) 0.0268 1.0000 Uani . . . . . .
C10 C 0.9450(3) 0.41541(15) 0.2680(2) 0.0318 1.0000 Uani . . . . . .
C11 C 1.0163(2) 0.27379(19) 0.34666(19) 0.0283 1.0000 Uani . . . . . .
C12 C 0.8012(2) 0.46288(11) 0.5670(2) 0.0183 1.0000 Uani . . . . . .
C13 C 0.7292(3) 0.45157(14) 0.6975(2) 0.0255 1.0000 Uani . . . . . .
C14 C 0.6574(2) 0.49145(12) 0.4426(2) 0.0240 1.0000 Uani . . . . . .
C15 C 0.9407(3) 0.52518(12) 0.5985(2) 0.0281 1.0000 Uani . . . . . .
C16 C 1.1217(2) 0.20180(13) 0.8276(2) 0.0183 1.0000 Uani . . . . . .
C17 C 1.2557(3) 0.16518(13) 0.7642(2) 0.0266 1.0000 Uani . . . . . .
C18 C 1.1647(3) 0.19833(14) 0.9891(2) 0.0251 1.0000 Uani . . . . . .
C19 C 1.1728(2) 0.35579(12) 0.8160(2) 0.0155 1.0000 Uani . . . . . .
C20 C 1.1333(2) 0.38934(14) 0.9518(2) 0.0217 1.0000 Uani . . . . . .
C21 C 1.3615(2) 0.34647(12) 0.8378(2) 0.0217 1.0000 Uani . . . . . .
C22 C 0.6130(3) 0.09066(13) 1.1971(2) 0.0260 1.0000 Uani . . . . . .
H21 H 0.7153 0.0979 0.6409 0.0219 1.0000 Uiso . . . . . .
H31 H 0.6480 0.0178 0.8200 0.0229 1.0000 Uiso . . . . . .
H51 H 0.6835 0.2120 1.0756 0.0209 1.0000 Uiso . . . . . .
H61 H 0.7564 0.2891 0.8998 0.0205 1.0000 Uiso . . . . . .
H91 H 1.2582 0.3852 0.4017 0.0420 1.0000 Uiso . . . . . .
H92 H 1.1993 0.4381 0.5118 0.0421 1.0000 Uiso . . . . . .
H93 H 1.2407 0.3471 0.5462 0.0415 1.0000 Uiso . . . . . .
H101 H 1.0148 0.4061 0.2029 0.0493 1.0000 Uiso . . . . . .
H102 H 0.9525 0.4711 0.2974 0.0487 1.0000 Uiso . . . . . .
H103 H 0.8300 0.4021 0.2229 0.0488 1.0000 Uiso . . . . . .
H111 H 1.0942 0.2688 0.2875 0.0432 1.0000 Uiso . . . . . .
H112 H 1.0480 0.2357 0.4259 0.0431 1.0000 Uiso . . . . . .
H113 H 0.9072 0.2591 0.2909 0.0423 1.0000 Uiso . . . . . .
H131 H 0.6840 0.5019 0.7170 0.0383 1.0000 Uiso . . . . . .
H132 H 0.8162 0.4372 0.7757 0.0390 1.0000 Uiso . . . . . .
H133 H 0.6416 0.4105 0.6775 0.0379 1.0000 Uiso . . . . . .
H141 H 0.6197 0.5438 0.4660 0.0384 1.0000 Uiso . . . . . .
H142 H 0.6937 0.4969 0.3548 0.0387 1.0000 Uiso . . . . . .
H143 H 0.5633 0.4544 0.4279 0.0396 1.0000 Uiso . . . . . .
H151 H 0.8951 0.5748 0.6195 0.0414 1.0000 Uiso . . . . . .
H152 H 1.0298 0.5111 0.6765 0.0424 1.0000 Uiso . . . . . .
H153 H 0.9838 0.5337 0.5154 0.0414 1.0000 Uiso . . . . . .
H161 H 1.0194 0.1695 0.7911 0.0223 1.0000 Uiso . . . . . .
H171 H 1.2688 0.1106 0.7923 0.0421 1.0000 Uiso . . . . . .
H172 H 1.3633 0.1930 0.7960 0.0432 1.0000 Uiso . . . . . .
H173 H 1.2238 0.1672 0.6613 0.0428 1.0000 Uiso . . . . . .
H181 H 1.1812 0.1422 1.0178 0.0393 1.0000 Uiso . . . . . .
H182 H 1.2697 0.2284 1.0295 0.0390 1.0000 Uiso . . . . . .
H183 H 1.0741 0.2202 1.0266 0.0389 1.0000 Uiso . . . . . .
H191 H 1.1338 0.3960 0.7384 0.0166 1.0000 Uiso . . . . . .
H203 H 1.1589 0.4463 0.9590 0.0343 1.0000 Uiso . . . . . .
H202 H 1.1986 0.3651 1.0376 0.0355 1.0000 Uiso . . . . . .
H201 H 1.0144 0.3818 0.9489 0.0337 1.0000 Uiso . . . . . .
H211 H 1.4127 0.3974 0.8595 0.0340 1.0000 Uiso . . . . . .
H212 H 1.4052 0.3122 0.9159 0.0336 1.0000 Uiso . . . . . .
H213 H 1.3882 0.3268 0.7510 0.0338 1.0000 Uiso . . . . . .
H221 H 0.5889 0.0479 1.2537 0.0397 1.0000 Uiso . . . . . .
H222 H 0.7221 0.1153 1.2438 0.0403 1.0000 Uiso . . . . . .
H223 H 0.5227 0.1292 1.1838 0.0403 1.0000 Uiso . . . . . .

_refine_ls_extinction_coef       4.509
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.6695(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Cl1 . 2.3075(4) yes
Pd1 . Cl2 . 2.3473(4) yes
Pd1 . P1 . 2.2217(4) yes
Pd1 . N1 . 2.0380(14) yes
P1 . C1 . 1.8815(17) yes
P1 . C8 . 1.8642(18) yes
P1 . C12 . 1.8791(18) yes
O1 . C4 . 1.363(2) yes
O1 . C22 . 1.432(2) yes
N1 . C1 . 1.317(2) yes
N1 . C7 . 1.431(2) yes
N2 . C1 . 1.352(2) yes
N2 . C16 . 1.500(3) yes
N2 . C19 . 1.487(3) yes
C2 . C3 . 1.388(3) yes
C2 . C7 . 1.393(3) yes
C2 . H21 . 0.952 no
C3 . C4 . 1.402(3) yes
C3 . H31 . 0.947 no
C4 . C5 . 1.389(3) yes
C5 . C6 . 1.389(2) yes
C5 . H51 . 0.945 no
C6 . C7 . 1.385(2) yes
C6 . H61 . 0.946 no
C8 . C9 . 1.532(3) yes
C8 . C10 . 1.544(3) yes
C8 . C11 . 1.536(3) yes
C9 . H91 . 0.949 no
C9 . H92 . 0.970 no
C9 . H93 . 0.980 no
C10 . H101 . 0.962 no
C10 . H102 . 0.974 no
C10 . H103 . 0.968 no
C11 . H111 . 0.960 no
C11 . H112 . 0.984 no
C11 . H113 . 0.961 no
C12 . C13 . 1.530(3) yes
C12 . C14 . 1.547(3) yes
C12 . C15 . 1.528(3) yes
C13 . H131 . 0.959 no
C13 . H132 . 0.939 no
C13 . H133 . 0.982 no
C14 . H141 . 0.977 no
C14 . H142 . 0.970 no
C14 . H143 . 0.977 no
C15 . H151 . 0.955 no
C15 . H152 . 0.947 no
C15 . H153 . 0.964 no
C16 . C17 . 1.516(3) yes
C16 . C18 . 1.518(3) yes
C16 . H161 . 0.991 no
C17 . H171 . 0.954 no
C17 . H172 . 0.982 no
C17 . H173 . 0.966 no
C18 . H181 . 0.982 no
C18 . H182 . 0.995 no
C18 . H183 . 0.976 no
C19 . C20 . 1.535(3) yes
C19 . C21 . 1.524(3) yes
C19 . H191 . 1.003 no
C20 . H203 . 0.978 no
C20 . H202 . 0.963 no
C20 . H201 . 0.980 no
C21 . H211 . 0.953 no
C21 . H212 . 0.949 no
C21 . H213 . 0.976 no
C22 . H221 . 0.953 no
C22 . H222 . 0.993 no
C22 . H223 . 0.970 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Pd1 . Cl2 . 91.303(16) yes
Cl1 . Pd1 . P1 . 99.739(17) yes
Cl2 . Pd1 . P1 . 168.776(15) yes
Cl1 . Pd1 . N1 . 169.87(4) yes
Cl2 . Pd1 . N1 . 98.65(4) yes
P1 . Pd1 . N1 . 70.39(4) yes
Pd1 . P1 . C1 . 82.69(5) yes
Pd1 . P1 . C8 . 116.57(6) yes
C1 . P1 . C8 . 112.26(8) yes
Pd1 . P1 . C12 . 112.29(6) yes
C1 . P1 . C12 . 112.03(8) yes
C8 . P1 . C12 . 116.37(9) yes
C4 . O1 . C22 . 116.75(15) yes
Pd1 . N1 . C1 . 106.50(11) yes
Pd1 . N1 . C7 . 128.81(11) yes
C1 . N1 . C7 . 124.41(14) yes
C1 . N2 . C16 . 119.43(17) yes
C1 . N2 . C19 . 117.45(18) yes
C16 . N2 . C19 . 122.97(12) yes
P1 . C1 . N2 . 131.43(14) yes
P1 . C1 . N1 . 99.01(11) yes
N2 . C1 . N1 . 129.37(17) yes
C3 . C2 . C7 . 119.94(17) yes
C3 . C2 . H21 . 121.4 no
C7 . C2 . H21 . 118.6 no
C2 . C3 . C4 . 119.86(17) yes
C2 . C3 . H31 . 120.3 no
C4 . C3 . H31 . 119.8 no
C3 . C4 . O1 . 115.89(16) yes
C3 . C4 . C5 . 120.03(16) yes
O1 . C4 . C5 . 124.08(16) yes
C4 . C5 . C6 . 119.49(16) yes
C4 . C5 . H51 . 120.5 no
C6 . C5 . H51 . 120.0 no
C5 . C6 . C7 . 120.76(16) yes
C5 . C6 . H61 . 119.5 no
C7 . C6 . H61 . 119.7 no
N1 . C7 . C2 . 121.22(16) yes
N1 . C7 . C6 . 118.91(16) yes
C2 . C7 . C6 . 119.84(17) yes
P1 . C8 . C9 . 115.14(12) yes
P1 . C8 . C10 . 107.95(13) yes
C9 . C8 . C10 . 109.82(17) yes
P1 . C8 . C11 . 105.25(13) yes
C9 . C8 . C11 . 108.65(16) yes
C10 . C8 . C11 . 109.88(16) yes
C8 . C9 . H91 . 108.4 no
C8 . C9 . H92 . 112.8 no
H91 . C9 . H92 . 108.0 no
C8 . C9 . H93 . 109.6 no
H91 . C9 . H93 . 109.4 no
H92 . C9 . H93 . 108.6 no
C8 . C10 . H101 . 105.7 no
C8 . C10 . H102 . 110.6 no
H101 . C10 . H102 . 110.0 no
C8 . C10 . H103 . 110.8 no
H101 . C10 . H103 . 109.9 no
H102 . C10 . H103 . 109.8 no
C8 . C11 . H111 . 109.4 no
C8 . C11 . H112 . 113.0 no
H111 . C11 . H112 . 108.5 no
C8 . C11 . H113 . 109.8 no
H111 . C11 . H113 . 108.1 no
H112 . C11 . H113 . 107.9 no
P1 . C12 . C13 . 107.69(13) yes
P1 . C12 . C14 . 105.55(13) yes
C13 . C12 . C14 . 107.74(16) yes
P1 . C12 . C15 . 115.61(13) yes
C13 . C12 . C15 . 110.02(17) yes
C14 . C12 . C15 . 109.88(16) yes
C12 . C13 . H131 . 107.4 no
C12 . C13 . H132 . 109.0 no
H131 . C13 . H132 . 108.9 no
C12 . C13 . H133 . 109.7 no
H131 . C13 . H133 . 110.8 no
H132 . C13 . H133 . 111.0 no
C12 . C14 . H141 . 109.0 no
C12 . C14 . H142 . 111.8 no
H141 . C14 . H142 . 107.5 no
C12 . C14 . H143 . 110.3 no
H141 . C14 . H143 . 108.7 no
H142 . C14 . H143 . 109.5 no
C12 . C15 . H151 . 108.9 no
C12 . C15 . H152 . 112.8 no
H151 . C15 . H152 . 108.5 no
C12 . C15 . H153 . 110.2 no
H151 . C15 . H153 . 106.8 no
H152 . C15 . H153 . 109.4 no
N2 . C16 . C17 . 111.14(16) yes
N2 . C16 . C18 . 114.48(16) yes
C17 . C16 . C18 . 112.92(16) yes
N2 . C16 . H161 . 103.4 no
C17 . C16 . H161 . 105.8 no
C18 . C16 . H161 . 108.2 no
C16 . C17 . H171 . 108.5 no
C16 . C17 . H172 . 111.7 no
H171 . C17 . H172 . 109.6 no
C16 . C17 . H173 . 111.0 no
H171 . C17 . H173 . 108.1 no
H172 . C17 . H173 . 107.9 no
C16 . C18 . H181 . 108.0 no
C16 . C18 . H182 . 110.4 no
H181 . C18 . H182 . 109.1 no
C16 . C18 . H183 . 111.0 no
H181 . C18 . H183 . 108.7 no
H182 . C18 . H183 . 109.5 no
N2 . C19 . C20 . 111.23(15) yes
N2 . C19 . C21 . 115.26(16) yes
C20 . C19 . C21 . 109.76(16) yes
N2 . C19 . H191 . 105.1 no
C20 . C19 . H191 . 107.3 no
C21 . C19 . H191 . 107.7 no
C19 . C20 . H203 . 109.4 no
C19 . C20 . H202 . 113.2 no
H203 . C20 . H202 . 106.6 no
C19 . C20 . H201 . 110.1 no
H203 . C20 . H201 . 109.0 no
H202 . C20 . H201 . 108.4 no
C19 . C21 . H211 . 108.7 no
C19 . C21 . H212 . 110.5 no
H211 . C21 . H212 . 107.8 no
C19 . C21 . H213 . 110.4 no
H211 . C21 . H213 . 108.3 no
H212 . C21 . H213 . 111.0 no
O1 . C22 . H221 . 106.5 no
O1 . C22 . H222 . 109.0 no
H221 . C22 . H222 . 110.1 no
O1 . C22 . H223 . 111.4 no
H221 . C22 . H223 . 108.6 no
H222 . C22 . H223 . 111.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C16 . H161 . C7 . 131.31(13) 0.991 2.265 3.012(3) yes
####################################################################### 
# 
# 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_1
_audit_block_doi                 10.5517/cc13wwhc
_database_code_depnum_ccdc_archive 'CCDC 1039693'
_audit_update_record             
;
2014-12-16 deposited with the CCDC.
2015-07-30 downloaded from the CCDC.
;

_cell_length_a                   10.1264(13)
_cell_length_b                   13.7129(17)
_cell_length_c                   17.5394(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2435.6(5)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21 '
_symmetry_space_group_name_Hall  'P 2ac 2 ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,-y+1/2,-z
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C21 H40 Cl2 N2 P1 Pd1 
# Dc =      1.44 Fooo =   1088.00 Mu =     10.56 M =    528.84
# Found Formula = C21 H37 Cl2 N2 P1 Pd1 
# Dc =      1.43 FOOO =   1088.00 Mu =     10.56 M =    525.82

_chemical_formula_sum            'C21 H37 Cl2 N2 P1 Pd1'
_chemical_formula_moiety         'C21 H37 Cl2 N2 P1 Pd1'
_chemical_compound_source        ?
_chemical_formula_weight         525.82


_cell_measurement_reflns_used    484
_cell_measurement_theta_min      0
_cell_measurement_theta_max      0
_cell_measurement_temperature    173

_exptl_crystal_description       prism
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_min          0.23
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_max          0.40

_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    1.056

# Sheldrick geometric approximatio 0.67 0.78 
# No experimental values of Tmin/max available 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.78
_diffrn_measurement_device       'Bruker Apex2'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω/2θ

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      173
_diffrn_reflns_number            14061
_reflns_number_total             4854
_diffrn_reflns_av_R_equivalents  0.054
# Number of reflections with Friedels Law is 2763 
# Number of reflections without Friedels Law is 4854 
# Theoretical number of reflections is about 2479 


_diffrn_reflns_theta_min         1.885
_diffrn_reflns_theta_max         26.328
_diffrn_measured_fraction_theta_max 0.984

_diffrn_reflns_theta_full        25.012
_diffrn_measured_fraction_theta_full 0.989


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              21

_oxford_diffrn_Wilson_B_factor   1.57
_oxford_diffrn_Wilson_scale      9.88

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   geom

_refine_diff_density_min         -0.85
_refine_diff_density_max         0.55


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         4053
_refine_ls_number_restraints     0
_refine_ls_number_parameters     245
_oxford_refine_ls_R_factor_ref   0.0331
_refine_ls_wR_factor_ref         0.0268
_refine_ls_goodness_of_fit_ref   1.0325
_refine_ls_shift/su_max          0.001575


# The values computed from all data 
_oxford_reflns_number_all        4835
_refine_ls_R_factor_all          0.0454
_refine_ls_wR_factor_all         0.0348

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4294
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_gt          0.0280

_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_abs_structure_details 'Flack (1983), 2091 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.614 -0.699 0.135 -0.278 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd 0.08883(3) 0.55968(2) 0.554054(17) 0.0166 1.0000 Uani . . . . . . .
Cl1 Cl 0.06708(11) 0.64873(8) 0.66984(6) 0.0295 1.0000 Uani . . . . . . .
Cl2 Cl 0.31880(9) 0.54379(8) 0.57890(6) 0.0232 1.0000 Uani . . . . . . .
P1 P -0.12389(9) 0.54178(8) 0.53153(6) 0.0179 1.0000 Uani . . . . . . .
N1 N -0.0781(3) 0.4716(2) 0.45330(19) 0.0176 1.0000 Uani . . . . . . .
N2 N 0.1272(3) 0.4789(3) 0.38918(19) 0.0196 1.0000 Uani . . . . . . .
C1 C 0.0567(3) 0.4920(3) 0.4511(2) 0.0183 1.0000 Uani . . . . . . .
C2 C -0.0996(5) 0.2984(3) 0.4270(2) 0.0224 1.0000 Uani . . . . . . .
C3 C -0.1658(5) 0.2196(4) 0.3950(3) 0.0327 1.0000 Uani . . . . . . .
C4 C -0.2781(5) 0.2361(4) 0.3509(3) 0.0366 1.0000 Uani . . . . . . .
C5 C -0.3244(5) 0.3297(4) 0.3401(3) 0.0326 1.0000 Uani . . . . . . .
C6 C -0.2585(4) 0.4087(3) 0.3722(3) 0.0255 1.0000 Uani . . . . . . .
C7 C -0.1456(4) 0.3923(3) 0.4157(2) 0.0191 1.0000 Uani . . . . . . .
C8 C -0.2210(4) 0.6477(3) 0.4959(3) 0.0243 1.0000 Uani . . . . . . .
C9 C -0.2105(4) 0.7309(3) 0.5562(3) 0.0292 1.0000 Uani . . . . . . .
C10 C -0.3669(4) 0.6272(4) 0.4818(3) 0.0356 1.0000 Uani . . . . . . .
C11 C -0.1552(5) 0.6824(4) 0.4215(3) 0.0319 1.0000 Uani . . . . . . .
C12 C -0.2092(4) 0.4628(3) 0.6028(2) 0.0242 1.0000 Uani . . . . . . .
C13 C -0.3282(4) 0.4050(3) 0.5721(3) 0.0307 1.0000 Uani . . . . . . .
C14 C -0.2554(5) 0.5297(4) 0.6692(3) 0.0375 1.0000 Uani . . . . . . .
C15 C -0.1049(5) 0.3906(4) 0.6338(3) 0.0332 1.0000 Uani . . . . . . .
C16 C 0.0646(4) 0.4641(3) 0.3121(2) 0.0250 1.0000 Uani . . . . . . .
C17 C 0.0781(5) 0.5550(4) 0.2618(2) 0.0345 1.0000 Uani . . . . . . .
C18 C 0.1053(6) 0.3713(4) 0.2720(3) 0.0364 1.0000 Uani . . . . . . .
C19 C 0.2752(4) 0.4812(4) 0.3982(3) 0.0290 1.0000 Uani . . . . . . .
C20 C 0.3494(4) 0.5356(4) 0.3360(3) 0.0362 1.0000 Uani . . . . . . .
C21 C 0.3263(6) 0.3788(5) 0.4104(3) 0.0466 1.0000 Uani . . . . . . .
H21 H -0.0253 0.2885 0.4564 0.0259 1.0000 Uiso . . . . . . .
H31 H -0.1363 0.1536 0.4041 0.0343 1.0000 Uiso . . . . . . .
H41 H -0.3258 0.1841 0.3307 0.0432 1.0000 Uiso . . . . . . .
H51 H -0.3944 0.3411 0.3059 0.0391 1.0000 Uiso . . . . . . .
H61 H -0.2891 0.4728 0.3664 0.0290 1.0000 Uiso . . . . . . .
H91 H -0.2550 0.7895 0.5393 0.0350 1.0000 Uiso . . . . . . .
H92 H -0.1197 0.7468 0.5678 0.0354 1.0000 Uiso . . . . . . .
H93 H -0.2527 0.7104 0.6046 0.0348 1.0000 Uiso . . . . . . .
H101 H -0.3787 0.5742 0.4477 0.0539 1.0000 Uiso . . . . . . .
H102 H -0.4080 0.6857 0.4593 0.0541 1.0000 Uiso . . . . . . .
H103 H -0.4108 0.6139 0.5292 0.0538 1.0000 Uiso . . . . . . .
H111 H -0.1980 0.7435 0.4033 0.0390 1.0000 Uiso . . . . . . .
H112 H -0.1637 0.6345 0.3817 0.0388 1.0000 Uiso . . . . . . .
H113 H -0.0631 0.6965 0.4294 0.0389 1.0000 Uiso . . . . . . .
H131 H -0.3942 0.4477 0.5536 0.0440 1.0000 Uiso . . . . . . .
H132 H -0.2999 0.3612 0.5322 0.0438 1.0000 Uiso . . . . . . .
H133 H -0.3649 0.3652 0.6134 0.0440 1.0000 Uiso . . . . . . .
H141 H -0.2900 0.4908 0.7093 0.0510 1.0000 Uiso . . . . . . .
H142 H -0.1807 0.5670 0.6880 0.0511 1.0000 Uiso . . . . . . .
H143 H -0.3223 0.5750 0.6514 0.0508 1.0000 Uiso . . . . . . .
H151 H -0.0729 0.3497 0.5919 0.0468 1.0000 Uiso . . . . . . .
H152 H -0.0361 0.4232 0.6571 0.0469 1.0000 Uiso . . . . . . .
H153 H -0.1483 0.3459 0.6706 0.0471 1.0000 Uiso . . . . . . .
H161 H -0.0309 0.4561 0.3217 0.0289 1.0000 Uiso . . . . . . .
H171 H 0.0185 0.5501 0.2184 0.0530 1.0000 Uiso . . . . . . .
H172 H 0.0561 0.6121 0.2905 0.0528 1.0000 Uiso . . . . . . .
H173 H 0.1673 0.5600 0.2430 0.0530 1.0000 Uiso . . . . . . .
H181 H 0.0908 0.3145 0.3053 0.0490 1.0000 Uiso . . . . . . .
H182 H 0.0570 0.3628 0.2259 0.0490 1.0000 Uiso . . . . . . .
H183 H 0.1998 0.3733 0.2606 0.0491 1.0000 Uiso . . . . . . .
H191 H 0.2924 0.5190 0.4452 0.0380 1.0000 Uiso . . . . . . .
H201 H 0.3133 0.6037 0.3312 0.0450 1.0000 Uiso . . . . . . .
H202 H 0.3331 0.5040 0.2862 0.0449 1.0000 Uiso . . . . . . .
H203 H 0.4384 0.5385 0.3467 0.0451 1.0000 Uiso . . . . . . .
H211 H 0.4178 0.3788 0.4221 0.0691 1.0000 Uiso . . . . . . .
H212 H 0.2782 0.3480 0.4535 0.0692 1.0000 Uiso . . . . . . .
H213 H 0.3100 0.3383 0.3663 0.0689 1.0000 Uiso . . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3235(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Cl1 . 2.3798(11) yes
Pd1 . Cl2 . 2.3792(10) yes
Pd1 . P1 . 2.2037(10) yes
Pd1 . C1 . 2.056(4) yes
P1 . N1 . 1.739(3) yes
P1 . C8 . 1.862(4) yes
P1 . C12 . 1.865(4) yes
N1 . C1 . 1.394(4) yes
N1 . C7 . 1.444(5) yes
N2 . C1 . 1.312(5) yes
N2 . C16 . 1.507(5) yes
N2 . C19 . 1.508(5) yes
C2 . C3 . 1.390(6) yes
C2 . C7 . 1.384(6) yes
C2 . H21 . 0.921 no
C3 . C4 . 1.393(7) yes
C3 . H31 . 0.966 no
C4 . C5 . 1.379(7) yes
C4 . H41 . 0.933 no
C5 . C6 . 1.391(6) yes
C5 . H51 . 0.942 no
C6 . C7 . 1.393(6) yes
C6 . H61 . 0.938 no
C8 . C9 . 1.559(6) yes
C8 . C10 . 1.524(6) yes
C8 . C11 . 1.542(6) yes
C9 . H91 . 0.968 no
C9 . H92 . 0.967 no
C9 . H93 . 0.991 no
C10 . H101 . 0.949 no
C10 . H102 . 0.986 no
C10 . H103 . 0.959 no
C11 . H111 . 0.995 no
C11 . H112 . 0.962 no
C11 . H113 . 0.962 no
C12 . C13 . 1.539(6) yes
C12 . C14 . 1.555(6) yes
C12 . C15 . 1.547(6) yes
C13 . H131 . 0.946 no
C13 . H132 . 0.965 no
C13 . H133 . 0.980 no
C14 . H141 . 0.950 no
C14 . H142 . 0.971 no
C14 . H143 . 0.971 no
C15 . H151 . 0.980 no
C15 . H152 . 0.923 no
C15 . H153 . 0.993 no
C16 . C17 . 1.534(6) yes
C16 . C18 . 1.511(6) yes
C16 . H161 . 0.988 no
C17 . H171 . 0.973 no
C17 . H172 . 0.956 no
C17 . H173 . 0.964 no
C18 . H181 . 0.985 no
C18 . H182 . 0.952 no
C18 . H183 . 0.978 no
C19 . C20 . 1.521(7) yes
C19 . C21 . 1.512(7) yes
C19 . H191 . 0.988 no
C20 . H201 . 1.007 no
C20 . H202 . 0.988 no
C20 . H203 . 0.921 no
C21 . H211 . 0.949 no
C21 . H212 . 0.994 no
C21 . H213 . 0.966 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Pd1 . Cl2 . 88.93(4) yes
Cl1 . Pd1 . P1 . 96.88(4) yes
Cl2 . Pd1 . P1 . 168.34(4) yes
Cl1 . Pd1 . C1 . 165.09(10) yes
Cl2 . Pd1 . C1 . 105.92(10) yes
P1 . Pd1 . C1 . 68.75(10) yes
Pd1 . P1 . N1 . 86.71(11) yes
Pd1 . P1 . C8 . 119.31(14) yes
N1 . P1 . C8 . 107.93(19) yes
Pd1 . P1 . C12 . 113.42(14) yes
N1 . P1 . C12 . 109.31(17) yes
C8 . P1 . C12 . 115.6(2) yes
P1 . N1 . C1 . 99.9(3) yes
P1 . N1 . C7 . 130.6(3) yes
C1 . N1 . C7 . 127.0(3) yes
C1 . N2 . C16 . 122.1(3) yes
C1 . N2 . C19 . 116.8(3) yes
C16 . N2 . C19 . 121.1(3) yes
N1 . C1 . N2 . 121.9(4) yes
N1 . C1 . Pd1 . 102.8(3) yes
N2 . C1 . Pd1 . 134.6(3) yes
C3 . C2 . C7 . 120.2(4) yes
C3 . C2 . H21 . 120.4 no
C7 . C2 . H21 . 119.5 no
C2 . C3 . C4 . 119.5(5) yes
C2 . C3 . H31 . 120.8 no
C4 . C3 . H31 . 119.8 no
C3 . C4 . C5 . 120.3(4) yes
C3 . C4 . H41 . 120.7 no
C5 . C4 . H41 . 118.9 no
C4 . C5 . C6 . 120.4(4) yes
C4 . C5 . H51 . 119.8 no
C6 . C5 . H51 . 119.3 no
C5 . C6 . C7 . 119.3(4) yes
C5 . C6 . H61 . 121.9 no
C7 . C6 . H61 . 118.8 no
N1 . C7 . C6 . 121.2(4) yes
N1 . C7 . C2 . 118.4(4) yes
C6 . C7 . C2 . 120.3(4) yes
P1 . C8 . C9 . 107.9(3) yes
P1 . C8 . C10 . 115.0(3) yes
C9 . C8 . C10 . 108.1(4) yes
P1 . C8 . C11 . 107.3(3) yes
C9 . C8 . C11 . 108.6(4) yes
C10 . C8 . C11 . 109.8(4) yes
C8 . C9 . H91 . 111.6 no
C8 . C9 . H92 . 111.9 no
H91 . C9 . H92 . 108.7 no
C8 . C9 . H93 . 110.1 no
H91 . C9 . H93 . 107.3 no
H92 . C9 . H93 . 107.0 no
C8 . C10 . H101 . 111.4 no
C8 . C10 . H102 . 108.9 no
H101 . C10 . H102 . 108.5 no
C8 . C10 . H103 . 110.1 no
H101 . C10 . H103 . 110.0 no
H102 . C10 . H103 . 107.7 no
C8 . C11 . H111 . 110.1 no
C8 . C11 . H112 . 111.3 no
H111 . C11 . H112 . 107.7 no
C8 . C11 . H113 . 111.0 no
H111 . C11 . H113 . 107.4 no
H112 . C11 . H113 . 109.2 no
P1 . C12 . C13 . 115.3(3) yes
P1 . C12 . C14 . 107.4(3) yes
C13 . C12 . C14 . 109.3(4) yes
P1 . C12 . C15 . 106.9(3) yes
C13 . C12 . C15 . 109.1(4) yes
C14 . C12 . C15 . 108.6(4) yes
C12 . C13 . H131 . 110.7 no
C12 . C13 . H132 . 110.0 no
H131 . C13 . H132 . 110.3 no
C12 . C13 . H133 . 109.0 no
H131 . C13 . H133 . 109.3 no
H132 . C13 . H133 . 107.6 no
C12 . C14 . H141 . 109.5 no
C12 . C14 . H142 . 109.3 no
H141 . C14 . H142 . 109.5 no
C12 . C14 . H143 . 110.2 no
H141 . C14 . H143 . 109.8 no
H142 . C14 . H143 . 108.4 no
C12 . C15 . H151 . 109.2 no
C12 . C15 . H152 . 111.2 no
H151 . C15 . H152 . 111.0 no
C12 . C15 . H153 . 108.8 no
H151 . C15 . H153 . 106.2 no
H152 . C15 . H153 . 110.2 no
N2 . C16 . C17 . 111.6(3) yes
N2 . C16 . C18 . 114.6(4) yes
C17 . C16 . C18 . 113.1(4) yes
N2 . C16 . H161 . 105.9 no
C17 . C16 . H161 . 105.9 no
C18 . C16 . H161 . 104.7 no
C16 . C17 . H171 . 109.8 no
C16 . C17 . H172 . 110.0 no
H171 . C17 . H172 . 108.9 no
C16 . C17 . H173 . 109.7 no
H171 . C17 . H173 . 108.5 no
H172 . C17 . H173 . 109.9 no
C16 . C18 . H181 . 110.4 no
C16 . C18 . H182 . 111.1 no
H181 . C18 . H182 . 109.3 no
C16 . C18 . H183 . 109.8 no
H181 . C18 . H183 . 106.8 no
H182 . C18 . H183 . 109.4 no
N2 . C19 . C20 . 115.2(4) yes
N2 . C19 . C21 . 109.6(4) yes
C20 . C19 . C21 . 112.8(4) yes
N2 . C19 . H191 . 105.9 no
C20 . C19 . H191 . 104.8 no
C21 . C19 . H191 . 108.0 no
C19 . C20 . H201 . 109.6 no
C19 . C20 . H202 . 109.7 no
H201 . C20 . H202 . 105.8 no
C19 . C20 . H203 . 110.9 no
H201 . C20 . H203 . 109.4 no
H202 . C20 . H203 . 111.3 no
C19 . C21 . H211 . 111.3 no
C19 . C21 . H212 . 109.6 no
H211 . C21 . H212 . 108.2 no
C19 . C21 . H213 . 111.3 no
H211 . C21 . H213 . 110.0 no
H212 . C21 . H213 . 106.3 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C16 . H161 . C6 . 166 0.99 2.55 3.520(7) yes
C16 . H161 . C7 . 134 0.99 2.20 2.966(7) yes
####################################################################### 
# 
# 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_1
_audit_block_doi                 10.5517/cc13wwjd
_database_code_depnum_ccdc_archive 'CCDC 1039694'
_audit_update_record             
;
2014-12-16 deposited with the CCDC.
2015-07-30 downloaded from the CCDC.
;


_cell_length_a                   10.2491(14)
_cell_length_b                   12.2572(16)
_cell_length_c                   19.524(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2452.7(6)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21 '
_symmetry_space_group_name_Hall  'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,-y+1/2,-z
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

_chemical_formula_sum            'C22 H39 Cl2 N2 P1 Pd1'
_chemical_formula_moiety         'C22 H39 Cl2 N2 P1 Pd1'
_chemical_compound_source        ?
_chemical_formula_weight         539.84


_cell_measurement_reflns_used    6686
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      24.68
_cell_measurement_temperature    173

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_min          0.22
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_max          0.40

_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1120
_exptl_absorpt_coefficient_mu    1.051

# Sheldrick geometric approximatio 0.67 0.79 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.67
_exptl_absorpt_correction_T_max  0.79
_diffrn_measurement_device       'Bruker Apex2'
_diffrn_measurement_device_type  Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω/2θ

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      173
_diffrn_reflns_number            24875
_reflns_number_total             5027
_diffrn_reflns_av_R_equivalents  0.092
# Number of reflections with Friedels Law is 2853 
# Number of reflections without Friedels Law is 5027 
# Theoretical number of reflections is about 2521 


_diffrn_reflns_theta_min         1.962
_diffrn_reflns_theta_max         26.419
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        26.419
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       19
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              15
_reflns_limit_l_min              0
_reflns_limit_l_max              24

_oxford_diffrn_Wilson_B_factor   1.80
_oxford_diffrn_Wilson_scale      10.89

_atom_sites_solution_primary     direct
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -2.09
_refine_diff_density_max         1.70


_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         3839
_refine_ls_number_restraints     6
_refine_ls_number_parameters     254
_oxford_refine_ls_R_factor_ref   0.0724
_refine_ls_wR_factor_ref         0.0545
_refine_ls_goodness_of_fit_ref   1.0370
_refine_ls_shift/su_max          0.000233


# The values computed from all data 
_oxford_reflns_number_all        5006
_refine_ls_R_factor_all          0.0907
_refine_ls_wR_factor_all         0.0586

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4181
_refine_ls_R_factor_gt           0.0777
_refine_ls_wR_factor_gt          0.0556

_refine_ls_abs_structure_Flack   0.08(5)
_refine_ls_abs_structure_details 'Flack (1983), 2174 Friedel-pairs'
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 3.39 -1.67 2.76 
;

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Pd1 Pd -0.05112(5) 0.48362(4) 0.49602(3) 0.0218 1.0000 Uani . . . . . . .
Cl1 Cl -0.0540(2) 0.42048(14) 0.38153(9) 0.0313 1.0000 Uani . . . . . . .
Cl2 Cl -0.27864(16) 0.52451(18) 0.48456(9) 0.0340 1.0000 Uani . . . . . . .
P1 P 0.16112(19) 0.49399(18) 0.51340(9) 0.0285 1.0000 Uani . . . . . . .
N1 N 0.1239(5) 0.5618(5) 0.5883(3) 0.0202 1.0000 Uani . . . . . . .
N2 N -0.0804(5) 0.5405(5) 0.6485(3) 0.0260 1.0000 Uani . U . . . . .
C1 C -0.0072(7) 0.5336(6) 0.5928(3) 0.0224 1.0000 Uani . U . . . . .
C2 C 0.2122(6) 0.6236(6) 0.6330(4) 0.0211 1.0000 Uani . . . . . . .
C3 C 0.2249(7) 0.7340(6) 0.6228(4) 0.0260 1.0000 Uani . . . . . . .
C4 C 0.3208(8) 0.7924(6) 0.6582(4) 0.0267 1.0000 Uani . . . . . . .
C5 C 0.4009(7) 0.7386(5) 0.7059(4) 0.0199 1.0000 Uani . . . . . . .
C6 C 0.3828(7) 0.6294(6) 0.7181(4) 0.0259 1.0000 Uani . . . . . . .
C7 C 0.2890(7) 0.5696(6) 0.6811(4) 0.0258 1.0000 Uani . . . . . . .
C8 C 0.5059(8) 0.8022(7) 0.7431(5) 0.0375 1.0000 Uani . . . . . . .
C9 C -0.0402(8) 0.5973(6) 0.7126(4) 0.0338 1.0000 Uani . . . . . . .
C10 C -0.0948(8) 0.7122(6) 0.7115(5) 0.0341 1.0000 Uani . . . . . . .
C11 C -0.0688(9) 0.5388(8) 0.7792(4) 0.0452 1.0000 Uani . . . . . . .
C12 C -0.2059(6) 0.4759(6) 0.6458(3) 0.0277 1.0000 Uani . . . . . . .
C13 C -0.3233(7) 0.5362(7) 0.6716(4) 0.0357 1.0000 Uani . . . . . . .
C14 C -0.1900(8) 0.3616(7) 0.6781(4) 0.0379 1.0000 Uani . . . . . . .
C15 C 0.2464(7) 0.3635(6) 0.5341(4) 0.0270 1.0000 Uani . . . . . . .
C16 C 0.1737(8) 0.3090(8) 0.5929(5) 0.0399 1.0000 Uani . . . . . . .
C17 C 0.2379(9) 0.2907(7) 0.4719(4) 0.0395 1.0000 Uani . . . . . . .
C18 C 0.3916(8) 0.3787(7) 0.5540(5) 0.0381 1.0000 Uani . . . . . . .
C19 C 0.2501(6) 0.5859(6) 0.4553(4) 0.0247 1.0000 Uani . . . . . . .
C20 C 0.2775(8) 0.5243(8) 0.3884(4) 0.0410 1.0000 Uani . . . . . . .
C21 C 0.3765(7) 0.6332(7) 0.4823(4) 0.0392 1.0000 Uani . . . . . . .
C22 C 0.1539(7) 0.6798(7) 0.4397(4) 0.0309 1.0000 Uani . . . . . . .
H31 H 0.1713 0.7703 0.5919 0.0280 1.0000 Uiso . . . . . . .
H41 H 0.3297 0.8671 0.6504 0.0320 1.0000 Uiso . . . . . . .
H61 H 0.4340 0.5953 0.7504 0.0291 1.0000 Uiso . . . . . . .
H71 H 0.2790 0.4951 0.6895 0.0319 1.0000 Uiso . . . . . . .
H81 H 0.5049 0.7840 0.7912 0.0518 1.0000 Uiso . . . . . . .
H82 H 0.4886 0.8800 0.7388 0.0520 1.0000 Uiso . . . . . . .
H83 H 0.5886 0.7860 0.7243 0.0522 1.0000 Uiso . . . . . . .
H91 H 0.0542 0.6058 0.7104 0.0390 1.0000 Uiso . . . . . . .
H101 H -0.0611 0.7519 0.7487 0.0580 1.0000 Uiso . . . . . . .
H102 H -0.0737 0.7476 0.6689 0.0580 1.0000 Uiso . . . . . . .
H103 H -0.1889 0.7096 0.7150 0.0580 1.0000 Uiso . . . . . . .
H111 H -0.0323 0.4681 0.7781 0.0590 1.0000 Uiso . . . . . . .
H112 H -0.0325 0.5803 0.8164 0.0590 1.0000 Uiso . . . . . . .
H113 H -0.1622 0.5346 0.7854 0.0590 1.0000 Uiso . . . . . . .
H121 H -0.2196 0.4619 0.5977 0.0317 1.0000 Uiso . . . . . . .
H131 H -0.3994 0.4931 0.6635 0.0510 1.0000 Uiso . . . . . . .
H132 H -0.3132 0.5494 0.7196 0.0508 1.0000 Uiso . . . . . . .
H133 H -0.3307 0.6048 0.6482 0.0510 1.0000 Uiso . . . . . . .
H141 H -0.1877 0.3678 0.7277 0.0519 1.0000 Uiso . . . . . . .
H142 H -0.1078 0.3296 0.6638 0.0520 1.0000 Uiso . . . . . . .
H143 H -0.2594 0.3157 0.6648 0.0521 1.0000 Uiso . . . . . . .
H161 H 0.1671 0.3538 0.6315 0.0558 1.0000 Uiso . . . . . . .
H162 H 0.2193 0.2408 0.6069 0.0560 1.0000 Uiso . . . . . . .
H163 H 0.0872 0.2851 0.5785 0.0560 1.0000 Uiso . . . . . . .
H171 H 0.2891 0.3160 0.4354 0.0589 1.0000 Uiso . . . . . . .
H172 H 0.2662 0.2154 0.4832 0.0589 1.0000 Uiso . . . . . . .
H173 H 0.1475 0.2831 0.4566 0.0590 1.0000 Uiso . . . . . . .
H181 H 0.4426 0.4038 0.5145 0.0488 1.0000 Uiso . . . . . . .
H182 H 0.4289 0.3138 0.5707 0.0489 1.0000 Uiso . . . . . . .
H183 H 0.4009 0.4359 0.5891 0.0489 1.0000 Uiso . . . . . . .
H201 H 0.3452 0.4681 0.3975 0.0569 1.0000 Uiso . . . . . . .
H202 H 0.3071 0.5719 0.3552 0.0570 1.0000 Uiso . . . . . . .
H203 H 0.2008 0.4852 0.3741 0.0570 1.0000 Uiso . . . . . . .
H211 H 0.4114 0.6870 0.4509 0.0500 1.0000 Uiso . . . . . . .
H212 H 0.3633 0.6719 0.5261 0.0500 1.0000 Uiso . . . . . . .
H213 H 0.4404 0.5780 0.4899 0.0500 1.0000 Uiso . . . . . . .
H221 H 0.1274 0.7151 0.4811 0.0489 1.0000 Uiso . . . . . . .
H222 H 0.1949 0.7323 0.4099 0.0490 1.0000 Uiso . . . . . . .
H223 H 0.0764 0.6520 0.4167 0.0490 1.0000 Uiso . . . . . . .

_refine_ls_extinction_coef       19.901
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.3137(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Cl1 . 2.3657(18) yes
Pd1 . Cl2 . 2.3956(18) yes
Pd1 . P1 . 2.2052(18) yes
Pd1 . C1 . 2.037(7) yes
P1 . N1 . 1.725(6) yes
P1 . C15 . 1.866(7) yes
P1 . C19 . 1.840(7) yes
N1 . C1 . 1.390(8) yes
N1 . C2 . 1.468(8) yes
N2 . C1 . 1.323(9) yes
N2 . C9 . 1.490(9) yes
N2 . C12 . 1.511(9) yes
C2 . C3 . 1.374(10) yes
C2 . C7 . 1.392(10) yes
C3 . C4 . 1.399(11) yes
C3 . H31 . 0.930 no
C4 . C5 . 1.406(10) yes
C4 . H41 . 0.932 no
C5 . C6 . 1.372(10) yes
C5 . C8 . 1.513(10) yes
C6 . C7 . 1.407(10) yes
C6 . H61 . 0.921 no
C7 . H71 . 0.934 no
C8 . H81 . 0.966 no
C8 . H82 . 0.973 no
C8 . H83 . 0.945 no
C9 . C10 . 1.515(11) yes
C9 . C11 . 1.514(11) yes
C9 . H91 . 0.974 no
C10 . H101 . 0.940 no
C10 . H102 . 0.963 no
C10 . H103 . 0.968 no
C11 . H111 . 0.943 no
C11 . H112 . 0.963 no
C11 . H113 . 0.967 no
C12 . C13 . 1.499(10) yes
C12 . C14 . 1.546(11) yes
C12 . H121 . 0.964 no
C13 . H131 . 0.955 no
C13 . H132 . 0.957 no
C13 . H133 . 0.959 no
C14 . H141 . 0.970 no
C14 . H142 . 0.971 no
C14 . H143 . 0.943 no
C15 . C16 . 1.523(10) yes
C15 . C17 . 1.509(11) yes
C15 . C18 . 1.549(11) yes
C16 . H161 . 0.936 no
C16 . H162 . 0.996 no
C16 . H163 . 0.975 no
C17 . H171 . 0.938 no
C17 . H172 . 0.993 no
C17 . H173 . 0.978 no
C18 . H181 . 0.981 no
C18 . H182 . 0.940 no
C18 . H183 . 0.984 no
C19 . C20 . 1.535(10) yes
C19 . C21 . 1.514(10) yes
C19 . C22 . 1.546(10) yes
C20 . H201 . 0.994 no
C20 . H202 . 0.922 no
C20 . H203 . 0.962 no
C21 . H211 . 0.970 no
C21 . H212 . 0.987 no
C21 . H213 . 0.953 no
C22 . H221 . 0.956 no
C22 . H222 . 0.964 no
C22 . H223 . 0.974 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Pd1 . Cl2 . 88.16(7) yes
Cl1 . Pd1 . P1 . 100.18(7) yes
Cl2 . Pd1 . P1 . 164.26(8) yes
Cl1 . Pd1 . C1 . 167.9(2) yes
Cl2 . Pd1 . C1 . 103.8(2) yes
P1 . Pd1 . C1 . 67.8(2) yes
Pd1 . P1 . N1 . 86.56(18) yes
Pd1 . P1 . C15 . 116.5(3) yes
N1 . P1 . C15 . 109.5(3) yes
Pd1 . P1 . C19 . 115.4(2) yes
N1 . P1 . C19 . 109.7(3) yes
C15 . P1 . C19 . 115.2(3) yes
P1 . N1 . C1 . 98.5(4) yes
P1 . N1 . C2 . 128.1(4) yes
C1 . N1 . C2 . 133.3(6) yes
C1 . N2 . C9 . 124.3(6) yes
C1 . N2 . C12 . 114.9(5) yes
C9 . N2 . C12 . 120.6(6) yes
N1 . C1 . N2 . 125.7(6) yes
N1 . C1 . Pd1 . 103.3(5) yes
N2 . C1 . Pd1 . 131.0(5) yes
N1 . C2 . C3 . 118.7(6) yes
N1 . C2 . C7 . 120.3(6) yes
C3 . C2 . C7 . 120.8(7) yes
C2 . C3 . C4 . 120.0(7) yes
C2 . C3 . H31 . 120.6 no
C4 . C3 . H31 . 119.4 no
C3 . C4 . C5 . 119.8(7) yes
C3 . C4 . H41 . 119.4 no
C5 . C4 . H41 . 120.8 no
C4 . C5 . C6 . 119.5(7) yes
C4 . C5 . C8 . 119.4(6) yes
C6 . C5 . C8 . 121.0(7) yes
C5 . C6 . C7 . 120.8(6) yes
C5 . C6 . H61 . 118.9 no
C7 . C6 . H61 . 120.3 no
C6 . C7 . C2 . 119.0(7) yes
C6 . C7 . H71 . 119.7 no
C2 . C7 . H71 . 121.3 no
C5 . C8 . H81 . 109.9 no
C5 . C8 . H82 . 109.5 no
H81 . C8 . H82 . 107.9 no
C5 . C8 . H83 . 110.1 no
H81 . C8 . H83 . 109.9 no
H82 . C8 . H83 . 109.5 no
N2 . C9 . C10 . 108.7(6) yes
N2 . C9 . C11 . 116.6(7) yes
C10 . C9 . C11 . 112.4(7) yes
N2 . C9 . H91 . 106.8 no
C10 . C9 . H91 . 105.5 no
C11 . C9 . H91 . 106.2 no
C9 . C10 . H101 . 109.6 no
C9 . C10 . H102 . 110.4 no
H101 . C10 . H102 . 110.5 no
C9 . C10 . H103 . 109.7 no
H101 . C10 . H103 . 109.3 no
H102 . C10 . H103 . 107.4 no
C9 . C11 . H111 . 109.8 no
C9 . C11 . H112 . 108.9 no
H111 . C11 . H112 . 110.5 no
C9 . C11 . H113 . 108.9 no
H111 . C11 . H113 . 110.2 no
H112 . C11 . H113 . 108.4 no
N2 . C12 . C13 . 114.4(6) yes
N2 . C12 . C14 . 111.8(6) yes
C13 . C12 . C14 . 113.2(6) yes
N2 . C12 . H121 . 104.5 no
C13 . C12 . H121 . 107.3 no
C14 . C12 . H121 . 104.6 no
C12 . C13 . H131 . 109.2 no
C12 . C13 . H132 . 109.0 no
H131 . C13 . H132 . 110.1 no
C12 . C13 . H133 . 109.6 no
H131 . C13 . H133 . 110.0 no
H132 . C13 . H133 . 109.0 no
C12 . C14 . H141 . 109.8 no
C12 . C14 . H142 . 109.8 no
H141 . C14 . H142 . 107.3 no
C12 . C14 . H143 . 110.4 no
H141 . C14 . H143 . 109.8 no
H142 . C14 . H143 . 109.6 no
P1 . C15 . C16 . 108.1(5) yes
P1 . C15 . C17 . 107.8(5) yes
C16 . C15 . C17 . 108.5(7) yes
P1 . C15 . C18 . 113.7(5) yes
C16 . C15 . C18 . 109.5(6) yes
C17 . C15 . C18 . 109.2(6) yes
C15 . C16 . H161 . 112.6 no
C15 . C16 . H162 . 110.3 no
H161 . C16 . H162 . 107.8 no
C15 . C16 . H163 . 111.0 no
H161 . C16 . H163 . 110.1 no
H162 . C16 . H163 . 104.7 no
C15 . C17 . H171 . 112.6 no
C15 . C17 . H172 . 110.8 no
H171 . C17 . H172 . 108.3 no
C15 . C17 . H173 . 110.9 no
H171 . C17 . H173 . 109.2 no
H172 . C17 . H173 . 104.7 no
C15 . C18 . H181 . 110.6 no
C15 . C18 . H182 . 112.1 no
H181 . C18 . H182 . 108.6 no
C15 . C18 . H183 . 110.7 no
H181 . C18 . H183 . 105.7 no
H182 . C18 . H183 . 108.8 no
P1 . C19 . C20 . 108.3(5) yes
P1 . C19 . C21 . 116.3(5) yes
C20 . C19 . C21 . 109.2(6) yes
P1 . C19 . C22 . 105.2(4) yes
C20 . C19 . C22 . 108.3(6) yes
C21 . C19 . C22 . 109.2(6) yes
C19 . C20 . H201 . 108.4 no
C19 . C20 . H202 . 110.3 no
H201 . C20 . H202 . 109.6 no
C19 . C20 . H203 . 110.1 no
H201 . C20 . H203 . 106.1 no
H202 . C20 . H203 . 112.3 no
C19 . C21 . H211 . 110.8 no
C19 . C21 . H212 . 111.6 no
H211 . C21 . H212 . 105.8 no
C19 . C21 . H213 . 111.7 no
H211 . C21 . H213 . 109.1 no
H212 . C21 . H213 . 107.5 no
C19 . C22 . H221 . 110.6 no
C19 . C22 . H222 . 109.8 no
H221 . C22 . H222 . 109.3 no
C19 . C22 . H223 . 110.5 no
H221 . C22 . H223 . 108.5 no
H222 . C22 . H223 . 108.1 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C9 . H91 . C2 . 140 0.97 2.22 3.034(11) yes
C9 . H91 . C7 . 160 0.97 2.51 3.447(11) yes
C21 . H212 . C3 . 152 0.99 2.48 3.386(11) yes
####################################################################### 
# 
# 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_1
_audit_block_doi                 10.5517/cc13wwkf
_database_code_depnum_ccdc_archive 'CCDC 1039695'
_audit_update_record             
;
2014-12-16 deposited with the CCDC.
2015-07-30 downloaded from the CCDC.
;

_cell_length_a                   12.6614(3)
_cell_length_b                   15.7007(3)
_cell_length_c                   16.8900(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3357.61(13)

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21 '
_symmetry_space_group_name_Hall  'P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,-y+1/2,-z
-x,y+1/2,-z+1/2
-x+1/2,-y,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C33 H54 Cl3 F4.50 N3 P1.50 Pd1.50 
# Dc =      1.76 Fooo =   1480.00 Mu =     11.79 M =    890.72
# Found Formula = C28 H45 Cl2 F3 N5 P1 Pd1 
# Dc =      1.42 FOOO =   1480.00 Mu =      8.02 M =    716.97

_chemical_formula_sum            'C28 H45 Cl2 F3 N5 P1 Pd1'
_chemical_formula_moiety         'C28 H45 Cl2 F3 N5 P1 Pd1'
_chemical_compound_source        ?
_chemical_formula_weight         716.97


_cell_measurement_reflns_used    7996
_cell_measurement_theta_min      2
_cell_measurement_theta_max      26
_cell_measurement_temperature    123

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.360
_exptl_crystal_size_mid          0.490
_exptl_crystal_size_max          0.600

_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1480
_exptl_absorpt_coefficient_mu    0.802

# Sheldrick geometric approximatio 0.68 0.75 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.75
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω/2θ

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      123
_diffrn_reflns_number            15793
_reflns_number_total             6840
_diffrn_reflns_av_R_equivalents  0.032
# Number of reflections without Friedels Law is 6840 
# Number of reflections with Friedels Law is 3859 
# Theoretical number of reflections is about 3454 


_diffrn_reflns_theta_min         1.771
_diffrn_reflns_theta_max         26.431
_diffrn_measured_fraction_theta_max 1.000

_diffrn_reflns_theta_full        26.431
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       21
_reflns_limit_h_min              -15
_reflns_limit_h_max              15
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              21

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Direct
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.56
_refine_diff_density_max         0.61


_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         6167
_refine_ls_number_restraints     0
_refine_ls_number_parameters     362
_oxford_refine_ls_R_factor_ref   0.0267
_refine_ls_wR_factor_ref         0.0220
_refine_ls_goodness_of_fit_ref   1.1110
_refine_ls_shift/su_max          0.0020539
_refine_ls_shift/su_mean         0.0000407


# The values computed from all data 
_oxford_reflns_number_all        6814
_refine_ls_R_factor_all          0.0314
_refine_ls_wR_factor_all         0.0246

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                6368
_refine_ls_R_factor_gt           0.0277
_refine_ls_wR_factor_gt          0.0224

_refine_ls_abs_structure_Flack   0.023(19)
_refine_ls_abs_structure_details 'Flack (1983), 2981 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.206 -0.678 -0.102 -0.249 
;

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Pd1 Pd 0.618101(16) 0.539128(12) 0.227060(11) 0.0128 1.0000 Uani . . . . . .
Cl1 Cl 0.60402(6) 0.41451(4) 0.30410(4) 0.0201 1.0000 Uani . . . . . .
Cl2 Cl 0.64803(5) 0.44679(4) 0.11570(4) 0.0215 1.0000 Uani . . . . . .
P1 P 0.58528(5) 0.62836(4) 0.32395(4) 0.0132 1.0000 Uani . . . . . .
F1 F 0.70783(16) 1.07673(13) 0.40622(14) 0.0416 1.0000 Uani . . . . . .
F2 F 0.83032(17) 1.07433(12) 0.31978(13) 0.0420 1.0000 Uani . . . . . .
F3 F 0.85457(19) 1.01427(13) 0.43142(13) 0.0486 1.0000 Uani . . . . . .
N1 N 0.62878(19) 0.70820(12) 0.26226(12) 0.0144 1.0000 Uani . . . . . .
N2 N 0.64685(18) 0.70095(14) 0.12183(13) 0.0147 1.0000 Uani . . . . . .
N3 N 0.9311(3) 0.6829(3) 0.1628(2) 0.0599 1.0000 Uani . . . . . .
N4 N -0.0493(3) 0.2859(3) 0.1452(2) 0.0588 1.0000 Uani . . . . . .
N5 N 0.0552(3) 0.4851(2) 0.33981(19) 0.0457 1.0000 Uani . . . . . .
C1 C 0.6361(2) 0.66362(16) 0.19110(16) 0.0149 1.0000 Uani . . . . . .
C2 C 0.7737(2) 0.80869(17) 0.28404(17) 0.0185 1.0000 Uani . . . . . .
C3 C 0.8107(2) 0.88533(19) 0.31264(18) 0.0215 1.0000 Uani . . . . . .
C4 C 0.7402(2) 0.94529(17) 0.34265(16) 0.0183 1.0000 Uani . . . . . .
C5 C 0.6327(2) 0.92909(17) 0.34278(15) 0.0182 1.0000 Uani . . . . . .
C6 C 0.5951(2) 0.85197(16) 0.31429(15) 0.0151 1.0000 Uani . . . . . .
C7 C 0.6660(2) 0.79209(17) 0.28540(16) 0.0145 1.0000 Uani . . . . . .
C8 C 0.6704(2) 0.62194(19) 0.41302(17) 0.0201 1.0000 Uani . . . . . .
C9 C 0.6236(3) 0.55349(18) 0.46869(15) 0.0237 1.0000 Uani . . . . . .
C10 C 0.6829(3) 0.7059(2) 0.45932(18) 0.0253 1.0000 Uani . . . . . .
C11 C 0.7803(2) 0.5914(2) 0.38455(19) 0.0245 1.0000 Uani . . . . . .
C12 C 0.4415(2) 0.64476(18) 0.34518(17) 0.0188 1.0000 Uani . . . . . .
C13 C 0.4167(3) 0.70415(19) 0.41486(19) 0.0256 1.0000 Uani . . . . . .
C14 C 0.3933(2) 0.55596(17) 0.36176(17) 0.0235 1.0000 Uani . . . . . .
C15 C 0.3921(2) 0.67974(16) 0.26853(19) 0.0224 1.0000 Uani . . . . . .
C16 C 0.6321(2) 0.79558(16) 0.11081(15) 0.0181 1.0000 Uani . . . . . .
C17 C 0.7365(3) 0.84277(19) 0.09730(19) 0.0243 1.0000 Uani . . . . . .
C18 C 0.5504(3) 0.8157(2) 0.04791(18) 0.0243 1.0000 Uani . . . . . .
C19 C 0.6633(2) 0.64398(19) 0.05167(16) 0.0201 1.0000 Uani . . . . . .
C20 C 0.7450(3) 0.6783(2) -0.00591(19) 0.0276 1.0000 Uani . . . . . .
C21 C 0.5602(3) 0.6197(2) 0.01154(19) 0.0301 1.0000 Uani . . . . . .
C22 C 0.7826(2) 1.0275(2) 0.37492(19) 0.0266 1.0000 Uani . . . . . .
C23 C 0.9229(3) 0.6115(3) 0.1686(2) 0.0413 1.0000 Uani . . . . . .
C24 C 0.9125(3) 0.5201(3) 0.1755(2) 0.0447 1.0000 Uani . . . . . .
C25 C -0.0867(3) 0.2965(3) 0.2052(2) 0.0422 1.0000 Uani . . . . . .
C26 C -0.1328(3) 0.3124(2) 0.2824(3) 0.0509 1.0000 Uani . . . . . .
C27 C 0.0645(2) 0.5337(3) 0.38905(18) 0.0320 1.0000 Uani . . . . . .
C28 C 0.0751(3) 0.5953(3) 0.4525(2) 0.0431 1.0000 Uani . . . . . .
H21 H 0.8205 0.7664 0.2637 0.0221 1.0000 Uiso . . . . . .
H31 H 0.8844 0.8982 0.3134 0.0261 1.0000 Uiso . . . . . .
H51 H 0.5854 0.9701 0.3637 0.0238 1.0000 Uiso . . . . . .
H61 H 0.5211 0.8403 0.3157 0.0192 1.0000 Uiso . . . . . .
H91 H 0.6143 0.5016 0.4395 0.0382 1.0000 Uiso . . . . . .
H92 H 0.6717 0.5426 0.5115 0.0382 1.0000 Uiso . . . . . .
H93 H 0.5564 0.5714 0.4898 0.0377 1.0000 Uiso . . . . . .
H101 H 0.6138 0.7281 0.4723 0.0389 1.0000 Uiso . . . . . .
H102 H 0.7223 0.6928 0.5066 0.0384 1.0000 Uiso . . . . . .
H103 H 0.7217 0.7475 0.4270 0.0388 1.0000 Uiso . . . . . .
H111 H 0.8099 0.6320 0.3477 0.0379 1.0000 Uiso . . . . . .
H112 H 0.8267 0.5875 0.4302 0.0380 1.0000 Uiso . . . . . .
H113 H 0.7755 0.5364 0.3577 0.0382 1.0000 Uiso . . . . . .
H131 H 0.3416 0.7080 0.4191 0.0385 1.0000 Uiso . . . . . .
H132 H 0.4463 0.6821 0.4644 0.0381 1.0000 Uiso . . . . . .
H133 H 0.4446 0.7603 0.4044 0.0379 1.0000 Uiso . . . . . .
H141 H 0.4104 0.5161 0.3206 0.0381 1.0000 Uiso . . . . . .
H142 H 0.4209 0.5338 0.4125 0.0384 1.0000 Uiso . . . . . .
H143 H 0.3179 0.5621 0.3656 0.0377 1.0000 Uiso . . . . . .
H151 H 0.3169 0.6804 0.2740 0.0340 1.0000 Uiso . . . . . .
H152 H 0.4153 0.7369 0.2568 0.0342 1.0000 Uiso . . . . . .
H153 H 0.4113 0.6449 0.2227 0.0341 1.0000 Uiso . . . . . .
H161 H 0.6039 0.8166 0.1617 0.0223 1.0000 Uiso . . . . . .
H171 H 0.7569 0.8393 0.0421 0.0368 1.0000 Uiso . . . . . .
H172 H 0.7276 0.9021 0.1114 0.0369 1.0000 Uiso . . . . . .
H173 H 0.7908 0.8206 0.1308 0.0370 1.0000 Uiso . . . . . .
H181 H 0.4854 0.7835 0.0555 0.0359 1.0000 Uiso . . . . . .
H182 H 0.5316 0.8756 0.0482 0.0360 1.0000 Uiso . . . . . .
H183 H 0.5774 0.8028 -0.0039 0.0354 1.0000 Uiso . . . . . .
H191 H 0.6941 0.5913 0.0729 0.0260 1.0000 Uiso . . . . . .
H201 H 0.7606 0.6365 -0.0467 0.0416 1.0000 Uiso . . . . . .
H202 H 0.7208 0.7290 -0.0305 0.0406 1.0000 Uiso . . . . . .
H203 H 0.8110 0.6905 0.0206 0.0412 1.0000 Uiso . . . . . .
H211 H 0.5058 0.6053 0.0505 0.0459 1.0000 Uiso . . . . . .
H212 H 0.5328 0.6654 -0.0196 0.0467 1.0000 Uiso . . . . . .
H213 H 0.5713 0.5716 -0.0226 0.0460 1.0000 Uiso . . . . . .
H241 H 0.9534 0.4908 0.1344 0.0664 1.0000 Uiso . . . . . .
H242 H 0.9412 0.5017 0.2263 0.0663 1.0000 Uiso . . . . . .
H243 H 0.8406 0.5039 0.1712 0.0667 1.0000 Uiso . . . . . .
H261 H -0.1998 0.3405 0.2799 0.0759 1.0000 Uiso . . . . . .
H262 H -0.0853 0.3474 0.3136 0.0760 1.0000 Uiso . . . . . .
H263 H -0.1431 0.2598 0.3112 0.0761 1.0000 Uiso . . . . . .
H281 H 0.0675 0.6512 0.4295 0.0641 1.0000 Uiso . . . . . .
H282 H 0.0218 0.5836 0.4922 0.0638 1.0000 Uiso . . . . . .
H283 H 0.1453 0.5890 0.4767 0.0642 1.0000 Uiso . . . . . .

_refine_ls_extinction_coef       2.374
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.24945(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Cl1 . 2.3565(7) yes
Pd1 . Cl2 . 2.4049(7) yes
Pd1 . P1 . 2.1940(7) yes
Pd1 . C1 . 2.059(3) yes
P1 . N1 . 1.721(2) yes
P1 . C8 . 1.854(3) yes
P1 . C12 . 1.873(3) yes
F1 . C22 . 1.331(4) yes
F2 . C22 . 1.331(4) yes
F3 . C22 . 1.336(4) yes
N1 . C1 . 1.394(3) yes
N1 . C7 . 1.452(3) yes
N2 . C1 . 1.316(3) yes
N2 . C16 . 1.509(3) yes
N2 . C19 . 1.499(3) yes
N3 . C23 . 1.131(5) yes
N4 . C25 . 1.131(5) yes
N5 . C27 . 1.136(5) yes
C2 . C3 . 1.379(4) yes
C2 . C7 . 1.389(4) yes
C2 . H21 . 0.954 no
C3 . C4 . 1.393(4) yes
C3 . H31 . 0.955 no
C4 . C5 . 1.385(4) yes
C4 . C22 . 1.501(4) yes
C5 . C6 . 1.387(4) yes
C5 . H51 . 0.948 no
C6 . C7 . 1.389(4) yes
C6 . H61 . 0.954 no
C8 . C9 . 1.546(4) yes
C8 . C10 . 1.541(4) yes
C8 . C11 . 1.548(4) yes
C9 . H91 . 0.959 no
C9 . H92 . 0.960 no
C9 . H93 . 0.964 no
C10 . H101 . 0.967 no
C10 . H102 . 0.964 no
C10 . H103 . 0.983 no
C11 . H111 . 0.967 no
C11 . H112 . 0.971 no
C11 . H113 . 0.976 no
C12 . C13 . 1.534(4) yes
C12 . C14 . 1.548(4) yes
C12 . C15 . 1.539(4) yes
C13 . H131 . 0.954 no
C13 . H132 . 0.980 no
C13 . H133 . 0.965 no
C14 . H141 . 0.960 no
C14 . H142 . 0.989 no
C14 . H143 . 0.962 no
C15 . H151 . 0.956 no
C15 . H152 . 0.965 no
C15 . H153 . 0.979 no
C16 . C17 . 1.533(4) yes
C16 . C18 . 1.516(4) yes
C16 . H161 . 0.988 no
C17 . H171 . 0.970 no
C17 . H172 . 0.968 no
C17 . H173 . 0.956 no
C18 . H181 . 0.974 no
C18 . H182 . 0.969 no
C18 . H183 . 0.961 no
C19 . C20 . 1.519(4) yes
C19 . C21 . 1.519(4) yes
C19 . H191 . 0.982 no
C20 . H201 . 0.972 no
C20 . H202 . 0.948 no
C20 . H203 . 0.967 no
C21 . H211 . 0.979 no
C21 . H212 . 0.955 no
C21 . H213 . 0.960 no
C23 . C24 . 1.445(6) yes
C24 . H241 . 0.981 no
C24 . H242 . 0.975 no
C24 . H243 . 0.948 no
C25 . C26 . 1.450(6) yes
C26 . H261 . 0.957 no
C26 . H262 . 0.970 no
C26 . H263 . 0.968 no
C27 . C28 . 1.450(5) yes
C28 . H281 . 0.964 no
C28 . H282 . 0.969 no
C28 . H283 . 0.983 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Pd1 . Cl2 . 86.74(2) yes
Cl1 . Pd1 . P1 . 95.97(3) yes
Cl2 . Pd1 . P1 . 176.56(3) yes
Cl1 . Pd1 . C1 . 163.58(8) yes
Cl2 . Pd1 . C1 . 108.91(8) yes
P1 . Pd1 . C1 . 68.59(8) yes
Pd1 . P1 . N1 . 87.30(7) yes
Pd1 . P1 . C8 . 117.41(10) yes
N1 . P1 . C8 . 110.17(12) yes
Pd1 . P1 . C12 . 114.49(10) yes
N1 . P1 . C12 . 109.08(12) yes
C8 . P1 . C12 . 114.68(13) yes
P1 . N1 . C1 . 100.24(15) yes
P1 . N1 . C7 . 126.98(17) yes
C1 . N1 . C7 . 131.7(2) yes
C1 . N2 . C16 . 122.4(2) yes
C1 . N2 . C19 . 116.8(2) yes
C16 . N2 . C19 . 120.5(2) yes
N1 . C1 . N2 . 123.4(2) yes
N1 . C1 . Pd1 . 102.41(16) yes
N2 . C1 . Pd1 . 134.1(2) yes
C3 . C2 . C7 . 119.4(3) yes
C3 . C2 . H21 . 121.6 no
C7 . C2 . H21 . 119.0 no
C2 . C3 . C4 . 120.0(3) yes
C2 . C3 . H31 . 121.4 no
C4 . C3 . H31 . 118.6 no
C3 . C4 . C5 . 120.4(2) yes
C3 . C4 . C22 . 119.0(3) yes
C5 . C4 . C22 . 120.6(3) yes
C4 . C5 . C6 . 119.8(2) yes
C4 . C5 . H51 . 119.8 no
C6 . C5 . H51 . 120.4 no
C5 . C6 . C7 . 119.4(2) yes
C5 . C6 . H61 . 119.8 no
C7 . C6 . H61 . 120.8 no
N1 . C7 . C6 . 119.9(2) yes
N1 . C7 . C2 . 119.0(2) yes
C6 . C7 . C2 . 120.9(2) yes
P1 . C8 . C9 . 108.0(2) yes
P1 . C8 . C10 . 115.1(2) yes
C9 . C8 . C10 . 109.0(2) yes
P1 . C8 . C11 . 106.70(19) yes
C9 . C8 . C11 . 108.5(2) yes
C10 . C8 . C11 . 109.4(3) yes
C8 . C9 . H91 . 109.0 no
C8 . C9 . H92 . 109.8 no
H91 . C9 . H92 . 108.3 no
C8 . C9 . H93 . 111.2 no
H91 . C9 . H93 . 109.2 no
H92 . C9 . H93 . 109.4 no
C8 . C10 . H101 . 109.4 no
C8 . C10 . H102 . 106.9 no
H101 . C10 . H102 . 111.0 no
C8 . C10 . H103 . 109.7 no
H101 . C10 . H103 . 109.8 no
H102 . C10 . H103 . 109.9 no
C8 . C11 . H111 . 110.1 no
C8 . C11 . H112 . 108.5 no
H111 . C11 . H112 . 108.5 no
C8 . C11 . H113 . 111.3 no
H111 . C11 . H113 . 107.9 no
H112 . C11 . H113 . 110.5 no
P1 . C12 . C13 . 115.4(2) yes
P1 . C12 . C14 . 107.12(18) yes
C13 . C12 . C14 . 109.1(2) yes
P1 . C12 . C15 . 106.44(19) yes
C13 . C12 . C15 . 110.2(2) yes
C14 . C12 . C15 . 108.3(2) yes
C12 . C13 . H131 . 107.4 no
C12 . C13 . H132 . 111.2 no
H131 . C13 . H132 . 109.9 no
C12 . C13 . H133 . 109.9 no
H131 . C13 . H133 . 108.7 no
H132 . C13 . H133 . 109.7 no
C12 . C14 . H141 . 111.5 no
C12 . C14 . H142 . 109.5 no
H141 . C14 . H142 . 108.5 no
C12 . C14 . H143 . 108.3 no
H141 . C14 . H143 . 109.8 no
H142 . C14 . H143 . 109.2 no
C12 . C15 . H151 . 109.1 no
C12 . C15 . H152 . 112.4 no
H151 . C15 . H152 . 108.3 no
C12 . C15 . H153 . 111.4 no
H151 . C15 . H153 . 109.2 no
H152 . C15 . H153 . 106.4 no
N2 . C16 . C17 . 112.8(2) yes
N2 . C16 . C18 . 112.1(2) yes
C17 . C16 . C18 . 112.5(2) yes
N2 . C16 . H161 . 105.5 no
C17 . C16 . H161 . 106.2 no
C18 . C16 . H161 . 107.1 no
C16 . C17 . H171 . 110.2 no
C16 . C17 . H172 . 109.2 no
H171 . C17 . H172 . 108.8 no
C16 . C17 . H173 . 110.9 no
H171 . C17 . H173 . 110.9 no
H172 . C17 . H173 . 106.8 no
C16 . C18 . H181 . 112.1 no
C16 . C18 . H182 . 111.4 no
H181 . C18 . H182 . 107.2 no
C16 . C18 . H183 . 110.5 no
H181 . C18 . H183 . 108.1 no
H182 . C18 . H183 . 107.3 no
N2 . C19 . C20 . 112.9(2) yes
N2 . C19 . C21 . 112.5(2) yes
C20 . C19 . C21 . 112.9(3) yes
N2 . C19 . H191 . 105.6 no
C20 . C19 . H191 . 105.1 no
C21 . C19 . H191 . 107.1 no
C19 . C20 . H201 . 110.6 no
C19 . C20 . H202 . 110.9 no
H201 . C20 . H202 . 108.8 no
C19 . C20 . H203 . 111.3 no
H201 . C20 . H203 . 106.7 no
H202 . C20 . H203 . 108.5 no
C19 . C21 . H211 . 111.2 no
C19 . C21 . H212 . 111.7 no
H211 . C21 . H212 . 106.7 no
C19 . C21 . H213 . 109.9 no
H211 . C21 . H213 . 108.9 no
H212 . C21 . H213 . 108.3 no
C4 . C22 . F3 . 111.7(3) yes
C4 . C22 . F1 . 112.9(2) yes
F3 . C22 . F1 . 107.0(3) yes
C4 . C22 . F2 . 112.5(3) yes
F3 . C22 . F2 . 106.0(3) yes
F1 . C22 . F2 . 106.3(3) yes
N3 . C23 . C24 . 179.7(5) yes
C23 . C24 . H241 . 111.1 no
C23 . C24 . H242 . 109.4 no
H241 . C24 . H242 . 106.7 no
C23 . C24 . H243 . 110.3 no
H241 . C24 . H243 . 109.1 no
H242 . C24 . H243 . 110.3 no
N4 . C25 . C26 . 178.3(4) yes
C25 . C26 . H261 . 113.3 no
C25 . C26 . H262 . 109.7 no
H261 . C26 . H262 . 108.1 no
C25 . C26 . H263 . 111.1 no
H261 . C26 . H263 . 107.2 no
H262 . C26 . H263 . 107.1 no
N5 . C27 . C28 . 179.2(4) yes
C27 . C28 . H281 . 107.4 no
C27 . C28 . H282 . 108.6 no
H281 . C28 . H282 . 112.5 no
C27 . C28 . H283 . 108.9 no
H281 . C28 . H283 . 110.4 no
H282 . C28 . H283 . 108.9 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C2 . H21 . N3 . 159.0(2) 0.954 2.566 3.474(4) yes
C10 . H103 . C7 . 123.77(19) 0.983 2.590 3.241(4) yes
C16 . H161 . C7 . 128.40(18) 0.988 2.265 2.981(4) yes
C24 . H242 . N5 1_655 162.4(2) 0.975 2.415 3.357(4) yes
C28 . H281 . N4 3_555 173.1(3) 0.964 2.474 3.432(4) yes
####################################################################### 
# 
# 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_1
_audit_block_doi                 10.5517/cc13wwlg
_database_code_depnum_ccdc_archive 'CCDC 1039696'
_audit_update_record             
;
2014-12-16 deposited with the CCDC.
2015-07-30 downloaded from the CCDC.
;

_cell_length_a                   15.5317(3)
_cell_length_b                   10.2561(2)
_cell_length_c                   33.1968(6)
_cell_angle_alpha                90
_cell_angle_beta                 92.1090(10)
_cell_angle_gamma                90
_cell_volume                     5284.49(17)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pd -0.9988 1.0072 19.3319 0.6987 15.5017 7.9893 5.2954 25.2052 0.6058 76.8986
5.2659 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C44 H76 Cl4 N4 O2 P2 Pd2 
# Dc =      1.39 Fooo =   2392.00 Mu =      9.80 M =   1109.67
# Found Formula = C46 H81 Cl4 N5 O2 P2 Pd2 
# Dc =      1.45 FOOO =   2392.00 Mu =      9.84 M =   1152.74

_chemical_formula_sum            'C46 H81 Cl4 N5 O2 P2 Pd2'
_chemical_formula_moiety         'C46 H81 Cl4 N5 O2 P2 Pd2'
_chemical_compound_source        ?
_chemical_formula_weight         1152.74


_cell_measurement_reflns_used    9891
_cell_measurement_theta_min      2
_cell_measurement_theta_max      26
_cell_measurement_temperature    123

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.280
_exptl_crystal_size_mid          0.390
_exptl_crystal_size_max          0.460

_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2392
_exptl_absorpt_coefficient_mu    0.984

# Sheldrick geometric approximatio 0.68 0.76 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_T_max  0.76
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω/2θ

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      123
_diffrn_reflns_number            42280
_reflns_number_total             10769
_diffrn_reflns_av_R_equivalents  0.045
# Number of reflections without Friedels Law is 10769 
# Number of reflections with Friedels Law is 0 
# Theoretical number of reflections is about 10823 


_diffrn_reflns_theta_min         1.228
_diffrn_reflns_theta_max         26.385
_diffrn_measured_fraction_theta_max 0.995

_diffrn_reflns_theta_full        26.385
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       37
_reflns_limit_h_min              -19
_reflns_limit_h_max              19
_reflns_limit_k_min              0
_reflns_limit_k_max              12
_reflns_limit_l_min              0
_reflns_limit_l_max              41

_oxford_diffrn_Wilson_B_factor   1.08
_oxford_diffrn_Wilson_scale      30.93

_atom_sites_solution_primary     Direct
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.80
_refine_diff_density_max         0.51

_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_refine_ls_number_reflns         8616
_refine_ls_number_restraints     0
_refine_ls_number_parameters     550
_oxford_refine_ls_R_factor_ref   0.0334
_refine_ls_wR_factor_ref         0.0395
_refine_ls_goodness_of_fit_ref   1.0675
_refine_ls_shift/su_max          0.0036086
_refine_ls_shift/su_mean         0.0000503


# The values computed from all data 
_oxford_reflns_number_all        10727
_refine_ls_R_factor_all          0.0470
_refine_ls_wR_factor_all         0.0426

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9170
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_gt          0.0404

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    noref
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 1.54 0.489 1.26 
;

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Pd1 Pd 0.341359(12) 0.384127(18) 0.539823(6) 0.0110 1.0000 Uani . . . . . .
Pd2 Pd 0.052433(12) 0.405121(19) 0.708639(6) 0.0116 1.0000 Uani . . . . . .
Cl1 Cl 0.22593(5) 0.41632(7) 0.49273(2) 0.0217 1.0000 Uani . . . . . .
Cl2 Cl 0.36339(4) 0.17751(6) 0.50854(2) 0.0178 1.0000 Uani . . . . . .
Cl3 Cl 0.08343(4) 0.41161(7) 0.77885(2) 0.0192 1.0000 Uani . . . . . .
Cl4 Cl 0.07540(5) 0.63462(7) 0.70666(2) 0.0252 1.0000 Uani . . . . . .
P1 P 0.34421(4) 0.58249(6) 0.56516(2) 0.0119 1.0000 Uani . . . . . .
P2 P 0.05892(4) 0.19177(6) 0.70028(2) 0.0113 1.0000 Uani . . . . . .
O1 O 0.69510(14) 0.8880(2) 0.64035(6) 0.0226 1.0000 Uani . . . . . .
O2 O 0.11110(13) -0.0449(2) 0.50736(6) 0.0198 1.0000 Uani . . . . . .
N1 N 0.43823(14) 0.5372(2) 0.59043(7) 0.0127 1.0000 Uani . . . . . .
N2 N 0.47595(14) 0.3191(2) 0.60783(7) 0.0128 1.0000 Uani . . . . . .
N3 N 0.04636(14) 0.2231(2) 0.64926(6) 0.0125 1.0000 Uani . . . . . .
N4 N -0.03000(14) 0.4082(2) 0.62288(7) 0.0135 1.0000 Uani . . . . . .
N5 N -0.2522(2) 0.3741(4) 0.74208(11) 0.0462 1.0000 Uani . . . . . .
C1 C 0.43385(17) 0.4034(3) 0.58473(8) 0.0125 1.0000 Uani . . . . . .
C2 C 0.58289(18) 0.6264(3) 0.58389(8) 0.0159 1.0000 Uani . . . . . .
C3 C 0.64781(17) 0.7129(3) 0.59516(8) 0.0158 1.0000 Uani . . . . . .
C4 C 0.63720(18) 0.7943(3) 0.62807(8) 0.0154 1.0000 Uani . . . . . .
C5 C 0.56337(18) 0.7866(3) 0.65029(8) 0.0146 1.0000 Uani . . . . . .
C6 C 0.49932(17) 0.6983(3) 0.63907(8) 0.0138 1.0000 Uani . . . . . .
C7 C 0.50828(17) 0.6195(2) 0.60556(8) 0.0119 1.0000 Uani . . . . . .
C8 C 0.26248(18) 0.6224(3) 0.60315(9) 0.0178 1.0000 Uani . . . . . .
C9 C 0.17241(19) 0.6020(3) 0.58301(10) 0.0248 1.0000 Uani . . . . . .
C10 C 0.2674(2) 0.7605(3) 0.62103(10) 0.0236 1.0000 Uani . . . . . .
C11 C 0.27455(19) 0.5218(3) 0.63710(9) 0.0214 1.0000 Uani . . . . . .
C12 C 0.36645(18) 0.7161(3) 0.52922(8) 0.0147 1.0000 Uani . . . . . .
C13 C 0.4166(2) 0.8309(3) 0.54829(9) 0.0217 1.0000 Uani . . . . . .
C14 C 0.2803(2) 0.7639(3) 0.51103(10) 0.0239 1.0000 Uani . . . . . .
C15 C 0.4183(2) 0.6565(3) 0.49579(9) 0.0217 1.0000 Uani . . . . . .
C16 C 0.52413(18) 0.3587(3) 0.64606(8) 0.0163 1.0000 Uani . . . . . .
C17 C 0.4938(2) 0.2847(3) 0.68266(9) 0.0253 1.0000 Uani . . . . . .
C18 C 0.6215(2) 0.3541(3) 0.64237(11) 0.0274 1.0000 Uani . . . . . .
C19 C 0.46249(18) 0.1779(3) 0.59754(8) 0.0154 1.0000 Uani . . . . . .
C20 C 0.3852(2) 0.1214(3) 0.61830(9) 0.0224 1.0000 Uani . . . . . .
C21 C 0.5437(2) 0.0960(3) 0.60284(10) 0.0229 1.0000 Uani . . . . . .
C22 C 0.7585(2) 0.9225(3) 0.61256(11) 0.0319 1.0000 Uani . . . . . .
C23 C 0.01827(17) 0.3519(3) 0.65132(8) 0.0133 1.0000 Uani . . . . . .
C24 C 0.02971(18) 0.0292(3) 0.60505(9) 0.0172 1.0000 Uani . . . . . .
C25 C 0.04804(18) -0.0348(3) 0.56997(9) 0.0176 1.0000 Uani . . . . . .
C26 C 0.10262(18) 0.0217(3) 0.54259(8) 0.0158 1.0000 Uani . . . . . .
C27 C 0.14363(17) 0.1393(3) 0.55203(8) 0.0164 1.0000 Uani . . . . . .
C28 C 0.12603(17) 0.2019(3) 0.58797(8) 0.0152 1.0000 Uani . . . . . .
C29 C 0.06697(17) 0.1491(3) 0.61412(8) 0.0127 1.0000 Uani . . . . . .
C30 C -0.03468(18) 0.0906(3) 0.71538(8) 0.0159 1.0000 Uani . . . . . .
C31 C -0.0244(2) -0.0569(3) 0.71038(9) 0.0198 1.0000 Uani . . . . . .
C32 C -0.04923(19) 0.1214(3) 0.76003(9) 0.0205 1.0000 Uani . . . . . .
C33 C -0.11405(18) 0.1403(3) 0.69063(9) 0.0204 1.0000 Uani . . . . . .
C34 C 0.16659(18) 0.1178(3) 0.71166(9) 0.0171 1.0000 Uani . . . . . .
C35 C 0.23331(19) 0.2241(3) 0.70322(9) 0.0211 1.0000 Uani . . . . . .
C36 C 0.18479(19) -0.0022(3) 0.68630(9) 0.0191 1.0000 Uani . . . . . .
C37 C 0.1738(2) 0.0842(3) 0.75677(9) 0.0229 1.0000 Uani . . . . . .
C38 C -0.07417(18) 0.3313(3) 0.58965(9) 0.0184 1.0000 Uani . . . . . .
C39 C -0.0440(2) 0.3614(3) 0.54733(9) 0.0252 1.0000 Uani . . . . . .
C40 C -0.17212(19) 0.3400(3) 0.59196(9) 0.0227 1.0000 Uani . . . . . .
C41 C -0.05287(18) 0.5486(3) 0.63002(9) 0.0177 1.0000 Uani . . . . . .
C42 C -0.1311(2) 0.5624(3) 0.65633(10) 0.0269 1.0000 Uani . . . . . .
C43 C -0.06284(19) 0.6290(3) 0.5914(1) 0.0212 1.0000 Uani . . . . . .
C44 C 0.1560(2) 0.0211(3) 0.47664(9) 0.0215 1.0000 Uani . . . . . .
C45 C -0.2069(2) 0.4527(3) 0.75467(10) 0.0294 1.0000 Uani . . . . . .
C46 C -0.1502(2) 0.5549(3) 0.77039(10) 0.0289 1.0000 Uani . . . . . .
H21 H 0.5893 0.5733 0.5616 0.0193 1.0000 Uiso . . . . . .
H31 H 0.6971 0.7160 0.5803 0.0189 1.0000 Uiso . . . . . .
H51 H 0.5575 0.8398 0.6728 0.0179 1.0000 Uiso . . . . . .
H61 H 0.4498 0.6933 0.6540 0.0162 1.0000 Uiso . . . . . .
H91 H 0.1678 0.5165 0.5708 0.0369 1.0000 Uiso . . . . . .
H92 H 0.1305 0.6098 0.6037 0.0366 1.0000 Uiso . . . . . .
H93 H 0.1607 0.6688 0.5628 0.0372 1.0000 Uiso . . . . . .
H101 H 0.2531 0.8247 0.6007 0.0343 1.0000 Uiso . . . . . .
H102 H 0.3242 0.7765 0.6321 0.0346 1.0000 Uiso . . . . . .
H103 H 0.2270 0.7662 0.6425 0.0354 1.0000 Uiso . . . . . .
H111 H 0.3292 0.5331 0.6511 0.0316 1.0000 Uiso . . . . . .
H112 H 0.2712 0.4357 0.6258 0.0323 1.0000 Uiso . . . . . .
H113 H 0.2296 0.5331 0.6559 0.0316 1.0000 Uiso . . . . . .
H131 H 0.3912 0.8568 0.5725 0.0330 1.0000 Uiso . . . . . .
H132 H 0.4759 0.8056 0.5540 0.0328 1.0000 Uiso . . . . . .
H133 H 0.4158 0.9012 0.5296 0.0328 1.0000 Uiso . . . . . .
H141 H 0.2503 0.8129 0.5309 0.0361 1.0000 Uiso . . . . . .
H142 H 0.2920 0.8190 0.4885 0.0359 1.0000 Uiso . . . . . .
H143 H 0.2460 0.6915 0.5017 0.0359 1.0000 Uiso . . . . . .
H151 H 0.3847 0.5942 0.4805 0.0332 1.0000 Uiso . . . . . .
H152 H 0.4697 0.6161 0.5069 0.0322 1.0000 Uiso . . . . . .
H153 H 0.4362 0.7247 0.4780 0.0331 1.0000 Uiso . . . . . .
H161 H 0.5093 0.4493 0.6505 0.0192 1.0000 Uiso . . . . . .
H171 H 0.5242 0.3171 0.7060 0.0374 1.0000 Uiso . . . . . .
H172 H 0.4330 0.2983 0.6856 0.0376 1.0000 Uiso . . . . . .
H173 H 0.5040 0.1931 0.6804 0.0372 1.0000 Uiso . . . . . .
H181 H 0.6498 0.4039 0.6637 0.0412 1.0000 Uiso . . . . . .
H182 H 0.6418 0.2656 0.6449 0.0407 1.0000 Uiso . . . . . .
H183 H 0.6392 0.3876 0.6167 0.0407 1.0000 Uiso . . . . . .
H191 H 0.4486 0.1792 0.5689 0.0172 1.0000 Uiso . . . . . .
H201 H 0.3398 0.1842 0.6181 0.0340 1.0000 Uiso . . . . . .
H202 H 0.3651 0.0453 0.6040 0.0341 1.0000 Uiso . . . . . .
H203 H 0.3994 0.0986 0.6457 0.0342 1.0000 Uiso . . . . . .
H211 H 0.5592 0.0829 0.6310 0.0337 1.0000 Uiso . . . . . .
H212 H 0.5917 0.1351 0.5896 0.0337 1.0000 Uiso . . . . . .
H213 H 0.5322 0.0133 0.5905 0.0339 1.0000 Uiso . . . . . .
H221 H 0.7992 0.8532 0.6112 0.0473 1.0000 Uiso . . . . . .
H222 H 0.7325 0.9380 0.5865 0.0476 1.0000 Uiso . . . . . .
H223 H 0.7865 0.9997 0.6223 0.0478 1.0000 Uiso . . . . . .
H241 H -0.0092 -0.0074 0.6231 0.0208 1.0000 Uiso . . . . . .
H251 H 0.0245 -0.1148 0.5641 0.0210 1.0000 Uiso . . . . . .
H271 H 0.1821 0.1758 0.5346 0.0199 1.0000 Uiso . . . . . .
H281 H 0.1534 0.2810 0.5950 0.0182 1.0000 Uiso . . . . . .
H311 H 0.0238 -0.0897 0.7270 0.0303 1.0000 Uiso . . . . . .
H312 H -0.0145 -0.0786 0.6829 0.0302 1.0000 Uiso . . . . . .
H313 H -0.0761 -0.0982 0.7184 0.0300 1.0000 Uiso . . . . . .
H321 H -0.0007 0.0945 0.7766 0.0306 1.0000 Uiso . . . . . .
H322 H -0.0983 0.0756 0.7690 0.0308 1.0000 Uiso . . . . . .
H323 H -0.0580 0.2138 0.7639 0.0306 1.0000 Uiso . . . . . .
H331 H -0.1217 0.2321 0.6940 0.0306 1.0000 Uiso . . . . . .
H332 H -0.1646 0.0955 0.6993 0.0301 1.0000 Uiso . . . . . .
H333 H -0.1067 0.1212 0.6626 0.0312 1.0000 Uiso . . . . . .
H351 H 0.2276 0.2511 0.6757 0.0314 1.0000 Uiso . . . . . .
H352 H 0.2269 0.2980 0.7208 0.0312 1.0000 Uiso . . . . . .
H353 H 0.2901 0.1874 0.7080 0.0319 1.0000 Uiso . . . . . .
H361 H 0.1428 -0.0696 0.6894 0.0293 1.0000 Uiso . . . . . .
H362 H 0.1858 0.0189 0.6582 0.0288 1.0000 Uiso . . . . . .
H363 H 0.2409 -0.0370 0.6937 0.0284 1.0000 Uiso . . . . . .
H371 H 0.1590 0.1572 0.7730 0.0332 1.0000 Uiso . . . . . .
H372 H 0.1375 0.0107 0.7625 0.0336 1.0000 Uiso . . . . . .
H373 H 0.2325 0.0592 0.7631 0.0336 1.0000 Uiso . . . . . .
H381 H -0.0593 0.2412 0.5960 0.0202 1.0000 Uiso . . . . . .
H391 H -0.0563 0.2871 0.5300 0.0380 1.0000 Uiso . . . . . .
H392 H 0.0168 0.3759 0.5484 0.0378 1.0000 Uiso . . . . . .
H393 H -0.0737 0.4363 0.5367 0.0378 1.0000 Uiso . . . . . .
H401 H -0.1890 0.3217 0.6190 0.0336 1.0000 Uiso . . . . . .
H402 H -0.1976 0.2770 0.5745 0.0338 1.0000 Uiso . . . . . .
H403 H -0.1917 0.4245 0.5839 0.0343 1.0000 Uiso . . . . . .
H411 H -0.0032 0.5851 0.6450 0.0206 1.0000 Uiso . . . . . .
H421 H -0.1268 0.5022 0.6785 0.0393 1.0000 Uiso . . . . . .
H422 H -0.1333 0.6497 0.6669 0.0399 1.0000 Uiso . . . . . .
H423 H -0.1842 0.5468 0.6410 0.0395 1.0000 Uiso . . . . . .
H431 H -0.1143 0.6079 0.5763 0.0321 1.0000 Uiso . . . . . .
H432 H -0.0141 0.6146 0.5753 0.0322 1.0000 Uiso . . . . . .
H433 H -0.0646 0.7204 0.5989 0.0320 1.0000 Uiso . . . . . .
H441 H 0.1495 -0.0318 0.4528 0.0319 1.0000 Uiso . . . . . .
H442 H 0.1287 0.1043 0.4715 0.0320 1.0000 Uiso . . . . . .
H443 H 0.2161 0.0332 0.4845 0.0316 1.0000 Uiso . . . . . .
H461 H -0.1502 0.5543 0.7989 0.0429 1.0000 Uiso . . . . . .
H462 H -0.0922 0.5393 0.7620 0.0435 1.0000 Uiso . . . . . .
H463 H -0.1707 0.6376 0.7607 0.0429 1.0000 Uiso . . . . . .

_refine_ls_extinction_coef       13.862
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_oxford_refine_ls_scale          0.1840(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 . Cl1 . 2.3582(7) yes
Pd1 . Cl2 . 2.3901(7) yes
Pd1 . P1 . 2.2013(7) yes
Pd1 . C1 . 2.042(3) yes
Pd2 . Cl3 . 2.3634(7) yes
Pd2 . Cl4 . 2.3819(7) yes
Pd2 . P2 . 2.2085(7) yes
Pd2 . C23 . 2.031(3) yes
P1 . N1 . 1.721(2) yes
P1 . C8 . 1.867(3) yes
P1 . C12 . 1.858(3) yes
P2 . N3 . 1.728(2) yes
P2 . C30 . 1.870(3) yes
P2 . C34 . 1.862(3) yes
O1 . C4 . 1.368(3) yes
O1 . C22 . 1.418(4) yes
O2 . C26 . 1.365(3) yes
O2 . C44 . 1.427(4) yes
N1 . C1 . 1.386(3) yes
N1 . C7 . 1.452(3) yes
N2 . C1 . 1.314(3) yes
N2 . C16 . 1.505(3) yes
N2 . C19 . 1.500(3) yes
N3 . C23 . 1.394(3) yes
N3 . C29 . 1.438(3) yes
N4 . C23 . 1.317(4) yes
N4 . C38 . 1.501(3) yes
N4 . C41 . 1.504(3) yes
N5 . C45 . 1.139(5) yes
C2 . C3 . 1.384(4) yes
C2 . C7 . 1.388(4) yes
C2 . H21 . 0.926 no
C3 . C4 . 1.389(4) yes
C3 . H31 . 0.926 no
C4 . C5 . 1.388(4) yes
C5 . C6 . 1.386(4) yes
C5 . H51 . 0.932 no
C6 . C7 . 1.386(4) yes
C6 . H61 . 0.931 no
C8 . C9 . 1.542(4) yes
C8 . C10 . 1.537(4) yes
C8 . C11 . 1.534(4) yes
C9 . H91 . 0.968 no
C9 . H92 . 0.968 no
C9 . H93 . 0.971 no
C10 . H101 . 0.963 no
C10 . H102 . 0.957 no
C10 . H103 . 0.968 no
C11 . H111 . 0.960 no
C11 . H112 . 0.960 no
C11 . H113 . 0.960 no
C12 . C13 . 1.535(4) yes
C12 . C14 . 1.528(4) yes
C12 . C15 . 1.523(4) yes
C13 . H131 . 0.947 no
C13 . H132 . 0.969 no
C13 . H133 . 0.951 no
C14 . H141 . 0.963 no
C14 . H142 . 0.959 no
C14 . H143 . 0.958 no
C15 . H151 . 0.958 no
C15 . H152 . 0.961 no
C15 . H153 . 0.962 no
C16 . C17 . 1.521(4) yes
C16 . C18 . 1.522(4) yes
C16 . H161 . 0.970 no
C17 . H171 . 0.951 no
C17 . H172 . 0.963 no
C17 . H173 . 0.955 no
C18 . H181 . 0.964 no
C18 . H182 . 0.964 no
C18 . H183 . 0.968 no
C19 . C20 . 1.520(4) yes
C19 . C21 . 1.520(4) yes
C19 . H191 . 0.967 no
C20 . H201 . 0.956 no
C20 . H202 . 0.961 no
C20 . H203 . 0.957 no
C21 . H211 . 0.966 no
C21 . H212 . 0.967 no
C21 . H213 . 0.955 no
C22 . H221 . 0.953 no
C22 . H222 . 0.954 no
C22 . H223 . 0.954 no
C24 . C25 . 1.376(4) yes
C24 . C29 . 1.387(4) yes
C24 . H241 . 0.945 no
C25 . C26 . 1.392(4) yes
C25 . H251 . 0.917 no
C26 . C27 . 1.394(4) yes
C27 . C28 . 1.391(4) yes
C27 . H271 . 0.926 no
C28 . C29 . 1.396(4) yes
C28 . H281 . 0.940 no
C30 . C31 . 1.530(4) yes
C30 . C32 . 1.540(4) yes
C30 . C33 . 1.543(4) yes
C31 . H311 . 0.973 no
C31 . H312 . 0.957 no
C31 . H313 . 0.955 no
C32 . H321 . 0.958 no
C32 . H322 . 0.952 no
C32 . H323 . 0.966 no
C33 . H331 . 0.956 no
C33 . H332 . 0.963 no
C33 . H333 . 0.963 no
C34 . C35 . 1.538(4) yes
C34 . C36 . 1.524(4) yes
C34 . C37 . 1.536(4) yes
C35 . H351 . 0.955 no
C35 . H352 . 0.964 no
C35 . H353 . 0.967 no
C36 . H361 . 0.958 no
C36 . H362 . 0.958 no
C36 . H363 . 0.966 no
C37 . H371 . 0.955 no
C37 . H372 . 0.964 no
C37 . H373 . 0.962 no
C38 . C39 . 1.528(4) yes
C38 . C40 . 1.529(4) yes
C38 . H381 . 0.973 no
C39 . H391 . 0.968 no
C39 . H392 . 0.955 no
C39 . H393 . 0.957 no
C40 . H401 . 0.962 no
C40 . H402 . 0.946 no
C40 . H403 . 0.953 no
C41 . C42 . 1.528(4) yes
C41 . C43 . 1.526(4) yes
C41 . H411 . 0.977 no
C42 . H421 . 0.962 no
C42 . H422 . 0.962 no
C42 . H423 . 0.967 no
C43 . H431 . 0.953 no
C43 . H432 . 0.955 no
C43 . H433 . 0.971 no
C44 . H441 . 0.962 no
C44 . H442 . 0.965 no
C44 . H443 . 0.969 no
C45 . C46 . 1.453(5) yes
C46 . H461 . 0.948 no
C46 . H462 . 0.967 no
C46 . H463 . 0.958 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Pd1 . Cl2 . 87.34(2) yes
Cl1 . Pd1 . P1 . 97.36(3) yes
Cl2 . Pd1 . P1 . 169.82(3) yes
Cl1 . Pd1 . C1 . 165.45(7) yes
Cl2 . Pd1 . C1 . 107.16(7) yes
P1 . Pd1 . C1 . 68.14(7) yes
Cl3 . Pd2 . Cl4 . 88.51(3) yes
Cl3 . Pd2 . P2 . 98.23(3) yes
Cl4 . Pd2 . P2 . 165.48(3) yes
Cl3 . Pd2 . C23 . 165.49(8) yes
Cl4 . Pd2 . C23 . 105.89(8) yes
P2 . Pd2 . C23 . 68.14(8) yes
Pd1 . P1 . N1 . 86.64(8) yes
Pd1 . P1 . C8 . 117.14(9) yes
N1 . P1 . C8 . 108.41(12) yes
Pd1 . P1 . C12 . 115.97(9) yes
N1 . P1 . C12 . 109.74(12) yes
C8 . P1 . C12 . 114.78(12) yes
Pd2 . P2 . N3 . 86.25(8) yes
Pd2 . P2 . C30 . 118.48(9) yes
N3 . P2 . C30 . 107.77(12) yes
Pd2 . P2 . C34 . 115.03(10) yes
N3 . P2 . C34 . 110.05(12) yes
C30 . P2 . C34 . 114.87(13) yes
C4 . O1 . C22 . 116.5(2) yes
C26 . O2 . C44 . 116.1(2) yes
P1 . N1 . C1 . 99.46(17) yes
P1 . N1 . C7 . 128.55(18) yes
C1 . N1 . C7 . 130.9(2) yes
C1 . N2 . C16 . 122.4(2) yes
C1 . N2 . C19 . 116.1(2) yes
C16 . N2 . C19 . 120.9(2) yes
P2 . N3 . C23 . 98.77(17) yes
P2 . N3 . C29 . 132.55(18) yes
C23 . N3 . C29 . 128.3(2) yes
C23 . N4 . C38 . 122.0(2) yes
C23 . N4 . C41 . 116.0(2) yes
C38 . N4 . C41 . 121.0(2) yes
N1 . C1 . N2 . 123.4(2) yes
N1 . C1 . Pd1 . 103.01(18) yes
N2 . C1 . Pd1 . 133.15(19) yes
C3 . C2 . C7 . 120.4(2) yes
C3 . C2 . H21 . 119.6 no
C7 . C2 . H21 . 120.0 no
C2 . C3 . C4 . 119.4(2) yes
C2 . C3 . H31 . 119.1 no
C4 . C3 . H31 . 121.5 no
C3 . C4 . O1 . 124.1(3) yes
C3 . C4 . C5 . 120.5(2) yes
O1 . C4 . C5 . 115.4(2) yes
C4 . C5 . C6 . 119.5(2) yes
C4 . C5 . H51 . 119.9 no
C6 . C5 . H51 . 120.5 no
C5 . C6 . C7 . 120.3(2) yes
C5 . C6 . H61 . 119.5 no
C7 . C6 . H61 . 120.2 no
N1 . C7 . C2 . 118.7(2) yes
N1 . C7 . C6 . 121.4(2) yes
C2 . C7 . C6 . 119.8(2) yes
P1 . C8 . C9 . 107.8(2) yes
P1 . C8 . C10 . 116.0(2) yes
C9 . C8 . C10 . 108.9(2) yes
P1 . C8 . C11 . 106.31(19) yes
C9 . C8 . C11 . 108.2(2) yes
C10 . C8 . C11 . 109.5(2) yes
C8 . C9 . H91 . 110.9 no
C8 . C9 . H92 . 107.7 no
H91 . C9 . H92 . 109.4 no
C8 . C9 . H93 . 110.4 no
H91 . C9 . H93 . 109.8 no
H92 . C9 . H93 . 108.6 no
C8 . C10 . H101 . 110.6 no
C8 . C10 . H102 . 109.7 no
H101 . C10 . H102 . 109.7 no
C8 . C10 . H103 . 108.4 no
H101 . C10 . H103 . 109.6 no
H102 . C10 . H103 . 108.8 no
C8 . C11 . H111 . 110.9 no
C8 . C11 . H112 . 109.2 no
H111 . C11 . H112 . 109.5 no
C8 . C11 . H113 . 108.9 no
H111 . C11 . H113 . 108.9 no
H112 . C11 . H113 . 109.5 no
P1 . C12 . C13 . 113.86(19) yes
P1 . C12 . C14 . 108.02(19) yes
C13 . C12 . C14 . 109.9(2) yes
P1 . C12 . C15 . 106.74(18) yes
C13 . C12 . C15 . 109.6(2) yes
C14 . C12 . C15 . 108.6(2) yes
C12 . C13 . H131 . 110.2 no
C12 . C13 . H132 . 109.8 no
H131 . C13 . H132 . 109.4 no
C12 . C13 . H133 . 108.6 no
H131 . C13 . H133 . 110.2 no
H132 . C13 . H133 . 108.7 no
C12 . C14 . H141 . 109.6 no
C12 . C14 . H142 . 107.9 no
H141 . C14 . H142 . 109.6 no
C12 . C14 . H143 . 110.3 no
H141 . C14 . H143 . 110.4 no
H142 . C14 . H143 . 108.9 no
C12 . C15 . H151 . 111.2 no
C12 . C15 . H152 . 110.4 no
H151 . C15 . H152 . 110.1 no
C12 . C15 . H153 . 109.1 no
H151 . C15 . H153 . 108.9 no
H152 . C15 . H153 . 107.0 no
N2 . C16 . C17 . 112.3(2) yes
N2 . C16 . C18 . 112.9(2) yes
C17 . C16 . C18 . 112.7(2) yes
N2 . C16 . H161 . 105.8 no
C17 . C16 . H161 . 106.0 no
C18 . C16 . H161 . 106.5 no
C16 . C17 . H171 . 108.5 no
C16 . C17 . H172 . 109.9 no
H171 . C17 . H172 . 109.1 no
C16 . C17 . H173 . 111.8 no
H171 . C17 . H173 . 109.2 no
H172 . C17 . H173 . 108.3 no
C16 . C18 . H181 . 110.6 no
C16 . C18 . H182 . 110.2 no
H181 . C18 . H182 . 107.1 no
C16 . C18 . H183 . 112.0 no
H181 . C18 . H183 . 108.7 no
H182 . C18 . H183 . 108.0 no
N2 . C19 . C20 . 111.7(2) yes
N2 . C19 . C21 . 113.5(2) yes
C20 . C19 . C21 . 113.7(2) yes
N2 . C19 . H191 . 103.6 no
C20 . C19 . H191 . 107.4 no
C21 . C19 . H191 . 106.0 no
C19 . C20 . H201 . 109.5 no
C19 . C20 . H202 . 109.5 no
H201 . C20 . H202 . 108.5 no
C19 . C20 . H203 . 111.5 no
H201 . C20 . H203 . 108.4 no
H202 . C20 . H203 . 109.4 no
C19 . C21 . H211 . 111.4 no
C19 . C21 . H212 . 111.6 no
H211 . C21 . H212 . 109.1 no
C19 . C21 . H213 . 107.4 no
H211 . C21 . H213 . 109.1 no
H212 . C21 . H213 . 108.0 no
O1 . C22 . H221 . 108.8 no
O1 . C22 . H222 . 110.5 no
H221 . C22 . H222 . 109.9 no
O1 . C22 . H223 . 107.8 no
H221 . C22 . H223 . 109.8 no
H222 . C22 . H223 . 109.9 no
N3 . C23 . N4 . 123.4(2) yes
N3 . C23 . Pd2 . 103.26(18) yes
N4 . C23 . Pd2 . 132.5(2) yes
C25 . C24 . C29 . 120.6(3) yes
C25 . C24 . H241 . 120.3 no
C29 . C24 . H241 . 119.1 no
C24 . C25 . C26 . 120.3(3) yes
C24 . C25 . H251 . 121.0 no
C26 . C25 . H251 . 118.7 no
C25 . C26 . O2 . 115.6(2) yes
C25 . C26 . C27 . 119.8(3) yes
O2 . C26 . C27 . 124.6(3) yes
C26 . C27 . C28 . 119.3(2) yes
C26 . C27 . H271 . 120.7 no
C28 . C27 . H271 . 120.0 no
C27 . C28 . C29 . 120.6(2) yes
C27 . C28 . H281 . 120.5 no
C29 . C28 . H281 . 118.9 no
N3 . C29 . C28 . 118.1(2) yes
N3 . C29 . C24 . 122.7(2) yes
C28 . C29 . C24 . 119.2(2) yes
P2 . C30 . C31 . 115.7(2) yes
P2 . C30 . C32 . 106.67(18) yes
C31 . C30 . C32 . 109.1(2) yes
P2 . C30 . C33 . 106.72(18) yes
C31 . C30 . C33 . 110.7(2) yes
C32 . C30 . C33 . 107.6(2) yes
C30 . C31 . H311 . 111.2 no
C30 . C31 . H312 . 110.8 no
H311 . C31 . H312 . 108.3 no
C30 . C31 . H313 . 108.4 no
H311 . C31 . H313 . 109.0 no
H312 . C31 . H313 . 109.2 no
C30 . C32 . H321 . 110.7 no
C30 . C32 . H322 . 110.2 no
H321 . C32 . H322 . 107.5 no
C30 . C32 . H323 . 110.8 no
H321 . C32 . H323 . 108.6 no
H322 . C32 . H323 . 109.0 no
C30 . C33 . H331 . 111.3 no
C30 . C33 . H332 . 109.1 no
H331 . C33 . H332 . 109.2 no
C30 . C33 . H333 . 109.1 no
H331 . C33 . H333 . 109.5 no
H332 . C33 . H333 . 108.7 no
P2 . C34 . C35 . 106.27(19) yes
P2 . C34 . C36 . 113.6(2) yes
C35 . C34 . C36 . 109.4(2) yes
P2 . C34 . C37 . 108.79(19) yes
C35 . C34 . C37 . 108.1(2) yes
C36 . C34 . C37 . 110.4(2) yes
C34 . C35 . H351 . 109.9 no
C34 . C35 . H352 . 111.2 no
H351 . C35 . H352 . 110.1 no
C34 . C35 . H353 . 108.1 no
H351 . C35 . H353 . 108.8 no
H352 . C35 . H353 . 108.6 no
C34 . C36 . H361 . 112.4 no
C34 . C36 . H362 . 111.4 no
H361 . C36 . H362 . 107.8 no
C34 . C36 . H363 . 110.0 no
H361 . C36 . H363 . 108.5 no
H362 . C36 . H363 . 106.5 no
C34 . C37 . H371 . 111.2 no
C34 . C37 . H372 . 110.1 no
H371 . C37 . H372 . 110.3 no
C34 . C37 . H373 . 107.9 no
H371 . C37 . H373 . 109.4 no
H372 . C37 . H373 . 107.8 no
N4 . C38 . C39 . 115.0(2) yes
N4 . C38 . C40 . 111.2(2) yes
C39 . C38 . C40 . 111.9(2) yes
N4 . C38 . H381 . 104.0 no
C39 . C38 . H381 . 108.2 no
C40 . C38 . H381 . 105.9 no
C38 . C39 . H391 . 109.0 no
C38 . C39 . H392 . 109.5 no
H391 . C39 . H392 . 108.5 no
C38 . C39 . H393 . 110.0 no
H391 . C39 . H393 . 109.3 no
H392 . C39 . H393 . 110.5 no
C38 . C40 . H401 . 109.9 no
C38 . C40 . H402 . 108.9 no
H401 . C40 . H402 . 108.4 no
C38 . C40 . H403 . 110.3 no
H401 . C40 . H403 . 110.1 no
H402 . C40 . H403 . 109.1 no
N4 . C41 . C42 . 112.1(2) yes
N4 . C41 . C43 . 113.7(2) yes
C42 . C41 . C43 . 111.8(2) yes
N4 . C41 . H411 . 105.1 no
C42 . C41 . H411 . 107.6 no
C43 . C41 . H411 . 105.9 no
C41 . C42 . H421 . 110.1 no
C41 . C42 . H422 . 109.5 no
H421 . C42 . H422 . 108.8 no
C41 . C42 . H423 . 111.3 no
H421 . C42 . H423 . 109.3 no
H422 . C42 . H423 . 107.7 no
C41 . C43 . H431 . 112.1 no
C41 . C43 . H432 . 109.2 no
H431 . C43 . H432 . 109.6 no
C41 . C43 . H433 . 108.1 no
H431 . C43 . H433 . 108.9 no
H432 . C43 . H433 . 108.8 no
O2 . C44 . H441 . 106.4 no
O2 . C44 . H442 . 108.8 no
H441 . C44 . H442 . 108.8 no
O2 . C44 . H443 . 111.1 no
H441 . C44 . H443 . 111.4 no
H442 . C44 . H443 . 110.3 no
N5 . C45 . C46 . 178.9(4) yes
C45 . C46 . H461 . 109.4 no
C45 . C46 . H462 . 109.6 no
H461 . C46 . H462 . 108.8 no
C45 . C46 . H463 . 109.2 no
H461 . C46 . H463 . 109.3 no
H462 . C46 . H463 . 110.5 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C16 . H161 . C6 . 159.67(18) 0.970 2.586 3.511(4) yes
C16 . H161 . C7 . 128.81(18) 0.970 2.295 3.000(4) yes
C38 . H381 . C24 . 160.74(18) 0.973 2.588 3.521(4) yes
C38 . H381 . C29 . 131.10(18) 0.973 2.239 2.971(4) yes
