# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_PtBpy
_database_code_depnum_ccdc_archive 'CCDC 1444414'
_audit_update_record             
;
2015-12-28 deposited with the CCDC.
2016-04-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        Fe(H2O)2(bpy)[Pt(CN)4]?H2O
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H8 Fe N6 O2 Pt'
_chemical_formula_weight         543.20

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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+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                   15.667(2)
_cell_length_b                   15.136(2)
_cell_length_c                   7.3104(11)
_cell_angle_alpha                90
_cell_angle_beta                 110.570(2)
_cell_angle_gamma                90
_cell_volume                     1623.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    2885
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      28.39

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    2.223
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   'not measured'
_exptl_transmission_factor_max   'not measured'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    9.523
_shelx_estimated_absorpt_T_min   0.162
_shelx_estimated_absorpt_T_max   0.162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1422
_exptl_absorpt_correction_T_max  0.162
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            3949
_diffrn_reflns_av_unetI/netI     0.1000
_diffrn_reflns_av_R_equivalents  0.1483
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         1.933
_diffrn_reflns_theta_max         25.496
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1515
_reflns_number_gt                1383
_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       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0631P)²+6.9898P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1515
_refine_ls_number_parameters     112
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0501
_refine_ls_wR_factor_ref         0.1257
_refine_ls_wR_factor_gt          0.1232
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.5000 0.50336(2) 0.7500 0.0215(2) Uani 1 2 d S T P . .
Fe1 Fe 0.2500 0.7500 0.5000 0.0244(4) Uani 1 2 d S . P . .
O0 O 0.2930(4) 0.7899(4) 0.2606(7) 0.0351(13) Uani 1 1 d . . . . .
C1 C 0.5954(7) 0.4107(7) 0.8582(14) 0.035(2) Uani 1 1 d . . . . .
C3 C 0.4070(6) 0.5977(7) 0.6449(12) 0.0281(19) Uani 1 1 d . . . . .
N2 N 0.3545(5) 0.6531(6) 0.5873(12) 0.0320(17) Uani 1 1 d . . . . .
N4 N 0.1587(4) 0.6549(4) 0.2997(9) 0.0333(15) Uani 1 1 d . . . . .
C6 C 0.1740(6) 0.5675(6) 0.3153(15) 0.051(2) Uani 1 1 d . . . . .
H6 H 0.2284 0.5478 0.4074 0.061 Uiso 1 1 calc R U . . .
C7 C 0.1146(13) 0.5055(6) 0.204(3) 0.059(4) Uani 1 1 d . . . . .
H7 H 0.1281 0.4458 0.2263 0.071 Uiso 1 1 calc R U . . .
C8 C 0.0336(7) 0.5318(7) 0.0582(14) 0.043(2) Uani 1 1 d . . . . .
C9 C 0.0207(7) 0.6234(7) 0.0276(13) 0.043(2) Uani 1 1 d . . . . .
H9 H -0.0299 0.6451 -0.0725 0.052 Uiso 1 1 calc R U . . .
C10 C 0.0845(6) 0.6804(6) 0.1490(13) 0.045(2) Uani 1 1 d . . . . .
H10 H 0.0756 0.7406 0.1250 0.054 Uiso 1 1 calc R U . . .
N3 N 0.6509(7) 0.3586(7) 0.9207(14) 0.049(2) Uani 1 1 d . . . . .

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 0.0202(3) 0.0115(3) 0.0257(3) 0.000 -0.0009(2) 0.000
Fe1 0.0200(7) 0.0159(7) 0.0259(7) -0.0049(6) -0.0062(5) 0.0019(5)
O0 0.034(3) 0.029(3) 0.033(3) -0.001(2) 0.000(2) 0.001(2)
C1 0.043(5) 0.028(5) 0.033(4) -0.001(4) 0.012(4) -0.002(5)
C3 0.028(4) 0.019(4) 0.027(4) -0.009(4) -0.003(3) -0.007(4)
N2 0.027(4) 0.022(4) 0.035(4) -0.003(3) -0.004(3) 0.008(3)
N4 0.030(3) 0.020(3) 0.038(3) -0.009(3) -0.003(3) 0.000(3)
C6 0.028(4) 0.027(4) 0.071(6) -0.005(4) -0.017(4) -0.001(4)
C7 0.056(9) 0.023(5) 0.071(10) -0.007(4) -0.013(7) -0.003(4)
C8 0.039(5) 0.032(5) 0.046(5) -0.009(5) 0.001(4) -0.004(5)
C9 0.046(5) 0.030(5) 0.036(4) -0.010(4) -0.008(4) -0.010(5)
C10 0.042(5) 0.028(4) 0.047(5) -0.003(4) -0.005(4) -0.010(4)
N3 0.052(5) 0.040(5) 0.050(5) 0.013(5) 0.011(4) 0.032(5)

_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 C3 1.992(10) 2_656 ?
Pt1 C3 1.992(10) . ?
Pt1 C1 1.998(11) . ?
Pt1 C1 1.998(11) 2_656 ?
Fe1 N2 2.122(8) 7_566 ?
Fe1 N2 2.122(8) . ?
Fe1 O0 2.170(5) . ?
Fe1 O0 2.170(5) 7_566 ?
Fe1 N4 2.189(6) . ?
Fe1 N4 2.189(6) 7_566 ?
C1 N3 1.144(15) . ?
C3 N2 1.146(14) . ?
N4 C6 1.343(11) . ?
N4 C10 1.346(10) . ?
C6 C7 1.369(16) . ?
C6 H6 0.9300 . ?
C7 C8 1.399(19) . ?
C7 H7 0.9300 . ?
C8 C9 1.407(15) . ?
C8 C8 1.46(2) 5_565 ?
C9 C10 1.381(12) . ?
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
C3 Pt1 C3 88.3(5) 2_656 . ?
C3 Pt1 C1 90.4(5) 2_656 . ?
C3 Pt1 C1 178.7(3) . . ?
C3 Pt1 C1 178.7(3) 2_656 2_656 ?
C3 Pt1 C1 90.4(5) . 2_656 ?
C1 Pt1 C1 90.9(6) . 2_656 ?
N2 Fe1 N2 180.0 7_566 . ?
N2 Fe1 O0 89.5(3) 7_566 . ?
N2 Fe1 O0 90.5(3) . . ?
N2 Fe1 O0 90.5(3) 7_566 7_566 ?
N2 Fe1 O0 89.5(3) . 7_566 ?
O0 Fe1 O0 180.0(2) . 7_566 ?
N2 Fe1 N4 89.9(3) 7_566 . ?
N2 Fe1 N4 90.1(3) . . ?
O0 Fe1 N4 87.6(2) . . ?
O0 Fe1 N4 92.4(2) 7_566 . ?
N2 Fe1 N4 90.1(3) 7_566 7_566 ?
N2 Fe1 N4 89.9(3) . 7_566 ?
O0 Fe1 N4 92.4(2) . 7_566 ?
O0 Fe1 N4 87.6(2) 7_566 7_566 ?
N4 Fe1 N4 180.0(3) . 7_566 ?
N3 C1 Pt1 179.1(10) . . ?
N2 C3 Pt1 178.7(9) . . ?
C3 N2 Fe1 173.9(9) . . ?
C6 N4 C10 115.4(7) . . ?
C6 N4 Fe1 122.4(5) . . ?
C10 N4 Fe1 122.2(6) . . ?
N4 C6 C7 124.1(9) . . ?
N4 C6 H6 117.9 . . ?
C7 C6 H6 117.9 . . ?
C6 C7 C8 120.2(9) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C7 C8 C9 116.3(9) . . ?
C7 C8 C8 122.2(13) . 5_565 ?
C9 C8 C8 121.5(12) . 5_565 ?
C10 C9 C8 118.8(9) . . ?
C10 C9 H9 120.6 . . ?
C8 C9 H9 120.6 . . ?
N4 C10 C9 124.6(9) . . ?
N4 C10 H10 117.7 . . ?
C9 C10 H10 117.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N4 C6 C7 -7.8(18) . . . . ?
Fe1 N4 C6 C7 173.9(13) . . . . ?
N4 C6 C7 C8 3(3) . . . . ?
C6 C7 C8 C9 3(2) . . . . ?
C6 C7 C8 C8 -177.4(15) . . . 5_565 ?
C7 C8 C9 C10 -3.9(17) . . . . ?
C8 C8 C9 C10 176.7(11) 5_565 . . . ?
C6 N4 C10 C9 7.0(14) . . . . ?
Fe1 N4 C10 C9 -174.6(7) . . . . ?
C8 C9 C10 N4 -1.3(14) . . . . ?

_refine_diff_density_max         4.100
_refine_diff_density_min         -2.807
_refine_diff_density_rms         0.311

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL 160_Ptbpy_300K
REM  Yadorkari-X generated
CELL 0.71073 15.6672 15.1357 7.3104 90.0000 110.5700 90.0000
ZERR 4.0 0.0024 0.0023 0.0011 0.0000 0.0020 0.0000
LATT 7
SYMM -X, +Y, 1/2-Z

REM  SPGR C2/c monoclinic
SFAC C H N Fe Pt O
UNIT 56 32 24 4 4 8
SIZE 0.30 0.30 0.30
TEMP 23.0
L.S. 50
FMAP 2
PLAN -1
ACTA
CONF
WPDB -1
BOND $H
MERG 2
OMIT -10.000000 51.000000

WGHT    0.063100    6.989800
FVAR       0.11615   0.00000
PT1   5    0.500000    0.503357    0.750000    10.50000    0.02016    0.01147 =
         0.02565    0.00000   -0.00094    0.00000
FE1   4    0.250000    0.750000    0.500000    10.50000    0.02002    0.01590 =
         0.02588   -0.00489   -0.00620    0.00195
O0    6    0.293015    0.789894    0.260586    11.00000    0.03397    0.02895 =
         0.03291   -0.00077    0.00003    0.00064
C1    1    0.595402    0.410746    0.858169    11.00000    0.04280    0.02778 =
         0.03343   -0.00139    0.01206   -0.00209
C3    1    0.407026    0.597739    0.644922    11.00000    0.02798    0.01901 =
         0.02731   -0.00854   -0.00281   -0.00735
N2    3    0.354524    0.653131    0.587341    11.00000    0.02688    0.02193 =
         0.03499   -0.00318   -0.00428    0.00753
N4    3    0.158652    0.654919    0.299658    11.00000    0.03042    0.01974 =
         0.03763   -0.00909   -0.00332   -0.00039
C6    1    0.173978    0.567473    0.315341    11.00000    0.02761    0.02671 =
         0.07120   -0.00507   -0.01694   -0.00110
AFIX  43
H6    2    0.228379    0.547778    0.407355    11.00000   -1.20000
AFIX   0
C7    1    0.114568    0.505520    0.204419    11.00000    0.05556    0.02273 =
         0.07129   -0.00697   -0.01265   -0.00265
AFIX  43
H7    2    0.128056    0.445751    0.226322    11.00000   -1.20000
AFIX   0
C8    1    0.033623    0.531805    0.058209    11.00000    0.03884    0.03245 =
         0.04632   -0.00871    0.00112   -0.00391
C9    1    0.020719    0.623394    0.027637    11.00000    0.04591    0.02960 =
         0.03626   -0.00951   -0.00824   -0.00956
AFIX  43
H9    2   -0.029863    0.645145   -0.072541    11.00000   -1.20000
AFIX   0
C10   1    0.084485    0.680385    0.149003    11.00000    0.04187    0.02838 =
         0.04722   -0.00252   -0.00502   -0.00963
AFIX  43
H10   2    0.075568    0.740641    0.124971    11.00000   -1.20000
AFIX   0
N3    3    0.650873    0.358557    0.920723    11.00000    0.05229    0.04019 =
         0.04970    0.01262    0.01103    0.03247

HKLF 4 1 1 0 0 0 1 0 0 0 1

REM  160_Ptbpy_300K
REM R1 =  0.0501 for    1383 Fo > 4sig(Fo)  and  0.0531 for all    1515 data
REM    112 parameters refined using      0 restraints

END

WGHT      0.0630      7.0542

REM Highest difference peak  4.100,  deepest hole -2.807,  1-sigma level  0.311
Q1    1   0.4684  0.5015  0.8329  11.00000  0.05    4.10
;
_shelx_res_checksum              87032
