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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1053822'
_audit_update_record             
;
2015-03-13 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H31 N3 O6'
_chemical_formula_weight         517.57

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

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                   19.2486(2)
_cell_length_b                   10.91640(10)
_cell_length_c                   12.41140(10)
_cell_angle_alpha                90
_cell_angle_beta                 93.1170(10)
_cell_angle_gamma                90
_cell_volume                     2604.09(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.0(2)
_cell_measurement_reflns_used    22382
_cell_measurement_theta_min      4.0480
_cell_measurement_theta_max      76.5820

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_F_000             1096
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    0.763
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.0(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40606
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         4.601
_diffrn_reflns_theta_max         76.776
_diffrn_reflns_theta_full        67.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5459
_reflns_number_gt                5027
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0390P)²+1.6586P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5459
_refine_ls_number_parameters     345
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.1046
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C 0.50973(9) -0.61250(15) 0.39259(13) 0.0324(3) Uani 1 1 d . . . . .
H1A H 0.5540 -0.6120 0.4321 0.049 Uiso 1 1 calc R U . . .
H1B H 0.4748 -0.5806 0.4373 0.049 Uiso 1 1 calc R U . . .
H1C H 0.5122 -0.5625 0.3293 0.049 Uiso 1 1 calc R U . . .
C2 C 0.54464(8) -0.79551(13) 0.30638(12) 0.0255(3) Uani 1 1 d . . . . .
H2A H 0.5377 -0.8831 0.3132 0.031 Uiso 1 1 calc R U . . .
H2B H 0.5896 -0.7759 0.3412 0.031 Uiso 1 1 calc R U . . .
C3 C 0.54613(8) -0.76412(13) 0.18832(12) 0.0234(3) Uani 1 1 d . . . . .
H3A H 0.5732 -0.8248 0.1517 0.028 Uiso 1 1 calc R U . . .
H3B H 0.4992 -0.7644 0.1557 0.028 Uiso 1 1 calc R U . . .
C4 C 0.58155(8) -0.61409(13) 0.06734(11) 0.0222(3) Uani 1 1 d . . . . .
H4A H 0.5360 -0.6167 0.0298 0.027 Uiso 1 1 calc R U . . .
H4B H 0.6120 -0.6708 0.0325 0.027 Uiso 1 1 calc R U . . .
C5 C 0.61099(8) -0.48579(12) 0.06510(11) 0.0205(3) Uani 1 1 d . . . . .
H5A H 0.5792 -0.4278 0.0955 0.025 Uiso 1 1 calc R U . . .
H5B H 0.6553 -0.4817 0.1060 0.025 Uiso 1 1 calc R U . . .
C6 C 0.64214(7) -0.31693(13) -0.18071(11) 0.0214(3) Uani 1 1 d . . . . .
H6 H 0.6341 -0.3804 -0.2298 0.026 Uiso 1 1 calc R U . . .
C7 C 0.63802(7) -0.34239(12) -0.07085(11) 0.0188(3) Uani 1 1 d . . . . .
C8 C 0.65225(7) -0.25060(12) 0.00403(11) 0.0189(3) Uani 1 1 d . . . . .
H8 H 0.6512 -0.2655 0.0777 0.023 Uiso 1 1 calc R U . . .
C9 C 0.66832(7) -0.13447(12) -0.03529(11) 0.0192(3) Uani 1 1 d . . . . .
C10 C 0.66895(8) -0.11674(13) -0.14694(11) 0.0229(3) Uani 1 1 d . . . . .
H10 H 0.6782 -0.0386 -0.1724 0.027 Uiso 1 1 calc R U . . .
C11 C 0.68565(7) -0.03370(13) 0.03535(11) 0.0208(3) Uani 1 1 d . . . . .
C12 C 0.70251(7) 0.05200(13) 0.08974(11) 0.0200(3) Uani 1 1 d . . . . .
C13 C 0.72676(7) 0.15914(12) 0.14965(11) 0.0176(3) Uani 1 1 d . . . . .
C14 C 0.72660(7) 0.16454(13) 0.26220(11) 0.0194(3) Uani 1 1 d . . . . .
H14 H 0.7099 0.0993 0.3014 0.023 Uiso 1 1 calc R U . . .
C15 C 0.75178(7) 0.26903(13) 0.31399(10) 0.0208(3) Uani 1 1 d . . . . .
H15 H 0.7525 0.2750 0.3888 0.025 Uiso 1 1 calc R U . . .
C16 C 0.77591(7) 0.36464(13) 0.25269(11) 0.0200(3) Uani 1 1 d . . . . .
H16 H 0.7935 0.4355 0.2857 0.024 Uiso 1 1 calc R U . . .
C17 C 0.77331(7) 0.35268(12) 0.14042(11) 0.0177(3) Uani 1 1 d . . . . .
C18 C 0.79588(7) 0.45108(13) 0.07194(11) 0.0198(3) Uani 1 1 d . . . . .
C19 C 0.81206(7) 0.53196(13) 0.01412(11) 0.0209(3) Uani 1 1 d . . . . .
C20 C 0.83114(8) 0.60892(13) -0.16820(11) 0.0227(3) Uani 1 1 d . . . . .
H20 H 0.8215 0.5304 -0.1941 0.027 Uiso 1 1 calc R U . . .
C21 C 0.83010(7) 0.62952(13) -0.05699(11) 0.0194(3) Uani 1 1 d . . . . .
C22 C 0.84583(7) 0.74692(12) -0.01645(11) 0.0187(3) Uani 1 1 d . . . . .
H22 H 0.8455 0.7640 0.0569 0.022 Uiso 1 1 calc R U . . .
C23 C 0.86180(7) 0.83639(12) -0.09043(11) 0.0184(3) Uani 1 1 d . . . . .
C24 C 0.86002(7) 0.80768(13) -0.20027(11) 0.0206(3) Uani 1 1 d . . . . .
H24 H 0.8696 0.8695 -0.2488 0.025 Uiso 1 1 calc R U . . .
C25 C 0.88731(8) 0.98355(12) 0.04829(10) 0.0201(3) Uani 1 1 d . . . . .
H25A H 0.9193 0.9272 0.0855 0.024 Uiso 1 1 calc R U . . .
H25B H 0.8428 0.9790 0.0810 0.024 Uiso 1 1 calc R U . . .
C26 C 0.91546(8) 1.11255(13) 0.05409(11) 0.0216(3) Uani 1 1 d . . . . .
H26A H 0.9605 1.1164 0.0227 0.026 Uiso 1 1 calc R U . . .
H26B H 0.8840 1.1682 0.0149 0.026 Uiso 1 1 calc R U . . .
C27 C 0.95245(8) 1.26289(13) 0.17974(11) 0.0223(3) Uani 1 1 d . . . . .
H27A H 0.9250 1.3236 0.1393 0.027 Uiso 1 1 calc R U . . .
H27B H 0.9990 1.2628 0.1534 0.027 Uiso 1 1 calc R U . . .
C28 C 0.95570(8) 1.29475(13) 0.29831(12) 0.0247(3) Uani 1 1 d . . . . .
H28A H 0.9633 1.3822 0.3059 0.030 Uiso 1 1 calc R U . . .
H28B H 0.9110 1.2762 0.3270 0.030 Uiso 1 1 calc R U . . .
C29 C 0.98974(9) 1.11203(14) 0.39132(13) 0.0310(3) Uani 1 1 d . . . . .
H29A H 0.9463 1.1142 0.4259 0.047 Uiso 1 1 calc R U . . .
H29B H 1.0253 1.0791 0.4404 0.047 Uiso 1 1 calc R U . . .
H29C H 0.9851 1.0612 0.3282 0.047 Uiso 1 1 calc R U . . .
N1 N 0.65700(7) -0.20643(11) -0.21866(10) 0.0244(3) Uani 1 1 d . . . . .
N2 N 0.74948(6) 0.25150(10) 0.08881(9) 0.0182(2) Uani 1 1 d . . . . .
N3 N 0.84526(7) 0.69632(11) -0.23897(9) 0.0234(3) Uani 1 1 d . . . . .
O1 O 0.49233(6) -0.73406(10) 0.36181(9) 0.0275(2) Uani 1 1 d . . . . .
O2 O 0.57647(6) -0.64594(9) 0.17725(8) 0.0244(2) Uani 1 1 d . . . . .
O3 O 0.61959(6) -0.45936(9) -0.04674(8) 0.0228(2) Uani 1 1 d . . . . .
O4 O 0.87969(6) 0.95419(9) -0.06476(7) 0.0224(2) Uani 1 1 d . . . . .
O5 O 0.92176(6) 1.14491(9) 0.16475(8) 0.0236(2) Uani 1 1 d . . . . .
O6 O 1.00831(5) 1.23237(10) 0.36108(8) 0.0262(2) 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
C1 O1 1.4161(19) . ?
C2 O1 1.4186(18) . ?
C2 C3 1.507(2) . ?
C3 O2 1.4258(17) . ?
C4 O2 1.4163(16) . ?
C4 C5 1.5117(19) . ?
C5 O3 1.4362(16) . ?
C6 N1 1.3317(19) . ?
C6 C7 1.3980(19) . ?
C7 O3 1.3628(16) . ?
C7 C8 1.3839(19) . ?
C8 C9 1.3990(19) . ?
C9 C10 1.3999(19) . ?
C9 C11 1.4347(19) . ?
C10 N1 1.3348(19) . ?
C11 C12 1.188(2) . ?
C12 C13 1.4494(19) . ?
C13 N2 1.3467(17) . ?
C13 C14 1.3983(18) . ?
C14 C15 1.384(2) . ?
C15 C16 1.386(2) . ?
C16 C17 1.3977(18) . ?
C17 N2 1.3449(17) . ?
C17 C18 1.4509(19) . ?
C18 C19 1.190(2) . ?
C19 C21 1.4376(19) . ?
C20 N3 1.3348(19) . ?
C20 C21 1.3998(19) . ?
C21 C22 1.4039(19) . ?
C22 C23 1.3864(19) . ?
C23 O4 1.3645(16) . ?
C23 C24 1.3975(18) . ?
C24 N3 1.3320(18) . ?
C25 O4 1.4389(15) . ?
C25 C26 1.5092(19) . ?
C26 O5 1.4169(16) . ?
C27 O5 1.4250(16) . ?
C27 C28 1.5101(19) . ?
C28 O6 1.4178(17) . ?
C29 O6 1.4174(18) . ?

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 C2 C3 114.56(12) . . ?
O2 C3 C2 109.21(12) . . ?
O2 C4 C5 106.90(11) . . ?
O3 C5 C4 105.48(11) . . ?
N1 C6 C7 123.35(13) . . ?
O3 C7 C8 125.12(12) . . ?
O3 C7 C6 115.45(12) . . ?
C8 C7 C6 119.43(13) . . ?
C7 C8 C9 117.47(12) . . ?
C8 C9 C10 118.98(12) . . ?
C8 C9 C11 122.02(12) . . ?
C10 C9 C11 118.99(12) . . ?
N1 C10 C9 123.25(13) . . ?
C12 C11 C9 176.33(15) . . ?
C11 C12 C13 175.51(15) . . ?
N2 C13 C14 123.16(12) . . ?
N2 C13 C12 114.95(11) . . ?
C14 C13 C12 121.89(12) . . ?
C15 C14 C13 118.62(12) . . ?
C14 C15 C16 119.01(12) . . ?
C15 C16 C17 118.80(12) . . ?
N2 C17 C16 122.98(12) . . ?
N2 C17 C18 115.74(11) . . ?
C16 C17 C18 121.28(12) . . ?
C19 C18 C17 177.67(15) . . ?
C18 C19 C21 178.71(15) . . ?
N3 C20 C21 123.25(13) . . ?
C20 C21 C22 119.06(12) . . ?
C20 C21 C19 120.21(13) . . ?
C22 C21 C19 120.72(12) . . ?
C23 C22 C21 117.20(12) . . ?
O4 C23 C22 124.86(12) . . ?
O4 C23 C24 115.57(12) . . ?
C22 C23 C24 119.57(13) . . ?
N3 C24 C23 123.36(13) . . ?
O4 C25 C26 105.77(11) . . ?
O5 C26 C25 106.89(11) . . ?
O5 C27 C28 109.29(12) . . ?
O6 C28 C27 114.54(12) . . ?
C6 N1 C10 117.45(12) . . ?
C17 N2 C13 117.42(11) . . ?
C24 N3 C20 117.53(12) . . ?
C1 O1 C2 114.22(12) . . ?
C4 O2 C3 111.41(11) . . ?
C7 O3 C5 116.46(10) . . ?
C23 O4 C25 116.66(10) . . ?
C26 O5 C27 111.41(10) . . ?
C29 O6 C28 114.06(12) . . ?

_refine_diff_density_max         0.267
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.047

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_dp217
_database_code_depnum_ccdc_archive 'CCDC 1053823'
_audit_update_record             
;
2015-03-13 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C116 H132 B4 F16 N12 O28 Pd2'
_chemical_formula_weight         2702.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   14.8562(5)
_cell_length_b                   16.5839(5)
_cell_length_c                   16.9982(4)
_cell_angle_alpha                117.401(3)
_cell_angle_beta                 93.110(2)
_cell_angle_gamma                114.691(3)
_cell_volume                     3216.53(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    100.0(1)
_cell_measurement_reflns_used    10769
_cell_measurement_theta_min      3.4610
_cell_measurement_theta_max      75.1950

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1392
_exptl_absorpt_coefficient_mu    3.098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.679
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.0(1)
_diffrn_radiation_wavelength     1.54180
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 5.1725
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39257
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         76.54
_reflns_number_total             13327
_reflns_number_gt                9722
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SIR97 (Altomare et al., 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1381P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         13327
_refine_ls_number_parameters     869
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0749
_refine_ls_wR_factor_ref         0.2251
_refine_ls_wR_factor_gt          0.2070
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6499(9) 0.4257(10) -0.1930(9) 0.094(4) Uani 1 1 d . . .
H1A H 0.6957 0.4346 -0.2297 0.141 Uiso 1 1 calc R . .
H1B H 0.6194 0.4691 -0.1833 0.141 Uiso 1 1 calc R . .
H1C H 0.5959 0.3536 -0.2249 0.141 Uiso 1 1 calc R . .
C2 C 0.7701(9) 0.4099(9) -0.1142(8) 0.081(3) Uani 1 1 d . . .
H2A H 0.8292 0.4558 -0.0582 0.097 Uiso 1 1 calc R . .
H2B H 0.7969 0.4066 -0.1658 0.097 Uiso 1 1 calc R . .
C3 C 0.7208(10) 0.3071(9) -0.1289(8) 0.085(3) Uani 1 1 d . . .
H3A H 0.7622 0.2744 -0.1527 0.103 Uiso 1 1 calc R . .
H3B H 0.6530 0.2646 -0.1752 0.103 Uiso 1 1 calc R . .
C4 C 0.6934(6) 0.2183(5) -0.0488(5) 0.0453(15) Uani 1 1 d . . .
H4A H 0.7580 0.2167 -0.0463 0.054 Uiso 1 1 calc R . .
H4B H 0.6418 0.1575 -0.1073 0.054 Uiso 1 1 calc R . .
C5 C 0.6573(5) 0.2146(4) 0.0307(4) 0.0357(12) Uani 1 1 d . . .
H5A H 0.7082 0.2748 0.0898 0.043 Uiso 1 1 calc R . .
H5B H 0.5915 0.2137 0.0281 0.043 Uiso 1 1 calc R . .
C6 C 0.5903(4) 0.1556(4) 0.1565(3) 0.0276(10) Uani 1 1 d . . .
H6 H 0.5892 0.2132 0.1610 0.033 Uiso 1 1 calc R . .
C7 C 0.6184(4) 0.0970(4) 0.0848(3) 0.0289(10) Uani 1 1 d . . .
C8 C 0.6192(4) 0.0107(4) 0.0776(4) 0.0310(10) Uani 1 1 d . . .
H8 H 0.6373 -0.0298 0.0293 0.037 Uiso 1 1 calc R . .
C9 C 0.5927(4) -0.0146(4) 0.1438(3) 0.0286(10) Uani 1 1 d . . .
C10 C 0.5658(4) 0.0482(4) 0.2158(3) 0.0304(10) Uani 1 1 d . . .
H10 H 0.5487 0.0325 0.2607 0.036 Uiso 1 1 calc R . .
C11 C 0.5938(5) -0.1018(4) 0.1407(4) 0.0340(11) Uani 1 1 d . . .
C12 C 0.4053(5) 0.1746(5) 0.8618(4) 0.0362(12) Uani 1 1 d . . .
C13 C 0.3977(5) 0.2590(4) 0.8633(4) 0.0349(11) Uani 1 1 d . . .
C14 C 0.3886(5) 0.3330(5) 0.9416(4) 0.0386(12) Uani 1 1 d . . .
H14 H 0.3932 0.3328 0.9963 0.046 Uiso 1 1 calc R . .
C15 C 0.3725(5) 0.4069(5) 0.9356(4) 0.0390(13) Uani 1 1 d . . .
H15 H 0.3640 0.4559 0.9858 0.047 Uiso 1 1 calc R . .
C16 C 0.3692(5) 0.4069(5) 0.8537(4) 0.0393(13) Uani 1 1 d . . .
H16 H 0.3580 0.4553 0.8477 0.047 Uiso 1 1 calc R . .
C17 C 0.3833(5) 0.3324(4) 0.7809(4) 0.0359(12) Uani 1 1 d . . .
C18 C 0.3865(5) 0.3331(5) 0.6964(4) 0.0403(13) Uani 1 1 d . . .
C19 C 0.3938(5) 0.3356(5) 0.6277(4) 0.0380(12) Uani 1 1 d . . .
C20 C 0.4448(5) 0.2855(4) 0.4856(4) 0.0346(11) Uani 1 1 d . . .
H20 H 0.4666 0.2465 0.4982 0.042 Uiso 1 1 calc R . .
C21 C 0.4033(5) 0.3403(4) 0.5467(4) 0.0341(11) Uani 1 1 d . . .
C22 C 0.3718(5) 0.3996(4) 0.5275(4) 0.0358(12) Uani 1 1 d . . .
H22 H 0.3450 0.4376 0.5678 0.043 Uiso 1 1 calc R . .
C23 C 0.3812(5) 0.4006(4) 0.4468(4) 0.0338(11) Uani 1 1 d . . .
C24 C 0.4215(5) 0.3436(4) 0.3886(3) 0.0331(11) Uani 1 1 d . . .
H24 H 0.4267 0.3430 0.3341 0.040 Uiso 1 1 calc R . .
C25 C 0.3439(6) 0.4555(5) 0.3446(4) 0.0410(13) Uani 1 1 d . . .
H25A H 0.3991 0.4455 0.3216 0.049 Uiso 1 1 calc R . .
H25B H 0.3531 0.5211 0.3540 0.049 Uiso 1 1 calc R . .
C26 C 0.2423(6) 0.3684(6) 0.2750(5) 0.0522(17) Uani 1 1 d . . .
H26A H 0.1869 0.3712 0.3018 0.063 Uiso 1 1 calc R . .
H26B H 0.2329 0.3751 0.2218 0.063 Uiso 1 1 calc R . .
C27 C 0.1376(6) 0.1915(6) 0.2312(5) 0.0543(16) Uani 1 1 d . . .
H27A H 0.1231 0.1246 0.1787 0.065 Uiso 1 1 calc R . .
H27B H 0.0849 0.2066 0.2163 0.065 Uiso 1 1 calc R . .
C28 C 0.1319(6) 0.1840(7) 0.3146(5) 0.0574(18) Uani 1 1 d . . .
H28A H 0.1542 0.2526 0.3689 0.069 Uiso 1 1 calc R . .
H28B H 0.0607 0.1371 0.3064 0.069 Uiso 1 1 calc R . .
C29 C 0.1804(7) 0.1142(7) 0.3941(6) 0.0618(19) Uani 1 1 d . . .
H29A H 0.1937 0.1732 0.4534 0.093 Uiso 1 1 calc R . .
H29B H 0.2265 0.0891 0.4000 0.093 Uiso 1 1 calc R . .
H29C H 0.1096 0.0594 0.3732 0.093 Uiso 1 1 calc R . .
C30 C 1.1181(11) 1.1249(10) 0.7201(13) 0.139(7) Uani 1 1 d . . .
H30A H 1.1821 1.1316 0.7452 0.209 Uiso 1 1 calc R . .
H30B H 1.0752 1.1204 0.7599 0.209 Uiso 1 1 calc R . .
H30C H 1.1329 1.1850 0.7164 0.209 Uiso 1 1 calc R . .
C31 C 1.1345(9) 1.0132(8) 0.5812(11) 0.101(4) Uani 1 1 d . . .
H31A H 1.1860 1.0115 0.6172 0.121 Uiso 1 1 calc R . .
H31B H 1.1703 1.0666 0.5672 0.121 Uiso 1 1 calc R . .
C32 C 1.0664(13) 0.9051(10) 0.4905(11) 0.118(5) Uani 1 1 d . . .
H32A H 1.0041 0.9003 0.4631 0.142 Uiso 1 1 calc R . .
H32B H 1.1046 0.8937 0.4458 0.142 Uiso 1 1 calc R . .
C33 C 0.9532(7) 0.7313(6) 0.4503(6) 0.0577(18) Uani 1 1 d . . .
H33A H 0.9633 0.7073 0.3894 0.069 Uiso 1 1 calc R . .
H33B H 0.8910 0.7373 0.4474 0.069 Uiso 1 1 calc R . .
C34 C 0.9426(6) 0.6544(6) 0.4805(5) 0.0490(15) Uani 1 1 d . . .
H34A H 0.9980 0.6378 0.4720 0.059 Uiso 1 1 calc R . .
H34B H 0.9454 0.6842 0.5454 0.059 Uiso 1 1 calc R . .
C35 C 0.8056(5) 0.4882(5) 0.4431(4) 0.0376(12) Uani 1 1 d . . .
C36 C 0.7073(5) 0.4032(4) 0.3847(4) 0.0327(11) Uani 1 1 d . . .
H36 H 0.6757 0.4000 0.3338 0.039 Uiso 1 1 calc R . .
C37 C 0.8547(5) 0.4918(5) 0.5174(4) 0.0368(12) Uani 1 1 d . . .
H37 H 0.9209 0.5473 0.5563 0.044 Uiso 1 1 calc R . .
C38 C 0.8027(5) 0.4103(5) 0.5324(4) 0.0371(12) Uani 1 1 d . . .
C39 C 0.7039(5) 0.3282(5) 0.4726(4) 0.0352(11) Uani 1 1 d . . .
H39 H 0.6693 0.2740 0.4827 0.042 Uiso 1 1 calc R . .
C40 C 0.8518(5) 0.4086(5) 0.6059(4) 0.0400(12) Uani 1 1 d . . .
C41 C 0.8961(5) 0.4063(5) 0.6639(4) 0.0429(13) Uani 1 1 d . . .
C42 C 0.9588(5) 0.4027(5) 0.7306(4) 0.0400(13) Uani 1 1 d . . .
C43 C 1.0610(6) 0.4795(5) 0.7791(5) 0.0507(16) Uani 1 1 d . . .
H43 H 1.0909 0.5375 0.7734 0.061 Uiso 1 1 calc R . .
C44 C 1.1188(6) 0.4685(6) 0.8370(6) 0.063(2) Uani 1 1 d . . .
H44 H 1.1885 0.5184 0.8696 0.076 Uiso 1 1 calc R . .
C45 C 1.0703(6) 0.3816(6) 0.8451(6) 0.061(2) Uani 1 1 d . . .
H45 H 1.1068 0.3725 0.8836 0.073 Uiso 1 1 calc R . .
C46 C 0.9667(6) 0.3093(5) 0.7947(5) 0.0453(14) Uani 1 1 d . . .
C47 C 0.0908(5) -0.2178(5) 0.1989(5) 0.0441(14) Uani 1 1 d . . .
C48 C 0.1412(5) -0.1448(5) 0.1919(4) 0.0402(13) Uani 1 1 d . . .
C49 C 0.2047(5) -0.0598(5) 0.1806(4) 0.0354(11) Uani 1 1 d . . .
C50 C 0.3036(5) 0.0160(4) 0.2420(4) 0.0342(11) Uani 1 1 d . . .
H50 H 0.3285 0.0115 0.2904 0.041 Uiso 1 1 calc R . .
C51 C 0.1661(5) -0.0556(5) 0.1056(4) 0.0348(11) Uani 1 1 d . . .
H51 H 0.0999 -0.1060 0.0635 0.042 Uiso 1 1 calc R . .
C52 C 0.2315(5) 0.0272(5) 0.0980(4) 0.0343(11) Uani 1 1 d . . .
C53 C 0.3291(5) 0.1023(4) 0.1627(4) 0.0321(11) Uani 1 1 d . . .
H53 H 0.3710 0.1584 0.1573 0.038 Uiso 1 1 calc R . .
C54 C 0.1177(5) -0.0348(5) -0.0469(4) 0.0446(14) Uani 1 1 d . . .
H54A H 0.0561 -0.0490 -0.0267 0.054 Uiso 1 1 calc R . .
H54B H 0.1202 -0.0991 -0.0801 0.054 Uiso 1 1 calc R . .
C55 C 0.1160(6) 0.0080(6) -0.1088(5) 0.0498(16) Uani 1 1 d . . .
H55A H 0.1853 0.0398 -0.1138 0.060 Uiso 1 1 calc R . .
H55B H 0.0696 -0.0496 -0.1707 0.060 Uiso 1 1 calc R . .
C56 C 0.1636(6) 0.1860(6) -0.0079(5) 0.0530(16) Uani 1 1 d . . .
H56A H 0.2238 0.2025 -0.0299 0.064 Uiso 1 1 calc R . .
H56B H 0.1838 0.1905 0.0498 0.064 Uiso 1 1 calc R . .
C57 C 0.1289(6) 0.2627(6) 0.0093(5) 0.0542(17) Uani 1 1 d . . .
H57A H 0.1881 0.3333 0.0453 0.065 Uiso 1 1 calc R . .
H57B H 0.0978 0.2507 -0.0495 0.065 Uiso 1 1 calc R . .
C58 C 0.0280(8) 0.3310(7) 0.0833(7) 0.069(2) Uani 1 1 d . . .
H58A H 0.0867 0.3982 0.1287 0.103 Uiso 1 1 calc R . .
H58B H -0.0283 0.3163 0.1092 0.103 Uiso 1 1 calc R . .
H58C H 0.0065 0.3314 0.0293 0.103 Uiso 1 1 calc R . .
B1 B 0.5104(6) 0.3521(5) 0.1592(4) 0.0362(13) Uani 1 1 d . . .
N1 N 0.5645(4) 0.1303(3) 0.2205(3) 0.0281(8) Uani 1 1 d . . .
N2 N 0.3971(4) 0.2588(4) 0.7840(3) 0.0349(10) Uani 1 1 d . . .
N3 N 0.4532(4) 0.2889(4) 0.4095(3) 0.0327(9) Uani 1 1 d . . .
N4 N 0.6571(4) 0.3254(3) 0.3999(3) 0.0305(9) Uani 1 1 d . . .
N5 N 0.9095(4) 0.3182(4) 0.7367(3) 0.0409(11) Uani 1 1 d . . .
N6 N 0.3648(4) 0.0965(3) 0.2327(3) 0.0301(9) Uani 1 1 d . . .
O1 O 0.7072(7) 0.4551(6) -0.1057(5) 0.082(2) Uani 1 1 d . . .
O2 O 0.7087(5) 0.3109(4) -0.0434(4) 0.0603(14) Uani 1 1 d . . .
O3 O 0.6457(3) 0.1183(3) 0.0192(2) 0.0329(8) Uani 1 1 d . . .
O4 O 0.3511(4) 0.4609(3) 0.4325(3) 0.0403(9) Uani 1 1 d . . .
O5 O 0.2372(4) 0.2711(4) 0.2458(3) 0.0523(11) Uani 1 1 d . . .
O6 O 0.1974(4) 0.1454(4) 0.3281(4) 0.0559(12) Uani 1 1 d . . .
O7 O 1.0662(5) 1.0349(6) 0.6318(6) 0.089(2) Uani 1 1 d . . .
O8 O 1.0400(6) 0.8285(5) 0.5174(6) 0.084(2) Uani 1 1 d . . .
O9 O 0.8433(4) 0.5624(4) 0.4219(3) 0.0449(10) Uani 1 1 d . . .
O10 O 0.2092(3) 0.0446(3) 0.0310(3) 0.0392(9) Uani 1 1 d . . .
O11 O 0.0832(4) 0.0832(4) -0.0746(3) 0.0510(11) Uani 1 1 d . . .
O12 O 0.0564(4) 0.2520(4) 0.0575(4) 0.0537(11) Uani 1 1 d . . .
F1 F 0.6089(3) 0.3977(3) 0.1517(3) 0.0530(10) Uani 1 1 d . . .
F2 F 0.4611(3) 0.4088(3) 0.1653(3) 0.0482(9) Uani 1 1 d . . .
F3 F 0.4505(3) 0.2494(3) 0.0832(2) 0.0490(9) Uani 1 1 d . . .
F4 F 0.5194(3) 0.3466(3) 0.2395(2) 0.0477(9) Uani 1 1 d . . .
Pd1 Pd 0.51102(3) 0.20918(3) 0.31760(2) 0.02893(13) Uani 1 1 d . . .
B2 B 0.881(2) 0.2839(16) 0.2760(9) 0.051(6) Uani 0.60 1 d PD A 1
F5 F 0.9601(10) 0.2635(11) 0.2832(10) 0.063(3) Uani 0.60 1 d PD A 1
F6 F 0.9215(7) 0.3932(7) 0.3342(6) 0.072(2) Uani 0.60 1 d PD A 1
F7 F 0.8485(14) 0.2630(15) 0.1871(8) 0.082(4) Uani 0.60 1 d PD A 1
F8 F 0.8008(8) 0.2352(9) 0.3014(8) 0.091(3) Uani 0.60 1 d PD A 1
B3 B 0.890(3) 0.271(2) 0.2725(16) 0.09(2) Uani 0.40 1 d PD B 2
F9 F 0.8262(13) 0.1688(10) 0.2444(13) 0.113(7) Uani 0.40 1 d PD B 2
F10 F 0.8923(13) 0.3340(15) 0.3648(9) 0.104(6) Uani 0.40 1 d PD B 2
F11 F 0.8380(18) 0.294(2) 0.2222(19) 0.117(11) Uani 0.40 1 d PD B 2
F12 F 0.9882(16) 0.294(2) 0.273(2) 0.118(12) Uani 0.40 1 d PD B 2
O50 O 0.4231(8) 0.1011(5) 0.6402(5) 0.056(2) Uani 0.50 1 d PDU C 1
H50A H 0.4147 0.1485 0.6827 0.067 Uiso 0.50 1 d PD D 1
H50B H 0.4585 0.1196 0.6074 0.067 Uiso 0.50 1 d PD E 1
O51 O 0.7160(3) 0.1603(6) 0.6089(4) 0.059(2) Uani 0.50 1 d PDU F 2
H51A H 0.7760 0.2061 0.6527 0.071 Uiso 0.50 1 d PD G 2
H51B H 0.6553 0.1474 0.6156 0.071 Uiso 0.50 1 d PD H 2
O52 O 0.5448(5) 0.1643(4) 0.5325(4) 0.0424(19) Uani 0.50 1 d PD I 1
H52A H 0.5956 0.1625 0.5557 0.051 Uiso 0.50 1 d PD J 1
H52B H 0.5129 0.1067 0.4799 0.051 Uiso 0.50 1 d PD K 1
O53 O 0.4419(5) -0.0216(4) 0.3611(4) 0.047(2) Uani 0.50 1 d PD L 2
H53A H 0.4829 -0.0453 0.3612 0.057 Uiso 0.50 1 d PD M 2
H53B H 0.4734 0.0356 0.4140 0.057 Uiso 0.50 1 d PD N 2


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 O1 1.420(13) . ?
C2 O1 1.399(12) . ?
C2 C3 1.431(13) . ?
C3 O2 1.450(10) . ?
C4 O2 1.413(7) . ?
C4 C5 1.497(8) . ?
C5 O3 1.449(6) . ?
C6 N1 1.355(6) . ?
C6 C7 1.381(7) . ?
C7 O3 1.350(6) . ?
C7 C8 1.385(7) . ?
C8 C9 1.394(7) . ?
C9 C10 1.403(7) . ?
C9 C11 1.431(7) . ?
C10 N1 1.335(6) . ?
C11 C12 1.193(8) 2_656 ?
C12 C11 1.193(8) 2_656 ?
C12 C13 1.440(7) . ?
C13 N2 1.345(7) . ?
C13 C14 1.397(8) . ?
C14 C15 1.387(8) . ?
C15 C16 1.391(8) . ?
C16 C17 1.392(8) . ?
C17 N2 1.342(7) . ?
C17 C18 1.444(7) . ?
C18 C19 1.196(8) . ?
C19 C21 1.426(7) . ?
C20 N3 1.329(7) . ?
C20 C21 1.397(8) . ?
C21 C22 1.399(7) . ?
C22 C23 1.394(7) . ?
C23 O4 1.359(6) . ?
C23 C24 1.380(8) . ?
C24 N3 1.345(7) . ?
C25 O4 1.450(6) . ?
C25 C26 1.476(10) . ?
C26 O5 1.420(8) . ?
C27 O5 1.422(9) . ?
C27 C28 1.482(11) . ?
C28 O6 1.428(10) . ?
C29 O6 1.431(10) . ?
C30 O7 1.388(16) . ?
C31 O7 1.419(14) . ?
C31 C32 1.545(19) . ?
C32 O8 1.454(12) . ?
C33 O8 1.405(11) . ?
C33 C34 1.535(10) . ?
C34 O9 1.434(9) . ?
C35 O9 1.347(7) . ?
C35 C37 1.387(8) . ?
C35 C36 1.393(9) . ?
C36 N4 1.346(7) . ?
C37 C38 1.399(8) . ?
C38 C39 1.391(9) . ?
C38 C40 1.429(8) . ?
C39 N4 1.357(7) . ?
C40 C41 1.181(9) . ?
C41 C42 1.466(8) . ?
C42 N5 1.340(8) . ?
C42 C43 1.374(10) . ?
C43 C44 1.393(10) . ?
C44 C45 1.394(10) . ?
C45 C46 1.382(10) . ?
C46 N5 1.364(8) . ?
C46 C47 1.457(9) 2_656 ?
C47 C48 1.194(9) . ?
C47 C46 1.457(9) 2_656 ?
C48 C49 1.440(8) . ?
C49 C50 1.383(9) . ?
C49 C51 1.412(7) . ?
C50 N6 1.352(7) . ?
C51 C52 1.381(8) . ?
C52 O10 1.353(6) . ?
C52 C53 1.386(8) . ?
C53 N6 1.337(6) . ?
C54 O10 1.428(8) . ?
C54 C55 1.519(9) . ?
C55 O11 1.415(9) . ?
C56 O11 1.411(9) . ?
C56 C57 1.480(11) . ?
C57 O12 1.390(10) . ?
C58 O12 1.428(9) . ?
B1 F2 1.388(7) . ?
B1 F1 1.384(8) . ?
B1 F3 1.394(8) . ?
B1 F4 1.412(6) . ?
N1 Pd1 2.023(4) . ?
N3 Pd1 2.030(5) . ?
N4 Pd1 2.019(5) . ?
N6 Pd1 2.019(5) . ?
B2 F8 1.35(3) . ?
B2 F5 1.36(3) . ?
B2 F7 1.392(18) . ?
B2 F6 1.41(2) . ?
B3 F12 1.34(4) . ?
B3 F9 1.36(3) . ?
B3 F11 1.39(2) . ?
B3 F10 1.42(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 C2 C3 115.8(10) . . ?
C2 C3 O2 111.3(9) . . ?
O2 C4 C5 109.6(5) . . ?
O3 C5 C4 104.9(4) . . ?
N1 C6 C7 120.9(4) . . ?
O3 C7 C6 123.9(5) . . ?
O3 C7 C8 116.5(5) . . ?
C6 C7 C8 119.6(5) . . ?
C7 C8 C9 119.1(5) . . ?
C8 C9 C10 119.0(4) . . ?
C8 C9 C11 121.5(5) . . ?
C10 C9 C11 119.5(4) . . ?
N1 C10 C9 120.7(4) . . ?
C12 C11 C9 179.9(7) 2_656 . ?
C11 C12 C13 176.6(7) 2_656 . ?
N2 C13 C14 123.6(5) . . ?
N2 C13 C12 115.2(5) . . ?
C14 C13 C12 121.2(5) . . ?
C13 C14 C15 118.1(5) . . ?
C14 C15 C16 119.4(5) . . ?
C17 C16 C15 117.9(5) . . ?
N2 C17 C16 124.0(5) . . ?
N2 C17 C18 116.0(5) . . ?
C16 C17 C18 120.0(5) . . ?
C19 C18 C17 177.1(7) . . ?
C18 C19 C21 179.2(6) . . ?
N3 C20 C21 120.4(5) . . ?
C20 C21 C22 119.3(5) . . ?
C20 C21 C19 120.0(5) . . ?
C22 C21 C19 120.7(5) . . ?
C21 C22 C23 118.6(5) . . ?
O4 C23 C24 124.7(5) . . ?
O4 C23 C22 116.1(5) . . ?
C24 C23 C22 119.2(5) . . ?
N3 C24 C23 121.1(5) . . ?
O4 C25 C26 111.0(5) . . ?
O5 C26 C25 109.9(5) . . ?
O5 C27 C28 111.5(6) . . ?
O6 C28 C27 109.5(6) . . ?
O7 C31 C32 106.6(9) . . ?
O8 C32 C31 105.7(11) . . ?
O8 C33 C34 106.6(7) . . ?
O9 C34 C33 105.5(6) . . ?
O9 C35 C37 125.7(6) . . ?
O9 C35 C36 114.7(5) . . ?
C37 C35 C36 119.5(5) . . ?
N4 C36 C35 121.6(5) . . ?
C35 C37 C38 118.6(6) . . ?
C39 C38 C37 119.3(5) . . ?
C39 C38 C40 120.0(5) . . ?
C37 C38 C40 120.6(6) . . ?
N4 C39 C38 121.3(5) . . ?
C41 C40 C38 176.2(7) . . ?
C40 C41 C42 174.2(7) . . ?
N5 C42 C43 124.3(6) . . ?
N5 C42 C41 114.7(6) . . ?
C43 C42 C41 121.0(6) . . ?
C42 C43 C44 118.5(6) . . ?
C43 C44 C45 118.9(7) . . ?
C46 C45 C44 118.4(6) . . ?
N5 C46 C45 123.4(6) . . ?
N5 C46 C47 114.5(6) . 2_656 ?
C45 C46 C47 122.0(6) . 2_656 ?
C48 C47 C46 176.6(7) . 2_656 ?
C47 C48 C49 176.9(7) . . ?
C50 C49 C51 120.4(5) . . ?
C50 C49 C48 119.9(5) . . ?
C51 C49 C48 119.7(6) . . ?
N6 C50 C49 121.0(5) . . ?
C52 C51 C49 116.7(5) . . ?
O10 C52 C51 125.6(5) . . ?
O10 C52 C53 113.9(5) . . ?
C51 C52 C53 120.5(5) . . ?
N6 C53 C52 122.0(5) . . ?
O10 C54 C55 106.0(5) . . ?
O11 C55 C54 112.7(6) . . ?
O11 C56 C57 110.7(6) . . ?
O12 C57 C56 109.5(6) . . ?
F2 B1 F1 111.8(5) . . ?
F2 B1 F3 110.0(5) . . ?
F1 B1 F3 109.9(5) . . ?
F2 B1 F4 109.5(5) . . ?
F1 B1 F4 108.5(5) . . ?
F3 B1 F4 107.0(5) . . ?
C10 N1 C6 120.8(4) . . ?
C10 N1 Pd1 119.1(3) . . ?
C6 N1 Pd1 119.9(3) . . ?
C17 N2 C13 116.9(5) . . ?
C20 N3 C24 121.4(5) . . ?
C20 N3 Pd1 122.0(4) . . ?
C24 N3 Pd1 116.6(3) . . ?
C36 N4 C39 119.5(5) . . ?
C36 N4 Pd1 119.7(4) . . ?
C39 N4 Pd1 120.8(4) . . ?
C42 N5 C46 116.5(6) . . ?
C53 N6 C50 119.3(5) . . ?
C53 N6 Pd1 116.9(4) . . ?
C50 N6 Pd1 123.8(4) . . ?
C2 O1 C1 112.7(8) . . ?
C4 O2 C3 111.5(6) . . ?
C7 O3 C5 117.8(4) . . ?
C23 O4 C25 120.1(4) . . ?
C26 O5 C27 113.4(6) . . ?
C28 O6 C29 113.5(6) . . ?
C30 O7 C31 113.0(10) . . ?
C33 O8 C32 111.9(10) . . ?
C35 O9 C34 118.4(5) . . ?
C52 O10 C54 119.1(5) . . ?
C56 O11 C55 114.1(6) . . ?
C57 O12 C58 111.4(6) . . ?
N4 Pd1 N6 177.50(17) . . ?
N4 Pd1 N1 91.68(18) . . ?
N6 Pd1 N1 88.43(18) . . ?
N4 Pd1 N3 89.90(19) . . ?
N6 Pd1 N3 89.88(19) . . ?
N1 Pd1 N3 176.76(17) . . ?
F8 B2 F5 114.0(17) . . ?
F8 B2 F7 112(2) . . ?
F5 B2 F7 110.1(17) . . ?
F8 B2 F6 108.0(16) . . ?
F5 B2 F6 108.3(19) . . ?
F7 B2 F6 103.7(16) . . ?
F12 B3 F9 113(2) . . ?
F12 B3 F11 118(3) . . ?
F9 B3 F11 107(2) . . ?
F12 B3 F10 108(2) . . ?
F9 B3 F10 108(3) . . ?
F11 B3 F10 103(2) . . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        67.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         3.169
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.141
# SQUEEZE RESULTS (APPEND TO CIF)
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.264 0.877 0.595 26.1 9.2
2 0.736 0.122 0.405 26.1 8.2
_platon_squeeze_details          
;
 Solvent water molecules that could not be appropriately
 modelled. The number of electrons is consistent with
 two water molecules.
;
####################################################################### 
# 
# 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_Pd2macrocyle
_database_code_depnum_ccdc_archive 'CCDC 1053824'
_audit_update_record             
;
2015-03-13 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C58 H62 Cl4 N6 O12 Pd2'
_chemical_formula_weight         1389.73

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'

_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.
;

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

_cell_length_a                   13.8958(6)
_cell_length_b                   21.0537(7)
_cell_length_c                   11.1192(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.982(4)
_cell_angle_gamma                90
_cell_volume                     3182.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.00(10)
_cell_measurement_reflns_used    4205
_cell_measurement_theta_min      4.0560
_cell_measurement_theta_max      76.3740

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_F_000             1416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1658
_exptl_crystal_size_mid          0.1298
_exptl_crystal_size_min          0.0837
_exptl_absorpt_coefficient_mu    6.618
_exptl_absorpt_correction_T_min  0.47054
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7617
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.871
_diffrn_reflns_theta_max         76.318
_diffrn_reflns_theta_full        67.000
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             3299
_reflns_number_gt                2898
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    Superflip
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1128P)²+4.7545P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3299
_refine_ls_number_parameters     191
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0552
_refine_ls_wR_factor_ref         0.1674
_refine_ls_wR_factor_gt          0.1589
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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 0.56380(3) 0.0000 0.18379(4) 0.0399(2) Uani 1 2 d S T P . .
Cl1 Cl 0.6906(2) 0.0000 0.0807(3) 0.0849(8) Uani 1 2 d S T P . .
Cl2 Cl 0.43409(11) 0.0000 0.28253(17) 0.0476(4) Uani 1 2 d S T P . .
N1 N 0.5710(3) 0.09538(17) 0.1932(3) 0.0394(8) Uani 1 1 d . . . . .
O3 O 0.4231(2) 0.23357(14) 0.1039(3) 0.0428(7) Uani 1 1 d . . . . .
O1 O 0.3469(3) 0.36954(15) -0.3140(3) 0.0528(8) Uani 1 1 d . . . . .
O2 O 0.3528(2) 0.34456(16) -0.0614(3) 0.0488(7) Uani 1 1 d . . . . .
N2 N 1.0000 0.2374(2) 0.5000 0.0352(9) Uani 1 2 d S T P . .
C5 C 0.4254(3) 0.30108(19) 0.1315(4) 0.0408(9) Uani 1 1 d . . . . .
H5A H 0.4849 0.3206 0.1113 0.049 Uiso 1 1 calc R U . . .
H5B H 0.4275 0.3076 0.2202 0.049 Uiso 1 1 calc R U . . .
C4 C 0.3348(3) 0.3314(2) 0.0567(5) 0.0459(10) Uani 1 1 d . . . . .
H4A H 0.2780 0.3023 0.0500 0.055 Uiso 1 1 calc R U . . .
H4B H 0.3196 0.3711 0.0965 0.055 Uiso 1 1 calc R U . . .
C11 C 0.7579(3) 0.21107(19) 0.3424(4) 0.0387(9) Uani 1 1 d . . . . .
C12 C 0.8318(3) 0.23610(19) 0.3942(4) 0.0389(9) Uani 1 1 d . . . . .
C13 C 0.9194(3) 0.27077(19) 0.4502(4) 0.0387(9) Uani 1 1 d . . . . .
C8 C 0.5890(3) 0.22615(18) 0.2274(4) 0.0364(8) Uani 1 1 d . . . . .
H8 H 0.5948 0.2707 0.2407 0.044 Uiso 1 1 calc R U . . .
C7 C 0.5029(3) 0.19968(19) 0.1594(4) 0.0381(9) Uani 1 1 d . . . . .
C10 C 0.6554(3) 0.12037(19) 0.2564(4) 0.0400(9) Uani 1 1 d . . . . .
H10 H 0.7087 0.0929 0.2888 0.048 Uiso 1 1 calc R U . . .
C6 C 0.4953(3) 0.13390(19) 0.1450(4) 0.0406(9) Uani 1 1 d . . . . .
H6 H 0.4358 0.1160 0.1005 0.049 Uiso 1 1 calc R U . . .
C1 C 0.3901(5) 0.4024(3) -0.4022(6) 0.0690(16) Uani 1 1 d . . . . .
H1A H 0.4138 0.3716 -0.4553 0.104 Uiso 1 1 calc R U . . .
H1B H 0.3408 0.4301 -0.4523 0.104 Uiso 1 1 calc R U . . .
H1C H 0.4454 0.4282 -0.3593 0.104 Uiso 1 1 calc R U . . .
C2 C 0.3117(4) 0.4124(2) -0.2353(5) 0.0504(11) Uani 1 1 d . . . . .
H2A H 0.2583 0.4387 -0.2837 0.060 Uiso 1 1 calc R U . . .
H2B H 0.3656 0.4411 -0.1959 0.060 Uiso 1 1 calc R U . . .
C9 C 0.6668(3) 0.18522(19) 0.2755(4) 0.0377(8) Uani 1 1 d . . . . .
C14 C 0.9161(4) 0.3373(2) 0.4495(4) 0.0467(10) Uani 1 1 d . . . . .
H14 H 0.8569 0.3590 0.4147 0.056 Uiso 1 1 calc R U . . .
C15 C 1.0000 0.3707(3) 0.5000 0.0548(17) Uani 1 2 d S T P . .
H15 H 1.0000 0.4158 0.5000 0.066 Uiso 1 2 calc R U P . .
C3 C 0.2739(3) 0.3766(2) -0.1387(5) 0.0503(11) Uani 1 1 d . . . . .
H3A H 0.2427 0.4063 -0.0895 0.060 Uiso 1 1 calc R U . . .
H3B H 0.2237 0.3455 -0.1780 0.060 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 2.012(4) . ?
Pd1 N1 2.012(4) 6 ?
Pd1 Cl1 2.2926(17) . ?
Pd1 Cl2 2.2969(15) . ?
N1 C10 1.343(6) . ?
N1 C6 1.348(6) . ?
O3 C7 1.355(5) . ?
O3 C5 1.453(5) . ?
O1 C2 1.413(6) . ?
O1 C1 1.430(7) . ?
O2 C4 1.414(6) . ?
O2 C3 1.416(6) . ?
N2 C13 1.340(5) 2_756 ?
N2 C13 1.340(5) . ?
C5 C4 1.499(6) . ?
C11 C12 1.191(6) . ?
C11 C9 1.435(6) . ?
C12 C13 1.445(6) . ?
C13 C14 1.401(6) . ?
C8 C7 1.392(6) . ?
C8 C9 1.399(6) . ?
C7 C6 1.395(6) . ?
C10 C9 1.386(6) . ?
C2 C3 1.494(8) . ?
C14 C15 1.378(6) . ?
C15 C14 1.378(6) 2_756 ?

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 N1 172.6(2) . 6 ?
N1 Pd1 Cl1 89.49(9) . . ?
N1 Pd1 Cl1 89.49(9) 6 . ?
N1 Pd1 Cl2 90.60(9) . . ?
N1 Pd1 Cl2 90.60(9) 6 . ?
Cl1 Pd1 Cl2 178.58(9) . . ?
C10 N1 C6 119.8(4) . . ?
C10 N1 Pd1 116.6(3) . . ?
C6 N1 Pd1 123.6(3) . . ?
C7 O3 C5 116.0(3) . . ?
C2 O1 C1 111.3(4) . . ?
C4 O2 C3 113.2(3) . . ?
C13 N2 C13 116.8(5) 2_756 . ?
O3 C5 C4 108.6(4) . . ?
O2 C4 C5 108.0(3) . . ?
C12 C11 C9 175.9(4) . . ?
C11 C12 C13 175.3(4) . . ?
N2 C13 C14 123.4(4) . . ?
N2 C13 C12 118.0(4) . . ?
C14 C13 C12 118.6(4) . . ?
C7 C8 C9 118.0(4) . . ?
O3 C7 C8 124.5(4) . . ?
O3 C7 C6 115.8(4) . . ?
C8 C7 C6 119.7(4) . . ?
N1 C10 C9 121.7(4) . . ?
N1 C6 C7 121.2(4) . . ?
O1 C2 C3 110.0(4) . . ?
C10 C9 C8 119.6(4) . . ?
C10 C9 C11 120.9(4) . . ?
C8 C9 C11 119.5(4) . . ?
C15 C14 C13 119.0(4) . . ?
C14 C15 C14 118.5(6) . 2_756 ?
O2 C3 C2 109.5(4) . . ?

_refine_diff_density_max         2.795
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.180

_shelxl_version_number           2014-3



# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.006 145 54 ' '
2 0.500 0.500 0.016 145 54 ' '
3 0.165 0.500 0.475 24 2 ' '
4 0.665 0.000 0.475 24 2 ' '
5 0.335 0.000 0.525 24 2 ' '
6 0.835 0.500 0.525 24 2 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
The crystal lattice contained a large amount of diffuse
 electron density that could not be appropriately modelled. The 
SQUEEZE routine within PLATON was employed to resolve this problem, 
resulting in void electrons
count of 116 that we assign to 2.5 DMF solvent molecules (100
electrons in total). 
;
####################################################################### 
# 
# 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_dp217mes
_database_code_depnum_ccdc_archive 'CCDC 1053825'
_audit_update_record             
;
2015-03-13 deposited with the CCDC.
2015-04-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C126 H150 N16 O38 Pd2 S4'
_chemical_formula_weight         2837.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'

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

_cell_length_a                   13.099
_cell_length_b                   17.179
_cell_length_c                   32.2500(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.566(2)
_cell_angle_gamma                90.00
_cell_volume                     7254.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.01(10)
_cell_measurement_reflns_used    37475
_cell_measurement_theta_min      3.0970
_cell_measurement_theta_max      29.4700

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.3331
_exptl_crystal_size_mid          0.1913
_exptl_crystal_size_min          0.1555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2956
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_type   Gaussian
_exptl_absorpt_correction_T_min  0.63630
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
squeeze used to account for missing DMF molecules and disordered
peg chain. hydrogens refined freely using riding model or positioned
at sensible geometries.
;

_diffrn_ambient_temperature      100.01(10)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            105476
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         26.02
_reflns_number_total             14267
_reflns_number_gt                12733
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    Sir-2011
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          SQUEEZE

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14267
_refine_ls_number_parameters     838
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.1103
_refine_ls_wR_factor_ref         0.3871
_refine_ls_wR_factor_gt          0.3733
_refine_ls_goodness_of_fit_ref   1.860
_refine_ls_restrained_S_all      1.871
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7781(6) 0.5477(4) 0.27791(18) 0.0443(15) Uani 1 1 d . . .
H1 H 0.7862 0.5167 0.2538 0.053 Uiso 1 1 calc R . .
C2 C 0.8238(5) 0.5263(3) 0.31632(17) 0.0357(13) Uani 1 1 d . . .
C3 C 0.8789(5) 0.4537(4) 0.31975(17) 0.0380(13) Uani 1 1 d . . .
C4 C 0.9214(5) 0.3923(4) 0.32235(18) 0.0378(13) Uani 1 1 d . . .
C5 C 1.0150(4) 0.2993(3) 0.36526(18) 0.0301(12) Uani 1 1 d . . .
H5 H 1.0108 0.3347 0.3878 0.036 Uiso 1 1 calc R . .
C6 C 0.9717(4) 0.3194(3) 0.32693(17) 0.0306(11) Uani 1 1 d . . .
C7 C 0.9795(5) 0.2664(3) 0.29387(17) 0.0335(12) Uani 1 1 d . . .
H7 H 0.9510 0.2789 0.2673 0.040 Uiso 1 1 calc R . .
C8 C 1.0276(5) 0.1975(3) 0.30004(19) 0.0355(13) Uani 1 1 d . . .
C9 C 1.0694(4) 0.1795(3) 0.33921(16) 0.0306(11) Uani 1 1 d . . .
H9 H 1.1029 0.1310 0.3435 0.037 Uiso 1 1 calc R . .
C10 C 1.0563(7) 0.1597(5) 0.2304(2) 0.064(2) Uani 1 1 d . . .
H10A H 1.0306 0.2126 0.2238 0.077 Uiso 1 1 calc R . .
H10B H 1.0252 0.1228 0.2102 0.077 Uiso 1 1 calc R . .
C11 C 1.1707(8) 0.1579(6) 0.2276(3) 0.079(3) Uani 1 1 d . . .
H11A H 1.1901 0.1758 0.1997 0.095 Uiso 1 1 calc R . .
H11B H 1.2012 0.1943 0.2483 0.095 Uiso 1 1 calc R . .
C12 C 1.2178(11) 0.0343(6) 0.1974(5) 0.103(4) Uani 1 1 d . . .
H12A H 1.1480 0.0234 0.1863 0.124 Uiso 1 1 calc R . .
H12B H 1.2544 0.0644 0.1762 0.124 Uiso 1 1 calc R . .
C13 C 1.2693(11) -0.0363(8) 0.2052(4) 0.107(4) Uani 1 1 d . . .
H13A H 1.3319 -0.0267 0.2224 0.128 Uiso 1 1 calc R . .
H13B H 1.2894 -0.0603 0.1788 0.128 Uiso 1 1 calc R . .
C14 C 1.2461(11) -0.1593(7) 0.2348(5) 0.118(5) Uani 1 1 d . . .
H14A H 1.1984 -0.1924 0.2497 0.177 Uiso 1 1 calc R . .
H14B H 1.3086 -0.1521 0.2517 0.177 Uiso 1 1 calc R . .
H14C H 1.2628 -0.1843 0.2085 0.177 Uiso 1 1 calc R . .
C15 C 1.3785(5) 0.5305(4) 0.4048(2) 0.0441(15) Uani 1 1 d . . .
C16 C 1.3856(5) 0.6118(3) 0.40711(18) 0.0352(12) Uani 1 1 d . . .
C17 C 1.4610(5) 0.6516(3) 0.38480(17) 0.0351(13) Uani 1 1 d . . .
H17 H 1.5097 0.6237 0.3694 0.042 Uiso 1 1 calc R . .
C18 C 1.4623(5) 0.7313(4) 0.38593(19) 0.0393(14) Uani 1 1 d . . .
H18 H 1.5117 0.7597 0.3711 0.047 Uiso 1 1 calc R . .
C19 C 1.3893(5) 0.7705(3) 0.40944(18) 0.0341(12) Uani 1 1 d . . .
H19 H 1.3867 0.8258 0.4099 0.041 Uiso 1 1 calc R . .
C20 C 1.3213(4) 0.7269(3) 0.43193(17) 0.0315(11) Uani 1 1 d . . .
C21 C 0.7510(5) 0.2358(4) 0.54180(19) 0.0388(13) Uani 1 1 d . . .
C22 C 0.8062(5) 0.2022(4) 0.5197(2) 0.0413(15) Uani 1 1 d . . .
C23 C 0.9508(4) 0.1945(4) 0.47396(18) 0.0323(12) Uani 1 1 d . . .
H23 H 0.9610 0.2487 0.4783 0.039 Uiso 1 1 calc R . .
C24 C 0.8722(5) 0.1581(4) 0.49278(18) 0.0381(13) Uani 1 1 d . . .
C25 C 0.8547(5) 0.0800(4) 0.48579(17) 0.0397(14) Uani 1 1 d . . .
H25 H 0.7993 0.0543 0.4984 0.048 Uiso 1 1 calc R . .
C26 C 0.9984(4) 0.0786(3) 0.44178(16) 0.0302(11) Uani 1 1 d . . .
H26 H 1.0422 0.0515 0.4237 0.036 Uiso 1 1 calc R . .
C27 C 0.9193(4) 0.0390(3) 0.45995(17) 0.0325(12) Uani 1 1 d . . .
C28 C 0.9543(5) -0.0841(4) 0.4248(2) 0.0424(14) Uani 1 1 d . . .
H28A H 0.9528 -0.1395 0.4331 0.051 Uiso 1 1 calc R . .
H28B H 1.0264 -0.0667 0.4251 0.051 Uiso 1 1 calc R . .
C29 C 0.9070(5) -0.0748(4) 0.3812(2) 0.0457(15) Uani 1 1 d . . .
H29A H 0.9263 -0.1198 0.3640 0.055 Uiso 1 1 calc R . .
H29B H 0.8317 -0.0740 0.3828 0.055 Uiso 1 1 calc R . .
C30 C 0.8742(7) 0.0220(6) 0.3307(2) 0.062(2) Uani 1 1 d . . .
H30A H 0.8373 -0.0219 0.3172 0.074 Uiso 1 1 calc R . .
H30B H 0.9163 0.0473 0.3095 0.074 Uiso 1 1 calc R . .
C31 C 0.7987(6) 0.0791(6) 0.3460(3) 0.066(2) Uani 1 1 d . . .
H31A H 0.7507 0.0933 0.3230 0.079 Uiso 1 1 calc R . .
H31B H 0.7588 0.0547 0.3681 0.079 Uiso 1 1 calc R . .
C32 C 0.7747(8) 0.1993(6) 0.3800(4) 0.079(3) Uani 1 1 d . . .
H32A H 0.8123 0.2453 0.3900 0.118 Uiso 1 1 calc R . .
H32B H 0.7418 0.1740 0.4034 0.118 Uiso 1 1 calc R . .
H32C H 0.7225 0.2152 0.3594 0.118 Uiso 1 1 calc R . .
C33 C 0.7222(6) 0.6140(4) 0.2767(2) 0.0517(18) Uani 1 1 d . . .
H33 H 0.6834 0.6269 0.2524 0.062 Uiso 1 1 calc R . .
C34 C 0.7208(6) 0.6638(4) 0.3111(2) 0.0536(19) Uani 1 1 d . . .
H34 H 0.6879 0.7130 0.3096 0.064 Uiso 1 1 calc R . .
C35 C 0.7704(5) 0.6377(3) 0.34781(18) 0.0388(14) Uani 1 1 d . . .
C36 C 0.7642(5) 0.6825(4) 0.38482(18) 0.0399(14) Uani 1 1 d . . .
C37 C 0.7589(5) 0.7248(3) 0.41516(18) 0.0324(12) Uani 1 1 d . . .
C38 C 0.7976(4) 0.7603(3) 0.48729(17) 0.0290(11) Uani 1 1 d . . .
H38 H 0.8422 0.7169 0.4900 0.035 Uiso 1 1 calc R . .
C39 C 0.7462(4) 0.7726(3) 0.45025(17) 0.0274(11) Uani 1 1 d . . .
C40 C 0.6813(4) 0.8368(3) 0.44573(15) 0.0258(10) Uani 1 1 d . . .
H40 H 0.6476 0.8477 0.4199 0.031 Uiso 1 1 calc R . .
C41 C 0.6672(4) 0.8844(3) 0.48013(18) 0.0345(12) Uani 1 1 d . . .
C42 C 0.7230(4) 0.8682(4) 0.51702(17) 0.0345(12) Uani 1 1 d . . .
H42 H 0.7151 0.9011 0.5404 0.041 Uiso 1 1 calc R . .
C43 C 0.5419(5) 0.9654(4) 0.4465(2) 0.0431(14) Uani 1 1 d . . .
H43A H 0.4767 0.9892 0.4547 0.052 Uiso 1 1 calc R . .
H43B H 0.5260 0.9188 0.4294 0.052 Uiso 1 1 calc R . .
C44 C 0.5997(5) 1.0204(4) 0.4229(2) 0.0437(14) Uani 1 1 d . . .
H44A H 0.6666 0.9970 0.4166 0.052 Uiso 1 1 calc R . .
H44B H 0.5630 1.0302 0.3961 0.052 Uiso 1 1 calc R . .
C45 C 0.5347(5) 1.1448(4) 0.4371(2) 0.0466(15) Uani 1 1 d . . .
H45A H 0.4692 1.1167 0.4397 0.056 Uiso 1 1 calc R . .
H45B H 0.5368 1.1672 0.4088 0.056 Uiso 1 1 calc R . .
C46 C 0.5429(6) 1.2089(4) 0.4691(3) 0.0494(18) Uani 1 1 d . . .
H46A H 0.5411 1.1862 0.4973 0.059 Uiso 1 1 calc R . .
H46B H 0.6086 1.2366 0.4664 0.059 Uiso 1 1 calc R . .
C47 C 0.4664(6) 1.3221(5) 0.4926(3) 0.0557(18) Uani 1 1 d . . .
H47A H 0.4083 1.3570 0.4875 0.083 Uiso 1 1 calc R . .
H47B H 0.5302 1.3511 0.4898 0.083 Uiso 1 1 calc R . .
H47C H 0.4633 1.3006 0.5207 0.083 Uiso 1 1 calc R . .
C48 C 1.3693(6) 0.4604(4) 0.4004(2) 0.0454(15) Uani 1 1 d . . .
C49 C 1.2775(5) 0.3392(3) 0.41103(18) 0.0347(12) Uani 1 1 d . . .
H49 H 1.2347 0.3656 0.4297 0.042 Uiso 1 1 calc R . .
C50 C 1.3562(5) 0.3791(3) 0.3930(2) 0.0383(13) Uani 1 1 d . . .
C51 C 1.4181(5) 0.3407(4) 0.3653(2) 0.0454(15) Uani 1 1 d . . .
H51 H 1.4718 0.3675 0.3522 0.054 Uiso 1 1 calc R . .
C52 C 1.3997(5) 0.2617(4) 0.3572(2) 0.0424(15) Uani 1 1 d . . .
C53 C 1.3195(5) 0.2251(4) 0.3772(2) 0.0380(14) Uani 1 1 d . . .
H53 H 1.3071 0.1714 0.3723 0.046 Uiso 1 1 calc R . .
C61 C 1.2039(10) -0.0419(11) 0.3350(5) 0.144(7) Uani 1 1 d . . .
H61A H 1.1292 -0.0428 0.3361 0.215 Uiso 1 1 calc R . .
H61B H 1.2291 -0.0946 0.3296 0.215 Uiso 1 1 calc R . .
H61C H 1.2248 -0.0070 0.3128 0.215 Uiso 1 1 calc R . .
C91 C 1.0175(18) 0.4491(14) 0.4591(7) 0.162(7) Uani 1 1 d U . .
H91 H 0.9707 0.4554 0.4809 0.194 Uiso 1 1 calc R . .
C93 C 1.0950(12) 0.5161(9) 0.4003(5) 0.122(5) Uani 1 1 d U . .
H93A H 1.0895 0.5694 0.3896 0.182 Uiso 1 1 calc R . .
H93B H 1.0728 0.4794 0.3786 0.182 Uiso 1 1 calc R . .
H93C H 1.1661 0.5053 0.4086 0.182 Uiso 1 1 calc R . .
C92 C 1.0022(19) 0.5948(15) 0.4437(8) 0.176(8) Uani 1 1 d U . .
H92A H 0.9554 0.6017 0.4685 0.263 Uiso 1 1 d . . .
H92B H 0.9648 0.6147 0.4210 0.263 Uiso 1 1 d . . .
H92C H 1.0600 0.6242 0.4500 0.263 Uiso 1 1 d . . .
C81 C 0.5329(10) 0.4590(9) 0.2840(5) 0.098(4) Uani 1 1 d . . .
H81 H 0.4858 0.4835 0.2653 0.118 Uiso 1 1 calc R . .
C82 C 0.6512(8) 0.3529(7) 0.2967(4) 0.096(4) Uani 1 1 d . . .
H82A H 0.6724 0.3060 0.2819 0.143 Uiso 1 1 calc R . .
H82B H 0.6228 0.3380 0.3234 0.143 Uiso 1 1 calc R . .
H82C H 0.7105 0.3868 0.3016 0.143 Uiso 1 1 calc R . .
C83 C 0.5509(11) 0.3543(9) 0.2321(5) 0.114(4) Uani 1 1 d . . .
H83A H 0.5917 0.3067 0.2301 0.171 Uiso 1 1 calc R . .
H83B H 0.5670 0.3892 0.2092 0.171 Uiso 1 1 calc R . .
H83C H 0.4781 0.3410 0.2305 0.171 Uiso 1 1 calc R . .
N1 N 0.8200(4) 0.5699(3) 0.35093(15) 0.0376(11) Uani 1 1 d . . .
N2 N 1.0628(3) 0.2304(3) 0.37110(14) 0.0270(9) Uani 1 1 d . . .
N3 N 1.3177(4) 0.6485(3) 0.43092(16) 0.0355(11) Uani 1 1 d . . .
N4 N 1.0144(3) 0.1552(3) 0.44929(13) 0.0288(9) Uani 1 1 d . . .
N5 N 0.7863(3) 0.8084(3) 0.51993(14) 0.0261(9) Uani 1 1 d . . .
N6 N 1.2602(4) 0.2637(3) 0.40275(14) 0.0300(10) Uani 1 1 d . . .
N91 N 1.0307(10) 0.5076(7) 0.4359(4) 0.108(4) Uani 1 1 d . . .
N81 N 0.5749(8) 0.3937(8) 0.2722(3) 0.101(3) Uani 1 1 d . . .
O1 O 1.0293(4) 0.1393(3) 0.27019(14) 0.0540(13) Uani 1 1 d . . .
O2 O 1.2119(7) 0.0796(6) 0.2349(3) 0.106(3) Uani 1 1 d . . .
O3 O 1.2015(7) -0.0880(5) 0.2269(3) 0.109(3) Uani 1 1 d . . .
O4 O 0.8968(4) -0.0375(3) 0.45391(14) 0.0479(12) Uani 1 1 d . . .
O5 O 0.9396(4) -0.0074(3) 0.36307(15) 0.0494(11) Uani 1 1 d . . .
O6 O 0.8450(4) 0.1453(3) 0.3612(2) 0.0656(15) Uani 1 1 d . . .
O7 O 0.6018(4) 0.9430(3) 0.48319(14) 0.0495(12) Uani 1 1 d . . .
O8 O 0.6166(4) 1.0936(3) 0.44366(17) 0.0532(12) Uani 1 1 d . . .
O9 O 0.4627(4) 1.2609(3) 0.46352(18) 0.0607(14) Uani 1 1 d . . .
O10 O 1.4589(5) 0.2271(3) 0.33040(19) 0.0633(16) Uani 1 1 d . . .
O61 O 1.2102(4) 0.0670(3) 0.38971(18) 0.0559(13) Uani 1 1 d . . .
O62 O 1.2184(6) -0.0642(4) 0.4115(3) 0.096(2) Uani 1 1 d . . .
O63 O 1.3635(4) -0.0079(5) 0.3808(2) 0.081(2) Uani 1 1 d . . .
O91 O 1.0626(8) 0.3794(4) 0.4563(3) 0.112(3) Uani 1 1 d . . .
O81 O 0.5505(7) 0.4912(5) 0.3183(3) 0.100(3) Uani 1 1 d . . .
S61 S 1.25518(11) -0.00874(8) 0.38251(5) 0.0353(4) Uani 1 1 d . . .
Pd1 Pd 1.13685(3) 0.20929(2) 0.425895(11) 0.0244(2) Uani 1 1 d . . .
S71 S 0.38791(12) 0.11355(8) 0.68757(4) 0.0371(4) Uani 1 1 d D . .
O71 O 0.3639(5) 0.1189(4) 0.64443(13) 0.083(2) Uani 1 1 d D . .
O72 O 0.4387(6) 0.1885(4) 0.6985(2) 0.103(2) Uani 1 1 d DU . .
O73 O 0.2980(5) 0.1114(5) 0.7133(2) 0.112(3) Uani 1 1 d DU . .
C71 C 0.4661(8) 0.0395(5) 0.6999(3) 0.110(4) Uani 1 1 d DU . .
H71A H 0.4794 0.0389 0.7300 0.166 Uiso 1 1 calc R . .
H71B H 0.5306 0.0458 0.6856 0.166 Uiso 1 1 calc R . .
H71C H 0.4339 -0.0097 0.6914 0.166 Uiso 1 1 calc R . .
C54 C 1.4300(10) 0.1498(5) 0.3151(4) 0.099(4) Uani 1 1 d . . .
H54A H 1.3561 0.1488 0.3077 0.119 Uiso 1 1 calc R . .
H54B H 1.4435 0.1104 0.3370 0.119 Uiso 1 1 calc R . .
C55 C 1.4903(13) 0.1310(9) 0.2777(5) 0.120(4) Uani 1 1 d U . .
H55A H 1.5637 0.1425 0.2829 0.144 Uiso 1 1 calc R . .
H55B H 1.4827 0.0754 0.2701 0.144 Uiso 1 1 calc R . .
O11 O 1.4461(11) 0.1826(9) 0.2442(5) 0.166(5) Uani 1 1 d U . .


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
C1 C33 1.355(9) . ?
C1 C2 1.409(8) . ?
C2 N1 1.346(7) . ?
C2 C3 1.445(8) . ?
C3 C4 1.194(9) . ?
C4 C6 1.420(8) . ?
C5 N2 1.350(7) . ?
C5 C6 1.389(8) . ?
C6 C7 1.408(8) . ?
C7 C8 1.353(8) . ?
C8 O1 1.388(7) . ?
C8 C9 1.398(9) . ?
C9 N2 1.354(7) . ?
C10 O1 1.384(9) . ?
C10 C11 1.505(14) . ?
C11 O2 1.466(14) . ?
C12 C13 1.407(17) . ?
C12 O2 1.443(15) . ?
C13 O3 1.449(16) . ?
C14 O3 1.378(14) . ?
C15 C48 1.218(9) . ?
C15 C16 1.401(9) . ?
C16 N3 1.348(8) . ?
C16 C17 1.414(8) . ?
C17 C18 1.369(8) . ?
C18 C19 1.408(8) . ?
C19 C20 1.384(8) . ?
C20 N3 1.348(7) . ?
C20 C21 1.439(8) 3_766 ?
C21 C22 1.179(9) . ?
C21 C20 1.439(8) 3_766 ?
C22 C24 1.455(8) . ?
C23 N4 1.350(7) . ?
C23 C24 1.362(9) . ?
C24 C25 1.379(10) . ?
C25 C27 1.394(8) . ?
C26 N4 1.354(7) . ?
C26 C27 1.383(8) . ?
C27 O4 1.360(7) . ?
C28 O4 1.459(8) . ?
C28 C29 1.528(10) . ?
C29 O5 1.370(9) . ?
C30 O5 1.425(10) . ?
C30 C31 1.486(13) . ?
C31 O6 1.373(11) . ?
C32 O6 1.453(11) . ?
C33 C34 1.399(9) . ?
C34 C35 1.409(9) . ?
C35 N1 1.337(7) . ?
C35 C36 1.425(8) . ?
C36 C37 1.222(8) . ?
C37 C39 1.412(8) . ?
C38 N5 1.350(7) . ?
C38 C39 1.371(8) . ?
C39 C40 1.398(8) . ?
C40 C41 1.394(7) . ?
C41 O7 1.327(7) . ?
C41 C42 1.407(8) . ?
C42 N5 1.322(7) . ?
C43 O7 1.455(8) . ?
C43 C44 1.442(10) . ?
C44 O8 1.439(8) . ?
C45 O8 1.400(8) . ?
C45 C46 1.512(10) . ?
C46 O9 1.386(9) . ?
C47 O9 1.409(10) . ?
C48 C50 1.426(8) . ?
C49 N6 1.342(7) . ?
C49 C50 1.379(8) . ?
C50 C51 1.389(10) . ?
C51 C52 1.402(9) . ?
C52 O10 1.321(8) . ?
C52 C53 1.396(9) . ?
C53 N6 1.326(8) . ?
C61 S61 1.751(12) . ?
C91 N91 1.27(2) . ?
C91 O91 1.34(2) . ?
C93 N91 1.451(17) . ?
C92 N91 1.57(3) . ?
C81 O81 1.252(16) . ?
C81 N81 1.311(18) . ?
C82 N81 1.441(15) . ?
C83 N81 1.485(19) . ?
N2 Pd1 2.025(5) . ?
N4 Pd1 2.018(4) . ?
N5 Pd1 2.016(4) 3_766 ?
N6 Pd1 2.026(5) . ?
O10 C54 1.463(11) . ?
O61 S61 1.450(5) . ?
O62 S61 1.428(7) . ?
O63 S61 1.422(6) . ?
Pd1 N5 2.016(4) 3_766 ?
S71 O71 1.421(4) . ?
S71 O73 1.459(6) . ?
S71 O72 1.487(6) . ?
S71 C71 1.675(6) . ?
C54 C55 1.493(16) . ?
C55 O11 1.50(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
C33 C1 C2 117.4(5) . . ?
N1 C2 C1 124.1(5) . . ?
N1 C2 C3 116.5(5) . . ?
C1 C2 C3 119.4(5) . . ?
C4 C3 C2 177.8(7) . . ?
C3 C4 C6 178.0(6) . . ?
N2 C5 C6 121.2(5) . . ?
C5 C6 C7 118.5(5) . . ?
C5 C6 C4 119.2(5) . . ?
C7 C6 C4 122.3(5) . . ?
C8 C7 C6 119.8(5) . . ?
C7 C8 O1 122.9(6) . . ?
C7 C8 C9 119.7(5) . . ?
O1 C8 C9 117.0(5) . . ?
N2 C9 C8 120.8(5) . . ?
O1 C10 C11 109.4(7) . . ?
O2 C11 C10 111.8(8) . . ?
C13 C12 O2 110.5(13) . . ?
C12 C13 O3 108.5(11) . . ?
C48 C15 C16 176.0(8) . . ?
N3 C16 C15 117.0(5) . . ?
N3 C16 C17 122.9(5) . . ?
C15 C16 C17 120.1(5) . . ?
C18 C17 C16 118.6(5) . . ?
C17 C18 C19 118.9(5) . . ?
C20 C19 C18 118.7(5) . . ?
N3 C20 C19 123.4(5) . . ?
N3 C20 C21 115.9(5) . 3_766 ?
C19 C20 C21 120.7(5) . 3_766 ?
C22 C21 C20 176.3(7) . 3_766 ?
C21 C22 C24 177.8(8) . . ?
N4 C23 C24 121.3(6) . . ?
C23 C24 C25 119.9(5) . . ?
C23 C24 C22 119.7(6) . . ?
C25 C24 C22 120.4(6) . . ?
C24 C25 C27 119.2(5) . . ?
N4 C26 C27 121.1(5) . . ?
O4 C27 C26 125.2(5) . . ?
O4 C27 C25 116.1(5) . . ?
C26 C27 C25 118.7(5) . . ?
O4 C28 C29 109.3(5) . . ?
O5 C29 C28 111.0(5) . . ?
O5 C30 C31 112.6(6) . . ?
O6 C31 C30 111.9(7) . . ?
C1 C33 C34 120.7(6) . . ?
C35 C34 C33 117.1(6) . . ?
N1 C35 C34 123.5(5) . . ?
N1 C35 C36 116.5(5) . . ?
C34 C35 C36 119.8(5) . . ?
C37 C36 C35 176.3(7) . . ?
C36 C37 C39 176.5(7) . . ?
N5 C38 C39 121.5(5) . . ?
C38 C39 C40 119.7(5) . . ?
C38 C39 C37 122.9(5) . . ?
C40 C39 C37 117.4(5) . . ?
C41 C40 C39 118.2(5) . . ?
O7 C41 C40 127.1(5) . . ?
O7 C41 C42 114.1(5) . . ?
C40 C41 C42 118.7(5) . . ?
N5 C42 C41 121.6(5) . . ?
O7 C43 C44 108.9(6) . . ?
O8 C44 C43 113.8(6) . . ?
O8 C45 C46 108.4(6) . . ?
O9 C46 C45 109.9(6) . . ?
C15 C48 C50 176.9(8) . . ?
N6 C49 C50 121.4(6) . . ?
C49 C50 C51 119.4(5) . . ?
C49 C50 C48 120.3(6) . . ?
C51 C50 C48 120.1(5) . . ?
C52 C51 C50 118.6(5) . . ?
O10 C52 C53 124.2(6) . . ?
O10 C52 C51 117.2(5) . . ?
C53 C52 C51 118.6(6) . . ?
N6 C53 C52 121.5(6) . . ?
N91 C91 O91 126.9(19) . . ?
O81 C81 N81 124.5(14) . . ?
C2 N1 C35 116.8(5) . . ?
C5 N2 C9 119.9(5) . . ?
C5 N2 Pd1 119.2(4) . . ?
C9 N2 Pd1 120.5(4) . . ?
C16 N3 C20 117.3(5) . . ?
C23 N4 C26 119.8(5) . . ?
C23 N4 Pd1 120.0(4) . . ?
C26 N4 Pd1 120.1(3) . . ?
C42 N5 C38 120.2(5) . . ?
C42 N5 Pd1 118.4(4) . 3_766 ?
C38 N5 Pd1 121.4(4) . 3_766 ?
C53 N6 C49 120.5(5) . . ?
C53 N6 Pd1 119.0(4) . . ?
C49 N6 Pd1 120.3(4) . . ?
C91 N91 C93 129.8(15) . . ?
C91 N91 C92 128.8(16) . . ?
C93 N91 C92 100.1(13) . . ?
C81 N81 C82 123.2(13) . . ?
C81 N81 C83 124.3(12) . . ?
C82 N81 C83 112.6(13) . . ?
C8 O1 C10 118.0(6) . . ?
C12 O2 C11 112.8(9) . . ?
C14 O3 C13 111.9(11) . . ?
C27 O4 C28 120.6(4) . . ?
C29 O5 C30 115.2(6) . . ?
C31 O6 C32 113.5(7) . . ?
C41 O7 C43 118.4(5) . . ?
C45 O8 C44 111.8(5) . . ?
C46 O9 C47 112.4(6) . . ?
C52 O10 C54 118.6(6) . . ?
O63 S61 O62 112.8(5) . . ?
O63 S61 O61 114.0(4) . . ?
O62 S61 O61 110.4(4) . . ?
O63 S61 C61 109.2(5) . . ?
O62 S61 C61 103.1(8) . . ?
O61 S61 C61 106.5(6) . . ?
N5 Pd1 N4 89.43(18) 3_766 . ?
N5 Pd1 N2 177.94(17) 3_766 . ?
N4 Pd1 N2 92.43(18) . . ?
N5 Pd1 N6 90.24(18) 3_766 . ?
N4 Pd1 N6 179.65(18) . . ?
N2 Pd1 N6 87.90(18) . . ?
O71 S71 O73 113.4(4) . . ?
O71 S71 O72 105.2(4) . . ?
O73 S71 O72 104.5(4) . . ?
O71 S71 C71 113.5(4) . . ?
O73 S71 C71 110.1(5) . . ?
O72 S71 C71 109.6(5) . . ?
O10 C54 C55 109.3(9) . . ?
O11 C55 C54 104.6(12) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         4.230
_refine_diff_density_min         -1.480
_refine_diff_density_rms         0.264

# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 288 55 ' '
2 0.082 0.730 0.357 73 18 ' '
3 -0.082 0.270 0.643 73 18 ' '
4 0.500 0.500 0.500 288 55 ' '
5 0.418 0.230 0.143 73 18 ' '
6 0.582 0.770 0.857 73 18 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
there was residual electron density which could not be
resolved consisting of a total electron count of 868,
which we attribute to the missing ends (CH2CH2OCH3) of two
diglyme chains per cage (4 in total, 156 electrons) and 18 
DMF solvent molecules (720 electrons).
;
