metal-organic compounds
1,1,2,2,2,3,3,3-Octacarbonyl-1,1,2,3-tetrakis(1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]decane-κP)-triangulo-triosmium(0)
aDepartment of Chemistry & Biochemistry, Abilene Christian University, Abilene, Texas 79699-8132, USA, and bDepartment of Chemistry, University of Texas, Austin, Texas 78712, USA
*Correspondence e-mail: powellg@acu.edu
The title compound, [Os3(C6H12N3P)4(CO)8], crystallizes in the orthorhombic Pbca with Z = 8. The molecule consists of a triangular triosmium(0) core surrounded by eight carbonyl ligands and four 1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]decane (or PTA) ligands. One Os atom is coordinated by two PTA ligands and two CO ligands, while the other two Os atoms are each bonded to a single PTA ligand and three CO ligands. There is a small disorder associated with the Os3 unit so that a minor orientation has an occupancy of 2.17 (4)%. The title compound represents the first structurally characterized triangular Os3 carbonyl cluster with four monodentate tertiary phosphane ligands.
Keywords: crystal structure; osmium carbonyl; trinuclear cluster; PTA ligands.
CCDC reference: 1949128
Structure description
The water-soluble, air-stable, and non-toxic phosphane ligand 1,3,5-triaza-7-phosphatricyclo[3.3.1.13,7]decane (PTA) is often used in attempts to prepare metal complexes that are soluble in water (Phillips et al., 2004; Bravo et al., 2010). A series of triangular trinuclear metal carbonyl cluster complexes with the formula M3(CO)12–x(PTA)x, where M = Ru or Os and x = 1, 2, or 3, was recently synthesized by reactions of PTA with M3(CO)12 (Mager et al., 2015; Dugan et al., 2016; Nazarov et al., 2016). The complexes M3(CO)11(PTA) and M3(CO)10(PTA)2 are insoluble in water, while the complexes M3(CO)9(PTA)3 dissolve in water with a pH lower than 4. The title complex, Os3(CO)8(PTA)4, was also prepared and found to be soluble under acidic, neutral and basic aqueous conditions (Dugan et al., 2016). As a result, tests are currently underway to determine if the title complex displays anticancer activity. An X-ray crystallographic analysis of Os3(CO)8(PTA)4 is warranted because there are no reports describing the of a triosmium carbonyl cluster containing four monodentate phosphane ligands. Previous efforts to produce triangular triosmium with more than three phosphane ligands have typically resulted in cluster fragmentation (Alex et al., 1987).
In the title compound, the four phosphane ligands adopt positions that maximize the distance between them (Fig. 1). Two PTA ligands coordinate to Os1 through their P atoms, and the other two PTA ligands coordinate one each to Os2 and Os3 through their P atoms. All PTA ligands are located in equatorial coordination sites so that the four phosphorus atoms are within 1 Å of residing in the same plane as the three osmium atoms. Two carbonyl ligands occupy equatorial sites (one each on Os2 and Os3), while the other six CO ligands occupy axial sites (two per Os atom). Each Os atom exhibits a pseudo-octahedral coordination environment, but the three coordination spheres are twisted relative to one another so that the axial CO ligands are no longer perpendicular to the Os3 plane as they are in Os3(CO)12 (Corey & Dahl, 1962). The average Cax—Os—Os—Cax torsion angle is 29 (3)°. Crystal structures have been reported for five Ru3(CO)12–xLx complexes: one [L = P(OMe)2Ph] with two bridging CO ligands (Bruce et al., 1985), two [L = P(OEt)3, PMe2Ph] with two semi-bridging CO ligands, and two [L = P(OMe)3, P(OPh)3] with only terminal CO ligands (Bruce et al., 1989). In all cases, the phosphane or phosphite ligands adopt the same coordination geometry as in the title complex. The average Cax—Ru—Ru—Cax torsion angles in the latter two are similar to that in the title complex with 35 (3)° for L = P(OMe)3 and 30 (2)° for L = P(OPh)3. Such torsional twisting was also noted in the cases of Ru3(CO)9(PTA)3 and Os3(CO)9(PTA)3, albeit to a significantly lower degree with average Cax—M—M—Cax torsion angles of 19 (2) and 17 (2)°, respectively (Mager et al., 2015; Dugan et al., 2016). The average Os—Os bond length of 2.903 (22) Å in the title complex is virtually the same as that of 2.90 (2) Å in Os3(CO)9(PTA)3, suggesting that torsional distortion is preferred over metal–metal bond lengthening.
In the structure of the title complex, the molecules are stacked parallel to the a axis of the with every other Os3 triangle facing in the opposite direction and tilted at an angle of 9 (1)° from the previous Os3 triangle in the same stack (Fig. 2). The planes defined by the Os3 units appear to be roughly perpendicular to the b axis, but actually form 21 (1)° angles with the ac plane. There is a slight disorder in the title complex associated with the triangular Os3 unit so that two different orientations are observed with a 0.9783 (4)/0.0217 (4) ratio of major-to-minor components (Fig. 3). This type of disorder is rather common in M3(CO)12–xLx complexes in which M = Ru or Os. For example, a 50/50 disorder of the M3 unit exists in Os3(CO)6[P(OMe)3]6, Ru3(CO)8(PMe2Ph)4, and Ru3(CO)8[P(OEt)3]4, while an 85/15 disorder is present in Ru3(CO)8[P(OMe)3]4 (Alex et al., 1987; Bruce et al., 1989).
Synthesis and crystallization
Dodcecacarbonyltriosmium (63.3 mg, 0.0698 mmol), PTA (87.6 mg, 0.557 mmol), 1,2-dichlorobenzene (6 ml), and acetonitrile (2 ml) were added to a 35 ml glass reaction vessel, then sealed with a PTFE cap and placed in a CEM Discover-SP microwave reactor. The mixture was stirred and heated at 458 K for 24 min to produce a vibrant orange solution. The solvent was removed and water (15 ml) was added to dissolve the residue. The resulting solution was filtered through a glass frit and the orange filtrate collected. After 16 h, a precipitate had formed. Filtering again allowed for the isolation of the title complex as an orange solid. IR (νCO cm−1 in CHCl3): 2033(w), 1970(sh), 1953(vs), 1921(m). Crystals grew as thin, reddish orange plates via diffusion of n-hexane into a CH2Cl2 solution.
Refinement
Crystal data, data collection and structure . Three rather large electron density peaks located near the Os atoms persisted in the difference electron-density map after all of the expected atoms were included in the model. The position of these peaks suggested there was a slight disorder in the complex resulting from an approximately 60° rotation about an axis perpendicular to the plane through the three Os atoms. A disorder model with this in mind was proposed where these three electron-density peaks represented the alternate orientation of the Os3 core. The variable x was assigned to the site occupancy for Os1, Os2 and Os3, while the site occupancy for Os1A, Os2A and Os3A was set to (1 − x). The displacement parameters for the lower occupancy Os atoms were set to be equal to those of the major component. The variable x refined to 0.9783 (4). Disorder of the associated CO and PTA ligands could not be resolved.
details are summarized in Table 1Structural data
CCDC reference: 1949128
https://doi.org/10.1107/S2414314620009359/wm4135sup1.cif
contains datablock I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314620009359/wm4135Isup2.hkl
Supporting information file. DOI: https://doi.org/10.1107/S2414314620009359/wm4135Isup4.cml
Data collection: CrysAlis PRO (Agilent, 2016); cell
CrysAlis PRO (Agilent, 2016); data reduction: CrysAlis PRO (Agilent, 2016); program(s) used to solve structure: SUPERFLIP (Palatinus & Chapuis, 2007); program(s) used to refine structure: SHELXL2014/7 (Sheldrick 2015); molecular graphics: XP in SHELXTL/PC (Sheldrick, 2008); software used to prepare material for publication: SHELXL2014/7 (Sheldrick 2015).[Os3(C6H12N3P)4(CO)8] | Dx = 2.300 Mg m−3 |
Mr = 1423.30 | Cu Kα radiation, λ = 1.54184 Å |
Orthorhombic, Pbca | Cell parameters from 21014 reflections |
a = 18.7500 (2) Å | θ = 3.9–74.1° |
b = 15.8889 (2) Å | µ = 19.16 mm−1 |
c = 27.5984 (3) Å | T = 100 K |
V = 8222.03 (16) Å3 | Plates, red-orange |
Z = 8 | 0.18 × 0.09 × 0.01 mm |
F(000) = 5408 |
Agilent SuperNova with AtlasS2 CCD diffractometer | 7535 reflections with I > 2σ(I) |
Radiation source: sealed microfocus tube | Rint = 0.048 |
ω–scans | θmax = 74.3°, θmin = 3.2° |
Absorption correction: gaussian (CrysAlisPro; Agilent, 2016) | h = −23→23 |
Tmin = 0.142, Tmax = 0.783 | k = −19→19 |
38755 measured reflections | l = −33→33 |
8184 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.032 | H-atom parameters constrained |
wR(F2) = 0.076 | w = 1/[σ2(Fo2) + (0.0225P)2 + 60.4468P] where P = (Fo2 + 2Fc2)/3 |
S = 1.14 | (Δ/σ)max = 0.002 |
8184 reflections | Δρmax = 1.24 e Å−3 |
542 parameters | Δρmin = −1.34 e Å−3 |
Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. |
Refinement. Three rather large peaks persisted in the difference electron density map after all the expected atoms were included in the model. These peaks, all greater than 4 e-/A3, were located near the Os atoms. The position of these peaks suggested there was a slight disorder in the complex. The disorder resulted from an approximately 60 degree rotation about an axis perpendicular to the plane through the three Os atoms. A disorder model with this in mind was proposed where these three peaks represented the alternate orientation of the Os atoms. The variable x was assigned to the site occupancy for Os1, Os2 and Os3, while the site occupancy factors for Os1a, Os2a and Os3a was set to (1-x). The displacement parameters for the lower occupancy Os atoms was set to be equal to that of the major component. The variable x refined to 0.9783 (4). The other atoms of the alternate component were not included in the disorder model because the very low electron density of a 2% component would be lost in the noise. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Os1 | 0.13660 (2) | 0.51582 (2) | 0.16473 (2) | 0.01732 (6) | 0.9783 (4) |
Os1A | 0.1385 (5) | 0.5007 (6) | 0.2876 (4) | 0.017* | 0.0217 (4) |
Os2 | 0.06461 (2) | 0.53429 (2) | 0.25694 (2) | 0.01999 (7) | 0.9783 (4) |
Os2A | 0.2036 (6) | 0.4728 (7) | 0.1943 (4) | 0.020* | 0.0217 (4) |
Os3 | 0.21112 (2) | 0.47110 (2) | 0.25254 (2) | 0.01941 (7) | 0.9783 (4) |
Os3A | 0.0633 (6) | 0.5501 (7) | 0.2014 (4) | 0.019* | 0.0217 (4) |
P1 | 0.19602 (7) | 0.44377 (9) | 0.10564 (5) | 0.0205 (3) | |
P2 | 0.06469 (7) | 0.59975 (9) | 0.11836 (5) | 0.0204 (3) | |
P3 | 0.03369 (8) | 0.56927 (10) | 0.33489 (5) | 0.0231 (3) | |
P4 | 0.24364 (8) | 0.41978 (9) | 0.32711 (5) | 0.0215 (3) | |
O1 | 0.2497 (2) | 0.6564 (3) | 0.16584 (15) | 0.0343 (10) | |
O2 | 0.0236 (2) | 0.3749 (3) | 0.16316 (15) | 0.0288 (9) | |
O3 | 0.1199 (2) | 0.7154 (3) | 0.24106 (15) | 0.0298 (9) | |
O4 | −0.0818 (2) | 0.5625 (4) | 0.21312 (16) | 0.0422 (12) | |
O5 | 0.0292 (3) | 0.3491 (3) | 0.28011 (17) | 0.0379 (11) | |
O6 | 0.2521 (2) | 0.6475 (3) | 0.28886 (16) | 0.0354 (10) | |
O7 | 0.3580 (2) | 0.4501 (4) | 0.20884 (17) | 0.0442 (12) | |
O8 | 0.1579 (2) | 0.2948 (3) | 0.22133 (16) | 0.0336 (10) | |
N1 | 0.2921 (3) | 0.3214 (3) | 0.07410 (17) | 0.0263 (10) | |
N2 | 0.2723 (3) | 0.4408 (3) | 0.01888 (18) | 0.0291 (11) | |
N3 | 0.1794 (3) | 0.3322 (3) | 0.02862 (18) | 0.0310 (11) | |
N4 | −0.0582 (3) | 0.6146 (3) | 0.0632 (2) | 0.0350 (12) | |
N5 | 0.0450 (3) | 0.6985 (3) | 0.03545 (17) | 0.0287 (11) | |
N6 | −0.0219 (3) | 0.7418 (3) | 0.10798 (19) | 0.0297 (11) | |
N7 | −0.0301 (3) | 0.5304 (4) | 0.4224 (2) | 0.0414 (14) | |
N8 | −0.0477 (3) | 0.6759 (4) | 0.3919 (2) | 0.0389 (13) | |
N9 | 0.0689 (3) | 0.6327 (3) | 0.42524 (18) | 0.0327 (12) | |
N10 | 0.2154 (3) | 0.3296 (3) | 0.41086 (17) | 0.0302 (11) | |
N11 | 0.3084 (3) | 0.4396 (3) | 0.41678 (17) | 0.0279 (11) | |
N12 | 0.3330 (3) | 0.3066 (3) | 0.37345 (18) | 0.0269 (10) | |
C1 | 0.2665 (3) | 0.3640 (4) | 0.1184 (2) | 0.0276 (12) | |
H1A | 0.3073 | 0.3920 | 0.1345 | 0.033* | |
H1B | 0.2473 | 0.3213 | 0.1410 | 0.033* | |
C2 | 0.3233 (3) | 0.3817 (4) | 0.0398 (2) | 0.0308 (13) | |
H2A | 0.3611 | 0.4140 | 0.0566 | 0.037* | |
H2B | 0.3463 | 0.3500 | 0.0131 | 0.037* | |
C3 | 0.2143 (3) | 0.3926 (4) | −0.0037 (2) | 0.0342 (14) | |
H3A | 0.1780 | 0.4326 | −0.0158 | 0.041* | |
H3B | 0.2337 | 0.3619 | −0.0319 | 0.041* | |
C4 | 0.2333 (3) | 0.2771 (4) | 0.0496 (2) | 0.0307 (13) | |
H4A | 0.2536 | 0.2417 | 0.0235 | 0.037* | |
H4B | 0.2100 | 0.2392 | 0.0732 | 0.037* | |
C5 | 0.2442 (3) | 0.4983 (4) | 0.0563 (2) | 0.0282 (13) | |
H5A | 0.2115 | 0.5391 | 0.0407 | 0.034* | |
H5B | 0.2844 | 0.5305 | 0.0704 | 0.034* | |
C6 | 0.1397 (3) | 0.3753 (4) | 0.0674 (2) | 0.0300 (13) | |
H6A | 0.1166 | 0.3325 | 0.0882 | 0.036* | |
H6B | 0.1015 | 0.4099 | 0.0525 | 0.036* | |
C7 | −0.0174 (3) | 0.5548 (4) | 0.0924 (2) | 0.0293 (13) | |
H7A | −0.0046 | 0.5059 | 0.0720 | 0.035* | |
H7B | −0.0480 | 0.5341 | 0.1191 | 0.035* | |
C8 | −0.0167 (4) | 0.6460 (4) | 0.0227 (2) | 0.0346 (14) | |
H8A | −0.0486 | 0.6793 | 0.0015 | 0.042* | |
H8B | 0.0004 | 0.5973 | 0.0036 | 0.042* | |
C9 | 0.0183 (3) | 0.7678 (4) | 0.0658 (2) | 0.0282 (13) | |
H9A | 0.0594 | 0.8020 | 0.0767 | 0.034* | |
H9B | −0.0124 | 0.8044 | 0.0456 | 0.034* | |
C10 | −0.0806 (3) | 0.6871 (4) | 0.0926 (3) | 0.0369 (15) | |
H10A | −0.1150 | 0.7210 | 0.0736 | 0.044* | |
H10B | −0.1057 | 0.6661 | 0.1217 | 0.044* | |
C11 | 0.0986 (3) | 0.6478 (4) | 0.0616 (2) | 0.0285 (13) | |
H11A | 0.1398 | 0.6842 | 0.0696 | 0.034* | |
H11B | 0.1157 | 0.6025 | 0.0400 | 0.034* | |
C12 | 0.0250 (3) | 0.6981 (4) | 0.1431 (2) | 0.0295 (13) | |
H12A | −0.0029 | 0.6843 | 0.1725 | 0.035* | |
H12B | 0.0639 | 0.7367 | 0.1528 | 0.035* | |
C13 | −0.0117 (4) | 0.4926 (4) | 0.3748 (2) | 0.0326 (14) | |
H13A | −0.0558 | 0.4726 | 0.3587 | 0.039* | |
H13B | 0.0198 | 0.4434 | 0.3799 | 0.039* | |
C14 | −0.0783 (4) | 0.6017 (5) | 0.4161 (3) | 0.0469 (19) | |
H14A | −0.0957 | 0.6191 | 0.4485 | 0.056* | |
H14B | −0.1201 | 0.5825 | 0.3972 | 0.056* | |
C15 | 0.0165 (4) | 0.7002 (4) | 0.4186 (2) | 0.0368 (15) | |
H15A | 0.0021 | 0.7213 | 0.4509 | 0.044* | |
H15B | 0.0398 | 0.7473 | 0.4012 | 0.044* | |
C16 | 0.0344 (4) | 0.5607 (5) | 0.4480 (2) | 0.0382 (16) | |
H16A | 0.0211 | 0.5762 | 0.4815 | 0.046* | |
H16B | 0.0692 | 0.5140 | 0.4499 | 0.046* | |
C17 | −0.0309 (4) | 0.6568 (4) | 0.3413 (2) | 0.0351 (14) | |
H17A | −0.0109 | 0.7077 | 0.3257 | 0.042* | |
H17B | −0.0754 | 0.6418 | 0.3240 | 0.042* | |
C18 | 0.1000 (3) | 0.6076 (4) | 0.3782 (2) | 0.0283 (13) | |
H18A | 0.1358 | 0.5628 | 0.3839 | 0.034* | |
H18B | 0.1251 | 0.6565 | 0.3640 | 0.034* | |
C19 | 0.1803 (3) | 0.3634 (4) | 0.3669 (2) | 0.0269 (12) | |
H19A | 0.1417 | 0.4024 | 0.3767 | 0.032* | |
H19B | 0.1584 | 0.3164 | 0.3486 | 0.032* | |
C20 | 0.2474 (4) | 0.3985 (4) | 0.4397 (2) | 0.0311 (13) | |
H20A | 0.2102 | 0.4413 | 0.4461 | 0.037* | |
H20B | 0.2627 | 0.3754 | 0.4714 | 0.037* | |
C21 | 0.3610 (3) | 0.3745 (4) | 0.4040 (2) | 0.0296 (13) | |
H21A | 0.4014 | 0.4016 | 0.3869 | 0.036* | |
H21B | 0.3800 | 0.3496 | 0.4342 | 0.036* | |
C22 | 0.2710 (3) | 0.2698 (4) | 0.3978 (2) | 0.0300 (13) | |
H22A | 0.2501 | 0.2265 | 0.3763 | 0.036* | |
H22B | 0.2875 | 0.2412 | 0.4276 | 0.036* | |
C23 | 0.2860 (3) | 0.4874 (4) | 0.3736 (2) | 0.0239 (12) | |
H23A | 0.3281 | 0.5154 | 0.3593 | 0.029* | |
H23B | 0.2518 | 0.5316 | 0.3835 | 0.029* | |
C24 | 0.3136 (3) | 0.3386 (4) | 0.3252 (2) | 0.0255 (12) | |
H24A | 0.2969 | 0.2911 | 0.3049 | 0.031* | |
H24B | 0.3567 | 0.3625 | 0.3096 | 0.031* | |
C25 | 0.2074 (3) | 0.6038 (4) | 0.16749 (19) | 0.0253 (12) | |
C26 | 0.0661 (3) | 0.4266 (4) | 0.1660 (2) | 0.0253 (12) | |
C27 | 0.1014 (3) | 0.6473 (4) | 0.24557 (19) | 0.0252 (12) | |
C28 | −0.0263 (3) | 0.5543 (4) | 0.2306 (2) | 0.0295 (13) | |
C29 | 0.0443 (3) | 0.4157 (4) | 0.2700 (2) | 0.0279 (13) | |
C30 | 0.2336 (3) | 0.5838 (4) | 0.2740 (2) | 0.0258 (12) | |
C31 | 0.3020 (3) | 0.4568 (4) | 0.2250 (2) | 0.0315 (14) | |
C32 | 0.1761 (3) | 0.3613 (4) | 0.2316 (2) | 0.0273 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Os1 | 0.01825 (11) | 0.01878 (12) | 0.01494 (12) | 0.00020 (9) | 0.00030 (8) | −0.00033 (8) |
Os2 | 0.01924 (12) | 0.02431 (13) | 0.01642 (12) | −0.00041 (10) | 0.00185 (9) | −0.00012 (9) |
Os3 | 0.01938 (12) | 0.02142 (13) | 0.01743 (12) | −0.00041 (9) | −0.00109 (8) | 0.00100 (9) |
P1 | 0.0214 (6) | 0.0223 (7) | 0.0178 (6) | 0.0011 (6) | 0.0014 (5) | −0.0025 (5) |
P2 | 0.0193 (6) | 0.0222 (7) | 0.0198 (6) | −0.0015 (5) | −0.0012 (5) | 0.0016 (5) |
P3 | 0.0234 (7) | 0.0283 (7) | 0.0175 (6) | −0.0014 (6) | 0.0037 (5) | −0.0003 (6) |
P4 | 0.0235 (7) | 0.0227 (7) | 0.0183 (6) | −0.0024 (6) | −0.0023 (5) | 0.0011 (5) |
O1 | 0.035 (2) | 0.034 (2) | 0.034 (2) | −0.018 (2) | −0.0030 (19) | 0.0064 (19) |
O2 | 0.025 (2) | 0.029 (2) | 0.032 (2) | −0.0116 (18) | 0.0010 (17) | −0.0036 (17) |
O3 | 0.037 (2) | 0.023 (2) | 0.029 (2) | −0.0034 (19) | −0.0014 (18) | −0.0023 (17) |
O4 | 0.022 (2) | 0.072 (3) | 0.033 (2) | −0.008 (2) | −0.0003 (18) | 0.014 (2) |
O5 | 0.044 (3) | 0.028 (2) | 0.041 (3) | −0.008 (2) | 0.010 (2) | 0.004 (2) |
O6 | 0.036 (2) | 0.029 (2) | 0.041 (3) | −0.001 (2) | −0.010 (2) | −0.005 (2) |
O7 | 0.022 (2) | 0.076 (4) | 0.034 (3) | −0.008 (2) | 0.0049 (19) | −0.020 (2) |
O8 | 0.035 (2) | 0.026 (2) | 0.040 (2) | −0.0007 (19) | −0.0056 (19) | −0.0040 (19) |
N1 | 0.026 (2) | 0.030 (3) | 0.023 (2) | 0.009 (2) | 0.0000 (19) | −0.002 (2) |
N2 | 0.028 (3) | 0.034 (3) | 0.025 (2) | 0.008 (2) | 0.005 (2) | 0.002 (2) |
N3 | 0.028 (3) | 0.038 (3) | 0.026 (3) | 0.004 (2) | −0.003 (2) | −0.012 (2) |
N4 | 0.023 (2) | 0.032 (3) | 0.050 (3) | −0.002 (2) | −0.011 (2) | 0.006 (3) |
N5 | 0.030 (3) | 0.035 (3) | 0.022 (2) | 0.001 (2) | −0.005 (2) | 0.006 (2) |
N6 | 0.028 (3) | 0.028 (3) | 0.032 (3) | 0.005 (2) | −0.001 (2) | 0.002 (2) |
N7 | 0.045 (3) | 0.049 (4) | 0.030 (3) | −0.014 (3) | 0.016 (3) | −0.002 (3) |
N8 | 0.034 (3) | 0.046 (3) | 0.036 (3) | 0.006 (3) | 0.010 (2) | −0.008 (3) |
N9 | 0.040 (3) | 0.035 (3) | 0.023 (3) | −0.010 (2) | 0.002 (2) | −0.002 (2) |
N10 | 0.038 (3) | 0.032 (3) | 0.021 (2) | −0.007 (2) | 0.003 (2) | 0.003 (2) |
N11 | 0.029 (3) | 0.030 (3) | 0.025 (3) | −0.003 (2) | −0.010 (2) | 0.000 (2) |
N12 | 0.027 (2) | 0.026 (2) | 0.029 (3) | −0.001 (2) | −0.003 (2) | 0.002 (2) |
C1 | 0.029 (3) | 0.033 (3) | 0.021 (3) | 0.001 (3) | −0.004 (2) | −0.003 (2) |
C2 | 0.022 (3) | 0.042 (4) | 0.029 (3) | 0.008 (3) | 0.002 (2) | −0.001 (3) |
C3 | 0.036 (3) | 0.044 (4) | 0.022 (3) | 0.011 (3) | −0.002 (2) | −0.005 (3) |
C4 | 0.035 (3) | 0.026 (3) | 0.031 (3) | 0.004 (3) | 0.002 (3) | −0.004 (3) |
C5 | 0.025 (3) | 0.032 (3) | 0.028 (3) | 0.005 (3) | 0.009 (2) | 0.000 (2) |
C6 | 0.022 (3) | 0.037 (3) | 0.031 (3) | 0.003 (3) | 0.001 (2) | −0.012 (3) |
C7 | 0.021 (3) | 0.026 (3) | 0.040 (3) | −0.003 (2) | −0.004 (2) | 0.005 (3) |
C8 | 0.039 (4) | 0.035 (3) | 0.030 (3) | 0.004 (3) | −0.015 (3) | −0.002 (3) |
C9 | 0.029 (3) | 0.024 (3) | 0.032 (3) | −0.005 (2) | −0.008 (2) | 0.006 (2) |
C10 | 0.023 (3) | 0.036 (3) | 0.052 (4) | 0.003 (3) | 0.004 (3) | 0.008 (3) |
C11 | 0.025 (3) | 0.032 (3) | 0.028 (3) | 0.002 (3) | 0.001 (2) | 0.004 (3) |
C12 | 0.032 (3) | 0.028 (3) | 0.028 (3) | 0.004 (3) | −0.002 (2) | −0.001 (2) |
C13 | 0.034 (3) | 0.035 (3) | 0.028 (3) | −0.008 (3) | 0.005 (3) | 0.000 (3) |
C14 | 0.036 (4) | 0.064 (5) | 0.041 (4) | −0.007 (4) | 0.015 (3) | −0.012 (4) |
C15 | 0.041 (4) | 0.039 (4) | 0.030 (3) | −0.004 (3) | 0.012 (3) | −0.007 (3) |
C16 | 0.050 (4) | 0.047 (4) | 0.018 (3) | −0.004 (3) | 0.001 (3) | 0.000 (3) |
C17 | 0.037 (3) | 0.040 (4) | 0.028 (3) | 0.008 (3) | 0.000 (3) | −0.002 (3) |
C18 | 0.024 (3) | 0.031 (3) | 0.029 (3) | −0.002 (3) | 0.004 (2) | −0.003 (2) |
C19 | 0.022 (3) | 0.033 (3) | 0.026 (3) | −0.005 (2) | −0.002 (2) | 0.004 (2) |
C20 | 0.038 (3) | 0.034 (3) | 0.022 (3) | −0.003 (3) | −0.001 (3) | −0.002 (2) |
C21 | 0.029 (3) | 0.030 (3) | 0.030 (3) | −0.001 (3) | −0.007 (2) | 0.003 (3) |
C22 | 0.038 (3) | 0.025 (3) | 0.027 (3) | −0.006 (3) | −0.003 (3) | 0.007 (2) |
C23 | 0.025 (3) | 0.022 (3) | 0.025 (3) | −0.001 (2) | −0.002 (2) | 0.002 (2) |
C24 | 0.025 (3) | 0.026 (3) | 0.025 (3) | 0.000 (2) | 0.001 (2) | 0.001 (2) |
C25 | 0.035 (3) | 0.024 (3) | 0.017 (3) | 0.002 (3) | 0.001 (2) | 0.000 (2) |
C26 | 0.027 (3) | 0.031 (3) | 0.018 (3) | 0.006 (3) | 0.001 (2) | −0.001 (2) |
C27 | 0.024 (3) | 0.036 (3) | 0.015 (3) | −0.004 (3) | 0.002 (2) | 0.000 (2) |
C28 | 0.026 (3) | 0.039 (3) | 0.023 (3) | −0.008 (3) | 0.005 (2) | 0.003 (3) |
C29 | 0.025 (3) | 0.033 (3) | 0.025 (3) | −0.005 (3) | 0.007 (2) | −0.001 (3) |
C30 | 0.028 (3) | 0.019 (3) | 0.030 (3) | −0.004 (2) | −0.004 (2) | 0.003 (2) |
C31 | 0.034 (3) | 0.036 (3) | 0.025 (3) | −0.003 (3) | −0.005 (3) | −0.004 (3) |
C32 | 0.025 (3) | 0.029 (3) | 0.028 (3) | 0.004 (3) | 0.000 (2) | 0.002 (2) |
Os1—C25 | 1.929 (6) | N6—C12 | 1.481 (8) |
Os1—C26 | 1.938 (6) | N7—C14 | 1.459 (10) |
Os1—P1 | 2.2831 (13) | N7—C16 | 1.481 (9) |
Os1—P2 | 2.2879 (14) | N7—C13 | 1.487 (8) |
Os1—Os3 | 2.8861 (3) | N8—C17 | 1.464 (8) |
Os1—Os2 | 2.8954 (3) | N8—C15 | 1.464 (9) |
Os1A—C30 | 2.252 (12) | N8—C14 | 1.472 (9) |
Os1A—C29 | 2.275 (12) | N9—C16 | 1.456 (8) |
Os1A—P4 | 2.595 (10) | N9—C15 | 1.466 (9) |
Os1A—P3 | 2.599 (10) | N9—C18 | 1.477 (8) |
Os1A—Os3A | 2.872 (15) | N10—C22 | 1.456 (8) |
Os1A—Os2A | 2.882 (15) | N10—C20 | 1.479 (8) |
Os2—C28 | 1.880 (6) | N10—C19 | 1.481 (7) |
Os2—C27 | 1.948 (6) | N11—C20 | 1.463 (8) |
Os2—C29 | 1.957 (6) | N11—C21 | 1.473 (8) |
Os2—P3 | 2.2965 (14) | N11—C23 | 1.473 (7) |
Os2—Os3 | 2.9272 (3) | N12—C22 | 1.464 (8) |
Os2A—C31 | 2.046 (13) | N12—C21 | 1.466 (8) |
Os2A—C32 | 2.113 (12) | N12—C24 | 1.472 (7) |
Os2A—C25 | 2.211 (12) | C1—H1A | 0.9900 |
Os2A—P1 | 2.495 (11) | C1—H1B | 0.9900 |
Os2A—Os3A | 2.910 (15) | C2—H2A | 0.9900 |
Os3—C31 | 1.880 (7) | C2—H2B | 0.9900 |
Os3—C30 | 1.933 (6) | C3—H3A | 0.9900 |
Os3—C32 | 1.951 (6) | C3—H3B | 0.9900 |
Os3—P4 | 2.2963 (14) | C4—H4A | 0.9900 |
Os3A—C28 | 1.866 (12) | C4—H4B | 0.9900 |
Os3A—C27 | 2.092 (12) | C5—H5A | 0.9900 |
Os3A—C26 | 2.193 (12) | C5—H5B | 0.9900 |
Os3A—P2 | 2.425 (11) | C6—H6A | 0.9900 |
P1—C6 | 1.848 (6) | C6—H6B | 0.9900 |
P1—C5 | 1.850 (6) | C7—H7A | 0.9900 |
P1—C1 | 1.864 (6) | C7—H7B | 0.9900 |
P2—C7 | 1.841 (6) | C8—H8A | 0.9900 |
P2—C11 | 1.854 (6) | C8—H8B | 0.9900 |
P2—C12 | 1.861 (6) | C9—H9A | 0.9900 |
P3—C18 | 1.830 (6) | C9—H9B | 0.9900 |
P3—C13 | 1.849 (6) | C10—H10A | 0.9900 |
P3—C17 | 1.851 (7) | C10—H10B | 0.9900 |
P4—C24 | 1.841 (6) | C11—H11A | 0.9900 |
P4—C19 | 1.849 (6) | C11—H11B | 0.9900 |
P4—C23 | 1.852 (6) | C12—H12A | 0.9900 |
O1—C25 | 1.153 (7) | C12—H12B | 0.9900 |
O2—C26 | 1.147 (7) | C13—H13A | 0.9900 |
O3—C27 | 1.144 (7) | C13—H13B | 0.9900 |
O4—C28 | 1.154 (7) | C14—H14A | 0.9900 |
O5—C29 | 1.130 (7) | C14—H14B | 0.9900 |
O6—C30 | 1.146 (7) | C15—H15A | 0.9900 |
O7—C31 | 1.146 (8) | C15—H15B | 0.9900 |
O8—C32 | 1.146 (7) | C16—H16A | 0.9900 |
N1—C2 | 1.469 (8) | C16—H16B | 0.9900 |
N1—C4 | 1.472 (8) | C17—H17A | 0.9900 |
N1—C1 | 1.477 (7) | C17—H17B | 0.9900 |
N2—C2 | 1.459 (7) | C18—H18A | 0.9900 |
N2—C3 | 1.468 (8) | C18—H18B | 0.9900 |
N2—C5 | 1.476 (7) | C19—H19A | 0.9900 |
N3—C4 | 1.457 (8) | C19—H19B | 0.9900 |
N3—C3 | 1.465 (9) | C20—H20A | 0.9900 |
N3—C6 | 1.473 (7) | C20—H20B | 0.9900 |
N4—C8 | 1.452 (9) | C21—H21A | 0.9900 |
N4—C7 | 1.462 (8) | C21—H21B | 0.9900 |
N4—C10 | 1.470 (9) | C22—H22A | 0.9900 |
N5—C8 | 1.470 (8) | C22—H22B | 0.9900 |
N5—C9 | 1.471 (8) | C23—H23A | 0.9900 |
N5—C11 | 1.476 (7) | C23—H23B | 0.9900 |
N6—C9 | 1.448 (8) | C24—H24A | 0.9900 |
N6—C10 | 1.465 (8) | C24—H24B | 0.9900 |
C25—Os1—C26 | 176.7 (2) | C21—N12—C24 | 110.8 (5) |
C25—Os1—P1 | 93.20 (17) | N1—C1—P1 | 112.7 (4) |
C26—Os1—P1 | 88.80 (17) | N1—C1—H1A | 109.1 |
C25—Os1—P2 | 90.29 (17) | P1—C1—H1A | 109.1 |
C26—Os1—P2 | 91.96 (17) | N1—C1—H1B | 109.1 |
P1—Os1—P2 | 100.38 (5) | P1—C1—H1B | 109.1 |
C25—Os1—Os3 | 79.18 (16) | H1A—C1—H1B | 107.8 |
C26—Os1—Os3 | 97.76 (16) | N2—C2—N1 | 114.4 (5) |
P1—Os1—Os3 | 103.89 (4) | N2—C2—H2A | 108.7 |
P2—Os1—Os3 | 153.97 (4) | N1—C2—H2A | 108.7 |
C25—Os1—Os2 | 102.28 (16) | N2—C2—H2B | 108.7 |
C26—Os1—Os2 | 74.96 (16) | N1—C2—H2B | 108.7 |
P1—Os1—Os2 | 154.98 (4) | H2A—C2—H2B | 107.6 |
P2—Os1—Os2 | 99.09 (4) | N3—C3—N2 | 114.5 (5) |
Os3—Os1—Os2 | 60.835 (8) | N3—C3—H3A | 108.6 |
C30—Os1A—C29 | 158.1 (6) | N2—C3—H3A | 108.6 |
C30—Os1A—P4 | 76.0 (3) | N3—C3—H3B | 108.6 |
C29—Os1A—P4 | 112.6 (4) | N2—C3—H3B | 108.6 |
C30—Os1A—P3 | 115.9 (4) | H3A—C3—H3B | 107.6 |
C29—Os1A—P3 | 76.6 (3) | N3—C4—N1 | 114.5 (5) |
P4—Os1A—P3 | 124.8 (4) | N3—C4—H4A | 108.6 |
C30—Os1A—Os3A | 95.2 (4) | N1—C4—H4A | 108.6 |
C29—Os1A—Os3A | 66.8 (4) | N3—C4—H4B | 108.6 |
P4—Os1A—Os3A | 148.9 (5) | N1—C4—H4B | 108.6 |
P3—Os1A—Os3A | 86.0 (4) | H4A—C4—H4B | 107.6 |
C30—Os1A—Os2A | 66.8 (4) | N2—C5—P1 | 113.5 (4) |
C29—Os1A—Os2A | 92.8 (4) | N2—C5—H5A | 108.9 |
P4—Os1A—Os2A | 88.7 (4) | P1—C5—H5A | 108.9 |
P3—Os1A—Os2A | 146.5 (5) | N2—C5—H5B | 108.9 |
Os3A—Os1A—Os2A | 60.8 (4) | P1—C5—H5B | 108.9 |
C28—Os2—C27 | 95.9 (3) | H5A—C5—H5B | 107.7 |
C28—Os2—C29 | 93.3 (3) | N3—C6—P1 | 113.6 (4) |
C27—Os2—C29 | 170.4 (3) | N3—C6—H6A | 108.9 |
C28—Os2—P3 | 95.26 (18) | P1—C6—H6A | 108.9 |
C27—Os2—P3 | 91.00 (16) | N3—C6—H6B | 108.9 |
C29—Os2—P3 | 90.61 (17) | P1—C6—H6B | 108.9 |
C28—Os2—Os1 | 95.78 (18) | H6A—C6—H6B | 107.7 |
C27—Os2—Os1 | 77.69 (16) | N4—C7—P2 | 113.6 (4) |
C29—Os2—Os1 | 98.95 (17) | N4—C7—H7A | 108.8 |
P3—Os2—Os1 | 164.93 (4) | P2—C7—H7A | 108.8 |
C28—Os2—Os3 | 153.25 (19) | N4—C7—H7B | 108.8 |
C27—Os2—Os3 | 88.68 (18) | P2—C7—H7B | 108.8 |
C29—Os2—Os3 | 81.95 (17) | H7A—C7—H7B | 107.7 |
P3—Os2—Os3 | 111.03 (4) | N4—C8—N5 | 115.6 (5) |
Os1—Os2—Os3 | 59.425 (8) | N4—C8—H8A | 108.4 |
C31—Os2A—C32 | 85.1 (5) | N5—C8—H8A | 108.4 |
C31—Os2A—C25 | 103.2 (5) | N4—C8—H8B | 108.4 |
C32—Os2A—C25 | 163.9 (6) | N5—C8—H8B | 108.4 |
C31—Os2A—P1 | 115.8 (5) | H8A—C8—H8B | 107.4 |
C32—Os2A—P1 | 108.0 (5) | N6—C9—N5 | 114.9 (5) |
C25—Os2A—P1 | 81.2 (4) | N6—C9—H9A | 108.5 |
C31—Os2A—Os1A | 91.8 (5) | N5—C9—H9A | 108.5 |
C32—Os2A—Os1A | 65.8 (4) | N6—C9—H9B | 108.5 |
C25—Os2A—Os1A | 99.7 (5) | N5—C9—H9B | 108.5 |
P1—Os2A—Os1A | 151.6 (5) | H9A—C9—H9B | 107.5 |
C31—Os2A—Os3A | 147.1 (6) | N6—C10—N4 | 114.3 (5) |
C32—Os2A—Os3A | 95.8 (5) | N6—C10—H10A | 108.7 |
C25—Os2A—Os3A | 69.7 (4) | N4—C10—H10A | 108.7 |
P1—Os2A—Os3A | 95.3 (4) | N6—C10—H10B | 108.7 |
Os1A—Os2A—Os3A | 59.4 (4) | N4—C10—H10B | 108.7 |
C31—Os3—C30 | 92.2 (3) | H10A—C10—H10B | 107.6 |
C31—Os3—C32 | 94.4 (3) | N5—C11—P2 | 113.9 (4) |
C30—Os3—C32 | 173.0 (2) | N5—C11—H11A | 108.8 |
C31—Os3—P4 | 94.47 (19) | P2—C11—H11A | 108.8 |
C30—Os3—P4 | 89.81 (17) | N5—C11—H11B | 108.8 |
C32—Os3—P4 | 92.11 (18) | P2—C11—H11B | 108.8 |
C31—Os3—Os1 | 97.47 (19) | H11A—C11—H11B | 107.7 |
C30—Os3—Os1 | 97.74 (17) | N6—C12—P2 | 113.0 (4) |
C32—Os3—Os1 | 79.00 (17) | N6—C12—H12A | 109.0 |
P4—Os3—Os1 | 165.60 (4) | P2—C12—H12A | 109.0 |
C31—Os3—Os2 | 155.42 (19) | N6—C12—H12B | 109.0 |
C30—Os3—Os2 | 82.79 (18) | P2—C12—H12B | 109.0 |
C32—Os3—Os2 | 90.20 (17) | H12A—C12—H12B | 107.8 |
P4—Os3—Os2 | 109.50 (4) | N7—C13—P3 | 111.5 (4) |
Os1—Os3—Os2 | 59.740 (8) | N7—C13—H13A | 109.3 |
C28—Os3A—C27 | 91.7 (5) | P3—C13—H13A | 109.3 |
C28—Os3A—C26 | 104.2 (5) | N7—C13—H13B | 109.3 |
C27—Os3A—C26 | 155.8 (6) | P3—C13—H13B | 109.3 |
C28—Os3A—P2 | 114.0 (5) | H13A—C13—H13B | 108.0 |
C27—Os3A—P2 | 107.9 (5) | N7—C14—N8 | 115.7 (6) |
C26—Os3A—P2 | 82.5 (4) | N7—C14—H14A | 108.3 |
C28—Os3A—Os1A | 95.4 (5) | N8—C14—H14A | 108.3 |
C27—Os3A—Os1A | 63.4 (4) | N7—C14—H14B | 108.3 |
C26—Os3A—Os1A | 96.5 (4) | N8—C14—H14B | 108.3 |
P2—Os3A—Os1A | 150.0 (5) | H14A—C14—H14B | 107.4 |
C28—Os3A—Os2A | 149.2 (6) | N8—C15—N9 | 114.9 (5) |
C27—Os3A—Os2A | 92.4 (4) | N8—C15—H15A | 108.6 |
C26—Os3A—Os2A | 64.6 (4) | N9—C15—H15A | 108.6 |
P2—Os3A—Os2A | 93.7 (4) | N8—C15—H15B | 108.6 |
Os1A—Os3A—Os2A | 59.8 (4) | N9—C15—H15B | 108.6 |
C6—P1—C5 | 97.7 (3) | H15A—C15—H15B | 107.5 |
C6—P1—C1 | 96.5 (3) | N9—C16—N7 | 114.3 (5) |
C5—P1—C1 | 96.4 (3) | N9—C16—H16A | 108.7 |
C6—P1—Os1 | 115.11 (19) | N7—C16—H16A | 108.7 |
C5—P1—Os1 | 122.0 (2) | N9—C16—H16B | 108.7 |
C1—P1—Os1 | 123.49 (18) | N7—C16—H16B | 108.7 |
C6—P1—Os2A | 134.6 (3) | H16A—C16—H16B | 107.6 |
C5—P1—Os2A | 127.4 (3) | N8—C17—P3 | 112.8 (5) |
C1—P1—Os2A | 84.2 (3) | N8—C17—H17A | 109.0 |
C7—P2—C11 | 96.8 (3) | P3—C17—H17A | 109.0 |
C7—P2—C12 | 97.7 (3) | N8—C17—H17B | 109.0 |
C11—P2—C12 | 95.7 (3) | P3—C17—H17B | 109.0 |
C7—P2—Os1 | 119.0 (2) | H17A—C17—H17B | 107.8 |
C11—P2—Os1 | 120.71 (19) | N9—C18—P3 | 113.3 (4) |
C12—P2—Os1 | 121.3 (2) | N9—C18—H18A | 108.9 |
C7—P2—Os3A | 103.5 (3) | P3—C18—H18A | 108.9 |
C11—P2—Os3A | 159.4 (3) | N9—C18—H18B | 108.9 |
C12—P2—Os3A | 85.5 (3) | P3—C18—H18B | 108.9 |
C18—P3—C13 | 98.2 (3) | H18A—C18—H18B | 107.7 |
C18—P3—C17 | 97.6 (3) | N10—C19—P4 | 112.1 (4) |
C13—P3—C17 | 97.9 (3) | N10—C19—H19A | 109.2 |
C18—P3—Os2 | 121.42 (19) | P4—C19—H19A | 109.2 |
C13—P3—Os2 | 120.9 (2) | N10—C19—H19B | 109.2 |
C17—P3—Os2 | 115.8 (2) | P4—C19—H19B | 109.2 |
C18—P3—Os1A | 87.4 (3) | H19A—C19—H19B | 107.9 |
C13—P3—Os1A | 111.8 (3) | N11—C20—N10 | 114.5 (5) |
C17—P3—Os1A | 148.9 (3) | N11—C20—H20A | 108.6 |
C24—P4—C19 | 97.8 (3) | N10—C20—H20A | 108.6 |
C24—P4—C23 | 96.9 (3) | N11—C20—H20B | 108.6 |
C19—P4—C23 | 98.3 (3) | N10—C20—H20B | 108.6 |
C24—P4—Os3 | 114.33 (19) | H20A—C20—H20B | 107.6 |
C19—P4—Os3 | 122.26 (19) | N12—C21—N11 | 114.5 (5) |
C23—P4—Os3 | 121.95 (19) | N12—C21—H21A | 108.6 |
C24—P4—Os1A | 151.2 (3) | N11—C21—H21A | 108.6 |
C19—P4—Os1A | 90.1 (3) | N12—C21—H21B | 108.6 |
C23—P4—Os1A | 109.3 (3) | N11—C21—H21B | 108.6 |
C2—N1—C4 | 108.3 (5) | H21A—C21—H21B | 107.6 |
C2—N1—C1 | 111.4 (5) | N10—C22—N12 | 115.0 (5) |
C4—N1—C1 | 110.9 (5) | N10—C22—H22A | 108.5 |
C2—N2—C3 | 108.5 (5) | N12—C22—H22A | 108.5 |
C2—N2—C5 | 110.9 (5) | N10—C22—H22B | 108.5 |
C3—N2—C5 | 110.8 (5) | N12—C22—H22B | 108.5 |
C4—N3—C3 | 108.9 (5) | H22A—C22—H22B | 107.5 |
C4—N3—C6 | 110.0 (5) | N11—C23—P4 | 112.6 (4) |
C3—N3—C6 | 111.3 (5) | N11—C23—H23A | 109.1 |
C8—N4—C7 | 111.6 (5) | P4—C23—H23A | 109.1 |
C8—N4—C10 | 107.9 (5) | N11—C23—H23B | 109.1 |
C7—N4—C10 | 110.7 (5) | P4—C23—H23B | 109.1 |
C8—N5—C9 | 107.0 (5) | H23A—C23—H23B | 107.8 |
C8—N5—C11 | 110.2 (5) | N12—C24—P4 | 113.1 (4) |
C9—N5—C11 | 111.2 (5) | N12—C24—H24A | 109.0 |
C9—N6—C10 | 109.1 (5) | P4—C24—H24A | 109.0 |
C9—N6—C12 | 110.5 (5) | N12—C24—H24B | 109.0 |
C10—N6—C12 | 111.0 (5) | P4—C24—H24B | 109.0 |
C14—N7—C16 | 108.1 (6) | H24A—C24—H24B | 107.8 |
C14—N7—C13 | 110.6 (6) | O1—C25—Os1 | 175.5 (5) |
C16—N7—C13 | 111.3 (5) | O1—C25—Os2A | 135.8 (6) |
C17—N8—C15 | 111.0 (5) | O2—C26—Os1 | 175.0 (5) |
C17—N8—C14 | 110.6 (6) | O2—C26—Os3A | 130.9 (5) |
C15—N8—C14 | 107.6 (6) | O3—C27—Os2 | 175.6 (5) |
C16—N9—C15 | 109.4 (5) | O3—C27—Os3A | 137.6 (5) |
C16—N9—C18 | 110.0 (5) | O4—C28—Os3A | 129.4 (6) |
C15—N9—C18 | 110.6 (5) | O4—C28—Os2 | 176.3 (6) |
C22—N10—C20 | 109.0 (5) | O5—C29—Os2 | 175.0 (5) |
C22—N10—C19 | 110.6 (5) | O5—C29—Os1A | 134.3 (6) |
C20—N10—C19 | 110.7 (5) | O6—C30—Os3 | 173.8 (5) |
C20—N11—C21 | 108.2 (5) | O6—C30—Os1A | 134.3 (6) |
C20—N11—C23 | 110.9 (5) | O7—C31—Os3 | 178.1 (6) |
C21—N11—C23 | 111.1 (5) | O7—C31—Os2A | 132.5 (6) |
C22—N12—C21 | 108.3 (5) | O8—C32—Os3 | 176.2 (5) |
C22—N12—C24 | 110.9 (5) | O8—C32—Os2A | 136.4 (6) |
C2—N1—C1—P1 | 60.5 (5) | C17—P3—C13—N7 | −50.2 (5) |
C4—N1—C1—P1 | −60.1 (6) | Os2—P3—C13—N7 | −176.8 (4) |
C6—P1—C1—N1 | 49.1 (5) | Os1A—P3—C13—N7 | 139.2 (5) |
C5—P1—C1—N1 | −49.4 (5) | C16—N7—C14—N8 | 54.6 (7) |
Os1—P1—C1—N1 | 175.1 (3) | C13—N7—C14—N8 | −67.5 (8) |
Os2A—P1—C1—N1 | −176.6 (5) | C17—N8—C14—N7 | 66.7 (8) |
C3—N2—C2—N1 | −55.2 (6) | C15—N8—C14—N7 | −54.7 (7) |
C5—N2—C2—N1 | 66.7 (7) | C17—N8—C15—N9 | −67.3 (7) |
C4—N1—C2—N2 | 55.2 (6) | C14—N8—C15—N9 | 53.9 (7) |
C1—N1—C2—N2 | −67.0 (6) | C16—N9—C15—N8 | −54.7 (7) |
C4—N3—C3—N2 | −54.1 (6) | C18—N9—C15—N8 | 66.7 (7) |
C6—N3—C3—N2 | 67.4 (6) | C15—N9—C16—N7 | 54.0 (7) |
C2—N2—C3—N3 | 54.5 (6) | C18—N9—C16—N7 | −67.8 (7) |
C5—N2—C3—N3 | −67.5 (6) | C14—N7—C16—N9 | −53.6 (7) |
C3—N3—C4—N1 | 54.2 (6) | C13—N7—C16—N9 | 68.1 (8) |
C6—N3—C4—N1 | −68.0 (6) | C15—N8—C17—P3 | 60.0 (7) |
C2—N1—C4—N3 | −54.6 (6) | C14—N8—C17—P3 | −59.4 (7) |
C1—N1—C4—N3 | 67.9 (6) | C18—P3—C17—N8 | −49.2 (5) |
C2—N2—C5—P1 | −61.1 (6) | C13—P3—C17—N8 | 50.3 (5) |
C3—N2—C5—P1 | 59.5 (6) | Os2—P3—C17—N8 | −179.6 (4) |
C6—P1—C5—N2 | −47.5 (5) | Os1A—P3—C17—N8 | −146.8 (6) |
C1—P1—C5—N2 | 49.9 (5) | C16—N9—C18—P3 | 61.2 (6) |
Os1—P1—C5—N2 | −173.6 (3) | C15—N9—C18—P3 | −59.8 (6) |
Os2A—P1—C5—N2 | 137.6 (5) | C13—P3—C18—N9 | −50.1 (5) |
C4—N3—C6—P1 | 61.8 (6) | C17—P3—C18—N9 | 49.1 (5) |
C3—N3—C6—P1 | −59.1 (6) | Os2—P3—C18—N9 | 175.7 (3) |
C5—P1—C6—N3 | 47.2 (5) | Os1A—P3—C18—N9 | −161.7 (5) |
C1—P1—C6—N3 | −50.2 (5) | C22—N10—C19—P4 | −60.8 (6) |
Os1—P1—C6—N3 | 178.0 (4) | C20—N10—C19—P4 | 60.1 (6) |
Os2A—P1—C6—N3 | −138.5 (5) | C24—P4—C19—N10 | 49.3 (5) |
C8—N4—C7—P2 | 59.8 (6) | C23—P4—C19—N10 | −48.9 (5) |
C10—N4—C7—P2 | −60.5 (6) | Os3—P4—C19—N10 | 174.7 (3) |
C11—P2—C7—N4 | −48.7 (5) | Os1A—P4—C19—N10 | −158.4 (5) |
C12—P2—C7—N4 | 48.1 (5) | C21—N11—C20—N10 | −54.0 (6) |
Os1—P2—C7—N4 | −179.5 (4) | C23—N11—C20—N10 | 68.0 (7) |
Os3A—P2—C7—N4 | 135.3 (5) | C22—N10—C20—N11 | 53.6 (6) |
C7—N4—C8—N5 | −66.4 (7) | C19—N10—C20—N11 | −68.3 (7) |
C10—N4—C8—N5 | 55.5 (7) | C22—N12—C21—N11 | −55.3 (6) |
C9—N5—C8—N4 | −55.4 (7) | C24—N12—C21—N11 | 66.5 (6) |
C11—N5—C8—N4 | 65.6 (7) | C20—N11—C21—N12 | 55.4 (6) |
C10—N6—C9—N5 | −55.0 (6) | C23—N11—C21—N12 | −66.6 (6) |
C12—N6—C9—N5 | 67.3 (6) | C20—N10—C22—N12 | −53.8 (6) |
C8—N5—C9—N6 | 54.6 (6) | C19—N10—C22—N12 | 68.1 (6) |
C11—N5—C9—N6 | −65.7 (6) | C21—N12—C22—N10 | 54.6 (6) |
C9—N6—C10—N4 | 54.3 (7) | C24—N12—C22—N10 | −67.1 (6) |
C12—N6—C10—N4 | −67.7 (7) | C20—N11—C23—P4 | −59.9 (6) |
C8—N4—C10—N6 | −54.0 (7) | C21—N11—C23—P4 | 60.4 (5) |
C7—N4—C10—N6 | 68.4 (7) | C24—P4—C23—N11 | −50.1 (4) |
C8—N5—C11—P2 | −59.1 (6) | C19—P4—C23—N11 | 48.8 (5) |
C9—N5—C11—P2 | 59.4 (6) | Os3—P4—C23—N11 | −174.6 (3) |
C7—P2—C11—N5 | 49.0 (5) | Os1A—P4—C23—N11 | 141.9 (4) |
C12—P2—C11—N5 | −49.5 (5) | C22—N12—C24—P4 | 59.2 (6) |
Os1—P2—C11—N5 | 178.6 (3) | C21—N12—C24—P4 | −61.1 (6) |
Os3A—P2—C11—N5 | −142.1 (8) | C19—P4—C24—N12 | −48.9 (4) |
C9—N6—C12—P2 | −62.4 (6) | C23—P4—C24—N12 | 50.6 (4) |
C10—N6—C12—P2 | 58.8 (6) | Os3—P4—C24—N12 | −179.6 (3) |
C7—P2—C12—N6 | −47.0 (5) | Os1A—P4—C24—N12 | −153.5 (5) |
C11—P2—C12—N6 | 50.7 (5) | C27—Os3A—C28—O4 | 125.6 (8) |
Os1—P2—C12—N6 | −177.9 (3) | C26—Os3A—C28—O4 | −72.8 (9) |
Os3A—P2—C12—N6 | −150.0 (5) | P2—Os3A—C28—O4 | 15.1 (10) |
C14—N7—C13—P3 | 60.7 (6) | Os1A—Os3A—C28—O4 | −171.0 (7) |
C16—N7—C13—P3 | −59.5 (7) | Os2A—Os3A—C28—O4 | −136.8 (10) |
C18—P3—C13—N7 | 48.7 (5) |
Acknowledgements
We are thankful for the support of the Abilene Christian University Scholars Lab.
Funding information
Funding for this research was provided by: The Welch Foundation (grant No. R-0021).
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