# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2008

data_global

_journal_coden_Cambridge         222

loop_
_publ_author_name
'Neil Robertson'
'J Durrant'
'James R. Jennings'
'Lucy P. Moorcraft'
'Ana Morandeira'
'Simon Parsons'
'L M Peter'
'Andrew R Turner'
'Lesley Yellowlees'

_publ_contact_author_name        'Neil Robertson'
_publ_contact_author_email       NEIL.ROBERTSON@ED.AC.UK

_publ_section_title              
;
Synthesis and Properties of [Pt(4-CO2CH3-py)2(mnt)];
comparison of pyridyl and bipyridyl-based dyes for Solar Cells

;

# Attachment 'Robertson_-_Ptpy2Cl2.cif.cif'

data_nr0508
_database_code_depnum_ccdc_archive 'CCDC 694836'

_audit_creation_method           SHELXL-97
_audit_creation_date             05-08-02
_chemical_compound_source        'Lucy Moorcraft reaction XD1'

_exptl_crystal_recrystallization_method 
;
>From a mixtire of CH2Cl2 and heptane.
;

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[PtCl2(C7H7NO2)2]'
_chemical_formula_sum            'C14 H14 Cl2 N2 O4 Pt'
_chemical_formula_weight         540.26

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
_symmetry_space_group_name_Hall  '-C 2yc'

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                   13.0562(3)
_cell_length_b                   8.2030(2)
_cell_length_c                   15.3120(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.4710(10)
_cell_angle_gamma                90.00
_cell_volume                     1625.99(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6769
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      30

_exptl_crystal_description       tablet
_exptl_crystal_colour            Colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1024
_exptl_absorpt_coefficient_mu    8.978
_exptl_absorpt_correction_type   Multiscan
_exptl_absorpt_correction_T_min  0.137
_exptl_absorpt_correction_T_max  0.280
_exptl_absorpt_process_details   'Sadabs v 2.10'

_exptl_special_details           
;
Data collection strategy optimised with COSMO.
Oxford Cryosystems LT device.
;

_diffrn_ambient_temperature      150(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 Smart APEX CCD'
_diffrn_measurement_method       'Omega and Phi'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9237
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0267
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         29.68
_reflns_number_total             2175
_reflns_number_gt                2084
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       Smart
_computing_cell_refinement       Saint
_computing_data_reduction        Saint
_computing_structure_solution    Dirdif
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    XP
_computing_publication_material  'XCIF, PLATON'

_refine_special_details          
;

The molecule resides on a .2. axis. The H-atoms attached to C10 were
located in a difference synthesis; the CH distances and HCH angles were
fixed at ideal values, but the methyl-torion was refined.

Checkcif output:

761_ALERT_1_A CIF Contains no X-H Bonds ...................... ?
762_ALERT_1_A CIF Contains no X-Y-H or H-Y-H Angles .......... ?

These have ideal values; see above.

912_ALERT_3_B # Missing FCF Reflections Above STH/L=0.6 ...... 133

The data collection strategy used aimed to achieve a complete data set to
2\q = 54 deg. Some higher angle data were collected in the process and these
have been included in the refinement.

#===============================================================================
Resolution & Completeness Statistics (Cumulative)
#===============================================================================
Theta sin(th)/Lambda Complete Expected Measured Missing
#-------------------------------------------------------------------------------
20.82 0.500 1.000 851 851 0
23.01 0.550 1.000 1131 1131 0
25.24 0.600 1.000 1476 1476 0
#----------------------------------------------------------- ACTA Min. Res. ----
27.51 0.650 0.999 1861 1860 1
29.68 0.697 0.942 2308 2175 133

042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?

The one given is more chemically meaningful.

060_ALERT_3_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.38

Sadabs corrects for all systematic errors that lead to disparities in the
intensities of symmetry-equivalent data. These may include absorption by the
mount, crystal decay etc.

094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.14

There is a relatively large difference peak (1.33 e/Ang^3) next to Pt1,
but this is to be expected in a caompound like this, where absorption
effects are significant.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0213P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     'Patterson in Cc'
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom/difmap
_refine_ls_hydrogen_treatment    'riding/rotating group'
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2175
_refine_ls_number_parameters     106
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0182
_refine_ls_wR_factor_ref         0.0431
_refine_ls_wR_factor_gt          0.0426
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.002
_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 -0.115143(13) 0.2500 0.01871(5) Uani 1 2 d S . .
Cl1 Cl 0.07770(5) -0.30915(8) 0.17260(4) 0.02814(13) Uani 1 1 d . . .
N1 N 0.06498(14) 0.0604(3) 0.18304(13) 0.0190(4) Uani 1 1 d . . .
C2 C 0.15240(19) 0.1383(3) 0.21812(18) 0.0237(5) Uani 1 1 d . . .
H2 H 0.1838 0.1092 0.2755 0.028 Uiso 1 1 calc R . .
C3 C 0.19672(17) 0.2584(3) 0.17268(16) 0.0243(5) Uani 1 1 d . . .
H3 H 0.2586 0.3100 0.1981 0.029 Uiso 1 1 calc R . .
C4 C 0.15038(17) 0.3035(3) 0.08950(16) 0.0203(4) Uani 1 1 d . . .
C5 C 0.05988(17) 0.2259(3) 0.05396(16) 0.0246(5) Uani 1 1 d . . .
H5 H 0.0264 0.2551 -0.0027 0.030 Uiso 1 1 calc R . .
C6 C 0.01961(19) 0.1058(3) 0.10239(18) 0.0235(5) Uani 1 1 d . . .
H6 H -0.0424 0.0530 0.0782 0.028 Uiso 1 1 calc R . .
C7 C 0.19879(18) 0.4347(3) 0.04031(16) 0.0223(5) Uani 1 1 d . . .
O8 O 0.27758(13) 0.5038(2) 0.06910(13) 0.0302(4) Uani 1 1 d . . .
O9 O 0.14562(14) 0.4608(2) -0.03768(12) 0.0305(4) Uani 1 1 d . . .
C10 C 0.1844(3) 0.5850(3) -0.0911(2) 0.0355(6) Uani 1 1 d . . .
H10A H 0.1739 0.6924 -0.0658 0.053 Uiso 1 1 calc R . .
H10B H 0.1475 0.5796 -0.1510 0.053 Uiso 1 1 calc R . .
H10C H 0.2584 0.5674 -0.0930 0.053 Uiso 1 1 calc R . .

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 0.01888(7) 0.01910(8) 0.01829(7) 0.000 0.00296(5) 0.000
Cl1 0.0294(3) 0.0269(3) 0.0276(3) -0.0070(2) 0.0019(2) 0.0050(2)
N1 0.0172(8) 0.0202(10) 0.0201(10) -0.0027(8) 0.0036(7) -0.0012(8)
C2 0.0217(11) 0.0253(12) 0.0229(12) -0.0005(9) -0.0015(9) -0.0030(9)
C3 0.0210(10) 0.0258(13) 0.0252(12) -0.0022(10) -0.0004(9) -0.0036(9)
C4 0.0218(10) 0.0191(12) 0.0208(11) -0.0020(9) 0.0056(8) -0.0011(8)
C5 0.0235(10) 0.0295(13) 0.0201(12) -0.0001(10) 0.0005(9) -0.0036(9)
C6 0.0198(10) 0.0303(14) 0.0201(12) 0.0001(9) 0.0018(9) -0.0039(8)
C7 0.0237(10) 0.0201(11) 0.0245(13) -0.0023(10) 0.0084(9) -0.0001(9)
O8 0.0260(8) 0.0283(10) 0.0364(11) 0.0016(8) 0.0049(7) -0.0066(7)
O9 0.0353(9) 0.0300(10) 0.0261(10) 0.0059(8) 0.0035(8) -0.0084(8)
C10 0.0452(16) 0.0295(14) 0.0340(16) 0.0092(12) 0.0135(13) -0.0049(12)

_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 N1 2.018(2) 2 ?
Pt1 N1 2.018(2) . ?
Pt1 Cl1 2.2976(6) . ?
Pt1 Cl1 2.2976(6) 2 ?
N1 C6 1.351(3) . ?
N1 C2 1.356(3) . ?
C2 C3 1.376(4) . ?
C3 C4 1.387(3) . ?
C4 C5 1.389(3) . ?
C4 C7 1.500(3) . ?
C5 C6 1.378(3) . ?
C7 O8 1.206(3) . ?
C7 O9 1.318(3) . ?
O9 C10 1.440(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
N1 Pt1 N1 88.91(11) 2 . ?
N1 Pt1 Cl1 178.20(6) 2 . ?
N1 Pt1 Cl1 89.39(6) . . ?
N1 Pt1 Cl1 89.39(6) 2 2 ?
N1 Pt1 Cl1 178.20(5) . 2 ?
Cl1 Pt1 Cl1 92.32(3) . 2 ?
C6 N1 C2 118.6(2) . . ?
C6 N1 Pt1 119.87(16) . . ?
C2 N1 Pt1 121.50(17) . . ?
N1 C2 C3 121.6(2) . . ?
C2 C3 C4 119.6(2) . . ?
C3 C4 C5 119.0(2) . . ?
C3 C4 C7 119.4(2) . . ?
C5 C4 C7 121.6(2) . . ?
C6 C5 C4 118.8(2) . . ?
N1 C6 C5 122.5(2) . . ?
O8 C7 O9 125.3(2) . . ?
O8 C7 C4 123.3(2) . . ?
O9 C7 C4 111.4(2) . . ?
C7 O9 C10 116.6(2) . . ?

_diffrn_measured_fraction_theta_max 0.942
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.326
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.125