# Electronic Supplementary Material (ESI) for Chemical Science
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_name_full 'Chemical Science'
_journal_coden_cambridge 1475
_journal_year ?
_journal_volume ?
_journal_page_first ?
_publ_contact_author_email doerrer@bu.edu
_publ_contact_author_name 'Linda Doerrer'
loop_
_publ_author_name
'Linda Doerrer'
'Eric Dahl'
'Frederick Baddour'
'Wesley Hoffert'
'Stephanie Fiedler'
'Matthew Shores'
'Gordon Yee'
'Jean-Pierre Djukic'
'Jeffrey Bacon'
'Arnold Rheingold'
data_dahl2_0m_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 842000'
#TrackingRef '- Dahl-Doerrer-PtMtba-all_compounds-v4.cif'
_symmetry_space_group_name_hall '-P 2yn'
#Added by publCIF
_audit_update_record
;
2010-08-23 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C28 H22 Fe O5 Pt S4, C3 H6 O'
_chemical_formula_sum 'C31 H28 Fe O6 Pt S4'
_chemical_formula_weight 875.71
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 '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'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 1 21/n 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.6379(6)
_cell_length_b 11.5625(5)
_cell_length_c 18.7162(8)
_cell_angle_alpha 90.00
_cell_angle_beta 96.152(2)
_cell_angle_gamma 90.00
_cell_volume 3149.5(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9696
_cell_measurement_theta_min 9.003
_cell_measurement_theta_max 131.653
_exptl_crystal_description needle
_exptl_crystal_colour 'red dichroic'
_exptl_crystal_size_max 0.093
_exptl_crystal_size_mid 0.043
_exptl_crystal_size_min 0.030
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.847
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1720
_exptl_absorpt_coefficient_mu 14.721
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.5111
_exptl_absorpt_correction_T_max 0.7528
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Proteum-R'
_diffrn_measurement_method '\f & \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 37259
_diffrn_reflns_av_R_equivalents 0.0540
_diffrn_reflns_av_sigmaI/netI 0.0257
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 3.65
_diffrn_reflns_theta_max 66.23
_reflns_number_total 5450
_reflns_number_gt 5116
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'APEX2 (Bruker, 2006)'
_computing_data_reduction 'SAINT (Bruker, 2006)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics ?
_computing_publication_material ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0455P)^2^+2.8083P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 5450
_refine_ls_number_parameters 396
_refine_ls_number_restraints 4
_refine_ls_R_factor_all 0.0285
_refine_ls_R_factor_gt 0.0266
_refine_ls_wR_factor_ref 0.0741
_refine_ls_wR_factor_gt 0.0724
_refine_ls_goodness_of_fit_ref 1.096
_refine_ls_restrained_S_all 1.096
_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 0.435707(8) 0.623554(11) 0.062243(7) 0.01703(7) Uani 1 1 d . . .
Fe1 Fe 0.43925(3) 0.85065(5) 0.07165(3) 0.01562(12) Uani 1 1 d D . .
C24 C 0.3479(2) 0.9230(3) -0.17571(18) 0.0218(7) Uani 1 1 d . . .
H24 H 0.3704 0.9795 -0.1414 0.026 Uiso 1 1 calc R . .
C21 C 0.7775(2) 0.6845(3) 0.01046(18) 0.0232(7) Uani 1 1 d . . .
H21 H 0.7539 0.6079 0.0102 0.028 Uiso 1 1 calc R . .
S1 S 0.29530(6) 0.61742(6) 0.11054(5) 0.02140(19) Uani 1 1 d . . .
S3 S 0.57443(6) 0.63053(7) 0.01364(5) 0.02153(19) Uani 1 1 d . . .
S2 S 0.51392(6) 0.60814(7) 0.17750(5) 0.02217(18) Uani 1 1 d . . .
S4 S 0.35921(6) 0.63696(7) -0.05324(5) 0.02075(18) Uani 1 1 d . . .
O3 O 0.58379(14) 0.8407(2) 0.06877(12) 0.0199(5) Uani 1 1 d . . .
O1 O 0.29643(14) 0.8369(2) 0.07258(12) 0.0211(5) Uani 1 1 d . . .
O4 O 0.42327(15) 0.8490(2) -0.04132(12) 0.0193(5) Uani 1 1 d . . .
O2 O 0.46064(15) 0.8248(2) 0.18116(12) 0.0228(5) Uani 1 1 d . . .
C1S C 0.2950(3) 0.2132(4) 0.1763(2) 0.0346(9) Uani 1 1 d . . .
C13 C 0.6323(2) 0.7143(4) 0.4003(2) 0.0325(9) Uani 1 1 d . . .
H13 H 0.6707 0.6608 0.4278 0.039 Uiso 1 1 calc R . .
C8 C 0.5010(2) 0.7431(3) 0.21436(19) 0.0223(7) Uani 1 1 d . . .
C20 C 0.8675(2) 0.7040(3) -0.00427(19) 0.0291(8) Uani 1 1 d . . .
H20 H 0.9051 0.6405 -0.0146 0.035 Uiso 1 1 calc R . .
C12 C 0.6128(2) 0.8207(4) 0.4296(2) 0.0336(9) Uani 1 1 d . . .
H12 H 0.6380 0.8398 0.4770 0.040 Uiso 1 1 calc R . .
C26 C 0.2795(2) 0.8749(3) -0.2947(2) 0.0262(8) Uani 1 1 d . . .
H26 H 0.2548 0.8987 -0.3414 0.031 Uiso 1 1 calc R . .
C4 C 0.0571(2) 0.9312(3) 0.1542(2) 0.0320(8) Uani 1 1 d . . .
H4 H 0.0421 1.0105 0.1589 0.038 Uiso 1 1 calc R . .
C9 C 0.5399(2) 0.7650(3) 0.29057(18) 0.0223(7) Uani 1 1 d . . .
C14 C 0.5963(2) 0.6858(3) 0.33104(19) 0.0260(7) Uani 1 1 d . . .
H14 H 0.6097 0.6130 0.3112 0.031 Uiso 1 1 calc R . .
C2 C 0.1630(2) 0.7843(3) 0.12407(18) 0.0211(7) Uani 1 1 d . . .
C11 C 0.5566(3) 0.8991(4) 0.3899(2) 0.0316(8) Uani 1 1 d . . .
H11 H 0.5428 0.9716 0.4101 0.038 Uiso 1 1 calc R . .
C17 C 0.7573(2) 0.8896(3) 0.0257(2) 0.0238(7) Uani 1 1 d . . .
H17 H 0.7199 0.9534 0.0358 0.029 Uiso 1 1 calc R . .
C1 C 0.2538(2) 0.7568(3) 0.09883(18) 0.0193(7) Uani 1 1 d . . .
C27 C 0.2813(2) 0.7591(3) -0.27647(19) 0.0263(8) Uani 1 1 d . . .
H27 H 0.2582 0.7030 -0.3109 0.032 Uiso 1 1 calc R . .
C2S C 0.3601(3) 0.3088(4) 0.1667(2) 0.0413(10) Uani 1 1 d . . .
H2SA H 0.3385 0.3530 0.1235 0.062 Uiso 1 1 calc R . .
H2SB H 0.4211 0.2768 0.1616 0.062 Uiso 1 1 calc R . .
H2SC H 0.3639 0.3599 0.2087 0.062 Uiso 1 1 calc R . .
C28 C 0.3166(2) 0.7243(3) -0.20801(18) 0.0232(7) Uani 1 1 d . . .
H28 H 0.3188 0.6444 -0.1961 0.028 Uiso 1 1 calc R . .
C16 C 0.7220(2) 0.7776(3) 0.02560(17) 0.0192(6) Uani 1 1 d . . .
C19 C 0.9022(2) 0.8143(3) -0.0039(2) 0.0310(8) Uani 1 1 d . . .
H19 H 0.9638 0.8269 -0.0138 0.037 Uiso 1 1 calc R . .
C23 C 0.3489(2) 0.8062(3) -0.15654(18) 0.0185(6) Uani 1 1 d . . .
C6 C 0.0176(2) 0.7310(3) 0.1642(2) 0.0300(8) Uani 1 1 d . . .
H6 H -0.0246 0.6734 0.1760 0.036 Uiso 1 1 calc R . .
C22 C 0.3821(2) 0.7736(3) -0.08129(18) 0.0188(7) Uani 1 1 d . . .
C10 C 0.5208(3) 0.8710(3) 0.3206(2) 0.0273(8) Uani 1 1 d . . .
H10 H 0.4827 0.9250 0.2933 0.033 Uiso 1 1 calc R . .
C25 C 0.3143(2) 0.9567(3) -0.24431(18) 0.0240(7) Uani 1 1 d . . .
H25 H 0.3149 1.0361 -0.2572 0.029 Uiso 1 1 calc R . .
O1S O 0.3135(2) 0.1132(3) 0.16531(19) 0.0489(9) Uani 1 1 d . . .
C3 C 0.1404(2) 0.9003(3) 0.1313(2) 0.0272(8) Uani 1 1 d . . .
H3 H 0.1825 0.9586 0.1204 0.033 Uiso 1 1 calc R . .
C7 C 0.1008(2) 0.6986(3) 0.14110(19) 0.0264(7) Uani 1 1 d . . .
H7 H 0.1157 0.6191 0.1368 0.032 Uiso 1 1 calc R . .
C5 C -0.0043(2) 0.8469(4) 0.1702(2) 0.0327(8) Uani 1 1 d . . .
H5 H -0.0619 0.8684 0.1854 0.039 Uiso 1 1 calc R . .
C18 C 0.8473(2) 0.9080(3) 0.0109(2) 0.0292(8) Uani 1 1 d . . .
H18 H 0.8713 0.9844 0.0110 0.035 Uiso 1 1 calc R . .
C15 C 0.6243(2) 0.7608(3) 0.04034(17) 0.0173(6) Uani 1 1 d . . .
O1W O 0.43405(14) 1.02464(19) 0.08300(13) 0.0218(5) Uani 1 1 d D . .
C3S C 0.2034(3) 0.2442(5) 0.1995(2) 0.0522(13) Uani 1 1 d . . .
H3SA H 0.1607 0.2634 0.1573 0.078 Uiso 1 1 calc R . .
H3SC H 0.2102 0.3110 0.2319 0.078 Uiso 1 1 calc R . .
H3SB H 0.1793 0.1783 0.2247 0.078 Uiso 1 1 calc R . .
H2W H 0.480(2) 1.069(2) 0.075(3) 0.078 Uiso 1 1 d D . .
H1W H 0.401(3) 1.057(2) 0.113(2) 0.078 Uiso 1 1 d 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 0.01647(10) 0.01547(11) 0.01921(11) 0.00074(4) 0.00216(6) 0.00016(4)
Fe1 0.0144(2) 0.0162(2) 0.0163(3) 0.00019(19) 0.0019(2) 0.00049(17)
C24 0.0173(14) 0.0252(18) 0.0227(18) -0.0026(14) 0.0021(13) 0.0005(13)
C21 0.0213(15) 0.0273(18) 0.0208(17) 0.0011(13) 0.0009(13) 0.0020(13)
S1 0.0181(4) 0.0214(4) 0.0253(5) 0.0027(3) 0.0049(3) -0.0008(3)
S3 0.0197(4) 0.0187(4) 0.0272(5) -0.0029(3) 0.0071(4) -0.0003(3)
S2 0.0213(4) 0.0230(4) 0.0215(4) 0.0037(3) -0.0008(3) 0.0016(3)
S4 0.0225(4) 0.0182(4) 0.0210(4) 0.0000(3) -0.0004(3) -0.0026(3)
O3 0.0173(10) 0.0203(11) 0.0221(12) -0.0017(10) 0.0016(9) 0.0012(9)
O1 0.0174(10) 0.0219(12) 0.0242(12) 0.0010(10) 0.0027(9) -0.0011(9)
O4 0.0204(11) 0.0193(11) 0.0181(12) -0.0007(9) 0.0019(9) -0.0013(9)
O2 0.0242(11) 0.0231(13) 0.0207(12) 0.0024(9) 0.0010(9) 0.0034(10)
C1S 0.0314(19) 0.049(3) 0.023(2) -0.0103(17) 0.0027(15) 0.0074(18)
C13 0.0191(16) 0.053(2) 0.0248(19) 0.0141(17) -0.0013(14) -0.0046(16)
C8 0.0157(15) 0.0290(19) 0.0229(18) 0.0020(14) 0.0048(14) -0.0030(13)
C20 0.0217(16) 0.039(2) 0.0266(19) 0.0000(15) 0.0041(14) 0.0091(15)
C12 0.0261(17) 0.055(3) 0.0195(18) 0.0017(17) 0.0013(14) -0.0120(17)
C26 0.0198(16) 0.039(2) 0.0203(19) 0.0021(13) 0.0022(14) 0.0015(13)
C4 0.0267(17) 0.035(2) 0.035(2) 0.0038(16) 0.0075(16) 0.0062(15)
C9 0.0150(14) 0.0330(19) 0.0190(17) 0.0036(13) 0.0022(13) -0.0050(13)
C14 0.0177(15) 0.034(2) 0.0262(18) 0.0061(15) 0.0043(13) -0.0043(14)
C2 0.0159(14) 0.0282(18) 0.0187(16) 0.0010(13) 0.0005(13) 0.0009(13)
C11 0.0316(19) 0.038(2) 0.025(2) -0.0053(16) 0.0050(16) -0.0082(16)
C17 0.0204(17) 0.0282(19) 0.0222(19) -0.0001(13) -0.0002(14) 0.0007(13)
C1 0.0183(15) 0.0225(17) 0.0166(16) 0.0002(12) 0.0001(13) 0.0000(12)
C27 0.0239(17) 0.034(2) 0.0203(18) -0.0052(14) 0.0011(14) -0.0039(14)
C2S 0.059(3) 0.034(2) 0.031(2) -0.0001(17) 0.0064(19) 0.0041(19)
C28 0.0210(15) 0.0262(18) 0.0227(18) -0.0016(14) 0.0038(13) -0.0015(13)
C16 0.0173(15) 0.0238(17) 0.0162(16) 0.0011(13) 0.0010(13) 0.0002(13)
C19 0.0187(16) 0.046(2) 0.028(2) 0.0022(16) 0.0052(14) -0.0011(15)
C23 0.0129(13) 0.0199(16) 0.0233(17) 0.0009(13) 0.0041(12) 0.0005(12)
C6 0.0192(16) 0.039(2) 0.032(2) 0.0009(16) 0.0046(15) -0.0068(15)
C22 0.0156(14) 0.0184(16) 0.0228(17) -0.0049(13) 0.0040(13) -0.0017(12)
C10 0.0253(18) 0.034(2) 0.022(2) 0.0021(14) 0.0037(15) -0.0030(14)
C25 0.0214(15) 0.0265(18) 0.0247(18) 0.0045(14) 0.0044(14) 0.0048(13)
O1S 0.0435(17) 0.046(2) 0.062(2) -0.0166(14) 0.0275(17) -0.0085(13)
C3 0.0221(16) 0.0316(19) 0.028(2) 0.0043(15) 0.0026(15) 0.0001(15)
C7 0.0234(16) 0.0309(19) 0.0254(19) 0.0001(14) 0.0048(14) -0.0036(14)
C5 0.0210(17) 0.047(2) 0.031(2) 0.0024(17) 0.0064(15) 0.0050(16)
C18 0.0252(17) 0.0341(19) 0.029(2) 0.0019(16) 0.0040(15) -0.0059(16)
C15 0.0175(15) 0.0193(16) 0.0148(16) 0.0016(12) -0.0004(13) 0.0021(12)
O1W 0.0200(11) 0.0198(12) 0.0262(12) 0.0007(10) 0.0053(9) -0.0004(9)
C3S 0.037(2) 0.088(4) 0.033(2) -0.010(2) 0.0061(19) 0.019(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 S3 2.3136(8) . ?
Pt1 S4 2.3304(9) . ?
Pt1 S1 2.3333(8) . ?
Pt1 S2 2.3381(9) . ?
Pt1 Fe1 2.6319(6) . ?
Fe1 O1W 2.025(2) . ?
Fe1 O2 2.062(2) . ?
Fe1 O1 2.099(2) . ?
Fe1 O4 2.102(2) . ?
Fe1 O3 2.125(2) . ?
C24 C25 1.381(5) . ?
C24 C23 1.396(5) . ?
C24 H24 0.9500 . ?
C21 C20 1.393(5) . ?
C21 C16 1.397(5) . ?
C21 H21 0.9500 . ?
S1 C1 1.728(3) . ?
S3 C15 1.724(3) . ?
S2 C8 1.724(3) . ?
S4 C22 1.710(3) . ?
O3 C15 1.248(4) . ?
O1 C1 1.247(4) . ?
O4 C22 1.259(4) . ?
O2 C8 1.245(4) . ?
C1S O1S 1.210(5) . ?
C1S C2S 1.484(6) . ?
C1S C3S 1.497(5) . ?
C13 C14 1.385(5) . ?
C13 C12 1.390(6) . ?
C13 H13 0.9500 . ?
C8 C9 1.499(5) . ?
C20 C19 1.374(6) . ?
C20 H20 0.9500 . ?
C12 C11 1.384(6) . ?
C12 H12 0.9500 . ?
C26 C27 1.382(5) . ?
C26 C25 1.393(5) . ?
C26 H26 0.9500 . ?
C4 C5 1.381(5) . ?
C4 C3 1.382(5) . ?
C4 H4 0.9500 . ?
C9 C10 1.390(5) . ?
C9 C14 1.399(5) . ?
C14 H14 0.9500 . ?
C2 C3 1.391(5) . ?
C2 C7 1.404(5) . ?
C2 C1 1.492(4) . ?
C11 C10 1.384(6) . ?
C11 H11 0.9500 . ?
C17 C18 1.390(5) . ?
C17 C16 1.394(5) . ?
C17 H17 0.9500 . ?
C27 C28 1.389(5) . ?
C27 H27 0.9500 . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C28 C23 1.397(5) . ?
C28 H28 0.9500 . ?
C16 C15 1.497(4) . ?
C19 C18 1.395(5) . ?
C19 H19 0.9500 . ?
C23 C22 1.488(5) . ?
C6 C7 1.387(5) . ?
C6 C5 1.385(6) . ?
C6 H6 0.9500 . ?
C10 H10 0.9500 . ?
C25 H25 0.9500 . ?
C3 H3 0.9500 . ?
C7 H7 0.9500 . ?
C5 H5 0.9500 . ?
C18 H18 0.9500 . ?
O1W H2W 0.865(10) . ?
O1W H1W 0.865(10) . ?
C3S H3SA 0.9800 . ?
C3S H3SC 0.9800 . ?
C3S H3SB 0.9800 . ?
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
S3 Pt1 S4 89.30(3) . . ?
S3 Pt1 S1 179.56(3) . . ?
S4 Pt1 S1 90.33(3) . . ?
S3 Pt1 S2 90.10(3) . . ?
S4 Pt1 S2 179.17(3) . . ?
S1 Pt1 S2 90.28(3) . . ?
S3 Pt1 Fe1 88.84(2) . . ?
S4 Pt1 Fe1 89.98(2) . . ?
S1 Pt1 Fe1 90.93(2) . . ?
S2 Pt1 Fe1 90.58(2) . . ?
O1W Fe1 O2 92.48(10) . . ?
O1W Fe1 O1 91.48(9) . . ?
O2 Fe1 O1 91.49(9) . . ?
O1W Fe1 O4 96.49(10) . . ?
O2 Fe1 O4 170.82(10) . . ?
O1 Fe1 O4 90.24(9) . . ?
O1W Fe1 O3 96.03(9) . . ?
O2 Fe1 O3 88.39(9) . . ?
O1 Fe1 O3 172.49(10) . . ?
O4 Fe1 O3 88.73(9) . . ?
O1W Fe1 Pt1 175.86(6) . . ?
O2 Fe1 Pt1 85.50(7) . . ?
O1 Fe1 Pt1 84.97(7) . . ?
O4 Fe1 Pt1 85.67(6) . . ?
O3 Fe1 Pt1 87.53(6) . . ?
C25 C24 C23 120.3(3) . . ?
C25 C24 H24 119.8 . . ?
C23 C24 H24 119.8 . . ?
C20 C21 C16 119.9(3) . . ?
C20 C21 H21 120.0 . . ?
C16 C21 H21 120.0 . . ?
C1 S1 Pt1 103.59(11) . . ?
C15 S3 Pt1 106.19(11) . . ?
C8 S2 Pt1 103.67(12) . . ?
C22 S4 Pt1 104.82(12) . . ?
C15 O3 Fe1 124.8(2) . . ?
C1 O1 Fe1 126.9(2) . . ?
C22 O4 Fe1 126.7(2) . . ?
C8 O2 Fe1 128.3(2) . . ?
O1S C1S C2S 122.2(3) . . ?
O1S C1S C3S 120.1(4) . . ?
C2S C1S C3S 117.7(4) . . ?
C14 C13 C12 120.4(4) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
O2 C8 C9 117.3(3) . . ?
O2 C8 S2 123.6(3) . . ?
C9 C8 S2 119.1(2) . . ?
C19 C20 C21 120.5(3) . . ?
C19 C20 H20 119.8 . . ?
C21 C20 H20 119.8 . . ?
C11 C12 C13 120.2(4) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C27 C26 C25 119.6(3) . . ?
C27 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C5 C4 C3 120.1(4) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C10 C9 C14 119.4(3) . . ?
C10 C9 C8 117.5(3) . . ?
C14 C9 C8 123.1(3) . . ?
C13 C14 C9 119.6(4) . . ?
C13 C14 H14 120.2 . . ?
C9 C14 H14 120.2 . . ?
C3 C2 C7 119.5(3) . . ?
C3 C2 C1 117.7(3) . . ?
C7 C2 C1 122.9(3) . . ?
C10 C11 C12 119.5(4) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
O1 C1 C2 117.9(3) . . ?
O1 C1 S1 124.0(2) . . ?
C2 C1 S1 118.1(2) . . ?
C26 C27 C28 120.3(3) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
C27 C28 C23 120.3(3) . . ?
C27 C28 H28 119.9 . . ?
C23 C28 H28 119.9 . . ?
C17 C16 C21 119.5(3) . . ?
C17 C16 C15 118.8(3) . . ?
C21 C16 C15 121.7(3) . . ?
C20 C19 C18 120.1(3) . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C28 C23 C24 119.0(3) . . ?
C28 C23 C22 122.2(3) . . ?
C24 C23 C22 118.8(3) . . ?
C7 C6 C5 120.4(3) . . ?
C7 C6 H6 119.8 . . ?
C5 C6 H6 119.8 . . ?
O4 C22 C23 118.3(3) . . ?
O4 C22 S4 123.7(3) . . ?
C23 C22 S4 118.0(2) . . ?
C11 C10 C9 120.9(4) . . ?
C11 C10 H10 119.5 . . ?
C9 C10 H10 119.5 . . ?
C24 C25 C26 120.4(3) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C2 C3 C4 120.4(3) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C6 C7 C2 119.5(3) . . ?
C6 C7 H7 120.3 . . ?
C2 C7 H7 120.3 . . ?
C4 C5 C6 120.2(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C17 C18 C19 120.0(3) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
O3 C15 C16 119.3(3) . . ?
O3 C15 S3 124.4(2) . . ?
C16 C15 S3 116.3(2) . . ?
Fe1 O1W H2W 122(2) . . ?
Fe1 O1W H1W 122(2) . . ?
H2W O1W H1W 111(2) . . ?
C1S C3S H3SA 109.5 . . ?
C1S C3S H3SC 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
C1S C3S H3SB 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SC C3S H3SB 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full 66.23
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max 1.565
_refine_diff_density_min -0.725
_refine_diff_density_rms 0.124
# publcif dahl2_0m _publcif_jmolscript.group loop start
loop_
_publcif_jmolscript.group
_publcif_jmolscript.id
_publcif_jmolscript.model
_publcif_jmolscript.model_type
_publcif_jmolscript.type
_publcif_jmolscript.type_group
_publcif_jmolscript.caption
_publcif_jmolscript.script
? ? ? ? ? ? ? ?
# publcif dahl2_0m _publcif_jmolscript.group loop end
###END
data_lhd256sq_Compound_2a
_database_code_depnum_ccdc_archive 'CCDC 842001'
#TrackingRef '- Dahl-Doerrer-PtMtba-all_compounds-v4.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
rem squeeze used to account for unresolved solvent
rem squeeze found 1511e with a void of 3874 angstroms
rem associated with 38 THF "C4H8O" = C152,304H, 38O
rem old formula C224,H176, O40, S32, Co8 Pt8
REM NEW FORMULA C376 H480, O78, S32, Co8, Pt8
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C47 H60 Co O9.75 Pt S4'
_chemical_formula_weight 1163.21
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 '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'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M I2/a
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
_cell_length_a 22.8140(8)
_cell_length_b 16.6711(7)
_cell_length_c 23.2989(14)
_cell_angle_alpha 90.00
_cell_angle_beta 92.135(2)
_cell_angle_gamma 90.00
_cell_volume 8855.2(7)
_cell_formula_units_Z 8
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9982
_cell_measurement_theta_min 3.26
_cell_measurement_theta_max 65.54
_exptl_crystal_description block
_exptl_crystal_colour 'pale yellow'
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.745
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 4712
_exptl_absorpt_coefficient_mu 11.013
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.2889
_exptl_absorpt_correction_T_max 0.4055
_exptl_absorpt_process_details sadabs
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(2)
_diffrn_radiation_wavelength 1.54184
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'CCD area detector'
_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 32723
_diffrn_reflns_av_R_equivalents 0.0451
_diffrn_reflns_av_sigmaI/netI 0.0354
_diffrn_reflns_limit_h_min -23
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_k_max 19
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 3.26
_diffrn_reflns_theta_max 66.02
_reflns_number_total 7410
_reflns_number_gt 5941
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0616P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7410
_refine_ls_number_parameters 452
_refine_ls_number_restraints 21
_refine_ls_R_factor_all 0.0434
_refine_ls_R_factor_gt 0.0340
_refine_ls_wR_factor_ref 0.1003
_refine_ls_wR_factor_gt 0.0964
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_restrained_S_all 1.042
_refine_ls_shift/su_max 0.046
_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
C1 C 0.6879(2) 0.1965(3) 0.1226(2) 0.0397(12) Uani 1 1 d D . .
C2 C 0.6613(2) 0.1158(3) 0.1279(2) 0.0489(13) Uani 1 1 d . . .
C3 C 0.6478(3) 0.0684(4) 0.0811(3) 0.076(2) Uani 1 1 d . . .
H3 H 0.6564 0.0862 0.0436 0.092 Uiso 1 1 calc R A .
C4 C 0.6212(4) -0.0061(5) 0.0891(3) 0.097(3) Uani 1 1 d . . .
H4 H 0.6101 -0.0374 0.0564 0.117 Uiso 1 1 calc R . .
C5 C 0.6110(4) -0.0353(5) 0.1425(4) 0.092(2) Uani 1 1 d . . .
H5 H 0.5940 -0.0868 0.1471 0.110 Uiso 1 1 calc R A .
C6 C 0.6255(3) 0.0108(4) 0.1892(3) 0.0718(19) Uani 1 1 d . . .
H6 H 0.6181 -0.0086 0.2265 0.086 Uiso 1 1 calc R . .
C7 C 0.6512(2) 0.0866(3) 0.1828(2) 0.0485(13) Uani 1 1 d . . .
H7 H 0.6616 0.1179 0.2157 0.058 Uiso 1 1 calc R A .
C8 C 0.8455(2) 0.2936(3) 0.14914(19) 0.0370(11) Uani 1 1 d D . .
C9 C 0.9048(2) 0.2654(4) 0.1690(2) 0.0488(13) Uani 1 1 d . . .
C10 C 0.9487(3) 0.2520(5) 0.1306(3) 0.074(2) Uani 1 1 d . . .
H10 H 0.9411 0.2605 0.0907 0.089 Uiso 1 1 calc R A .
C11 C 1.0049(3) 0.2258(6) 0.1505(3) 0.104(3) Uani 1 1 d . . .
H11 H 1.0345 0.2150 0.1240 0.124 Uiso 1 1 calc R . .
C12 C 1.0159(3) 0.2162(7) 0.2071(3) 0.119(4) Uani 1 1 d . . .
H12 H 1.0539 0.2008 0.2209 0.143 Uiso 1 1 calc R A .
C13 C 0.9719(4) 0.2288(8) 0.2454(3) 0.146(5) Uani 1 1 d . . .
H13 H 0.9796 0.2196 0.2852 0.175 Uiso 1 1 calc R . .
C14 C 0.9179(2) 0.2542(5) 0.2268(2) 0.070(2) Uani 1 1 d . . .
H14 H 0.8887 0.2644 0.2539 0.083 Uiso 1 1 calc R A .
C15 C 0.7762(2) 0.5082(3) 0.1421(2) 0.0416(12) Uani 1 1 d D . .
C16 C 0.7983(2) 0.5889(3) 0.1598(2) 0.0470(13) Uani 1 1 d . . .
C17 C 0.7926(3) 0.6128(4) 0.2148(3) 0.0704(18) Uani 1 1 d . . .
H17 H 0.7755 0.5769 0.2411 0.085 Uiso 1 1 calc R A .
C18 C 0.8106(4) 0.6874(5) 0.2342(4) 0.092(2) Uani 1 1 d . . .
H18 H 0.8044 0.7030 0.2727 0.110 Uiso 1 1 calc R . .
C19 C 0.8374(4) 0.7389(5) 0.1974(5) 0.113(3) Uani 1 1 d . . .
H19 H 0.8492 0.7909 0.2098 0.136 Uiso 1 1 calc R A .
C20 C 0.8468(4) 0.7131(5) 0.1413(5) 0.115(3) Uani 1 1 d . . .
H20 H 0.8675 0.7466 0.1161 0.138 Uiso 1 1 calc R . .
C21 C 0.8266(4) 0.6402(4) 0.1226(4) 0.088(2) Uani 1 1 d . . .
H21 H 0.8319 0.6244 0.0840 0.106 Uiso 1 1 calc R A .
C22 C 0.6192(2) 0.4154(3) 0.1148(2) 0.0454(13) Uani 1 1 d D . .
C23 C 0.5608(4) 0.4544(7) 0.1249(5) 0.047(5) Uani 0.470(7) 1 d PGD A 3
C24 C 0.5196(6) 0.4532(8) 0.0794(5) 0.086(5) Uani 0.470(7) 1 d PG A 3
H24A H 0.5290 0.4291 0.0440 0.103 Uiso 0.470(7) 1 calc PR A 3
C25 C 0.4646(6) 0.4872(8) 0.0859(5) 0.094(5) Uani 0.470(7) 1 d PG A 3
H25A H 0.4364 0.4863 0.0548 0.113 Uiso 0.470(7) 1 calc PR A 3
C26 C 0.4508(4) 0.5224(7) 0.1377(6) 0.072(6) Uani 0.470(7) 1 d PG A 3
H26A H 0.4132 0.5456 0.1421 0.086 Uiso 0.470(7) 1 calc PR A 3
C27 C 0.4920(4) 0.5236(8) 0.1832(5) 0.092(6) Uani 0.470(7) 1 d PG A 3
H27A H 0.4826 0.5477 0.2186 0.110 Uiso 0.470(7) 1 calc PR A 3
C28 C 0.5470(4) 0.4896(7) 0.1768(5) 0.076(5) Uani 0.470(7) 1 d PG A 3
H28A H 0.5752 0.4905 0.2078 0.091 Uiso 0.470(7) 1 calc PR A 3
C23A C 0.5565(3) 0.4462(6) 0.1120(4) 0.046(5) Uani 0.530(7) 1 d PGD A 4
C24A C 0.5330(5) 0.4994(8) 0.0714(4) 0.086(5) Uani 0.530(7) 1 d PG A 4
H24B H 0.5562 0.5172 0.0408 0.103 Uiso 0.530(7) 1 calc PR A 4
C25A C 0.4758(5) 0.5266(7) 0.0755(5) 0.094(5) Uani 0.530(7) 1 d PG A 4
H25B H 0.4597 0.5630 0.0477 0.113 Uiso 0.530(7) 1 calc PR A 4
C26A C 0.4419(3) 0.5006(7) 0.1203(5) 0.070(6) Uani 0.530(7) 1 d PG A 4
H26B H 0.4028 0.5192 0.1231 0.084 Uiso 0.530(7) 1 calc PR A 4
C27A C 0.4653(3) 0.4474(6) 0.1609(4) 0.080(5) Uani 0.530(7) 1 d PG A 4
H27B H 0.4422 0.4296 0.1915 0.096 Uiso 0.530(7) 1 calc PR A 4
C28A C 0.5226(3) 0.4202(5) 0.1568(4) 0.057(3) Uani 0.530(7) 1 d PG A 4
H28B H 0.5386 0.3838 0.1846 0.069 Uiso 0.530(7) 1 calc PR A 4
O1 O 0.7084(4) 0.2294(6) 0.1657(4) 0.037(3) Uani 0.496(6) 1 d PD A 1
O2 O 0.8129(4) 0.3286(5) 0.1848(4) 0.033(2) Uani 0.496(6) 1 d PD A 1
O3 O 0.7751(4) 0.4565(5) 0.1820(3) 0.043(2) Uani 0.496(6) 1 d PD A 1
O4 O 0.6507(4) 0.4172(6) 0.1614(4) 0.048(2) Uani 0.496(6) 1 d PD A 1
O1A O 0.6830(4) 0.2461(7) 0.1642(5) 0.049(3) Uani 0.504(6) 1 d PD A 2
O2A O 0.8052(4) 0.2902(6) 0.1840(4) 0.037(2) Uani 0.504(6) 1 d PD A 2
O3A O 0.7423(4) 0.4712(4) 0.1744(3) 0.0371(19) Uani 0.504(6) 1 d PD A 2
O4A O 0.6374(4) 0.3731(5) 0.1551(4) 0.044(2) Uani 0.504(6) 1 d PD A 2
O5 O 0.71317(19) 0.3507(2) 0.26066(16) 0.0470(9) Uani 1 1 d D A .
Co1 Co 0.72593(3) 0.35244(5) 0.17486(3) 0.03307(18) Uani 1 1 d D . .
Pt1 Pt 0.740472(8) 0.355662(13) 0.064765(8) 0.03491(9) Uani 1 1 d . . .
S1A S 0.7222(2) 0.21960(18) 0.06234(11) 0.0410(10) Uani 0.496(6) 1 d P A 1
S2A S 0.84115(13) 0.3300(3) 0.08219(11) 0.0370(9) Uani 0.496(6) 1 d P A 1
S3A S 0.7617(2) 0.4935(2) 0.07179(12) 0.0430(9) Uani 0.496(6) 1 d P A 1
S4A S 0.65352(15) 0.4302(3) 0.05003(12) 0.0396(9) Uani 0.496(6) 1 d P A 1
S1B S 0.68429(19) 0.23795(18) 0.05389(10) 0.0396(9) Uani 0.504(6) 1 d P A 2
S2B S 0.82445(14) 0.2809(3) 0.07793(10) 0.0394(10) Uani 0.504(6) 1 d P A 2
S3B S 0.7930(2) 0.4723(2) 0.07491(11) 0.0386(9) Uani 0.504(6) 1 d P A 2
S4B S 0.64261(15) 0.3847(4) 0.05176(13) 0.0473(10) Uani 0.504(6) 1 d P A 2
H5B H 0.6799(15) 0.353(6) 0.251(4) 0.16(5) Uiso 1 1 d D . .
H5A H 0.716(4) 0.370(5) 0.291(2) 0.14(4) Uiso 1 1 d 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
C1 0.032(3) 0.051(3) 0.036(3) 0.011(2) 0.001(2) 0.004(2)
C2 0.048(3) 0.047(3) 0.052(3) 0.002(3) 0.002(2) -0.001(3)
C3 0.105(6) 0.059(4) 0.065(4) -0.003(3) -0.007(4) -0.024(4)
C4 0.143(8) 0.070(5) 0.078(5) -0.013(4) -0.015(5) -0.031(5)
C5 0.110(7) 0.063(5) 0.103(6) 0.006(4) 0.011(5) -0.033(5)
C6 0.072(5) 0.058(4) 0.087(5) 0.022(4) 0.020(4) -0.010(4)
C7 0.039(3) 0.050(3) 0.056(3) 0.009(3) 0.005(2) 0.001(3)
C8 0.032(3) 0.044(3) 0.035(2) 0.001(2) 0.006(2) -0.003(2)
C9 0.040(3) 0.067(4) 0.039(3) 0.003(3) 0.007(2) 0.014(3)
C10 0.043(4) 0.125(7) 0.055(4) 0.006(4) 0.008(3) 0.032(4)
C11 0.057(5) 0.174(9) 0.081(5) 0.003(6) 0.012(4) 0.045(5)
C12 0.057(5) 0.222(12) 0.077(5) -0.020(6) -0.014(4) 0.064(6)
C13 0.082(6) 0.311(16) 0.043(4) 0.005(6) -0.005(4) 0.107(8)
C14 0.042(3) 0.131(6) 0.035(3) 0.000(3) -0.001(2) 0.032(4)
C15 0.033(3) 0.050(3) 0.042(3) 0.003(2) 0.004(2) 0.008(2)
C16 0.039(3) 0.043(3) 0.059(3) 0.001(3) -0.001(2) -0.003(2)
C17 0.076(5) 0.065(4) 0.069(4) -0.012(3) -0.010(3) 0.003(4)
C18 0.115(7) 0.068(5) 0.091(6) -0.029(5) -0.015(5) -0.001(5)
C19 0.129(8) 0.063(6) 0.144(9) -0.022(6) -0.039(7) -0.008(5)
C20 0.135(8) 0.059(5) 0.152(9) 0.012(6) 0.003(7) -0.037(5)
C21 0.119(7) 0.061(5) 0.085(5) -0.001(4) 0.008(5) -0.031(5)
C22 0.031(3) 0.055(3) 0.051(3) 0.016(3) 0.009(2) 0.011(2)
C23 0.028(10) 0.054(11) 0.059(9) 0.021(7) 0.003(6) 0.004(8)
C24 0.038(7) 0.155(16) 0.066(6) 0.034(8) 0.007(4) 0.021(8)
C25 0.062(7) 0.123(16) 0.096(8) 0.036(9) -0.017(6) 0.039(9)
C26 0.035(9) 0.066(11) 0.114(16) 0.006(12) -0.007(9) 0.008(8)
C27 0.060(10) 0.107(15) 0.109(13) 0.010(11) 0.017(9) 0.043(10)
C28 0.039(8) 0.097(13) 0.092(11) -0.004(9) 0.020(7) 0.040(8)
C23A 0.036(9) 0.067(11) 0.036(6) 0.011(6) 0.001(5) 0.021(8)
C24A 0.038(7) 0.155(16) 0.066(6) 0.034(8) 0.007(4) 0.021(8)
C25A 0.062(7) 0.123(16) 0.096(8) 0.036(9) -0.017(6) 0.039(9)
C26A 0.037(8) 0.101(14) 0.071(10) -0.010(9) 0.002(7) 0.019(8)
C27A 0.028(6) 0.116(13) 0.098(10) 0.033(9) 0.020(6) 0.014(7)
C28A 0.042(6) 0.072(9) 0.059(7) 0.022(6) 0.007(5) 0.028(6)
O1 0.041(6) 0.052(6) 0.017(4) 0.003(4) -0.006(4) -0.016(5)
O2 0.024(4) 0.046(6) 0.030(4) -0.002(4) 0.004(3) -0.008(4)
O3 0.056(6) 0.040(5) 0.034(4) 0.011(3) 0.002(4) 0.010(4)
O4 0.036(5) 0.065(7) 0.043(5) 0.022(5) 0.010(4) 0.028(5)
O1A 0.047(7) 0.067(7) 0.032(4) 0.011(4) -0.003(5) -0.009(5)
O2A 0.022(4) 0.061(7) 0.027(4) 0.000(5) 0.004(3) -0.001(5)
O3A 0.062(6) 0.023(4) 0.026(4) 0.003(3) 0.009(4) 0.010(4)
O4A 0.037(5) 0.046(5) 0.051(5) 0.007(5) 0.005(3) 0.009(4)
O5 0.054(3) 0.057(2) 0.031(2) 0.0019(17) 0.0110(16) 0.0099(19)
Co1 0.0305(4) 0.0409(5) 0.0282(4) 0.0038(3) 0.0055(3) 0.0062(3)
Pt1 0.03171(14) 0.04686(14) 0.02630(12) 0.00321(8) 0.00307(8) 0.00212(10)
S1A 0.047(3) 0.0485(16) 0.0279(13) 0.0003(10) 0.0063(12) -0.0023(15)
S2A 0.0316(15) 0.051(2) 0.0289(13) 0.0024(12) 0.0062(10) 0.0013(14)
S3A 0.042(2) 0.0506(18) 0.0369(14) 0.0085(12) 0.0065(14) 0.0033(16)
S4A 0.0347(16) 0.051(2) 0.0331(13) 0.0058(14) 0.0004(10) 0.0075(16)
S1B 0.036(2) 0.0509(16) 0.0316(13) -0.0018(11) -0.0018(11) -0.0049(15)
S2B 0.0330(16) 0.056(3) 0.0291(12) -0.0048(12) 0.0016(9) 0.0129(16)
S3B 0.035(2) 0.0469(17) 0.0338(13) 0.0016(11) 0.0063(13) -0.0044(15)
S4B 0.0364(17) 0.065(3) 0.0404(15) 0.0144(16) -0.0005(11) 0.0056(17)
_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
C1 O1 1.222(10) . ?
C1 O1A 1.281(11) . ?
C1 C2 1.483(7) . ?
C1 S1A 1.678(5) . ?
C1 S1B 1.743(5) . ?
C2 C3 1.373(8) . ?
C2 C7 1.396(7) . ?
C3 C4 1.398(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.365(10) . ?
C4 H4 0.9500 . ?
C5 C6 1.362(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.403(8) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 O2A 1.249(9) . ?
C8 O2 1.276(10) . ?
C8 C9 1.490(7) . ?
C8 S2A 1.673(5) . ?
C8 S2B 1.723(5) . ?
C9 C14 1.383(7) . ?
C9 C10 1.385(7) . ?
C10 C11 1.415(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.342(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.383(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.360(9) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 O3A 1.260(8) . ?
C15 O3 1.269(8) . ?
C15 C16 1.489(7) . ?
C15 S3A 1.678(6) . ?
C15 S3B 1.733(6) . ?
C16 C17 1.353(8) . ?
C16 C21 1.394(9) . ?
C17 C18 1.381(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.372(12) . ?
C18 H18 0.9500 . ?
C19 C20 1.401(12) . ?
C19 H19 0.9500 . ?
C20 C21 1.365(10) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 O4A 1.234(9) . ?
C22 O4 1.281(10) . ?
C22 C23 1.509(9) . ?
C22 C23A 1.519(8) . ?
C22 S4B 1.662(6) . ?
C22 S4A 1.743(6) . ?
C23 C24 1.3900 . ?
C23 C28 1.3900 . ?
C24 C25 1.3900 . ?
C24 H24A 0.9500 . ?
C25 C26 1.3900 . ?
C25 H25A 0.9500 . ?
C26 C27 1.3900 . ?
C26 H26A 0.9500 . ?
C27 C28 1.3900 . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C23A C24A 1.3900 . ?
C23A C28A 1.3900 . ?
C24A C25A 1.3900 . ?
C24A H24B 0.9500 . ?
C25A C26A 1.3900 . ?
C25A H25B 0.9500 . ?
C26A C27A 1.3900 . ?
C26A H26B 0.9500 . ?
C27A C28A 1.3900 . ?
C27A H27B 0.9500 . ?
C28A H28B 0.9500 . ?
O1 Co1 2.099(10) . ?
O2 Co1 2.029(9) . ?
O3 Co1 2.069(8) . ?
O4 Co1 2.041(8) . ?
O1A Co1 2.036(11) . ?
O2A Co1 2.090(9) . ?
O3A Co1 2.015(7) . ?
O4A Co1 2.083(8) . ?
O5 Co1 2.031(4) . ?
O5 H5B 0.79(2) . ?
O5 H5A 0.77(2) . ?
Co1 Pt1 2.5993(8) . ?
Pt1 S3B 2.292(3) . ?
Pt1 S4B 2.293(3) . ?
Pt1 S2B 2.297(2) . ?
Pt1 S1A 2.307(3) . ?
Pt1 S3A 2.352(3) . ?
Pt1 S1B 2.352(3) . ?
Pt1 S4A 2.355(3) . ?
Pt1 S2A 2.357(3) . ?
Pt1 Pt1 3.0651(4) 2_655 ?
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
O1 C1 O1A 29.6(5) . . ?
O1 C1 C2 118.9(7) . . ?
O1A C1 C2 118.4(7) . . ?
O1 C1 S1A 114.1(6) . . ?
O1A C1 S1A 122.8(7) . . ?
C2 C1 S1A 118.9(4) . . ?
O1 C1 S1B 125.5(6) . . ?
O1A C1 S1B 115.9(7) . . ?
C2 C1 S1B 115.5(4) . . ?
S1A C1 S1B 31.54(14) . . ?
C3 C2 C7 119.2(6) . . ?
C3 C2 C1 122.4(5) . . ?
C7 C2 C1 118.4(5) . . ?
C2 C3 C4 119.5(7) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 121.8(7) . . ?
C5 C4 H4 119.1 . . ?
C3 C4 H4 119.1 . . ?
C6 C5 C4 118.9(7) . . ?
C6 C5 H5 120.6 . . ?
C4 C5 H5 120.6 . . ?
C5 C6 C7 121.0(6) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C2 C7 C6 119.6(6) . . ?
C2 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
O2A C8 O2 30.5(4) . . ?
O2A C8 C9 117.7(6) . . ?
O2 C8 C9 119.1(6) . . ?
O2A C8 S2A 127.1(6) . . ?
O2 C8 S2A 115.2(6) . . ?
C9 C8 S2A 115.1(3) . . ?
O2A C8 S2B 115.8(6) . . ?
O2 C8 S2B 122.4(6) . . ?
C9 C8 S2B 118.5(3) . . ?
S2A C8 S2B 30.94(14) . . ?
C14 C9 C10 118.2(5) . . ?
C14 C9 C8 120.3(4) . . ?
C10 C9 C8 121.5(5) . . ?
C9 C10 C11 120.4(6) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C12 C11 C10 119.5(7) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 120.2(7) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 120.8(7) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C9 120.9(6) . . ?
C13 C14 H14 119.6 . . ?
C9 C14 H14 119.6 . . ?
O3A C15 O3 36.9(4) . . ?
O3A C15 C16 119.1(5) . . ?
O3 C15 C16 115.3(6) . . ?
O3A C15 S3A 114.1(5) . . ?
O3 C15 S3A 127.4(5) . . ?
C16 C15 S3A 117.0(4) . . ?
O3A C15 S3B 122.1(5) . . ?
O3 C15 S3B 116.0(5) . . ?
C16 C15 S3B 118.5(4) . . ?
S3A C15 S3B 26.98(13) . . ?
C17 C16 C21 118.1(6) . . ?
C17 C16 C15 119.0(5) . . ?
C21 C16 C15 122.9(6) . . ?
C16 C17 C18 122.5(7) . . ?
C16 C17 H17 118.7 . . ?
C18 C17 H17 118.7 . . ?
C19 C18 C17 119.6(8) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C18 C19 C20 118.5(8) . . ?
C18 C19 H19 120.7 . . ?
C20 C19 H19 120.7 . . ?
C21 C20 C19 120.6(9) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
C20 C21 C16 120.5(8) . . ?
C20 C21 H21 119.8 . . ?
C16 C21 H21 119.8 . . ?
O4A C22 O4 37.4(5) . . ?
O4A C22 C23 113.7(7) . . ?
O4 C22 C23 109.2(7) . . ?
O4A C22 C23A 121.0(6) . . ?
O4 C22 C23A 121.8(6) . . ?
C23 C22 C23A 12.9(7) . . ?
O4A C22 S4B 112.7(6) . . ?
O4 C22 S4B 124.6(5) . . ?
C23 C22 S4B 125.8(6) . . ?
C23A C22 S4B 113.6(5) . . ?
O4A C22 S4A 126.2(5) . . ?
O4 C22 S4A 118.3(5) . . ?
C23 C22 S4A 120.1(6) . . ?
C23A C22 S4A 111.6(4) . . ?
S4B C22 S4A 27.07(15) . . ?
C24 C23 C28 120.0 . . ?
C24 C23 C22 116.8(8) . . ?
C28 C23 C22 123.2(8) . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24A 120.0 . . ?
C23 C24 H24A 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25A 120.0 . . ?
C26 C25 H25A 120.0 . . ?
C27 C26 C25 120.0 . . ?
C27 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C28 C27 C26 120.0 . . ?
C28 C27 H27A 120.0 . . ?
C26 C27 H27A 120.0 . . ?
C27 C28 C23 120.0 . . ?
C27 C28 H28A 120.0 . . ?
C23 C28 H28A 120.0 . . ?
C24A C23A C28A 120.0 . . ?
C24A C23A C22 125.6(6) . . ?
C28A C23A C22 114.3(6) . . ?
C23A C24A C25A 120.0 . . ?
C23A C24A H24B 120.0 . . ?
C25A C24A H24B 120.0 . . ?
C26A C25A C24A 120.0 . . ?
C26A C25A H25B 120.0 . . ?
C24A C25A H25B 120.0 . . ?
C27A C26A C25A 120.0 . . ?
C27A C26A H26B 120.0 . . ?
C25A C26A H26B 120.0 . . ?
C26A C27A C28A 120.0 . . ?
C26A C27A H27B 120.0 . . ?
C28A C27A H27B 120.0 . . ?
C27A C28A C23A 120.0 . . ?
C27A C28A H28B 120.0 . . ?
C23A C28A H28B 120.0 . . ?
C1 O1 Co1 126.0(8) . . ?
C8 O2 Co1 127.2(7) . . ?
C15 O3 Co1 122.4(6) . . ?
C22 O4 Co1 124.1(6) . . ?
C1 O1A Co1 126.8(8) . . ?
C8 O2A Co1 124.4(7) . . ?
C15 O3A Co1 127.0(5) . . ?
C22 O4A Co1 124.0(6) . . ?
Co1 O5 H5B 84(7) . . ?
Co1 O5 H5A 151(7) . . ?
H5B O5 H5A 107(3) . . ?
O3A Co1 O2 90.7(4) . . ?
O3A Co1 O5 93.0(2) . . ?
O2 Co1 O5 93.5(3) . . ?
O3A Co1 O1A 160.6(4) . . ?
O2 Co1 O1A 107.9(4) . . ?
O5 Co1 O1A 91.2(4) . . ?
O3A Co1 O4 68.6(4) . . ?
O2 Co1 O4 159.1(4) . . ?
O5 Co1 O4 90.5(3) . . ?
O1A Co1 O4 92.5(5) . . ?
O3A Co1 O3 22.6(2) . . ?
O2 Co1 O3 68.3(4) . . ?
O5 Co1 O3 91.7(3) . . ?
O1A Co1 O3 175.3(4) . . ?
O4 Co1 O3 91.1(4) . . ?
O3A Co1 O4A 90.8(3) . . ?
O2 Co1 O4A 173.6(4) . . ?
O5 Co1 O4A 92.7(3) . . ?
O1A Co1 O4A 70.1(4) . . ?
O4 Co1 O4A 22.5(3) . . ?
O3 Co1 O4A 113.4(3) . . ?
O3A Co1 O2A 109.2(4) . . ?
O2 Co1 O2A 18.5(3) . . ?
O5 Co1 O2A 92.8(3) . . ?
O1A Co1 O2A 89.4(4) . . ?
O4 Co1 O2A 176.2(4) . . ?
O3 Co1 O2A 86.8(4) . . ?
O4A Co1 O2A 158.9(4) . . ?
O3A Co1 O1 173.9(4) . . ?
O2 Co1 O1 90.2(4) . . ?
O5 Co1 O1 93.0(3) . . ?
O1A Co1 O1 17.8(3) . . ?
O4 Co1 O1 110.2(4) . . ?
O3 Co1 O1 158.2(4) . . ?
O4A Co1 O1 87.7(4) . . ?
O2A Co1 O1 71.7(4) . . ?
O3A Co1 Pt1 86.8(2) . . ?
O2 Co1 Pt1 87.5(3) . . ?
O5 Co1 Pt1 179.02(13) . . ?
O1A Co1 Pt1 88.6(3) . . ?
O4 Co1 Pt1 88.6(2) . . ?
O3 Co1 Pt1 88.5(2) . . ?
O4A Co1 Pt1 86.4(3) . . ?
O2A Co1 Pt1 88.2(3) . . ?
O1 Co1 Pt1 87.2(3) . . ?
S3B Pt1 S4B 109.7(2) . . ?
S3B Pt1 S2B 90.94(12) . . ?
S4B Pt1 S2B 159.3(2) . . ?
S3B Pt1 S1A 158.47(12) . . ?
S4B Pt1 S1A 91.7(2) . . ?
S2B Pt1 S1A 67.57(13) . . ?
S3B Pt1 S3A 19.72(8) . . ?
S4B Pt1 S3A 90.0(2) . . ?
S2B Pt1 S3A 110.63(13) . . ?
S1A Pt1 S3A 177.06(10) . . ?
S3B Pt1 S1B 178.49(12) . . ?
S4B Pt1 S1B 68.8(2) . . ?
S2B Pt1 S1B 90.57(12) . . ?
S1A Pt1 S1B 23.04(8) . . ?
S3A Pt1 S1B 158.78(12) . . ?
S3B Pt1 S4A 90.1(2) . . ?
S4B Pt1 S4A 19.79(9) . . ?
S2B Pt1 S4A 178.81(18) . . ?
S1A Pt1 S4A 111.4(2) . . ?
S3A Pt1 S4A 70.4(2) . . ?
S1B Pt1 S4A 88.4(2) . . ?
S3B Pt1 S2A 68.52(12) . . ?
S4B Pt1 S2A 177.16(17) . . ?
S2B Pt1 S2A 22.43(8) . . ?
S1A Pt1 S2A 89.98(12) . . ?
S3A Pt1 S2A 88.20(13) . . ?
S1B Pt1 S2A 112.99(12) . . ?
S4A Pt1 S2A 158.6(2) . . ?
S3B Pt1 Co1 90.07(7) . . ?
S4B Pt1 Co1 88.59(8) . . ?
S2B Pt1 Co1 89.63(6) . . ?
S1A Pt1 Co1 88.52(6) . . ?
S3A Pt1 Co1 89.14(7) . . ?
S1B Pt1 Co1 90.00(6) . . ?
S4A Pt1 Co1 90.98(7) . . ?
S2A Pt1 Co1 89.18(6) . . ?
S3B Pt1 Pt1 90.50(6) . 2_655 ?
S4B Pt1 Pt1 92.46(8) . 2_655 ?
S2B Pt1 Pt1 89.04(6) . 2_655 ?
S1A Pt1 Pt1 90.46(6) . 2_655 ?
S3A Pt1 Pt1 91.84(7) . 2_655 ?
S1B Pt1 Pt1 89.46(6) . 2_655 ?
S4A Pt1 Pt1 90.35(7) . 2_655 ?
S2A Pt1 Pt1 89.80(6) . 2_655 ?
Co1 Pt1 Pt1 178.560(18) . 2_655 ?
C1 S1A Pt1 107.1(2) . . ?
C8 S2A Pt1 104.4(2) . . ?
C15 S3A Pt1 104.1(2) . . ?
C22 S4A Pt1 101.6(2) . . ?
C1 S1B Pt1 103.0(2) . . ?
C8 S2B Pt1 105.2(2) . . ?
C15 S3B Pt1 104.7(2) . . ?
C22 S4B Pt1 107.0(2) . . ?
_diffrn_measured_fraction_theta_max 0.959
_diffrn_reflns_theta_full 66.02
_diffrn_measured_fraction_theta_full 0.959
_refine_diff_density_max 0.660
_refine_diff_density_min -0.666
_refine_diff_density_rms 0.091
###END
data_lhd236_compound_2b
_database_code_depnum_ccdc_archive 'CCDC 842002'
#TrackingRef '- Dahl-Doerrer-PtMtba-all_compounds-v4.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C28 H22 Co O5 Pt S4'
_chemical_formula_weight 820.72
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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 Pc
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
_cell_length_a 11.3784(7)
_cell_length_b 11.8220(8)
_cell_length_c 22.0722(14)
_cell_angle_alpha 90.00
_cell_angle_beta 90.4290(10)
_cell_angle_gamma 90.00
_cell_volume 2969.0(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 100(2)
_cell_measurement_reflns_used 9936
_cell_measurement_theta_min 2.52
_cell_measurement_theta_max 27.86
_exptl_crystal_description block
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.40
_exptl_crystal_size_mid 0.33
_exptl_crystal_size_min 0.26
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.836
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1596
_exptl_absorpt_coefficient_mu 5.583
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.2136
_exptl_absorpt_correction_T_max 0.3247
_exptl_absorpt_process_details sadabs
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 100(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 'CCD area detector'
_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 25090
_diffrn_reflns_av_R_equivalents 0.0256
_diffrn_reflns_av_sigmaI/netI 0.0449
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 1.95
_diffrn_reflns_theta_max 27.93
_reflns_number_total 12405
_reflns_number_gt 11912
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SMART'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0257P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack 0.721(3)
_refine_ls_number_reflns 12405
_refine_ls_number_parameters 720
_refine_ls_number_restraints 8
_refine_ls_R_factor_all 0.0279
_refine_ls_R_factor_gt 0.0262
_refine_ls_wR_factor_ref 0.0567
_refine_ls_wR_factor_gt 0.0561
_refine_ls_goodness_of_fit_ref 1.015
_refine_ls_restrained_S_all 1.015
_refine_ls_shift/su_max 0.006
_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
C1 C 0.2367(5) -0.0140(4) 0.6808(2) 0.0187(10) Uani 1 1 d . . .
C2 C 0.2810(4) -0.0541(4) 0.6217(2) 0.0192(10) Uani 1 1 d . . .
C3 C 0.2756(5) -0.1695(4) 0.6076(2) 0.0250(11) Uani 1 1 d . . .
H3 H 0.2416 -0.2212 0.6354 0.030 Uiso 1 1 calc R . .
C4 C 0.3196(5) -0.2081(5) 0.5532(2) 0.0333(13) Uani 1 1 d . . .
H4 H 0.3147 -0.2863 0.5436 0.040 Uiso 1 1 calc R . .
C5 C 0.3709(6) -0.1344(5) 0.5125(2) 0.0339(14) Uani 1 1 d . . .
H5 H 0.4009 -0.1615 0.4752 0.041 Uiso 1 1 calc R . .
C6 C 0.3779(6) -0.0209(5) 0.5269(2) 0.0355(14) Uani 1 1 d . . .
H6 H 0.4132 0.0303 0.4993 0.043 Uiso 1 1 calc R . .
C7 C 0.3340(5) 0.0186(4) 0.5811(2) 0.0281(12) Uani 1 1 d . . .
H7 H 0.3404 0.0967 0.5907 0.034 Uiso 1 1 calc R . .
C8 C 0.4015(5) 0.0186(4) 0.8410(2) 0.0187(10) Uani 1 1 d . . .
C9 C 0.5202(5) 0.0042(4) 0.8684(2) 0.0191(10) Uani 1 1 d . . .
C10 C 0.5465(5) -0.0959(4) 0.8991(2) 0.0235(11) Uani 1 1 d . . .
H10 H 0.4903 -0.1553 0.9000 0.028 Uiso 1 1 calc R . .
C11 C 0.6535(5) -0.1095(4) 0.9282(2) 0.0295(12) Uani 1 1 d . . .
H11 H 0.6699 -0.1775 0.9497 0.035 Uiso 1 1 calc R . .
C12 C 0.7374(5) -0.0240(5) 0.9261(2) 0.0334(12) Uani 1 1 d . . .
H12 H 0.8110 -0.0332 0.9461 0.040 Uiso 1 1 calc R . .
C13 C 0.7125(5) 0.0745(5) 0.8947(3) 0.0341(13) Uani 1 1 d . . .
H13 H 0.7703 0.1322 0.8923 0.041 Uiso 1 1 calc R . .
C14 C 0.6055(5) 0.0899(5) 0.8672(2) 0.0283(13) Uani 1 1 d . . .
H14 H 0.5888 0.1591 0.8471 0.034 Uiso 1 1 calc R . .
C15 C 0.0854(5) 0.0684(4) 0.9189(2) 0.0213(10) Uani 1 1 d . . .
C16 C 0.0286(5) 0.0742(4) 0.9798(2) 0.0243(11) Uani 1 1 d . . .
C17 C 0.0219(5) -0.0239(5) 1.0150(2) 0.0287(12) Uani 1 1 d . . .
H17 H 0.0571 -0.0919 1.0012 0.034 Uiso 1 1 calc R . .
C18 C -0.0354(6) -0.0218(6) 1.0693(3) 0.0430(16) Uani 1 1 d . . .
H18 H -0.0382 -0.0881 1.0936 0.052 Uiso 1 1 calc R . .
C19 C -0.0891(7) 0.0757(6) 1.0891(3) 0.058(2) Uani 1 1 d . . .
H19 H -0.1299 0.0763 1.1265 0.069 Uiso 1 1 calc R . .
C20 C -0.0833(7) 0.1729(5) 1.0543(3) 0.060(2) Uani 1 1 d . . .
H20 H -0.1199 0.2403 1.0680 0.072 Uiso 1 1 calc R . .
C21 C -0.0249(6) 0.1723(5) 1.0000(2) 0.0386(14) Uani 1 1 d . . .
H21 H -0.0212 0.2393 0.9763 0.046 Uiso 1 1 calc R . .
C22 C -0.0725(5) 0.0321(4) 0.7632(2) 0.0211(10) Uani 1 1 d . . .
C23 C -0.1946(5) 0.0142(4) 0.7409(2) 0.0204(10) Uani 1 1 d . . .
C24 C -0.2408(5) -0.0946(4) 0.7448(2) 0.0273(12) Uani 1 1 d . . .
H24 H -0.1963 -0.1527 0.7639 0.033 Uiso 1 1 calc R . .
C25 C -0.3507(5) -0.1192(5) 0.7211(3) 0.0352(14) Uani 1 1 d . . .
H25 H -0.3820 -0.1935 0.7242 0.042 Uiso 1 1 calc R . .
C26 C -0.4152(5) -0.0338(5) 0.6927(3) 0.0394(15) Uani 1 1 d . . .
H26 H -0.4899 -0.0503 0.6754 0.047 Uiso 1 1 calc R . .
C27 C -0.3707(5) 0.0748(5) 0.6897(3) 0.0363(14) Uani 1 1 d . . .
H27 H -0.4155 0.1331 0.6710 0.044 Uiso 1 1 calc R . .
C28 C -0.2615(5) 0.0986(4) 0.7138(2) 0.0264(12) Uani 1 1 d . . .
H28 H -0.2316 0.1736 0.7118 0.032 Uiso 1 1 calc R . .
C29 C 0.3267(5) 0.5364(4) 0.8794(2) 0.0176(10) Uani 1 1 d . . .
C30 C 0.2796(4) 0.5630(4) 0.9402(2) 0.0166(10) Uani 1 1 d . . .
C31 C 0.2344(5) 0.4795(4) 0.9778(2) 0.0258(11) Uani 1 1 d . . .
H31 H 0.2357 0.4027 0.9652 0.031 Uiso 1 1 calc R . .
C32 C 0.1870(6) 0.5077(5) 1.0340(2) 0.0352(14) Uani 1 1 d . . .
H32 H 0.1548 0.4504 1.0590 0.042 Uiso 1 1 calc R . .
C33 C 0.1868(6) 0.6196(5) 1.0532(3) 0.0333(15) Uani 1 1 d . . .
H33 H 0.1567 0.6390 1.0919 0.040 Uiso 1 1 calc R . .
C34 C 0.2310(5) 0.7026(4) 1.0155(2) 0.0287(12) Uani 1 1 d . . .
H34 H 0.2300 0.7793 1.0284 0.034 Uiso 1 1 calc R . .
C35 C 0.2767(5) 0.6758(4) 0.9593(2) 0.0231(11) Uani 1 1 d . . .
H35 H 0.3060 0.7339 0.9338 0.028 Uiso 1 1 calc R . .
C36 C 0.6465(5) 0.5276(4) 0.8059(2) 0.0181(10) Uani 1 1 d . . .
C37 C 0.7654(5) 0.5505(4) 0.8324(2) 0.0186(10) Uani 1 1 d . . .
C38 C 0.8519(5) 0.4675(4) 0.8387(2) 0.0242(11) Uani 1 1 d . . .
H38 H 0.8393 0.3944 0.8221 0.029 Uiso 1 1 calc R . .
C39 C 0.9558(5) 0.4912(5) 0.8690(2) 0.0297(13) Uani 1 1 d . . .
H39 H 1.0145 0.4344 0.8728 0.036 Uiso 1 1 calc R . .
C40 C 0.9748(5) 0.5977(4) 0.8937(2) 0.0285(12) Uani 1 1 d . . .
H40 H 1.0450 0.6129 0.9158 0.034 Uiso 1 1 calc R . .
C41 C 0.8914(5) 0.6815(4) 0.8860(2) 0.0279(11) Uani 1 1 d . . .
H41 H 0.9054 0.7551 0.9017 0.034 Uiso 1 1 calc R . .
C42 C 0.7877(5) 0.6585(4) 0.8556(2) 0.0225(10) Uani 1 1 d . . .
H42 H 0.7309 0.7166 0.8504 0.027 Uiso 1 1 calc R . .
C43 C 0.4968(5) 0.5109(4) 0.6417(2) 0.0181(10) Uani 1 1 d . . .
C44 C 0.5434(5) 0.5290(4) 0.5794(2) 0.0239(11) Uani 1 1 d . . .
C45 C 0.5775(5) 0.6390(4) 0.5636(2) 0.0295(12) Uani 1 1 d . . .
H45 H 0.5683 0.6992 0.5917 0.035 Uiso 1 1 calc R . .
C46 C 0.6244(6) 0.6599(5) 0.5072(2) 0.0375(14) Uani 1 1 d . . .
H46 H 0.6479 0.7345 0.4967 0.045 Uiso 1 1 calc R . .
C47 C 0.6374(6) 0.5737(6) 0.4663(2) 0.0396(15) Uani 1 1 d . . .
H47 H 0.6701 0.5886 0.4276 0.047 Uiso 1 1 calc R . .
C48 C 0.6032(6) 0.4659(6) 0.4811(3) 0.0455(16) Uani 1 1 d . . .
H48 H 0.6115 0.4067 0.4523 0.055 Uiso 1 1 calc R . .
C49 C 0.5567(6) 0.4425(5) 0.5373(2) 0.0351(14) Uani 1 1 d . . .
H49 H 0.5339 0.3675 0.5471 0.042 Uiso 1 1 calc R . .
C50 C 0.1798(5) 0.5219(4) 0.7180(2) 0.0185(10) Uani 1 1 d . . .
C51 C 0.0552(5) 0.5360(4) 0.6991(2) 0.0198(11) Uani 1 1 d . . .
C52 C -0.0177(5) 0.4432(5) 0.6862(2) 0.0268(12) Uani 1 1 d . . .
H52 H 0.0135 0.3687 0.6877 0.032 Uiso 1 1 calc R . .
C53 C -0.1346(6) 0.4598(5) 0.6714(2) 0.0354(14) Uani 1 1 d . . .
H53 H -0.1836 0.3970 0.6623 0.042 Uiso 1 1 calc R . .
C54 C -0.1800(5) 0.5690(5) 0.6700(2) 0.0401(14) Uani 1 1 d . . .
H54 H -0.2607 0.5806 0.6605 0.048 Uiso 1 1 calc R . .
C55 C -0.1080(5) 0.6609(5) 0.6824(2) 0.0372(14) Uani 1 1 d . . .
H55 H -0.1396 0.7353 0.6813 0.045 Uiso 1 1 calc R . .
C56 C 0.0093(5) 0.6451(4) 0.6965(2) 0.0262(12) Uani 1 1 d . . .
H56 H 0.0585 0.7084 0.7043 0.031 Uiso 1 1 calc R . .
O1 O 0.2311(3) -0.0844(2) 0.72415(14) 0.0193(7) Uani 1 1 d . . .
O2 O 0.3273(3) -0.0591(3) 0.84765(15) 0.0206(7) Uani 1 1 d . . .
O3 O 0.0838(3) -0.0245(3) 0.89199(14) 0.0221(8) Uani 1 1 d . . .
O4 O -0.0081(3) -0.0534(2) 0.77064(15) 0.0222(8) Uani 1 1 d . . .
O5 O 0.1460(3) -0.2301(3) 0.82139(15) 0.0196(7) Uani 1 1 d D . .
O6 O 0.3244(3) 0.6123(2) 0.83915(15) 0.0188(7) Uani 1 1 d . . .
O7 O 0.5747(3) 0.6069(2) 0.80339(15) 0.0204(8) Uani 1 1 d . . .
O8 O 0.4965(3) 0.5940(2) 0.67694(14) 0.0199(7) Uani 1 1 d . . .
O9 O 0.2513(3) 0.6014(2) 0.71269(15) 0.0194(8) Uani 1 1 d . . .
O10 O 0.4068(3) 0.7784(2) 0.75615(15) 0.0197(7) Uani 1 1 d D . .
S1 S 0.19362(13) 0.12391(11) 0.68596(6) 0.0235(3) Uani 1 1 d . . .
S2 S 0.37533(17) 0.14029(12) 0.80110(8) 0.0247(4) Uani 1 1 d . . .
S3 S 0.14964(13) 0.18955(11) 0.89218(6) 0.0236(3) Uani 1 1 d . . .
S4 S -0.02919(16) 0.16887(10) 0.77707(8) 0.0228(3) Uani 1 1 d . . .
S5 S 0.38464(14) 0.40447(10) 0.86890(6) 0.0203(3) Uani 1 1 d . . .
S6 S 0.61875(17) 0.39177(9) 0.78118(8) 0.0208(4) Uani 1 1 d . . .
S7 S 0.44610(15) 0.37813(10) 0.66088(6) 0.0232(3) Uani 1 1 d . . .
S8 S 0.21472(17) 0.39283(9) 0.75063(9) 0.0225(4) Uani 1 1 d . . .
Co1 Co 0.15713(6) -0.05831(5) 0.80948(3) 0.01587(13) Uani 1 1 d . . .
Co2 Co 0.41399(7) 0.60643(4) 0.75761(3) 0.01529(13) Uani 1 1 d . . .
Pt1 Pt 0.172844(15) 0.155058(13) 0.789446(9) 0.01807(4) Uani 1 1 d . . .
Pt2 Pt 0.416319(13) 0.390989(12) 0.764882(8) 0.01746(4) Uani 1 1 d . . .
H5C H 0.193(3) -0.274(4) 0.833(3) 0.06(2) Uiso 1 1 d D . .
H5D H 0.084(2) -0.258(4) 0.824(2) 0.033(18) Uiso 1 1 d D . .
H10C H 0.409(6) 0.803(5) 0.7896(14) 0.07(2) Uiso 1 1 d D . .
H10D H 0.353(4) 0.810(5) 0.740(2) 0.05(2) Uiso 1 1 d 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
C1 0.018(3) 0.017(2) 0.021(2) -0.0008(18) -0.002(2) -0.002(2)
C2 0.018(3) 0.019(2) 0.021(2) 0.0032(18) -0.002(2) 0.001(2)
C3 0.027(3) 0.023(2) 0.024(2) -0.0036(19) 0.000(2) -0.002(2)
C4 0.033(4) 0.036(3) 0.030(3) -0.012(2) 0.002(2) -0.003(3)
C5 0.036(4) 0.047(3) 0.019(2) -0.006(2) 0.004(3) 0.007(3)
C6 0.038(4) 0.044(3) 0.025(3) 0.012(2) 0.008(2) 0.005(3)
C7 0.034(4) 0.025(2) 0.026(3) 0.007(2) 0.005(2) 0.003(2)
C8 0.023(3) 0.0130(19) 0.020(2) -0.0048(17) 0.004(2) 0.004(2)
C9 0.016(3) 0.024(2) 0.017(2) -0.0026(17) 0.0010(19) -0.0027(19)
C10 0.025(3) 0.023(2) 0.022(2) -0.0049(19) 0.001(2) 0.000(2)
C11 0.026(3) 0.033(3) 0.030(3) -0.002(2) -0.001(2) 0.003(2)
C12 0.019(3) 0.045(3) 0.036(3) -0.004(2) -0.003(2) 0.001(3)
C13 0.023(3) 0.041(3) 0.039(3) -0.001(2) -0.001(3) -0.006(3)
C14 0.028(3) 0.030(3) 0.027(3) 0.000(2) 0.002(2) -0.007(2)
C15 0.019(3) 0.019(2) 0.027(2) -0.0015(19) -0.002(2) 0.001(2)
C16 0.021(3) 0.027(2) 0.025(2) -0.003(2) -0.002(2) 0.002(2)
C17 0.030(3) 0.031(3) 0.025(3) 0.002(2) -0.003(2) 0.004(2)
C18 0.055(5) 0.047(3) 0.027(3) 0.011(3) 0.003(3) 0.008(3)
C19 0.080(6) 0.066(4) 0.028(3) 0.006(3) 0.027(3) 0.026(4)
C20 0.099(7) 0.043(3) 0.037(3) 0.000(3) 0.026(4) 0.026(4)
C21 0.054(4) 0.033(3) 0.029(3) -0.003(2) 0.010(3) 0.008(3)
C22 0.023(3) 0.021(2) 0.019(2) 0.002(2) 0.0024(19) 0.008(2)
C23 0.020(3) 0.020(2) 0.022(2) 0.0042(18) 0.006(2) 0.002(2)
C24 0.024(3) 0.023(2) 0.035(3) 0.010(2) 0.002(2) 0.003(2)
C25 0.022(3) 0.035(3) 0.049(4) 0.006(2) -0.003(3) -0.004(2)
C26 0.022(4) 0.044(3) 0.052(4) 0.016(3) -0.009(3) 0.001(3)
C27 0.025(4) 0.033(3) 0.051(4) 0.018(3) -0.001(3) 0.006(3)
C28 0.023(3) 0.021(2) 0.035(3) 0.008(2) -0.004(2) 0.005(2)
C29 0.016(3) 0.013(2) 0.024(2) 0.0016(17) -0.001(2) -0.0023(19)
C30 0.015(3) 0.017(2) 0.017(2) 0.0017(17) -0.0011(18) -0.0002(19)
C31 0.031(3) 0.020(2) 0.026(2) 0.0038(19) 0.000(2) 0.006(2)
C32 0.049(4) 0.035(3) 0.022(2) 0.007(2) 0.009(2) 0.008(3)
C33 0.043(4) 0.036(3) 0.021(3) -0.005(2) -0.002(3) 0.011(3)
C34 0.027(3) 0.029(3) 0.029(3) -0.009(2) -0.005(2) 0.004(2)
C35 0.022(3) 0.020(2) 0.027(2) -0.0012(19) -0.006(2) -0.002(2)
C36 0.019(3) 0.0165(19) 0.018(2) 0.0012(17) -0.0003(19) -0.001(2)
C37 0.018(3) 0.019(2) 0.019(2) 0.0036(17) 0.0012(19) 0.0022(19)
C38 0.024(3) 0.021(2) 0.027(2) 0.0038(19) 0.002(2) 0.004(2)
C39 0.021(3) 0.030(3) 0.039(3) 0.008(2) 0.003(2) 0.007(2)
C40 0.019(3) 0.036(3) 0.030(3) 0.009(2) -0.003(2) -0.003(2)
C41 0.026(3) 0.027(2) 0.031(3) 0.002(2) 0.000(2) -0.002(2)
C42 0.025(3) 0.020(2) 0.023(2) 0.0055(18) 0.001(2) 0.003(2)
C43 0.018(3) 0.016(2) 0.020(2) -0.0028(17) -0.003(2) 0.0032(19)
C44 0.019(3) 0.032(2) 0.021(2) -0.003(2) -0.004(2) 0.004(2)
C45 0.036(4) 0.030(2) 0.022(2) 0.000(2) 0.006(2) 0.005(2)
C46 0.040(4) 0.043(3) 0.030(3) 0.003(2) 0.006(3) -0.001(3)
C47 0.036(4) 0.062(4) 0.021(3) 0.004(3) 0.008(2) 0.005(3)
C48 0.056(5) 0.055(4) 0.026(3) -0.009(3) 0.008(3) 0.006(3)
C49 0.043(4) 0.035(3) 0.027(3) -0.006(2) 0.006(3) 0.002(3)
C50 0.022(3) 0.017(2) 0.017(2) -0.0040(17) 0.001(2) 0.001(2)
C51 0.023(3) 0.021(2) 0.015(2) -0.0002(18) 0.0020(19) 0.000(2)
C52 0.031(4) 0.026(3) 0.023(3) 0.002(2) 0.001(2) -0.007(2)
C53 0.029(4) 0.048(3) 0.030(3) 0.004(2) -0.003(2) -0.014(3)
C54 0.020(3) 0.068(4) 0.032(3) 0.009(3) -0.007(2) 0.000(3)
C55 0.033(4) 0.047(3) 0.031(3) 0.004(2) -0.003(3) 0.012(3)
C56 0.029(3) 0.029(2) 0.021(2) -0.001(2) -0.003(2) 0.001(2)
O1 0.024(2) 0.0131(14) 0.0209(17) 0.0012(12) 0.0011(15) 0.0001(14)
O2 0.023(2) 0.0147(15) 0.0238(17) 0.0000(13) -0.0009(15) -0.0029(15)
O3 0.026(2) 0.0174(15) 0.0225(17) 0.0000(13) 0.0022(15) 0.0014(15)
O4 0.023(2) 0.0155(15) 0.0280(18) 0.0024(13) -0.0044(15) 0.0003(14)
O5 0.021(2) 0.0098(13) 0.0278(18) 0.0035(13) 0.0009(16) -0.0014(15)
O6 0.022(2) 0.0115(14) 0.0226(17) 0.0015(12) 0.0004(15) 0.0011(13)
O7 0.021(2) 0.0151(15) 0.0247(18) 0.0003(12) -0.0016(15) 0.0026(14)
O8 0.025(2) 0.0169(14) 0.0178(16) -0.0022(12) 0.0037(14) -0.0015(14)
O9 0.023(2) 0.0137(15) 0.0217(17) 0.0013(12) 0.0010(15) -0.0017(14)
O10 0.022(2) 0.0132(14) 0.0239(18) 0.0009(13) -0.0003(15) 0.0036(15)
S1 0.0336(9) 0.0133(5) 0.0236(6) 0.0039(5) 0.0028(6) 0.0066(6)
S2 0.0251(10) 0.0127(5) 0.0362(8) 0.0036(5) 0.0028(7) -0.0004(5)
S3 0.0297(8) 0.0159(5) 0.0252(6) -0.0039(5) 0.0027(5) -0.0017(6)
S4 0.0232(9) 0.0132(5) 0.0319(8) -0.0007(5) 0.0008(7) 0.0029(5)
S5 0.0247(8) 0.0129(5) 0.0233(6) 0.0021(4) 0.0040(5) 0.0040(5)
S6 0.0235(9) 0.0144(6) 0.0244(7) -0.0006(4) 0.0012(6) 0.0035(5)
S7 0.0297(9) 0.0169(5) 0.0230(6) -0.0036(5) -0.0003(6) 0.0007(5)
S8 0.0211(9) 0.0118(6) 0.0348(8) 0.0035(4) 0.0003(7) -0.0021(5)
Co1 0.0187(4) 0.0108(2) 0.0182(3) 0.0002(2) 0.0015(3) 0.0003(3)
Co2 0.0176(3) 0.0098(2) 0.0185(3) 0.0004(2) 0.0012(2) 0.0005(3)
Pt1 0.02233(10) 0.00917(7) 0.02274(8) 0.00012(7) 0.00250(7) 0.00100(8)
Pt2 0.02154(10) 0.00917(7) 0.02168(8) -0.00034(6) 0.00139(7) 0.00077(7)
_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
C1 O1 1.270(5) . ?
C1 C2 1.481(7) . ?
C1 S1 1.706(5) . ?
C2 C7 1.383(7) . ?
C2 C3 1.401(6) . ?
C3 C4 1.381(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.380(8) . ?
C5 H5 0.9500 . ?
C6 C7 1.382(8) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 O2 1.257(6) . ?
C8 C9 1.486(7) . ?
C8 S2 1.712(5) . ?
C9 C10 1.395(7) . ?
C9 C14 1.403(7) . ?
C10 C11 1.381(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.391(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.384(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.368(8) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 O3 1.248(5) . ?
C15 C16 1.498(7) . ?
C15 S3 1.714(5) . ?
C16 C21 1.384(7) . ?
C16 C17 1.398(7) . ?
C17 C18 1.370(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.377(9) . ?
C18 H18 0.9500 . ?
C19 C20 1.383(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.374(9) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C22 O4 1.258(6) . ?
C22 C23 1.486(8) . ?
C22 S4 1.718(5) . ?
C23 C28 1.388(6) . ?
C23 C24 1.392(7) . ?
C24 C25 1.382(8) . ?
C24 H24 0.9500 . ?
C25 C26 1.394(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.382(8) . ?
C26 H26 0.9500 . ?
C27 C28 1.376(8) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 O6 1.264(5) . ?
C29 C30 1.483(7) . ?
C29 S5 1.709(5) . ?
C30 C31 1.390(7) . ?
C30 C35 1.399(6) . ?
C31 C32 1.396(8) . ?
C31 H31 0.9500 . ?
C32 C33 1.390(8) . ?
C32 H32 0.9500 . ?
C33 C34 1.383(8) . ?
C33 H33 0.9500 . ?
C34 C35 1.385(7) . ?
C34 H34 0.9500 . ?
C35 H35 0.9500 . ?
C36 O7 1.244(6) . ?
C36 C37 1.494(7) . ?
C36 S6 1.725(5) . ?
C37 C38 1.396(7) . ?
C37 C42 1.398(6) . ?
C38 C39 1.382(8) . ?
C38 H38 0.9500 . ?
C39 C40 1.388(7) . ?
C39 H39 0.9500 . ?
C40 C41 1.382(7) . ?
C40 H40 0.9500 . ?
C41 C42 1.380(7) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 O8 1.253(5) . ?
C43 C44 1.491(7) . ?
C43 S7 1.726(5) . ?
C44 C49 1.392(7) . ?
C44 C45 1.402(7) . ?
C45 C46 1.380(8) . ?
C45 H45 0.9500 . ?
C46 C47 1.371(8) . ?
C46 H46 0.9500 . ?
C47 C48 1.373(9) . ?
C47 H47 0.9500 . ?
C48 C49 1.380(8) . ?
C48 H48 0.9500 . ?
C49 H49 0.9500 . ?
C50 O9 1.249(6) . ?
C50 C51 1.484(7) . ?
C50 S8 1.732(5) . ?
C51 C56 1.392(7) . ?
C51 C52 1.404(7) . ?
C52 C53 1.381(8) . ?
C52 H52 0.9500 . ?
C53 C54 1.390(9) . ?
C53 H53 0.9500 . ?
C54 C55 1.388(8) . ?
C54 H54 0.9500 . ?
C55 C56 1.381(8) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
O1 Co1 2.091(3) . ?
O2 Co1 2.106(4) . ?
O3 Co1 2.048(3) . ?
O4 Co1 2.062(3) . ?
O5 Co1 2.052(3) . ?
O5 H5C 0.790(19) . ?
O5 H5D 0.782(19) . ?
O6 Co2 2.076(4) . ?
O7 Co2 2.083(4) . ?
O8 Co2 2.025(3) . ?
O9 Co2 2.094(4) . ?
O10 Co2 2.035(3) . ?
O10 H10C 0.795(19) . ?
O10 H10D 0.796(19) . ?
S1 Pt1 2.3275(13) . ?
S2 Pt1 2.3229(19) . ?
S3 Pt1 2.3210(13) . ?
S4 Pt1 2.3187(18) . ?
S5 Pt2 2.3321(14) . ?
S6 Pt2 2.3286(19) . ?
S7 Pt2 2.3278(15) . ?
S8 Pt2 2.3131(19) . ?
Co1 Pt1 2.5674(6) . ?
Co2 Pt2 2.5521(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
O1 C1 C2 118.2(4) . . ?
O1 C1 S1 124.1(4) . . ?
C2 C1 S1 117.7(3) . . ?
C7 C2 C3 118.7(5) . . ?
C7 C2 C1 121.7(4) . . ?
C3 C2 C1 119.6(4) . . ?
C4 C3 C2 119.9(5) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 120.9(5) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 H4 119.5 . . ?
C6 C5 C4 119.1(5) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C7 120.4(5) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C6 C7 C2 120.9(5) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
O2 C8 C9 118.5(4) . . ?
O2 C8 S2 124.1(4) . . ?
C9 C8 S2 117.4(4) . . ?
C10 C9 C14 118.4(5) . . ?
C10 C9 C8 119.1(4) . . ?
C14 C9 C8 122.4(4) . . ?
C11 C10 C9 120.7(5) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
C10 C11 C12 120.1(5) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 119.4(5) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C14 C13 C12 120.8(6) . . ?
C14 C13 H13 119.6 . . ?
C12 C13 H13 119.6 . . ?
C13 C14 C9 120.6(5) . . ?
C13 C14 H14 119.7 . . ?
C9 C14 H14 119.7 . . ?
O3 C15 C16 117.5(4) . . ?
O3 C15 S3 125.2(4) . . ?
C16 C15 S3 117.2(3) . . ?
C21 C16 C17 119.3(5) . . ?
C21 C16 C15 121.4(5) . . ?
C17 C16 C15 119.1(5) . . ?
C18 C17 C16 120.0(6) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C19 120.5(6) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C20 119.8(6) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C21 C20 C19 120.4(6) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C16 120.1(5) . . ?
C20 C21 H21 119.9 . . ?
C16 C21 H21 119.9 . . ?
O4 C22 C23 118.1(4) . . ?
O4 C22 S4 124.5(4) . . ?
C23 C22 S4 117.4(3) . . ?
C28 C23 C24 119.0(5) . . ?
C28 C23 C22 123.3(4) . . ?
C24 C23 C22 117.6(4) . . ?
C25 C24 C23 120.8(5) . . ?
C25 C24 H24 119.6 . . ?
C23 C24 H24 119.6 . . ?
C24 C25 C26 119.2(5) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C27 C26 C25 120.2(6) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C28 C27 C26 120.1(5) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C23 120.7(5) . . ?
C27 C28 H28 119.7 . . ?
C23 C28 H28 119.7 . . ?
O6 C29 C30 118.7(4) . . ?
O6 C29 S5 124.0(4) . . ?
C30 C29 S5 117.3(3) . . ?
C31 C30 C35 119.2(4) . . ?
C31 C30 C29 121.8(4) . . ?
C35 C30 C29 119.0(4) . . ?
C30 C31 C32 120.5(5) . . ?
C30 C31 H31 119.8 . . ?
C32 C31 H31 119.8 . . ?
C33 C32 C31 120.0(6) . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C34 C33 C32 119.4(6) . . ?
C34 C33 H33 120.3 . . ?
C32 C33 H33 120.3 . . ?
C33 C34 C35 121.1(5) . . ?
C33 C34 H34 119.4 . . ?
C35 C34 H34 119.4 . . ?
C34 C35 C30 119.9(5) . . ?
C34 C35 H35 120.1 . . ?
C30 C35 H35 120.1 . . ?
O7 C36 C37 118.2(4) . . ?
O7 C36 S6 124.7(4) . . ?
C37 C36 S6 117.1(4) . . ?
C38 C37 C42 118.6(5) . . ?
C38 C37 C36 123.2(4) . . ?
C42 C37 C36 118.0(4) . . ?
C39 C38 C37 120.4(5) . . ?
C39 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
C38 C39 C40 120.2(5) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C41 C40 C39 119.8(5) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
C42 C41 C40 120.2(5) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C41 C42 C37 120.7(5) . . ?
C41 C42 H42 119.7 . . ?
C37 C42 H42 119.7 . . ?
O8 C43 C44 117.5(4) . . ?
O8 C43 S7 123.9(4) . . ?
C44 C43 S7 118.6(3) . . ?
C49 C44 C45 118.9(5) . . ?
C49 C44 C43 123.5(5) . . ?
C45 C44 C43 117.6(4) . . ?
C46 C45 C44 120.0(5) . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C47 C46 C45 120.4(6) . . ?
C47 C46 H46 119.8 . . ?
C45 C46 H46 119.8 . . ?
C46 C47 C48 120.1(6) . . ?
C46 C47 H47 120.0 . . ?
C48 C47 H47 120.0 . . ?
C47 C48 C49 120.7(6) . . ?
C47 C48 H48 119.6 . . ?
C49 C48 H48 119.6 . . ?
C48 C49 C44 119.9(5) . . ?
C48 C49 H49 120.1 . . ?
C44 C49 H49 120.1 . . ?
O9 C50 C51 120.7(4) . . ?
O9 C50 S8 123.7(4) . . ?
C51 C50 S8 115.6(4) . . ?
C56 C51 C52 119.6(5) . . ?
C56 C51 C50 118.2(5) . . ?
C52 C51 C50 122.1(5) . . ?
C53 C52 C51 120.2(5) . . ?
C53 C52 H52 119.9 . . ?
C51 C52 H52 119.9 . . ?
C52 C53 C54 119.7(6) . . ?
C52 C53 H53 120.2 . . ?
C54 C53 H53 120.2 . . ?
C55 C54 C53 120.2(6) . . ?
C55 C54 H54 119.9 . . ?
C53 C54 H54 119.9 . . ?
C56 C55 C54 120.4(5) . . ?
C56 C55 H55 119.8 . . ?
C54 C55 H55 119.8 . . ?
C55 C56 C51 119.8(5) . . ?
C55 C56 H56 120.1 . . ?
C51 C56 H56 120.1 . . ?
C1 O1 Co1 127.2(3) . . ?
C8 O2 Co1 124.5(3) . . ?
C15 O3 Co1 126.1(3) . . ?
C22 O4 Co1 127.2(3) . . ?
Co1 O5 H5C 131(4) . . ?
Co1 O5 H5D 119(4) . . ?
H5C O5 H5D 108(3) . . ?
C29 O6 Co2 125.3(3) . . ?
C36 O7 Co2 126.4(3) . . ?
C43 O8 Co2 127.3(3) . . ?
C50 O9 Co2 123.4(3) . . ?
Co2 O10 H10C 111(5) . . ?
Co2 O10 H10D 120(5) . . ?
H10C O10 H10D 105(3) . . ?
C1 S1 Pt1 104.33(16) . . ?
C8 S2 Pt1 106.8(2) . . ?
C15 S3 Pt1 103.92(17) . . ?
C22 S4 Pt1 103.8(2) . . ?
C29 S5 Pt2 104.99(17) . . ?
C36 S6 Pt2 103.35(19) . . ?
C43 S7 Pt2 103.55(16) . . ?
C50 S8 Pt2 106.80(19) . . ?
O3 Co1 O5 93.05(14) . . ?
O3 Co1 O4 89.31(14) . . ?
O5 Co1 O4 91.38(14) . . ?
O3 Co1 O1 177.18(13) . . ?
O5 Co1 O1 89.72(13) . . ?
O4 Co1 O1 90.10(14) . . ?
O3 Co1 O2 91.40(14) . . ?
O5 Co1 O2 90.10(14) . . ?
O4 Co1 O2 178.32(13) . . ?
O1 Co1 O2 89.12(13) . . ?
O3 Co1 Pt1 89.48(9) . . ?
O5 Co1 Pt1 177.39(10) . . ?
O4 Co1 Pt1 88.01(8) . . ?
O1 Co1 Pt1 87.74(8) . . ?
O2 Co1 Pt1 90.47(8) . . ?
O8 Co2 O10 94.44(13) . . ?
O8 Co2 O6 177.19(13) . . ?
O10 Co2 O6 87.72(13) . . ?
O8 Co2 O7 90.88(15) . . ?
O10 Co2 O7 92.29(13) . . ?
O6 Co2 O7 90.83(14) . . ?
O8 Co2 O9 89.76(14) . . ?
O10 Co2 O9 89.18(13) . . ?
O6 Co2 O9 88.47(14) . . ?
O7 Co2 O9 178.35(12) . . ?
O8 Co2 Pt2 88.75(9) . . ?
O10 Co2 Pt2 176.80(11) . . ?
O6 Co2 Pt2 89.08(8) . . ?
O7 Co2 Pt2 87.92(8) . . ?
O9 Co2 Pt2 90.57(8) . . ?
S4 Pt1 S3 89.01(6) . . ?
S4 Pt1 S2 179.51(7) . . ?
S3 Pt1 S2 91.44(6) . . ?
S4 Pt1 S1 90.20(6) . . ?
S3 Pt1 S1 178.75(5) . . ?
S2 Pt1 S1 89.36(6) . . ?
S4 Pt1 Co1 91.10(3) . . ?
S3 Pt1 Co1 89.76(4) . . ?
S2 Pt1 Co1 88.71(4) . . ?
S1 Pt1 Co1 91.22(3) . . ?
S8 Pt2 S7 91.04(6) . . ?
S8 Pt2 S6 178.68(7) . . ?
S7 Pt2 S6 90.08(6) . . ?
S8 Pt2 S5 88.44(6) . . ?
S7 Pt2 S5 179.45(7) . . ?
S6 Pt2 S5 90.44(6) . . ?
S8 Pt2 Co2 88.41(3) . . ?
S7 Pt2 Co2 90.27(3) . . ?
S6 Pt2 Co2 90.89(3) . . ?
S5 Pt2 Co2 89.55(3) . . ?
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
O5 H5C O6 0.790(19) 2.01(3) 2.780(5) 164(7) 1_545
O10 H10C O2 0.795(19) 2.27(4) 2.935(5) 141(5) 1_565
O10 H10D O1 0.796(19) 1.90(3) 2.666(5) 160(6) 1_565
_diffrn_measured_fraction_theta_max 0.944
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 2.175
_refine_diff_density_min -1.335
_refine_diff_density_rms 0.119
###END
data_dahl1a_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 842003'
#TrackingRef '- Dahl-Doerrer-PtMtba-all_compounds-v4.cif'
_symmetry_space_group_name_hall 'I -4 -2c'
#Added by publCIF
# TEXT
_publ_section_references
;
Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany.
Sheldrick, G. M. (1997). SHELXL97. University of G\"ottingen, Germany.
Bruker (2006). SAINT. Bruker Analytical X-ray Instruments Inc., Madison,
Wisconsin, USA.
Bruker (2006). APEX2. Bruker Analytical X-ray Instruments Inc., Madison,
Wisconsin, USA.
Dolmanov, O. V., et al. (2009). OLEX2: A complete structure solution,
refinement and analysis program. J. Appl. Cryst. 42, 339-341 (2009).
;
#==============================================================================
_audit_update_record
;
2011-03-10 # Formatted by publCIF
;
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C28 H21 Ni O5 Pt S4, C4.35 H8.70 O1.09'
_chemical_formula_sum 'C32.35 H29.70 Ni O6.09 Pt S4'
_chemical_formula_weight 897.95
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 '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'
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_H-M 'I -4 c 2'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z'
'-x, -y, z'
'-y, x, -z'
'-x, y, z+1/2'
'y, x, -z+1/2'
'x, -y, z+1/2'
'-y, -x, -z+1/2'
'x+1/2, y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, -z+1/2'
'-x+1/2, y+1/2, z+1'
'y+1/2, x+1/2, -z+1'
'x+1/2, -y+1/2, z+1'
'-y+1/2, -x+1/2, -z+1'
_cell_length_a 19.0697(15)
_cell_length_b 19.0697(15)
_cell_length_c 22.6005(19)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 8218.8(11)
_cell_formula_units_Z 8
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 9689
_cell_measurement_theta_min 6.064
_cell_measurement_theta_max 132.080
_exptl_crystal_description block
_exptl_crystal_colour 'light green'
_exptl_crystal_size_max 0.224
_exptl_crystal_size_mid 0.194
_exptl_crystal_size_min 0.184
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.451
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 3540
_exptl_absorpt_coefficient_mu 9.052
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.5953
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 1.54178
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'rotating anode'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker Proteum-R'
_diffrn_measurement_method '\w & \f scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time 0
_diffrn_standards_decay_% 0
_diffrn_reflns_number 101221
_diffrn_reflns_av_R_equivalents 0.0459
_diffrn_reflns_av_sigmaI/netI 0.0123
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 21
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_l_min -25
_diffrn_reflns_limit_l_max 26
_diffrn_reflns_theta_min 5.54
_diffrn_reflns_theta_max 66.49
_reflns_number_total 3586
_reflns_number_gt 3536
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'APEX2 (Bruker, 2006)'
_computing_cell_refinement 'SAINT (Bruker, 2006)'
_computing_data_reduction 'SAINT (Bruker, 2006)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'OLEX2 (Dolmanov et al., 2009)'
_computing_publication_material ?
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based on F,
with F set to zero for negative F^2^. The threshold expression of F^2^ >
2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not
relevant to the choice of reflections for refinement. R-factors based on F^2^
are statistically about twice as large as those based on F, and R- factors
based on ALL data will be even larger.
CheckCIF Alerts and responses:
PLAT420_ALERT_2_B D-H Without Acceptor O3 - *H3 ... ?
Response: The position H3, constrained with a riding model to the water
oxygen atom O3, did not refine to the torsion angle expected for a hydrogen
bond to the disordered tetrahydrofuran molecule, despite the O...O distances
of 2.71 and 2.68 angstroms to the two disordered THF oxygen positions, O1S
and O1SA, respectively. This is likely due to the partial absence of the
THF molecule, which refines to a total occupancy of 0.54; the water ligand
the fraction with the THF absent may be free to rotate.
PLAT601_ALERT_2_B Structure Contains Solvent Accessible VOIDS of . 154
A**3
Response: This void was likely occupied by another solvent molecule. The
large crystals in this sample invariably cracked upon cooling for low
temperature data collection, and thus data collection had to be carried out
at room temperature. If this void was occupied by another solvent
molecule, nearly all of the solvent in this position most likely diffused
out of the crystal before and/or during data collection. The remaining
THF observed is oriented to hydrogen bond to the water ligand,
decreasing its mobility. The void position lacks a potential hydrogen
bonding interaction. Since only one residual electron density peak with a
magnitude of 0.55 electrons per cubic angstrom was observed in the void
region of asymmetric unit, refinement of a partial occupancy solvent
molecule in this position was not appropriate, and the use of SQUEEZE
was not necessary to improve the model. The occupancy of solvent in the
void region appears to be near zero.
PLAT042_ALERT_1_C Calc. and Reported MoietyFormula Strings Differ ?
Response: This is a specious alert, since the calculated and reported
moiety formulas are identical. The alert likely arises due to the
inclusion of a disordered THF molecule with a total occupance less than 1
in the refinement model.
;
_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^)+(0.0742P)^2^+17.0623P] where P=(Fo^2^+2Fc^2^)/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 SHELXL
_refine_ls_extinction_coef 0.00057(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack -0.050(13)
_refine_ls_number_reflns 3586
_refine_ls_number_parameters 211
_refine_ls_number_restraints 578
_refine_ls_R_factor_all 0.0334
_refine_ls_R_factor_gt 0.0330
_refine_ls_wR_factor_ref 0.1073
_refine_ls_wR_factor_gt 0.1064
_refine_ls_goodness_of_fit_ref 1.131
_refine_ls_restrained_S_all 1.067
_refine_ls_shift/su_max 0.008
_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 0.442868(8) 0.057132(8) 0.5000 0.03897(16) Uani 1 2 d SU . .
Ni1 Ni 0.34776(3) 0.15224(3) 0.5000 0.0399(2) Uani 1 2 d SU A .
S1 S 0.47969(15) 0.09343(16) 0.59294(10) 0.0524(6) Uani 0.782(6) 1 d PU A 1
S1A S 0.4559(5) 0.0710(6) 0.6002(5) 0.0524(6) Uani 0.218(6) 1 d PU A 2
S2 S 0.52013(11) 0.13662(11) 0.45622(15) 0.0504(6) Uani 0.782(6) 1 d PU A 1
S2A S 0.5270(5) 0.1444(4) 0.4843(5) 0.0504(6) Uani 0.218(6) 1 d PU A 2
O1 O 0.3604(4) 0.1640(4) 0.5898(3) 0.055(2) Uani 0.782(6) 1 d PU A 1
O1A O 0.3825(15) 0.1855(17) 0.5835(13) 0.055(2) Uani 0.218(6) 1 d PU A 2
O2 O 0.4202(5) 0.2263(4) 0.4879(3) 0.058(2) Uani 0.782(6) 1 d PU A 1
O2A O 0.419(2) 0.2190(18) 0.4639(14) 0.058(2) Uani 0.218(6) 1 d PU A 2
O3 O 0.27192(15) 0.22808(15) 0.5000 0.0538(10) Uani 1 2 d SU . .
H3 H 0.2416 0.2181 0.4757 0.081 Uiso 0.50 1 calc PR A .
C1 C 0.4145(3) 0.1456(3) 0.6188(2) 0.0451(11) Uani 1 1 d DU . .
C2A C 0.4219(17) 0.1784(19) 0.6769(10) 0.0595(18) Uani 0.218(6) 1 d PGU A 1
C3A C 0.3643(16) 0.2157(18) 0.6975(11) 0.087(3) Uani 0.218(6) 1 d PGDU A 1
H3A H 0.3303 0.2314 0.6711 0.104 Uiso 0.218(6) 1 calc PR A 1
C4A C 0.3574(18) 0.229(2) 0.7576(12) 0.119(4) Uani 0.218(6) 1 d PGU A 1
H4A H 0.3188 0.2544 0.7715 0.142 Uiso 0.218(6) 1 calc PR A 1
C5A C 0.408(2) 0.206(2) 0.7971(9) 0.126(5) Uani 0.218(6) 1 d PGU A 1
H5A H 0.4035 0.2151 0.8373 0.152 Uiso 0.218(6) 1 calc PR A 1
C6A C 0.4657(19) 0.169(2) 0.7764(12) 0.115(3) Uani 0.218(6) 1 d PGU A 1
H6A H 0.4997 0.1528 0.8028 0.137 Uiso 0.218(6) 1 calc PR A 1
C7A C 0.4726(16) 0.155(2) 0.7163(13) 0.077(3) Uani 0.218(6) 1 d PGDU A 1
H7A H 0.5112 0.1299 0.7025 0.092 Uiso 0.218(6) 1 calc PR A 1
C2B C 0.4209(5) 0.1679(4) 0.6822(3) 0.0595(18) Uani 0.782(6) 1 d PGU A 2
C3B C 0.3930(5) 0.2327(4) 0.6977(3) 0.087(3) Uani 0.782(6) 1 d PGDU A 2
H3B H 0.3660 0.2577 0.6707 0.104 Uiso 0.782(6) 1 calc PR A 2
C4B C 0.4054(6) 0.2602(5) 0.7538(4) 0.119(4) Uani 0.782(6) 1 d PGU A 2
H4B H 0.3867 0.3035 0.7642 0.142 Uiso 0.782(6) 1 calc PR A 2
C5B C 0.4457(6) 0.2229(6) 0.7942(3) 0.126(5) Uani 0.782(6) 1 d PGU A 2
H5B H 0.4540 0.2412 0.8317 0.152 Uiso 0.782(6) 1 calc PR A 2
C6B C 0.4736(5) 0.1581(6) 0.7786(3) 0.115(3) Uani 0.782(6) 1 d PGU A 2
H6B H 0.5005 0.1331 0.8057 0.137 Uiso 0.782(6) 1 calc PR A 2
C7B C 0.4612(5) 0.1306(4) 0.7226(4) 0.077(3) Uani 0.782(6) 1 d PGDU A 2
H7B H 0.4799 0.0873 0.7122 0.092 Uiso 0.782(6) 1 calc PR A 2
C8 C 0.4809(3) 0.2165(3) 0.4666(2) 0.0458(11) Uani 1 1 d DU . .
C9 C 0.5236(17) 0.2785(14) 0.451(2) 0.0530(13) Uani 0.218(6) 1 d PGU A 1
C10 C 0.4928(19) 0.3441(16) 0.457(2) 0.088(4) Uani 0.218(6) 1 d PGDU A 1
H10 H 0.4463 0.3477 0.4696 0.105 Uiso 0.218(6) 1 calc PR A 1
C11 C 0.531(3) 0.4043(14) 0.446(3) 0.109(5) Uani 0.218(6) 1 d PGU A 1
H11 H 0.5108 0.4482 0.4502 0.130 Uiso 0.218(6) 1 calc PR A 1
C12 C 0.601(3) 0.399(2) 0.428(3) 0.110(4) Uani 0.218(6) 1 d PGU A 1
H12 H 0.6268 0.4392 0.4200 0.132 Uiso 0.218(6) 1 calc PR A 1
C13 C 0.632(2) 0.333(3) 0.421(3) 0.077(3) Uani 0.218(6) 1 d PGU A 1
H13 H 0.6782 0.3297 0.4093 0.092 Uiso 0.218(6) 1 calc PR A 1
C14 C 0.5931(17) 0.273(2) 0.4330(18) 0.060(2) Uani 0.218(6) 1 d PGDU A 1
H14 H 0.6137 0.2292 0.4287 0.072 Uiso 0.218(6) 1 calc PR A 1
C9B C 0.5215(4) 0.2801(4) 0.4496(5) 0.0530(13) Uani 0.782(6) 1 d PGU A 2
C10B C 0.4829(4) 0.3397(5) 0.4355(6) 0.088(4) Uani 0.782(6) 1 d PGDU A 2
H10A H 0.4342 0.3384 0.4368 0.105 Uiso 0.782(6) 1 calc PR A 2
C11B C 0.5172(6) 0.4012(4) 0.4196(6) 0.109(5) Uani 0.782(6) 1 d PGU A 2
H11A H 0.4914 0.4410 0.4101 0.130 Uiso 0.782(6) 1 calc PR A 2
C12B C 0.5900(6) 0.4031(5) 0.4177(7) 0.110(4) Uani 0.782(6) 1 d PGU A 2
H12A H 0.6130 0.4443 0.4070 0.132 Uiso 0.782(6) 1 calc PR A 2
C13B C 0.6286(5) 0.3436(6) 0.4318(6) 0.077(3) Uani 0.782(6) 1 d PGU A 2
H13A H 0.6773 0.3448 0.4305 0.092 Uiso 0.782(6) 1 calc PR A 2
C14B C 0.5943(4) 0.2821(5) 0.4477(4) 0.060(2) Uani 0.782(6) 1 d PGDU A 2
H14A H 0.6201 0.2422 0.4572 0.072 Uiso 0.782(6) 1 calc PR A 2
O1S O 0.6988(7) 0.2480(7) 0.6015(6) 0.050 Uiso 0.294(7) 1 d PDU B 1
C1S C 0.7034(9) 0.2833(10) 0.6552(8) 0.050 Uiso 0.294(7) 1 d PDU B 1
H1SC H 0.7354 0.3227 0.6524 0.060 Uiso 0.294(7) 1 calc PR B 1
H1SD H 0.7192 0.2522 0.6864 0.060 Uiso 0.294(7) 1 calc PR B 1
C2S C 0.5807(9) 0.2709(10) 0.6224(8) 0.050 Uiso 0.294(7) 1 d PDU B 1
H2SC H 0.5676 0.3007 0.5894 0.060 Uiso 0.294(7) 1 calc PR B 1
H2SD H 0.5391 0.2512 0.6406 0.060 Uiso 0.294(7) 1 calc PR B 1
C3S C 0.6271(8) 0.3088(10) 0.6670(8) 0.050 Uiso 0.294(7) 1 d PDU B 1
H3SC H 0.6129 0.2974 0.7070 0.060 Uiso 0.294(7) 1 calc PR B 1
H3SD H 0.6237 0.3592 0.6616 0.060 Uiso 0.294(7) 1 calc PR B 1
C4S C 0.6334(8) 0.2148(9) 0.6048(9) 0.050 Uiso 0.294(7) 1 d PDU B 1
H4SC H 0.6344 0.1776 0.6340 0.060 Uiso 0.294(7) 1 calc PR B 1
H4SD H 0.6210 0.1947 0.5667 0.060 Uiso 0.294(7) 1 calc PR B 1
O1SA O 0.6776(8) 0.2717(9) 0.5880(7) 0.050 Uiso 0.25 1 d PDU C 2
C3SA C 0.6001(10) 0.2500(12) 0.6620(8) 0.050 Uiso 0.25 1 d PDU C 2
H3SA H 0.5776 0.2096 0.6798 0.060 Uiso 0.25 1 calc PR C 2
H3SB H 0.5709 0.2910 0.6681 0.060 Uiso 0.25 1 calc PR C 2
C4SA C 0.6140(11) 0.2380(13) 0.5971(9) 0.050 Uiso 0.25 1 d PDU C 2
H4SA H 0.6176 0.1884 0.5883 0.060 Uiso 0.25 1 calc PR C 2
H4SB H 0.5774 0.2585 0.5729 0.060 Uiso 0.25 1 calc PR C 2
C1SA C 0.6969(12) 0.3117(11) 0.6377(8) 0.050 Uiso 0.25 1 d PDU C 2
H1SA H 0.6710 0.3554 0.6396 0.060 Uiso 0.25 1 calc PR C 2
H1SB H 0.7468 0.3215 0.6381 0.060 Uiso 0.25 1 calc PR C 2
C2SA C 0.6758(10) 0.2614(12) 0.6877(9) 0.050 Uiso 0.25 1 d PDU C 2
H2SA H 0.6757 0.2836 0.7264 0.060 Uiso 0.25 1 calc PR C 2
H2SB H 0.7036 0.2188 0.6885 0.060 Uiso 0.25 1 calc PR C 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 0.03546(17) 0.03546(17) 0.0460(2) -0.00009(14) -0.00009(14) 0.00678(7)
Ni1 0.0383(3) 0.0383(3) 0.0431(5) 0.0003(5) 0.0003(5) 0.0081(4)
S1 0.0407(13) 0.0603(15) 0.0562(10) -0.0110(10) -0.0086(9) 0.0142(10)
S1A 0.0407(13) 0.0603(15) 0.0562(10) -0.0110(10) -0.0086(9) 0.0142(10)
S2 0.0471(8) 0.0411(8) 0.0631(17) 0.0002(11) 0.0151(11) 0.0057(6)
S2A 0.0471(8) 0.0411(8) 0.0631(17) 0.0002(11) 0.0151(11) 0.0057(6)
O1 0.051(5) 0.064(5) 0.048(2) -0.008(3) -0.003(3) 0.024(4)
O1A 0.051(5) 0.064(5) 0.048(2) -0.008(3) -0.003(3) 0.024(4)
O2 0.047(2) 0.041(2) 0.086(7) 0.001(4) 0.020(5) 0.0133(19)
O2A 0.047(2) 0.041(2) 0.086(7) 0.001(4) 0.020(5) 0.0133(19)
O3 0.0485(15) 0.0485(15) 0.064(3) -0.002(3) -0.002(3) 0.0166(18)
C1 0.044(3) 0.048(3) 0.043(2) 0.005(2) -0.001(2) 0.006(2)
C2A 0.072(4) 0.064(4) 0.043(3) 0.004(3) 0.002(3) 0.014(3)
C3A 0.110(7) 0.092(6) 0.059(4) -0.019(4) -0.017(5) 0.042(6)
C4A 0.157(9) 0.134(9) 0.065(4) -0.041(5) -0.018(6) 0.072(8)
C5A 0.136(10) 0.183(10) 0.060(5) -0.038(6) -0.027(5) 0.063(8)
C6A 0.125(7) 0.162(8) 0.057(4) -0.014(5) -0.027(5) 0.062(6)
C7A 0.086(5) 0.091(7) 0.054(4) 0.005(4) -0.016(4) 0.024(6)
C2B 0.072(4) 0.064(4) 0.043(3) 0.004(3) 0.002(3) 0.014(3)
C3B 0.110(7) 0.092(6) 0.059(4) -0.019(4) -0.017(5) 0.042(6)
C4B 0.157(9) 0.134(9) 0.065(4) -0.041(5) -0.018(6) 0.072(8)
C5B 0.136(10) 0.183(10) 0.060(5) -0.038(6) -0.027(5) 0.063(8)
C6B 0.125(7) 0.162(8) 0.057(4) -0.014(5) -0.027(5) 0.062(6)
C7B 0.086(5) 0.091(7) 0.054(4) 0.005(4) -0.016(4) 0.024(6)
C8 0.052(3) 0.038(2) 0.047(3) -0.005(2) 0.000(2) 0.000(2)
C9 0.056(3) 0.045(2) 0.058(3) -0.004(2) 0.005(3) -0.009(2)
C10 0.063(5) 0.043(3) 0.157(13) 0.006(5) 0.009(6) -0.002(3)
C11 0.095(7) 0.051(4) 0.180(16) 0.031(7) 0.002(8) -0.005(4)
C12 0.103(7) 0.073(5) 0.154(12) 0.038(6) 0.009(8) -0.027(5)
C13 0.075(4) 0.076(6) 0.078(7) 0.010(5) 0.002(4) -0.032(4)
C14 0.061(3) 0.063(4) 0.054(6) 0.000(4) -0.009(4) -0.012(3)
C9B 0.056(3) 0.045(2) 0.058(3) -0.004(2) 0.005(3) -0.009(2)
C10B 0.063(5) 0.043(3) 0.157(13) 0.006(5) 0.009(6) -0.002(3)
C11B 0.095(7) 0.051(4) 0.180(16) 0.031(7) 0.002(8) -0.005(4)
C12B 0.103(7) 0.073(5) 0.154(12) 0.038(6) 0.009(8) -0.027(5)
C13B 0.075(4) 0.076(6) 0.078(7) 0.010(5) 0.002(4) -0.032(4)
C14B 0.061(3) 0.063(4) 0.054(6) 0.000(4) -0.009(4) -0.012(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 S1A 2.293(10) 16 ?
Pt1 S1A 2.293(10) . ?
Pt1 S1 2.320(2) . ?
Pt1 S1 2.321(2) 16 ?
Pt1 S2A 2.339(9) 16 ?
Pt1 S2A 2.339(9) . ?
Pt1 S2 2.334(2) . ?
Pt1 S2 2.334(2) 16 ?
Pt1 Ni1 2.5649(10) . ?
Pt1 Pt1 3.0816(5) 3_655 ?
Ni1 O2 1.995(9) . ?
Ni1 O2 1.995(9) 16 ?
Ni1 O3 2.045(4) . ?
Ni1 O2A 2.03(4) 16 ?
Ni1 O2A 2.03(4) . ?
Ni1 O1 2.055(7) . ?
Ni1 O1 2.055(7) 16 ?
Ni1 O1A 2.10(3) 16 ?
Ni1 O1A 2.10(3) . ?
S1 C1 1.696(6) . ?
S1A C1 1.680(10) . ?
S2 C8 1.713(6) . ?
S2A C8 1.679(10) . ?
O1 C1 1.272(9) . ?
O1A C1 1.26(3) . ?
O2 C8 1.268(11) . ?
O2A C8 1.19(4) . ?
O3 H3 0.8200 . ?
C1 C2A 1.46(2) . ?
C1 C2B 1.499(8) . ?
C2A C3A 1.3900 . ?
C2A C7A 1.3900 . ?
C3A C4A 1.3900 . ?
C3A H3A 0.9300 . ?
C4A C5A 1.3900 . ?
C4A H4A 0.9300 . ?
C5A C6A 1.3900 . ?
C5A H5A 0.9300 . ?
C6A C7A 1.3900 . ?
C6A H6A 0.9300 . ?
C7A H7A 0.9300 . ?
C2B C3B 1.3900 . ?
C2B C7B 1.3900 . ?
C3B C4B 1.3900 . ?
C3B H3B 0.9300 . ?
C4B C5B 1.3900 . ?
C4B H4B 0.9300 . ?
C5B C6B 1.3900 . ?
C5B H5B 0.9300 . ?
C6B C7B 1.3900 . ?
C6B H6B 0.9300 . ?
C7B H7B 0.9300 . ?
C8 C9 1.48(2) . ?
C8 C9B 1.490(9) . ?
C9 C10 1.3900 . ?
C9 C14 1.3900 . ?
C10 C11 1.3900 . ?
C10 H10 0.9300 . ?
C11 C12 1.3900 . ?
C11 H11 0.9300 . ?
C12 C13 1.3900 . ?
C12 H12 0.9300 . ?
C13 C14 1.3900 . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C9B C10B 1.3900 . ?
C9B C14B 1.3900 . ?
C10B C11B 1.3900 . ?
C10B H10A 0.9300 . ?
C11B C12B 1.3900 . ?
C11B H11A 0.9300 . ?
C12B C13B 1.3900 . ?
C12B H12A 0.9300 . ?
C13B C14B 1.3900 . ?
C13B H13A 0.9300 . ?
C14B H14A 0.9300 . ?
O1S C1S 1.391(15) . ?
O1S C4S 1.400(15) . ?
C1S C3S 1.557(16) . ?
C1S H1SC 0.9700 . ?
C1S H1SD 0.9700 . ?
C2S C3S 1.522(16) . ?
C2S C4S 1.521(16) . ?
C2S H2SC 0.9700 . ?
C2S H2SD 0.9700 . ?
C3S H3SC 0.9700 . ?
C3S H3SD 0.9700 . ?
C4S H4SC 0.9700 . ?
C4S H4SD 0.9700 . ?
O1SA C4SA 1.387(16) . ?
O1SA C1SA 1.407(16) . ?
C3SA C4SA 1.507(17) . ?
C3SA C2SA 1.572(17) . ?
C3SA H3SA 0.9700 . ?
C3SA H3SB 0.9700 . ?
C4SA H4SA 0.9700 . ?
C4SA H4SB 0.9700 . ?
C1SA C2SA 1.536(17) . ?
C1SA H1SA 0.9700 . ?
C1SA H1SB 0.9700 . ?
C2SA H2SA 0.9700 . ?
C2SA H2SB 0.9700 . ?
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
S1A Pt1 S1A 179.4(4) 16 . ?
S1A Pt1 S1 164.0(3) 16 . ?
S1A Pt1 S1 16.0(3) . . ?
S1A Pt1 S1 16.0(3) 16 16 ?
S1A Pt1 S1 164.0(3) . 16 ?
S1 Pt1 S1 179.65(10) . 16 ?
S1A Pt1 S2A 89.6(3) 16 16 ?
S1A Pt1 S2A 90.4(3) . 16 ?
S1 Pt1 S2A 106.4(3) . 16 ?
S1 Pt1 S2A 73.6(3) 16 16 ?
S1A Pt1 S2A 90.4(3) 16 . ?
S1A Pt1 S2A 89.6(3) . . ?
S1 Pt1 S2A 73.6(3) . . ?
S1 Pt1 S2A 106.4(3) 16 . ?
S2A Pt1 S2A 177.9(4) 16 . ?
S1A Pt1 S2 74.0(3) 16 . ?
S1A Pt1 S2 106.0(3) . . ?
S1 Pt1 S2 89.94(9) . . ?
S1 Pt1 S2 90.06(9) 16 . ?
S2A Pt1 S2 163.5(2) 16 . ?
S2A Pt1 S2 16.4(2) . . ?
S1A Pt1 S2 106.0(3) 16 16 ?
S1A Pt1 S2 74.0(3) . 16 ?
S1 Pt1 S2 90.06(9) . 16 ?
S1 Pt1 S2 89.94(9) 16 16 ?
S2A Pt1 S2 16.4(2) 16 16 ?
S2A Pt1 S2 163.5(2) . 16 ?
S2 Pt1 S2 178.53(9) . 16 ?
S1A Pt1 Ni1 89.7(2) 16 . ?
S1A Pt1 Ni1 89.7(2) . . ?
S1 Pt1 Ni1 90.17(5) . . ?
S1 Pt1 Ni1 90.18(5) 16 . ?
S2A Pt1 Ni1 88.94(19) 16 . ?
S2A Pt1 Ni1 88.94(19) . . ?
S2 Pt1 Ni1 89.26(5) . . ?
S2 Pt1 Ni1 89.26(5) 16 . ?
S1A Pt1 Pt1 90.3(2) 16 3_655 ?
S1A Pt1 Pt1 90.3(2) . 3_655 ?
S1 Pt1 Pt1 89.83(5) . 3_655 ?
S1 Pt1 Pt1 89.83(5) 16 3_655 ?
S2A Pt1 Pt1 91.06(19) 16 3_655 ?
S2A Pt1 Pt1 91.06(19) . 3_655 ?
S2 Pt1 Pt1 90.74(5) . 3_655 ?
S2 Pt1 Pt1 90.74(5) 16 3_655 ?
Ni1 Pt1 Pt1 179.998(4) . 3_655 ?
O2 Ni1 O2 178.7(5) . 16 ?
O2 Ni1 O3 89.3(2) . . ?
O2 Ni1 O3 89.3(2) 16 . ?
O2 Ni1 O2A 164.1(9) . 16 ?
O2 Ni1 O2A 16.0(9) 16 16 ?
O3 Ni1 O2A 91.6(10) . 16 ?
O2 Ni1 O2A 16.0(9) . . ?
O2 Ni1 O2A 164.1(9) 16 . ?
O3 Ni1 O2A 91.6(10) . . ?
O2A Ni1 O2A 177(2) 16 . ?
O2 Ni1 O1 88.6(3) . . ?
O2 Ni1 O1 91.4(3) 16 . ?
O3 Ni1 O1 90.4(2) . . ?
O2A Ni1 O1 75.5(10) 16 . ?
O2A Ni1 O1 104.5(10) . . ?
O2 Ni1 O1 91.4(3) . 16 ?
O2 Ni1 O1 88.6(3) 16 16 ?
O3 Ni1 O1 90.4(2) . 16 ?
O2A Ni1 O1 104.5(10) 16 16 ?
O2A Ni1 O1 75.5(10) . 16 ?
O1 Ni1 O1 179.3(4) . 16 ?
O2 Ni1 O1A 108.1(8) . 16 ?
O2 Ni1 O1A 72.0(8) 16 16 ?
O3 Ni1 O1A 90.5(8) . 16 ?
O2A Ni1 O1A 87.8(12) 16 16 ?
O2A Ni1 O1A 92.2(12) . 16 ?
O1 Ni1 O1A 163.3(7) . 16 ?
O1 Ni1 O1A 16.7(7) 16 16 ?
O2 Ni1 O1A 72.0(8) . . ?
O2 Ni1 O1A 108.1(8) 16 . ?
O3 Ni1 O1A 90.5(8) . . ?
O2A Ni1 O1A 92.2(12) 16 . ?
O2A Ni1 O1A 87.8(12) . . ?
O1 Ni1 O1A 16.7(7) . . ?
O1 Ni1 O1A 163.3(7) 16 . ?
O1A Ni1 O1A 179.0(17) 16 . ?
O2 Ni1 Pt1 90.7(2) . . ?
O2 Ni1 Pt1 90.7(2) 16 . ?
O3 Ni1 Pt1 180.00(5) . . ?
O2A Ni1 Pt1 88.4(10) 16 . ?
O2A Ni1 Pt1 88.4(10) . . ?
O1 Ni1 Pt1 89.6(2) . . ?
O1 Ni1 Pt1 89.6(2) 16 . ?
O1A Ni1 Pt1 89.5(8) 16 . ?
O1A Ni1 Pt1 89.5(8) . . ?
C1 S1 Pt1 105.4(2) . . ?
C1 S1A Pt1 107.1(5) . . ?
C8 S2 Pt1 104.1(2) . . ?
C8 S2A Pt1 105.1(5) . . ?
C1 O1 Ni1 125.1(5) . . ?
C1 O1A Ni1 123(2) . . ?
C8 O2 Ni1 125.4(5) . . ?
C8 O2A Ni1 128(2) . . ?
Ni1 O3 H3 109.5 . . ?
O1A C1 O1 27.6(12) . . ?
O1A C1 C2A 111(2) . . ?
O1 C1 C2A 115.1(12) . . ?
O1A C1 C2B 118.1(15) . . ?
O1 C1 C2B 118.7(6) . . ?
C2A C1 C2B 8.9(17) . . ?
O1A C1 S1A 125.5(16) . . ?
O1 C1 S1A 119.0(6) . . ?
C2A C1 S1A 122.9(12) . . ?
C2B C1 S1A 116.3(6) . . ?
O1A C1 S1 119.4(14) . . ?
O1 C1 S1 125.3(5) . . ?
C2A C1 S1 119.4(11) . . ?
C2B C1 S1 115.9(5) . . ?
S1A C1 S1 22.0(4) . . ?
C3A C2A C7A 120.0 . . ?
C3A C2A C1 116.4(16) . . ?
C7A C2A C1 120.3(17) . . ?
C4A C3A C2A 120.0 . . ?
C4A C3A H3A 120.0 . . ?
C2A C3A H3A 120.0 . . ?
C5A C4A C3A 120.0 . . ?
C5A C4A H4A 120.0 . . ?
C3A C4A H4A 120.0 . . ?
C4A C5A C6A 120.0 . . ?
C4A C5A H5A 120.0 . . ?
C6A C5A H5A 120.0 . . ?
C7A C6A C5A 120.0 . . ?
C7A C6A H6A 120.0 . . ?
C5A C6A H6A 120.0 . . ?
C6A C7A C2A 120.0 . . ?
C6A C7A H7A 120.0 . . ?
C2A C7A H7A 120.0 . . ?
C3B C2B C7B 120.0 . . ?
C3B C2B C1 117.6(5) . . ?
C7B C2B C1 121.8(5) . . ?
C4B C3B C2B 120.0 . . ?
C4B C3B H3B 120.0 . . ?
C2B C3B H3B 120.0 . . ?
C3B C4B C5B 120.0 . . ?
C3B C4B H4B 120.0 . . ?
C5B C4B H4B 120.0 . . ?
C6B C5B C4B 120.0 . . ?
C6B C5B H5B 120.0 . . ?
C4B C5B H5B 120.0 . . ?
C5B C6B C7B 120.0 . . ?
C5B C6B H6B 120.0 . . ?
C7B C6B H6B 120.0 . . ?
C6B C7B C2B 120.0 . . ?
C6B C7B H7B 120.0 . . ?
C2B C7B H7B 120.0 . . ?
O2A C8 O2 26.1(15) . . ?
O2A C8 C9 120(2) . . ?
O2 C8 C9 118.4(14) . . ?
O2A C8 C9B 118.2(18) . . ?
O2 C8 C9B 116.9(6) . . ?
C9 C8 C9B 2(2) . . ?
O2A C8 S2A 124.5(18) . . ?
O2 C8 S2A 120.5(6) . . ?
C9 C8 S2A 115.0(15) . . ?
C9B C8 S2A 117.2(6) . . ?
O2A C8 S2 117.7(17) . . ?
O2 C8 S2 125.6(5) . . ?
C9 C8 S2 116.0(13) . . ?
C9B C8 S2 117.5(5) . . ?
S2A C8 S2 22.6(3) . . ?
C10 C9 C14 120.0 . . ?
C10 C9 C8 117.5(18) . . ?
C14 C9 C8 122.4(18) . . ?
C11 C10 C9 120.0 . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C12 C13 C14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 C9 120.0 . . ?
C13 C14 H14 120.0 . . ?
C9 C14 H14 120.0 . . ?
C10B C9B C14B 120.0 . . ?
C10B C9B C8 116.8(6) . . ?
C14B C9B C8 123.2(6) . . ?
C9B C10B C11B 120.0 . . ?
C9B C10B H10A 120.0 . . ?
C11B C10B H10A 120.0 . . ?
C12B C11B C10B 120.0 . . ?
C12B C11B H11A 120.0 . . ?
C10B C11B H11A 120.0 . . ?
C13B C12B C11B 120.0 . . ?
C13B C12B H12A 120.0 . . ?
C11B C12B H12A 120.0 . . ?
C12B C13B C14B 120.0 . . ?
C12B C13B H13A 120.0 . . ?
C14B C13B H13A 120.0 . . ?
C13B C14B C9B 120.0 . . ?
C13B C14B H14A 120.0 . . ?
C9B C14B H14A 120.0 . . ?
C1S O1S C4S 103.3(14) . . ?
O1S C1S C3S 103.9(14) . . ?
O1S C1S H1SC 111.0 . . ?
C3S C1S H1SC 111.0 . . ?
O1S C1S H1SD 111.0 . . ?
C3S C1S H1SD 111.0 . . ?
H1SC C1S H1SD 109.0 . . ?
C3S C2S C4S 97.2(14) . . ?
C3S C2S H2SC 112.3 . . ?
C4S C2S H2SC 112.3 . . ?
C3S C2S H2SD 112.3 . . ?
C4S C2S H2SD 112.3 . . ?
H2SC C2S H2SD 109.9 . . ?
C2S C3S C1S 106.4(14) . . ?
C2S C3S H3SC 110.5 . . ?
C1S C3S H3SC 110.5 . . ?
C2S C3S H3SD 110.5 . . ?
C1S C3S H3SD 110.5 . . ?
H3SC C3S H3SD 108.6 . . ?
O1S C4S C2S 106.5(14) . . ?
O1S C4S H4SC 110.4 . . ?
C2S C4S H4SC 110.4 . . ?
O1S C4S H4SD 110.4 . . ?
C2S C4S H4SD 110.4 . . ?
H4SC C4S H4SD 108.6 . . ?
C4SA O1SA C1SA 111.1(16) . . ?
C4SA C3SA C2SA 102.6(16) . . ?
C4SA C3SA H3SA 111.2 . . ?
C2SA C3SA H3SA 111.2 . . ?
C4SA C3SA H3SB 111.2 . . ?
C2SA C3SA H3SB 111.2 . . ?
H3SA C3SA H3SB 109.2 . . ?
O1SA C4SA C3SA 103.3(16) . . ?
O1SA C4SA H4SA 111.1 . . ?
C3SA C4SA H4SA 111.1 . . ?
O1SA C4SA H4SB 111.1 . . ?
C3SA C4SA H4SB 111.1 . . ?
H4SA C4SA H4SB 109.1 . . ?
O1SA C1SA C2SA 100.5(16) . . ?
O1SA C1SA H1SA 111.7 . . ?
C2SA C1SA H1SA 111.7 . . ?
O1SA C1SA H1SB 111.7 . . ?
C2SA C1SA H1SB 111.7 . . ?
H1SA C1SA H1SB 109.4 . . ?
C1SA C2SA C3SA 93.1(15) . . ?
C1SA C2SA H2SA 113.1 . . ?
C3SA C2SA H2SA 113.1 . . ?
C1SA C2SA H2SB 113.1 . . ?
C3SA C2SA H2SB 113.1 . . ?
H2SA C2SA H2SB 110.5 . . ?
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
S1A Pt1 Ni1 O2 -91.2(4) 16 . . . ?
S1A Pt1 Ni1 O2 88.8(4) . . . . ?
S1 Pt1 Ni1 O2 72.7(3) . . . . ?
S1 Pt1 Ni1 O2 -107.3(3) 16 . . . ?
S2A Pt1 Ni1 O2 179.1(4) 16 . . . ?
S2A Pt1 Ni1 O2 -0.9(4) . . . . ?
S2 Pt1 Ni1 O2 -17.2(2) . . . . ?
S2 Pt1 Ni1 O2 162.8(2) 16 . . . ?
Pt1 Pt1 Ni1 O2 122(9) 3_655 . . . ?
S1A Pt1 Ni1 O2 88.8(4) 16 . . 16 ?
S1A Pt1 Ni1 O2 -91.2(4) . . . 16 ?
S1 Pt1 Ni1 O2 -107.3(3) . . . 16 ?
S1 Pt1 Ni1 O2 72.7(3) 16 . . 16 ?
S2A Pt1 Ni1 O2 -0.9(4) 16 . . 16 ?
S2A Pt1 Ni1 O2 179.1(4) . . . 16 ?
S2 Pt1 Ni1 O2 162.8(2) . . . 16 ?
S2 Pt1 Ni1 O2 -17.2(2) 16 . . 16 ?
Pt1 Pt1 Ni1 O2 -58(9) 3_655 . . 16 ?
S1A Pt1 Ni1 O3 -99.1(3) 16 . . . ?
S1A Pt1 Ni1 O3 80.9(3) . . . . ?
S1 Pt1 Ni1 O3 64.85(9) . . . . ?
S1 Pt1 Ni1 O3 -115.15(9) 16 . . . ?
S2A Pt1 Ni1 O3 171.3(3) 16 . . . ?
S2A Pt1 Ni1 O3 -8.7(3) . . . . ?
S2 Pt1 Ni1 O3 -25.09(9) . . . . ?
S2 Pt1 Ni1 O3 154.91(9) 16 . . . ?
Pt1 Pt1 Ni1 O3 114(9) 3_655 . . . ?
S1A Pt1 Ni1 O2A 104.6(11) 16 . . 16 ?
S1A Pt1 Ni1 O2A -75.4(11) . . . 16 ?
S1 Pt1 Ni1 O2A -91.4(10) . . . 16 ?
S1 Pt1 Ni1 O2A 88.6(10) 16 . . 16 ?
S2A Pt1 Ni1 O2A 15.0(10) 16 . . 16 ?
S2A Pt1 Ni1 O2A -165.0(10) . . . 16 ?
S2 Pt1 Ni1 O2A 178.6(10) . . . 16 ?
S2 Pt1 Ni1 O2A -1.4(10) 16 . . 16 ?
Pt1 Pt1 Ni1 O2A -42(9) 3_655 . . 16 ?
S1A Pt1 Ni1 O2A -75.4(11) 16 . . . ?
S1A Pt1 Ni1 O2A 104.6(11) . . . . ?
S1 Pt1 Ni1 O2A 88.6(10) . . . . ?
S1 Pt1 Ni1 O2A -91.4(10) 16 . . . ?
S2A Pt1 Ni1 O2A -165.0(10) 16 . . . ?
S2A Pt1 Ni1 O2A 15.0(10) . . . . ?
S2 Pt1 Ni1 O2A -1.4(10) . . . . ?
S2 Pt1 Ni1 O2A 178.6(10) 16 . . . ?
Pt1 Pt1 Ni1 O2A 138(9) 3_655 . . . ?
S1A Pt1 Ni1 O1 -179.9(4) 16 . . . ?
S1A Pt1 Ni1 O1 0.1(4) . . . . ?
S1 Pt1 Ni1 O1 -15.9(2) . . . . ?
S1 Pt1 Ni1 O1 164.1(2) 16 . . . ?
S2A Pt1 Ni1 O1 90.5(4) 16 . . . ?
S2A Pt1 Ni1 O1 -89.5(4) . . . . ?
S2 Pt1 Ni1 O1 -105.9(2) . . . . ?
S2 Pt1 Ni1 O1 74.1(2) 16 . . . ?
Pt1 Pt1 Ni1 O1 33(9) 3_655 . . . ?
S1A Pt1 Ni1 O1 0.1(4) 16 . . 16 ?
S1A Pt1 Ni1 O1 -179.9(4) . . . 16 ?
S1 Pt1 Ni1 O1 164.1(2) . . . 16 ?
S1 Pt1 Ni1 O1 -15.9(2) 16 . . 16 ?
S2A Pt1 Ni1 O1 -89.5(4) 16 . . 16 ?
S2A Pt1 Ni1 O1 90.5(4) . . . 16 ?
S2 Pt1 Ni1 O1 74.1(2) . . . 16 ?
S2 Pt1 Ni1 O1 -105.9(2) 16 . . 16 ?
Pt1 Pt1 Ni1 O1 -147(9) 3_655 . . 16 ?
S1A Pt1 Ni1 O1A 16.8(9) 16 . . 16 ?
S1A Pt1 Ni1 O1A -163.2(9) . . . 16 ?
S1 Pt1 Ni1 O1A -179.2(8) . . . 16 ?
S1 Pt1 Ni1 O1A 0.8(8) 16 . . 16 ?
S2A Pt1 Ni1 O1A -72.8(9) 16 . . 16 ?
S2A Pt1 Ni1 O1A 107.2(9) . . . 16 ?
S2 Pt1 Ni1 O1A 90.8(8) . . . 16 ?
S2 Pt1 Ni1 O1A -89.2(8) 16 . . 16 ?
Pt1 Pt1 Ni1 O1A -130(9) 3_655 . . 16 ?
S1A Pt1 Ni1 O1A -163.2(9) 16 . . . ?
S1A Pt1 Ni1 O1A 16.8(9) . . . . ?
S1 Pt1 Ni1 O1A 0.8(8) . . . . ?
S1 Pt1 Ni1 O1A -179.2(8) 16 . . . ?
S2A Pt1 Ni1 O1A 107.2(9) 16 . . . ?
S2A Pt1 Ni1 O1A -72.8(9) . . . . ?
S2 Pt1 Ni1 O1A -89.2(8) . . . . ?
S2 Pt1 Ni1 O1A 90.8(8) 16 . . . ?
Pt1 Pt1 Ni1 O1A 50(9) 3_655 . . . ?
S1A Pt1 S1 C1 104.0(8) 16 . . . ?
S1A Pt1 S1 C1 -73.9(9) . . . . ?
S1 Pt1 S1 C1 -165(100) 16 . . . ?
S2A Pt1 S1 C1 -74.5(3) 16 . . . ?
S2A Pt1 S1 C1 103.3(3) . . . . ?
S2 Pt1 S1 C1 103.7(3) . . . . ?
S2 Pt1 S1 C1 -74.8(3) 16 . . . ?
Ni1 Pt1 S1 C1 14.5(2) . . . . ?
Pt1 Pt1 S1 C1 -165.5(2) 3_655 . . . ?
S1A Pt1 S1A C1 -13.6(6) 16 . . . ?
S1 Pt1 S1A C1 78.1(10) . . . . ?
S1 Pt1 S1A C1 -103.1(8) 16 . . . ?
S2A Pt1 S1A C1 -102.4(6) 16 . . . ?
S2A Pt1 S1A C1 75.4(6) . . . . ?
S2 Pt1 S1A C1 75.7(6) . . . . ?
S2 Pt1 S1A C1 -102.8(6) 16 . . . ?
Ni1 Pt1 S1A C1 -13.5(6) . . . . ?
Pt1 Pt1 S1A C1 166.5(6) 3_655 . . . ?
S1A Pt1 S2 C8 105.5(3) 16 . . . ?
S1A Pt1 S2 C8 -73.9(3) . . . . ?
S1 Pt1 S2 C8 -74.6(2) . . . . ?
S1 Pt1 S2 C8 105.7(2) 16 . . . ?
S2A Pt1 S2 C8 99.3(7) 16 . . . ?
S2A Pt1 S2 C8 -73.2(8) . . . . ?
S2 Pt1 S2 C8 15.5(2) 16 . . . ?
Ni1 Pt1 S2 C8 15.6(2) . . . . ?
Pt1 Pt1 S2 C8 -164.4(2) 3_655 . . . ?
S1A Pt1 S2A C8 77.5(6) 16 . . . ?
S1A Pt1 S2A C8 -101.9(6) . . . . ?
S1 Pt1 S2A C8 -102.7(5) . . . . ?
S1 Pt1 S2A C8 77.7(5) 16 . . . ?
S2A Pt1 S2A C8 -12.2(5) 16 . . . ?
S2 Pt1 S2A C8 78.8(9) . . . . ?
S2 Pt1 S2A C8 -96.0(8) 16 . . . ?
Ni1 Pt1 S2A C8 -12.2(5) . . . . ?
Pt1 Pt1 S2A C8 167.8(5) 3_655 . . . ?
O2 Ni1 O1 C1 -69.9(6) . . . . ?
O2 Ni1 O1 C1 111.4(7) 16 . . . ?
O3 Ni1 O1 C1 -159.2(6) . . . . ?
O2A Ni1 O1 C1 109.2(12) 16 . . . ?
O2A Ni1 O1 C1 -67.5(12) . . . . ?
O1 Ni1 O1 C1 20.8(6) 16 . . . ?
O1A Ni1 O1 C1 108(3) 16 . . . ?
O1A Ni1 O1 C1 -69(3) . . . . ?
Pt1 Ni1 O1 C1 20.8(6) . . . . ?
O2 Ni1 O1A C1 -116(2) . . . . ?
O2 Ni1 O1A C1 66(2) 16 . . . ?
O3 Ni1 O1A C1 155(2) . . . . ?
O2A Ni1 O1A C1 64(2) 16 . . . ?
O2A Ni1 O1A C1 -113(2) . . . . ?
O1 Ni1 O1A C1 66(3) . . . . ?
O1 Ni1 O1A C1 -112(3) 16 . . . ?
O1A Ni1 O1A C1 -25(2) 16 . . . ?
Pt1 Ni1 O1A C1 -25(2) . . . . ?
O2 Ni1 O2 C8 -158.2(7) 16 . . . ?
O3 Ni1 O2 C8 -158.3(7) . . . . ?
O2A Ni1 O2 C8 108(4) 16 . . . ?
O2A Ni1 O2 C8 -60(4) . . . . ?
O1 Ni1 O2 C8 111.4(8) . . . . ?
O1 Ni1 O2 C8 -67.9(7) 16 . . . ?
O1A Ni1 O2 C8 -67.9(12) 16 . . . ?
O1A Ni1 O2 C8 111.0(12) . . . . ?
Pt1 Ni1 O2 C8 21.7(7) . . . . ?
O2 Ni1 O2A C8 74(5) . . . . ?
O2 Ni1 O2A C8 -111(4) 16 . . . ?
O3 Ni1 O2A C8 156(3) . . . . ?
O2A Ni1 O2A C8 -24(3) 16 . . . ?
O1 Ni1 O2A C8 65(3) . . . . ?
O1 Ni1 O2A C8 -114(3) 16 . . . ?
O1A Ni1 O2A C8 -113(3) 16 . . . ?
O1A Ni1 O2A C8 66(3) . . . . ?
Pt1 Ni1 O2A C8 -24(3) . . . . ?
Ni1 O1A C1 O1 -66(3) . . . . ?
Ni1 O1A C1 C2A -170(2) . . . . ?
Ni1 O1A C1 C2B -164.8(12) . . . . ?
Ni1 O1A C1 S1A 20(3) . . . . ?
Ni1 O1A C1 S1 45(2) . . . . ?
Ni1 O1 C1 O1A 74(4) . . . . ?
Ni1 O1 C1 C2A 161.1(17) . . . . ?
Ni1 O1 C1 C2B 170.2(5) . . . . ?
Ni1 O1 C1 S1A -38.0(9) . . . . ?
Ni1 O1 C1 S1 -13.0(9) . . . . ?
Pt1 S1A C1 O1A 0.1(18) . . . . ?
Pt1 S1A C1 O1 32.0(8) . . . . ?
Pt1 S1A C1 C2A -168.7(18) . . . . ?
Pt1 S1A C1 C2B -175.6(6) . . . . ?
Pt1 S1A C1 S1 -81.0(11) . . . . ?
Pt1 S1 C1 O1A -37.2(17) . . . . ?
Pt1 S1 C1 O1 -5.1(6) . . . . ?
Pt1 S1 C1 C2A -179.0(18) . . . . ?
Pt1 S1 C1 C2B 171.7(5) . . . . ?
Pt1 S1 C1 S1A 75.3(10) . . . . ?
O1A C1 C2A C3A 40(3) . . . . ?
O1 C1 C2A C3A 11(3) . . . . ?
C2B C1 C2A C3A -105(10) . . . . ?
S1A C1 C2A C3A -149.4(18) . . . . ?
S1 C1 C2A C3A -174.9(15) . . . . ?
O1A C1 C2A C7A -160(2) . . . . ?
O1 C1 C2A C7A 170.3(17) . . . . ?
C2B C1 C2A C7A 54(8) . . . . ?
S1A C1 C2A C7A 10(3) . . . . ?
S1 C1 C2A C7A -15(3) . . . . ?
C7A C2A C3A C4A 0.0 . . . . ?
C1 C2A C3A C4A 160(3) . . . . ?
C2A C3A C4A C5A 0.0 . . . . ?
C3A C4A C5A C6A 0.0 . . . . ?
C4A C5A C6A C7A 0.0 . . . . ?
C5A C6A C7A C2A 0.0 . . . . ?
C3A C2A C7A C6A 0.0 . . . . ?
C1 C2A C7A C6A -159(3) . . . . ?
O1A C1 C2B C3B -2.1(18) . . . . ?
O1 C1 C2B C3B -33.5(10) . . . . ?
C2A C1 C2B C3B 35(9) . . . . ?
S1A C1 C2B C3B 174.0(8) . . . . ?
S1 C1 C2B C3B 149.4(6) . . . . ?
O1A C1 C2B C7B -173.5(16) . . . . ?
O1 C1 C2B C7B 155.1(7) . . . . ?
C2A C1 C2B C7B -137(10) . . . . ?
S1A C1 C2B C7B 2.5(10) . . . . ?
S1 C1 C2B C7B -22.0(9) . . . . ?
C7B C2B C3B C4B 0.0 . . . . ?
C1 C2B C3B C4B -171.6(9) . . . . ?
C2B C3B C4B C5B 0.0 . . . . ?
C3B C4B C5B C6B 0.0 . . . . ?
C4B C5B C6B C7B 0.0 . . . . ?
C5B C6B C7B C2B 0.0 . . . . ?
C3B C2B C7B C6B 0.0 . . . . ?
C1 C2B C7B C6B 171.2(9) . . . . ?
Ni1 O2A C8 O2 -71(4) . . . . ?
Ni1 O2A C8 C9 -164(3) . . . . ?
Ni1 O2A C8 C9B -165.1(17) . . . . ?
Ni1 O2A C8 S2A 19(3) . . . . ?
Ni1 O2A C8 S2 44(3) . . . . ?
Ni1 O2 C8 O2A 68(4) . . . . ?
Ni1 O2 C8 C9 170(2) . . . . ?
Ni1 O2 C8 C9B 167.6(7) . . . . ?
Ni1 O2 C8 S2A -39.1(10) . . . . ?
Ni1 O2 C8 S2 -12.7(10) . . . . ?
Pt1 S2A C8 O2A 0.5(19) . . . . ?
Pt1 S2A C8 O2 31.3(8) . . . . ?
Pt1 S2A C8 C9 -177(2) . . . . ?
Pt1 S2A C8 C9B -175.5(6) . . . . ?
Pt1 S2A C8 S2 -78.7(9) . . . . ?
Pt1 S2 C8 O2A -36.0(17) . . . . ?
Pt1 S2 C8 O2 -6.6(7) . . . . ?
Pt1 S2 C8 C9 171(2) . . . . ?
Pt1 S2 C8 C9B 173.0(6) . . . . ?
Pt1 S2 C8 S2A 78.0(8) . . . . ?
O2A C8 C9 C10 26(3) . . . . ?
O2 C8 C9 C10 -4(3) . . . . ?
C9B C8 C9 C10 46(51) . . . . ?
S2A C8 C9 C10 -157(2) . . . . ?
S2 C8 C9 C10 178.3(18) . . . . ?
O2A C8 C9 C14 -156(3) . . . . ?
O2 C8 C9 C14 174(3) . . . . ?
C9B C8 C9 C14 -137(54) . . . . ?
S2A C8 C9 C14 21(4) . . . . ?
S2 C8 C9 C14 -4(4) . . . . ?
C14 C9 C10 C11 0.0 . . . . ?
C8 C9 C10 C11 177(4) . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C10 C11 C12 C13 0.0 . . . . ?
C11 C12 C13 C14 0.0 . . . . ?
C12 C13 C14 C9 0.0 . . . . ?
C10 C9 C14 C13 0.0 . . . . ?
C8 C9 C14 C13 -177(4) . . . . ?
O2A C8 C9B C10B 4.2(19) . . . . ?
O2 C8 C9B C10B -25.3(10) . . . . ?
C9 C8 C9B C10B -157(52) . . . . ?
S2A C8 C9B C10B -179.5(7) . . . . ?
S2 C8 C9B C10B 155.0(5) . . . . ?
O2A C8 C9B C14B -176.1(18) . . . . ?
O2 C8 C9B C14B 154.4(8) . . . . ?
C9 C8 C9B C14B 23(51) . . . . ?
S2A C8 C9B C14B 0.1(12) . . . . ?
S2 C8 C9B C14B -25.3(11) . . . . ?
C14B C9B C10B C11B 0.0 . . . . ?
C8 C9B C10B C11B 179.6(11) . . . . ?
C9B C10B C11B C12B 0.0 . . . . ?
C10B C11B C12B C13B 0.0 . . . . ?
C11B C12B C13B C14B 0.0 . . . . ?
C12B C13B C14B C9B 0.0 . . . . ?
C10B C9B C14B C13B 0.0 . . . . ?
C8 C9B C14B C13B -179.6(12) . . . . ?
C4S O1S C1S C3S -37.0(19) . . . . ?
C4S C2S C3S C1S 16(2) . . . . ?
O1S C1S C3S C2S 12(2) . . . . ?
C1S O1S C4S C2S 50.6(19) . . . . ?
C3S C2S C4S O1S -39.7(19) . . . . ?
C1SA O1SA C4SA C3SA -10(3) . . . . ?
C2SA C3SA C4SA O1SA -25(2) . . . . ?
C4SA O1SA C1SA C2SA 41(2) . . . . ?
O1SA C1SA C2SA C3SA -50.8(19) . . . . ?
C4SA C3SA C2SA C1SA 46(2) . . . . ?
_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full 66.49
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max 1.098
_refine_diff_density_min -0.907
_refine_diff_density_rms 0.152
###END