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

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

data_Fe-pic-Pd(CN)4-LS
_database_code_depnum_ccdc_archive 'CCDC 1050970'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Fe-pic-Pd(CN)4-LS
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C16 H16 Fe N8 Pd'
_chemical_formula_sum            'C16 H16 Fe N8 Pd'
_chemical_formula_weight         482.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.0448(11)
_cell_length_b                   15.2279(16)
_cell_length_c                   15.6122(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 125.869(4)
_cell_angle_gamma                90.00
_cell_volume                     1935.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    6264
_cell_measurement_theta_min      2.479
_cell_measurement_theta_max      27.499

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    1.695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3441
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   
; 
SADABS v.2.10 (Bruker,2008) was used for absorption correction.
R(int) was 0.1623 before and 0.1423 after correction.
The Ratio of minimum to maximum transmission is 0.4611.
The l/2 correction factor is 0.0015. 
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexDuo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            17154
_diffrn_reflns_av_R_equivalents  0.1431
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.09
_diffrn_reflns_theta_max         27.44
_reflns_number_total             4417
_reflns_number_gt                3577
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0500P)²+2.0176P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4417
_refine_ls_number_parameters     284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0438
_refine_ls_wR_factor_ref         0.1259
_refine_ls_wR_factor_gt          0.1183
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.0000 1.0000 0.5000 0.01369(12) Uani 1 2 d S . .
Pd2 Pd 1.0000 0.5000 0.5000 0.01889(12) Uani 1 2 d S . .
Fe1 Fe 0.72049(5) 0.748210(19) 0.55112(3) 0.01549(13) Uani 1 1 d . A .
N1 N 0.8424(3) 0.84345(15) 0.54334(18) 0.0190(5) Uani 1 1 d . . .
N2 N 0.7994(4) 0.93939(18) 0.2631(2) 0.0432(8) Uani 1 1 d . . .
N3 N 0.8427(3) 0.66049(16) 0.5350(2) 0.0215(5) Uani 1 1 d . . .
N4 N 0.7863(5) 0.3706(2) 0.5295(3) 0.0586(10) Uani 1 1 d . . .
N5 N 0.5474(4) 0.74817(12) 0.3975(2) 0.0200(5) Uani 1 1 d . . .
N6 N 0.5795(3) 0.64925(15) 0.54518(19) 0.0230(5) Uani 1 1 d . . .
H6A H 0.6434 0.6090 0.5952 0.028 Uiso 1 1 d R . .
H6B H 0.5081 0.6705 0.5571 0.028 Uiso 1 1 d R . .
N7 N 0.6084(3) 0.83130(15) 0.5856(2) 0.0224(5) Uani 1 1 d . . .
N8 N 0.8816(4) 0.74334(14) 0.7102(2) 0.0249(6) Uani 1 1 d . . .
H8A H 0.9193 0.6881 0.7301 0.030 Uiso 0.447(11) 1 d PR A 1
H8B H 0.9678 0.7784 0.7310 0.030 Uiso 0.447(11) 1 d PR A 1
H8'A H 0.8603 0.6967 0.7357 0.030 Uiso 0.553(11) 1 d PR A 2
H8'B H 0.9849 0.7385 0.7291 0.030 Uiso 0.553(11) 1 d PR A 2
C1 C 0.9056(3) 0.89998(18) 0.5310(2) 0.0183(6) Uani 1 1 d . . .
C2 C 0.8735(4) 0.96081(17) 0.3500(2) 0.0262(6) Uani 1 1 d . . .
C3 C 0.9058(4) 0.60291(19) 0.5250(2) 0.0225(6) Uani 1 1 d . . .
C4 C 0.8645(4) 0.4193(2) 0.5206(3) 0.0357(8) Uani 1 1 d . . .
C5 C 0.5184(4) 0.81171(19) 0.3283(2) 0.0295(7) Uani 1 1 d . . .
H5 H 0.5920 0.8582 0.3520 0.035 Uiso 1 1 calc R . .
C6 C 0.3836(5) 0.8106(2) 0.2233(2) 0.0392(8) Uani 1 1 d . . .
H6 H 0.3686 0.8551 0.1776 0.047 Uiso 1 1 calc R . .
C7 C 0.2725(5) 0.7433(2) 0.1875(3) 0.0364(9) Uani 1 1 d . . .
H7 H 0.1797 0.7423 0.1178 0.044 Uiso 1 1 calc R . .
C8 C 0.3009(4) 0.67656(19) 0.2572(2) 0.0301(7) Uani 1 1 d . . .
H8 H 0.2269 0.6304 0.2349 0.036 Uiso 1 1 calc R . .
C9 C 0.4410(3) 0.67978(17) 0.3602(2) 0.0220(6) Uani 1 1 d . . .
C10 C 0.4897(4) 0.60844(17) 0.4397(2) 0.0233(6) Uani 1 1 d . . .
H10A H 0.3927 0.5784 0.4244 0.028 Uiso 1 1 calc R . .
H10B H 0.5590 0.5658 0.4371 0.028 Uiso 1 1 calc R . .
C13 C 0.4727(5) 0.9445(2) 0.6558(3) 0.0432(9) Uani 1 1 d . . .
H13 H 0.4188 0.9778 0.6767 0.052 Uiso 1 1 calc R A 1
C11 C 0.4925(16) 0.8917(7) 0.5223(11) 0.032(2) Uani 0.447(11) 1 d P A 1
H11 H 0.4611 0.8967 0.4534 0.038 Uiso 0.447(11) 1 calc PR A 1
C12 C 0.417(2) 0.9465(8) 0.5528(15) 0.040(3) Uani 0.447(11) 1 d P A 1
H12 H 0.3318 0.9835 0.5044 0.048 Uiso 0.447(11) 1 calc PR A 1
C14 C 0.607(3) 0.8944(11) 0.7304(15) 0.032(3) Uani 0.447(11) 1 d P A 1
H14 H 0.6538 0.8988 0.8023 0.038 Uiso 0.447(11) 1 calc PR A 1
C15 C 0.668(2) 0.8365(9) 0.6911(14) 0.020(2) Uani 0.447(11) 1 d P A 1
C16 C 0.8024(10) 0.7724(5) 0.7639(5) 0.030(2) Uani 0.447(11) 1 d P A 1
H16A H 0.7569 0.7222 0.7768 0.036 Uiso 0.447(11) 1 calc PR A 1
H16B H 0.8833 0.8002 0.8312 0.036 Uiso 0.447(11) 1 calc PR A 1
C11' C 0.4483(13) 0.8618(6) 0.5154(8) 0.034(2) Uani 0.553(11) 1 d P A 2
H11' H 0.3876 0.8452 0.4447 0.041 Uiso 0.553(11) 1 calc PR A 2
C12' C 0.3800(18) 0.9156(7) 0.5494(12) 0.048(3) Uani 0.553(11) 1 d P A 2
H12' H 0.2714 0.9336 0.5024 0.057 Uiso 0.553(11) 1 calc PR A 2
C14' C 0.629(2) 0.9112(11) 0.7169(12) 0.038(3) Uani 0.553(11) 1 d P A 2
H14' H 0.6948 0.9275 0.7877 0.046 Uiso 0.553(11) 1 calc PR A 2
C15' C 0.6932(18) 0.8573(7) 0.6831(12) 0.024(2) Uani 0.553(11) 1 d P A 2
C16' C 0.8638(7) 0.8220(4) 0.7506(4) 0.0313(19) Uani 0.553(11) 1 d P A 2
H16C H 0.9389 0.8657 0.7563 0.038 Uiso 0.553(11) 1 calc PR A 2
H16D H 0.8936 0.8111 0.8211 0.038 Uiso 0.553(11) 1 calc PR 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
Pd1 C2 1.992(3) . ?
Pd1 C2 1.992(3) 3_776 ?
Pd1 C1 1.998(3) 3_776 ?
Pd1 C1 1.998(3) . ?
Pd2 C3 1.984(3) 3_766 ?
Pd2 C3 1.984(3) . ?
Pd2 C4 1.995(4) 3_766 ?
Pd2 C4 1.995(4) . ?
Fe1 N3 1.928(2) . ?
Fe1 N1 1.948(3) . ?
Fe1 N7 1.967(2) . ?
Fe1 N5 1.972(3) . ?
Fe1 N8 2.020(3) . ?
Fe1 N6 2.032(2) . ?
N1 C1 1.150(4) . ?
N2 C2 1.147(4) . ?
N3 C3 1.145(4) . ?
N4 C4 1.147(5) . ?
N5 C5 1.349(4) . ?
N5 C9 1.355(4) . ?
N6 C10 1.473(4) . ?
N7 C15' 1.296(15) . ?
N7 C11 1.353(13) . ?
N7 C15 1.385(16) . ?
N7 C11' 1.392(10) . ?
N8 C16' 1.413(6) . ?
N8 C16 1.522(8) . ?
C5 C6 1.385(4) . ?
C6 C7 1.370(5) . ?
C7 C8 1.391(5) . ?
C8 C9 1.385(4) . ?
C9 C10 1.499(4) . ?
C13 C12 1.359(19) . ?
C13 C14' 1.367(19) . ?
C13 C14 1.38(2) . ?
C13 C12' 1.416(16) . ?
C11 C12 1.38(2) . ?
C14 C15 1.41(2) . ?
C15 C16 1.504(19) . ?
C11' C12' 1.361(17) . ?
C14' C15' 1.33(2) . ?
C15' C16' 1.490(16) . ?

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
C2 Pd1 C2 180.000(1) . 3_776 ?
C2 Pd1 C1 90.55(11) . 3_776 ?
C2 Pd1 C1 89.45(11) 3_776 3_776 ?
C2 Pd1 C1 89.45(11) . . ?
C2 Pd1 C1 90.55(11) 3_776 . ?
C1 Pd1 C1 180.000(1) 3_776 . ?
C3 Pd2 C3 180.000(1) 3_766 . ?
C3 Pd2 C4 90.35(12) 3_766 3_766 ?
C3 Pd2 C4 89.65(12) . 3_766 ?
C3 Pd2 C4 89.65(12) 3_766 . ?
C3 Pd2 C4 90.35(12) . . ?
C4 Pd2 C4 180.0(2) 3_766 . ?
N3 Fe1 N1 92.07(12) . . ?
N3 Fe1 N7 172.67(10) . . ?
N1 Fe1 N7 91.15(10) . . ?
N3 Fe1 N5 90.93(10) . . ?
N1 Fe1 N5 93.62(10) . . ?
N7 Fe1 N5 95.44(11) . . ?
N3 Fe1 N8 91.28(11) . . ?
N1 Fe1 N8 91.36(11) . . ?
N7 Fe1 N8 82.06(11) . . ?
N5 Fe1 N8 174.48(12) . . ?
N3 Fe1 N6 87.71(10) . . ?
N1 Fe1 N6 174.97(10) . . ?
N7 Fe1 N6 89.66(10) . . ?
N5 Fe1 N6 81.37(10) . . ?
N8 Fe1 N6 93.66(11) . . ?
C1 N1 Fe1 175.0(2) . . ?
C3 N3 Fe1 173.8(2) . . ?
C5 N5 C9 117.5(3) . . ?
C5 N5 Fe1 126.6(2) . . ?
C9 N5 Fe1 115.73(18) . . ?
C10 N6 Fe1 108.55(17) . . ?
C15' N7 C11 110.1(8) . . ?
C11 N7 C15 114.8(9) . . ?
C15' N7 C11' 119.0(8) . . ?
C15 N7 C11' 114.5(8) . . ?
C15' N7 Fe1 115.5(7) . . ?
C11 N7 Fe1 128.5(6) . . ?
C15 N7 Fe1 116.2(7) . . ?
C11' N7 Fe1 125.5(4) . . ?
C16' N8 Fe1 107.3(3) . . ?
C16 N8 Fe1 111.5(3) . . ?
N1 C1 Pd1 176.0(3) . . ?
N2 C2 Pd1 179.0(3) . . ?
N3 C3 Pd2 176.1(3) . . ?
N4 C4 Pd2 177.2(3) . . ?
N5 C5 C6 122.8(3) . . ?
C7 C6 C5 119.3(3) . . ?
C6 C7 C8 118.9(3) . . ?
C9 C8 C7 119.1(3) . . ?
N5 C9 C8 122.3(3) . . ?
N5 C9 C10 114.1(2) . . ?
C8 C9 C10 123.5(3) . . ?
N6 C10 C9 108.0(2) . . ?
C12 C13 C14' 110.0(8) . . ?
C12 C13 C14 122.0(9) . . ?
C14' C13 C12' 113.6(8) . . ?
C14 C13 C12' 117.6(9) . . ?
N7 C11 C12 124.6(13) . . ?
C13 C12 C11 117.8(13) . . ?
C13 C14 C15 116.0(14) . . ?
N7 C15 C14 123.9(15) . . ?
N7 C15 C16 115.8(11) . . ?
C14 C15 C16 120.2(14) . . ?
C15 C16 N8 107.3(7) . . ?
C12' C11' N7 120.5(10) . . ?
C11' C12' C13 120.6(11) . . ?
C15' C14' C13 125.2(14) . . ?
N7 C15' C14' 121.0(14) . . ?
N7 C15' C16' 114.4(10) . . ?
C14' C15' C16' 124.6(13) . . ?
N8 C16' C15' 112.6(6) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.44
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.002
_refine_diff_density_min         -1.931
_refine_diff_density_rms         0.171
####################################################################### 
# 
# 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_Fe-pic-Pd(CN)4-HS
_database_code_depnum_ccdc_archive 'CCDC 1050971'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Fe-pic-Pd(CN)4-HS
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C16 H16 Fe N8 Pd'
_chemical_formula_sum            'C16 H16 Fe N8 Pd'
_chemical_formula_weight         482.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.2201(11)
_cell_length_b                   15.6565(16)
_cell_length_c                   15.9375(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 126.500(4)
_cell_angle_gamma                90.00
_cell_volume                     2050.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6264
_cell_measurement_theta_min      2.479
_cell_measurement_theta_max      27.499

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.564
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             960
_exptl_absorpt_coefficient_mu    1.600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3494
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
; 
SADABS v.2.10 (Bruker,2008) was used for absorption correction.
R(int) was 0.0713 before and 0.0338 after correction.
The Ratio of minimum to maximum transmission is 0.4686.
The l/2 correction factor is 0.0015. 
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexDuo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18089
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         27.50
_reflns_number_total             4698
_reflns_number_gt                3715
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0302P)²+1.1499P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4698
_refine_ls_number_parameters     284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0808
_refine_ls_wR_factor_gt          0.0737
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 1.0000 1.0000 0.5000 0.03300(8) Uani 1 2 d S . .
Pd2 Pd 1.0000 0.5000 0.5000 0.04422(9) Uani 1 2 d S . .
Fe1 Fe 0.73635(4) 0.746890(18) 0.56577(3) 0.03413(9) Uani 1 1 d . A .
N1 N 0.8561(3) 0.84939(13) 0.55141(17) 0.0448(5) Uani 1 1 d . . .
N2 N 0.7894(4) 0.93849(18) 0.2679(2) 0.0835(9) Uani 1 1 d . . .
N3 N 0.8770(3) 0.65570(15) 0.5572(2) 0.0563(6) Uani 1 1 d . . .
N4 N 0.7825(5) 0.3764(2) 0.5235(3) 0.1071(13) Uani 1 1 d . . .
N5 N 0.5474(3) 0.74413(11) 0.40022(16) 0.0410(5) Uani 1 1 d . . .
N6 N 0.5783(3) 0.64304(13) 0.54810(17) 0.0483(5) Uani 1 1 d . . .
H6A H 0.6382 0.6022 0.5960 0.058 Uiso 1 1 d R . .
H6B H 0.5056 0.6630 0.5577 0.058 Uiso 1 1 d R . .
N7 N 0.6150(3) 0.83353(14) 0.6041(2) 0.0547(6) Uani 1 1 d . . .
N8 N 0.8929(3) 0.74599(15) 0.7366(2) 0.0609(7) Uani 1 1 d . . .
H8A H 0.9319 0.6929 0.7594 0.073 Uiso 0.51(3) 1 d PR A 1
H8B H 0.9781 0.7810 0.7604 0.073 Uiso 0.51(3) 1 d PR A 1
H8'A H 0.8816 0.6960 0.7596 0.073 Uiso 0.49(3) 1 d PR A 2
H8'B H 0.9976 0.7512 0.7608 0.073 Uiso 0.49(3) 1 d PR A 2
C1 C 0.9111(3) 0.90418(15) 0.53475(18) 0.0391(5) Uani 1 1 d . . .
C2 C 0.8682(3) 0.96027(16) 0.3523(2) 0.0497(6) Uani 1 1 d . . .
C3 C 0.9267(3) 0.59924(17) 0.5395(2) 0.0498(6) Uani 1 1 d . . .
C4 C 0.8610(4) 0.4231(2) 0.5155(3) 0.0682(9) Uani 1 1 d . . .
C5 C 0.5154(4) 0.80569(18) 0.3319(2) 0.0583(7) Uani 1 1 d . . .
H5 H 0.5873 0.8513 0.3552 0.070 Uiso 1 1 calc R . .
C6 C 0.3817(4) 0.8046(2) 0.2295(2) 0.0761(10) Uani 1 1 d . . .
H6 H 0.3651 0.8480 0.1842 0.091 Uiso 1 1 calc R . .
C7 C 0.2726(5) 0.7385(2) 0.1949(3) 0.0762(11) Uani 1 1 d . . .
H7 H 0.1791 0.7371 0.1264 0.091 Uiso 1 1 calc R . .
C8 C 0.3045(4) 0.6741(2) 0.2636(2) 0.0631(8) Uani 1 1 d . . .
H8 H 0.2325 0.6287 0.2421 0.076 Uiso 1 1 calc R . .
C9 C 0.4451(3) 0.67791(15) 0.36548(19) 0.0420(5) Uani 1 1 d . . .
C10 C 0.4935(3) 0.60734(16) 0.4428(2) 0.0475(6) Uani 1 1 d . . .
H10A H 0.3973 0.5767 0.4244 0.057 Uiso 1 1 calc R . .
H10B H 0.5642 0.5674 0.4409 0.057 Uiso 1 1 calc R . .
C13 C 0.4897(7) 0.9474(3) 0.6720(5) 0.1026(15) Uani 1 1 d . . .
H13 H 0.4424 0.9836 0.6933 0.123 Uiso 1 1 calc R A 1
C11 C 0.501(3) 0.8909(15) 0.540(2) 0.083(5) Uani 0.51(3) 1 d P A 1
H11 H 0.4625 0.8935 0.4704 0.099 Uiso 0.51(3) 1 calc PR A 1
C12 C 0.440(3) 0.9480(15) 0.579(2) 0.093(6) Uani 0.51(3) 1 d P A 1
H12 H 0.3598 0.9871 0.5330 0.112 Uiso 0.51(3) 1 calc PR A 1
C14 C 0.619(3) 0.8913(11) 0.746(2) 0.065(3) Uani 0.51(3) 1 d P A 1
H14 H 0.6631 0.8926 0.8170 0.078 Uiso 0.51(3) 1 calc PR A 1
C15 C 0.674(2) 0.8358(8) 0.7073(15) 0.041(2) Uani 0.51(3) 1 d P A 1
C16 C 0.8042(13) 0.7737(6) 0.7794(8) 0.052(2) Uani 0.51(3) 1 d P A 1
H16A H 0.7561 0.7245 0.7884 0.062 Uiso 0.51(3) 1 calc PR A 1
H16B H 0.8797 0.8001 0.8471 0.062 Uiso 0.51(3) 1 calc PR A 1
C11' C 0.461(3) 0.8680(18) 0.534(3) 0.086(6) Uani 0.49(3) 1 d P A 2
H11' H 0.4026 0.8510 0.4642 0.104 Uiso 0.49(3) 1 calc PR A 2
C12' C 0.393(4) 0.9228(17) 0.559(3) 0.109(8) Uani 0.49(3) 1 d P A 2
H12' H 0.2907 0.9454 0.5092 0.131 Uiso 0.49(3) 1 calc PR A 2
C14' C 0.628(4) 0.9136(15) 0.734(3) 0.092(6) Uani 0.49(3) 1 d P A 2
H14' H 0.6886 0.9285 0.8040 0.111 Uiso 0.49(3) 1 calc PR A 2
C15' C 0.697(3) 0.8546(12) 0.703(2) 0.067(4) Uani 0.49(3) 1 d P A 2
C16' C 0.852(2) 0.812(2) 0.7728(12) 0.146(10) Uani 0.49(3) 1 d P A 2
H16C H 0.9366 0.8546 0.8005 0.175 Uiso 0.49(3) 1 calc PR A 2
H16D H 0.8553 0.7901 0.8312 0.175 Uiso 0.49(3) 1 calc PR 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
Pd1 C2 1.992(3) . ?
Pd1 C2 1.992(3) 3_776 ?
Pd1 C1 1.995(2) 3_776 ?
Pd1 C1 1.995(2) . ?
Pd2 C3 1.983(2) . ?
Pd2 C3 1.983(2) 3_766 ?
Pd2 C4 1.985(4) 3_766 ?
Pd2 C4 1.985(4) . ?
Fe1 N3 2.088(2) . ?
Fe1 N1 2.111(2) . ?
Fe1 N5 2.152(2) . ?
Fe1 N7 2.157(2) . ?
Fe1 N8 2.188(3) . ?
Fe1 N6 2.189(2) . ?
N1 C1 1.140(3) . ?
N2 C2 1.135(3) . ?
N3 C3 1.135(3) . ?
N4 C4 1.148(4) . ?
N5 C9 1.336(3) . ?
N5 C5 1.341(3) . ?
N6 C10 1.466(3) . ?
N7 C15' 1.31(2) . ?
N7 C11 1.34(3) . ?
N7 C15 1.374(18) . ?
N7 C11' 1.39(3) . ?
N8 C16' 1.362(14) . ?
N8 C16 1.487(9) . ?
C5 C6 1.371(4) . ?
C6 C7 1.374(5) . ?
C7 C8 1.377(4) . ?
C8 C9 1.389(4) . ?
C9 C10 1.503(3) . ?
C13 C12 1.25(3) . ?
C13 C14' 1.26(3) . ?
C13 C14 1.44(3) . ?
C13 C12' 1.50(4) . ?
C11 C12 1.43(4) . ?
C14 C15 1.37(2) . ?
C15 C16 1.49(2) . ?
C11' C12' 1.31(4) . ?
C14' C15' 1.42(3) . ?
C15' C16' 1.45(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
C2 Pd1 C2 180.000(1) . 3_776 ?
C2 Pd1 C1 90.37(10) . 3_776 ?
C2 Pd1 C1 89.63(10) 3_776 3_776 ?
C2 Pd1 C1 89.63(10) . . ?
C2 Pd1 C1 90.37(10) 3_776 . ?
C1 Pd1 C1 180.0 3_776 . ?
C3 Pd2 C3 180.000(1) . 3_766 ?
C3 Pd2 C4 89.89(12) . 3_766 ?
C3 Pd2 C4 90.11(12) 3_766 3_766 ?
C3 Pd2 C4 90.11(12) . . ?
C3 Pd2 C4 89.89(12) 3_766 . ?
C4 Pd2 C4 180.00(16) 3_766 . ?
N3 Fe1 N1 92.67(10) . . ?
N3 Fe1 N5 93.23(9) . . ?
N1 Fe1 N5 92.15(8) . . ?
N3 Fe1 N7 169.46(10) . . ?
N1 Fe1 N7 91.17(9) . . ?
N5 Fe1 N7 96.43(9) . . ?
N3 Fe1 N8 93.15(10) . . ?
N1 Fe1 N8 95.61(9) . . ?
N5 Fe1 N8 169.70(10) . . ?
N7 Fe1 N8 76.69(10) . . ?
N3 Fe1 N6 88.15(9) . . ?
N1 Fe1 N6 168.97(8) . . ?
N5 Fe1 N6 76.83(8) . . ?
N7 Fe1 N6 89.95(9) . . ?
N8 Fe1 N6 95.32(9) . . ?
C1 N1 Fe1 174.2(2) . . ?
C3 N3 Fe1 167.4(2) . . ?
C9 N5 C5 117.9(2) . . ?
C9 N5 Fe1 115.71(16) . . ?
C5 N5 Fe1 126.08(17) . . ?
C10 N6 Fe1 108.61(15) . . ?
C15' N7 C11 113.1(16) . . ?
C11 N7 C15 117.5(14) . . ?
C15' N7 C11' 118.7(17) . . ?
C15 N7 C11' 116.1(15) . . ?
C15' N7 Fe1 115.7(10) . . ?
C11 N7 Fe1 126.2(12) . . ?
C15 N7 Fe1 115.8(7) . . ?
C11' N7 Fe1 125.6(14) . . ?
C16' N8 Fe1 110.0(7) . . ?
C16 N8 Fe1 112.0(4) . . ?
N1 C1 Pd1 177.8(2) . . ?
N2 C2 Pd1 178.1(3) . . ?
N3 C3 Pd2 176.4(3) . . ?
N4 C4 Pd2 177.6(3) . . ?
N5 C5 C6 123.2(3) . . ?
C5 C6 C7 118.9(3) . . ?
C6 C7 C8 118.7(3) . . ?
C7 C8 C9 119.3(3) . . ?
N5 C9 C8 121.9(2) . . ?
N5 C9 C10 115.9(2) . . ?
C8 C9 C10 122.3(2) . . ?
N6 C10 C9 109.9(2) . . ?
C12 C13 C14' 114.0(17) . . ?
C12 C13 C14 120.7(14) . . ?
C14' C13 C12' 117.3(17) . . ?
C14 C13 C12' 117.3(14) . . ?
N7 C11 C12 120(2) . . ?
C13 C12 C11 122(2) . . ?
C15 C14 C13 116(2) . . ?
C14 C15 N7 123.5(18) . . ?
C14 C15 C16 118.8(17) . . ?
N7 C15 C16 117.7(10) . . ?
C15 C16 N8 110.1(7) . . ?
C12' C11' N7 124(3) . . ?
C11' C12' C13 117(2) . . ?
C13 C14' C15' 124(3) . . ?
N7 C15' C14' 119(2) . . ?
N7 C15' C16' 115.6(16) . . ?
C14' C15' C16' 125(2) . . ?
N8 C16' C15' 119.7(12) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.071
####################################################################### 
# 
# 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_Fe-pic-Pt(CN)4-LS
_database_code_depnum_ccdc_archive 'CCDC 1050972'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Fe-pic-Pt(CN)4-LS
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C16 H16 Fe N8 Pt'
_chemical_formula_sum            'C16 H16 Fe N8 Pt'
_chemical_formula_weight         571.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/m

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

_cell_length_a                   7.8428(6)
_cell_length_b                   15.2262(12)
_cell_length_c                   8.4043(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.3670(10)
_cell_angle_gamma                90.00
_cell_volume                     976.42(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    5145
_cell_measurement_theta_min      2.828
_cell_measurement_theta_max      27.545

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             544
_exptl_absorpt_coefficient_mu    7.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3005
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2008) was used for absorption correction.
R(int) was 0.0441 before and 0.0394 after correction.
The Ratio of minimum to maximum transmission is 0.4030.
The l/2 correction factor is 0.0015.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexDuo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6875
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.49
_diffrn_reflns_theta_max         25.02
_reflns_number_total             1772
_reflns_number_gt                1650
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0560P)²+1.6537P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1772
_refine_ls_number_parameters     248
_refine_ls_number_restraints     65
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0264
_refine_ls_wR_factor_ref         0.0952
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_restrained_S_all      1.206
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.0000 0.0000 0.0000 0.01444(17) Uani 1 2 d S . .
Fe1 Fe 0.38175(11) 0.2500 0.27654(11) 0.0153(2) Uani 1 2 d S . .
N1 N 0.2356(6) 0.1589(3) 0.1569(5) 0.0212(10) Uani 1 1 d . . .
N2 N -0.2665(15) 0.1276(9) -0.2214(16) 0.051(3) Uani 0.50 1 d P . .
N3 N -0.2631(16) 0.0598(7) 0.2083(16) 0.050(3) Uani 0.50 1 d P . .
N4 N 0.2498(7) 0.2500 0.4503(7) 0.0189(12) Uani 1 2 d S . .
N5 N 0.509(2) 0.1509(11) 0.416(2) 0.022(3) Uani 0.50 1 d PU . -1
H5A H 0.5472 0.1114 0.3528 0.027 Uiso 0.50 1 d PR . -1
H5B H 0.6029 0.1725 0.4888 0.027 Uiso 0.50 1 d PR . -1
N6 N 0.5630(18) 0.3321(11) 0.389(2) 0.019(3) Uani 0.50 1 d P . .
N7 N 0.5346(8) 0.2500 0.1150(8) 0.0304(14) Uani 1 2 d SD . .
H7A H 0.4916 0.2888 0.0349 0.037 Uiso 0.274(16) 1 d PR A -2
H7B H 0.5317 0.1964 0.0694 0.037 Uiso 0.274(16) 1 d PR A -2
H7C H 0.4664 0.2420 0.0130 0.037 Uiso 0.226(16) 1 d PR A -3
H7D H 0.6033 0.2020 0.1304 0.037 Uiso 0.226(16) 1 d PR A -3
C1 C 0.1489(7) 0.1010(4) 0.0934(7) 0.0203(12) Uani 1 1 d . . .
C2 C -0.1723(17) 0.0791(8) -0.1398(17) 0.032(3) Uani 0.50 1 d P . .
C3 C -0.1693(14) 0.0382(7) 0.1302(13) 0.026(2) Uani 0.50 1 d P . .
C4 C 0.3910(14) 0.1084(8) 0.5060(15) 0.022(3) Uani 0.50 1 d PU . -1
H4A H 0.4556 0.0764 0.6007 0.027 Uiso 0.50 1 d PR . -1
H4B H 0.3156 0.0674 0.4339 0.027 Uiso 0.50 1 d PR . -1
C5 C 0.2835(13) 0.1802(6) 0.5548(12) 0.021(2) Uani 0.50 1 d P . -1
C6 C 0.2131(17) 0.1779(8) 0.6950(15) 0.031(3) Uani 0.50 1 d P . -1
H6 H 0.2372 0.1308 0.7672 0.037 Uiso 0.50 1 d PR . -1
C7 C 0.1054(12) 0.2500 0.7236(11) 0.039(2) Uani 1 2 d S . .
H7 H 0.0629 0.2500 0.8180 0.047 Uiso 1 2 d SR . .
C8 C 0.0663(16) 0.3115(8) 0.6139(16) 0.037(3) Uani 0.50 1 d P . -1
H8 H -0.0103 0.3562 0.6268 0.045 Uiso 0.50 1 d PR . -1
C9 C 0.1426(14) 0.3128(7) 0.4797(14) 0.028(2) Uani 0.50 1 d P . -1
H9 H 0.1142 0.3584 0.4047 0.034 Uiso 0.50 1 d PR . -1
C10 C 0.7193(16) 0.2714(12) 0.190(2) 0.033(9) Uani 0.274(16) 1 d PD . -2
H10A H 0.7799 0.2929 0.1108 0.040 Uiso 0.274(16) 1 d PR A -2
H10B H 0.7815 0.2218 0.2454 0.040 Uiso 0.274(16) 1 d PR A -2
C10' C 0.645(3) 0.3269(12) 0.135(3) 0.033(8) Uani 0.226(16) 1 d PD . -3
H10C H 0.5790 0.3758 0.0805 0.039 Uiso 0.226(16) 1 d PR A -3
H10D H 0.7450 0.3177 0.0891 0.039 Uiso 0.226(16) 1 d PR A -3
C13 C 0.8434(15) 0.4425(8) 0.5206(17) 0.043(3) Uani 0.50 1 d PU . .
H13A H 0.9403 0.4794 0.5706 0.052 Uiso 0.50 1 d PR A .
C11 C 0.713(4) 0.341(2) 0.315(3) 0.026(8) Uani 0.274(16) 1 d PDU . -2
C12 C 0.856(5) 0.391(2) 0.393(5) 0.043(7) Uani 0.274(16) 1 d PU . -2
H12A H 0.9627 0.3898 0.3562 0.052 Uiso 0.274(16) 1 d PR A -2
C14 C 0.693(5) 0.443(2) 0.580(5) 0.041(8) Uani 0.274(16) 1 d P . -2
H14 H 0.6853 0.4789 0.6721 0.049 Uiso 0.274(16) 1 d PR A -2
C15 C 0.558(5) 0.388(2) 0.509(4) 0.025(6) Uani 0.274(16) 1 d P . -2
H15 H 0.4522 0.3900 0.5475 0.030 Uiso 0.274(16) 1 d PR A -2
C11' C 0.661(5) 0.353(3) 0.310(5) 0.027(8) Uani 0.226(16) 1 d PU . -3
C12' C 0.808(6) 0.410(3) 0.358(6) 0.043(8) Uani 0.226(16) 1 d PU . -3
H12B H 0.8798 0.4263 0.2841 0.052 Uiso 0.226(16) 1 d PR A -3
C14' C 0.734(6) 0.410(3) 0.617(6) 0.041(10) Uani 0.226(16) 1 d P . -3
H14' H 0.7560 0.4257 0.7309 0.049 Uiso 0.226(16) 1 d PR A -3
C15' C 0.593(5) 0.355(2) 0.552(4) 0.024(7) Uani 0.226(16) 1 d P . -3
H15' H 0.5192 0.3324 0.6194 0.029 Uiso 0.226(16) 1 d PR A -3


_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
Pt1 C1 1.980(6) . ?
Pt1 C1 1.980(6) 3 ?
Pt1 C2 1.981(13) . ?
Pt1 C2 1.981(13) 3 ?
Pt1 C3 1.992(10) . ?
Pt1 C3 1.992(10) 3 ?
Fe1 N1 1.928(4) . ?
Fe1 N1 1.928(4) 4_565 ?
Fe1 N6 1.964(17) . ?
Fe1 N6 1.964(17) 4_565 ?
Fe1 N4 1.975(6) . ?
Fe1 N7 2.008(7) . ?
Fe1 N5 2.028(18) 4_565 ?
Fe1 N5 2.028(17) . ?
N1 C1 1.164(7) . ?
N2 C2 1.152(17) . ?
N2 C14' 1.47(5) 4_464 ?
N2 C14 1.95(4) 4_464 ?
N3 C3 1.142(15) . ?
N3 C12' 1.33(5) 4_465 ?
N3 C11' 1.76(6) 4_465 ?
N3 C12 1.78(4) 4_465 ?
N3 C11 1.79(4) 4_465 ?
N3 C10' 1.916(17) 4_465 ?
N4 C9 1.334(11) 4_565 ?
N4 C9 1.334(11) . ?
N4 C5 1.366(11) 4_565 ?
N4 C5 1.366(11) . ?
N5 N6 0.584(12) 4_565 ?
N5 C4 1.47(2) . ?
N6 N5 0.584(12) 4_565 ?
N6 C11' 1.17(6) . ?
N6 C15 1.32(3) . ?
N6 C15' 1.38(4) . ?
N6 C11 1.46(4) . ?
N7 C10' 1.443(10) . ?
N7 C10' 1.443(10) 4_565 ?
N7 C10 1.477(10) . ?
N7 C10 1.477(10) 4_565 ?
C4 C5 1.494(15) . ?
C5 C6 1.413(16) . ?
C6 C7 1.438(13) . ?
C7 C8 1.300(14) 4_565 ?
C7 C8 1.300(14) . ?
C7 C6 1.438(13) 4_565 ?
C8 C9 1.393(16) . ?
C10 C11 1.499(10) . ?
C10' C11' 1.50(5) . ?
C10' N3 1.916(17) 4_665 ?
C13 C12 1.34(4) . ?
C13 C14 1.38(5) . ?
C13 C14' 1.40(6) . ?
C13 C12' 1.42(5) . ?
C11 C12 1.39(4) . ?
C11 N3 1.79(4) 4_665 ?
C12 N3 1.78(4) 4_665 ?
C14 C15 1.38(5) . ?
C14 N2 1.95(4) 4_666 ?
C11' C12' 1.44(5) . ?
C11' N3 1.76(6) 4_665 ?
C12' N3 1.33(5) 4_665 ?
C14' C15' 1.40(6) . ?
C14' N2 1.47(5) 4_666 ?

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
C1 Pt1 C1 180.0(4) . 3 ?
C1 Pt1 C2 91.2(3) . . ?
C1 Pt1 C2 88.8(3) 3 . ?
C1 Pt1 C2 88.8(3) . 3 ?
C1 Pt1 C2 91.2(3) 3 3 ?
C2 Pt1 C2 180.0(6) . 3 ?
C1 Pt1 C3 87.9(3) . . ?
C1 Pt1 C3 92.1(3) 3 . ?
C2 Pt1 C3 72.4(5) . . ?
C2 Pt1 C3 107.6(5) 3 . ?
C1 Pt1 C3 92.1(3) . 3 ?
C1 Pt1 C3 87.9(3) 3 3 ?
C2 Pt1 C3 107.6(5) . 3 ?
C2 Pt1 C3 72.4(5) 3 3 ?
C3 Pt1 C3 180.0(7) . 3 ?
N1 Fe1 N1 92.1(3) . 4_565 ?
N1 Fe1 N6 170.5(4) . . ?
N1 Fe1 N6 94.0(5) 4_565 . ?
N1 Fe1 N6 94.0(5) . 4_565 ?
N1 Fe1 N6 170.5(4) 4_565 4_565 ?
N6 Fe1 N6 79.1(9) . 4_565 ?
N1 Fe1 N4 92.04(18) . . ?
N1 Fe1 N4 92.04(18) 4_565 . ?
N6 Fe1 N4 95.1(4) . . ?
N6 Fe1 N4 95.1(4) 4_565 . ?
N1 Fe1 N7 91.33(19) . . ?
N1 Fe1 N7 91.33(19) 4_565 . ?
N6 Fe1 N7 81.2(4) . . ?
N6 Fe1 N7 81.2(4) 4_565 . ?
N4 Fe1 N7 175.1(2) . . ?
N1 Fe1 N5 172.6(5) . 4_565 ?
N1 Fe1 N5 85.5(5) 4_565 4_565 ?
N6 Fe1 N5 16.7(3) . 4_565 ?
N6 Fe1 N5 89.4(5) 4_565 4_565 ?
N4 Fe1 N5 81.0(5) . 4_565 ?
N7 Fe1 N5 95.8(5) . 4_565 ?
N1 Fe1 N5 85.5(5) . . ?
N1 Fe1 N5 172.6(5) 4_565 . ?
N6 Fe1 N5 89.4(5) . . ?
N6 Fe1 N5 16.7(3) 4_565 . ?
N4 Fe1 N5 81.0(5) . . ?
N7 Fe1 N5 95.8(5) . . ?
N5 Fe1 N5 96.1(9) 4_565 . ?
C1 N1 Fe1 175.9(4) . . ?
C2 N2 C14' 99(2) . 4_464 ?
C2 N2 C14 96.4(16) . 4_464 ?
C3 N3 C12' 117(2) . 4_465 ?
C3 N3 C11' 146.4(18) . 4_465 ?
C12' N3 C11' 53(2) 4_465 4_465 ?
C3 N3 C12 110.3(18) . 4_465 ?
C11' N3 C12 55.2(19) 4_465 4_465 ?
C3 N3 C11 133.4(14) . 4_465 ?
C12' N3 C11 46(2) 4_465 4_465 ?
C12 N3 C11 45.8(13) 4_465 4_465 ?
C3 N3 C10' 108.6(11) . 4_465 ?
C12' N3 C10' 92(2) 4_465 4_465 ?
C11' N3 C10' 47.9(16) 4_465 4_465 ?
C12 N3 C10' 89.3(15) 4_465 4_465 ?
C11 N3 C10' 47.6(6) 4_465 4_465 ?
C9 N4 C9 91.6(10) 4_565 . ?
C9 N4 C5 118.4(8) 4_565 4_565 ?
C9 N4 C5 50.1(7) . 4_565 ?
C9 N4 C5 50.1(7) 4_565 . ?
C9 N4 C5 118.4(8) . . ?
C5 N4 C5 102.3(9) 4_565 . ?
C9 N4 Fe1 126.7(5) 4_565 . ?
C9 N4 Fe1 126.7(5) . . ?
C5 N4 Fe1 114.8(5) 4_565 . ?
C5 N4 Fe1 114.8(5) . . ?
N6 N5 C4 172(4) 4_565 . ?
N6 N5 Fe1 75(3) 4_565 . ?
C4 N5 Fe1 109.8(10) . . ?
N5 N6 C11' 137(4) 4_565 . ?
C11' N6 C15 114(3) . . ?
N5 N6 C15' 58(3) 4_565 . ?
C11' N6 C15' 121(3) . . ?
N5 N6 C11 149(4) 4_565 . ?
C15 N6 C11 116(2) . . ?
C15' N6 C11 115.5(19) . . ?
N5 N6 Fe1 88(3) 4_565 . ?
C11' N6 Fe1 113(2) . . ?
C15 N6 Fe1 129.0(17) . . ?
C15' N6 Fe1 125.1(16) . . ?
C11 N6 Fe1 114.7(12) . . ?
C10' N7 C10' 108(2) . 4_565 ?
C10' N7 Fe1 111.0(10) . . ?
C10' N7 Fe1 111.0(10) 4_565 . ?
C10 N7 Fe1 113.0(8) . . ?
C10 N7 Fe1 113.0(8) 4_565 . ?
N1 C1 Pt1 176.2(5) . . ?
N2 C2 Pt1 176.9(11) . . ?
N2 C2 C14' 46.4(15) . 4_464 ?
Pt1 C2 C14' 133.6(15) . 4_464 ?
N3 C3 Pt1 178.2(12) . . ?
N5 C4 C5 106.3(11) . . ?
N4 C5 C6 120.0(9) . . ?
N4 C5 C4 115.5(9) . . ?
C6 C5 C4 124.4(10) . . ?
C5 C6 C7 118.6(10) . . ?
C8 C7 C8 92.1(12) 4_565 . ?
C8 C7 C6 52.0(7) 4_565 . ?
C8 C7 C6 118.9(9) . . ?
C8 C7 C6 118.9(9) 4_565 4_565 ?
C8 C7 C6 52.0(7) . 4_565 ?
C6 C7 C6 99.5(11) . 4_565 ?
C7 C8 C9 120.6(10) . . ?
N4 C9 C8 123.2(10) . . ?
N7 C10 C11 105.5(15) . . ?
N7 C10' C11' 104(3) . . ?
N7 C10' N3 159.9(17) . 4_665 ?
C11' C10' N3 61(2) . 4_665 ?
C12 C13 C14 121(2) . . ?
C12 C13 C14' 115(3) . . ?
C14 C13 C12' 111(3) . . ?
C14' C13 C12' 115(3) . . ?
C12 C11 N6 119(2) . . ?
C12 C11 C10 125(3) . . ?
N6 C11 C10 113(2) . . ?
C12 C11 N3 67(2) . 4_665 ?
N6 C11 N3 118(2) . 4_665 ?
C10 C11 N3 103(2) . 4_665 ?
C13 C12 C11 120(3) . . ?
C13 C12 N3 110(2) . 4_665 ?
C11 C12 N3 68(2) . 4_665 ?
C15 C14 C13 118(3) . . ?
C15 C14 N2 90(2) . 4_666 ?
C13 C14 N2 109(2) . 4_666 ?
N6 C15 C14 125(3) . . ?
N6 C11' C12' 126(4) . . ?
N6 C11' C10' 125(3) . . ?
C12' C11' C10' 108(4) . . ?
N6 C11' N3 145(4) . 4_665 ?
C12' C11' N3 48(2) . 4_665 ?
C10' C11' N3 72(2) . 4_665 ?
N3 C12' C13 138(4) 4_665 . ?
N3 C12' C11' 79(3) 4_665 . ?
C13 C12' C11' 117(4) . . ?
C13 C14' C15' 121(4) . . ?
C13 C14' N2 143(4) . 4_666 ?
C15' C14' N2 87(3) . 4_666 ?
C13 C14' C2 116(3) . 4_666 ?
C15' C14' C2 121(3) . 4_666 ?
N6 C15' C14' 118(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.306
_refine_diff_density_min         -1.993
_refine_diff_density_rms         0.305
####################################################################### 
# 
# 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_Fe-pic-Pt(CN)4-HS
_database_code_depnum_ccdc_archive 'CCDC 1050973'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Fe-pic-Pt(CN)4-HS
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C16 H16 Fe N8 Pt'
_chemical_formula_sum            'C16 H16 Fe N8 Pt'
_chemical_formula_weight         571.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   10.2838(11)
_cell_length_b                   15.6772(16)
_cell_length_c                   16.0125(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 126.470(4)
_cell_angle_gamma                90.00
_cell_volume                     2076.0(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5232
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      31.10

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1088
_exptl_absorpt_coefficient_mu    7.445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4140
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2008) was used for absorption correction.
R(int) was 0.0446 before and 0.0214 after correction.
The Ratio of minimum to maximum transmission is 0.5552.
The l/2 correction factor is 0.0015.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexDuo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13175
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.05
_diffrn_reflns_theta_max         26.73
_reflns_number_total             4405
_reflns_number_gt                3434
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0373P)²+2.7380P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4405
_refine_ls_number_parameters     284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0247
_refine_ls_wR_factor_ref         0.0817
_refine_ls_wR_factor_gt          0.0757
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 1.0000 1.0000 0.5000 0.03355(8) Uani 1 2 d S . .
Pt2 Pt 1.0000 0.5000 0.5000 0.04308(9) Uani 1 2 d S . .
Fe1 Fe 0.73854(7) 0.74718(3) 0.56684(5) 0.03503(14) Uani 1 1 d . A .
N1 N 0.8588(4) 0.8504(2) 0.5528(3) 0.0464(8) Uani 1 1 d . . .
N2 N 0.7834(6) 0.9402(3) 0.2685(3) 0.0843(14) Uani 1 1 d . . .
N3 N 0.8783(5) 0.6558(2) 0.5568(3) 0.0558(10) Uani 1 1 d . . .
N4 N 0.7782(7) 0.3780(4) 0.5201(5) 0.111(2) Uani 1 1 d . . .
N5 N 0.5493(4) 0.74456(19) 0.4017(3) 0.0430(8) Uani 1 1 d . . .
N6 N 0.5795(5) 0.6424(2) 0.5484(3) 0.0498(9) Uani 1 1 d . . .
H6A H 0.6388 0.6013 0.5954 0.060 Uiso 1 1 d R . .
H6B H 0.5077 0.6622 0.5585 0.060 Uiso 1 1 d R . .
N7 N 0.6192(5) 0.8334(2) 0.6070(3) 0.0548(9) Uani 1 1 d . . .
N8 N 0.8946(5) 0.7457(2) 0.7370(3) 0.0616(11) Uani 1 1 d . . .
H8A H 0.9328 0.6925 0.7593 0.074 Uiso 0.52(4) 1 d PR A 1
H8B H 0.9796 0.7803 0.7607 0.074 Uiso 0.52(4) 1 d PR A 1
H8'A H 0.8826 0.6960 0.7598 0.074 Uiso 0.48(4) 1 d PR A 2
H8'B H 0.9988 0.7505 0.7612 0.074 Uiso 0.48(4) 1 d PR A 2
C1 C 0.9123(5) 0.9044(2) 0.5350(3) 0.0391(9) Uani 1 1 d . . .
C2 C 0.8651(5) 0.9615(3) 0.3533(3) 0.0504(10) Uani 1 1 d . . .
C3 C 0.9257(5) 0.5997(3) 0.5373(4) 0.0485(10) Uani 1 1 d . . .
C4 C 0.8589(7) 0.4239(3) 0.5130(4) 0.0675(14) Uani 1 1 d . . .
C5 C 0.5163(6) 0.8062(3) 0.3331(3) 0.0599(12) Uani 1 1 d . . .
H5 H 0.5877 0.8518 0.3558 0.072 Uiso 1 1 calc R . .
C6 C 0.3826(7) 0.8050(4) 0.2312(4) 0.0778(16) Uani 1 1 d . . .
H6 H 0.3655 0.8486 0.1862 0.093 Uiso 1 1 calc R . .
C7 C 0.2749(8) 0.7391(4) 0.1966(4) 0.0789(18) Uani 1 1 d . . .
H7 H 0.1821 0.7377 0.1284 0.095 Uiso 1 1 calc R . .
C8 C 0.3069(6) 0.6750(3) 0.2651(4) 0.0655(13) Uani 1 1 d . . .
H8 H 0.2356 0.6295 0.2437 0.079 Uiso 1 1 calc R . .
C9 C 0.4466(5) 0.6788(2) 0.3666(3) 0.0435(9) Uani 1 1 d . . .
C10 C 0.4948(5) 0.6080(3) 0.4435(3) 0.0492(10) Uani 1 1 d . . .
H10A H 0.3991 0.5774 0.4252 0.059 Uiso 1 1 calc R . .
H10B H 0.5645 0.5681 0.4410 0.059 Uiso 1 1 calc R . .
C13 C 0.4914(10) 0.9444(4) 0.6751(8) 0.097(2) Uani 1 1 d . . .
H13 H 0.4411 0.9767 0.6972 0.117 Uiso 1 1 calc R A 1
C11 C 0.505(4) 0.8932(17) 0.544(2) 0.070(6) Uani 0.52(4) 1 d P A 1
H11 H 0.4680 0.8989 0.4752 0.084 Uiso 0.52(4) 1 calc PR A 1
C12 C 0.442(3) 0.9472(17) 0.585(2) 0.078(6) Uani 0.52(4) 1 d P A 1
H12 H 0.3605 0.9857 0.5410 0.093 Uiso 0.52(4) 1 calc PR A 1
C14 C 0.633(7) 0.889(2) 0.751(4) 0.065(6) Uani 0.52(4) 1 d P A 1
H14 H 0.6833 0.8915 0.8223 0.078 Uiso 0.52(4) 1 calc PR A 1
C15 C 0.682(6) 0.837(3) 0.711(3) 0.047(5) Uani 0.52(4) 1 d P A 1
C16 C 0.810(2) 0.7729(10) 0.7799(11) 0.052(4) Uani 0.52(4) 1 d P A 1
H16A H 0.8868 0.7977 0.8480 0.062 Uiso 0.52(4) 1 calc PR A 1
H16B H 0.7611 0.7237 0.7879 0.062 Uiso 0.52(4) 1 calc PR A 1
C11' C 0.462(4) 0.8653(19) 0.533(3) 0.075(6) Uani 0.48(4) 1 d P A 2
H11' H 0.4053 0.8471 0.4649 0.090 Uiso 0.48(4) 1 calc PR A 2
C12' C 0.393(4) 0.9197(19) 0.558(3) 0.094(8) Uani 0.48(4) 1 d P A 2
H12' H 0.2911 0.9423 0.5083 0.112 Uiso 0.48(4) 1 calc PR A 2
C14' C 0.617(7) 0.912(3) 0.733(4) 0.082(9) Uani 0.48(4) 1 d P A 2
H14' H 0.6732 0.9243 0.8033 0.099 Uiso 0.48(4) 1 calc PR A 2
C15' C 0.696(7) 0.851(3) 0.703(4) 0.068(9) Uani 0.48(4) 1 d P A 2
C16' C 0.853(3) 0.813(2) 0.7732(17) 0.122(11) Uani 0.48(4) 1 d P A 2
H16C H 0.9327 0.8581 0.7963 0.146 Uiso 0.48(4) 1 calc PR A 2
H16D H 0.8612 0.7938 0.8337 0.146 Uiso 0.48(4) 1 calc PR 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
Pt1 C2 1.983(4) . ?
Pt1 C2 1.983(4) 3_776 ?
Pt1 C1 1.993(4) 3_776 ?
Pt1 C1 1.993(4) . ?
Pt2 C3 1.982(4) 3_766 ?
Pt2 C3 1.982(4) . ?
Pt2 C4 1.983(6) 3_766 ?
Pt2 C4 1.983(6) . ?
Fe1 N3 2.102(3) . ?
Fe1 N1 2.129(4) . ?
Fe1 N5 2.160(4) . ?
Fe1 N7 2.165(4) . ?
Fe1 N8 2.191(4) . ?
Fe1 N6 2.210(3) . ?
N1 C1 1.135(5) . ?
N2 C2 1.142(5) . ?
N3 C3 1.136(5) . ?
N4 C4 1.154(7) . ?
N5 C9 1.338(5) . ?
N5 C5 1.346(5) . ?
N6 C10 1.460(5) . ?
N7 C15' 1.27(5) . ?
N7 C11 1.37(3) . ?
N7 C15 1.38(4) . ?
N7 C11' 1.41(3) . ?
N8 C16' 1.395(19) . ?
N8 C16 1.456(14) . ?
C5 C6 1.373(6) . ?
C6 C7 1.368(8) . ?
C7 C8 1.376(7) . ?
C8 C9 1.390(6) . ?
C9 C10 1.505(6) . ?
C13 C14' 1.17(5) . ?
C13 C12 1.21(3) . ?
C13 C14 1.50(4) . ?
C13 C12' 1.56(4) . ?
C11 C12 1.44(4) . ?
C14 C15 1.31(6) . ?
C15 C16 1.49(6) . ?
C11' C12' 1.31(4) . ?
C14' C15' 1.51(7) . ?
C15' C16' 1.43(6) . ?

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
C2 Pt1 C2 180.000(1) . 3_776 ?
C2 Pt1 C1 90.59(17) . 3_776 ?
C2 Pt1 C1 89.41(17) 3_776 3_776 ?
C2 Pt1 C1 89.41(17) . . ?
C2 Pt1 C1 90.59(17) 3_776 . ?
C1 Pt1 C1 180.000(1) 3_776 . ?
C3 Pt2 C3 180.000(1) 3_766 . ?
C3 Pt2 C4 90.34(18) 3_766 3_766 ?
C3 Pt2 C4 89.66(18) . 3_766 ?
C3 Pt2 C4 89.66(18) 3_766 . ?
C3 Pt2 C4 90.34(18) . . ?
C4 Pt2 C4 180.0(2) 3_766 . ?
N3 Fe1 N1 92.48(16) . . ?
N3 Fe1 N5 93.02(15) . . ?
N1 Fe1 N5 92.42(13) . . ?
N3 Fe1 N7 169.27(16) . . ?
N1 Fe1 N7 91.39(14) . . ?
N5 Fe1 N7 96.81(15) . . ?
N3 Fe1 N8 93.38(15) . . ?
N1 Fe1 N8 95.60(15) . . ?
N5 Fe1 N8 169.50(16) . . ?
N7 Fe1 N8 76.28(15) . . ?
N3 Fe1 N6 88.20(14) . . ?
N1 Fe1 N6 168.85(13) . . ?
N5 Fe1 N6 76.44(13) . . ?
N7 Fe1 N6 89.94(15) . . ?
N8 Fe1 N6 95.46(15) . . ?
C1 N1 Fe1 173.2(4) . . ?
C3 N3 Fe1 166.8(4) . . ?
C9 N5 C5 117.3(4) . . ?
C9 N5 Fe1 116.1(3) . . ?
C5 N5 Fe1 126.3(3) . . ?
C10 N6 Fe1 108.5(2) . . ?
C15' N7 C11 113(3) . . ?
C11 N7 C15 116(2) . . ?
C15' N7 C11' 121(3) . . ?
C15 N7 C11' 118(3) . . ?
C15' N7 Fe1 116(3) . . ?
C11 N7 Fe1 126.8(12) . . ?
C15 N7 Fe1 116(2) . . ?
C11' N7 Fe1 123.0(14) . . ?
C16' N8 Fe1 109.3(10) . . ?
C16 N8 Fe1 112.5(6) . . ?
N1 C1 Pt1 178.4(4) . . ?
N2 C2 Pt1 178.0(5) . . ?
N3 C3 Pt2 177.8(4) . . ?
N4 C4 Pt2 178.4(5) . . ?
N5 C5 C6 123.3(4) . . ?
C7 C6 C5 119.3(5) . . ?
C6 C7 C8 118.5(5) . . ?
C7 C8 C9 119.5(5) . . ?
N5 C9 C8 122.1(4) . . ?
N5 C9 C10 115.6(4) . . ?
C8 C9 C10 122.3(4) . . ?
N6 C10 C9 110.4(3) . . ?
C14' C13 C12 116(3) . . ?
C12 C13 C14 120(2) . . ?
C14' C13 C12' 118(3) . . ?
C14 C13 C12' 117(2) . . ?
N7 C11 C12 119(2) . . ?
C13 C12 C11 123(2) . . ?
C15 C14 C13 116(4) . . ?
C14 C15 N7 125(4) . . ?
C14 C15 C16 119(3) . . ?
N7 C15 C16 116(3) . . ?
N8 C16 C15 111.1(14) . . ?
C12' C11' N7 123(3) . . ?
C11' C12' C13 116(3) . . ?
C13 C14' C15' 125(5) . . ?
N7 C15' C16' 118(4) . . ?
N7 C15' C14' 117(5) . . ?
C16' C15' C14' 125(4) . . ?
N8 C16' C15' 118(2) . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.73
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.897
_refine_diff_density_rms         0.101
####################################################################### 
# 
# 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_fe-pypz-pd(cn)4-ls
_database_code_depnum_ccdc_archive 'CCDC 1050974'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Fe-pypz-Pd(CN)4-LS
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C20 H14 Fe N10 Pd'
_chemical_formula_sum            'C20 H14 Fe N10 Pd'
_chemical_formula_weight         556.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   14.255(3)
_cell_length_b                   10.247(2)
_cell_length_c                   14.539(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.489(4)
_cell_angle_gamma                90.00
_cell_volume                     2094.8(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2775
_cell_measurement_theta_min      2.4595
_cell_measurement_theta_max      27.34

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    1.582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5676
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2008) was used for absorption correction.
R(int) was 0.0925 before and 0.0456 after correction.
The Ratio of minimum to maximum transmission is 0.7612.
The l/2 correction factor is 0.0015.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexDuo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9008
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.46
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2404
_reflns_number_gt                2092
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0392P)²+0.8806P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2404
_refine_ls_number_parameters     147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0308
_refine_ls_wR_factor_ref         0.0756
_refine_ls_wR_factor_gt          0.0721
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.0000 0.5000 0.5000 0.01274(10) Uani 1 2 d S . .
Fe1 Fe 0.0000 0.84040(5) 0.2500 0.01227(13) Uani 1 2 d S . .
N1 N 0.02352(15) 0.7052(2) 0.34562(15) 0.0144(5) Uani 1 1 d . . .
N2 N -0.21681(18) 0.5093(3) 0.41407(19) 0.0273(6) Uani 1 1 d . . .
N3 N 0.13276(15) 0.8533(2) 0.22576(14) 0.0141(4) Uani 1 1 d . . .
N4 N 0.01598(16) 0.9778(2) 0.34445(15) 0.0147(5) Uani 1 1 d . . .
N5 N 0.08639(16) 1.0552(2) 0.38552(15) 0.0168(5) Uani 1 1 d . . .
H5A H 0.1451 1.0468 0.3796 0.020 Uiso 1 1 calc R . .
C1 C 0.01998(18) 0.6285(3) 0.40186(18) 0.0154(5) Uani 1 1 d . . .
C2 C -0.1379(2) 0.5041(3) 0.44558(19) 0.0186(6) Uani 1 1 d . . .
C3 C 0.2056(2) 0.7754(3) 0.26007(19) 0.0195(6) Uani 1 1 d . . .
H3 H 0.1955 0.7093 0.3012 0.023 Uiso 1 1 calc R . .
C4 C 0.2950(2) 0.7896(3) 0.2366(2) 0.0226(6) Uani 1 1 d . . .
H4 H 0.3441 0.7340 0.2620 0.027 Uiso 1 1 calc R . .
C5 C 0.3111(2) 0.8864(3) 0.17545(19) 0.0218(6) Uani 1 1 d . . .
H5 H 0.3710 0.8973 0.1591 0.026 Uiso 1 1 calc R . .
C6 C 0.2366(2) 0.9673(3) 0.13875(19) 0.0182(6) Uani 1 1 d . . .
H6 H 0.2454 1.0333 0.0971 0.022 Uiso 1 1 calc R . .
C7 C 0.14862(19) 0.9483(3) 0.16517(18) 0.0152(5) Uani 1 1 d . . .
C8 C -0.0637(2) 1.0228(2) 0.37041(18) 0.0152(5) Uani 1 1 d . . .
C9 C -0.04346(19) 1.1309(3) 0.42980(18) 0.0186(6) Uani 1 1 d . . .
H9 H -0.0859 1.1799 0.4578 0.022 Uiso 1 1 calc R . .
C10 C 0.05300(19) 1.1480(3) 0.43725(18) 0.0188(6) Uani 1 1 d . . .
H10 H 0.0889 1.2122 0.4719 0.023 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C2 1.995(3) 5_566 ?
Pd1 C2 1.995(3) . ?
Pd1 C1 1.996(3) . ?
Pd1 C1 1.996(3) 5_566 ?
Fe1 N1 1.952(2) 2 ?
Fe1 N1 1.952(2) . ?
Fe1 N4 1.953(2) . ?
Fe1 N4 1.953(2) 2 ?
Fe1 N3 1.986(2) . ?
Fe1 N3 1.986(2) 2 ?
N1 C1 1.142(3) . ?
N2 C2 1.144(4) . ?
N3 C3 1.339(3) . ?
N3 C7 1.356(3) . ?
N4 C8 1.337(4) . ?
N4 N5 1.340(3) . ?
N5 C10 1.347(3) . ?
N5 H5A 0.8600 . ?
C3 C4 1.380(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.383(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.384(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.452(4) 2 ?
C8 C9 1.405(4) . ?
C8 C7 1.452(4) 2 ?
C9 C10 1.373(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Pd1 C2 180.00(7) 5_566 . ?
C2 Pd1 C1 92.86(11) 5_566 . ?
C2 Pd1 C1 87.14(11) . . ?
C2 Pd1 C1 87.14(11) 5_566 5_566 ?
C2 Pd1 C1 92.86(11) . 5_566 ?
C1 Pd1 C1 180.000(1) . 5_566 ?
N1 Fe1 N1 89.58(13) 2 . ?
N1 Fe1 N4 176.82(9) 2 . ?
N1 Fe1 N4 91.39(9) . . ?
N1 Fe1 N4 91.39(9) 2 2 ?
N1 Fe1 N4 176.82(9) . 2 ?
N4 Fe1 N4 87.80(13) . 2 ?
N1 Fe1 N3 88.72(9) 2 . ?
N1 Fe1 N3 96.71(9) . . ?
N4 Fe1 N3 94.17(9) . . ?
N4 Fe1 N3 80.29(9) 2 . ?
N1 Fe1 N3 96.71(9) 2 2 ?
N1 Fe1 N3 88.72(9) . 2 ?
N4 Fe1 N3 80.29(9) . 2 ?
N4 Fe1 N3 94.17(9) 2 2 ?
N3 Fe1 N3 172.36(13) . 2 ?
C1 N1 Fe1 167.5(2) . . ?
C3 N3 C7 117.9(2) . . ?
C3 N3 Fe1 126.66(19) . . ?
C7 N3 Fe1 115.39(17) . . ?
C8 N4 N5 106.2(2) . . ?
C8 N4 Fe1 116.17(18) . . ?
N5 N4 Fe1 137.04(18) . . ?
N4 N5 C10 111.0(2) . . ?
N4 N5 H5A 124.5 . . ?
C10 N5 H5A 124.5 . . ?
N1 C1 Pd1 174.1(2) . . ?
N2 C2 Pd1 178.5(3) . . ?
N3 C3 C4 122.4(3) . . ?
N3 C3 H3 118.8 . . ?
C4 C3 H3 118.8 . . ?
C5 C4 C3 119.6(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 118.8(3) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C5 C6 C7 118.8(3) . . ?
C5 C6 H6 120.6 . . ?
C7 C6 H6 120.6 . . ?
N3 C7 C6 122.5(2) . . ?
N3 C7 C8 113.0(2) . 2 ?
C6 C7 C8 124.5(3) . 2 ?
N4 C8 C9 110.3(2) . . ?
N4 C8 C7 114.5(2) . 2 ?
C9 C8 C7 135.1(3) . 2 ?
C10 C9 C8 104.5(2) . . ?
C10 C9 H9 127.7 . . ?
C8 C9 H9 127.7 . . ?
N5 C10 C9 107.9(2) . . ?
N5 C10 H10 126.0 . . ?
C9 C10 H10 126.0 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.105
####################################################################### 
# 
# 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_fe-pypz-pd(cn)4-HS
_database_code_depnum_ccdc_archive 'CCDC 1050975'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Fe-pypz-Pd(CN)4
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C20 H14 Fe N10 Pd'
_chemical_formula_sum            'C20 H14 Fe N10 Pd'
_chemical_formula_weight         556.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   14.377(3)
_cell_length_b                   10.470(2)
_cell_length_c                   15.253(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.588(4)
_cell_angle_gamma                90.00
_cell_volume                     2241.0(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1534
_cell_measurement_theta_min      2.627
_cell_measurement_theta_max      23.435

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1104
_exptl_absorpt_coefficient_mu    1.479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6796
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2008) was used for absorption correction.
R(int) was 0.1310 before and 0.0395 after correction.
The Ratio of minimum to maximum transmission is 0.9114.
The l/2 correction factor is 0.0015.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexDuo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7510
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.43
_diffrn_reflns_theta_max         27.55
_reflns_number_total             2588
_reflns_number_gt                2018
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0309P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2588
_refine_ls_number_parameters     147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0718
_refine_ls_wR_factor_gt          0.0660
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.005
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.0000 0.5000 0.5000 0.02720(10) Uani 1 2 d S . .
Fe1 Fe 0.0000 0.83492(5) 0.2500 0.02720(15) Uani 1 2 d S . .
N1 N 0.03464(18) 0.6919(2) 0.35224(17) 0.0372(6) Uani 1 1 d . . .
N2 N -0.2185(2) 0.5292(3) 0.4171(2) 0.0622(9) Uani 1 1 d . . .
N3 N 0.14307(16) 0.8623(2) 0.22511(16) 0.0315(6) Uani 1 1 d . . .
N4 N 0.01525(17) 0.9863(2) 0.35070(16) 0.0301(5) Uani 1 1 d . . .
N5 N 0.08298(18) 1.0673(2) 0.39356(17) 0.0370(6) Uani 1 1 d . . .
H5A H 0.1420 1.0637 0.3906 0.044 Uiso 1 1 calc R . .
C1 C 0.0248(2) 0.6199(3) 0.4062(2) 0.0303(7) Uani 1 1 d . . .
C2 C -0.1385(2) 0.5172(3) 0.4470(2) 0.0400(8) Uani 1 1 d . . .
C3 C 0.2196(2) 0.7903(3) 0.2593(2) 0.0461(9) Uani 1 1 d . . .
H3 H 0.2140 0.7274 0.3009 0.055 Uiso 1 1 calc R . .
C4 C 0.3058(2) 0.8055(3) 0.2356(3) 0.0528(10) Uani 1 1 d . . .
H4 H 0.3573 0.7540 0.2611 0.063 Uiso 1 1 calc R . .
C5 C 0.3152(2) 0.8973(3) 0.1741(3) 0.0509(9) Uani 1 1 d . . .
H5 H 0.3731 0.9091 0.1574 0.061 Uiso 1 1 calc R . .
C6 C 0.2376(2) 0.9717(3) 0.1373(2) 0.0406(8) Uani 1 1 d . . .
H6 H 0.2422 1.0341 0.0950 0.049 Uiso 1 1 calc R . .
C7 C 0.1527(2) 0.9524(3) 0.1641(2) 0.0297(6) Uani 1 1 d . . .
C8 C -0.0655(2) 1.0260(3) 0.3728(2) 0.0295(7) Uani 1 1 d . . .
C9 C -0.0483(2) 1.1315(3) 0.4299(2) 0.0397(8) Uani 1 1 d . . .
H9 H -0.0920 1.1765 0.4546 0.048 Uiso 1 1 calc R . .
C10 C 0.0468(2) 1.1539(3) 0.4411(2) 0.0409(8) Uani 1 1 d . . .
H10 H 0.0808 1.2185 0.4760 0.049 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C2 1.987(4) 5_566 ?
Pd1 C2 1.987(4) . ?
Pd1 C1 1.993(3) 5_566 ?
Pd1 C1 1.993(3) . ?
Fe1 N1 2.141(3) 2 ?
Fe1 N1 2.141(3) . ?
Fe1 N4 2.185(2) . ?
Fe1 N4 2.185(2) 2 ?
Fe1 N3 2.190(2) . ?
Fe1 N3 2.190(2) 2 ?
N1 C1 1.147(4) . ?
N2 C2 1.147(4) . ?
N3 C3 1.342(4) . ?
N3 C7 1.353(4) . ?
N4 C8 1.343(4) . ?
N4 N5 1.348(3) . ?
N5 C10 1.335(4) . ?
N5 H5A 0.8600 . ?
C3 C4 1.374(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.370(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.376(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.385(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.475(4) 2 ?
C8 C9 1.395(4) . ?
C8 C7 1.475(4) 2 ?
C9 C10 1.361(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Pd1 C2 180.0 5_566 . ?
C2 Pd1 C1 88.31(12) 5_566 5_566 ?
C2 Pd1 C1 91.69(12) . 5_566 ?
C2 Pd1 C1 91.69(12) 5_566 . ?
C2 Pd1 C1 88.31(12) . . ?
C1 Pd1 C1 180.0 5_566 . ?
N1 Fe1 N1 91.24(14) 2 . ?
N1 Fe1 N4 172.45(9) 2 . ?
N1 Fe1 N4 91.36(9) . . ?
N1 Fe1 N4 91.36(9) 2 2 ?
N1 Fe1 N4 172.45(9) . 2 ?
N4 Fe1 N4 86.96(12) . 2 ?
N1 Fe1 N3 92.50(9) 2 . ?
N1 Fe1 N3 98.04(9) . . ?
N4 Fe1 N3 94.16(9) . . ?
N4 Fe1 N3 74.76(9) 2 . ?
N1 Fe1 N3 98.04(9) 2 2 ?
N1 Fe1 N3 92.50(9) . 2 ?
N4 Fe1 N3 74.76(9) . 2 ?
N4 Fe1 N3 94.16(9) 2 2 ?
N3 Fe1 N3 164.93(13) . 2 ?
C1 N1 Fe1 159.5(2) . . ?
C3 N3 C7 117.4(3) . . ?
C3 N3 Fe1 125.5(2) . . ?
C7 N3 Fe1 116.81(19) . . ?
C8 N4 N5 104.8(2) . . ?
C8 N4 Fe1 116.17(18) . . ?
N5 N4 Fe1 138.47(19) . . ?
C10 N5 N4 111.4(3) . . ?
C10 N5 H5A 124.3 . . ?
N4 N5 H5A 124.3 . . ?
N1 C1 Pd1 176.5(3) . . ?
N2 C2 Pd1 178.8(3) . . ?
N3 C3 C4 122.9(3) . . ?
N3 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 119.0(3) . . ?
C4 C5 H5 120.5 . . ?
C6 C5 H5 120.5 . . ?
C5 C6 C7 119.0(3) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
N3 C7 C6 122.3(3) . . ?
N3 C7 C8 114.9(3) . 2 ?
C6 C7 C8 122.8(3) . 2 ?
N4 C8 C9 110.9(3) . . ?
N4 C8 C7 116.9(2) . 2 ?
C9 C8 C7 132.3(3) . 2 ?
C10 C9 C8 104.6(3) . . ?
C10 C9 H9 127.7 . . ?
C8 C9 H9 127.7 . . ?
N5 C10 C9 108.3(3) . . ?
N5 C10 H10 125.9 . . ?
C9 C10 H10 125.9 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N5 H5A N2 0.86 1.99 2.827(4) 163.6 3

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.081
####################################################################### 
# 
# 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_fe-pypz-pt(cn)4-ls
_database_code_depnum_ccdc_archive 'CCDC 1050976'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Fe-pypz-Pt(CN)4-LS
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C20 H14 Fe N10 Pt'
_chemical_formula_sum            'C20 H14 Fe N10 Pt'
_chemical_formula_weight         645.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   14.269(3)
_cell_length_b                   10.366(2)
_cell_length_c                   14.532(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.222(4)
_cell_angle_gamma                90.00
_cell_volume                     2121.7(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    2920
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      27.38

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.020
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    7.301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3536
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2008) was used for absorption correction.
R(int) was 0.1070 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.4742.
The l/2 correction factor is 0.0015.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexDuo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8699
_diffrn_reflns_av_R_equivalents  0.0587
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.44
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2420
_reflns_number_gt                1854
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0308P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2420
_refine_ls_number_parameters     147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0696
_refine_ls_wR_factor_gt          0.0635
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.0000 0.5000 0.5000 0.01193(9) Uani 1 2 d S . .
Fe1 Fe 0.0000 0.83910(9) 0.2500 0.0118(2) Uani 1 2 d S . .
N1 N 0.0236(3) 0.7063(3) 0.3461(2) 0.0141(8) Uani 1 1 d . . .
N2 N -0.2165(3) 0.5042(4) 0.4129(3) 0.0266(10) Uani 1 1 d . . .
N3 N 0.1332(3) 0.8522(4) 0.2255(2) 0.0145(8) Uani 1 1 d . . .
N4 N 0.0156(3) 0.9757(4) 0.3447(3) 0.0146(9) Uani 1 1 d . . .
N5 N 0.0863(3) 1.0534(4) 0.3852(3) 0.0155(8) Uani 1 1 d . . .
H5A H 0.1450 1.0450 0.3793 0.019 Uiso 1 1 calc R . .
C1 C 0.0198(3) 0.6284(4) 0.4028(3) 0.0151(9) Uani 1 1 d . . .
C2 C -0.1379(3) 0.5008(4) 0.4449(3) 0.0158(9) Uani 1 1 d . . .
C3 C 0.2053(4) 0.7739(5) 0.2586(3) 0.0206(11) Uani 1 1 d . . .
H3 H 0.1945 0.7075 0.2986 0.025 Uiso 1 1 calc R . .
C4 C 0.2954(3) 0.7877(5) 0.2358(4) 0.0212(11) Uani 1 1 d . . .
H4 H 0.3442 0.7324 0.2610 0.025 Uiso 1 1 calc R . .
C5 C 0.3119(4) 0.8851(5) 0.1747(3) 0.0215(11) Uani 1 1 d . . .
H5 H 0.3718 0.8961 0.1585 0.026 Uiso 1 1 calc R . .
C6 C 0.2376(4) 0.9660(5) 0.1382(4) 0.0178(10) Uani 1 1 d . . .
H6 H 0.2466 1.0315 0.0967 0.021 Uiso 1 1 calc R . .
C7 C 0.1493(3) 0.9470(4) 0.1649(3) 0.0137(9) Uani 1 1 d . . .
C8 C -0.0648(3) 1.0210(4) 0.3702(3) 0.0139(9) Uani 1 1 d . . .
C9 C -0.0447(3) 1.1296(5) 0.4282(3) 0.0204(11) Uani 1 1 d . . .
H9 H -0.0873 1.1792 0.4553 0.024 Uiso 1 1 calc R . .
C10 C 0.0524(3) 1.1459(5) 0.4361(3) 0.0191(10) Uani 1 1 d . . .
H10 H 0.0882 1.2097 0.4706 0.023 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C1 1.993(5) . ?
Pt1 C1 1.993(5) 5_566 ?
Pt1 C2 2.002(5) 5_566 ?
Pt1 C2 2.002(5) . ?
Fe1 N1 1.951(4) 2 ?
Fe1 N1 1.951(4) . ?
Fe1 N4 1.962(4) . ?
Fe1 N4 1.962(4) 2 ?
Fe1 N3 1.994(4) . ?
Fe1 N3 1.994(4) 2 ?
N1 C1 1.162(6) . ?
N2 C2 1.144(7) . ?
N3 C3 1.338(6) . ?
N3 C7 1.362(6) . ?
N4 C8 1.345(6) . ?
N4 N5 1.350(6) . ?
N5 C10 1.348(6) . ?
N5 H5A 0.8600 . ?
C3 C4 1.385(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.390(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.389(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.391(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.451(7) 2 ?
C8 C9 1.408(6) . ?
C8 C7 1.451(7) 2 ?
C9 C10 1.383(7) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Pt1 C1 180.000(1) . 5_566 ?
C1 Pt1 C2 92.56(18) . 5_566 ?
C1 Pt1 C2 87.44(18) 5_566 5_566 ?
C1 Pt1 C2 87.44(18) . . ?
C1 Pt1 C2 92.56(18) 5_566 . ?
C2 Pt1 C2 180.0 5_566 . ?
N1 Fe1 N1 90.3(2) 2 . ?
N1 Fe1 N4 176.52(17) 2 . ?
N1 Fe1 N4 91.13(15) . . ?
N1 Fe1 N4 91.13(15) 2 2 ?
N1 Fe1 N4 176.52(17) . 2 ?
N4 Fe1 N4 87.7(2) . 2 ?
N1 Fe1 N3 88.87(15) 2 . ?
N1 Fe1 N3 96.64(16) . . ?
N4 Fe1 N3 94.13(16) . . ?
N4 Fe1 N3 80.20(16) 2 . ?
N1 Fe1 N3 96.64(16) 2 2 ?
N1 Fe1 N3 88.87(15) . 2 ?
N4 Fe1 N3 80.20(16) . 2 ?
N4 Fe1 N3 94.13(16) 2 2 ?
N3 Fe1 N3 172.2(2) . 2 ?
C1 N1 Fe1 167.4(4) . . ?
C3 N3 C7 118.1(4) . . ?
C3 N3 Fe1 126.5(3) . . ?
C7 N3 Fe1 115.3(3) . . ?
C8 N4 N5 106.4(4) . . ?
C8 N4 Fe1 116.1(3) . . ?
N5 N4 Fe1 136.8(3) . . ?
C10 N5 N4 110.8(4) . . ?
C10 N5 H5A 124.6 . . ?
N4 N5 H5A 124.6 . . ?
N1 C1 Pt1 174.4(4) . . ?
N2 C2 Pt1 178.4(5) . . ?
N3 C3 C4 122.8(5) . . ?
N3 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C3 C4 C5 119.1(5) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 119.1(5) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C7 118.5(4) . . ?
C5 C6 H6 120.7 . . ?
C7 C6 H6 120.7 . . ?
N3 C7 C6 122.4(4) . . ?
N3 C7 C8 113.1(4) . 2 ?
C6 C7 C8 124.4(4) . 2 ?
N4 C8 C9 110.1(4) . . ?
N4 C8 C7 114.5(4) . 2 ?
C9 C8 C7 135.3(4) . 2 ?
C10 C9 C8 104.6(4) . . ?
C10 C9 H9 127.7 . . ?
C8 C9 H9 127.7 . . ?
N5 C10 C9 108.1(4) . . ?
N5 C10 H10 126.0 . . ?
C9 C10 H10 126.0 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         2.895
_refine_diff_density_min         -2.055
_refine_diff_density_rms         0.182
####################################################################### 
# 
# 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_fe-pypz-pt(cn)4-hs
_database_code_depnum_ccdc_archive 'CCDC 1050977'
_audit_update_record             
;
2015-04-10 deposited with the CCDC.
2015-04-29 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            Fe-pypz-Pt(CN)4-HS
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C20 H14 Fe N10 Pt'
_chemical_formula_sum            'C20 H14 Fe N10 Pt'
_chemical_formula_weight         645.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   14.304(3)
_cell_length_b                   10.523(2)
_cell_length_c                   15.157(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.323(4)
_cell_angle_gamma                90.00
_cell_volume                     2228.9(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3190
_cell_measurement_theta_min      2.42
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    6.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5242
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   
;
SADABS v.2.10 (Bruker,2008) was used for absorption correction.
R(int) was 0.0545 before and 0.0230 after correction.
The Ratio of minimum to maximum transmission is 0.7030.
The l/2 correction factor is 0.0015.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker ApexDuo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7442
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.42
_diffrn_reflns_theta_max         27.54
_reflns_number_total             2575
_reflns_number_gt                2108
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0185P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2575
_refine_ls_number_parameters     147
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0174
_refine_ls_wR_factor_ref         0.0408
_refine_ls_wR_factor_gt          0.0379
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.0000 0.5000 0.5000 0.02616(5) Uani 1 2 d S . .
Fe1 Fe 0.0000 0.83374(5) 0.2500 0.02677(12) Uani 1 2 d S . .
N1 N 0.03525(16) 0.6916(2) 0.35260(14) 0.0381(6) Uani 1 1 d . . .
N2 N -0.2185(2) 0.5268(3) 0.4155(2) 0.0610(9) Uani 1 1 d . . .
N3 N 0.14357(14) 0.8602(2) 0.22469(14) 0.0320(5) Uani 1 1 d . . .
N4 N 0.01492(16) 0.9846(2) 0.35086(16) 0.0297(5) Uani 1 1 d . . .
N5 N 0.08262(16) 1.0659(2) 0.39308(15) 0.0364(6) Uani 1 1 d . . .
H5A H 0.1420 1.0620 0.3902 0.044 Uiso 1 1 calc R . .
C1 C 0.02432(18) 0.6208(3) 0.40641(17) 0.0308(6) Uani 1 1 d . . .
C2 C -0.1386(2) 0.5151(3) 0.4465(2) 0.0389(7) Uani 1 1 d . . .
C3 C 0.2196(2) 0.7884(3) 0.2584(2) 0.0436(7) Uani 1 1 d . . .
H3 H 0.2136 0.7251 0.2997 0.052 Uiso 1 1 calc R . .
C4 C 0.3070(2) 0.8043(3) 0.2348(2) 0.0524(9) Uani 1 1 d . . .
H4 H 0.3588 0.7531 0.2602 0.063 Uiso 1 1 calc R . .
C5 C 0.3162(2) 0.8954(3) 0.1739(2) 0.0506(8) Uani 1 1 d . . .
H5 H 0.3744 0.9072 0.1570 0.061 Uiso 1 1 calc R . .
C6 C 0.2392(2) 0.9700(3) 0.1373(2) 0.0407(8) Uani 1 1 d . . .
H6 H 0.2444 1.0325 0.0953 0.049 Uiso 1 1 calc R . .
C7 C 0.15339(19) 0.9508(3) 0.16413(18) 0.0290(6) Uani 1 1 d . . .
C8 C -0.0663(2) 1.0246(2) 0.37250(18) 0.0293(6) Uani 1 1 d . . .
C9 C -0.0496(2) 1.1300(3) 0.42880(18) 0.0391(7) Uani 1 1 d . . .
H9 H -0.0941 1.1747 0.4534 0.047 Uiso 1 1 calc R . .
C10 C 0.0458(2) 1.1538(3) 0.44029(18) 0.0425(7) Uani 1 1 d . . .
H10 H 0.0793 1.2190 0.4746 0.051 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pt1 C2 1.982(3) 5_566 ?
Pt1 C2 1.982(3) . ?
Pt1 C1 1.990(3) 5_566 ?
Pt1 C1 1.990(3) . ?
Fe1 N1 2.139(2) 2 ?
Fe1 N1 2.139(2) . ?
Fe1 N4 2.182(2) . ?
Fe1 N4 2.182(2) 2 ?
Fe1 N3 2.186(2) 2 ?
Fe1 N3 2.186(2) . ?
N1 C1 1.140(3) . ?
N2 C2 1.146(4) . ?
N3 C3 1.333(3) . ?
N3 C7 1.352(3) . ?
N4 C8 1.340(4) . ?
N4 N5 1.347(3) . ?
N5 C10 1.344(4) . ?
N5 H5A 0.8600 . ?
C3 C4 1.382(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.357(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.369(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.388(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.472(4) 2 ?
C8 C9 1.389(4) . ?
C8 C7 1.472(4) 2 ?
C9 C10 1.361(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Pt1 C2 180.000(1) 5_566 . ?
C2 Pt1 C1 88.21(11) 5_566 5_566 ?
C2 Pt1 C1 91.79(11) . 5_566 ?
C2 Pt1 C1 91.79(11) 5_566 . ?
C2 Pt1 C1 88.21(11) . . ?
C1 Pt1 C1 180.000(1) 5_566 . ?
N1 Fe1 N1 91.26(13) 2 . ?
N1 Fe1 N4 172.10(9) 2 . ?
N1 Fe1 N4 91.53(9) . . ?
N1 Fe1 N4 91.53(9) 2 2 ?
N1 Fe1 N4 172.10(9) . 2 ?
N4 Fe1 N4 86.67(12) . 2 ?
N1 Fe1 N3 97.59(8) 2 2 ?
N1 Fe1 N3 92.63(8) . 2 ?
N4 Fe1 N3 74.90(8) . 2 ?
N4 Fe1 N3 94.31(8) 2 2 ?
N1 Fe1 N3 92.63(8) 2 . ?
N1 Fe1 N3 97.59(8) . . ?
N4 Fe1 N3 94.31(8) . . ?
N4 Fe1 N3 74.90(8) 2 . ?
N3 Fe1 N3 165.37(13) 2 . ?
C1 N1 Fe1 158.5(2) . . ?
C3 N3 C7 117.8(2) . . ?
C3 N3 Fe1 125.50(19) . . ?
C7 N3 Fe1 116.53(17) . . ?
C8 N4 N5 104.9(2) . . ?
C8 N4 Fe1 116.07(18) . . ?
N5 N4 Fe1 138.38(18) . . ?
C10 N5 N4 111.5(2) . . ?
C10 N5 H5A 124.3 . . ?
N4 N5 H5A 124.3 . . ?
N1 C1 Pt1 177.7(2) . . ?
N2 C2 Pt1 178.4(3) . . ?
N3 C3 C4 122.8(3) . . ?
N3 C3 H3 118.6 . . ?
C4 C3 H3 118.6 . . ?
C5 C4 C3 119.1(3) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 119.6(3) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C5 C6 C7 118.9(3) . . ?
C5 C6 H6 120.5 . . ?
C7 C6 H6 120.5 . . ?
N3 C7 C6 121.9(3) . . ?
N3 C7 C8 115.2(2) . 2 ?
C6 C7 C8 122.9(3) . 2 ?
N4 C8 C9 110.9(2) . . ?
N4 C8 C7 116.7(2) . 2 ?
C9 C8 C7 132.3(3) . 2 ?
C10 C9 C8 105.2(3) . . ?
C10 C9 H9 127.4 . . ?
C8 C9 H9 127.4 . . ?
N5 C10 C9 107.5(3) . . ?
N5 C10 H10 126.2 . . ?
C9 C10 H10 126.2 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.54
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.083


