# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

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

data_1_sq_sq
_database_code_depnum_ccdc_archive 'CCDC 1524463'
_audit_update_record             
;
2018-05-29 deposited with the CCDC.
2018-05-31 downloaded from the CCDC.
;
_audit_creation_date             2018-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C176 H128 Cl16 N32 O40 Pd8 Sm4)'
_chemical_formula_sum            'C44 H43 Cl4 N14 O13 Pd2 Sm'
_chemical_formula_weight         1480.87
_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 0.0181 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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -5.3236 12.2178 '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           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'x, -y+1/2, -z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'-x, y-1/2, z-1/2'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.1010(6)
_cell_length_b                   40.7504(15)
_cell_length_c                   15.1414(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6232.5(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6434
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      73.6230
_cell_measurement_theta_min      4.3040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.716
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.992
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2924
_exptl_crystal_size_max          0.1116
_exptl_crystal_size_mid          0.0671
_exptl_crystal_size_min          0.0629
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            22154
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        64.997
_diffrn_reflns_theta_max         64.997
_diffrn_reflns_theta_min         4.340
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -48.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8048   29.0000  -36.0000 83

#__ type_ start__ end____ width___ exp.time_
  2 omega   46.00  145.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316 -165.0000  -61.0000 99

#__ type_ start__ end____ width___ exp.time_
  3 omega   33.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -29.0000  162.0000 58

#__ type_ start__ end____ width___ exp.time_
  4 omega  101.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   97.0000   90.0000 77

#__ type_ start__ end____ width___ exp.time_
  5 omega  -39.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8048   38.0000 -120.0000 71

#__ type_ start__ end____ width___ exp.time_
  6 omega -117.00  -86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8048 -165.0000  -61.0000 31

#__ type_ start__ end____ width___ exp.time_
  7 omega    2.00   83.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.8048  -99.0000  -90.0000 81

#__ type_ start__ end____ width___ exp.time_
  8 omega   34.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000 -150.0000 56

#__ type_ start__ end____ width___ exp.time_
  9 omega   95.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  125.0000 -180.0000 81

#__ type_ start__ end____ width___ exp.time_
 10 omega  106.00  176.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  125.0000  120.0000 70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4222
_reflns_number_total             5175
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         5175
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0889
_refine_ls_restrained_S_all      1.176
_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)+(0.0500P)²+30.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1926
_refine_ls_wR_factor_ref         0.2009
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C27 \\sim C9 \\sim C8 \\sim C7 \\sim C6 \\sim C5: within 0.01A with sigma of
3.8 and sigma for terminal atoms of 0.01
Uanis(C27) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Fixed Sof: C4(0.5) H4(0.5) C5(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5) C8(0.5)
 C9(0.5) H9(0.5) O3(0.5) H19C(0.5) H19D(0.5) H19A(0.5) H19B(0.5) C22(0.5)
 C23(0.5) H23(0.5) C24(0.5) H24(0.5) C25(0.5) C26(0.5) H26(0.5) C27(0.5)
 H27(0.5) C28(0.5) O6(0.5) C29(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19C,H19D), C19(H19A,H19B), C20(H20A,H20B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27)
4.c Fitted hexagon refined as free rotating group:
 C4(C5,C6,C7,C8,C9), C23(C24,C25,C26,C27,C28)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Sm1 Sm 0.250000 0.500000 0.99488(8) 0.0995(4) Uani 1 2 d S T P . .
Pd1 Pd 0.70676(9) 0.23458(2) 0.92746(6) 0.0870(3) Uani 1 1 d . . . . .
Cl2 Cl 0.6301(3) 0.26047(8) 1.05124(19) 0.0989(8) Uani 1 1 d . . . . .
Cl1 Cl 0.8146(5) 0.19758(9) 1.0137(3) 0.1316(13) Uani 1 1 d . . . . .
N2 N 0.5873(9) 0.26539(19) 0.8562(6) 0.081(2) Uani 1 1 d . . . . .
O1 O 1.1255(9) 0.4547(2) 0.9449(7) 0.123(3) Uani 1 1 d . . . . .
N1 N 0.8018(9) 0.2848(2) 0.6804(6) 0.089(2) Uani 1 1 d . . . . .
N4 N 0.5167(9) 0.3026(2) 0.7647(6) 0.084(2) Uani 1 1 d . . . . .
C1 C 0.7615(13) 0.2908(3) 0.7616(8) 0.091(3) Uani 1 1 d . . . . .
O2 O 0.9189(9) 0.4673(2) 0.9562(8) 0.124(3) Uani 1 1 d . . . . .
C2 C 0.4578(11) 0.2675(2) 0.8664(7) 0.080(3) Uani 1 1 d . . . . .
H2 H 0.406793 0.255550 0.906067 0.096 Uiso 1 1 calc R . . . .
N3 N 0.8621(9) 0.3007(2) 0.8129(6) 0.090(2) Uani 1 1 d . . . . .
C3 C 0.4122(12) 0.2904(3) 0.8081(8) 0.094(3) Uani 1 1 d . . . . .
H3 H 0.324317 0.296537 0.800054 0.112 Uiso 1 1 calc R . . . .
C4 C 0.4930(13) 0.3776(4) 0.7940(11) 0.091(8) Uani 0.5 1 d . U . A 2
H4 H 0.418578 0.368168 0.819587 0.109 Uiso 0.5 1 calc R . . A 2
C5 C 0.5602(16) 0.3613(3) 0.7270(11) 0.084(6) Uani 0.5 1 d G U . A 2
C6 C 0.6715(17) 0.3755(4) 0.6887(10) 0.117(8) Uani 0.5 1 d G U . A 2
H6 H 0.716414 0.364521 0.643925 0.141 Uiso 0.5 1 calc R . . A 2
C7 C 0.7155(15) 0.4060(4) 0.7174(11) 0.117(8) Uani 0.5 1 d G U . A 2
H7 H 0.789958 0.415442 0.691762 0.141 Uiso 0.5 1 calc R . . A 2
C8 C 0.6483(16) 0.4223(3) 0.7843(11) 0.091(6) Uani 0.5 1 d G U . A 2
C9 C 0.5371(14) 0.4082(3) 0.8226(10) 0.082(5) Uani 0.5 1 d G U . A 2
H9 H 0.492124 0.419090 0.867424 0.098 Uiso 0.5 1 calc R . . A 2
C10 C 0.9006(11) 0.3465(3) 0.9143(7) 0.084(3) Uani 1 1 d . . . . .
C11 C 0.9330(14) 0.2899(3) 0.6793(9) 0.104(4) Uani 1 1 d . . . . .
H11 H 0.988543 0.287567 0.630656 0.125 Uiso 1 1 calc R . . . .
C12 C 1.0633(14) 0.3885(3) 0.9190(10) 0.116(4) Uani 1 1 d . . . . .
H12 H 1.152220 0.394169 0.914694 0.140 Uiso 1 1 calc R . . . .
C13 C 0.9728(12) 0.4120(3) 0.9314(8) 0.088(3) Uani 1 1 d . . . . .
C14 C 0.8438(15) 0.4026(4) 0.9376(11) 0.123(4) Uani 1 1 d . U . . .
H14 H 0.778501 0.418250 0.947487 0.147 Uiso 1 1 calc R . . . .
O3 O 0.7942(19) 0.4677(5) 0.7711(14) 0.123(6) Uani 0.5 1 d . . . A 2
C15 C 0.8090(14) 0.3695(3) 0.9292(13) 0.135(6) Uani 1 1 d . . . . .
H15 H 0.720608 0.363379 0.934130 0.162 Uiso 1 1 calc R . . . .
C16 C 1.0083(11) 0.4479(3) 0.9455(8) 0.086(3) Uani 1 1 d . . . . .
O5 O 0.3646(10) 0.4771(3) 0.8662(7) 0.135(4) Uani 1 1 d . . . A 1
C17 C 0.9699(13) 0.2989(3) 0.7614(11) 0.111(4) Uani 1 1 d . . . . .
H17 H 1.056167 0.303234 0.779335 0.133 Uiso 1 1 calc R . . . .
O4 O 0.6511(9) 0.4727(2) 0.8759(7) 0.119(3) Uani 1 1 d . . . . .
C18 C 0.6215(11) 0.2871(3) 0.7933(8) 0.085(3) Uani 1 1 d . . . . .
C19 C 0.5124(12) 0.3278(3) 0.6972(8) 0.096(3) Uani 1 1 d . . . . .
H19C H 0.422020 0.329815 0.676352 0.115 Uiso 0.5 1 calc R . . A 2
H19D H 0.566273 0.320706 0.647685 0.115 Uiso 0.5 1 calc R . . A 2
H19A H 0.455000 0.320232 0.650047 0.115 Uiso 0.5 1 calc R . . A 1
H19B H 0.600633 0.330117 0.672672 0.115 Uiso 0.5 1 calc R . . A 1
C20 C 0.8581(12) 0.3107(3) 0.9058(7) 0.089(3) Uani 1 1 d . . . . .
H20A H 0.916886 0.296901 0.940203 0.107 Uiso 1 1 calc R . . . .
H20B H 0.768991 0.308053 0.928602 0.107 Uiso 1 1 calc R . . . .
C21 C 1.0260(14) 0.3555(3) 0.9124(11) 0.113(4) Uani 1 1 d . . . . .
H21 H 1.091241 0.339580 0.906668 0.136 Uiso 1 1 calc R . . . .
C22 C 0.698(3) 0.4560(6) 0.813(2) 0.100(7) Uani 0.5 1 d . . . A 2
C23 C 0.393(2) 0.3801(5) 0.6670(10) 0.155(12) Uani 0.5 1 d . U . A 1
H23 H 0.376722 0.372243 0.610384 0.186 Uiso 0.5 1 calc R . . A 1
C24 C 0.345(2) 0.4107(5) 0.6921(12) 0.178(15) Uani 0.5 1 d G U . A 1
H24 H 0.296473 0.423271 0.652223 0.213 Uiso 0.5 1 calc R . . A 1
C25 C 0.369(2) 0.4225(4) 0.7767(14) 0.102(7) Uani 0.5 1 d G U . A 1
C26 C 0.441(2) 0.4037(5) 0.8363(11) 0.127(11) Uani 0.5 1 d G . . A 1
H26 H 0.457328 0.411571 0.892898 0.152 Uiso 0.5 1 calc R . . A 1
C27 C 0.489(2) 0.3731(5) 0.8112(12) 0.144(17) Uani 0.5 1 d G U . A 1
H27 H 0.537577 0.360542 0.851060 0.173 Uiso 0.5 1 calc R . . A 1
C28 C 0.465(2) 0.3613(4) 0.7266(13) 0.091(6) Uani 0.5 1 d G . . A 1
O6 O 0.228(2) 0.4675(6) 0.7577(14) 0.143(8) Uani 0.5 1 d . . . A 1
C29 C 0.318(3) 0.4567(8) 0.805(2) 0.117(8) Uani 0.5 1 d . U . A 1


_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
Sm1 O1 2.358(8) 1_455 ?
Sm1 O1 2.358(8) 2_665 ?
Sm1 O2 2.288(9) 6_557 ?
Sm1 O2 2.288(9) 5_667 ?
Sm1 O5 2.451(9) . ?
Sm1 O5 2.451(9) 2_565 ?
Sm1 O4 2.463(9) 5_667 ?
Sm1 O4 2.463(9) 6_557 ?
Pd1 Cl2 2.286(3) . ?
Pd1 Cl1 2.273(4) . ?
Pd1 N2 2.049(9) . ?
Pd1 N1 2.052(10) 3_556 ?
N2 C2 1.320(13) . ?
N2 C18 1.346(13) . ?
O1 C16 1.216(13) . ?
N1 C1 1.319(14) . ?
N1 C11 1.341(15) . ?
N4 C3 1.338(14) . ?
N4 C18 1.305(13) . ?
N4 C19 1.449(15) . ?
C1 N3 1.340(14) . ?
C1 C18 1.501(16) . ?
O2 C16 1.212(14) . ?
C2 C3 1.365(15) . ?
N3 C17 1.341(15) . ?
N3 C20 1.466(13) . ?
C4 C5 1.3900 . ?
C4 C9 1.3900 . ?
C5 C6 1.3900 . ?
C5 C19 1.518(16) . ?
C6 C7 1.3900 . ?
C7 C8 1.3900 . ?
C8 C9 1.3900 . ?
C8 C22 1.52(3) . ?
C10 C15 1.334(17) . ?
C10 C20 1.527(15) . ?
C10 C21 1.320(16) . ?
C11 C17 1.349(19) . ?
C12 C13 1.335(17) . ?
C12 C21 1.399(18) . ?
C13 C14 1.361(18) . ?
C13 C16 1.523(16) . ?
C14 C15 1.400(19) . ?
O3 C22 1.26(3) . ?
O5 C29 1.33(3) . ?
O4 C22 1.26(3) . ?
C19 C28 1.516(18) . ?
C23 C24 1.3900 . ?
C23 C28 1.3900 . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
C25 C29 1.55(3) . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
O6 C29 1.24(3) . ?

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 Sm1 O1 142.6(5) 1_455 2_665 ?
O1 Sm1 O5 78.0(4) 2_665 . ?
O1 Sm1 O5 72.4(3) 1_455 . ?
O1 Sm1 O5 72.4(3) 2_665 2_565 ?
O1 Sm1 O5 78.0(4) 1_455 2_565 ?
O1 Sm1 O4 71.6(4) 1_455 6_557 ?
O1 Sm1 O4 145.6(4) 2_665 6_557 ?
O1 Sm1 O4 71.6(4) 2_665 5_667 ?
O1 Sm1 O4 145.6(4) 1_455 5_667 ?
O2 Sm1 O1 99.3(3) 5_667 1_455 ?
O2 Sm1 O1 92.6(3) 6_557 1_455 ?
O2 Sm1 O1 92.6(3) 5_667 2_665 ?
O2 Sm1 O1 99.3(3) 6_557 2_665 ?
O2 Sm1 O2 142.2(6) 6_557 5_667 ?
O2 Sm1 O5 71.5(4) 5_667 2_565 ?
O2 Sm1 O5 146.3(4) 5_667 . ?
O2 Sm1 O5 71.5(4) 6_557 . ?
O2 Sm1 O5 146.3(4) 6_557 2_565 ?
O2 Sm1 O4 72.8(3) 6_557 5_667 ?
O2 Sm1 O4 72.8(3) 5_667 6_557 ?
O2 Sm1 O4 77.4(3) 6_557 6_557 ?
O2 Sm1 O4 77.4(3) 5_667 5_667 ?
O5 Sm1 O5 74.8(6) 2_565 . ?
O5 Sm1 O4 127.8(3) . 5_667 ?
O5 Sm1 O4 130.5(4) 2_565 5_667 ?
O5 Sm1 O4 130.5(4) . 6_557 ?
O5 Sm1 O4 127.8(3) 2_565 6_557 ?
O4 Sm1 O4 74.8(5) 5_667 6_557 ?
Cl1 Pd1 Cl2 89.86(13) . . ?
N2 Pd1 Cl2 87.1(3) . . ?
N2 Pd1 Cl1 172.6(3) . . ?
N2 Pd1 N1 95.3(4) . 3_556 ?
N1 Pd1 Cl2 171.2(3) 3_556 . ?
N1 Pd1 Cl1 88.7(3) 3_556 . ?
C2 N2 Pd1 124.2(7) . . ?
C2 N2 C18 107.1(9) . . ?
C18 N2 Pd1 128.7(8) . . ?
C16 O1 Sm1 134.1(8) . 1_655 ?
C1 N1 Pd1 132.0(8) . 3_556 ?
C1 N1 C11 106.7(11) . . ?
C11 N1 Pd1 120.8(8) . 3_556 ?
C3 N4 C19 125.8(10) . . ?
C18 N4 C3 107.4(10) . . ?
C18 N4 C19 126.8(10) . . ?
N1 C1 N3 111.2(11) . . ?
N1 C1 C18 124.7(11) . . ?
N3 C1 C18 124.0(10) . . ?
C16 O2 Sm1 168.3(10) . 5_667 ?
N2 C2 C3 107.7(10) . . ?
C1 N3 C17 105.2(11) . . ?
C1 N3 C20 128.2(10) . . ?
C17 N3 C20 126.6(11) . . ?
N4 C3 C2 107.7(10) . . ?
C5 C4 C9 120.0 . . ?
C4 C5 C19 119.5(11) . . ?
C6 C5 C4 120.0 . . ?
C6 C5 C19 120.5(11) . . ?
C7 C6 C5 120.0 . . ?
C6 C7 C8 120.0 . . ?
C7 C8 C22 118.8(15) . . ?
C9 C8 C7 120.0 . . ?
C9 C8 C22 121.2(15) . . ?
C8 C9 C4 120.0 . . ?
C15 C10 C20 119.3(11) . . ?
C21 C10 C15 118.3(12) . . ?
C21 C10 C20 122.3(11) . . ?
N1 C11 C17 107.7(12) . . ?
C13 C12 C21 120.9(13) . . ?
C12 C13 C14 117.6(12) . . ?
C12 C13 C16 123.2(12) . . ?
C14 C13 C16 119.1(12) . . ?
C13 C14 C15 120.3(14) . . ?
C10 C15 C14 121.1(14) . . ?
O1 C16 C13 116.6(11) . . ?
O2 C16 O1 125.3(11) . . ?
O2 C16 C13 118.1(10) . . ?
C29 O5 Sm1 128.5(15) . . ?
N3 C17 C11 109.1(12) . . ?
N2 C18 C1 122.3(10) . . ?
N4 C18 N2 110.1(10) . . ?
N4 C18 C1 127.6(11) . . ?
N4 C19 C5 114.7(11) . . ?
N4 C19 C28 116.2(12) . . ?
N3 C20 C10 109.9(9) . . ?
C10 C21 C12 121.6(13) . . ?
O3 C22 C8 117(2) . . ?
O4 C22 C8 126(2) . . ?
O4 C22 O3 118(2) . . ?
C24 C23 C28 120.0 . . ?
C23 C24 C25 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 C29 120.7(18) . . ?
C26 C25 C29 119.3(18) . . ?
C27 C26 C25 120.0 . . ?
C26 C27 C28 120.0 . . ?
C23 C28 C19 118.2(14) . . ?
C27 C28 C19 121.8(14) . . ?
C27 C28 C23 120.0 . . ?
O5 C29 C25 130(3) . . ?
O6 C29 O5 116(3) . . ?
O6 C29 C25 114(3) . . ?

_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_2_sq_sq
_database_code_depnum_ccdc_archive 'CCDC 1524464'
_audit_update_record             
;
2018-05-29 deposited with the CCDC.
2018-05-31 downloaded from the CCDC.
;
_audit_creation_date             2018-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C176 H128 Cl16 Eu4 N32 O40 Pd8)'
_chemical_formula_sum            'C44 H38 Cl4 Eu N8 O10.50 Pd2'
_chemical_formula_weight         1353.38
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Pd1 Pr1 N1 C1 O1'
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -8.9294 11.1857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   10.1709(7)
_cell_length_b                   40.820(2)
_cell_length_c                   15.1189(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6277.0(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5868
_cell_measurement_temperature    101.98(18)
_cell_measurement_theta_max      75.4520
_cell_measurement_theta_min      4.3090
_shelx_estimated_absorpt_T_max   0.516
_shelx_estimated_absorpt_T_min   0.348
_exptl_absorpt_coefficient_mu    13.632
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.0982
_exptl_crystal_size_mid          0.0681
_exptl_crystal_size_min          0.056
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21140
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.832
_diffrn_reflns_theta_min         4.332
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      101.98(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -11.00  122.20   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6798   15.0000 -104.0000 444

#__ type_ start__ end____ width___ exp.time_
  2 omega   54.00   88.80   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6798 -112.0000  -70.0000 116

#__ type_ start__ end____ width___ exp.time_
  3 omega   35.00  104.00   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816 -112.0000  -70.0000 230

#__ type_ start__ end____ width___ exp.time_
  4 omega   46.00  123.10   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816 -142.0000 -142.0000 257

#__ type_ start__ end____ width___ exp.time_
  5 omega   58.00  141.10   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816   15.0000 -104.0000 277

#__ type_ start__ end____ width___ exp.time_
  6 omega  -37.00    9.20   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798   38.0000 -150.0000 154

#__ type_ start__ end____ width___ exp.time_
  7 omega  -49.00   32.00   0.3000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798   38.0000  -30.0000 270

#__ type_ start__ end____ width___ exp.time_
  8 omega   53.00   87.20   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -45.0000  -30.0000 114

#__ type_ start__ end____ width___ exp.time_
  9 omega   34.00   86.20   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -30.0000   60.0000 174

#__ type_ start__ end____ width___ exp.time_
 10 omega   40.00   74.80   0.3000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -30.0000  -60.0000 116
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.1351181000
_diffrn_orient_matrix_UB_12      -0.0153719000
_diffrn_orient_matrix_UB_13      -0.0199987000
_diffrn_orient_matrix_UB_21      -0.0618992000
_diffrn_orient_matrix_UB_22      -0.0344288000
_diffrn_orient_matrix_UB_23      0.0037704000
_diffrn_orient_matrix_UB_31      -0.0291204000
_diffrn_orient_matrix_UB_32      0.0018302000
_diffrn_orient_matrix_UB_33      -0.0998479000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4073
_reflns_number_total             6132
_reflns_odcompleteness_completeness 99.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.666
_refine_diff_density_min         -1.348
_refine_diff_density_rms         0.140
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.872
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         6132
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0840
_refine_ls_restrained_S_all      0.868
_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)+100.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1839
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C16-O3
 1.3 with sigma of 0.01
 C16-C20
 1.5 with sigma of 0.01
 O4-C16
 1.3 with sigma of 0.01
 C29-C27
 1.5 with sigma of 0.01
 O5_$1-C29
 1.3 with sigma of 0.01
 O6-C29
 1.3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C25 \\sim C24 \\sim C23 \\sim C28 \\sim C27 \\sim C26 \\sim C29 \\sim O6:
within 0.01A with sigma of 3.8 and sigma for terminal atoms of 0.01
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C25) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C19) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H14A(0.5) H14B(0.5) H14C(0.5) H14D(0.5) O4(0.5) C16(0.5) C17(0.5)
 C18(0.5) H18(0.5) C19(0.5) H19(0.5) C20(0.5) C21(0.5) H21(0.5) C22(0.5)
 H22(0.5) C23(0.5) H23(0.5) C24(0.5) C25(0.5) H25(0.5) C26(0.5) H26(0.5)
 C27(0.5) C28(0.5) H28(0.5) O6(0.5) C29(0.5)
5.a :
 N005(C1,C2,N008,C3), N006(C4,C5,N007,C6)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C14(H14C,H14D)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28)
5.d Fitted hexagon refined as free rotating group:
 C8(C9,C10,C11,C12,C13), C17(C18,C19,C20,C21,C22), C23(C24,C25,C26,C27,C28)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Eu1 Eu 0.250000 0.500000 0.49599(9) 0.0769(3) Uani 1 2 d S T P . .
Pd1 Pd 0.20068(9) 0.73451(2) 0.92791(6) 0.0703(3) Uani 1 1 d . . . . .
Cl2 Cl 0.1257(3) 0.75967(7) 1.0523(2) 0.0840(8) Uani 1 1 d . . . . .
Cl1 Cl 0.3068(5) 0.69815(10) 1.0144(3) 0.1341(16) Uani 1 1 d . . . . .
N005 N 0.0856(6) 0.73485(14) 0.6437(5) 0.066(2) Uani 1 1 d . . . . .
C1 C -0.0471(7) 0.73275(16) 0.6322(5) 0.074(3) Uani 1 1 d G . . . .
H1 H -0.097962 0.745071 0.591378 0.089 Uiso 1 1 calc R . . . .
C2 C -0.0939(6) 0.70983(18) 0.6899(5) 0.076(3) Uani 1 1 d G . . . .
H2 H -0.183145 0.703368 0.696128 0.091 Uiso 1 1 calc R . . . .
N008 N 0.0098(6) 0.69782(16) 0.7368(5) 0.069(2) Uani 1 1 d G . . . .
C3 C 0.1208(6) 0.71331(15) 0.7083(5) 0.065(3) Uani 1 1 d G . . . .
N006 N 0.2958(7) 0.71614(16) 0.8189(4) 0.070(2) Uani 1 1 d . . . . .
C4 C 0.4266(8) 0.7107(2) 0.8210(5) 0.086(4) Uani 1 1 d G . . . .
H4 H 0.482460 0.713472 0.870782 0.103 Uiso 1 1 calc R . . . .
C5 C 0.4642(7) 0.7006(2) 0.7399(5) 0.090(4) Uani 1 1 d G . . . .
H5 H 0.551123 0.695044 0.722515 0.108 Uiso 1 1 calc R . . . .
N007 N 0.3566(7) 0.69978(17) 0.6878(5) 0.070(2) Uani 1 1 d G . . . .
C6 C 0.2526(6) 0.70944(17) 0.7367(5) 0.068(3) Uani 1 1 d G . . . .
O1 O 0.4259(8) 0.53272(18) 0.5441(8) 0.117(4) Uani 1 1 d . . . . .
O2 O 0.6301(8) 0.54742(17) 0.5532(8) 0.115(4) Uani 1 1 d . . . . .
C7 C 0.3508(11) 0.6895(2) 0.5934(8) 0.074(3) Uani 1 1 d . . . . .
H7A H 0.406994 0.704205 0.557522 0.088 Uiso 1 1 calc R . . . .
H7B H 0.259343 0.691554 0.571643 0.088 Uiso 1 1 calc R . . . .
O3 O 0.1507(9) 0.5270(2) 0.6303(8) 0.117(4) Uani 1 1 d D . . A 1
C8 C 0.3970(7) 0.65439(12) 0.5826(6) 0.071(3) Uani 1 1 d . . . . .
C9 C 0.3021(5) 0.63027(17) 0.5709(7) 0.115(6) Uani 1 1 d G . . . .
H9 H 0.211731 0.636065 0.568518 0.138 Uiso 1 1 calc R . . . .
C10 C 0.3395(6) 0.59765(15) 0.5628(7) 0.114(6) Uani 1 1 d G . . . .
H10 H 0.274667 0.581161 0.554806 0.136 Uiso 1 1 calc R . . . .
C11 C 0.4718(7) 0.58917(12) 0.5663(7) 0.074(3) Uani 1 1 d G . . . .
C12 C 0.5666(5) 0.61330(17) 0.5779(7) 0.104(5) Uani 1 1 d G . . . .
H12 H 0.657006 0.607496 0.580336 0.125 Uiso 1 1 calc R . . . .
C13 C 0.5292(6) 0.64591(14) 0.5861(7) 0.116(6) Uani 1 1 d G . . . .
H13 H 0.594072 0.662400 0.594047 0.139 Uiso 1 1 calc R . . . .
C14 C 0.0063(12) 0.6725(3) 0.8050(8) 0.079(3) Uani 1 1 d . . . . .
H14A H -0.085746 0.669175 0.824325 0.095 Uiso 0.5 1 calc R . . B 1
H14B H 0.057667 0.679933 0.856846 0.095 Uiso 0.5 1 calc R . . B 1
H14C H -0.054831 0.679649 0.852140 0.095 Uiso 0.5 1 calc R . . C 2
H14D H 0.094932 0.670784 0.831645 0.095 Uiso 0.5 1 calc R . . C 2
C15 C 0.5124(11) 0.5540(2) 0.5540(9) 0.075(3) Uani 1 1 d . . . . .
O4 O 0.2912(17) 0.5322(4) 0.7359(14) 0.116(7) Uani 0.5 1 d D . . A 1
C16 C 0.1962(19) 0.5453(4) 0.6927(13) 0.093(8) Uani 0.5 1 d D . . A 1
C17 C 0.0618(14) 0.6401(2) 0.7723(10) 0.065(5) Uani 0.5 1 d . . . A 1
C18 C -0.0014(12) 0.6234(3) 0.7044(10) 0.068(7) Uani 0.5 1 d G U . A 1
H18 H -0.074308 0.633126 0.675116 0.082 Uiso 0.5 1 calc R . . A 1
C19 C 0.0419(15) 0.5925(3) 0.6793(9) 0.073(6) Uani 0.5 1 d G U . A 1
H19 H -0.001346 0.581056 0.632911 0.088 Uiso 0.5 1 calc R . . A 1
C20 C 0.1485(16) 0.5782(3) 0.7221(11) 0.079(6) Uani 0.5 1 d DG U . A 1
C21 C 0.2118(15) 0.5949(3) 0.7900(11) 0.102(8) Uani 0.5 1 d G U . A 1
H21 H 0.284651 0.585216 0.819246 0.122 Uiso 0.5 1 calc R . . A 1
C22 C 0.1684(15) 0.6259(3) 0.8151(9) 0.099(9) Uani 0.5 1 d G . . A 1
H22 H 0.211690 0.637286 0.861453 0.118 Uiso 0.5 1 calc R . . A 1
C23 C -0.019(2) 0.6275(5) 0.6874(15) 0.128(16) Uani 0.5 1 d . U . A 2
H23 H 0.026008 0.640811 0.645754 0.153 Uiso 0.5 1 calc R . . A 2
C24 C -0.036(2) 0.6383(4) 0.7738(16) 0.092(7) Uani 0.5 1 d G U . A 2
C25 C -0.102(3) 0.6187(6) 0.8348(13) 0.191(19) Uani 0.5 1 d G U . A 2
H25 H -0.113004 0.626128 0.893840 0.229 Uiso 0.5 1 calc R . . A 2
C26 C -0.150(3) 0.5884(5) 0.8093(16) 0.25(3) Uani 0.5 1 d G U . A 2
H26 H -0.195401 0.575023 0.850898 0.298 Uiso 0.5 1 calc R . . A 2
C27 C -0.134(2) 0.5776(4) 0.7228(18) 0.103(8) Uani 0.5 1 d DG U . A 2
C28 C -0.068(2) 0.5971(5) 0.6619(13) 0.119(10) Uani 0.5 1 d G U . A 2
H28 H -0.056391 0.589705 0.602811 0.142 Uiso 0.5 1 calc R . . A 2
O5 O 0.3681(9) 0.5222(3) 0.3628(7) 0.123(4) Uani 1 1 d D . . D 2
O6 O -0.269(2) 0.5326(5) 0.7453(14) 0.121(7) Uani 0.5 1 d D U . A 2
C29 C -0.175(2) 0.5436(4) 0.6944(16) 0.108(9) Uani 0.5 1 d D U . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.348(9) . ?
Eu1 O1 2.348(9) 2_565 ?
Eu1 O2 2.406(8) 5_666 ?
Eu1 O2 2.406(8) 6_556 ?
Eu1 O3 2.522(10) . ?
Eu1 O3 2.522(10) 2_565 ?
Eu1 O5 2.514(10) 2_565 ?
Eu1 O5 2.514(10) . ?
Pd1 Cl2 2.274(3) . ?
Pd1 Cl1 2.253(4) . ?
Pd1 N005 2.026(6) 4_566 ?
Pd1 N006 2.053(6) . ?
N005 C1 1.363(5) . ?
N005 C3 1.363(5) . ?
C1 C2 1.364(5) . ?
C2 N008 1.363(5) . ?
N008 C3 1.363(5) . ?
N008 C14 1.460(13) . ?
C3 C6 1.416(9) . ?
N006 C4 1.349(5) . ?
N006 C6 1.347(5) . ?
C4 C5 1.349(5) . ?
C5 N007 1.349(5) . ?
N007 C6 1.349(5) . ?
N007 C7 1.487(12) . ?
O1 C15 1.244(12) . ?
O2 C15 1.227(12) . ?
C7 C8 1.519(10) . ?
O3 C16 1.289(9) . ?
C8 C9 1.3900 . ?
C8 C13 1.3900 . ?
C9 C10 1.3900 . ?
C10 C11 1.3900 . ?
C11 C12 1.3900 . ?
C11 C15 1.506(11) . ?
C12 C13 1.3900 . ?
C14 C17 1.521(14) . ?
C14 C24 1.535(17) . ?
O4 C16 1.284(9) . ?
C16 C20 1.496(9) . ?
C17 C18 1.3900 . ?
C17 C22 1.3900 . ?
C18 C19 1.3900 . ?
C19 C20 1.3900 . ?
C20 C21 1.3900 . ?
C21 C22 1.3900 . ?
C23 C24 1.3900 . ?
C23 C28 1.3900 . ?
C24 C25 1.3900 . ?
C25 C26 1.3900 . ?
C26 C27 1.3900 . ?
C27 C28 1.3900 . ?
C27 C29 1.513(10) . ?
O5 C29 1.305(9) 6_656 ?
O6 C29 1.300(10) . ?

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 Eu1 O1 143.9(6) . 2_565 ?
O1 Eu1 O2 91.4(3) . 6_556 ?
O1 Eu1 O2 99.6(3) . 5_666 ?
O1 Eu1 O2 99.6(3) 2_565 6_556 ?
O1 Eu1 O2 91.4(3) 2_565 5_666 ?
O1 Eu1 O3 72.2(3) 2_565 . ?
O1 Eu1 O3 78.9(3) . . ?
O1 Eu1 O3 72.2(3) . 2_565 ?
O1 Eu1 O3 78.9(3) 2_565 2_565 ?
O1 Eu1 O5 144.8(4) 2_565 . ?
O1 Eu1 O5 144.8(4) . 2_565 ?
O1 Eu1 O5 71.2(4) . . ?
O1 Eu1 O5 71.2(4) 2_565 2_565 ?
O2 Eu1 O2 144.0(6) 5_666 6_556 ?
O2 Eu1 O3 72.2(4) 6_556 . ?
O2 Eu1 O3 72.2(4) 5_666 2_565 ?
O2 Eu1 O3 143.5(4) 5_666 . ?
O2 Eu1 O3 143.5(4) 6_556 2_565 ?
O2 Eu1 O5 72.8(3) 5_666 2_565 ?
O2 Eu1 O5 78.5(4) 5_666 . ?
O2 Eu1 O5 78.5(4) 6_556 2_565 ?
O2 Eu1 O5 72.8(3) 6_556 . ?
O3 Eu1 O3 72.8(5) 2_565 . ?
O5 Eu1 O5 73.6(5) 2_565 . ?
Cl1 Pd1 Cl2 88.77(15) . . ?
N005 Pd1 Cl2 88.2(2) 4_566 . ?
N005 Pd1 Cl1 173.3(2) 4_566 . ?
N005 Pd1 N006 94.0(3) 4_566 . ?
N006 Pd1 Cl2 170.7(2) . . ?
N006 Pd1 Cl1 89.9(2) . . ?
C1 N005 Pd1 122.9(4) . 4_566 ?
C3 N005 Pd1 129.0(4) . 4_566 ?
C3 N005 C1 108.1 . . ?
N005 C1 C2 107.9 . . ?
N008 C2 C1 108.0 . . ?
C2 N008 C3 108.0 . . ?
C2 N008 C14 127.1(7) . . ?
C3 N008 C14 124.9(7) . . ?
N005 C3 N008 108.0 . . ?
N005 C3 C6 122.5(6) . . ?
N008 C3 C6 129.5(6) . . ?
C4 N006 Pd1 120.4(4) . . ?
C6 N006 Pd1 131.4(4) . . ?
C6 N006 C4 108.0 . . ?
C5 C4 N006 108.0 . . ?
C4 C5 N007 108.0 . . ?
C5 N007 C6 108.0 . . ?
C5 N007 C7 126.8(7) . . ?
C6 N007 C7 125.2(7) . . ?
N006 C6 C3 124.4(6) . . ?
N006 C6 N007 108.0 . . ?
N007 C6 C3 127.5(6) . . ?
C15 O1 Eu1 166.5(10) . . ?
C15 O2 Eu1 132.3(7) . 5_666 ?
N007 C7 C8 110.9(8) . . ?
C16 O3 Eu1 134.4(12) . . ?
C9 C8 C7 117.9(6) . . ?
C9 C8 C13 120.0 . . ?
C13 C8 C7 122.1(6) . . ?
C8 C9 C10 120.0 . . ?
C11 C10 C9 120.0 . . ?
C10 C11 C12 120.0 . . ?
C10 C11 C15 119.9(6) . . ?
C12 C11 C15 120.1(6) . . ?
C13 C12 C11 120.0 . . ?
C12 C13 C8 120.0 . . ?
N008 C14 C17 112.1(10) . . ?
N008 C14 C24 115.8(13) . . ?
O1 C15 C11 119.1(9) . . ?
O2 C15 O1 122.4(10) . . ?
O2 C15 C11 118.5(9) . . ?
O3 C16 C20 128.4(13) . . ?
O4 C16 O3 113.6(13) . . ?
O4 C16 C20 117.9(14) . . ?
C18 C17 C14 119.7(11) . . ?
C18 C17 C22 120.0 . . ?
C22 C17 C14 120.1(11) . . ?
C19 C18 C17 120.0 . . ?
C18 C19 C20 120.0 . . ?
C19 C20 C16 119.3(11) . . ?
C19 C20 C21 120.0 . . ?
C21 C20 C16 120.7(11) . . ?
C22 C21 C20 120.0 . . ?
C21 C22 C17 120.0 . . ?
C24 C23 C28 120.0 . . ?
C23 C24 C14 122.9(17) . . ?
C25 C24 C14 116.9(17) . . ?
C25 C24 C23 120.0 . . ?
C24 C25 C26 120.0 . . ?
C27 C26 C25 120.0 . . ?
C26 C27 C29 122(2) . . ?
C28 C27 C26 120.0 . . ?
C28 C27 C29 118.2(19) . . ?
C27 C28 C23 120.0 . . ?
C29 O5 Eu1 127.5(14) 6_656 . ?
O5 C29 C27 134.8(19) 6_556 . ?
O6 C29 C27 110.7(17) . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1 -12 9 0.0381 0.9944 -11.9866 9.0018 0.1386 0.3851 -0.9497
-1 -26 2 0.0299 -1.0039 -25.9925 2.0226 0.2235 0.9647 -0.2203
-1 -1 -10 0.0230 -0.9951 -1.0127 -9.9904 0.0809 0.0588 1.0246
1 26 0 0.0377 1.0029 25.9953 -0.0239 -0.2636 -0.9572 0.0208
6 -4 -4 0.0509 6.0043 -4.0088 -4.0082 0.9531 -0.2488 0.2180
6 -5 3 0.0550 6.0004 -4.9991 2.9881 0.8279 -0.1880 -0.4822
4 -3 8 0.0462 3.9971 -2.9913 7.9879 0.4263 -0.1143 -0.9194
0 0 10 0.0334 -0.0054 0.0136 9.9936 -0.2008 0.0375 -0.9977
-6 7 3 0.0396 -6.0035 7.0070 3.0064 -0.9790 0.1417 -0.1125
-2 -25 1 0.0230 -2.0037 -24.9934 1.0247 0.0930 0.9884 -0.0897
4 5 -8 0.0406 4.0065 4.9857 -8.0084 0.6249 -0.4498 0.6921
-6 -6 5 0.0384 -6.0058 -5.9883 5.0158 -0.8198 0.5968 -0.3369
-1 1 -10 0.0180 -0.9949 0.9869 -9.9920 0.0502 -0.0101 1.0285
-6 -5 -2 0.0363 -6.0019 -4.9979 -1.9805 -0.6945 0.5361 0.3634
-4 17 4 0.0370 -4.0023 17.0054 3.9928 -0.8820 -0.3227 -0.2510
5 -17 -1 0.0476 5.0011 -17.0020 -0.9970 0.9570 0.2720 -0.0772
3 -14 -7 0.0414 3.0037 -14.0093 -6.9910 0.7610 0.2700 0.5849


_ins_header                      
;
TITL SY-3 in Pnna 
REM Pnna (#52, found as Pnan in a-cb setting)
CELL 1.54184  10.170935  40.819757  15.118875  90.0000  90.0000  90.0000
ZERR    4.00   0.000718   0.002252   0.001224   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z 
SYMM -x+1/2, y+1/2,-z+1/2 
SYMM  x,-y+1/2,-z+1/2 
SFAC C N O Pd Pr
UNIT 4.00 4.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_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_3_sq
_database_code_depnum_ccdc_archive 'CCDC 1524465'
_audit_update_record             
;
2018-05-29 deposited with the CCDC.
2018-05-31 downloaded from the CCDC.
;
_audit_creation_date             2018-05-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C176 H128 Cl16 N32 O40 Pd8 Tb4)'
_chemical_formula_sum            'C44 H46 Cl4 N8 O14.50 Pd2 Tb'
_chemical_formula_weight         1432.41
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Sm1 C1 N1 O1 Pd1 H1 Cl1'
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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 '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           52
_space_group_name_H-M_alt        'P n n a'
_space_group_name_Hall           '-P 2a 2bc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x, y-1/2, z-1/2'

_cell_length_a                   10.1189(4)
_cell_length_b                   40.7335(17)
_cell_length_c                   15.0742(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6213.3(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4095
_cell_measurement_temperature    102.23(10)
_cell_measurement_theta_max      71.9550
_cell_measurement_theta_min      4.3200
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    12.221
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2828
_exptl_crystal_size_max          0.0994
_exptl_crystal_size_mid          0.0634
_exptl_crystal_size_min          0.0616
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_av_unetI/netI     0.0670
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24751
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.922
_diffrn_reflns_theta_min         5.265
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      102.23(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   16.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5548   43.0000  177.0000 99

#__ type_ start__ end____ width___ exp.time_
  2 omega   95.00  178.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816   79.0000   -4.0000 83

#__ type_ start__ end____ width___ exp.time_
  3 omega   37.00   97.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -43.0000   25.0000 60

#__ type_ start__ end____ width___ exp.time_
  4 omega   78.00  172.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  150.0000   42.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega  -50.00   33.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5548   38.0000  -60.0000 83

#__ type_ start__ end____ width___ exp.time_
  6 omega  -50.00   33.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.5548   38.0000 -150.0000 83

#__ type_ start__ end____ width___ exp.time_
  7 omega   36.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       41.5548 -150.0000   -2.0000 78

#__ type_ start__ end____ width___ exp.time_
  8 omega   37.00   98.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -45.0000 -180.0000 61

#__ type_ start__ end____ width___ exp.time_
  9 omega   47.00   74.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -30.0000  -30.0000 27

#__ type_ start__ end____ width___ exp.time_
 10 omega   38.00  109.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      110.3816  -94.0000   60.0000 71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0162534000
_diffrn_orient_matrix_UB_12      -0.0127654000
_diffrn_orient_matrix_UB_13      0.0956715000
_diffrn_orient_matrix_UB_21      0.0800770000
_diffrn_orient_matrix_UB_22      0.0294608000
_diffrn_orient_matrix_UB_23      0.0348029000
_diffrn_orient_matrix_UB_31      -0.1284289000
_diffrn_orient_matrix_UB_32      0.0199519000
_diffrn_orient_matrix_UB_33      0.0097072000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3151
_reflns_number_total             6261
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.466
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6261
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.0987
_refine_ls_restrained_S_all      1.042
_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)+50.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.2050
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Restrained distances
 C26-O2
 1.36 with sigma of 0.01
 O1-C26
 1.36 with sigma of 0.01
 C24-C26
 1.5 with sigma of 0.01
 C23-O4
 1.36 with sigma of 0.01
 O3-C23
 1.36 with sigma of 0.01
 O4-C18
 2.8 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C19 \\sim C16 \\sim C28 \\sim C25: within 0.01A with sigma of 3.8 and sigma for
terminal atoms of 0.01
C27 \\sim C14B \\sim C12: within 0.01A with sigma of 3.8 and sigma for terminal
atoms of 0.01
Uanis(C25) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C28)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C24) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C20)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C14A) \\sim Ueq, Uanis(C14B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(C14B)=Sof(H14B)=1-FVAR(1)
 Sof(C14A)=Sof(H14A)=FVAR(1)
 Fixed Sof: H3BC(0.5) H3BD(0.5) H3AA(0.5) H3AB(0.5) C27(0.5) H27(0.5) C24(0.5)
 C28(0.5) H28(0.5) C25(0.5) H25(0.5) C19(0.5) O4(0.5) C23(0.5) O1(0.5) C26(0.5)
 C22(0.5) H22(0.5) C21(0.5) C18(0.5) H18(0.5) C20(0.5) H20(0.5) C17(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3BC,H3BD), C3(H3AA,H3AB), C7(H7A,H7B)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C11(H11), C12(H12), C14B(H14B), C27(H27), C28(H28), C25(H25),
 C16(H16), C6(H6), C13(H13), C15(H15), C14A(H14A), C22(H22), C18(H18), C20(H20)
5.c Fitted hexagon refined as free rotating group:
 C14B(C27,C24,C28,C25,C19), C16(C8,C6,C13,C9,C15), C14A(C22,C21,C18,C20,C17)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.79747(11) 0.26542(2) 0.42818(7) 0.1006(4) Uani 1 1 d . . . . .
Tb1 Tb 0.250000 0.500000 0.00423(9) 0.1017(4) Uani 1 2 d S T P . .
Cl2 Cl 0.8726(4) 0.23983(9) 0.5530(2) 0.1117(11) Uani 1 1 d . . . . .
Cl1 Cl 0.6934(6) 0.30188(11) 0.5137(4) 0.166(2) Uani 1 1 d . . . . .
N3 N 0.7032(11) 0.2843(2) 0.3202(8) 0.097(3) Uani 1 1 d . . . . .
N4 N 0.6421(11) 0.3007(2) 0.1884(8) 0.098(3) Uani 1 1 d . . . . .
N1 N 0.9164(11) 0.2651(2) 0.1438(7) 0.090(3) Uani 1 1 d . . . . .
O5 O 0.5804(9) 0.4672(2) 0.0396(9) 0.134(4) Uani 1 1 d . . . . .
C1 C 0.8816(13) 0.2872(3) 0.2069(9) 0.090(3) Uani 1 1 d . . . . .
O6 O 0.3726(10) 0.4543(2) 0.0520(8) 0.135(4) Uani 1 1 d . . . . .
C2 C 0.4896(13) 0.4478(3) 0.0511(10) 0.094(4) Uani 1 1 d . . . . .
O3 O 0.8477(9) 0.4730(3) 0.1255(8) 0.133(4) Uani 1 1 d D . . . .
N2 N 0.9882(11) 0.3024(2) 0.2352(8) 0.092(3) Uani 1 1 d . . . . .
C3 C 0.9907(14) 0.3279(3) 0.3034(10) 0.105(4) Uani 1 1 d . . . . .
H3BC H 1.045068 0.319997 0.353568 0.126 Uiso 0.5 1 calc R . . A 2
H3BD H 0.899537 0.331041 0.325766 0.126 Uiso 0.5 1 calc R . . A 2
H3AA H 1.083092 0.331177 0.323086 0.126 Uiso 0.5 1 calc R . . B 1
H3AB H 0.939087 0.320288 0.355211 0.126 Uiso 0.5 1 calc R . . B 1
C4 C 0.5713(16) 0.2894(4) 0.3249(13) 0.128(6) Uani 1 1 d . . . . .
H4 H 0.516101 0.286574 0.375299 0.154 Uiso 1 1 calc R . . . .
C5 C 1.0920(13) 0.2899(3) 0.1904(10) 0.103(4) Uani 1 1 d . . . . .
H5 H 1.181666 0.296204 0.197860 0.124 Uiso 1 1 calc R . . . .
C7 C 0.6472(14) 0.3114(3) 0.0939(10) 0.107(4) Uani 1 1 d . . . . .
H7A H 0.589719 0.296995 0.057578 0.128 Uiso 1 1 calc R . . . .
H7B H 0.738718 0.309417 0.071360 0.128 Uiso 1 1 calc R . . . .
C10 C 0.7466(15) 0.2913(3) 0.2373(10) 0.101(4) Uani 1 1 d . . . . .
C11 C 0.5346(16) 0.2994(4) 0.2438(13) 0.133(6) Uani 1 1 d . . . . .
H11 H 0.446655 0.304722 0.227038 0.160 Uiso 1 1 calc R . . . .
C12 C 1.0487(13) 0.2672(3) 0.1341(9) 0.091(3) Uani 1 1 d . U . . .
H12 H 1.101279 0.254716 0.094217 0.109 Uiso 1 1 calc R . . . .
C14B C 1.025(3) 0.3718(5) 0.1885(15) 0.06(2) Uani 0.19(6) 1 d . U . C 2
H14B H 0.982049 0.358249 0.146119 0.073 Uiso 0.19(6) 1 calc R . . C 2
C27 C 1.070(3) 0.4028(5) 0.1642(13) 0.125(11) Uani 0.5 1 d G U . C 2
H27 H 1.057759 0.410376 0.105216 0.151 Uiso 0.5 1 calc R . . C 2
C24 C 1.133(2) 0.4226(4) 0.2262(17) 0.120(9) Uani 0.5 1 d DG U . C 2
C28 C 1.151(3) 0.4115(6) 0.3126(16) 0.29(3) Uani 0.5 1 d G U . C 2
H28 H 1.193914 0.425012 0.354962 0.344 Uiso 0.5 1 calc R . . C 2
C25 C 1.106(3) 0.3805(7) 0.3369(13) 0.197(18) Uani 0.5 1 d G U . C 2
H25 H 1.118204 0.372885 0.395866 0.237 Uiso 0.5 1 calc R . . C 2
C19 C 1.043(2) 0.3607(5) 0.2748(17) 0.110(9) Uani 0.5 1 d G U . C 2
C16 C 0.6602(8) 0.4031(2) 0.0660(7) 0.135(5) Uani 1 1 d . U . . .
H16 H 0.725636 0.419556 0.058175 0.162 Uiso 1 1 calc R . . . .
C8 C 0.5273(10) 0.41169(15) 0.0686(7) 0.095(4) Uani 1 1 d G . . . .
C6 C 0.4315(7) 0.3876(2) 0.0800(8) 0.128(6) Uani 1 1 d G . . . .
H6 H 0.340713 0.393469 0.081788 0.153 Uiso 1 1 calc R . . . .
C13 C 0.4686(8) 0.35490(18) 0.0889(8) 0.141(7) Uani 1 1 d G . . . .
H13 H 0.403183 0.338434 0.096700 0.170 Uiso 1 1 calc R . . . .
C9 C 0.6015(10) 0.34630(16) 0.0863(7) 0.100(4) Uani 1 1 d G . . . .
C15 C 0.6973(7) 0.3704(2) 0.0749(8) 0.142(7) Uani 1 1 d G . . . .
H15 H 0.788107 0.364520 0.073088 0.171 Uiso 1 1 calc R . . . .
O4 O 0.702(2) 0.4679(4) 0.2373(16) 0.148(8) Uani 0.5 1 d D . . C 1
C23 C 0.797(3) 0.4533(6) 0.1893(16) 0.126(10) Uani 0.5 1 d D U . C 1
O2 O 1.1322(11) 0.4774(3) 0.1351(8) 0.146(4) Uani 1 1 d D . . . .
O1 O 1.282(3) 0.4642(7) 0.2488(19) 0.197(12) Uani 0.5 1 d D U . C 2
C26 C 1.183(3) 0.4551(6) 0.193(2) 0.182(17) Uani 0.5 1 d D U . C 2
C14A C 1.0023(14) 0.3770(4) 0.2063(12) 0.152(10) Uani 0.81(6) 1 d . U . C 1
H14A H 1.077799 0.367414 0.179135 0.182 Uiso 0.81(6) 1 calc R . . C 1
C22 C 0.9578(18) 0.4076(4) 0.1790(12) 0.114(10) Uani 0.5 1 d G . . C 1
H22 H 1.002985 0.419033 0.133107 0.137 Uiso 0.5 1 calc R . . C 1
C21 C 0.847(2) 0.4216(3) 0.2187(13) 0.106(8) Uani 0.5 1 d G U . C 1
C18 C 0.7813(17) 0.4049(4) 0.2858(13) 0.144(12) Uani 0.5 1 d DG U . C 1
H18 H 0.705778 0.414409 0.312917 0.173 Uiso 0.5 1 calc R . . C 1
C20 C 0.8257(18) 0.3742(4) 0.3131(11) 0.130(10) Uani 0.5 1 d G U . C 1
H20 H 0.780590 0.362790 0.358946 0.156 Uiso 0.5 1 calc R . . C 1
C17 C 0.9362(16) 0.3602(3) 0.2734(12) 0.086(6) Uani 0.5 1 d G . . C 1


_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 2.281(4) . ?
Pd1 Cl1 2.231(5) . ?
Pd1 N3 2.038(11) . ?
Pd1 N1 2.042(10) 4 ?
Tb1 O5 2.273(9) 5_665 ?
Tb1 O5 2.273(9) 6 ?
Tb1 O6 2.348(8) 2_565 ?
Tb1 O6 2.348(8) . ?
Tb1 O3 2.452(11) 6 ?
Tb1 O3 2.452(11) 5_665 ?
Tb1 O2 2.481(12) 2_665 ?
Tb1 O2 2.481(12) 1_455 ?
N3 C4 1.352(16) . ?
N3 C10 1.356(17) . ?
N4 C7 1.490(16) . ?
N4 C10 1.344(16) . ?
N4 C11 1.373(17) . ?
N1 C1 1.356(15) . ?
N1 C12 1.349(15) . ?
O5 C2 1.223(14) . ?
C1 N2 1.316(14) . ?
C1 C10 1.451(18) . ?
O6 C2 1.214(14) . ?
C2 C8 1.544(12) . ?
O3 C23 1.352(10) . ?
N2 C3 1.462(16) . ?
N2 C5 1.350(15) . ?
C3 C19 1.497(19) . ?
C3 C17 1.496(17) . ?
C4 C11 1.34(2) . ?
C5 C12 1.329(17) . ?
C7 C9 1.501(14) . ?
C14B C27 1.3900 . ?
C14B C19 1.3900 . ?
C27 C24 1.3900 . ?
C24 C28 1.3900 . ?
C24 C26 1.504(10) . ?
C28 C25 1.3900 . ?
C25 C19 1.3900 . ?
C16 C8 1.3900 . ?
C16 C15 1.3900 . ?
C8 C6 1.3900 . ?
C6 C13 1.3900 . ?
C13 C9 1.3900 . ?
C9 C15 1.3900 . ?
O4 C23 1.347(10) . ?
C23 C21 1.46(2) . ?
O2 C26 1.362(10) . ?
O1 C26 1.358(10) . ?
C14A C22 1.3900 . ?
C14A C17 1.3900 . ?
C22 C21 1.3900 . ?
C21 C18 1.3900 . ?
C18 C20 1.3900 . ?
C20 C17 1.3900 . ?

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 Cl2 89.14(18) . . ?
N3 Pd1 Cl2 170.9(3) . . ?
N3 Pd1 Cl1 89.4(4) . . ?
N3 Pd1 N1 94.6(4) . 4 ?
N1 Pd1 Cl2 87.9(3) 4 . ?
N1 Pd1 Cl1 172.1(4) 4 . ?
O5 Tb1 O5 146.2(6) 6 5_665 ?
O5 Tb1 O6 99.0(4) 6 2_565 ?
O5 Tb1 O6 91.3(4) 5_665 2_565 ?
O5 Tb1 O6 91.3(4) 6 . ?
O5 Tb1 O6 99.0(4) 5_665 . ?
O5 Tb1 O3 79.0(4) 6 6 ?
O5 Tb1 O3 74.2(4) 5_665 6 ?
O5 Tb1 O3 79.0(4) 5_665 5_665 ?
O5 Tb1 O3 74.2(4) 6 5_665 ?
O5 Tb1 O2 69.6(4) 5_665 2_665 ?
O5 Tb1 O2 69.6(4) 6 1_455 ?
O5 Tb1 O2 144.3(4) 5_665 1_455 ?
O5 Tb1 O2 144.3(4) 6 2_665 ?
O6 Tb1 O6 144.3(6) 2_565 . ?
O6 Tb1 O3 144.4(4) 2_565 6 ?
O6 Tb1 O3 71.1(4) 2_565 5_665 ?
O6 Tb1 O3 144.4(4) . 5_665 ?
O6 Tb1 O3 71.1(4) . 6 ?
O6 Tb1 O2 78.2(4) 2_565 1_455 ?
O6 Tb1 O2 73.6(4) 2_565 2_665 ?
O6 Tb1 O2 78.2(4) . 2_665 ?
O6 Tb1 O2 73.6(4) . 1_455 ?
O3 Tb1 O3 74.2(5) 6 5_665 ?
O3 Tb1 O2 131.4(4) 6 1_455 ?
O3 Tb1 O2 127.3(4) 6 2_665 ?
O3 Tb1 O2 131.4(4) 5_665 2_665 ?
O3 Tb1 O2 127.3(4) 5_665 1_455 ?
O2 Tb1 O2 74.7(6) 2_665 1_455 ?
C4 N3 Pd1 118.6(11) . . ?
C4 N3 C10 109.6(13) . . ?
C10 N3 Pd1 131.6(10) . . ?
C10 N4 C7 125.4(13) . . ?
C10 N4 C11 106.2(14) . . ?
C11 N4 C7 128.3(13) . . ?
C1 N1 Pd1 128.6(9) . 4 ?
C12 N1 Pd1 124.5(9) . 4 ?
C12 N1 C1 106.9(10) . . ?
C2 O5 Tb1 170.8(12) . 5_665 ?
N1 C1 C10 122.9(12) . . ?
N2 C1 N1 109.2(11) . . ?
N2 C1 C10 127.9(13) . . ?
C2 O6 Tb1 133.2(9) . . ?
O5 C2 C8 117.0(11) . . ?
O6 C2 O5 126.4(11) . . ?
O6 C2 C8 116.6(11) . . ?
C23 O3 Tb1 132.9(15) . 5_665 ?
C1 N2 C3 125.3(12) . . ?
C1 N2 C5 107.2(12) . . ?
C5 N2 C3 127.5(12) . . ?
N2 C3 C19 115.9(15) . . ?
N2 C3 C17 114.0(13) . . ?
C11 C4 N3 105.8(15) . . ?
C12 C5 N2 109.1(13) . . ?
N4 C7 C9 109.8(11) . . ?
N3 C10 C1 124.9(13) . . ?
N4 C10 N3 108.0(13) . . ?
N4 C10 C1 126.9(14) . . ?
C4 C11 N4 110.3(15) . . ?
C5 C12 N1 107.6(12) . . ?
C27 C14B C19 120.0 . . ?
C24 C27 C14B 120.0 . . ?
C27 C24 C28 120.0 . . ?
C27 C24 C26 116(2) . . ?
C28 C24 C26 124(2) . . ?
C24 C28 C25 120.0 . . ?
C19 C25 C28 120.0 . . ?
C14B C19 C3 120.9(18) . . ?
C25 C19 C3 119.1(18) . . ?
C25 C19 C14B 120.0 . . ?
C8 C16 C15 120.0 . . ?
C16 C8 C2 118.3(8) . . ?
C16 C8 C6 120.0 . . ?
C6 C8 C2 121.5(8) . . ?
C13 C6 C8 120.0 . . ?
C6 C13 C9 120.0 . . ?
C13 C9 C7 122.3(8) . . ?
C15 C9 C7 117.7(8) . . ?
C15 C9 C13 120.0 . . ?
C9 C15 C16 120.0 . . ?
O3 C23 C21 128(2) . . ?
O4 C23 O3 113(2) . . ?
O4 C23 C21 118.6(17) . . ?
O2 C26 C24 132(2) . . ?
O1 C26 C24 106(2) . . ?
O1 C26 O2 119(2) . . ?
C22 C14A C17 120.0 . . ?
C21 C22 C14A 120.0 . . ?
C22 C21 C23 120.7(15) . . ?
C18 C21 C23 119.3(15) . . ?
C18 C21 C22 120.0 . . ?
C21 C18 C20 120.0 . . ?
C18 C20 C17 120.0 . . ?
C14A C17 C3 118.3(13) . . ?
C20 C17 C3 121.7(13) . . ?
C20 C17 C14A 120.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Pd1 N3 C4 C11 -175.4(11) . . . . ?
Pd1 N3 C10 N4 174.8(8) . . . . ?
Pd1 N3 C10 C1 -2(2) . . . . ?
Pd1 N1 C1 N2 -178.3(8) 4 . . . ?
Pd1 N1 C1 C10 3.5(18) 4 . . . ?
Pd1 N1 C12 C5 178.8(8) 4 . . . ?
Tb1 O6 C2 O5 16(3) . . . . ?
Tb1 O6 C2 C8 -165.8(9) . . . . ?
Tb1 O3 C23 O4 -61(3) 5_665 . . . ?
Tb1 O3 C23 C21 129(2) 5_665 . . . ?
Tb1 O2 C26 C24 -127(4) 1_655 . . . ?
Tb1 O2 C26 O1 70(5) 1_655 . . . ?
N3 C4 C11 N4 0(2) . . . . ?
N4 C7 C9 C13 -77.8(12) . . . . ?
N4 C7 C9 C15 103.2(11) . . . . ?
N1 C1 N2 C3 -179.9(11) . . . . ?
N1 C1 N2 C5 -0.4(14) . . . . ?
N1 C1 C10 N3 113.9(15) . . . . ?
N1 C1 C10 N4 -61.8(19) . . . . ?
O5 C2 C8 C16 -3.1(17) . . . . ?
O5 C2 C8 C6 -178.3(11) . . . . ?
C1 N1 C12 C5 0.4(14) . . . . ?
C1 N2 C3 C19 -119.8(17) . . . . ?
C1 N2 C3 C17 -72.9(17) . . . . ?
C1 N2 C5 C12 0.6(15) . . . . ?
O6 C2 C8 C16 178.5(11) . . . . ?
O6 C2 C8 C6 3.4(18) . . . . ?
C2 C8 C6 C13 175.0(10) . . . . ?
O3 C23 C21 C22 -2(4) . . . . ?
O3 C23 C21 C18 -180(2) . . . . ?
N2 C1 C10 N3 -63.9(19) . . . . ?
N2 C1 C10 N4 120.4(16) . . . . ?
N2 C3 C19 C14B 32(2) . . . . ?
N2 C3 C19 C25 -150.1(15) . . . . ?
N2 C3 C17 C14A -64.4(16) . . . . ?
N2 C3 C17 C20 118.1(13) . . . . ?
N2 C5 C12 N1 -0.6(15) . . . . ?
C3 N2 C5 C12 -179.9(12) . . . . ?
C4 N3 C10 N4 -0.6(16) . . . . ?
C4 N3 C10 C1 -177.0(13) . . . . ?
C5 N2 C3 C19 61(2) . . . . ?
C5 N2 C3 C17 107.8(16) . . . . ?
C7 N4 C10 N3 178.5(11) . . . . ?
C7 N4 C10 C1 -5(2) . . . . ?
C7 N4 C11 C4 -178.1(14) . . . . ?
C7 C9 C15 C16 179.0(10) . . . . ?
C10 N3 C4 C11 0.6(19) . . . . ?
C10 N4 C7 C9 -117.8(13) . . . . ?
C10 N4 C11 C4 0.1(19) . . . . ?
C10 C1 N2 C3 -2(2) . . . . ?
C10 C1 N2 C5 177.7(13) . . . . ?
C11 N4 C7 C9 60.0(18) . . . . ?
C11 N4 C10 N3 0.3(15) . . . . ?
C11 N4 C10 C1 176.6(14) . . . . ?
C12 N1 C1 N2 0.0(14) . . . . ?
C12 N1 C1 C10 -178.2(12) . . . . ?
C14B C27 C24 C28 0.0 . . . . ?
C14B C27 C24 C26 177(3) . . . . ?
C27 C14B C19 C3 178(2) . . . . ?
C27 C14B C19 C25 0.0 . . . . ?
C27 C24 C28 C25 0.0 . . . . ?
C27 C24 C26 O2 40(6) . . . . ?
C27 C24 C26 O1 -156(3) . . . . ?
C24 C28 C25 C19 0.0 . . . . ?
C28 C24 C26 O2 -143(4) . . . . ?
C28 C24 C26 O1 21(4) . . . . ?
C28 C25 C19 C3 -178(2) . . . . ?
C28 C25 C19 C14B 0.0 . . . . ?
C19 C14B C27 C24 0.0 . . . . ?
C16 C8 C6 C13 0.0 . . . . ?
C8 C16 C15 C9 0.0 . . . . ?
C8 C6 C13 C9 0.0 . . . . ?
C6 C13 C9 C7 -178.9(11) . . . . ?
C6 C13 C9 C15 0.0 . . . . ?
C13 C9 C15 C16 0.0 . . . . ?
C15 C16 C8 C2 -175.2(10) . . . . ?
C15 C16 C8 C6 0.0 . . . . ?
O4 C23 C21 C22 -171(2) . . . . ?
O4 C23 C21 C18 11(4) . . . . ?
C23 C21 C18 C20 178(2) . . . . ?
C26 C24 C28 C25 -177(3) . . . . ?
C14A C22 C21 C23 -178(2) . . . . ?
C14A C22 C21 C18 0.0 . . . . ?
C22 C14A C17 C3 -177.5(15) . . . . ?
C22 C14A C17 C20 0.0 . . . . ?
C22 C21 C18 C20 0.0 . . . . ?
C21 C18 C20 C17 0.0 . . . . ?
C18 C20 C17 C3 177.4(16) . . . . ?
C18 C20 C17 C14A 0.0 . . . . ?
C17 C14A C22 C21 0.0 . . . . ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6 -10 0 0.0724 6.0068 -10.0213 -0.0015 0.0302 0.1857 -0.9714
-6 0 -3 0.0269 -6.0082 0.0140 -2.9941 -0.1890 -0.5849 0.7428
0 -23 -5 0.0559 -0.0005 -23.0094 -4.9904 -0.1837 -0.8516 -0.5075
0 22 5 0.0147 0.0008 22.0098 4.9908 0.1965 0.8222 0.4875
-6 5 -1 0.0198 -6.0068 5.0196 -0.9965 -0.0618 -0.3678 0.8619
6 -2 2 0.0678 6.0074 -2.0170 1.9951 0.1190 0.4911 -0.7924
0 -22 -5 0.0470 -0.0008 -22.0098 -4.9908 -0.1965 -0.8222 -0.4875
0 -16 8 0.0553 0.0154 -15.9615 8.0027 0.9691 -0.1905 -0.2428
5 0 -6 0.0394 4.9952 -0.0450 -6.0020 -0.6548 0.1898 -0.7007
-6 6 5 0.0220 -5.9989 6.0427 5.0011 0.4988 -0.1283 0.9395
0 17 -8 0.0068 -0.0156 16.9611 -8.0030 -0.9819 0.2199 0.2627
-6 11 2 0.0100 -6.0044 11.0287 2.0004 0.1482 -0.0863 1.0106


_ins_header                      
;
TITL SY-7 in Pnna 
REM Pnna (#52, found as Pnan in a-cb setting)
CELL 1.54184  10.118859  40.733550  15.074250  90.0000  90.0000  90.0000
ZERR    4.00   0.000446   0.001704   0.001030   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z 
SYMM -x+1/2, y+1/2,-z+1/2 
SYMM  x,-y+1/2,-z+1/2 
SFAC C H N O Cl Pd Sm
UNIT 4.00 4.00 4.00 4.00 4.00 4.00 4.00
TREF
HKLF 4
END
;
_olex2_submission_special_instructions 'No special instructions were received'


