# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_shelxl
_database_code_depnum_ccdc_archive 'CCDC 1472612'
_audit_update_record             
;
2016-04-06 deposited with the CCDC.
2017-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H10.40 Fe N8 O1.20 Pt'
_chemical_formula_weight         536.82

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'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           10
_space_group_name_H-M_alt        'P 2/m'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z'

_cell_length_a                   7.2727(2)
_cell_length_b                   7.46810(10)
_cell_length_c                   7.4416(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.9390(10)
_cell_angle_gamma                90
_cell_volume                     402.008(16)
_cell_formula_units_Z            1
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    4620
_cell_measurement_theta_min      16.22
_cell_measurement_theta_max      143.62

_exptl_crystal_description       parallepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.217
_exptl_crystal_F_000             252
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    23.441
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.550
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4431
_diffrn_reflns_av_unetI/netI     0.0850
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         8.111
_diffrn_reflns_theta_max         64.909
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.942
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.942
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.942
_reflns_number_total             742
_reflns_number_gt                723
_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       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.0453P)²+1.1717P] 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         742
_refine_ls_number_parameters     63
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.0941
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Pt Pt 0.5000 0.0000 0.5000 0.0128(3) Uani 1 4 d S T P . .
Fe Fe 0.5000 0.5000 0.0000 0.0092(6) Uani 1 4 d S T P . .
N1 N 0.1903(11) 0.5000 -0.0110(12) 0.012(2) Uani 1 2 d S T P . .
C1 C 0.0947(10) 0.3480(11) -0.0053(10) 0.0160(18) Uani 1 1 d . . . . .
H1 H 0.1579 0.2369 -0.0086 0.022 Uiso 1 1 calc R U . . .
N11 N 0.1680(17) 0.5000 0.4417(17) 0.050(4) Uani 1 2 d S T P . .
C11 C 0.0811(10) 0.3422(11) 0.4708(12) 0.024(2) Uani 1 1 d . . . . .
H11 H 0.1396 0.2319 0.4483 0.033 Uiso 1 1 calc R U . . .
N21 N 0.5098(8) 0.2944(10) 0.2029(9) 0.0157(15) Uani 1 1 d . . . . .
C21 C 0.5094(10) 0.1864(11) 0.3101(11) 0.0122(18) Uani 1 1 d . . . . .
OW O 0.050(2) 1.0000 0.247(2) 0.056(5) Uani 0.6 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt 0.0213(4) 0.0078(4) 0.0093(5) 0.000 0.0016(3) 0.000
Fe 0.0138(12) 0.0046(12) 0.0091(14) 0.000 0.0003(10) 0.000
N1 0.015(4) 0.014(5) 0.007(5) 0.000 0.006(4) 0.000
C1 0.022(4) 0.009(4) 0.017(5) -0.001(3) 0.004(4) 0.001(3)
N11 0.055(8) 0.054(9) 0.038(9) 0.000 -0.001(7) 0.000
C11 0.021(4) 0.007(4) 0.046(6) -0.004(4) 0.011(4) 0.004(3)
N21 0.016(3) 0.020(4) 0.010(4) -0.005(3) 0.000(3) -0.001(3)
C21 0.019(4) 0.012(4) 0.005(4) 0.005(3) -0.001(3) -0.003(3)
OW 0.057(11) 0.057(13) 0.051(13) 0.000 -0.005(9) 0.000

_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
Pt C21 1.990(8) . ?
Pt C21 1.990(8) 4 ?
Pt C21 1.990(8) 2_656 ?
Pt C21 1.990(8) 3_656 ?
Fe N21 2.149(7) . ?
Fe N21 2.149(7) 4_565 ?
Fe N21 2.149(7) 2_655 ?
Fe N21 2.149(7) 3_665 ?
Fe N1 2.245(8) 3_665 ?
Fe N1 2.245(8) . ?
N1 C1 1.334(9) . ?
N1 C1 1.334(9) 4_565 ?
C1 C1 1.388(14) 2 ?
C1 H1 0.9500 . ?
N11 C11 1.365(10) . ?
N11 C11 1.365(10) 4_565 ?
C11 C11 1.299(15) 2_556 ?
C11 H11 0.9500 . ?
N21 C21 1.135(11) . ?

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
C21 Pt C21 88.8(5) . 4 ?
C21 Pt C21 91.2(5) . 2_656 ?
C21 Pt C21 180.0 4 2_656 ?
C21 Pt C21 180.0 . 3_656 ?
C21 Pt C21 91.2(5) 4 3_656 ?
C21 Pt C21 88.8(5) 2_656 3_656 ?
N21 Fe N21 91.2(4) . 4_565 ?
N21 Fe N21 88.8(4) . 2_655 ?
N21 Fe N21 180.0 4_565 2_655 ?
N21 Fe N21 180.0 . 3_665 ?
N21 Fe N21 88.8(4) 4_565 3_665 ?
N21 Fe N21 91.2(4) 2_655 3_665 ?
N21 Fe N1 90.8(2) . 3_665 ?
N21 Fe N1 90.8(2) 4_565 3_665 ?
N21 Fe N1 89.2(2) 2_655 3_665 ?
N21 Fe N1 89.2(2) 3_665 3_665 ?
N21 Fe N1 89.2(2) . . ?
N21 Fe N1 89.2(2) 4_565 . ?
N21 Fe N1 90.8(2) 2_655 . ?
N21 Fe N1 90.8(2) 3_665 . ?
N1 Fe N1 180.0 3_665 . ?
C1 N1 C1 116.6(9) . 4_565 ?
C1 N1 Fe 121.5(4) . . ?
C1 N1 Fe 121.5(4) 4_565 . ?
N1 C1 C1 121.7(4) . 2 ?
N1 C1 H1 119.1 . . ?
C1 C1 H1 119.1 2 . ?
C11 N11 C11 119.4(12) . 4_565 ?
C11 C11 N11 120.3(6) 2_556 . ?
C11 C11 H11 119.9 2_556 . ?
N11 C11 H11 119.9 . . ?
C21 N21 Fe 177.9(7) . . ?
N21 C21 Pt 178.0(8) . . ?

_refine_diff_density_max         2.589
_refine_diff_density_min         -2.500
_refine_diff_density_rms         0.279

_shelxl_version_number           2014/6

_shelx_res_file                  
;
TITL *****ta_5****** P2/M
CELL  1.54178   7.2727   7.4681  7.4416   90.000    95.939   90.000
ZERR     1.00   0.0002   0.0001   0.0002    0.000    0.001    0.000
LATT   1
SYMM  - X,   Y, - Z
SFAC  C    H       N    O    FE   PT
UNIT  12   10.4    8    1.2    1    1
ACTA
OMIT    -2.00 130.00
OMIT    -6   5   3    !    221.62        846.05       4.88       0.221
OMIT     2   1   6   !      89.07        517.42       3.90       0.173
OMIT     1   8   0   !     491.62        939.95       3.70       0.233
FMAP   2
PLAN   -20
BOND  $H
TEMP  -113
L.S. 4
WGHT    0.045300    1.171700
FVAR       4.29855
PT    6    0.500000    0.000000    0.500000    10.25000    0.02129    0.00782 =
         0.00928    0.00000    0.00163    0.00000
FE    5    0.500000    0.500000    0.000000    10.25000    0.01377    0.00462 =
         0.00906    0.00000    0.00032    0.00000
N1    3    0.190349    0.500000   -0.011043    10.50000    0.01543    0.01436 =
         0.00746    0.00000    0.00637    0.00000
C1    1    0.094710    0.347994   -0.005309    11.00000    0.02247    0.00930 =
         0.01670   -0.00066    0.00443    0.00114
AFIX  43
H1    2    0.157900    0.236895   -0.008576    11.00000   -1.40000
AFIX   0
N11   3    0.167967    0.500000    0.441719    10.50000    0.05525    0.05438 =
         0.03829    0.00000   -0.00107    0.00000
C11   1    0.081145    0.342236    0.470815    11.00000    0.02085    0.00655 =
         0.04578   -0.00377    0.01062    0.00391
AFIX  43
H11   2    0.139630    0.231919    0.448293    11.00000   -1.40000
AFIX   0
N21   3    0.509802    0.294403    0.202881    11.00000    0.01626    0.02001 =
         0.01039   -0.00516   -0.00007   -0.00088
C21   1    0.509400    0.186445    0.310116    11.00000    0.01899    0.01176 =
         0.00547    0.00546   -0.00079   -0.00345
OW    4    0.050264    1.000000    0.247462    10.30000    0.05733    0.05728 =
         0.05077    0.00000   -0.00464    0.00000
HKLF    4

REM  *****ta_5****** P2/M
REM R1 =  0.0438 for     723 Fo > 4sig(Fo)  and  0.0464 for all     742 data
REM     63 parameters refined using      0 restraints

END

WGHT      0.0450      1.1662

REM Highest difference peak  2.589,  deepest hole -2.500,  1-sigma level  0.279
Q1    1   0.4633  0.0873  0.5770  11.00000  0.05    2.59
Q2    1   0.3854  0.0000  0.4819  10.50000  0.05    1.91
Q3    1   0.5000  0.1938  0.5000  10.50000  0.05    1.75
Q4    1   0.4762  0.0000  0.7039  10.50000  0.05    1.58
Q5    1   0.3286  0.0000  0.5976  10.50000  0.05    1.08
Q6    1   0.5000  0.0000  0.0000  10.25000  0.05    0.96
Q7    1   0.4671  0.4128  0.0742  11.00000  0.05    0.91
Q8    1   0.3860  0.3054 -0.1622  11.00000  0.05    0.85
Q9    1   0.1608  0.0000  0.5008  10.50000  0.05    0.82
Q10   1   0.2603  0.0000  0.7132  10.50000  0.05    0.81
Q11   1   0.2917  0.5000  0.3708  10.50000  0.05    0.77
Q12   1   0.4424  0.2531  0.6546  11.00000  0.05    0.76
Q13   1   0.4259  0.0745  0.3508  11.00000  0.05    0.76
Q14   1   0.2778  0.0721  0.7197  11.00000  0.05    0.73
Q15   1   0.4745  0.3635  0.2609  11.00000  0.05    0.70
Q16   1   0.4909  0.3538  0.3442  11.00000  0.05    0.69
Q17   1   0.4997  0.5000 -0.3130  10.50000  0.05    0.67
Q18   1   0.5000  0.3049  0.0000  10.50000  0.05    0.66
Q19   1   0.1118  0.2852  0.4184  11.00000  0.05    0.65
Q20   1   0.0314  0.5000  0.0585  10.50000  0.05    0.64
;
_shelx_res_checksum              43913
####################################################################### 
# 
# 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_shelxl_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1472613'
_audit_update_record             
;
2016-04-06 deposited with the CCDC.
2017-09-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H10.40 Fe N8 O1.20 Pd'
_chemical_formula_weight         448.13

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'
Fe Fe -1.1336 3.1974 '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           10
_space_group_name_H-M_alt        'P 2/m'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z'

_cell_length_a                   7.28000(10)
_cell_length_b                   7.47000(10)
_cell_length_c                   7.43870(10)
_cell_angle_alpha                90
_cell_angle_beta                 95.8800(10)
_cell_angle_gamma                90
_cell_volume                     402.400(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    4370
_cell_measurement_theta_min      16.23
_cell_measurement_theta_max      143.32

_exptl_crystal_description       parallepiped
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_F_000             220
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.024
_exptl_absorpt_coefficient_mu    16.410
_shelx_estimated_absorpt_T_min   0.243
_shelx_estimated_absorpt_T_max   0.694
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4498
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_av_R_equivalents  0.0625
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         8.112
_diffrn_reflns_theta_max         64.978
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.948
_reflns_number_total             747
_reflns_number_gt                723
_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       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.0442P)²+1.6923P] 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         747
_refine_ls_number_parameters     63
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0433
_refine_ls_wR_factor_ref         0.1065
_refine_ls_wR_factor_gt          0.1055
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
Pd Pd 0.5000 0.0000 0.5000 0.0128(3) Uani 1 4 d S T P . .
Fe Fe 0.5000 0.5000 0.0000 0.0091(4) Uani 1 4 d S T P . .
N1 N 0.1905(7) 0.5000 -0.0112(7) 0.0122(12) Uani 1 2 d S T P . .
C1 C 0.0946(6) 0.3470(6) -0.0060(7) 0.0176(11) Uani 1 1 d . . . . .
H1 H 0.1575 0.2360 -0.0107 0.025 Uiso 1 1 calc R U . . .
N11 N 0.1683(11) 0.5000 0.4454(11) 0.047(2) Uani 1 2 d S T P . .
C11 C 0.0819(6) 0.3429(7) 0.4701(8) 0.0236(13) Uani 1 1 d . . . . .
H11 H 0.1395 0.2330 0.4443 0.033 Uiso 1 1 calc R U . . .
N21 N 0.5104(5) 0.2957(6) 0.2006(6) 0.0160(10) Uani 1 1 d . . . . .
C21 C 0.5072(6) 0.1858(7) 0.3112(7) 0.0129(10) Uani 1 1 d . . . . .
OW O 0.0508(16) 1.0000 0.2493(16) 0.054(3) Uani 0.6 2 d S T P . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd 0.0194(4) 0.0080(4) 0.0113(5) 0.000 0.0038(3) 0.000
Fe 0.0131(7) 0.0063(8) 0.0082(9) 0.000 0.0026(6) 0.000
N1 0.013(3) 0.014(3) 0.010(3) 0.000 0.003(2) 0.000
C1 0.020(2) 0.010(3) 0.022(3) 0.000(2) 0.003(2) 0.002(2)
N11 0.040(4) 0.061(6) 0.041(5) 0.000 0.007(4) 0.000
C11 0.019(2) 0.011(3) 0.042(4) 0.003(2) 0.007(2) 0.001(2)
N21 0.018(2) 0.017(2) 0.014(2) -0.003(2) 0.0043(18) -0.0013(18)
C21 0.018(2) 0.014(3) 0.007(2) -0.001(2) 0.000(2) -0.001(2)
OW 0.060(7) 0.044(7) 0.056(8) 0.000 -0.008(6) 0.000

_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
Pd C21 1.979(5) . ?
Pd C21 1.979(5) 4 ?
Pd C21 1.979(5) 2_656 ?
Pd C21 1.979(5) 3_656 ?
Fe N21 2.130(5) 4_565 ?
Fe N21 2.130(5) 2_655 ?
Fe N21 2.130(5) 3_665 ?
Fe N21 2.130(5) . ?
Fe N1 2.246(5) 3_665 ?
Fe N1 2.246(5) . ?
N1 C1 1.342(5) 4_565 ?
N1 C1 1.342(5) . ?
C1 C1 1.389(9) 2 ?
C1 H1 0.9500 . ?
N11 C11 1.353(6) 4_565 ?
N11 C11 1.353(6) . ?
C11 C11 1.315(9) 2_556 ?
C11 H11 0.9500 . ?
N21 C21 1.164(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 Pd C21 89.1(3) . 4 ?
C21 Pd C21 90.9(3) . 2_656 ?
C21 Pd C21 180.0 4 2_656 ?
C21 Pd C21 180.0 . 3_656 ?
C21 Pd C21 90.9(3) 4 3_656 ?
C21 Pd C21 89.1(3) 2_656 3_656 ?
N21 Fe N21 180.00(17) 4_565 2_655 ?
N21 Fe N21 88.5(2) 4_565 3_665 ?
N21 Fe N21 91.5(2) 2_655 3_665 ?
N21 Fe N21 91.5(2) 4_565 . ?
N21 Fe N21 88.5(2) 2_655 . ?
N21 Fe N21 180.0 3_665 . ?
N21 Fe N1 90.60(14) 4_565 3_665 ?
N21 Fe N1 89.40(14) 2_655 3_665 ?
N21 Fe N1 89.40(14) 3_665 3_665 ?
N21 Fe N1 90.60(14) . 3_665 ?
N21 Fe N1 89.40(14) 4_565 . ?
N21 Fe N1 90.60(14) 2_655 . ?
N21 Fe N1 90.60(14) 3_665 . ?
N21 Fe N1 89.40(14) . . ?
N1 Fe N1 180.0 3_665 . ?
C1 N1 C1 116.7(5) 4_565 . ?
C1 N1 Fe 121.5(3) 4_565 . ?
C1 N1 Fe 121.5(3) . . ?
N1 C1 C1 121.6(3) . 2 ?
N1 C1 H1 119.2 . . ?
C1 C1 H1 119.2 2 . ?
C11 N11 C11 120.4(7) 4_565 . ?
C11 C11 N11 119.7(3) 2_556 . ?
C11 C11 H11 120.1 2_556 . ?
N11 C11 H11 120.1 . . ?
C21 N21 Fe 176.7(4) . . ?
N21 C21 Pd 179.6(5) . . ?

_refine_diff_density_max         1.081
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.166

_shelxl_version_number           2014/6

_shelx_res_file                  
;
TITL *****ta_5****** P2/M
CELL  1.54178   7.2800   7.4700   7.4387   90.000   95.880   90.000
ZERR     1.00   0.0001   0.0001   0.0001    0.000    0.001    0.000
LATT   1
SYMM  - X,   Y, - Z
SFAC  C    H    N    O    FE   PD
UNIT  12   10.4 8    1.2  1    1
ACTA
OMIT    -2.00 130.00
OMIT  -5   0   1  !       436.07        155.65       7.74       0.117       1.45
TEMP -113
SIZE  0.024 0.044 0.120
FMAP   2
PLAN   -20
SIZE   0.024 0.044 0.120
BOND  $H
L.S.   5
WGHT    0.044200    1.692300
FVAR       4.05608
PD    6    0.500000    0.000000    0.500000    10.25000    0.01943    0.00804 =
         0.01134    0.00000    0.00382    0.00000
FE    5    0.500000    0.500000    0.000000    10.25000    0.01314    0.00629 =
         0.00824    0.00000    0.00265    0.00000
N1    3    0.190545    0.500000   -0.011156    10.50000    0.01344    0.01368 =
         0.00979    0.00000    0.00284    0.00000
C1    1    0.094568    0.347041   -0.006011    11.00000    0.02035    0.01024 =
         0.02232    0.00041    0.00328    0.00208
AFIX  43
H1    2    0.157539    0.236016   -0.010710    11.00000   -1.40000
AFIX   0
N11   3    0.168286    0.500000    0.445382    10.50000    0.03994    0.06092 =
         0.04052    0.00000    0.00660    0.00000
C11   1    0.081947    0.342880    0.470092    11.00000    0.01883    0.01103 =
         0.04157    0.00322    0.00658    0.00066
AFIX  43
H11   2    0.139457    0.232969    0.444347    11.00000   -1.40000
AFIX   0
N21   3    0.510421    0.295656    0.200554    11.00000    0.01757    0.01651 =
         0.01439   -0.00271    0.00428   -0.00125
C21   1    0.507157    0.185769    0.311190    11.00000    0.01761    0.01440 =
         0.00656   -0.00138    0.00016   -0.00095
OW    4    0.050793    1.000000    0.249279    10.30000    0.05979    0.04354 =
         0.05557    0.00000   -0.00849    0.00000
HKLF    4

REM  *****ta_5****** P2/M
REM R1 =  0.0433 for     723 Fo > 4sig(Fo)  and  0.0446 for all     747 data
REM     63 parameters refined using      0 restraints

END

WGHT      0.0442      1.6756

REM Highest difference peak  1.081,  deepest hole -1.258,  1-sigma level  0.166
Q1    1   0.3720  0.0000  0.5319  10.50000  0.05    1.08
Q2    1   0.5000  0.0000  0.3167  10.50000  0.05    1.06
Q3    1   0.4670  0.0869  0.4155  11.00000  0.05    1.01
Q4    1   0.3856  0.5000  0.0331  10.50000  0.05    0.91
Q5    1   0.1054  0.0000  0.5166  10.50000  0.05    0.83
Q6    1   0.3062  0.5000  0.3966  10.50000  0.05    0.81
Q7    1   0.4797  0.4137 -0.0864  11.00000  0.05    0.69
Q8    1   0.3093  0.0000  0.4287  10.50000  0.05    0.67
Q9    1   0.5000  0.1866  0.5000  10.50000  0.05    0.65
Q10   1   0.3774  0.1087  0.5820  11.00000  0.05    0.62
Q11   1   0.0000  0.5000  0.0000  10.25000  0.05    0.53
Q12   1   0.1235  0.2838  0.5023  11.00000  0.05    0.48
Q13   1   0.3500  0.1142  0.4163  11.00000  0.05    0.48
Q14   1   0.4333  0.2937  0.2344  11.00000  0.05    0.47
Q15   1   0.1097  0.3971  0.5421  11.00000  0.05    0.46
Q16   1   0.5117  0.0478  0.1770  11.00000  0.05    0.42
Q17   1   0.5000  0.2995  0.0000  10.50000  0.05    0.41
Q18   1   0.2349  0.5000  0.0252  10.50000  0.05    0.39
Q19   1   0.0000  0.3429  0.0000  10.50000  0.05    0.36
Q20   1   0.1545  0.5000  0.0145  10.50000  0.05    0.36
;
_shelx_res_checksum              8175
