# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full Chem.Commun.
#TrackingRef '- U3.cif'
_journal_coden_Cambridge 0182
_publ_contact_author_name 'Anne E. V. Gorden'
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
Auburn University
179 Chemistry Building
Auburn, Alabama 36849
;
_publ_contact_author_phone '1 (334) 844-4043'
_publ_contact_author_fax '1 (334) 844-6959'
_publ_contact_author_email gordeae@auburn.edu
#=========================================================================
# TITLE AND AUTHOR LIST
_publ_section_title
;
Actinide Tetracyanoplatinates: Synthesis and Structural Characterization
Featuring Unique Fluorescent Properties from d-f Orbital Interactions
;
# The loop structure below should contain the names and addesses of all
# authors, in the required order of publication. Repeat as necessary.
loop_
_publ_author_name
_publ_author_address
B.A.Maynard
;
Department of Chemistry and Biochemistry
Auburn University
179 Chemistry Building
Auburn, Alabama 36849
;
R.E.Sykora
;
Chemistry Building, Room 223
University of South Alabama
Mobile, AL 36688
;
J.T.Mague
;
Department of Chemistry
Tulane University
2015 Percival Stern Hall
New Orleans, LA 70118
;
A.E.V.Gorden
;
Department of Chemistry and Biochemistry
Auburn University
179 Chemistry Building
Auburn, Alabama 36849
;
# Attachment 'Th1f.cif.txt'
data_fpbca
_database_code_depnum_ccdc_archive 'CCDC 769470'
#TrackingRef 'Th1f.cif.txt'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
;
C8 H14 N8 O7 Pt2 Th1, 10(H2O)
;
_chemical_formula_sum 'C8 H34 N8 O17 Pt2 Th'
_chemical_formula_weight 1136.65
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Orthorhombic
_symmetry_space_group_name_H-M 'P b c a'
_symmetry_space_group_name_Hall '-P 2ac 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
_cell_length_a 13.2464(6)
_cell_length_b 20.5599(10)
_cell_length_c 22.4536(11)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 6115.1(5)
_cell_formula_units_Z 8
_cell_measurement_temperature 193(2)
_cell_measurement_reflns_used 7574
_cell_measurement_theta_min 1.81
_cell_measurement_theta_max 28.27
_exptl_crystal_description plate
_exptl_crystal_colour yellow-green
_exptl_crystal_size_max 0.80
_exptl_crystal_size_mid 0.80
_exptl_crystal_size_min 0.09
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.469
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 4160
_exptl_absorpt_coefficient_mu 14.053
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.0314
_exptl_absorpt_correction_T_max 0.3645
_exptl_absorpt_process_details 'Alcock, N.W. (1974). Acta Cryst, A40, 332-335'
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 193(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 59819
_diffrn_reflns_av_R_equivalents 0.0737
_diffrn_reflns_av_sigmaI/netI 0.0366
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_l_min -29
_diffrn_reflns_limit_l_max 29
_diffrn_reflns_theta_min 1.81
_diffrn_reflns_theta_max 28.27
_reflns_number_total 7574
_reflns_number_gt 6225
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'SMART (Bruker, 2000)'
_computing_cell_refinement 'SMART, SAINT (Bruker, 1999)'
_computing_data_reduction 'SAINT (Bruker, 1999)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'ATOMS v6.1 (Shape Software, 2004)'
_computing_publication_material 'SHELXCIF-97 (Sheldrick, 1997)'
_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^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens none
_refine_ls_hydrogen_treatment none
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 7574
_refine_ls_number_parameters 325
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0373
_refine_ls_R_factor_gt 0.0301
_refine_ls_wR_factor_ref 0.0781
_refine_ls_wR_factor_gt 0.0766
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_restrained_S_all 1.036
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Th1 Th 0.361670(13) 0.395629(9) 0.866901(8) 0.01401(6) Uani 1 1 d . . .
Pt1 Pt 0.374701(14) 0.625938(10) 0.734453(9) 0.01641(6) Uani 1 1 d . . .
O1 O 0.2519(3) 0.39467(18) 0.77834(18) 0.0278(9) Uani 1 1 d . . .
N1 N 0.3683(3) 0.5121(2) 0.8278(2) 0.0217(10) Uani 1 1 d . . .
C1 C 0.3711(4) 0.5557(2) 0.7954(2) 0.0180(11) Uani 1 1 d . . .
O2 O 0.4947(3) 0.3941(2) 0.79219(18) 0.0253(9) Uani 1 1 d . . .
Pt2 Pt 0.373276(14) 0.142084(10) 0.766798(9) 0.01542(6) Uani 1 1 d . . .
N2 N 0.1312(3) 0.2367(3) 0.8310(3) 0.0332(13) Uani 1 1 d . . .
C2 C 0.3733(4) 0.6956(3) 0.7957(3) 0.0210(12) Uani 1 1 d . . .
O3 O 0.2275(3) 0.32249(17) 0.90356(17) 0.0225(8) Uani 1 1 d . . .
N3 N 0.6121(4) 0.2301(2) 0.8688(2) 0.0313(12) Uani 1 1 d . . .
C3 C 0.3809(4) 0.6923(3) 0.6703(3) 0.0237(12) Uani 1 1 d . . .
O4 O 0.2058(3) 0.46017(18) 0.88652(18) 0.0247(9) Uani 1 1 d . . .
N4 N 0.3619(4) 0.5162(3) 0.6382(2) 0.0348(13) Uani 1 1 d . . .
C4 C 0.3683(4) 0.5561(3) 0.6732(3) 0.0258(13) Uani 1 1 d . . .
O5 O 0.5104(3) 0.45590(19) 0.90517(19) 0.0253(9) Uani 1 1 d . . .
N5 N 0.3705(3) 0.2874(2) 0.8098(2) 0.0181(9) Uani 1 1 d . . .
C5 C 0.3725(4) 0.2356(3) 0.7925(2) 0.0183(11) Uani 1 1 d . . .
O6 O 0.4743(3) 0.31806(18) 0.91970(18) 0.0236(8) Uani 1 1 d . . .
N6 N 0.3954(4) 0.1798(3) 0.6321(2) 0.0333(12) Uani 1 1 d . . .
C6 C 0.3872(4) 0.1663(3) 0.6813(3) 0.0216(11) Uani 1 1 d . . .
O7 O 0.3459(3) 0.4136(2) 0.97302(18) 0.0267(9) Uani 1 1 d . . .
C7 C 0.3567(4) 0.1168(3) 0.8520(3) 0.0199(11) Uani 1 1 d . . .
N7 N 0.3449(4) 0.1006(2) 0.9002(2) 0.0311(12) Uani 1 1 d . . .
O8 O 0.0127(3) 0.4252(2) 0.8998(2) 0.0323(10) Uani 1 1 d . . .
N8 N 0.6239(3) 0.4929(3) 0.7635(2) 0.0280(12) Uani 1 1 d . . .
C8 C 0.3755(4) 0.0487(3) 0.7462(2) 0.0208(12) Uani 1 1 d . . .
O9 O 0.4100(4) 0.2602(2) 1.01999(18) 0.0356(11) Uani 1 1 d . . .
O10 O 0.4764(3) 0.3339(2) 0.68651(19) 0.0301(10) Uani 1 1 d . . .
O11 O 0.4819(3) 0.1362(2) 0.9962(2) 0.0381(11) Uani 1 1 d . . .
O12 O 0.6790(3) 0.3788(2) 0.0177(2) 0.0346(10) Uani 1 1 d . . .
O13 O 0.2101(3) 0.4223(2) 0.5978(2) 0.0315(10) Uani 1 1 d . . .
O14 O 0.5082(3) 0.58130(19) 0.94193(19) 0.0278(9) Uani 1 1 d . . .
O15 O 0.2691(3) 0.32581(19) 0.67595(18) 0.0300(9) Uani 1 1 d . . .
O16 O 0.2020(4) 0.2537(2) 1.0071(2) 0.0380(11) Uani 1 1 d . . .
O17 O 0.1751(4) 0.4061(3) 1.0301(3) 0.074(2) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Th1 0.01808(10) 0.01418(9) 0.00978(10) -0.00029(7) 0.00019(7) 0.00005(7)
Pt1 0.01883(11) 0.01621(11) 0.01417(11) 0.00185(8) 0.00067(8) 0.00014(7)
O1 0.038(2) 0.026(2) 0.019(2) -0.0027(17) -0.0077(18) 0.0055(18)
N1 0.027(3) 0.018(2) 0.020(3) 0.002(2) -0.002(2) -0.0006(17)
C1 0.024(3) 0.016(3) 0.014(3) -0.004(2) 0.000(2) 0.0001(19)
O2 0.036(2) 0.024(2) 0.016(2) -0.0018(19) 0.0099(17) -0.0030(16)
Pt2 0.01879(11) 0.01494(10) 0.01252(11) -0.00163(7) 0.00105(8) -0.00018(7)
N2 0.031(3) 0.030(3) 0.038(3) -0.008(3) 0.003(2) -0.001(2)
C2 0.021(3) 0.019(3) 0.023(3) -0.001(2) 0.000(2) -0.001(2)
O3 0.0243(19) 0.0237(19) 0.019(2) -0.0005(16) 0.0034(16) -0.0063(15)
N3 0.035(3) 0.030(3) 0.029(3) -0.009(2) 0.003(2) 0.000(2)
C3 0.025(3) 0.021(3) 0.025(3) -0.001(2) 0.000(2) 0.000(2)
O4 0.023(2) 0.024(2) 0.027(2) 0.0017(18) 0.0049(17) 0.0054(15)
N4 0.047(3) 0.036(3) 0.021(3) -0.007(2) -0.004(2) 0.000(2)
C4 0.035(3) 0.026(3) 0.016(3) 0.009(2) 0.000(2) -0.001(2)
O5 0.026(2) 0.027(2) 0.023(2) -0.0032(18) -0.0063(17) -0.0030(15)
N5 0.026(2) 0.015(2) 0.013(2) -0.0017(18) 0.0021(18) -0.0008(16)
C5 0.016(3) 0.025(3) 0.013(3) 0.004(2) 0.001(2) 0.000(2)
O6 0.031(2) 0.0241(19) 0.016(2) 0.0010(17) -0.0006(17) 0.0062(16)
N6 0.040(3) 0.039(3) 0.021(3) 0.000(2) 0.003(3) -0.004(2)
C6 0.024(3) 0.023(3) 0.018(3) -0.006(2) 0.000(2) 0.000(2)
O7 0.026(2) 0.042(2) 0.012(2) -0.0029(18) 0.0025(17) -0.0005(17)
C7 0.022(3) 0.018(3) 0.019(3) -0.004(2) 0.001(2) -0.0030(19)
N7 0.043(3) 0.027(3) 0.024(3) 0.002(2) 0.003(2) -0.006(2)
O8 0.031(2) 0.031(2) 0.035(3) -0.002(2) -0.001(2) -0.0005(17)
N8 0.032(3) 0.020(3) 0.032(3) 0.004(2) 0.005(2) -0.0010(18)
C8 0.028(3) 0.023(3) 0.011(3) -0.003(2) 0.004(2) 0.000(2)
O9 0.056(3) 0.035(2) 0.016(2) 0.0008(19) 0.004(2) -0.001(2)
O10 0.037(2) 0.032(2) 0.021(2) -0.0025(19) 0.0004(19) 0.0013(18)
O11 0.045(3) 0.041(3) 0.028(3) -0.001(2) -0.006(2) 0.004(2)
O12 0.036(2) 0.040(3) 0.028(3) 0.001(2) 0.000(2) 0.004(2)
O13 0.030(2) 0.036(2) 0.029(3) -0.003(2) -0.0037(19) -0.0016(18)
O14 0.037(2) 0.029(2) 0.018(2) -0.0061(19) -0.0043(18) -0.0030(16)
O15 0.039(2) 0.030(2) 0.021(2) -0.0019(18) -0.0028(19) -0.0006(18)
O16 0.058(3) 0.036(2) 0.020(2) 0.007(2) 0.006(2) -0.001(2)
O17 0.044(3) 0.139(6) 0.040(3) -0.045(4) 0.017(3) -0.024(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
Th1 O7 2.420(4) . ?
Th1 O2 2.434(4) . ?
Th1 O1 2.464(4) . ?
Th1 O3 2.469(4) . ?
Th1 O5 2.481(4) . ?
Th1 O6 2.485(4) . ?
Th1 O4 2.494(4) . ?
Th1 N1 2.552(5) . ?
Th1 N5 2.570(4) . ?
Pt1 C2 1.985(6) . ?
Pt1 C3 1.986(6) . ?
Pt1 C1 1.990(6) . ?
Pt1 C4 1.991(6) . ?
N1 C1 1.155(7) . ?
Pt2 C8 1.975(6) . ?
Pt2 C6 1.991(6) . ?
Pt2 C7 1.995(6) . ?
Pt2 C5 2.007(6) . ?
N2 C2 1.160(8) 8_655 ?
C2 N2 1.160(8) 8_665 ?
N3 C3 1.176(8) 3_646 ?
C3 N3 1.176(8) 3_656 ?
N4 C4 1.139(8) . ?
N5 C5 1.135(7) . ?
N6 C6 1.146(7) . ?
C7 N7 1.142(8) . ?
N8 C8 1.168(8) 3_656 ?
C8 N8 1.168(8) 3_646 ?
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
O7 Th1 O2 138.02(13) . . ?
O7 Th1 O1 138.15(13) . . ?
O2 Th1 O1 82.58(15) . . ?
O7 Th1 O3 72.68(13) . . ?
O2 Th1 O3 138.01(13) . . ?
O1 Th1 O3 80.77(13) . . ?
O7 Th1 O5 69.61(14) . . ?
O2 Th1 O5 70.74(14) . . ?
O1 Th1 O5 138.78(14) . . ?
O3 Th1 O5 139.48(14) . . ?
O7 Th1 O6 71.35(13) . . ?
O2 Th1 O6 83.43(13) . . ?
O1 Th1 O6 137.26(12) . . ?
O3 Th1 O6 83.24(13) . . ?
O5 Th1 O6 71.25(13) . . ?
O7 Th1 O4 70.93(13) . . ?
O2 Th1 O4 136.75(13) . . ?
O1 Th1 O4 70.01(13) . . ?
O3 Th1 O4 70.69(12) . . ?
O5 Th1 O4 109.29(13) . . ?
O6 Th1 O4 138.98(13) . . ?
O7 Th1 N1 101.46(15) . . ?
O2 Th1 N1 75.52(14) . . ?
O1 Th1 N1 75.52(14) . . ?
O3 Th1 N1 135.31(13) . . ?
O5 Th1 N1 67.86(14) . . ?
O6 Th1 N1 138.21(13) . . ?
O4 Th1 N1 65.79(13) . . ?
O7 Th1 N5 128.82(15) . . ?
O2 Th1 N5 67.17(13) . . ?
O1 Th1 N5 67.51(13) . . ?
O3 Th1 N5 70.85(13) . . ?
O5 Th1 N5 124.67(13) . . ?
O6 Th1 N5 69.82(13) . . ?
O4 Th1 N5 125.91(13) . . ?
N1 Th1 N5 129.71(15) . . ?
C2 Pt1 C3 90.4(2) . . ?
C2 Pt1 C1 92.6(2) . . ?
C3 Pt1 C1 176.8(2) . . ?
C2 Pt1 C4 177.0(2) . . ?
C3 Pt1 C4 89.8(2) . . ?
C1 Pt1 C4 87.2(2) . . ?
C1 N1 Th1 161.2(4) . . ?
N1 C1 Pt1 175.5(5) . . ?
C8 Pt2 C6 90.9(2) . . ?
C8 Pt2 C7 88.5(2) . . ?
C6 Pt2 C7 178.8(2) . . ?
C8 Pt2 C5 176.8(2) . . ?
C6 Pt2 C5 92.2(2) . . ?
C7 Pt2 C5 88.5(2) . . ?
N2 C2 Pt1 177.5(5) 8_665 . ?
N3 C3 Pt1 177.1(5) 3_656 . ?
N4 C4 Pt1 178.1(5) . . ?
C5 N5 Th1 170.1(4) . . ?
N5 C5 Pt2 176.4(5) . . ?
N6 C6 Pt2 179.5(6) . . ?
N7 C7 Pt2 177.6(5) . . ?
N8 C8 Pt2 177.1(5) 3_646 . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 28.27
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 2.154
_refine_diff_density_min -3.034
_refine_diff_density_rms 0.295
# Attachment '- Th2f.cif'
data_final
_database_code_depnum_ccdc_archive 'CCDC 769471'
#TrackingRef '- Th2f.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
;
C12 H22 N12 O12 Pt3 Th2, 5(H2O)
;
_chemical_formula_sum 'C12 H32 N12 O17 Pt3 Th2'
_chemical_formula_weight 1665.85
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Th Th -7.2400 8.8979 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'C 2/c'
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 16.4915(4)
_cell_length_b 12.1941(4)
_cell_length_c 19.5380(5)
_cell_angle_alpha 90.00
_cell_angle_beta 114.016(4)
_cell_angle_gamma 90.00
_cell_volume 3588.9(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 295(2)
_cell_measurement_reflns_used 19188
_cell_measurement_theta_min 3.3277
_cell_measurement_theta_max 30.5434
_exptl_crystal_description needle
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.03
_exptl_crystal_size_min 0.03
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 3.083
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2952
_exptl_absorpt_coefficient_mu 19.989
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.30
_exptl_absorpt_correction_T_max 1.0
_exptl_absorpt_process_details CrysAlis
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 295(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 'Oxford Xcalibur Eos'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 16.0514
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 32269
_diffrn_reflns_av_R_equivalents 0.0281
_diffrn_reflns_av_sigmaI/netI 0.0235
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 23
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -27
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 3.34
_diffrn_reflns_theta_max 30.61
_reflns_number_total 5166
_reflns_number_gt 4300
_reflns_threshold_expression >2\s(I)
_computing_data_collection 'CrysAlisPro Oxford Diffraction (2009)'
_computing_cell_refinement 'CrysAlisPro Oxford Diffraction (2009)'
_computing_data_reduction 'CrysAlisPro Oxford Diffraction (2009)'
_computing_structure_solution 'Sheldrick (2008)'
_computing_structure_refinement 'Sheldrick (2008)'
_computing_molecular_graphics 'Sheldrick (2008)'
_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^ > 2\s(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^)+(0.0110P)^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 constr
_refine_ls_extinction_method SHELXL
_refine_ls_extinction_coef 0.000167(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns 5166
_refine_ls_number_parameters 211
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0211
_refine_ls_R_factor_gt 0.0141
_refine_ls_wR_factor_ref 0.0244
_refine_ls_wR_factor_gt 0.0239
_refine_ls_goodness_of_fit_ref 0.918
_refine_ls_restrained_S_all 0.918
_refine_ls_shift/su_max 0.004
_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
Th1 Th 0.143944(6) 0.194976(7) 0.014912(5) 0.01512(3) Uani 1 1 d . . .
Pt1 Pt -0.083845(7) 0.271132(8) 0.166660(5) 0.01920(3) Uani 1 1 d . . .
Pt2 Pt 0.2500 -0.2500 0.0000 0.01855(3) Uani 1 2 d S . .
O1 O 0.29122(11) 0.16736(13) 0.03212(10) 0.0213(4) Uani 1 1 d . . .
H1A H 0.3224 0.1161 0.0599 0.032 Uiso 1 1 d . . .
O2 O 0.03267(12) 0.33467(17) -0.04699(12) 0.0386(5) Uani 1 1 d . . .
H2A H -0.0179 0.3287 -0.0455 0.058 Uiso 1 1 d . . .
H2B H 0.0404 0.3789 -0.0774 0.058 Uiso 1 1 d . . .
O3 O 0.21378(13) 0.11279(17) 0.14070(10) 0.0360(5) Uani 1 1 d . . .
H3A H 0.2634 0.1337 0.1739 0.054 Uiso 1 1 d . . .
H3B H 0.1864 0.0649 0.1548 0.054 Uiso 1 1 d . . .
O4 O 0.09783(13) 0.15406(15) -0.11926(10) 0.0318(5) Uani 1 1 d . . .
H4A H 0.1123 0.0964 -0.1361 0.048 Uiso 1 1 d . . .
H4B H 0.0686 0.1975 -0.1548 0.048 Uiso 1 1 d . . .
O5 O 0.19925(15) 0.34618(17) 0.10873(11) 0.0405(6) Uani 1 1 d . . .
H5A H 0.2123 0.4017 0.0890 0.061 Uiso 1 1 d . . .
H5B H 0.2032 0.3478 0.1535 0.061 Uiso 1 1 d . . .
O6 O -0.00403(12) 0.10049(16) -0.04121(10) 0.0312(5) Uani 1 1 d . . .
H6A H -0.0392 0.0931 -0.0870 0.047 Uiso 1 1 d . . .
H6B H -0.0316 0.1026 -0.0127 0.047 Uiso 1 1 d . . .
O7 O 0.0000 0.2667(3) -0.2500 0.0478(9) Uani 1 2 d S . .
H7 H -0.0404 0.3069 -0.2467 0.072 Uiso 1 1 d . . .
O8 O 0.12524(15) -0.0571(2) 0.17723(11) 0.0520(6) Uani 1 1 d . . .
H8A H 0.1693 -0.1006 0.1930 0.078 Uiso 1 1 d . . .
H8B H 0.1195 -0.0358 0.2164 0.078 Uiso 1 1 d . . .
O9 O -0.13706(15) 0.6087(2) 0.26897(12) 0.0506(6) Uani 1 1 d . . .
H9A H -0.1049 0.5514 0.2794 0.076 Uiso 1 1 d . . .
H9B H -0.1483 0.6254 0.3064 0.076 Uiso 1 1 d . . .
C1 C -0.00392(18) 0.2306(2) 0.11725(15) 0.0247(6) Uani 1 1 d . . .
C2 C -0.1040(2) 0.1152(2) 0.18375(15) 0.0296(6) Uani 1 1 d . . .
C3 C -0.16089(19) 0.3159(2) 0.21756(15) 0.0276(6) Uani 1 1 d . . .
C4 C -0.07055(19) 0.4284(2) 0.14631(15) 0.0296(6) Uani 1 1 d . . .
C5 C 0.19848(17) -0.1034(2) 0.00463(14) 0.0220(6) Uani 1 1 d . . .
C6 C 0.18546(18) -0.3191(2) 0.05501(17) 0.0315(7) Uani 1 1 d . . .
N1 N 0.04293(15) 0.2110(2) 0.08882(13) 0.0301(5) Uani 1 1 d . . .
N2 N -0.1182(2) 0.0261(2) 0.19274(16) 0.0532(8) Uani 1 1 d . . .
N3 N -0.20279(19) 0.3433(2) 0.24856(15) 0.0473(8) Uani 1 1 d . . .
N4 N -0.0661(2) 0.5176(2) 0.13292(16) 0.0489(8) Uani 1 1 d . . .
N5 N 0.16941(15) -0.01806(18) 0.00513(12) 0.0266(5) Uani 1 1 d . . .
N6 N 0.14904(19) -0.3589(3) 0.08727(17) 0.0626(10) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Th1 0.01516(4) 0.01525(5) 0.01834(5) 0.00111(4) 0.01028(3) 0.00092(3)
Pt1 0.02093(5) 0.02114(5) 0.01920(5) 0.00114(4) 0.01194(4) 0.00176(4)
Pt2 0.01646(7) 0.01598(7) 0.02386(8) -0.00046(5) 0.00887(6) 0.00217(5)
O1 0.0186(9) 0.0168(9) 0.0328(10) 0.0090(7) 0.0149(8) 0.0054(7)
O2 0.0238(11) 0.0382(12) 0.0606(14) 0.0261(10) 0.0240(10) 0.0109(9)
O3 0.0319(12) 0.0484(13) 0.0245(11) 0.0099(9) 0.0083(9) -0.0020(10)
O4 0.0435(13) 0.0289(11) 0.0227(10) 0.0002(8) 0.0133(10) 0.0049(9)
O5 0.0613(15) 0.0389(13) 0.0335(12) -0.0151(9) 0.0318(11) -0.0234(11)
O6 0.0231(10) 0.0430(12) 0.0294(11) -0.0025(9) 0.0128(9) -0.0089(9)
O7 0.061(2) 0.0419(19) 0.0387(19) 0.000 0.0180(17) 0.000
O8 0.0412(14) 0.0795(18) 0.0322(13) -0.0049(12) 0.0117(11) 0.0090(13)
O9 0.0450(15) 0.0656(17) 0.0359(13) -0.0036(12) 0.0110(11) 0.0056(12)
C1 0.0232(14) 0.0281(15) 0.0231(14) -0.0007(11) 0.0097(12) -0.0016(11)
C2 0.0389(18) 0.0301(17) 0.0268(15) -0.0025(12) 0.0204(14) 0.0037(13)
C3 0.0334(16) 0.0274(16) 0.0269(14) 0.0063(12) 0.0174(13) 0.0060(12)
C4 0.0291(16) 0.0344(18) 0.0283(15) 0.0027(13) 0.0147(13) 0.0006(13)
C5 0.0171(13) 0.0230(14) 0.0248(14) -0.0005(11) 0.0073(11) -0.0022(11)
C6 0.0216(14) 0.0363(18) 0.0373(17) 0.0065(14) 0.0125(13) 0.0035(12)
N1 0.0267(12) 0.0411(15) 0.0293(13) -0.0030(11) 0.0183(11) -0.0014(11)
N2 0.090(2) 0.0276(16) 0.0550(19) -0.0009(13) 0.0424(18) -0.0019(15)
N3 0.0573(19) 0.0547(19) 0.0445(17) 0.0105(14) 0.0358(15) 0.0228(15)
N4 0.0574(19) 0.0314(16) 0.0595(19) 0.0136(14) 0.0254(16) 0.0000(14)
N5 0.0262(13) 0.0195(12) 0.0328(14) -0.0019(10) 0.0108(11) 0.0020(10)
N6 0.0348(17) 0.097(3) 0.064(2) 0.0306(19) 0.0284(16) 0.0056(16)
_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
Th1 O1 2.3369(17) . ?
Th1 O1 2.3675(17) 7 ?
Th1 O2 2.4342(18) . ?
Th1 O3 2.4631(18) . ?
Th1 O4 2.4650(18) . ?
Th1 O5 2.4962(19) . ?
Th1 O6 2.5113(18) . ?
Th1 N1 2.619(2) . ?
Th1 N5 2.651(2) . ?
Th1 Th1 4.0045(2) 7 ?
Pt1 C2 1.982(3) . ?
Pt1 C3 1.982(3) . ?
Pt1 C1 1.987(3) . ?
Pt1 C4 1.988(3) . ?
Pt2 C6 1.982(3) 7_545 ?
Pt2 C6 1.982(3) . ?
Pt2 C5 1.997(3) 7_545 ?
Pt2 C5 1.997(3) . ?
O1 Th1 2.3675(17) 7 ?
O1 H1A 0.8501 . ?
O2 H2A 0.8500 . ?
O2 H2B 0.8499 . ?
O3 H3A 0.8500 . ?
O3 H3B 0.8501 . ?
O4 H4A 0.8500 . ?
O4 H4B 0.8500 . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8500 . ?
O6 H6A 0.8500 . ?
O6 H6B 0.8501 . ?
O7 H7 0.8501 . ?
O8 H8A 0.8499 . ?
O8 H8B 0.8500 . ?
O9 H9A 0.8500 . ?
O9 H9B 0.8500 . ?
C1 N1 1.145(3) . ?
C2 N2 1.140(4) . ?
C3 N3 1.139(4) . ?
C4 N4 1.129(4) . ?
C5 N5 1.147(3) . ?
C6 N6 1.141(4) . ?
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 Th1 O1 63.31(7) . 7 ?
O1 Th1 O2 134.55(6) . . ?
O1 Th1 O2 71.29(6) 7 . ?
O1 Th1 O3 76.19(6) . . ?
O1 Th1 O3 125.04(6) 7 . ?
O2 Th1 O3 137.08(7) . . ?
O1 Th1 O4 88.66(7) . . ?
O1 Th1 O4 73.94(6) 7 . ?
O2 Th1 O4 76.67(7) . . ?
O3 Th1 O4 142.68(7) . . ?
O1 Th1 O5 87.31(7) . . ?
O1 Th1 O5 70.95(6) 7 . ?
O2 Th1 O5 79.88(8) . . ?
O3 Th1 O5 71.65(7) . . ?
O4 Th1 O5 142.45(6) . . ?
O1 Th1 O6 139.91(6) . . ?
O1 Th1 O6 131.91(6) 7 . ?
O2 Th1 O6 72.66(7) . . ?
O3 Th1 O6 103.04(6) . . ?
O4 Th1 O6 67.57(6) . . ?
O5 Th1 O6 131.24(7) . . ?
O1 Th1 N1 142.06(7) . . ?
O1 Th1 N1 130.56(7) 7 . ?
O2 Th1 N1 72.63(7) . . ?
O3 Th1 N1 67.93(7) . . ?
O4 Th1 N1 127.69(7) . . ?
O5 Th1 N1 70.37(7) . . ?
O6 Th1 N1 63.37(7) . . ?
O1 Th1 N5 71.54(6) . . ?
O1 Th1 N5 123.85(7) 7 . ?
O2 Th1 N5 139.42(7) . . ?
O3 Th1 N5 69.49(7) . . ?
O4 Th1 N5 73.40(6) . . ?
O5 Th1 N5 139.08(7) . . ?
O6 Th1 N5 70.93(7) . . ?
N1 Th1 N5 105.55(7) . . ?
O1 Th1 Th1 31.89(4) . 7 ?
O1 Th1 Th1 31.43(4) 7 7 ?
O2 Th1 Th1 102.69(5) . 7 ?
O3 Th1 Th1 101.54(5) . 7 ?
O4 Th1 Th1 79.79(5) . 7 ?
O5 Th1 Th1 77.27(5) . 7 ?
O6 Th1 Th1 147.28(4) . 7 ?
N1 Th1 Th1 147.64(5) . 7 ?
N5 Th1 Th1 98.31(5) . 7 ?
C2 Pt1 C3 89.65(11) . . ?
C2 Pt1 C1 91.90(11) . . ?
C3 Pt1 C1 178.04(11) . . ?
C2 Pt1 C4 176.96(12) . . ?
C3 Pt1 C4 88.88(12) . . ?
C1 Pt1 C4 89.63(11) . . ?
C6 Pt2 C6 180.00(19) 7_545 . ?
C6 Pt2 C5 91.37(11) 7_545 7_545 ?
C6 Pt2 C5 88.63(11) . 7_545 ?
C6 Pt2 C5 88.63(11) 7_545 . ?
C6 Pt2 C5 91.37(11) . . ?
C5 Pt2 C5 180.00(15) 7_545 . ?
Th1 O1 Th1 116.69(7) . 7 ?
Th1 O1 H1A 121.4 . . ?
Th1 O1 H1A 121.1 7 . ?
Th1 O2 H2A 118.3 . . ?
Th1 O2 H2B 119.7 . . ?
H2A O2 H2B 120.5 . . ?
Th1 O3 H3A 123.6 . . ?
Th1 O3 H3B 120.5 . . ?
H3A O3 H3B 115.6 . . ?
Th1 O4 H4A 124.4 . . ?
Th1 O4 H4B 124.7 . . ?
H4A O4 H4B 110.7 . . ?
Th1 O5 H5A 109.8 . . ?
Th1 O5 H5B 128.6 . . ?
H5A O5 H5B 121.4 . . ?
Th1 O6 H6A 129.4 . . ?
Th1 O6 H6B 112.5 . . ?
H6A O6 H6B 112.0 . . ?
H8A O8 H8B 104.9 . . ?
H9A O9 H9B 108.9 . . ?
N1 C1 Pt1 177.6(3) . . ?
N2 C2 Pt1 177.9(3) . . ?
N3 C3 Pt1 177.7(3) . . ?
N4 C4 Pt1 177.5(3) . . ?
N5 C5 Pt2 177.6(3) . . ?
N6 C6 Pt2 179.4(3) . . ?
C1 N1 Th1 171.5(2) . . ?
C5 N5 Th1 165.5(2) . . ?
_diffrn_measured_fraction_theta_max 0.933
_diffrn_reflns_theta_full 29.00
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max 0.652
_refine_diff_density_min -0.703
_refine_diff_density_rms 0.126
data_3
_database_code_depnum_ccdc_archive 'CCDC 769472'
#TrackingRef '- U3.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety
;
4(C8 N8 O5 Pt2 U2), N2 O6, 2(O), 8(O0.13), 6(k)
;
_chemical_formula_sum 'C16 H5 K3 N17 O14.50 Pt4 U4'
_chemical_formula_weight 2517.15
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Tetragonal
_symmetry_space_group_name_H-M 'P 4/m b m'
_symmetry_space_group_name_Hall '-P 4 2ab'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'y+1/2, x+1/2, -z'
'-y+1/2, -x+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-y-1/2, -x-1/2, z'
'y-1/2, x-1/2, z'
_cell_length_a 22.1073(2)
_cell_length_b 22.1073(2)
_cell_length_c 12.6202(2)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 6167.90(13)
_cell_formula_units_Z 4
_cell_measurement_temperature 290(2)
_cell_measurement_reflns_used 12069
_cell_measurement_theta_min 2.9093
_cell_measurement_theta_max 30.9579
_exptl_crystal_description prism
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.344
_exptl_crystal_size_mid 0.174
_exptl_crystal_size_min 0.096
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.711
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 4292
_exptl_absorpt_coefficient_mu 19.750
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.31193
_exptl_absorpt_correction_T_max 1.00
_exptl_absorpt_process_details CrysAlis
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 290(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 'Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 16.0514
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 26733
_diffrn_reflns_av_R_equivalents 0.0564
_diffrn_reflns_av_sigmaI/netI 0.0347
_diffrn_reflns_limit_h_min -27
_diffrn_reflns_limit_h_max 27
_diffrn_reflns_limit_k_min -25
_diffrn_reflns_limit_k_max 26
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_theta_min 2.91
_diffrn_reflns_theta_max 26.37
_reflns_number_total 3423
_reflns_number_gt 2702
_reflns_threshold_expression >2sigma(I)
_computing_data_collection ?
_computing_cell_refinement ?
_computing_data_reduction ?
_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. Due to the large channels
in the open-framework structure, there are solvent accessible voids in the
structure.The total number of restraints was 55. The DELU command was used
on all atom types to improve the thermal ellipsoid parameters. The DFIX
command was applied to the N-O bond lengths in the nitrate anion. The minimum
high residual electron density is associated with the heavy atoms, Pt and U.
;
_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^)+(0.0906P)^2^+166.2893P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens none
_refine_ls_hydrogen_treatment none
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3423
_refine_ls_number_parameters 146
_refine_ls_number_restraints 55
_refine_ls_R_factor_all 0.0687
_refine_ls_R_factor_gt 0.0522
_refine_ls_wR_factor_ref 0.1562
_refine_ls_wR_factor_gt 0.1500
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_restrained_S_all 1.056
_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
K1 K 0.0607(3) 0.5607(3) 0.0000 0.051(2) Uani 1 4 d SU . .
K2 K 0.3616(7) 0.3695(7) -0.5000 0.152 Uiso 1 2 d S . .
U1 U 0.23789(3) 0.50724(2) -0.17133(4) 0.01857(19) Uani 1 1 d U . .
Pt1 Pt 0.14640(4) 0.64640(4) -0.5000 0.0216(3) Uani 1 4 d SU . .
Pt2 Pt 0.12336(4) 0.37664(4) -0.5000 0.0217(3) Uani 1 4 d SU . .
Pt3 Pt 0.24316(2) 0.25684(2) -0.12763(6) 0.0149(2) Uani 1 2 d SU . .
C1 C 0.1902(7) 0.6004(6) -0.3904(11) 0.022(3) Uani 1 1 d U . .
C2 C 0.1676(8) 0.4216(7) -0.3896(12) 0.026(3) Uani 1 1 d U . .
C3 C 0.2423(7) 0.3463(7) -0.1306(12) 0.024(3) Uani 1 1 d U . .
C4 C 0.3325(6) 0.2575(7) -0.1294(11) 0.020(3) Uani 1 1 d U . .
N1 N 0.2118(7) 0.5718(6) -0.3255(11) 0.039(3) Uani 1 1 d U . .
N2 N 0.1938(7) 0.4471(7) -0.3235(11) 0.039(3) Uani 1 1 d U . .
N3 N 0.2409(7) 0.3985(6) -0.1344(11) 0.039(3) Uani 1 1 d U . .
N4 N 0.2579(7) 0.6157(6) -0.1344(11) 0.038(3) Uani 1 1 d U . .
N5 N 0.0000 0.5000 -0.266(2) 0.074(11) Uani 1 4 d SDU . .
O1 O 0.1634(5) 0.5159(5) -0.1214(9) 0.036(2) Uani 1 1 d U . .
O2 O 0.3103(5) 0.5001(5) -0.2198(9) 0.033(2) Uani 1 1 d U . .
O3 O 0.2746(8) 0.5044(7) 0.0000 0.029(3) Uani 1 2 d SU . .
O4 O 0.0000 0.5000 -0.1682(19) 0.055(5) Uani 1 4 d SDU . .
O5 O 0.0326(12) 0.5326(12) -0.327(3) 0.21(2) Uani 1 2 d SDU . .
O6 O 0.0728(10) 0.4272(10) 0.0000 0.063(6) Uani 1 4 d SU . .
O7 O 0.0000 0.0000 0.5000 0.056(12) Uani 1 8 d S . .
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
K1 0.050(3) 0.050(3) 0.053(5) 0.000 0.000 0.005(4)
U1 0.0267(3) 0.0112(3) 0.0178(3) -0.00015(19) -0.0016(2) -0.0008(2)
Pt1 0.0253(4) 0.0253(4) 0.0142(5) 0.000 0.000 0.0049(5)
Pt2 0.0251(4) 0.0251(4) 0.0148(5) 0.000 0.000 -0.0080(5)
Pt3 0.0108(3) 0.0108(3) 0.0233(4) -0.0001(2) 0.0001(2) -0.0002(3)
C1 0.036(9) 0.013(7) 0.017(6) -0.005(5) 0.000(6) -0.001(6)
C2 0.036(9) 0.022(8) 0.021(7) 0.004(6) 0.002(6) -0.012(7)
C3 0.024(8) 0.016(5) 0.033(8) -0.008(6) 0.001(7) 0.002(6)
C4 0.009(6) 0.027(8) 0.024(7) 0.004(6) -0.005(5) -0.001(5)
N1 0.055(10) 0.029(7) 0.033(6) 0.009(5) -0.012(6) 0.000(7)
N2 0.053(9) 0.032(7) 0.030(6) -0.002(5) -0.011(6) -0.013(7)
N3 0.058(10) 0.020(4) 0.039(7) 0.002(5) -0.010(7) 0.002(5)
N4 0.055(10) 0.022(5) 0.036(7) 0.002(5) -0.008(7) -0.008(6)
N5 0.086(17) 0.086(17) 0.048(10) 0.000 0.000 0.02(2)
O1 0.031(5) 0.037(6) 0.041(6) -0.004(5) 0.001(4) 0.000(4)
O2 0.034(5) 0.031(6) 0.035(5) 0.001(5) 0.001(4) 0.000(4)
O3 0.036(8) 0.029(8) 0.022(5) 0.000 0.000 -0.003(7)
O4 0.061(8) 0.061(8) 0.045(10) 0.000 0.000 -0.008(12)
O5 0.24(3) 0.24(3) 0.14(3) 0.10(2) 0.10(2) 0.02(4)
O6 0.054(8) 0.054(8) 0.083(18) 0.000 0.000 -0.016(10)
O7 0.072(19) 0.072(19) 0.022(17) 0.000 0.000 0.000
_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
K1 O4 2.848(19) . ?
K1 O4 2.848(19) 9_565 ?
K1 O1 2.912(12) 10 ?
K1 O1 2.912(12) 7_455 ?
K1 O1 2.912(12) . ?
K1 O1 2.912(12) 16_565 ?
K1 O6 2.96(3) 9_565 ?
K1 O6 2.96(3) . ?
K1 K1 3.80(2) 9_565 ?
U1 O2 1.720(12) . ?
U1 O1 1.774(12) . ?
U1 O3 2.310(6) . ?
U1 N3 2.449(14) . ?
U1 N1 2.482(13) . ?
U1 N4 2.483(14) . ?
U1 N2 2.531(14) . ?
Pt1 C1 1.971(15) 7_454 ?
Pt1 C1 1.971(15) 16_565 ?
Pt1 C1 1.971(15) . ?
Pt1 C1 1.971(15) 10_554 ?
Pt2 C2 1.971(15) 8_554 ?
Pt2 C2 1.971(15) . ?
Pt2 C2 1.971(15) 15_665 ?
Pt2 C2 1.971(15) 10_554 ?
Pt3 C4 1.975(14) . ?
Pt3 C4 1.975(14) 15_665 ?
Pt3 C3 1.978(15) . ?
Pt3 C3 1.978(15) 15_665 ?
Pt3 Pt3 3.2214(15) 10 ?
C1 N1 1.139(19) . ?
C2 N2 1.16(2) . ?
C3 N3 1.16(2) . ?
C4 N4 1.15(2) 3_655 ?
N4 C4 1.15(2) 4_565 ?
N5 O4 1.238(18) . ?
N5 O5 1.279(18) 2_565 ?
N5 O5 1.279(18) . ?
O3 U1 2.310(6) 10 ?
O4 K1 2.848(19) 9_565 ?
O6 K1 2.96(3) 9_565 ?
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
O4 K1 O4 96.4(7) . 9_565 ?
O4 K1 O1 126.8(3) . 10 ?
O4 K1 O1 79.3(3) 9_565 10 ?
O4 K1 O1 126.8(3) . 7_455 ?
O4 K1 O1 79.3(3) 9_565 7_455 ?
O1 K1 O1 104.7(5) 10 7_455 ?
O4 K1 O1 79.3(3) . . ?
O4 K1 O1 126.8(3) 9_565 . ?
O1 K1 O1 63.5(5) 10 . ?
O1 K1 O1 143.8(6) 7_455 . ?
O4 K1 O1 79.3(3) . 16_565 ?
O4 K1 O1 126.8(3) 9_565 16_565 ?
O1 K1 O1 143.8(6) 10 16_565 ?
O1 K1 O1 63.5(5) 7_455 16_565 ?
O1 K1 O1 104.7(5) . 16_565 ?
O4 K1 O6 64.7(3) . 9_565 ?
O4 K1 O6 64.7(3) 9_565 9_565 ?
O1 K1 O6 143.8(3) 10 9_565 ?
O1 K1 O6 65.9(4) 7_455 9_565 ?
O1 K1 O6 143.8(3) . 9_565 ?
O1 K1 O6 65.9(4) 16_565 9_565 ?
O4 K1 O6 64.7(3) . . ?
O4 K1 O6 64.7(3) 9_565 . ?
O1 K1 O6 65.9(4) 10 . ?
O1 K1 O6 143.8(3) 7_455 . ?
O1 K1 O6 65.9(4) . . ?
O1 K1 O6 143.8(3) 16_565 . ?
O6 K1 O6 100.3(9) 9_565 . ?
O4 K1 K1 48.2(4) . 9_565 ?
O4 K1 K1 48.2(4) 9_565 9_565 ?
O1 K1 K1 108.1(3) 10 9_565 ?
O1 K1 K1 108.1(3) 7_455 9_565 ?
O1 K1 K1 108.1(3) . 9_565 ?
O1 K1 K1 108.1(3) 16_565 9_565 ?
O6 K1 K1 50.1(4) 9_565 9_565 ?
O6 K1 K1 50.1(4) . 9_565 ?
O2 U1 O1 179.1(5) . . ?
O2 U1 O3 90.2(5) . . ?
O1 U1 O3 89.8(5) . . ?
O2 U1 N3 87.3(5) . . ?
O1 U1 N3 93.7(5) . . ?
O3 U1 N3 77.6(5) . . ?
O2 U1 N1 89.4(5) . . ?
O1 U1 N1 90.0(5) . . ?
O3 U1 N1 146.2(5) . . ?
N3 U1 N1 136.1(5) . . ?
O2 U1 N4 89.4(5) . . ?
O1 U1 N4 89.7(5) . . ?
O3 U1 N4 77.8(5) . . ?
N3 U1 N4 155.1(5) . . ?
N1 U1 N4 68.5(5) . . ?
O2 U1 N2 92.3(5) . . ?
O1 U1 N2 88.2(5) . . ?
O3 U1 N2 146.2(5) . . ?
N3 U1 N2 68.9(5) . . ?
N1 U1 N2 67.5(5) . . ?
N4 U1 N2 135.9(5) . . ?
C1 Pt1 C1 89.1(8) 7_454 16_565 ?
C1 Pt1 C1 178.0(9) 7_454 . ?
C1 Pt1 C1 90.8(8) 16_565 . ?
C1 Pt1 C1 90.8(8) 7_454 10_554 ?
C1 Pt1 C1 178.0(9) 16_565 10_554 ?
C1 Pt1 C1 89.1(8) . 10_554 ?
C2 Pt2 C2 179.3(10) 8_554 . ?
C2 Pt2 C2 90.0(8) 8_554 15_665 ?
C2 Pt2 C2 90.0(8) . 15_665 ?
C2 Pt2 C2 90.0(8) 8_554 10_554 ?
C2 Pt2 C2 90.0(8) . 10_554 ?
C2 Pt2 C2 179.3(10) 15_665 10_554 ?
C4 Pt3 C4 90.8(9) . 15_665 ?
C4 Pt3 C3 90.1(6) . . ?
C4 Pt3 C3 178.0(6) 15_665 . ?
C4 Pt3 C3 178.0(6) . 15_665 ?
C4 Pt3 C3 90.1(6) 15_665 15_665 ?
C3 Pt3 C3 88.9(9) . 15_665 ?
C4 Pt3 Pt3 90.6(4) . 10 ?
C4 Pt3 Pt3 90.6(4) 15_665 10 ?
C3 Pt3 Pt3 91.1(4) . 10 ?
C3 Pt3 Pt3 91.1(4) 15_665 10 ?
N1 C1 Pt1 175.3(15) . . ?
N2 C2 Pt2 178.8(15) . . ?
N3 C3 Pt3 178.3(15) . . ?
N4 C4 Pt3 177.5(13) 3_655 . ?
C1 N1 U1 168.5(15) . . ?
C2 N2 U1 172.8(15) . . ?
C3 N3 U1 171.4(13) . . ?
C4 N4 U1 166.7(13) 4_565 . ?
O4 N5 O5 127(2) . 2_565 ?
O4 N5 O5 127(2) . . ?
O5 N5 O5 106(5) 2_565 . ?
U1 O1 K1 161.3(6) . . ?
U1 O3 U1 138.7(8) . 10 ?
N5 O4 K1 138.2(4) . . ?
N5 O4 K1 138.2(4) . 9_565 ?
K1 O4 K1 83.6(7) . 9_565 ?
K1 O6 K1 79.7(9) . 9_565 ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 26.37
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 4.241
_refine_diff_density_min -9.542
_refine_diff_density_rms 0.423