metal-organic compounds
Poly[octacarbonylheptakis(tetrahydrofuran)diironmanganesedisodium(2 Mn—Fe)]
aDepartment of Chemistry, PO Box 6949, Radford University, Radford, VA 24142, USA, and bDepartment of Chemistry, 1204 Boston Avenue, Texas Tech University, Lubbock, TX 79409, USA
*Correspondence e-mail: gharakas@radford.edu
The reaction of Na2Fe(CO)4 with an excess of MnCl2 in tetrahydrofuran (THF) produced {Fe2Mn(C4H8O)2Na2(C4H8O)5(CO)8]n or C36H56Fe2MnNa2O15. The compound is a xenophilic dianion with short iron–manganese bond lengths of 2.6274 (10) and 2.6294 (10) Å. The sodium cations of the dianion are coordinated to THF ligands and have isocarbonyl interactions forming a polymeric (two-dimensional) structure in the crystal. One of the THF molecules was modeled with the carbon atoms being statistically disordered.
Keywords: crystal structure; metal cluster; iron; manganese.
CCDC reference: 2103160
Structure description
The term xenophilic transition-metal cluster was first used to describe the unusual structure of {μ-Mn(THF)2}Fe2(CO)8 (Harakas & Whittlesey, 1996). In a xenophilic cluster, two transition metals with open d-shells form a direct, unbridged bond between a metal center attached to π-acceptor ligands and one that is bound only to donor ligands that have no π-acceptor capabilities (Whittlesey, 2000). The title compound, Na2{μ-Mn(THF)2}Fe2(CO)8, has unsupported metal–metal bonds of 2.6274 (10) and 2.6294 (10) Å between the Mn(THF)2 and two Fe(CO)4 fragments (Fig. 1). The Mn—Fe bond lengths are significantly shorter than those of 2.813 (3) Å observed for FeMn2(CO)14 (Agron et al.,1967) and 2.841 (4) Å for (μ-C5H5)(OC)2FeMn(CO)5 (Hansen, et al., 1966). The Fe—Mn bond distances for {μ-Mn(THF)2}Fe2(CO)8 are 2.633 (1) and 2.601 (1) Å (Harakas & Whittlesey, 1996). Despite the similarity of metal–metal bond lengths, the Fe—Mn—Fe bond angle of 136.81 (3)° for the dianion is considerable larger than 112.8 (1)°, which was observed for neutral {μ-Mn(THF)2}Fe2(CO)8. The sodium cations of the title complex are bound to the dianion via isocarbonyl linkages. The isocarbonyl linkages to the sodium cations create a two-dimensional network (Fig. 2).
Synthesis and crystallization
All manipulations were conducted using inert atmosphere techniques. In a dry box Na2Fe(CO)4 (0.997 g, 4.66 mmol) and MnCl2 (1.181 g, 9.384 mmol) were added to a 150 mL Schlenk flask with a magnetic stirring bar. The flask was closed with a rubber septum then transferred to a Schlenk line. To this flask, 75 mL of anhydrous THF were added and the reaction mixture was stirred rapidly. The solution formed a deep yellow–orange color as the THF was added. The mixture was stirred for 30 minutes then allowed to settle for 24 h. The bright-orange solution was decanted from the solids into another Schlenk flask. The solution was placed into a freezer at −15°C. Large block-like yellow crystals formed after several days. At 25 °C the complex rapidly decomposes when exposed to oxygen and when the crystals are removed from the mother liquor. A single crystal was coated with NVH oil and mounted on a MiTeGen loop under a stream of argon gas then cooled to −45°C for data collection.
Refinement
Crystal data, data collection, and structure . One tetrahydrofuran molecule coordinating Na2 was modeled for disorder with the C33—C36 atoms statistically disordered. The H atoms on the disordered THF molecule C33–C36/C33A–C36A were not located.
details are summarized in Table 1Structural data
CCDC reference: 2103160
https://doi.org/10.1107/S2414314621008452/tk4070sup1.cif
contains datablocks global, I. DOI:Structure factors: contains datablock I. DOI: https://doi.org/10.1107/S2414314621008452/tk4070Isup2.hkl
Data collection: APEX3 (Bruker, 2019); cell
SAINT (Bruker, 2019); data reduction: SAINT (Bruker, 2019); program(s) used to solve structure: SHELXT2018/2 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2018/2 (Sheldrick, 2015b); molecular graphics: OLEX2 (Dolomanov et al., 2009); software used to prepare material for publication: shelXle (Hübschle et al., 2011).[Fe2MnNa2(C4H8O)7(CO)8] | Z = 2 |
Mr = 933.36 | F(000) = 966 |
Triclinic, P1 | Dx = 1.391 Mg m−3 |
a = 9.3839 (11) Å | Mo Kα radiation, λ = 0.71073 Å |
b = 9.9442 (11) Å | Cell parameters from 9427 reflections |
c = 24.348 (3) Å | θ = 2.8–29.7° |
α = 95.154 (5)° | µ = 1.00 mm−1 |
β = 92.640 (5)° | T = 228 K |
γ = 99.414 (5)° | Cube, yellow |
V = 2228.1 (4) Å3 | 0.39 × 0.35 × 0.31 mm |
Bruker D8 Quest Eco, Photon PII 7 diffractometer | 10027 reflections with I > 2σ(I) |
Detector resolution: 7.3910 pixels mm-1 | Rint = 0.057 |
phi and ω scans | θmax = 29.9°, θmin = 2.3° |
Absorption correction: multi-scan (SADABS; Krause et al., 2015) | h = −13→13 |
Tmin = 0.68, Tmax = 0.73 | k = −13→13 |
154320 measured reflections | l = −34→34 |
12761 independent reflections |
Refinement on F2 | 0 restraints |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.090 | H-atom parameters constrained |
wR(F2) = 0.217 | w = 1/[σ2(Fo2) + (0.0431P)2 + 11.8029P] where P = (Fo2 + 2Fc2)/3 |
S = 1.12 | (Δ/σ)max = 0.001 |
12761 reflections | Δρmax = 0.89 e Å−3 |
541 parameters | Δρmin = −1.77 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. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Fe1 | 0.48239 (8) | 0.26076 (7) | 0.18023 (3) | 0.03809 (18) | |
Fe2 | 0.79486 (7) | 0.55567 (7) | 0.32428 (3) | 0.03322 (16) | |
Mn1 | 0.71446 (8) | 0.35449 (7) | 0.24588 (3) | 0.03290 (16) | |
Na1 | 0.2691 (2) | 0.3843 (3) | 0.36059 (10) | 0.0526 (6) | |
Na2 | 0.6115 (3) | 0.7720 (2) | 0.16011 (9) | 0.0469 (5) | |
O1 | 0.7818 (6) | 0.7222 (5) | 0.23192 (19) | 0.0660 (12) | |
O2 | 0.8840 (8) | 0.7683 (5) | 0.4142 (2) | 0.0891 (19) | |
O3 | 0.5154 (5) | 0.4355 (7) | 0.3595 (2) | 0.0789 (16) | |
O4 | 1.0325 (4) | 0.4044 (5) | 0.33895 (19) | 0.0599 (11) | |
O5 | 0.5983 (7) | 0.5281 (5) | 0.1459 (2) | 0.0813 (17) | |
O6 | 0.6271 (5) | 0.0226 (4) | 0.17057 (19) | 0.0570 (11) | |
O7 | 0.3016 (6) | 0.2677 (6) | 0.2747 (2) | 0.0799 (16) | |
O8 | 0.2773 (8) | 0.1757 (8) | 0.0860 (3) | 0.121 (3) | |
O9 | 0.7649 (4) | 0.1760 (4) | 0.28376 (16) | 0.0454 (8) | |
O10 | 0.8976 (5) | 0.3564 (5) | 0.19223 (17) | 0.0568 (10) | |
O11 | 0.2429 (7) | 0.1979 (6) | 0.4098 (2) | 0.0818 (16) | |
O12 | 0.2849 (6) | 0.5508 (7) | 0.4348 (3) | 0.095 (2) | |
O13 | 0.4276 (6) | 0.7701 (6) | 0.2220 (2) | 0.0802 (16) | |
O14 | 0.4509 (7) | 0.7502 (5) | 0.0810 (2) | 0.0772 (15) | |
O15 | 0.8067 (8) | 0.8112 (8) | 0.1062 (3) | 0.103 (2) | |
C1 | 0.7869 (6) | 0.6505 (6) | 0.2674 (2) | 0.0420 (11) | |
C2 | 0.8491 (8) | 0.6852 (6) | 0.3783 (2) | 0.0539 (15) | |
C3 | 0.6276 (6) | 0.4794 (7) | 0.3437 (2) | 0.0492 (13) | |
C4 | 0.9358 (5) | 0.4632 (5) | 0.3307 (2) | 0.0383 (10) | |
C5 | 0.5563 (7) | 0.4215 (6) | 0.1616 (2) | 0.0520 (14) | |
C6 | 0.5742 (6) | 0.1216 (5) | 0.1755 (2) | 0.0399 (10) | |
C7 | 0.3776 (7) | 0.2664 (7) | 0.2378 (2) | 0.0527 (14) | |
C8 | 0.3572 (7) | 0.2088 (7) | 0.1237 (3) | 0.0628 (17) | |
C9 | 0.8819 (7) | 0.0999 (6) | 0.2771 (3) | 0.0598 (16) | |
H9A | 0.973803 | 0.161725 | 0.275033 | 0.072* | |
H9B | 0.864289 | 0.036212 | 0.243395 | 0.072* | |
C10 | 0.8842 (10) | 0.0245 (8) | 0.3269 (4) | 0.086 (3) | |
H10A | 0.94729 | 0.078928 | 0.356835 | 0.103* | |
H10B | 0.918117 | −0.062826 | 0.318562 | 0.103* | |
C11 | 0.7309 (13) | 0.0016 (10) | 0.3420 (4) | 0.106 (3) | |
H11A | 0.678883 | −0.085972 | 0.324062 | 0.127* | |
H11B | 0.725456 | 0.001604 | 0.382053 | 0.127* | |
C12 | 0.6697 (9) | 0.1166 (9) | 0.3220 (4) | 0.079 (2) | |
H12A | 0.573156 | 0.08388 | 0.304011 | 0.095* | |
H12B | 0.661356 | 0.184459 | 0.352987 | 0.095* | |
C13 | 1.0337 (9) | 0.4396 (13) | 0.2019 (3) | 0.111 (4) | |
H13A | 1.095579 | 0.396952 | 0.226162 | 0.133* | |
H13B | 1.023152 | 0.528918 | 0.220231 | 0.133* | |
C14 | 1.0999 (10) | 0.4576 (12) | 0.1496 (4) | 0.096 (3) | |
H14A | 1.110652 | 0.553584 | 0.141814 | 0.115* | |
H14B | 1.195631 | 0.430306 | 0.150653 | 0.115* | |
C15 | 1.0039 (12) | 0.3712 (15) | 0.1082 (4) | 0.129 (5) | |
H15A | 1.056239 | 0.308318 | 0.087191 | 0.155* | |
H15B | 0.962303 | 0.426854 | 0.082469 | 0.155* | |
C16 | 0.8913 (12) | 0.2957 (12) | 0.1373 (4) | 0.129 (5) | |
H16A | 0.796391 | 0.297377 | 0.119036 | 0.155* | |
H16B | 0.904888 | 0.199993 | 0.137059 | 0.155* | |
C17 | 0.1889 (12) | 0.1797 (12) | 0.4620 (4) | 0.103 (3) | |
H17A | 0.084358 | 0.179603 | 0.460333 | 0.124* | |
H17B | 0.235543 | 0.25449 | 0.489131 | 0.124* | |
C18 | 0.2193 (18) | 0.0494 (12) | 0.4780 (5) | 0.140 (5) | |
H18A | 0.290831 | 0.063918 | 0.509484 | 0.168* | |
H18B | 0.130854 | −0.007246 | 0.488238 | 0.168* | |
C19 | 0.274 (2) | −0.0141 (13) | 0.4315 (6) | 0.178 (8) | |
H19A | 0.368185 | −0.038239 | 0.441643 | 0.214* | |
H19B | 0.207838 | −0.098531 | 0.41783 | 0.214* | |
C20 | 0.2889 (13) | 0.0753 (10) | 0.3900 (4) | 0.104 (3) | |
H20A | 0.22986 | 0.033685 | 0.356656 | 0.125* | |
H20B | 0.390167 | 0.094416 | 0.380624 | 0.125* | |
C21 | 0.1654 (10) | 0.5705 (13) | 0.4651 (4) | 0.114 (4) | |
H21A | 0.108313 | 0.481587 | 0.470617 | 0.137* | |
H21B | 0.103597 | 0.621606 | 0.444536 | 0.137* | |
C22 | 0.2130 (12) | 0.6441 (13) | 0.5170 (4) | 0.114 (4) | |
H22A | 0.19841 | 0.583595 | 0.546576 | 0.137* | |
H22B | 0.158879 | 0.719473 | 0.524342 | 0.137* | |
C23 | 0.3688 (11) | 0.6981 (10) | 0.5141 (4) | 0.090 (3) | |
H23A | 0.42569 | 0.671067 | 0.544781 | 0.108* | |
H23B | 0.385726 | 0.798283 | 0.515469 | 0.108* | |
C24 | 0.4078 (10) | 0.6345 (10) | 0.4593 (4) | 0.088 (3) | |
H24A | 0.442022 | 0.706119 | 0.435602 | 0.105* | |
H24B | 0.485049 | 0.580785 | 0.465058 | 0.105* | |
C25 | 0.3947 (9) | 0.6781 (9) | 0.2624 (3) | 0.076 (2) | |
H25A | 0.482244 | 0.670929 | 0.284741 | 0.091* | |
H25B | 0.352261 | 0.586772 | 0.244962 | 0.091* | |
C26 | 0.2899 (12) | 0.7358 (13) | 0.2970 (4) | 0.108 (3) | |
H26A | 0.339321 | 0.793617 | 0.329264 | 0.129* | |
H26B | 0.219405 | 0.662848 | 0.309665 | 0.129* | |
C27 | 0.2170 (10) | 0.8196 (11) | 0.2590 (4) | 0.094 (3) | |
H27A | 0.121279 | 0.770332 | 0.245063 | 0.113* | |
H27B | 0.205903 | 0.90761 | 0.278391 | 0.113* | |
C28 | 0.3118 (9) | 0.8401 (11) | 0.2142 (5) | 0.104 (4) | |
H28A | 0.258339 | 0.805669 | 0.178838 | 0.125* | |
H28B | 0.347993 | 0.938086 | 0.213421 | 0.125* | |
C29 | 0.3942 (12) | 0.6280 (9) | 0.0499 (4) | 0.097 (3) | |
H29A | 0.313456 | 0.579395 | 0.068406 | 0.116* | |
H29B | 0.468602 | 0.569649 | 0.046549 | 0.116* | |
C30 | 0.3450 (16) | 0.6546 (11) | −0.0033 (4) | 0.129 (5) | |
H30A | 0.243118 | 0.613051 | −0.010931 | 0.155* | |
H30B | 0.401758 | 0.615319 | −0.031526 | 0.155* | |
C31 | 0.3622 (11) | 0.8036 (10) | −0.0046 (3) | 0.089 (3) | |
H31A | 0.267887 | 0.833208 | −0.00809 | 0.107* | |
H31B | 0.419165 | 0.833161 | −0.035416 | 0.107* | |
C32 | 0.4391 (13) | 0.8591 (9) | 0.0489 (4) | 0.108 (4) | |
H32A | 0.535733 | 0.907845 | 0.042802 | 0.13* | |
H32B | 0.385772 | 0.923916 | 0.068191 | 0.13* | |
C33 | 0.947 (3) | 0.872 (4) | 0.1287 (10) | 0.118 (10) | 0.5 |
C34 | 1.020 (5) | 0.819 (9) | 0.094 (4) | 0.31 (4) | 0.5 |
C33A | 0.876 (5) | 0.924 (3) | 0.085 (2) | 0.184 (19) | 0.5 |
C35 | 0.963 (3) | 0.752 (3) | 0.0441 (12) | 0.111 (8) | 0.5 |
C34A | 1.037 (4) | 0.884 (5) | 0.0834 (15) | 0.20 (3) | 0.5 |
C36 | 0.849 (6) | 0.705 (3) | 0.080 (3) | 0.27 (3) | 0.5 |
C35A | 0.952 (3) | 0.862 (4) | 0.0364 (10) | 0.111 (8) | 0.5 |
C36A | 0.826 (3) | 0.782 (5) | 0.0497 (8) | 0.167 (18) | 0.5 |
U11 | U22 | U33 | U12 | U13 | U23 | |
Fe1 | 0.0406 (4) | 0.0376 (4) | 0.0362 (3) | 0.0126 (3) | −0.0065 (3) | −0.0024 (3) |
Fe2 | 0.0342 (3) | 0.0371 (3) | 0.0296 (3) | 0.0117 (3) | 0.0000 (2) | 0.0004 (2) |
Mn1 | 0.0361 (4) | 0.0339 (3) | 0.0300 (3) | 0.0113 (3) | −0.0008 (3) | 0.0019 (3) |
Na1 | 0.0336 (10) | 0.0715 (15) | 0.0541 (13) | 0.0139 (10) | 0.0075 (9) | 0.0017 (11) |
Na2 | 0.0604 (13) | 0.0418 (11) | 0.0404 (11) | 0.0134 (10) | 0.0029 (9) | 0.0065 (9) |
O1 | 0.079 (3) | 0.063 (3) | 0.055 (3) | 0.005 (2) | −0.009 (2) | 0.022 (2) |
O2 | 0.158 (6) | 0.055 (3) | 0.052 (3) | 0.028 (3) | −0.017 (3) | −0.016 (2) |
O3 | 0.037 (2) | 0.131 (5) | 0.065 (3) | 0.005 (3) | 0.016 (2) | 0.002 (3) |
O4 | 0.043 (2) | 0.074 (3) | 0.066 (3) | 0.028 (2) | −0.0087 (19) | −0.008 (2) |
O5 | 0.130 (5) | 0.041 (2) | 0.068 (3) | 0.004 (3) | −0.031 (3) | 0.016 (2) |
O6 | 0.059 (3) | 0.038 (2) | 0.073 (3) | 0.0169 (18) | −0.007 (2) | −0.0112 (19) |
O7 | 0.065 (3) | 0.119 (5) | 0.059 (3) | 0.028 (3) | 0.017 (2) | −0.003 (3) |
O8 | 0.113 (5) | 0.135 (6) | 0.103 (5) | 0.043 (4) | −0.067 (4) | −0.048 (4) |
O9 | 0.051 (2) | 0.0416 (19) | 0.048 (2) | 0.0212 (16) | −0.0018 (16) | 0.0069 (16) |
O10 | 0.049 (2) | 0.072 (3) | 0.048 (2) | 0.009 (2) | 0.0145 (18) | −0.001 (2) |
O11 | 0.100 (4) | 0.085 (4) | 0.069 (3) | 0.028 (3) | 0.029 (3) | 0.022 (3) |
O12 | 0.055 (3) | 0.127 (5) | 0.089 (4) | 0.005 (3) | 0.007 (3) | −0.042 (4) |
O13 | 0.078 (3) | 0.092 (4) | 0.088 (4) | 0.040 (3) | 0.033 (3) | 0.041 (3) |
O14 | 0.120 (5) | 0.057 (3) | 0.053 (3) | 0.022 (3) | −0.025 (3) | 0.001 (2) |
O15 | 0.110 (5) | 0.114 (5) | 0.094 (4) | 0.027 (4) | 0.057 (4) | 0.022 (4) |
C1 | 0.044 (3) | 0.046 (3) | 0.036 (2) | 0.009 (2) | −0.005 (2) | 0.002 (2) |
C2 | 0.082 (4) | 0.042 (3) | 0.039 (3) | 0.021 (3) | −0.009 (3) | −0.002 (2) |
C3 | 0.036 (3) | 0.071 (4) | 0.042 (3) | 0.016 (3) | 0.002 (2) | 0.004 (3) |
C4 | 0.030 (2) | 0.042 (3) | 0.041 (2) | 0.0052 (19) | 0.0004 (18) | −0.005 (2) |
C5 | 0.076 (4) | 0.043 (3) | 0.037 (3) | 0.020 (3) | −0.016 (3) | −0.001 (2) |
C6 | 0.046 (3) | 0.031 (2) | 0.041 (2) | 0.008 (2) | −0.004 (2) | −0.0037 (19) |
C7 | 0.049 (3) | 0.062 (4) | 0.049 (3) | 0.020 (3) | −0.003 (3) | −0.004 (3) |
C8 | 0.059 (4) | 0.063 (4) | 0.062 (4) | 0.019 (3) | −0.026 (3) | −0.016 (3) |
C9 | 0.059 (4) | 0.042 (3) | 0.079 (4) | 0.017 (3) | −0.008 (3) | 0.004 (3) |
C10 | 0.089 (6) | 0.064 (5) | 0.110 (7) | 0.029 (4) | −0.027 (5) | 0.020 (4) |
C11 | 0.139 (9) | 0.091 (7) | 0.106 (7) | 0.050 (6) | 0.031 (7) | 0.050 (6) |
C12 | 0.088 (5) | 0.086 (5) | 0.082 (5) | 0.039 (4) | 0.033 (4) | 0.045 (4) |
C13 | 0.060 (5) | 0.193 (11) | 0.061 (5) | −0.025 (6) | 0.017 (4) | −0.015 (6) |
C14 | 0.074 (5) | 0.139 (9) | 0.071 (5) | −0.008 (5) | 0.021 (4) | 0.022 (5) |
C15 | 0.091 (7) | 0.220 (14) | 0.060 (5) | −0.011 (8) | 0.015 (5) | −0.018 (7) |
C16 | 0.118 (8) | 0.143 (9) | 0.094 (7) | −0.043 (7) | 0.054 (6) | −0.069 (7) |
C17 | 0.122 (8) | 0.121 (8) | 0.083 (6) | 0.047 (7) | 0.044 (6) | 0.029 (6) |
C18 | 0.237 (16) | 0.101 (8) | 0.103 (8) | 0.056 (9) | 0.075 (10) | 0.040 (7) |
C19 | 0.34 (2) | 0.095 (9) | 0.129 (11) | 0.083 (12) | 0.087 (14) | 0.034 (8) |
C20 | 0.137 (9) | 0.084 (6) | 0.097 (7) | 0.031 (6) | 0.038 (6) | 0.005 (5) |
C21 | 0.063 (5) | 0.160 (10) | 0.105 (7) | 0.013 (6) | 0.010 (5) | −0.055 (7) |
C22 | 0.105 (8) | 0.150 (10) | 0.068 (5) | −0.015 (7) | 0.020 (5) | −0.029 (6) |
C23 | 0.103 (7) | 0.088 (6) | 0.070 (5) | 0.006 (5) | −0.018 (5) | −0.004 (4) |
C24 | 0.075 (5) | 0.089 (6) | 0.094 (6) | 0.014 (5) | −0.005 (5) | −0.013 (5) |
C25 | 0.070 (5) | 0.080 (5) | 0.083 (5) | 0.013 (4) | 0.016 (4) | 0.033 (4) |
C26 | 0.097 (7) | 0.154 (10) | 0.074 (6) | 0.013 (7) | 0.014 (5) | 0.028 (6) |
C27 | 0.073 (5) | 0.105 (7) | 0.105 (7) | 0.024 (5) | 0.019 (5) | −0.005 (6) |
C28 | 0.063 (5) | 0.123 (8) | 0.148 (9) | 0.045 (5) | 0.032 (5) | 0.065 (7) |
C29 | 0.134 (8) | 0.062 (5) | 0.083 (6) | −0.002 (5) | −0.035 (6) | 0.003 (4) |
C30 | 0.213 (14) | 0.100 (8) | 0.071 (6) | 0.042 (8) | −0.055 (7) | −0.016 (5) |
C31 | 0.106 (7) | 0.100 (7) | 0.061 (5) | 0.019 (5) | −0.008 (4) | 0.018 (4) |
C32 | 0.159 (10) | 0.060 (5) | 0.099 (7) | 0.020 (5) | −0.056 (7) | 0.003 (5) |
C33 | 0.078 (14) | 0.18 (3) | 0.082 (14) | −0.008 (16) | 0.030 (11) | −0.031 (15) |
C34 | 0.14 (4) | 0.46 (11) | 0.38 (10) | 0.15 (6) | −0.09 (5) | 0.12 (9) |
C33A | 0.22 (4) | 0.074 (15) | 0.28 (5) | 0.04 (2) | 0.17 (4) | 0.03 (2) |
C35 | 0.084 (15) | 0.14 (2) | 0.104 (17) | 0.014 (15) | 0.041 (13) | −0.031 (16) |
C34A | 0.14 (3) | 0.28 (5) | 0.12 (2) | −0.12 (3) | 0.08 (2) | −0.08 (3) |
C36 | 0.30 (5) | 0.077 (16) | 0.47 (7) | 0.04 (2) | 0.32 (6) | 0.02 (3) |
C35A | 0.13 (2) | 0.14 (2) | 0.070 (13) | 0.006 (18) | 0.040 (13) | 0.036 (15) |
C36A | 0.092 (17) | 0.34 (5) | 0.049 (10) | −0.03 (3) | −0.002 (10) | 0.017 (19) |
Fe1—C6 | 1.743 (5) | O15—C36 | 1.31 (3) |
Fe1—C5 | 1.744 (6) | O15—C33A | 1.36 (3) |
Fe1—C8 | 1.750 (6) | O15—C36A | 1.41 (2) |
Fe1—C7 | 1.752 (6) | O15—C33 | 1.42 (3) |
Fe1—Mn1 | 2.6294 (10) | C9—C10 | 1.483 (10) |
Fe2—C3 | 1.733 (6) | C10—C11 | 1.488 (13) |
Fe2—C4 | 1.739 (5) | C11—C12 | 1.470 (10) |
Fe2—C1 | 1.749 (5) | C13—C14 | 1.454 (11) |
Fe2—C2 | 1.750 (6) | C14—C15 | 1.440 (13) |
Fe2—Mn1 | 2.6274 (10) | C15—C16 | 1.445 (13) |
Mn1—O9 | 2.180 (4) | C17—C18 | 1.454 (14) |
Mn1—O10 | 2.205 (4) | C18—C19 | 1.405 (15) |
Na1—O11 | 2.283 (6) | C19—C20 | 1.402 (14) |
Na1—O3 | 2.285 (5) | C21—C22 | 1.416 (12) |
Na1—O4i | 2.303 (4) | C22—C23 | 1.479 (13) |
Na1—O12 | 2.321 (6) | C23—C24 | 1.512 (12) |
Na1—O7 | 2.355 (5) | C25—C26 | 1.477 (13) |
Na2—O15 | 2.305 (6) | C26—C27 | 1.512 (13) |
Na2—O13 | 2.341 (5) | C27—C28 | 1.446 (12) |
Na2—O14 | 2.362 (5) | C29—C30 | 1.418 (12) |
Na2—O5 | 2.401 (5) | C30—C31 | 1.468 (13) |
Na2—O1 | 2.452 (5) | C31—C32 | 1.474 (11) |
Na2—O6ii | 2.462 (4) | C33—C34 | 1.25 (8) |
O1—C1 | 1.173 (6) | C33—C33A | 1.41 (5) |
O2—C2 | 1.145 (7) | C33—C34A | 1.42 (3) |
O3—C3 | 1.168 (7) | C33—C36 | 2.01 (6) |
O4—C4 | 1.176 (6) | C34—C34A | 0.71 (9) |
O5—C5 | 1.172 (7) | C34—C35 | 1.36 (8) |
O6—C6 | 1.173 (6) | C34—C35A | 1.62 (6) |
O7—C7 | 1.173 (7) | C34—C36 | 1.80 (8) |
O8—C8 | 1.147 (7) | C34—C33A | 1.85 (6) |
O9—C12 | 1.421 (8) | C34—C36A | 2.03 (5) |
O9—C9 | 1.438 (7) | C33A—C35A | 1.54 (4) |
O10—C13 | 1.400 (9) | C33A—C36A | 1.58 (5) |
O10—C16 | 1.412 (9) | C33A—C34A | 1.62 (6) |
O11—C17 | 1.405 (9) | C35—C35A | 1.14 (3) |
O11—C20 | 1.411 (10) | C35—C36A | 1.37 (4) |
O12—C24 | 1.383 (10) | C35—C36 | 1.46 (4) |
O12—C21 | 1.400 (10) | C35—C34A | 1.59 (4) |
O13—C28 | 1.398 (9) | C34A—C35A | 1.34 (5) |
O13—C25 | 1.415 (8) | C36—C36A | 1.15 (6) |
O14—C29 | 1.386 (9) | C35A—C36A | 1.38 (4) |
O14—C32 | 1.407 (9) | ||
C6—Fe1—C5 | 122.8 (3) | O13—C25—C26 | 105.7 (7) |
C6—Fe1—C8 | 98.7 (3) | C25—C26—C27 | 103.9 (7) |
C5—Fe1—C8 | 98.5 (3) | C28—C27—C26 | 105.3 (7) |
C6—Fe1—C7 | 113.2 (3) | O13—C28—C27 | 109.0 (8) |
C5—Fe1—C7 | 114.0 (3) | O14—C29—C30 | 109.8 (8) |
C8—Fe1—C7 | 104.9 (3) | C29—C30—C31 | 108.0 (8) |
C6—Fe1—Mn1 | 78.41 (16) | C30—C31—C32 | 104.0 (7) |
C5—Fe1—Mn1 | 72.21 (18) | O14—C32—C31 | 109.0 (7) |
C8—Fe1—Mn1 | 165.8 (3) | C34—C33—C33A | 88 (3) |
C7—Fe1—Mn1 | 88.9 (2) | C34—C33—O15 | 99 (3) |
C3—Fe2—C4 | 116.5 (3) | C33A—C33—O15 | 57.5 (18) |
C3—Fe2—C1 | 114.4 (3) | C34—C33—C34A | 30 (4) |
C4—Fe2—C1 | 118.3 (2) | C33A—C33—C34A | 70 (3) |
C3—Fe2—C2 | 102.2 (3) | O15—C33—C34A | 106 (2) |
C4—Fe2—C2 | 99.4 (3) | C34—C33—C36 | 62 (4) |
C1—Fe2—C2 | 101.7 (3) | C33A—C33—C36 | 75 (2) |
C3—Fe2—Mn1 | 77.0 (2) | O15—C33—C36 | 40.4 (15) |
C4—Fe2—Mn1 | 79.23 (16) | C34A—C33—C36 | 81.2 (19) |
C1—Fe2—Mn1 | 80.45 (17) | C34A—C34—C33 | 88 (9) |
C2—Fe2—Mn1 | 177.86 (19) | C34A—C34—C35 | 95 (8) |
O9—Mn1—O10 | 92.17 (16) | C33—C34—C35 | 124 (3) |
O9—Mn1—Fe2 | 103.15 (11) | C34A—C34—C35A | 54 (6) |
O10—Mn1—Fe2 | 106.01 (12) | C33—C34—C35A | 102 (3) |
O9—Mn1—Fe1 | 104.77 (11) | C35—C34—C35A | 44 (2) |
O10—Mn1—Fe1 | 105.15 (12) | C34A—C34—C36 | 125 (6) |
Fe2—Mn1—Fe1 | 136.81 (3) | C33—C34—C36 | 80 (4) |
O11—Na1—O3 | 101.2 (2) | C35—C34—C36 | 53 (3) |
O11—Na1—O4i | 102.2 (2) | C35A—C34—C36 | 75 (3) |
O3—Na1—O4i | 156.5 (2) | C34A—C34—C33A | 60 (5) |
O11—Na1—O12 | 97.5 (3) | C33—C34—C33A | 50 (2) |
O3—Na1—O12 | 87.6 (2) | C35—C34—C33A | 84 (3) |
O4i—Na1—O12 | 91.3 (2) | C35A—C34—C33A | 52 (2) |
O11—Na1—O7 | 96.9 (2) | C36—C34—C33A | 72 (2) |
O3—Na1—O7 | 80.4 (2) | C34A—C34—C36A | 91 (6) |
O4i—Na1—O7 | 94.89 (19) | C33—C34—C36A | 82 (2) |
O12—Na1—O7 | 162.8 (3) | C35—C34—C36A | 42.3 (17) |
O15—Na2—O13 | 170.2 (3) | C35A—C34—C36A | 42.7 (17) |
O15—Na2—O14 | 90.4 (3) | C36—C34—C36A | 34 (2) |
O13—Na2—O14 | 94.0 (2) | C33A—C34—C36A | 47.7 (19) |
O15—Na2—O5 | 92.4 (3) | O15—C33A—C33 | 61.4 (19) |
O13—Na2—O5 | 96.5 (2) | O15—C33A—C35A | 103 (2) |
O14—Na2—O5 | 86.82 (18) | C33—C33A—C35A | 99 (2) |
O15—Na2—O1 | 86.8 (2) | O15—C33A—C36A | 56.7 (15) |
O13—Na2—O1 | 91.5 (2) | C33—C33A—C36A | 96 (2) |
O14—Na2—O1 | 162.5 (2) | C35A—C33A—C36A | 52.6 (19) |
O5—Na2—O1 | 76.04 (17) | O15—C33A—C34A | 99 (3) |
O15—Na2—O6ii | 85.7 (2) | C33—C33A—C34A | 55 (3) |
O13—Na2—O6ii | 85.38 (19) | C35A—C33A—C34A | 50.1 (17) |
O14—Na2—O6ii | 91.60 (17) | C36A—C33A—C34A | 85 (2) |
O5—Na2—O6ii | 177.6 (2) | O15—C33A—C34 | 77 (3) |
O1—Na2—O6ii | 105.41 (17) | C33—C33A—C34 | 43 (3) |
C1—O1—Na2 | 140.3 (4) | C35A—C33A—C34 | 56 (3) |
C3—O3—Na1 | 158.0 (5) | C36A—C33A—C34 | 72 (3) |
C4—O4—Na1iii | 155.7 (4) | C34A—C33A—C34 | 22 (3) |
C5—O5—Na2 | 146.8 (5) | C35A—C35—C34 | 80 (4) |
C6—O6—Na2iv | 151.9 (4) | C35A—C35—C36A | 66 (3) |
C7—O7—Na1 | 143.9 (5) | C34—C35—C36A | 96 (3) |
C12—O9—C9 | 109.7 (5) | C35A—C35—C36 | 107 (2) |
C12—O9—Mn1 | 118.7 (4) | C34—C35—C36 | 79 (4) |
C9—O9—Mn1 | 131.6 (4) | C36A—C35—C36 | 48 (2) |
C13—O10—C16 | 106.6 (6) | C35A—C35—C34A | 56 (3) |
C13—O10—Mn1 | 126.2 (4) | C34—C35—C34A | 26 (4) |
C16—O10—Mn1 | 126.2 (5) | C36A—C35—C34A | 93 (3) |
C17—O11—C20 | 107.7 (7) | C36—C35—C34A | 97 (3) |
C17—O11—Na1 | 130.8 (6) | C34—C34A—C35A | 100 (7) |
C20—O11—Na1 | 121.4 (5) | C34—C34A—C33 | 62 (7) |
C24—O12—C21 | 109.6 (7) | C35A—C34A—C33 | 109 (3) |
C24—O12—Na1 | 127.9 (5) | C34—C34A—C35 | 59 (8) |
C21—O12—Na1 | 122.3 (5) | C35A—C34A—C35 | 45.0 (17) |
C28—O13—C25 | 109.1 (6) | C33—C34A—C35 | 100 (2) |
C28—O13—Na2 | 122.1 (5) | C34—C34A—C33A | 98 (6) |
C25—O13—Na2 | 127.1 (4) | C35A—C34A—C33A | 62 (3) |
C29—O14—C32 | 108.7 (6) | C33—C34A—C33A | 55 (2) |
C29—O14—Na2 | 125.1 (5) | C35—C34A—C33A | 86 (3) |
C32—O14—Na2 | 123.0 (5) | C36A—C36—O15 | 70 (2) |
C36—O15—C33A | 106.7 (18) | C36A—C36—C35 | 62 (3) |
C36—O15—C36A | 50 (3) | O15—C36—C35 | 109 (2) |
C33A—O15—C36A | 69 (2) | C36A—C36—C34 | 84 (3) |
C36—O15—C33 | 95 (3) | O15—C36—C34 | 80 (4) |
C33A—O15—C33 | 61 (2) | C35—C36—C34 | 48 (3) |
C36A—O15—C33 | 103.9 (14) | C36A—C36—C33 | 85 (3) |
C36—O15—Na2 | 118.1 (13) | O15—C36—C33 | 44.7 (19) |
C33A—O15—Na2 | 133.7 (12) | C35—C36—C33 | 82 (2) |
C36A—O15—Na2 | 133.8 (12) | C34—C36—C33 | 38 (3) |
C33—O15—Na2 | 122.2 (10) | C35—C35A—C34A | 79 (3) |
O1—C1—Fe2 | 175.2 (5) | C35—C35A—C36A | 65 (3) |
O2—C2—Fe2 | 178.9 (6) | C34A—C35A—C36A | 104.7 (19) |
O3—C3—Fe2 | 175.4 (6) | C35—C35A—C33A | 108 (2) |
O4—C4—Fe2 | 175.3 (5) | C34A—C35A—C33A | 68 (3) |
O5—C5—Fe1 | 175.1 (5) | C36A—C35A—C33A | 65 (2) |
O6—C6—Fe1 | 175.2 (5) | C35—C35A—C34 | 56 (3) |
O7—C7—Fe1 | 176.7 (6) | C34A—C35A—C34 | 25 (4) |
O8—C8—Fe1 | 178.7 (9) | C36A—C35A—C34 | 84 (3) |
O9—C9—C10 | 104.7 (6) | C33A—C35A—C34 | 72 (3) |
C9—C10—C11 | 104.1 (6) | C36—C36A—C35 | 70 (3) |
C12—C11—C10 | 105.0 (7) | C36—C36A—C35A | 112 (4) |
O9—C12—C11 | 107.2 (7) | C35—C36A—C35A | 49.1 (16) |
O10—C13—C14 | 109.5 (7) | C36—C36A—O15 | 60.5 (19) |
C15—C14—C13 | 106.0 (8) | C35—C36A—O15 | 109 (2) |
C14—C15—C16 | 106.5 (8) | C35A—C36A—O15 | 109 (3) |
O10—C16—C15 | 108.8 (7) | C36—C36A—C33A | 102 (4) |
O11—C17—C18 | 108.0 (8) | C35—C36A—C33A | 96 (2) |
C19—C18—C17 | 105.9 (9) | C35A—C36A—C33A | 62 (2) |
C20—C19—C18 | 109.5 (10) | O15—C36A—C33A | 53.9 (17) |
C19—C20—O11 | 108.3 (9) | C36—C36A—C34 | 62 (3) |
O12—C21—C22 | 109.8 (8) | C35—C36A—C34 | 42 (3) |
C21—C22—C23 | 106.8 (8) | C35A—C36A—C34 | 53 (3) |
C22—C23—C24 | 104.5 (7) | O15—C36A—C34 | 70 (3) |
O12—C24—C23 | 107.7 (7) | C33A—C36A—C34 | 60 (3) |
Symmetry codes: (i) x−1, y, z; (ii) x, y+1, z; (iii) x+1, y, z; (iv) x, y−1, z. |
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