# 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_f:\mrc090a\mrc090a
_audit_block_doi                 10.5517/cc13mq2j
_database_code_depnum_ccdc_archive 'CCDC 1031837'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C4CC10163D 2015
_audit_update_record             
;
2014-10-30 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        2
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H29 N7 O2 Pd, 2(F6 P)'
_chemical_formula_sum            'C26 H29 F12 N7 O2 P2 Pd'
_chemical_formula_weight         867.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   17.4973(8)
_cell_length_b                   9.5790(5)
_cell_length_c                   20.1652(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.859(4)
_cell_angle_gamma                90.00
_cell_volume                     3339.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(5)
_cell_measurement_reflns_used    5033
_cell_measurement_theta_min      3.7290
_cell_measurement_theta_max      30.2060

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1736
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7993
_exptl_absorpt_correction_T_max  0.9214
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;
_diffrn_ambient_temperature      100.0(5)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            15136
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.29
_diffrn_reflns_theta_max         28.28
_reflns_number_total             8234
_reflns_number_gt                6352
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_structure_solution    
;
SHELXS-97 (Sheldrick, G. M.    Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_structure_refinement  
;
SHELXS-97 (Sheldrick, G. M.    Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_molecular_graphics    'ORTEP-III Version 1.08 (Farrugia, 2005)'
_computing_publication_material  
;
enCIFer: A program for viewing, editing and visualising CIFs.
F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler,
J. Applied Cryst., 37, 331-334, 2004
;
_refine_special_details          
;
All H atoms were placed in calculated positions and refined using a riding model. C-H distances: CH3 0.98Α, CH2 0.99Α, aromatic 0.95Α.

All Uiso(H) values were constrained to be 1.2 times (1.5 times for methyl) Ueq of the parent atom.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0508P)²+5.7683P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8234
_refine_ls_number_parameters     454
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1374
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.196990(16) 0.63412(3) 0.373355(15) 0.02304(10) Uani 1 1 d . . .
P2 P 0.01217(7) 0.05702(12) 0.34642(5) 0.0292(2) Uani 1 1 d . . .
P1 P 0.35912(6) 0.17579(13) 0.68067(5) 0.0301(3) Uani 1 1 d . . .
F7 F 0.0950(2) 0.1203(6) 0.34812(17) 0.0978(17) Uani 1 1 d . . .
F12 F 0.03008(16) 0.0312(3) 0.42589(12) 0.0401(6) Uani 1 1 d . . .
F8 F -0.0192(2) 0.2081(3) 0.36253(15) 0.0636(10) Uani 1 1 d . . .
F1 F 0.39003(16) 0.1142(3) 0.61576(13) 0.0431(7) Uani 1 1 d . . .
O2 O 0.5091(2) 0.2137(4) 0.42858(17) 0.0451(8) Uani 1 1 d . . .
F4 F 0.32842(15) 0.2372(3) 0.74514(13) 0.0475(7) Uani 1 1 d . . .
F3 F 0.43851(15) 0.1290(3) 0.72609(13) 0.0414(7) Uani 1 1 d . . .
F10 F -0.07329(19) 0.0003(4) 0.34643(16) 0.0669(10) Uani 1 1 d . . .
C14 C 0.2293(3) 0.8232(5) 0.1861(2) 0.0379(11) Uani 1 1 d . . .
H14 H 0.2112 0.7310 0.1758 0.046 Uiso 1 1 calc R . .
C24 C 0.5404(4) 0.2130(7) 0.3664(3) 0.072(2) Uani 1 1 d . . .
H24A H 0.4981 0.2055 0.3286 0.109 Uiso 1 1 calc R . .
H24B H 0.5754 0.1332 0.3659 0.109 Uiso 1 1 calc R . .
H24C H 0.5690 0.2998 0.3625 0.109 Uiso 1 1 calc R . .
F11 F 0.0393(3) -0.0961(4) 0.33327(17) 0.0854(13) Uani 1 1 d . . .
F2 F 0.39640(15) 0.3244(3) 0.66746(15) 0.0433(7) Uani 1 1 d . . .
F5 F 0.28079(14) 0.2223(3) 0.63353(13) 0.0430(7) Uani 1 1 d . . .
O1 O -0.12718(15) 0.6094(3) 0.45884(14) 0.0278(6) Uani 1 1 d . . .
C13 C 0.2434(3) 0.9039(5) 0.1365(2) 0.0402(11) Uani 1 1 d . . .
H13A H 0.2615 0.9965 0.1455 0.048 Uiso 1 1 calc R . .
H13B H 0.2356 0.8694 0.0918 0.048 Uiso 1 1 calc R . .
C10 C -0.0393(2) 0.5183(4) 0.39515(19) 0.0228(8) Uani 1 1 d . . .
H10 H -0.0777 0.4539 0.3758 0.027 Uiso 1 1 calc R . .
F6 F 0.32128(17) 0.0288(3) 0.69227(15) 0.0518(8) Uani 1 1 d . . .
F9 F -0.00712(19) 0.0831(4) 0.26835(13) 0.0552(8) Uani 1 1 d . . .
N7 N 0.18220(18) 0.4716(4) 0.30579(17) 0.0270(7) Uani 1 1 d . . .
C12 C -0.1483(2) 0.7120(5) 0.5052(2) 0.0318(9) Uani 1 1 d . . .
H12A H -0.1144 0.7026 0.5484 0.048 Uiso 1 1 calc R . .
H12B H -0.2021 0.6973 0.5115 0.048 Uiso 1 1 calc R . .
H12C H -0.1427 0.8058 0.4871 0.048 Uiso 1 1 calc R . .
N1 N 0.25260(19) 0.8631(3) 0.48081(17) 0.0268(7) Uani 1 1 d . . .
C26 C 0.1474(2) 0.2603(4) 0.2269(2) 0.0281(9) Uani 1 1 d . . .
H26A H 0.1708 0.1754 0.2482 0.042 Uiso 1 1 calc R . .
H26B H 0.1664 0.2756 0.1843 0.042 Uiso 1 1 calc R . .
H26C H 0.0910 0.2501 0.2186 0.042 Uiso 1 1 calc R . .
C11 C 0.0330(2) 0.5174(4) 0.37656(18) 0.0224(8) Uani 1 1 d . . .
H11 H 0.0436 0.4522 0.3437 0.027 Uiso 1 1 calc R . .
N6 N 0.3575(2) 0.5292(4) 0.46293(18) 0.0332(8) Uani 1 1 d . . .
C23 C 0.3790(3) 0.4264(5) 0.5068(2) 0.0358(10) Uani 1 1 d . . .
H23 H 0.3571 0.4248 0.5471 0.043 Uiso 1 1 calc R . .
C22 C 0.4310(3) 0.3224(5) 0.4972(2) 0.0337(10) Uani 1 1 d . . .
H22 H 0.4458 0.2541 0.5309 0.040 Uiso 1 1 calc R . .
C15 C 0.2401(3) 0.8691(5) 0.2576(2) 0.0354(10) Uani 1 1 d . . .
H15A H 0.2526 0.9699 0.2604 0.043 Uiso 1 1 calc R . .
H15B H 0.1915 0.8545 0.2762 0.043 Uiso 1 1 calc R . .
N3 N 0.08960(18) 0.6058(3) 0.40332(15) 0.0208(7) Uani 1 1 d . . .
C21 C 0.4611(2) 0.3198(5) 0.4372(2) 0.0335(10) Uani 1 1 d . . .
C6 C 0.1455(2) 0.8778(4) 0.5263(2) 0.0254(8) Uani 1 1 d . . .
H6 H 0.1080 0.9026 0.5536 0.030 Uiso 1 1 calc R . .
C3 C 0.3323(2) 0.8940(5) 0.4710(2) 0.0371(11) Uani 1 1 d . . .
H3A H 0.3546 0.8100 0.4527 0.045 Uiso 1 1 calc R . .
H3B H 0.3635 0.9147 0.5152 0.045 Uiso 1 1 calc R . .
C20 C 0.4382(2) 0.4237(5) 0.3901(2) 0.0299(9) Uani 1 1 d . . .
H20 H 0.4564 0.4255 0.3481 0.036 Uiso 1 1 calc R . .
N2 N 0.13639(17) 0.7836(3) 0.47331(16) 0.0220(7) Uani 1 1 d . . .
N5 N 0.36695(18) 0.6353(3) 0.35970(16) 0.0233(7) Uani 1 1 d . . .
C25 C 0.1681(2) 0.3790(4) 0.2710(2) 0.0255(8) Uani 1 1 d . . .
C5 C 0.2177(2) 0.9264(4) 0.5310(2) 0.0289(9) Uani 1 1 d . . .
H5 H 0.2412 0.9924 0.5629 0.035 Uiso 1 1 calc R . .
N4 N 0.30335(19) 0.7888(4) 0.29724(17) 0.0295(8) Uani 1 1 d . . .
C19 C 0.3879(2) 0.5242(4) 0.4070(2) 0.0255(8) Uani 1 1 d . . .
C9 C -0.0556(2) 0.6156(4) 0.44306(18) 0.0214(8) Uani 1 1 d . . .
C18 C 0.4197(2) 0.7034(5) 0.3264(2) 0.0313(9) Uani 1 1 d . . .
H18 H 0.4736 0.6856 0.3304 0.038 Uiso 1 1 calc R . .
C2 C 0.3386(3) 1.0150(6) 0.4245(3) 0.0452(12) Uani 1 1 d . . .
H2 H 0.3889 1.0366 0.4155 0.054 Uiso 1 1 calc R . .
C8 C 0.0021(2) 0.7083(4) 0.47091(19) 0.0218(8) Uani 1 1 d . . .
H8 H -0.0070 0.7757 0.5034 0.026 Uiso 1 1 calc R . .
C17 C 0.3790(2) 0.7996(5) 0.2871(2) 0.0310(9) Uani 1 1 d . . .
H17 H 0.3989 0.8631 0.2578 0.037 Uiso 1 1 calc R . .
C1 C 0.2825(3) 1.0933(6) 0.3954(3) 0.0494(13) Uani 1 1 d . . .
H1A H 0.2309 1.0765 0.4027 0.059 Uiso 1 1 calc R . .
H1B H 0.2931 1.1674 0.3668 0.059 Uiso 1 1 calc R . .
C16 C 0.2954(2) 0.6894(4) 0.3426(2) 0.0258(8) Uani 1 1 d . . .
C7 C 0.0730(2) 0.6974(4) 0.44904(18) 0.0201(7) Uani 1 1 d . . .
C4 C 0.2023(2) 0.7751(4) 0.4446(2) 0.0246(8) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C4 1.964(4) . ?
Pd1 C16 1.989(4) . ?
Pd1 N7 2.059(4) . ?
Pd1 N3 2.078(3) . ?
P2 F7 1.566(3) . ?
P2 F11 1.577(3) . ?
P2 F9 1.578(3) . ?
P2 F10 1.591(3) . ?
P2 F8 1.599(3) . ?
P2 F12 1.604(3) . ?
P1 F6 1.589(3) . ?
P1 F4 1.593(3) . ?
P1 F1 1.604(3) . ?
P1 F2 1.605(3) . ?
P1 F3 1.606(3) . ?
P1 F5 1.606(3) . ?
O2 C21 1.347(5) . ?
O2 C24 1.444(6) . ?
C14 C13 1.317(7) . ?
C14 C15 1.491(7) . ?
C14 H14 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
O1 C9 1.341(4) . ?
O1 C12 1.443(5) . ?
C13 H13A 0.9500 . ?
C13 H13B 0.9500 . ?
C10 C11 1.374(5) . ?
C10 C9 1.403(5) . ?
C10 H10 0.9500 . ?
N7 C25 1.134(5) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
N1 C4 1.349(5) . ?
N1 C5 1.398(5) . ?
N1 C3 1.469(5) . ?
C26 C25 1.454(6) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C11 N3 1.351(5) . ?
C11 H11 0.9500 . ?
N6 C19 1.319(5) . ?
N6 C23 1.339(6) . ?
C23 C22 1.383(7) . ?
C23 H23 0.9500 . ?
C22 C21 1.392(6) . ?
C22 H22 0.9500 . ?
C15 N4 1.478(5) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
N3 C7 1.336(5) . ?
C21 C20 1.392(6) . ?
C6 C5 1.336(6) . ?
C6 N2 1.388(5) . ?
C6 H6 0.9500 . ?
C3 C2 1.505(7) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C20 C19 1.383(6) . ?
C20 H20 0.9500 . ?
N2 C4 1.370(5) . ?
N2 C7 1.409(5) . ?
N5 C16 1.350(5) . ?
N5 C18 1.385(5) . ?
N5 C19 1.439(5) . ?
C5 H5 0.9500 . ?
N4 C16 1.342(5) . ?
N4 C17 1.375(5) . ?
C9 C8 1.395(5) . ?
C18 C17 1.345(6) . ?
C18 H18 0.9500 . ?
C2 C1 1.301(8) . ?
C2 H2 0.9500 . ?
C8 C7 1.384(5) . ?
C8 H8 0.9500 . ?
C17 H17 0.9500 . ?
C1 H1A 0.9500 . ?
C1 H1B 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 Pd1 C16 95.71(16) . . ?
C4 Pd1 N7 172.42(15) . . ?
C16 Pd1 N7 91.24(15) . . ?
C4 Pd1 N3 79.63(14) . . ?
C16 Pd1 N3 171.86(15) . . ?
N7 Pd1 N3 93.81(12) . . ?
F7 P2 F11 93.6(3) . . ?
F7 P2 F9 90.88(18) . . ?
F11 P2 F9 90.19(19) . . ?
F7 P2 F10 176.9(2) . . ?
F11 P2 F10 89.4(2) . . ?
F9 P2 F10 89.87(17) . . ?
F7 P2 F8 89.5(2) . . ?
F11 P2 F8 176.4(2) . . ?
F9 P2 F8 91.82(18) . . ?
F10 P2 F8 87.6(2) . . ?
F7 P2 F12 90.00(18) . . ?
F11 P2 F12 90.41(17) . . ?
F9 P2 F12 178.90(18) . . ?
F10 P2 F12 89.21(16) . . ?
F8 P2 F12 87.53(15) . . ?
F6 P1 F4 90.37(17) . . ?
F6 P1 F1 89.68(17) . . ?
F4 P1 F1 180.0(2) . . ?
F6 P1 F2 178.86(17) . . ?
F4 P1 F2 90.28(17) . . ?
F1 P1 F2 89.68(16) . . ?
F6 P1 F3 90.68(16) . . ?
F4 P1 F3 90.48(15) . . ?
F1 P1 F3 89.54(15) . . ?
F2 P1 F3 90.25(15) . . ?
F6 P1 F5 89.78(16) . . ?
F4 P1 F5 90.94(15) . . ?
F1 P1 F5 89.05(15) . . ?
F2 P1 F5 89.27(16) . . ?
F3 P1 F5 178.51(15) . . ?
C21 O2 C24 116.3(4) . . ?
C13 C14 C15 123.4(5) . . ?
C13 C14 H14 118.3 . . ?
C15 C14 H14 118.3 . . ?
O2 C24 H24A 109.5 . . ?
O2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
O2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C9 O1 C12 117.7(3) . . ?
C14 C13 H13A 120.0 . . ?
C14 C13 H13B 120.0 . . ?
H13A C13 H13B 120.0 . . ?
C11 C10 C9 119.0(4) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C25 N7 Pd1 173.7(3) . . ?
O1 C12 H12A 109.5 . . ?
O1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
O1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C4 N1 C5 109.9(3) . . ?
C4 N1 C3 127.4(3) . . ?
C5 N1 C3 122.6(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N3 C11 C10 122.4(4) . . ?
N3 C11 H11 118.8 . . ?
C10 C11 H11 118.8 . . ?
C19 N6 C23 115.4(4) . . ?
N6 C23 C22 124.1(4) . . ?
N6 C23 H23 117.9 . . ?
C22 C23 H23 117.9 . . ?
C23 C22 C21 118.7(4) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
N4 C15 C14 110.0(4) . . ?
N4 C15 H15A 109.7 . . ?
C14 C15 H15A 109.7 . . ?
N4 C15 H15B 109.7 . . ?
C14 C15 H15B 109.7 . . ?
H15A C15 H15B 108.2 . . ?
C7 N3 C11 117.6(3) . . ?
C7 N3 Pd1 114.6(2) . . ?
C11 N3 Pd1 127.3(3) . . ?
O2 C21 C22 116.9(4) . . ?
O2 C21 C20 124.8(4) . . ?
C22 C21 C20 118.2(4) . . ?
C5 C6 N2 106.0(3) . . ?
C5 C6 H6 127.0 . . ?
N2 C6 H6 127.0 . . ?
N1 C3 C2 113.6(4) . . ?
N1 C3 H3A 108.8 . . ?
C2 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
C19 C20 C21 117.1(4) . . ?
C19 C20 H20 121.4 . . ?
C21 C20 H20 121.4 . . ?
C4 N2 C6 111.1(3) . . ?
C4 N2 C7 119.2(3) . . ?
C6 N2 C7 129.7(3) . . ?
C16 N5 C18 110.9(3) . . ?
C16 N5 C19 125.8(3) . . ?
C18 N5 C19 123.3(3) . . ?
N7 C25 C26 178.0(4) . . ?
C6 C5 N1 108.1(3) . . ?
C6 C5 H5 125.9 . . ?
N1 C5 H5 125.9 . . ?
C16 N4 C17 111.0(3) . . ?
C16 N4 C15 126.2(4) . . ?
C17 N4 C15 122.6(4) . . ?
N6 C19 C20 126.3(4) . . ?
N6 C19 N5 116.5(3) . . ?
C20 C19 N5 117.2(4) . . ?
O1 C9 C8 125.2(3) . . ?
O1 C9 C10 115.5(3) . . ?
C8 C9 C10 119.3(3) . . ?
C17 C18 N5 106.1(4) . . ?
C17 C18 H18 127.0 . . ?
N5 C18 H18 127.0 . . ?
C1 C2 C3 127.1(5) . . ?
C1 C2 H2 116.4 . . ?
C3 C2 H2 116.4 . . ?
C7 C8 C9 116.9(3) . . ?
C7 C8 H8 121.6 . . ?
C9 C8 H8 121.6 . . ?
C18 C17 N4 107.2(4) . . ?
C18 C17 H17 126.4 . . ?
N4 C17 H17 126.4 . . ?
C2 C1 H1A 120.0 . . ?
C2 C1 H1B 120.0 . . ?
H1A C1 H1B 120.0 . . ?
N4 C16 N5 104.9(3) . . ?
N4 C16 Pd1 126.0(3) . . ?
N5 C16 Pd1 129.1(3) . . ?
N3 C7 C8 124.8(3) . . ?
N3 C7 N2 112.4(3) . . ?
C8 C7 N2 122.8(3) . . ?
N1 C4 N2 104.8(3) . . ?
N1 C4 Pd1 141.2(3) . . ?
N2 C4 Pd1 113.7(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C4 Pd1 N7 C25 21(4) . . . . ?
C16 Pd1 N7 C25 177(3) . . . . ?
N3 Pd1 N7 C25 -9(3) . . . . ?
C9 C10 C11 N3 0.8(6) . . . . ?
C19 N6 C23 C22 1.8(7) . . . . ?
N6 C23 C22 C21 -2.6(7) . . . . ?
C13 C14 C15 N4 -113.6(5) . . . . ?
C10 C11 N3 C7 -0.6(5) . . . . ?
C10 C11 N3 Pd1 -172.3(3) . . . . ?
C4 Pd1 N3 C7 5.3(3) . . . . ?
C16 Pd1 N3 C7 -50.3(11) . . . . ?
N7 Pd1 N3 C7 -178.6(3) . . . . ?
C4 Pd1 N3 C11 177.2(3) . . . . ?
C16 Pd1 N3 C11 121.6(10) . . . . ?
N7 Pd1 N3 C11 -6.6(3) . . . . ?
C24 O2 C21 C22 -179.5(5) . . . . ?
C24 O2 C21 C20 2.3(7) . . . . ?
C23 C22 C21 O2 -177.4(4) . . . . ?
C23 C22 C21 C20 1.0(7) . . . . ?
C4 N1 C3 C2 90.4(5) . . . . ?
C5 N1 C3 C2 -88.7(5) . . . . ?
O2 C21 C20 C19 179.4(4) . . . . ?
C22 C21 C20 C19 1.2(6) . . . . ?
C5 C6 N2 C4 -0.8(5) . . . . ?
C5 C6 N2 C7 176.3(4) . . . . ?
Pd1 N7 C25 C26 19(16) . . . . ?
N2 C6 C5 N1 0.5(5) . . . . ?
C4 N1 C5 C6 0.1(5) . . . . ?
C3 N1 C5 C6 179.3(4) . . . . ?
C14 C15 N4 C16 -108.2(5) . . . . ?
C14 C15 N4 C17 65.8(5) . . . . ?
C23 N6 C19 C20 0.6(6) . . . . ?
C23 N6 C19 N5 -178.7(4) . . . . ?
C21 C20 C19 N6 -2.1(7) . . . . ?
C21 C20 C19 N5 177.2(4) . . . . ?
C16 N5 C19 N6 -42.5(6) . . . . ?
C18 N5 C19 N6 136.1(4) . . . . ?
C16 N5 C19 C20 138.2(4) . . . . ?
C18 N5 C19 C20 -43.2(6) . . . . ?
C12 O1 C9 C8 4.1(6) . . . . ?
C12 O1 C9 C10 -176.8(3) . . . . ?
C11 C10 C9 O1 -179.6(3) . . . . ?
C11 C10 C9 C8 -0.4(6) . . . . ?
C16 N5 C18 C17 -1.1(5) . . . . ?
C19 N5 C18 C17 -179.8(4) . . . . ?
N1 C3 C2 C1 2.2(7) . . . . ?
O1 C9 C8 C7 178.9(3) . . . . ?
C10 C9 C8 C7 -0.2(5) . . . . ?
N5 C18 C17 N4 0.2(5) . . . . ?
C16 N4 C17 C18 0.8(5) . . . . ?
C15 N4 C17 C18 -173.9(4) . . . . ?
C17 N4 C16 N5 -1.4(5) . . . . ?
C15 N4 C16 N5 173.1(4) . . . . ?
C17 N4 C16 Pd1 -179.5(3) . . . . ?
C15 N4 C16 Pd1 -5.0(6) . . . . ?
C18 N5 C16 N4 1.5(5) . . . . ?
C19 N5 C16 N4 -179.7(4) . . . . ?
C18 N5 C16 Pd1 179.5(3) . . . . ?
C19 N5 C16 Pd1 -1.8(6) . . . . ?
C4 Pd1 C16 N4 -86.7(4) . . . . ?
N7 Pd1 C16 N4 96.3(4) . . . . ?
N3 Pd1 C16 N4 -32.1(12) . . . . ?
C4 Pd1 C16 N5 95.7(4) . . . . ?
N7 Pd1 C16 N5 -81.3(4) . . . . ?
N3 Pd1 C16 N5 150.3(8) . . . . ?
C11 N3 C7 C8 -0.1(5) . . . . ?
Pd1 N3 C7 C8 172.7(3) . . . . ?
C11 N3 C7 N2 179.9(3) . . . . ?
Pd1 N3 C7 N2 -7.3(4) . . . . ?
C9 C8 C7 N3 0.4(6) . . . . ?
C9 C8 C7 N2 -179.5(3) . . . . ?
C4 N2 C7 N3 6.1(5) . . . . ?
C6 N2 C7 N3 -170.9(4) . . . . ?
C4 N2 C7 C8 -173.9(4) . . . . ?
C6 N2 C7 C8 9.1(6) . . . . ?
C5 N1 C4 N2 -0.6(4) . . . . ?
C3 N1 C4 N2 -179.8(4) . . . . ?
C5 N1 C4 Pd1 -173.2(4) . . . . ?
C3 N1 C4 Pd1 7.6(8) . . . . ?
C6 N2 C4 N1 0.9(4) . . . . ?
C7 N2 C4 N1 -176.6(3) . . . . ?
C6 N2 C4 Pd1 175.9(3) . . . . ?
C7 N2 C4 Pd1 -1.7(4) . . . . ?
C16 Pd1 C4 N1 -16.3(5) . . . . ?
N7 Pd1 C4 N1 140.1(9) . . . . ?
N3 Pd1 C4 N1 170.4(5) . . . . ?
C16 Pd1 C4 N2 171.4(3) . . . . ?
N7 Pd1 C4 N2 -32.2(13) . . . . ?
N3 Pd1 C4 N2 -1.8(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.988
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.116
####################################################################### 
# 
# 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_brml285
_database_code_depnum_ccdc_archive 'CCDC 1405826'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        3c
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C22 H20 Br N8 O4 Pd), C H4 O, 2(Br)'
_chemical_formula_sum            'C45 H44 Br4 N16 O9 Pd2'
_chemical_formula_weight         1485.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

_cell_length_a                   7.3047(9)
_cell_length_b                   11.7658(11)
_cell_length_c                   31.200(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.115(10)
_cell_angle_gamma                90.00
_cell_volume                     2679.7(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    99.97(13)
_cell_measurement_reflns_used    1303
_cell_measurement_theta_min      4.2490
_cell_measurement_theta_max      23.3280

_exptl_crystal_description       needle
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1460
_exptl_absorpt_coefficient_mu    3.722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5873
_exptl_absorpt_correction_T_max  0.9293
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      99.97(13)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11046
_diffrn_reflns_av_R_equivalents  0.0951
_diffrn_reflns_av_sigmaI/netI    0.1411
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         25.06
_reflns_number_total             4707
_reflns_number_gt                2890
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_structure_solution    
;
SHELXS-97 (Sheldrick, G. M.    Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_structure_refinement  
;
SHELXS-97 (Sheldrick, G. M.    Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_molecular_graphics    'ORTEP-III Version 1.08 (Farrugia, 2005)'
_computing_publication_material  
;
enCIFer: A program for viewing, editing and visualising CIFs.
F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler,
J. Applied Cryst., 37, 331-334, 2004
;
_refine_special_details          
;
 All H atoms were placed in calculated positions and refined using a riding
 model. C-H distances : CH3 0.98Α, CH2 0.99Α, aromatic 0.95Α.

 All Uiso(H) values were constrained to be 1.2 times (1.5 for methyl) Ueq
 of the parent atom.

All of the crystals obtained were either of very poor quality or were small, hence little/no diffraction was observed beyond 0.84Α.
 
Residual electron density in the vicinity of Br1 was successfully modelled as a molecule of methanol with a SOF of 50%. 

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0391P)²+3.5271P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4707
_refine_ls_number_parameters     354
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.1364
_refine_ls_wR_factor_gt          0.1184
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.020
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.79650(10) 0.22339(6) 0.37914(2) 0.0217(2) Uani 1 1 d . . .
Br1 Br 0.56589(15) 0.14881(8) 0.42683(3) 0.0365(3) Uani 1 1 d . . .
Br2 Br 0.58314(14) 0.25390(8) 0.24685(3) 0.0354(3) Uani 1 1 d . . .
O1 O 0.1702(10) 0.4763(6) 0.4092(2) 0.046(2) Uani 1 1 d . . .
O2 O 0.1935(11) 0.6413(6) 0.3798(2) 0.048(2) Uani 1 1 d . . .
O3 O 1.403(2) 0.2434(9) 0.5780(4) 0.127(5) Uani 1 1 d . . .
O4 O 1.2990(16) 0.3942(8) 0.5472(3) 0.091(3) Uani 1 1 d . . .
O5 O 0.717(3) 0.2520(12) 0.5162(5) 0.058(5) Uani 0.50 1 d P . .
H5A H 0.6880 0.2152 0.4939 0.070 Uiso 0.50 1 calc PR . .
N1 N 1.1272(10) 0.2810(7) 0.3217(2) 0.0267(18) Uani 1 1 d . . .
N2 N 0.9169(10) 0.4048(6) 0.3282(2) 0.0234(18) Uani 1 1 d . . .
N3 N 0.6678(10) 0.3804(6) 0.3693(2) 0.0218(18) Uani 1 1 d . . .
N4 N 0.2533(12) 0.5476(7) 0.3889(3) 0.034(2) Uani 1 1 d . . .
N5 N 0.8792(10) -0.0156(6) 0.3576(2) 0.0226(18) Uani 1 1 d . . .
N6 N 1.0416(11) 0.0336(6) 0.4136(2) 0.027(2) Uani 1 1 d . . .
N7 N 1.0929(11) 0.2074(8) 0.4467(3) 0.041(2) Uani 1 1 d . . .
N8 N 1.3225(18) 0.2913(10) 0.5490(4) 0.076(4) Uani 1 1 d . . .
C1 C 1.0401(15) 0.0976(8) 0.2637(3) 0.035(3) Uani 1 1 d . . .
H1A H 0.9660 0.1640 0.2625 0.042 Uiso 1 1 calc R . .
H1B H 1.0138 0.0362 0.2447 0.042 Uiso 1 1 calc R . .
C2 C 1.1786(14) 0.0908(9) 0.2915(3) 0.033(3) Uani 1 1 d . . .
H2 H 1.2480 0.0225 0.2912 0.039 Uiso 1 1 calc R . .
C3 C 1.2388(13) 0.1777(8) 0.3232(3) 0.027(2) Uani 1 1 d . . .
H3A H 1.2349 0.1444 0.3523 0.032 Uiso 1 1 calc R . .
H3B H 1.3676 0.1983 0.3181 0.032 Uiso 1 1 calc R . .
C4 C 0.9690(13) 0.2987(7) 0.3400(3) 0.022(2) Uani 1 1 d . . .
C5 C 1.1699(14) 0.3744(9) 0.2963(3) 0.032(3) Uani 1 1 d . . .
H5 H 1.2733 0.3806 0.2789 0.038 Uiso 1 1 calc R . .
C6 C 1.0412(14) 0.4536(8) 0.3008(3) 0.027(2) Uani 1 1 d . . .
H6 H 1.0354 0.5269 0.2880 0.033 Uiso 1 1 calc R . .
C7 C 0.7551(13) 0.4520(8) 0.3436(3) 0.024(2) Uani 1 1 d . . .
C8 C 0.6918(14) 0.5596(8) 0.3325(3) 0.026(2) Uani 1 1 d . . .
H8 H 0.7596 0.6090 0.3150 0.031 Uiso 1 1 calc R . .
C9 C 0.5262(15) 0.5910(8) 0.3482(3) 0.034(3) Uani 1 1 d . . .
H9 H 0.4747 0.6633 0.3416 0.041 Uiso 1 1 calc R . .
C10 C 0.4372(13) 0.5164(7) 0.3735(3) 0.022(2) Uani 1 1 d . . .
C11 C 0.5065(14) 0.4123(8) 0.3844(3) 0.026(2) Uani 1 1 d . . .
H11 H 0.4410 0.3630 0.4024 0.032 Uiso 1 1 calc R . .
C12 C 0.4701(17) -0.1419(8) 0.3126(4) 0.049(3) Uani 1 1 d . . .
H12A H 0.5162 -0.1656 0.2859 0.059 Uiso 1 1 calc R . .
H12B H 0.3581 -0.1721 0.3221 0.059 Uiso 1 1 calc R . .
C13 C 0.5599(15) -0.0684(9) 0.3359(4) 0.039(3) Uani 1 1 d . . .
H13 H 0.5112 -0.0458 0.3624 0.047 Uiso 1 1 calc R . .
C14 C 0.7386(13) -0.0167(8) 0.3228(3) 0.027(2) Uani 1 1 d . . .
H14A H 0.7851 -0.0602 0.2983 0.033 Uiso 1 1 calc R . .
H14B H 0.7160 0.0623 0.3130 0.033 Uiso 1 1 calc R . .
C15 C 0.9181(12) 0.0734(7) 0.3835(3) 0.020(2) Uani 1 1 d . . .
C16 C 0.9773(14) -0.1094(8) 0.3711(3) 0.031(3) Uani 1 1 d . . .
H16 H 0.9733 -0.1823 0.3580 0.037 Uiso 1 1 calc R . .
C17 C 1.0785(14) -0.0807(8) 0.4056(3) 0.031(3) Uani 1 1 d . . .
H17 H 1.1601 -0.1286 0.4216 0.037 Uiso 1 1 calc R . .
C18 C 1.1134(13) 0.0941(8) 0.4491(3) 0.028(2) Uani 1 1 d . . .
C19 C 1.2002(14) 0.0408(8) 0.4826(3) 0.029(2) Uani 1 1 d . . .
H19 H 1.2124 -0.0396 0.4825 0.035 Uiso 1 1 calc R . .
C20 C 1.2698(13) 0.1021(9) 0.5163(3) 0.033(3) Uani 1 1 d . . .
H20 H 1.3301 0.0665 0.5403 0.040 Uiso 1 1 calc R . .
C21 C 1.2485(15) 0.2188(9) 0.5142(3) 0.038(3) Uani 1 1 d . . .
C22 C 1.1629(15) 0.2712(9) 0.4806(4) 0.043(3) Uani 1 1 d . . .
H22 H 1.1508 0.3516 0.4803 0.051 Uiso 1 1 calc R . .
C23 C 0.741(3) 0.3673(19) 0.5058(7) 0.051(7) Uani 0.50 1 d P . .
H23A H 0.6312 0.4103 0.5128 0.077 Uiso 0.50 1 calc PR . .
H23B H 0.7618 0.3742 0.4750 0.077 Uiso 0.50 1 calc PR . .
H23C H 0.8471 0.3975 0.5222 0.077 Uiso 0.50 1 calc PR . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C15 1.978(8) . ?
Pd1 C4 1.994(9) . ?
Pd1 N3 2.090(7) . ?
Pd1 Br1 2.4508(12) . ?
O1 N4 1.225(10) . ?
O2 N4 1.216(10) . ?
O3 N8 1.204(14) . ?
O4 N8 1.223(13) . ?
O5 C23 1.41(2) . ?
O5 H5A 0.8400 . ?
N1 C4 1.325(11) . ?
N1 C5 1.396(12) . ?
N1 C3 1.464(11) . ?
N2 C4 1.352(11) . ?
N2 C6 1.394(11) . ?
N2 C7 1.406(11) . ?
N3 C11 1.338(12) . ?
N3 C7 1.342(11) . ?
N4 C10 1.489(12) . ?
N5 C15 1.347(11) . ?
N5 C16 1.373(11) . ?
N5 C14 1.466(12) . ?
N6 C15 1.362(12) . ?
N6 C17 1.397(12) . ?
N6 C18 1.400(12) . ?
N7 C18 1.344(12) . ?
N7 C22 1.380(14) . ?
N8 C21 1.469(15) . ?
C1 C2 1.310(14) . ?
C1 H1A 0.9500 . ?
C1 H1B 0.9500 . ?
C2 C3 1.479(13) . ?
C2 H2 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C5 C6 1.335(13) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.387(12) . ?
C8 C9 1.373(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.362(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.363(12) . ?
C11 H11 0.9500 . ?
C12 C13 1.293(14) . ?
C12 H12A 0.9500 . ?
C12 H12B 0.9500 . ?
C13 C14 1.510(14) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C16 C17 1.326(14) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.357(13) . ?
C19 C20 1.359(13) . ?
C19 H19 0.9500 . ?
C20 C21 1.382(14) . ?
C20 H20 0.9500 . ?
C21 C22 1.349(14) . ?
C22 H22 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 Pd1 C4 98.4(4) . . ?
C15 Pd1 N3 175.5(3) . . ?
C4 Pd1 N3 79.0(3) . . ?
C15 Pd1 Br1 87.5(2) . . ?
C4 Pd1 Br1 174.1(3) . . ?
N3 Pd1 Br1 95.16(19) . . ?
C23 O5 H5A 109.5 . . ?
C4 N1 C5 109.7(8) . . ?
C4 N1 C3 127.6(8) . . ?
C5 N1 C3 122.4(8) . . ?
C4 N2 C6 111.4(8) . . ?
C4 N2 C7 120.2(8) . . ?
C6 N2 C7 128.4(8) . . ?
C11 N3 C7 118.6(8) . . ?
C11 N3 Pd1 126.4(6) . . ?
C7 N3 Pd1 114.9(6) . . ?
O2 N4 O1 124.2(9) . . ?
O2 N4 C10 117.9(8) . . ?
O1 N4 C10 117.9(8) . . ?
C15 N5 C16 110.1(8) . . ?
C15 N5 C14 125.3(7) . . ?
C16 N5 C14 124.3(8) . . ?
C15 N6 C17 109.5(8) . . ?
C15 N6 C18 126.1(8) . . ?
C17 N6 C18 124.2(8) . . ?
C18 N7 C22 117.4(9) . . ?
O3 N8 O4 124.2(12) . . ?
O3 N8 C21 116.2(11) . . ?
O4 N8 C21 119.6(11) . . ?
C2 C1 H1A 120.0 . . ?
C2 C1 H1B 120.0 . . ?
H1A C1 H1B 120.0 . . ?
C1 C2 C3 127.1(9) . . ?
C1 C2 H2 116.4 . . ?
C3 C2 H2 116.4 . . ?
N1 C3 C2 113.6(8) . . ?
N1 C3 H3A 108.8 . . ?
C2 C3 H3A 108.8 . . ?
N1 C3 H3B 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
N1 C4 N2 105.6(8) . . ?
N1 C4 Pd1 140.8(7) . . ?
N2 C4 Pd1 113.5(6) . . ?
C6 C5 N1 108.5(8) . . ?
C6 C5 H5 125.7 . . ?
N1 C5 H5 125.7 . . ?
C5 C6 N2 104.7(8) . . ?
C5 C6 H6 127.7 . . ?
N2 C6 H6 127.7 . . ?
N3 C7 C8 124.1(9) . . ?
N3 C7 N2 112.3(8) . . ?
C8 C7 N2 123.5(8) . . ?
C9 C8 C7 116.5(9) . . ?
C9 C8 H8 121.7 . . ?
C7 C8 H8 121.7 . . ?
C10 C9 C8 118.7(9) . . ?
C10 C9 H9 120.7 . . ?
C8 C9 H9 120.7 . . ?
C9 C10 C11 122.8(9) . . ?
C9 C10 N4 118.9(8) . . ?
C11 C10 N4 118.2(8) . . ?
N3 C11 C10 119.3(9) . . ?
N3 C11 H11 120.4 . . ?
C10 C11 H11 120.4 . . ?
C13 C12 H12A 120.0 . . ?
C13 C12 H12B 120.0 . . ?
H12A C12 H12B 120.0 . . ?
C12 C13 C14 122.9(11) . . ?
C12 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
N5 C14 C13 113.1(8) . . ?
N5 C14 H14A 109.0 . . ?
C13 C14 H14A 109.0 . . ?
N5 C14 H14B 109.0 . . ?
C13 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
N5 C15 N6 105.5(7) . . ?
N5 C15 Pd1 124.6(7) . . ?
N6 C15 Pd1 129.7(7) . . ?
C17 C16 N5 108.3(9) . . ?
C17 C16 H16 125.8 . . ?
N5 C16 H16 125.8 . . ?
C16 C17 N6 106.6(9) . . ?
C16 C17 H17 126.7 . . ?
N6 C17 H17 126.7 . . ?
N7 C18 C19 123.3(9) . . ?
N7 C18 N6 115.1(9) . . ?
C19 C18 N6 121.6(9) . . ?
C18 C19 C20 120.2(9) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C19 C20 C21 116.8(9) . . ?
C19 C20 H20 121.6 . . ?
C21 C20 H20 121.6 . . ?
C22 C21 C20 122.7(10) . . ?
C22 C21 N8 117.1(10) . . ?
C20 C21 N8 120.2(10) . . ?
C21 C22 N7 119.7(10) . . ?
C21 C22 H22 120.2 . . ?
N7 C22 H22 120.2 . . ?
O5 C23 H23A 109.5 . . ?
O5 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
O5 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         1.505
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.155
####################################################################### 
# 
# 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_brml290
_database_code_depnum_ccdc_archive 'CCDC 1405827'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        3a
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H22 Br N6 Pd, C H4 O, Br'
_chemical_formula_sum            'C23 H26 Br2 N6 O Pd'
_chemical_formula_weight         668.70

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   23.0939(12)
_cell_length_b                   9.6206(5)
_cell_length_c                   25.3916(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.426(5)
_cell_angle_gamma                90.00
_cell_volume                     5214.8(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    99.9(2)
_cell_measurement_reflns_used    2402
_cell_measurement_theta_min      3.7350
_cell_measurement_theta_max      72.2770

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2640
_exptl_absorpt_coefficient_mu    9.546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5982
_exptl_absorpt_correction_T_max  0.8320
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      99.9(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            26524
_diffrn_reflns_av_R_equivalents  0.1150
_diffrn_reflns_av_sigmaI/netI    0.1203
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         66.60
_reflns_number_total             8977
_reflns_number_gt                4782
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_structure_solution    
;
SHELXS-97 (Sheldrick, G. M.    Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_structure_refinement  
;
SHELXS-97 (Sheldrick, G. M.    Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_molecular_graphics    'ORTEP-III Version 1.08 (Farrugia, 2005)'
_computing_publication_material  
;
enCIFer: A program for viewing, editing and visualising CIFs.
F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler,
J. Applied Cryst., 37, 331-334, 2004
;
_refine_special_details          
;
All H atoms were placed in calculated positions and refined using a riding model. C-H distances : CH3 0.98Α, CH2 0.99Α, aromatic 0.95Α, OH 0.84Α.

All Uiso(H) values were constrained to be 1.2 times (1.5 times for methyl) Ueq of the parent atom.

 All crystals obtained (using various solvent systems) were of extremely poor quality. A very small single crystalline fragment (0.06 x 0.04 x 0.02 mm) was eventually isolated from a batch of crystals grown by the vapor diffusion of diethyl ether in to a concentrated solution of the product in methanol. This fragment proved suitable for a data collection using Cu Ka radiation, though the data obtained was weak, with almost no diffraction being observed beyond 0.84Α resolution.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0415P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8977
_refine_ls_number_parameters     600
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1350
_refine_ls_R_factor_gt           0.0583
_refine_ls_wR_factor_ref         0.1479
_refine_ls_wR_factor_gt          0.1148
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.003
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.46139(3) 0.83086(9) 0.68752(3) 0.02882(19) Uani 1 1 d . . .
Pd2 Pd 0.04493(3) 0.94853(9) 0.31023(3) 0.03030(19) Uani 1 1 d . . .
Br1 Br 0.52661(5) 0.95189(13) 0.77521(4) 0.0356(3) Uani 1 1 d . . .
Br2 Br -0.02545(5) 0.82541(14) 0.22536(4) 0.0377(3) Uani 1 1 d . . .
Br3 Br 0.30726(6) 0.43993(15) 0.39743(5) 0.0449(3) Uani 1 1 d . . .
Br4 Br -0.20903(5) 0.66900(14) 0.40754(4) 0.0395(3) Uani 1 1 d . . .
O1 O 0.3233(5) 0.7780(12) 0.4105(4) 0.072(3) Uani 1 1 d . . .
H1 H 0.3125 0.6998 0.3952 0.086 Uiso 1 1 calc R . .
O2 O -0.2034(6) 1.0045(14) 0.4203(7) 0.096(4) Uani 1 1 d . . .
H2 H -0.2081 0.9178 0.4179 0.115 Uiso 1 1 calc R . .
N1 N 0.3990(4) 0.6869(10) 0.5683(3) 0.035(2) Uani 1 1 d . . .
N2 N 0.3578(4) 0.6592(10) 0.6302(3) 0.032(2) Uani 1 1 d . . .
N3 N 0.3941(4) 0.7616(10) 0.7179(3) 0.031(2) Uani 1 1 d . . .
N4 N 0.5762(4) 0.8166(11) 0.6622(4) 0.037(2) Uani 1 1 d . . .
N5 N 0.5208(4) 0.9932(11) 0.6199(3) 0.036(2) Uani 1 1 d . . .
N6 N 0.4521(5) 1.1114(11) 0.5407(4) 0.043(2) Uani 1 1 d . . .
N7 N 0.1137(4) 1.1016(11) 0.4267(4) 0.041(2) Uani 1 1 d . . .
N8 N 0.1492(4) 1.1220(10) 0.3606(4) 0.036(2) Uani 1 1 d . . .
N9 N 0.1071(4) 1.0168(9) 0.2739(3) 0.030(2) Uani 1 1 d . . .
N10 N -0.0656(4) 0.9549(12) 0.3425(4) 0.044(2) Uani 1 1 d . . .
N11 N -0.0065(4) 0.7846(12) 0.3835(4) 0.044(3) Uani 1 1 d . . .
N12 N 0.0658(6) 0.6762(13) 0.4618(4) 0.061(3) Uani 1 1 d . . .
C1 C 0.5011(6) 0.4988(16) 0.5837(5) 0.052(3) Uani 1 1 d . . .
H1A H 0.4717 0.4761 0.6002 0.062 Uiso 1 1 calc R . .
H1B H 0.5360 0.4397 0.5894 0.062 Uiso 1 1 calc R . .
C2 C 0.4934(6) 0.6142(16) 0.5521(5) 0.055(4) Uani 1 1 d . . .
H2A H 0.5241 0.6322 0.5366 0.066 Uiso 1 1 calc R . .
C3 C 0.4415(5) 0.7173(13) 0.5390(4) 0.041(3) Uani 1 1 d . . .
H3A H 0.4596 0.8111 0.5504 0.049 Uiso 1 1 calc R . .
H3B H 0.4172 0.7184 0.4974 0.049 Uiso 1 1 calc R . .
C4 C 0.4063(5) 0.7247(13) 0.6214(5) 0.037(3) Uani 1 1 d . . .
C5 C 0.3473(5) 0.6004(13) 0.5444(4) 0.039(3) Uani 1 1 d . . .
H5 H 0.3330 0.5612 0.5072 0.047 Uiso 1 1 calc R . .
C6 C 0.3211(5) 0.5815(13) 0.5830(5) 0.041(3) Uani 1 1 d . . .
H6 H 0.2853 0.5271 0.5789 0.049 Uiso 1 1 calc R . .
C7 C 0.3518(4) 0.6745(13) 0.6829(4) 0.035(2) Uani 1 1 d . . .
C8 C 0.3078(5) 0.6079(13) 0.6972(5) 0.042(3) Uani 1 1 d . . .
H8 H 0.2775 0.5488 0.6709 0.051 Uiso 1 1 calc R . .
C9 C 0.3089(5) 0.6296(15) 0.7512(5) 0.050(3) Uani 1 1 d . . .
H9 H 0.2799 0.5818 0.7629 0.060 Uiso 1 1 calc R . .
C10 C 0.3511(5) 0.7186(14) 0.7882(5) 0.044(3) Uani 1 1 d . . .
H10 H 0.3511 0.7357 0.8250 0.053 Uiso 1 1 calc R . .
C11 C 0.3944(5) 0.7837(14) 0.7698(4) 0.039(3) Uani 1 1 d . . .
H11 H 0.4246 0.8450 0.7950 0.047 Uiso 1 1 calc R . .
C12 C 0.6936(5) 0.6167(15) 0.7725(6) 0.054(3) Uani 1 1 d . . .
H12A H 0.6960 0.5386 0.7505 0.064 Uiso 1 1 calc R . .
H12B H 0.7250 0.6308 0.8094 0.064 Uiso 1 1 calc R . .
C13 C 0.6466(5) 0.7059(12) 0.7518(4) 0.037(3) Uani 1 1 d . . .
H13 H 0.6444 0.7838 0.7740 0.045 Uiso 1 1 calc R . .
C14 C 0.5976(5) 0.6854(13) 0.6947(5) 0.042(3) Uani 1 1 d . . .
H14A H 0.5611 0.6393 0.6987 0.050 Uiso 1 1 calc R . .
H14B H 0.6139 0.6225 0.6727 0.050 Uiso 1 1 calc R . .
C15 C 0.5230(5) 0.8832(12) 0.6547(4) 0.032(2) Uani 1 1 d . . .
C16 C 0.6054(5) 0.8786(14) 0.6303(5) 0.043(3) Uani 1 1 d . . .
H16 H 0.6430 0.8476 0.6272 0.051 Uiso 1 1 calc R . .
C17 C 0.5720(5) 0.9906(13) 0.6042(5) 0.041(3) Uani 1 1 d . . .
H17 H 0.5816 1.0545 0.5801 0.049 Uiso 1 1 calc R . .
C18 C 0.4688(5) 1.0842(12) 0.5963(5) 0.036(3) Uani 1 1 d . . .
C19 C 0.4369(5) 1.1352(12) 0.6297(5) 0.040(3) Uani 1 1 d . . .
H19 H 0.4512 1.1168 0.6694 0.048 Uiso 1 1 calc R . .
C20 C 0.3834(6) 1.2135(13) 0.6019(5) 0.044(3) Uani 1 1 d . . .
H20 H 0.3601 1.2507 0.6224 0.053 Uiso 1 1 calc R . .
C21 C 0.3645(6) 1.2367(14) 0.5442(5) 0.048(3) Uani 1 1 d . . .
H21 H 0.3268 1.2855 0.5240 0.057 Uiso 1 1 calc R . .
C22 C 0.4011(6) 1.1881(15) 0.5161(5) 0.051(3) Uani 1 1 d . . .
H22 H 0.3891 1.2107 0.4770 0.061 Uiso 1 1 calc R . .
C23 C 0.0156(6) 1.2902(16) 0.4246(5) 0.055(3) Uani 1 1 d . . .
H23A H 0.0422 1.3176 0.4057 0.066 Uiso 1 1 calc R . .
H23B H -0.0183 1.3480 0.4231 0.066 Uiso 1 1 calc R . .
C24 C 0.0258(5) 1.1728(16) 0.4528(5) 0.053(4) Uani 1 1 d . . .
H24 H -0.0026 1.1519 0.4707 0.063 Uiso 1 1 calc R . .
C25 C 0.0767(5) 1.0657(15) 0.4608(4) 0.045(3) Uani 1 1 d . . .
H25A H 0.1046 1.0610 0.5016 0.054 Uiso 1 1 calc R . .
H25B H 0.0574 0.9730 0.4492 0.054 Uiso 1 1 calc R . .
C26 C 0.1037(5) 1.0591(12) 0.3745(4) 0.032(2) Uani 1 1 d . . .
C27 C 0.1656(5) 1.1867(14) 0.4482(5) 0.046(3) Uani 1 1 d . . .
H27 H 0.1820 1.2269 0.4852 0.056 Uiso 1 1 calc R . .
C28 C 0.1890(5) 1.2025(12) 0.4073(4) 0.038(3) Uani 1 1 d . . .
H28 H 0.2244 1.2559 0.4093 0.046 Uiso 1 1 calc R . .
C29 C 0.1515(4) 1.1027(11) 0.3073(4) 0.027(2) Uani 1 1 d . . .
C30 C 0.1947(5) 1.1668(14) 0.2897(5) 0.041(3) Uani 1 1 d . . .
H30 H 0.2259 1.2269 0.3144 0.049 Uiso 1 1 calc R . .
C31 C 0.1908(5) 1.1401(13) 0.2350(5) 0.042(3) Uani 1 1 d . . .
H31 H 0.2195 1.1829 0.2214 0.050 Uiso 1 1 calc R . .
C32 C 0.1456(5) 1.0522(15) 0.2001(5) 0.045(3) Uani 1 1 d . . .
H32 H 0.1422 1.0335 0.1623 0.054 Uiso 1 1 calc R . .
C33 C 0.1052(5) 0.9919(13) 0.2219(4) 0.040(3) Uani 1 1 d . . .
H33 H 0.0745 0.9291 0.1984 0.048 Uiso 1 1 calc R . .
C34 C -0.1970(7) 1.1232(19) 0.2406(7) 0.074(5) Uani 1 1 d . . .
H34A H -0.2016 1.1984 0.2629 0.088 Uiso 1 1 calc R . .
H34B H -0.2306 1.0987 0.2062 0.088 Uiso 1 1 calc R . .
C35 C -0.1454(6) 1.0548(18) 0.2569(5) 0.059(4) Uani 1 1 d . . .
H35 H -0.1425 0.9803 0.2334 0.071 Uiso 1 1 calc R . .
C36 C -0.0902(5) 1.0832(14) 0.3093(6) 0.052(3) Uani 1 1 d . . .
H36A H -0.1019 1.1502 0.3332 0.062 Uiso 1 1 calc R . .
H36B H -0.0569 1.1261 0.2991 0.062 Uiso 1 1 calc R . .
C37 C -0.0118(5) 0.8954(13) 0.3475(4) 0.037(3) Uani 1 1 d . . .
C38 C -0.0943(6) 0.8887(16) 0.3744(6) 0.053(4) Uani 1 1 d . . .
H38 H -0.1329 0.9134 0.3771 0.063 Uiso 1 1 calc R . .
C39 C -0.0574(6) 0.7844(15) 0.4001(5) 0.050(3) Uani 1 1 d . . .
H39 H -0.0643 0.7203 0.4256 0.060 Uiso 1 1 calc R . .
C40 C 0.0472(6) 0.6985(13) 0.4061(4) 0.043(3) Uani 1 1 d . . .
C41 C 0.0771(6) 0.6432(14) 0.3726(5) 0.048(3) Uani 1 1 d . . .
H41 H 0.0594 0.6555 0.3324 0.057 Uiso 1 1 calc R . .
C42 C 0.1319(6) 0.5711(15) 0.3974(6) 0.057(3) Uani 1 1 d . . .
H42 H 0.1540 0.5356 0.3755 0.069 Uiso 1 1 calc R . .
C43 C 0.1537(7) 0.5520(17) 0.4559(6) 0.067(4) Uani 1 1 d . . .
H43 H 0.1920 0.5044 0.4753 0.081 Uiso 1 1 calc R . .
C44 C 0.1189(8) 0.6034(18) 0.4858(6) 0.072(5) Uani 1 1 d . . .
H44 H 0.1337 0.5860 0.5256 0.086 Uiso 1 1 calc R . .
C45 C 0.2708(8) 0.849(2) 0.4097(8) 0.104(7) Uani 1 1 d . . .
H45A H 0.2692 0.8467 0.4477 0.156 Uiso 1 1 calc R . .
H45B H 0.2330 0.8059 0.3822 0.156 Uiso 1 1 calc R . .
H45C H 0.2730 0.9463 0.3987 0.156 Uiso 1 1 calc R . .
C46 C -0.2559(10) 1.067(2) 0.4296(11) 0.128(9) Uani 1 1 d . . .
H46A H -0.2429 1.1566 0.4491 0.192 Uiso 1 1 calc R . .
H46B H -0.2699 1.0054 0.4530 0.192 Uiso 1 1 calc R . .
H46C H -0.2904 1.0826 0.3928 0.192 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C4 1.961(12) . ?
Pd1 C15 1.968(10) . ?
Pd1 N3 2.091(8) . ?
Pd1 Br1 2.4542(13) . ?
Pd2 C37 1.955(11) . ?
Pd2 C26 1.987(11) . ?
Pd2 N9 2.086(8) . ?
Pd2 Br2 2.4528(13) . ?
O1 C45 1.388(18) . ?
O1 H1 0.8400 . ?
O2 C46 1.45(2) . ?
O2 H2 0.8400 . ?
N1 C4 1.345(13) . ?
N1 C5 1.389(14) . ?
N1 C3 1.468(12) . ?
N2 C4 1.376(14) . ?
N2 C6 1.392(14) . ?
N2 C7 1.404(13) . ?
N3 C11 1.333(12) . ?
N3 C7 1.335(14) . ?
N4 C15 1.335(13) . ?
N4 C16 1.372(13) . ?
N4 C14 1.485(15) . ?
N5 C15 1.368(14) . ?
N5 C17 1.384(13) . ?
N5 C18 1.421(15) . ?
N6 C22 1.327(16) . ?
N6 C18 1.338(13) . ?
N7 C26 1.320(13) . ?
N7 C27 1.381(15) . ?
N7 C25 1.470(12) . ?
N8 C26 1.370(13) . ?
N8 C29 1.387(13) . ?
N8 C28 1.421(14) . ?
N9 C33 1.327(13) . ?
N9 C29 1.339(13) . ?
N10 C37 1.330(15) . ?
N10 C38 1.382(15) . ?
N10 C36 1.480(17) . ?
N11 C37 1.378(15) . ?
N11 C39 1.393(14) . ?
N11 C40 1.418(16) . ?
N12 C40 1.328(14) . ?
N12 C44 1.340(19) . ?
C1 C2 1.340(19) . ?
C1 H1A 0.9500 . ?
C1 H1B 0.9500 . ?
C2 C3 1.493(18) . ?
C2 H2A 0.9500 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C5 C6 1.347(15) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C8 1.363(16) . ?
C8 C9 1.377(16) . ?
C8 H8 0.9500 . ?
C9 C10 1.366(18) . ?
C9 H9 0.9500 . ?
C10 C11 1.400(15) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
C12 C13 1.326(17) . ?
C12 H12A 0.9500 . ?
C12 H12B 0.9500 . ?
C13 C14 1.473(15) . ?
C13 H13 0.9500 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C16 C17 1.343(17) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.408(15) . ?
C19 C20 1.387(17) . ?
C19 H19 0.9500 . ?
C20 C21 1.378(16) . ?
C20 H20 0.9500 . ?
C21 C22 1.378(17) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C24 1.310(19) . ?
C23 H23A 0.9500 . ?
C23 H23B 0.9500 . ?
C24 C25 1.518(19) . ?
C24 H24 0.9500 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C27 C28 1.348(15) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C30 1.384(15) . ?
C30 C31 1.383(15) . ?
C30 H30 0.9500 . ?
C31 C32 1.372(17) . ?
C31 H31 0.9500 . ?
C32 C33 1.381(15) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.285(19) . ?
C34 H34A 0.9500 . ?
C34 H34B 0.9500 . ?
C35 C36 1.476(18) . ?
C35 H35 0.9500 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C38 C39 1.318(19) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C41 1.390(16) . ?
C41 C42 1.368(18) . ?
C41 H41 0.9500 . ?
C42 C43 1.386(19) . ?
C42 H42 0.9500 . ?
C43 C44 1.39(2) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 Pd1 C15 96.2(4) . . ?
C4 Pd1 N3 79.6(4) . . ?
C15 Pd1 N3 175.4(4) . . ?
C4 Pd1 Br1 175.1(3) . . ?
C15 Pd1 Br1 88.3(3) . . ?
N3 Pd1 Br1 95.8(2) . . ?
C37 Pd2 C26 96.6(4) . . ?
C37 Pd2 N9 176.2(4) . . ?
C26 Pd2 N9 80.0(4) . . ?
C37 Pd2 Br2 87.6(3) . . ?
C26 Pd2 Br2 175.1(3) . . ?
N9 Pd2 Br2 95.8(2) . . ?
C45 O1 H1 109.5 . . ?
C46 O2 H2 109.5 . . ?
C4 N1 C5 111.1(9) . . ?
C4 N1 C3 126.9(9) . . ?
C5 N1 C3 121.8(8) . . ?
C4 N2 C6 111.9(9) . . ?
C4 N2 C7 119.2(9) . . ?
C6 N2 C7 128.9(9) . . ?
C11 N3 C7 119.1(9) . . ?
C11 N3 Pd1 126.2(7) . . ?
C7 N3 Pd1 114.3(6) . . ?
C15 N4 C16 109.9(10) . . ?
C15 N4 C14 125.4(9) . . ?
C16 N4 C14 124.3(9) . . ?
C15 N5 C17 110.3(9) . . ?
C15 N5 C18 124.4(9) . . ?
C17 N5 C18 124.6(9) . . ?
C22 N6 C18 116.8(10) . . ?
C26 N7 C27 111.9(9) . . ?
C26 N7 C25 126.9(10) . . ?
C27 N7 C25 121.2(9) . . ?
C26 N8 C29 120.7(9) . . ?
C26 N8 C28 109.9(9) . . ?
C29 N8 C28 129.3(9) . . ?
C33 N9 C29 117.9(9) . . ?
C33 N9 Pd2 128.1(8) . . ?
C29 N9 Pd2 113.8(6) . . ?
C37 N10 C38 112.7(12) . . ?
C37 N10 C36 123.7(10) . . ?
C38 N10 C36 123.5(11) . . ?
C37 N11 C39 109.2(11) . . ?
C37 N11 C40 124.2(9) . . ?
C39 N11 C40 125.9(10) . . ?
C40 N12 C44 115.9(12) . . ?
C2 C1 H1A 120.0 . . ?
C2 C1 H1B 120.0 . . ?
H1A C1 H1B 120.0 . . ?
C1 C2 C3 126.6(11) . . ?
C1 C2 H2A 116.7 . . ?
C3 C2 H2A 116.7 . . ?
N1 C3 C2 113.0(10) . . ?
N1 C3 H3A 109.0 . . ?
C2 C3 H3A 109.0 . . ?
N1 C3 H3B 109.0 . . ?
C2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
N1 C4 N2 103.8(10) . . ?
N1 C4 Pd1 142.4(8) . . ?
N2 C4 Pd1 113.7(7) . . ?
C6 C5 N1 108.2(9) . . ?
C6 C5 H5 125.9 . . ?
N1 C5 H5 125.9 . . ?
C5 C6 N2 105.0(10) . . ?
C5 C6 H6 127.5 . . ?
N2 C6 H6 127.5 . . ?
N3 C7 C8 123.1(10) . . ?
N3 C7 N2 112.9(9) . . ?
C8 C7 N2 124.0(10) . . ?
C7 C8 C9 117.5(11) . . ?
C7 C8 H8 121.2 . . ?
C9 C8 H8 121.2 . . ?
C10 C9 C8 121.1(11) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 117.7(11) . . ?
C9 C10 H10 121.2 . . ?
C11 C10 H10 121.2 . . ?
N3 C11 C10 121.5(11) . . ?
N3 C11 H11 119.3 . . ?
C10 C11 H11 119.3 . . ?
C13 C12 H12A 120.0 . . ?
C13 C12 H12B 120.0 . . ?
H12A C12 H12B 120.0 . . ?
C12 C13 C14 120.6(12) . . ?
C12 C13 H13 119.7 . . ?
C14 C13 H13 119.7 . . ?
C13 C14 N4 113.7(10) . . ?
C13 C14 H14A 108.8 . . ?
N4 C14 H14A 108.8 . . ?
C13 C14 H14B 108.8 . . ?
N4 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
N4 C15 N5 105.5(9) . . ?
N4 C15 Pd1 126.3(9) . . ?
N5 C15 Pd1 128.2(8) . . ?
C17 C16 N4 108.7(10) . . ?
C17 C16 H16 125.6 . . ?
N4 C16 H16 125.6 . . ?
C16 C17 N5 105.4(10) . . ?
C16 C17 H17 127.3 . . ?
N5 C17 H17 127.3 . . ?
N6 C18 C19 124.1(11) . . ?
N6 C18 N5 114.9(9) . . ?
C19 C18 N5 120.9(9) . . ?
C20 C19 C18 116.8(10) . . ?
C20 C19 H19 121.6 . . ?
C18 C19 H19 121.6 . . ?
C21 C20 C19 119.2(11) . . ?
C21 C20 H20 120.4 . . ?
C19 C20 H20 120.4 . . ?
C22 C21 C20 119.1(12) . . ?
C22 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?
N6 C22 C21 123.7(11) . . ?
N6 C22 H22 118.2 . . ?
C21 C22 H22 118.2 . . ?
C24 C23 H23A 120.0 . . ?
C24 C23 H23B 120.0 . . ?
H23A C23 H23B 120.0 . . ?
C23 C24 C25 128.8(11) . . ?
C23 C24 H24 115.6 . . ?
C25 C24 H24 115.6 . . ?
N7 C25 C24 110.8(10) . . ?
N7 C25 H25A 109.5 . . ?
C24 C25 H25A 109.5 . . ?
N7 C25 H25B 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 108.1 . . ?
N7 C26 N8 105.3(10) . . ?
N7 C26 Pd2 142.5(8) . . ?
N8 C26 Pd2 112.0(7) . . ?
C28 C27 N7 107.8(10) . . ?
C28 C27 H27 126.1 . . ?
N7 C27 H27 126.1 . . ?
C27 C28 N8 105.1(9) . . ?
C27 C28 H28 127.5 . . ?
N8 C28 H28 127.5 . . ?
N9 C29 C30 122.9(9) . . ?
N9 C29 N8 113.3(8) . . ?
C30 C29 N8 123.8(9) . . ?
C31 C30 C29 117.6(11) . . ?
C31 C30 H30 121.2 . . ?
C29 C30 H30 121.2 . . ?
C32 C31 C30 120.4(10) . . ?
C32 C31 H31 119.8 . . ?
C30 C31 H31 119.8 . . ?
C31 C32 C33 117.6(10) . . ?
C31 C32 H32 121.2 . . ?
C33 C32 H32 121.2 . . ?
N9 C33 C32 123.6(11) . . ?
N9 C33 H33 118.2 . . ?
C32 C33 H33 118.2 . . ?
C35 C34 H34A 120.0 . . ?
C35 C34 H34B 120.0 . . ?
H34A C34 H34B 120.0 . . ?
C34 C35 C36 124.8(15) . . ?
C34 C35 H35 117.6 . . ?
C36 C35 H35 117.6 . . ?
C35 C36 N10 111.8(11) . . ?
C35 C36 H36A 109.3 . . ?
N10 C36 H36A 109.3 . . ?
C35 C36 H36B 109.3 . . ?
N10 C36 H36B 109.3 . . ?
H36A C36 H36B 107.9 . . ?
N10 C37 N11 103.9(9) . . ?
N10 C37 Pd2 128.0(9) . . ?
N11 C37 Pd2 128.1(9) . . ?
C39 C38 N10 106.1(11) . . ?
C39 C38 H38 127.0 . . ?
N10 C38 H38 127.0 . . ?
C38 C39 N11 108.1(10) . . ?
C38 C39 H39 125.9 . . ?
N11 C39 H39 125.9 . . ?
N12 C40 C41 123.8(13) . . ?
N12 C40 N11 113.7(11) . . ?
C41 C40 N11 122.5(10) . . ?
C42 C41 C40 120.0(12) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C43 117.1(14) . . ?
C41 C42 H42 121.5 . . ?
C43 C42 H42 121.5 . . ?
C42 C43 C44 119.2(14) . . ?
C42 C43 H43 120.4 . . ?
C44 C43 H43 120.4 . . ?
N12 C44 C43 123.8(12) . . ?
N12 C44 H44 118.1 . . ?
C43 C44 H44 118.1 . . ?
O1 C45 H45A 109.5 . . ?
O1 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
O1 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
O2 C46 H46A 109.5 . . ?
O2 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
O2 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        66.60
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.150
####################################################################### 
# 
# 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_mrc029
_database_code_depnum_ccdc_archive 'CCDC 1405828'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        1f
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H15 N4, Br'
_chemical_formula_sum            'C15 H15 Br N4'
_chemical_formula_weight         331.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'


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

_cell_length_a                   8.1157(2)
_cell_length_b                   16.6921(4)
_cell_length_c                   10.8193(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.625(3)
_cell_angle_gamma                90.00
_cell_volume                     1449.09(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    99.99(10)
_cell_measurement_reflns_used    5384
_cell_measurement_theta_min      3.5040
_cell_measurement_theta_max      29.9290

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    2.832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3688
_exptl_absorpt_correction_T_max  0.6296
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      99.99(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            11471
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.94
_diffrn_reflns_theta_max         28.70
_reflns_number_total             6309
_reflns_number_gt                5815
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_structure_solution    
;
SHELXS-97 (Sheldrick, G. M.    Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_structure_refinement  
;
SHELXS-97 (Sheldrick, G. M.    Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_molecular_graphics    'ORTEP-III Version 1.08 (Farrugia, 2005)'
_computing_publication_material  
;
enCIFer: A program for viewing, editing and visualising CIFs.
F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler,
J. Applied Cryst., 37, 331-334, 2004
;
_refine_special_details          
;
All H atoms were placed in calculated positions and refined using a riding
 model. C-H distances : CH2 0.99Α, aromatic, 0.95Α.

All Uiso(H) values were constrained to be 1.2 times Ueq
 of the parent atom.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0374P)²+0.0740P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.377(8)
_refine_ls_number_reflns         6309
_refine_ls_number_parameters     362
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0790
_refine_ls_wR_factor_gt          0.0765
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.01660(4) 0.164970(17) 0.62260(3) 0.01798(8) Uani 1 1 d . . .
Br2 Br 0.08901(4) 0.319780(19) 0.14240(3) 0.01800(9) Uani 1 1 d . . .
N1 N 0.4972(4) 0.3248(2) 0.7404(3) 0.0203(6) Uani 1 1 d . . .
N2 N 0.1797(4) 0.38854(17) 0.7140(3) 0.0165(6) Uani 1 1 d . . .
N3 N 0.0747(4) 0.43639(17) 0.5338(3) 0.0144(6) Uani 1 1 d . . .
N4 N -0.2706(4) 0.45252(19) 0.5042(3) 0.0238(7) Uani 1 1 d . . .
N5 N 0.4289(4) 0.13624(18) 0.2284(3) 0.0226(7) Uani 1 1 d . . .
N6 N 0.1101(4) 0.08319(17) 0.2043(3) 0.0169(6) Uani 1 1 d . . .
N7 N 0.0008(4) 0.04578(16) 0.0185(3) 0.0154(6) Uani 1 1 d . . .
N8 N -0.3474(5) 0.0294(2) -0.0171(3) 0.0231(8) Uani 1 1 d . . .
C1 C 0.6618(4) 0.3105(2) 0.7612(4) 0.0213(8) Uani 1 1 d . . .
H1 H 0.7223 0.3152 0.6929 0.026 Uiso 1 1 calc R . .
C2 C 0.7477(5) 0.2894(2) 0.8759(4) 0.0226(8) Uani 1 1 d . . .
H2 H 0.8644 0.2800 0.8858 0.027 Uiso 1 1 calc R . .
C3 C 0.6622(6) 0.2819(2) 0.9765(4) 0.0259(9) Uani 1 1 d . . .
H3 H 0.7188 0.2677 1.0568 0.031 Uiso 1 1 calc R . .
C4 C 0.4909(5) 0.2958(2) 0.9575(4) 0.0224(9) Uani 1 1 d . . .
H4 H 0.4275 0.2901 1.0240 0.027 Uiso 1 1 calc R . .
C5 C 0.4150(4) 0.3181(2) 0.8383(3) 0.0174(7) Uani 1 1 d . . .
C6 C 0.2283(4) 0.3308(2) 0.8149(3) 0.0174(8) Uani 1 1 d . . .
H6A H 0.1722 0.2790 0.7927 0.021 Uiso 1 1 calc R . .
H6B H 0.1910 0.3505 0.8925 0.021 Uiso 1 1 calc R . .
C7 C 0.0921(5) 0.3700(2) 0.6030(3) 0.0160(7) Uani 1 1 d . . .
H7 H 0.0496 0.3185 0.5779 0.019 Uiso 1 1 calc R . .
C8 C 0.2204(4) 0.4689(2) 0.7154(3) 0.0178(7) Uani 1 1 d . . .
H8 H 0.2826 0.4976 0.7825 0.021 Uiso 1 1 calc R . .
C9 C 0.1544(5) 0.4988(2) 0.6025(3) 0.0176(7) Uani 1 1 d . . .
H9 H 0.1615 0.5527 0.5755 0.021 Uiso 1 1 calc R . .
C10 C -0.0211(5) 0.4427(2) 0.4073(3) 0.0178(8) Uani 1 1 d . . .
H10A H 0.0211 0.4022 0.3529 0.021 Uiso 1 1 calc R . .
H10B H -0.0018 0.4962 0.3729 0.021 Uiso 1 1 calc R . .
C11 C -0.2049(5) 0.4307(2) 0.4033(3) 0.0168(8) Uani 1 1 d . . .
C12 C -0.2983(5) 0.4008(2) 0.2956(4) 0.0223(8) Uani 1 1 d . . .
H12 H -0.2457 0.3851 0.2266 0.027 Uiso 1 1 calc R . .
C13 C -0.4707(5) 0.3939(2) 0.2897(4) 0.0260(9) Uani 1 1 d . . .
H13 H -0.5383 0.3742 0.2167 0.031 Uiso 1 1 calc R . .
C14 C -0.5403(5) 0.4168(3) 0.3938(4) 0.0252(9) Uani 1 1 d . . .
H14 H -0.6571 0.4129 0.3938 0.030 Uiso 1 1 calc R . .
C15 C -0.4368(6) 0.4452(3) 0.4975(4) 0.0302(11) Uani 1 1 d . . .
H15 H -0.4859 0.4604 0.5684 0.036 Uiso 1 1 calc R . .
C16 C 0.5900(5) 0.1564(2) 0.2388(4) 0.0264(9) Uani 1 1 d . . .
H16 H 0.6474 0.1451 0.1705 0.032 Uiso 1 1 calc R . .
C17 C 0.6776(6) 0.1926(2) 0.3431(5) 0.0304(10) Uani 1 1 d . . .
H17 H 0.7917 0.2064 0.3463 0.037 Uiso 1 1 calc R . .
C18 C 0.5929(6) 0.2085(3) 0.4443(4) 0.0325(11) Uani 1 1 d . . .
H18 H 0.6493 0.2326 0.5183 0.039 Uiso 1 1 calc R . .
C19 C 0.4289(6) 0.1889(2) 0.4349(4) 0.0254(9) Uani 1 1 d . . .
H19 H 0.3685 0.1997 0.5018 0.030 Uiso 1 1 calc R . .
C20 C 0.3510(5) 0.1528(2) 0.3259(3) 0.0169(8) Uani 1 1 d . . .
C21 C 0.1675(5) 0.1335(2) 0.3128(3) 0.0204(8) Uani 1 1 d . . .
H21A H 0.1449 0.1057 0.3893 0.025 Uiso 1 1 calc R . .
H21B H 0.1033 0.1841 0.3055 0.025 Uiso 1 1 calc R . .
C22 C 0.0270(5) 0.1089(2) 0.0959(3) 0.0167(7) Uani 1 1 d . . .
H22 H -0.0075 0.1625 0.0768 0.020 Uiso 1 1 calc R . .
C23 C 0.1389(5) 0.0022(2) 0.1965(3) 0.0197(8) Uani 1 1 d . . .
H23 H 0.1951 -0.0309 0.2608 0.024 Uiso 1 1 calc R . .
C24 C 0.0714(4) -0.0215(2) 0.0792(3) 0.0167(7) Uani 1 1 d . . .
H24 H 0.0727 -0.0740 0.0458 0.020 Uiso 1 1 calc R . .
C25 C -0.0914(5) 0.0466(2) -0.1084(4) 0.0168(8) Uani 1 1 d . . .
H25A H -0.0723 -0.0047 -0.1499 0.020 Uiso 1 1 calc R . .
H25B H -0.0475 0.0902 -0.1563 0.020 Uiso 1 1 calc R . .
C26 C -0.2763(5) 0.0585(2) -0.1118(3) 0.0160(8) Uani 1 1 d . . .
C27 C -0.3675(5) 0.0964(2) -0.2154(4) 0.0199(8) Uani 1 1 d . . .
H27 H -0.3130 0.1167 -0.2806 0.024 Uiso 1 1 calc R . .
C28 C -0.5373(5) 0.1038(2) -0.2216(4) 0.0262(9) Uani 1 1 d . . .
H28 H -0.6022 0.1283 -0.2918 0.031 Uiso 1 1 calc R . .
C29 C -0.6118(5) 0.0749(3) -0.1234(4) 0.0276(9) Uani 1 1 d . . .
H29 H -0.7285 0.0803 -0.1238 0.033 Uiso 1 1 calc R . .
C30 C -0.5126(6) 0.0379(3) -0.0248(4) 0.0279(10) Uani 1 1 d . . .
H30 H -0.5647 0.0174 0.0416 0.034 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C5 1.339(4) . ?
N1 C1 1.342(5) . ?
N2 C7 1.336(5) . ?
N2 C8 1.382(4) . ?
N2 C6 1.466(4) . ?
N3 C7 1.334(4) . ?
N3 C9 1.383(4) . ?
N3 C10 1.472(4) . ?
N4 C11 1.335(5) . ?
N4 C15 1.346(5) . ?
N5 C20 1.337(5) . ?
N5 C16 1.339(5) . ?
N6 C22 1.333(5) . ?
N6 C23 1.376(5) . ?
N6 C21 1.462(5) . ?
N7 C22 1.343(5) . ?
N7 C24 1.381(4) . ?
N7 C25 1.462(5) . ?
N8 C30 1.338(5) . ?
N8 C26 1.340(5) . ?
C1 C2 1.375(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.381(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.394(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.513(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7 0.9500 . ?
C8 C9 1.353(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C11 1.500(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.385(5) . ?
C12 C13 1.396(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.387(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.380(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.402(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.360(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.390(5) . ?
C19 H19 0.9500 . ?
C20 C21 1.510(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22 0.9500 . ?
C23 C24 1.363(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.509(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.399(5) . ?
C27 C28 1.375(6) . ?
C27 H27 0.9500 . ?
C28 C29 1.386(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.382(6) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 N1 C1 117.0(3) . . ?
C7 N2 C8 109.2(3) . . ?
C7 N2 C6 124.4(3) . . ?
C8 N2 C6 126.4(3) . . ?
C7 N3 C9 108.8(3) . . ?
C7 N3 C10 125.3(3) . . ?
C9 N3 C10 125.8(3) . . ?
C11 N4 C15 116.8(4) . . ?
C20 N5 C16 116.9(3) . . ?
C22 N6 C23 109.4(3) . . ?
C22 N6 C21 125.4(3) . . ?
C23 N6 C21 125.2(3) . . ?
C22 N7 C24 109.0(3) . . ?
C22 N7 C25 126.1(3) . . ?
C24 N7 C25 124.9(3) . . ?
C30 N8 C26 117.1(4) . . ?
N1 C1 C2 123.7(3) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 119.2(4) . . ?
C1 C2 H2 120.4 . . ?
C3 C2 H2 120.4 . . ?
C2 C3 C4 118.5(4) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C5 C4 C3 118.3(4) . . ?
C5 C4 H4 120.9 . . ?
C3 C4 H4 120.9 . . ?
N1 C5 C4 123.4(3) . . ?
N1 C5 C6 117.5(3) . . ?
C4 C5 C6 119.0(3) . . ?
N2 C6 C5 111.6(3) . . ?
N2 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
N2 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 108.0 . . ?
N3 C7 N2 108.0(3) . . ?
N3 C7 H7 126.0 . . ?
N2 C7 H7 126.0 . . ?
C9 C8 N2 106.6(3) . . ?
C9 C8 H8 126.7 . . ?
N2 C8 H8 126.7 . . ?
C8 C9 N3 107.3(3) . . ?
C8 C9 H9 126.3 . . ?
N3 C9 H9 126.3 . . ?
N3 C10 C11 113.7(3) . . ?
N3 C10 H10A 108.8 . . ?
C11 C10 H10A 108.8 . . ?
N3 C10 H10B 108.8 . . ?
C11 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
N4 C11 C12 123.4(4) . . ?
N4 C11 C10 117.2(3) . . ?
C12 C11 C10 119.3(3) . . ?
C11 C12 C13 119.1(4) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
C14 C13 C12 117.9(4) . . ?
C14 C13 H13 121.1 . . ?
C12 C13 H13 121.1 . . ?
C15 C14 C13 118.9(4) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
N4 C15 C14 123.9(4) . . ?
N4 C15 H15 118.1 . . ?
C14 C15 H15 118.1 . . ?
N5 C16 C17 123.7(4) . . ?
N5 C16 H16 118.1 . . ?
C17 C16 H16 118.1 . . ?
C16 C17 C18 118.0(4) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 H17 121.0 . . ?
C19 C18 C17 119.1(4) . . ?
C19 C18 H18 120.5 . . ?
C17 C18 H18 120.5 . . ?
C18 C19 C20 118.9(4) . . ?
C18 C19 H19 120.6 . . ?
C20 C19 H19 120.6 . . ?
N5 C20 C19 123.4(4) . . ?
N5 C20 C21 117.3(3) . . ?
C19 C20 C21 119.2(3) . . ?
N6 C21 C20 112.9(3) . . ?
N6 C21 H21A 109.0 . . ?
C20 C21 H21A 109.0 . . ?
N6 C21 H21B 109.0 . . ?
C20 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
N6 C22 N7 107.9(3) . . ?
N6 C22 H22 126.1 . . ?
N7 C22 H22 126.1 . . ?
C24 C23 N6 107.1(3) . . ?
C24 C23 H23 126.5 . . ?
N6 C23 H23 126.5 . . ?
C23 C24 N7 106.7(3) . . ?
C23 C24 H24 126.7 . . ?
N7 C24 H24 126.7 . . ?
N7 C25 C26 113.0(3) . . ?
N7 C25 H25A 109.0 . . ?
C26 C25 H25A 109.0 . . ?
N7 C25 H25B 109.0 . . ?
C26 C25 H25B 109.0 . . ?
H25A C25 H25B 107.8 . . ?
N8 C26 C27 122.7(4) . . ?
N8 C26 C25 118.3(3) . . ?
C27 C26 C25 119.0(4) . . ?
C28 C27 C26 119.1(4) . . ?
C28 C27 H27 120.5 . . ?
C26 C27 H27 120.5 . . ?
C27 C28 C29 118.7(4) . . ?
C27 C28 H28 120.6 . . ?
C29 C28 H28 120.6 . . ?
C30 C29 C28 118.4(4) . . ?
C30 C29 H29 120.8 . . ?
C28 C29 H29 120.8 . . ?
N8 C30 C29 123.9(4) . . ?
N8 C30 H30 118.0 . . ?
C29 C30 H30 118.0 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        28.70
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.829
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.089
####################################################################### 
# 
# 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_e:\mrc055\mrc055
_database_code_depnum_ccdc_archive 'CCDC 1405829'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        7e
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H26 N6 Pd, 2(F6 P)'
_chemical_formula_sum            'C24 H26 F12 N6 P2 Pd'
_chemical_formula_weight         794.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   8.1012(3)
_cell_length_b                   10.9063(4)
_cell_length_c                   16.9064(7)
_cell_angle_alpha                96.373(3)
_cell_angle_beta                 98.659(3)
_cell_angle_gamma                97.265(3)
_cell_volume                     1451.93(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    99.9(4)
_cell_measurement_reflns_used    6910
_cell_measurement_theta_min      3.7380
_cell_measurement_theta_max      30.7200

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9118
_exptl_absorpt_correction_T_max  0.9748
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;
_diffrn_ambient_temperature      99.9(4)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            14671
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0555
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         28.28
_reflns_number_total             7152
_reflns_number_gt                6083
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28e (release 10-06-2013 CrysAlis171 .NET)
(compiled Jun 10 2013,11:58:50)
;
_computing_structure_solution    
;
SHELXS-97 (Sheldrick, G. M.    Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_structure_refinement  
;
SHELXS-97 (Sheldrick, G. M.    Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_molecular_graphics    'ORTEP-III Version 1.08 (Farrugia, 2005)'
_computing_publication_material  
;
enCIFer: A program for viewing, editing and visualising CIFs.
F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler,
J. Applied Cryst., 37, 331-334, 2004
;
_refine_special_details          
;
All H atoms were placed in calculated positions and refined using a riding model. C-H distances: CH2 0.99Α, aromatic 0.95Α.

All Uiso(H) values were constrained to be 1.2 times Ueq of the parent atom.

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0312P)²+1.6538P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7152
_refine_ls_number_parameters     406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0835
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.88864(3) 0.291095(19) 0.238762(13) 0.01245(7) Uani 1 1 d . . .
P1 P 0.24169(10) 0.64257(8) 0.42160(5) 0.02172(18) Uani 1 1 d . . .
P2 P 0.31142(11) 0.77701(9) 0.04260(5) 0.0273(2) Uani 1 1 d . . .
F3 F 0.3870(3) 0.5778(3) 0.46923(16) 0.0608(8) Uani 1 1 d . . .
F1 F 0.3554(4) 0.6613(3) 0.35437(17) 0.0742(10) Uani 1 1 d . . .
F4 F 0.3229(3) 0.7762(2) 0.46931(15) 0.0475(6) Uani 1 1 d . . .
F10 F 0.3692(3) 0.64316(19) 0.03152(12) 0.0363(5) Uani 1 1 d . . .
F11 F 0.5051(3) 0.8388(2) 0.07055(14) 0.0435(6) Uani 1 1 d . . .
F12 F 0.2930(3) 0.7620(2) 0.13448(12) 0.0438(6) Uani 1 1 d . . .
F5 F 0.0946(4) 0.7019(2) 0.37554(16) 0.0626(8) Uani 1 1 d . . .
F2 F 0.1598(2) 0.50814(17) 0.37384(11) 0.0260(4) Uani 1 1 d . . .
F9 F 0.3277(3) 0.79232(19) -0.04915(12) 0.0326(5) Uani 1 1 d . . .
F7 F 0.2575(3) 0.9142(2) 0.05387(14) 0.0477(6) Uani 1 1 d . . .
F6 F 0.1340(3) 0.61875(19) 0.49096(13) 0.0401(5) Uani 1 1 d . . .
F8 F 0.1196(3) 0.7193(2) 0.01381(14) 0.0482(6) Uani 1 1 d . . .
C17 C 1.0393(4) -0.0447(3) 0.3032(2) 0.0229(7) Uani 1 1 d . . .
H17 H 1.0637 -0.1050 0.3380 0.027 Uiso 1 1 calc R . .
N5 N 1.0076(3) 0.0569(2) 0.19929(15) 0.0163(5) Uani 1 1 d . . .
N1 N 0.5500(3) 0.1760(2) 0.27804(15) 0.0157(5) Uani 1 1 d . . .
N4 N 0.9763(3) 0.0655(2) 0.32332(15) 0.0170(5) Uani 1 1 d . . .
C9 C 0.7247(4) 0.6555(3) 0.2583(2) 0.0210(6) Uani 1 1 d . . .
H9 H 0.6872 0.7072 0.2990 0.025 Uiso 1 1 calc R . .
N6 N 1.0994(3) 0.3163(2) 0.18136(14) 0.0155(5) Uani 1 1 d . . .
N3 N 0.8207(3) 0.4650(2) 0.21572(14) 0.0142(5) Uani 1 1 d . . .
N2 N 0.6365(3) 0.3650(2) 0.33164(15) 0.0149(5) Uani 1 1 d . . .
C11 C 0.7961(4) 0.6199(3) 0.1269(2) 0.0221(7) Uani 1 1 d . . .
H11 H 0.8065 0.6457 0.0758 0.027 Uiso 1 1 calc R . .
C10 C 0.7412(4) 0.6963(3) 0.1854(2) 0.0231(7) Uani 1 1 d . . .
H10 H 0.7152 0.7762 0.1753 0.028 Uiso 1 1 calc R . .
C14 C 1.1380(4) 0.1406(3) 0.4565(2) 0.0290(8) Uani 1 1 d . . .
H14 H 1.1984 0.0727 0.4648 0.035 Uiso 1 1 calc R . .
C21 C 1.2746(4) 0.2365(3) 0.0926(2) 0.0238(7) Uani 1 1 d . . .
H21 H 1.3001 0.1688 0.0584 0.029 Uiso 1 1 calc R . .
C24 C 1.1994(4) 0.4264(3) 0.19327(18) 0.0179(6) Uani 1 1 d . . .
H24 H 1.1745 0.4921 0.2294 0.021 Uiso 1 1 calc R . .
C22 C 1.3756(4) 0.3520(3) 0.1040(2) 0.0249(7) Uani 1 1 d . . .
H22 H 1.4698 0.3644 0.0769 0.030 Uiso 1 1 calc R . .
C15 C 0.9642(4) 0.1139(3) 0.40660(19) 0.0217(7) Uani 1 1 d . . .
H15A H 0.8922 0.0518 0.4297 0.026 Uiso 1 1 calc R . .
H15B H 0.9120 0.1913 0.4070 0.026 Uiso 1 1 calc R . .
C18 C 1.0592(4) -0.0498(3) 0.2258(2) 0.0207(7) Uani 1 1 d . . .
H18 H 1.1006 -0.1140 0.1952 0.025 Uiso 1 1 calc R . .
C3 C 0.5351(4) 0.0511(3) 0.2339(2) 0.0209(6) Uani 1 1 d . . .
H3A H 0.6345 0.0460 0.2067 0.025 Uiso 1 1 calc R . .
H3B H 0.4334 0.0372 0.1916 0.025 Uiso 1 1 calc R . .
C8 C 0.7630(3) 0.5384(3) 0.27225(18) 0.0151(6) Uani 1 1 d . . .
C23 C 1.3380(4) 0.4483(3) 0.15490(19) 0.0221(7) Uani 1 1 d . . .
H23 H 1.4054 0.5280 0.1635 0.027 Uiso 1 1 calc R . .
C13 C 1.2093(5) 0.2517(4) 0.4885(2) 0.0374(9) Uani 1 1 d . . .
H13A H 1.1515 0.3212 0.4810 0.045 Uiso 1 1 calc R . .
H13B H 1.3194 0.2637 0.5195 0.045 Uiso 1 1 calc R . .
C19 C 1.0203(4) 0.0991(3) 0.12044(18) 0.0198(6) Uani 1 1 d . . .
H19A H 0.9070 0.1096 0.0931 0.024 Uiso 1 1 calc R . .
H19B H 1.0640 0.0355 0.0860 0.024 Uiso 1 1 calc R . .
C4 C 0.6811(3) 0.2677(3) 0.28732(17) 0.0144(6) Uani 1 1 d . . .
C2 C 0.5234(4) -0.0497(3) 0.2865(2) 0.0263(7) Uani 1 1 d . . .
H2 H 0.5002 -0.1332 0.2603 0.032 Uiso 1 1 calc R . .
C1 C 0.5421(4) -0.0339(3) 0.3664(2) 0.0318(8) Uani 1 1 d . . .
H1A H 0.5653 0.0478 0.3954 0.038 Uiso 1 1 calc R . .
H1B H 0.5322 -0.1043 0.3947 0.038 Uiso 1 1 calc R . .
C12 C 0.8355(4) 0.5051(3) 0.14444(18) 0.0189(6) Uani 1 1 d . . .
H12 H 0.8745 0.4527 0.1047 0.023 Uiso 1 1 calc R . .
C5 C 0.4226(4) 0.2165(3) 0.31591(19) 0.0191(6) Uani 1 1 d . . .
H5 H 0.3171 0.1690 0.3181 0.023 Uiso 1 1 calc R . .
C6 C 0.4759(4) 0.3351(3) 0.34881(18) 0.0185(6) Uani 1 1 d . . .
H6 H 0.4153 0.3881 0.3781 0.022 Uiso 1 1 calc R . .
C20 C 1.1367(4) 0.2210(3) 0.13152(18) 0.0173(6) Uani 1 1 d . . .
C16 C 0.9566(3) 0.1281(3) 0.25915(18) 0.0151(6) Uani 1 1 d . . .
C7 C 0.7409(4) 0.4872(3) 0.34948(18) 0.0171(6) Uani 1 1 d . . .
H7A H 0.8526 0.4797 0.3801 0.021 Uiso 1 1 calc R . .
H7B H 0.6866 0.5449 0.3832 0.021 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C16 1.977(3) . ?
Pd1 C4 1.979(3) . ?
Pd1 N6 2.091(2) . ?
Pd1 N3 2.101(2) . ?
P1 F5 1.573(2) . ?
P1 F1 1.582(2) . ?
P1 F6 1.588(2) . ?
P1 F4 1.595(2) . ?
P1 F2 1.604(2) . ?
P1 F3 1.607(2) . ?
P2 F8 1.583(2) . ?
P2 F10 1.589(2) . ?
P2 F9 1.602(2) . ?
P2 F11 1.606(2) . ?
P2 F12 1.607(2) . ?
P2 F7 1.610(2) . ?
C17 C18 1.338(5) . ?
C17 N4 1.391(4) . ?
C17 H17 0.9500 . ?
N5 C16 1.353(4) . ?
N5 C18 1.383(4) . ?
N5 C19 1.471(4) . ?
N1 C4 1.342(4) . ?
N1 C5 1.386(4) . ?
N1 C3 1.460(4) . ?
N4 C16 1.345(4) . ?
N4 C15 1.470(4) . ?
C9 C10 1.376(5) . ?
C9 C8 1.388(4) . ?
C9 H9 0.9500 . ?
N6 C24 1.338(4) . ?
N6 C20 1.357(4) . ?
N3 C12 1.344(4) . ?
N3 C8 1.354(4) . ?
N2 C4 1.349(4) . ?
N2 C6 1.382(4) . ?
N2 C7 1.460(4) . ?
C11 C10 1.383(5) . ?
C11 C12 1.384(4) . ?
C11 H11 0.9500 . ?
C10 H10 0.9500 . ?
C14 C13 1.295(5) . ?
C14 C15 1.504(4) . ?
C14 H14 0.9500 . ?
C21 C20 1.381(4) . ?
C21 C22 1.390(5) . ?
C21 H21 0.9500 . ?
C24 C23 1.387(4) . ?
C24 H24 0.9500 . ?
C22 C23 1.377(5) . ?
C22 H22 0.9500 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C18 H18 0.9500 . ?
C3 C2 1.492(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C8 C7 1.502(4) . ?
C23 H23 0.9500 . ?
C13 H13A 0.9500 . ?
C13 H13B 0.9500 . ?
C19 C20 1.506(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C2 C1 1.326(5) . ?
C2 H2 0.9500 . ?
C1 H1A 0.9500 . ?
C1 H1B 0.9500 . ?
C12 H12 0.9500 . ?
C5 C6 1.340(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C16 Pd1 C4 95.25(11) . . ?
C16 Pd1 N6 86.22(10) . . ?
C4 Pd1 N6 176.83(10) . . ?
C16 Pd1 N3 178.77(11) . . ?
C4 Pd1 N3 85.97(10) . . ?
N6 Pd1 N3 92.55(9) . . ?
F5 P1 F1 92.81(18) . . ?
F5 P1 F6 90.17(15) . . ?
F1 P1 F6 176.92(17) . . ?
F5 P1 F4 90.32(14) . . ?
F1 P1 F4 90.75(13) . . ?
F6 P1 F4 90.02(12) . . ?
F5 P1 F2 89.69(12) . . ?
F1 P1 F2 89.41(12) . . ?
F6 P1 F2 89.81(11) . . ?
F4 P1 F2 179.84(14) . . ?
F5 P1 F3 177.87(16) . . ?
F1 P1 F3 88.68(18) . . ?
F6 P1 F3 88.32(14) . . ?
F4 P1 F3 91.18(14) . . ?
F2 P1 F3 88.79(12) . . ?
F8 P2 F10 91.58(14) . . ?
F8 P2 F9 89.19(12) . . ?
F10 P2 F9 90.26(11) . . ?
F8 P2 F11 178.40(14) . . ?
F10 P2 F11 89.71(12) . . ?
F9 P2 F11 89.85(12) . . ?
F8 P2 F12 90.29(13) . . ?
F10 P2 F12 90.11(11) . . ?
F9 P2 F12 179.37(12) . . ?
F11 P2 F12 90.67(13) . . ?
F8 P2 F7 89.75(14) . . ?
F10 P2 F7 178.61(15) . . ?
F9 P2 F7 89.35(12) . . ?
F11 P2 F7 88.96(13) . . ?
F12 P2 F7 90.29(12) . . ?
C18 C17 N4 107.3(3) . . ?
C18 C17 H17 126.3 . . ?
N4 C17 H17 126.3 . . ?
C16 N5 C18 110.9(3) . . ?
C16 N5 C19 122.0(2) . . ?
C18 N5 C19 126.8(2) . . ?
C4 N1 C5 110.1(2) . . ?
C4 N1 C3 127.0(2) . . ?
C5 N1 C3 122.8(3) . . ?
C16 N4 C17 110.2(3) . . ?
C16 N4 C15 125.8(2) . . ?
C17 N4 C15 123.1(3) . . ?
C10 C9 C8 119.7(3) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C24 N6 C20 119.1(3) . . ?
C24 N6 Pd1 120.49(19) . . ?
C20 N6 Pd1 120.4(2) . . ?
C12 N3 C8 119.1(2) . . ?
C12 N3 Pd1 120.05(19) . . ?
C8 N3 Pd1 120.82(19) . . ?
C4 N2 C6 110.6(2) . . ?
C4 N2 C7 122.5(2) . . ?
C6 N2 C7 126.6(2) . . ?
C10 C11 C12 118.5(3) . . ?
C10 C11 H11 120.8 . . ?
C12 C11 H11 120.8 . . ?
C9 C10 C11 119.4(3) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C13 C14 C15 123.2(3) . . ?
C13 C14 H14 118.4 . . ?
C15 C14 H14 118.4 . . ?
C20 C21 C22 119.4(3) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
N6 C24 C23 122.5(3) . . ?
N6 C24 H24 118.8 . . ?
C23 C24 H24 118.8 . . ?
C23 C22 C21 119.4(3) . . ?
C23 C22 H22 120.3 . . ?
C21 C22 H22 120.3 . . ?
N4 C15 C14 109.3(2) . . ?
N4 C15 H15A 109.8 . . ?
C14 C15 H15A 109.8 . . ?
N4 C15 H15B 109.8 . . ?
C14 C15 H15B 109.8 . . ?
H15A C15 H15B 108.3 . . ?
C17 C18 N5 106.4(3) . . ?
C17 C18 H18 126.8 . . ?
N5 C18 H18 126.8 . . ?
N1 C3 C2 113.3(3) . . ?
N1 C3 H3A 108.9 . . ?
C2 C3 H3A 108.9 . . ?
N1 C3 H3B 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
N3 C8 C9 120.8(3) . . ?
N3 C8 C7 117.2(2) . . ?
C9 C8 C7 121.9(3) . . ?
C22 C23 C24 118.5(3) . . ?
C22 C23 H23 120.7 . . ?
C24 C23 H23 120.7 . . ?
C14 C13 H13A 120.0 . . ?
C14 C13 H13B 120.0 . . ?
H13A C13 H13B 120.0 . . ?
N5 C19 C20 110.1(2) . . ?
N5 C19 H19A 109.6 . . ?
C20 C19 H19A 109.6 . . ?
N5 C19 H19B 109.6 . . ?
C20 C19 H19B 109.6 . . ?
H19A C19 H19B 108.2 . . ?
N1 C4 N2 105.5(2) . . ?
N1 C4 Pd1 134.0(2) . . ?
N2 C4 Pd1 119.7(2) . . ?
C1 C2 C3 126.2(3) . . ?
C1 C2 H2 116.9 . . ?
C3 C2 H2 116.9 . . ?
C2 C1 H1A 120.0 . . ?
C2 C1 H1B 120.0 . . ?
H1A C1 H1B 120.0 . . ?
N3 C12 C11 122.4(3) . . ?
N3 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
C6 C5 N1 107.3(3) . . ?
C6 C5 H5 126.3 . . ?
N1 C5 H5 126.3 . . ?
C5 C6 N2 106.4(3) . . ?
C5 C6 H6 126.8 . . ?
N2 C6 H6 126.8 . . ?
N6 C20 C21 121.1(3) . . ?
N6 C20 C19 116.9(3) . . ?
C21 C20 C19 122.0(3) . . ?
N4 C16 N5 105.2(2) . . ?
N4 C16 Pd1 135.6(2) . . ?
N5 C16 Pd1 119.1(2) . . ?
N2 C7 C8 109.8(2) . . ?
N2 C7 H7A 109.7 . . ?
C8 C7 H7A 109.7 . . ?
N2 C7 H7B 109.7 . . ?
C8 C7 H7B 109.7 . . ?
H7A C7 H7B 108.2 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 C17 N4 C16 0.2(3) . . . . ?
C18 C17 N4 C15 -169.7(3) . . . . ?
C16 Pd1 N6 C24 -137.4(2) . . . . ?
C4 Pd1 N6 C24 104.8(19) . . . . ?
N3 Pd1 N6 C24 42.6(2) . . . . ?
C16 Pd1 N6 C20 42.5(2) . . . . ?
C4 Pd1 N6 C20 -75.2(19) . . . . ?
N3 Pd1 N6 C20 -137.4(2) . . . . ?
C16 Pd1 N3 C12 37(5) . . . . ?
C4 Pd1 N3 C12 -137.5(2) . . . . ?
N6 Pd1 N3 C12 39.7(2) . . . . ?
C16 Pd1 N3 C8 -142(5) . . . . ?
C4 Pd1 N3 C8 43.0(2) . . . . ?
N6 Pd1 N3 C8 -139.8(2) . . . . ?
C8 C9 C10 C11 -0.1(5) . . . . ?
C12 C11 C10 C9 -1.1(5) . . . . ?
C20 N6 C24 C23 1.7(4) . . . . ?
Pd1 N6 C24 C23 -178.3(2) . . . . ?
C20 C21 C22 C23 1.0(5) . . . . ?
C16 N4 C15 C14 -106.6(3) . . . . ?
C17 N4 C15 C14 61.6(4) . . . . ?
C13 C14 C15 N4 115.3(4) . . . . ?
N4 C17 C18 N5 -0.3(3) . . . . ?
C16 N5 C18 C17 0.2(3) . . . . ?
C19 N5 C18 C17 174.0(3) . . . . ?
C4 N1 C3 C2 116.1(3) . . . . ?
C5 N1 C3 C2 -65.2(4) . . . . ?
C12 N3 C8 C9 -2.1(4) . . . . ?
Pd1 N3 C8 C9 177.3(2) . . . . ?
C12 N3 C8 C7 177.2(2) . . . . ?
Pd1 N3 C8 C7 -3.3(3) . . . . ?
C10 C9 C8 N3 1.7(4) . . . . ?
C10 C9 C8 C7 -177.6(3) . . . . ?
C21 C22 C23 C24 0.0(4) . . . . ?
N6 C24 C23 C22 -1.4(4) . . . . ?
C16 N5 C19 C20 57.0(3) . . . . ?
C18 N5 C19 C20 -116.1(3) . . . . ?
C5 N1 C4 N2 0.6(3) . . . . ?
C3 N1 C4 N2 179.5(3) . . . . ?
C5 N1 C4 Pd1 -169.0(2) . . . . ?
C3 N1 C4 Pd1 9.9(4) . . . . ?
C6 N2 C4 N1 -1.2(3) . . . . ?
C7 N2 C4 N1 -174.9(2) . . . . ?
C6 N2 C4 Pd1 170.23(19) . . . . ?
C7 N2 C4 Pd1 -3.5(3) . . . . ?
C16 Pd1 C4 N1 -50.3(3) . . . . ?
N6 Pd1 C4 N1 67.2(19) . . . . ?
N3 Pd1 C4 N1 129.5(3) . . . . ?
C16 Pd1 C4 N2 141.2(2) . . . . ?
N6 Pd1 C4 N2 -101.3(19) . . . . ?
N3 Pd1 C4 N2 -38.9(2) . . . . ?
N1 C3 C2 C1 -7.2(5) . . . . ?
C8 N3 C12 C11 0.9(4) . . . . ?
Pd1 N3 C12 C11 -178.6(2) . . . . ?
C10 C11 C12 N3 0.7(5) . . . . ?
C4 N1 C5 C6 0.2(3) . . . . ?
C3 N1 C5 C6 -178.7(3) . . . . ?
N1 C5 C6 N2 -0.9(3) . . . . ?
C4 N2 C6 C5 1.3(3) . . . . ?
C7 N2 C6 C5 174.7(3) . . . . ?
C24 N6 C20 C21 -0.6(4) . . . . ?
Pd1 N6 C20 C21 179.4(2) . . . . ?
C24 N6 C20 C19 179.9(2) . . . . ?
Pd1 N6 C20 C19 -0.1(3) . . . . ?
C22 C21 C20 N6 -0.7(4) . . . . ?
C22 C21 C20 C19 178.8(3) . . . . ?
N5 C19 C20 N6 -55.6(3) . . . . ?
N5 C19 C20 C21 124.9(3) . . . . ?
C17 N4 C16 N5 -0.1(3) . . . . ?
C15 N4 C16 N5 169.5(3) . . . . ?
C17 N4 C16 Pd1 -175.9(2) . . . . ?
C15 N4 C16 Pd1 -6.3(5) . . . . ?
C18 N5 C16 N4 -0.1(3) . . . . ?
C19 N5 C16 N4 -174.2(2) . . . . ?
C18 N5 C16 Pd1 176.5(2) . . . . ?
C19 N5 C16 Pd1 2.5(4) . . . . ?
C4 Pd1 C16 N4 -50.5(3) . . . . ?
N6 Pd1 C16 N4 132.3(3) . . . . ?
N3 Pd1 C16 N4 135(5) . . . . ?
C4 Pd1 C16 N5 134.1(2) . . . . ?
N6 Pd1 C16 N5 -43.0(2) . . . . ?
N3 Pd1 C16 N5 -41(5) . . . . ?
C4 N2 C7 C8 60.1(3) . . . . ?
C6 N2 C7 C8 -112.6(3) . . . . ?
N3 C8 C7 N2 -53.1(3) . . . . ?
C9 C8 C7 N2 126.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        28.28
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.106
####################################################################### 
# 
# 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_mrc99_mo
_database_code_depnum_ccdc_archive 'CCDC 1405831'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_audit_creation_date             2014-06-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_chemical_name_common            ?
_chemical_name_systematic        4d
_chemical_formula_moiety         'C12 H13 Br2 N3 O Pd'
_chemical_formula_sum            'C12 H13 Br2 N3 O Pd'
_chemical_formula_weight         481.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C48 H52 Br8 N12 O4 Pd4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.5090(8)
_cell_length_b                   7.9393(3)
_cell_length_c                   13.9341(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.376(6)
_cell_angle_gamma                90.00
_cell_volume                     1418.25(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1953
_cell_measurement_temperature    120.01(11)
_cell_measurement_theta_max      26.6150
_cell_measurement_theta_min      3.6600
_exptl_absorpt_coefficient_mu    6.937
_exptl_absorpt_correction_T_max  0.761
_exptl_absorpt_correction_T_min  0.510
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_unetI/netI     0.0789
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8045
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.15
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0350740000
_diffrn_orient_matrix_UB_12      0.0077306000
_diffrn_orient_matrix_UB_13      -0.0283626000
_diffrn_orient_matrix_UB_21      -0.0145629000
_diffrn_orient_matrix_UB_22      0.0856391000
_diffrn_orient_matrix_UB_23      -0.0100380000
_diffrn_orient_matrix_UB_31      0.0401992000
_diffrn_orient_matrix_UB_32      0.0244159000
_diffrn_orient_matrix_UB_33      0.0444159000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2195
_reflns_number_total             2885
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.451
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.212
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2885
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0569
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0470P)²+8.5887P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1280
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C14(H14), C15(H15), C17(H17)
2.c X=CH2 refined with riding coordinates:
 C11(H11A,H11B)
2.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Pd1 Pd 0.00146(5) 0.07337(7) 0.31932(4) 0.01615(19) Uani 1 d . . .
Br2 Br 0.02868(8) -0.04365(13) 0.16944(7) 0.0349(3) Uani 1 d . . .
Br3 Br -0.18015(7) -0.02997(11) 0.25715(7) 0.0287(3) Uani 1 d . . .
C4 C 0.1469(6) 0.1519(10) 0.3893(6) 0.0163(16) Uani 1 d . . .
N5 N 0.2437(5) 0.1510(8) 0.3838(5) 0.0184(15) Uani 1 d . . .
C6 C 0.3108(7) 0.2368(11) 0.4640(6) 0.027(2) Uani 1 d . . .
H6 H 0.3816 0.2535 0.4750 0.033 Uiso 1 calc . . R
C7 C 0.2565(6) 0.2927(10) 0.5241(6) 0.0213(18) Uani 1 d . . .
H7 H 0.2818 0.3534 0.5839 0.026 Uiso 1 calc . . R
N8 N 0.1534(5) 0.2392(8) 0.4767(5) 0.0184(15) Uani 1 d . . .
C9 C 0.2826(6) 0.0643(11) 0.3099(6) 0.0238(19) Uani 1 d . . .
H9A H 0.3298 0.1385 0.2900 0.029 Uiso 1 calc . . R
H9B H 0.2244 0.0390 0.2500 0.029 Uiso 1 calc . . R
C10 C 0.3393(6) -0.0979(11) 0.3516(7) 0.0235(19) Uani 1 d . . .
H10 H 0.3633 -0.1613 0.3073 0.028 Uiso 1 calc . . R
C11 C 0.3583(7) -0.1589(12) 0.4438(7) 0.034(2) Uani 1 d . . .
H11A H 0.3360 -0.1005 0.4911 0.041 Uiso 1 calc . . R
H11B H 0.3939 -0.2602 0.4615 0.041 Uiso 1 calc . . R
C12 C 0.0650(6) 0.2647(9) 0.5065(6) 0.0149(16) Uani 1 d . . .
N13 N -0.0217(5) 0.1959(8) 0.4405(5) 0.0191(15) Uani 1 d . . .
C14 C -0.1126(6) 0.2237(10) 0.4603(6) 0.0223(19) Uani 1 d . . .
H14 H -0.1741 0.1827 0.4149 0.027 Uiso 1 calc . . R
C15 C -0.1180(6) 0.3095(11) 0.5440(6) 0.0241(19) Uani 1 d . . .
H15 H -0.1819 0.3250 0.5548 0.029 Uiso 1 calc . . R
C16 C -0.0264(6) 0.3735(10) 0.6131(6) 0.0182(17) Uani 1 d . . .
C17 C 0.0676(6) 0.3520(10) 0.5932(6) 0.0164(16) Uani 1 d . . .
H17 H 0.1298 0.3947 0.6365 0.020 Uiso 1 calc . . R
O18 O -0.0364(4) 0.4537(7) 0.6937(4) 0.0243(13) Uani 1 d . . .
C19 C 0.0580(6) 0.4955(12) 0.7727(6) 0.0248(19) Uani 1 d . . .
H19A H 0.0913 0.5890 0.7517 0.037 Uiso 1 calc . . GR
H19B H 0.1040 0.4002 0.7864 0.037 Uiso 1 calc . . GR
H19C H 0.0417 0.5254 0.8327 0.037 Uiso 1 calc . . GR


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Br2 2.4175(11) . ?
Pd1 Br3 2.4703(10) . ?
Pd1 C4 1.998(8) . ?
Pd1 N13 2.057(7) . ?
C4 N5 1.334(10) . ?
C4 N8 1.380(10) . ?
N5 C6 1.377(10) . ?
N5 C9 1.467(10) . ?
C6 H6 0.9300 . ?
C6 C7 1.350(12) . ?
C7 H7 0.9300 . ?
C7 N8 1.406(10) . ?
N8 C12 1.396(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.517(12) . ?
C10 H10 0.9300 . ?
C10 C11 1.321(12) . ?
C11 H11A 0.9300 . ?
C11 H11B 0.9300 . ?
C12 N13 1.355(10) . ?
C12 C17 1.384(11) . ?
N13 C14 1.359(10) . ?
C14 H14 0.9300 . ?
C14 C15 1.372(12) . ?
C15 H15 0.9300 . ?
C15 C16 1.403(11) . ?
C16 C17 1.393(11) . ?
C16 O18 1.334(10) . ?
C17 H17 0.9300 . ?
O18 C19 1.436(10) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pd1 Br3 88.52(4) . . ?
C4 Pd1 Br2 98.5(2) . . ?
C4 Pd1 Br3 171.9(2) . . ?
C4 Pd1 N13 80.3(3) . . ?
N13 Pd1 Br2 174.36(18) . . ?
N13 Pd1 Br3 93.08(18) . . ?
N5 C4 Pd1 143.3(6) . . ?
N5 C4 N8 105.3(6) . . ?
N8 C4 Pd1 111.5(5) . . ?
C4 N5 C6 110.9(7) . . ?
C4 N5 C9 128.1(6) . . ?
C6 N5 C9 120.8(7) . . ?
N5 C6 H6 125.7 . . ?
C7 C6 N5 108.6(7) . . ?
C7 C6 H6 125.7 . . ?
C6 C7 H7 127.4 . . ?
C6 C7 N8 105.2(7) . . ?
N8 C7 H7 127.4 . . ?
C4 N8 C7 110.1(7) . . ?
C4 N8 C12 120.9(6) . . ?
C12 N8 C7 129.1(7) . . ?
N5 C9 H9A 109.2 . . ?
N5 C9 H9B 109.2 . . ?
N5 C9 C10 112.3(7) . . ?
H9A C9 H9B 107.9 . . ?
C10 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C9 C10 H10 116.4 . . ?
C11 C10 C9 127.1(8) . . ?
C11 C10 H10 116.4 . . ?
C10 C11 H11A 120.0 . . ?
C10 C11 H11B 120.0 . . ?
H11A C11 H11B 120.0 . . ?
N13 C12 N8 112.2(6) . . ?
N13 C12 C17 125.0(7) . . ?
C17 C12 N8 122.9(7) . . ?
C12 N13 Pd1 115.2(5) . . ?
C12 N13 C14 116.1(7) . . ?
C14 N13 Pd1 128.6(5) . . ?
N13 C14 H14 118.4 . . ?
N13 C14 C15 123.1(8) . . ?
C15 C14 H14 118.4 . . ?
C14 C15 H15 120.3 . . ?
C14 C15 C16 119.4(8) . . ?
C16 C15 H15 120.3 . . ?
C17 C16 C15 118.8(7) . . ?
O18 C16 C15 116.7(7) . . ?
O18 C16 C17 124.5(7) . . ?
C12 C17 C16 117.5(7) . . ?
C12 C17 H17 121.3 . . ?
C16 C17 H17 121.3 . . ?
C16 O18 C19 117.0(6) . . ?
O18 C19 H19A 109.5 . . ?
O18 C19 H19B 109.5 . . ?
O18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 C4 N5 C6 179.8(8) . . . . ?
Pd1 C4 N5 C9 -4.4(15) . . . . ?
Pd1 C4 N8 C7 180.0(5) . . . . ?
Pd1 C4 N8 C12 -0.5(8) . . . . ?
Pd1 N13 C14 C15 -179.3(6) . . . . ?
Br2 Pd1 C4 N5 -5.6(10) . . . . ?
Br2 Pd1 C4 N8 175.1(5) . . . . ?
Br2 Pd1 N13 C12 -79.3(19) . . . . ?
Br2 Pd1 N13 C14 97.1(18) . . . . ?
Br3 Pd1 C4 N5 143.4(11) . . . . ?
Br3 Pd1 C4 N8 -35.9(19) . . . . ?
Br3 Pd1 N13 C12 174.3(5) . . . . ?
Br3 Pd1 N13 C14 -9.3(7) . . . . ?
C4 Pd1 N13 C12 -0.8(5) . . . . ?
C4 Pd1 N13 C14 175.6(7) . . . . ?
C4 N5 C6 C7 1.0(10) . . . . ?
C4 N5 C9 C10 -100.6(9) . . . . ?
C4 N8 C12 N13 -0.2(10) . . . . ?
C4 N8 C12 C17 -179.7(7) . . . . ?
N5 C4 N8 C7 0.4(8) . . . . ?
N5 C4 N8 C12 180.0(7) . . . . ?
N5 C6 C7 N8 -0.6(9) . . . . ?
N5 C9 C10 C11 -2.6(12) . . . . ?
C6 N5 C9 C10 74.8(9) . . . . ?
C6 C7 N8 C4 0.1(9) . . . . ?
C6 C7 N8 C12 -179.4(7) . . . . ?
C7 N8 C12 N13 179.2(7) . . . . ?
C7 N8 C12 C17 -0.3(12) . . . . ?
N8 C4 N5 C6 -0.8(9) . . . . ?
N8 C4 N5 C9 174.9(7) . . . . ?
N8 C12 N13 Pd1 0.8(8) . . . . ?
N8 C12 N13 C14 -176.1(6) . . . . ?
N8 C12 C17 C16 178.1(7) . . . . ?
C9 N5 C6 C7 -175.2(7) . . . . ?
C12 N13 C14 C15 -2.9(11) . . . . ?
N13 Pd1 C4 N5 180.0(10) . . . . ?
N13 Pd1 C4 N8 0.7(5) . . . . ?
N13 C12 C17 C16 -1.3(11) . . . . ?
N13 C14 C15 C16 0.5(12) . . . . ?
C14 C15 C16 C17 1.7(12) . . . . ?
C14 C15 C16 O18 -179.1(7) . . . . ?
C15 C16 C17 C12 -1.3(11) . . . . ?
C15 C16 O18 C19 170.2(7) . . . . ?
C17 C12 N13 Pd1 -179.7(6) . . . . ?
C17 C12 N13 C14 3.4(11) . . . . ?
C17 C16 O18 C19 -10.8(11) . . . . ?
O18 C16 C17 C12 179.6(7) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
15 -2 7 0.0426 14.9910 -2.0013 7.0042 0.3117 -0.4600 0.8649
-15 2 -7 0.0426 -14.9910 2.0013 -7.0042 -0.3117 0.4600 -0.8649
6 11 -3 0.0594 5.9878 11.0069 -2.9997 0.3802 0.8855 0.3762
-6 -11 3 0.0594 -5.9878 -11.0069 2.9997 -0.3802 -0.8855 -0.3762
17 -1 -13 0.0214 16.9771 -0.9987 -12.9941 0.9563 -0.2023 0.0809
-17 1 13 0.0214 -16.9771 0.9987 12.9941 -0.9563 0.2023 -0.0809
0 7 14 0.0506 0.0050 7.0027 13.9981 -0.3427 0.4591 0.7929
-2 -2 -18 0.0459 -2.0077 -1.9995 -17.9992 0.4246 0.0387 -0.9290
2 3 17 0.0311 2.0067 3.0002 16.9991 -0.3886 0.0571 0.9089
2 -11 -1 0.0477 2.0025 -11.0062 -0.9977 0.0134 -0.9617 -0.2325

_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
####################################################################### 
# 
# 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_mrc100_mo
_database_code_depnum_ccdc_archive 'CCDC 1405832'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_audit_creation_date             2014-08-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_chemical_name_common            ?
_chemical_name_systematic        7f
_chemical_formula_moiety         'C30 H28 N8 Pd, 2(F6 P)'
_chemical_formula_sum            'C30 H28 F12 N8 P2 Pd'
_chemical_formula_weight         896.94
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C120 H112 F48 N32 P8 Pd4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   8.0821(4)
_cell_length_b                   20.5140(10)
_cell_length_c                   20.6555(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.704(4)
_cell_angle_gamma                90.00
_cell_volume                     3401.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4655
_cell_measurement_temperature    119.99(13)
_cell_measurement_theta_max      24.7990
_cell_measurement_theta_min      3.3970
_exptl_absorpt_coefficient_mu    0.743
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_av_unetI/netI     0.1003
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            31660
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.72
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   31.00   59.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000   30.0000 28

#__ type_ start__ end____ width___ exp.time_
  2 omega   -6.00   80.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000 -150.0000 86

#__ type_ start__ end____ width___ exp.time_
  3 omega  -20.00   16.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000 -150.0000 36

#__ type_ start__ end____ width___ exp.time_
  4 omega   54.00   83.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   37.0000   60.0000 29

#__ type_ start__ end____ width___ exp.time_
  5 omega  -27.00   32.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000   60.0000 59

#__ type_ start__ end____ width___ exp.time_
  6 omega  -28.00   24.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000  120.0000 52

#__ type_ start__ end____ width___ exp.time_
  7 omega   11.00   36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -57.0000    0.0000 25

#__ type_ start__ end____ width___ exp.time_
  8 omega   -8.00   17.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   57.0000   30.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0278782000
_diffrn_orient_matrix_UB_12      -0.0279914000
_diffrn_orient_matrix_UB_13      -0.0157337000
_diffrn_orient_matrix_UB_21      0.0631823000
_diffrn_orient_matrix_UB_22      0.0188787000
_diffrn_orient_matrix_UB_23      -0.0121039000
_diffrn_orient_matrix_UB_31      0.0551026000
_diffrn_orient_matrix_UB_32      -0.0074802000
_diffrn_orient_matrix_UB_33      0.0283122000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                5822
_reflns_number_total             8440
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max         1.761
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8440
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0731
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0368P)²+16.5313P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1464
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P2-F10B = P2-F7A = P2-F7B = P2-F8A = P2-F8B = P2-F9A = P2-F9B = P2-F10A
 1.58 with sigma of 0.01
 F9A-F10A
 2.25 with sigma of 0.02
 F10A-F7A
 2.25 with sigma of 0.02
 F7A-F8A
 2.25 with sigma of 0.02
 F8A-F9A
 2.25 with sigma of 0.02
 F9B-F10B
 2.25 with sigma of 0.02
 F10B-F7B
 2.25 with sigma of 0.02
 F7B-F8B
 2.25 with sigma of 0.02
 F8B-F9B
 2.25 with sigma of 0.02
3. Others
 Fixed Sof: F9A(0.7) F10A(0.7) F7A(0.7) F8A(0.7) F7B(0.3) F8B(0.3) F10B(0.3)
 F9B(0.3)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C10(H10A,H10B), C21(H21A,H21B), C6(H6A,H6B)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C14(H14), C2(H2), C9(H9), C18(H18), C8(H8), C27(H27), C16(H16),
 C17(H17), C19(H19), C4(H4), C28(H28), C23(H23), C1(H1), C24(H24), C13(H13),
 C3(H3), C30(H30), C29(H29), C12(H12)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Pd1 Pd 0.97484(5) 0.76307(2) 0.358493(19) 0.01621(11) Uani 1 d . . .
P1 P 1.3224(2) 0.63389(8) 0.56389(7) 0.0277(4) Uani 1 d . . .
P2 P 0.82079(19) 0.64696(7) 0.15501(7) 0.0255(3) Uani 1 d . . D
F4 F 1.4441(5) 0.6766(3) 0.52525(19) 0.0627(13) Uani 1 d . . .
F9A F 0.9430(7) 0.5868(3) 0.1446(3) 0.0474(14) Uiso 0.70 d A 1 D
F3 F 1.4621(7) 0.5797(2) 0.5732(2) 0.0818(17) Uani 1 d . . .
F5 F 1.4002(5) 0.66749(19) 0.63058(17) 0.0425(9) Uani 1 d . . .
F11 F 0.9501(5) 0.69525(17) 0.12831(16) 0.0363(9) Uani 1 d A . .
F1 F 1.1895(5) 0.6896(2) 0.5527(3) 0.0663(14) Uani 1 d . . .
F12 F 0.6908(5) 0.59781(18) 0.18208(19) 0.0427(9) Uani 1 d A . .
F10A F 0.7410(7) 0.6343(3) 0.0812(2) 0.0424(13) Uiso 0.70 d A 1 D
F2 F 1.2030(7) 0.5920(2) 0.60257(19) 0.0728(16) Uani 1 d . . .
F7A F 0.6964(8) 0.7047(3) 0.1591(3) 0.0671(19) Uiso 0.70 d A 1 D
F6 F 1.2436(5) 0.60010(19) 0.49765(17) 0.0475(10) Uani 1 d . . .
C15 C 0.7196(8) 1.0160(3) 0.2789(3) 0.0374(16) Uani 1 d . . .
H15 H 0.7154 1.0510 0.3073 0.045 Uiso 1 calc . . R
N4 N 0.6699(6) 0.9576(2) 0.2981(2) 0.0308(12) Uani 1 d . . .
N3 N 0.6365(5) 0.8299(2) 0.3471(2) 0.0201(10) Uani 1 d . . .
F8A F 0.9046(8) 0.6563(3) 0.2265(3) 0.0596(17) Uiso 0.70 d A 1 D
N1 N 0.9037(5) 0.6780(2) 0.4038(2) 0.0198(9) Uani 1 d . . .
N8 N 1.1307(6) 0.8629(2) 0.4860(2) 0.0266(11) Uani 1 d . . .
C14 C 0.7760(9) 1.0271(4) 0.2205(3) 0.0436(18) Uani 1 d . . .
H14 H 0.8050 1.0690 0.2090 0.052 Uiso 1 calc . . R
N6 N 1.1216(5) 0.8443(2) 0.26601(19) 0.0173(9) Uani 1 d . . .
N5 N 1.1974(5) 0.7239(2) 0.3324(2) 0.0185(9) Uani 1 d . . .
C2 C 0.8689(7) 0.5631(3) 0.4053(3) 0.0295(13) Uani 1 d . . .
H2 H 0.8766 0.5232 0.3844 0.035 Uiso 1 calc . . R
N7 N 1.0613(5) 0.9073(2) 0.3419(2) 0.0169(9) Uani 1 d . . .
C9 C 0.5124(7) 0.8416(3) 0.3867(3) 0.0279(13) Uani 1 d . . .
H9 H 0.4126 0.8634 0.3749 0.033 Uiso 1 calc . . R
N2 N 0.7193(5) 0.7890(2) 0.4405(2) 0.0210(10) Uani 1 d . . .
C18 C 1.4861(7) 0.6689(3) 0.2970(3) 0.0314(14) Uani 1 d . . .
H18 H 1.5817 0.6495 0.2847 0.038 Uiso 1 calc . . R
C25 C 1.0017(7) 0.9336(3) 0.4015(2) 0.0219(12) Uani 1 d . . .
H25A H 0.8976 0.9125 0.4082 0.026 Uiso 1 calc . . R
H25B H 0.9801 0.9798 0.3959 0.026 Uiso 1 calc . . R
C10 C 0.6221(7) 0.8426(3) 0.2769(3) 0.0242(12) Uani 1 d . . .
H10A H 0.5059 0.8384 0.2593 0.029 Uiso 1 calc . . R
H10B H 0.6839 0.8093 0.2566 0.029 Uiso 1 calc . . R
C8 C 0.5634(7) 0.8156(3) 0.4453(3) 0.0268(13) Uani 1 d . . .
H8 H 0.5057 0.8154 0.4817 0.032 Uiso 1 calc . . R
C21 C 1.1396(7) 0.7828(3) 0.2301(2) 0.0220(12) Uani 1 d . . .
H21A H 1.1912 0.7915 0.1909 0.026 Uiso 1 calc . . R
H21B H 1.0308 0.7638 0.2174 0.026 Uiso 1 calc . . R
C27 C 1.2225(7) 0.9746(3) 0.4872(3) 0.0294(13) Uani 1 d . . .
H27 H 1.2134 1.0159 0.4687 0.035 Uiso 1 calc . . R
C16 C 1.2944(7) 0.6868(3) 0.3744(3) 0.0235(12) Uani 1 d . . .
H16 H 1.2631 0.6797 0.4158 0.028 Uiso 1 calc . . R
C17 C 1.4402(7) 0.6587(3) 0.3583(3) 0.0288(13) Uani 1 d . . .
H17 H 1.5060 0.6333 0.3885 0.035 Uiso 1 calc . . R
C7 C 0.7645(6) 0.7982(2) 0.3807(2) 0.0173(11) Uani 1 d . . .
C19 C 1.3875(7) 0.7084(3) 0.2540(3) 0.0241(12) Uani 1 d . . .
H19 H 1.4168 0.7162 0.2124 0.029 Uiso 1 calc . . R
C4 C 0.7984(7) 0.6265(3) 0.4934(3) 0.0261(13) Uani 1 d . . .
H4 H 0.7597 0.6300 0.5339 0.031 Uiso 1 calc . . R
C28 C 1.3341(8) 0.9619(4) 0.5425(3) 0.0396(17) Uani 1 d . . .
H28 H 1.4026 0.9949 0.5613 0.048 Uiso 1 calc . . R
C23 C 1.1863(7) 0.9042(3) 0.2536(2) 0.0201(11) Uani 1 d . . .
H23 H 1.2453 0.9149 0.2191 0.024 Uiso 1 calc . . R
C1 C 0.9140(7) 0.6193(3) 0.3764(3) 0.0230(12) Uani 1 d . . .
H1 H 0.9535 0.6166 0.3360 0.028 Uiso 1 calc . . R
C24 C 1.1483(7) 0.9445(3) 0.3006(3) 0.0208(11) Uani 1 d . . .
H24 H 1.1747 0.9885 0.3049 0.025 Uiso 1 calc . . R
C13 C 0.7899(9) 0.9762(4) 0.1784(3) 0.0477(19) Uani 1 d . . .
H13 H 0.8295 0.9824 0.1384 0.057 Uiso 1 calc . . R
C6 C 0.8202(7) 0.7494(3) 0.4893(2) 0.0220(12) Uani 1 d . . .
H6A H 0.7655 0.7463 0.5285 0.026 Uiso 1 calc . . R
H6B H 0.9282 0.7696 0.5005 0.026 Uiso 1 calc . . R
C22 C 1.0463(6) 0.8450(3) 0.3207(2) 0.0181(11) Uani 1 d . . .
C26 C 1.1260(6) 0.9233(3) 0.4610(2) 0.0195(11) Uani 1 d . . .
C3 C 0.8117(8) 0.5660(3) 0.4657(3) 0.0308(14) Uani 1 d . . .
H3 H 0.7830 0.5284 0.4869 0.037 Uiso 1 calc . . R
C11 C 0.6832(7) 0.9081(3) 0.2579(3) 0.0238(12) Uani 1 d . . .
C5 C 0.8420(6) 0.6819(3) 0.4617(3) 0.0206(11) Uani 1 d . . .
C30 C 1.2386(7) 0.8532(3) 0.5395(3) 0.0314(14) Uani 1 d . . .
H30 H 1.2437 0.8118 0.5580 0.038 Uiso 1 calc . . R
C20 C 1.2454(6) 0.7363(3) 0.2730(2) 0.0203(11) Uani 1 d . . .
C29 C 1.3421(7) 0.9005(4) 0.5689(3) 0.0362(16) Uani 1 d . . .
H29 H 1.4157 0.8910 0.6058 0.043 Uiso 1 calc . . R
C12 C 0.7425(8) 0.9149(4) 0.1979(3) 0.0390(16) Uani 1 d . . .
H12 H 0.7504 0.8789 0.1711 0.047 Uiso 1 calc . . R
F7B F 0.7786(16) 0.7021(6) 0.2070(5) 0.052(4) Uiso 0.30 d A 2 D
F8B F 0.9662(13) 0.6267(6) 0.2108(5) 0.043(3) Uiso 0.30 d A 2 D
F10B F 0.6685(16) 0.6734(7) 0.1077(7) 0.073(5) Uiso 0.30 d A 2 D
F9B F 0.861(2) 0.5912(7) 0.1085(7) 0.083(5) Uiso 0.30 d A 2 D


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 2.093(4) . ?
Pd1 N5 2.097(4) . ?
Pd1 C7 1.950(5) . ?
Pd1 C22 1.969(5) . ?
P1 F4 1.599(4) . ?
P1 F3 1.580(5) . ?
P1 F5 1.602(4) . ?
P1 F1 1.567(4) . ?
P1 F2 1.577(4) . ?
P1 F6 1.598(4) . ?
P2 F9A 1.610(5) . ?
P2 F11 1.585(4) . ?
P2 F12 1.603(4) . ?
P2 F10A 1.606(5) . ?
P2 F7A 1.562(6) . ?
P2 F8A 1.562(5) . ?
P2 F7B 1.623(8) . ?
P2 F8B 1.602(8) . ?
P2 F10B 1.575(8) . ?
P2 F9B 1.552(8) . ?
C15 H15 0.9300 . ?
C15 N4 1.339(8) . ?
C15 C14 1.358(9) . ?
N4 C11 1.324(7) . ?
N3 C9 1.386(7) . ?
N3 C10 1.466(7) . ?
N3 C7 1.345(6) . ?
N1 C1 1.338(7) . ?
N1 C5 1.350(7) . ?
N8 C26 1.340(7) . ?
N8 C30 1.340(7) . ?
C14 H14 0.9300 . ?
C14 C13 1.371(10) . ?
N6 C21 1.477(7) . ?
N6 C23 1.372(7) . ?
N6 C22 1.344(6) . ?
N5 C16 1.337(7) . ?
N5 C20 1.353(6) . ?
C2 H2 0.9300 . ?
C2 C1 1.366(8) . ?
C2 C3 1.382(8) . ?
N7 C25 1.476(7) . ?
N7 C24 1.394(7) . ?
N7 C22 1.351(7) . ?
C9 H9 0.9300 . ?
C9 C8 1.342(8) . ?
N2 C8 1.387(7) . ?
N2 C7 1.342(7) . ?
N2 C6 1.466(7) . ?
C18 H18 0.9300 . ?
C18 C17 1.377(9) . ?
C18 C19 1.385(8) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.509(7) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.498(8) . ?
C8 H8 0.9300 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C20 1.501(8) . ?
C27 H27 0.9300 . ?
C27 C28 1.394(8) . ?
C27 C26 1.381(8) . ?
C16 H16 0.9300 . ?
C16 C17 1.387(8) . ?
C17 H17 0.9300 . ?
C19 H19 0.9300 . ?
C19 C20 1.380(7) . ?
C4 H4 0.9300 . ?
C4 C3 1.375(8) . ?
C4 C5 1.378(7) . ?
C28 H28 0.9300 . ?
C28 C29 1.372(10) . ?
C23 H23 0.9300 . ?
C23 C24 1.336(7) . ?
C1 H1 0.9300 . ?
C24 H24 0.9300 . ?
C13 H13 0.9300 . ?
C13 C12 1.387(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.515(7) . ?
C3 H3 0.9300 . ?
C11 C12 1.386(8) . ?
C30 H30 0.9300 . ?
C30 C29 1.375(9) . ?
C29 H29 0.9300 . ?
C12 H12 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 N5 94.83(17) . . ?
C7 Pd1 N1 84.85(19) . . ?
C7 Pd1 N5 178.39(19) . . ?
C7 Pd1 C22 94.7(2) . . ?
C22 Pd1 N1 176.79(19) . . ?
C22 Pd1 N5 85.71(19) . . ?
F4 P1 F5 89.5(2) . . ?
F3 P1 F4 88.5(3) . . ?
F3 P1 F5 89.7(2) . . ?
F3 P1 F6 90.4(2) . . ?
F1 P1 F4 88.7(3) . . ?
F1 P1 F3 177.2(3) . . ?
F1 P1 F5 90.4(2) . . ?
F1 P1 F2 91.3(3) . . ?
F1 P1 F6 89.5(2) . . ?
F2 P1 F4 179.5(3) . . ?
F2 P1 F3 91.5(3) . . ?
F2 P1 F5 90.0(2) . . ?
F2 P1 F6 89.5(2) . . ?
F6 P1 F4 91.0(2) . . ?
F6 P1 F5 179.5(2) . . ?
F9A P2 F7B 143.3(5) . . ?
F11 P2 F9A 89.6(3) . . ?
F11 P2 F12 179.7(2) . . ?
F11 P2 F10A 88.8(2) . . ?
F11 P2 F7B 89.6(5) . . ?
F11 P2 F8B 87.4(5) . . ?
F12 P2 F9A 90.1(3) . . ?
F12 P2 F10A 91.3(3) . . ?
F12 P2 F7B 90.6(5) . . ?
F10A P2 F9A 86.2(3) . . ?
F10A P2 F7B 130.5(5) . . ?
F7A P2 F9A 175.3(3) . . ?
F7A P2 F11 90.0(3) . . ?
F7A P2 F12 90.3(3) . . ?
F7A P2 F10A 89.1(3) . . ?
F7A P2 F8A 93.8(3) . . ?
F7A P2 F7B 41.4(4) . . ?
F7A P2 F8B 125.5(5) . . ?
F7A P2 F10B 46.5(5) . . ?
F8A P2 F9A 90.9(3) . . ?
F8A P2 F11 91.2(3) . . ?
F8A P2 F12 88.7(3) . . ?
F8A P2 F10A 177.1(3) . . ?
F8A P2 F7B 52.5(5) . . ?
F8A P2 F8B 32.0(4) . . ?
F8A P2 F10B 139.9(6) . . ?
F8B P2 F9A 59.2(5) . . ?
F8B P2 F12 92.4(5) . . ?
F8B P2 F10A 145.1(5) . . ?
F8B P2 F7B 84.2(6) . . ?
F10B P2 F9A 128.9(6) . . ?
F10B P2 F11 93.9(7) . . ?
F10B P2 F12 86.3(7) . . ?
F10B P2 F10A 43.0(5) . . ?
F10B P2 F7B 87.8(6) . . ?
F10B P2 F8B 171.8(7) . . ?
F9B P2 F9A 34.6(5) . . ?
F9B P2 F11 93.0(7) . . ?
F9B P2 F12 86.8(7) . . ?
F9B P2 F10A 51.8(6) . . ?
F9B P2 F7A 140.7(6) . . ?
F9B P2 F8A 125.2(6) . . ?
F9B P2 F7B 176.6(8) . . ?
F9B P2 F8B 93.8(7) . . ?
F9B P2 F10B 94.2(7) . . ?
N4 C15 H15 118.1 . . ?
N4 C15 C14 123.8(6) . . ?
C14 C15 H15 118.1 . . ?
C11 N4 C15 116.9(6) . . ?
C9 N3 C10 125.0(4) . . ?
C7 N3 C9 110.2(4) . . ?
C7 N3 C10 124.4(5) . . ?
C1 N1 Pd1 121.9(4) . . ?
C1 N1 C5 118.4(5) . . ?
C5 N1 Pd1 119.7(4) . . ?
C26 N8 C30 116.2(5) . . ?
C15 C14 H14 120.1 . . ?
C15 C14 C13 119.7(7) . . ?
C13 C14 H14 120.1 . . ?
C23 N6 C21 127.5(4) . . ?
C22 N6 C21 120.8(4) . . ?
C22 N6 C23 111.4(4) . . ?
C16 N5 Pd1 120.4(4) . . ?
C16 N5 C20 119.2(5) . . ?
C20 N5 Pd1 120.4(3) . . ?
C1 C2 H2 120.3 . . ?
C1 C2 C3 119.4(6) . . ?
C3 C2 H2 120.3 . . ?
C24 N7 C25 123.2(4) . . ?
C22 N7 C25 126.2(4) . . ?
C22 N7 C24 110.6(4) . . ?
N3 C9 H9 126.4 . . ?
C8 C9 N3 107.2(5) . . ?
C8 C9 H9 126.4 . . ?
C8 N2 C6 127.3(5) . . ?
C7 N2 C8 110.9(5) . . ?
C7 N2 C6 121.4(4) . . ?
C17 C18 H18 120.6 . . ?
C17 C18 C19 118.8(5) . . ?
C19 C18 H18 120.6 . . ?
N7 C25 H25A 109.2 . . ?
N7 C25 H25B 109.2 . . ?
N7 C25 C26 112.2(4) . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 H25A 109.2 . . ?
C26 C25 H25B 109.2 . . ?
N3 C10 H10A 108.4 . . ?
N3 C10 H10B 108.4 . . ?
N3 C10 C11 115.4(5) . . ?
H10A C10 H10B 107.5 . . ?
C11 C10 H10A 108.4 . . ?
C11 C10 H10B 108.4 . . ?
C9 C8 N2 106.1(5) . . ?
C9 C8 H8 126.9 . . ?
N2 C8 H8 126.9 . . ?
N6 C21 H21A 109.8 . . ?
N6 C21 H21B 109.8 . . ?
N6 C21 C20 109.3(4) . . ?
H21A C21 H21B 108.3 . . ?
C20 C21 H21A 109.8 . . ?
C20 C21 H21B 109.8 . . ?
C28 C27 H27 121.3 . . ?
C26 C27 H27 121.3 . . ?
C26 C27 C28 117.4(6) . . ?
N5 C16 H16 119.0 . . ?
N5 C16 C17 122.0(5) . . ?
C17 C16 H16 119.0 . . ?
C18 C17 C16 119.1(5) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
N3 C7 Pd1 134.2(4) . . ?
N2 C7 Pd1 120.2(4) . . ?
N2 C7 N3 105.5(4) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 C18 119.7(5) . . ?
C20 C19 H19 120.2 . . ?
C3 C4 H4 119.7 . . ?
C3 C4 C5 120.6(5) . . ?
C5 C4 H4 119.7 . . ?
C27 C28 H28 120.2 . . ?
C29 C28 C27 119.5(6) . . ?
C29 C28 H28 120.2 . . ?
N6 C23 H23 126.5 . . ?
C24 C23 N6 107.1(5) . . ?
C24 C23 H23 126.5 . . ?
N1 C1 C2 122.9(5) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
N7 C24 H24 126.8 . . ?
C23 C24 N7 106.3(5) . . ?
C23 C24 H24 126.8 . . ?
C14 C13 H13 121.3 . . ?
C14 C13 C12 117.4(7) . . ?
C12 C13 H13 121.3 . . ?
N2 C6 H6A 109.8 . . ?
N2 C6 H6B 109.8 . . ?
N2 C6 C5 109.2(4) . . ?
H6A C6 H6B 108.3 . . ?
C5 C6 H6A 109.8 . . ?
C5 C6 H6B 109.8 . . ?
N6 C22 Pd1 120.4(4) . . ?
N6 C22 N7 104.6(4) . . ?
N7 C22 Pd1 134.3(4) . . ?
N8 C26 C25 115.4(5) . . ?
N8 C26 C27 124.3(5) . . ?
C27 C26 C25 120.3(5) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 C2 117.8(6) . . ?
C4 C3 H3 121.1 . . ?
N4 C11 C10 118.0(5) . . ?
N4 C11 C12 123.0(6) . . ?
C12 C11 C10 118.9(5) . . ?
N1 C5 C4 120.9(5) . . ?
N1 C5 C6 117.3(5) . . ?
C4 C5 C6 121.9(5) . . ?
N8 C30 H30 117.9 . . ?
N8 C30 C29 124.2(6) . . ?
C29 C30 H30 117.9 . . ?
N5 C20 C21 116.8(5) . . ?
N5 C20 C19 121.1(5) . . ?
C19 C20 C21 122.1(5) . . ?
C28 C29 C30 118.3(6) . . ?
C28 C29 H29 120.9 . . ?
C30 C29 H29 120.9 . . ?
C13 C12 H12 120.4 . . ?
C11 C12 C13 119.1(7) . . ?
C11 C12 H12 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N1 C1 C2 179.8(4) . . . . ?
Pd1 N1 C5 C4 -178.2(4) . . . . ?
Pd1 N1 C5 C6 2.8(6) . . . . ?
Pd1 N5 C16 C17 178.3(4) . . . . ?
Pd1 N5 C20 C21 4.7(6) . . . . ?
Pd1 N5 C20 C19 -177.0(4) . . . . ?
C15 N4 C11 C10 -177.6(5) . . . . ?
C15 N4 C11 C12 -1.1(9) . . . . ?
C15 C14 C13 C12 0.9(10) . . . . ?
N4 C15 C14 C13 -2.4(11) . . . . ?
N4 C11 C12 C13 -0.3(9) . . . . ?
N3 C9 C8 N2 0.7(6) . . . . ?
N3 C10 C11 N4 -31.2(7) . . . . ?
N3 C10 C11 C12 152.2(5) . . . . ?
N1 Pd1 N5 C16 -42.2(4) . . . . ?
N1 Pd1 N5 C20 138.4(4) . . . . ?
N1 Pd1 C7 N3 -130.3(5) . . . . ?
N1 Pd1 C7 N2 45.6(4) . . . . ?
N1 Pd1 C22 N6 139(3) . . . . ?
N1 Pd1 C22 N7 -29(4) . . . . ?
N8 C30 C29 C28 0.7(9) . . . . ?
C14 C15 N4 C11 2.5(9) . . . . ?
C14 C13 C12 C11 0.4(10) . . . . ?
N6 C21 C20 N5 53.7(6) . . . . ?
N6 C21 C20 C19 -124.6(5) . . . . ?
N6 C23 C24 N7 0.7(6) . . . . ?
N5 Pd1 N1 C1 -45.3(4) . . . . ?
N5 Pd1 N1 C5 136.3(4) . . . . ?
N5 Pd1 C7 N3 -52(7) . . . . ?
N5 Pd1 C7 N2 124(7) . . . . ?
N5 Pd1 C22 N6 39.0(4) . . . . ?
N5 Pd1 C22 N7 -129.2(5) . . . . ?
N5 C16 C17 C18 -0.4(8) . . . . ?
N7 C25 C26 N8 -77.9(6) . . . . ?
N7 C25 C26 C27 103.7(6) . . . . ?
C9 N3 C10 C11 92.8(6) . . . . ?
C9 N3 C7 Pd1 177.5(4) . . . . ?
C9 N3 C7 N2 1.1(6) . . . . ?
N2 C6 C5 N1 54.1(6) . . . . ?
N2 C6 C5 C4 -124.9(5) . . . . ?
C18 C19 C20 N5 -2.2(8) . . . . ?
C18 C19 C20 C21 176.1(5) . . . . ?
C25 N7 C24 C23 177.9(4) . . . . ?
C25 N7 C22 Pd1 -9.1(8) . . . . ?
C25 N7 C22 N6 -178.6(4) . . . . ?
C10 N3 C9 C8 171.6(5) . . . . ?
C10 N3 C7 Pd1 4.6(8) . . . . ?
C10 N3 C7 N2 -171.7(5) . . . . ?
C10 C11 C12 C13 176.2(6) . . . . ?
C8 N2 C7 Pd1 -177.7(4) . . . . ?
C8 N2 C7 N3 -0.7(6) . . . . ?
C8 N2 C6 C5 116.3(6) . . . . ?
C21 N6 C23 C24 -176.0(5) . . . . ?
C21 N6 C22 Pd1 5.2(6) . . . . ?
C21 N6 C22 N7 176.4(4) . . . . ?
C27 C28 C29 C30 0.0(9) . . . . ?
C16 N5 C20 C21 -174.8(5) . . . . ?
C16 N5 C20 C19 3.6(7) . . . . ?
C17 C18 C19 C20 -0.5(8) . . . . ?
C7 Pd1 N1 C1 133.1(4) . . . . ?
C7 Pd1 N1 C5 -45.3(4) . . . . ?
C7 Pd1 N5 C16 -120(7) . . . . ?
C7 Pd1 N5 C20 60(7) . . . . ?
C7 Pd1 C22 N6 -139.5(4) . . . . ?
C7 Pd1 C22 N7 52.4(5) . . . . ?
C7 N3 C9 C8 -1.2(6) . . . . ?
C7 N3 C10 C11 -95.3(6) . . . . ?
C7 N2 C8 C9 0.0(6) . . . . ?
C7 N2 C6 C5 -56.4(6) . . . . ?
C19 C18 C17 C16 1.8(8) . . . . ?
C28 C27 C26 N8 1.3(9) . . . . ?
C28 C27 C26 C25 179.6(5) . . . . ?
C23 N6 C21 C20 111.7(5) . . . . ?
C23 N6 C22 Pd1 -169.9(3) . . . . ?
C23 N6 C22 N7 1.4(5) . . . . ?
C1 N1 C5 C4 3.3(7) . . . . ?
C1 N1 C5 C6 -175.7(5) . . . . ?
C1 C2 C3 C4 1.8(9) . . . . ?
C24 N7 C25 C26 -92.3(6) . . . . ?
C24 N7 C22 Pd1 168.5(4) . . . . ?
C24 N7 C22 N6 -1.0(5) . . . . ?
C6 N2 C8 C9 -173.4(5) . . . . ?
C6 N2 C7 Pd1 -3.9(7) . . . . ?
C6 N2 C7 N3 173.1(4) . . . . ?
C22 Pd1 N1 C1 -145(3) . . . . ?
C22 Pd1 N1 C5 37(4) . . . . ?
C22 Pd1 N5 C16 134.7(4) . . . . ?
C22 Pd1 N5 C20 -44.8(4) . . . . ?
C22 Pd1 C7 N3 52.9(5) . . . . ?
C22 Pd1 C7 N2 -131.2(4) . . . . ?
C22 N6 C21 C20 -62.5(6) . . . . ?
C22 N6 C23 C24 -1.3(6) . . . . ?
C22 N7 C25 C26 85.0(6) . . . . ?
C22 N7 C24 C23 0.2(6) . . . . ?
C26 N8 C30 C29 -0.4(8) . . . . ?
C26 C27 C28 C29 -1.0(9) . . . . ?
C3 C2 C1 N1 -0.8(9) . . . . ?
C3 C4 C5 N1 -2.2(8) . . . . ?
C3 C4 C5 C6 176.7(5) . . . . ?
C5 N1 C1 C2 -1.8(8) . . . . ?
C5 C4 C3 C2 -0.3(9) . . . . ?
C30 N8 C26 C25 -178.9(5) . . . . ?
C30 N8 C26 C27 -0.6(8) . . . . ?
C20 N5 C16 C17 -2.3(8) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 22 -19 0.0359 1.0113 22.0091 -19.0012 -0.2889 0.7094 -0.6469
4 -26 5 0.0128 3.9805 -26.0196 5.0021 0.7606 -0.3003 0.5556
-2 10 27 0.0500 -1.9885 10.0172 26.9999 -0.7606 -0.2633 0.5799
5 6 24 0.0445 5.0031 6.0092 24.0017 -0.4064 0.1390 0.9103
-9 -16 8 0.0199 -9.0025 -16.0036 7.9987 0.0711 -0.9677 -0.1499
-4 -5 -25 0.0476 -4.0033 -5.0094 -25.0015 0.4220 -0.0449 -0.8910
-10 12 -4 0.0177 -9.9849 12.0133 -4.0030 -0.5516 -0.3556 -0.7534
-2 -27 8 0.0088 -2.0151 -27.0157 8.0008 0.5741 -0.7342 0.3176
5 25 -4 0.0148 5.0120 25.0138 -3.9999 -0.4975 0.8373 -0.0242
10 -13 -1 0.0139 9.9836 -13.0157 -0.9971 0.6583 0.3971 0.6193

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mrc118_171114_mo
_database_code_depnum_ccdc_archive 'CCDC 1405833'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_audit_creation_date             2014-12-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_chemical_name_common            ?
_chemical_name_systematic        5c
_chemical_formula_moiety         'C24 H23 N9 O4 Pd, 2(F6 P)'
_chemical_formula_sum            'C24 H23 F12 N9 O4 P2 Pd'
_chemical_formula_weight         897.85
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C96 H92 F48 N36 O16 P8 Pd4'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -y-1/2, z-1/2'

_cell_length_a                   11.9415(9)
_cell_length_b                   16.7247(9)
_cell_length_c                   16.7259(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.857(6)
_cell_angle_gamma                90.00
_cell_volume                     3256.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6525
_cell_measurement_temperature    120.00(13)
_cell_measurement_theta_max      30.8420
_cell_measurement_theta_min      3.3890
_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23620
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.10
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   29.00   63.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322   19.0000    0.0000 34

#__ type_ start__ end____ width___ exp.time_
  2 omega   11.00   60.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509   37.0000   90.0000 49

#__ type_ start__ end____ width___ exp.time_
  3 omega   12.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322   37.0000  -90.0000 43

#__ type_ start__ end____ width___ exp.time_
  4 omega  -56.00    1.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -37.0000  150.0000 57

#__ type_ start__ end____ width___ exp.time_
  5 omega  -79.00    8.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -57.0000   90.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0585471000
_diffrn_orient_matrix_UB_12      0.0090203000
_diffrn_orient_matrix_UB_13      -0.0167796000
_diffrn_orient_matrix_UB_21      0.0146725000
_diffrn_orient_matrix_UB_22      0.0148838000
_diffrn_orient_matrix_UB_23      -0.0360920000
_diffrn_orient_matrix_UB_31      -0.0079417000
_diffrn_orient_matrix_UB_32      -0.0386624000
_diffrn_orient_matrix_UB_33      -0.0176912000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                5808
_reflns_number_total             8072
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8072
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0432
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0273P)²+0.6521P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0873
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2aa(H3A,H3B), C3(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C1aa(H2), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C2(H13), C16(H16),
 C17(H17), C19(H19), C20(H20), C22(H22)
2.c X=CH2 refined with riding coordinates:
 C0aa(H1A,H1B), C1(H12A,H12B)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Pd1 Pd 0.215815(19) 0.253237(12) 0.416895(13) 0.01498(7) Uani 1 d . . .
O1 O -0.1627(2) 0.04349(14) 0.33181(14) 0.0346(6) Uani 1 d . . .
N1 N 0.4517(2) 0.22334(14) 0.53966(15) 0.0217(6) Uani 1 d . . .
C1 C 0.6471(3) 0.33193(19) 0.6863(2) 0.0342(8) Uani 1 d . . .
H1A H 0.7059 0.3332 0.6580 0.041 Uiso 1 calc . . R
H1B H 0.6635 0.3406 0.7426 0.041 Uiso 1 calc . . R
O2 O -0.1026(2) -0.07499(14) 0.36928(16) 0.0483(7) Uani 1 d . . .
N2 N 0.3367(2) 0.12525(13) 0.50304(14) 0.0186(5) Uani 1 d . . .
C2 C 0.5419(3) 0.31804(19) 0.6471(2) 0.0318(8) Uani 1 d . . .
H2 H 0.4855 0.3172 0.6774 0.038 Uiso 1 calc . . R
O3 O -0.0405(2) 0.50096(14) 0.69471(15) 0.0420(7) Uani 1 d . . .
N3 N 0.1534(2) 0.13747(13) 0.42571(14) 0.0165(5) Uani 1 d . . .
C3 C 0.5052(3) 0.30332(18) 0.55696(19) 0.0266(7) Uani 1 d . . .
H3A H 0.4505 0.3441 0.5323 0.032 Uiso 1 calc . . R
H3B H 0.5713 0.3071 0.5324 0.032 Uiso 1 calc . . R
O4 O -0.0302(2) 0.37137(14) 0.69963(13) 0.0348(6) Uani 1 d . . .
N4 N -0.0881(2) -0.00290(16) 0.36345(16) 0.0271(6) Uani 1 d . . .
C4 C 0.3483(3) 0.20607(16) 0.49299(17) 0.0179(6) Uani 1 d . . .
N5 N 0.3654(2) 0.37793(14) 0.36394(14) 0.0198(5) Uani 1 d . . .
C5 C 0.5048(3) 0.15465(17) 0.57756(19) 0.0235(7) Uani 1 d . . .
H5 H 0.5771 0.1521 0.6125 0.028 Uiso 1 calc . . R
N6 N 0.2690(2) 0.42714(13) 0.44714(14) 0.0190(5) Uani 1 d . . .
C6 C 0.4333(3) 0.09322(18) 0.55483(18) 0.0243(7) Uani 1 d . . .
H6 H 0.4457 0.0400 0.5705 0.029 Uiso 1 calc . . R
N7 N 0.1488(2) 0.36479(14) 0.51993(15) 0.0223(6) Uani 1 d . . .
C7 C 0.2330(3) 0.08747(17) 0.46816(17) 0.0182(6) Uani 1 d . . .
N8 N -0.0091(2) 0.43648(17) 0.67265(16) 0.0291(6) Uani 1 d . . .
C8 C 0.2145(3) 0.00653(17) 0.47760(18) 0.0206(7) Uani 1 d . . .
H8 H 0.2720 -0.0262 0.5072 0.025 Uiso 1 calc . . R
N9 N 0.0742(2) 0.28879(14) 0.33027(14) 0.0196(5) Uani 1 d . . .
C9 C 0.1086(3) -0.02353(17) 0.44181(18) 0.0229(7) Uani 1 d . . .
H9 H 0.0922 -0.0775 0.4461 0.027 Uiso 1 calc . . R
C10 C 0.0271(3) 0.02806(17) 0.39946(17) 0.0210(7) Uani 1 d . . .
C11 C 0.0493(3) 0.10829(17) 0.39135(17) 0.0185(6) Uani 1 d . . .
H11 H -0.0075 0.1418 0.3623 0.022 Uiso 1 calc . . R
C12 C 0.2660(3) 0.2729(2) 0.1837(2) 0.0305(8) Uani 1 d . . .
H12A H 0.2715 0.2221 0.2069 0.037 Uiso 1 calc . . R
H12B H 0.2182 0.2816 0.1325 0.037 Uiso 1 calc . . R
C13 C 0.3252(3) 0.33157(19) 0.22292(18) 0.0253(7) Uani 1 d . . .
H13 H 0.3176 0.3816 0.1979 0.030 Uiso 1 calc . . R
C14 C 0.4048(3) 0.32442(18) 0.30566(18) 0.0244(7) Uani 1 d . . .
H14A H 0.4059 0.2696 0.3248 0.029 Uiso 1 calc . . R
H14B H 0.4821 0.3389 0.3020 0.029 Uiso 1 calc . . R
C15 C 0.2898(3) 0.35780(17) 0.40882(17) 0.0180(6) Uani 1 d . . .
C16 C 0.3915(3) 0.45919(18) 0.37192(19) 0.0293(8) Uani 1 d . . .
H16 H 0.4410 0.4870 0.3461 0.035 Uiso 1 calc . . R
C17 C 0.3321(3) 0.48938(18) 0.4235(2) 0.0296(8) Uani 1 d . . .
H17 H 0.3326 0.5423 0.4406 0.036 Uiso 1 calc . . R
C18 C 0.1945(3) 0.43349(17) 0.50263(17) 0.0191(6) Uani 1 d . . .
C19 C 0.1746(3) 0.50679(17) 0.53550(18) 0.0239(7) Uani 1 d . . .
H19 H 0.2072 0.5534 0.5205 0.029 Uiso 1 calc . . R
C20 C 0.1056(3) 0.50865(18) 0.59073(18) 0.0254(7) Uani 1 d . . .
H20 H 0.0891 0.5567 0.6137 0.030 Uiso 1 calc . . R
C21 C 0.0613(3) 0.43757(18) 0.61141(17) 0.0208(7) Uani 1 d . . .
C22 C 0.0816(3) 0.36742(18) 0.57383(18) 0.0221(7) Uani 1 d . . .
H22 H 0.0475 0.3205 0.5864 0.027 Uiso 1 calc . . R
C23 C -0.0070(3) 0.30514(17) 0.28335(18) 0.0209(7) Uani 1 d . . .
C24 C -0.1124(3) 0.3248(2) 0.2248(2) 0.0340(8) Uani 1 d . . .
H24A H -0.1125 0.2994 0.1733 0.051 Uiso 1 calc . . GR
H24B H -0.1174 0.3817 0.2172 0.051 Uiso 1 calc . . GR
H24C H -0.1770 0.3064 0.2450 0.051 Uiso 1 calc . . GR
P1 P -0.20459(8) 0.24990(5) 0.46661(5) 0.0289(2) Uani 1 d . . .
F1 F -0.1908(2) 0.31303(12) 0.54026(12) 0.0458(6) Uani 1 d . . .
F2 F -0.1366(2) 0.31009(13) 0.42060(14) 0.0587(7) Uani 1 d . . .
F3 F -0.08384(18) 0.21043(12) 0.51103(13) 0.0448(5) Uani 1 d . . .
F4 F -0.2150(3) 0.18812(18) 0.39558(17) 0.0906(10) Uani 1 d . . .
F5 F -0.26846(19) 0.19157(13) 0.51752(16) 0.0599(7) Uani 1 d . . .
F6 F -0.3220(2) 0.29041(16) 0.42472(14) 0.0645(7) Uani 1 d . . .
P2 P 0.35669(8) 0.03092(5) 0.27642(5) 0.02565(19) Uani 1 d . . .
F7 F 0.3888(2) 0.11718(12) 0.31253(13) 0.0655(8) Uani 1 d . . .
F8 F 0.48858(17) 0.01202(14) 0.28127(12) 0.0466(6) Uani 1 d . . .
F9 F 0.3239(2) -0.05562(13) 0.24086(14) 0.0592(7) Uani 1 d . . .
F10 F 0.22391(18) 0.04828(16) 0.27262(12) 0.0609(7) Uani 1 d . . .
F11 F 0.34294(18) 0.06434(12) 0.18565(11) 0.0394(5) Uani 1 d . . .
F12 F 0.36973(17) -0.00213(13) 0.36791(11) 0.0423(5) Uani 1 d . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N3 2.092(2) . ?
Pd1 C4 1.962(3) . ?
Pd1 N9 2.055(2) . ?
Pd1 C15 1.978(3) . ?
O1 N4 1.211(3) . ?
N1 C3 1.483(4) . ?
N1 C4 1.337(4) . ?
N1 C5 1.395(4) . ?
C1 H1A 0.9300 . ?
C1 H1B 0.9300 . ?
C1 C2 1.302(4) . ?
O2 N4 1.225(3) . ?
N2 C4 1.373(3) . ?
N2 C6 1.387(4) . ?
N2 C7 1.397(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.493(4) . ?
O3 N8 1.225(3) . ?
N3 C7 1.344(4) . ?
N3 C11 1.340(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
O4 N8 1.226(3) . ?
N4 C10 1.468(4) . ?
N5 C14 1.475(4) . ?
N5 C15 1.339(4) . ?
N5 C16 1.394(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.336(4) . ?
N6 C15 1.374(4) . ?
N6 C17 1.393(4) . ?
N6 C18 1.425(4) . ?
C6 H6 0.9300 . ?
N7 C18 1.331(4) . ?
N7 C22 1.334(4) . ?
C7 C8 1.386(4) . ?
N8 C21 1.463(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.369(4) . ?
N9 C23 1.136(4) . ?
C9 H9 0.9300 . ?
C9 C10 1.373(4) . ?
C10 C11 1.380(4) . ?
C11 H11 0.9300 . ?
C12 H12A 0.9300 . ?
C12 H12B 0.9300 . ?
C12 C13 1.299(4) . ?
C13 H13 0.9300 . ?
C13 C14 1.499(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C16 H16 0.9300 . ?
C16 C17 1.333(5) . ?
C17 H17 0.9300 . ?
C18 C19 1.386(4) . ?
C19 H19 0.9300 . ?
C19 C20 1.368(4) . ?
C20 H20 0.9300 . ?
C20 C21 1.376(4) . ?
C21 C22 1.378(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.450(4) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
P1 F1 1.603(2) . ?
P1 F2 1.595(2) . ?
P1 F3 1.609(2) . ?
P1 F4 1.558(2) . ?
P1 F5 1.596(2) . ?
P1 F6 1.575(2) . ?
P2 F7 1.578(2) . ?
P2 F8 1.591(2) . ?
P2 F9 1.581(2) . ?
P2 F10 1.599(2) . ?
P2 F11 1.5915(19) . ?
P2 F12 1.6017(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 Pd1 N3 80.25(10) . . ?
C4 Pd1 N9 172.81(10) . . ?
C4 Pd1 C15 95.26(12) . . ?
N9 Pd1 N3 93.85(9) . . ?
C15 Pd1 N3 174.32(11) . . ?
C15 Pd1 N9 90.36(10) . . ?
C4 N1 C3 127.6(2) . . ?
C4 N1 C5 110.8(2) . . ?
C5 N1 C3 121.5(2) . . ?
H1A C1 H1B 120.0 . . ?
C2 C1 H1A 120.0 . . ?
C2 C1 H1B 120.0 . . ?
C4 N2 C6 111.4(2) . . ?
C4 N2 C7 119.9(2) . . ?
C6 N2 C7 128.5(2) . . ?
C1 C2 H2 117.6 . . ?
C1 C2 C3 124.9(3) . . ?
C3 C2 H2 117.6 . . ?
C7 N3 Pd1 113.06(19) . . ?
C11 N3 Pd1 128.17(19) . . ?
C11 N3 C7 118.7(2) . . ?
N1 C3 C2 111.3(3) . . ?
N1 C3 H3A 109.4 . . ?
N1 C3 H3B 109.4 . . ?
C2 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
O1 N4 O2 124.2(3) . . ?
O1 N4 C10 119.0(3) . . ?
O2 N4 C10 116.8(3) . . ?
N1 C4 Pd1 143.0(2) . . ?
N1 C4 N2 104.3(2) . . ?
N2 C4 Pd1 112.7(2) . . ?
C15 N5 C14 124.9(2) . . ?
C15 N5 C16 110.8(2) . . ?
C16 N5 C14 123.9(3) . . ?
N1 C5 H5 126.1 . . ?
C6 C5 N1 107.9(3) . . ?
C6 C5 H5 126.1 . . ?
C15 N6 C17 109.5(3) . . ?
C15 N6 C18 124.8(2) . . ?
C17 N6 C18 125.7(2) . . ?
N2 C6 H6 127.1 . . ?
C5 C6 N2 105.7(3) . . ?
C5 C6 H6 127.1 . . ?
C18 N7 C22 117.1(3) . . ?
N3 C7 N2 113.3(2) . . ?
N3 C7 C8 123.8(3) . . ?
C8 C7 N2 122.9(3) . . ?
O3 N8 O4 124.7(3) . . ?
O3 N8 C21 117.5(3) . . ?
O4 N8 C21 117.8(3) . . ?
C7 C8 H8 121.2 . . ?
C9 C8 C7 117.6(3) . . ?
C9 C8 H8 121.2 . . ?
C23 N9 Pd1 176.5(2) . . ?
C8 C9 H9 120.8 . . ?
C8 C9 C10 118.3(3) . . ?
C10 C9 H9 120.8 . . ?
C9 C10 N4 118.8(3) . . ?
C9 C10 C11 122.1(3) . . ?
C11 C10 N4 119.0(3) . . ?
N3 C11 C10 119.5(3) . . ?
N3 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
H12A C12 H12B 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C13 C12 H12B 120.0 . . ?
C12 C13 H13 117.7 . . ?
C12 C13 C14 124.6(3) . . ?
C14 C13 H13 117.7 . . ?
N5 C14 C13 109.4(2) . . ?
N5 C14 H14A 109.8 . . ?
N5 C14 H14B 109.8 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
H14A C14 H14B 108.3 . . ?
N5 C15 Pd1 128.9(2) . . ?
N5 C15 N6 105.3(2) . . ?
N6 C15 Pd1 125.8(2) . . ?
N5 C16 H16 126.5 . . ?
C17 C16 N5 106.9(3) . . ?
C17 C16 H16 126.5 . . ?
N6 C17 H17 126.3 . . ?
C16 C17 N6 107.4(3) . . ?
C16 C17 H17 126.3 . . ?
N7 C18 N6 115.0(3) . . ?
N7 C18 C19 124.2(3) . . ?
C19 C18 N6 120.8(3) . . ?
C18 C19 H19 121.0 . . ?
C20 C19 C18 118.1(3) . . ?
C20 C19 H19 121.0 . . ?
C19 C20 H20 120.9 . . ?
C19 C20 C21 118.2(3) . . ?
C21 C20 H20 120.9 . . ?
C20 C21 N8 120.0(3) . . ?
C20 C21 C22 120.3(3) . . ?
C22 C21 N8 119.7(3) . . ?
N7 C22 C21 122.0(3) . . ?
N7 C22 H22 119.0 . . ?
C21 C22 H22 119.0 . . ?
N9 C23 C24 178.5(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
F1 P1 F3 89.26(12) . . ?
F2 P1 F1 88.78(13) . . ?
F2 P1 F3 88.95(12) . . ?
F2 P1 F5 176.73(15) . . ?
F4 P1 F1 178.70(15) . . ?
F4 P1 F2 90.78(17) . . ?
F4 P1 F3 89.51(14) . . ?
F4 P1 F5 92.00(17) . . ?
F4 P1 F6 91.94(15) . . ?
F5 P1 F1 88.41(13) . . ?
F5 P1 F3 89.34(12) . . ?
F6 P1 F1 89.29(13) . . ?
F6 P1 F2 90.70(14) . . ?
F6 P1 F3 178.51(14) . . ?
F6 P1 F5 90.94(14) . . ?
F7 P2 F8 90.49(14) . . ?
F7 P2 F9 179.48(16) . . ?
F7 P2 F10 90.20(15) . . ?
F7 P2 F11 90.50(12) . . ?
F7 P2 F12 89.21(12) . . ?
F8 P2 F10 178.82(13) . . ?
F8 P2 F11 90.54(11) . . ?
F8 P2 F12 89.89(11) . . ?
F9 P2 F8 89.83(13) . . ?
F9 P2 F10 89.47(14) . . ?
F9 P2 F11 89.91(12) . . ?
F9 P2 F12 90.38(12) . . ?
F10 P2 F12 89.16(11) . . ?
F11 P2 F10 90.42(11) . . ?
F11 P2 F12 179.49(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N3 C7 N2 5.3(3) . . . . ?
Pd1 N3 C7 C8 -175.5(2) . . . . ?
Pd1 N3 C11 C10 175.1(2) . . . . ?
Pd1 N9 C23 C24 26(16) . . . . ?
O1 N4 C10 C9 174.1(3) . . . . ?
O1 N4 C10 C11 -4.4(4) . . . . ?
N1 C5 C6 N2 0.0(3) . . . . ?
C1 C2 C3 N1 119.6(4) . . . . ?
O2 N4 C10 C9 -4.4(4) . . . . ?
O2 N4 C10 C11 177.2(3) . . . . ?
N2 C7 C8 C9 178.8(3) . . . . ?
O3 N8 C21 C20 10.7(4) . . . . ?
O3 N8 C21 C22 -168.4(3) . . . . ?
N3 Pd1 C4 N1 -174.9(4) . . . . ?
N3 Pd1 C4 N2 7.2(2) . . . . ?
N3 Pd1 N9 C23 15(4) . . . . ?
N3 Pd1 C15 N5 42.0(11) . . . . ?
N3 Pd1 C15 N6 -141.0(9) . . . . ?
N3 C7 C8 C9 -0.4(4) . . . . ?
C3 N1 C4 Pd1 7.1(5) . . . . ?
C3 N1 C4 N2 -174.9(3) . . . . ?
C3 N1 C5 C6 175.5(3) . . . . ?
O4 N8 C21 C20 -167.6(3) . . . . ?
O4 N8 C21 C22 13.3(4) . . . . ?
N4 C10 C11 N3 178.4(2) . . . . ?
C4 Pd1 N3 C7 -7.0(2) . . . . ?
C4 Pd1 N3 C11 176.8(2) . . . . ?
C4 Pd1 N9 C23 50(4) . . . . ?
C4 Pd1 C15 N5 79.6(3) . . . . ?
C4 Pd1 C15 N6 -103.4(2) . . . . ?
C4 N1 C3 C2 125.6(3) . . . . ?
C4 N1 C5 C6 -0.5(4) . . . . ?
C4 N2 C6 C5 0.5(3) . . . . ?
C4 N2 C7 N3 0.9(4) . . . . ?
C4 N2 C7 C8 -178.4(3) . . . . ?
N5 C16 C17 N6 -0.3(4) . . . . ?
C5 N1 C3 C2 -49.7(4) . . . . ?
C5 N1 C4 Pd1 -177.2(3) . . . . ?
C5 N1 C4 N2 0.7(3) . . . . ?
N6 C18 C19 C20 -177.7(3) . . . . ?
C6 N2 C4 Pd1 177.9(2) . . . . ?
C6 N2 C4 N1 -0.8(3) . . . . ?
C6 N2 C7 N3 175.1(3) . . . . ?
C6 N2 C7 C8 -4.2(5) . . . . ?
N7 C18 C19 C20 1.6(5) . . . . ?
C7 N2 C4 Pd1 -7.0(3) . . . . ?
C7 N2 C4 N1 174.4(2) . . . . ?
C7 N2 C6 C5 -174.1(3) . . . . ?
C7 N3 C11 C10 -0.8(4) . . . . ?
C7 C8 C9 C10 -0.5(4) . . . . ?
N8 C21 C22 N7 -177.4(3) . . . . ?
C8 C9 C10 N4 -177.7(3) . . . . ?
C8 C9 C10 C11 0.7(4) . . . . ?
N9 Pd1 N3 C7 168.81(19) . . . . ?
N9 Pd1 N3 C11 -7.3(2) . . . . ?
N9 Pd1 C4 N1 149.8(7) . . . . ?
N9 Pd1 C4 N2 -28.1(10) . . . . ?
N9 Pd1 C15 N5 -95.9(3) . . . . ?
N9 Pd1 C15 N6 81.1(2) . . . . ?
C9 C10 C11 N3 0.0(4) . . . . ?
C11 N3 C7 N2 -178.2(2) . . . . ?
C11 N3 C7 C8 1.1(4) . . . . ?
C12 C13 C14 N5 -119.8(3) . . . . ?
C14 N5 C15 Pd1 3.7(4) . . . . ?
C14 N5 C15 N6 -173.8(2) . . . . ?
C14 N5 C16 C17 173.6(3) . . . . ?
C15 Pd1 N3 C7 31.1(11) . . . . ?
C15 Pd1 N3 C11 -145.1(9) . . . . ?
C15 Pd1 C4 N1 8.6(4) . . . . ?
C15 Pd1 C4 N2 -169.3(2) . . . . ?
C15 Pd1 N9 C23 -169(4) . . . . ?
C15 N5 C14 C13 88.5(3) . . . . ?
C15 N5 C16 C17 0.8(4) . . . . ?
C15 N6 C17 C16 -0.4(4) . . . . ?
C15 N6 C18 N7 3.7(4) . . . . ?
C15 N6 C18 C19 -177.0(3) . . . . ?
C16 N5 C14 C13 -83.3(3) . . . . ?
C16 N5 C15 Pd1 176.5(2) . . . . ?
C16 N5 C15 N6 -1.0(3) . . . . ?
C17 N6 C15 Pd1 -176.7(2) . . . . ?
C17 N6 C15 N5 0.9(3) . . . . ?
C17 N6 C18 N7 -176.0(3) . . . . ?
C17 N6 C18 C19 3.3(4) . . . . ?
C18 N6 C15 Pd1 3.5(4) . . . . ?
C18 N6 C15 N5 -178.9(3) . . . . ?
C18 N6 C17 C16 179.4(3) . . . . ?
C18 N7 C22 C21 -1.0(4) . . . . ?
C18 C19 C20 C21 0.9(4) . . . . ?
C19 C20 C21 N8 177.6(3) . . . . ?
C19 C20 C21 C22 -3.4(4) . . . . ?
C20 C21 C22 N7 3.5(5) . . . . ?
C22 N7 C18 N6 177.7(3) . . . . ?
C22 N7 C18 C19 -1.5(4) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-16 -4 -1 0.0052 -16.1112 -3.8385 -0.5866 0.9185 -0.2724 0.2867
-7 3 23 0.0697 -7.4400 2.6836 22.7669 0.0778 -0.8909 -0.4474
8 -6 -22 0.0538 7.7655 -5.8159 -22.0153 -0.1377 0.8220 0.5527
2 17 -16 0.0616 1.9536 17.0127 -16.2485 0.3117 0.8683 -0.3858
-4 23 -1 0.0536 -3.6415 22.8764 -1.3562 0.4423 0.3360 -0.8315
16 -1 4 0.0299 15.5946 -1.0649 3.7641 -0.9858 0.0771 -0.1493
4 -16 -17 0.0714 4.0746 -16.1551 -17.0899 -0.0975 0.4361 0.8946
-16 4 -1 0.0148 -16.0620 3.7069 -0.9056 0.9890 -0.1478 0.0003
7 21 1 0.0666 7.2479 20.9762 1.3751 -0.2582 0.3689 -0.8929
-7 -9 -16 0.0420 -7.2013 -9.3013 -16.4512 0.6138 0.3497 0.7078
-6 -22 5 0.0924 -5.9429 -21.8391 4.9372 0.0681 -0.5904 0.8042
4 -2 21 0.0576 4.4257 -2.3429 20.6452 -0.6267 -0.7151 -0.3098
7 21 2 0.0663 7.3239 20.8214 1.8794 -0.2725 0.3495 -0.8964

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mrc125_mo_a
_database_code_depnum_ccdc_archive 'CCDC 1405834'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_audit_creation_date             2014-09-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.06.18 svn.r2945 for OlexSys, GUI svn.r4846)
;
_chemical_name_common            ?
_chemical_name_systematic        4b
_chemical_formula_moiety         'C12 H13 Br2 N3 Pd'
_chemical_formula_sum            'C12 H13 Br2 N3 Pd'
_chemical_formula_weight         465.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C24 H26 Br4 N6 Pd2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'

_cell_length_a                   7.9713(7)
_cell_length_b                   9.1926(8)
_cell_length_c                   9.8150(4)
_cell_angle_alpha                80.496(5)
_cell_angle_beta                 79.638(6)
_cell_angle_gamma                87.116(7)
_cell_volume                     697.61(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6257
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      30.3740
_cell_measurement_theta_min      3.3990
_exptl_absorpt_coefficient_mu    7.043
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14130
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.06
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -47.00  -20.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072  -37.0000 -150.0000 27

#__ type_ start__ end____ width___ exp.time_
  2 omega  -76.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -57.0000  -60.0000 76

#__ type_ start__ end____ width___ exp.time_
  3 omega  -73.00   11.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -57.0000   90.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega  -80.00   11.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -57.0000 -150.0000 91

#__ type_ start__ end____ width___ exp.time_
  5 omega  -66.00  -17.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -57.0000   30.0000 49

#__ type_ start__ end____ width___ exp.time_
  6 omega   20.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   19.0000   30.0000 42

#__ type_ start__ end____ width___ exp.time_
  7 omega  -39.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   57.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
  8 omega  -39.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   57.0000 -150.0000 94

#__ type_ start__ end____ width___ exp.time_
  9 omega  -39.00   38.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   57.0000    0.0000 77

#__ type_ start__ end____ width___ exp.time_
 10 omega  -39.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884   57.0000  -60.0000 94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0271274000
_diffrn_orient_matrix_UB_12      -0.0716237000
_diffrn_orient_matrix_UB_13      -0.0137796000
_diffrn_orient_matrix_UB_21      0.0837400000
_diffrn_orient_matrix_UB_22      0.0143997000
_diffrn_orient_matrix_UB_23      0.0086063000
_diffrn_orient_matrix_UB_31      -0.0209248000
_diffrn_orient_matrix_UB_32      -0.0280365000
_diffrn_orient_matrix_UB_33      0.0726150000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                2945
_reflns_number_total             3472
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.994
_refine_diff_density_min         -1.023
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3472
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0331P)²+1.7606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0778
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11)
2.c X=CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Pd1 Pd 0.24732(4) 0.44096(3) 0.50612(3) 0.01628(9) Uani 1 d . . .
Br1 Br 0.13438(5) 0.20714(4) 0.65003(4) 0.02349(11) Uani 1 d . . .
N1 N 0.4235(4) 0.7126(4) 0.2988(3) 0.0190(7) Uani 1 d . . .
C1 C 0.3129(6) 0.7471(5) 0.0314(5) 0.0350(11) Uani 1 d . . .
H1A H 0.2392 0.7778 0.1065 0.042 Uiso 1 calc . . R
H1B H 0.2829 0.7623 -0.0572 0.042 Uiso 1 calc . . R
Br2 Br 0.40678(6) 0.29733(5) 0.33768(5) 0.02731(12) Uani 1 d . . .
N2 N 0.2523(4) 0.7498(3) 0.4852(3) 0.0167(6) Uani 1 d . . .
C2 C 0.4602(6) 0.6820(5) 0.0506(5) 0.0274(9) Uani 1 d . . .
H2 H 0.5291 0.6536 -0.0280 0.033 Uiso 1 calc . . R
N3 N 0.1172(4) 0.5670(3) 0.6486(3) 0.0156(6) Uani 1 d . . .
C3 C 0.5282(5) 0.6493(5) 0.1844(4) 0.0225(8) Uani 1 d . . .
H3A H 0.5360 0.5432 0.2118 0.027 Uiso 1 calc . . R
H3B H 0.6426 0.6873 0.1689 0.027 Uiso 1 calc . . R
C4 C 0.4185(5) 0.8636(4) 0.3035(4) 0.0223(8) Uani 1 d . . .
H4 H 0.4787 0.9351 0.2371 0.027 Uiso 1 calc . . R
C5 C 0.3120(5) 0.8876(4) 0.4200(4) 0.0212(8) Uani 1 d . . .
H5 H 0.2840 0.9776 0.4507 0.025 Uiso 1 calc . . R
C6 C 0.3218(5) 0.6406(4) 0.4117(4) 0.0181(8) Uani 1 d . . .
C7 C 0.1417(5) 0.7128(4) 0.6130(4) 0.0172(8) Uani 1 d . . .
C8 C 0.0666(5) 0.8149(4) 0.6933(4) 0.0204(8) Uani 1 d . . .
H8 H 0.0865 0.9149 0.6635 0.024 Uiso 1 calc . . R
C9 C -0.0394(5) 0.7671(4) 0.8196(4) 0.0215(8) Uani 1 d . . .
C10 C -0.0648(5) 0.6164(4) 0.8569(4) 0.0216(8) Uani 1 d . . .
H10 H -0.1355 0.5800 0.9406 0.026 Uiso 1 calc . . R
C11 C 0.0144(5) 0.5208(4) 0.7703(4) 0.0205(8) Uani 1 d . . .
H11 H -0.0042 0.4202 0.7972 0.025 Uiso 1 calc . . R
C12 C -0.1258(6) 0.8742(5) 0.9104(5) 0.0279(9) Uani 1 d . . .
H12A H -0.0790 0.9703 0.8762 0.042 Uiso 1 calc . . GR
H12B H -0.1079 0.8428 1.0050 0.042 Uiso 1 calc . . GR
H12C H -0.2458 0.8783 0.9082 0.042 Uiso 1 calc . . GR


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Br1 2.4820(5) . ?
Pd1 Br2 2.4266(5) . ?
Pd1 N3 2.065(3) . ?
Pd1 C6 1.982(4) . ?
N1 C3 1.458(5) . ?
N1 C4 1.394(5) . ?
N1 C6 1.347(5) . ?
C1 H1A 0.9300 . ?
C1 H1B 0.9300 . ?
C1 C2 1.321(7) . ?
N2 C5 1.387(5) . ?
N2 C6 1.369(5) . ?
N2 C7 1.400(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.490(6) . ?
N3 C7 1.343(5) . ?
N3 C11 1.340(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4 0.9300 . ?
C4 C5 1.339(6) . ?
C5 H5 0.9300 . ?
C7 C8 1.370(6) . ?
C8 H8 0.9300 . ?
C8 C9 1.388(6) . ?
C9 C10 1.389(6) . ?
C9 C12 1.496(6) . ?
C10 H10 0.9300 . ?
C10 C11 1.375(6) . ?
C11 H11 0.9300 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br2 Pd1 Br1 88.570(18) . . ?
N3 Pd1 Br1 92.67(8) . . ?
N3 Pd1 Br2 178.42(9) . . ?
C6 Pd1 Br1 172.47(11) . . ?
C6 Pd1 Br2 98.93(12) . . ?
C6 Pd1 N3 79.83(14) . . ?
C4 N1 C3 122.1(3) . . ?
C6 N1 C3 127.4(3) . . ?
C6 N1 C4 110.5(3) . . ?
H1A C1 H1B 120.0 . . ?
C2 C1 H1A 120.0 . . ?
C2 C1 H1B 120.0 . . ?
C5 N2 C7 128.6(3) . . ?
C6 N2 C5 111.8(3) . . ?
C6 N2 C7 119.5(3) . . ?
C1 C2 H2 116.5 . . ?
C1 C2 C3 127.1(4) . . ?
C3 C2 H2 116.5 . . ?
C7 N3 Pd1 114.8(2) . . ?
C11 N3 Pd1 128.0(3) . . ?
C11 N3 C7 117.2(3) . . ?
N1 C3 C2 113.3(3) . . ?
N1 C3 H3A 108.9 . . ?
N1 C3 H3B 108.9 . . ?
C2 C3 H3A 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
N1 C4 H4 125.9 . . ?
C5 C4 N1 108.2(3) . . ?
C5 C4 H4 125.9 . . ?
N2 C5 H5 127.3 . . ?
C4 C5 N2 105.4(3) . . ?
C4 C5 H5 127.3 . . ?
N1 C6 Pd1 142.9(3) . . ?
N1 C6 N2 104.1(3) . . ?
N2 C6 Pd1 113.0(3) . . ?
N3 C7 N2 112.9(3) . . ?
N3 C7 C8 123.7(4) . . ?
C8 C7 N2 123.4(3) . . ?
C7 C8 H8 120.4 . . ?
C7 C8 C9 119.1(4) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 C10 117.4(4) . . ?
C8 C9 C12 121.2(4) . . ?
C10 C9 C12 121.4(4) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 C9 120.1(4) . . ?
C11 C10 H10 120.0 . . ?
N3 C11 C10 122.5(3) . . ?
N3 C11 H11 118.7 . . ?
C10 C11 H11 118.7 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N3 C7 N2 -0.2(4) . . . . ?
Pd1 N3 C7 C8 179.9(3) . . . . ?
Pd1 N3 C11 C10 179.7(3) . . . . ?
Br1 Pd1 N3 C7 179.7(3) . . . . ?
Br1 Pd1 N3 C11 0.2(3) . . . . ?
Br1 Pd1 C6 N1 172.8(5) . . . . ?
Br1 Pd1 C6 N2 -4.6(10) . . . . ?
N1 C4 C5 N2 -0.3(4) . . . . ?
C1 C2 C3 N1 -7.0(6) . . . . ?
Br2 Pd1 N3 C7 38(3) . . . . ?
Br2 Pd1 N3 C11 -141(3) . . . . ?
Br2 Pd1 C6 N1 -1.8(5) . . . . ?
Br2 Pd1 C6 N2 -179.2(2) . . . . ?
N2 C7 C8 C9 -179.1(4) . . . . ?
N3 Pd1 C6 N1 177.2(5) . . . . ?
N3 Pd1 C6 N2 -0.2(3) . . . . ?
N3 C7 C8 C9 0.8(6) . . . . ?
C3 N1 C4 C5 -180.0(4) . . . . ?
C3 N1 C6 Pd1 2.9(7) . . . . ?
C3 N1 C6 N2 -179.6(3) . . . . ?
C4 N1 C3 C2 -72.6(5) . . . . ?
C4 N1 C6 Pd1 -176.8(4) . . . . ?
C4 N1 C6 N2 0.8(4) . . . . ?
C5 N2 C6 Pd1 177.4(3) . . . . ?
C5 N2 C6 N1 -1.0(4) . . . . ?
C5 N2 C7 N3 -176.7(4) . . . . ?
C5 N2 C7 C8 3.2(6) . . . . ?
C6 Pd1 N3 C7 0.2(3) . . . . ?
C6 Pd1 N3 C11 -179.3(4) . . . . ?
C6 N1 C3 C2 107.8(4) . . . . ?
C6 N1 C4 C5 -0.3(5) . . . . ?
C6 N2 C5 C4 0.8(4) . . . . ?
C6 N2 C7 N3 0.1(5) . . . . ?
C6 N2 C7 C8 180.0(4) . . . . ?
C7 N2 C5 C4 177.8(4) . . . . ?
C7 N2 C6 Pd1 0.1(4) . . . . ?
C7 N2 C6 N1 -178.2(3) . . . . ?
C7 N3 C11 C10 0.2(6) . . . . ?
C7 C8 C9 C10 -0.7(6) . . . . ?
C7 C8 C9 C12 -179.4(4) . . . . ?
C8 C9 C10 C11 0.3(6) . . . . ?
C9 C10 C11 N3 -0.1(6) . . . . ?
C11 N3 C7 N2 179.3(3) . . . . ?
C11 N3 C7 C8 -0.6(6) . . . . ?
C12 C9 C10 C11 179.0(4) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3 8 -8 0.0192 3.0001 8.0000 -8.0000 -0.3814 0.2976 -0.8680
-3 -8 8 0.0192 -3.0001 -8.0000 8.0000 0.3814 -0.2976 0.8680
10 0 8 0.0286 10.0000 0.0000 8.0000 0.1610 0.9063 0.3717
1 12 -2 0.0177 1.0001 12.0000 -2.0000 -0.8048 0.2393 -0.5026
-1 -12 2 0.0177 -1.0001 -12.0000 2.0000 0.8048 -0.2393 0.5026
-6 3 10 0.0492 -5.9999 3.0000 10.0000 -0.5154 -0.3732 0.7676
-10 -4 -7 0.0151 -10.0000 -4.0000 -7.0000 0.1117 -0.9552 -0.1869
0 -3 -14 0.0283 -0.0001 -3.0000 -14.0000 0.4078 -0.1637 -0.9325
-6 9 -5 0.0118 -5.9999 9.0000 -5.0000 -0.7385 -0.4159 -0.4899
8 7 9 0.0244 8.0001 7.0000 9.0000 -0.4084 0.8482 0.2899

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_mrc147_mo
_database_code_depnum_ccdc_archive 'CCDC 1405835'
_audit_update_record             
;
2015-06-09 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_audit_creation_date             2014-11-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_chemical_name_common            ?
_chemical_name_systematic        6f
_chemical_formula_moiety         'C30 H26 N8 Pd, C2 H6 O S, 2(Br)'
_chemical_formula_sum            'C32 H32 Br2 N8 O Pd S'
_chemical_formula_weight         842.94
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C256 H256 Br16 N64 O8 Pd8 S8'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   30.370(4)
_cell_length_b                   12.2010(19)
_cell_length_c                   18.606(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.066(14)
_cell_angle_gamma                90.00
_cell_volume                     6590.9(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2743
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      24.1970
_cell_measurement_theta_min      3.6350
_exptl_absorpt_coefficient_mu    3.091
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.1187
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            23167
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.75
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -25.00    3.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072  -57.0000  -30.0000 28

#__ type_ start__ end____ width___ exp.time_
  2 omega  -22.00   36.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072  -57.0000  -90.0000 58

#__ type_ start__ end____ width___ exp.time_
  3 omega  -30.00    8.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -63.0000 -110.3798 38

#__ type_ start__ end____ width___ exp.time_
  4 omega  -78.00  -14.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.8884  -57.0000 -150.0000 64

#__ type_ start__ end____ width___ exp.time_
  5 omega   -5.00   77.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       13.1072   37.0000   90.0000 82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0217878000
_diffrn_orient_matrix_UB_12      -0.0244417000
_diffrn_orient_matrix_UB_13      0.0032144000
_diffrn_orient_matrix_UB_21      0.0096947000
_diffrn_orient_matrix_UB_22      0.0526414000
_diffrn_orient_matrix_UB_23      -0.0003651000
_diffrn_orient_matrix_UB_31      0.0055530000
_diffrn_orient_matrix_UB_32      0.0025653000
_diffrn_orient_matrix_UB_33      0.0396804000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_reflns_number_gt                4905
_reflns_number_total             8170
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.464
_refine_diff_density_min         -2.792
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         8170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1442
_refine_ls_R_factor_gt           0.0803
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0666P)²+75.5018P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1898
_refine_special_details          
;
 One of the unbound pyrdine rings (N5 C16 C17 C18 C19 C20) shows disorder. This 
 has been modelled as two pyridine rings, each with 50% occupancy and refined 
 isotropically.

 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H21A(0.5) H21B(0.5) H21C(0.5) H21D(0.5) N5B(0.5) C16B(0.5)
 H16B(0.5) C17B(0.5) H17B(0.5) C18B(0.5) H18B(0.5) C19B(0.5) H19B(0.5)
 C20B(0.5) N5A(0.5) C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5) C18A(0.5) H18A(0.5)
 C19A(0.5) H19A(0.5) C20A(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C21(H21A,H21B), C21(H21C,H21D), C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C15(H15), C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30),
 C16B(H16B), C17B(H17B), C18B(H18B), C19B(H19B), C16A(H16A), C17A(H17A),
 C18A(H18A), C19A(H19A)
3.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Pd1 Pd 0.11635(2) 0.42898(5) 0.42606(3) 0.02391(16) Uani 1 d . . 1 . . .
N1 N 0.1432(3) 0.6201(7) 0.2346(4) 0.046(2) Uani 1 d . . 1 . . .
N2 N 0.0934(2) 0.6637(5) 0.3704(4) 0.0273(14) Uani 1 d . . 1 . . .
N3 N 0.1131(2) 0.6438(5) 0.4901(4) 0.0301(15) Uani 1 d . . 1 . . .
N4 N 0.0768(2) 0.4286(6) 0.5022(3) 0.0299(15) Uani 1 d . . 1 . . .
N6 N 0.1968(2) 0.4871(5) 0.3660(3) 0.0235(13) Uani 1 d . . 1 . . .
N7 N 0.1546(2) 0.3557(5) 0.3084(3) 0.0226(13) Uani 1 d B . 1 . . .
N8 N 0.1250(2) 0.2579(5) 0.4264(3) 0.0273(14) Uani 1 d . . 1 . . .
C1 C 0.1744(3) 0.6602(9) 0.2035(5) 0.050(3) Uani 1 d . . 1 . . .
H1 H 0.1942 0.6110 0.1905 0.060 Uiso 1 calc . . 1 R . .
C2 C 0.1791(3) 0.7698(9) 0.1897(5) 0.049(3) Uani 1 d . . 1 . . .
H2 H 0.2019 0.7943 0.1692 0.059 Uiso 1 calc . . 1 R . .
C3 C 0.1487(4) 0.8418(9) 0.2074(5) 0.052(3) Uani 1 d . . 1 . . .
H3 H 0.1498 0.9163 0.1974 0.063 Uiso 1 calc . . 1 R . .
C4 C 0.1169(3) 0.8013(7) 0.2401(5) 0.039(2) Uani 1 d . . 1 . . .
H4 H 0.0967 0.8486 0.2535 0.047 Uiso 1 calc . . 1 R . .
C5 C 0.1152(3) 0.6907(7) 0.2530(4) 0.0288(17) Uani 1 d . . 1 . . .
C6 C 0.0801(3) 0.6423(6) 0.2880(4) 0.0267(17) Uani 1 d . . 1 . . .
C7 C 0.1081(3) 0.5887(7) 0.4247(4) 0.0282(18) Uani 1 d . . 1 . . .
C8 C 0.0888(3) 0.7661(6) 0.4006(5) 0.0337(19) Uani 1 d . . 1 . . .
H8 H 0.0788 0.8304 0.3740 0.040 Uiso 1 calc . . 1 R . .
C9 C 0.1017(3) 0.7535(7) 0.4765(5) 0.035(2) Uani 1 d . . 1 . . .
H9 H 0.1026 0.8076 0.5122 0.042 Uiso 1 calc . . 1 R . .
C10 C 0.1216(3) 0.5875(7) 0.5614(4) 0.036(2) Uani 1 d . . 1 . . .
H10A H 0.1225 0.6403 0.6008 0.043 Uiso 1 calc . . 1 R . .
H10B H 0.1512 0.5508 0.5736 0.043 Uiso 1 calc . . 1 R . .
C11 C 0.0844(3) 0.5046(7) 0.5579(4) 0.0289(17) Uani 1 d . . 1 . . .
C12 C 0.0583(3) 0.5071(8) 0.6071(4) 0.036(2) Uani 1 d . . 1 . . .
H12 H 0.0637 0.5604 0.6444 0.043 Uiso 1 calc . . 1 R . .
C13 C 0.0237(3) 0.4290(8) 0.6007(4) 0.038(2) Uani 1 d . . 1 . . .
H13 H 0.0062 0.4286 0.6342 0.045 Uiso 1 calc . . 1 R . .
C14 C 0.0158(3) 0.3525(7) 0.5438(5) 0.037(2) Uani 1 d . . 1 . . .
H14 H -0.0073 0.3002 0.5378 0.045 Uiso 1 calc . . 1 R . .
C15 C 0.0429(3) 0.3552(7) 0.4955(5) 0.0336(19) Uani 1 d . . 1 . . .
H15 H 0.0374 0.3040 0.4568 0.040 Uiso 1 calc . . 1 R . .
C21 C 0.2157(3) 0.5759(7) 0.4178(4) 0.0300(17) Uani 1 d . . 1 . . .
H21A H 0.2416 0.6059 0.4039 0.036 Uiso 0.50 calc A 1 1 R . .
H21B H 0.1925 0.6329 0.4091 0.036 Uiso 0.50 calc A 1 1 R . .
H21C H 0.1923 0.6306 0.4166 0.036 Uiso 0.50 calc A 2 1 R . .
H21D H 0.2412 0.6106 0.4052 0.036 Uiso 0.50 calc A 2 1 R . .
C22 C 0.1577(3) 0.4320(6) 0.3613(4) 0.0243(15) Uani 1 d . . 1 . . .
C23 C 0.2183(3) 0.4447(6) 0.3156(4) 0.0275(17) Uani 1 d . . 1 . . .
H23 H 0.2457 0.4691 0.3083 0.033 Uiso 1 calc B . 1 R . .
C24 C 0.1919(3) 0.3617(7) 0.2795(4) 0.0291(18) Uani 1 d B . 1 . . .
H24 H 0.1975 0.3171 0.2425 0.035 Uiso 1 calc . . 1 R . .
C25 C 0.1194(3) 0.2700(6) 0.2928(4) 0.0266(17) Uani 1 d . . 1 . . .
H25A H 0.1227 0.2234 0.2524 0.032 Uiso 1 calc B . 1 R . .
H25B H 0.0890 0.3030 0.2770 0.032 Uiso 1 calc . . 1 R . .
C26 C 0.1247(2) 0.2021(6) 0.3630(4) 0.0265(17) Uani 1 d . . 1 . . .
C27 C 0.1315(3) 0.0903(7) 0.3638(5) 0.036(2) Uani 1 d . . 1 . . .
H27 H 0.1305 0.0537 0.3194 0.043 Uiso 1 calc B . 1 R . .
C28 C 0.1398(3) 0.0330(7) 0.4298(5) 0.038(2) Uani 1 d . . 1 . . .
H28 H 0.1444 -0.0424 0.4308 0.045 Uiso 1 calc . . 1 R . .
C29 C 0.1413(3) 0.0897(7) 0.4954(5) 0.038(2) Uani 1 d . . 1 . . .
H29 H 0.1476 0.0534 0.5413 0.046 Uiso 1 calc B . 1 R . .
C30 C 0.1332(3) 0.1994(7) 0.4909(4) 0.0313(18) Uani 1 d . . 1 . . .
H30 H 0.1333 0.2364 0.5347 0.038 Uiso 1 calc . . 1 R . .
N5B N 0.2378(5) 0.4444(14) 0.5203(8) 0.026(3) Uiso 0.50 d B 1 1 . . .
C16B C 0.2528(7) 0.4231(18) 0.5948(12) 0.038(4) Uiso 0.50 d B 1 1 . . .
H16B H 0.2567 0.3506 0.6110 0.045 Uiso 0.50 calc B 1 1 R . .
C17B C 0.2621(6) 0.5031(19) 0.6457(9) 0.026(3) Uiso 0.50 d B 1 1 . . .
H17B H 0.2735 0.4870 0.6967 0.031 Uiso 0.50 calc B 1 1 R . .
C18B C 0.2542(6) 0.6166(17) 0.6201(10) 0.037(4) Uiso 0.50 d B 1 1 . . .
H18B H 0.2591 0.6733 0.6550 0.044 Uiso 0.50 calc B 1 1 R . .
C19B C 0.2400(6) 0.6386(17) 0.5466(10) 0.029(4) Uiso 0.50 d B 1 1 . . .
H19B H 0.2364 0.7107 0.5296 0.035 Uiso 0.50 calc B 1 1 R . .
C20B C 0.2310(6) 0.5549(17) 0.4975(10) 0.022(4) Uiso 0.50 d B 1 1 . . .
N5A N 0.2383(6) 0.4111(16) 0.5033(11) 0.046(5) Uiso 0.50 d B 2 1 . . .
C16A C 0.2545(8) 0.376(2) 0.5758(13) 0.063(7) Uiso 0.50 d B 2 1 . . .
H16A H 0.2598 0.3017 0.5834 0.075 Uiso 0.50 calc B 2 1 R . .
C17A C 0.2638(7) 0.441(2) 0.6392(14) 0.049(5) Uiso 0.50 d B 2 1 . . .
H17A H 0.2744 0.4092 0.6866 0.058 Uiso 0.50 calc B 2 1 R . .
C18A C 0.2574(7) 0.555(2) 0.6326(11) 0.039(4) Uiso 0.50 d B 2 1 . . .
H18A H 0.2650 0.6011 0.6743 0.047 Uiso 0.50 calc B 2 1 R . .
C19A C 0.2383(7) 0.5969(17) 0.5575(11) 0.035(5) Uiso 0.50 d B 2 1 . . .
H19A H 0.2300 0.6700 0.5477 0.042 Uiso 0.50 calc B 2 1 R . .
C20A C 0.2330(7) 0.5184(19) 0.4996(11) 0.028(5) Uiso 0.50 d B 2 1 . . .
S1 S -0.04378(9) 0.1234(3) 0.35481(16) 0.0654(9) Uani 1 d . . 1 . . .
O1 O -0.0500(3) 0.2135(10) 0.4057(6) 0.116(4) Uani 1 d . . 1 . . .
C31 C 0.0148(3) 0.1189(10) 0.3585(7) 0.065(3) Uani 1 d . . 1 . . .
H31A H 0.0238 0.1884 0.3432 0.097 Uiso 1 calc . . 1 GR . .
H31B H 0.0194 0.0626 0.3255 0.097 Uiso 1 calc . . 1 GR . .
H31C H 0.0331 0.1032 0.4090 0.097 Uiso 1 calc . . 1 GR . .
C32 C -0.0464(6) -0.0025(15) 0.4027(8) 0.125(7) Uani 1 d . . 1 . . .
H32A H -0.0267 0.0021 0.4534 0.187 Uiso 1 calc . . 1 GR . .
H32B H -0.0365 -0.0617 0.3772 0.187 Uiso 1 calc . . 1 GR . .
H32C H -0.0776 -0.0155 0.4030 0.187 Uiso 1 calc . . 1 GR . .
Br1 Br 0.32089(3) 0.62575(7) 0.34626(5) 0.0334(2) Uani 1 d . . 1 . . .
Br3 Br 0.0000 0.87311(19) 0.2500 0.1069(8) Uani 1 d . . 2 S T P
Br2 Br 0.0000 0.39210(11) 0.2500 0.0466(4) Uani 1 d . . 2 S T P


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N4 2.109(6) . ?
Pd1 N8 2.103(7) . ?
Pd1 C7 1.964(8) . ?
Pd1 C22 1.980(7) . ?
N1 C1 1.341(11) . ?
N1 C5 1.323(11) . ?
N2 C6 1.490(9) . ?
N2 C7 1.339(10) . ?
N2 C8 1.394(10) . ?
N3 C7 1.359(9) . ?
N3 C9 1.387(10) . ?
N3 C10 1.450(10) . ?
N4 C11 1.359(10) . ?
N4 C15 1.342(10) . ?
N6 C21 1.451(9) . ?
N6 C22 1.343(9) . ?
N6 C23 1.393(9) . ?
N7 C22 1.338(9) . ?
N7 C24 1.392(9) . ?
N7 C25 1.462(9) . ?
N8 C26 1.360(9) . ?
N8 C30 1.356(10) . ?
C1 H1 0.9300 . ?
C1 C2 1.376(14) . ?
C2 H2 0.9300 . ?
C2 C3 1.383(14) . ?
C3 H3 0.9300 . ?
C3 C4 1.377(12) . ?
C4 H4 0.9300 . ?
C4 C5 1.374(11) . ?
C5 C6 1.521(10) . ?
C8 H8 0.9300 . ?
C8 C9 1.358(12) . ?
C9 H9 0.9300 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.503(11) . ?
C11 C12 1.375(10) . ?
C12 H12 0.9300 . ?
C12 C13 1.399(12) . ?
C13 H13 0.9300 . ?
C13 C14 1.379(12) . ?
C14 H14 0.9300 . ?
C14 C15 1.386(11) . ?
C15 H15 0.9300 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C21 H21D 0.9700 . ?
C21 C20B 1.440(19) . ?
C21 C20A 1.62(2) . ?
C23 H23 0.9300 . ?
C23 C24 1.343(11) . ?
C24 H24 0.9300 . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C25 C26 1.515(11) . ?
C26 C27 1.380(11) . ?
C27 H27 0.9300 . ?
C27 C28 1.372(12) . ?
C28 H28 0.9300 . ?
C28 C29 1.392(12) . ?
C29 H29 0.9300 . ?
C29 C30 1.358(11) . ?
C30 H30 0.9300 . ?
N5B C16B 1.35(2) . ?
N5B C20B 1.41(2) . ?
C16B H16B 0.9300 . ?
C16B C17B 1.33(3) . ?
C17B H17B 0.9300 . ?
C17B C18B 1.46(3) . ?
C18B H18B 0.9300 . ?
C18B C19B 1.34(3) . ?
C19B H19B 0.9300 . ?
C19B C20B 1.34(3) . ?
N5A C16A 1.36(3) . ?
N5A C20A 1.32(3) . ?
C16A H16A 0.9300 . ?
C16A C17A 1.38(3) . ?
C17A H17A 0.9300 . ?
C17A C18A 1.41(3) . ?
C18A H18A 0.9300 . ?
C18A C19A 1.44(3) . ?
C19A H19A 0.9300 . ?
C19A C20A 1.41(3) . ?
S1 O1 1.498(9) . ?
S1 C31 1.760(10) . ?
S1 C32 1.789(16) . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Pd1 N4 95.2(2) . . ?
C7 Pd1 N4 85.1(3) . . ?
C7 Pd1 N8 179.5(3) . . ?
C7 Pd1 C22 94.3(3) . . ?
C22 Pd1 N4 175.5(3) . . ?
C22 Pd1 N8 85.4(3) . . ?
C5 N1 C1 117.6(9) . . ?
C7 N2 C6 125.9(6) . . ?
C7 N2 C8 111.1(7) . . ?
C8 N2 C6 122.9(7) . . ?
C7 N3 C9 111.0(7) . . ?
C7 N3 C10 121.8(7) . . ?
C9 N3 C10 126.3(7) . . ?
C11 N4 Pd1 120.6(5) . . ?
C15 N4 Pd1 120.7(5) . . ?
C15 N4 C11 118.6(6) . . ?
C22 N6 C21 125.9(6) . . ?
C22 N6 C23 110.5(6) . . ?
C23 N6 C21 123.5(6) . . ?
C22 N7 C24 111.0(6) . . ?
C22 N7 C25 122.2(6) . . ?
C24 N7 C25 126.3(6) . . ?
C26 N8 Pd1 121.6(5) . . ?
C30 N8 Pd1 121.1(5) . . ?
C30 N8 C26 117.2(7) . . ?
N1 C1 H1 117.9 . . ?
N1 C1 C2 124.1(9) . . ?
C2 C1 H1 117.9 . . ?
C1 C2 H2 121.3 . . ?
C1 C2 C3 117.3(8) . . ?
C3 C2 H2 121.3 . . ?
C2 C3 H3 120.6 . . ?
C4 C3 C2 118.8(9) . . ?
C4 C3 H3 120.6 . . ?
C3 C4 H4 120.1 . . ?
C5 C4 C3 119.8(9) . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 122.3(8) . . ?
N1 C5 C6 116.2(7) . . ?
C4 C5 C6 121.5(8) . . ?
N2 C6 C5 111.1(6) . . ?
N2 C7 Pd1 134.5(6) . . ?
N2 C7 N3 105.2(7) . . ?
N3 C7 Pd1 120.0(6) . . ?
N2 C8 H8 126.7 . . ?
C9 C8 N2 106.6(7) . . ?
C9 C8 H8 126.7 . . ?
N3 C9 H9 126.9 . . ?
C8 C9 N3 106.2(7) . . ?
C8 C9 H9 126.9 . . ?
N3 C10 H10A 109.5 . . ?
N3 C10 H10B 109.5 . . ?
N3 C10 C11 110.5(7) . . ?
H10A C10 H10B 108.1 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
N4 C11 C10 116.6(6) . . ?
N4 C11 C12 121.5(8) . . ?
C12 C11 C10 121.8(7) . . ?
C11 C12 H12 120.2 . . ?
C11 C12 C13 119.6(8) . . ?
C13 C12 H12 120.2 . . ?
C12 C13 H13 120.6 . . ?
C14 C13 C12 118.9(7) . . ?
C14 C13 H13 120.6 . . ?
C13 C14 H14 120.6 . . ?
C13 C14 C15 118.7(8) . . ?
C15 C14 H14 120.6 . . ?
N4 C15 C14 122.7(8) . . ?
N4 C15 H15 118.6 . . ?
C14 C15 H15 118.6 . . ?
N6 C21 H21A 107.4 . . ?
N6 C21 H21B 107.4 . . ?
N6 C21 H21C 110.8 . . ?
N6 C21 H21D 110.8 . . ?
N6 C21 C20A 104.9(9) . . ?
H21A C21 H21B 106.9 . . ?
H21A C21 H21C 112.3 . . ?
H21A C21 H21D 3.9 . . ?
H21B C21 H21C 8.5 . . ?
H21B C21 H21D 103.8 . . ?
H21C C21 H21D 108.8 . . ?
C20B C21 N6 119.7(10) . . ?
C20B C21 H21A 107.4 . . ?
C20B C21 H21B 107.4 . . ?
C20B C21 H21C 99.2 . . ?
C20B C21 H21D 106.6 . . ?
C20B C21 C20A 15.6(10) . . ?
C20A C21 H21A 110.4 . . ?
C20A C21 H21B 119.2 . . ?
C20A C21 H21C 110.8 . . ?
C20A C21 H21D 110.8 . . ?
N6 C22 Pd1 132.4(5) . . ?
N7 C22 Pd1 121.0(5) . . ?
N7 C22 N6 105.5(6) . . ?
N6 C23 H23 126.7 . . ?
C24 C23 N6 106.7(7) . . ?
C24 C23 H23 126.7 . . ?
N7 C24 H24 126.9 . . ?
C23 C24 N7 106.3(6) . . ?
C23 C24 H24 126.9 . . ?
N7 C25 H25A 109.8 . . ?
N7 C25 H25B 109.8 . . ?
N7 C25 C26 109.5(6) . . ?
H25A C25 H25B 108.2 . . ?
C26 C25 H25A 109.8 . . ?
C26 C25 H25B 109.8 . . ?
N8 C26 C25 116.6(7) . . ?
N8 C26 C27 121.6(7) . . ?
C27 C26 C25 121.8(7) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 120.0(8) . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.6 . . ?
C27 C28 C29 118.9(8) . . ?
C29 C28 H28 120.6 . . ?
C28 C29 H29 120.8 . . ?
C30 C29 C28 118.5(8) . . ?
C30 C29 H29 120.8 . . ?
N8 C30 C29 123.8(8) . . ?
N8 C30 H30 118.1 . . ?
C29 C30 H30 118.1 . . ?
C16B N5B C20B 117.9(17) . . ?
N5B C16B H16B 119.1 . . ?
C17B C16B N5B 122(2) . . ?
C17B C16B H16B 119.1 . . ?
C16B C17B H17B 120.5 . . ?
C16B C17B C18B 118.9(17) . . ?
C18B C17B H17B 120.5 . . ?
C17B C18B H18B 120.1 . . ?
C19B C18B C17B 119.8(18) . . ?
C19B C18B H18B 120.1 . . ?
C18B C19B H19B 120.5 . . ?
C18B C19B C20B 119(2) . . ?
C20B C19B H19B 120.5 . . ?
N5B C20B C21 117.0(14) . . ?
C19B C20B C21 120.3(17) . . ?
C19B C20B N5B 122.6(17) . . ?
C20A N5A C16A 111(2) . . ?
N5A C16A H16A 116.7 . . ?
N5A C16A C17A 127(3) . . ?
C17A C16A H16A 116.7 . . ?
C16A C17A H17A 119.9 . . ?
C16A C17A C18A 120(2) . . ?
C18A C17A H17A 119.9 . . ?
C17A C18A H18A 121.9 . . ?
C17A C18A C19A 116.2(18) . . ?
C19A C18A H18A 121.9 . . ?
C18A C19A H19A 122.5 . . ?
C20A C19A C18A 115(2) . . ?
C20A C19A H19A 122.5 . . ?
N5A C20A C21 118.7(16) . . ?
N5A C20A C19A 130(2) . . ?
C19A C20A C21 110.9(18) . . ?
O1 S1 C31 108.1(5) . . ?
O1 S1 C32 106.5(7) . . ?
C31 S1 C32 98.4(7) . . ?
S1 C31 H31A 109.5 . . ?
S1 C31 H31B 109.5 . . ?
S1 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
S1 C32 H32A 109.5 . . ?
S1 C32 H32B 109.5 . . ?
S1 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N4 C11 C10 0.4(10) . . . . ?
Pd1 N4 C11 C12 178.6(6) . . . . ?
Pd1 N4 C15 C14 -179.4(6) . . . . ?
Pd1 N8 C26 C25 2.0(8) . . . . ?
Pd1 N8 C26 C27 178.3(5) . . . . ?
Pd1 N8 C30 C29 -176.7(6) . . . . ?
N1 C1 C2 C3 -1.8(15) . . . . ?
N1 C5 C6 N2 105.2(8) . . . . ?
N2 C8 C9 N3 -0.8(9) . . . . ?
N3 C10 C11 N4 55.3(10) . . . . ?
N3 C10 C11 C12 -123.0(8) . . . . ?
N4 Pd1 N8 C26 142.7(5) . . . . ?
N4 Pd1 N8 C30 -40.4(6) . . . . ?
N4 Pd1 C7 N2 -128.1(8) . . . . ?
N4 Pd1 C7 N3 44.0(6) . . . . ?
N4 Pd1 C22 N6 -30(4) . . . . ?
N4 Pd1 C22 N7 137(3) . . . . ?
N4 C11 C12 C13 0.9(12) . . . . ?
N6 C21 C20B N5B 15.8(18) . . . . ?
N6 C21 C20B C19B -166.9(13) . . . . ?
N6 C21 C20A N5A 16.7(18) . . . . ?
N6 C21 C20A C19A -160.9(13) . . . . ?
N6 C23 C24 N7 0.4(8) . . . . ?
N7 C25 C26 N8 53.9(8) . . . . ?
N7 C25 C26 C27 -122.5(7) . . . . ?
N8 Pd1 N4 C11 137.9(6) . . . . ?
N8 Pd1 N4 C15 -43.9(6) . . . . ?
N8 Pd1 C7 N2 2(28) . . . . ?
N8 Pd1 C7 N3 174(100) . . . . ?
N8 Pd1 C22 N6 -127.1(8) . . . . ?
N8 Pd1 C22 N7 39.0(6) . . . . ?
N8 C26 C27 C28 -1.4(11) . . . . ?
C1 N1 C5 C4 1.0(13) . . . . ?
C1 N1 C5 C6 179.9(7) . . . . ?
C1 C2 C3 C4 2.4(14) . . . . ?
C2 C3 C4 C5 -1.5(14) . . . . ?
C3 C4 C5 N1 -0.3(13) . . . . ?
C3 C4 C5 C6 -179.1(8) . . . . ?
C4 C5 C6 N2 -75.9(9) . . . . ?
C5 N1 C1 C2 0.1(14) . . . . ?
C6 N2 C7 Pd1 -3.3(12) . . . . ?
C6 N2 C7 N3 -176.1(6) . . . . ?
C6 N2 C8 C9 176.7(7) . . . . ?
C7 Pd1 N4 C11 -42.5(6) . . . . ?
C7 Pd1 N4 C15 135.7(7) . . . . ?
C7 Pd1 N8 C26 13(28) . . . . ?
C7 Pd1 N8 C30 -170(100) . . . . ?
C7 Pd1 C22 N6 53.3(8) . . . . ?
C7 Pd1 C22 N7 -140.6(6) . . . . ?
C7 N2 C6 C5 -109.8(8) . . . . ?
C7 N2 C8 C9 0.7(9) . . . . ?
C7 N3 C9 C8 0.6(9) . . . . ?
C7 N3 C10 C11 -56.2(10) . . . . ?
C8 N2 C6 C5 74.8(9) . . . . ?
C8 N2 C7 Pd1 172.5(6) . . . . ?
C8 N2 C7 N3 -0.3(8) . . . . ?
C9 N3 C7 Pd1 -174.3(5) . . . . ?
C9 N3 C7 N2 -0.2(8) . . . . ?
C9 N3 C10 C11 112.4(9) . . . . ?
C10 N3 C7 Pd1 -4.1(10) . . . . ?
C10 N3 C7 N2 170.0(7) . . . . ?
C10 N3 C9 C8 -169.0(7) . . . . ?
C10 C11 C12 C13 179.1(8) . . . . ?
C11 N4 C15 C14 -1.1(12) . . . . ?
C11 C12 C13 C14 -1.4(12) . . . . ?
C12 C13 C14 C15 0.7(12) . . . . ?
C13 C14 C15 N4 0.5(13) . . . . ?
C15 N4 C11 C10 -177.9(7) . . . . ?
C15 N4 C11 C12 0.3(12) . . . . ?
C21 N6 C22 Pd1 -10.2(12) . . . . ?
C21 N6 C22 N7 -177.9(7) . . . . ?
C21 N6 C23 C24 177.7(7) . . . . ?
C22 Pd1 N4 C11 41(4) . . . . ?
C22 Pd1 N4 C15 -141(4) . . . . ?
C22 Pd1 N8 C26 -41.8(6) . . . . ?
C22 Pd1 N8 C30 135.1(6) . . . . ?
C22 Pd1 C7 N2 56.4(8) . . . . ?
C22 Pd1 C7 N3 -131.6(6) . . . . ?
C22 N6 C21 C20B 64.8(13) . . . . ?
C22 N6 C21 C20A 69.9(11) . . . . ?
C22 N6 C23 C24 -0.2(9) . . . . ?
C22 N7 C24 C23 -0.5(9) . . . . ?
C22 N7 C25 C26 -59.9(9) . . . . ?
C23 N6 C21 C20B -112.8(11) . . . . ?
C23 N6 C21 C20A -107.6(10) . . . . ?
C23 N6 C22 Pd1 167.6(6) . . . . ?
C23 N6 C22 N7 -0.1(8) . . . . ?
C24 N7 C22 Pd1 -169.0(5) . . . . ?
C24 N7 C22 N6 0.4(8) . . . . ?
C24 N7 C25 C26 111.0(7) . . . . ?
C25 N7 C22 Pd1 3.1(9) . . . . ?
C25 N7 C22 N6 172.5(6) . . . . ?
C25 N7 C24 C23 -172.3(7) . . . . ?
C25 C26 C27 C28 174.7(7) . . . . ?
C26 N8 C30 C29 0.3(11) . . . . ?
C26 C27 C28 C29 -0.1(12) . . . . ?
C27 C28 C29 C30 1.6(12) . . . . ?
C28 C29 C30 N8 -1.8(12) . . . . ?
C30 N8 C26 C25 -175.0(6) . . . . ?
C30 N8 C26 C27 1.3(10) . . . . ?
N5B C16B C17B C18B 2(2) . . . . ?
C16B N5B C20B C21 179.2(14) . . . . ?
C16B N5B C20B C19B 2(2) . . . . ?
C16B C17B C18B C19B -3(2) . . . . ?
C17B C18B C19B C20B 3(3) . . . . ?
C18B C19B C20B C21 -179.9(15) . . . . ?
C18B C19B C20B N5B -3(3) . . . . ?
C20B C21 C20A N5A 180(100) . . . . ?
C20B C21 C20A C19A 2(4) . . . . ?
C20B N5B C16B C17B -2(2) . . . . ?
N5A C16A C17A C18A -1(3) . . . . ?
C16A N5A C20A C21 177.9(16) . . . . ?
C16A N5A C20A C19A -5(3) . . . . ?
C16A C17A C18A C19A 4(3) . . . . ?
C17A C18A C19A C20A -6(2) . . . . ?
C18A C19A C20A C21 -174.9(14) . . . . ?
C18A C19A C20A N5A 8(3) . . . . ?
C20A C21 C20B N5B -3(4) . . . . ?
C20A C21 C20B C19B 174(6) . . . . ?
C20A N5A C16A C17A 1(3) . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
15 -1 21 0.0954 15.0555 -0.9808 20.9009 0.4192 0.0867 0.9104
7 17 -2 0.0246 7.0713 17.0276 -2.0444 -0.2687 0.9657 0.0018
-19 6 24 0.0680 -18.9132 5.9915 24.0803 -0.4811 0.1233 0.8659
0 -17 -1 0.0148 -0.0778 -17.0206 -0.9913 0.4111 -0.8964 -0.0834
43 -1 -7 0.0263 42.9864 -0.9561 -7.2279 0.9367 0.3690 -0.0506
1 7 -23 0.0920 0.9693 7.0049 -22.9892 -0.2240 0.3865 -0.8889
-1 -7 23 0.0920 -0.9693 -7.0049 22.9892 0.2240 -0.3865 0.8889
5 17 1 0.0248 5.0789 17.0260 0.9640 -0.3024 0.9452 0.1101
-15 1 -21 0.0954 -15.0555 0.9808 -20.9009 -0.4192 -0.0867 -0.9104
-43 0 8 0.0148 -42.9881 -0.0449 8.2275 -0.9091 -0.4221 0.0876
21 -1 -26 0.1033 20.9304 -0.9837 -26.0919 0.3962 0.1607 -0.9216

_olex2_submission_special_instructions 'No special instructions were received'
