# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
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# Audit and citation data items may have been added by the CCDC. 
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data_complex_2
_database_code_depnum_ccdc_archive 'CCDC 1544213'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2016-12-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C26 H36 N4 O6 Pd2)'
_chemical_formula_sum            'C52 H72 N8 O12 Pd4'
_chemical_formula_weight         1426.77
_chemical_melting_point          ?
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.609(3)
_cell_length_b                   12.998(3)
_cell_length_c                   18.154(4)
_cell_angle_alpha                81.932(7)
_cell_angle_beta                 84.577(7)
_cell_angle_gamma                82.253(7)
_cell_volume                     2910.0(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      2.26
_shelx_estimated_absorpt_T_max   0.841
_shelx_estimated_absorpt_T_min   0.685
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. 
wR2(int) was 0.0671 before and 0.0577 after correction. 
The Ratio of minimum to maximum transmission is 0.8689. 
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0871
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35886
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.432
_diffrn_reflns_theta_min         2.139
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8251
_reflns_number_total             11497
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material  
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_refine_diff_density_max         1.481
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         11497
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0510
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0375P)²+11.6691P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0998
_refine_ls_wR_factor_ref         0.1112
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-H3
 0.84 with sigma of 0.02
 N4-H4
 0.84 with sigma of 0.02
 N7-H7
 0.84 with sigma of 0.02
 N8-H8
 0.84 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C16(H16A,H16B), C20(H20A,H20B), C24(H24A,H24B), C33(H33A,H33B),
 C42(H42A,H42B), C46(H46A,H46B), C50(H50A,H50B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C4(H4A), C5(H5), C11(H11), C12(H12), C13(H13), C14(H14),
 C28(H28), C29(H29), C30(H30), C31(H31), C37(H37), C38(H38), C39(H39), C40(H40)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C48(H48A,H48B,H48C), C52(H52A,
 H52B,H52C)
;
_atom_sites_solution_hydrogens   mixed
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.19562(3) 0.76441(3) 0.81453(2) 0.01366(12) Uani 1 1 d . . . . .
Pd2 Pd 0.15927(3) 0.76955(3) 0.65426(2) 0.01300(11) Uani 1 1 d . . . . .
Pd3 Pd 0.67073(4) 0.43203(4) 0.72852(2) 0.01532(12) Uani 1 1 d . . . . .
Pd4 Pd 0.50637(4) 0.29185(4) 0.78136(2) 0.01465(12) Uani 1 1 d . . . . .
N1 N 0.0534(4) 0.7480(4) 0.8783(3) 0.0160(11) Uani 1 1 d . . . . .
N2 N 0.1468(4) 0.9279(4) 0.6176(3) 0.0145(11) Uani 1 1 d . . . . .
N3 N 0.5483(4) 0.7592(4) 0.6141(3) 0.0134(11) Uani 1 1 d D . . . .
H3 H 0.568(4) 0.711(3) 0.589(3) 0.016 Uiso 1 1 d DR . . . .
N4 N 0.2274(4) 0.3910(4) 0.8223(3) 0.0184(12) Uani 1 1 d D . . . .
H4 H 0.291(2) 0.397(5) 0.828(3) 0.022 Uiso 1 1 d DR . . . .
N5 N 0.7925(4) 0.4030(4) 0.7997(3) 0.0173(11) Uani 1 1 d . . . . .
N6 N 0.5426(4) 0.1692(4) 0.7195(3) 0.0208(12) Uani 1 1 d . . . . .
N7 N 0.3061(4) 0.4946(4) 0.5777(3) 0.0169(11) Uani 1 1 d D . . . .
H7 H 0.249(3) 0.520(5) 0.598(3) 0.020 Uiso 1 1 d DR . . . .
N8 N 0.4662(4) 0.6640(4) 0.8900(3) 0.0190(12) Uani 1 1 d D . . . .
H8 H 0.429(4) 0.712(4) 0.866(3) 0.023 Uiso 1 1 d DR . . . .
O1 O 0.3491(3) 0.7820(3) 0.7675(2) 0.0161(9) Uani 1 1 d . . . . .
O2 O 0.3302(3) 0.7517(3) 0.6503(2) 0.0149(9) Uani 1 1 d . . . . .
O3 O 0.5128(3) 0.9321(3) 0.6165(2) 0.0208(10) Uani 1 1 d . . . . .
O4 O 0.2191(3) 0.6028(3) 0.7965(2) 0.0151(9) Uani 1 1 d . . . . .
O5 O 0.1578(3) 0.6106(3) 0.6829(2) 0.0157(9) Uani 1 1 d . . . . .
O6 O 0.0676(3) 0.3817(3) 0.8884(2) 0.0255(10) Uani 1 1 d . . . . .
O7 O 0.5667(3) 0.4780(3) 0.6466(2) 0.0198(9) Uani 1 1 d . . . . .
O8 O 0.4249(3) 0.3960(3) 0.6950(2) 0.0200(10) Uani 1 1 d . . . . .
O9 O 0.3867(3) 0.3701(3) 0.5096(2) 0.0252(10) Uani 1 1 d . . . . .
O10 O 0.4564(3) 0.4002(3) 0.8542(2) 0.0165(9) Uani 1 1 d . . . . .
O11 O 0.5622(3) 0.5204(3) 0.8015(2) 0.0172(9) Uani 1 1 d . . . . .
O12 O 0.6212(4) 0.6054(3) 0.9426(2) 0.0291(11) Uani 1 1 d . . . . .
C1 C 0.1666(5) 0.9077(5) 0.8411(3) 0.0192(14) Uani 1 1 d . . . . .
C2 C 0.2369(5) 0.9792(5) 0.8374(3) 0.0189(14) Uani 1 1 d . . . . .
H2 H 0.310032 0.960166 0.821522 0.023 Uiso 1 1 calc R . . . .
C3 C 0.2045(5) 1.0797(5) 0.8562(3) 0.0238(15) Uani 1 1 d . . . . .
H3A H 0.254515 1.129167 0.851905 0.029 Uiso 1 1 calc R . . . .
C4 C 0.0978(5) 1.1066(5) 0.8814(4) 0.0284(16) Uani 1 1 d . . . . .
H4A H 0.074330 1.174970 0.893960 0.034 Uiso 1 1 calc R . . . .
C5 C 0.0267(5) 1.0340(5) 0.8881(4) 0.0273(16) Uani 1 1 d . . . . .
H5 H -0.045525 1.051841 0.906525 0.033 Uiso 1 1 calc R . . . .
C6 C 0.0592(5) 0.9357(5) 0.8684(3) 0.0196(14) Uani 1 1 d . . . . .
C7 C -0.0131(5) 0.8515(5) 0.8714(4) 0.0210(14) Uani 1 1 d . . . . .
H7A H -0.066700 0.855261 0.914770 0.025 Uiso 1 1 calc R . . . .
H7B H -0.051851 0.861704 0.825513 0.025 Uiso 1 1 calc R . . . .
C8 C -0.0090(5) 0.6676(5) 0.8582(4) 0.0219(14) Uani 1 1 d . . . . .
H8A H -0.077161 0.668460 0.889013 0.033 Uiso 1 1 calc GR . . . .
H8B H 0.032508 0.598258 0.867068 0.033 Uiso 1 1 calc GR . . . .
H8C H -0.023192 0.683376 0.805424 0.033 Uiso 1 1 calc GR . . . .
C9 C 0.0817(5) 0.7171(5) 0.9569(3) 0.0243(15) Uani 1 1 d . . . . .
H9A H 0.016106 0.708109 0.989487 0.037 Uiso 1 1 calc GR . . . .
H9B H 0.117671 0.771853 0.972523 0.037 Uiso 1 1 calc GR . . . .
H9C H 0.129766 0.651069 0.960487 0.037 Uiso 1 1 calc GR . . . .
C10 C 0.0028(5) 0.7951(4) 0.6537(3) 0.0147(13) Uani 1 1 d . . . . .
C11 C -0.0671(5) 0.7208(5) 0.6542(3) 0.0185(14) Uani 1 1 d . . . . .
H11 H -0.039905 0.649555 0.651510 0.022 Uiso 1 1 calc R . . . .
C12 C -0.1773(5) 0.7519(5) 0.6586(4) 0.0242(15) Uani 1 1 d . . . . .
H12 H -0.225392 0.701130 0.660315 0.029 Uiso 1 1 calc R . . . .
C13 C -0.2176(5) 0.8558(5) 0.6605(3) 0.0256(16) Uani 1 1 d . . . . .
H13 H -0.292959 0.876088 0.664317 0.031 Uiso 1 1 calc R . . . .
C14 C -0.1480(5) 0.9300(5) 0.6569(3) 0.0221(14) Uani 1 1 d . . . . .
H14 H -0.175743 1.001713 0.656675 0.027 Uiso 1 1 calc R . . . .
C15 C -0.0380(5) 0.9006(5) 0.6537(3) 0.0183(14) Uani 1 1 d . . . . .
C16 C 0.0424(4) 0.9750(5) 0.6531(3) 0.0178(13) Uani 1 1 d . . . . .
H16A H 0.051590 0.986837 0.704724 0.021 Uiso 1 1 calc R . . . .
H16B H 0.017857 1.043192 0.624332 0.021 Uiso 1 1 calc R . . . .
C17 C 0.2346(5) 0.9818(5) 0.6369(3) 0.0190(14) Uani 1 1 d . . . . .
H17A H 0.302320 0.955243 0.610912 0.029 Uiso 1 1 calc GR . . . .
H17B H 0.240835 0.968490 0.690910 0.029 Uiso 1 1 calc GR . . . .
H17C H 0.218869 1.057260 0.621655 0.029 Uiso 1 1 calc GR . . . .
C18 C 0.1428(5) 0.9433(5) 0.5350(3) 0.0217(14) Uani 1 1 d . . . . .
H18A H 0.137103 1.018266 0.516643 0.033 Uiso 1 1 calc GR . . . .
H18B H 0.080312 0.914260 0.521917 0.033 Uiso 1 1 calc GR . . . .
H18C H 0.208442 0.907446 0.512044 0.033 Uiso 1 1 calc GR . . . .
C19 C 0.3843(5) 0.7610(4) 0.7028(3) 0.0138(13) Uani 1 1 d . . . . .
C20 C 0.5062(4) 0.7393(5) 0.6902(3) 0.0157(13) Uani 1 1 d . . . . .
H20A H 0.538827 0.782921 0.720205 0.019 Uiso 1 1 calc R . . . .
H20B H 0.528689 0.665066 0.708952 0.019 Uiso 1 1 calc R . . . .
C21 C 0.5502(5) 0.8586(5) 0.5823(3) 0.0166(13) Uani 1 1 d . . . . .
C22 C 0.6055(5) 0.8752(5) 0.5056(3) 0.0210(14) Uani 1 1 d . . . . .
H22A H 0.561160 0.928059 0.473977 0.032 Uiso 1 1 calc GR . . . .
H22B H 0.616224 0.809109 0.484067 0.032 Uiso 1 1 calc GR . . . .
H22C H 0.675239 0.899109 0.508483 0.032 Uiso 1 1 calc GR . . . .
C23 C 0.1884(4) 0.5626(4) 0.7447(3) 0.0147(13) Uani 1 1 d . . . . .
C24 C 0.1835(5) 0.4453(4) 0.7548(3) 0.0164(13) Uani 1 1 d . . . . .
H24A H 0.107682 0.432736 0.755357 0.020 Uiso 1 1 calc R . . . .
H24B H 0.223369 0.415585 0.711419 0.020 Uiso 1 1 calc R . . . .
C25 C 0.1662(5) 0.3667(5) 0.8854(3) 0.0185(14) Uani 1 1 d . . . . .
C26 C 0.2267(5) 0.3182(5) 0.9518(4) 0.0298(17) Uani 1 1 d . . . . .
H26A H 0.226620 0.370442 0.985813 0.045 Uiso 1 1 calc GR . . . .
H26B H 0.300811 0.293861 0.934979 0.045 Uiso 1 1 calc GR . . . .
H26C H 0.191983 0.258789 0.977733 0.045 Uiso 1 1 calc GR . . . .
C27 C 0.7800(5) 0.3600(4) 0.6617(3) 0.0185(14) Uani 1 1 d . . . . .
C28 C 0.7770(5) 0.3617(5) 0.5856(3) 0.0213(14) Uani 1 1 d . . . . .
H28 H 0.716402 0.396724 0.561085 0.026 Uiso 1 1 calc R . . . .
C29 C 0.8630(5) 0.3118(5) 0.5452(4) 0.0268(16) Uani 1 1 d . . . . .
H29 H 0.859906 0.311439 0.493161 0.032 Uiso 1 1 calc R . . . .
C30 C 0.9528(5) 0.2630(5) 0.5793(4) 0.0272(16) Uani 1 1 d . . . . .
H30 H 1.012288 0.231160 0.550871 0.033 Uiso 1 1 calc R . . . .
C31 C 0.9552(5) 0.2609(5) 0.6569(4) 0.0266(16) Uani 1 1 d . . . . .
H31 H 1.015975 0.225870 0.681225 0.032 Uiso 1 1 calc R . . . .
C32 C 0.8701(5) 0.3092(5) 0.6977(3) 0.0207(14) Uani 1 1 d . . . . .
C33 C 0.8634(5) 0.3074(5) 0.7808(3) 0.0209(14) Uani 1 1 d . . . . .
H33A H 0.833330 0.243777 0.805761 0.025 Uiso 1 1 calc R . . . .
H33B H 0.935809 0.306896 0.797801 0.025 Uiso 1 1 calc R . . . .
C34 C 0.8535(5) 0.4945(5) 0.7844(4) 0.0257(15) Uani 1 1 d . . . . .
H34A H 0.912995 0.484017 0.816834 0.039 Uiso 1 1 calc GR . . . .
H34B H 0.805838 0.557943 0.794241 0.039 Uiso 1 1 calc GR . . . .
H34C H 0.882083 0.502085 0.732089 0.039 Uiso 1 1 calc GR . . . .
C35 C 0.7578(5) 0.3895(5) 0.8814(3) 0.0284(16) Uani 1 1 d . . . . .
H35A H 0.821193 0.374082 0.910209 0.043 Uiso 1 1 calc GR . . . .
H35B H 0.714034 0.331611 0.892791 0.043 Uiso 1 1 calc GR . . . .
H35C H 0.715312 0.454191 0.894552 0.043 Uiso 1 1 calc GR . . . .
C36 C 0.5792(5) 0.1925(5) 0.8576(3) 0.0183(14) Uani 1 1 d . . . . .
C37 C 0.5740(5) 0.1981(5) 0.9339(3) 0.0235(15) Uani 1 1 d . . . . .
H37 H 0.528407 0.253157 0.954320 0.028 Uiso 1 1 calc R . . . .
C38 C 0.6351(6) 0.1238(6) 0.9804(4) 0.0350(18) Uani 1 1 d . . . . .
H38 H 0.631890 0.128412 1.032399 0.042 Uiso 1 1 calc R . . . .
C39 C 0.7009(6) 0.0429(6) 0.9506(4) 0.0369(18) Uani 1 1 d . . . . .
H39 H 0.743999 -0.006861 0.982237 0.044 Uiso 1 1 calc R . . . .
C40 C 0.7044(5) 0.0340(5) 0.8750(4) 0.0315(17) Uani 1 1 d . . . . .
H40 H 0.747843 -0.022832 0.855199 0.038 Uiso 1 1 calc R . . . .
C41 C 0.6437(5) 0.1091(5) 0.8287(4) 0.0233(15) Uani 1 1 d . . . . .
C42 C 0.6442(5) 0.1088(5) 0.7468(4) 0.0238(15) Uani 1 1 d . . . . .
H42A H 0.650151 0.035859 0.735355 0.029 Uiso 1 1 calc R . . . .
H42B H 0.706803 0.141000 0.721080 0.029 Uiso 1 1 calc R . . . .
C43 C 0.5550(5) 0.1985(5) 0.6376(3) 0.0280(16) Uani 1 1 d . . . . .
H43A H 0.572692 0.135043 0.613259 0.042 Uiso 1 1 calc GR . . . .
H43B H 0.612884 0.242795 0.625109 0.042 Uiso 1 1 calc GR . . . .
H43C H 0.487755 0.237063 0.620384 0.042 Uiso 1 1 calc GR . . . .
C44 C 0.4545(5) 0.1005(5) 0.7381(4) 0.0298(16) Uani 1 1 d . . . . .
H44A H 0.385724 0.141098 0.725891 0.045 Uiso 1 1 calc GR . . . .
H44B H 0.451454 0.074085 0.791408 0.045 Uiso 1 1 calc GR . . . .
H44C H 0.468997 0.041372 0.708952 0.045 Uiso 1 1 calc GR . . . .
C45 C 0.4704(5) 0.4605(5) 0.6492(3) 0.0187(14) Uani 1 1 d . . . . .
C46 C 0.4057(4) 0.5285(4) 0.5906(3) 0.0155(13) Uani 1 1 d . . . . .
H46A H 0.390069 0.599879 0.605183 0.019 Uiso 1 1 calc R . . . .
H46B H 0.450798 0.533425 0.542859 0.019 Uiso 1 1 calc R . . . .
C47 C 0.3033(5) 0.4167(5) 0.5370(3) 0.0212(14) Uani 1 1 d . . . . .
C48 C 0.1934(5) 0.3893(6) 0.5271(4) 0.0351(18) Uani 1 1 d . . . . .
H48A H 0.178404 0.406342 0.474500 0.053 Uiso 1 1 calc GR . . . .
H48B H 0.139261 0.429581 0.557664 0.053 Uiso 1 1 calc GR . . . .
H48C H 0.191082 0.314322 0.542750 0.053 Uiso 1 1 calc GR . . . .
C49 C 0.4900(5) 0.4886(5) 0.8467(3) 0.0156(13) Uani 1 1 d . . . . .
C50 C 0.4299(5) 0.5627(4) 0.8991(3) 0.0181(13) Uani 1 1 d . . . . .
H50A H 0.352611 0.571611 0.890697 0.022 Uiso 1 1 calc R . . . .
H50B H 0.437785 0.529918 0.951237 0.022 Uiso 1 1 calc R . . . .
C51 C 0.5636(5) 0.6764(5) 0.9074(3) 0.0228(15) Uani 1 1 d . . . . .
C52 C 0.5995(6) 0.7826(5) 0.8830(4) 0.0318(17) Uani 1 1 d . . . . .
H52A H 0.622507 0.809360 0.926042 0.048 Uiso 1 1 calc GR . . . .
H52B H 0.539827 0.830820 0.862334 0.048 Uiso 1 1 calc GR . . . .
H52C H 0.659635 0.776837 0.844857 0.048 Uiso 1 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 Pd2 2.9780(9) . ?
Pd1 N1 2.059(5) . ?
Pd1 O1 2.068(4) . ?
Pd1 O4 2.148(4) . ?
Pd1 C1 1.968(6) . ?
Pd2 N2 2.062(5) . ?
Pd2 O2 2.131(4) . ?
Pd2 O5 2.060(4) . ?
Pd2 C10 1.957(6) . ?
Pd3 Pd4 2.9473(8) . ?
Pd3 N5 2.062(5) . ?
Pd3 O7 2.050(4) . ?
Pd3 O11 2.146(4) . ?
Pd3 C27 1.975(6) . ?
Pd4 N6 2.054(5) . ?
Pd4 O8 2.164(4) . ?
Pd4 O10 2.063(4) . ?
Pd4 C36 1.961(6) . ?
N1 C7 1.482(7) . ?
N1 C8 1.491(7) . ?
N1 C9 1.491(7) . ?
N2 C16 1.502(7) . ?
N2 C17 1.480(7) . ?
N2 C18 1.490(7) . ?
N3 H3 0.82(2) . ?
N3 C20 1.433(7) . ?
N3 C21 1.342(7) . ?
N4 H4 0.83(2) . ?
N4 C24 1.444(7) . ?
N4 C25 1.344(8) . ?
N5 C33 1.490(8) . ?
N5 C34 1.483(7) . ?
N5 C35 1.499(8) . ?
N6 C42 1.498(8) . ?
N6 C43 1.481(8) . ?
N6 C44 1.502(8) . ?
N7 H7 0.83(2) . ?
N7 C46 1.434(7) . ?
N7 C47 1.340(8) . ?
N8 H8 0.82(2) . ?
N8 C50 1.435(8) . ?
N8 C51 1.331(8) . ?
O1 C19 1.269(7) . ?
O2 C19 1.251(7) . ?
O3 C21 1.230(7) . ?
O4 C23 1.252(7) . ?
O5 C23 1.273(7) . ?
O6 C25 1.230(7) . ?
O7 C45 1.260(7) . ?
O8 C45 1.252(7) . ?
O9 C47 1.239(7) . ?
O10 C49 1.262(7) . ?
O11 C49 1.240(7) . ?
O12 C51 1.237(7) . ?
C1 C2 1.359(8) . ?
C1 C6 1.414(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.395(9) . ?
C3 H3A 0.9500 . ?
C3 C4 1.395(9) . ?
C4 H4A 0.9500 . ?
C4 C5 1.372(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.374(9) . ?
C6 C7 1.508(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.391(8) . ?
C10 C15 1.398(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.392(8) . ?
C12 H12 0.9500 . ?
C12 C13 1.381(9) . ?
C13 H13 0.9500 . ?
C13 C14 1.379(9) . ?
C14 H14 0.9500 . ?
C14 C15 1.387(8) . ?
C15 C16 1.491(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.527(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 C22 1.498(8) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.519(8) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.503(8) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.383(8) . ?
C27 C32 1.403(8) . ?
C28 H28 0.9500 . ?
C28 C29 1.388(9) . ?
C29 H29 0.9500 . ?
C29 C30 1.377(9) . ?
C30 H30 0.9500 . ?
C30 C31 1.408(9) . ?
C31 H31 0.9500 . ?
C31 C32 1.376(9) . ?
C32 C33 1.500(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.392(9) . ?
C36 C41 1.398(8) . ?
C37 H37 0.9500 . ?
C37 C38 1.391(9) . ?
C38 H38 0.9500 . ?
C38 C39 1.388(10) . ?
C39 H39 0.9500 . ?
C39 C40 1.390(10) . ?
C40 H40 0.9500 . ?
C40 C41 1.392(9) . ?
C41 C42 1.487(9) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C46 1.511(8) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.510(9) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 C50 1.527(8) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.506(9) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 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
N1 Pd1 Pd2 109.24(13) . . ?
N1 Pd1 O1 170.27(17) . . ?
N1 Pd1 O4 92.66(17) . . ?
O1 Pd1 Pd2 80.49(11) . . ?
O1 Pd1 O4 90.14(15) . . ?
O4 Pd1 Pd2 75.56(10) . . ?
C1 Pd1 Pd2 109.00(16) . . ?
C1 Pd1 N1 82.3(2) . . ?
C1 Pd1 O1 94.4(2) . . ?
C1 Pd1 O4 174.0(2) . . ?
N2 Pd2 Pd1 101.66(13) . . ?
N2 Pd2 O2 93.90(17) . . ?
O2 Pd2 Pd1 78.61(10) . . ?
O5 Pd2 Pd1 83.63(11) . . ?
O5 Pd2 N2 173.32(16) . . ?
O5 Pd2 O2 91.15(15) . . ?
C10 Pd2 Pd1 103.15(16) . . ?
C10 Pd2 N2 82.4(2) . . ?
C10 Pd2 O2 176.1(2) . . ?
C10 Pd2 O5 92.5(2) . . ?
N5 Pd3 Pd4 109.42(14) . . ?
N5 Pd3 O11 94.55(17) . . ?
O7 Pd3 Pd4 80.55(11) . . ?
O7 Pd3 N5 169.96(18) . . ?
O7 Pd3 O11 88.76(15) . . ?
O11 Pd3 Pd4 76.65(11) . . ?
C27 Pd3 Pd4 108.48(17) . . ?
C27 Pd3 N5 82.6(2) . . ?
C27 Pd3 O7 93.4(2) . . ?
C27 Pd3 O11 174.7(2) . . ?
N6 Pd4 Pd3 104.83(14) . . ?
N6 Pd4 O8 94.95(18) . . ?
N6 Pd4 O10 171.37(18) . . ?
O8 Pd4 Pd3 79.43(11) . . ?
O10 Pd4 Pd3 83.42(11) . . ?
O10 Pd4 O8 89.00(15) . . ?
C36 Pd4 Pd3 101.95(16) . . ?
C36 Pd4 N6 82.8(2) . . ?
C36 Pd4 O8 177.6(2) . . ?
C36 Pd4 O10 93.1(2) . . ?
C7 N1 Pd1 107.6(4) . . ?
C7 N1 C8 109.5(5) . . ?
C7 N1 C9 109.7(5) . . ?
C8 N1 Pd1 115.1(4) . . ?
C8 N1 C9 108.2(5) . . ?
C9 N1 Pd1 106.5(4) . . ?
C16 N2 Pd2 106.2(3) . . ?
C17 N2 Pd2 115.0(3) . . ?
C17 N2 C16 108.9(5) . . ?
C17 N2 C18 108.8(4) . . ?
C18 N2 Pd2 108.4(4) . . ?
C18 N2 C16 109.4(4) . . ?
C20 N3 H3 121(4) . . ?
C21 N3 H3 119(4) . . ?
C21 N3 C20 119.1(5) . . ?
C24 N4 H4 117(4) . . ?
C25 N4 H4 115(4) . . ?
C25 N4 C24 122.9(5) . . ?
C33 N5 Pd3 108.0(3) . . ?
C33 N5 C35 109.4(5) . . ?
C34 N5 Pd3 106.4(4) . . ?
C34 N5 C33 109.5(5) . . ?
C34 N5 C35 107.5(5) . . ?
C35 N5 Pd3 115.8(4) . . ?
C42 N6 Pd4 106.2(4) . . ?
C42 N6 C44 108.2(5) . . ?
C43 N6 Pd4 115.6(4) . . ?
C43 N6 C42 110.2(5) . . ?
C43 N6 C44 109.0(5) . . ?
C44 N6 Pd4 107.4(4) . . ?
C46 N7 H7 121(4) . . ?
C47 N7 H7 118(4) . . ?
C47 N7 C46 121.5(5) . . ?
C50 N8 H8 116(5) . . ?
C51 N8 H8 121(5) . . ?
C51 N8 C50 121.5(5) . . ?
C19 O1 Pd1 124.4(4) . . ?
C19 O2 Pd2 125.4(4) . . ?
C23 O4 Pd1 128.2(4) . . ?
C23 O5 Pd2 122.4(4) . . ?
C45 O7 Pd3 126.7(4) . . ?
C45 O8 Pd4 123.4(4) . . ?
C49 O10 Pd4 122.6(4) . . ?
C49 O11 Pd3 127.7(4) . . ?
C2 C1 Pd1 127.7(5) . . ?
C2 C1 C6 118.3(6) . . ?
C6 C1 Pd1 114.0(4) . . ?
C1 C2 H2 119.1 . . ?
C1 C2 C3 121.7(6) . . ?
C3 C2 H2 119.1 . . ?
C2 C3 H3A 120.5 . . ?
C4 C3 C2 119.1(6) . . ?
C4 C3 H3A 120.5 . . ?
C3 C4 H4A 120.1 . . ?
C5 C4 C3 119.8(6) . . ?
C5 C4 H4A 120.1 . . ?
C4 C5 H5 119.7 . . ?
C4 C5 C6 120.5(6) . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C7 114.8(5) . . ?
C5 C6 C1 120.5(6) . . ?
C5 C6 C7 124.7(6) . . ?
N1 C7 C6 108.8(5) . . ?
N1 C7 H7A 109.9 . . ?
N1 C7 H7B 109.9 . . ?
C6 C7 H7A 109.9 . . ?
C6 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 Pd2 127.0(4) . . ?
C11 C10 C15 119.8(5) . . ?
C15 C10 Pd2 113.2(4) . . ?
C10 C11 H11 120.3 . . ?
C10 C11 C12 119.4(6) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.7(6) . . ?
C13 C12 H12 119.6 . . ?
C12 C13 H13 120.1 . . ?
C14 C13 C12 119.8(6) . . ?
C14 C13 H13 120.1 . . ?
C13 C14 H14 119.8 . . ?
C13 C14 C15 120.5(6) . . ?
C15 C14 H14 119.8 . . ?
C10 C15 C16 116.4(5) . . ?
C14 C15 C10 119.7(6) . . ?
C14 C15 C16 123.9(6) . . ?
N2 C16 H16A 110.1 . . ?
N2 C16 H16B 110.1 . . ?
C15 C16 N2 107.9(5) . . ?
C15 C16 H16A 110.1 . . ?
C15 C16 H16B 110.1 . . ?
H16A C16 H16B 108.4 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O1 C19 C20 115.3(5) . . ?
O2 C19 O1 127.2(5) . . ?
O2 C19 C20 117.3(5) . . ?
N3 C20 C19 115.0(5) . . ?
N3 C20 H20A 108.5 . . ?
N3 C20 H20B 108.5 . . ?
C19 C20 H20A 108.5 . . ?
C19 C20 H20B 108.5 . . ?
H20A C20 H20B 107.5 . . ?
N3 C21 C22 116.9(5) . . ?
O3 C21 N3 120.9(6) . . ?
O3 C21 C22 122.1(5) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O4 C23 O5 126.6(5) . . ?
O4 C23 C24 118.9(5) . . ?
O5 C23 C24 114.5(5) . . ?
N4 C24 C23 113.7(5) . . ?
N4 C24 H24A 108.8 . . ?
N4 C24 H24B 108.8 . . ?
C23 C24 H24A 108.8 . . ?
C23 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
N4 C25 C26 115.4(5) . . ?
O6 C25 N4 122.3(5) . . ?
O6 C25 C26 122.4(6) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 Pd3 126.2(5) . . ?
C28 C27 C32 120.1(6) . . ?
C32 C27 Pd3 113.5(4) . . ?
C27 C28 H28 120.2 . . ?
C27 C28 C29 119.6(6) . . ?
C29 C28 H28 120.2 . . ?
C28 C29 H29 119.4 . . ?
C30 C29 C28 121.1(6) . . ?
C30 C29 H29 119.4 . . ?
C29 C30 H30 120.5 . . ?
C29 C30 C31 119.0(6) . . ?
C31 C30 H30 120.5 . . ?
C30 C31 H31 119.8 . . ?
C32 C31 C30 120.4(6) . . ?
C32 C31 H31 119.8 . . ?
C27 C32 C33 116.0(5) . . ?
C31 C32 C27 119.7(6) . . ?
C31 C32 C33 124.2(6) . . ?
N5 C33 C32 107.8(5) . . ?
N5 C33 H33A 110.1 . . ?
N5 C33 H33B 110.1 . . ?
C32 C33 H33A 110.1 . . ?
C32 C33 H33B 110.1 . . ?
H33A C33 H33B 108.5 . . ?
N5 C34 H34A 109.5 . . ?
N5 C34 H34B 109.5 . . ?
N5 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N5 C35 H35A 109.5 . . ?
N5 C35 H35B 109.5 . . ?
N5 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 Pd4 127.4(5) . . ?
C37 C36 C41 119.2(6) . . ?
C41 C36 Pd4 113.4(5) . . ?
C36 C37 H37 119.8 . . ?
C38 C37 C36 120.5(6) . . ?
C38 C37 H37 119.8 . . ?
C37 C38 H38 120.2 . . ?
C39 C38 C37 119.7(7) . . ?
C39 C38 H38 120.2 . . ?
C38 C39 H39 119.7 . . ?
C38 C39 C40 120.7(6) . . ?
C40 C39 H39 119.7 . . ?
C39 C40 H40 120.3 . . ?
C39 C40 C41 119.3(6) . . ?
C41 C40 H40 120.3 . . ?
C36 C41 C42 115.7(6) . . ?
C40 C41 C36 120.6(6) . . ?
C40 C41 C42 123.7(6) . . ?
N6 C42 H42A 109.8 . . ?
N6 C42 H42B 109.8 . . ?
C41 C42 N6 109.4(5) . . ?
C41 C42 H42A 109.8 . . ?
C41 C42 H42B 109.8 . . ?
H42A C42 H42B 108.2 . . ?
N6 C43 H43A 109.5 . . ?
N6 C43 H43B 109.5 . . ?
N6 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N6 C44 H44A 109.5 . . ?
N6 C44 H44B 109.5 . . ?
N6 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O7 C45 C46 114.1(5) . . ?
O8 C45 O7 127.1(5) . . ?
O8 C45 C46 118.8(5) . . ?
N7 C46 C45 116.4(5) . . ?
N7 C46 H46A 108.2 . . ?
N7 C46 H46B 108.2 . . ?
C45 C46 H46A 108.2 . . ?
C45 C46 H46B 108.2 . . ?
H46A C46 H46B 107.3 . . ?
N7 C47 C48 116.2(6) . . ?
O9 C47 N7 121.4(6) . . ?
O9 C47 C48 122.4(6) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O10 C49 C50 113.7(5) . . ?
O11 C49 O10 127.5(6) . . ?
O11 C49 C50 118.8(5) . . ?
N8 C50 C49 114.2(5) . . ?
N8 C50 H50A 108.7 . . ?
N8 C50 H50B 108.7 . . ?
C49 C50 H50A 108.7 . . ?
C49 C50 H50B 108.7 . . ?
H50A C50 H50B 107.6 . . ?
N8 C51 C52 116.3(6) . . ?
O12 C51 N8 122.2(6) . . ?
O12 C51 C52 121.4(6) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

_shelx_SHELXL_version_number     2016/6
_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_complex_S1_4
_database_code_depnum_ccdc_archive 'CCDC 1544216'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2016-12-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'I6 Pd2, 2(I), 2(C19 H17 F6 I2 N2)'
_chemical_formula_sum            'C38 H34 F12 I12 N4 Pd2'
_chemical_formula_weight         2510.29
_chemical_melting_point          ?
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'
I I -0.4742 1.8119 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   28.337(5)
_cell_length_b                   13.971(3)
_cell_length_c                   14.982(3)
_cell_angle_alpha                90
_cell_angle_beta                 102.276(5)
_cell_angle_gamma                90
_cell_volume                     5795.8(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9296
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      2.24
_shelx_estimated_absorpt_T_max   0.437
_shelx_estimated_absorpt_T_min   0.210
_exptl_absorpt_coefficient_mu    7.083
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1267 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.7148.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.877
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             4504
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            155125
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.196
_diffrn_reflns_theta_min         2.207
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10741
_reflns_number_total             12881
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_refine_diff_density_max         2.702
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.177
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         12881
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0279
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0242P)²+17.4770P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0603
_refine_special_details          ?
_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:
 C8(H8A,H8B), C12(H12A,H12B), C27(H27A,H27B), C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C15(H15), C16(H16), C17(H17), C22(H22),
 C23(H23), C24(H24), C29(H29), C34(H34), C35(H35), C36(H36)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.20096(2) 0.35790(2) 0.47878(2) 0.01411(7) Uani 1 1 d . . . . .
Pd2 Pd 0.30070(2) 0.17360(2) 0.50916(2) 0.01497(7) Uani 1 1 d . . . . .
I1 I 0.13283(2) 0.40639(2) 0.34200(2) 0.01923(7) Uani 1 1 d . . . . .
I2 I 0.17185(2) 0.47362(2) 0.59183(2) 0.02049(7) Uani 1 1 d . . . . .
I3 I 0.23367(2) 0.23668(2) 0.37580(2) 0.02140(7) Uani 1 1 d . . . . .
I4 I 0.27035(2) 0.30044(2) 0.61054(2) 0.01900(7) Uani 1 1 d . . . . .
I5 I 0.33100(2) 0.06094(2) 0.39539(2) 0.02329(7) Uani 1 1 d . . . . .
I6 I 0.36502(2) 0.11636(2) 0.64896(2) 0.02008(7) Uani 1 1 d . . . . .
I7 I 0.04916(2) 0.48752(2) 0.52270(2) 0.02355(7) Uani 1 1 d . . . . .
I8 I 0.45196(2) 1.02399(2) 0.47197(2) 0.02339(7) Uani 1 1 d . . . . .
I9 I 0.21362(2) 1.06323(3) 0.61700(2) 0.03342(9) Uani 1 1 d . . . . .
I10 I 0.21559(2) 0.91667(2) 0.37329(2) 0.02688(8) Uani 1 1 d . . . . .
F1 F 0.00643(11) 0.8390(2) 0.2026(2) 0.0391(8) Uani 1 1 d . . . . .
F2 F -0.01509(11) 0.7805(2) 0.3202(2) 0.0381(7) Uani 1 1 d . . . . .
F3 F 0.00909(10) 0.9253(2) 0.32066(18) 0.0269(6) Uani 1 1 d . . . . .
F4 F 0.02419(9) 0.9087(2) 0.51028(18) 0.0272(6) Uani 1 1 d . . . . .
F5 F 0.02280(10) 0.8843(2) 0.65106(19) 0.0309(7) Uani 1 1 d . . . . .
F6 F 0.02612(10) 0.76573(19) 0.5613(2) 0.0320(7) Uani 1 1 d . . . . .
N1 N 0.10021(13) 1.0435(2) 0.3482(2) 0.0148(7) Uani 1 1 d . . . . .
N2 N 0.09594(13) 1.0828(2) 0.5013(2) 0.0157(8) Uani 1 1 d . . . . .
C1 C 0.01635(19) 0.8389(4) 0.2901(4) 0.0323(13) Uani 1 1 d . . . . .
C2 C 0.06839(17) 0.8038(3) 0.3300(3) 0.0195(10) Uani 1 1 d . . . . .
C3 C 0.07528(19) 0.7127(3) 0.3651(3) 0.0252(11) Uani 1 1 d . . . . .
H3 H 0.048269 0.672404 0.365183 0.030 Uiso 1 1 calc R . . . .
C4 C 0.1218(2) 0.6793(3) 0.4005(3) 0.0293(12) Uani 1 1 d . . . . .
H4 H 0.126539 0.616012 0.423743 0.035 Uiso 1 1 calc R . . . .
C5 C 0.16104(18) 0.7379(3) 0.4018(3) 0.0250(11) Uani 1 1 d . . . . .
H5 H 0.192754 0.715499 0.426801 0.030 Uiso 1 1 calc R . . . .
C6 C 0.15384(17) 0.8306(3) 0.3661(3) 0.0189(9) Uani 1 1 d . . . . .
C7 C 0.10818(16) 0.8650(3) 0.3279(3) 0.0166(9) Uani 1 1 d . . . . .
C8 C 0.10137(16) 0.9623(3) 0.2845(3) 0.0168(9) Uani 1 1 d . . . . .
H8A H 0.127880 0.973572 0.252136 0.020 Uiso 1 1 calc R . . . .
H8B H 0.070728 0.962188 0.238164 0.020 Uiso 1 1 calc R . . . .
C9 C 0.0983(2) 1.1371(3) 0.3031(3) 0.0310(12) Uani 1 1 d . . . . .
H9A H 0.064951 1.160512 0.289404 0.047 Uiso 1 1 calc GR . . . .
H9B H 0.109853 1.130737 0.246208 0.047 Uiso 1 1 calc GR . . . .
H9C H 0.118865 1.182529 0.343638 0.047 Uiso 1 1 calc GR . . . .
C10 C 0.09914(15) 1.0261(3) 0.4335(3) 0.0140(8) Uani 1 1 d . . . . .
H10 H 0.101045 0.960093 0.449024 0.017 Uiso 1 1 calc R . . . .
C11 C 0.0919(2) 1.1880(3) 0.4998(3) 0.0279(11) Uani 1 1 d . . . . .
H11A H 0.124215 1.216360 0.512498 0.042 Uiso 1 1 calc GR . . . .
H11B H 0.074487 1.208661 0.546456 0.042 Uiso 1 1 calc GR . . . .
H11C H 0.074135 1.208827 0.439503 0.042 Uiso 1 1 calc GR . . . .
C12 C 0.09741(17) 1.0403(3) 0.5925(3) 0.0192(10) Uani 1 1 d . . . . .
H12A H 0.063891 1.033178 0.601033 0.023 Uiso 1 1 calc R . . . .
H12B H 0.114288 1.085211 0.639743 0.023 Uiso 1 1 calc R . . . .
C13 C 0.12226(16) 0.9436(3) 0.6076(3) 0.0172(9) Uani 1 1 d . . . . .
C14 C 0.17245(16) 0.9396(3) 0.6257(3) 0.0205(10) Uani 1 1 d . . . . .
C15 C 0.19668(18) 0.8540(4) 0.6454(3) 0.0314(12) Uani 1 1 d . . . . .
H15 H 0.230980 0.852827 0.657833 0.038 Uiso 1 1 calc R . . . .
C16 C 0.17111(19) 0.7698(4) 0.6471(3) 0.0304(12) Uani 1 1 d . . . . .
H16 H 0.187885 0.711201 0.662240 0.036 Uiso 1 1 calc R . . . .
C17 C 0.12159(18) 0.7710(4) 0.6270(3) 0.0250(11) Uani 1 1 d . . . . .
H17 H 0.103977 0.713127 0.626681 0.030 Uiso 1 1 calc R . . . .
C18 C 0.09730(16) 0.8574(3) 0.6069(3) 0.0182(9) Uani 1 1 d . . . . .
C19 C 0.04312(17) 0.8540(3) 0.5830(3) 0.0213(10) Uani 1 1 d . . . . .
I11 I 0.28797(2) 0.61098(2) 0.63202(2) 0.02593(7) Uani 1 1 d . . . . .
I12 I 0.27399(2) 0.50506(3) 0.37223(2) 0.04412(11) Uani 1 1 d . . . . .
F7 F 0.49890(11) 0.6588(2) 0.7878(2) 0.0420(8) Uani 1 1 d . . . . .
F8 F 0.52111(11) 0.7267(2) 0.6767(2) 0.0431(8) Uani 1 1 d . . . . .
F9 F 0.49396(10) 0.5835(2) 0.6634(2) 0.0354(7) Uani 1 1 d . . . . .
F10 F 0.48622(12) 0.7291(3) 0.4328(3) 0.0521(10) Uani 1 1 d . . . . .
F11 F 0.47609(11) 0.5852(2) 0.4740(2) 0.0433(9) Uani 1 1 d . . . . .
F12 F 0.47470(12) 0.6152(3) 0.3338(2) 0.0472(9) Uani 1 1 d . . . . .
N3 N 0.39402(14) 0.4397(3) 0.4801(2) 0.0185(8) Uani 1 1 d . . . . .
N4 N 0.40169(13) 0.4724(2) 0.6392(2) 0.0159(8) Uani 1 1 d . . . . .
C20 C 0.48847(18) 0.6676(4) 0.7012(4) 0.0323(13) Uani 1 1 d . . . . .
C21 C 0.43743(17) 0.7076(3) 0.6663(3) 0.0196(10) Uani 1 1 d . . . . .
C22 C 0.43204(18) 0.8016(3) 0.6357(3) 0.0246(11) Uani 1 1 d . . . . .
H22 H 0.459771 0.839251 0.634115 0.030 Uiso 1 1 calc R . . . .
C23 C 0.38648(19) 0.8406(3) 0.6076(3) 0.0269(11) Uani 1 1 d . . . . .
H23 H 0.383093 0.905230 0.587635 0.032 Uiso 1 1 calc R . . . .
C24 C 0.34616(18) 0.7867(3) 0.6082(3) 0.0239(11) Uani 1 1 d . . . . .
H24 H 0.314869 0.813645 0.588736 0.029 Uiso 1 1 calc R . . . .
C25 C 0.35167(16) 0.6907(3) 0.6382(3) 0.0177(9) Uani 1 1 d . . . . .
C26 C 0.39665(16) 0.6507(3) 0.6688(3) 0.0153(9) Uani 1 1 d . . . . .
C27 C 0.40219(17) 0.5501(3) 0.7071(3) 0.0189(9) Uani 1 1 d . . . . .
H27A H 0.433009 0.546496 0.752792 0.023 Uiso 1 1 calc R . . . .
H27B H 0.375766 0.538136 0.739543 0.023 Uiso 1 1 calc R . . . .
C28 C 0.40837(19) 0.3777(3) 0.6818(3) 0.0263(11) Uani 1 1 d . . . . .
H28A H 0.417560 0.384849 0.748335 0.039 Uiso 1 1 calc GR . . . .
H28B H 0.433886 0.343337 0.660030 0.039 Uiso 1 1 calc GR . . . .
H28C H 0.378126 0.341512 0.665656 0.039 Uiso 1 1 calc GR . . . .
C29 C 0.39622(15) 0.4935(3) 0.5521(3) 0.0150(9) Uani 1 1 d . . . . .
H29 H 0.393318 0.560057 0.539242 0.018 Uiso 1 1 calc R . . . .
C30 C 0.3949(2) 0.3351(3) 0.4754(3) 0.0281(12) Uani 1 1 d . . . . .
H30A H 0.368881 0.313094 0.425582 0.042 Uiso 1 1 calc GR . . . .
H30B H 0.390216 0.308226 0.533328 0.042 Uiso 1 1 calc GR . . . .
H30C H 0.426059 0.314031 0.464126 0.042 Uiso 1 1 calc GR . . . .
C31 C 0.39103(19) 0.4858(3) 0.3895(3) 0.0246(11) Uani 1 1 d . . . . .
H31A H 0.368266 0.448736 0.342850 0.030 Uiso 1 1 calc R . . . .
H31B H 0.423200 0.482439 0.373752 0.030 Uiso 1 1 calc R . . . .
C32 C 0.37479(17) 0.5892(3) 0.3848(3) 0.0199(10) Uani 1 1 d . . . . .
C33 C 0.32591(18) 0.6118(4) 0.3724(3) 0.0242(11) Uani 1 1 d . . . . .
C34 C 0.31032(19) 0.7062(4) 0.3647(3) 0.0280(11) Uani 1 1 d . . . . .
H34 H 0.276872 0.720266 0.356362 0.034 Uiso 1 1 calc R . . . .
C35 C 0.3428(2) 0.7787(4) 0.3690(3) 0.0304(12) Uani 1 1 d . . . . .
H35 H 0.331829 0.843090 0.362033 0.037 Uiso 1 1 calc R . . . .
C36 C 0.39141(19) 0.7596(3) 0.3832(3) 0.0251(11) Uani 1 1 d . . . . .
H36 H 0.413873 0.810801 0.387627 0.030 Uiso 1 1 calc R . . . .
C37 C 0.40773(17) 0.6658(3) 0.3913(3) 0.0216(10) Uani 1 1 d . . . . .
C38 C 0.46073(19) 0.6488(4) 0.4073(4) 0.0329(12) 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 I1 2.5891(5) . ?
Pd1 I2 2.5994(5) . ?
Pd1 I3 2.5916(5) . ?
Pd1 I4 2.5996(5) . ?
Pd2 I3 2.6004(5) . ?
Pd2 I4 2.5965(5) . ?
Pd2 I5 2.5967(5) . ?
Pd2 I6 2.5934(5) . ?
I7 I7 2.7460(8) 3_566 ?
I8 I8 2.7560(8) 3_676 ?
I9 C14 2.104(5) . ?
I10 C6 2.107(5) . ?
F1 C1 1.281(6) . ?
F2 C1 1.355(6) . ?
F3 C1 1.322(5) . ?
F4 C19 1.346(5) . ?
F5 C19 1.341(5) . ?
F6 C19 1.338(5) . ?
N1 C8 1.487(5) . ?
N1 C9 1.467(5) . ?
N1 C10 1.308(5) . ?
N2 C10 1.306(5) . ?
N2 C11 1.473(5) . ?
N2 C12 1.483(5) . ?
C1 C2 1.549(7) . ?
C2 C3 1.375(6) . ?
C2 C7 1.421(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.393(7) . ?
C4 H4 0.9500 . ?
C4 C5 1.376(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.400(6) . ?
C6 C7 1.385(6) . ?
C7 C8 1.501(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.517(6) . ?
C13 C14 1.391(6) . ?
C13 C18 1.396(6) . ?
C14 C15 1.379(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.384(8) . ?
C16 H16 0.9500 . ?
C16 C17 1.371(7) . ?
C17 H17 0.9500 . ?
C17 C18 1.390(6) . ?
C18 C19 1.502(6) . ?
I11 C25 2.106(5) . ?
I12 C33 2.095(5) . ?
F7 C20 1.273(6) . ?
F8 C20 1.348(6) . ?
F9 C20 1.329(5) . ?
F10 C38 1.345(6) . ?
F11 C38 1.340(6) . ?
F12 C38 1.332(6) . ?
N3 C29 1.305(5) . ?
N3 C30 1.463(5) . ?
N3 C31 1.489(6) . ?
N4 C27 1.486(5) . ?
N4 C28 1.464(5) . ?
N4 C29 1.314(5) . ?
C20 C21 1.535(7) . ?
C21 C22 1.389(6) . ?
C21 C26 1.410(6) . ?
C22 H22 0.9500 . ?
C22 C23 1.382(7) . ?
C23 H23 0.9500 . ?
C23 C24 1.370(7) . ?
C24 H24 0.9500 . ?
C24 C25 1.414(6) . ?
C25 C26 1.378(6) . ?
C26 C27 1.513(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.513(6) . ?
C32 C33 1.394(7) . ?
C32 C37 1.410(6) . ?
C33 C34 1.388(7) . ?
C34 H34 0.9500 . ?
C34 C35 1.362(7) . ?
C35 H35 0.9500 . ?
C35 C36 1.373(7) . ?
C36 H36 0.9500 . ?
C36 C37 1.387(6) . ?
C37 C38 1.489(7) . ?

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
I1 Pd1 I2 93.815(18) . . ?
I1 Pd1 I3 90.043(18) . . ?
I1 Pd1 I4 176.602(17) . . ?
I2 Pd1 I4 89.471(18) . . ?
I3 Pd1 I2 176.015(17) . . ?
I3 Pd1 I4 86.656(18) . . ?
I4 Pd2 I3 86.536(18) . . ?
I5 Pd2 I3 89.453(18) . . ?
I5 Pd2 I4 174.013(17) . . ?
I6 Pd2 I3 176.518(17) . . ?
I6 Pd2 I4 90.075(18) . . ?
I6 Pd2 I5 93.988(19) . . ?
Pd1 I3 Pd2 93.401(18) . . ?
Pd2 I4 Pd1 93.305(18) . . ?
C9 N1 C8 112.9(3) . . ?
C10 N1 C8 119.5(3) . . ?
C10 N1 C9 127.5(4) . . ?
C10 N2 C11 127.7(4) . . ?
C10 N2 C12 118.7(4) . . ?
C11 N2 C12 113.6(3) . . ?
F1 C1 F2 109.0(4) . . ?
F1 C1 F3 109.7(5) . . ?
F1 C1 C2 112.3(4) . . ?
F2 C1 C2 108.7(4) . . ?
F3 C1 F2 105.8(4) . . ?
F3 C1 C2 111.2(4) . . ?
C3 C2 C1 119.2(4) . . ?
C3 C2 C7 121.1(4) . . ?
C7 C2 C1 119.7(4) . . ?
C2 C3 H3 120.0 . . ?
C2 C3 C4 120.0(5) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(4) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 H5 120.2 . . ?
C4 C5 C6 119.5(5) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 I10 117.2(3) . . ?
C7 C6 I10 121.1(3) . . ?
C7 C6 C5 121.8(4) . . ?
C2 C7 C8 121.7(4) . . ?
C6 C7 C2 117.3(4) . . ?
C6 C7 C8 121.0(4) . . ?
N1 C8 C7 115.6(3) . . ?
N1 C8 H8A 108.4 . . ?
N1 C8 H8B 108.4 . . ?
C7 C8 H8A 108.4 . . ?
C7 C8 H8B 108.4 . . ?
H8A C8 H8B 107.4 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 H10 114.1 . . ?
N2 C10 N1 131.8(4) . . ?
N2 C10 H10 114.1 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 108.6 . . ?
N2 C12 H12B 108.6 . . ?
N2 C12 C13 114.6(3) . . ?
H12A C12 H12B 107.6 . . ?
C13 C12 H12A 108.6 . . ?
C13 C12 H12B 108.6 . . ?
C14 C13 C12 119.2(4) . . ?
C14 C13 C18 117.5(4) . . ?
C18 C13 C12 123.3(4) . . ?
C13 C14 I9 120.8(3) . . ?
C15 C14 I9 117.9(4) . . ?
C15 C14 C13 121.3(4) . . ?
C14 C15 H15 119.9 . . ?
C14 C15 C16 120.1(5) . . ?
C16 C15 H15 119.9 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 120.1(5) . . ?
C17 C16 H16 120.0 . . ?
C16 C17 H17 120.2 . . ?
C16 C17 C18 119.6(5) . . ?
C18 C17 H17 120.2 . . ?
C13 C18 C19 121.3(4) . . ?
C17 C18 C13 121.4(4) . . ?
C17 C18 C19 117.3(4) . . ?
F4 C19 C18 112.7(4) . . ?
F5 C19 F4 105.9(4) . . ?
F5 C19 C18 113.0(4) . . ?
F6 C19 F4 105.4(4) . . ?
F6 C19 F5 106.6(4) . . ?
F6 C19 C18 112.6(4) . . ?
C29 N3 C30 128.1(4) . . ?
C29 N3 C31 119.2(4) . . ?
C30 N3 C31 112.7(3) . . ?
C28 N4 C27 112.3(3) . . ?
C29 N4 C27 119.8(3) . . ?
C29 N4 C28 127.8(4) . . ?
F7 C20 F8 108.2(4) . . ?
F7 C20 F9 109.1(5) . . ?
F7 C20 C21 112.4(4) . . ?
F8 C20 C21 109.6(5) . . ?
F9 C20 F8 106.0(4) . . ?
F9 C20 C21 111.3(4) . . ?
C22 C21 C20 119.1(4) . . ?
C22 C21 C26 120.6(4) . . ?
C26 C21 C20 120.3(4) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.2(5) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 119.7 . . ?
C24 C23 C22 120.6(4) . . ?
C24 C23 H23 119.7 . . ?
C23 C24 H24 120.4 . . ?
C23 C24 C25 119.2(4) . . ?
C25 C24 H24 120.4 . . ?
C24 C25 I11 116.9(3) . . ?
C26 C25 I11 121.6(3) . . ?
C26 C25 C24 121.5(4) . . ?
C21 C26 C27 121.0(4) . . ?
C25 C26 C21 117.9(4) . . ?
C25 C26 C27 121.1(4) . . ?
N4 C27 C26 115.7(3) . . ?
N4 C27 H27A 108.3 . . ?
N4 C27 H27B 108.3 . . ?
C26 C27 H27A 108.3 . . ?
C26 C27 H27B 108.3 . . ?
H27A C27 H27B 107.4 . . ?
N4 C28 H28A 109.5 . . ?
N4 C28 H28B 109.5 . . ?
N4 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C29 N4 131.8(4) . . ?
N3 C29 H29 114.1 . . ?
N4 C29 H29 114.1 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N3 C31 H31A 108.7 . . ?
N3 C31 H31B 108.7 . . ?
N3 C31 C32 114.4(4) . . ?
H31A C31 H31B 107.6 . . ?
C32 C31 H31A 108.7 . . ?
C32 C31 H31B 108.7 . . ?
C33 C32 C31 120.4(4) . . ?
C33 C32 C37 117.5(4) . . ?
C37 C32 C31 122.1(4) . . ?
C32 C33 I12 121.1(4) . . ?
C34 C33 I12 117.7(4) . . ?
C34 C33 C32 121.1(5) . . ?
C33 C34 H34 119.9 . . ?
C35 C34 C33 120.2(5) . . ?
C35 C34 H34 119.9 . . ?
C34 C35 H35 119.7 . . ?
C34 C35 C36 120.6(5) . . ?
C36 C35 H35 119.7 . . ?
C35 C36 H36 119.9 . . ?
C35 C36 C37 120.1(5) . . ?
C37 C36 H36 119.9 . . ?
C32 C37 C38 121.4(4) . . ?
C36 C37 C32 120.5(4) . . ?
C36 C37 C38 118.1(4) . . ?
F10 C38 C37 112.1(5) . . ?
F11 C38 F10 105.8(4) . . ?
F11 C38 C37 112.5(4) . . ?
F12 C38 F10 107.0(4) . . ?
F12 C38 F11 106.0(4) . . ?
F12 C38 C37 113.0(4) . . ?

_shelx_SHELXL_version_number     2016/6
_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_complex_16
_database_code_depnum_ccdc_archive 'CCDC 1544220'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2016-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H23.60 Cl2.40 N2 Pd2'
_chemical_formula_sum            'C18 H23.60 Cl2.40 N2 Pd2'
_chemical_formula_weight         565.87
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.8606(4)
_cell_length_b                   15.7100(9)
_cell_length_c                   8.3499(4)
_cell_angle_alpha                90
_cell_angle_beta                 108.6070(13)
_cell_angle_gamma                90
_cell_volume                     977.23(9)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.95
_cell_measurement_theta_min      2.59
_shelx_estimated_absorpt_T_max   0.696
_shelx_estimated_absorpt_T_min   0.526
_exptl_absorpt_coefficient_mu    2.171
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1092 before and 0.0492 after correction.
The Ratio of minimum to maximum transmission is 0.8585.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             556.8
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            54669
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.246
_diffrn_reflns_theta_min         2.593
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2990
_reflns_number_total             3456
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material  
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_refine_diff_density_max         1.629
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.290
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         3456
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0529
_refine_ls_R_factor_gt           0.0419
_refine_ls_restrained_S_all      1.290
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0236P)²+2.2097P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0907
_refine_special_details          ?
_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. Others
 Fixed Sof: Cl2(0.2) H5(0.8)
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.31586(3) 0.05853(2) 0.01430(3) 0.03069(9) Uani 1 1 d . . . . .
Cl1 Cl 0.61218(13) 0.01182(11) 0.20060(12) 0.0648(4) Uani 1 1 d . . . . .
Cl2 Cl -0.3532(6) 0.1737(4) -0.0385(7) 0.0467(12) Uani 0.2 1 d . . P A 1
N1 N 0.2415(3) 0.12323(16) 0.1971(3) 0.0217(5) Uani 1 1 d . . . . .
C1 C 0.0823(4) 0.1002(2) -0.1334(4) 0.0259(6) Uani 1 1 d . . . . .
C2 C 0.0233(5) 0.1024(2) -0.3101(4) 0.0304(7) Uani 1 1 d . . . . .
H2 H 0.098041 0.081204 -0.370674 0.036 Uiso 1 1 calc R . . . .
C3 C -0.1444(5) 0.1356(2) -0.3970(4) 0.0365(8) Uani 1 1 d . . . . .
H3 H -0.182864 0.138088 -0.516892 0.044 Uiso 1 1 calc R . . . .
C4 C -0.2552(6) 0.1648(3) -0.3109(5) 0.0425(9) Uani 1 1 d . . . . .
H4 H -0.370818 0.186343 -0.371212 0.051 Uiso 1 1 calc R . . . .
C5 C -0.1979(5) 0.1628(3) -0.1354(5) 0.0402(8) Uani 1 1 d . . . . .
H5 H -0.274267 0.183389 -0.075766 0.048 Uiso 0.8 1 calc R . P A 2
C6 C -0.0288(4) 0.1308(2) -0.0466(4) 0.0284(6) Uani 1 1 d . . . . .
C7 C 0.0406(4) 0.1252(2) 0.1426(4) 0.0276(6) Uani 1 1 d . . . . .
H7A H -0.000398 0.175087 0.192854 0.033 Uiso 1 1 calc R . . . .
H7B H -0.005304 0.073051 0.181115 0.033 Uiso 1 1 calc R . . . .
C8 C 0.3128(6) 0.2108(2) 0.2065(4) 0.0349(8) Uani 1 1 d . . . . .
H8A H 0.443300 0.208707 0.231625 0.052 Uiso 1 1 calc GR . . . .
H8B H 0.284097 0.242212 0.295982 0.052 Uiso 1 1 calc GR . . . .
H8C H 0.258180 0.239551 0.098004 0.052 Uiso 1 1 calc GR . . . .
C9 C 0.3104(5) 0.0844(2) 0.3665(4) 0.0270(6) Uani 1 1 d . . . . .
H9A H 0.268181 0.025482 0.361458 0.040 Uiso 1 1 calc GR . . . .
H9B H 0.266894 0.116820 0.445925 0.040 Uiso 1 1 calc GR . . . .
H9C H 0.441943 0.085188 0.404698 0.040 Uiso 1 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 Cl1 2.3257(9) 3_655 ?
Pd1 Cl1 2.4641(10) . ?
Pd1 N1 2.068(2) . ?
Pd1 C1 1.969(3) . ?
Cl2 C5 1.674(6) . ?
N1 C7 1.497(4) . ?
N1 C8 1.478(4) . ?
N1 C9 1.475(4) . ?
C1 C2 1.399(4) . ?
C1 C6 1.386(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.387(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.373(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.394(5) . ?
C6 C7 1.500(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 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
Cl1 Pd1 Cl1 86.10(3) 3_655 . ?
N1 Pd1 Cl1 96.50(7) . . ?
N1 Pd1 Cl1 177.38(8) . 3_655 ?
C1 Pd1 Cl1 94.74(10) . 3_655 ?
C1 Pd1 Cl1 177.88(10) . . ?
C1 Pd1 N1 82.65(12) . . ?
Pd1 Cl1 Pd1 93.91(3) 3_655 . ?
C7 N1 Pd1 107.75(18) . . ?
C8 N1 Pd1 107.74(19) . . ?
C8 N1 C7 110.0(3) . . ?
C9 N1 Pd1 113.64(19) . . ?
C9 N1 C7 109.2(2) . . ?
C9 N1 C8 108.5(3) . . ?
C2 C1 Pd1 126.7(3) . . ?
C6 C1 Pd1 113.9(2) . . ?
C6 C1 C2 119.4(3) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 C1 120.1(3) . . ?
C3 C2 H2 120.0 . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.5(3) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 119.9(4) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 Cl2 117.8(4) . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.1(4) . . ?
C6 C5 Cl2 119.9(4) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C5 120.0(3) . . ?
C1 C6 C7 116.9(3) . . ?
C5 C6 C7 123.1(3) . . ?
N1 C7 C6 108.4(2) . . ?
N1 C7 H7A 110.0 . . ?
N1 C7 H7B 110.0 . . ?
C6 C7 H7A 110.0 . . ?
C6 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?

_shelx_SHELXL_version_number     2016/6
_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_complex_17
_database_code_depnum_ccdc_archive 'CCDC 1544219'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2016-12-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 Pd, 2(C9 H12 Cl2 N)'
_chemical_formula_sum            'C18 H24 Cl8 N2 Pd'
_chemical_formula_weight         658.39
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3725(10)
_cell_length_b                   8.0905(8)
_cell_length_c                   14.2505(13)
_cell_angle_alpha                90
_cell_angle_beta                 90.468(2)
_cell_angle_gamma                90
_cell_volume                     1195.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5657
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.26
_cell_measurement_theta_min      2.41
_shelx_estimated_absorpt_T_max   0.906
_shelx_estimated_absorpt_T_min   0.709
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_T_max  0.6465
_exptl_absorpt_correction_T_min  0.5249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0909 before and 0.0576 after correction.
The Ratio of minimum to maximum transmission is 0.8119.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15065
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.431
_diffrn_reflns_theta_min         2.859
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1836
_reflns_number_total             2444
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material  
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_refine_diff_density_max         1.824
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2444
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0435
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0534P)²+2.8955P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1154
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1
 0.88 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8)
3.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.000000 0.000000 0.500000 0.02030(17) Uani 1 2 d S T P . .
Cl1 Cl 0.16252(11) 0.00946(15) 0.61197(9) 0.0284(3) Uani 1 1 d . . . . .
Cl2 Cl 0.07402(11) 0.23923(15) 0.43092(9) 0.0263(3) Uani 1 1 d . . . . .
Cl3 Cl 0.51894(12) 0.47885(16) 0.74137(9) 0.0315(3) Uani 1 1 d . . . . .
Cl4 Cl 0.23226(12) 0.66609(16) 0.44148(8) 0.0302(3) Uani 1 1 d . . . . .
N1 N 0.1598(4) 0.5492(5) 0.6598(3) 0.0203(9) Uani 1 1 d D . . . .
H1 H 0.131(4) 0.642(4) 0.629(3) 0.024 Uiso 1 1 d DR . . . .
C1 C 0.2735(4) 0.4649(6) 0.6158(3) 0.0224(11) Uani 1 1 d . . . . .
H1A H 0.308192 0.381549 0.660205 0.027 Uiso 1 1 calc R . . . .
H1B H 0.244202 0.405911 0.558654 0.027 Uiso 1 1 calc R . . . .
C2 C 0.1944(5) 0.6343(6) 0.7490(3) 0.0271(11) Uani 1 1 d . . . . .
H2A H 0.231656 0.554173 0.793081 0.041 Uiso 1 1 calc GR . . . .
H2B H 0.116862 0.683255 0.776280 0.041 Uiso 1 1 calc GR . . . .
H2C H 0.257498 0.721458 0.736335 0.041 Uiso 1 1 calc GR . . . .
C3 C 0.0566(5) 0.4255(6) 0.6767(4) 0.0268(11) Uani 1 1 d . . . . .
H3A H 0.031954 0.373374 0.617115 0.040 Uiso 1 1 calc GR . . . .
H3B H -0.018533 0.480654 0.703714 0.040 Uiso 1 1 calc GR . . . .
H3C H 0.088489 0.340971 0.720309 0.040 Uiso 1 1 calc GR . . . .
C4 C 0.3797(4) 0.5826(6) 0.5900(3) 0.0208(10) Uani 1 1 d . . . . .
C5 C 0.3704(4) 0.6789(6) 0.5091(3) 0.0232(10) Uani 1 1 d . . . . .
C6 C 0.4692(5) 0.7828(6) 0.4801(4) 0.0269(11) Uani 1 1 d . . . . .
H6 H 0.459520 0.846938 0.424631 0.032 Uiso 1 1 calc R . . . .
C7 C 0.5812(5) 0.7917(6) 0.5324(4) 0.0283(12) Uani 1 1 d . . . . .
H7 H 0.648899 0.862783 0.513200 0.034 Uiso 1 1 calc R . . . .
C8 C 0.5956(5) 0.6973(6) 0.6131(4) 0.0268(11) Uani 1 1 d . . . . .
H8 H 0.672928 0.702827 0.649126 0.032 Uiso 1 1 calc R . . . .
C9 C 0.4961(4) 0.5955(6) 0.6404(3) 0.0235(11) 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 Cl1 2.3129(12) 3_556 ?
Pd1 Cl1 2.3129(12) . ?
Pd1 Cl2 2.3058(12) 3_556 ?
Pd1 Cl2 2.3059(12) . ?
Cl3 C9 1.736(5) . ?
Cl4 C5 1.724(5) . ?
N1 H1 0.920(19) . ?
N1 C1 1.504(6) . ?
N1 C2 1.486(6) . ?
N1 C3 1.486(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C4 1.504(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.394(7) . ?
C4 C9 1.403(7) . ?
C5 C6 1.391(7) . ?
C6 H6 0.9500 . ?
C6 C7 1.377(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.387(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.379(7) . ?

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
Cl1 Pd1 Cl1 180.0 3_556 . ?
Cl2 Pd1 Cl1 91.34(4) 3_556 3_556 ?
Cl2 Pd1 Cl1 91.34(4) . . ?
Cl2 Pd1 Cl1 88.66(4) . 3_556 ?
Cl2 Pd1 Cl1 88.66(4) 3_556 . ?
Cl2 Pd1 Cl2 180.00(5) 3_556 . ?
C1 N1 H1 115(3) . . ?
C2 N1 H1 96(3) . . ?
C2 N1 C1 112.4(4) . . ?
C3 N1 H1 113(3) . . ?
C3 N1 C1 109.3(4) . . ?
C3 N1 C2 110.1(4) . . ?
N1 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.8 . . ?
C4 C1 N1 113.2(4) . . ?
C4 C1 H1A 108.9 . . ?
C4 C1 H1B 108.9 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 C1 120.7(4) . . ?
C5 C4 C9 115.7(4) . . ?
C9 C4 C1 123.4(4) . . ?
C4 C5 Cl4 118.7(4) . . ?
C6 C5 Cl4 118.8(4) . . ?
C6 C5 C4 122.5(5) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 C5 119.4(5) . . ?
C7 C6 H6 120.3 . . ?
C6 C7 H7 119.8 . . ?
C6 C7 C8 120.3(4) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 120.4 . . ?
C9 C8 C7 119.1(5) . . ?
C9 C8 H8 120.4 . . ?
C4 C9 Cl3 119.7(4) . . ?
C8 C9 Cl3 117.5(4) . . ?
C8 C9 C4 122.9(5) . . ?

_shelx_SHELXL_version_number     2016/6
_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_complex_6c
_database_code_depnum_ccdc_archive 'CCDC 1544221'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2016-12-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C36 H50 F6 N4 O6 Pd2, C7 H8'
_chemical_formula_sum            'C43 H58 F6 N4 O6 Pd2'
_chemical_formula_weight         1053.73
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.2657(11)
_cell_length_b                   29.630(4)
_cell_length_c                   19.311(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5301.8(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9626
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.17
_cell_measurement_theta_min      2.30
_shelx_estimated_absorpt_T_max   0.943
_shelx_estimated_absorpt_T_min   0.819
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6038
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0918 before and 0.0694 after correction.
The Ratio of minimum to maximum transmission is 0.8103.
The λ/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0778
_diffrn_reflns_Laue_measured_fraction_full 0.932
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21110
_diffrn_reflns_point_group_measured_fraction_full 0.892
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.30
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.709
_reflns_Friedel_fraction_full    0.840
_reflns_Friedel_fraction_max     0.840
_reflns_number_gt                3262
_reflns_number_total             4174
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material  
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_refine_diff_density_max         2.100
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 
;
 Flack x determined using 1165 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4174
_refine_ls_number_restraints     105
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0650
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0525P)²+57.4330P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1400
_refine_ls_wR_factor_ref         0.1490
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F1-C18 = F3-C18 = F2-C18
 1.33 with sigma of 0.02
 C18-C13
 1.45 with sigma of 0.02
 C21-C20 \\sim C22-C21 \\sim C23-C22 \\sim C23-C22_$1 \\sim C22_$1-C21_$1 \\sim
C21_$1-C20
 with sigma of 0.005
3. Rigid body (RIGU) restrains
 C21, C22, C19, C20, C21, C22, C23
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 C1, C2, N2, O3, C7, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C16, C17, N1, C15, C9, C10, C11, C12, C13, C14, C18, F1, F2, F3} sigma for
1-2: 0.02, 1-3: 0.04
as
{C16A, C17A, N1A, C15A, C9A, C10A, C11A, C12A, C13A, C14A, C18A, F1A, F3A, F2A}
5. Others
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=
 Sof(H17F)=Sof(N1A)=Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C9A)=Sof(C10A)=Sof(H10A)=
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(C14A)=Sof(C18A)=Sof(F1A)=
 Sof(F3A)=Sof(F2A)=1-FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=
 Sof(N1)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C9)=Sof(C10)=Sof(H10)=Sof(C11)=
 Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(C14)=Sof(C18)=Sof(F1)=Sof(F2)=Sof(F3)=
 FVAR(1)
 Fixed Sof: H19A(0.5) H19B(0.5) H19C(0.5)
6.a Ternary CH refined with riding coordinates:
 C5(H5), C7(H7)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C15(H15A,H15B), C15A(H15C,H15D)
6.c Me refined with riding coordinates:
 C19(H19A,H19B,H19C)
6.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C21(H21), C22(H22), C23(H23), C10(H10), C11(H11), C12(H12),
 C10A(H10A), C11A(H11A), C12A(H12A)
6.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C16A(H16D,H16E,H16F), C17A(H17D,H17E,H17F)
;
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.15381(10) 0.67289(3) 0.77020(5) 0.0355(3) Uani 1 1 d . . . . .
O1 O 0.1496(12) 0.7217(3) 0.6969(5) 0.051(2) Uani 1 1 d . . . . .
O2 O -0.0741(10) 0.7191(3) 0.6559(6) 0.059(3) Uani 1 1 d . . . . .
O3 O 0.2682(10) 0.7262(4) 0.5159(5) 0.057(3) Uani 1 1 d . U . . .
N2 N 0.0512(11) 0.7579(4) 0.5366(6) 0.038(3) Uani 1 1 d . U . . .
H2 H -0.035671 0.763978 0.520677 0.046 Uiso 1 1 calc R . . . .
C1 C 0.0982(16) 0.7247(6) 0.4255(8) 0.059(4) Uani 1 1 d . U . . .
H1A H 0.164509 0.737733 0.391322 0.089 Uiso 1 1 calc GR . . . .
H1B H 0.000839 0.736634 0.417736 0.089 Uiso 1 1 calc GR . . . .
H1C H 0.097067 0.691822 0.420613 0.089 Uiso 1 1 calc GR . . . .
C2 C 0.1470(16) 0.7369(4) 0.4962(7) 0.044(3) Uani 1 1 d . U . . .
C3 C -0.048(2) 0.8955(5) 0.6034(10) 0.093(7) Uani 1 1 d . . . . .
H3A H -0.022482 0.901442 0.651742 0.139 Uiso 1 1 calc GR . . . .
H3B H -0.151667 0.889146 0.600073 0.139 Uiso 1 1 calc GR . . . .
H3C H -0.024899 0.922033 0.575140 0.139 Uiso 1 1 calc GR . . . .
C4 C 0.1991(19) 0.8656(6) 0.5717(9) 0.075(6) Uani 1 1 d . . . . .
H4A H 0.211625 0.893424 0.544833 0.112 Uiso 1 1 calc GR . . . .
H4B H 0.250102 0.840829 0.548650 0.112 Uiso 1 1 calc GR . . . .
H4C H 0.238503 0.869879 0.618291 0.112 Uiso 1 1 calc GR . . . .
C5 C 0.038(2) 0.8543(5) 0.5766(8) 0.061(5) Uani 1 1 d . . . . .
H5 H 0.002639 0.846382 0.529309 0.073 Uiso 1 1 calc R . . . .
C6 C 0.0114(16) 0.8144(4) 0.6243(8) 0.046(4) Uani 1 1 d . U . . .
H6A H -0.093608 0.808265 0.624841 0.055 Uiso 1 1 calc R . . . .
H6B H 0.039584 0.823289 0.671829 0.055 Uiso 1 1 calc R . . . .
C7 C 0.0897(15) 0.7705(5) 0.6062(7) 0.042(3) Uani 1 1 d . U . . .
H7 H 0.196112 0.776056 0.608085 0.050 Uiso 1 1 calc R . . . .
C8 C 0.0521(14) 0.7342(4) 0.6578(7) 0.037(3) Uani 1 1 d . . . . .
C19 C 0.500000 0.7357(6) 0.750000 0.048(6) Uani 1 2 d S TU P . .
H19A H 0.400418 0.724696 0.752490 0.071 Uiso 0.5 1 calc R . . A -1
H19B H 0.545296 0.724696 0.707376 0.071 Uiso 0.5 1 calc R . . A -1
H19C H 0.554286 0.724696 0.790134 0.071 Uiso 0.5 1 calc R . . A -1
C20 C 0.500000 0.7860(6) 0.750000 0.048(5) Uani 1 2 d DS TU P . .
C21 C 0.3748(13) 0.8115(3) 0.7531(7) 0.045(4) Uani 1 1 d D U . . .
H21 H 0.285944 0.795499 0.754306 0.054 Uiso 1 1 calc R . . . .
C22 C 0.3677(13) 0.8582(3) 0.7547(8) 0.053(4) Uani 1 1 d D U . . .
H22 H 0.279042 0.874088 0.758687 0.063 Uiso 1 1 calc R . . . .
C23 C 0.500000 0.8800(6) 0.750000 0.063(7) Uani 1 2 d DS TU P . .
H23 H 0.500000 0.912030 0.750000 0.075 Uiso 1 2 calc RS T P . .
C16 C 0.337(2) 0.6295(9) 0.8738(15) 0.038(7) Uiso 0.571(16) 1 d D . . B 1
H16A H 0.402712 0.622515 0.835562 0.057 Uiso 0.571(16) 1 calc GR . . B 1
H16B H 0.353272 0.608182 0.911858 0.057 Uiso 0.571(16) 1 calc GR . . B 1
H16C H 0.354814 0.660302 0.890132 0.057 Uiso 0.571(16) 1 calc GR . . B 1
C17 C 0.088(3) 0.6309(10) 0.9091(13) 0.043(7) Uiso 0.571(16) 1 d D . . B 1
H17A H 0.091723 0.662162 0.925469 0.065 Uiso 0.571(16) 1 calc GR . . B 1
H17B H 0.118776 0.610583 0.946345 0.065 Uiso 0.571(16) 1 calc GR . . B 1
H17C H -0.010732 0.623421 0.895177 0.065 Uiso 0.571(16) 1 calc GR . . B 1
N1 N 0.1851(19) 0.6256(6) 0.8495(12) 0.030(7) Uiso 0.571(16) 1 d D . . B 1
C15 C 0.165(3) 0.5814(6) 0.8205(15) 0.041(7) Uiso 0.571(16) 1 d D . . B 1
H15A H 0.060530 0.573755 0.819936 0.049 Uiso 0.571(16) 1 calc R . . B 1
H15B H 0.215745 0.558641 0.848781 0.049 Uiso 0.571(16) 1 calc R . . B 1
C9 C 0.231(3) 0.6225(7) 0.7188(16) 0.044(9) Uiso 0.571(16) 1 d D . . B 1
C10 C 0.277(3) 0.6283(10) 0.6492(14) 0.043(7) Uiso 0.571(16) 1 d D . . B 1
H10 H 0.274540 0.657549 0.629011 0.052 Uiso 0.571(16) 1 calc R . . B 1
C11 C 0.325(4) 0.5910(11) 0.6095(17) 0.068(9) Uiso 0.571(16) 1 d D . . B 1
H11 H 0.361706 0.593349 0.563632 0.081 Uiso 0.571(16) 1 calc R . . B 1
C12 C 0.313(3) 0.5504(9) 0.6456(16) 0.052(8) Uiso 0.571(16) 1 d D . . B 1
H12 H 0.333544 0.524050 0.619371 0.063 Uiso 0.571(16) 1 calc R . . B 1
C13 C 0.275(3) 0.5427(6) 0.7144(14) 0.053(7) Uiso 0.571(16) 1 d D . . B 1
C14 C 0.222(2) 0.5816(6) 0.7495(17) 0.026(6) Uiso 0.571(16) 1 d D . . B 1
C18 C 0.274(2) 0.4970(6) 0.7485(10) 0.047(7) Uiso 0.571(16) 1 d D . . B 1
F1 F 0.1411(15) 0.4896(4) 0.7759(8) 0.064(5) Uiso 0.571(16) 1 d D . . B 1
F2 F 0.3704(17) 0.4977(5) 0.8017(9) 0.069(5) Uiso 0.571(16) 1 d D . . B 1
F3 F 0.307(2) 0.4643(6) 0.7024(10) 0.096(7) Uiso 0.571(16) 1 d D . . B 1
C16A C 0.354(3) 0.6269(14) 0.849(2) 0.061(13) Uiso 0.429(16) 1 d D . . B 2
H16D H 0.413443 0.632171 0.808110 0.092 Uiso 0.429(16) 1 calc GR . . B 2
H16E H 0.387901 0.599811 0.873317 0.092 Uiso 0.429(16) 1 calc GR . . B 2
H16F H 0.360432 0.652942 0.880254 0.092 Uiso 0.429(16) 1 calc GR . . B 2
C17A C 0.112(4) 0.6170(14) 0.8909(18) 0.058(13) Uiso 0.429(16) 1 d D . . B 2
H17D H 0.123761 0.644365 0.918786 0.088 Uiso 0.429(16) 1 calc GR . . B 2
H17E H 0.141583 0.590645 0.917919 0.088 Uiso 0.429(16) 1 calc GR . . B 2
H17F H 0.009999 0.613804 0.877685 0.088 Uiso 0.429(16) 1 calc GR . . B 2
N1A N 0.201(3) 0.6204(9) 0.8278(16) 0.050(12) Uiso 0.429(16) 1 d D . . B 2
C15A C 0.188(3) 0.5783(8) 0.7911(17) 0.033(9) Uiso 0.429(16) 1 d D . . B 2
H15C H 0.087036 0.567352 0.793197 0.039 Uiso 0.429(16) 1 calc R . . B 2
H15D H 0.251509 0.555210 0.811971 0.039 Uiso 0.429(16) 1 calc R . . B 2
C9A C 0.228(3) 0.6297(8) 0.6970(15) 0.017(8) Uiso 0.429(16) 1 d D . . B 2
C10A C 0.266(3) 0.6430(11) 0.6285(15) 0.032(8) Uiso 0.429(16) 1 d D . . B 2
H10A H 0.261304 0.673571 0.613986 0.039 Uiso 0.429(16) 1 calc R . . B 2
C11A C 0.311(6) 0.6083(15) 0.583(2) 0.104(19) Uiso 0.429(16) 1 d D . . B 2
H11A H 0.339250 0.614455 0.536936 0.124 Uiso 0.429(16) 1 calc R . . B 2
C12A C 0.311(4) 0.5646(11) 0.6101(19) 0.050(10) Uiso 0.429(16) 1 d D . . B 2
H12A H 0.335871 0.541290 0.578512 0.060 Uiso 0.429(16) 1 calc R . . B 2
C13A C 0.279(3) 0.5507(8) 0.6770(17) 0.044(9) Uiso 0.429(16) 1 d D . . B 2
C14A C 0.230(3) 0.5869(7) 0.719(2) 0.033(9) Uiso 0.429(16) 1 d D . . B 2
C18A C 0.273(3) 0.5020(9) 0.6997(15) 0.063(11) Uiso 0.429(16) 1 d D . . B 2
F1A F 0.1386(19) 0.4918(6) 0.7230(11) 0.063(6) Uiso 0.429(16) 1 d D . . B 2
F3A F 0.290(3) 0.4759(10) 0.6433(16) 0.133(12) Uiso 0.429(16) 1 d D . . B 2
F2A F 0.377(2) 0.4968(7) 0.7489(13) 0.076(8) Uiso 0.429(16) 1 d D . . B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Pd1 2.9552(19) 3_556 ?
Pd1 O1 2.024(8) . ?
Pd1 O2 2.113(10) 3_556 ?
Pd1 N1 2.095(19) . ?
Pd1 C9 1.93(2) . ?
Pd1 N1A 1.96(3) . ?
Pd1 C9A 2.03(2) . ?
O1 C8 1.234(16) . ?
O2 C8 1.252(15) . ?
O3 C2 1.228(17) . ?
N2 H2 0.8800 . ?
N2 C2 1.335(16) . ?
N2 C7 1.441(17) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C1 C2 1.48(2) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3 C5 1.55(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4 C5 1.53(3) . ?
C5 H5 1.0000 . ?
C5 C6 1.518(18) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C6 C7 1.529(18) . ?
C7 H7 1.0000 . ?
C7 C8 1.508(18) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 C20 1.49(2) . ?
C20 C21 1.385(8) . ?
C20 C21 1.385(8) 3_656 ?
C21 H21 0.9500 . ?
C21 C22 1.386(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.388(8) . ?
C23 H23 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 N1 1.49(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 N1 1.47(3) . ?
N1 C15 1.44(3) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C14 1.47(3) . ?
C9 C10 1.42(3) . ?
C9 C14 1.35(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.42(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.39(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.39(4) . ?
C13 C14 1.42(3) . ?
C13 C18 1.51(2) . ?
C18 F1 1.360(18) . ?
C18 F2 1.359(19) . ?
C18 F3 1.350(17) . ?
C16A H16D 0.9800 . ?
C16A H16E 0.9800 . ?
C16A H16F 0.9800 . ?
C16A N1A 1.48(3) . ?
C17A H17D 0.9800 . ?
C17A H17E 0.9800 . ?
C17A H17F 0.9800 . ?
C17A N1A 1.48(3) . ?
N1A C15A 1.44(3) . ?
C15A H15C 0.9900 . ?
C15A H15D 0.9900 . ?
C15A C14A 1.47(4) . ?
C9A C10A 1.42(3) . ?
C9A C14A 1.34(3) . ?
C10A H10A 0.9500 . ?
C10A C11A 1.41(3) . ?
C11A H11A 0.9500 . ?
C11A C12A 1.40(4) . ?
C12A H12A 0.9500 . ?
C12A C13A 1.39(4) . ?
C13A C14A 1.42(3) . ?
C13A C18A 1.51(3) . ?
C18A F1A 1.36(2) . ?
C18A F3A 1.34(3) . ?
C18A F2A 1.37(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pd1 Pd1 78.3(3) . 3_556 ?
O1 Pd1 O2 90.2(4) . 3_556 ?
O1 Pd1 N1 172.5(6) . . ?
O1 Pd1 C9A 88.2(9) . . ?
O2 Pd1 Pd1 80.9(3) 3_556 3_556 ?
N1 Pd1 Pd1 109.0(5) . 3_556 ?
N1 Pd1 O2 89.3(7) . 3_556 ?
C9 Pd1 Pd1 102.8(9) . 3_556 ?
C9 Pd1 O1 101.5(10) . . ?
C9 Pd1 O2 168.2(10) . 3_556 ?
C9 Pd1 N1 78.9(11) . . ?
N1A Pd1 O1 165.3(10) . . ?
N1A Pd1 O2 102.1(10) . 3_556 ?
N1A Pd1 C9A 79.6(13) . . ?
C9A Pd1 O2 178.3(10) . 3_556 ?
C8 O1 Pd1 131.0(9) . . ?
C8 O2 Pd1 122.5(9) . 3_556 ?
C2 N2 H2 119.9 . . ?
C2 N2 C7 120.1(11) . . ?
C7 N2 H2 119.9 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
O3 C2 N2 123.2(13) . . ?
O3 C2 C1 120.1(12) . . ?
N2 C2 C1 116.7(13) . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C3 H3A 109.5 . . ?
C5 C3 H3B 109.5 . . ?
C5 C3 H3C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
C3 C5 H5 108.5 . . ?
C4 C5 C3 110.6(15) . . ?
C4 C5 H5 108.5 . . ?
C6 C5 C3 109.0(13) . . ?
C6 C5 C4 111.7(14) . . ?
C6 C5 H5 108.5 . . ?
C5 C6 H6A 108.2 . . ?
C5 C6 H6B 108.2 . . ?
C5 C6 C7 116.4(13) . . ?
H6A C6 H6B 107.3 . . ?
C7 C6 H6A 108.2 . . ?
C7 C6 H6B 108.2 . . ?
N2 C7 C6 108.5(11) . . ?
N2 C7 H7 108.7 . . ?
N2 C7 C8 111.9(11) . . ?
C6 C7 H7 108.7 . . ?
C8 C7 C6 110.3(11) . . ?
C8 C7 H7 108.7 . . ?
O1 C8 O2 126.5(12) . . ?
O1 C8 C7 116.7(11) . . ?
O2 C8 C7 116.8(12) . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
C21 C20 C19 123.0(8) . . ?
C21 C20 C19 123.0(8) 3_656 . ?
C21 C20 C21 113.9(16) 3_656 . ?
C20 C21 H21 117.1 . . ?
C20 C21 C22 125.8(13) . . ?
C22 C21 H21 117.1 . . ?
C21 C22 H22 122.6 . . ?
C21 C22 C23 114.9(13) . . ?
C23 C22 H22 122.6 . . ?
C22 C23 C22 124.6(16) . 3_656 ?
C22 C23 H23 117.7 3_656 . ?
C22 C23 H23 117.7 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
C16 N1 Pd1 108.1(14) . . ?
C17 N1 Pd1 114.6(15) . . ?
C17 N1 C16 109(2) . . ?
C15 N1 Pd1 107.8(16) . . ?
C15 N1 C16 108.6(18) . . ?
C15 N1 C17 108.7(19) . . ?
N1 C15 H15A 110.1 . . ?
N1 C15 H15B 110.1 . . ?
N1 C15 C14 108.2(17) . . ?
H15A C15 H15B 108.4 . . ?
C14 C15 H15A 110.1 . . ?
C14 C15 H15B 110.1 . . ?
C10 C9 Pd1 120.2(19) . . ?
C14 C9 Pd1 116(2) . . ?
C14 C9 C10 123(2) . . ?
C9 C10 H10 119.6 . . ?
C9 C10 C11 121(3) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 124.0 . . ?
C12 C11 C10 112(3) . . ?
C12 C11 H11 124.0 . . ?
C11 C12 H12 115.2 . . ?
C13 C12 C11 130(2) . . ?
C13 C12 H12 115.2 . . ?
C12 C13 C14 114(2) . . ?
C12 C13 C18 124.4(19) . . ?
C14 C13 C18 121(2) . . ?
C9 C14 C15 115.7(18) . . ?
C9 C14 C13 120(3) . . ?
C13 C14 C15 124(2) . . ?
F1 C18 C13 108.6(16) . . ?
F2 C18 C13 108.3(17) . . ?
F2 C18 F1 107.7(15) . . ?
F3 C18 C13 110.9(16) . . ?
F3 C18 F1 110.0(16) . . ?
F3 C18 F2 111.3(17) . . ?
H16D C16A H16E 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
N1A C16A H16D 109.5 . . ?
N1A C16A H16E 109.5 . . ?
N1A C16A H16F 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
N1A C17A H17D 109.5 . . ?
N1A C17A H17E 109.5 . . ?
N1A C17A H17F 109.5 . . ?
C16A N1A Pd1 106(2) . . ?
C17A N1A Pd1 113(2) . . ?
C17A N1A C16A 108(3) . . ?
C15A N1A Pd1 113(2) . . ?
C15A N1A C16A 109(3) . . ?
C15A N1A C17A 107(2) . . ?
N1A C15A H15C 110.3 . . ?
N1A C15A H15D 110.3 . . ?
N1A C15A C14A 107(2) . . ?
H15C C15A H15D 108.5 . . ?
C14A C15A H15C 110.3 . . ?
C14A C15A H15D 110.3 . . ?
C10A C9A Pd1 123.9(19) . . ?
C14A C9A Pd1 112(2) . . ?
C14A C9A C10A 123(2) . . ?
C9A C10A H10A 121.7 . . ?
C11A C10A C9A 117(3) . . ?
C11A C10A H10A 121.7 . . ?
C10A C11A H11A 121.8 . . ?
C12A C11A C10A 116(3) . . ?
C12A C11A H11A 121.8 . . ?
C11A C12A H12A 115.8 . . ?
C13A C12A C11A 128(3) . . ?
C13A C12A H12A 115.8 . . ?
C12A C13A C14A 112(3) . . ?
C12A C13A C18A 124(2) . . ?
C14A C13A C18A 123(3) . . ?
C9A C14A C15A 117(2) . . ?
C9A C14A C13A 123(3) . . ?
C13A C14A C15A 120(3) . . ?
F1A C18A C13A 110(2) . . ?
F1A C18A F2A 113(2) . . ?
F3A C18A C13A 108(2) . . ?
F3A C18A F1A 104(2) . . ?
F3A C18A F2A 115(2) . . ?
F2A C18A C13A 106(2) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.406 0.000 0.000 210.8 39.5 ?
2 0.406 0.000 0.500 210.8 39.5 ?
3 -0.094 0.500 0.500 210.8 39.5 ?
4 0.094 0.500 1.000 210.8 39.5 ?

_shelx_SHELXL_version_number     2016/6
_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_complex_6a
_database_code_depnum_ccdc_archive 'CCDC 1544215'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2016-12-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C14 H17 F3 N2 O3 Pd)'
_chemical_formula_sum            'C28 H34 F6 N4 O6 Pd2'
_chemical_formula_weight         849.39
_chemical_melting_point          ?
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.2283(14)
_cell_length_b                   17.6933(14)
_cell_length_c                   18.9065(15)
_cell_angle_alpha                90
_cell_angle_beta                 93.545(3)
_cell_angle_gamma                90
_cell_volume                     6419.9(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9579
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.78
_cell_measurement_theta_min      2.30
_shelx_estimated_absorpt_T_max   0.879
_shelx_estimated_absorpt_T_min   0.822
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0622 before and 0.0420 after correction.
The Ratio of minimum to maximum transmission is 0.9498.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            86726
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.808
_diffrn_reflns_theta_min         2.122
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6157
_reflns_number_total             6867
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material  
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6867
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0213
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0232P)²+10.9772P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0522
_refine_special_details          ?
_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:
 C7(H7A,H7B), C12(H12A,H12B), C21(H21A,H21B), C26(H26A,H26B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C16(H16), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C28(H28A,H28B,H28C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.52399(2) 0.25073(2) 0.67473(2) 0.01722(4) Uani 1 1 d . . . . .
F1 F 0.64243(8) -0.07896(9) 0.59815(10) 0.0598(5) Uani 1 1 d . . . . .
F2 F 0.56930(14) -0.02644(10) 0.52360(9) 0.0935(8) Uani 1 1 d . . . . .
F9 F 0.54099(8) -0.05252(8) 0.62737(10) 0.0595(5) Uani 1 1 d . . . . .
O1 O 0.59726(7) 0.32732(7) 0.71503(7) 0.0211(3) Uani 1 1 d . . . . .
O2 O 0.55916(7) 0.32967(8) 0.82411(7) 0.0227(3) Uani 1 1 d . . . . .
O3 O 0.72970(8) 0.30435(8) 0.87808(8) 0.0335(3) Uani 1 1 d . . . . .
N1 N 0.45924(8) 0.17163(9) 0.62663(8) 0.0192(3) Uani 1 1 d . . . . .
N2 N 0.67077(9) 0.41343(10) 0.87572(9) 0.0225(3) Uani 1 1 d . . . . .
H2 H 0.6527(12) 0.4458(14) 0.8968(13) 0.029(7) Uiso 1 1 d . . . . .
C1 C 0.59604(10) 0.17820(11) 0.65247(9) 0.0212(4) Uani 1 1 d . . . . .
C2 C 0.66694(10) 0.19368(13) 0.65071(11) 0.0279(4) Uani 1 1 d . . . . .
H2A H 0.684150 0.242434 0.663539 0.033 Uiso 1 1 calc R . . . .
C3 C 0.71249(11) 0.13817(15) 0.63031(12) 0.0369(5) Uani 1 1 d . . . . .
H3 H 0.760617 0.149467 0.628223 0.044 Uiso 1 1 calc R . . . .
C4 C 0.68848(12) 0.06675(15) 0.61304(12) 0.0371(6) Uani 1 1 d . . . . .
H4 H 0.720228 0.028592 0.600518 0.045 Uiso 1 1 calc R . . . .
C5 C 0.61818(11) 0.05061(13) 0.61394(10) 0.0293(5) Uani 1 1 d . . . . .
C6 C 0.57105(10) 0.10655(11) 0.63230(10) 0.0220(4) Uani 1 1 d . . . . .
C7 C 0.49384(10) 0.09598(11) 0.63420(10) 0.0224(4) Uani 1 1 d . . . . .
H7A H 0.476721 0.062318 0.595077 0.027 Uiso 1 1 calc R . . . .
H7B H 0.482698 0.072389 0.679614 0.027 Uiso 1 1 calc R . . . .
C8 C 0.59329(14) -0.02585(14) 0.59145(13) 0.0420(6) Uani 1 1 d . . . . .
C9 C 0.45027(10) 0.19315(12) 0.55059(10) 0.0252(4) Uani 1 1 d . . . . .
H9A H 0.415601 0.160003 0.526373 0.038 Uiso 1 1 calc GR . . . .
H9B H 0.494872 0.187921 0.528632 0.038 Uiso 1 1 calc GR . . . .
H9C H 0.434441 0.245715 0.546662 0.038 Uiso 1 1 calc GR . . . .
C10 C 0.38908(10) 0.16607(12) 0.65497(11) 0.0249(4) Uani 1 1 d . . . . .
H10A H 0.393961 0.156372 0.706063 0.037 Uiso 1 1 calc GR . . . .
H10B H 0.363123 0.124571 0.631329 0.037 Uiso 1 1 calc GR . . . .
H10C H 0.363851 0.213618 0.646201 0.037 Uiso 1 1 calc GR . . . .
C11 C 0.59937(9) 0.34994(10) 0.77896(10) 0.0195(4) Uani 1 1 d . . . . .
C12 C 0.65555(10) 0.40780(11) 0.80030(10) 0.0233(4) Uani 1 1 d . . . . .
H12A H 0.698823 0.394117 0.777557 0.028 Uiso 1 1 calc R . . . .
H12B H 0.640445 0.457968 0.781956 0.028 Uiso 1 1 calc R . . . .
C13 C 0.70765(10) 0.35835(12) 0.90991(11) 0.0247(4) Uani 1 1 d . . . . .
C14 C 0.72155(13) 0.36665(14) 0.98871(12) 0.0359(5) Uani 1 1 d . . . . .
H14A H 0.767917 0.388595 0.998694 0.054 Uiso 1 1 calc GR . . . .
H14B H 0.719465 0.316894 1.011248 0.054 Uiso 1 1 calc GR . . . .
H14C H 0.686330 0.399876 1.007511 0.054 Uiso 1 1 calc GR . . . .
Pd2 Pd 0.42426(2) 0.61547(2) 0.73107(2) 0.02307(5) Uani 1 1 d . . . . .
F4 F 0.42178(8) 0.92513(8) 0.72479(9) 0.0513(4) Uani 1 1 d . . . . .
F6 F 0.36664(7) 0.96085(8) 0.62808(9) 0.0481(4) Uani 1 1 d . . . . .
F8 F 0.31099(7) 0.91140(8) 0.71137(9) 0.0478(4) Uani 1 1 d . . . . .
O4 O 0.45283(7) 0.54021(8) 0.65573(7) 0.0268(3) Uani 1 1 d . . . . .
O5 O 0.56616(7) 0.52924(8) 0.69075(7) 0.0269(3) Uani 1 1 d . . . . .
O6 O 0.61976(8) 0.49360(10) 0.50087(9) 0.0431(4) Uani 1 1 d . . . . .
N3 N 0.38331(8) 0.69236(10) 0.79821(9) 0.0270(4) Uani 1 1 d . . . . .
N4 N 0.58859(9) 0.42320(10) 0.59190(9) 0.0238(4) Uani 1 1 d . . . . .
H4A H 0.6010(12) 0.3972(13) 0.6240(13) 0.024(6) Uiso 1 1 d . . . . .
C15 C 0.40506(10) 0.69600(12) 0.66192(11) 0.0258(4) Uani 1 1 d . . . . .
C16 C 0.40209(10) 0.68759(13) 0.58856(11) 0.0288(4) Uani 1 1 d . . . . .
H16 H 0.409586 0.639283 0.568464 0.035 Uiso 1 1 calc R . . . .
C17 C 0.38823(11) 0.74933(13) 0.54459(13) 0.0334(5) Uani 1 1 d . . . . .
H17 H 0.385787 0.742970 0.494608 0.040 Uiso 1 1 calc R . . . .
C18 C 0.37797(11) 0.82015(13) 0.57337(13) 0.0339(5) Uani 1 1 d . . . . .
H18 H 0.369400 0.862464 0.543143 0.041 Uiso 1 1 calc R . . . .
C19 C 0.38022(11) 0.82925(12) 0.64632(13) 0.0323(5) Uani 1 1 d . . . . .
C20 C 0.39259(10) 0.76701(12) 0.69120(12) 0.0285(4) Uani 1 1 d . . . . .
C21 C 0.39640(12) 0.76986(12) 0.77079(12) 0.0319(5) Uani 1 1 d . . . . .
H21A H 0.442992 0.787690 0.788779 0.038 Uiso 1 1 calc R . . . .
H21B H 0.361023 0.805432 0.787119 0.038 Uiso 1 1 calc R . . . .
C22 C 0.37006(12) 0.90605(14) 0.67737(15) 0.0409(6) Uani 1 1 d . . . . .
C23 C 0.41041(11) 0.68783(13) 0.87296(11) 0.0322(5) Uani 1 1 d . . . . .
H23A H 0.399822 0.637956 0.892123 0.048 Uiso 1 1 calc GR . . . .
H23B H 0.388392 0.727009 0.900609 0.048 Uiso 1 1 calc GR . . . .
H23C H 0.460976 0.695513 0.875719 0.048 Uiso 1 1 calc GR . . . .
C24 C 0.30698(11) 0.67679(15) 0.79632(13) 0.0371(5) Uani 1 1 d . . . . .
H24A H 0.286275 0.686329 0.748490 0.056 Uiso 1 1 calc GR . . . .
H24B H 0.285214 0.709924 0.830130 0.056 Uiso 1 1 calc GR . . . .
H24C H 0.299310 0.623904 0.809116 0.056 Uiso 1 1 calc GR . . . .
C25 C 0.51322(10) 0.51328(11) 0.65236(10) 0.0225(4) Uani 1 1 d . . . . .
C26 C 0.51984(11) 0.45502(13) 0.59401(10) 0.0274(4) Uani 1 1 d . . . . .
H26A H 0.486234 0.413649 0.600814 0.033 Uiso 1 1 calc R . . . .
H26B H 0.507024 0.479052 0.547741 0.033 Uiso 1 1 calc R . . . .
C27 C 0.63439(10) 0.44687(12) 0.54709(10) 0.0256(4) Uani 1 1 d . . . . .
C28 C 0.70559(12) 0.41156(16) 0.55593(13) 0.0390(5) Uani 1 1 d . . . . .
H28A H 0.713720 0.380431 0.514367 0.059 Uiso 1 1 calc GR . . . .
H28B H 0.708447 0.379842 0.598509 0.059 Uiso 1 1 calc GR . . . .
H28C H 0.740985 0.451392 0.560677 0.059 Uiso 1 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 O1 2.0661(13) . ?
Pd1 O2 2.1239(13) 2_656 ?
Pd1 N1 2.0485(16) . ?
Pd1 C1 1.9534(18) . ?
F1 C8 1.333(3) . ?
F2 C8 1.336(3) . ?
F9 C8 1.334(3) . ?
O1 C11 1.272(2) . ?
O2 C11 1.240(2) . ?
O3 C13 1.219(3) . ?
N1 C7 1.498(2) . ?
N1 C9 1.487(2) . ?
N1 C10 1.485(2) . ?
N2 H2 0.79(2) . ?
N2 C12 1.441(3) . ?
N2 C13 1.347(3) . ?
C1 C2 1.393(3) . ?
C1 C6 1.400(3) . ?
C2 H2A 0.9500 . ?
C2 C3 1.386(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.378(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(3) . ?
C5 C6 1.400(3) . ?
C5 C8 1.488(3) . ?
C6 C7 1.499(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.524(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.504(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
Pd2 O4 2.0497(14) . ?
Pd2 O5 2.1244(14) 2_656 ?
Pd2 N3 2.0506(17) . ?
Pd2 C15 1.954(2) . ?
F4 C22 1.340(3) . ?
F6 C22 1.344(3) . ?
F8 C22 1.342(3) . ?
O4 C25 1.260(2) . ?
O5 C25 1.245(2) . ?
O6 C27 1.223(3) . ?
N3 C21 1.493(3) . ?
N3 C23 1.478(3) . ?
N3 C24 1.491(3) . ?
N4 H4A 0.79(2) . ?
N4 C26 1.440(3) . ?
N4 C27 1.327(3) . ?
C15 C16 1.393(3) . ?
C15 C20 1.399(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(3) . ?
C17 H17 0.9500 . ?
C17 C18 1.385(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(3) . ?
C19 C20 1.402(3) . ?
C19 C22 1.498(3) . ?
C20 C21 1.503(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.521(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.505(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 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
O1 Pd1 O2 93.52(5) . 2_656 ?
N1 Pd1 O1 173.57(6) . . ?
N1 Pd1 O2 90.95(6) . 2_656 ?
C1 Pd1 O1 91.93(7) . . ?
C1 Pd1 O2 168.11(6) . 2_656 ?
C1 Pd1 N1 82.83(7) . . ?
C11 O1 Pd1 122.55(12) . . ?
C11 O2 Pd1 134.37(12) . 2_656 ?
C7 N1 Pd1 108.30(11) . . ?
C9 N1 Pd1 106.57(12) . . ?
C9 N1 C7 110.22(14) . . ?
C10 N1 Pd1 115.20(11) . . ?
C10 N1 C7 108.33(15) . . ?
C10 N1 C9 108.19(15) . . ?
C12 N2 H2 118.7(18) . . ?
C13 N2 H2 121.1(18) . . ?
C13 N2 C12 119.58(17) . . ?
C2 C1 Pd1 125.75(16) . . ?
C2 C1 C6 119.43(18) . . ?
C6 C1 Pd1 114.67(14) . . ?
C1 C2 H2A 119.9 . . ?
C3 C2 C1 120.2(2) . . ?
C3 C2 H2A 119.9 . . ?
C2 C3 H3 119.7 . . ?
C4 C3 C2 120.5(2) . . ?
C4 C3 H3 119.7 . . ?
C3 C4 H4 120.0 . . ?
C3 C4 C5 120.0(2) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 120.3(2) . . ?
C4 C5 C8 118.8(2) . . ?
C6 C5 C8 120.8(2) . . ?
C1 C6 C7 115.48(16) . . ?
C5 C6 C1 119.41(19) . . ?
C5 C6 C7 125.09(19) . . ?
N1 C7 C6 108.73(16) . . ?
N1 C7 H7A 109.9 . . ?
N1 C7 H7B 109.9 . . ?
C6 C7 H7A 109.9 . . ?
C6 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
F1 C8 F2 106.6(2) . . ?
F1 C8 F9 104.7(2) . . ?
F1 C8 C5 113.6(2) . . ?
F2 C8 C5 111.6(2) . . ?
F9 C8 F2 105.0(2) . . ?
F9 C8 C5 114.54(19) . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C11 C12 116.33(16) . . ?
O2 C11 O1 125.37(17) . . ?
O2 C11 C12 118.29(17) . . ?
N2 C12 C11 113.93(16) . . ?
N2 C12 H12A 108.8 . . ?
N2 C12 H12B 108.8 . . ?
C11 C12 H12A 108.8 . . ?
C11 C12 H12B 108.8 . . ?
H12A C12 H12B 107.7 . . ?
O3 C13 N2 121.26(19) . . ?
O3 C13 C14 121.3(2) . . ?
N2 C13 C14 117.43(19) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O4 Pd2 O5 90.09(6) . 2_656 ?
O4 Pd2 N3 172.24(6) . . ?
N3 Pd2 O5 93.78(6) . 2_656 ?
C15 Pd2 O4 93.23(7) . . ?
C15 Pd2 O5 173.83(7) . 2_656 ?
C15 Pd2 N3 82.33(8) . . ?
C25 O4 Pd2 124.62(13) . . ?
C25 O5 Pd2 126.94(13) . 2_656 ?
C21 N3 Pd2 108.36(13) . . ?
C23 N3 Pd2 115.45(13) . . ?
C23 N3 C21 108.96(17) . . ?
C23 N3 C24 107.52(17) . . ?
C24 N3 Pd2 106.12(13) . . ?
C24 N3 C21 110.37(17) . . ?
C26 N4 H4A 116.3(17) . . ?
C27 N4 H4A 119.6(17) . . ?
C27 N4 C26 122.75(18) . . ?
C16 C15 Pd2 125.66(16) . . ?
C16 C15 C20 119.50(19) . . ?
C20 C15 Pd2 114.83(16) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 C15 120.4(2) . . ?
C17 C16 H16 119.8 . . ?
C16 C17 H17 119.9 . . ?
C18 C17 C16 120.2(2) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 120.0 . . ?
C17 C18 C19 119.9(2) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 120.3(2) . . ?
C18 C19 C22 119.9(2) . . ?
C20 C19 C22 119.8(2) . . ?
C15 C20 C19 119.5(2) . . ?
C15 C20 C21 115.29(19) . . ?
C19 C20 C21 125.1(2) . . ?
N3 C21 C20 108.54(17) . . ?
N3 C21 H21A 110.0 . . ?
N3 C21 H21B 110.0 . . ?
C20 C21 H21A 110.0 . . ?
C20 C21 H21B 110.0 . . ?
H21A C21 H21B 108.4 . . ?
F4 C22 F6 106.54(19) . . ?
F4 C22 F8 106.1(2) . . ?
F4 C22 C19 112.41(19) . . ?
F6 C22 C19 112.6(2) . . ?
F8 C22 F6 105.95(18) . . ?
F8 C22 C19 112.7(2) . . ?
N3 C23 H23A 109.5 . . ?
N3 C23 H23B 109.5 . . ?
N3 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O4 C25 C26 114.30(17) . . ?
O5 C25 O4 127.38(19) . . ?
O5 C25 C26 118.32(17) . . ?
N4 C26 C25 113.78(17) . . ?
N4 C26 H26A 108.8 . . ?
N4 C26 H26B 108.8 . . ?
C25 C26 H26A 108.8 . . ?
C25 C26 H26B 108.8 . . ?
H26A C26 H26B 107.7 . . ?
O6 C27 N4 122.5(2) . . ?
O6 C27 C28 121.8(2) . . ?
N4 C27 C28 115.67(19) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?

_shelx_SHELXL_version_number     2016/6
_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_complex_6b
_database_code_depnum_ccdc_archive 'CCDC 1544214'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2016-12-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H38 F6 N4 O6 Pd2, C2 H3 N'
_chemical_formula_sum            'C32 H41 F6 N5 O6 Pd2'
_chemical_formula_weight         918.50
_chemical_absolute_configuration ad
_chemical_melting_point          ?
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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.3180(4)
_cell_length_b                   9.8627(4)
_cell_length_c                   40.0507(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3680.7(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9911
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.26
_cell_measurement_theta_min      2.41
_shelx_estimated_absorpt_T_max   0.866
_shelx_estimated_absorpt_T_min   0.715
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. 
wR2(int) was 0.0725 before and 0.0638 after correction. 
The Ratio of minimum to maximum transmission is 0.9320. 
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0715
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            39996
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         2.127
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.695
_reflns_Friedel_fraction_full    0.951
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                5570
_reflns_number_total             6909
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material  
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details 
;
 Flack x determined using 1989 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         6909
_refine_ls_number_restraints     45
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0435
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0157P)²+4.0298P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0620
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O5, O4, C26, C27
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 F3, F1, F2, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C31, N5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C12(H12), C27(H27)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C22(H22A,H22B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4A), C17(H17), C18(H18), C19(H19)
3.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C), C15(H15A,H15B,
 H15C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.66735(5) 0.44898(5) 0.36143(2) 0.01437(13) Uani 1 1 d . . . . .
Pd2 Pd 0.58328(5) 0.16175(5) 0.37214(2) 0.01413(13) Uani 1 1 d . . . . .
O1 O 0.4982(4) 0.4453(5) 0.32903(10) 0.0173(10) Uani 1 1 d . . . . .
O2 O 0.4574(4) 0.2196(4) 0.32996(10) 0.0160(11) Uani 1 1 d . . . . .
O3 O 0.1787(6) 0.3112(4) 0.23245(11) 0.0270(12) Uani 1 1 d . . . . .
O4 O 0.7965(4) 0.3473(5) 0.32571(10) 0.0185(11) Uani 1 1 d . U . . .
O5 O 0.7493(5) 0.1304(4) 0.34009(11) 0.0171(11) Uani 1 1 d . U . . .
O6 O 1.0869(5) 0.1046(5) 0.34242(12) 0.0284(12) Uani 1 1 d . . . . .
N1 N 0.8350(6) 0.4864(5) 0.39366(13) 0.0151(13) Uani 1 1 d . . . . .
N2 N 0.2989(6) 0.2259(6) 0.27598(14) 0.0163(14) Uani 1 1 d . . . . .
H2 H 0.328(7) 0.158(6) 0.2864(15) 0.020 Uiso 1 1 d R . . . .
N3 N 0.4183(6) 0.1588(5) 0.40623(12) 0.0137(11) Uani 1 1 d . . . . .
N4 N 0.9567(5) 0.0399(6) 0.29815(13) 0.0151(14) Uani 1 1 d . . . . .
H4 H 0.915(7) -0.028(6) 0.2883(15) 0.018 Uiso 1 1 d R . . . .
C1 C 0.5577(6) 0.5491(6) 0.39517(15) 0.0130(15) Uani 1 1 d . . . . .
C2 C 0.4211(7) 0.6058(6) 0.39130(17) 0.0171(15) Uani 1 1 d . . . . .
H2A H 0.371470 0.597309 0.370695 0.020 Uiso 1 1 calc R . . . .
C3 C 0.3592(7) 0.6742(6) 0.41762(16) 0.0184(16) Uani 1 1 d . . . . .
H3 H 0.266214 0.711955 0.414886 0.022 Uiso 1 1 calc R . . . .
C4 C 0.4279(8) 0.6891(6) 0.44756(17) 0.0186(16) Uani 1 1 d . . . . .
H4A H 0.382488 0.737046 0.465218 0.022 Uiso 1 1 calc R . . . .
C5 C 0.5639(7) 0.6345(6) 0.45227(15) 0.0129(15) Uani 1 1 d . . . . .
C6 C 0.6292(6) 0.5629(6) 0.42575(15) 0.0122(15) Uani 1 1 d . . . . .
C7 C 0.7726(7) 0.4941(7) 0.42778(16) 0.0165(17) Uani 1 1 d . . . . .
H7A H 0.837302 0.545980 0.442647 0.020 Uiso 1 1 calc R . . . .
H7B H 0.761200 0.401725 0.437085 0.020 Uiso 1 1 calc R . . . .
C8 C 0.6417(7) 0.6518(7) 0.48418(17) 0.0222(16) Uani 1 1 d . U . . .
C9 C 0.8949(7) 0.6198(6) 0.38479(17) 0.0230(18) Uani 1 1 d . . . . .
H9A H 0.929764 0.617559 0.361712 0.035 Uiso 1 1 calc GR . . . .
H9B H 0.974552 0.641450 0.399836 0.035 Uiso 1 1 calc GR . . . .
H9C H 0.820073 0.689115 0.386908 0.035 Uiso 1 1 calc GR . . . .
C10 C 0.9502(7) 0.3858(7) 0.39300(17) 0.0254(19) Uani 1 1 d . . . . .
H10A H 0.910411 0.295757 0.397591 0.038 Uiso 1 1 calc GR . . . .
H10B H 1.021889 0.408394 0.410024 0.038 Uiso 1 1 calc GR . . . .
H10C H 0.995668 0.385849 0.370927 0.038 Uiso 1 1 calc GR . . . .
C11 C 0.4411(6) 0.3386(8) 0.31896(15) 0.0159(15) Uani 1 1 d . . . . .
C12 C 0.3282(7) 0.3572(6) 0.29151(15) 0.0151(15) Uani 1 1 d . . . . .
H12 H 0.367165 0.420280 0.274176 0.018 Uiso 1 1 calc R . . . .
C13 C 0.1951(6) 0.4205(6) 0.30695(16) 0.0176(16) Uani 1 1 d . . . . .
H13A H 0.121528 0.432420 0.289723 0.026 Uiso 1 1 calc GR . . . .
H13B H 0.219816 0.508977 0.316524 0.026 Uiso 1 1 calc GR . . . .
H13C H 0.158259 0.361069 0.324578 0.026 Uiso 1 1 calc GR . . . .
C14 C 0.2300(8) 0.2139(7) 0.24691(17) 0.0191(18) Uani 1 1 d . . . . .
C15 C 0.2185(7) 0.0736(6) 0.23287(17) 0.0249(18) Uani 1 1 d . . . . .
H15A H 0.120542 0.058272 0.224800 0.037 Uiso 1 1 calc GR . . . .
H15B H 0.241189 0.007314 0.250319 0.037 Uiso 1 1 calc GR . . . .
H15C H 0.286183 0.063401 0.214316 0.037 Uiso 1 1 calc GR . . . .
C16 C 0.6923(7) 0.1031(6) 0.41113(16) 0.0145(16) Uani 1 1 d . . . . .
C17 C 0.8267(7) 0.0423(7) 0.41064(16) 0.0211(16) Uani 1 1 d . . . . .
H17 H 0.872704 0.024704 0.389916 0.025 Uiso 1 1 calc R . . . .
C18 C 0.8947(7) 0.0070(6) 0.44052(18) 0.0245(18) Uani 1 1 d . . . . .
H18 H 0.986956 -0.034055 0.440053 0.029 Uiso 1 1 calc R . . . .
C19 C 0.8285(7) 0.0315(7) 0.47052(16) 0.0228(16) Uani 1 1 d . . . . .
H19 H 0.875771 0.008301 0.490745 0.027 Uiso 1 1 calc R . . . .
C20 C 0.6946(7) 0.0890(6) 0.47157(16) 0.0144(16) Uani 1 1 d . . . . .
C21 C 0.6250(6) 0.1247(6) 0.44149(16) 0.0130(16) Uani 1 1 d . . . . .
C22 C 0.4804(7) 0.1913(6) 0.43925(16) 0.0157(17) Uani 1 1 d . . . . .
H22A H 0.417036 0.157216 0.457229 0.019 Uiso 1 1 calc R . . . .
H22B H 0.490344 0.290655 0.441817 0.019 Uiso 1 1 calc R . . . .
C23 C 0.6230(8) 0.1118(8) 0.50421(17) 0.026(2) Uani 1 1 d . . . . .
C24 C 0.3597(7) 0.0195(6) 0.40669(17) 0.0205(18) Uani 1 1 d . . . . .
H24A H 0.322139 -0.003204 0.384529 0.031 Uiso 1 1 calc GR . . . .
H24B H 0.282182 0.013875 0.423162 0.031 Uiso 1 1 calc GR . . . .
H24C H 0.435986 -0.044426 0.412672 0.031 Uiso 1 1 calc GR . . . .
C25 C 0.2971(6) 0.2526(6) 0.39877(16) 0.0181(17) Uani 1 1 d . . . . .
H25A H 0.332427 0.346144 0.398293 0.027 Uiso 1 1 calc GR . . . .
H25B H 0.223417 0.243691 0.416094 0.027 Uiso 1 1 calc GR . . . .
H25C H 0.255657 0.229559 0.377001 0.027 Uiso 1 1 calc GR . . . .
C26 C 0.8076(7) 0.2215(7) 0.32273(15) 0.0144(15) Uani 1 1 d . U . . .
C27 C 0.8965(7) 0.1726(7) 0.29280(15) 0.0178(16) Uani 1 1 d . U . . .
H27 H 0.977126 0.237912 0.289202 0.021 Uiso 1 1 calc R . . . .
C28 C 0.8022(8) 0.1737(7) 0.26215(16) 0.0264(18) Uani 1 1 d . . . . .
H28A H 0.859866 0.151154 0.242458 0.040 Uiso 1 1 calc GR . . . .
H28B H 0.760141 0.264082 0.259339 0.040 Uiso 1 1 calc GR . . . .
H28C H 0.725368 0.106718 0.264768 0.040 Uiso 1 1 calc GR . . . .
C29 C 1.0476(7) 0.0164(7) 0.32348(18) 0.0205(18) Uani 1 1 d . . . . .
C30 C 1.0955(8) -0.1299(6) 0.32719(18) 0.0301(19) Uani 1 1 d . . . . .
H30A H 1.195755 -0.138335 0.320085 0.045 Uiso 1 1 calc GR . . . .
H30B H 1.034974 -0.188217 0.313267 0.045 Uiso 1 1 calc GR . . . .
H30C H 1.086765 -0.157467 0.350605 0.045 Uiso 1 1 calc GR . . . .
F1 F 0.5677(5) 0.7206(4) 0.50723(9) 0.0318(11) Uani 1 1 d . U . . .
F2 F 0.7666(4) 0.7193(4) 0.48031(9) 0.0286(10) Uani 1 1 d . U . . .
F3 F 0.6785(4) 0.5330(4) 0.49850(9) 0.0277(10) Uani 1 1 d . U . . .
F4 F 0.5840(5) 0.2417(4) 0.50874(10) 0.0407(12) Uani 1 1 d . . . . .
F5 F 0.7050(4) 0.0783(4) 0.53020(9) 0.0398(12) Uani 1 1 d . . . . .
F6 F 0.5018(4) 0.0381(5) 0.50750(10) 0.0393(11) Uani 1 1 d . . . . .
N5 N 0.4461(7) -0.0687(8) 0.2906(2) 0.056(2) Uani 1 1 d . U . . .
C31 C 0.5232(9) -0.1163(8) 0.3086(2) 0.042(2) Uani 1 1 d . U . . .
C32 C 0.6262(9) -0.1742(8) 0.33332(19) 0.046(2) Uani 1 1 d . U . . .
H32A H 0.724185 -0.147494 0.327318 0.070 Uiso 1 1 calc GR . . . .
H32B H 0.618739 -0.273313 0.333215 0.070 Uiso 1 1 calc GR . . . .
H32C H 0.603364 -0.139841 0.355653 0.070 Uiso 1 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 O1 2.042(4) . ?
Pd1 O4 2.121(4) . ?
Pd1 N1 2.060(5) . ?
Pd1 C1 1.961(6) . ?
Pd2 O2 2.134(4) . ?
Pd2 O5 2.034(4) . ?
Pd2 N3 2.056(5) . ?
Pd2 C16 1.951(6) . ?
O1 C11 1.246(8) . ?
O2 C11 1.263(8) . ?
O3 C14 1.219(8) . ?
O4 C26 1.251(8) . ?
O5 C26 1.260(7) . ?
O6 C29 1.211(8) . ?
N1 C7 1.487(8) . ?
N1 C9 1.472(7) . ?
N1 C10 1.462(8) . ?
N2 H2 0.84(6) . ?
N2 C12 1.463(8) . ?
N2 C14 1.335(8) . ?
N3 C22 1.479(8) . ?
N3 C24 1.479(8) . ?
N3 C25 1.490(7) . ?
N4 H4 0.87(6) . ?
N4 C27 1.440(8) . ?
N4 C29 1.342(8) . ?
C1 C2 1.398(9) . ?
C1 C6 1.401(8) . ?
C2 H2A 0.9500 . ?
C2 C3 1.378(9) . ?
C3 H3 0.9500 . ?
C3 C4 1.367(9) . ?
C4 H4A 0.9500 . ?
C4 C5 1.390(9) . ?
C5 C6 1.413(8) . ?
C5 C8 1.479(9) . ?
C6 C7 1.501(8) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 F1 1.337(7) . ?
C8 F2 1.350(7) . ?
C8 F3 1.349(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.533(8) . ?
C12 H12 1.0000 . ?
C12 C13 1.520(8) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.497(9) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.389(9) . ?
C16 C21 1.385(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.398(9) . ?
C18 H18 0.9500 . ?
C18 C19 1.372(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.372(9) . ?
C20 C21 1.413(8) . ?
C20 C23 1.485(9) . ?
C21 C22 1.501(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 F4 1.343(8) . ?
C23 F5 1.333(7) . ?
C23 F6 1.350(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.535(8) . ?
C27 H27 1.0000 . ?
C27 C28 1.510(9) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.517(9) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
N5 C31 1.120(10) . ?
C31 C32 1.493(11) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 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
O1 Pd1 O4 90.04(16) . . ?
O1 Pd1 N1 170.72(19) . . ?
N1 Pd1 O4 94.41(18) . . ?
C1 Pd1 O1 92.6(2) . . ?
C1 Pd1 O4 176.7(2) . . ?
C1 Pd1 N1 82.7(2) . . ?
O5 Pd2 O2 87.66(16) . . ?
O5 Pd2 N3 170.3(2) . . ?
N3 Pd2 O2 96.80(18) . . ?
C16 Pd2 O2 177.6(2) . . ?
C16 Pd2 O5 93.7(2) . . ?
C16 Pd2 N3 81.6(2) . . ?
C11 O1 Pd1 123.4(4) . . ?
C11 O2 Pd2 126.2(4) . . ?
C26 O4 Pd1 125.5(4) . . ?
C26 O5 Pd2 124.6(4) . . ?
C7 N1 Pd1 106.8(4) . . ?
C9 N1 Pd1 107.2(4) . . ?
C9 N1 C7 108.9(5) . . ?
C10 N1 Pd1 115.1(4) . . ?
C10 N1 C7 109.8(5) . . ?
C10 N1 C9 108.9(5) . . ?
C12 N2 H2 116(4) . . ?
C14 N2 H2 121(4) . . ?
C14 N2 C12 122.7(6) . . ?
C22 N3 Pd2 107.3(4) . . ?
C22 N3 C25 110.0(5) . . ?
C24 N3 Pd2 107.3(4) . . ?
C24 N3 C22 109.5(5) . . ?
C24 N3 C25 107.4(5) . . ?
C25 N3 Pd2 115.1(4) . . ?
C27 N4 H4 117(4) . . ?
C29 N4 H4 119(4) . . ?
C29 N4 C27 121.0(6) . . ?
C2 C1 Pd1 126.8(5) . . ?
C2 C1 C6 119.4(6) . . ?
C6 C1 Pd1 113.8(4) . . ?
C1 C2 H2A 120.3 . . ?
C3 C2 C1 119.5(6) . . ?
C3 C2 H2A 120.3 . . ?
C2 C3 H3 119.1 . . ?
C4 C3 C2 121.9(6) . . ?
C4 C3 H3 119.1 . . ?
C3 C4 H4A 119.9 . . ?
C3 C4 C5 120.2(6) . . ?
C5 C4 H4A 119.9 . . ?
C4 C5 C6 119.0(6) . . ?
C4 C5 C8 121.2(6) . . ?
C6 C5 C8 119.8(6) . . ?
C1 C6 C5 120.1(5) . . ?
C1 C6 C7 115.3(5) . . ?
C5 C6 C7 124.6(6) . . ?
N1 C7 C6 108.8(5) . . ?
N1 C7 H7A 109.9 . . ?
N1 C7 H7B 109.9 . . ?
C6 C7 H7A 109.9 . . ?
C6 C7 H7B 109.9 . . ?
H7A C7 H7B 108.3 . . ?
F1 C8 C5 113.8(6) . . ?
F1 C8 F2 105.9(5) . . ?
F1 C8 F3 106.2(5) . . ?
F2 C8 C5 112.3(5) . . ?
F3 C8 C5 113.0(6) . . ?
F3 C8 F2 104.9(5) . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
N1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C11 O2 128.3(6) . . ?
O1 C11 C12 115.1(6) . . ?
O2 C11 C12 116.4(6) . . ?
N2 C12 C11 109.1(5) . . ?
N2 C12 H12 108.9 . . ?
N2 C12 C13 112.6(5) . . ?
C11 C12 H12 108.9 . . ?
C13 C12 C11 108.5(5) . . ?
C13 C12 H12 108.9 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O3 C14 N2 122.2(6) . . ?
O3 C14 C15 121.4(6) . . ?
N2 C14 C15 116.4(6) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 Pd2 125.9(5) . . ?
C21 C16 Pd2 114.9(5) . . ?
C21 C16 C17 119.2(6) . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.3(6) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.1(6) . . ?
C19 C18 H18 119.9 . . ?
C18 C19 H19 119.7 . . ?
C20 C19 C18 120.6(6) . . ?
C20 C19 H19 119.7 . . ?
C19 C20 C21 119.6(6) . . ?
C19 C20 C23 119.9(6) . . ?
C21 C20 C23 120.5(6) . . ?
C16 C21 C20 120.2(6) . . ?
C16 C21 C22 114.9(5) . . ?
C20 C21 C22 124.9(6) . . ?
N3 C22 C21 108.1(5) . . ?
N3 C22 H22A 110.1 . . ?
N3 C22 H22B 110.1 . . ?
C21 C22 H22A 110.1 . . ?
C21 C22 H22B 110.1 . . ?
H22A C22 H22B 108.4 . . ?
F4 C23 C20 112.6(6) . . ?
F4 C23 F6 105.9(6) . . ?
F5 C23 C20 113.1(6) . . ?
F5 C23 F4 106.6(6) . . ?
F5 C23 F6 105.7(6) . . ?
F6 C23 C20 112.4(6) . . ?
N3 C24 H24A 109.5 . . ?
N3 C24 H24B 109.5 . . ?
N3 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N3 C25 H25A 109.5 . . ?
N3 C25 H25B 109.5 . . ?
N3 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O4 C26 O5 128.3(6) . . ?
O4 C26 C27 115.5(6) . . ?
O5 C26 C27 116.1(6) . . ?
N4 C27 C26 112.3(5) . . ?
N4 C27 H27 108.4 . . ?
N4 C27 C28 110.8(5) . . ?
C26 C27 H27 108.4 . . ?
C28 C27 C26 108.5(5) . . ?
C28 C27 H27 108.4 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O6 C29 N4 122.7(6) . . ?
O6 C29 C30 122.2(6) . . ?
N4 C29 C30 115.1(6) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N5 C31 C32 177.6(10) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 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 O1 C11 O2 12.4(9) . . . . ?
Pd1 O1 C11 C12 -172.8(4) . . . . ?
Pd1 O4 C26 O5 -1.7(10) . . . . ?
Pd1 O4 C26 C27 174.3(4) . . . . ?
Pd1 N1 C7 C6 -37.3(5) . . . . ?
Pd1 C1 C2 C3 -179.6(5) . . . . ?
Pd1 C1 C6 C5 179.1(4) . . . . ?
Pd1 C1 C6 C7 -2.6(7) . . . . ?
Pd2 O2 C11 O1 3.4(9) . . . . ?
Pd2 O2 C11 C12 -171.3(4) . . . . ?
Pd2 O5 C26 O4 14.4(9) . . . . ?
Pd2 O5 C26 C27 -161.6(4) . . . . ?
Pd2 N3 C22 C21 -37.8(5) . . . . ?
Pd2 C16 C17 C18 178.9(5) . . . . ?
Pd2 C16 C21 C20 -178.6(4) . . . . ?
Pd2 C16 C21 C22 -0.8(7) . . . . ?
O1 C11 C12 N2 165.0(5) . . . . ?
O1 C11 C12 C13 -72.0(7) . . . . ?
O2 C11 C12 N2 -19.6(7) . . . . ?
O2 C11 C12 C13 103.4(6) . . . . ?
O4 C26 C27 N4 154.9(6) . . . . ?
O4 C26 C27 C28 -82.3(7) . . . . ?
O5 C26 C27 N4 -28.5(8) . . . . ?
O5 C26 C27 C28 94.3(7) . . . . ?
C1 C2 C3 C4 0.4(10) . . . . ?
C1 C6 C7 N1 27.5(7) . . . . ?
C2 C1 C6 C5 -0.5(9) . . . . ?
C2 C1 C6 C7 177.8(5) . . . . ?
C2 C3 C4 C5 -0.2(10) . . . . ?
C3 C4 C5 C6 -0.3(9) . . . . ?
C3 C4 C5 C8 178.7(6) . . . . ?
C4 C5 C6 C1 0.7(9) . . . . ?
C4 C5 C6 C7 -177.4(6) . . . . ?
C4 C5 C8 F1 1.4(9) . . . . ?
C4 C5 C8 F2 -118.9(6) . . . . ?
C4 C5 C8 F3 122.6(6) . . . . ?
C5 C6 C7 N1 -154.3(6) . . . . ?
C6 C1 C2 C3 -0.1(9) . . . . ?
C6 C5 C8 F1 -179.6(5) . . . . ?
C6 C5 C8 F2 60.1(8) . . . . ?
C6 C5 C8 F3 -58.4(8) . . . . ?
C8 C5 C6 C1 -178.3(6) . . . . ?
C8 C5 C6 C7 3.5(9) . . . . ?
C9 N1 C7 C6 78.1(6) . . . . ?
C10 N1 C7 C6 -162.7(5) . . . . ?
C12 N2 C14 O3 -4.9(10) . . . . ?
C12 N2 C14 C15 175.2(6) . . . . ?
C14 N2 C12 C11 -165.0(6) . . . . ?
C14 N2 C12 C13 74.5(8) . . . . ?
C16 C17 C18 C19 0.4(10) . . . . ?
C16 C21 C22 N3 26.5(7) . . . . ?
C17 C16 C21 C20 2.0(9) . . . . ?
C17 C16 C21 C22 179.8(6) . . . . ?
C17 C18 C19 C20 0.8(10) . . . . ?
C18 C19 C20 C21 -0.6(10) . . . . ?
C18 C19 C20 C23 178.5(6) . . . . ?
C19 C20 C21 C16 -0.8(9) . . . . ?
C19 C20 C21 C22 -178.4(6) . . . . ?
C19 C20 C23 F4 124.5(7) . . . . ?
C19 C20 C23 F5 3.5(9) . . . . ?
C19 C20 C23 F6 -116.0(7) . . . . ?
C20 C21 C22 N3 -155.8(6) . . . . ?
C21 C16 C17 C18 -1.8(10) . . . . ?
C21 C20 C23 F4 -56.3(8) . . . . ?
C21 C20 C23 F5 -177.3(6) . . . . ?
C21 C20 C23 F6 63.2(8) . . . . ?
C23 C20 C21 C16 -180.0(6) . . . . ?
C23 C20 C21 C22 2.4(9) . . . . ?
C24 N3 C22 C21 78.4(6) . . . . ?
C25 N3 C22 C21 -163.7(5) . . . . ?
C27 N4 C29 O6 -2.1(10) . . . . ?
C27 N4 C29 C30 176.7(6) . . . . ?
C29 N4 C27 C26 -60.5(7) . . . . ?
C29 N4 C27 C28 178.0(6) . . . . ?

_shelx_SHELXL_version_number     2016/6
_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_complex_15
_database_code_depnum_ccdc_archive 'CCDC 1544218'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2016-12-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;

_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C13 H17.5 Cl0.5 N2 O3 Pd)'
_chemical_formula_sum            'C26 H35 Cl N4 O6 Pd2'
_chemical_formula_weight         747.83
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0010 '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'
Cl Cl 0.0550 0.0530 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0020 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.5290 2.5730 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.2982(5)
_cell_length_b                   16.4180(5)
_cell_length_c                   19.7030(6)
_cell_angle_alpha                90
_cell_angle_beta                 96.7390(10)
_cell_angle_gamma                90
_cell_volume                     6199.5(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.45
_cell_measurement_theta_min      2.25
_shelx_estimated_absorpt_T_max   0.968
_shelx_estimated_absorpt_T_min   0.938
_exptl_absorpt_coefficient_mu    1.630
_exptl_absorpt_correction_T_max  0.7443
_exptl_absorpt_correction_T_min  0.6334
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1561 before and 0.0870 after correction.
The Ratio of minimum to maximum transmission is 0.8510.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1001
_diffrn_reflns_av_unetI/netI     0.0708
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            85500
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         18.875
_diffrn_reflns_theta_min         1.086
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker D8 fixed-chi'
_diffrn_measurement_method       'phi rotation'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_source                   synchrotron
_diffrn_source_type              
"Insertion Device, Station 15 ID-B, APS, Argonne Nat'l Lab"
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8921
_reflns_number_total             12148
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material  
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_refine_diff_density_max         1.058
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         12148
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0402
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0310P)²+2.4065P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0921
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N4-H4A
 0.88 with sigma of 0.02
 N2-H2
 0.88 with sigma of 0.02
3. Others
 Fixed Sof: Cl1(0.5) H5(0.5) Cl2(0.5) H18(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C11(H11A,H11B), C20(H20A,H20B), C24(H24A,H24B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C18(H18)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C), C26(H26A,H26B,H26C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.57502(2) 0.87001(2) 0.73455(2) 0.01732(5) Uani 1 1 d . . . . .
Cl1 Cl 0.66229(7) 1.18566(8) 0.69811(8) 0.0315(3) Uani 0.5 1 d . . P A 1
O1 O 0.53229(10) 0.79513(11) 0.65733(9) 0.0240(4) Uani 1 1 d . . . . .
O2 O 0.42634(10) 0.77373(11) 0.69113(9) 0.0238(4) Uani 1 1 d . . . . .
O3 O 0.34940(12) 0.72544(14) 0.49007(11) 0.0397(5) Uani 1 1 d . . . . .
N1 N 0.63303(11) 0.94609(14) 0.80223(11) 0.0223(4) Uani 1 1 d . . . . .
N2 N 0.39289(12) 0.66213(14) 0.58729(11) 0.0207(4) Uani 1 1 d D . . . .
H2 H 0.3854(16) 0.6264(15) 0.6170(13) 0.025 Uiso 1 1 d DR . . . .
C1 C 0.58619(14) 0.95925(16) 0.67034(13) 0.0219(5) Uani 1 1 d . . . . .
C2 C 0.57385(15) 0.95533(19) 0.59893(14) 0.0289(6) Uani 1 1 d . . . . .
H2A H 0.558034 0.906087 0.576991 0.035 Uiso 1 1 calc R . . . .
C3 C 0.58498(18) 1.0245(2) 0.56015(17) 0.0385(8) Uani 1 1 d . . . . .
H3 H 0.575571 1.022087 0.511773 0.046 Uiso 1 1 calc R . . . .
C4 C 0.60915(18) 1.0955(2) 0.59055(19) 0.0445(9) Uani 1 1 d . . . . .
H4 H 0.616546 1.141872 0.563531 0.053 Uiso 1 1 calc R . . . .
C5 C 0.62293(18) 1.0992(2) 0.66201(19) 0.0407(8) Uani 1 1 d . . . . .
H5 H 0.640873 1.147868 0.683398 0.049 Uiso 0.5 1 calc R . P A 2
C6 C 0.61046(16) 1.03195(17) 0.70161(15) 0.0283(6) Uani 1 1 d . . . . .
C7 C 0.61969(18) 1.03126(17) 0.77844(15) 0.0326(7) Uani 1 1 d . . . . .
H7A H 0.659444 1.066499 0.795920 0.039 Uiso 1 1 calc R . . . .
H7B H 0.577113 1.052457 0.795854 0.039 Uiso 1 1 calc R . . . .
C8 C 0.70745(15) 0.9249(2) 0.79877(17) 0.0358(7) Uani 1 1 d . . . . .
H8A H 0.715366 0.867781 0.811828 0.054 Uiso 1 1 calc GR . . . .
H8B H 0.737295 0.959899 0.830164 0.054 Uiso 1 1 calc GR . . . .
H8C H 0.718748 0.933133 0.752043 0.054 Uiso 1 1 calc GR . . . .
C9 C 0.61888(16) 0.9393(2) 0.87459(13) 0.0311(6) Uani 1 1 d . . . . .
H9A H 0.569011 0.947809 0.877283 0.047 Uiso 1 1 calc GR . . . .
H9B H 0.645878 0.980699 0.902111 0.047 Uiso 1 1 calc GR . . . .
H9C H 0.632431 0.885040 0.892065 0.047 Uiso 1 1 calc GR . . . .
C10 C 0.47243(14) 0.76203(15) 0.65267(12) 0.0197(5) Uani 1 1 d . . . . .
C11 C 0.45930(14) 0.70369(17) 0.59275(13) 0.0241(5) Uani 1 1 d . . . . .
H11A H 0.462294 0.734512 0.550007 0.029 Uiso 1 1 calc R . . . .
H11B H 0.496911 0.662357 0.596665 0.029 Uiso 1 1 calc R . . . .
C12 C 0.34232(15) 0.67669(18) 0.53585(14) 0.0267(6) Uani 1 1 d . . . . .
C13 C 0.27731(17) 0.6259(2) 0.53648(19) 0.0434(9) Uani 1 1 d . . . . .
H13A H 0.236141 0.661194 0.529382 0.065 Uiso 1 1 calc GR . . . .
H13B H 0.278374 0.598195 0.580645 0.065 Uiso 1 1 calc GR . . . .
H13C H 0.275156 0.585311 0.499826 0.065 Uiso 1 1 calc GR . . . .
Pd2 Pd 0.52565(2) 0.47686(2) 0.82386(2) 0.01586(5) Uani 1 1 d . . . . .
Cl2 Cl 0.56169(8) 0.15682(8) 0.90914(7) 0.0275(3) Uani 0.5 1 d . . P B 1
O4 O 0.60181(9) 0.55190(11) 0.79337(9) 0.0208(4) Uani 1 1 d . . . . .
O5 O 0.54988(9) 0.57377(11) 0.68624(9) 0.0202(4) Uani 1 1 d . . . . .
O6 O 0.70429(11) 0.57773(13) 0.60917(11) 0.0335(5) Uani 1 1 d . . . . .
N3 N 0.45951(11) 0.39938(13) 0.86773(10) 0.0191(4) Uani 1 1 d . . . . .
N4 N 0.64963(12) 0.68100(14) 0.65774(12) 0.0232(5) Uani 1 1 d D . . . .
H4A H 0.6194(14) 0.7197(15) 0.6481(15) 0.028 Uiso 1 1 d DR . . . .
C14 C 0.59141(13) 0.38617(16) 0.84246(12) 0.0195(5) Uani 1 1 d . . . . .
C15 C 0.66385(13) 0.38903(17) 0.84252(13) 0.0230(5) Uani 1 1 d . . . . .
H15 H 0.686033 0.438840 0.833407 0.028 Uiso 1 1 calc R . . . .
C16 C 0.70341(15) 0.31856(19) 0.85600(15) 0.0308(6) Uani 1 1 d . . . . .
H16 H 0.752481 0.320415 0.854995 0.037 Uiso 1 1 calc R . . . .
C17 C 0.67191(17) 0.24572(19) 0.87087(18) 0.0389(8) Uani 1 1 d . . . . .
H17 H 0.699081 0.197800 0.879615 0.047 Uiso 1 1 calc R . . . .
C18 C 0.60011(17) 0.24371(19) 0.87281(19) 0.0398(8) Uani 1 1 d . . . . .
H18 H 0.578480 0.194536 0.884574 0.048 Uiso 0.5 1 calc R . P B 2
C19 C 0.55976(15) 0.31269(17) 0.85777(15) 0.0265(6) Uani 1 1 d . . . . .
C20 C 0.48201(15) 0.31407(17) 0.85528(17) 0.0318(7) Uani 1 1 d . . . . .
H20A H 0.460297 0.295134 0.810006 0.038 Uiso 1 1 calc R . . . .
H20B H 0.467056 0.277288 0.890627 0.038 Uiso 1 1 calc R . . . .
C21 C 0.38403(13) 0.40723(17) 0.84433(13) 0.0224(5) Uani 1 1 d . . . . .
H21A H 0.367673 0.460993 0.857070 0.034 Uiso 1 1 calc GR . . . .
H21B H 0.358292 0.364867 0.865893 0.034 Uiso 1 1 calc GR . . . .
H21C H 0.376186 0.401021 0.794556 0.034 Uiso 1 1 calc GR . . . .
C22 C 0.47021(15) 0.4175(2) 0.94211(13) 0.0324(7) Uani 1 1 d . . . . .
H22A H 0.519505 0.409836 0.959368 0.049 Uiso 1 1 calc GR . . . .
H22B H 0.441513 0.380643 0.966225 0.049 Uiso 1 1 calc GR . . . .
H22C H 0.456679 0.473985 0.949807 0.049 Uiso 1 1 calc GR . . . .
C23 C 0.59683(13) 0.58509(15) 0.73464(12) 0.0187(5) Uani 1 1 d . . . . .
C24 C 0.65612(14) 0.64362(17) 0.72449(13) 0.0232(5) Uani 1 1 d . . . . .
H24A H 0.657651 0.686966 0.759571 0.028 Uiso 1 1 calc R . . . .
H24B H 0.700868 0.613602 0.731679 0.028 Uiso 1 1 calc R . . . .
C25 C 0.67113(14) 0.64192(18) 0.60368(14) 0.0255(6) Uani 1 1 d . . . . .
C26 C 0.65509(17) 0.6849(2) 0.53609(15) 0.0368(7) Uani 1 1 d . . . . .
H26A H 0.696269 0.715392 0.525876 0.055 Uiso 1 1 calc GR . . . .
H26B H 0.616054 0.722562 0.538421 0.055 Uiso 1 1 calc GR . . . .
H26C H 0.642515 0.644643 0.500001 0.055 Uiso 1 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 Pd1 3.0279(4) 2_656 ?
Pd1 O1 2.0522(18) . ?
Pd1 O2 2.1571(17) 2_656 ?
Pd1 N1 2.060(2) . ?
Pd1 C1 1.964(3) . ?
Cl1 C5 1.724(4) . ?
O1 C10 1.270(3) . ?
O2 C10 1.249(3) . ?
O3 C12 1.225(3) . ?
N1 C7 1.487(4) . ?
N1 C8 1.487(4) . ?
N1 C9 1.487(3) . ?
N2 H2 0.853(17) . ?
N2 C11 1.445(3) . ?
N2 C12 1.343(3) . ?
C1 C2 1.401(4) . ?
C1 C6 1.398(4) . ?
C2 H2A 0.9500 . ?
C2 C3 1.399(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.367(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.403(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.389(4) . ?
C6 C7 1.503(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.518(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.508(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
Pd2 Pd2 2.9621(4) 2_656 ?
Pd2 O4 2.0606(18) . ?
Pd2 O5 2.1512(17) 2_656 ?
Pd2 N3 2.063(2) . ?
Pd2 C14 1.963(2) . ?
Cl2 C18 1.795(4) . ?
O4 C23 1.272(3) . ?
O5 C23 1.250(3) . ?
O6 C25 1.231(4) . ?
N3 C20 1.495(4) . ?
N3 C21 1.481(3) . ?
N3 C22 1.486(3) . ?
N4 H4A 0.868(17) . ?
N4 C24 1.443(3) . ?
N4 C25 1.350(4) . ?
C14 C15 1.399(4) . ?
C14 C19 1.401(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.394(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.388(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.391(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.387(4) . ?
C19 C20 1.496(4) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.525(3) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.507(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 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
O1 Pd1 Pd1 80.71(5) . 2_656 ?
O1 Pd1 O2 91.63(7) . 2_656 ?
O1 Pd1 N1 169.72(8) . . ?
O2 Pd1 Pd1 77.02(5) 2_656 2_656 ?
N1 Pd1 Pd1 109.26(6) . 2_656 ?
N1 Pd1 O2 93.09(8) . 2_656 ?
C1 Pd1 Pd1 108.02(8) . 2_656 ?
C1 Pd1 O1 91.96(10) . . ?
C1 Pd1 O2 174.23(10) . 2_656 ?
C1 Pd1 N1 82.65(10) . . ?
C10 O1 Pd1 126.35(16) . . ?
C10 O2 Pd1 126.20(17) . 2_656 ?
C7 N1 Pd1 107.77(16) . . ?
C7 N1 C8 109.7(2) . . ?
C7 N1 C9 109.1(2) . . ?
C8 N1 Pd1 106.45(17) . . ?
C8 N1 C9 108.3(2) . . ?
C9 N1 Pd1 115.37(17) . . ?
C11 N2 H2 120(2) . . ?
C12 N2 H2 118(2) . . ?
C12 N2 C11 122.1(2) . . ?
C2 C1 Pd1 126.4(2) . . ?
C6 C1 Pd1 114.2(2) . . ?
C6 C1 C2 119.4(2) . . ?
C1 C2 H2A 120.3 . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2A 120.3 . . ?
C2 C3 H3 119.4 . . ?
C4 C3 C2 121.3(3) . . ?
C4 C3 H3 119.4 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 Cl1 118.2(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 Cl1 121.3(3) . . ?
C6 C5 C4 120.3(3) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 C7 115.5(2) . . ?
C5 C6 C1 120.1(3) . . ?
C5 C6 C7 124.3(3) . . ?
N1 C7 C6 108.7(2) . . ?
N1 C7 H7A 110.0 . . ?
N1 C7 H7B 110.0 . . ?
C6 C7 H7A 110.0 . . ?
C6 C7 H7B 110.0 . . ?
H7A C7 H7B 108.3 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 H9A 109.5 . . ?
N1 C9 H9B 109.5 . . ?
N1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O1 C10 C11 113.2(2) . . ?
O2 C10 O1 126.6(2) . . ?
O2 C10 C11 120.2(2) . . ?
N2 C11 C10 114.9(2) . . ?
N2 C11 H11A 108.5 . . ?
N2 C11 H11B 108.5 . . ?
C10 C11 H11A 108.5 . . ?
C10 C11 H11B 108.5 . . ?
H11A C11 H11B 107.5 . . ?
O3 C12 N2 122.5(3) . . ?
O3 C12 C13 122.1(3) . . ?
N2 C12 C13 115.3(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O4 Pd2 Pd2 83.18(5) . 2_656 ?
O4 Pd2 O5 91.70(7) . 2_656 ?
O4 Pd2 N3 171.35(8) . . ?
O5 Pd2 Pd2 76.37(5) 2_656 2_656 ?
N3 Pd2 Pd2 105.06(6) . 2_656 ?
N3 Pd2 O5 92.80(8) . 2_656 ?
C14 Pd2 Pd2 108.53(7) . 2_656 ?
C14 Pd2 O4 92.32(9) . . ?
C14 Pd2 O5 174.01(9) . 2_656 ?
C14 Pd2 N3 82.66(10) . . ?
C23 O4 Pd2 122.73(16) . . ?
C23 O5 Pd2 127.10(16) . 2_656 ?
C20 N3 Pd2 107.64(16) . . ?
C21 N3 Pd2 116.76(15) . . ?
C21 N3 C20 108.9(2) . . ?
C21 N3 C22 107.9(2) . . ?
C22 N3 Pd2 105.58(17) . . ?
C22 N3 C20 109.9(2) . . ?
C24 N4 H4A 120(2) . . ?
C25 N4 H4A 116(2) . . ?
C25 N4 C24 121.0(2) . . ?
C15 C14 Pd2 126.8(2) . . ?
C15 C14 C19 119.3(2) . . ?
C19 C14 Pd2 113.88(19) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 C14 119.8(3) . . ?
C16 C15 H15 120.1 . . ?
C15 C16 H16 119.6 . . ?
C17 C16 C15 120.8(3) . . ?
C17 C16 H16 119.6 . . ?
C16 C17 H17 120.4 . . ?
C16 C17 C18 119.2(3) . . ?
C18 C17 H17 120.4 . . ?
C17 C18 Cl2 119.3(2) . . ?
C17 C18 H18 119.6 . . ?
C19 C18 Cl2 119.1(3) . . ?
C19 C18 C17 120.7(3) . . ?
C19 C18 H18 119.6 . . ?
C14 C19 C20 116.2(2) . . ?
C18 C19 C14 120.1(3) . . ?
C18 C19 C20 123.7(3) . . ?
N3 C20 C19 108.6(2) . . ?
N3 C20 H20A 110.0 . . ?
N3 C20 H20B 110.0 . . ?
C19 C20 H20A 110.0 . . ?
C19 C20 H20B 110.0 . . ?
H20A C20 H20B 108.4 . . ?
N3 C21 H21A 109.5 . . ?
N3 C21 H21B 109.5 . . ?
N3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N3 C22 H22A 109.5 . . ?
N3 C22 H22B 109.5 . . ?
N3 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O4 C23 C24 114.3(2) . . ?
O5 C23 O4 126.9(2) . . ?
O5 C23 C24 118.8(2) . . ?
N4 C24 C23 113.7(2) . . ?
N4 C24 H24A 108.8 . . ?
N4 C24 H24B 108.8 . . ?
C23 C24 H24A 108.8 . . ?
C23 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
O6 C25 N4 122.8(3) . . ?
O6 C25 C26 122.0(3) . . ?
N4 C25 C26 115.1(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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 O1 C10 O2 6.0(4) . . . . ?
Pd1 O1 C10 C11 -174.51(17) . . . . ?
Pd1 O2 C10 O1 12.7(4) 2_656 . . . ?
Pd1 O2 C10 C11 -166.77(18) 2_656 . . . ?
Pd1 N1 C7 C6 -35.3(3) . . . . ?
Pd1 C1 C2 C3 -179.4(2) . . . . ?
Pd1 C1 C6 C5 177.8(2) . . . . ?
Pd1 C1 C6 C7 -3.5(3) . . . . ?
Cl1 C5 C6 C1 -172.4(3) . . . . ?
Cl1 C5 C6 C7 9.1(5) . . . . ?
O1 C10 C11 N2 177.5(2) . . . . ?
O2 C10 C11 N2 -2.9(4) . . . . ?
C1 C2 C3 C4 1.4(5) . . . . ?
C1 C6 C7 N1 26.5(4) . . . . ?
C2 C1 C6 C5 -0.8(4) . . . . ?
C2 C1 C6 C7 177.9(3) . . . . ?
C2 C3 C4 C5 -0.1(5) . . . . ?
C3 C4 C5 Cl1 173.0(3) . . . . ?
C3 C4 C5 C6 -1.6(5) . . . . ?
C4 C5 C6 C1 2.1(5) . . . . ?
C4 C5 C6 C7 -176.4(3) . . . . ?
C5 C6 C7 N1 -154.9(3) . . . . ?
C6 C1 C2 C3 -1.0(4) . . . . ?
C8 N1 C7 C6 80.2(3) . . . . ?
C9 N1 C7 C6 -161.3(2) . . . . ?
C11 N2 C12 O3 0.6(4) . . . . ?
C11 N2 C12 C13 177.9(3) . . . . ?
C12 N2 C11 C10 112.2(3) . . . . ?
Pd2 O4 C23 O5 -5.4(4) . . . . ?
Pd2 O4 C23 C24 175.37(16) . . . . ?
Pd2 O5 C23 O4 -14.6(4) 2_656 . . . ?
Pd2 O5 C23 C24 164.63(17) 2_656 . . . ?
Pd2 N3 C20 C19 34.9(3) . . . . ?
Pd2 C14 C15 C16 -179.2(2) . . . . ?
Pd2 C14 C19 C18 -179.2(2) . . . . ?
Pd2 C14 C19 C20 2.0(3) . . . . ?
Cl2 C18 C19 C14 167.2(2) . . . . ?
Cl2 C18 C19 C20 -14.0(5) . . . . ?
O4 C23 C24 N4 -179.8(2) . . . . ?
O5 C23 C24 N4 0.9(3) . . . . ?
C14 C15 C16 C17 -1.4(4) . . . . ?
C14 C19 C20 N3 -25.3(4) . . . . ?
C15 C14 C19 C18 0.0(4) . . . . ?
C15 C14 C19 C20 -178.8(3) . . . . ?
C15 C16 C17 C18 -0.6(5) . . . . ?
C16 C17 C18 Cl2 -167.0(3) . . . . ?
C16 C17 C18 C19 2.3(5) . . . . ?
C17 C18 C19 C14 -2.0(5) . . . . ?
C17 C18 C19 C20 176.7(3) . . . . ?
C18 C19 C20 N3 155.9(3) . . . . ?
C19 C14 C15 C16 1.7(4) . . . . ?
C21 N3 C20 C19 162.4(2) . . . . ?
C22 N3 C20 C19 -79.6(3) . . . . ?
C24 N4 C25 O6 -8.7(4) . . . . ?
C24 N4 C25 C26 174.6(2) . . . . ?
C25 N4 C24 C23 -82.8(3) . . . . ?

_shelx_SHELXL_version_number     2016/6
_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_complex_S5_1
_database_code_depnum_ccdc_archive 'CCDC 1544217'
_audit_update_record             
;
2017-04-15 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_audit_creation_date             2016-12-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl6 Pd2, 2(C2 H8 N)'
_chemical_formula_sum            'C4 H16 Cl6 N2 Pd2'
_chemical_formula_weight         517.69
_chemical_melting_point          ?
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'
Cl Cl 0.1484 0.1585 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   7.6908(5)
_cell_length_b                   13.0776(8)
_cell_length_c                   7.1107(4)
_cell_angle_alpha                90
_cell_angle_beta                 90.8831(14)
_cell_angle_gamma                90
_cell_volume                     715.09(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.72
_cell_measurement_theta_min      3.07
_shelx_estimated_absorpt_T_max   0.693
_shelx_estimated_absorpt_T_min   0.392
_exptl_absorpt_coefficient_mu    3.603
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1256 before and 0.0359 after correction.
The Ratio of minimum to maximum transmission is 0.8080.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.404
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17218
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.747
_diffrn_reflns_theta_min         3.073
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'INCOATEC ImuS micro-focus source'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1339
_reflns_number_total             1435
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX3 v.2015.9-0 (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V.8.35A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    
;
OLEX2: a complete structure solution, refinement and analysis program 
Dolomanov et al., 2009

Mercury: visualization and analysis of crystal structures
Macrae, et al., 2006

O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann.
J. Appl. Cryst. (2009). 42, 339-341;

C. F. Macrae, P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
M. Towler and J. van de Streek, J. Appl. Cryst. (2006). 39, 453-457.
;
_computing_publication_material  
;
 APEX3 v.2015.5-2 (Bruker AXS Inc., 2015)
 OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement  'XL-2014/7 (Sheldrick, 2015b)'
_computing_structure_solution    'XT 2014/5 (Sheldrick, 2015a)'
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         1435
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0137
_refine_ls_R_factor_gt           0.0115
_refine_ls_restrained_S_all      1.137
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0085P)²+0.5992P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0247
_refine_ls_wR_factor_ref         0.0253
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   mixed
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.500000 0.500000 0.500000 0.00892(3) Uani 1 2 d S T P . .
Cl2 Cl 0.500000 0.61254(2) 0.750000 0.01304(6) Uani 1 2 d S T P . .
Cl1 Cl 0.75317(3) 0.42697(2) 0.61408(3) 0.01399(5) Uani 1 1 d . . . . .
N1 N 1.000000 0.37417(10) 0.250000 0.0137(2) Uani 1 2 d S T P . .
H1 H 1.0732(19) 0.4132(12) 0.203(2) 0.024(4) Uiso 1 1 d . . . . .
C2 C 1.08362(14) 0.31040(9) 0.39908(16) 0.01868(19) Uani 1 1 d . . . . .
H2A H 1.171901 0.266390 0.342874 0.028 Uiso 1 1 calc GR . . . .
H2B H 0.995356 0.267911 0.459059 0.028 Uiso 1 1 calc GR . . . .
H2C H 1.138704 0.354890 0.493552 0.028 Uiso 1 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 Cl2 2.3079(2) . ?
Pd1 Cl2 2.3079(2) 5_666 ?
Pd1 Cl1 2.3049(3) . ?
Pd1 Cl1 2.3049(3) 5_666 ?
N1 H1 0.834(15) 2_755 ?
N1 H1 0.834(15) . ?
N1 C2 1.4872(13) . ?
N1 C2 1.4872(13) 2_755 ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 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
Cl2 Pd1 Cl2 180.0 . 5_666 ?
Cl1 Pd1 Cl2 90.182(7) 5_666 5_666 ?
Cl1 Pd1 Cl2 90.183(7) . . ?
Cl1 Pd1 Cl2 89.817(7) . 5_666 ?
Cl1 Pd1 Cl2 89.818(7) 5_666 . ?
Cl1 Pd1 Cl1 180.0 . 5_666 ?
Pd1 Cl2 Pd1 100.756(13) . 2_656 ?
H1 N1 H1 104(2) . 2_755 ?
C2 N1 H1 110.0(11) . . ?
C2 N1 H1 110.2(11) . 2_755 ?
C2 N1 H1 110.2(11) 2_755 . ?
C2 N1 H1 110.0(11) 2_755 2_755 ?
C2 N1 C2 111.79(12) . 2_755 ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_shelx_SHELXL_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'
