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

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

data_1-Pd-2H2O-200K
_database_code_depnum_ccdc_archive 'CCDC 1519487'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
#==========================================================================
_title                           
;
Guest-Modulated Room Temperature Spin Crossover with Wide Hysteresis in a
2-D Hofmann-Type Material
;

#==========================================================================  

_audit_creation_method           SHELXL-2013

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Fe(proptrz)2Pd(CN)4].2H2O'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C26 H20 Fe N12 Pd, 2(O)'
_chemical_formula_sum            'C26 H20 Fe N12 O2 Pd'
_chemical_formula_weight         694.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.2613(2)
_cell_length_b                   7.6635(3)
_cell_length_c                   13.5746(5)
_cell_angle_alpha                95.988(3)
_cell_angle_beta                 98.931(3)
_cell_angle_gamma                90.085(3)
_cell_volume                     742.04(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    4686
_cell_measurement_theta_min      71.7670
_cell_measurement_theta_max      5.8400

_exptl_crystal_description       'square plate'
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.027
_exptl_absorpt_coefficient_mu    9.196
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.440
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
 Analytical numeric absorption correction using a multifaceted crystal
 model based on expressions derived by R.C. Clark & J.S. Reid.
 (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 Crystal was mounted on a cactus needle in a thin film of paratone oil
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.0662
_diffrn_reflns_number            6469
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.314
_diffrn_reflns_theta_max         71.994
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2898
_reflns_number_gt                2822
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013), Xseed'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;Hydrogen atoms were fixed using the riding model. All non-hydrogen
 atoms, except for water oxygens, were modelled anisotropically.
 Water oxygen atoms were modelled as disordered over two positions.
 Hydrogen atoms on water guest molecules were not included due to the 
 highly disordered oxygen atoms, thus the location of these hydrogen
 atoms are ambiguous. However, for chemical completeness, the hydrogens
 are included in the chemical formula and molecular weight., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0410P)²+0.5070P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         2898
_refine_ls_number_parameters     192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0258
_refine_ls_wR_factor_ref         0.0690
_refine_ls_wR_factor_gt          0.0684
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.014
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.0000 -0.5000 0.0000 0.01753(8) Uani 1 2 d S . P . .
Fe1 Fe 0.5000 0.0000 0.0000 0.01793(11) Uani 1 2 d S . P . .
N2 N -0.2992(3) -0.2057(3) -0.00417(16) 0.0249(4) Uani 1 1 d . . . . .
N5 N 0.6249(3) 0.1431(3) 0.31937(17) 0.0339(5) Uani 1 1 d . . . . .
N4 N 0.5417(3) -0.1026(3) 0.22633(18) 0.0375(5) Uani 1 1 d . . . . .
N1 N 0.2924(3) -0.1986(3) 0.00030(16) 0.0250(4) Uani 1 1 d . . . . .
N3 N 0.5603(3) 0.0270(3) 0.16465(15) 0.0268(4) Uani 1 1 d . . . . .
N6 N 0.6763(4) 0.2523(3) 0.40866(18) 0.0439(6) Uani 1 1 d . . . . .
C2 C -0.1933(3) -0.3156(3) -0.00234(18) 0.0220(4) Uani 1 1 d . . . . .
C1 C 0.1884(3) -0.3108(3) -0.00021(17) 0.0216(4) Uani 1 1 d . . . . .
C13 C 0.8699(4) 0.7865(4) 0.7229(2) 0.0442(7) Uani 1 1 d . . . . .
H13 H 0.8548 0.6752 0.7458 0.053 Uiso 1 1 calc R U . . .
C7 C 0.7831(4) 0.6583(4) 0.5468(2) 0.0438(7) Uani 1 1 d . . . . .
C11 C 0.9449(5) 1.0934(5) 0.7586(2) 0.0482(7) Uani 1 1 d . . . . .
H11 H 0.9830 1.1920 0.8059 0.058 Uiso 1 1 calc R U . . .
C8 C 0.8371(4) 0.8047(4) 0.6208(2) 0.0373(6) Uani 1 1 d . . . . .
C12 C 0.9248(4) 0.9321(5) 0.7910(2) 0.0469(7) Uani 1 1 d . . . . .
H12 H 0.9487 0.9197 0.8608 0.056 Uiso 1 1 calc R U . . .
C3 C 0.6104(4) 0.1723(3) 0.2214(2) 0.0320(5) Uani 1 1 d . . . . .
H3 H 0.6331 0.2817 0.1979 0.038 Uiso 1 1 calc R U . . .
C10 C 0.9099(5) 1.1136(5) 0.6577(3) 0.0549(8) Uani 1 1 d . . . . .
H10 H 0.9222 1.2259 0.6354 0.066 Uiso 1 1 calc R U . . .
C4 C 0.5821(4) -0.0295(4) 0.3181(2) 0.0421(6) Uani 1 1 d . . . . .
H4 H 0.5817 -0.0888 0.3761 0.051 Uiso 1 1 calc R U . . .
C9 C 0.8570(5) 0.9692(4) 0.5890(2) 0.0468(7) Uani 1 1 d . . . . .
H9 H 0.8340 0.9827 0.5194 0.056 Uiso 1 1 calc R U . . .
C5 C 0.6871(5) 0.4137(4) 0.3987(2) 0.0455(7) Uani 1 1 d . . . . .
H5 H 0.6597 0.4515 0.3336 0.055 Uiso 1 1 calc R U . . .
C6 C 0.7395(5) 0.5403(4) 0.4829(2) 0.0489(7) Uani 1 1 d . . . . .
O1WA O 0.4629(9) -0.4638(7) 0.1929(4) 0.0555(9) Uiso 0.500(6) 1 d . U P A 7
O1WB O 0.5487(9) -0.4616(7) 0.1728(4) 0.0555(9) Uiso 0.500(6) 1 d . U P A 8

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.01035(12) 0.00828(11) 0.03427(13) 0.00156(8) 0.00495(8) -0.00022(7)
Fe1 0.0105(2) 0.0087(2) 0.0347(3) 0.00147(17) 0.00453(17) -0.00021(16)
N2 0.0168(9) 0.0155(9) 0.0428(11) 0.0026(8) 0.0059(8) 0.0035(7)
N5 0.0366(11) 0.0274(11) 0.0357(11) -0.0006(8) 0.0020(9) 0.0013(9)
N4 0.0462(13) 0.0230(10) 0.0417(12) 0.0058(9) 0.0006(10) -0.0036(9)
N1 0.0172(9) 0.0161(9) 0.0423(11) 0.0030(8) 0.0063(8) -0.0026(7)
N3 0.0247(9) 0.0184(9) 0.0371(10) 0.0017(8) 0.0046(8) 0.0006(7)
N6 0.0537(15) 0.0385(13) 0.0358(12) -0.0052(10) 0.0013(10) 0.0009(11)
C2 0.0157(10) 0.0137(10) 0.0365(12) 0.0005(8) 0.0048(8) -0.0034(8)
C1 0.0149(10) 0.0148(10) 0.0355(11) 0.0029(8) 0.0053(8) 0.0011(8)
C13 0.0477(17) 0.0442(16) 0.0401(14) 0.0051(12) 0.0040(12) 0.0035(13)
C7 0.0420(16) 0.0432(16) 0.0442(15) -0.0066(13) 0.0073(12) 0.0002(13)
C11 0.0466(17) 0.0526(19) 0.0404(15) -0.0137(13) 0.0040(12) -0.0064(14)
C8 0.0331(13) 0.0415(15) 0.0347(13) -0.0075(11) 0.0048(10) -0.0010(11)
C12 0.0446(17) 0.064(2) 0.0293(13) -0.0019(13) 0.0021(11) 0.0027(14)
C3 0.0347(13) 0.0225(11) 0.0387(13) 0.0010(10) 0.0062(10) 0.0000(10)
C10 0.071(2) 0.0442(18) 0.0470(17) 0.0019(14) 0.0048(15) -0.0149(16)
C4 0.0537(17) 0.0303(14) 0.0409(14) 0.0071(11) 0.0003(12) -0.0044(12)
C9 0.0579(19) 0.0499(18) 0.0302(13) 0.0004(12) 0.0017(12) -0.0075(15)
C5 0.0517(18) 0.0387(16) 0.0424(15) -0.0079(12) 0.0034(13) -0.0007(13)
C6 0.0495(17) 0.0450(17) 0.0485(17) -0.0082(14) 0.0053(13) 0.0001(14)

_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 C1 1.992(2) . ?
Pd1 C1 1.992(2) 2_545 ?
Pd1 C2 1.992(2) 2_545 ?
Pd1 C2 1.992(2) . ?
Fe1 N1 2.141(2) 2_655 ?
Fe1 N1 2.142(2) . ?
Fe1 N2 2.1512(19) 2 ?
Fe1 N2 2.1512(19) 1_655 ?
Fe1 N3 2.198(2) . ?
Fe1 N3 2.198(2) 2_655 ?
N2 C2 1.141(3) . ?
N2 Fe1 2.1512(19) 1_455 ?
N5 C4 1.356(4) . ?
N5 C3 1.360(3) . ?
N5 N6 1.399(3) . ?
N4 C4 1.301(4) . ?
N4 N3 1.383(3) . ?
N1 C1 1.142(3) . ?
N3 C3 1.303(3) . ?
N6 C5 1.261(4) . ?
C13 C12 1.389(4) . ?
C13 C8 1.391(4) . ?
C13 H13 0.9500 . ?
C7 C6 1.192(4) . ?
C7 C8 1.437(4) . ?
C11 C12 1.369(5) . ?
C11 C10 1.380(5) . ?
C11 H11 0.9500 . ?
C8 C9 1.389(4) . ?
C12 H12 0.9500 . ?
C3 H3 0.9500 . ?
C10 C9 1.383(4) . ?
C10 H10 0.9500 . ?
C4 H4 0.9500 . ?
C9 H9 0.9500 . ?
C5 C6 1.423(4) . ?
C5 H5 0.9500 . ?

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 Pd1 C1 180.0 . 2_545 ?
C1 Pd1 C2 92.04(9) . 2_545 ?
C1 Pd1 C2 87.96(9) 2_545 2_545 ?
C1 Pd1 C2 87.96(9) . . ?
C1 Pd1 C2 92.04(9) 2_545 . ?
C2 Pd1 C2 180.00(9) 2_545 . ?
N1 Fe1 N1 180.00(11) 2_655 . ?
N1 Fe1 N2 87.78(7) 2_655 2 ?
N1 Fe1 N2 92.22(7) . 2 ?
N1 Fe1 N2 92.22(7) 2_655 1_655 ?
N1 Fe1 N2 87.78(7) . 1_655 ?
N2 Fe1 N2 180.00(8) 2 1_655 ?
N1 Fe1 N3 88.95(8) 2_655 . ?
N1 Fe1 N3 91.05(8) . . ?
N2 Fe1 N3 90.65(7) 2 . ?
N2 Fe1 N3 89.35(7) 1_655 . ?
N1 Fe1 N3 91.05(8) 2_655 2_655 ?
N1 Fe1 N3 88.95(8) . 2_655 ?
N2 Fe1 N3 89.35(7) 2 2_655 ?
N2 Fe1 N3 90.65(7) 1_655 2_655 ?
N3 Fe1 N3 180.00(10) . 2_655 ?
C2 N2 Fe1 177.2(2) . 1_455 ?
C4 N5 C3 105.3(2) . . ?
C4 N5 N6 122.4(2) . . ?
C3 N5 N6 132.3(2) . . ?
C4 N4 N3 106.6(2) . . ?
C1 N1 Fe1 176.5(2) . . ?
C3 N3 N4 108.0(2) . . ?
C3 N3 Fe1 125.28(17) . . ?
N4 N3 Fe1 126.57(15) . . ?
C5 N6 N5 115.1(3) . . ?
N2 C2 Pd1 177.5(2) . . ?
N1 C1 Pd1 177.9(2) . . ?
C12 C13 C8 119.5(3) . . ?
C12 C13 H13 120.2 . . ?
C8 C13 H13 120.2 . . ?
C6 C7 C8 177.8(4) . . ?
C12 C11 C10 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C9 C8 C13 119.3(3) . . ?
C9 C8 C7 118.7(3) . . ?
C13 C8 C7 122.0(3) . . ?
C11 C12 C13 120.6(3) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
N3 C3 N5 109.4(2) . . ?
N3 C3 H3 125.3 . . ?
N5 C3 H3 125.3 . . ?
C11 C10 C9 119.6(3) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
N4 C4 N5 110.6(2) . . ?
N4 C4 H4 124.7 . . ?
N5 C4 H4 124.7 . . ?
C10 C9 C8 120.6(3) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
N6 C5 C6 121.4(3) . . ?
N6 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C7 C6 C5 173.5(4) . . ?

_refine_diff_density_max         0.991
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.075

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_PLAT041_1-Pd-2H2O-200K      
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: Hydrogen atoms on water guest molecules were not included due 
to the highly disordered oxygen atoms, thus the locations of these hydrogen
atoms are ambiguous. However, for chemical completeness, the hydrogens
are included in the chemical formula and molecular weight.
;
_vrf_PLAT043_1-Pd-2H2O-200K      
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.03 Check 
RESPONSE: Hydrogen atoms on water guest molecules were not included due 
to the highly disordered oxygen atoms, thus the locations of these hydrogen
atoms are ambiguous. However, for chemical completeness, the hydrogens
are included in the chemical formula and molecular weight.
;
_vrf_PLAT430_1-Pd-2H2O-200K      
;
PROBLEM: Short Inter D...A Contact  O1WA   ..  N4      ..       2.80 Ang.  
RESPONSE: The water oxygen atom is split over two sites leading to some
uncertainty in the relative positions of these.
;

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

data_1-Pd-2H2O-110K
_database_code_depnum_ccdc_archive 'CCDC 1519488'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
#==========================================================================
_title                           
;
Guest-Modulated Room Temperature Spin Crossover with Wide Hysteresis in a
2-D Hofmann-Type Material
;

#==========================================================================  

_audit_creation_method           SHELXL-2013

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Fe(proptrz)2Pd(CN)4].2H2O'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C26 H20 Fe N12 Pd, 2(O)'
_chemical_formula_sum            'C26 H20 Fe N12 O2 Pd'
_chemical_formula_weight         694.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.0836(3)
_cell_length_b                   15.1242(6)
_cell_length_c                   13.5688(6)
_cell_angle_alpha                96.424(4)
_cell_angle_beta                 97.878(4)
_cell_angle_gamma                90.090(4)
_cell_volume                     1430.70(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    5228
_cell_measurement_theta_min      5.9070
_cell_measurement_theta_max      71.4890

_exptl_crystal_description       'square plate'
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.131
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.027
_exptl_absorpt_coefficient_mu    9.539
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.434
_exptl_absorpt_correction_T_max  0.727
_exptl_absorpt_process_details   
;
 CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
 Analytical numeric absorption correction using a multifaceted crystal
 model based on expressions derived by R.C. Clark & J.S. Reid.
 (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 Crystal was mounted on a cactus needle in a thin film of paratone oil
;

_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.0662
_diffrn_reflns_number            11871
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.309
_diffrn_reflns_theta_max         71.999
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             5555
_reflns_number_gt                4888
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013), Xseed'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;Appearance of the supercell peaks the along b* axis leads to cell doubling,
 thus resulting in two crystallographically distinct Fe sites, one which is 
 in the high spin state and the other in the low spin state.

 Hydrogen atoms were fixed using the riding model. All non-hydrogen
 atoms, except for water oxygens, were modelled anisotropically.
 Water oxygen atoms were modelled as disordered over two positions.
 Hydrogen atoms on water guest molecules were not included due to the 
 highly disordered oxygen atoms, thus the locations of these hydrogen
 atoms are ambiguous. However, for chemical completeness, the hydrogens
 are included in the chemical formula and molecular weight., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0556P)²+1.2121P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         5555
_refine_ls_number_parameters     380
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0993
_refine_ls_wR_factor_gt          0.0941
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.49999(3) 0.74240(2) 0.49954(2) 0.01317(9) Uani 1 1 d . . . . .
Fe1 Fe 0.0000 0.5000 0.5000 0.01059(13) Uani 1 2 d S . P . .
Fe2 Fe 1.0000 1.0000 0.5000 0.01177(14) Uani 1 2 d S . P . .
N5 N 0.0547(3) 0.51666(15) 0.64951(18) 0.0165(5) Uani 1 1 d . . . . .
N3 N 0.7899(4) 0.90002(16) 0.50147(19) 0.0167(5) Uani 1 1 d . . . . .
N6 N 0.0491(4) 0.44914(16) 0.7094(2) 0.0224(5) Uani 1 1 d . . . . .
N10 N 0.9587(4) 1.04986(17) 0.2755(2) 0.0245(5) Uani 1 1 d . . . . .
N12 N 0.8086(4) 0.86946(18) 0.0950(2) 0.0261(6) Uani 1 1 d . . . . .
N7 N 0.1277(4) 0.57384(16) 0.80436(19) 0.0211(5) Uani 1 1 d . . . . .
N8 N 0.1810(4) 0.62792(18) 0.8944(2) 0.0255(6) Uani 1 1 d . . . . .
N11 N 0.8636(4) 0.92600(17) 0.18356(19) 0.0215(5) Uani 1 1 d . . . . .
N9 N 0.9349(4) 0.98542(16) 0.33780(19) 0.0189(5) Uani 1 1 d . . . . .
N1 N 0.1904(4) 0.40613(16) 0.49749(18) 0.0149(5) Uani 1 1 d . . . . .
N4 N 0.8001(4) 1.10552(16) 0.50478(19) 0.0178(5) Uani 1 1 d . . . . .
N2 N 0.1948(4) 0.59089(15) 0.49644(18) 0.0142(5) Uani 1 1 d . . . . .
C10 C 0.3287(4) 0.9044(2) 1.1158(2) 0.0228(6) Uani 1 1 d . . . . .
C18 C 0.8144(5) 0.7870(2) 0.1054(3) 0.0279(7) Uani 1 1 d . . . . .
H18 H 0.8556 0.7686 0.1694 0.033 Uiso 1 1 calc R U . . .
C13 C 0.4409(5) 1.0469(2) 1.2605(2) 0.0288(7) Uani 1 1 d . . . . .
H13 H 0.4807 1.0953 1.3098 0.035 Uiso 1 1 calc R U . . .
C21 C 0.6679(5) 0.5868(2) -0.1167(2) 0.0238(6) Uani 1 1 d . . . . .
C1 C 0.2989(4) 0.35139(18) 0.4989(2) 0.0153(5) Uani 1 1 d . . . . .
C6 C 0.0934(5) 0.4850(2) 0.8013(2) 0.0246(6) Uani 1 1 d . . . . .
H6 H 0.1007 0.4535 0.8584 0.029 Uiso 1 1 calc R U . . .
C17 C 0.9142(5) 1.0126(2) 0.1843(2) 0.0252(6) Uani 1 1 d . . . . .
H17 H 0.9168 1.0419 0.1261 0.030 Uiso 1 1 calc R U . . .
C25 C 0.5738(5) 0.5248(2) -0.2879(2) 0.0283(7) Uani 1 1 d . . . . .
H25 H 0.5453 0.5324 -0.3569 0.034 Uiso 1 1 calc R U . . .
C20 C 0.7188(5) 0.6608(2) -0.0423(2) 0.0265(7) Uani 1 1 d . . . . .
C14 C 0.4171(5) 0.9634(2) 1.2886(2) 0.0283(7) Uani 1 1 d . . . . .
H14 H 0.4398 0.9548 1.3575 0.034 Uiso 1 1 calc R U . . .
C7 C 0.1788(5) 0.7111(2) 0.8874(2) 0.0279(7) Uani 1 1 d . . . . .
H7 H 0.1416 0.7318 0.8242 0.033 Uiso 1 1 calc R U . . .
C12 C 0.4068(5) 1.0606(2) 1.1600(3) 0.0300(7) Uani 1 1 d . . . . .
H12 H 0.4218 1.1184 1.1407 0.036 Uiso 1 1 calc R U . . .
C19 C 0.7599(5) 0.7221(2) 0.0222(3) 0.0282(7) Uani 1 1 d . . . . .
C22 C 0.6572(5) 0.5017(2) -0.0869(2) 0.0280(7) Uani 1 1 d . . . . .
H22 H 0.6858 0.4936 -0.0181 0.034 Uiso 1 1 calc R U . . .
C4 C 0.6953(4) 1.16339(18) 0.5020(2) 0.0163(6) Uani 1 1 d . . . . .
C11 C 0.3508(5) 0.9896(2) 1.0881(2) 0.0266(7) Uani 1 1 d . . . . .
H11 H 0.3273 0.9990 1.0194 0.032 Uiso 1 1 calc R U . . .
C9 C 0.2752(5) 0.8324(2) 1.0393(2) 0.0273(7) Uani 1 1 d . . . . .
C2 C 0.3047(4) 0.64668(19) 0.4985(2) 0.0149(5) Uani 1 1 d . . . . .
C5 C 0.1018(4) 0.59048(19) 0.7067(2) 0.0199(6) Uani 1 1 d . . . . .
H5 H 0.1159 0.6470 0.6841 0.024 Uiso 1 1 calc R U . . .
C3 C 0.6882(4) 0.83972(19) 0.5002(2) 0.0159(6) Uani 1 1 d . . . . .
C24 C 0.5626(5) 0.4409(2) -0.2574(2) 0.0307(7) Uani 1 1 d . . . . .
H24 H 0.5256 0.3912 -0.3055 0.037 Uiso 1 1 calc R U . . .
C8 C 0.2316(5) 0.7735(2) 0.9736(2) 0.0271(7) Uani 1 1 d . . . . .
C26 C 0.6266(5) 0.5981(2) -0.2182(2) 0.0271(7) Uani 1 1 d . . . . .
H26 H 0.6346 0.6556 -0.2394 0.033 Uiso 1 1 calc R U . . .
C16 C 0.8776(4) 0.9120(2) 0.2812(2) 0.0219(6) Uani 1 1 d . . . . .
H16 H 0.8502 0.8572 0.3049 0.026 Uiso 1 1 calc R U . . .
C23 C 0.6052(5) 0.4292(2) -0.1571(3) 0.0302(7) Uani 1 1 d . . . . .
H23 H 0.5986 0.3714 -0.1364 0.036 Uiso 1 1 calc R U . . .
C15 C 0.3604(5) 0.8916(2) 1.2176(2) 0.0257(7) Uani 1 1 d . . . . .
H15 H 0.3432 0.8342 1.2376 0.031 Uiso 1 1 calc R U . . .
O1WA O 0.0167(10) 0.2669(3) 0.6760(4) 0.0281(7) Uiso 0.529(9) 1 d . U P A 1
O1WB O -0.0522(11) 0.2690(3) 0.6950(4) 0.0281(7) Uiso 0.471(9) 1 d . U P A 2
O2WA O 1.0881(8) 1.2280(3) 0.2984(3) 0.0299(8) Uiso 0.607(7) 1 d . U P B 3
O2WB O 1.0139(12) 1.2285(4) 0.3199(5) 0.0299(8) Uiso 0.393(7) 1 d . U P B 4

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.00911(12) 0.01205(12) 0.01822(13) 0.00177(7) 0.00140(8) 0.00001(8)
Fe1 0.0081(3) 0.0076(3) 0.0157(3) 0.0008(2) 0.0010(2) -0.0005(2)
Fe2 0.0084(3) 0.0089(3) 0.0178(3) 0.0013(2) 0.0013(2) 0.0001(2)
N5 0.0134(12) 0.0129(11) 0.0230(12) 0.0017(9) 0.0023(9) 0.0001(8)
N3 0.0138(12) 0.0136(11) 0.0231(12) 0.0025(9) 0.0031(9) 0.0017(9)
N6 0.0251(14) 0.0146(12) 0.0265(13) 0.0039(9) -0.0016(10) 0.0002(10)
N10 0.0235(14) 0.0179(12) 0.0314(14) 0.0049(10) -0.0002(11) -0.0020(10)
N12 0.0294(15) 0.0243(14) 0.0233(13) -0.0024(10) 0.0038(11) 0.0003(11)
N7 0.0228(13) 0.0178(12) 0.0219(13) -0.0018(9) 0.0033(10) 0.0004(10)
N8 0.0292(15) 0.0236(14) 0.0221(13) -0.0025(10) 0.0024(11) -0.0016(11)
N11 0.0211(13) 0.0182(12) 0.0242(13) -0.0015(9) 0.0027(10) -0.0005(10)
N9 0.0154(12) 0.0153(11) 0.0259(13) 0.0016(9) 0.0031(10) -0.0002(9)
N1 0.0116(12) 0.0128(11) 0.0203(12) 0.0024(9) 0.0015(9) -0.0027(9)
N4 0.0138(12) 0.0143(11) 0.0248(13) 0.0013(9) 0.0021(9) -0.0009(10)
N2 0.0134(12) 0.0111(11) 0.0180(11) 0.0014(8) 0.0015(9) 0.0027(9)
C10 0.0170(15) 0.0279(16) 0.0217(15) -0.0037(12) 0.0017(11) 0.0000(11)
C18 0.0304(19) 0.0254(16) 0.0258(16) -0.0015(12) 0.0003(13) 0.0012(13)
C13 0.0248(17) 0.0326(18) 0.0252(16) -0.0095(13) 0.0008(13) -0.0028(13)
C21 0.0220(16) 0.0273(16) 0.0215(15) -0.0009(12) 0.0036(12) 0.0002(12)
C1 0.0123(13) 0.0139(13) 0.0199(14) 0.0023(10) 0.0023(10) -0.0019(11)
C6 0.0277(17) 0.0194(15) 0.0262(16) 0.0056(11) -0.0003(13) -0.0029(12)
C17 0.0290(17) 0.0184(15) 0.0277(16) 0.0050(11) 0.0002(13) -0.0032(12)
C25 0.0302(18) 0.0376(19) 0.0166(14) 0.0012(12) 0.0031(12) 0.0022(14)
C20 0.0255(17) 0.0300(17) 0.0232(15) -0.0006(13) 0.0028(12) 0.0004(13)
C14 0.0270(17) 0.0417(19) 0.0151(14) -0.0011(12) 0.0022(12) 0.0045(14)
C7 0.0343(19) 0.0249(16) 0.0221(15) -0.0021(12) -0.0006(13) 0.0023(13)
C12 0.0333(19) 0.0263(17) 0.0298(17) -0.0007(13) 0.0052(14) -0.0053(14)
C19 0.0286(18) 0.0271(17) 0.0274(16) -0.0007(13) 0.0023(13) 0.0018(13)
C22 0.0318(18) 0.0326(18) 0.0191(15) 0.0021(12) 0.0022(13) -0.0023(14)
C4 0.0123(13) 0.0131(13) 0.0230(14) 0.0007(10) 0.0015(11) -0.0035(10)
C11 0.0288(17) 0.0323(18) 0.0185(14) 0.0039(12) 0.0011(12) -0.0036(13)
C9 0.0265(17) 0.0289(17) 0.0262(16) 0.0022(13) 0.0036(13) 0.0021(13)
C2 0.0107(13) 0.0156(13) 0.0183(13) 0.0011(10) 0.0021(10) 0.0027(10)
C5 0.0216(15) 0.0160(13) 0.0223(14) 0.0009(10) 0.0048(11) -0.0007(11)
C3 0.0131(14) 0.0144(13) 0.0199(14) 0.0010(10) 0.0024(10) 0.0038(10)
C24 0.0304(18) 0.0350(18) 0.0240(16) -0.0073(13) 0.0030(13) -0.0044(14)
C8 0.0291(18) 0.0255(16) 0.0246(16) -0.0022(13) 0.0009(13) 0.0015(13)
C26 0.0267(17) 0.0288(17) 0.0257(16) 0.0025(12) 0.0034(13) 0.0030(13)
C16 0.0213(15) 0.0186(14) 0.0257(15) 0.0006(11) 0.0045(12) -0.0018(11)
C23 0.039(2) 0.0259(17) 0.0255(16) 0.0010(12) 0.0054(14) -0.0049(14)
C15 0.0257(17) 0.0276(16) 0.0241(15) 0.0036(12) 0.0034(12) 0.0036(13)

_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 C3 1.983(3) . ?
Pd1 C4 1.987(3) 2_676 ?
Pd1 C2 1.998(3) . ?
Pd1 C1 2.012(3) 2_666 ?
Fe1 N2 1.955(3) 2_566 ?
Fe1 N2 1.955(3) . ?
Fe1 N1 1.961(2) 2_566 ?
Fe1 N1 1.961(2) . ?
Fe1 N5 2.000(2) 2_566 ?
Fe1 N5 2.000(2) . ?
Fe2 N3 2.124(3) . ?
Fe2 N3 2.124(3) 2_776 ?
Fe2 N4 2.137(3) 2_776 ?
Fe2 N4 2.137(3) . ?
Fe2 N9 2.172(3) . ?
Fe2 N9 2.172(3) 2_776 ?
N5 C5 1.302(4) . ?
N5 N6 1.378(3) . ?
N3 C3 1.158(4) . ?
N6 C6 1.299(4) . ?
N10 C17 1.298(4) . ?
N10 N9 1.384(3) . ?
N12 C18 1.270(4) . ?
N12 N11 1.403(4) . ?
N7 C6 1.361(4) . ?
N7 C5 1.364(4) . ?
N7 N8 1.398(3) . ?
N8 C7 1.272(4) . ?
N11 C17 1.355(4) . ?
N11 C16 1.355(4) . ?
N9 C16 1.308(4) . ?
N1 C1 1.130(4) . ?
N4 C4 1.149(4) . ?
N2 C2 1.143(4) . ?
C10 C11 1.397(5) . ?
C10 C15 1.403(4) . ?
C10 C9 1.430(4) . ?
C18 C19 1.421(4) . ?
C18 H18 0.9500 . ?
C13 C14 1.376(5) . ?
C13 C12 1.391(5) . ?
C13 H13 0.9500 . ?
C21 C22 1.396(5) . ?
C21 C26 1.398(4) . ?
C21 C20 1.432(4) . ?
C1 Pd1 2.012(3) 2_666 ?
C6 H6 0.9500 . ?
C17 H17 0.9500 . ?
C25 C24 1.384(5) . ?
C25 C26 1.390(5) . ?
C25 H25 0.9500 . ?
C20 C19 1.207(5) . ?
C14 C15 1.389(5) . ?
C14 H14 0.9500 . ?
C7 C8 1.424(4) . ?
C7 H7 0.9500 . ?
C12 C11 1.385(5) . ?
C12 H12 0.9500 . ?
C22 C23 1.383(5) . ?
C22 H22 0.9500 . ?
C4 Pd1 1.987(3) 2_676 ?
C11 H11 0.9500 . ?
C9 C8 1.197(5) . ?
C5 H5 0.9500 . ?
C24 C23 1.385(5) . ?
C24 H24 0.9500 . ?
C26 H26 0.9500 . ?
C16 H16 0.9500 . ?
C23 H23 0.9500 . ?
C15 H15 0.9500 . ?

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
C3 Pd1 C4 86.20(11) . 2_676 ?
C3 Pd1 C2 178.46(10) . . ?
C4 Pd1 C2 92.26(11) 2_676 . ?
C3 Pd1 C1 92.81(11) . 2_666 ?
C4 Pd1 C1 179.01(10) 2_676 2_666 ?
C2 Pd1 C1 88.72(11) . 2_666 ?
N2 Fe1 N2 180.0 2_566 . ?
N2 Fe1 N1 91.13(10) 2_566 2_566 ?
N2 Fe1 N1 88.87(10) . 2_566 ?
N2 Fe1 N1 88.87(10) 2_566 . ?
N2 Fe1 N1 91.13(10) . . ?
N1 Fe1 N1 180.0 2_566 . ?
N2 Fe1 N5 88.68(10) 2_566 2_566 ?
N2 Fe1 N5 91.32(10) . 2_566 ?
N1 Fe1 N5 89.33(10) 2_566 2_566 ?
N1 Fe1 N5 90.67(10) . 2_566 ?
N2 Fe1 N5 91.32(10) 2_566 . ?
N2 Fe1 N5 88.68(10) . . ?
N1 Fe1 N5 90.67(10) 2_566 . ?
N1 Fe1 N5 89.33(10) . . ?
N5 Fe1 N5 180.0 2_566 . ?
N3 Fe2 N3 180.0 . 2_776 ?
N3 Fe2 N4 86.48(9) . 2_776 ?
N3 Fe2 N4 93.53(9) 2_776 2_776 ?
N3 Fe2 N4 93.52(9) . . ?
N3 Fe2 N4 86.47(9) 2_776 . ?
N4 Fe2 N4 180.0 2_776 . ?
N3 Fe2 N9 88.08(9) . . ?
N3 Fe2 N9 91.92(9) 2_776 . ?
N4 Fe2 N9 91.61(9) 2_776 . ?
N4 Fe2 N9 88.39(9) . . ?
N3 Fe2 N9 91.92(9) . 2_776 ?
N3 Fe2 N9 88.08(9) 2_776 2_776 ?
N4 Fe2 N9 88.39(9) 2_776 2_776 ?
N4 Fe2 N9 91.61(9) . 2_776 ?
N9 Fe2 N9 180.0 . 2_776 ?
C5 N5 N6 108.4(2) . . ?
C5 N5 Fe1 127.3(2) . . ?
N6 N5 Fe1 124.32(18) . . ?
C3 N3 Fe2 173.5(3) . . ?
C6 N6 N5 106.7(2) . . ?
C17 N10 N9 106.7(2) . . ?
C18 N12 N11 114.6(3) . . ?
C6 N7 C5 105.1(2) . . ?
C6 N7 N8 122.1(3) . . ?
C5 N7 N8 132.8(3) . . ?
C7 N8 N7 115.0(3) . . ?
C17 N11 C16 105.4(3) . . ?
C17 N11 N12 122.9(3) . . ?
C16 N11 N12 131.7(3) . . ?
C16 N9 N10 107.7(3) . . ?
C16 N9 Fe2 125.7(2) . . ?
N10 N9 Fe2 126.44(19) . . ?
C1 N1 Fe1 177.8(3) . . ?
C4 N4 Fe2 176.0(3) . . ?
C2 N2 Fe1 176.3(3) . . ?
C11 C10 C15 119.4(3) . . ?
C11 C10 C9 118.9(3) . . ?
C15 C10 C9 121.8(3) . . ?
N12 C18 C19 120.7(3) . . ?
N12 C18 H18 119.7 . . ?
C19 C18 H18 119.7 . . ?
C14 C13 C12 120.2(3) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C22 C21 C26 119.4(3) . . ?
C22 C21 C20 119.2(3) . . ?
C26 C21 C20 121.4(3) . . ?
N1 C1 Pd1 177.6(3) . 2_666 ?
N6 C6 N7 110.6(3) . . ?
N6 C6 H6 124.7 . . ?
N7 C6 H6 124.7 . . ?
N10 C17 N11 110.6(3) . . ?
N10 C17 H17 124.7 . . ?
N11 C17 H17 124.7 . . ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C19 C20 C21 178.4(4) . . ?
C13 C14 C15 120.8(3) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
N8 C7 C8 120.6(3) . . ?
N8 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C11 C12 C13 119.7(3) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C20 C19 C18 173.6(4) . . ?
C23 C22 C21 120.4(3) . . ?
C23 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
N4 C4 Pd1 175.8(3) . 2_676 ?
C12 C11 C10 120.4(3) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C8 C9 C10 178.4(4) . . ?
N2 C2 Pd1 178.6(3) . . ?
N5 C5 N7 109.2(3) . . ?
N5 C5 H5 125.4 . . ?
N7 C5 H5 125.4 . . ?
N3 C3 Pd1 176.0(3) . . ?
C23 C24 C25 120.2(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C9 C8 C7 173.3(4) . . ?
C25 C26 C21 119.7(3) . . ?
C25 C26 H26 120.2 . . ?
C21 C26 H26 120.2 . . ?
N9 C16 N11 109.5(3) . . ?
N9 C16 H16 125.3 . . ?
N11 C16 H16 125.3 . . ?
C22 C23 C24 120.0(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C14 C15 C10 119.4(3) . . ?
C14 C15 H15 120.3 . . ?
C10 C15 H15 120.3 . . ?

_refine_diff_density_max         1.436
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.091

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_PLAT110_1-Pd-2H2O-110K      
;
PROBLEM: ADDSYM Detects Potential Lattice Translation ...          ? Check
RESPONSE: The asymmetric unit contains two crystallographically distinct 
Fe sites, one in the high spin state and the other in the low spin state; 
this is consistent with the magnetic data collected.
;
_vrf_PLAT112_1-Pd-2H2O-110K      
;
PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem.      b/2        100 %Fit  
RESPONSE: The asymmetric unit contains two crystallographically distinct 
Fe sites, one in the high spin state and the other in the low spin state; 
this is consistent with the magnetic data collected.
;
_vrf_PLAT113_1-Pd-2H2O-110K      
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New  Space Group        P-1 Check 
RESPONSE: The asymmetric unit contains two crystallographically distinct 
Fe sites, one in the high spin state and the other in the low spin state; 
this is consistent with the magnetic data collected.
;
_vrf_PLAT430_1-Pd-2H2O-110K      
;
PROBLEM: Short Inter D...A Contact  O1WA   ..  N6      ..       2.75 Ang.  
RESPONSE: The water oxygen atom is split over two sites leading to some
uncertainty in the relative positions of these.
;
_vrf_PLAT041_1-Pd-2H2O-110K      
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: Hydrogen atoms on water guest molecules were not included due 
to the highly disordered oxygen atoms, thus the locations of these hydrogen
atoms are ambiguous. However, for chemical completeness, the hydrogens
are included in the chemical formula and molecular weight.
;
_vrf_PLAT043_1-Pd-2H2O-110K      
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.03 Check 
RESPONSE: Hydrogen atoms on water guest molecules were not included due 
to the highly disordered oxygen atoms, thus the locations of these hydrogen
atoms are ambiguous. However, for chemical completeness, the hydrogens
are included in the chemical formula and molecular weight.
;
_vrf_PLAT155_1-Pd-2H2O-110K      
;
PROBLEM: The Triclinic Unitcell is NOT Reduced ..........     Please Do ! 
RESPONSE: This unit cell has been adopted to allow comparison with the 
high spin structure, which is in a triclinic cell with half the volume.
;
_vrf_PLAT202_1-Pd-2H2O-110K      
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          2 Check 
RESPONSE: Since the water molecule is disordered, refining the oxygen atoms
over two positions with paritial occupanices creates high correlation between
refinement parameters.
;

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

data_1-Pt-2H2O-200K
_database_code_depnum_ccdc_archive 'CCDC 1519489'
_audit_update_record             
;
2016-11-28 deposited with the CCDC.
2018-05-29 downloaded from the CCDC.
;
#==========================================================================
_title                           
;
Guest-Modulated Room Temperature Spin Crossover with Wide Hysteresis in a
2-D Hofmann-Type Material
;

#==========================================================================  

_audit_creation_method           SHELXL-2013

_chemical_name_systematic        
;
 ?
;
_chemical_name_common            '[Fe(proptrz)2Pt(CN)4].2H2O'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'C26 H20 Fe N12 Pt, 2(O)'
_chemical_formula_sum            'C26 H20 Fe N12 O2 Pt'
_chemical_formula_weight         783.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.27720(10)
_cell_length_b                   7.64320(10)
_cell_length_c                   13.5928(3)
_cell_angle_alpha                95.997(2)
_cell_angle_beta                 98.598(2)
_cell_angle_gamma                90.080(2)
_cell_volume                     743.35(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    11818
_cell_measurement_theta_min      3.2620
_cell_measurement_theta_max      75.8870

_exptl_crystal_description       'square plate'
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    12.973
_shelx_estimated_absorpt_T_min   0.181
_shelx_estimated_absorpt_T_max   0.357
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.142
_exptl_absorpt_correction_T_max  0.273
_exptl_absorpt_process_details   
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.31d (release 11-02-2014 CrysAlis171 .NET)
 (compiled Feb 11 2014,18:09:27)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 Crystal was mounted on a loop in a thin film of paratone oil
;

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.5861
_diffrn_reflns_number            15540
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.307
_diffrn_reflns_theta_max         76.450
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3066
_reflns_number_gt                3064
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31d
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31d
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31d
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013), Xseed'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;Hydrogen atoms were fixed using the riding model. All non-hydrogen
 atoms, except for water oxygens, were modelled anisotropically.
 Water oxygen atoms were modelled as disordered over two positions.
 Hydrogen atoms on water guest molecules were not included due to the 
 highly disordered oxygen atoms, thus the location of these hydrogen
 atoms are ambiguous. However, for chemical completeness, the hydrogens
 are included in the chemical formula and molecular weight., Twin
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1258P)²+2.1693P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         3066
_refine_ls_number_parameters     192
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0560
_refine_ls_wR_factor_ref         0.1545
_refine_ls_wR_factor_gt          0.1544
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 1.0000 0.0000 0.0000 0.02148(18) Uani 1 2 d S . P . .
Fe1 Fe 0.5000 0.5000 0.0000 0.0214(3) Uani 1 2 d S . P . .
C2 C 0.8104(11) -0.1894(10) -0.0002(6) 0.0237(14) Uani 1 1 d . . . . .
N2 N 0.7081(10) -0.3015(9) -0.0007(6) 0.0280(14) Uani 1 1 d . . . . .
C1 C 0.8081(12) 0.1856(12) -0.0024(6) 0.0294(16) Uani 1 1 d . . . . .
N1 N 0.6995(10) 0.2936(10) -0.0041(6) 0.0292(14) Uani 1 1 d . . . . .
C3 C 0.6077(15) 0.6737(12) 0.2212(7) 0.0407(19) Uani 1 1 d . . . . .
H3 H 0.6306 0.7836 0.1981 0.049 Uiso 1 1 calc R U . . .
N3 N 0.5567(11) 0.5285(9) 0.1639(5) 0.0339(14) Uani 1 1 d . . . . .
C4 C 0.5815(17) 0.4709(14) 0.3174(8) 0.049(2) Uani 1 1 d . . . . .
H4 H 0.5819 0.4112 0.3753 0.059 Uiso 1 1 calc R U . . .
N4 N 0.5410(14) 0.3973(11) 0.2256(6) 0.0470(19) Uani 1 1 d . . . . .
C5 C 0.684(2) 0.9177(18) 0.3977(9) 0.060(3) Uani 1 1 d . . . . .
H5 H 0.6536 0.9568 0.3333 0.072 Uiso 1 1 calc R U . . .
N5 N 0.6229(13) 0.6440(11) 0.3186(6) 0.0438(18) Uani 1 1 d . . . . .
C6 C 0.739(2) 1.0421(18) 0.4830(9) 0.059(3) Uani 1 1 d . . . . .
N6 N 0.6770(16) 0.7544(13) 0.4081(6) 0.055(2) Uani 1 1 d . . . . .
C7 C 0.7840(19) 1.1595(17) 0.5463(8) 0.057(3) Uani 1 1 d . . . . .
C8 C 0.8389(16) 1.3054(16) 0.6197(7) 0.050(2) Uani 1 1 d . . . . .
C9 C 0.855(2) 1.472(2) 0.5892(8) 0.066(3) Uani 1 1 d . . . . .
H9 H 0.8283 1.4870 0.5201 0.079 Uiso 1 1 calc R U . . .
C10 C 0.908(2) 1.6159(19) 0.6579(10) 0.067(3) Uani 1 1 d . . . . .
H10 H 0.9187 1.7290 0.6361 0.081 Uiso 1 1 calc R U . . .
C11 C 0.9459(18) 1.5944(19) 0.7579(8) 0.062(3) Uani 1 1 d . . . . .
H11 H 0.9849 1.6930 0.8050 0.074 Uiso 1 1 calc R U . . .
C12 C 0.9284(17) 1.433(2) 0.7905(8) 0.058(3) Uani 1 1 d . . . . .
H12 H 0.9546 1.4207 0.8599 0.070 Uiso 1 1 calc R U . . .
C13 C 0.8720(19) 1.2870(17) 0.7224(8) 0.056(3) Uani 1 1 d . . . . .
H13 H 0.8562 1.1756 0.7454 0.067 Uiso 1 1 calc R U . . .
O1WA O 0.546(3) 0.038(3) 0.1737(14) 0.064(3) Uiso 0.52(2) 1 d . U P A 1
O1WB O 0.456(4) 0.038(3) 0.1949(15) 0.064(3) Uiso 0.48(2) 1 d . U P A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.0125(3) 0.0092(2) 0.0432(3) 0.00162(15) 0.00647(15) 0.00108(15)
Fe1 0.0128(8) 0.0050(7) 0.0471(8) 0.0019(6) 0.0068(6) 0.0034(6)
C2 0.018(3) 0.011(3) 0.041(3) 0.003(3) 0.005(3) 0.004(3)
N2 0.017(3) 0.014(3) 0.054(4) 0.002(2) 0.006(3) -0.003(3)
C1 0.022(4) 0.026(4) 0.041(4) 0.002(3) 0.010(3) 0.013(3)
N1 0.014(3) 0.021(3) 0.054(4) 0.004(3) 0.006(2) 0.011(3)
C3 0.048(6) 0.025(4) 0.048(4) -0.001(3) 0.008(4) 0.001(4)
N3 0.031(4) 0.023(3) 0.048(3) 0.001(3) 0.008(3) -0.002(3)
C4 0.062(7) 0.034(5) 0.050(5) 0.011(4) 0.001(4) -0.001(5)
N4 0.055(5) 0.031(4) 0.053(4) 0.007(3) 0.001(4) -0.006(4)
C5 0.070(8) 0.054(7) 0.052(5) -0.004(5) 0.005(5) 0.001(6)
N5 0.052(5) 0.032(4) 0.045(4) -0.001(3) 0.004(3) -0.003(4)
C6 0.061(7) 0.054(7) 0.059(6) -0.008(5) 0.007(5) 0.001(6)
N6 0.066(6) 0.047(5) 0.047(4) -0.004(4) -0.001(4) 0.005(5)
C7 0.058(7) 0.055(7) 0.055(5) -0.007(5) 0.008(5) 0.000(6)
C8 0.044(6) 0.056(6) 0.047(5) -0.007(4) 0.007(4) -0.001(5)
C9 0.081(9) 0.075(9) 0.039(5) 0.006(5) 0.005(5) -0.009(7)
C10 0.086(10) 0.051(7) 0.062(6) 0.004(5) 0.006(6) -0.014(7)
C11 0.053(7) 0.074(9) 0.051(5) -0.013(5) 0.001(5) -0.006(6)
C12 0.049(6) 0.084(9) 0.040(4) -0.004(5) 0.004(4) 0.010(6)
C13 0.068(8) 0.051(6) 0.051(5) 0.014(4) 0.009(5) 0.007(6)

_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 1.991(8) 2_755 ?
Pt1 C1 1.991(8) . ?
Pt1 C2 1.998(8) 2_755 ?
Pt1 C2 1.998(8) . ?
Fe1 N2 2.144(7) 2_655 ?
Fe1 N2 2.144(7) 1_565 ?
Fe1 N1 2.148(7) . ?
Fe1 N1 2.148(7) 2_665 ?
Fe1 N3 2.191(7) 2_665 ?
Fe1 N3 2.191(7) . ?
C2 N2 1.133(12) . ?
N2 Fe1 2.144(7) 1_545 ?
C1 N1 1.143(13) . ?
C3 N3 1.307(11) . ?
C3 N5 1.355(12) . ?
C3 H3 0.9500 . ?
N3 N4 1.388(11) . ?
C4 N4 1.305(14) . ?
C4 N5 1.355(13) . ?
C4 H4 0.9500 . ?
C5 N6 1.273(17) . ?
C5 C6 1.427(16) . ?
C5 H5 0.9500 . ?
N5 N6 1.410(11) . ?
C6 C7 1.186(17) . ?
C7 C8 1.430(15) . ?
C8 C9 1.388(19) . ?
C8 C13 1.403(15) . ?
C9 C10 1.382(18) . ?
C9 H9 0.9500 . ?
C10 C11 1.373(17) . ?
C10 H10 0.9500 . ?
C11 C12 1.36(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.394(18) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?

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 2_755 . ?
C1 Pt1 C2 92.0(3) 2_755 2_755 ?
C1 Pt1 C2 88.0(3) . 2_755 ?
C1 Pt1 C2 88.0(3) 2_755 . ?
C1 Pt1 C2 92.0(3) . . ?
C2 Pt1 C2 180.0 2_755 . ?
N2 Fe1 N2 180.0(5) 2_655 1_565 ?
N2 Fe1 N1 87.9(3) 2_655 . ?
N2 Fe1 N1 92.1(3) 1_565 . ?
N2 Fe1 N1 92.1(3) 2_655 2_665 ?
N2 Fe1 N1 87.9(3) 1_565 2_665 ?
N1 Fe1 N1 180.0 . 2_665 ?
N2 Fe1 N3 89.1(3) 2_655 2_665 ?
N2 Fe1 N3 90.9(3) 1_565 2_665 ?
N1 Fe1 N3 90.2(3) . 2_665 ?
N1 Fe1 N3 89.8(3) 2_665 2_665 ?
N2 Fe1 N3 90.9(3) 2_655 . ?
N2 Fe1 N3 89.1(3) 1_565 . ?
N1 Fe1 N3 89.8(3) . . ?
N1 Fe1 N3 90.2(3) 2_665 . ?
N3 Fe1 N3 180.0(4) 2_665 . ?
N2 C2 Pt1 177.3(8) . . ?
C2 N2 Fe1 176.0(8) . 1_545 ?
N1 C1 Pt1 179.1(9) . . ?
C1 N1 Fe1 177.3(8) . . ?
N3 C3 N5 109.7(8) . . ?
N3 C3 H3 125.1 . . ?
N5 C3 H3 125.1 . . ?
C3 N3 N4 107.6(7) . . ?
C3 N3 Fe1 125.9(6) . . ?
N4 N3 Fe1 126.4(5) . . ?
N4 C4 N5 110.6(8) . . ?
N4 C4 H4 124.7 . . ?
N5 C4 H4 124.7 . . ?
C4 N4 N3 106.6(8) . . ?
N6 C5 C6 120.0(12) . . ?
N6 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C4 N5 C3 105.4(8) . . ?
C4 N5 N6 122.6(8) . . ?
C3 N5 N6 131.9(9) . . ?
C7 C6 C5 172.5(15) . . ?
C5 N6 N5 114.9(9) . . ?
C6 C7 C8 177.7(15) . . ?
C9 C8 C13 118.5(10) . . ?
C9 C8 C7 119.4(10) . . ?
C13 C8 C7 122.0(12) . . ?
C10 C9 C8 121.0(10) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C11 C10 C9 119.6(13) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C12 C11 C10 120.8(12) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 120.4(10) . . ?
C11 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C12 C13 C8 119.5(11) . . ?
C12 C13 H13 120.2 . . ?
C8 C13 H13 120.2 . . ?

_refine_diff_density_max         7.227
_refine_diff_density_min         -1.474
_refine_diff_density_rms         0.309

_shelxl_version_number           2013-4


# start Validation Reply Form
_vrf_PLAT094_1-Pt-2H2O-200K      
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.90 Report
RESPONSE: There is a high electron density around the heavy metal atom Fe1.
;
_vrf_PLAT430_1-Pt-2H2O-200K      
;
PROBLEM: Short Inter D...A Contact  O1WA   ..  N4      ..       2.77 Ang.  
RESPONSE: The water oxygen atom is split over two sites leading to some
uncertainty in the relative positions of these. 
;
_vrf_DIFMX02_1-Pt-2H2O-200K      
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: There is a high electron density around the heavy metal atom Fe1.
;
_vrf_PLAT041_1-Pt-2H2O-200K      
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check
RESPONSE: Hydrogen atoms on water guest molecules were not included due 
to the highly disordered oxygen atoms, thus the locations of these hydrogen
atoms are ambiguous. However, for chemical completeness, the hydrogens
are included in the chemical formula and molecular weight.
;
_vrf_PLAT043_1-Pt-2H2O-200K      
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       4.04 Check 
RESPONSE: Hydrogen atoms on water guest molecules were not included due 
to the highly disordered oxygen atoms, thus the locations of these hydrogen
atoms are ambiguous. However, for chemical completeness, the hydrogens
are included in the chemical formula and molecular weight.
;
_vrf_PLAT097_1-Pt-2H2O-200K      
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       7.23 eA-3  
RESPONSE: There is a high electron density around the heavy metal atom Fe1.
;
_vrf_PLAT202_1-Pt-2H2O-200K      
;
PROBLEM: Isotropic non-H Atoms in Anion/Solvent .........          1 Check 
RESPONSE: Since the water molecule is disordered, refining the oxygen atoms
over two positions with paritial occupanices creates high correlation between
refinement parameters if refined anisotropically. 
;
_vrf_PLAT213_1-Pt-2H2O-200K      
;
PROBLEM: Atom Fe1             has ADP max/min Ratio .....        3.6 prolat
RESPONSE: There may be dynamic motion or static disorder over the Fe1 site as
can be seen by the presence of the large Q peak in the vicinity of the Fe1 
atom.
;
_vrf_PLAT342_1-Pt-2H2O-200K      
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01767 Ang.  
RESPONSE: Systematic errors in the data may have contributed to this
slightly larger value.
;

_exptl_crystal_recrystallization_method 'solvent diffusion'
_exptl_crystal_preparation       ', Magnetic properties'
