# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012
data_global
_journal_coden_Cambridge 222
loop_
_publ_author_name
'Pan, Baofei'
'Bezpalko, Mark'
'Foxman, Bruce'
'Thomas, Christine'
_publ_contact_author_name 'Thomas, Christine'
_publ_contact_author_email thomasc@brandeis.edu
_publ_section_title
;
Heterolytic Activation of E-H Bonds Across Pt-P Bonds
in Pt NHP (N-heterocyclic Phosphenium/Phosphido) Complexes
;
# Attachment '- combined_bf.cif'
data_4
_database_code_depnum_ccdc_archive 'CCDC 869435'
#TrackingRef '- combined_bf.cif'
_audit_creation_date 11-10-05
_audit_creation_method CRYSTALS_ver_14.30
_oxford_structure_analysis_title 'bfpan_614_0ma in P2(1)/c'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 14.8742(10)
_cell_length_b 35.625(3)
_cell_length_c 11.9635(9)
_cell_angle_alpha 90
_cell_angle_beta 107.599(4)
_cell_angle_gamma 90
_cell_volume 6042.7(8)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'P 1 21/c 1 '
_symmetry_space_group_name_Hall '-P 2ybc '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x,y+1/2,-z+1/2
x,-y+1/2,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103
11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C64 H57 Cl4 F6 N2 O1 P5 Pt1
# Dc = 1.62 Fooo = 2952.00 Mu = 26.95 M = 1475.93
# Found Formula = C64 H57 Cl4 F6 N2 O1 P5 Pt1
# Dc = 1.62 FOOO = 2952.00 Mu = 26.95 M = 1475.93
_chemical_formula_sum 'C64 H57 Cl4 F6 N2 O1 P5 Pt1'
_chemical_formula_moiety 'C62 H53 N2 O P4 Pt, F6 P,2(C H2 Cl2)'
_chemical_compound_source ?
_chemical_formula_weight 1475.93
_cell_measurement_reflns_used 9788
_cell_measurement_theta_min 2
_cell_measurement_theta_max 30
_cell_measurement_temperature 120
_exptl_crystal_description 'plate fragment'
_exptl_crystal_colour 'light yellow'
_exptl_crystal_size_min 0.064
_exptl_crystal_size_mid 0.140
_exptl_crystal_size_max 0.750
_exptl_crystal_density_diffrn 1.622
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 2952
_exptl_absorpt_coefficient_mu 2.695
# Sheldrick geometric approximatio 0.69 0.84
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_absorpt_correction_T_min 0.69
_exptl_absorpt_correction_T_max 0.84
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 120
_diffrn_reflns_number 86823
_reflns_number_total 17579
_diffrn_reflns_av_R_equivalents 0.048
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 17579
# Theoretical number of reflections is about 35504
_diffrn_reflns_theta_min 1.436
_diffrn_reflns_theta_max 30.079
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full 29.477
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min -20
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_k_min -50
_diffrn_reflns_limit_k_max 50
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_limit_l_max 16
_reflns_limit_h_min -20
_reflns_limit_h_max 19
_reflns_limit_k_min 0
_reflns_limit_k_max 50
_reflns_limit_l_min 0
_reflns_limit_l_max 16
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -2.76
_refine_diff_density_max 1.59
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns 17579
_refine_ls_number_restraints 6
_refine_ls_number_parameters 743
_oxford_refine_ls_R_factor_ref 0.0550
_refine_ls_wR_factor_ref 0.1067
_refine_ls_goodness_of_fit_ref 0.9711
_refine_ls_shift/su_max 0.0041448
_refine_ls_shift/su_mean 0.0000778
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 17579
_refine_ls_R_factor_all 0.0550
_refine_ls_wR_factor_all 0.1067
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 14355
_refine_ls_R_factor_gt 0.0418
_refine_ls_wR_factor_gt 0.1021
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.05P)^2^ +28.72P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014.
Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Pt1 Pt 0.300430(9) 0.400414(4) -0.006385(11) 0.0116 1.0000 Uani . . . . . .
Cl1 Cl -0.1779(2) 0.27365(10) -0.2481(3) 0.1135 1.0000 Uani . U . . . .
Cl2 Cl -0.2230(2) 0.29523(9) -0.0342(3) 0.1064 1.0000 Uani . . . . . .
Cl3 Cl 0.6786(3) 0.36651(7) 0.7295(2) 0.1123 1.0000 Uani . . . . . .
Cl4 Cl 0.59619(17) 0.31908(7) 0.5362(2) 0.0907 1.0000 Uani . . . . . .
P1 P -0.13112(10) 0.36750(4) -0.59037(13) 0.0353 1.0000 Uani . . . . . .
P2 P 0.19384(7) 0.35472(3) -0.07349(8) 0.0131 1.0000 Uani . . . . . .
P3 P 0.36122(7) 0.39028(3) -0.16140(8) 0.0142 1.0000 Uani . . . . . .
P4 P 0.39693(7) 0.37382(3) 0.16945(8) 0.0132 1.0000 Uani . . . . . .
P5 P 0.18096(6) 0.44129(3) -0.00483(8) 0.0128 1.0000 Uani . . . . . .
F10 F -0.2389(5) 0.3620(2) -0.6051(7) 0.066(2) 0.588(7) Uiso . . P 1 1 .
F11 F -0.2334(8) 0.3840(4) -0.6095(9) 0.063(3) 0.412(7) Uiso . . P 1 2 .
F20 F -0.1281(8) 0.4026(3) -0.5146(11) 0.112(4) 0.588(7) Uiso . . P 1 1 .
F21 F -0.1174(10) 0.3801(4) -0.4577(13) 0.097(4) 0.412(7) Uiso . . P 1 2 .
F30 F -0.1065(5) 0.34262(19) -0.4755(6) 0.0564(19) 0.588(7) Uiso . . P 1 1 .
F31 F -0.1818(9) 0.3293(4) -0.5660(12) 0.090(4) 0.412(7) Uiso . . P 1 2 .
F40 F -0.1334(5) 0.3315(2) -0.6680(7) 0.069(2) 0.588(7) Uiso . . P 1 1 .
F41 F -0.1506(10) 0.3553(4) -0.7202(13) 0.096(4) 0.412(7) Uiso . . P 1 2 .
F50 F -0.1591(6) 0.3905(3) -0.7091(8) 0.082(3) 0.588(7) Uiso . . P 1 1 .
F51 F -0.0884(8) 0.4052(3) -0.6154(10) 0.073(3) 0.412(7) Uiso . . P 1 2 .
F60 F -0.0220(9) 0.3727(4) -0.5769(11) 0.124(4) 0.588(7) Uiso . . P 1 1 .
F61 F -0.0256(8) 0.3507(3) -0.5553(9) 0.064(3) 0.412(7) Uiso . . P 1 2 .
O1 O 0.2029(2) 0.32130(8) 0.0217(2) 0.0187 1.0000 Uani . . . . . .
N1 N 0.0816(2) 0.36889(9) -0.1213(3) 0.0173 1.0000 Uani . . . . . .
N2 N 0.1888(2) 0.33568(9) -0.2014(3) 0.0167 1.0000 Uani . . . . . .
C1 C 0.2119(3) 0.47882(10) 0.1037(3) 0.0141 1.0000 Uani . . . . . .
C2 C 0.1592(3) 0.51208(11) 0.0891(3) 0.0178 1.0000 Uani . . . . . .
C3 C 0.1849(3) 0.54029(11) 0.1716(4) 0.0207 1.0000 Uani . . . . . .
C4 C 0.2619(3) 0.53582(12) 0.2712(4) 0.0225 1.0000 Uani . . . . . .
C5 C 0.3146(3) 0.50325(12) 0.2859(4) 0.0237 1.0000 Uani . . . . . .
C6 C 0.2903(3) 0.47483(11) 0.2031(3) 0.0178 1.0000 Uani . . . . . .
C7 C 0.1319(3) 0.46802(10) -0.1394(3) 0.0158 1.0000 Uani . . . . . .
C8 C 0.0397(3) 0.46423(12) -0.2109(4) 0.0214 1.0000 Uani . . . . . .
C9 C 0.0061(3) 0.48565(14) -0.3125(4) 0.0267 1.0000 Uani . . . . . .
C10 C 0.0647(3) 0.51179(13) -0.3412(4) 0.0257 1.0000 Uani . . . . . .
C11 C 0.1571(3) 0.51562(12) -0.2707(4) 0.0224 1.0000 Uani . . . . . .
C12 C 0.1911(3) 0.49370(11) -0.1710(3) 0.0201 1.0000 Uani . . . . . .
C13 C 0.0791(3) 0.41834(10) 0.0205(3) 0.0156 1.0000 Uani . . . . . .
C14 C 0.0399(3) 0.43225(11) 0.1058(4) 0.0198 1.0000 Uani . . . . . .
C15 C -0.0373(3) 0.41517(13) 0.1252(4) 0.0251 1.0000 Uani . . . . . .
C16 C -0.0786(3) 0.38437(12) 0.0589(4) 0.0253 1.0000 Uani . . . . . .
C17 C -0.0410(3) 0.36978(12) -0.0247(4) 0.0223 1.0000 Uani . . . . . .
C18 C 0.0396(3) 0.38566(11) -0.0415(3) 0.0165 1.0000 Uani . . . . . .
C19 C 0.0256(3) 0.34619(14) -0.2212(4) 0.0266 1.0000 Uani . . . . . .
C20 C 0.0941(3) 0.33488(14) -0.2873(4) 0.0269 1.0000 Uani . . . . . .
C21 C 0.2686(3) 0.32088(11) -0.2299(3) 0.0167 1.0000 Uani . . . . . .
C22 C 0.2617(3) 0.28480(12) -0.2759(4) 0.0217 1.0000 Uani . . . . . .
C23 C 0.3363(3) 0.26879(12) -0.3065(4) 0.0241 1.0000 Uani . . . . . .
C24 C 0.4179(3) 0.28927(12) -0.2928(4) 0.0262 1.0000 Uani . . . . . .
C25 C 0.4247(3) 0.32557(12) -0.2495(4) 0.0227 1.0000 Uani . . . . . .
C26 C 0.3517(3) 0.34174(11) -0.2150(3) 0.0160 1.0000 Uani . . . . . .
C27 C 0.3080(3) 0.41437(11) -0.3000(3) 0.0186 1.0000 Uani . . . . . .
C28 C 0.2115(3) 0.42035(12) -0.3348(4) 0.0230 1.0000 Uani . . . . . .
C29 C 0.1654(4) 0.43485(14) -0.4456(4) 0.0307 1.0000 Uani . . . . . .
C30 C 0.2168(4) 0.44461(14) -0.5200(4) 0.0332 1.0000 Uani . . . . . .
C31 C 0.3129(4) 0.43877(14) -0.4861(4) 0.0306 1.0000 Uani . . . . . .
C32 C 0.3589(3) 0.42321(12) -0.3780(4) 0.0244 1.0000 Uani . . . . . .
C33 C 0.4858(3) 0.40301(11) -0.1153(3) 0.0174 1.0000 Uani . . . . . .
C34 C 0.5093(3) 0.44094(12) -0.1219(4) 0.0230 1.0000 Uani . . . . . .
C35 C 0.6002(3) 0.45337(13) -0.0676(4) 0.0284 1.0000 Uani . . . . . .
C36 C 0.6693(3) 0.42843(14) -0.0044(4) 0.0278 1.0000 Uani . . . . . .
C37 C 0.6457(3) 0.39089(13) 0.0029(4) 0.0263 1.0000 Uani . . . . . .
C38 C 0.5548(3) 0.37851(12) -0.0516(4) 0.0209 1.0000 Uani . . . . . .
C39 C 0.4752(3) 0.33616(11) 0.1516(3) 0.0169 1.0000 Uani . . . . . .
C40 C 0.5710(3) 0.33606(13) 0.2113(4) 0.0267 1.0000 Uani . . . . . .
C41 C 0.6296(3) 0.30860(14) 0.1876(5) 0.0385 1.0000 Uani . . . . . .
C42 C 0.5928(3) 0.28169(13) 0.1027(5) 0.0344 1.0000 Uani . . . . . .
C43 C 0.4973(3) 0.28100(12) 0.0447(4) 0.0248 1.0000 Uani . . . . . .
C44 C 0.4388(3) 0.30833(11) 0.0688(3) 0.0182 1.0000 Uani . . . . . .
C45 C 0.4786(3) 0.40735(11) 0.2642(3) 0.0169 1.0000 Uani . . . . . .
C46 C 0.5286(3) 0.43170(11) 0.2137(4) 0.0203 1.0000 Uani . . . . . .
C47 C 0.5909(3) 0.45760(12) 0.2825(4) 0.0250 1.0000 Uani . . . . . .
C48 C 0.6019(3) 0.46012(14) 0.4010(4) 0.0308 1.0000 Uani . . . . . .
C49 C 0.5524(4) 0.43632(14) 0.4516(4) 0.0319 1.0000 Uani . . . . . .
C50 C 0.4916(3) 0.40943(12) 0.3840(3) 0.0229 1.0000 Uani . . . . . .
C51 C 0.3349(3) 0.35352(11) 0.2654(3) 0.0167 1.0000 Uani . . . . . .
C52 C 0.3658(3) 0.32138(13) 0.3307(4) 0.0261 1.0000 Uani . . . . . .
C53 C 0.3184(4) 0.30784(14) 0.4058(4) 0.0346 1.0000 Uani . . . . . .
C54 C 0.2405(4) 0.32635(13) 0.4173(4) 0.0292 1.0000 Uani . . . . . .
C55 C 0.2074(3) 0.35773(13) 0.3511(4) 0.0273 1.0000 Uani . . . . . .
C56 C 0.2539(3) 0.37138(12) 0.2747(4) 0.0216 1.0000 Uani . . . . . .
C57 C 0.1340(3) 0.29400(12) 0.0171(4) 0.0223 1.0000 Uani . . . . . .
C58 C 0.0822(3) 0.29751(13) 0.0946(4) 0.0282 1.0000 Uani . . . . . .
C59 C 0.0145(4) 0.27121(15) 0.0945(5) 0.0377 1.0000 Uani . . . . . .
C60 C -0.0009(4) 0.24130(14) 0.0147(5) 0.0386 1.0000 Uani . . . . . .
C61 C 0.0525(4) 0.23794(14) -0.0598(5) 0.0360 1.0000 Uani . . . . . .
C62 C 0.1218(4) 0.26397(13) -0.0586(4) 0.0292 1.0000 Uani . . . . . .
C63 C -0.2466(9) 0.2640(4) -0.1508(11) 0.1240 1.0000 Uani . U . . . .
C64 C 0.6878(5) 0.3504(2) 0.5959(6) 0.0585 1.0000 Uani . . . . . .
H1 H 0.3571 0.4349 0.0175 0.0447 1.0000 Uiso R . . . . .
H21 H 0.1068 0.5154 0.0232 0.0230 1.0000 Uiso R . . . . .
H31 H 0.1502 0.5622 0.1589 0.0257 1.0000 Uiso R . . . . .
H41 H 0.2784 0.5547 0.3268 0.0282 1.0000 Uiso R . . . . .
H51 H 0.3667 0.5003 0.3518 0.0288 1.0000 Uiso R . . . . .
H61 H 0.3257 0.4530 0.2133 0.0221 1.0000 Uiso R . . . . .
H81 H -0.0002 0.4469 -0.1903 0.0271 1.0000 Uiso R . . . . .
H91 H -0.0554 0.4819 -0.3611 0.0329 1.0000 Uiso R . . . . .
H101 H 0.0416 0.5267 -0.4081 0.0319 1.0000 Uiso R . . . . .
H111 H 0.1975 0.5330 -0.2903 0.0281 1.0000 Uiso R . . . . .
H121 H 0.2536 0.4961 -0.1246 0.0262 1.0000 Uiso R . . . . .
H141 H 0.0668 0.4535 0.1502 0.0246 1.0000 Uiso R . . . . .
H151 H -0.0620 0.4244 0.1822 0.0312 1.0000 Uiso R . . . . .
H161 H -0.1304 0.3732 0.0711 0.0322 1.0000 Uiso R . . . . .
H171 H -0.0693 0.3491 -0.0685 0.0281 1.0000 Uiso R . . . . .
H191 H -0.0257 0.3613 -0.2703 0.0342 1.0000 Uiso R . . . . .
H192 H 0.0002 0.3239 -0.1927 0.0340 1.0000 Uiso R . . . . .
H201 H 0.0918 0.3524 -0.3498 0.0339 1.0000 Uiso R . . . . .
H202 H 0.0801 0.3101 -0.3202 0.0341 1.0000 Uiso R . . . . .
H221 H 0.2064 0.2710 -0.2855 0.0268 1.0000 Uiso R . . . . .
H231 H 0.3310 0.2444 -0.3359 0.0302 1.0000 Uiso R . . . . .
H241 H 0.4682 0.2791 -0.3125 0.0327 1.0000 Uiso R . . . . .
H251 H 0.4793 0.3395 -0.2443 0.0278 1.0000 Uiso R . . . . .
H281 H 0.1770 0.4152 -0.2838 0.0289 1.0000 Uiso R . . . . .
H291 H 0.1001 0.4378 -0.4693 0.0390 1.0000 Uiso R . . . . .
H301 H 0.1870 0.4549 -0.5930 0.0410 1.0000 Uiso R . . . . .
H311 H 0.3471 0.4455 -0.5372 0.0380 1.0000 Uiso R . . . . .
H321 H 0.4239 0.4187 -0.3566 0.0300 1.0000 Uiso R . . . . .
H341 H 0.4634 0.4579 -0.1628 0.0290 1.0000 Uiso R . . . . .
H351 H 0.6147 0.4785 -0.0741 0.0360 1.0000 Uiso R . . . . .
H361 H 0.7311 0.4369 0.0328 0.0350 1.0000 Uiso R . . . . .
H371 H 0.6909 0.3741 0.0452 0.0330 1.0000 Uiso R . . . . .
H381 H 0.5392 0.3532 -0.0457 0.0258 1.0000 Uiso R . . . . .
H401 H 0.5959 0.3545 0.2671 0.0341 1.0000 Uiso R . . . . .
H411 H 0.6937 0.3081 0.2296 0.0478 1.0000 Uiso R . . . . .
H421 H 0.6323 0.2647 0.0835 0.0429 1.0000 Uiso R . . . . .
H431 H 0.4732 0.2625 -0.0101 0.0311 1.0000 Uiso R . . . . .
H441 H 0.3746 0.3083 0.0294 0.0231 1.0000 Uiso R . . . . .
H461 H 0.5200 0.4308 0.1335 0.0259 1.0000 Uiso R . . . . .
H471 H 0.6260 0.4731 0.2491 0.0320 1.0000 Uiso R . . . . .
H481 H 0.6427 0.4778 0.4468 0.0381 1.0000 Uiso R . . . . .
H491 H 0.5593 0.4383 0.5315 0.0399 1.0000 Uiso R . . . . .
H501 H 0.4600 0.3929 0.4191 0.0288 1.0000 Uiso R . . . . .
H521 H 0.4180 0.3087 0.3238 0.0330 1.0000 Uiso R . . . . .
H531 H 0.3402 0.2863 0.4500 0.0430 1.0000 Uiso R . . . . .
H541 H 0.2107 0.3176 0.4698 0.0361 1.0000 Uiso R . . . . .
H551 H 0.1533 0.3699 0.3564 0.0343 1.0000 Uiso R . . . . .
H561 H 0.2304 0.3923 0.2287 0.0269 1.0000 Uiso R . . . . .
H581 H 0.0929 0.3176 0.1465 0.0348 1.0000 Uiso R . . . . .
H591 H -0.0203 0.2737 0.1474 0.0467 1.0000 Uiso R . . . . .
H601 H -0.0479 0.2233 0.0122 0.0480 1.0000 Uiso R . . . . .
H611 H 0.0416 0.2179 -0.1122 0.0445 1.0000 Uiso R . . . . .
H621 H 0.1589 0.2615 -0.1088 0.0358 1.0000 Uiso R . . . . .
H631 H -0.3153 0.2659 -0.1956 0.1523 1.0000 Uiso R . . . . .
H632 H -0.2317 0.2379 -0.1190 0.1525 1.0000 Uiso R . . . . .
H641 H 0.6872 0.3711 0.5423 0.0711 1.0000 Uiso R . . . . .
H642 H 0.7467 0.3367 0.6118 0.0711 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.01179(6) 0.01162(6) 0.01174(6) -0.00069(5) 0.00389(4) -0.00021(5)
Cl1 0.0889(19) 0.143(3) 0.0981(19) -0.0108(18) 0.0128(15) 0.0079(18)
Cl2 0.0926(18) 0.0970(19) 0.140(2) -0.0164(18) 0.0511(18) -0.0104(15)
Cl3 0.200(3) 0.0758(15) 0.0932(17) -0.0252(13) 0.092(2) -0.0498(18)
Cl4 0.0809(15) 0.0773(14) 0.0883(15) 0.0259(12) -0.0126(12) -0.0313(12)
P1 0.0297(6) 0.0338(7) 0.0397(7) 0.0054(5) 0.0066(5) -0.0024(5)
P2 0.0124(4) 0.0130(4) 0.0136(4) -0.0018(3) 0.0034(3) -0.0011(3)
P3 0.0169(4) 0.0137(4) 0.0134(4) -0.0004(3) 0.0067(3) -0.0005(3)
P4 0.0133(4) 0.0133(4) 0.0126(4) 0.0003(3) 0.0031(3) -0.0007(3)
P5 0.0125(4) 0.0127(4) 0.0132(4) 0.0000(3) 0.0040(3) 0.0004(3)
O1 0.0201(14) 0.0157(13) 0.0184(13) 0.0016(10) 0.0029(11) -0.0042(11)
N1 0.0126(15) 0.0195(16) 0.0185(15) -0.0056(12) 0.0027(12) -0.0023(12)
N2 0.0150(15) 0.0191(15) 0.0149(14) -0.0071(12) 0.0031(12) -0.0006(12)
C1 0.0159(17) 0.0135(16) 0.0144(15) 0.0005(13) 0.0070(13) 0.0002(13)
C2 0.0154(17) 0.0157(17) 0.0213(18) -0.0004(14) 0.0042(14) 0.0017(14)
C3 0.0213(19) 0.0153(17) 0.028(2) -0.0011(15) 0.0115(16) 0.0022(15)
C4 0.030(2) 0.0181(18) 0.0215(19) -0.0075(15) 0.0109(17) -0.0029(16)
C5 0.028(2) 0.023(2) 0.0178(18) -0.0010(15) 0.0038(16) 0.0021(17)
C6 0.0214(19) 0.0163(17) 0.0158(16) 0.0010(13) 0.0057(14) 0.0016(15)
C7 0.0177(18) 0.0139(16) 0.0159(16) -0.0004(13) 0.0053(14) 0.0028(14)
C8 0.0163(18) 0.025(2) 0.0215(18) 0.0024(15) 0.0040(15) 0.0025(16)
C9 0.018(2) 0.037(2) 0.0210(19) 0.0016(17) -0.0003(16) 0.0058(18)
C10 0.030(2) 0.029(2) 0.0170(18) 0.0041(16) 0.0058(16) 0.0106(18)
C11 0.029(2) 0.0205(19) 0.0193(18) 0.0037(15) 0.0090(16) 0.0038(16)
C12 0.0211(19) 0.0198(18) 0.0175(17) 0.0008(14) 0.0030(15) 0.0013(15)
C13 0.0133(17) 0.0133(16) 0.0208(17) 0.0013(13) 0.0060(14) 0.0024(13)
C14 0.0207(19) 0.0173(18) 0.0241(19) 0.0001(15) 0.0110(16) 0.0040(15)
C15 0.024(2) 0.025(2) 0.033(2) 0.0026(17) 0.0182(18) 0.0061(17)
C16 0.019(2) 0.022(2) 0.040(2) 0.0026(18) 0.0151(18) -0.0017(16)
C17 0.0155(18) 0.0204(19) 0.032(2) -0.0003(16) 0.0088(16) -0.0017(15)
C18 0.0128(17) 0.0172(17) 0.0202(17) 0.0011(14) 0.0059(14) 0.0026(14)
C19 0.0167(19) 0.034(2) 0.025(2) -0.0117(18) -0.0005(15) -0.0021(17)
C20 0.020(2) 0.038(2) 0.0181(18) -0.0118(17) -0.0018(15) 0.0008(18)
C21 0.0199(18) 0.0173(17) 0.0140(16) -0.0021(13) 0.0067(14) 0.0009(14)
C22 0.027(2) 0.0186(18) 0.0215(18) -0.0042(15) 0.0107(16) -0.0024(16)
C23 0.034(2) 0.0158(18) 0.025(2) -0.0060(15) 0.0120(18) 0.0028(17)
C24 0.028(2) 0.025(2) 0.030(2) -0.0072(17) 0.0137(18) 0.0047(17)
C25 0.023(2) 0.023(2) 0.0243(19) -0.0049(16) 0.0105(16) -0.0008(16)
C26 0.0209(18) 0.0153(17) 0.0134(15) -0.0004(13) 0.0074(14) 0.0007(14)
C27 0.026(2) 0.0174(17) 0.0140(16) 0.0003(14) 0.0081(15) 0.0026(15)
C28 0.027(2) 0.023(2) 0.0186(18) -0.0011(15) 0.0069(16) 0.0049(17)
C29 0.034(2) 0.035(2) 0.021(2) -0.0003(18) 0.0034(18) 0.013(2)
C30 0.051(3) 0.031(2) 0.0150(18) 0.0031(17) 0.0066(19) 0.015(2)
C31 0.044(3) 0.031(2) 0.0181(19) 0.0059(17) 0.0123(19) 0.002(2)
C32 0.031(2) 0.026(2) 0.0190(18) 0.0003(16) 0.0113(17) -0.0014(18)
C33 0.0175(17) 0.0214(18) 0.0170(16) -0.0044(14) 0.0107(14) -0.0036(15)
C34 0.027(2) 0.0208(19) 0.0229(19) 0.0006(15) 0.0094(16) -0.0025(17)
C35 0.033(2) 0.026(2) 0.030(2) -0.0025(18) 0.0147(19) -0.0126(19)
C36 0.021(2) 0.034(2) 0.031(2) -0.0064(18) 0.0113(17) -0.0111(18)
C37 0.0184(19) 0.029(2) 0.034(2) 0.0002(18) 0.0112(17) -0.0008(17)
C38 0.0209(19) 0.0206(19) 0.0248(19) -0.0010(15) 0.0122(16) -0.0023(15)
C39 0.0183(18) 0.0150(17) 0.0185(17) 0.0031(13) 0.0073(14) 0.0019(14)
C40 0.021(2) 0.022(2) 0.034(2) -0.0039(17) 0.0052(18) 0.0007(16)
C41 0.019(2) 0.031(3) 0.063(3) -0.006(2) 0.006(2) 0.0072(19)
C42 0.027(2) 0.019(2) 0.062(3) -0.003(2) 0.021(2) 0.0058(18)
C43 0.031(2) 0.0153(18) 0.033(2) 0.0016(16) 0.0162(19) -0.0013(17)
C44 0.0201(18) 0.0164(17) 0.0185(17) 0.0028(14) 0.0064(14) -0.0006(14)
C45 0.0133(17) 0.0171(18) 0.0184(17) -0.0019(13) 0.0017(13) -0.0002(13)
C46 0.0186(19) 0.0214(19) 0.0198(18) -0.0010(15) 0.0042(15) -0.0016(15)
C47 0.019(2) 0.023(2) 0.031(2) -0.0017(17) 0.0050(17) -0.0048(16)
C48 0.028(2) 0.032(2) 0.028(2) -0.0113(18) 0.0015(18) -0.0115(19)
C49 0.036(3) 0.039(3) 0.0178(19) -0.0114(18) 0.0050(18) -0.013(2)
C50 0.026(2) 0.026(2) 0.0152(17) -0.0009(15) 0.0030(15) -0.0034(16)
C51 0.0209(19) 0.0161(17) 0.0138(16) -0.0006(13) 0.0061(14) -0.0019(14)
C52 0.030(2) 0.025(2) 0.025(2) 0.0100(17) 0.0098(17) 0.0058(18)
C53 0.053(3) 0.029(2) 0.027(2) 0.0141(19) 0.021(2) 0.006(2)
C54 0.041(3) 0.026(2) 0.027(2) 0.0002(17) 0.019(2) -0.007(2)
C55 0.029(2) 0.032(2) 0.026(2) -0.0033(18) 0.0144(18) -0.0040(18)
C56 0.023(2) 0.023(2) 0.0208(18) 0.0021(15) 0.0082(16) -0.0005(16)
C57 0.0206(19) 0.0186(19) 0.0253(19) 0.0046(15) 0.0033(16) -0.0030(15)
C58 0.030(2) 0.025(2) 0.029(2) 0.0037(18) 0.0090(18) -0.0018(18)
C59 0.032(3) 0.035(3) 0.050(3) 0.016(2) 0.017(2) -0.001(2)
C60 0.030(3) 0.028(2) 0.053(3) 0.014(2) 0.005(2) -0.010(2)
C61 0.037(3) 0.025(2) 0.039(3) 0.001(2) 0.000(2) -0.009(2)
C62 0.035(3) 0.022(2) 0.029(2) 0.0004(17) 0.0088(19) -0.0013(19)
C63 0.110(7) 0.144(8) 0.107(7) -0.022(6) 0.017(6) -0.016(6)
C64 0.066(4) 0.054(4) 0.065(4) -0.008(3) 0.035(4) -0.015(3)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.054801(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 . P2 . 2.2445(9) yes
Pt1 . P3 . 2.3240(9) yes
Pt1 . P4 . 2.3573(9) yes
Pt1 . P5 . 2.3018(9) yes
Pt1 . H1 . 1.468 no
Cl1 . C63 . 1.799(13) yes
Cl2 . C63 . 1.737(12) yes
Cl3 . C64 . 1.741(7) yes
Cl4 . C64 . 1.738(7) yes
P1 . F10 . 1.572(8) yes
P1 . F20 . 1.536(11) yes
P1 . F30 . 1.583(7) yes
P1 . F40 . 1.578(8) yes
P1 . F50 . 1.583(9) yes
P1 . F60 . 1.593(13) yes
P1 . F11 . 1.582(11) yes
P1 . F21 . 1.602(15) yes
P1 . F31 . 1.624(13) yes
P1 . F41 . 1.553(14) yes
P1 . F51 . 1.554(11) yes
P1 . F61 . 1.612(11) yes
P2 . O1 . 1.625(3) yes
P2 . N1 . 1.671(3) yes
P2 . N2 . 1.654(3) yes
P3 . C26 . 1.835(4) yes
P3 . C27 . 1.822(4) yes
P3 . C33 . 1.824(4) yes
P4 . C39 . 1.831(4) yes
P4 . C45 . 1.832(4) yes
P4 . C51 . 1.826(4) yes
P5 . C1 . 1.823(4) yes
P5 . C7 . 1.822(4) yes
P5 . C13 . 1.826(4) yes
O1 . C57 . 1.402(5) yes
N1 . C18 . 1.421(5) yes
N1 . C19 . 1.474(5) yes
N2 . C20 . 1.472(5) yes
N2 . C21 . 1.431(5) yes
C1 . C2 . 1.402(5) yes
C1 . C6 . 1.398(5) yes
C2 . C3 . 1.379(5) yes
C2 . H21 . 0.933 no
C3 . C4 . 1.389(6) yes
C3 . H31 . 0.923 no
C4 . C5 . 1.382(6) yes
C4 . H41 . 0.926 no
C5 . C6 . 1.386(5) yes
C5 . H51 . 0.929 no
C6 . H61 . 0.927 no
C7 . C8 . 1.385(5) yes
C7 . C12 . 1.399(5) yes
C8 . C9 . 1.394(6) yes
C8 . H81 . 0.940 no
C9 . C10 . 1.388(7) yes
C9 . H91 . 0.933 no
C10 . C11 . 1.384(6) yes
C10 . H101 . 0.935 no
C11 . C12 . 1.387(5) yes
C11 . H111 . 0.941 no
C12 . H121 . 0.932 no
C13 . C14 . 1.409(5) yes
C13 . C18 . 1.410(5) yes
C14 . C15 . 1.380(6) yes
C14 . H141 . 0.941 no
C15 . C16 . 1.384(6) yes
C15 . H151 . 0.928 no
C16 . C17 . 1.386(6) yes
C16 . H161 . 0.916 no
C17 . C18 . 1.394(5) yes
C17 . H171 . 0.928 no
C19 . C20 . 1.521(6) yes
C19 . H191 . 0.974 no
C19 . H192 . 0.983 no
C20 . H201 . 0.967 no
C20 . H202 . 0.962 no
C21 . C22 . 1.390(5) yes
C21 . C26 . 1.407(5) yes
C22 . C23 . 1.392(6) yes
C22 . H221 . 0.935 no
C23 . C24 . 1.383(6) yes
C23 . H231 . 0.930 no
C24 . C25 . 1.385(6) yes
C24 . H241 . 0.924 no
C25 . C26 . 1.398(5) yes
C25 . H251 . 0.937 no
C27 . C28 . 1.384(6) yes
C27 . C32 . 1.404(5) yes
C28 . C29 . 1.395(6) yes
C28 . H281 . 0.927 no
C29 . C30 . 1.381(7) yes
C29 . H291 . 0.931 no
C30 . C31 . 1.378(7) yes
C30 . H301 . 0.928 no
C31 . C32 . 1.383(6) yes
C31 . H311 . 0.939 no
C32 . H321 . 0.937 no
C33 . C34 . 1.404(6) yes
C33 . C38 . 1.387(6) yes
C34 . C35 . 1.383(6) yes
C34 . H341 . 0.932 no
C35 . C36 . 1.396(7) yes
C35 . H351 . 0.931 no
C36 . C37 . 1.392(6) yes
C36 . H361 . 0.942 no
C37 . C38 . 1.384(6) yes
C37 . H371 . 0.927 no
C38 . H381 . 0.939 no
C39 . C40 . 1.388(6) yes
C39 . C44 . 1.391(5) yes
C40 . C41 . 1.396(6) yes
C40 . H401 . 0.929 no
C41 . C42 . 1.383(7) yes
C41 . H411 . 0.933 no
C42 . C43 . 1.380(7) yes
C42 . H421 . 0.920 no
C43 . C44 . 1.393(6) yes
C43 . H431 . 0.922 no
C44 . H441 . 0.928 no
C45 . C46 . 1.394(5) yes
C45 . C50 . 1.389(5) yes
C46 . C47 . 1.388(6) yes
C46 . H461 . 0.930 no
C47 . C48 . 1.380(6) yes
C47 . H471 . 0.929 no
C48 . C49 . 1.378(7) yes
C48 . H481 . 0.929 no
C49 . C50 . 1.395(6) yes
C49 . H491 . 0.933 no
C50 . H501 . 0.931 no
C51 . C52 . 1.384(5) yes
C51 . C56 . 1.396(6) yes
C52 . C53 . 1.386(6) yes
C52 . H521 . 0.924 no
C53 . C54 . 1.375(7) yes
C53 . H531 . 0.932 no
C54 . C55 . 1.373(7) yes
C54 . H541 . 0.926 no
C55 . C56 . 1.391(6) yes
C55 . H551 . 0.932 no
C56 . H561 . 0.930 no
C57 . C58 . 1.379(6) yes
C57 . C62 . 1.378(6) yes
C58 . C59 . 1.376(7) yes
C58 . H581 . 0.929 no
C59 . C60 . 1.403(8) yes
C59 . H591 . 0.935 no
C60 . C61 . 1.366(8) yes
C60 . H601 . 0.941 no
C61 . C62 . 1.384(7) yes
C61 . H611 . 0.932 no
C62 . H621 . 0.934 no
C63 . H631 . 1.003 no
C63 . H632 . 1.002 no
C64 . H641 . 0.976 no
C64 . H642 . 0.970 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P2 . Pt1 . P3 . 90.29(3) yes
P2 . Pt1 . P4 . 101.62(3) yes
P3 . Pt1 . P4 . 111.77(3) yes
P2 . Pt1 . P5 . 89.89(3) yes
P3 . Pt1 . P5 . 126.32(3) yes
P4 . Pt1 . P5 . 120.68(3) yes
P2 . Pt1 . H1 . 168.0 no
P3 . Pt1 . H1 . 86.9 no
P4 . Pt1 . H1 . 90.2 no
P5 . Pt1 . H1 . 82.4 no
F10 . P1 . F20 . 90.9(5) yes
F10 . P1 . F30 . 89.3(4) yes
F20 . P1 . F30 . 89.2(5) yes
F10 . P1 . F40 . 89.6(4) yes
F20 . P1 . F40 . 179.5(5) yes
F30 . P1 . F40 . 90.8(4) yes
F10 . P1 . F50 . 88.9(4) yes
F20 . P1 . F50 . 93.5(6) yes
F30 . P1 . F50 . 176.9(4) yes
F40 . P1 . F50 . 86.6(4) yes
F10 . P1 . F60 . 179.1(6) yes
F20 . P1 . F60 . 90.0(6) yes
F30 . P1 . F60 . 90.9(5) yes
F40 . P1 . F60 . 89.6(6) yes
F50 . P1 . F60 . 90.8(6) yes
F11 . P1 . F21 . 82.4(7) yes
F11 . P1 . F31 . 81.9(6) yes
F21 . P1 . F31 . 89.1(7) yes
F11 . P1 . F41 . 94.5(7) yes
F21 . P1 . F41 . 176.7(7) yes
F31 . P1 . F41 . 89.4(7) yes
F11 . P1 . F51 . 94.7(6) yes
F21 . P1 . F51 . 90.7(7) yes
F31 . P1 . F51 . 176.6(6) yes
F41 . P1 . F51 . 90.7(7) yes
F11 . P1 . F61 . 173.6(6) yes
F21 . P1 . F61 . 91.4(6) yes
F31 . P1 . F61 . 96.3(6) yes
F41 . P1 . F61 . 91.7(7) yes
F51 . P1 . F61 . 87.1(6) yes
Pt1 . P2 . O1 . 112.37(11) yes
Pt1 . P2 . N1 . 115.35(12) yes
O1 . P2 . N1 . 108.90(16) yes
Pt1 . P2 . N2 . 117.26(12) yes
O1 . P2 . N2 . 108.59(16) yes
N1 . P2 . N2 . 92.62(16) yes
Pt1 . P3 . C26 . 114.67(12) yes
Pt1 . P3 . C27 . 119.09(13) yes
C26 . P3 . C27 . 99.18(17) yes
Pt1 . P3 . C33 . 108.99(12) yes
C26 . P3 . C33 . 107.70(18) yes
C27 . P3 . C33 . 106.28(18) yes
Pt1 . P4 . C39 . 115.32(13) yes
Pt1 . P4 . C45 . 113.66(13) yes
C39 . P4 . C45 . 102.93(18) yes
Pt1 . P4 . C51 . 115.69(13) yes
C39 . P4 . C51 . 104.07(17) yes
C45 . P4 . C51 . 103.62(18) yes
Pt1 . P5 . C1 . 116.12(12) yes
Pt1 . P5 . C7 . 115.31(12) yes
C1 . P5 . C7 . 101.15(17) yes
Pt1 . P5 . C13 . 113.55(12) yes
C1 . P5 . C13 . 104.72(17) yes
C7 . P5 . C13 . 104.45(17) yes
P2 . O1 . C57 . 125.2(3) yes
P2 . N1 . C18 . 119.6(3) yes
P2 . N1 . C19 . 111.9(3) yes
C18 . N1 . C19 . 121.3(3) yes
P2 . N2 . C20 . 114.9(3) yes
P2 . N2 . C21 . 124.2(3) yes
C20 . N2 . C21 . 120.9(3) yes
P5 . C1 . C2 . 121.3(3) yes
P5 . C1 . C6 . 119.8(3) yes
C2 . C1 . C6 . 118.9(3) yes
C1 . C2 . C3 . 120.2(4) yes
C1 . C2 . H21 . 120.3 no
C3 . C2 . H21 . 119.5 no
C2 . C3 . C4 . 120.6(4) yes
C2 . C3 . H31 . 118.6 no
C4 . C3 . H31 . 120.8 no
C3 . C4 . C5 . 119.6(4) yes
C3 . C4 . H41 . 120.2 no
C5 . C4 . H41 . 120.1 no
C4 . C5 . C6 . 120.5(4) yes
C4 . C5 . H51 . 119.8 no
C6 . C5 . H51 . 119.7 no
C1 . C6 . C5 . 120.2(4) yes
C1 . C6 . H61 . 119.5 no
C5 . C6 . H61 . 120.3 no
P5 . C7 . C8 . 123.5(3) yes
P5 . C7 . C12 . 117.6(3) yes
C8 . C7 . C12 . 118.9(4) yes
C7 . C8 . C9 . 120.8(4) yes
C7 . C8 . H81 . 119.2 no
C9 . C8 . H81 . 120.0 no
C8 . C9 . C10 . 119.8(4) yes
C8 . C9 . H91 . 119.4 no
C10 . C9 . H91 . 120.8 no
C9 . C10 . C11 . 119.8(4) yes
C9 . C10 . H101 . 119.8 no
C11 . C10 . H101 . 120.4 no
C10 . C11 . C12 . 120.3(4) yes
C10 . C11 . H111 . 120.3 no
C12 . C11 . H111 . 119.3 no
C7 . C12 . C11 . 120.3(4) yes
C7 . C12 . H121 . 119.8 no
C11 . C12 . H121 . 119.9 no
P5 . C13 . C14 . 120.5(3) yes
P5 . C13 . C18 . 121.1(3) yes
C14 . C13 . C18 . 118.3(3) yes
C13 . C14 . C15 . 120.9(4) yes
C13 . C14 . H141 . 119.6 no
C15 . C14 . H141 . 119.5 no
C14 . C15 . C16 . 120.1(4) yes
C14 . C15 . H151 . 120.1 no
C16 . C15 . H151 . 119.8 no
C15 . C16 . C17 . 120.3(4) yes
C15 . C16 . H161 . 120.1 no
C17 . C16 . H161 . 119.6 no
C16 . C17 . C18 . 120.3(4) yes
C16 . C17 . H171 . 119.6 no
C18 . C17 . H171 . 120.2 no
N1 . C18 . C13 . 120.2(3) yes
N1 . C18 . C17 . 119.9(4) yes
C13 . C18 . C17 . 119.9(4) yes
N1 . C19 . C20 . 105.3(3) yes
N1 . C19 . H191 . 109.4 no
C20 . C19 . H191 . 111.0 no
N1 . C19 . H192 . 110.1 no
C20 . C19 . H192 . 110.8 no
H191 . C19 . H192 . 110.0 no
C19 . C20 . N2 . 106.3(3) yes
C19 . C20 . H201 . 111.0 no
N2 . C20 . H201 . 109.2 no
C19 . C20 . H202 . 111.1 no
N2 . C20 . H202 . 110.2 no
H201 . C20 . H202 . 108.9 no
N2 . C21 . C22 . 117.9(3) yes
N2 . C21 . C26 . 122.4(3) yes
C22 . C21 . C26 . 119.7(4) yes
C21 . C22 . C23 . 120.9(4) yes
C21 . C22 . H221 . 119.4 no
C23 . C22 . H221 . 119.7 no
C22 . C23 . C24 . 119.6(4) yes
C22 . C23 . H231 . 119.9 no
C24 . C23 . H231 . 120.5 no
C23 . C24 . C25 . 120.0(4) yes
C23 . C24 . H241 . 120.8 no
C25 . C24 . H241 . 119.3 no
C24 . C25 . C26 . 121.3(4) yes
C24 . C25 . H251 . 118.9 no
C26 . C25 . H251 . 119.8 no
P3 . C26 . C21 . 121.0(3) yes
P3 . C26 . C25 . 120.4(3) yes
C21 . C26 . C25 . 118.5(3) yes
P3 . C27 . C28 . 118.2(3) yes
P3 . C27 . C32 . 122.5(3) yes
C28 . C27 . C32 . 119.0(4) yes
C27 . C28 . C29 . 120.7(4) yes
C27 . C28 . H281 . 120.1 no
C29 . C28 . H281 . 119.2 no
C28 . C29 . C30 . 119.8(5) yes
C28 . C29 . H291 . 119.9 no
C30 . C29 . H291 . 120.4 no
C29 . C30 . C31 . 120.0(4) yes
C29 . C30 . H301 . 120.4 no
C31 . C30 . H301 . 119.6 no
C30 . C31 . C32 . 120.8(4) yes
C30 . C31 . H311 . 119.3 no
C32 . C31 . H311 . 120.0 no
C27 . C32 . C31 . 119.8(4) yes
C27 . C32 . H321 . 120.0 no
C31 . C32 . H321 . 120.2 no
P3 . C33 . C34 . 118.0(3) yes
P3 . C33 . C38 . 121.7(3) yes
C34 . C33 . C38 . 118.8(4) yes
C33 . C34 . C35 . 120.4(4) yes
C33 . C34 . H341 . 120.0 no
C35 . C34 . H341 . 119.6 no
C34 . C35 . C36 . 120.4(4) yes
C34 . C35 . H351 . 119.2 no
C36 . C35 . H351 . 120.5 no
C35 . C36 . C37 . 119.2(4) yes
C35 . C36 . H361 . 120.4 no
C37 . C36 . H361 . 120.4 no
C36 . C37 . C38 . 120.4(4) yes
C36 . C37 . H371 . 119.9 no
C38 . C37 . H371 . 119.7 no
C33 . C38 . C37 . 120.9(4) yes
C33 . C38 . H381 . 119.1 no
C37 . C38 . H381 . 120.0 no
P4 . C39 . C40 . 122.2(3) yes
P4 . C39 . C44 . 118.8(3) yes
C40 . C39 . C44 . 118.9(4) yes
C39 . C40 . C41 . 120.3(4) yes
C39 . C40 . H401 . 119.5 no
C41 . C40 . H401 . 120.2 no
C40 . C41 . C42 . 120.2(5) yes
C40 . C41 . H411 . 120.2 no
C42 . C41 . H411 . 119.6 no
C41 . C42 . C43 . 120.0(4) yes
C41 . C42 . H421 . 119.9 no
C43 . C42 . H421 . 120.1 no
C42 . C43 . C44 . 119.8(4) yes
C42 . C43 . H431 . 119.4 no
C44 . C43 . H431 . 120.9 no
C43 . C44 . C39 . 120.8(4) yes
C43 . C44 . H441 . 120.3 no
C39 . C44 . H441 . 118.8 no
P4 . C45 . C46 . 118.6(3) yes
P4 . C45 . C50 . 122.2(3) yes
C46 . C45 . C50 . 119.2(4) yes
C45 . C46 . C47 . 120.3(4) yes
C45 . C46 . H461 . 120.1 no
C47 . C46 . H461 . 119.6 no
C46 . C47 . C48 . 120.2(4) yes
C46 . C47 . H471 . 120.0 no
C48 . C47 . H471 . 119.7 no
C47 . C48 . C49 . 119.9(4) yes
C47 . C48 . H481 . 120.2 no
C49 . C48 . H481 . 120.0 no
C48 . C49 . C50 . 120.5(4) yes
C48 . C49 . H491 . 119.8 no
C50 . C49 . H491 . 119.8 no
C49 . C50 . C45 . 119.9(4) yes
C49 . C50 . H501 . 120.1 no
C45 . C50 . H501 . 120.0 no
P4 . C51 . C52 . 122.6(3) yes
P4 . C51 . C56 . 118.8(3) yes
C52 . C51 . C56 . 118.7(4) yes
C51 . C52 . C53 . 120.5(4) yes
C51 . C52 . H521 . 120.0 no
C53 . C52 . H521 . 119.6 no
C52 . C53 . C54 . 120.4(4) yes
C52 . C53 . H531 . 119.7 no
C54 . C53 . H531 . 119.8 no
C53 . C54 . C55 . 120.0(4) yes
C53 . C54 . H541 . 119.8 no
C55 . C54 . H541 . 120.2 no
C54 . C55 . C56 . 120.0(4) yes
C54 . C55 . H551 . 120.4 no
C56 . C55 . H551 . 119.5 no
C51 . C56 . C55 . 120.4(4) yes
C51 . C56 . H561 . 119.8 no
C55 . C56 . H561 . 119.8 no
O1 . C57 . C58 . 117.5(4) yes
O1 . C57 . C62 . 120.9(4) yes
C58 . C57 . C62 . 121.6(4) yes
C57 . C58 . C59 . 119.7(5) yes
C57 . C58 . H581 . 120.0 no
C59 . C58 . H581 . 120.2 no
C58 . C59 . C60 . 119.1(5) yes
C58 . C59 . H591 . 119.4 no
C60 . C59 . H591 . 121.5 no
C59 . C60 . C61 . 120.2(5) yes
C59 . C60 . H601 . 120.3 no
C61 . C60 . H601 . 119.4 no
C60 . C61 . C62 . 120.9(5) yes
C60 . C61 . H611 . 119.3 no
C62 . C61 . H611 . 119.8 no
C61 . C62 . C57 . 118.4(5) yes
C61 . C62 . H621 . 120.9 no
C57 . C62 . H621 . 120.7 no
Cl1 . C63 . Cl2 . 112.4(7) yes
Cl1 . C63 . H631 . 109.1 no
Cl2 . C63 . H631 . 108.1 no
Cl1 . C63 . H632 . 108.7 no
Cl2 . C63 . H632 . 108.7 no
H631 . C63 . H632 . 109.8 no
Cl3 . C64 . Cl4 . 108.6(4) yes
Cl3 . C64 . H641 . 111.5 no
Cl4 . C64 . H641 . 111.4 no
Cl3 . C64 . H642 . 107.6 no
Cl4 . C64 . H642 . 107.9 no
H641 . C64 . H642 . 109.7 no
_iucr_refine_instruction_details_constraints
;
#
# Punched on 05/10/11 at 09:09:15
#
#LIST 12
BLOCK
CONT SCALE
CONT PT ( 1 ,X'S,U'S) UNTIL P ( 5 )
CONT F ( 10 ,X'S,U[ISO]) UNTIL F ( 61 )
CONT O ( 1 ,X'S,U'S) UNTIL C ( 64 )
SUMFIX PART(1001,OCC) AND PART(1002,OCC)
RIDE PT ( 1,X'S) H ( 1,X'S)
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 29,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 301,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
RIDE C ( 34,X'S) H ( 341,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 38,X'S) H ( 381,X'S)
RIDE C ( 40,X'S) H ( 401,X'S)
RIDE C ( 41,X'S) H ( 411,X'S)
RIDE C ( 42,X'S) H ( 421,X'S)
RIDE C ( 43,X'S) H ( 431,X'S)
RIDE C ( 44,X'S) H ( 441,X'S)
RIDE C ( 46,X'S) H ( 461,X'S)
RIDE C ( 47,X'S) H ( 471,X'S)
RIDE C ( 48,X'S) H ( 481,X'S)
RIDE C ( 49,X'S) H ( 491,X'S)
RIDE C ( 50,X'S) H ( 501,X'S)
RIDE C ( 52,X'S) H ( 521,X'S)
RIDE C ( 53,X'S) H ( 531,X'S)
RIDE C ( 54,X'S) H ( 541,X'S)
RIDE C ( 55,X'S) H ( 551,X'S)
RIDE C ( 56,X'S) H ( 561,X'S)
RIDE C ( 58,X'S) H ( 581,X'S)
RIDE C ( 59,X'S) H ( 591,X'S)
RIDE C ( 60,X'S) H ( 601,X'S)
RIDE C ( 61,X'S) H ( 611,X'S)
RIDE C ( 62,X'S) H ( 621,X'S)
RIDE C ( 63,X'S) H ( 631,X'S) H ( 632,X'S)
RIDE C ( 64,X'S) H ( 641,X'S) H ( 642,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 05/10/11 at 09:09:15
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
U(IJ)'S 0.0, 0.010000 = CL(1) TO C(63)
END
;
#===
data_6PF6
_database_code_depnum_ccdc_archive 'CCDC 869436'
#TrackingRef '- combined_bf.cif'
_audit_creation_date 12-02-16
_audit_creation_method CRYSTALS_ver_14.40
_oxford_structure_analysis_title 'bfpan_740_0m in P2(1)/n'
_chemical_name_systematic ?
_chemical_melting_point ?
_vrf_PLAT112_6PF6
;
PROBLEM: ADDSYM Detects Additional (Pseudo) Symm. Elem... n
RESPONSE: There are two molecules of each platinum complex & anion
in the asymmetric unit; the second molecule has a numbering scheme
100 greater than the first molecule. The two molecules are
nearly related by the n-glide operation; however, it is apparent
that the condition is inexact, as 25% of the data for which the
condition I(h0l), h+l odd absent applies, has an I/sigma(I)
value greater than 3.0. Such an occurrence could also arise from
twinning. However, ROTAX, TwinRotMat, and a plot of Fo vs. Fc
revealed no evidence for twinning.
Finally, it is important to point out that CheckCIF ignores
disordered atoms in its assessment of missed symmetry. Here,
it is the disordered atoms that validate the choice of P21.
For example, the occupancies of the disordered central P atoms
are 94/6 in one molecule and 52/48 in the other.
;
_vrf_PLAT111_6PF6
;
PROBLEM: ADDSYM Detects (Pseudo) Centre of Symmetry ..... 100 PerFi
RESPONSE: There are two molecules of each platinum complex & anion
in the asymmetric unit; the second molecule has a numbering scheme
100 greater than the first molecule. The two molecules are
nearly related by the n-glide operation; however, it is apparent
that the condition is inexact, as 25% of the data for which the
condition I(h0l), h+l odd absent applies, has an I/sigma(I)
value greater than 3.0. For this Alert, the punch line is that
if we have no n glide, we have no 1-bar either. All this
could also arise from twinning. However, ROTAX, TwinRotMat,
and a plot of Fo vs. Fc revealed no evidence for twinning.
Finally, it is important to point out that CheckCIF ignores
disordered atoms in its assessment of missed symmetry. Here,
it is the disordered atoms that validate the choice of P21.
For example, the occupancies of the disordered central P atoms
are 94/6 in one molecule and 52/48 in the other.
;
_vrf_PLAT113_6PF6
;
PROBLEM: ADDSYM Suggests Possible Pseudo/New Space-group. P21/c
RESPONSE: CheckCIF is in fact referring to the transformed cell,
after acknowledging that the data fits P21/n fairly well.
There are two molecules of each platinum complex & anion
in the asymmetric unit; the second molecule has a numbering scheme
100 greater than the first molecule. The two molecules are
nearly related by the n-glide operation; however, it is apparent
that the condition is inexact, as 25% of the data for which the
condition I(h0l), h+l odd absent applies, has an I/sigma(I)
value greater than 3.0. For this Alert, the punch line is that
if we have no n glide, we have no 1-bar either. Then we do not
have P21/n, then we do not have P21/c. All this
could also arise from twinning. However, ROTAX, TwinRotMat,
and a plot of Fo vs. Fc revealed no evidence for twinning.
Finally, it is important to point out that CheckCIF ignores
disordered atoms in its assessment of missed symmetry. Here,
it is the disordered atoms that validate the choice of P21.
For example, the occupancies of the disordered central P atoms
are 94/6 in one molecule and 52/48 in the other.
;
_cell_length_a 12.1189(4)
_cell_length_b 13.4744(5)
_cell_length_c 22.8621(9)
_cell_angle_alpha 90
_cell_angle_beta 98.743(2)
_cell_angle_gamma 90
_cell_volume 3689.9(2)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 1 21 1 '
_symmetry_space_group_name_Hall 'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103
11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C38 H32 Cl1 F6 N2 P4 Pt1
# Dc = 1.77 Fooo = 1932.00 Mu = 41.11 M = 1970.22
# Found Formula = C38 H32 Cl1 F6.00 N2 P4 Pt1
# Dc = 1.77 FOOO = 1932.00 Mu = 41.11 M = 1970.22
_chemical_formula_sum 'C38 H32 Cl1 F6.00 N2 P4 Pt1'
_chemical_formula_moiety 'C38 H32 Cl N2 P3 Pt, F6 P'
_chemical_compound_source ?
_chemical_formula_weight 985.11
_cell_measurement_reflns_used 9915
_cell_measurement_theta_min 2
_cell_measurement_theta_max 29
_cell_measurement_temperature 120
_exptl_crystal_description needle
_exptl_crystal_colour colourless
_exptl_crystal_size_min 0.060
_exptl_crystal_size_mid 0.110
_exptl_crystal_size_max 0.550
_exptl_crystal_density_diffrn 1.773
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1932
_exptl_absorpt_coefficient_mu 4.111
# Sheldrick geometric approximatio 0.64 0.78
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_absorpt_correction_T_min 0.64
_exptl_absorpt_correction_T_max 0.78
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 120
_diffrn_reflns_number 21159
_reflns_number_total 21159
_diffrn_reflns_av_R_equivalents 0.044
# Number of reflections without Friedels Law is 21159
# Number of reflections with Friedels Law is 11176
# Theoretical number of reflections is about 10807
_diffrn_reflns_theta_min 1.700
_diffrn_reflns_theta_max 30.046
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full 30.046
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -18
_diffrn_reflns_limit_k_max 18
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 32
_reflns_limit_h_min -17
_reflns_limit_h_max 16
_reflns_limit_k_min -18
_reflns_limit_k_max 18
_reflns_limit_l_min 0
_reflns_limit_l_max 32
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -2.13
_refine_diff_density_max 2.16
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns 21159
_refine_ls_number_restraints 7
_refine_ls_number_parameters 952
_oxford_refine_ls_R_factor_ref 0.0552
_refine_ls_wR_factor_ref 0.0835
_refine_ls_goodness_of_fit_ref 0.9786
_refine_ls_shift/su_max 0.0061564
_refine_ls_shift/su_mean 0.0001530
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 21159
_refine_ls_R_factor_all 0.0552
_refine_ls_wR_factor_all 0.0835
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 17543
_refine_ls_R_factor_gt 0.0419
_refine_ls_wR_factor_gt 0.0794
_refine_ls_abs_structure_Flack 0.500(7)
_refine_ls_abs_structure_details 'Flack (1983), 9983 Friedel-pairs'
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration ad
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 6.59P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014.
Flack, H. D. (1983). Acta Cryst. A39, 876-881.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Pt1 Pt -0.008098(19) 0.19951(10) 0.567069(10) 0.0170 1.0000 Uani . . . . . .
Pt11 Pt 0.49966(2) 0.30558(10) 0.929336(11) 0.0223 1.0000 Uani . . . . . .
Cl1 Cl -0.05926(17) 0.3599(2) 0.53223(11) 0.0335 1.0000 Uani . . . . . .
Cl11 Cl 0.5644(2) 0.1601(2) 0.97594(13) 0.0530 1.0000 Uani . . . . . .
P1 P 0.13568(14) 0.1955(3) 0.51263(8) 0.0188 1.0000 Uani . . . . . .
P2 P 0.02130(17) 0.04393(19) 0.58669(10) 0.0175 0.940(5) Uani . U P . . .
P3 P 0.064(2) 0.080(3) 0.6248(14) 0.0162 0.060(5) Uani . U P . . .
P4 P -0.12394(14) 0.2109(2) 0.63758(8) 0.0180 1.0000 Uani . . . . . .
P5 P 0.0318(2) 0.8021(3) 0.84664(12) 0.0491 1.0000 Uani . . . . . .
P101 P 0.35689(15) 0.3088(3) 0.98560(8) 0.0208 1.0000 Uani . . . . . .
P102 P 0.4217(3) 0.4280(3) 0.87313(15) 0.0165 0.524(6) Uani . . P . . .
P103 P 0.4752(4) 0.4613(4) 0.9135(2) 0.0218 0.476(6) Uani . . P . . .
P104 P 0.61749(15) 0.2935(2) 0.85972(9) 0.0201 1.0000 Uani . . . . . .
P105 P 0.4605(2) 0.7035(3) 0.65536(12) 0.0489 1.0000 Uani . . . . . .
F1 F -0.0816(6) 0.8192(7) 0.8035(4) 0.0985 1.0000 Uani . . . . . .
F2 F -0.0085(7) 0.8775(7) 0.8954(4) 0.043(2) 0.615(10) Uiso . . P 1 2 .
F3 F -0.0113(7) 0.7136(8) 0.8763(4) 0.058(3) 0.615(10) Uiso . . P 1 2 .
F4 F 0.1004(9) 0.7266(9) 0.8044(5) 0.085(4) 0.615(10) Uiso . . P 1 2 .
F5 F 0.0818(10) 0.8933(10) 0.8185(5) 0.075(3) 0.615(10) Uiso . . P 1 2 .
F6 F 0.1478(5) 0.7864(7) 0.8901(3) 0.0795 1.0000 Uani . . . . . .
F21 F 0.0382(13) 0.9108(12) 0.8591(8) 0.066(5) 0.385(10) Uiso . . P 1 1 .
F22 F -0.0288(16) 0.776(2) 0.8984(9) 0.107(7) 0.385(10) Uiso . . P 1 1 .
F23 F 0.0247(8) 0.6869(8) 0.8257(5) 0.035(3) 0.385(10) Uiso . . P 1 1 .
F24 F 0.082(2) 0.818(2) 0.7860(12) 0.133(9) 0.385(10) Uiso . . P 1 1 .
F101 F 0.5775(6) 0.6921(8) 0.6950(3) 0.1025 1.0000 Uani . . . . . .
F102 F 0.4402(9) 0.8005(9) 0.6872(5) 0.067(3) 0.549(10) Uiso . . P 1 3 .
F103 F 0.3855(9) 0.6326(9) 0.6915(5) 0.067(3) 0.549(10) Uiso . . P 1 3 .
F104 F 0.4826(7) 0.6115(7) 0.6187(4) 0.041(2) 0.549(10) Uiso . . P 1 3 .
F105 F 0.5239(8) 0.7792(9) 0.6082(5) 0.055(3) 0.549(10) Uiso . . P 1 3 .
F106 F 0.3423(5) 0.7174(6) 0.6148(3) 0.0718 1.0000 Uani . . . . . .
F121 F 0.4201(16) 0.7248(17) 0.7175(9) 0.114(7) 0.451(10) Uiso . . P 1 4 .
F122 F 0.4442(10) 0.5853(10) 0.6686(6) 0.056(3) 0.451(10) Uiso . . P 1 4 .
F123 F 0.5127(11) 0.6635(13) 0.5991(6) 0.075(5) 0.451(10) Uiso . . P 1 4 .
F124 F 0.4939(8) 0.8103(8) 0.6468(5) 0.045(3) 0.451(10) Uiso . . P 1 4 .
N1 N 0.1492(5) -0.0004(5) 0.5981(3) 0.0207 1.0000 Uani . . . . . .
N2 N -0.0152(6) -0.0017(6) 0.6490(3) 0.0225 1.0000 Uani . . . . . .
N101 N 0.3443(5) 0.5077(6) 0.9028(3) 0.0255 1.0000 Uani . . . . . .
N102 N 0.5077(6) 0.5115(6) 0.8500(3) 0.0247 1.0000 Uani . . . . . .
C1 C 0.2001(6) 0.3176(8) 0.5156(3) 0.0240 1.0000 Uani . . . . . .
C2 C 0.2294(6) 0.3660(7) 0.4668(4) 0.0239 1.0000 Uani . . . . . .
C3 C 0.2769(6) 0.4602(8) 0.4738(4) 0.0280 1.0000 Uani . . . . . .
C4 C 0.2938(7) 0.5057(8) 0.5280(5) 0.0360 1.0000 Uani . . . . . .
C5 C 0.2648(7) 0.4584(8) 0.5786(4) 0.0327 1.0000 Uani . . . . . .
C6 C 0.2181(7) 0.3647(8) 0.5729(5) 0.0288 1.0000 Uani . . . . . .
C7 C 0.0905(6) 0.1635(6) 0.4357(3) 0.0204 1.0000 Uani . . . . . .
C8 C -0.0221(7) 0.1615(7) 0.4150(4) 0.0269 1.0000 Uani . . . . . .
C9 C -0.0592(9) 0.1394(7) 0.3559(4) 0.0375 1.0000 Uani . . . . . .
C10 C 0.0174(10) 0.1220(8) 0.3173(4) 0.0457 1.0000 Uani . . . . . .
C11 C 0.1303(10) 0.1242(8) 0.3376(4) 0.0403 1.0000 Uani . . . . . .
C12 C 0.1676(8) 0.1406(9) 0.3974(4) 0.0357 1.0000 Uani . . . . . .
C13 C 0.2513(6) 0.1170(6) 0.5407(3) 0.0169 1.0000 Uani . . . . . .
C14 C 0.3576(6) 0.1427(7) 0.5262(4) 0.0256 1.0000 Uani . . . . . .
C15 C 0.4494(6) 0.0831(7) 0.5418(4) 0.0261 1.0000 Uani . . . . . .
C16 C 0.4435(7) 0.0033(8) 0.5735(4) 0.0313 1.0000 Uani . . . . . .
C17 C 0.3423(6) -0.0270(7) 0.5903(4) 0.0226 1.0000 Uani . . . . . .
C18 C 0.2452(6) 0.0297(7) 0.5741(4) 0.0180 1.0000 Uani . . . . . .
C19 C 0.1611(8) -0.0834(8) 0.6415(5) 0.0425 1.0000 Uani . . . . . .
C20 C 0.0412(7) -0.0973(7) 0.6588(4) 0.0314 1.0000 Uani . . . . . .
C21 C -0.1257(7) 0.0055(8) 0.6621(4) 0.0249 1.0000 Uani . . . . . .
C22 C -0.1770(7) -0.0791(7) 0.6828(4) 0.0243 1.0000 Uani . . . . . .
C23 C -0.2842(7) -0.0745(7) 0.6958(4) 0.0234 1.0000 Uani . . . . . .
C24 C -0.3420(6) 0.0137(7) 0.6924(4) 0.0232 1.0000 Uani . . . . . .
C25 C -0.2901(7) 0.0974(7) 0.6739(4) 0.0227 1.0000 Uani . . . . . .
C26 C -0.1830(6) 0.0961(6) 0.6601(3) 0.0166 1.0000 Uani . . . . . .
C27 C -0.0378(6) 0.2590(6) 0.7026(3) 0.0186 1.0000 Uani . . . . . .
C28 C -0.0242(7) 0.2076(10) 0.7566(3) 0.0314 1.0000 Uani . . . . . .
C29 C 0.0433(8) 0.2423(8) 0.8057(4) 0.0417 1.0000 Uani . . . . . .
C30 C 0.1043(10) 0.3293(9) 0.8001(4) 0.0531 1.0000 Uani . . . . . .
C31 C 0.0932(7) 0.3805(8) 0.7478(5) 0.0373 1.0000 Uani . . . . . .
C32 C 0.0225(7) 0.3439(8) 0.6988(4) 0.0287 1.0000 Uani . . . . . .
C33 C -0.2410(5) 0.2932(7) 0.6179(3) 0.0190 1.0000 Uani . . . . . .
C34 C -0.2624(7) 0.3727(8) 0.6547(4) 0.0270 1.0000 Uani . . . . . .
C35 C -0.3523(7) 0.4342(7) 0.6367(5) 0.0372 1.0000 Uani . . . . . .
C36 C -0.4209(7) 0.4181(8) 0.5837(5) 0.0357 1.0000 Uani . . . . . .
C37 C -0.4005(7) 0.3404(7) 0.5480(4) 0.0373 1.0000 Uani . . . . . .
C38 C -0.3080(6) 0.2777(7) 0.5631(4) 0.0279 1.0000 Uani . . . . . .
C101 C 0.4012(7) 0.3437(7) 1.0619(4) 0.0301 1.0000 Uani . . . . . .
C102 C 0.5151(9) 0.3508(8) 1.0830(5) 0.0401 1.0000 Uani . . . . . .
C103 C 0.5526(10) 0.3692(10) 1.1423(5) 0.0544 1.0000 Uani . . . . . .
C104 C 0.4752(10) 0.3821(8) 1.1804(4) 0.0435 1.0000 Uani . . . . . .
C105 C 0.3655(11) 0.3798(10) 1.1573(5) 0.0563 1.0000 Uani . . . . . .
C106 C 0.3271(9) 0.3566(9) 1.1002(4) 0.0401 1.0000 Uani . . . . . .
C107 C 0.2963(5) 0.1854(7) 0.9810(3) 0.0190 1.0000 Uani . . . . . .
C108 C 0.2738(7) 0.1347(8) 1.0305(4) 0.0307 1.0000 Uani . . . . . .
C109 C 0.2324(7) 0.0382(8) 1.0238(4) 0.0369 1.0000 Uani . . . . . .
C110 C 0.2116(7) -0.0062(8) 0.9703(5) 0.0322 1.0000 Uani . . . . . .
C111 C 0.2285(7) 0.0479(8) 0.9205(5) 0.0368 1.0000 Uani . . . . . .
C112 C 0.2702(8) 0.1429(9) 0.9278(4) 0.0317 1.0000 Uani . . . . . .
C113 C 0.2391(7) 0.3909(7) 0.9584(4) 0.0267 1.0000 Uani . . . . . .
C114 C 0.1396(8) 0.3626(9) 0.9747(4) 0.0390 1.0000 Uani . . . . . .
C115 C 0.0416(8) 0.4161(8) 0.9594(4) 0.0366 1.0000 Uani . . . . . .
C116 C 0.0512(7) 0.5080(8) 0.9280(4) 0.0292 1.0000 Uani . . . . . .
C117 C 0.1480(7) 0.5336(8) 0.9101(4) 0.0337 1.0000 Uani . . . . . .
C118 C 0.2461(7) 0.4766(7) 0.9236(4) 0.0255 1.0000 Uani . . . . . .
C119 C 0.3397(6) 0.5949(9) 0.8630(5) 0.0432 1.0000 Uani . . . . . .
C120 C 0.4528(8) 0.6130(8) 0.8497(6) 0.0464 1.0000 Uani . . . . . .
C121 C 0.6150(7) 0.5007(6) 0.8340(4) 0.0193 1.0000 Uani . . . . . .
C122 C 0.6680(7) 0.5870(8) 0.8178(4) 0.0259 1.0000 Uani . . . . . .
C123 C 0.7735(8) 0.5820(9) 0.8046(4) 0.0335 1.0000 Uani . . . . . .
C124 C 0.8320(7) 0.4941(8) 0.8070(4) 0.0296 1.0000 Uani . . . . . .
C125 C 0.7831(7) 0.4070(8) 0.8229(4) 0.0266 1.0000 Uani . . . . . .
C126 C 0.6731(6) 0.4107(7) 0.8379(3) 0.0226 1.0000 Uani . . . . . .
C127 C 0.7346(6) 0.2121(9) 0.8796(4) 0.0273 1.0000 Uani . . . . . .
C128 C 0.7577(7) 0.1348(8) 0.8439(4) 0.0258 1.0000 Uani . . . . . .
C129 C 0.8491(7) 0.0741(8) 0.8629(4) 0.0352 1.0000 Uani . . . . . .
C130 C 0.9156(7) 0.0918(9) 0.9168(5) 0.0417 1.0000 Uani . . . . . .
C131 C 0.8920(6) 0.1702(8) 0.9524(4) 0.0341 1.0000 Uani . . . . . .
C132 C 0.8033(6) 0.2285(7) 0.9324(4) 0.0289 1.0000 Uani . . . . . .
C133 C 0.5289(7) 0.2441(7) 0.7948(4) 0.0283 1.0000 Uani . . . . . .
C134 C 0.5193(7) 0.2929(9) 0.7411(4) 0.0318 1.0000 Uani . . . . . .
C135 C 0.4416(8) 0.2572(9) 0.6941(4) 0.0423 1.0000 Uani . . . . . .
C136 C 0.3811(8) 0.1751(8) 0.6995(4) 0.0437 1.0000 Uani . . . . . .
C137 C 0.3928(9) 0.1244(8) 0.7535(5) 0.0465 1.0000 Uani . . . . . .
C138 C 0.4672(8) 0.1565(7) 0.8011(5) 0.0354 1.0000 Uani . . . . . .
H21 H 0.2173 0.3350 0.4297 0.0289 1.0000 Uiso R . . . . .
H31 H 0.2977 0.4921 0.4407 0.0331 1.0000 Uiso R . . . . .
H41 H 0.3251 0.5693 0.5319 0.0426 1.0000 Uiso R . . . . .
H51 H 0.2756 0.4903 0.6157 0.0392 1.0000 Uiso R . . . . .
H61 H 0.1999 0.3316 0.6059 0.0350 1.0000 Uiso R . . . . .
H81 H -0.0738 0.1776 0.4392 0.0318 1.0000 Uiso R . . . . .
H91 H -0.1359 0.1352 0.3421 0.0446 1.0000 Uiso R . . . . .
H101 H -0.0076 0.1102 0.2777 0.0533 1.0000 Uiso R . . . . .
H111 H 0.1813 0.1152 0.3116 0.0489 1.0000 Uiso R . . . . .
H121 H 0.2427 0.1356 0.4122 0.0427 1.0000 Uiso R . . . . .
H141 H 0.3660 0.2015 0.5058 0.0309 1.0000 Uiso R . . . . .
H151 H 0.5157 0.1002 0.5295 0.0319 1.0000 Uiso R . . . . .
H161 H 0.5070 -0.0344 0.5852 0.0381 1.0000 Uiso R . . . . .
H171 H 0.3391 -0.0841 0.6122 0.0269 1.0000 Uiso R . . . . .
H191 H 0.1855 -0.1428 0.6234 0.0512 1.0000 Uiso R . . . . .
H192 H 0.2156 -0.0653 0.6755 0.0509 1.0000 Uiso R . . . . .
H201 H 0.0002 -0.1490 0.6358 0.0377 1.0000 Uiso R . . . . .
H202 H 0.0499 -0.1129 0.7005 0.0381 1.0000 Uiso R . . . . .
H221 H -0.1377 -0.1385 0.6872 0.0288 1.0000 Uiso R . . . . .
H231 H -0.3184 -0.1322 0.7068 0.0280 1.0000 Uiso R . . . . .
H241 H -0.4144 0.0170 0.7021 0.0277 1.0000 Uiso R . . . . .
H251 H -0.3289 0.1573 0.6704 0.0269 1.0000 Uiso R . . . . .
H281 H -0.0606 0.1476 0.7592 0.0379 1.0000 Uiso R . . . . .
H291 H 0.0467 0.2097 0.8408 0.0500 1.0000 Uiso R . . . . .
H301 H 0.1551 0.3521 0.8326 0.0649 1.0000 Uiso R . . . . .
H311 H 0.1330 0.4389 0.7447 0.0451 1.0000 Uiso R . . . . .
H321 H 0.0163 0.3778 0.6630 0.0338 1.0000 Uiso R . . . . .
H341 H -0.2160 0.3839 0.6900 0.0323 1.0000 Uiso R . . . . .
H351 H -0.3665 0.4873 0.6605 0.0440 1.0000 Uiso R . . . . .
H361 H -0.4818 0.4592 0.5716 0.0429 1.0000 Uiso R . . . . .
H371 H -0.4484 0.3291 0.5130 0.0434 1.0000 Uiso R . . . . .
H381 H -0.2918 0.2285 0.5378 0.0342 1.0000 Uiso R . . . . .
H1021 H 0.5674 0.3423 1.0572 0.0479 1.0000 Uiso R . . . . .
H1031 H 0.6294 0.3733 1.1563 0.0648 1.0000 Uiso R . . . . .
H1041 H 0.4983 0.3912 1.2205 0.0525 1.0000 Uiso R . . . . .
H1061 H 0.2509 0.3491 1.0870 0.0478 1.0000 Uiso R . . . . .
H1081 H 0.2870 0.1644 1.0680 0.0370 1.0000 Uiso R . . . . .
H1091 H 0.2186 0.0032 1.0575 0.0454 1.0000 Uiso R . . . . .
H1101 H 0.1869 -0.0717 0.9661 0.0387 1.0000 Uiso R . . . . .
H1111 H 0.2116 0.0207 0.8824 0.0443 1.0000 Uiso R . . . . .
H1121 H 0.2839 0.1795 0.8951 0.0378 1.0000 Uiso R . . . . .
H1141 H 0.1374 0.3048 0.9970 0.0471 1.0000 Uiso R . . . . .
H1151 H -0.0259 0.3944 0.9697 0.0440 1.0000 Uiso R . . . . .
H1161 H -0.0108 0.5494 0.9193 0.0351 1.0000 Uiso R . . . . .
H1171 H 0.1504 0.5904 0.8881 0.0400 1.0000 Uiso R . . . . .
H1191 H 0.2887 0.5813 0.8272 0.0518 1.0000 Uiso R . . . . .
H1192 H 0.3142 0.6521 0.8827 0.0520 1.0000 Uiso R . . . . .
H1201 H 0.4493 0.6421 0.8108 0.0564 1.0000 Uiso R . . . . .
H1202 H 0.4945 0.6554 0.8794 0.0561 1.0000 Uiso R . . . . .
H1221 H 0.6315 0.6475 0.8164 0.0307 1.0000 Uiso R . . . . .
H1231 H 0.8067 0.6397 0.7931 0.0400 1.0000 Uiso R . . . . .
H1241 H 0.9046 0.4923 0.7986 0.0349 1.0000 Uiso R . . . . .
H1251 H 0.8226 0.3473 0.8244 0.0318 1.0000 Uiso R . . . . .
H1281 H 0.7135 0.1235 0.8082 0.0305 1.0000 Uiso R . . . . .
H1291 H 0.8660 0.0214 0.8396 0.0432 1.0000 Uiso R . . . . .
H1301 H 0.9762 0.0512 0.9293 0.0502 1.0000 Uiso R . . . . .
H1311 H 0.9359 0.1825 0.9887 0.0404 1.0000 Uiso R . . . . .
H1321 H 0.7872 0.2822 0.9548 0.0343 1.0000 Uiso R . . . . .
H1341 H 0.5613 0.3481 0.7363 0.0380 1.0000 Uiso R . . . . .
H1351 H 0.4336 0.2907 0.6586 0.0512 1.0000 Uiso R . . . . .
H1361 H 0.3306 0.1523 0.6675 0.0518 1.0000 Uiso R . . . . .
H1371 H 0.3493 0.0684 0.7570 0.0552 1.0000 Uiso R . . . . .
H1381 H 0.4763 0.1221 0.8366 0.0427 1.0000 Uiso R . . . . .
H1051 H 0.3135 0.3950 1.1821 0.0671 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pt1 0.01934(11) 0.01398(15) 0.01886(12) 0.00289(12) 0.00655(9) 0.00211(12)
Pt11 0.02796(14) 0.01483(17) 0.02653(15) 0.00233(13) 0.01193(12) 0.00150(12)
Cl1 0.0336(9) 0.0206(8) 0.0506(11) 0.0154(8) 0.0202(8) 0.0091(7)
Cl11 0.0487(12) 0.0473(15) 0.0704(15) 0.0432(13) 0.0322(11) 0.0239(10)
P1 0.0209(7) 0.0181(11) 0.0186(8) 0.0030(12) 0.0069(6) 0.0022(11)
P2 0.0203(9) 0.0122(12) 0.0203(10) -0.0006(9) 0.0042(9) 0.0007(9)
P3 0.019(3) 0.012(3) 0.019(3) -0.001(3) 0.005(3) 0.002(3)
P4 0.0189(7) 0.0167(14) 0.0191(8) -0.0011(10) 0.0049(6) 0.0024(9)
P5 0.0624(14) 0.0294(16) 0.0507(14) -0.0030(17) -0.0065(12) 0.0013(17)
P101 0.0256(8) 0.0177(11) 0.0211(8) -0.0009(12) 0.0097(7) -0.0006(11)
P102 0.0205(15) 0.0121(13) 0.0171(14) 0.0012(10) 0.0032(11) 0.0004(11)
P103 0.030(2) 0.017(3) 0.020(2) 0.002(2) 0.0113(19) 0.0004(19)
P104 0.0244(8) 0.0151(14) 0.0222(9) 0.0029(10) 0.0083(7) 0.0016(9)
P105 0.0661(14) 0.0221(14) 0.0525(14) -0.0083(17) -0.0101(12) 0.0046(17)
F1 0.109(5) 0.046(5) 0.113(6) 0.014(5) -0.072(5) -0.004(5)
F6 0.063(4) 0.055(6) 0.107(5) -0.019(5) -0.027(3) 0.019(4)
F101 0.119(5) 0.051(5) 0.110(6) 0.032(6) -0.072(5) -0.021(6)
F106 0.051(3) 0.039(5) 0.119(5) -0.015(4) -0.007(3) 0.012(3)
N1 0.027(3) 0.015(4) 0.021(3) 0.006(3) 0.007(2) -0.001(3)
N2 0.033(3) 0.011(3) 0.025(3) 0.005(3) 0.010(3) 0.003(3)
N101 0.024(3) 0.017(4) 0.036(4) -0.001(3) 0.006(3) 0.007(3)
N102 0.025(3) 0.019(4) 0.032(4) 0.005(3) 0.008(3) 0.001(3)
C1 0.023(3) 0.029(6) 0.021(3) -0.008(4) 0.006(3) -0.001(4)
C2 0.027(4) 0.022(4) 0.024(4) 0.012(3) 0.010(3) -0.003(3)
C3 0.021(3) 0.030(5) 0.032(4) 0.008(4) 0.000(3) 0.002(3)
C4 0.018(3) 0.026(5) 0.061(6) 0.004(5) -0.002(4) 0.003(3)
C5 0.032(4) 0.027(6) 0.039(5) -0.010(4) 0.005(4) -0.007(4)
C6 0.029(4) 0.028(5) 0.034(5) -0.005(4) 0.019(3) -0.008(3)
C7 0.036(4) 0.015(4) 0.012(3) -0.004(3) 0.010(3) 0.002(3)
C8 0.029(4) 0.022(4) 0.028(4) 0.000(4) 0.001(3) -0.009(3)
C9 0.052(5) 0.021(5) 0.039(5) -0.005(4) 0.003(4) -0.008(4)
C10 0.082(8) 0.029(7) 0.021(4) -0.003(4) -0.009(5) 0.008(5)
C11 0.069(7) 0.039(7) 0.018(4) 0.003(4) 0.024(4) 0.014(5)
C12 0.042(4) 0.044(6) 0.023(4) -0.002(4) 0.009(4) 0.013(4)
C13 0.016(3) 0.019(5) 0.016(3) 0.004(3) 0.007(3) 0.001(3)
C14 0.033(4) 0.014(4) 0.034(4) 0.001(4) 0.017(3) 0.006(3)
C15 0.015(3) 0.024(5) 0.042(4) -0.005(4) 0.011(3) 0.005(3)
C16 0.026(4) 0.030(5) 0.037(5) -0.008(4) 0.003(3) 0.008(4)
C17 0.022(3) 0.018(4) 0.029(4) 0.005(3) 0.007(3) -0.003(3)
C18 0.018(3) 0.016(4) 0.022(4) -0.010(3) 0.008(3) 0.002(3)
C19 0.053(5) 0.019(5) 0.056(6) 0.020(4) 0.010(5) -0.002(4)
C20 0.040(4) 0.012(3) 0.048(4) 0.016(3) 0.025(3) 0.012(3)
C21 0.022(3) 0.032(5) 0.022(4) -0.004(4) 0.006(3) 0.008(3)
C22 0.036(4) 0.014(4) 0.021(4) -0.001(3) 0.001(3) 0.005(3)
C23 0.029(4) 0.016(4) 0.027(4) 0.002(3) 0.011(3) -0.014(3)
C24 0.024(3) 0.027(5) 0.021(4) 0.007(3) 0.010(3) -0.002(3)
C25 0.026(4) 0.018(5) 0.023(4) 0.001(4) 0.002(3) 0.005(3)
C26 0.020(3) 0.009(4) 0.022(4) 0.002(3) 0.005(3) 0.003(3)
C27 0.019(3) 0.014(4) 0.024(4) -0.005(3) 0.005(3) 0.002(3)
C28 0.039(4) 0.025(5) 0.031(4) 0.004(5) 0.006(3) 0.003(5)
C29 0.059(5) 0.041(6) 0.025(4) 0.000(4) 0.007(4) 0.000(4)
C30 0.078(7) 0.038(8) 0.036(5) -0.019(5) -0.015(5) 0.000(5)
C31 0.034(4) 0.023(5) 0.053(6) -0.006(4) 0.001(4) -0.006(3)
C32 0.033(4) 0.034(6) 0.019(3) 0.000(3) 0.004(3) 0.001(3)
C33 0.019(3) 0.014(5) 0.025(3) 0.000(4) 0.009(3) 0.004(3)
C34 0.029(4) 0.023(5) 0.031(4) 0.004(4) 0.013(4) 0.002(4)
C35 0.032(4) 0.016(5) 0.066(7) 0.012(5) 0.015(4) 0.009(4)
C36 0.029(4) 0.022(5) 0.059(6) 0.014(5) 0.020(4) 0.006(4)
C37 0.024(4) 0.028(5) 0.056(5) 0.015(4) -0.005(4) -0.001(3)
C38 0.024(3) 0.028(6) 0.032(4) 0.008(4) 0.003(3) -0.001(3)
C101 0.036(4) 0.019(5) 0.036(4) 0.007(4) 0.009(4) -0.002(3)
C102 0.050(5) 0.035(6) 0.035(5) -0.007(5) 0.006(4) -0.007(4)
C103 0.069(7) 0.049(7) 0.037(6) 0.002(5) -0.019(6) -0.028(6)
C104 0.084(8) 0.019(6) 0.031(5) -0.010(4) 0.019(5) 0.006(5)
C105 0.075(8) 0.055(9) 0.036(6) -0.017(5) 0.001(5) 0.035(6)
C106 0.058(5) 0.033(5) 0.033(4) 0.001(4) 0.017(4) 0.014(4)
C107 0.020(3) 0.011(5) 0.027(3) 0.008(3) 0.010(3) 0.002(3)
C108 0.021(4) 0.032(5) 0.037(5) -0.004(4) -0.001(3) 0.005(3)
C109 0.041(4) 0.030(5) 0.038(5) 0.019(4) -0.001(4) -0.016(4)
C110 0.031(4) 0.018(5) 0.047(5) 0.005(4) 0.003(4) -0.005(3)
C111 0.034(4) 0.033(6) 0.048(6) -0.010(5) 0.019(4) -0.001(4)
C112 0.041(5) 0.030(5) 0.026(4) -0.002(4) 0.012(4) -0.004(4)
C113 0.028(4) 0.023(5) 0.028(4) -0.009(4) 0.003(3) 0.008(3)
C114 0.038(5) 0.040(6) 0.039(5) 0.005(5) 0.005(4) -0.001(5)
C115 0.038(4) 0.033(6) 0.040(5) 0.003(4) 0.008(4) -0.007(4)
C116 0.026(4) 0.025(5) 0.038(5) -0.006(4) 0.008(3) 0.005(3)
C117 0.038(4) 0.029(6) 0.034(5) -0.005(4) 0.004(4) 0.016(4)
C118 0.038(4) 0.015(5) 0.023(4) 0.001(3) 0.002(3) 0.001(4)
C119 0.021(4) 0.040(6) 0.073(7) 0.024(5) 0.023(4) 0.015(4)
C120 0.037(4) 0.023(5) 0.084(7) 0.016(5) 0.025(5) 0.012(4)
C121 0.030(4) 0.012(4) 0.015(3) 0.005(3) 0.002(3) -0.005(3)
C122 0.032(4) 0.024(5) 0.024(4) 0.004(4) 0.011(3) -0.007(4)
C123 0.043(5) 0.036(6) 0.023(4) 0.002(4) 0.009(4) -0.004(4)
C124 0.029(4) 0.034(6) 0.028(4) -0.006(4) 0.011(3) -0.008(4)
C125 0.029(4) 0.030(5) 0.024(4) -0.001(4) 0.010(3) -0.006(4)
C126 0.030(4) 0.025(5) 0.014(3) 0.002(3) 0.008(3) -0.007(3)
C127 0.030(4) 0.026(6) 0.029(4) 0.010(4) 0.011(3) -0.005(4)
C128 0.028(4) 0.019(5) 0.031(5) 0.004(4) 0.008(4) 0.007(3)
C129 0.044(5) 0.029(6) 0.036(5) 0.003(4) 0.017(4) 0.012(4)
C130 0.023(4) 0.040(7) 0.061(6) 0.023(6) 0.002(4) 0.004(4)
C131 0.026(3) 0.046(7) 0.032(4) 0.011(4) 0.008(3) -0.002(3)
C132 0.032(4) 0.024(5) 0.031(4) -0.008(3) 0.004(3) -0.004(3)
C133 0.031(4) 0.026(5) 0.028(4) -0.005(4) 0.004(4) 0.004(3)
C134 0.037(4) 0.031(6) 0.027(4) -0.001(4) 0.002(3) -0.001(4)
C135 0.042(5) 0.049(7) 0.031(4) 0.005(4) -0.008(4) 0.003(4)
C136 0.049(5) 0.034(7) 0.043(5) -0.008(4) -0.011(4) -0.002(4)
C137 0.057(6) 0.035(7) 0.041(5) -0.007(4) -0.014(5) -0.010(4)
C138 0.045(5) 0.013(4) 0.046(5) -0.004(4) 0.000(4) -0.008(4)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.074091(6)
loop_
_oxford_twin_element_scale_factors
0.500(7)
0.500(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 . Cl1 . 2.354(2) yes
Pt1 . P1 . 2.2906(19) yes
Pt1 . P2 . 2.162(2) yes
Pt1 . P3 . 2.18(3) yes
Pt1 . P4 . 2.298(2) yes
Pt11 . Cl11 . 2.310(2) yes
Pt11 . P101 . 2.308(2) yes
Pt11 . P102 . 2.212(4) yes
Pt11 . P103 . 2.142(5) yes
Pt11 . P104 . 2.300(2) yes
P1 . C1 . 1.819(11) yes
P1 . C7 . 1.812(7) yes
P1 . C13 . 1.794(8) yes
P2 . N1 . 1.644(7) yes
P2 . N2 . 1.672(8) yes
P3 . N1 . 1.67(4) yes
P3 . N2 . 1.62(4) yes
P4 . C26 . 1.813(9) yes
P4 . C27 . 1.802(7) yes
P4 . C33 . 1.803(8) yes
P5 . F1 . 1.582(6) yes
P5 . F6 . 1.607(6) yes
P5 . F21 . 1.491(16) yes
P5 . F22 . 1.53(2) yes
P5 . F23 . 1.623(12) yes
P5 . F24 . 1.61(3) yes
P5 . F1 . 1.582(6) yes
P5 . F2 . 1.637(9) yes
P5 . F3 . 1.505(11) yes
P5 . F4 . 1.703(12) yes
P5 . F5 . 1.553(12) yes
P5 . F6 . 1.607(6) yes
P101 . C101 . 1.808(9) yes
P101 . C107 . 1.815(10) yes
P101 . C113 . 1.838(9) yes
P102 . N101 . 1.640(8) yes
P102 . N102 . 1.674(9) yes
P103 . N101 . 1.688(8) yes
P103 . N102 . 1.701(9) yes
P104 . C126 . 1.816(10) yes
P104 . C127 . 1.797(10) yes
P104 . C133 . 1.821(8) yes
P105 . F101 . 1.569(6) yes
P105 . F102 . 1.535(12) yes
P105 . F103 . 1.628(12) yes
P105 . F104 . 1.543(9) yes
P105 . F105 . 1.745(12) yes
P105 . F106 . 1.595(6) yes
P105 . F101 . 1.569(6) yes
P105 . F106 . 1.595(6) yes
P105 . F121 . 1.60(2) yes
P105 . F122 . 1.639(14) yes
P105 . F123 . 1.611(15) yes
P105 . F124 . 1.516(12) yes
N1 . C18 . 1.419(11) yes
N1 . C19 . 1.489(11) yes
N2 . C20 . 1.460(11) yes
N2 . C21 . 1.420(11) yes
N101 . C118 . 1.409(12) yes
N101 . C119 . 1.482(13) yes
N102 . C120 . 1.521(13) yes
N102 . C121 . 1.409(11) yes
C1 . C2 . 1.383(12) yes
C1 . C6 . 1.443(13) yes
C2 . C3 . 1.393(13) yes
C2 . H21 . 0.937 no
C3 . C4 . 1.370(14) yes
C3 . H31 . 0.937 no
C4 . C5 . 1.411(15) yes
C4 . H41 . 0.936 no
C5 . C6 . 1.382(14) yes
C5 . H51 . 0.943 no
C6 . H61 . 0.929 no
C7 . C8 . 1.375(10) yes
C7 . C12 . 1.410(12) yes
C8 . C9 . 1.389(12) yes
C8 . H81 . 0.924 no
C9 . C10 . 1.395(16) yes
C9 . H91 . 0.937 no
C10 . C11 . 1.377(15) yes
C10 . H101 . 0.923 no
C11 . C12 . 1.391(13) yes
C11 . H111 . 0.928 no
C12 . H121 . 0.924 no
C13 . C14 . 1.422(11) yes
C13 . C18 . 1.410(12) yes
C14 . C15 . 1.375(11) yes
C14 . H141 . 0.933 no
C15 . C16 . 1.304(14) yes
C15 . H151 . 0.920 no
C16 . C17 . 1.402(12) yes
C16 . H161 . 0.927 no
C17 . C18 . 1.404(11) yes
C17 . H171 . 0.921 no
C19 . C20 . 1.573(13) yes
C19 . H191 . 0.969 no
C19 . H192 . 0.970 no
C20 . H201 . 0.964 no
C20 . H202 . 0.967 no
C21 . C22 . 1.414(14) yes
C21 . C26 . 1.402(13) yes
C22 . C23 . 1.377(12) yes
C22 . H221 . 0.929 no
C23 . C24 . 1.376(14) yes
C23 . H231 . 0.933 no
C24 . C25 . 1.388(13) yes
C24 . H241 . 0.938 no
C25 . C26 . 1.381(10) yes
C25 . H251 . 0.931 no
C27 . C28 . 1.404(12) yes
C27 . C32 . 1.367(13) yes
C28 . C29 . 1.367(12) yes
C28 . H281 . 0.928 no
C29 . C30 . 1.402(16) yes
C29 . H291 . 0.910 no
C30 . C31 . 1.370(15) yes
C30 . H301 . 0.941 no
C31 . C32 . 1.393(12) yes
C31 . H311 . 0.931 no
C32 . H321 . 0.928 no
C33 . C34 . 1.410(13) yes
C33 . C38 . 1.400(10) yes
C34 . C35 . 1.381(12) yes
C34 . H341 . 0.923 no
C35 . C36 . 1.380(13) yes
C35 . H351 . 0.930 no
C36 . C37 . 1.373(14) yes
C36 . H361 . 0.930 no
C37 . C38 . 1.404(11) yes
C37 . H371 . 0.926 no
C38 . H381 . 0.920 no
C101 . C102 . 1.394(12) yes
C101 . C106 . 1.358(14) yes
C102 . C103 . 1.386(14) yes
C102 . H1021 . 0.937 no
C103 . C104 . 1.384(17) yes
C103 . H1031 . 0.938 no
C104 . C105 . 1.355(16) yes
C104 . H1041 . 0.925 no
C105 . C106 . 1.352(14) yes
C105 . H1051 . 0.933 no
C106 . H1061 . 0.933 no
C107 . C108 . 1.384(13) yes
C107 . C112 . 1.338(12) yes
C108 . C109 . 1.393(14) yes
C108 . H1081 . 0.938 no
C109 . C110 . 1.352(14) yes
C109 . H1091 . 0.940 no
C110 . C111 . 1.393(14) yes
C110 . H1101 . 0.933 no
C111 . C112 . 1.377(15) yes
C111 . H1111 . 0.938 no
C112 . H1121 . 0.931 no
C113 . C114 . 1.370(13) yes
C113 . C118 . 1.413(14) yes
C114 . C115 . 1.388(14) yes
C114 . H1141 . 0.933 no
C115 . C116 . 1.444(14) yes
C115 . H1151 . 0.933 no
C116 . C117 . 1.345(13) yes
C116 . H1161 . 0.933 no
C117 . C118 . 1.410(12) yes
C117 . H1171 . 0.919 no
C119 . C120 . 1.469(12) yes
C119 . H1191 . 0.964 no
C119 . H1192 . 0.968 no
C120 . H1201 . 0.968 no
C120 . H1202 . 0.968 no
C121 . C122 . 1.405(12) yes
C121 . C126 . 1.399(13) yes
C122 . C123 . 1.360(12) yes
C122 . H1221 . 0.925 no
C123 . C124 . 1.376(15) yes
C123 . H1231 . 0.931 no
C124 . C125 . 1.388(14) yes
C124 . H1241 . 0.929 no
C125 . C126 . 1.427(11) yes
C125 . H1251 . 0.933 no
C127 . C128 . 1.379(15) yes
C127 . C132 . 1.376(10) yes
C128 . C129 . 1.393(12) yes
C128 . H1281 . 0.917 no
C129 . C130 . 1.386(13) yes
C129 . H1291 . 0.931 no
C130 . C131 . 1.390(15) yes
C130 . H1301 . 0.925 no
C131 . C132 . 1.353(12) yes
C131 . H1311 . 0.930 no
C132 . H1321 . 0.925 no
C133 . C134 . 1.381(13) yes
C133 . C138 . 1.417(13) yes
C134 . C135 . 1.402(12) yes
C134 . H1341 . 0.918 no
C135 . C136 . 1.344(15) yes
C135 . H1351 . 0.921 no
C136 . C137 . 1.400(15) yes
C136 . H1361 . 0.931 no
C137 . C138 . 1.373(12) yes
C137 . H1371 . 0.931 no
C138 . H1381 . 0.927 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Pt1 . P1 . 91.21(10) yes
Cl1 . Pt1 . P2 . 170.83(8) yes
P1 . Pt1 . P2 . 88.55(11) yes
Cl1 . Pt1 . P3 . 160.6(9) yes
P1 . Pt1 . P3 . 92.3(9) yes
Cl1 . Pt1 . P4 . 91.04(10) yes
P1 . Pt1 . P4 . 168.22(6) yes
P2 . Pt1 . P4 . 91.06(10) yes
P3 . Pt1 . P4 . 81.8(9) yes
Cl11 . Pt11 . P101 . 89.42(10) yes
Cl11 . Pt11 . P102 . 170.16(13) yes
P101 . Pt11 . P102 . 91.11(12) yes
Cl11 . Pt11 . P103 . 159.63(15) yes
P101 . Pt11 . P103 . 88.84(16) yes
P102 . Pt11 . P103 . 30.21(15) yes
Cl11 . Pt11 . P104 . 93.21(10) yes
P101 . Pt11 . P104 . 169.72(7) yes
P102 . Pt11 . P104 . 84.61(12) yes
P103 . Pt11 . P104 . 92.09(15) yes
Pt1 . P1 . C1 . 108.4(3) yes
Pt1 . P1 . C7 . 113.0(3) yes
C1 . P1 . C7 . 108.4(4) yes
Pt1 . P1 . C13 . 115.9(3) yes
C1 . P1 . C13 . 102.3(4) yes
C7 . P1 . C13 . 108.2(4) yes
Pt1 . P2 . N1 . 120.4(3) yes
Pt1 . P2 . N2 . 118.5(3) yes
N1 . P2 . N2 . 95.5(3) yes
Pt1 . P3 . N1 . 118.2(17) yes
Pt1 . P3 . N2 . 120.3(15) yes
N1 . P3 . N2 . 96.3(20) yes
Pt1 . P4 . C26 . 116.9(3) yes
Pt1 . P4 . C27 . 105.3(3) yes
C26 . P4 . C27 . 106.1(4) yes
Pt1 . P4 . C33 . 114.1(3) yes
C26 . P4 . C33 . 105.4(4) yes
C27 . P4 . C33 . 108.7(4) yes
F1 . P5 . F6 . 179.1(6) yes
F1 . P5 . F21 . 89.5(7) yes
F6 . P5 . F21 . 89.7(7) yes
F1 . P5 . F22 . 92.5(8) yes
F6 . P5 . F22 . 88.2(8) yes
F21 . P5 . F22 . 95.7(12) yes
F1 . P5 . F23 . 87.3(5) yes
F6 . P5 . F23 . 93.4(5) yes
F21 . P5 . F23 . 173.9(9) yes
F22 . P5 . F23 . 89.7(11) yes
F1 . P5 . F24 . 81.4(9) yes
F6 . P5 . F24 . 98.0(9) yes
F21 . P5 . F24 . 91.1(13) yes
F22 . P5 . F24 . 170.9(14) yes
F23 . P5 . F24 . 83.3(12) yes
F1 . P5 . F2 . 90.8(5) yes
F1 . P5 . F3 . 93.9(5) yes
F2 . P5 . F3 . 91.4(6) yes
F1 . P5 . F4 . 100.7(5) yes
F2 . P5 . F4 . 168.1(5) yes
F3 . P5 . F4 . 90.8(6) yes
F1 . P5 . F5 . 89.0(6) yes
F2 . P5 . F5 . 88.1(6) yes
F3 . P5 . F5 . 177.0(5) yes
F4 . P5 . F5 . 89.0(7) yes
F1 . P5 . F6 . 179.1(6) yes
F2 . P5 . F6 . 89.1(4) yes
F3 . P5 . F6 . 87.0(5) yes
F4 . P5 . F6 . 79.4(5) yes
F5 . P5 . F6 . 90.0(5) yes
Pt11 . P101 . C101 . 113.9(3) yes
Pt11 . P101 . C107 . 106.3(3) yes
C101 . P101 . C107 . 110.6(4) yes
Pt11 . P101 . C113 . 115.6(3) yes
C101 . P101 . C113 . 105.8(4) yes
C107 . P101 . C113 . 104.2(4) yes
Pt11 . P102 . N101 . 117.9(3) yes
Pt11 . P102 . N102 . 117.0(3) yes
N101 . P102 . N102 . 96.5(4) yes
Pt11 . P103 . N101 . 119.3(4) yes
Pt11 . P103 . N102 . 119.3(4) yes
N101 . P103 . N102 . 93.7(4) yes
Pt11 . P104 . C126 . 115.1(3) yes
Pt11 . P104 . C127 . 114.7(3) yes
C126 . P104 . C127 . 106.8(4) yes
Pt11 . P104 . C133 . 103.8(3) yes
C126 . P104 . C133 . 106.9(4) yes
C127 . P104 . C133 . 109.2(5) yes
F101 . P105 . F102 . 90.3(6) yes
F101 . P105 . F103 . 100.1(5) yes
F102 . P105 . F103 . 96.7(7) yes
F101 . P105 . F104 . 91.1(6) yes
F102 . P105 . F104 . 175.0(7) yes
F103 . P105 . F104 . 87.8(6) yes
F101 . P105 . F105 . 88.3(5) yes
F102 . P105 . F105 . 85.0(6) yes
F103 . P105 . F105 . 171.4(5) yes
F104 . P105 . F105 . 90.3(6) yes
F101 . P105 . F106 . 178.8(6) yes
F102 . P105 . F106 . 88.9(5) yes
F103 . P105 . F106 . 80.9(5) yes
F104 . P105 . F106 . 89.6(4) yes
F105 . P105 . F106 . 90.7(5) yes
F101 . P105 . F106 . 178.8(6) yes
F101 . P105 . F121 . 82.9(8) yes
F106 . P105 . F121 . 97.2(8) yes
F101 . P105 . F122 . 85.5(6) yes
F106 . P105 . F122 . 95.7(5) yes
F121 . P105 . F122 . 87.0(10) yes
F101 . P105 . F123 . 89.9(6) yes
F106 . P105 . F123 . 90.1(6) yes
F121 . P105 . F123 . 168.9(10) yes
F122 . P105 . F123 . 84.0(8) yes
F101 . P105 . F124 . 86.2(5) yes
F106 . P105 . F124 . 92.7(5) yes
F121 . P105 . F124 . 93.9(9) yes
F122 . P105 . F124 . 171.4(6) yes
F123 . P105 . F124 . 94.0(8) yes
P3 . N1 . C18 . 122.6(13) yes
P2 . N1 . C18 . 130.1(6) yes
P3 . N1 . C19 . 104.4(13) yes
P2 . N1 . C19 . 111.9(6) yes
C18 . N1 . C19 . 118.1(7) yes
P2 . N2 . C20 . 106.1(6) yes
P3 . N2 . C20 . 111.5(13) yes
P2 . N2 . C21 . 122.3(6) yes
P3 . N2 . C21 . 131.0(13) yes
C20 . N2 . C21 . 117.5(8) yes
P103 . N101 . C118 . 131.6(6) yes
P102 . N101 . C118 . 120.6(7) yes
P103 . N101 . C119 . 109.2(6) yes
P102 . N101 . C119 . 103.6(6) yes
C118 . N101 . C119 . 119.2(6) yes
P103 . N102 . C120 . 101.7(7) yes
P102 . N102 . C120 . 108.2(6) yes
P103 . N102 . C121 . 121.5(6) yes
P102 . N102 . C121 . 131.0(6) yes
C120 . N102 . C121 . 120.8(8) yes
P1 . C1 . C2 . 123.9(7) yes
P1 . C1 . C6 . 115.8(7) yes
C2 . C1 . C6 . 120.2(10) yes
C1 . C2 . C3 . 119.3(9) yes
C1 . C2 . H21 . 119.7 no
C3 . C2 . H21 . 120.9 no
C2 . C3 . C4 . 120.9(9) yes
C2 . C3 . H31 . 118.9 no
C4 . C3 . H31 . 120.2 no
C3 . C4 . C5 . 121.2(10) yes
C3 . C4 . H41 . 120.0 no
C5 . C4 . H41 . 118.9 no
C4 . C5 . C6 . 119.1(9) yes
C4 . C5 . H51 . 120.9 no
C6 . C5 . H51 . 120.0 no
C1 . C6 . C5 . 119.3(10) yes
C1 . C6 . H61 . 120.3 no
C5 . C6 . H61 . 120.4 no
P1 . C7 . C8 . 118.5(6) yes
P1 . C7 . C12 . 121.6(6) yes
C8 . C7 . C12 . 119.9(7) yes
C7 . C8 . C9 . 119.9(9) yes
C7 . C8 . H81 . 121.1 no
C9 . C8 . H81 . 118.9 no
C8 . C9 . C10 . 120.1(9) yes
C8 . C9 . H91 . 120.0 no
C10 . C9 . H91 . 119.9 no
C9 . C10 . C11 . 120.4(9) yes
C9 . C10 . H101 . 119.9 no
C11 . C10 . H101 . 119.7 no
C10 . C11 . C12 . 119.5(10) yes
C10 . C11 . H111 . 120.4 no
C12 . C11 . H111 . 120.1 no
C7 . C12 . C11 . 119.9(9) yes
C7 . C12 . H121 . 119.8 no
C11 . C12 . H121 . 120.2 no
P1 . C13 . C14 . 117.3(6) yes
P1 . C13 . C18 . 125.7(6) yes
C14 . C13 . C18 . 116.9(7) yes
C13 . C14 . C15 . 121.6(8) yes
C13 . C14 . H141 . 119.7 no
C15 . C14 . H141 . 118.8 no
C14 . C15 . C16 . 121.0(8) yes
C14 . C15 . H151 . 118.9 no
C16 . C15 . H151 . 120.1 no
C15 . C16 . C17 . 121.1(8) yes
C15 . C16 . H161 . 120.0 no
C17 . C16 . H161 . 118.9 no
C16 . C17 . C18 . 120.1(8) yes
C16 . C17 . H171 . 120.2 no
C18 . C17 . H171 . 119.7 no
N1 . C18 . C13 . 124.1(7) yes
N1 . C18 . C17 . 116.4(8) yes
C13 . C18 . C17 . 119.2(7) yes
N1 . C19 . C20 . 104.9(7) yes
N1 . C19 . H191 . 109.9 no
C20 . C19 . H191 . 111.3 no
N1 . C19 . H192 . 109.3 no
C20 . C19 . H192 . 111.8 no
H191 . C19 . H192 . 109.6 no
C19 . C20 . N2 . 106.6(7) yes
C19 . C20 . H201 . 111.6 no
N2 . C20 . H201 . 111.4 no
C19 . C20 . H202 . 107.9 no
N2 . C20 . H202 . 108.8 no
H201 . C20 . H202 . 110.5 no
N2 . C21 . C22 . 119.6(8) yes
N2 . C21 . C26 . 122.1(9) yes
C22 . C21 . C26 . 118.1(8) yes
C21 . C22 . C23 . 120.9(9) yes
C21 . C22 . H221 . 119.0 no
C23 . C22 . H221 . 120.1 no
C22 . C23 . C24 . 121.0(8) yes
C22 . C23 . H231 . 119.5 no
C24 . C23 . H231 . 119.5 no
C23 . C24 . C25 . 118.0(8) yes
C23 . C24 . H241 . 121.0 no
C25 . C24 . H241 . 121.1 no
C24 . C25 . C26 . 123.0(9) yes
C24 . C25 . H251 . 118.9 no
C26 . C25 . H251 . 118.1 no
P4 . C26 . C21 . 122.5(6) yes
P4 . C26 . C25 . 118.6(7) yes
C21 . C26 . C25 . 118.8(8) yes
P4 . C27 . C28 . 121.6(7) yes
P4 . C27 . C32 . 119.8(7) yes
C28 . C27 . C32 . 118.5(8) yes
C27 . C28 . C29 . 122.0(11) yes
C27 . C28 . H281 . 119.6 no
C29 . C28 . H281 . 118.4 no
C28 . C29 . C30 . 117.9(10) yes
C28 . C29 . H291 . 120.0 no
C30 . C29 . H291 . 122.0 no
C29 . C30 . C31 . 121.2(8) yes
C29 . C30 . H301 . 119.4 no
C31 . C30 . H301 . 119.3 no
C30 . C31 . C32 . 119.4(9) yes
C30 . C31 . H311 . 120.6 no
C32 . C31 . H311 . 120.0 no
C31 . C32 . C27 . 120.9(9) yes
C31 . C32 . H321 . 119.5 no
C27 . C32 . H321 . 119.6 no
P4 . C33 . C34 . 121.8(5) yes
P4 . C33 . C38 . 117.3(7) yes
C34 . C33 . C38 . 120.8(8) yes
C33 . C34 . C35 . 119.2(8) yes
C33 . C34 . H341 . 120.2 no
C35 . C34 . H341 . 120.6 no
C34 . C35 . C36 . 120.6(10) yes
C34 . C35 . H351 . 119.8 no
C36 . C35 . H351 . 119.6 no
C35 . C36 . C37 . 120.3(8) yes
C35 . C36 . H361 . 120.8 no
C37 . C36 . H361 . 118.9 no
C36 . C37 . C38 . 121.4(8) yes
C36 . C37 . H371 . 119.5 no
C38 . C37 . H371 . 119.1 no
C37 . C38 . C33 . 117.6(9) yes
C37 . C38 . H381 . 121.1 no
C33 . C38 . H381 . 121.2 no
P101 . C101 . C102 . 119.0(8) yes
P101 . C101 . C106 . 121.8(7) yes
C102 . C101 . C106 . 119.0(9) yes
C101 . C102 . C103 . 120.7(11) yes
C101 . C102 . H1021 . 120.2 no
C103 . C102 . H1021 . 119.0 no
C102 . C103 . C104 . 119.0(10) yes
C102 . C103 . H1031 . 120.3 no
C104 . C103 . H1031 . 120.7 no
C103 . C104 . C105 . 118.0(9) yes
C103 . C104 . H1041 . 120.6 no
C105 . C104 . H1041 . 121.3 no
C104 . C105 . C106 . 123.7(12) yes
C104 . C105 . H1051 . 118.0 no
C106 . C105 . H1051 . 118.2 no
C101 . C106 . C105 . 119.1(11) yes
C101 . C106 . H1061 . 119.7 no
C105 . C106 . H1061 . 121.1 no
P101 . C107 . C108 . 122.2(7) yes
P101 . C107 . C112 . 118.8(7) yes
C108 . C107 . C112 . 119.0(9) yes
C107 . C108 . C109 . 118.9(9) yes
C107 . C108 . H1081 . 120.7 no
C109 . C108 . H1081 . 120.5 no
C108 . C109 . C110 . 121.8(9) yes
C108 . C109 . H1091 . 119.0 no
C110 . C109 . H1091 . 119.2 no
C109 . C110 . C111 . 118.6(9) yes
C109 . C110 . H1101 . 121.7 no
C111 . C110 . H1101 . 119.8 no
C110 . C111 . C112 . 119.0(10) yes
C110 . C111 . H1111 . 121.0 no
C112 . C111 . H1111 . 120.0 no
C111 . C112 . C107 . 122.6(10) yes
C111 . C112 . H1121 . 120.2 no
C107 . C112 . H1121 . 117.2 no
P101 . C113 . C114 . 114.3(8) yes
P101 . C113 . C118 . 124.9(7) yes
C114 . C113 . C118 . 120.8(8) yes
C113 . C114 . C115 . 122.7(10) yes
C113 . C114 . H1141 . 118.7 no
C115 . C114 . H1141 . 118.5 no
C114 . C115 . C116 . 116.2(9) yes
C114 . C115 . H1151 . 121.5 no
C116 . C115 . H1151 . 122.3 no
C115 . C116 . C117 . 120.7(9) yes
C115 . C116 . H1161 . 119.8 no
C117 . C116 . H1161 . 119.5 no
C116 . C117 . C118 . 122.7(10) yes
C116 . C117 . H1171 . 118.8 no
C118 . C117 . H1171 . 118.5 no
C113 . C118 . C117 . 116.5(9) yes
C113 . C118 . N101 . 124.0(8) yes
C117 . C118 . N101 . 119.5(8) yes
N101 . C119 . C120 . 108.0(7) yes
N101 . C119 . H1191 . 109.3 no
C120 . C119 . H1191 . 110.8 no
N101 . C119 . H1192 . 109.3 no
C120 . C119 . H1192 . 109.8 no
H1191 . C119 . H1192 . 109.7 no
N102 . C120 . C119 . 105.8(9) yes
N102 . C120 . H1201 . 109.0 no
C119 . C120 . H1201 . 110.3 no
N102 . C120 . H1202 . 110.3 no
C119 . C120 . H1202 . 110.9 no
H1201 . C120 . H1202 . 110.4 no
N102 . C121 . C122 . 117.4(8) yes
N102 . C121 . C126 . 123.3(8) yes
C122 . C121 . C126 . 119.2(8) yes
C121 . C122 . C123 . 120.0(10) yes
C121 . C122 . H1221 . 120.1 no
C123 . C122 . H1221 . 119.8 no
C122 . C123 . C124 . 122.0(10) yes
C122 . C123 . H1231 . 118.8 no
C124 . C123 . H1231 . 119.2 no
C123 . C124 . C125 . 120.0(9) yes
C123 . C124 . H1241 . 120.8 no
C125 . C124 . H1241 . 119.1 no
C124 . C125 . C126 . 119.0(10) yes
C124 . C125 . H1251 . 120.1 no
C126 . C125 . H1251 . 120.9 no
P104 . C126 . C125 . 115.8(7) yes
P104 . C126 . C121 . 124.5(6) yes
C125 . C126 . C121 . 119.7(9) yes
P104 . C127 . C128 . 122.3(6) yes
P104 . C127 . C132 . 118.2(8) yes
C128 . C127 . C132 . 119.5(8) yes
C127 . C128 . C129 . 118.7(8) yes
C127 . C128 . H1281 . 120.6 no
C129 . C128 . H1281 . 120.7 no
C128 . C129 . C130 . 120.3(10) yes
C128 . C129 . H1291 . 120.2 no
C130 . C129 . H1291 . 119.5 no
C129 . C130 . C131 . 120.5(8) yes
C129 . C130 . H1301 . 120.0 no
C131 . C130 . H1301 . 119.5 no
C130 . C131 . C132 . 117.8(8) yes
C130 . C131 . H1311 . 121.1 no
C132 . C131 . H1311 . 121.0 no
C127 . C132 . C131 . 123.1(9) yes
C127 . C132 . H1321 . 117.5 no
C131 . C132 . H1321 . 119.4 no
P104 . C133 . C134 . 120.7(8) yes
P104 . C133 . C138 . 118.4(7) yes
C134 . C133 . C138 . 120.8(9) yes
C133 . C134 . C135 . 118.4(10) yes
C133 . C134 . H1341 . 121.2 no
C135 . C134 . H1341 . 120.4 no
C134 . C135 . C136 . 121.6(10) yes
C134 . C135 . H1351 . 118.5 no
C136 . C135 . H1351 . 119.9 no
C135 . C136 . C137 . 120.0(9) yes
C135 . C136 . H1361 . 120.1 no
C137 . C136 . H1361 . 119.9 no
C136 . C137 . C138 . 120.8(10) yes
C136 . C137 . H1371 . 119.2 no
C138 . C137 . H1371 . 119.9 no
C133 . C138 . C137 . 118.3(10) yes
C133 . C138 . H1381 . 120.8 no
C137 . C138 . H1381 . 120.9 no
_iucr_refine_instruction_details_constraints
;
#
# Punched on 16/02/12 at 14:12:10
#
#LIST 12
BLOCK
CONT SCALE
CONT PT ( 1 ,X'S,U'S) UNTIL F ( 1 )
CONT F ( 2 ,X'S,U[ISO]) UNTIL F ( 5 )
CONT F ( 6 ,X'S,U'S)
CONT F ( 21 ,X'S,U[ISO]) UNTIL F ( 24 )
CONT F ( 101 ,X'S,U'S)
CONT F ( 102 ,X'S,U[ISO]) UNTIL F ( 105 )
CONT F ( 106 ,X'S,U'S)
CONT F ( 121 ,X'S,U[ISO]) UNTIL F ( 124 )
CONT N ( 1 ,X'S,U'S) UNTIL C ( 138 )
SUMFIX P(2,OCC) AND P(3,OCC)
SUMFIX P(102,OCC) AND P(103,OCC)
SUMFIX PART(1001,OCC) AND PART(1002,OCC)
SUMFIX PART(1003,OCC) AND PART(1004,OCC)
SUMFIX ELEMENT SCALES
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S)
RIDE C ( 24,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 251,X'S)
RIDE C ( 28,X'S) H ( 281,X'S)
RIDE C ( 29,X'S) H ( 291,X'S)
RIDE C ( 30,X'S) H ( 301,X'S)
RIDE C ( 31,X'S) H ( 311,X'S)
RIDE C ( 32,X'S) H ( 321,X'S)
RIDE C ( 34,X'S) H ( 341,X'S)
RIDE C ( 35,X'S) H ( 351,X'S)
RIDE C ( 36,X'S) H ( 361,X'S)
RIDE C ( 37,X'S) H ( 371,X'S)
RIDE C ( 38,X'S) H ( 381,X'S)
RIDE C ( 102,X'S) H (1021,X'S)
RIDE C ( 103,X'S) H (1031,X'S)
RIDE C ( 104,X'S) H (1041,X'S)
RIDE C ( 105,X'S) H (1051,X'S)
RIDE C ( 106,X'S) H (1061,X'S)
RIDE C ( 108,X'S) H (1081,X'S)
RIDE C ( 109,X'S) H (1091,X'S)
RIDE C ( 110,X'S) H (1101,X'S)
RIDE C ( 111,X'S) H (1111,X'S)
RIDE C ( 112,X'S) H (1121,X'S)
RIDE C ( 114,X'S) H (1141,X'S)
RIDE C ( 115,X'S) H (1151,X'S)
RIDE C ( 116,X'S) H (1161,X'S)
RIDE C ( 117,X'S) H (1171,X'S)
RIDE C ( 119,X'S) H (1191,X'S) H (1192,X'S)
RIDE C ( 120,X'S) H (1201,X'S) H (1202,X'S)
RIDE C ( 122,X'S) H (1221,X'S)
RIDE C ( 123,X'S) H (1231,X'S)
RIDE C ( 124,X'S) H (1241,X'S)
RIDE C ( 125,X'S) H (1251,X'S)
RIDE C ( 128,X'S) H (1281,X'S)
RIDE C ( 129,X'S) H (1291,X'S)
RIDE C ( 130,X'S) H (1301,X'S)
RIDE C ( 131,X'S) H (1311,X'S)
RIDE C ( 132,X'S) H (1321,X'S)
RIDE C ( 134,X'S) H (1341,X'S)
RIDE C ( 135,X'S) H (1351,X'S)
RIDE C ( 136,X'S) H (1361,X'S)
RIDE C ( 137,X'S) H (1371,X'S)
RIDE C ( 138,X'S) H (1381,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 16/02/12 at 14:12:10
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
A-U(IJ)'S 0.0, 0.0030000 = P(2) TO P(3)
END
;
#===
data_7
_database_code_depnum_ccdc_archive 'CCDC 869437'
#TrackingRef '- combined_bf.cif'
_audit_creation_date 11-11-11
_audit_creation_method CRYSTALS_ver_14.30
_vrf_PLAT410_7
;
PROBLEM: Short Intra H...H Contact H171 .. H192 .. 1.88 Ang.
RESPONSE: This warning arises owing to unresolved disorder of
the methylene carbon atoms. Location and placement of H atoms
is thus subject to minor errors. Additional comment appears
in the experimental section.
;
_oxford_structure_analysis_title 'bfpan_6169_0m in C2/c'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 25.0443(7)
_cell_length_b 15.9342(5)
_cell_length_c 9.6935(3)
_cell_angle_alpha 90
_cell_angle_beta 110.393(1)
_cell_angle_gamma 90
_cell_volume 3625.85(19)
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M 'C 1 2/c 1 '
_symmetry_space_group_name_Hall '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pt -1.7033 8.3905 27.0059 1.5129 17.7639 8.8117 15.7131 0.4246 5.7837 38.6103
11.6883 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 4
# Given Formula = C38 H33 N2 O1 P3 Pt1
# Dc = 1.51 Fooo = 1620.00 Mu = 40.33 M = 410.85
# Found Formula = C38 H32 N2 O1 P3 Pt1
# Dc = 1.50 FOOO = 1620.00 Mu = 40.33 M = 410.35
_chemical_formula_sum 'C38 H32 N2 O1 P3 Pt1'
_chemical_formula_moiety 'C38 H32 N2 O1 P3 Pt1'
_chemical_compound_source ?
_chemical_formula_weight 820.70
_cell_measurement_reflns_used 9905
_cell_measurement_theta_min 2
_cell_measurement_theta_max 29
_cell_measurement_temperature 120
_exptl_crystal_description prism
_exptl_crystal_colour yellow
_exptl_crystal_size_min 0.130
_exptl_crystal_size_mid 0.210
_exptl_crystal_size_max 0.270
_exptl_crystal_density_diffrn 1.503
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 1620
_exptl_absorpt_coefficient_mu 4.033
# Sheldrick geometric approximatio 0.43 0.59
_exptl_absorpt_correction_type numerical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_absorpt_correction_T_min 0.43
_exptl_absorpt_correction_T_max 0.59
_diffrn_measurement_device_type 'Bruker Kappa Apex2'
_diffrn_measurement_device Area
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method '\f & \w scans'
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement 'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction 'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'CAMERON (Watkin et al., 1996)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 120
_diffrn_reflns_number 5303
_reflns_number_total 5303
_diffrn_reflns_av_R_equivalents 0.032
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 5303
# Theoretical number of reflections is about 10620
_diffrn_reflns_theta_min 1.545
_diffrn_reflns_theta_max 30.046
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 30.046
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_limit_h_min -35
_diffrn_reflns_limit_h_max 33
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_l_min 0
_diffrn_reflns_limit_l_max 13
_reflns_limit_h_min -35
_reflns_limit_h_max 33
_reflns_limit_k_min 0
_reflns_limit_k_max 22
_reflns_limit_l_min 0
_reflns_limit_l_max 13
_oxford_diffrn_Wilson_B_factor 0.00
_oxford_diffrn_Wilson_scale 0.00
_atom_sites_solution_primary Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -1.71
_refine_diff_density_max 2.01
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns 5303
_refine_ls_number_restraints 0
_refine_ls_number_parameters 231
_oxford_refine_ls_R_factor_ref 0.0348
_refine_ls_wR_factor_ref 0.0605
_refine_ls_goodness_of_fit_ref 0.9968
_refine_ls_shift/su_max 0.0014223
_refine_ls_shift/su_mean 0.0000334
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 5303
_refine_ls_R_factor_all 0.0348
_refine_ls_wR_factor_all 0.0605
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 4020
_refine_ls_R_factor_gt 0.0242
_refine_ls_wR_factor_gt 0.0550
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration .
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +12.81P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435.
Betteridge, P.W., Carruthers, J.R., Cooper, R.I.,
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487.
Bruker Analytical X-ray Systems, Inc., 2006. Apex2,
Version 2 User Manual, M86-E01078, Madison, WI.
De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014.
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Pt1 Pt 0.5000 0.752629(10) 0.2500 0.0232 1.0000 Uani S T . . . .
P1 P 0.59610(3) 0.75528(5) 0.34678(7) 0.0261 1.0000 Uani . . . . . .
P2 P 0.48900(6) 0.86751(9) 0.36769(17) 0.0260 0.5000 Uani . . . 1 1 .
O1 O 0.47583(18) 0.9488(3) 0.2878(5) 0.0334 0.5000 Uani . . . . . .
N1 N 0.5453(2) 0.8797(3) 0.5310(5) 0.0291 0.5000 Uani . . . 1 1 .
N2 N 0.4443(2) 0.8491(3) 0.4632(5) 0.0296 0.5000 Uani . . . 1 1 .
C1 C 0.62865(13) 0.6682(2) 0.4692(3) 0.0343 1.0000 Uani . . . . . .
C2 C 0.60921(17) 0.5876(3) 0.4252(4) 0.0512 1.0000 Uani . . . . . .
C3 C 0.63376(19) 0.5200(3) 0.5142(5) 0.0628 1.0000 Uani . . . . . .
C4 C 0.67610(19) 0.5331(3) 0.6497(5) 0.0605 1.0000 Uani . . . . . .
C5 C 0.69511(18) 0.6126(3) 0.6927(4) 0.0566 1.0000 Uani . . . . . .
C6 C 0.67212(16) 0.6806(3) 0.6024(4) 0.0453 1.0000 Uani . . . . . .
C7 C 0.62754(12) 0.75207(19) 0.2039(3) 0.0289 1.0000 Uani . . . . . .
C8 C 0.67512(14) 0.7022(2) 0.2221(4) 0.0360 1.0000 Uani . . . . . .
C9 C 0.69954(16) 0.6980(2) 0.1139(4) 0.0461 1.0000 Uani . . . . . .
C10 C 0.67720(17) 0.7441(3) -0.0108(4) 0.0516 1.0000 Uani . . . . . .
C11 C 0.63097(17) 0.7957(3) -0.0304(4) 0.0492 1.0000 Uani . . . . . .
C12 C 0.60411(14) 0.7996(2) 0.0744(4) 0.0378 1.0000 Uani . . . . . .
C13 C 0.62620(12) 0.8489(2) 0.4514(3) 0.0316 1.0000 Uani . . . . . .
C14 C 0.67785(12) 0.8812(2) 0.4505(3) 0.0324 1.0000 Uani . . . . . .
C15 C 0.70204(16) 0.9510(2) 0.5316(4) 0.0461 1.0000 Uani . . . . . .
C16 C 0.67446(19) 0.9891(3) 0.6166(4) 0.0571 1.0000 Uani . . . . . .
C17 C 0.62415(17) 0.9584(3) 0.6200(4) 0.0598 1.0000 Uani . . . . . .
C18 C 0.59868(14) 0.8901(3) 0.5370(4) 0.0485 1.0000 Uani . . . . . .
C19 C 0.5212(3) 0.9318(4) 0.6233(7) 0.0351 0.5000 Uani . . . . . .
C20 C 0.4652(3) 0.8894(4) 0.6098(7) 0.0370 0.5000 Uani . . . 1 1 .
H21 H 0.5778 0.5776 0.3350 0.0609 1.0000 Uiso R . . . . .
H31 H 0.6217 0.4657 0.4855 0.0755 1.0000 Uiso R . . . . .
H41 H 0.6917 0.4874 0.7104 0.0729 1.0000 Uiso R . . . . .
H51 H 0.7233 0.6214 0.7813 0.0682 1.0000 Uiso R . . . . .
H61 H 0.6856 0.7337 0.6302 0.0540 1.0000 Uiso R . . . . .
H81 H 0.6910 0.6714 0.3091 0.0427 1.0000 Uiso R . . . . .
H91 H 0.7307 0.6641 0.1277 0.0551 1.0000 Uiso R . . . . .
H101 H 0.6931 0.7410 -0.0842 0.0618 1.0000 Uiso R . . . . .
H111 H 0.6171 0.8288 -0.1137 0.0586 1.0000 Uiso R . . . . .
H141 H 0.6965 0.8553 0.3959 0.0387 1.0000 Uiso R . . . . .
H151 H 0.7353 0.9714 0.5277 0.0551 1.0000 Uiso R . . . . .
H161 H 0.6898 1.0367 0.6718 0.0694 1.0000 Uiso R . . . . .
H171 H 0.6070 0.9833 0.6804 0.0718 1.0000 Uiso R . . . . .
H191 H 0.5146 0.9891 0.5804 0.0417 0.5000 Uiso R . . . . .
H192 H 0.5470 0.9343 0.7263 0.0419 0.5000 Uiso R . . . . .
H201 H 0.4383 0.9314 0.6216 0.0441 0.5000 Uiso R . . 1 1 .
H202 H 0.4718 0.8462 0.6851 0.0440 0.5000 Uiso R . . 1 1 .
H121 H 0.5709 0.8327 0.0580 0.0451 0.5000 Uiso R . . 1 1 .
H181 H 0.5626 0.8711 0.5362 0.0575 0.5000 Uiso R . . 1 1 .
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 0.02035(7) 0.02384(7) 0.02465(7) 0.0000 0.00682(5) 0.0000
P1 0.0212(3) 0.0336(4) 0.0235(3) -0.0012(3) 0.0079(2) 0.0032(3)
P2 0.0222(6) 0.0278(7) 0.0283(7) -0.0023(5) 0.0092(6) 0.0019(5)
O1 0.031(2) 0.032(2) 0.038(2) 0.0032(18) 0.0134(19) 0.0014(17)
N1 0.021(2) 0.043(3) 0.025(2) -0.009(2) 0.0097(19) -0.003(2)
N2 0.027(2) 0.035(3) 0.029(2) -0.008(2) 0.013(2) -0.004(2)
C1 0.0301(16) 0.0452(18) 0.0303(16) 0.0065(13) 0.0139(13) 0.0092(13)
C2 0.043(2) 0.052(2) 0.050(2) 0.0130(18) 0.0060(17) 0.0022(17)
C3 0.056(3) 0.049(2) 0.077(3) 0.017(2) 0.015(2) 0.011(2)
C4 0.061(3) 0.070(3) 0.052(2) 0.026(2) 0.022(2) 0.032(2)
C5 0.057(2) 0.070(3) 0.0341(19) 0.0075(18) 0.0052(17) 0.031(2)
C6 0.046(2) 0.055(2) 0.0315(16) 0.0035(15) 0.0093(15) 0.0181(17)
C7 0.0292(12) 0.0325(13) 0.0265(12) -0.0010(13) 0.0119(10) 0.0027(13)
C8 0.0353(16) 0.0380(16) 0.0389(17) -0.0034(13) 0.0181(14) 0.0060(13)
C9 0.048(2) 0.048(2) 0.054(2) -0.0056(17) 0.0320(18) 0.0067(16)
C10 0.057(2) 0.066(2) 0.0447(19) -0.010(2) 0.0345(18) -0.001(2)
C11 0.052(2) 0.067(3) 0.0320(17) 0.0059(17) 0.0191(17) 0.0025(19)
C12 0.0344(17) 0.0455(18) 0.0352(16) 0.0071(14) 0.0142(14) 0.0061(14)
C13 0.0208(13) 0.0438(17) 0.0258(14) -0.0081(12) 0.0027(11) 0.0032(12)
C14 0.0234(14) 0.0383(16) 0.0334(15) -0.0049(12) 0.0073(12) 0.0015(12)
C15 0.0387(19) 0.049(2) 0.0430(19) -0.0079(16) 0.0052(15) -0.0082(16)
C16 0.059(3) 0.049(2) 0.046(2) -0.0202(18) -0.0025(19) 0.0058(19)
C17 0.042(2) 0.085(3) 0.042(2) -0.027(2) 0.0013(17) 0.026(2)
C18 0.0201(14) 0.086(3) 0.0365(18) -0.0240(18) 0.0063(13) 0.0045(16)
C19 0.034(3) 0.039(3) 0.035(3) -0.011(3) 0.017(3) -0.003(3)
C20 0.039(3) 0.039(3) 0.036(3) -0.009(3) 0.018(3) -0.005(3)
_refine_ls_extinction_method None
_oxford_refine_ls_scale 0.046447(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pt1 . P1 5_655 2.2586(7) yes
Pt1 . P2 5_655 2.2242(14) yes
Pt1 . P1 . 2.2586(7) yes
Pt1 . P2 . 2.2242(14) yes
P1 . C1 . 1.823(3) yes
P1 . C7 . 1.817(3) yes
P1 . C13 . 1.814(3) yes
P2 . P2 5_655 2.527(3) yes
P2 . O1 . 1.485(4) yes
P2 . N1 . 1.725(5) yes
P2 . N2 . 1.709(5) yes
O1 . O1 5_655 1.619(8) yes
N1 . C18 . 1.329(5) yes
N1 . C19 . 1.492(7) yes
N2 . C12 5_655 1.384(6) yes
N2 . C20 . 1.479(8) yes
C1 . C2 . 1.386(5) yes
C1 . C6 . 1.383(5) yes
C2 . C3 . 1.385(5) yes
C2 . H21 . 0.964 no
C3 . C4 . 1.387(6) yes
C3 . H31 . 0.926 no
C4 . C5 . 1.366(6) yes
C4 . H41 . 0.933 no
C5 . C6 . 1.385(5) yes
C5 . H51 . 0.913 no
C6 . H61 . 0.916 no
C7 . C8 . 1.392(4) yes
C7 . C12 . 1.407(4) yes
C8 . C9 . 1.388(4) yes
C8 . H81 . 0.936 no
C9 . C10 . 1.357(5) yes
C9 . H91 . 0.920 no
C10 . C11 . 1.378(6) yes
C10 . H101 . 0.931 no
C11 . C12 . 1.402(5) yes
C11 . H111 . 0.925 no
C12 . H121 . 0.950 no
C13 . C14 . 1.394(4) yes
C13 . C18 . 1.412(4) yes
C14 . C15 . 1.375(4) yes
C14 . H141 . 0.917 no
C15 . C16 . 1.387(5) yes
C15 . H151 . 0.908 no
C16 . C17 . 1.362(6) yes
C16 . H161 . 0.930 no
C17 . C18 . 1.372(5) yes
C17 . H171 . 0.927 no
C18 . H181 . 0.950 no
C19 . C20 . 1.521(9) yes
C19 . H191 . 0.993 no
C19 . H192 . 0.982 no
C20 . H201 . 0.985 no
C20 . H202 . 0.974 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P1 5_655 Pt1 . P2 5_655 94.36(4) yes
P1 5_655 Pt1 . P1 . 177.86(4) yes
P2 5_655 Pt1 . P1 . 83.86(4) yes
P1 5_655 Pt1 . P2 . 83.86(4) yes
P2 5_655 Pt1 . P2 . 69.23(8) yes
P1 . Pt1 . P2 . 94.36(4) yes
Pt1 . P1 . C1 . 115.22(11) yes
Pt1 . P1 . C7 . 111.40(9) yes
C1 . P1 . C7 . 105.10(14) yes
Pt1 . P1 . C13 . 115.01(10) yes
C1 . P1 . C13 . 104.95(15) yes
C7 . P1 . C13 . 104.07(14) yes
P2 5_655 P2 . Pt1 . 55.38(4) yes
P2 5_655 P2 . O1 . 66.91(17) yes
Pt1 . P2 . O1 . 119.64(18) yes
P2 5_655 P2 . N1 . 117.61(18) yes
Pt1 . P2 . N1 . 110.86(18) yes
O1 . P2 . N1 . 110.0(3) yes
P2 5_655 P2 . N2 . 151.57(19) yes
Pt1 . P2 . N2 . 111.02(18) yes
O1 . P2 . N2 . 111.3(2) yes
N1 . P2 . N2 . 90.1(2) yes
O1 5_655 O1 . P2 . 99.8(2) yes
P2 . N1 . C18 . 122.8(4) yes
P2 . N1 . C19 . 104.0(4) yes
C18 . N1 . C19 . 121.0(4) yes
C12 5_655 N2 . P2 . 129.3(4) yes
C12 5_655 N2 . C20 . 119.1(4) yes
P2 . N2 . C20 . 111.5(4) yes
P1 . C1 . C2 . 118.4(3) yes
P1 . C1 . C6 . 121.8(3) yes
C2 . C1 . C6 . 119.8(3) yes
C1 . C2 . C3 . 119.8(4) yes
C1 . C2 . H21 . 121.4 no
C3 . C2 . H21 . 118.7 no
C2 . C3 . C4 . 120.0(4) yes
C2 . C3 . H31 . 120.8 no
C4 . C3 . H31 . 119.2 no
C3 . C4 . C5 . 119.9(4) yes
C3 . C4 . H41 . 119.6 no
C5 . C4 . H41 . 120.5 no
C4 . C5 . C6 . 120.6(4) yes
C4 . C5 . H51 . 120.1 no
C6 . C5 . H51 . 119.3 no
C5 . C6 . C1 . 119.8(4) yes
C5 . C6 . H61 . 120.4 no
C1 . C6 . H61 . 119.7 no
P1 . C7 . C8 . 119.9(2) yes
P1 . C7 . C12 . 120.5(2) yes
C8 . C7 . C12 . 119.6(3) yes
C7 . C8 . C9 . 120.9(3) yes
C7 . C8 . H81 . 119.4 no
C9 . C8 . H81 . 119.7 no
C8 . C9 . C10 . 119.6(3) yes
C8 . C9 . H91 . 119.5 no
C10 . C9 . H91 . 120.8 no
C9 . C10 . C11 . 120.7(3) yes
C9 . C10 . H101 . 120.0 no
C11 . C10 . H101 . 119.3 no
C10 . C11 . C12 . 121.3(3) yes
C10 . C11 . H111 . 120.1 no
C12 . C11 . H111 . 118.6 no
C7 . C12 . C11 . 117.8(3) yes
C7 . C12 . N2 5_655 126.6(3) yes
C11 . C12 . N2 5_655 115.6(3) yes
C7 . C12 . H121 . 121.1 no
C11 . C12 . H121 . 121.1 no
P1 . C13 . C14 . 120.4(2) yes
P1 . C13 . C18 . 121.2(3) yes
C14 . C13 . C18 . 118.4(3) yes
C13 . C14 . C15 . 121.3(3) yes
C13 . C14 . H141 . 119.9 no
C15 . C14 . H141 . 118.8 no
C14 . C15 . C16 . 118.9(4) yes
C14 . C15 . H151 . 119.7 no
C16 . C15 . H151 . 121.4 no
C15 . C16 . C17 . 120.9(4) yes
C15 . C16 . H161 . 120.6 no
C17 . C16 . H161 . 118.5 no
C16 . C17 . C18 . 121.0(3) yes
C16 . C17 . H171 . 119.8 no
C18 . C17 . H171 . 119.1 no
C13 . C18 . C17 . 119.4(3) yes
C13 . C18 . N1 . 127.3(4) yes
C17 . C18 . N1 . 112.3(4) yes
C13 . C18 . H181 . 120.3 no
C17 . C18 . H181 . 120.3 no
N1 . C19 . C20 . 104.7(5) yes
N1 . C19 . H191 . 107.7 no
C20 . C19 . H191 . 111.0 no
N1 . C19 . H192 . 112.0 no
C20 . C19 . H192 . 111.4 no
H191 . C19 . H192 . 110.0 no
C19 . C20 . N2 . 106.5(5) yes
C19 . C20 . H201 . 109.6 no
N2 . C20 . H201 . 112.2 no
C19 . C20 . H202 . 109.8 no
N2 . C20 . H202 . 109.0 no
H201 . C20 . H202 . 109.7 no
_iucr_refine_instruction_details_constraints
;
#
# Punched on 11/11/11 at 11:19:10
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE C ( 2,X'S) H ( 21,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 4,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S)
RIDE C ( 6,X'S) H ( 61,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 9,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S)
RIDE C ( 11,X'S) H ( 111,X'S)
RIDE C ( 12,X'S) H ( 121,X'S)
RIDE C ( 14,X'S) H ( 141,X'S)
RIDE C ( 15,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S)
RIDE C ( 19,X'S) H ( 191,X'S) H ( 192,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 11/11/11 at 11:19:10
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.019 276 87 ' '
2 0.500 0.500 0.047 276 87 ' '
_platon_squeeze_details
;
During the structure solution, electron density difference
maps revealed that there were considerable disordered
solvent molecules, which could not be successfully modeled.
>From history, the remaining solvate was likely ether or THF
in a volume of 553.9 \%A3 per unit cell (15.3%). It appeared
that the cavity areas contained about four ether and/or THF
molecules, located near the centers of symmetry at (0, 0, 0)
and ( 1/2, 1/2 , 0 ). Modeling with or without restraints
was unsuccessful, as was step by step acquisition
of peaks using successive electron density difference maps.
Thus, the structure factors were modified using the PLATON
SQUEEZE technique, in order to produce a ?solvate-free?
structure factor set. PLATON reported a total electron
density of 174 e- per unit cell, likely representing four THF
or ether molecules, consistent with our earlier observations.
Use of the SQUEEZE technique resulted in a decrease of ca.
1.7 % in R.
;
#===END