The systematic twinning of three 2,6-diaminopyridine-based Fe-PNP complexes is interpreted using order–disorder (OD) theory. The monoclinic [Fe
0(PNP
Et-
iPr)(CO)
2] [
P112
1/
b,
Z′ = 4] possesses pseudo-orthorhombic metrics and crystallizes as a reflection twin by pseudo-merohedry with the twin plane (100). The structure is made up of layers with idealized
p2
1a(
b) symmetry. The
a glide planes of adjacent layers do not overlap, leading to OD polytypism.
trans-[Fe
II(PNP-Et)Br
2(CO)] [
P2
1/
n,
Z′ = 1] is systematically twinned
via twofold rotation about [001]. It is made up of OD layers with idealized
p2
12
1(2) symmetry. OD polytypism is caused by the twofold rotation axes of adjacent layers which do not overlap. [Fe
II(κ
2P,
N-PNP-
iPr,TAD)Cl
2]·THF [
P1,
] is systematically twinned
via a twofold rotation about [010]. It is made up of layers with idealized
p12
1(1) symmetry. OD polytypism is caused by screw rotations relating adjacent layers with an intrinsic translation along a fourth of a primitive lattice vector. In all three structures the twin individuals are a polytype with a maximum degree of order (MDO) and at the twin interface is located a fragment of the second MDO polytype.
Supporting information
CCDC references: 1418467; 1418468; 1418469
Data collection: APEX 2 (Bruker, 2014) for Fe_PNP-Et_Br2_CO, Fe_PNP-TADDOL-iPr_Cl2. Cell refinement: SAINT (Bruker, 2014) for Fe_PNP-Et_Br2_CO, Fe_PNP-TADDOL-iPr_Cl2. Data reduction: SAINT (Bruker, 2014) for Fe_PNP-Et_Br2_CO, Fe_PNP-TADDOL-iPr_Cl2. Program(s) used to solve structure: SUPERFLIP (Palatinus & Chapuis, 2007) for Fe_PNP-Et_Br2_CO, Fe_PNP-TADDOL-iPr_Cl2. Program(s) used to refine structure: JANA20006 (Petříček, M. Dušek & L. Palatinus, 2014) for Fe_PNP-Et_Br2_CO, Fe_PNP-TADDOL-iPr_Cl2.
Crystal data top
C23H41FeN3O2P2 | F(000) = 4352 |
Mr = 509.4 | Dx = 1.295 Mg m−3 |
Monoclinic, P1121/b | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2zbc | Cell parameters from 9703 reflections |
a = 31.781 (3) Å | θ = 2.4–30.0° |
b = 18.012 (5) Å | µ = 0.72 mm−1 |
c = 18.262 (3) Å | T = 100 K |
β = 90° | Block, dark red |
V = 10454 (3) Å3 | 0.80 × 0.75 × 0.55 mm |
Z = 16 | |
Data collection top
Bruker KAPPA APEX II CCD diffractometer | 30818 independent reflections |
Radiation source: X-ray tube | 25454 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.051 |
ω– and φ–scans | θmax = 30.2°, θmin = 0.6° |
Absorption correction: multi-scan SADABS | h = −44→44 |
Tmin = 0.57, Tmax = 0.67 | k = −25→25 |
450669 measured reflections | l = −25→25 |
Refinement top
Refinement on F | 1017 constraints |
R[F2 > 2σ(F2)] = 0.063 | H-atom parameters constrained |
wR(F2) = 0.079 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
S = 3.87 | (Δ/σ)max = 0.031 |
30818 reflections | Δρmax = 2.07 e Å−3 |
815 parameters | Δρmin = −0.87 e Å−3 |
0 restraints | |
Crystal data top
C23H41FeN3O2P2 | V = 10454 (3) Å3 |
Mr = 509.4 | Z = 16 |
Monoclinic, P1121/b | Mo Kα radiation |
a = 31.781 (3) Å | µ = 0.72 mm−1 |
b = 18.012 (5) Å | T = 100 K |
c = 18.262 (3) Å | 0.80 × 0.75 × 0.55 mm |
β = 90° | |
Data collection top
Bruker KAPPA APEX II CCD diffractometer | 30818 independent reflections |
Absorption correction: multi-scan SADABS | 25454 reflections with I > 3σ(I) |
Tmin = 0.57, Tmax = 0.67 | Rint = 0.051 |
450669 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.063 | 0 restraints |
wR(F2) = 0.079 | H-atom parameters constrained |
S = 3.87 | Δρmax = 2.07 e Å−3 |
30818 reflections | Δρmin = −0.87 e Å−3 |
815 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Fe1 | 0.63784 (3) | 0.67589 (5) | −0.74296 (3) | 0.0166 (2) | |
P1 | 0.58272 (5) | 0.60210 (10) | −0.74442 (6) | 0.0187 (4) | |
P2 | 0.70338 (5) | 0.71444 (10) | −0.74529 (5) | 0.0161 (4) | |
O1 | 0.60617 (13) | 0.7750 (3) | −0.63415 (19) | 0.0675 (18) | |
O2 | 0.61918 (10) | 0.7285 (2) | −0.8828 (2) | 0.0444 (12) | |
N2 | 0.59862 (10) | 0.53019 (19) | −0.68778 (18) | 0.0193 (5) | |
N1 | 0.66433 (10) | 0.58654 (18) | −0.69107 (17) | 0.0167 (5) | |
N3 | 0.72946 (10) | 0.64589 (18) | −0.69873 (17) | 0.0186 (5) | |
C1 | 0.63985 (12) | 0.5292 (2) | −0.6663 (2) | 0.0163 (6) | |
C2 | 0.65581 (13) | 0.4756 (2) | −0.6200 (2) | 0.0211 (7) | |
C3 | 0.69801 (13) | 0.4789 (2) | −0.5984 (2) | 0.0210 (7) | |
C4 | 0.72356 (13) | 0.5343 (2) | −0.6244 (2) | 0.0205 (6) | |
C5 | 0.70572 (12) | 0.5884 (2) | −0.67018 (19) | 0.0152 (6) | |
C6 | 0.57153 (12) | 0.4666 (2) | −0.6708 (2) | 0.0211 (7) | |
C7 | 0.58217 (14) | 0.3944 (2) | −0.7130 (3) | 0.0292 (8) | |
C8 | 0.77533 (12) | 0.6480 (2) | −0.6861 (2) | 0.0254 (7) | |
C9 | 0.79942 (16) | 0.5945 (3) | −0.7362 (3) | 0.0312 (8) | |
C10 | 0.53142 (13) | 0.6307 (3) | −0.6226 (2) | 0.0249 (7) | |
C11 | 0.53103 (12) | 0.6304 (2) | −0.7043 (2) | 0.0204 (6) | |
C12 | 0.51882 (17) | 0.7085 (3) | −0.7372 (2) | 0.0265 (7) | |
C13 | 0.60371 (15) | 0.5215 (3) | −0.8653 (3) | 0.0375 (9) | |
C14 | 0.56576 (14) | 0.5507 (3) | −0.8252 (2) | 0.0289 (8) | |
C15 | 0.53528 (16) | 0.6012 (3) | −0.8770 (2) | 0.0394 (11) | |
C16 | 0.71978 (15) | 0.7860 (3) | −0.6111 (3) | 0.0268 (8) | |
C17 | 0.72087 (14) | 0.7999 (2) | −0.6949 (2) | 0.0258 (7) | |
C18 | 0.69358 (16) | 0.8684 (3) | −0.7161 (3) | 0.0340 (9) | |
C19 | 0.72534 (15) | 0.6483 (3) | −0.8757 (2) | 0.0344 (9) | |
C20 | 0.73332 (13) | 0.7196 (2) | −0.8314 (2) | 0.0259 (7) | |
C21 | 0.72384 (16) | 0.7883 (3) | −0.8780 (3) | 0.0311 (8) | |
C22 | 0.61914 (13) | 0.7353 (3) | −0.6708 (3) | 0.0258 (8) | |
C23 | 0.62760 (15) | 0.7061 (3) | −0.8289 (3) | 0.0305 (8) | |
Fe2 | 0.40299 (3) | 0.85264 (5) | −0.75093 (3) | 0.0130 (2) | |
P3 | 0.39556 (4) | 0.83737 (7) | −0.63337 (7) | 0.0159 (3) | |
P4 | 0.40285 (4) | 0.83730 (7) | −0.86930 (7) | 0.0156 (3) | |
O3 | 0.48504 (15) | 0.9239 (3) | −0.74327 (15) | 0.0298 (12) | |
O4 | 0.33607 (13) | 0.9601 (3) | −0.75961 (17) | 0.0255 (12) | |
N5 | 0.39999 (12) | 0.7411 (2) | −0.62381 (19) | 0.0124 (6) | |
N4 | 0.40365 (16) | 0.7366 (2) | −0.75086 (13) | 0.0082 (4) | |
N6 | 0.40653 (14) | 0.7413 (2) | −0.87854 (19) | 0.0161 (6) | |
C24 | 0.40474 (13) | 0.7012 (2) | −0.6869 (2) | 0.0108 (6) | |
C25 | 0.41223 (14) | 0.6241 (2) | −0.6842 (3) | 0.0162 (6) | |
C26 | 0.41671 (17) | 0.5877 (3) | −0.75015 (18) | 0.0168 (5) | |
C27 | 0.41598 (14) | 0.6240 (3) | −0.8158 (3) | 0.0164 (6) | |
C28 | 0.40856 (15) | 0.7012 (3) | −0.8146 (2) | 0.0141 (6) | |
C29 | 0.39823 (15) | 0.7041 (2) | −0.5522 (2) | 0.0222 (9) | |
C30 | 0.35750 (15) | 0.6619 (3) | −0.5399 (2) | 0.0291 (10) | |
C31 | 0.41028 (17) | 0.7031 (3) | −0.9497 (2) | 0.0254 (8) | |
C32 | 0.37076 (18) | 0.6578 (3) | −0.9697 (3) | 0.0380 (10) | |
C33 | 0.47683 (15) | 0.8340 (3) | −0.5704 (3) | 0.0291 (10) | |
C34 | 0.43430 (13) | 0.8738 (2) | −0.5652 (2) | 0.0163 (8) | |
C35 | 0.44242 (18) | 0.9588 (3) | −0.5783 (3) | 0.0319 (10) | |
C36 | 0.30817 (13) | 0.8176 (3) | −0.6280 (2) | 0.0247 (9) | |
C37 | 0.34587 (15) | 0.8557 (3) | −0.5845 (3) | 0.0270 (9) | |
C38 | 0.33621 (16) | 0.9339 (3) | −0.5665 (3) | 0.0345 (10) | |
C39 | 0.48833 (15) | 0.8318 (3) | −0.9099 (2) | 0.0285 (10) | |
C40 | 0.44627 (16) | 0.8714 (2) | −0.9289 (3) | 0.0249 (9) | |
C41 | 0.45098 (16) | 0.9563 (3) | −0.9225 (3) | 0.0286 (10) | |
C42 | 0.31657 (16) | 0.8236 (3) | −0.8940 (3) | 0.0310 (10) | |
C43 | 0.35658 (13) | 0.8646 (3) | −0.9237 (2) | 0.0208 (9) | |
C44 | 0.3574 (2) | 0.8641 (4) | −1.0053 (3) | 0.0304 (15) | 0.612 (8) |
C45 | 0.45452 (18) | 0.8911 (3) | −0.74581 (17) | 0.0152 (5) | |
C46 | 0.36151 (18) | 0.9139 (3) | −0.75581 (17) | 0.0167 (5) | |
Fe1' | 0.13653 (2) | 0.57466 (5) | −0.75718 (3) | 0.01143 (18) | |
P1' | 0.08235 (4) | 0.64890 (9) | −0.75710 (5) | 0.0123 (3) | |
P2' | 0.20182 (5) | 0.53597 (9) | −0.75088 (5) | 0.0127 (4) | |
O1' | 0.10547 (9) | 0.46876 (16) | −0.86357 (15) | 0.0220 (8) | |
O2' | 0.11817 (8) | 0.53077 (15) | −0.61313 (15) | 0.0196 (8) | |
N2' | 0.09887 (10) | 0.72002 (19) | −0.81423 (18) | 0.0193 (5) | |
N1' | 0.16418 (10) | 0.66213 (18) | −0.81046 (17) | 0.0167 (5) | |
N3' | 0.22884 (10) | 0.60492 (18) | −0.79744 (18) | 0.0186 (5) | |
C1' | 0.14000 (12) | 0.7184 (2) | −0.8381 (2) | 0.0163 (6) | |
C2' | 0.15625 (13) | 0.7705 (2) | −0.8871 (2) | 0.0211 (7) | |
C3' | 0.19822 (13) | 0.7675 (2) | −0.9056 (2) | 0.0210 (7) | |
C4' | 0.22399 (13) | 0.7131 (2) | −0.8764 (2) | 0.0205 (6) | |
C5' | 0.20593 (12) | 0.6612 (2) | −0.82771 (19) | 0.0152 (6) | |
C6' | 0.07181 (12) | 0.7826 (2) | −0.8345 (2) | 0.0211 (7) | |
C7' | 0.08288 (13) | 0.8560 (2) | −0.7978 (3) | 0.0292 (8) | |
C8' | 0.27467 (12) | 0.6007 (2) | −0.8101 (2) | 0.0254 (7) | |
C9' | 0.29949 (16) | 0.6582 (3) | −0.7651 (3) | 0.0312 (8) | |
C10' | 0.03011 (13) | 0.6135 (2) | −0.8777 (2) | 0.0249 (7) | |
C11' | 0.03056 (12) | 0.6184 (2) | −0.7934 (2) | 0.0204 (6) | |
C12' | 0.01946 (17) | 0.5437 (3) | −0.7608 (2) | 0.0265 (7) | |
C13' | 0.10590 (15) | 0.7340 (3) | −0.6362 (3) | 0.0375 (9) | |
C14' | 0.06623 (14) | 0.7041 (3) | −0.6754 (2) | 0.0289 (8) | |
C15' | 0.03704 (16) | 0.6649 (3) | −0.6244 (2) | 0.0394 (11) | |
C16' | 0.21907 (16) | 0.4603 (3) | −0.8797 (3) | 0.0268 (8) | |
C17' | 0.22045 (14) | 0.4505 (2) | −0.7975 (2) | 0.0258 (7) | |
C18' | 0.19452 (17) | 0.3820 (3) | −0.7765 (3) | 0.0340 (9) | |
C19' | 0.22406 (15) | 0.6074 (3) | −0.6203 (2) | 0.0344 (9) | |
C20' | 0.23238 (13) | 0.5366 (2) | −0.6634 (2) | 0.0259 (7) | |
C21' | 0.22305 (17) | 0.4663 (3) | −0.6168 (3) | 0.0311 (8) | |
C22' | 0.11822 (13) | 0.5105 (2) | −0.8283 (3) | 0.0258 (8) | |
C23' | 0.12654 (14) | 0.5510 (3) | −0.6684 (3) | 0.0305 (8) | |
Fe2' | 0.09628 (3) | 0.60400 (5) | −0.24902 (2) | 0.00633 (17) | |
P3' | 0.09671 (4) | 0.59188 (6) | −0.36724 (5) | 0.0087 (3) | |
P4' | 0.10368 (4) | 0.58667 (6) | −0.13199 (6) | 0.0134 (3) | |
O3' | 0.01502 (11) | 0.6781 (3) | −0.23942 (16) | 0.0221 (10) | |
O4' | 0.16590 (14) | 0.7088 (3) | −0.25106 (13) | 0.0234 (11) | |
N5' | 0.09182 (12) | 0.49841 (19) | −0.37741 (18) | 0.0124 (6) | |
N4' | 0.09431 (16) | 0.4947 (2) | −0.25061 (13) | 0.0082 (4) | |
N6' | 0.09893 (14) | 0.4933 (2) | −0.12345 (19) | 0.0161 (6) | |
C24' | 0.08932 (13) | 0.4544 (2) | −0.3153 (2) | 0.0108 (6) | |
C25' | 0.08322 (14) | 0.3787 (2) | −0.3184 (3) | 0.0162 (6) | |
C26' | 0.08110 (17) | 0.3383 (3) | −0.25317 (18) | 0.0168 (5) | |
C27' | 0.08748 (14) | 0.3756 (2) | −0.1878 (3) | 0.0164 (6) | |
C28' | 0.09343 (14) | 0.4516 (3) | −0.1877 (2) | 0.0141 (6) | |
C29' | 0.08868 (15) | 0.4621 (2) | −0.4498 (2) | 0.0222 (9) | |
C30' | 0.12700 (15) | 0.4185 (3) | −0.4739 (2) | 0.0291 (10) | |
C31' | 0.09773 (17) | 0.4530 (3) | −0.0531 (2) | 0.0254 (8) | |
C32' | 0.13649 (18) | 0.4068 (3) | −0.0341 (3) | 0.0380 (10) | |
C33' | 0.01306 (15) | 0.5867 (3) | −0.4144 (3) | 0.0291 (10) | |
C34' | 0.05336 (13) | 0.6279 (2) | −0.4252 (2) | 0.0163 (8) | |
C35' | 0.04671 (17) | 0.7120 (3) | −0.4148 (2) | 0.0319 (10) | |
C36' | 0.18214 (13) | 0.5746 (3) | −0.3898 (3) | 0.0247 (9) | |
C37' | 0.14507 (15) | 0.6101 (3) | −0.4228 (3) | 0.0270 (9) | |
C38' | 0.15293 (16) | 0.6940 (3) | −0.4384 (3) | 0.0345 (10) | |
C39' | 0.02239 (16) | 0.5884 (3) | −0.0732 (3) | 0.0285 (10) | |
C40' | 0.06487 (16) | 0.6226 (3) | −0.0651 (2) | 0.0249 (9) | |
C41' | 0.06432 (15) | 0.7067 (2) | −0.0675 (2) | 0.0286 (10) | |
C42' | 0.18945 (16) | 0.5667 (3) | −0.1292 (2) | 0.0310 (10) | |
C43' | 0.15586 (13) | 0.6072 (3) | −0.0901 (2) | 0.0208 (9) | |
C44' | 0.16071 (19) | 0.6059 (3) | −0.0089 (3) | 0.0304 (15) | 0.747 (8) |
C45' | 0.04628 (18) | 0.6444 (3) | −0.24267 (17) | 0.0152 (5) | |
C46' | 0.13877 (18) | 0.6651 (3) | −0.25066 (17) | 0.0167 (5) | |
H21 | 0.638055 | 0.436178 | −0.602696 | 0.0253* | |
H31 | 0.709096 | 0.442362 | −0.565366 | 0.0252* | |
H41 | 0.752854 | 0.536064 | −0.611701 | 0.0247* | |
H61 | 0.542683 | 0.47968 | −0.679426 | 0.0253* | |
H62 | 0.572302 | 0.456999 | −0.619086 | 0.0253* | |
H71 | 0.5639 | 0.355175 | −0.696913 | 0.035* | |
H72 | 0.578305 | 0.402412 | −0.764516 | 0.035* | |
H73 | 0.610882 | 0.380795 | −0.703688 | 0.035* | |
H81 | 0.781131 | 0.636093 | −0.635863 | 0.0305* | |
H82 | 0.785462 | 0.697661 | −0.69353 | 0.0305* | |
H91 | 0.82882 | 0.595942 | −0.724206 | 0.0374* | |
H92 | 0.788929 | 0.545012 | −0.729395 | 0.0374* | |
H93 | 0.795588 | 0.60911 | −0.786299 | 0.0374* | |
H101 | 0.539806 | 0.582646 | −0.605099 | 0.0299* | |
H102 | 0.550946 | 0.667433 | −0.605523 | 0.0299* | |
H103 | 0.503762 | 0.64206 | −0.604756 | 0.0299* | |
H111 | 0.510011 | 0.594432 | −0.71722 | 0.0245* | |
H121 | 0.526796 | 0.710348 | −0.787857 | 0.0318* | |
H122 | 0.488992 | 0.715728 | −0.73297 | 0.0318* | |
H123 | 0.533247 | 0.746893 | −0.710761 | 0.0318* | |
H131 | 0.628105 | 0.526171 | −0.834636 | 0.045* | |
H132 | 0.599388 | 0.470248 | −0.877409 | 0.045* | |
H133 | 0.607825 | 0.549637 | −0.909386 | 0.045* | |
H141 | 0.549115 | 0.508833 | −0.810393 | 0.0346* | |
H151 | 0.516519 | 0.629654 | −0.846876 | 0.0472* | |
H152 | 0.552162 | 0.634204 | −0.906048 | 0.0472* | |
H153 | 0.519216 | 0.569482 | −0.908722 | 0.0472* | |
H161 | 0.738395 | 0.745783 | −0.599059 | 0.0322* | |
H162 | 0.728617 | 0.830025 | −0.585805 | 0.0322* | |
H163 | 0.691646 | 0.773419 | −0.596427 | 0.0322* | |
H171 | 0.749319 | 0.81079 | −0.708994 | 0.0309* | |
H181 | 0.692254 | 0.872539 | −0.768472 | 0.0408* | |
H182 | 0.665683 | 0.862325 | −0.696853 | 0.0408* | |
H183 | 0.705965 | 0.912557 | −0.696071 | 0.0408* | |
H191 | 0.718336 | 0.608532 | −0.842904 | 0.0413* | |
H192 | 0.702464 | 0.656326 | −0.909114 | 0.0413* | |
H193 | 0.750229 | 0.635593 | −0.902706 | 0.0413* | |
H201 | 0.762467 | 0.724117 | −0.81838 | 0.031* | |
H211 | 0.727131 | 0.832118 | −0.848608 | 0.0374* | |
H212 | 0.742974 | 0.790184 | −0.918594 | 0.0374* | |
H213 | 0.69548 | 0.785617 | −0.895851 | 0.0374* | |
H251 | 0.414119 | 0.598109 | −0.638439 | 0.0194* | |
H261 | 0.420496 | 0.534835 | −0.749921 | 0.0201* | |
H271 | 0.420349 | 0.597989 | −0.861057 | 0.0197* | |
H291 | 0.421609 | 0.670654 | −0.54752 | 0.0266* | |
H292 | 0.401799 | 0.740234 | −0.514041 | 0.0266* | |
H301 | 0.359826 | 0.632483 | −0.49623 | 0.035* | |
H302 | 0.334719 | 0.69648 | −0.534642 | 0.035* | |
H303 | 0.352201 | 0.630045 | −0.581007 | 0.035* | |
H311 | 0.434334 | 0.670836 | −0.948893 | 0.0305* | |
H313 | 0.415799 | 0.738837 | −0.987447 | 0.0305* | |
H321 | 0.377847 | 0.621532 | −1.00618 | 0.0456* | |
H322 | 0.360258 | 0.633245 | −0.926816 | 0.0456* | |
H323 | 0.349546 | 0.690567 | −0.988662 | 0.0456* | |
H331 | 0.474502 | 0.785354 | −0.549332 | 0.0349* | |
H332 | 0.484915 | 0.82976 | −0.620903 | 0.0349* | |
H333 | 0.497723 | 0.861978 | −0.544336 | 0.0349* | |
H341 | 0.422306 | 0.865219 | −0.517658 | 0.0196* | |
H351 | 0.417042 | 0.986086 | −0.568871 | 0.0383* | |
H352 | 0.46422 | 0.975717 | −0.545989 | 0.0383* | |
H353 | 0.450948 | 0.966575 | −0.628173 | 0.0383* | |
H361 | 0.31425 | 0.765869 | −0.635028 | 0.0297* | |
H362 | 0.28263 | 0.822658 | −0.600339 | 0.0297* | |
H363 | 0.304895 | 0.84126 | −0.67471 | 0.0297* | |
H371 | 0.349594 | 0.833897 | −0.536967 | 0.0324* | |
H381 | 0.352804 | 0.949214 | −0.525256 | 0.0414* | |
H382 | 0.342665 | 0.96484 | −0.607839 | 0.0414* | |
H383 | 0.30688 | 0.938527 | −0.554762 | 0.0414* | |
H391 | 0.491507 | 0.829288 | −0.857689 | 0.0342* | |
H392 | 0.488048 | 0.782428 | −0.929777 | 0.0342* | |
H393 | 0.511393 | 0.859099 | −0.930537 | 0.0342* | |
H401 | 0.439265 | 0.859861 | −0.978729 | 0.0299* | |
H411 | 0.424149 | 0.97943 | −0.930389 | 0.0343* | |
H412 | 0.461107 | 0.968725 | −0.874527 | 0.0343* | |
H413 | 0.470613 | 0.973583 | −0.958624 | 0.0343* | |
H421 | 0.311269 | 0.838805 | −0.8445 | 0.0372* | |
H422 | 0.292757 | 0.835893 | −0.924016 | 0.0372* | |
H423 | 0.321159 | 0.770923 | −0.895392 | 0.0372* | |
H431 | 0.356378 | 0.917288 | −0.915711 | 0.025* | 0.612 (8) |
H441 | 0.332932 | 0.889064 | −1.023725 | 0.0364* | 0.612 (8) |
H442 | 0.382251 | 0.889208 | −1.022176 | 0.0364* | 0.612 (8) |
H443 | 0.357655 | 0.813762 | −1.022505 | 0.0364* | 0.612 (8) |
H21' | 0.138358 | 0.807989 | −0.90778 | 0.0253* | |
H31' | 0.209683 | 0.803339 | −0.939002 | 0.0252* | |
H41' | 0.253296 | 0.710662 | −0.888937 | 0.0247* | |
H61' | 0.043015 | 0.77034 | −0.824264 | 0.0253* | |
H62' | 0.072196 | 0.788776 | −0.886752 | 0.0253* | |
H71' | 0.070827 | 0.896201 | −0.825229 | 0.035* | |
H72' | 0.071874 | 0.856458 | −0.748881 | 0.035* | |
H73' | 0.112906 | 0.861566 | −0.79626 | 0.035* | |
H81' | 0.280411 | 0.607746 | −0.861271 | 0.0305* | |
H82' | 0.284483 | 0.551674 | −0.798492 | 0.0305* | |
H91' | 0.32785 | 0.660861 | −0.782956 | 0.0374* | |
H92' | 0.286349 | 0.705921 | −0.769643 | 0.0374* | |
H93' | 0.299733 | 0.64351 | −0.714532 | 0.0374* | |
H101' | 0.034446 | 0.662005 | −0.898028 | 0.0299* | |
H102' | 0.052173 | 0.580904 | −0.893709 | 0.0299* | |
H103' | 0.003447 | 0.594442 | −0.893702 | 0.0299* | |
H111' | 0.010052 | 0.654955 | −0.779652 | 0.0245* | |
H121' | 0.027681 | 0.542654 | −0.710228 | 0.0318* | |
H122' | −0.010341 | 0.535882 | −0.764508 | 0.0318* | |
H123' | 0.033996 | 0.505284 | −0.786972 | 0.0318* | |
H131' | 0.121776 | 0.764329 | −0.6695 | 0.045* | |
H132' | 0.097628 | 0.763228 | −0.594655 | 0.045* | |
H133' | 0.12293 | 0.693135 | −0.620162 | 0.045* | |
H141' | 0.049726 | 0.745029 | −0.693006 | 0.0346* | |
H151' | 0.0093 | 0.663878 | −0.645198 | 0.0472* | |
H152' | 0.046728 | 0.615031 | −0.616829 | 0.0472* | |
H153' | 0.036303 | 0.690644 | −0.578385 | 0.0472* | |
H161' | 0.237747 | 0.499719 | −0.893678 | 0.0322* | |
H162' | 0.22767 | 0.415048 | −0.903036 | 0.0322* | |
H163' | 0.190909 | 0.472425 | −0.89447 | 0.0322* | |
H171' | 0.248892 | 0.442435 | −0.781678 | 0.0309* | |
H181' | 0.192356 | 0.379029 | −0.724195 | 0.0408* | |
H182' | 0.166884 | 0.386006 | −0.797384 | 0.0408* | |
H183' | 0.208077 | 0.338197 | −0.794894 | 0.0408* | |
H191' | 0.232235 | 0.64959 | −0.649142 | 0.0413* | |
H192' | 0.194627 | 0.610716 | −0.608944 | 0.0413* | |
H193' | 0.240056 | 0.606615 | −0.575745 | 0.0413* | |
H201' | 0.26177 | 0.535534 | −0.675477 | 0.031* | |
H211' | 0.234931 | 0.423546 | −0.640323 | 0.0374* | |
H212' | 0.235267 | 0.472012 | −0.569023 | 0.0374* | |
H213' | 0.193168 | 0.460016 | −0.612168 | 0.0374* | |
H251' | 0.08046 | 0.354001 | −0.36472 | 0.0194* | |
H261' | 0.075376 | 0.285928 | −0.253662 | 0.0201* | |
H271' | 0.087755 | 0.348648 | −0.142449 | 0.0197* | |
H291' | 0.081923 | 0.498564 | −0.486306 | 0.0266* | |
H292' | 0.064391 | 0.430424 | −0.450762 | 0.0266* | |
H301' | 0.122954 | 0.401032 | −0.52301 | 0.035* | |
H302' | 0.151376 | 0.449952 | −0.472072 | 0.035* | |
H303' | 0.130982 | 0.37692 | −0.441719 | 0.035* | |
H311' | 0.07315 | 0.422035 | −0.051455 | 0.0305* | |
H313' | 0.092098 | 0.487316 | −0.014101 | 0.0305* | |
H321' | 0.134881 | 0.391175 | 0.016087 | 0.0456* | |
H322' | 0.137613 | 0.363929 | −0.065302 | 0.0456* | |
H323' | 0.161363 | 0.436176 | −0.041144 | 0.0456* | |
H331' | 0.018414 | 0.534243 | −0.41586 | 0.0349* | |
H332' | 0.001197 | 0.599604 | −0.367744 | 0.0349* | |
H333' | −0.006344 | 0.599669 | −0.452577 | 0.0349* | |
H341' | 0.062065 | 0.619654 | −0.474874 | 0.0196* | |
H351' | 0.071315 | 0.738218 | −0.430983 | 0.0383* | |
H352' | 0.022832 | 0.727793 | −0.443002 | 0.0383* | |
H353' | 0.041825 | 0.722431 | −0.363955 | 0.0383* | |
H361' | 0.17462 | 0.526208 | −0.37214 | 0.0297* | |
H362' | 0.2039 | 0.570052 | −0.426018 | 0.0297* | |
H363' | 0.192112 | 0.60439 | −0.349854 | 0.0297* | |
H371' | 0.140129 | 0.587779 | −0.469743 | 0.0324* | |
H381' | 0.12856 | 0.714987 | −0.461535 | 0.0414* | |
H382' | 0.158263 | 0.719415 | −0.39314 | 0.0414* | |
H383' | 0.176821 | 0.699261 | −0.470151 | 0.0414* | |
H391' | 0.025113 | 0.535392 | −0.075688 | 0.0342* | |
H392' | 0.005263 | 0.601552 | −0.0319 | 0.0342* | |
H393' | 0.009438 | 0.606311 | −0.117305 | 0.0342* | |
H401' | 0.073687 | 0.607835 | −0.016941 | 0.0299* | |
H411' | 0.092624 | 0.725146 | −0.065011 | 0.0343* | |
H412' | 0.051507 | 0.722882 | −0.112382 | 0.0343* | |
H413' | 0.048471 | 0.725382 | −0.026737 | 0.0343* | |
H421' | 0.216403 | 0.584212 | −0.112866 | 0.0372* | |
H422' | 0.18704 | 0.51456 | −0.119106 | 0.0372* | |
H423' | 0.186758 | 0.575001 | −0.180873 | 0.0372* | |
H431' | 0.158546 | 0.65974 | −0.097601 | 0.025* | 0.747 (8) |
H441' | 0.141347 | 0.640415 | 0.012796 | 0.0364* | 0.747 (8) |
H442' | 0.154941 | 0.556838 | 0.00905 | 0.0364* | 0.747 (8) |
H443' | 0.188971 | 0.619631 | 0.003869 | 0.0364* | 0.747 (8) |
C44b | 0.3495 (4) | 0.9399 (6) | −0.9454 (6) | 0.024 (2)* | 0.388 (8) |
C44b' | 0.1632 (6) | 0.6897 (9) | −0.0688 (9) | 0.024 (2)* | 0.253 (8) |
H441b | 0.369756 | 0.953834 | −0.981781 | 0.0288* | 0.388 |
H442b | 0.321635 | 0.944528 | −0.96529 | 0.0288* | 0.388 |
H443b | 0.352213 | 0.971802 | −0.903533 | 0.0288* | 0.388 |
H441b' | 0.178259 | 0.714335 | −0.107357 | 0.0288* | 0.2528 |
H442b' | 0.136561 | 0.713688 | −0.061503 | 0.0288* | 0.2528 |
H443b' | 0.179312 | 0.691995 | −0.024411 | 0.0288* | 0.2528 |
H431b | 0.364346 | 0.847862 | −0.971747 | 0.025* | 0.388 |
H431b' | 0.156601 | 0.586934 | −0.041542 | 0.025* | 0.2528 |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0110 (3) | 0.0134 (4) | 0.0254 (3) | −0.0025 (3) | −0.0016 (2) | 0.0022 (2) |
P1 | 0.0166 (7) | 0.0167 (7) | 0.0228 (6) | 0.0010 (6) | −0.0002 (4) | 0.0021 (4) |
P2 | 0.0121 (7) | 0.0174 (7) | 0.0190 (6) | 0.0001 (6) | −0.0021 (4) | 0.0045 (4) |
O1 | 0.042 (2) | 0.136 (5) | 0.0243 (18) | −0.042 (3) | 0.0038 (17) | −0.012 (2) |
O2 | 0.0267 (19) | 0.055 (2) | 0.051 (2) | −0.0186 (17) | −0.0201 (16) | 0.0261 (19) |
N2 | 0.0139 (9) | 0.0169 (9) | 0.0270 (10) | −0.0049 (7) | 0.0019 (8) | 0.0016 (7) |
N1 | 0.0135 (9) | 0.0164 (9) | 0.0203 (9) | −0.0014 (7) | 0.0018 (7) | 0.0020 (7) |
N3 | 0.0115 (9) | 0.0196 (9) | 0.0248 (10) | −0.0019 (7) | −0.0013 (7) | 0.0048 (8) |
C1 | 0.0177 (11) | 0.0131 (9) | 0.0182 (10) | 0.0010 (8) | 0.0014 (9) | −0.0003 (8) |
C2 | 0.0221 (12) | 0.0172 (11) | 0.0239 (12) | −0.0013 (9) | 0.0030 (9) | 0.0072 (9) |
C3 | 0.0245 (12) | 0.0182 (11) | 0.0202 (11) | 0.0049 (9) | 0.0018 (9) | 0.0048 (9) |
C4 | 0.0165 (11) | 0.0214 (11) | 0.0237 (11) | 0.0037 (9) | −0.0018 (9) | 0.0032 (9) |
C5 | 0.0153 (10) | 0.0154 (10) | 0.0148 (9) | 0.0002 (8) | 0.0025 (8) | 0.0022 (7) |
C6 | 0.0179 (11) | 0.0168 (10) | 0.0287 (12) | −0.0030 (9) | 0.0050 (9) | 0.0020 (9) |
C7 | 0.0179 (12) | 0.0183 (12) | 0.0513 (17) | −0.0046 (9) | 0.0065 (12) | −0.0035 (11) |
C8 | 0.0130 (11) | 0.0284 (13) | 0.0348 (14) | −0.0026 (9) | −0.0025 (10) | 0.0094 (10) |
C9 | 0.0140 (11) | 0.0330 (13) | 0.0466 (17) | 0.0077 (9) | 0.0031 (11) | 0.0109 (11) |
C10 | 0.0216 (12) | 0.0291 (13) | 0.0241 (12) | 0.0029 (10) | 0.0036 (10) | −0.0003 (10) |
C11 | 0.0189 (12) | 0.0238 (11) | 0.0185 (10) | 0.0032 (9) | 0.0020 (9) | 0.0020 (9) |
C12 | 0.0169 (11) | 0.0235 (11) | 0.0391 (15) | 0.0052 (9) | −0.0035 (10) | 0.0044 (10) |
C13 | 0.0371 (16) | 0.0417 (17) | 0.0336 (15) | −0.0066 (13) | 0.0100 (12) | −0.0172 (13) |
C14 | 0.0264 (14) | 0.0392 (15) | 0.0210 (12) | −0.0056 (11) | 0.0044 (10) | −0.0084 (10) |
C15 | 0.0343 (16) | 0.072 (3) | 0.0116 (11) | −0.0115 (16) | −0.0019 (11) | −0.0025 (13) |
C16 | 0.0264 (14) | 0.0267 (14) | 0.0274 (14) | −0.0042 (11) | −0.0052 (11) | −0.0055 (11) |
C17 | 0.0224 (13) | 0.0175 (11) | 0.0374 (14) | −0.0039 (9) | −0.0027 (11) | 0.0012 (10) |
C18 | 0.0284 (14) | 0.0186 (12) | 0.0551 (17) | −0.0006 (10) | −0.0012 (13) | 0.0034 (12) |
C19 | 0.0296 (15) | 0.0445 (17) | 0.0292 (14) | −0.0004 (13) | 0.0075 (12) | −0.0028 (12) |
C20 | 0.0236 (13) | 0.0312 (14) | 0.0227 (12) | −0.0032 (10) | 0.0015 (10) | 0.0053 (10) |
C21 | 0.0264 (14) | 0.0359 (16) | 0.0311 (14) | −0.0049 (12) | 0.0009 (11) | 0.0162 (12) |
C22 | 0.0103 (11) | 0.0201 (12) | 0.0469 (16) | −0.0069 (9) | −0.0116 (11) | 0.0089 (11) |
C23 | 0.0233 (14) | 0.0305 (14) | 0.0378 (15) | −0.0117 (11) | −0.0033 (11) | 0.0032 (12) |
Fe2 | 0.0161 (4) | 0.0049 (3) | 0.0181 (4) | 0.0030 (4) | 0.00081 (19) | 0.00054 (17) |
P3 | 0.0181 (6) | 0.0103 (5) | 0.0193 (5) | 0.0036 (4) | −0.0001 (4) | 0.0016 (4) |
P4 | 0.0182 (6) | 0.0102 (5) | 0.0183 (5) | 0.0009 (4) | 0.0007 (4) | 0.0000 (4) |
O3 | 0.040 (2) | 0.026 (2) | 0.0232 (16) | −0.0103 (19) | −0.0004 (13) | 0.0030 (13) |
O4 | 0.0194 (19) | 0.030 (2) | 0.0273 (17) | 0.0124 (18) | 0.0059 (12) | 0.0081 (14) |
N5 | 0.0181 (13) | 0.0073 (9) | 0.0119 (8) | 0.0002 (9) | 0.0026 (8) | 0.0031 (7) |
N4 | 0.0089 (8) | 0.0031 (8) | 0.0127 (7) | −0.0023 (6) | 0.0007 (7) | −0.0009 (6) |
N6 | 0.0259 (12) | 0.0099 (8) | 0.0126 (8) | 0.0032 (8) | −0.0025 (8) | −0.0011 (7) |
C24 | 0.0071 (11) | 0.0111 (10) | 0.0143 (9) | 0.0004 (8) | 0.0020 (8) | 0.0038 (7) |
C25 | 0.0199 (13) | 0.0078 (10) | 0.0210 (11) | 0.0013 (9) | 0.0023 (9) | 0.0060 (8) |
C26 | 0.0175 (10) | 0.0064 (7) | 0.0264 (10) | 0.0015 (7) | −0.0001 (10) | 0.0001 (10) |
C27 | 0.0197 (12) | 0.0103 (10) | 0.0193 (11) | 0.0017 (9) | −0.0008 (9) | −0.0039 (8) |
C28 | 0.0147 (11) | 0.0100 (10) | 0.0175 (10) | 0.0004 (8) | −0.0011 (8) | −0.0008 (8) |
C29 | 0.038 (2) | 0.0150 (12) | 0.0139 (10) | 0.0015 (14) | 0.0055 (13) | 0.0064 (9) |
C30 | 0.040 (2) | 0.0235 (14) | 0.0242 (15) | −0.0027 (15) | 0.0090 (14) | 0.0087 (11) |
C31 | 0.045 (2) | 0.0163 (12) | 0.0155 (11) | 0.0043 (12) | −0.0007 (12) | −0.0047 (9) |
C32 | 0.064 (2) | 0.0214 (13) | 0.0282 (14) | −0.0023 (14) | −0.0192 (15) | −0.0088 (10) |
C33 | 0.0282 (19) | 0.0273 (15) | 0.0316 (18) | −0.0010 (14) | −0.0147 (14) | 0.0045 (13) |
C34 | 0.0250 (18) | 0.0154 (12) | 0.0084 (11) | −0.0020 (12) | −0.0020 (11) | 0.0019 (9) |
C35 | 0.054 (2) | 0.0188 (13) | 0.0230 (14) | −0.0039 (14) | −0.0142 (14) | −0.0028 (10) |
C36 | 0.0114 (15) | 0.0268 (15) | 0.0359 (18) | −0.0023 (13) | 0.0062 (13) | 0.0016 (14) |
C37 | 0.0355 (19) | 0.0239 (13) | 0.0216 (13) | 0.0109 (14) | 0.0138 (13) | 0.0011 (10) |
C38 | 0.041 (2) | 0.0306 (16) | 0.0317 (15) | 0.0152 (15) | 0.0072 (14) | −0.0059 (12) |
C39 | 0.032 (2) | 0.0274 (16) | 0.0257 (17) | 0.0001 (15) | 0.0116 (14) | −0.0029 (13) |
C40 | 0.040 (2) | 0.0159 (12) | 0.0185 (12) | −0.0019 (13) | 0.0092 (13) | −0.0006 (10) |
C41 | 0.048 (2) | 0.0168 (12) | 0.0207 (14) | −0.0049 (15) | 0.0073 (14) | 0.0038 (11) |
C42 | 0.0286 (17) | 0.0313 (17) | 0.033 (2) | 0.0049 (14) | −0.0173 (15) | −0.0046 (16) |
C43 | 0.0226 (18) | 0.0205 (14) | 0.0193 (14) | −0.0014 (13) | −0.0058 (12) | 0.0076 (11) |
C44 | 0.047 (3) | 0.025 (2) | 0.019 (2) | 0.009 (2) | −0.019 (2) | −0.0012 (16) |
C45 | 0.0235 (10) | 0.0112 (9) | 0.0108 (9) | 0.0027 (7) | −0.0023 (11) | 0.0025 (11) |
C46 | 0.0178 (10) | 0.0155 (9) | 0.0167 (9) | −0.0009 (7) | −0.0008 (12) | −0.0014 (9) |
Fe1' | 0.0084 (3) | 0.0119 (3) | 0.0141 (3) | 0.0023 (3) | −0.0028 (2) | 0.0003 (2) |
P1' | 0.0129 (6) | 0.0132 (6) | 0.0107 (5) | −0.0013 (5) | −0.0027 (3) | 0.0003 (4) |
P2' | 0.0118 (6) | 0.0090 (6) | 0.0172 (6) | 0.0009 (6) | 0.0013 (3) | 0.0033 (3) |
O1' | 0.0194 (15) | 0.0184 (14) | 0.0281 (15) | 0.0010 (11) | 0.0048 (12) | 0.0026 (12) |
O2' | 0.0159 (14) | 0.0137 (13) | 0.0292 (15) | 0.0001 (11) | 0.0024 (11) | 0.0078 (11) |
N2' | 0.0139 (9) | 0.0169 (9) | 0.0270 (10) | 0.0049 (7) | −0.0019 (8) | 0.0016 (7) |
N1' | 0.0135 (9) | 0.0164 (9) | 0.0203 (9) | 0.0014 (7) | −0.0018 (7) | 0.0020 (7) |
N3' | 0.0115 (9) | 0.0196 (9) | 0.0248 (10) | 0.0019 (7) | 0.0013 (7) | 0.0048 (8) |
C1' | 0.0177 (11) | 0.0131 (9) | 0.0182 (10) | −0.0010 (8) | −0.0014 (9) | −0.0003 (8) |
C2' | 0.0221 (12) | 0.0172 (11) | 0.0239 (12) | 0.0013 (9) | −0.0030 (9) | 0.0072 (9) |
C3' | 0.0245 (12) | 0.0182 (11) | 0.0202 (11) | −0.0049 (9) | −0.0018 (9) | 0.0048 (9) |
C4' | 0.0165 (11) | 0.0214 (11) | 0.0237 (11) | −0.0037 (9) | 0.0018 (9) | 0.0032 (9) |
C5' | 0.0153 (10) | 0.0154 (10) | 0.0148 (9) | −0.0002 (8) | −0.0025 (8) | 0.0022 (7) |
C6' | 0.0179 (11) | 0.0168 (10) | 0.0287 (12) | 0.0030 (9) | −0.0050 (9) | 0.0020 (9) |
C7' | 0.0179 (12) | 0.0183 (12) | 0.0513 (17) | 0.0046 (9) | −0.0065 (12) | −0.0035 (11) |
C8' | 0.0130 (11) | 0.0284 (13) | 0.0348 (14) | 0.0026 (9) | 0.0025 (10) | 0.0094 (10) |
C9' | 0.0140 (11) | 0.0330 (13) | 0.0466 (17) | −0.0077 (9) | −0.0031 (11) | 0.0109 (11) |
C10' | 0.0216 (12) | 0.0291 (13) | 0.0241 (12) | −0.0029 (10) | −0.0036 (10) | −0.0003 (10) |
C11' | 0.0189 (12) | 0.0238 (11) | 0.0185 (10) | −0.0032 (9) | −0.0020 (9) | 0.0020 (9) |
C12' | 0.0169 (11) | 0.0235 (11) | 0.0391 (15) | −0.0052 (9) | 0.0035 (10) | 0.0044 (10) |
C13' | 0.0371 (16) | 0.0417 (17) | 0.0336 (15) | 0.0066 (13) | −0.0100 (12) | −0.0172 (13) |
C14' | 0.0264 (14) | 0.0392 (15) | 0.0210 (12) | 0.0056 (11) | −0.0044 (10) | −0.0084 (10) |
C15' | 0.0343 (16) | 0.072 (3) | 0.0116 (11) | 0.0115 (16) | 0.0019 (11) | −0.0025 (13) |
C16' | 0.0264 (14) | 0.0267 (14) | 0.0274 (14) | 0.0042 (11) | 0.0052 (11) | −0.0055 (11) |
C17' | 0.0224 (13) | 0.0175 (11) | 0.0374 (14) | 0.0039 (9) | 0.0027 (11) | 0.0012 (10) |
C18' | 0.0284 (14) | 0.0186 (12) | 0.0551 (17) | 0.0006 (10) | 0.0012 (13) | 0.0034 (12) |
C19' | 0.0296 (15) | 0.0445 (17) | 0.0292 (14) | 0.0004 (13) | −0.0075 (12) | −0.0028 (12) |
C20' | 0.0236 (13) | 0.0312 (14) | 0.0227 (12) | 0.0032 (10) | −0.0015 (10) | 0.0053 (10) |
C21' | 0.0264 (14) | 0.0359 (16) | 0.0311 (14) | 0.0049 (12) | −0.0009 (11) | 0.0162 (12) |
C22' | 0.0103 (11) | 0.0201 (12) | 0.0469 (16) | 0.0069 (9) | 0.0116 (11) | 0.0089 (11) |
C23' | 0.0233 (14) | 0.0305 (14) | 0.0378 (15) | 0.0117 (11) | 0.0033 (11) | 0.0032 (12) |
Fe2' | 0.0058 (3) | 0.0099 (3) | 0.0032 (3) | 0.0007 (3) | −0.00049 (15) | −0.00064 (15) |
P3' | 0.0131 (5) | 0.0080 (5) | 0.0050 (4) | −0.0007 (4) | 0.0013 (4) | −0.0015 (3) |
P4' | 0.0258 (7) | 0.0087 (5) | 0.0056 (4) | −0.0049 (4) | −0.0037 (4) | −0.0005 (4) |
O3' | 0.0089 (16) | 0.033 (2) | 0.0244 (15) | 0.0029 (16) | 0.0012 (11) | −0.0058 (14) |
O4' | 0.029 (2) | 0.0124 (18) | 0.0284 (19) | −0.0103 (17) | −0.0045 (11) | 0.0009 (10) |
N5' | 0.0181 (13) | 0.0073 (9) | 0.0119 (8) | −0.0002 (9) | 0.0026 (8) | −0.0031 (7) |
N4' | 0.0089 (8) | 0.0031 (8) | 0.0127 (7) | 0.0023 (6) | 0.0007 (7) | 0.0009 (6) |
N6' | 0.0259 (12) | 0.0099 (8) | 0.0126 (8) | −0.0032 (8) | −0.0025 (8) | 0.0011 (7) |
C24' | 0.0071 (11) | 0.0111 (10) | 0.0143 (9) | −0.0004 (8) | 0.0020 (8) | −0.0038 (7) |
C25' | 0.0199 (13) | 0.0078 (10) | 0.0210 (11) | −0.0013 (9) | 0.0023 (9) | −0.0060 (8) |
C26' | 0.0175 (10) | 0.0064 (7) | 0.0264 (10) | −0.0015 (7) | −0.0001 (10) | −0.0001 (10) |
C27' | 0.0197 (12) | 0.0103 (10) | 0.0193 (11) | −0.0017 (9) | −0.0008 (9) | 0.0039 (8) |
C28' | 0.0147 (11) | 0.0100 (10) | 0.0175 (10) | −0.0004 (8) | −0.0011 (8) | 0.0008 (8) |
C29' | 0.038 (2) | 0.0150 (12) | 0.0139 (10) | −0.0015 (14) | 0.0055 (13) | −0.0064 (9) |
C30' | 0.040 (2) | 0.0235 (14) | 0.0242 (15) | 0.0027 (15) | 0.0090 (14) | −0.0087 (11) |
C31' | 0.045 (2) | 0.0163 (12) | 0.0155 (11) | −0.0043 (12) | −0.0007 (12) | 0.0047 (9) |
C32' | 0.064 (2) | 0.0214 (13) | 0.0282 (14) | 0.0023 (14) | −0.0192 (15) | 0.0088 (10) |
C33' | 0.0282 (19) | 0.0273 (15) | 0.0316 (18) | 0.0010 (14) | −0.0147 (14) | −0.0045 (13) |
C34' | 0.0250 (18) | 0.0154 (12) | 0.0084 (11) | 0.0020 (12) | −0.0020 (11) | −0.0019 (9) |
C35' | 0.054 (2) | 0.0188 (13) | 0.0230 (14) | 0.0039 (14) | −0.0142 (14) | 0.0028 (10) |
C36' | 0.0114 (15) | 0.0268 (15) | 0.0359 (18) | 0.0023 (13) | 0.0062 (13) | −0.0016 (14) |
C37' | 0.0355 (19) | 0.0239 (13) | 0.0216 (13) | −0.0109 (14) | 0.0138 (13) | −0.0011 (10) |
C38' | 0.041 (2) | 0.0306 (16) | 0.0317 (15) | −0.0152 (15) | 0.0072 (14) | 0.0059 (12) |
C39' | 0.032 (2) | 0.0274 (16) | 0.0257 (17) | −0.0001 (15) | 0.0116 (14) | 0.0029 (13) |
C40' | 0.040 (2) | 0.0159 (12) | 0.0185 (12) | 0.0019 (13) | 0.0092 (13) | 0.0006 (10) |
C41' | 0.048 (2) | 0.0168 (12) | 0.0207 (14) | 0.0049 (15) | 0.0073 (14) | −0.0038 (11) |
C42' | 0.0286 (17) | 0.0313 (17) | 0.033 (2) | −0.0049 (14) | −0.0173 (15) | 0.0046 (16) |
C43' | 0.0226 (18) | 0.0205 (14) | 0.0193 (14) | 0.0014 (13) | −0.0058 (12) | −0.0076 (11) |
C44' | 0.047 (3) | 0.025 (2) | 0.019 (2) | −0.009 (2) | −0.019 (2) | 0.0012 (16) |
C45' | 0.0235 (10) | 0.0112 (9) | 0.0108 (9) | −0.0027 (7) | −0.0023 (11) | −0.0025 (11) |
C46' | 0.0178 (10) | 0.0155 (9) | 0.0167 (9) | 0.0009 (7) | −0.0008 (12) | 0.0014 (9) |
Geometric parameters (Å, º) top
Fe1—P1 | 2.1990 (19) | P1'—C11' | 1.858 (4) |
Fe1—P2 | 2.1962 (18) | P1'—C14' | 1.865 (4) |
Fe1—N1 | 2.049 (3) | P2'—N3' | 1.733 (4) |
Fe1—C22 | 1.798 (5) | P2'—C17' | 1.857 (4) |
Fe1—C23 | 1.692 (5) | P2'—C20' | 1.870 (4) |
P1—N2 | 1.733 (4) | O1'—C22' | 1.071 (5) |
P1—C11 | 1.870 (4) | O2'—C23' | 1.106 (6) |
P1—C14 | 1.823 (4) | N2'—C1' | 1.378 (5) |
P2—N3 | 1.713 (4) | N2'—C6' | 1.465 (5) |
P2—C17 | 1.877 (4) | N1'—C1' | 1.369 (5) |
P2—C20 | 1.841 (4) | N1'—C5' | 1.364 (5) |
O1—C22 | 1.064 (7) | N3'—C5' | 1.365 (5) |
O2—C23 | 1.097 (6) | N3'—C8' | 1.477 (5) |
N2—C1 | 1.368 (5) | C1'—C2' | 1.396 (5) |
N2—C6 | 1.467 (5) | C2'—C3' | 1.377 (6) |
N1—C1 | 1.370 (5) | C2'—H21' | 0.96 |
N1—C5 | 1.370 (5) | C3'—C4' | 1.384 (6) |
N3—C5 | 1.383 (5) | C3'—H31' | 0.96 |
N3—C8 | 1.476 (5) | C4'—C5' | 1.412 (5) |
C1—C2 | 1.380 (5) | C4'—H41' | 0.96 |
C2—C3 | 1.399 (6) | C6'—C7' | 1.524 (6) |
C2—H21 | 0.96 | C6'—H61' | 0.96 |
C3—C4 | 1.372 (6) | C6'—H62' | 0.96 |
C3—H31 | 0.96 | C7'—H71' | 0.96 |
C4—C5 | 1.403 (5) | C7'—H72' | 0.96 |
C4—H41 | 0.96 | C7'—H73' | 0.96 |
C6—C7 | 1.549 (6) | C8'—C9' | 1.540 (7) |
C6—H61 | 0.96 | C8'—H81' | 0.96 |
C6—H62 | 0.96 | C8'—H82' | 0.96 |
C7—H71 | 0.96 | C9'—H91' | 0.96 |
C7—H72 | 0.96 | C9'—H92' | 0.96 |
C7—H73 | 0.96 | C9'—H93' | 0.96 |
C8—C9 | 1.534 (7) | C10'—C11' | 1.541 (5) |
C8—H81 | 0.96 | C10'—H101' | 0.96 |
C8—H82 | 0.96 | C10'—H102' | 0.96 |
C9—H91 | 0.96 | C10'—H103' | 0.96 |
C9—H92 | 0.96 | C11'—C12' | 1.512 (7) |
C9—H93 | 0.96 | C11'—H111' | 0.96 |
C10—C11 | 1.491 (5) | C12'—H121' | 0.96 |
C10—H101 | 0.96 | C12'—H122' | 0.96 |
C10—H102 | 0.96 | C12'—H123' | 0.96 |
C10—H103 | 0.96 | C13'—C14' | 1.547 (7) |
C11—H111 | 0.96 | C13'—H131' | 0.96 |
C12—H121 | 0.96 | C13'—H132' | 0.96 |
C12—H122 | 0.96 | C13'—H133' | 0.96 |
C12—H123 | 0.96 | C14'—C15' | 1.492 (6) |
C13—C14 | 1.505 (6) | C14'—H141' | 0.96 |
C13—H131 | 0.96 | C15'—H151' | 0.96 |
C13—H132 | 0.96 | C15'—H152' | 0.96 |
C13—H133 | 0.96 | C15'—H153' | 0.96 |
C14—H141 | 0.96 | C16'—C17' | 1.511 (6) |
C15—H151 | 0.96 | C16'—H161' | 0.96 |
C15—H152 | 0.96 | C16'—H162' | 0.96 |
C15—H153 | 0.96 | C16'—H163' | 0.96 |
C16—C17 | 1.553 (6) | C17'—C18' | 1.531 (6) |
C16—H161 | 0.96 | C17'—H171' | 0.96 |
C16—H162 | 0.96 | C18'—H181' | 0.96 |
C16—H163 | 0.96 | C18'—H182' | 0.96 |
C17—C18 | 1.557 (6) | C18'—H183' | 0.96 |
C17—H171 | 0.96 | C19'—C20' | 1.522 (6) |
C18—H181 | 0.96 | C19'—H191' | 0.96 |
C18—H182 | 0.96 | C19'—H192' | 0.96 |
C18—H183 | 0.96 | C19'—H193' | 0.96 |
C19—C20 | 1.538 (6) | C20'—C21' | 1.553 (7) |
C19—H191 | 0.96 | C20'—H201' | 0.96 |
C19—H192 | 0.96 | C21'—H211' | 0.96 |
C19—H193 | 0.96 | C21'—H212' | 0.96 |
C20—C21 | 1.531 (7) | C21'—H213' | 0.96 |
C20—H201 | 0.96 | Fe2'—P3' | 2.1701 (12) |
C21—H211 | 0.96 | Fe2'—P4' | 2.1728 (13) |
C21—H212 | 0.96 | Fe2'—N4' | 1.970 (4) |
C21—H213 | 0.96 | Fe2'—C45' | 1.752 (6) |
Fe2—P3 | 2.1772 (14) | Fe2'—C46' | 1.743 (6) |
Fe2—P4 | 2.1793 (14) | P3'—N5' | 1.701 (4) |
Fe2—N4 | 2.091 (4) | P3'—C34' | 1.855 (4) |
Fe2—C45 | 1.781 (6) | P3'—C37' | 1.870 (5) |
Fe2—C46 | 1.721 (6) | P4'—N6' | 1.696 (4) |
P3—N5 | 1.749 (4) | P4'—C40' | 1.853 (5) |
P3—C34 | 1.870 (4) | P4'—C43' | 1.863 (4) |
P3—C37 | 1.843 (5) | O3'—C45' | 1.166 (7) |
P4—N6 | 1.740 (4) | O4'—C46' | 1.167 (8) |
P4—C40 | 1.862 (5) | N5'—C24' | 1.386 (5) |
P4—C43 | 1.842 (4) | N5'—C29' | 1.478 (5) |
O3—C45 | 1.136 (8) | N4'—C24' | 1.396 (5) |
O4—C46 | 1.163 (8) | N4'—C28' | 1.387 (5) |
N5—C24 | 1.365 (5) | N6'—C28' | 1.404 (6) |
N5—C29 | 1.470 (5) | N6'—C31' | 1.477 (6) |
N4—C24 | 1.331 (5) | C24'—C25' | 1.379 (6) |
N4—C28 | 1.336 (5) | C25'—C26' | 1.397 (6) |
N6—C28 | 1.374 (6) | C25'—H251' | 0.96 |
N6—C31 | 1.476 (6) | C26'—C27' | 1.385 (6) |
C24—C25 | 1.410 (6) | C26'—H261' | 0.96 |
C25—C26 | 1.379 (6) | C27'—C28' | 1.381 (6) |
C25—H251 | 0.96 | C27'—H271' | 0.96 |
C26—C27 | 1.366 (6) | C29'—C30' | 1.514 (7) |
C26—H261 | 0.96 | C29'—H291' | 0.96 |
C27—C28 | 1.411 (6) | C29'—H292' | 0.96 |
C27—H271 | 0.96 | C30'—H301' | 0.96 |
C29—C30 | 1.517 (7) | C30'—H302' | 0.96 |
C29—H291 | 0.96 | C30'—H303' | 0.96 |
C29—H292 | 0.96 | C31'—C32' | 1.526 (8) |
C30—H301 | 0.96 | C31'—H311' | 0.96 |
C30—H302 | 0.96 | C31'—H313' | 0.96 |
C30—H303 | 0.96 | C32'—H321' | 0.96 |
C31—C32 | 1.541 (8) | C32'—H322' | 0.96 |
C31—H311 | 0.96 | C32'—H323' | 0.96 |
C31—H313 | 0.96 | C33'—C34' | 1.494 (7) |
C32—H321 | 0.96 | C33'—H331' | 0.96 |
C32—H322 | 0.96 | C33'—H332' | 0.96 |
C32—H323 | 0.96 | C33'—H333' | 0.96 |
C33—C34 | 1.533 (6) | C34'—C35' | 1.541 (6) |
C33—H331 | 0.96 | C34'—H341' | 0.96 |
C33—H332 | 0.96 | C35'—H351' | 0.96 |
C33—H333 | 0.96 | C35'—H352' | 0.96 |
C34—C35 | 1.572 (6) | C35'—H353' | 0.96 |
C34—H341 | 0.96 | C36'—C37' | 1.469 (7) |
C35—H351 | 0.96 | C36'—H361' | 0.96 |
C35—H352 | 0.96 | C36'—H362' | 0.96 |
C35—H353 | 0.96 | C36'—H363' | 0.96 |
C36—H361 | 0.96 | C37'—C38' | 1.558 (7) |
C36—H362 | 0.96 | C37'—H371' | 0.96 |
C36—H363 | 0.96 | C38'—H381' | 0.96 |
C37—C38 | 1.480 (7) | C38'—H382' | 0.96 |
C37—H371 | 0.96 | C38'—H383' | 0.96 |
C38—H381 | 0.96 | C39'—C40' | 1.491 (7) |
C38—H382 | 0.96 | C39'—H391' | 0.96 |
C38—H383 | 0.96 | C39'—H392' | 0.96 |
C39—C40 | 1.555 (7) | C39'—H393' | 0.96 |
C39—H391 | 0.96 | C40'—C41' | 1.516 (6) |
C39—H392 | 0.96 | C40'—H401' | 0.96 |
C39—H393 | 0.96 | C41'—H411' | 0.96 |
C40—C41 | 1.540 (6) | C41'—H412' | 0.96 |
C40—H401 | 0.96 | C41'—H413' | 0.96 |
C41—H411 | 0.96 | C42'—C43' | 1.476 (7) |
C41—H412 | 0.96 | C42'—H421' | 0.96 |
C41—H413 | 0.96 | C42'—H422' | 0.96 |
C42—C43 | 1.568 (7) | C42'—H423' | 0.96 |
C42—H421 | 0.96 | C43'—C44' | 1.493 (6) |
C42—H422 | 0.96 | C43'—H431' | 0.96 |
C42—H423 | 0.96 | C43'—C44b' | 1.554 (17) |
C43—C44 | 1.490 (7) | C43'—H431b' | 0.96 |
C43—H431 | 0.96 | C44'—H441' | 0.96 |
C43—C44b | 1.430 (12) | C44'—H442' | 0.96 |
C43—H431b | 0.96 | C44'—H443' | 0.96 |
C44—H441 | 0.96 | C44'—H431b' | 0.7001 |
C44—H442 | 0.96 | H431—C44b | 0.7121 |
C44—H443 | 0.96 | H431'—C44b' | 0.7675 |
C44—H431b | 0.7135 | C44b—H441b | 0.96 |
Fe1'—P1' | 2.1801 (17) | C44b—H442b | 0.96 |
Fe1'—P2' | 2.1922 (17) | C44b—H443b | 0.96 |
Fe1'—N1' | 2.050 (3) | C44b'—H441b' | 0.96 |
Fe1'—C22' | 1.833 (5) | C44b'—H442b' | 0.96 |
Fe1'—C23' | 1.706 (5) | C44b'—H443b' | 0.96 |
P1'—N2' | 1.733 (4) | | |
| | | |
P1—Fe1—P2 | 161.16 (8) | C17'—P2'—C20' | 103.4 (2) |
P1—Fe1—N1 | 81.85 (10) | P1'—N2'—C1' | 117.5 (3) |
P1—Fe1—C22 | 96.03 (15) | P1'—N2'—C6' | 122.9 (3) |
P1—Fe1—C23 | 91.71 (17) | C1'—N2'—C6' | 119.5 (3) |
P2—Fe1—N1 | 82.38 (10) | Fe1'—N1'—C1' | 120.2 (2) |
P2—Fe1—C22 | 98.03 (15) | Fe1'—N1'—C5' | 121.2 (2) |
P2—Fe1—C23 | 93.59 (16) | C1'—N1'—C5' | 118.0 (3) |
N1—Fe1—C22 | 105.31 (18) | P2'—N3'—C5' | 117.8 (3) |
N1—Fe1—C23 | 139.51 (19) | P2'—N3'—C8' | 121.9 (3) |
C22—Fe1—C23 | 115.1 (2) | C5'—N3'—C8' | 120.1 (3) |
Fe1—P1—N2 | 102.25 (13) | N2'—C1'—N1' | 115.6 (3) |
Fe1—P1—C11 | 122.03 (16) | N2'—C1'—C2' | 122.7 (3) |
Fe1—P1—C14 | 123.51 (15) | N1'—C1'—C2' | 121.8 (3) |
N2—P1—C11 | 103.06 (17) | C1'—C2'—C3' | 119.3 (4) |
N2—P1—C14 | 100.9 (2) | C1'—C2'—H21' | 120.36 |
C11—P1—C14 | 101.3 (2) | C3'—C2'—H21' | 120.36 |
Fe1—P2—N3 | 102.79 (13) | C2'—C3'—C4' | 120.5 (4) |
Fe1—P2—C17 | 122.04 (15) | C2'—C3'—H31' | 119.78 |
Fe1—P2—C20 | 121.52 (14) | C4'—C3'—H31' | 119.77 |
N3—P2—C17 | 101.82 (18) | C3'—C4'—C5' | 118.1 (4) |
N3—P2—C20 | 102.15 (19) | C3'—C4'—H41' | 120.96 |
C17—P2—C20 | 103.0 (2) | C5'—C4'—H41' | 120.96 |
P1—N2—C1 | 117.4 (3) | N1'—C5'—N3' | 115.8 (3) |
P1—N2—C6 | 122.6 (3) | N1'—C5'—C4' | 122.2 (3) |
C1—N2—C6 | 119.4 (3) | N3'—C5'—C4' | 122.0 (3) |
Fe1—N1—C1 | 120.8 (2) | N2'—C6'—C7' | 114.9 (3) |
Fe1—N1—C5 | 120.3 (2) | N2'—C6'—H61' | 109.47 |
C1—N1—C5 | 118.2 (3) | N2'—C6'—H62' | 109.47 |
P2—N3—C5 | 117.5 (3) | C7'—C6'—H61' | 109.47 |
P2—N3—C8 | 122.5 (3) | C7'—C6'—H62' | 109.47 |
C5—N3—C8 | 120.0 (3) | H61'—C6'—H62' | 103.47 |
N2—C1—N1 | 116.1 (3) | C6'—C7'—H71' | 109.47 |
N2—C1—C2 | 122.5 (4) | C6'—C7'—H72' | 109.47 |
N1—C1—C2 | 121.4 (3) | C6'—C7'—H73' | 109.47 |
C1—C2—C3 | 119.7 (4) | H71'—C7'—H72' | 109.47 |
C1—C2—H21 | 120.17 | H71'—C7'—H73' | 109.47 |
C3—C2—H21 | 120.17 | H72'—C7'—H73' | 109.47 |
C2—C3—C4 | 120.1 (4) | N3'—C8'—C9' | 112.7 (3) |
C2—C3—H31 | 119.96 | N3'—C8'—H81' | 109.47 |
C4—C3—H31 | 119.97 | N3'—C8'—H82' | 109.47 |
C3—C4—C5 | 118.2 (4) | C9'—C8'—H81' | 109.47 |
C3—C4—H41 | 120.9 | C9'—C8'—H82' | 109.47 |
C5—C4—H41 | 120.91 | H81'—C8'—H82' | 106 |
N1—C5—N3 | 116.0 (3) | C8'—C9'—H91' | 109.47 |
N1—C5—C4 | 122.4 (3) | C8'—C9'—H92' | 109.47 |
N3—C5—C4 | 121.6 (3) | C8'—C9'—H93' | 109.47 |
N2—C6—C7 | 115.0 (3) | H91'—C9'—H92' | 109.47 |
N2—C6—H61 | 109.47 | H91'—C9'—H93' | 109.47 |
N2—C6—H62 | 109.47 | H92'—C9'—H93' | 109.47 |
C7—C6—H61 | 109.47 | C11'—C10'—H101' | 109.47 |
C7—C6—H62 | 109.47 | C11'—C10'—H102' | 109.47 |
H61—C6—H62 | 103.31 | C11'—C10'—H103' | 109.47 |
C6—C7—H71 | 109.47 | H101'—C10'—H102' | 109.47 |
C6—C7—H72 | 109.47 | H101'—C10'—H103' | 109.47 |
C6—C7—H73 | 109.47 | H102'—C10'—H103' | 109.47 |
H71—C7—H72 | 109.47 | P1'—C11'—C10' | 112.4 (3) |
H71—C7—H73 | 109.47 | P1'—C11'—C12' | 109.2 (3) |
H72—C7—H73 | 109.47 | P1'—C11'—H111' | 107.77 |
N3—C8—C9 | 112.5 (3) | C10'—C11'—C12' | 109.9 (3) |
N3—C8—H81 | 109.47 | C10'—C11'—H111' | 107.11 |
N3—C8—H82 | 109.47 | C12'—C11'—H111' | 110.42 |
C9—C8—H81 | 109.47 | C11'—C12'—H121' | 109.47 |
C9—C8—H82 | 109.47 | C11'—C12'—H122' | 109.47 |
H81—C8—H82 | 106.21 | C11'—C12'—H123' | 109.47 |
C8—C9—H91 | 109.47 | H121'—C12'—H122' | 109.47 |
C8—C9—H92 | 109.47 | H121'—C12'—H123' | 109.47 |
C8—C9—H93 | 109.47 | H122'—C12'—H123' | 109.47 |
H91—C9—H92 | 109.47 | C14'—C13'—H131' | 109.47 |
H91—C9—H93 | 109.47 | C14'—C13'—H132' | 109.47 |
H92—C9—H93 | 109.47 | C14'—C13'—H133' | 109.47 |
C11—C10—H101 | 109.47 | H131'—C13'—H132' | 109.47 |
C11—C10—H102 | 109.47 | H131'—C13'—H133' | 109.47 |
C11—C10—H103 | 109.47 | H132'—C13'—H133' | 109.47 |
H101—C10—H102 | 109.47 | P1'—C14'—C13' | 109.4 (3) |
H101—C10—H103 | 109.47 | P1'—C14'—C15' | 114.7 (3) |
H102—C10—H103 | 109.47 | P1'—C14'—H141' | 106.96 |
P1—C11—C10 | 112.7 (3) | C13'—C14'—C15' | 112.5 (3) |
P1—C11—H111 | 109.31 | C13'—C14'—H141' | 109.44 |
C10—C11—H111 | 104.73 | C15'—C14'—H141' | 103.44 |
H121—C12—H122 | 109.47 | C14'—C15'—H151' | 109.47 |
H121—C12—H123 | 109.47 | C14'—C15'—H152' | 109.47 |
H122—C12—H123 | 109.47 | C14'—C15'—H153' | 109.47 |
C14—C13—H131 | 109.47 | H151'—C15'—H152' | 109.47 |
C14—C13—H132 | 109.47 | H151'—C15'—H153' | 109.47 |
C14—C13—H133 | 109.47 | H152'—C15'—H153' | 109.47 |
H131—C13—H132 | 109.47 | C17'—C16'—H161' | 109.47 |
H131—C13—H133 | 109.47 | C17'—C16'—H162' | 109.47 |
H132—C13—H133 | 109.47 | C17'—C16'—H163' | 109.47 |
P1—C14—C13 | 109.5 (3) | H161'—C16'—H162' | 109.47 |
P1—C14—H141 | 109.49 | H161'—C16'—H163' | 109.47 |
C13—C14—H141 | 107.74 | H162'—C16'—H163' | 109.47 |
H151—C15—H152 | 109.47 | P2'—C17'—C16' | 110.4 (3) |
H151—C15—H153 | 109.47 | P2'—C17'—C18' | 112.4 (3) |
H152—C15—H153 | 109.47 | P2'—C17'—H171' | 106.67 |
C17—C16—H161 | 109.47 | C16'—C17'—C18' | 109.1 (4) |
C17—C16—H162 | 109.47 | C16'—C17'—H171' | 110.14 |
C17—C16—H163 | 109.47 | C18'—C17'—H171' | 108.05 |
H161—C16—H162 | 109.47 | C17'—C18'—H181' | 109.47 |
H161—C16—H163 | 109.47 | C17'—C18'—H182' | 109.47 |
H162—C16—H163 | 109.47 | C17'—C18'—H183' | 109.47 |
P2—C17—C16 | 110.1 (3) | H181'—C18'—H182' | 109.47 |
P2—C17—C18 | 111.3 (3) | H181'—C18'—H183' | 109.47 |
P2—C17—H171 | 108.37 | H182'—C18'—H183' | 109.47 |
C16—C17—C18 | 111.2 (4) | C20'—C19'—H191' | 109.47 |
C16—C17—H171 | 108.52 | C20'—C19'—H192' | 109.47 |
C18—C17—H171 | 107.26 | C20'—C19'—H193' | 109.47 |
C17—C18—H181 | 109.47 | H191'—C19'—H192' | 109.47 |
C17—C18—H182 | 109.47 | H191'—C19'—H193' | 109.47 |
C17—C18—H183 | 109.47 | H192'—C19'—H193' | 109.47 |
H181—C18—H182 | 109.47 | P2'—C20'—C19' | 110.9 (3) |
H181—C18—H183 | 109.47 | P2'—C20'—C21' | 111.3 (3) |
H182—C18—H183 | 109.47 | P2'—C20'—H201' | 107.94 |
C20—C19—H191 | 109.47 | C19'—C20'—C21' | 111.5 (4) |
C20—C19—H192 | 109.47 | C19'—C20'—H201' | 107.75 |
C20—C19—H193 | 109.47 | C21'—C20'—H201' | 107.22 |
H191—C19—H192 | 109.47 | C20'—C21'—H211' | 109.47 |
H191—C19—H193 | 109.47 | C20'—C21'—H212' | 109.47 |
H192—C19—H193 | 109.47 | C20'—C21'—H213' | 109.47 |
P2—C20—C19 | 108.8 (3) | H211'—C21'—H212' | 109.47 |
P2—C20—C21 | 114.4 (3) | H211'—C21'—H213' | 109.47 |
P2—C20—H201 | 106.91 | H212'—C21'—H213' | 109.47 |
C19—C20—C21 | 110.5 (4) | Fe1'—C22'—O1' | 171.8 (4) |
C19—C20—H201 | 111.11 | Fe1'—C23'—O2' | 174.1 (4) |
C21—C20—H201 | 105.03 | P3'—Fe2'—P4' | 164.48 (6) |
C20—C21—H211 | 109.47 | P3'—Fe2'—N4' | 83.40 (8) |
C20—C21—H212 | 109.47 | P3'—Fe2'—C45' | 96.51 (11) |
C20—C21—H213 | 109.47 | P3'—Fe2'—C46' | 92.38 (11) |
H211—C21—H212 | 109.47 | P4'—Fe2'—N4' | 82.78 (8) |
H211—C21—H213 | 109.47 | P4'—Fe2'—C45' | 95.32 (11) |
H212—C21—H213 | 109.47 | P4'—Fe2'—C46' | 91.37 (11) |
Fe1—C22—O1 | 171.9 (5) | N4'—Fe2'—C45' | 112.8 (2) |
Fe1—C23—O2 | 175.7 (5) | N4'—Fe2'—C46' | 131.0 (3) |
P3—Fe2—P4 | 164.12 (6) | C45'—Fe2'—C46' | 116.2 (3) |
P3—Fe2—N4 | 82.77 (8) | Fe2'—P3'—N5' | 101.98 (12) |
P3—Fe2—C45 | 95.57 (11) | Fe2'—P3'—C34' | 121.86 (13) |
P3—Fe2—C46 | 92.80 (12) | Fe2'—P3'—C37' | 121.81 (16) |
P4—Fe2—N4 | 82.75 (8) | N5'—P3'—C34' | 102.49 (18) |
P4—Fe2—C45 | 95.92 (11) | N5'—P3'—C37' | 100.9 (2) |
P4—Fe2—C46 | 91.63 (11) | C34'—P3'—C37' | 103.9 (2) |
N4—Fe2—C45 | 112.3 (2) | Fe2'—P4'—N6' | 102.90 (13) |
N4—Fe2—C46 | 130.4 (2) | Fe2'—P4'—C40' | 121.78 (16) |
C45—Fe2—C46 | 117.3 (3) | Fe2'—P4'—C43' | 118.12 (14) |
Fe2—P3—N5 | 102.42 (13) | N6'—P4'—C40' | 103.1 (2) |
Fe2—P3—C34 | 122.76 (14) | N6'—P4'—C43' | 103.8 (2) |
Fe2—P3—C37 | 123.20 (16) | C40'—P4'—C43' | 104.6 (2) |
N5—P3—C34 | 103.18 (18) | P3'—N5'—C24' | 118.8 (3) |
N5—P3—C37 | 101.4 (2) | P3'—N5'—C29' | 122.8 (3) |
C34—P3—C37 | 100.3 (2) | C24'—N5'—C29' | 118.3 (3) |
Fe2—P4—N6 | 102.82 (13) | Fe2'—N4'—C24' | 122.4 (3) |
Fe2—P4—C40 | 122.44 (16) | Fe2'—N4'—C28' | 123.2 (3) |
Fe2—P4—C43 | 120.19 (15) | C24'—N4'—C28' | 114.1 (4) |
N6—P4—C40 | 102.8 (2) | P4'—N6'—C28' | 117.7 (3) |
N6—P4—C43 | 105.5 (2) | P4'—N6'—C31' | 124.7 (3) |
C40—P4—C43 | 100.8 (2) | C28'—N6'—C31' | 117.4 (4) |
P3—N5—C24 | 116.5 (3) | N5'—C24'—N4' | 112.9 (4) |
P3—N5—C29 | 122.4 (3) | N5'—C24'—C25' | 122.7 (4) |
C24—N5—C29 | 121.1 (4) | N4'—C24'—C25' | 124.4 (4) |
Fe2—N4—C24 | 118.6 (3) | C24'—C25'—C26' | 119.2 (4) |
Fe2—N4—C28 | 118.5 (3) | C24'—C25'—H251' | 120.41 |
C24—N4—C28 | 122.3 (4) | C26'—C25'—H251' | 120.41 |
P4—N6—C28 | 116.3 (3) | C25'—C26'—C27' | 118.3 (5) |
P4—N6—C31 | 123.7 (3) | C25'—C26'—H261' | 120.84 |
C28—N6—C31 | 119.9 (4) | C27'—C26'—H261' | 120.84 |
N5—C24—N4 | 119.1 (4) | C26'—C27'—C28' | 120.1 (4) |
N5—C24—C25 | 120.5 (4) | C26'—C27'—H271' | 119.93 |
N4—C24—C25 | 120.4 (4) | C28'—C27'—H271' | 119.93 |
C24—C25—C26 | 117.1 (4) | N4'—C28'—N6' | 113.0 (4) |
C24—C25—H251 | 121.44 | N4'—C28'—C27' | 123.8 (4) |
C26—C25—H251 | 121.44 | N6'—C28'—C27' | 123.2 (4) |
C25—C26—C27 | 122.5 (5) | N5'—C29'—C30' | 115.7 (4) |
C25—C26—H261 | 118.75 | N5'—C29'—H291' | 109.47 |
C27—C26—H261 | 118.75 | N5'—C29'—H292' | 109.47 |
C26—C27—C28 | 117.5 (4) | C30'—C29'—H291' | 109.47 |
C26—C27—H271 | 121.27 | C30'—C29'—H292' | 109.47 |
C28—C27—H271 | 121.27 | H291'—C29'—H292' | 102.37 |
N4—C28—N6 | 119.0 (4) | C29'—C30'—H301' | 109.47 |
N4—C28—C27 | 120.2 (4) | C29'—C30'—H302' | 109.47 |
N6—C28—C27 | 120.9 (4) | C29'—C30'—H303' | 109.47 |
N5—C29—C30 | 113.0 (4) | H301'—C30'—H302' | 109.47 |
N5—C29—H291 | 109.47 | H301'—C30'—H303' | 109.47 |
N5—C29—H292 | 109.47 | H302'—C30'—H303' | 109.47 |
C30—C29—H291 | 109.47 | N6'—C31'—C32' | 116.4 (4) |
C30—C29—H292 | 109.47 | N6'—C31'—H311' | 109.47 |
H291—C29—H292 | 105.67 | N6'—C31'—H313' | 109.47 |
C29—C30—H301 | 109.47 | C32'—C31'—H311' | 109.47 |
C29—C30—H302 | 109.47 | C32'—C31'—H313' | 109.47 |
C29—C30—H303 | 109.47 | H311'—C31'—H313' | 101.49 |
H301—C30—H302 | 109.47 | C31'—C32'—H321' | 109.47 |
H301—C30—H303 | 109.47 | C31'—C32'—H322' | 109.47 |
H302—C30—H303 | 109.47 | C31'—C32'—H323' | 109.47 |
N6—C31—C32 | 113.0 (4) | H321'—C32'—H322' | 109.47 |
N6—C31—H311 | 109.47 | H321'—C32'—H323' | 109.47 |
N6—C31—H313 | 109.47 | H322'—C32'—H323' | 109.47 |
C32—C31—H311 | 109.47 | C34'—C33'—H331' | 109.47 |
C32—C31—H313 | 109.47 | C34'—C33'—H332' | 109.47 |
H311—C31—H313 | 105.73 | C34'—C33'—H333' | 109.47 |
C31—C32—H321 | 109.47 | H331'—C33'—H332' | 109.47 |
C31—C32—H322 | 109.47 | H331'—C33'—H333' | 109.47 |
C31—C32—H323 | 109.47 | H332'—C33'—H333' | 109.47 |
H321—C32—H322 | 109.47 | P3'—C34'—C33' | 112.8 (3) |
H321—C32—H323 | 109.47 | P3'—C34'—C35' | 112.1 (3) |
H322—C32—H323 | 109.47 | P3'—C34'—H341' | 105.72 |
C34—C33—H331 | 109.47 | C33'—C34'—C35' | 110.8 (4) |
C34—C33—H332 | 109.47 | C33'—C34'—H341' | 107.15 |
C34—C33—H333 | 109.47 | C35'—C34'—H341' | 107.96 |
H331—C33—H332 | 109.47 | C34'—C35'—H351' | 109.47 |
H331—C33—H333 | 109.47 | C34'—C35'—H352' | 109.47 |
H332—C33—H333 | 109.47 | C34'—C35'—H353' | 109.47 |
P3—C34—C33 | 112.0 (3) | H351'—C35'—H352' | 109.47 |
P3—C34—C35 | 110.3 (3) | H351'—C35'—H353' | 109.47 |
P3—C34—H341 | 106.51 | H352'—C35'—H353' | 109.47 |
C33—C34—C35 | 107.5 (4) | C37'—C36'—H361' | 109.47 |
C33—C34—H341 | 109.38 | C37'—C36'—H362' | 109.47 |
C35—C34—H341 | 111.09 | C37'—C36'—H363' | 109.47 |
C34—C35—H351 | 109.47 | H361'—C36'—H362' | 109.47 |
C34—C35—H352 | 109.47 | H361'—C36'—H363' | 109.47 |
C34—C35—H353 | 109.47 | H362'—C36'—H363' | 109.47 |
H351—C35—H352 | 109.47 | P3'—C37'—C36' | 111.2 (3) |
H351—C35—H353 | 109.47 | P3'—C37'—C38' | 113.6 (3) |
H352—C35—H353 | 109.47 | P3'—C37'—H371' | 106.07 |
H361—C36—H362 | 109.47 | C36'—C37'—C38' | 111.6 (4) |
H361—C36—H363 | 109.47 | C36'—C37'—H371' | 108.36 |
H362—C36—H363 | 109.47 | C38'—C37'—H371' | 105.57 |
P3—C37—C38 | 117.1 (4) | C37'—C38'—H381' | 109.47 |
P3—C37—H371 | 105.03 | C37'—C38'—H382' | 109.47 |
C38—C37—H371 | 102.34 | C37'—C38'—H383' | 109.47 |
C37—C38—H381 | 109.47 | H381'—C38'—H382' | 109.47 |
C37—C38—H382 | 109.47 | H381'—C38'—H383' | 109.47 |
C37—C38—H383 | 109.47 | H382'—C38'—H383' | 109.47 |
H381—C38—H382 | 109.47 | C40'—C39'—H391' | 109.47 |
H381—C38—H383 | 109.47 | C40'—C39'—H392' | 109.47 |
H382—C38—H383 | 109.47 | C40'—C39'—H393' | 109.47 |
C40—C39—H391 | 109.47 | H391'—C39'—H392' | 109.47 |
C40—C39—H392 | 109.47 | H391'—C39'—H393' | 109.47 |
C40—C39—H393 | 109.47 | H392'—C39'—H393' | 109.47 |
H391—C39—H392 | 109.47 | P4'—C40'—C39' | 113.1 (3) |
H391—C39—H393 | 109.47 | P4'—C40'—C41' | 109.7 (3) |
H392—C39—H393 | 109.47 | P4'—C40'—H401' | 108.25 |
P4—C40—C39 | 110.8 (3) | C39'—C40'—C41' | 113.5 (4) |
P4—C40—C41 | 110.8 (3) | C39'—C40'—H401' | 103.98 |
P4—C40—H401 | 108.1 | C41'—C40'—H401' | 107.85 |
C39—C40—C41 | 110.8 (4) | C40'—C41'—H411' | 109.47 |
C39—C40—H401 | 108.1 | C40'—C41'—H412' | 109.47 |
C41—C40—H401 | 108.06 | C40'—C41'—H413' | 109.47 |
C40—C41—H411 | 109.47 | H411'—C41'—H412' | 109.47 |
C40—C41—H412 | 109.47 | H411'—C41'—H413' | 109.47 |
C40—C41—H413 | 109.47 | H412'—C41'—H413' | 109.47 |
H411—C41—H412 | 109.47 | C43'—C42'—H421' | 109.47 |
H411—C41—H413 | 109.47 | C43'—C42'—H422' | 109.47 |
H412—C41—H413 | 109.47 | C43'—C42'—H423' | 109.47 |
C43—C42—H421 | 109.47 | H421'—C42'—H422' | 109.47 |
C43—C42—H422 | 109.47 | H421'—C42'—H423' | 109.47 |
C43—C42—H423 | 109.47 | H422'—C42'—H423' | 109.47 |
H421—C42—H422 | 109.47 | P4'—C43'—C42' | 110.4 (3) |
H421—C42—H423 | 109.47 | P4'—C43'—C44' | 119.8 (3) |
H422—C42—H423 | 109.47 | P4'—C43'—H431' | 102.5 |
P4—C43—C42 | 109.6 (3) | P4'—C43'—C44b' | 115.2 (7) |
P4—C43—C44 | 121.6 (4) | P4'—C43'—H431b' | 109 |
P4—C43—H431 | 100.81 | C42'—C43'—C44' | 113.4 (4) |
P4—C43—C44b | 121.9 (5) | C42'—C43'—H431' | 110.76 |
P4—C43—H431b | 101.77 | C42'—C43'—C44b' | 119.0 (7) |
C42—C43—C44 | 110.9 (4) | C42'—C43'—H431b' | 103.93 |
C42—C43—H431 | 114.06 | C44'—C43'—H431' | 98.46 |
C42—C43—C44b | 114.5 (6) | C44'—C43'—C44b' | 75.5 (7) |
C42—C43—H431b | 112.11 | C44'—C43'—H431b' | 21.87 |
C44—C43—H431 | 99.09 | H431'—C43'—C44b' | 22.98 |
C44—C43—C44b | 74.5 (5) | H431'—C43'—H431b' | 120.24 |
C44—C43—H431b | 23.04 | C44b'—C43'—H431b' | 97.35 |
H431—C43—C44b | 26.38 | C43'—C44'—H441' | 109.47 |
H431—C43—H431b | 116.83 | C43'—C44'—H442' | 109.47 |
C44b—C43—H431b | 94.93 | C43'—C44'—H443' | 109.47 |
C43—C44—H441 | 109.47 | C43'—C44'—H431b' | 30.72 |
C43—C44—H442 | 109.47 | H441'—C44'—H442' | 109.47 |
C43—C44—H443 | 109.47 | H441'—C44'—H443' | 109.47 |
C43—C44—H431b | 31.77 | H441'—C44'—H431b' | 123.2 |
H441—C44—H442 | 109.47 | H442'—C44'—H443' | 109.47 |
H441—C44—H443 | 109.47 | H442'—C44'—H431b' | 78.78 |
H441—C44—H431b | 137.99 | H443'—C44'—H431b' | 120.44 |
H442—C44—H443 | 109.47 | Fe2'—C45'—O3' | 173.2 (5) |
H442—C44—H431b | 102.47 | Fe2'—C46'—O4' | 176.8 (5) |
H443—C44—H431b | 83.76 | C43—H431—C44b | 116.83 |
Fe2—C45—O3 | 171.6 (6) | C43'—H431'—C44b' | 127.79 |
Fe2—C46—O4 | 174.0 (5) | C43—C44b—H431 | 36.79 |
P1'—Fe1'—P2' | 160.50 (7) | C43—C44b—H441b | 109.47 |
P1'—Fe1'—N1' | 82.38 (10) | C43—C44b—H442b | 109.47 |
P1'—Fe1'—C22' | 97.82 (14) | C43—C44b—H443b | 109.47 |
P1'—Fe1'—C23' | 90.34 (16) | H431—C44b—H441b | 117.97 |
P2'—Fe1'—N1' | 82.15 (10) | H431—C44b—H442b | 128.5 |
P2'—Fe1'—C22' | 97.90 (14) | H431—C44b—H443b | 73.1 |
P2'—Fe1'—C23' | 92.68 (16) | H441b—C44b—H442b | 109.47 |
N1'—Fe1'—C22' | 106.51 (17) | H441b—C44b—H443b | 109.47 |
N1'—Fe1'—C23' | 136.30 (19) | H442b—C44b—H443b | 109.47 |
C22'—Fe1'—C23' | 117.2 (2) | C43'—C44b'—H431' | 29.23 |
Fe1'—P1'—N2' | 102.34 (12) | C43'—C44b'—H441b' | 109.47 |
Fe1'—P1'—C11' | 121.21 (15) | C43'—C44b'—H442b' | 109.47 |
Fe1'—P1'—C14' | 123.00 (15) | C43'—C44b'—H443b' | 109.47 |
N2'—P1'—C11' | 105.80 (17) | H431'—C44b'—H441b' | 85.35 |
N2'—P1'—C14' | 99.83 (19) | H431'—C44b'—H442b' | 104 |
C11'—P1'—C14' | 101.52 (19) | H431'—C44b'—H443b' | 135.38 |
Fe1'—P2'—N3' | 102.44 (13) | H441b'—C44b'—H442b' | 109.47 |
Fe1'—P2'—C17' | 122.79 (15) | H441b'—C44b'—H443b' | 109.47 |
Fe1'—P2'—C20' | 122.31 (14) | H442b'—C44b'—H443b' | 109.47 |
N3'—P2'—C17' | 102.20 (18) | C43—H431b—C44 | 125.19 |
N3'—P2'—C20' | 99.08 (18) | C43'—H431b'—C44' | 127.4 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C15—H151···C12 | 0.96 | 2.46 | 3.245 (7) | 139.30 |
C35—H353···O3 | 0.96 | 2.49 | 3.362 (6) | 151.59 |
C41—H411···C44b | 0.96 | 2.49 | 3.267 (12) | 137.55 |
C43—H431···C44b | 0.96 | 0.71 | 1.430 (12) | 116.83 |
C44b—H431···P4 | 0.71 | 2.23 | 2.868 (11) | 149.59 |
C44b—H431···C42 | 0.71 | 2.15 | 2.522 (12) | 114.06 |
C44b—H431···C43 | 0.71 | 0.96 | 1.430 (12) | 116.83 |
C41′—H411′···C44b′ | 0.96 | 2.33 | 3.158 (18) | 143.58 |
C43′—H431′···C44b′ | 0.96 | 0.77 | 1.554 (17) | 127.79 |
C44b′—H431′···P4′ | 0.77 | 2.27 | 2.890 (17) | 138.06 |
C44b′—H431′···C42′ | 0.77 | 2.03 | 2.611 (17) | 133.05 |
C44b′—H431′···C43′ | 0.77 | 0.96 | 1.554 (17) | 127.79 |
C44b′—H442b′···C41′ | 0.96 | 2.30 | 3.158 (18) | 148.03 |
C43—H431b···C44 | 0.96 | 0.71 | 1.490 (7) | 125.19 |
C44—H431b···P4 | 0.71 | 2.24 | 2.913 (7) | 156.71 |
C44—H431b···C42 | 0.71 | 2.12 | 2.519 (8) | 115.97 |
C44—H431b···C43 | 0.71 | 0.96 | 1.490 (7) | 125.19 |
C43′—H431b′···C44′ | 0.96 | 0.70 | 1.493 (6) | 127.40 |
C44′—H431b′···P4′ | 0.70 | 2.36 | 2.909 (5) | 137.02 |
C44′—H431b′···C42′ | 0.70 | 1.95 | 2.482 (7) | 133.84 |
C44′—H431b′···C43′ | 0.70 | 0.96 | 1.493 (6) | 127.40 |
Crystal data top
C14H25Br2FeN3OP2 | F(000) = 1056 |
Mr = 529 | Dx = 1.768 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71069 Å |
Hall symbol: -P 2yabc | Cell parameters from 5440 reflections |
a = 9.2939 (16) Å | θ = 2.3–27.1° |
b = 11.7224 (18) Å | µ = 4.95 mm−1 |
c = 18.307 (3) Å | T = 100 K |
β = 94.999 (10)° | Tabular, translucent blue |
V = 1986.9 (6) Å3 | 0.27 × 0.20 × 0.04 mm |
Z = 4 | |
Data collection top
Bruker KAPPA APEX II CCD diffractometer | 12579 independent reflections |
Radiation source: X-ray tube | 6782 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.091 |
ω– and φ–scans | θmax = 27.6°, θmin = 2.1° |
Absorption correction: multi-scan TWINABS | h = −11→12 |
Tmin = 0.32, Tmax = 0.82 | k = −14→14 |
13162 measured reflections | l = −23→23 |
Refinement top
Refinement on F | 120 constraints |
R[F2 > 2σ(F2)] = 0.090 | H-atom parameters constrained |
wR(F2) = 0.128 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
S = 1.61 | (Δ/σ)max = 0.036 |
12579 reflections | Δρmax = 1.93 e Å−3 |
99 parameters | Δρmin = −2.09 e Å−3 |
0 restraints | |
Crystal data top
C14H25Br2FeN3OP2 | V = 1986.9 (6) Å3 |
Mr = 529 | Z = 4 |
Monoclinic, P21/n | Mo Kα radiation |
a = 9.2939 (16) Å | µ = 4.95 mm−1 |
b = 11.7224 (18) Å | T = 100 K |
c = 18.307 (3) Å | 0.27 × 0.20 × 0.04 mm |
β = 94.999 (10)° | |
Data collection top
Bruker KAPPA APEX II CCD diffractometer | 12579 independent reflections |
Absorption correction: multi-scan TWINABS | 6782 reflections with I > 3σ(I) |
Tmin = 0.32, Tmax = 0.82 | Rint = 0.091 |
13162 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.090 | 0 restraints |
wR(F2) = 0.128 | H-atom parameters constrained |
S = 1.61 | Δρmax = 1.93 e Å−3 |
12579 reflections | Δρmin = −2.09 e Å−3 |
99 parameters | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe1 | 0.9744 (2) | 0.22645 (14) | 0.14457 (8) | 0.0141 (6) | |
Br1 | 0.75736 (19) | 0.34704 (10) | 0.14646 (7) | 0.0289 (4) | |
Br1' | 1.18939 (18) | 0.10544 (10) | 0.13766 (7) | 0.0289 (4) | |
P1 | 1.1156 (5) | 0.3834 (3) | 0.15824 (16) | 0.0204 (9) | |
P1' | 0.8470 (5) | 0.0687 (3) | 0.16106 (16) | 0.0204 (9) | |
N1 | 1.0079 (12) | 0.2210 (7) | 0.2544 (4) | 0.018 (2)* | |
N2 | 1.1307 (10) | 0.3938 (6) | 0.2500 (3) | 0.0173 (16)* | |
N2' | 0.8808 (10) | 0.0533 (6) | 0.2523 (3) | 0.0173 (16)* | |
C1 | 1.0881 (14) | 0.3095 (8) | 0.2949 (5) | 0.0147 (18)* | |
C2 | 1.1103 (13) | 0.3040 (8) | 0.3673 (5) | 0.0140 (19)* | |
C3 | 1.0718 (14) | 0.2179 (8) | 0.4101 (5) | 0.017 (3)* | |
C2' | 0.9870 (12) | 0.1283 (8) | 0.3715 (5) | 0.0140 (19)* | |
C1' | 0.9677 (14) | 0.1335 (8) | 0.2949 (5) | 0.0147 (18)* | |
C4 | 1.0476 (14) | 0.5248 (8) | 0.1266 (5) | 0.026 (2)* | |
C5 | 1.1067 (14) | 0.6228 (8) | 0.1704 (5) | 0.028 (2)* | |
C6 | 1.2930 (13) | 0.3758 (8) | 0.1363 (5) | 0.0160 (19)* | |
C7 | 1.3222 (13) | 0.3745 (10) | 0.0548 (5) | 0.034 (2)* | |
C4' | 0.8836 (14) | −0.0659 (8) | 0.1168 (5) | 0.026 (2)* | |
C5' | 0.8092 (13) | −0.1682 (8) | 0.1394 (5) | 0.028 (2)* | |
C6' | 0.6546 (13) | 0.0739 (8) | 0.1507 (5) | 0.0160 (19)* | |
C7' | 0.5722 (14) | 0.0829 (10) | 0.0737 (5) | 0.034 (2)* | |
C8 | 0.9503 (15) | 0.2260 (9) | 0.0487 (5) | 0.0203 (16)* | |
O1 | 0.9312 (9) | 0.2299 (6) | −0.0123 (3) | 0.0203 (16)* | |
H1c2 | 1.15859 | 0.367632 | 0.391556 | 0.0168* | |
H1c3 | 1.098095 | 0.215575 | 0.461933 | 0.0209* | |
H1c4 | 1.065536 | 0.535372 | 0.076198 | 0.0308* | |
H2c4 | 0.944058 | 0.52564 | 0.124966 | 0.0308* | |
H1c5 | 1.076545 | 0.692628 | 0.146325 | 0.0339* | |
H2c5 | 1.07179 | 0.620537 | 0.218198 | 0.0339* | |
H3c5 | 1.210313 | 0.618815 | 0.175095 | 0.0339* | |
H1c6 | 1.348239 | 0.435705 | 0.161062 | 0.0192* | |
H2c6 | 1.339764 | 0.311667 | 0.160728 | 0.0192* | |
H1c7 | 1.423601 | 0.364092 | 0.050711 | 0.0402* | |
H2c7 | 1.269407 | 0.313063 | 0.030322 | 0.0402* | |
H3c7 | 1.291655 | 0.445625 | 0.032451 | 0.0402* | |
H1c4' | 0.86764 | −0.057199 | 0.064587 | 0.0308* | |
H2c4' | 0.985806 | −0.079393 | 0.120571 | 0.0308* | |
H1c5' | 0.845594 | −0.233726 | 0.115544 | 0.0339* | |
H2c5' | 0.825761 | −0.177198 | 0.19162 | 0.0339* | |
H3c5' | 0.707449 | −0.160869 | 0.126027 | 0.0339* | |
H1c6' | 0.616253 | 0.011594 | 0.176977 | 0.0192* | |
H2c6' | 0.621218 | 0.132249 | 0.181852 | 0.0192* | |
H1c7' | 0.47041 | 0.087975 | 0.078522 | 0.0402* | |
H2c7' | 0.603553 | 0.149766 | 0.049293 | 0.0402* | |
H3c7' | 0.591655 | 0.016463 | 0.045465 | 0.0402* | |
H1c2' | 0.945551 | 0.067592 | 0.397902 | 0.0168* | |
H1n2 | 1.167412 | 0.455861 | 0.26989 | 0.0207* | |
H1n2' | 0.844519 | −0.004721 | 0.273897 | 0.0207* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.0028 (11) | 0.0084 (9) | 0.0314 (8) | −0.0001 (8) | 0.0035 (10) | 0.0002 (7) |
Br1 | 0.0308 (8) | 0.0116 (6) | 0.0448 (5) | 0.0019 (6) | 0.0051 (6) | −0.0027 (4) |
Br1' | 0.0304 (9) | 0.0116 (6) | 0.0448 (5) | 0.0024 (6) | 0.0027 (6) | 0.0027 (4) |
P1 | 0.022 (2) | 0.0036 (14) | 0.0358 (13) | 0.0016 (14) | 0.0059 (13) | −0.0015 (9) |
P1' | 0.022 (2) | 0.0036 (14) | 0.0358 (13) | 0.0019 (14) | 0.0003 (13) | 0.0015 (9) |
Geometric parameters (Å, º) top
Fe1—Br1 | 2.465 (3) | C2'—C1' | 1.400 (12) |
Fe1—Br1' | 2.463 (3) | C2'—H1c2' | 0.96 |
Fe1—P1 | 2.262 (4) | C4—C5 | 1.479 (14) |
Fe1—P1' | 2.230 (4) | C4—H1c4 | 0.96 |
Fe1—N1 | 2.008 (7) | C4—H2c4 | 0.96 |
Fe1—C8 | 1.749 (9) | C5—H1c5 | 0.96 |
Br1—N1 | 3.272 (9) | C5—H2c5 | 0.96 |
Br1—N2'i | 3.369 (8) | C5—H3c5 | 0.96 |
Br1'—N1 | 3.143 (9) | C6—C7 | 1.540 (13) |
Br1'—N2ii | 3.547 (7) | C6—H1c6 | 0.96 |
P1—N2 | 1.677 (7) | C6—H2c6 | 0.96 |
P1—C4 | 1.849 (10) | C7—H1c7 | 0.96 |
P1—C6 | 1.733 (13) | C7—H2c7 | 0.96 |
P1'—N2' | 1.681 (7) | C7—H3c7 | 0.96 |
P1'—C4' | 1.819 (10) | C4'—C5' | 1.462 (15) |
P1'—C6' | 1.783 (13) | C4'—H1c4' | 0.96 |
N1—C1 | 1.444 (13) | C4'—H2c4' | 0.96 |
N1—C1' | 1.338 (13) | C5'—H1c5' | 0.96 |
N2—C1 | 1.366 (12) | C5'—H2c5' | 0.96 |
N2—H1n2 | 0.87 | C5'—H3c5' | 0.96 |
N2'—C1' | 1.426 (13) | C6'—C7' | 1.548 (13) |
N2'—H1n2' | 0.87 | C6'—H1c6' | 0.96 |
C1—C2 | 1.324 (12) | C6'—H2c6' | 0.96 |
C2—C3 | 1.345 (14) | C7'—H1c7' | 0.96 |
C2—H1c2 | 0.96 | C7'—H2c7' | 0.96 |
C3—C2' | 1.457 (14) | C7'—H3c7' | 0.96 |
C3—H1c3 | 0.96 | C8—O1 | 1.117 (11) |
| | | |
Br1—Fe1—Br1' | 177.85 (8) | C3—C2—H1c2 | 116.8 |
Br1—Fe1—P1 | 89.98 (13) | C2—C3—C2' | 114.7 (8) |
Br1—Fe1—P1' | 91.67 (14) | C2—C3—H1c3 | 122.64 |
Br1—Fe1—N1 | 93.4 (3) | C2'—C3—H1c3 | 122.64 |
Br1—Fe1—C8 | 89.0 (4) | C3—C2'—C1' | 118.1 (9) |
Br1'—Fe1—P1 | 90.48 (14) | C3—C2'—H1c2' | 120.94 |
Br1'—Fe1—P1' | 88.39 (13) | C1'—C2'—H1c2' | 120.94 |
Br1'—Fe1—N1 | 88.7 (3) | N1—C1'—N2' | 112.0 (8) |
Br1'—Fe1—C8 | 88.9 (4) | N1—C1'—C2' | 124.8 (9) |
P1—Fe1—P1' | 165.80 (13) | N2'—C1'—C2' | 122.5 (9) |
P1—Fe1—N1 | 82.9 (3) | P1—C4—C5 | 115.2 (7) |
P1—Fe1—C8 | 97.8 (4) | P1—C4—H1c4 | 109.47 |
P1'—Fe1—N1 | 82.9 (3) | P1—C4—H2c4 | 109.47 |
P1'—Fe1—C8 | 96.3 (4) | C5—C4—H1c4 | 109.47 |
N1—Fe1—C8 | 177.5 (5) | C5—C4—H2c4 | 109.47 |
Fe1—Br1—N1 | 37.78 (15) | H1c4—C4—H2c4 | 103.08 |
Fe1—Br1—N2'i | 140.42 (15) | C4—C5—H1c5 | 109.47 |
N1—Br1—N2'i | 106.09 (19) | C4—C5—H2c5 | 109.47 |
Fe1—Br1'—N1 | 39.71 (16) | C4—C5—H3c5 | 109.47 |
Fe1—Br1'—N2ii | 135.77 (15) | H1c5—C5—H2c5 | 109.47 |
N1—Br1'—N2ii | 99.26 (19) | H1c5—C5—H3c5 | 109.47 |
Fe1—P1—N2 | 99.6 (3) | H2c5—C5—H3c5 | 109.47 |
Fe1—P1—C4 | 121.0 (4) | P1—C6—C7 | 118.5 (8) |
Fe1—P1—C6 | 119.2 (4) | P1—C6—H1c6 | 109.47 |
N2—P1—C4 | 104.2 (4) | P1—C6—H2c6 | 109.47 |
N2—P1—C6 | 103.8 (5) | C7—C6—H1c6 | 109.47 |
C4—P1—C6 | 106.2 (5) | C7—C6—H2c6 | 109.47 |
Fe1—P1'—N2' | 99.7 (3) | H1c6—C6—H2c6 | 98.65 |
Fe1—P1'—C4' | 122.5 (4) | C6—C7—H1c7 | 109.47 |
Fe1—P1'—C6' | 119.8 (3) | C6—C7—H2c7 | 109.47 |
N2'—P1'—C4' | 108.9 (4) | C6—C7—H3c7 | 109.47 |
N2'—P1'—C6' | 102.0 (5) | H1c7—C7—H2c7 | 109.47 |
C4'—P1'—C6' | 101.9 (5) | H1c7—C7—H3c7 | 109.47 |
Fe1—N1—Br1 | 48.8 (2) | H2c7—C7—H3c7 | 109.47 |
Fe1—N1—Br1' | 51.6 (2) | P1'—C4'—C5' | 118.3 (8) |
Fe1—N1—C1 | 121.3 (6) | P1'—C4'—H1c4' | 109.47 |
Fe1—N1—C1' | 123.5 (7) | P1'—C4'—H2c4' | 109.47 |
Br1—N1—Br1' | 100.4 (2) | C5'—C4'—H1c4' | 109.47 |
Br1—N1—C1 | 107.1 (6) | C5'—C4'—H2c4' | 109.47 |
Br1—N1—C1' | 117.6 (8) | H1c4'—C4'—H2c4' | 98.89 |
Br1'—N1—C1 | 112.0 (7) | C4'—C5'—H1c5' | 109.47 |
Br1'—N1—C1' | 103.8 (6) | C4'—C5'—H2c5' | 109.47 |
C1—N1—C1' | 115.0 (7) | C4'—C5'—H3c5' | 109.47 |
Br1'iii—N2—P1 | 128.7 (4) | H1c5'—C5'—H2c5' | 109.47 |
Br1'iii—N2—C1 | 107.7 (5) | H1c5'—C5'—H3c5' | 109.47 |
Br1'iii—N2—H1n2 | 12.66 | H2c5'—C5'—H3c5' | 109.47 |
P1—N2—C1 | 123.2 (6) | P1'—C6'—C7' | 120.8 (8) |
P1—N2—H1n2 | 118.42 | P1'—C6'—H1c6' | 109.47 |
C1—N2—H1n2 | 118.42 | P1'—C6'—H2c6' | 109.47 |
Br1iv—N2'—P1' | 125.2 (4) | C7'—C6'—H1c6' | 109.47 |
Br1iv—N2'—C1' | 113.4 (5) | C7'—C6'—H2c6' | 109.47 |
Br1iv—N2'—H1n2' | 6.57 | H1c6'—C6'—H2c6' | 95.19 |
P1'—N2'—C1' | 121.3 (6) | C6'—C7'—H1c7' | 109.47 |
P1'—N2'—H1n2' | 119.33 | C6'—C7'—H2c7' | 109.47 |
C1'—N2'—H1n2' | 119.33 | C6'—C7'—H3c7' | 109.47 |
N1—C1—N2 | 112.0 (7) | H1c7'—C7'—H2c7' | 109.47 |
N1—C1—C2 | 120.5 (9) | H1c7'—C7'—H3c7' | 109.47 |
N2—C1—C2 | 127.6 (9) | H2c7'—C7'—H3c7' | 109.47 |
C1—C2—C3 | 126.4 (9) | Fe1—C8—O1 | 176.9 (11) |
C1—C2—H1c2 | 116.8 | | |
Symmetry codes: (i) −x+3/2, y+1/2, −z+1/2; (ii) −x+5/2, y−1/2, −z+1/2; (iii) −x+5/2, y+1/2, −z+1/2; (iv) −x+3/2, y−1/2, −z+1/2. |
(Fe_PNP-TADDOL-iPr_Cl2)
top
Crystal data top
C46H55Cl2FeN3O5P2 | Z = 2 |
Mr = 918.7 | F(000) = 964 |
Triclinic, P1 | Dx = 1.311 Mg m−3 |
Hall symbol: P 1 | Mo Kα radiation, λ = 0.71069 Å |
a = 9.3389 (7) Å | Cell parameters from 9106 reflections |
b = 10.3155 (8) Å | θ = 2.3–25.8° |
c = 24.3224 (18) Å | µ = 0.55 mm−1 |
α = 96.277 (3)° | T = 100 K |
β = 92.393 (3)° | Plate, translucent yellow |
γ = 90.009 (2)° | 0.67 × 0.41 × 0.06 mm |
V = 2327.0 (3) Å3 | |
Data collection top
Bruker KAPPA APEX II CCD diffractometer | 39775 independent reflections |
Radiation source: X-ray tube | 35102 reflections with I > 3σ(I) |
Graphite monochromator | Rint = 0.066 |
ω– and φ–scans | θmax = 28.0°, θmin = 0.8° |
Absorption correction: multi-scan TWINABS | h = −12→12 |
Tmin = 0.23, Tmax = 0.85 | k = −12→12 |
40097 measured reflections | l = −32→32 |
Refinement top
Refinement on F | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.051 | Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2) |
wR(F2) = 0.070 | (Δ/σ)max = 0.048 |
S = 1.76 | Δρmax = 0.84 e Å−3 |
39775 reflections | Δρmin = −0.70 e Å−3 |
439 parameters | Absolute structure: 5587 of Friedel pairs used in the refinement |
0 restraints | Absolute structure parameter: 0.05 (2) |
527 constraints | |
Crystal data top
C46H55Cl2FeN3O5P2 | γ = 90.009 (2)° |
Mr = 918.7 | V = 2327.0 (3) Å3 |
Triclinic, P1 | Z = 2 |
a = 9.3389 (7) Å | Mo Kα radiation |
b = 10.3155 (8) Å | µ = 0.55 mm−1 |
c = 24.3224 (18) Å | T = 100 K |
α = 96.277 (3)° | 0.67 × 0.41 × 0.06 mm |
β = 92.393 (3)° | |
Data collection top
Bruker KAPPA APEX II CCD diffractometer | 39775 independent reflections |
Absorption correction: multi-scan TWINABS | 35102 reflections with I > 3σ(I) |
Tmin = 0.23, Tmax = 0.85 | Rint = 0.066 |
40097 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.051 | H-atom parameters constrained |
wR(F2) = 0.070 | Δρmax = 0.84 e Å−3 |
S = 1.76 | Δρmin = −0.70 e Å−3 |
39775 reflections | Absolute structure: 5587 of Friedel pairs used in the refinement |
439 parameters | Absolute structure parameter: 0.05 (2) |
0 restraints | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe1 | −0.524051 | 0.837572 | 0.414641 | 0.01355 (9) | |
Cl1 | −0.6549 (2) | 0.8137 (2) | 0.33478 (8) | 0.02670 (17) | |
Cl2 | −0.5217 (2) | 0.6875 (2) | 0.47380 (9) | 0.02682 (19) | |
P1 | −0.4882 (2) | 1.0515 (2) | 0.46065 (8) | 0.01661 (16) | |
P2 | −0.27212 (19) | 0.5643 (2) | 0.28631 (8) | 0.01528 (17) | |
O1 | −0.2950 (5) | 0.6448 (5) | 0.23528 (18) | 0.0184 (4)* | |
O2 | −0.4265 (4) | 0.4918 (4) | 0.28390 (16) | 0.0155 (3)* | |
O3 | −0.3101 (4) | 0.4141 (4) | 0.10871 (15) | 0.0178 (4)* | |
O4 | −0.5092 (4) | 0.3382 (4) | 0.14502 (17) | 0.0155 (4)* | |
N1 | −0.3075 (5) | 0.8642 (5) | 0.3990 (2) | 0.0131 (4)* | |
N2 | −0.3056 (5) | 1.0442 (5) | 0.45992 (19) | 0.0175 (4)* | |
N3 | −0.3235 (5) | 0.6813 (5) | 0.33445 (19) | 0.0165 (4)* | |
C1 | −0.2308 (7) | 0.9550 (7) | 0.4264 (3) | 0.0150 (5)* | |
C2 | −0.0786 (6) | 0.9675 (6) | 0.4235 (2) | 0.0159 (5)* | |
C3 | −0.0111 (6) | 0.8653 (6) | 0.3938 (2) | 0.0144 (5)* | |
C4 | −0.0901 (7) | 0.7698 (7) | 0.3611 (3) | 0.0159 (4)* | |
C5 | −0.2379 (6) | 0.7718 (6) | 0.3680 (2) | 0.0142 (5)* | |
C6 | −0.5481 (7) | 1.1848 (6) | 0.4202 (3) | 0.0212 (5)* | |
C7 | −0.4910 (6) | 1.3147 (6) | 0.4467 (2) | 0.0268 (7)* | |
C8 | −0.7032 (7) | 1.1785 (7) | 0.4030 (3) | 0.0307 (6)* | |
C9 | −0.5227 (6) | 1.0911 (6) | 0.5333 (2) | 0.0195 (5)* | |
C10 | −0.4313 (7) | 1.0130 (7) | 0.5699 (3) | 0.0296 (7)* | |
C11 | −0.6775 (6) | 1.0861 (5) | 0.5444 (2) | 0.0263 (6)* | |
C12 | −0.2500 (6) | 0.6041 (6) | 0.1782 (2) | 0.0161 (5)* | |
C13 | −0.3065 (6) | 0.4551 (6) | 0.1666 (2) | 0.0155 (5)* | |
C14 | −0.4532 (6) | 0.4206 (6) | 0.1881 (2) | 0.0153 (5)* | |
C15 | −0.4621 (7) | 0.3737 (6) | 0.2434 (2) | 0.0161 (5)* | |
C16 | −0.0925 (7) | 0.6176 (7) | 0.1753 (3) | 0.0214 (5)* | |
C17 | −0.0170 (6) | 0.5336 (7) | 0.1409 (2) | 0.0295 (7)* | |
C18 | 0.1327 (8) | 0.5481 (8) | 0.1352 (3) | 0.0419 (8)* | |
C19 | 0.2011 (7) | 0.6452 (6) | 0.1617 (2) | 0.0338 (8)* | |
C20 | 0.1313 (6) | 0.7303 (7) | 0.1984 (2) | 0.0287 (7)* | |
C21 | −0.0271 (6) | 0.7264 (6) | 0.2064 (2) | 0.0221 (6)* | |
C22 | −0.3293 (6) | 0.6990 (6) | 0.1410 (2) | 0.0189 (5)* | |
C23 | −0.2895 (6) | 0.6973 (6) | 0.0892 (2) | 0.0261 (6)* | |
C24 | −0.3551 (6) | 0.7810 (6) | 0.0555 (2) | 0.0305 (8)* | |
C25 | −0.4691 (6) | 0.8678 (6) | 0.0753 (3) | 0.0282 (8)* | |
C26 | −0.5043 (7) | 0.8644 (7) | 0.1265 (3) | 0.0277 (7)* | |
C27 | −0.4376 (6) | 0.7790 (7) | 0.1620 (2) | 0.0225 (6)* | |
C28 | −0.3635 (6) | 0.2692 (7) | 0.2559 (3) | 0.0176 (5)* | |
C29 | −0.3334 (6) | 0.1624 (7) | 0.2140 (3) | 0.0206 (6)* | |
C30 | −0.2392 (7) | 0.0611 (8) | 0.2313 (3) | 0.0294 (6)* | |
C31 | −0.1911 (7) | 0.0524 (8) | 0.2817 (3) | 0.0262 (5)* | |
C32 | −0.2198 (6) | 0.1435 (6) | 0.3199 (3) | 0.0239 (6)* | |
C33 | −0.3063 (6) | 0.2469 (6) | 0.3110 (3) | 0.0206 (5)* | |
C34 | −0.6200 (6) | 0.3400 (6) | 0.2521 (2) | 0.0170 (5)* | |
C35 | −0.6753 (7) | 0.2178 (7) | 0.2431 (3) | 0.0259 (6)* | |
C36 | −0.8255 (6) | 0.2077 (6) | 0.2520 (2) | 0.0256 (7)* | |
C37 | −0.9115 (7) | 0.3081 (6) | 0.2669 (2) | 0.0269 (6)* | |
C38 | −0.8561 (8) | 0.4257 (8) | 0.2749 (3) | 0.0319 (6)* | |
C39 | −0.7117 (6) | 0.4527 (7) | 0.2678 (2) | 0.0270 (6)* | |
C40 | −0.4518 (6) | 0.3617 (6) | 0.0962 (2) | 0.0162 (6)* | |
C41 | −0.4288 (6) | 0.2249 (6) | 0.0588 (2) | 0.0236 (6)* | |
C42 | −0.5387 (6) | 0.4478 (6) | 0.0639 (2) | 0.0223 (5)* | |
Fe1' | −0.04238 (5) | 0.38071 (17) | 0.59670 (2) | 0.01355 (9) | |
Cl1' | 0.0867 (2) | 0.3987 (2) | 0.67625 (8) | 0.02670 (17) | |
Cl2' | −0.0449 (2) | 0.1982 (2) | 0.53882 (9) | 0.0268 (2) | |
P1' | −0.0817 (2) | 0.5724 (2) | 0.55103 (8) | 0.01661 (17) | |
P2' | −0.30246 (19) | 0.1664 (2) | 0.72494 (8) | 0.01528 (17) | |
O1' | −0.2755 (5) | 0.2821 (5) | 0.77803 (18) | 0.0184 (4)* | |
O2' | −0.1465 (4) | 0.0895 (4) | 0.72509 (16) | 0.0155 (3)* | |
N1' | −0.2633 (5) | 0.4101 (5) | 0.61429 (19) | 0.0131 (4)* | |
N2' | −0.2637 (5) | 0.5830 (5) | 0.55459 (19) | 0.0175 (4)* | |
N3' | −0.2468 (5) | 0.2550 (5) | 0.67436 (19) | 0.0165 (4)* | |
O3' | −0.2691 (4) | 0.0980 (4) | 0.89876 (15) | 0.0178 (4)* | |
O4' | −0.0653 (4) | 0.0028 (4) | 0.86491 (16) | 0.0155 (4)* | |
C1' | −0.3387 (7) | 0.4973 (7) | 0.5836 (3) | 0.0150 (5)* | |
C2' | −0.4854 (6) | 0.4962 (6) | 0.5825 (2) | 0.0159 (5)* | |
C3' | −0.5569 (6) | 0.4302 (6) | 0.6207 (2) | 0.0144 (5)* | |
C4' | −0.4815 (7) | 0.3449 (7) | 0.6502 (3) | 0.0159 (4)* | |
C5' | −0.3331 (6) | 0.3378 (6) | 0.6494 (2) | 0.0142 (5)* | |
C6' | −0.0227 (7) | 0.7261 (6) | 0.5915 (3) | 0.0212 (5)* | |
C7' | −0.0502 (5) | 0.8558 (6) | 0.5639 (3) | 0.0268 (7)* | |
C8' | 0.1443 (7) | 0.7223 (7) | 0.6074 (3) | 0.0307 (6)* | |
C9' | −0.0507 (6) | 0.5952 (6) | 0.4780 (2) | 0.0195 (5)* | |
C10' | −0.1202 (7) | 0.4782 (7) | 0.4411 (3) | 0.0296 (7)* | |
C11' | 0.1102 (6) | 0.6022 (6) | 0.4694 (2) | 0.0263 (6)* | |
C12' | −0.3133 (7) | 0.2569 (6) | 0.8310 (2) | 0.0161 (5)* | |
C13' | −0.2749 (6) | 0.1207 (6) | 0.8420 (2) | 0.0155 (5)* | |
C14' | −0.1191 (6) | 0.0927 (6) | 0.8252 (2) | 0.0153 (5)* | |
C15' | −0.1115 (7) | 0.0090 (6) | 0.7647 (2) | 0.0161 (5)* | |
C16' | −0.4824 (7) | 0.2745 (7) | 0.8344 (3) | 0.0214 (5)* | |
C17' | −0.5639 (6) | 0.1950 (6) | 0.8650 (2) | 0.0295 (7)* | |
C18' | −0.7079 (7) | 0.2195 (8) | 0.8683 (3) | 0.0419 (8)* | |
C19' | −0.7719 (7) | 0.3221 (6) | 0.8377 (2) | 0.0338 (8)* | |
C20' | −0.6894 (6) | 0.3967 (7) | 0.8068 (2) | 0.0287 (7)* | |
C21' | −0.5545 (6) | 0.3649 (6) | 0.8077 (2) | 0.0221 (6)* | |
C22' | −0.2462 (6) | 0.3633 (6) | 0.8709 (2) | 0.0189 (5)* | |
C23' | −0.2841 (7) | 0.3907 (6) | 0.9274 (2) | 0.0261 (6)* | |
C24' | −0.2127 (6) | 0.4840 (6) | 0.9644 (2) | 0.0305 (8)* | |
C25' | −0.1162 (6) | 0.5611 (6) | 0.9476 (2) | 0.0282 (8)* | |
C26' | −0.0759 (7) | 0.5405 (7) | 0.8912 (3) | 0.0277 (7)* | |
C27' | −0.1394 (6) | 0.4440 (6) | 0.8549 (2) | 0.0225 (6)* | |
C28' | −0.2099 (6) | −0.1184 (7) | 0.7553 (3) | 0.0176 (5)* | |
C29' | −0.2472 (7) | −0.1942 (7) | 0.7930 (3) | 0.0206 (6)* | |
C30' | −0.3233 (7) | −0.3019 (8) | 0.7826 (3) | 0.0294 (6)* | |
C31' | −0.3884 (7) | −0.3312 (7) | 0.7283 (3) | 0.0262 (5)* | |
C32' | −0.3563 (6) | −0.2470 (6) | 0.6856 (2) | 0.0239 (6)* | |
C33' | −0.2652 (6) | −0.1367 (6) | 0.7013 (3) | 0.0206 (5)* | |
C34' | 0.0457 (6) | −0.0275 (6) | 0.7542 (2) | 0.0170 (5)* | |
C35' | 0.0967 (7) | −0.1514 (7) | 0.7655 (3) | 0.0259 (6)* | |
C36' | 0.2420 (6) | −0.1852 (6) | 0.7630 (2) | 0.0256 (7)* | |
C37' | 0.3360 (7) | −0.0982 (6) | 0.7465 (2) | 0.0269 (6)* | |
C38' | 0.2830 (8) | 0.0300 (8) | 0.7339 (3) | 0.0319 (6)* | |
C39' | 0.1376 (6) | 0.0571 (7) | 0.7373 (2) | 0.0270 (6)* | |
C40' | −0.1297 (5) | 0.0472 (5) | 0.9169 (2) | 0.0162 (6)* | |
C41' | −0.1508 (6) | −0.0664 (6) | 0.9458 (2) | 0.0236 (6)* | |
C42' | −0.0363 (6) | 0.1562 (6) | 0.9485 (2) | 0.0223 (5)* | |
C43 | 0.1177 (7) | −0.0541 (8) | 0.0750 (3) | 0.0526 (11)* | |
C44 | 0.0094 (8) | −0.0060 (9) | 0.1141 (3) | 0.0629 (13)* | |
C45 | 0.0113 (9) | 0.1277 (9) | 0.1074 (3) | 0.0475 (9)* | |
C46 | 0.1520 (8) | 0.1693 (9) | 0.0938 (3) | 0.0493 (9)* | |
O5 | 0.2196 (6) | 0.0469 (6) | 0.0663 (2) | 0.0799 (10)* | |
C46' | 0.2673 (8) | 0.8749 (9) | 0.9215 (3) | 0.0493 (9)* | |
O5' | 0.1969 (6) | 0.7611 (6) | 0.9302 (2) | 0.0799 (10)* | |
C43' | 0.2962 (7) | 0.6694 (7) | 0.9504 (3) | 0.0526 (11)* | |
C44' | 0.4271 (8) | 0.6910 (9) | 0.9118 (3) | 0.0629 (13)* | |
C45' | 0.4245 (8) | 0.8411 (9) | 0.9069 (3) | 0.0475 (9)* | |
H1c2 | −0.026909 | 1.042287 | 0.441129 | 0.019* | |
H1c3 | 0.091546 | 0.860234 | 0.395757 | 0.0172* | |
H1c4 | −0.045947 | 0.70638 | 0.33531 | 0.0191* | |
H1c6 | −0.505254 | 1.172293 | 0.384834 | 0.0254* | |
H1c7 | −0.391407 | 1.322244 | 0.439125 | 0.0321* | |
H2c7 | −0.543586 | 1.383715 | 0.431783 | 0.0321* | |
H3c7 | −0.501524 | 1.320714 | 0.485967 | 0.0321* | |
H1c8 | −0.722951 | 1.098596 | 0.379801 | 0.0368* | |
H2c8 | −0.759524 | 1.181687 | 0.435277 | 0.0368* | |
H3c8 | −0.727148 | 1.251141 | 0.382926 | 0.0368* | |
H1c9 | −0.494241 | 1.180363 | 0.54301 | 0.0234* | |
H1c10 | −0.340023 | 1.055298 | 0.577674 | 0.0355* | |
H2c10 | −0.47805 | 1.006821 | 0.603924 | 0.0355* | |
H3c10 | −0.417604 | 0.927137 | 0.551391 | 0.0355* | |
H1c11 | −0.728763 | 1.145583 | 0.523126 | 0.0315* | |
H2c11 | −0.713285 | 0.999226 | 0.534156 | 0.0315* | |
H3c11 | −0.690736 | 1.110433 | 0.583096 | 0.0315* | |
H1c13 | −0.237791 | 0.410214 | 0.187937 | 0.0186* | |
H1c14 | −0.506928 | 0.49864 | 0.197468 | 0.0184* | |
H1c17 | −0.066418 | 0.461815 | 0.119796 | 0.0355* | |
H1c18 | 0.183115 | 0.484886 | 0.111436 | 0.0502* | |
H1c19 | 0.300853 | 0.658023 | 0.155658 | 0.0405* | |
H1c20 | 0.187047 | 0.796639 | 0.220344 | 0.0344* | |
H1c21 | −0.077548 | 0.790152 | 0.229951 | 0.0265* | |
H1c24 | −0.324871 | 0.782009 | 0.018321 | 0.0366* | |
H1c26 | −0.578214 | 0.921714 | 0.140822 | 0.0332* | |
H1c27 | −0.466778 | 0.777093 | 0.199331 | 0.0269* | |
H1c29 | −0.373532 | 0.159058 | 0.176856 | 0.0247* | |
H1c30 | −0.210035 | −0.005098 | 0.203194 | 0.0353* | |
H1c31 | −0.134801 | −0.021219 | 0.290258 | 0.0314* | |
H1c32 | −0.178499 | 0.138836 | 0.356444 | 0.0287* | |
H1c33 | −0.330517 | 0.307125 | 0.342168 | 0.0247* | |
H1c35 | −0.618017 | 0.143226 | 0.231628 | 0.0311* | |
H1c37 | −1.011691 | 0.294197 | 0.271646 | 0.0323* | |
H1c38 | −0.917984 | 0.497148 | 0.286255 | 0.0383* | |
H1c41 | −0.404307 | 0.158618 | 0.082295 | 0.0283* | |
H2c41 | −0.515646 | 0.200679 | 0.037646 | 0.0283* | |
H3c41 | −0.352737 | 0.234008 | 0.034094 | 0.0283* | |
H1c2' | −0.539064 | 0.540431 | 0.555754 | 0.019* | |
H1c4' | −0.532275 | 0.289011 | 0.671893 | 0.0191* | |
H1c6' | −0.081892 | 0.729766 | 0.622922 | 0.0254* | |
H1c7' | −0.14903 | 0.859478 | 0.551736 | 0.0321* | |
H2c7' | −0.027699 | 0.9295 | 0.590535 | 0.0321* | |
H3c7' | 0.009458 | 0.857336 | 0.532816 | 0.0321* | |
H1c8' | 0.162145 | 0.76637 | 0.643854 | 0.0368* | |
H2c8' | 0.17492 | 0.633334 | 0.606549 | 0.0368* | |
H3c8' | 0.196466 | 0.765026 | 0.58125 | 0.0368* | |
H1c10' | −0.219383 | 0.471515 | 0.449269 | 0.0355* | |
H2c10' | −0.112571 | 0.491274 | 0.402815 | 0.0355* | |
H3c10' | −0.071618 | 0.399391 | 0.448213 | 0.0355* | |
H1c11' | 0.147013 | 0.685108 | 0.485693 | 0.0315* | |
H2c11' | 0.157939 | 0.533695 | 0.486577 | 0.0315* | |
H3c11' | 0.126778 | 0.592116 | 0.430459 | 0.0315* | |
H1c13' | −0.348475 | 0.067937 | 0.821916 | 0.0186* | |
H1c18' | −0.766146 | 0.170352 | 0.890191 | 0.0502* | |
H1c19' | −0.873029 | 0.337802 | 0.839202 | 0.0405* | |
H1c20' | −0.72793 | 0.464859 | 0.786832 | 0.0344* | |
H1c21' | −0.496065 | 0.413814 | 0.785757 | 0.0265* | |
H1c23' | −0.36187 | 0.342882 | 0.940309 | 0.0313* | |
H1c24' | −0.234669 | 0.491801 | 1.002806 | 0.0366* | |
H1c25' | −0.07329 | 0.629989 | 0.972653 | 0.0338* | |
H1c26' | −0.003524 | 0.594884 | 0.87855 | 0.0332* | |
H1c30' | −0.334962 | −0.359311 | 0.810617 | 0.0353* | |
H1c31' | −0.451778 | −0.404678 | 0.719994 | 0.0314* | |
H1c32' | −0.395066 | −0.265344 | 0.648373 | 0.0287* | |
H1c35' | 0.029382 | −0.214624 | 0.77519 | 0.0311* | |
H1c37' | 0.435398 | −0.120102 | 0.743089 | 0.0323* | |
H1c38' | 0.348097 | 0.094189 | 0.723429 | 0.0383* | |
H1c39' | 0.102434 | 0.139002 | 0.727123 | 0.0323* | |
H1c41' | −0.185998 | −0.039602 | 0.981806 | 0.0283* | |
H2c41' | −0.219017 | −0.124076 | 0.925111 | 0.0283* | |
H3c41' | −0.061211 | −0.110857 | 0.949737 | 0.0283* | |
H1c42' | −0.064721 | 0.170769 | 0.986177 | 0.0268* | |
H2c42' | 0.062492 | 0.130689 | 0.947896 | 0.0268* | |
H3c42' | −0.048564 | 0.234966 | 0.931232 | 0.0268* | |
H1c42 | −0.618235 | 0.399511 | 0.045618 | 0.0268* | |
H2c42 | −0.573837 | 0.519272 | 0.088261 | 0.0268* | |
H3c42 | −0.480892 | 0.480903 | 0.036827 | 0.0268* | |
H1c39 | −0.674426 | 0.54011 | 0.272982 | 0.0323* | |
H1c23 | −0.216252 | 0.638741 | 0.075325 | 0.0313* | |
H1c25 | −0.516189 | 0.925031 | 0.051784 | 0.0338* | |
H1c36 | −0.867733 | 0.122179 | 0.246826 | 0.0307* | |
H1c9' | −0.0926 | 0.675118 | 0.468454 | 0.0234* | |
H1c14' | −0.06776 | 0.173198 | 0.824831 | 0.0184* | |
H1c17' | −0.520123 | 0.125792 | 0.88303 | 0.0355* | |
H1c33' | −0.243111 | −0.076986 | 0.675157 | 0.0247* | |
H1c27' | −0.10946 | 0.431773 | 0.817396 | 0.0269* | |
H1c3' | −0.6572 | 0.444467 | 0.626069 | 0.0172* | |
H1n2 | −0.256727 | 1.100985 | 0.482298 | 0.0211* | |
H1n3 | −0.415221 | 0.686521 | 0.339229 | 0.0198* | |
H1n2' | −0.309933 | 0.642211 | 0.538219 | 0.0211* | |
H1n3' | −0.158764 | 0.246371 | 0.664244 | 0.0198* | |
H1c36' | 0.274363 | −0.26832 | 0.772828 | 0.0307* | |
H1c43 | 0.1677 | −0.126102 | 0.088641 | 0.0632* | |
H2c43 | 0.071328 | −0.086431 | 0.040186 | 0.0632* | |
H1c44 | 0.042566 | −0.01822 | 0.151017 | 0.0755* | |
H2c44 | −0.082418 | −0.042445 | 0.101576 | 0.0755* | |
H1c45 | −0.057124 | 0.144721 | 0.078507 | 0.057* | |
H2c45 | −0.016684 | 0.177141 | 0.140963 | 0.057* | |
H1c46 | 0.142648 | 0.232794 | 0.067794 | 0.0591* | |
H2c46 | 0.206092 | 0.199136 | 0.127211 | 0.0591* | |
H1c46' | 0.267222 | 0.934784 | 0.954629 | 0.0591* | |
H2c46' | 0.22001 | 0.912815 | 0.891379 | 0.0591* | |
H1c43' | 0.32404 | 0.697345 | 0.988273 | 0.0632* | |
H2c43' | 0.258874 | 0.582579 | 0.941515 | 0.0632* | |
H1c44' | 0.515289 | 0.668898 | 0.930134 | 0.0755* | |
H2c44' | 0.408773 | 0.644112 | 0.875888 | 0.0755* | |
H1c45' | 0.43877 | 0.85598 | 0.869214 | 0.057* | |
H2c45' | 0.489017 | 0.884975 | 0.934587 | 0.057* | |
H1c29' | −0.216317 | −0.168392 | 0.830771 | 0.0247* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Fe1 | 0.00779 (12) | 0.01374 (17) | 0.01891 (15) | −0.00044 (14) | 0.00167 (10) | 0.00038 (15) |
Cl1 | 0.0161 (2) | 0.0371 (4) | 0.0245 (2) | 0.0065 (3) | −0.00485 (18) | −0.0050 (3) |
Cl2 | 0.0149 (2) | 0.0268 (4) | 0.0416 (3) | −0.0026 (3) | −0.0016 (2) | 0.0182 (3) |
P1 | 0.0082 (2) | 0.0153 (3) | 0.0253 (3) | −0.0005 (2) | 0.0023 (2) | −0.0032 (2) |
P2 | 0.0088 (3) | 0.0158 (3) | 0.0205 (3) | 0.0014 (3) | 0.00242 (18) | −0.0020 (3) |
Fe1' | 0.00779 (12) | 0.01448 (18) | 0.01891 (15) | 0.00080 (14) | 0.00167 (10) | 0.00376 (15) |
Cl1' | 0.0161 (2) | 0.0405 (4) | 0.0245 (2) | −0.0075 (3) | −0.00485 (18) | 0.0104 (3) |
Cl2' | 0.0149 (2) | 0.0209 (4) | 0.0416 (3) | 0.0022 (3) | −0.0016 (2) | −0.0091 (3) |
P1' | 0.0082 (2) | 0.0179 (3) | 0.0253 (3) | 0.0010 (2) | 0.0023 (2) | 0.0087 (2) |
P2' | 0.0088 (3) | 0.0176 (4) | 0.0205 (3) | −0.0009 (3) | 0.00242 (18) | 0.0065 (3) |
Geometric parameters (Å, º) top
Fe1—Cl1 | 2.2416 (19) | N1'—C1' | 1.403 (9) |
Fe1—Cl2 | 2.225 (2) | N1'—C5' | 1.377 (8) |
Fe1—P1 | 2.380 (2) | N2'—C1' | 1.395 (9) |
Fe1—N1 | 2.097 (5) | N2'—H1n2' | 0.87 |
Cl1—N3 | 3.383 (5) | N3'—C5' | 1.350 (8) |
Cl2—N2' | 3.301 (5) | N3'—H1n3' | 0.87 |
P1—N2 | 1.707 (5) | O3'—C13' | 1.423 (7) |
P1—C6 | 1.849 (7) | O3'—C40' | 1.472 (6) |
P1—C9 | 1.813 (6) | O4'—C14' | 1.483 (7) |
P2—O1 | 1.575 (5) | O4'—C40' | 1.452 (7) |
P2—N3 | 1.672 (5) | C1'—C2' | 1.370 (9) |
O1—C12 | 1.484 (7) | C2'—C3' | 1.399 (9) |
O2—C15 | 1.508 (7) | C2'—H1c2' | 0.96 |
O3—C13 | 1.423 (6) | C3'—C4' | 1.373 (9) |
O3—C40 | 1.437 (6) | C3'—H1c3' | 0.96 |
O4—C14 | 1.362 (7) | C4'—C5' | 1.388 (9) |
O4—C40 | 1.367 (7) | C4'—H1c4' | 0.96 |
N1—C1 | 1.288 (8) | C6'—H1c6' | 0.96 |
N1—C5 | 1.336 (8) | C7'—H1c7' | 0.96 |
N2—C1 | 1.372 (8) | C7'—H2c7' | 0.96 |
N2—Cl2'i | 3.328 (5) | C7'—H3c7' | 0.96 |
N2—H1n2 | 0.87 | C8'—H1c8' | 0.96 |
N3—C5 | 1.399 (7) | C8'—H2c8' | 0.96 |
N3—H1n3 | 0.87 | C8'—H3c8' | 0.96 |
C1—C2 | 1.432 (9) | C9'—C10' | 1.548 (9) |
C2—C3 | 1.380 (8) | C9'—C11' | 1.529 (8) |
C2—H1c2 | 0.96 | C9'—H1c9' | 0.96 |
C3—C4 | 1.389 (8) | C10'—H1c10' | 0.96 |
C3—H1c3 | 0.96 | C10'—H2c10' | 0.96 |
C4—C5 | 1.397 (9) | C10'—H3c10' | 0.96 |
C4—H1c4 | 0.96 | C11'—H1c11' | 0.96 |
C6—C7 | 1.509 (8) | C11'—H2c11' | 0.96 |
C6—C8 | 1.490 (9) | C11'—H3c11' | 0.96 |
C6—H1c6 | 0.96 | C12'—C13' | 1.500 (9) |
C7—H1c7 | 0.96 | C12'—C22' | 1.502 (8) |
C7—H2c7 | 0.96 | C13'—C14' | 1.547 (8) |
C7—H3c7 | 0.96 | C13'—H1c13' | 0.96 |
C8—H1c8 | 0.96 | C14'—H1c14' | 0.96 |
C8—H2c8 | 0.96 | C15'—C34' | 1.540 (9) |
C8—H3c8 | 0.96 | C16'—C17' | 1.410 (9) |
C9—C10 | 1.503 (9) | C16'—C21' | 1.356 (9) |
C9—C11 | 1.484 (8) | C17'—C18' | 1.372 (9) |
C9—H1c9 | 0.96 | C17'—H1c17' | 0.96 |
C10—H1c10 | 0.96 | C18'—C19' | 1.471 (10) |
C10—H2c10 | 0.96 | C18'—H1c18' | 0.96 |
C10—H3c10 | 0.96 | C19'—C20' | 1.387 (9) |
C11—H1c11 | 0.96 | C19'—H1c19' | 0.96 |
C11—H2c11 | 0.96 | C20'—C21' | 1.302 (8) |
C11—H3c11 | 0.96 | C20'—H1c20' | 0.96 |
C12—C16 | 1.483 (9) | C21'—H1c21' | 0.96 |
C12—C22 | 1.569 (9) | C22'—C23' | 1.431 (8) |
C13—C14 | 1.543 (8) | C22'—C27' | 1.394 (9) |
C13—H1c13 | 0.96 | C23'—C24' | 1.393 (8) |
C14—C15 | 1.483 (9) | C23'—H1c23' | 0.96 |
C14—H1c14 | 0.96 | C24'—C25' | 1.309 (8) |
C15—C28 | 1.467 (9) | C24'—H1c24' | 0.96 |
C15—C34 | 1.544 (9) | C25'—C26' | 1.432 (8) |
C16—C17 | 1.355 (9) | C25'—H1c25' | 0.96 |
C16—C21 | 1.408 (9) | C26'—C27' | 1.373 (9) |
C17—C18 | 1.421 (9) | C26'—H1c26' | 0.96 |
C17—H1c17 | 0.96 | C27'—H1c27' | 0.96 |
C18—C19 | 1.285 (9) | C28'—C29' | 1.325 (10) |
C18—H1c18 | 0.96 | C28'—C33' | 1.385 (8) |
C19—C20 | 1.368 (9) | C29'—C30' | 1.314 (10) |
C19—H1c19 | 0.96 | C29'—H1c29' | 0.96 |
C20—C21 | 1.502 (8) | C30'—C31' | 1.433 (9) |
C20—H1c20 | 0.96 | C30'—H1c30' | 0.96 |
C21—H1c21 | 0.96 | C31'—C32' | 1.464 (10) |
C22—C23 | 1.327 (8) | C31'—H1c31' | 0.96 |
C22—C27 | 1.385 (8) | C32'—C33' | 1.429 (8) |
C23—C24 | 1.380 (9) | C32'—H1c32' | 0.96 |
C23—H1c23 | 0.96 | C33'—H1c33' | 0.96 |
C24—C25 | 1.454 (8) | C34'—C35' | 1.414 (10) |
C24—H1c24 | 0.96 | C34'—C39' | 1.333 (9) |
C25—C26 | 1.306 (9) | C35'—C36' | 1.404 (9) |
C25—H1c25 | 0.96 | C35'—H1c35' | 0.96 |
C26—C27 | 1.426 (9) | C36'—C37' | 1.359 (9) |
C26—H1c26 | 0.96 | C36'—H1c36' | 0.96 |
C27—H1c27 | 0.96 | C37'—C38' | 1.471 (10) |
C28—C29 | 1.453 (9) | C37'—H1c37' | 0.96 |
C28—C33 | 1.464 (9) | C38'—C39' | 1.391 (9) |
C29—C30 | 1.453 (10) | C38'—H1c38' | 0.96 |
C29—H1c29 | 0.96 | C39'—H1c39' | 0.96 |
C30—C31 | 1.300 (10) | C40'—C41' | 1.449 (8) |
C30—H1c30 | 0.96 | C40'—C42' | 1.539 (8) |
C31—C32 | 1.283 (9) | C41'—H1c41' | 0.96 |
C31—H1c31 | 0.96 | C41'—H2c41' | 0.96 |
C32—C33 | 1.369 (9) | C41'—H3c41' | 0.96 |
C32—H1c32 | 0.96 | C42'—H1c42' | 0.96 |
C33—H1c33 | 0.96 | C42'—H2c42' | 0.96 |
C34—C35 | 1.355 (10) | C42'—H3c42' | 0.96 |
C34—C39 | 1.470 (9) | C43—C44 | 1.467 (10) |
C35—C36 | 1.433 (9) | C43—O5 | 1.449 (10) |
C35—H1c35 | 0.96 | C43—H1c43 | 0.96 |
C36—C37 | 1.338 (8) | C43—H2c43 | 0.96 |
C36—H1c36 | 0.96 | C44—C45 | 1.407 (13) |
C37—C38 | 1.310 (10) | C44—H1c44 | 0.96 |
C37—H1c37 | 0.96 | C44—H2c44 | 0.96 |
C38—C39 | 1.399 (9) | C45—C46 | 1.445 (12) |
C38—H1c38 | 0.96 | C45—H1c45 | 0.96 |
C39—H1c39 | 0.96 | C45—H2c45 | 0.96 |
C40—C42 | 1.472 (8) | C46—O5 | 1.514 (11) |
C41—H1c41 | 0.96 | C46—H1c46 | 0.96 |
C41—H2c41 | 0.96 | C46—H2c46 | 0.96 |
C41—H3c41 | 0.96 | C46'—O5' | 1.386 (11) |
C42—H1c42 | 0.96 | C46'—C45' | 1.556 (11) |
C42—H2c42 | 0.96 | C46'—H1c46' | 0.96 |
C42—H3c42 | 0.96 | C46'—H2c46' | 0.96 |
Fe1'—Cl1' | 2.227 (2) | O5'—C43' | 1.435 (9) |
Fe1'—Cl2' | 2.224 (2) | C43'—H1c43' | 0.96 |
Fe1'—P1' | 2.393 (3) | C43'—H2c43' | 0.96 |
P1'—N2' | 1.709 (5) | C44'—C45' | 1.565 (13) |
P1'—C6' | 1.843 (6) | C44'—H1c44' | 0.96 |
P1'—C9' | 1.852 (6) | C44'—H2c44' | 0.96 |
P2'—N3' | 1.708 (6) | C45'—H1c45' | 0.96 |
O1'—C12' | 1.402 (8) | C45'—H2c45' | 0.96 |
O2'—C15' | 1.369 (8) | | |
| | | |
Cl1—Fe1—Cl2 | 122.17 (8) | C1'—N1'—C5' | 120.8 (5) |
Cl1—Fe1—P1 | 118.47 (8) | Cl2—N2'—P1' | 134.1 (2) |
Cl1—Fe1—N1 | 110.01 (14) | Cl2—N2'—C1' | 101.4 (3) |
Cl2—Fe1—P1 | 111.93 (7) | Cl2—N2'—H1n2' | 25.88 |
Cl2—Fe1—N1 | 104.34 (16) | P1'—N2'—C1' | 120.4 (4) |
P1—Fe1—N1 | 80.48 (15) | P1'—N2'—H1n2' | 119.78 |
Fe1—Cl1—N3 | 62.76 (9) | C1'—N2'—H1n2' | 119.78 |
Fe1—Cl2—N2' | 131.90 (12) | P2'—N3'—C5' | 123.0 (4) |
Fe1—P1—N2 | 94.50 (18) | P2'—N3'—H1n3' | 118.48 |
Fe1—P1—C6 | 114.9 (2) | C5'—N3'—H1n3' | 118.48 |
Fe1—P1—C9 | 122.0 (2) | C13'—O3'—C40' | 112.9 (4) |
N2—P1—C6 | 108.0 (3) | C14'—O4'—C40' | 105.4 (4) |
N2—P1—C9 | 103.5 (3) | N1'—C1'—N2' | 119.8 (5) |
C6—P1—C9 | 110.8 (3) | N1'—C1'—C2' | 119.0 (6) |
O1—P2—N3 | 96.7 (3) | N2'—C1'—C2' | 121.2 (6) |
P2—O1—C12 | 125.7 (4) | C1'—C2'—C3' | 119.8 (6) |
C13—O3—C40 | 104.8 (4) | C1'—C2'—H1c2' | 120.11 |
C14—O4—C40 | 111.1 (4) | C3'—C2'—H1c2' | 120.11 |
Fe1—N1—C1 | 121.9 (4) | C2'—C3'—C4' | 119.0 (6) |
Fe1—N1—C5 | 119.9 (4) | C2'—C3'—H1c3' | 120.51 |
C1—N1—C5 | 116.9 (5) | C4'—C3'—H1c3' | 120.51 |
P1—N2—C1 | 124.5 (4) | C3'—C4'—C5' | 121.2 (6) |
P1—N2—Cl2'i | 133.1 (2) | C3'—C4'—H1c4' | 119.39 |
P1—N2—H1n2 | 117.77 | C5'—C4'—H1c4' | 119.39 |
C1—N2—Cl2'i | 102.1 (3) | N1'—C5'—N3' | 113.7 (5) |
C1—N2—H1n2 | 117.77 | N1'—C5'—C4' | 118.5 (5) |
Cl2'i—N2—H1n2 | 16.49 | N3'—C5'—C4' | 127.3 (6) |
Cl1—N3—P2 | 123.5 (2) | P1'—C6'—H1c6' | 102.28 |
Cl1—N3—C5 | 104.8 (3) | H1c7'—C7'—H2c7' | 109.47 |
Cl1—N3—H1n3 | 22.28 | H1c7'—C7'—H3c7' | 109.47 |
P2—N3—C5 | 128.3 (4) | H2c7'—C7'—H3c7' | 109.47 |
P2—N3—H1n3 | 115.87 | H1c8'—C8'—H2c8' | 109.47 |
C5—N3—H1n3 | 115.86 | H1c8'—C8'—H3c8' | 109.47 |
N1—C1—N2 | 115.1 (6) | H2c8'—C8'—H3c8' | 109.47 |
N1—C1—C2 | 124.8 (6) | P1'—C9'—C10' | 107.8 (4) |
N2—C1—C2 | 120.2 (5) | P1'—C9'—C11' | 109.8 (4) |
C1—C2—C3 | 115.7 (5) | P1'—C9'—H1c9' | 110.86 |
C1—C2—H1c2 | 122.14 | C10'—C9'—C11' | 110.9 (5) |
C3—C2—H1c2 | 122.14 | C10'—C9'—H1c9' | 109.77 |
C2—C3—C4 | 120.8 (6) | C11'—C9'—H1c9' | 107.78 |
C2—C3—H1c3 | 119.62 | C9'—C10'—H1c10' | 109.47 |
C4—C3—H1c3 | 119.62 | C9'—C10'—H2c10' | 109.47 |
C3—C4—C5 | 115.7 (6) | C9'—C10'—H3c10' | 109.47 |
C3—C4—H1c4 | 122.16 | H1c10'—C10'—H2c10' | 109.47 |
C5—C4—H1c4 | 122.16 | H1c10'—C10'—H3c10' | 109.47 |
N1—C5—N3 | 116.0 (5) | H2c10'—C10'—H3c10' | 109.47 |
N1—C5—C4 | 125.1 (5) | C9'—C11'—H1c11' | 109.47 |
N3—C5—C4 | 118.2 (5) | C9'—C11'—H2c11' | 109.47 |
P1—C6—C7 | 110.9 (4) | C9'—C11'—H3c11' | 109.47 |
P1—C6—C8 | 114.0 (5) | H1c11'—C11'—H2c11' | 109.47 |
P1—C6—H1c6 | 108.29 | H1c11'—C11'—H3c11' | 109.47 |
C7—C6—C8 | 116.8 (5) | H2c11'—C11'—H3c11' | 109.47 |
C7—C6—H1c6 | 104.75 | O1'—C12'—C13' | 111.6 (5) |
C8—C6—H1c6 | 100.85 | O1'—C12'—C22' | 106.5 (5) |
C6—C7—H1c7 | 109.47 | C13'—C12'—C22' | 115.3 (5) |
C6—C7—H2c7 | 109.47 | O3'—C13'—C12' | 115.4 (5) |
C6—C7—H3c7 | 109.47 | O3'—C13'—C14' | 102.3 (4) |
H1c7—C7—H2c7 | 109.47 | O3'—C13'—H1c13' | 110.34 |
H1c7—C7—H3c7 | 109.47 | C12'—C13'—C14' | 109.0 (5) |
H2c7—C7—H3c7 | 109.47 | C12'—C13'—H1c13' | 103.77 |
C6—C8—H1c8 | 109.47 | C14'—C13'—H1c13' | 116.57 |
C6—C8—H2c8 | 109.47 | O4'—C14'—C13' | 103.7 (4) |
C6—C8—H3c8 | 109.47 | O4'—C14'—H1c14' | 117.01 |
H1c8—C8—H2c8 | 109.47 | C13'—C14'—H1c14' | 109.93 |
H1c8—C8—H3c8 | 109.47 | O2'—C15'—C34' | 103.9 (5) |
H2c8—C8—H3c8 | 109.47 | C17'—C16'—C21' | 117.0 (6) |
P1—C9—C10 | 112.3 (4) | C16'—C17'—C18' | 117.9 (6) |
P1—C9—C11 | 112.5 (4) | C16'—C17'—H1c17' | 121.06 |
P1—C9—H1c9 | 106.72 | C18'—C17'—H1c17' | 121.06 |
C10—C9—C11 | 113.3 (5) | C17'—C18'—C19' | 119.2 (6) |
C10—C9—H1c9 | 105.81 | C17'—C18'—H1c18' | 120.38 |
C11—C9—H1c9 | 105.56 | C19'—C18'—H1c18' | 120.38 |
C9—C10—H1c10 | 109.47 | C18'—C19'—C20' | 121.5 (6) |
C9—C10—H2c10 | 109.47 | C18'—C19'—H1c19' | 119.25 |
C9—C10—H3c10 | 109.47 | C20'—C19'—H1c19' | 119.25 |
H1c10—C10—H2c10 | 109.47 | C19'—C20'—C21' | 113.2 (6) |
H1c10—C10—H3c10 | 109.47 | C19'—C20'—H1c20' | 123.39 |
H2c10—C10—H3c10 | 109.47 | C21'—C20'—H1c20' | 123.39 |
C9—C11—H1c11 | 109.47 | C16'—C21'—C20' | 131.0 (6) |
C9—C11—H2c11 | 109.47 | C16'—C21'—H1c21' | 114.49 |
C9—C11—H3c11 | 109.47 | C20'—C21'—H1c21' | 114.49 |
H1c11—C11—H2c11 | 109.47 | C12'—C22'—C23' | 124.1 (5) |
H1c11—C11—H3c11 | 109.47 | C12'—C22'—C27' | 121.3 (5) |
H2c11—C11—H3c11 | 109.47 | C23'—C22'—C27' | 114.6 (5) |
O1—C12—C16 | 110.3 (5) | C22'—C23'—C24' | 122.6 (6) |
O1—C12—C22 | 105.3 (5) | C22'—C23'—H1c23' | 118.7 |
C16—C12—C22 | 110.5 (5) | C24'—C23'—H1c23' | 118.71 |
O3—C13—C14 | 107.3 (4) | C23'—C24'—C25' | 121.1 (5) |
O3—C13—H1c13 | 114.45 | C23'—C24'—H1c24' | 119.44 |
C14—C13—H1c13 | 104.83 | C25'—C24'—H1c24' | 119.44 |
O4—C14—C13 | 101.8 (4) | C24'—C25'—C26' | 118.6 (5) |
O4—C14—C15 | 115.2 (5) | C24'—C25'—H1c25' | 120.69 |
O4—C14—H1c14 | 115.55 | C26'—C25'—H1c25' | 120.69 |
C13—C14—C15 | 120.2 (5) | C25'—C26'—C27' | 120.9 (6) |
C13—C14—H1c14 | 110 | C25'—C26'—H1c26' | 119.54 |
C15—C14—H1c14 | 94.8 | C27'—C26'—H1c26' | 119.54 |
O2—C15—C14 | 104.7 (5) | C22'—C27'—C26' | 121.8 (6) |
O2—C15—C28 | 107.8 (5) | C22'—C27'—H1c27' | 119.08 |
O2—C15—C34 | 105.9 (4) | C26'—C27'—H1c27' | 119.09 |
C14—C15—C28 | 116.7 (5) | C29'—C28'—C33' | 122.0 (6) |
C14—C15—C34 | 108.4 (5) | C28'—C29'—C30' | 124.9 (7) |
C28—C15—C34 | 112.6 (5) | C28'—C29'—H1c29' | 117.56 |
C12—C16—C17 | 121.0 (6) | C30'—C29'—H1c29' | 117.56 |
C12—C16—C21 | 117.2 (6) | C29'—C30'—C31' | 118.2 (7) |
C17—C16—C21 | 121.7 (6) | C29'—C30'—H1c30' | 120.92 |
C16—C17—C18 | 122.2 (6) | C31'—C30'—H1c30' | 120.92 |
C16—C17—H1c17 | 118.92 | C30'—C31'—C32' | 118.7 (6) |
C18—C17—H1c17 | 118.92 | C30'—C31'—H1c31' | 120.65 |
C17—C18—C19 | 120.5 (6) | C32'—C31'—H1c31' | 120.64 |
C17—C18—H1c18 | 119.77 | C31'—C32'—C33' | 117.7 (5) |
C19—C18—H1c18 | 119.77 | C31'—C32'—H1c32' | 121.15 |
C18—C19—C20 | 119.7 (6) | C33'—C32'—H1c32' | 121.15 |
C18—C19—H1c19 | 120.14 | C28'—C33'—C32' | 118.0 (6) |
C20—C19—H1c19 | 120.14 | C28'—C33'—H1c33' | 121.02 |
C19—C20—C21 | 124.1 (5) | C32'—C33'—H1c33' | 121.02 |
C19—C20—H1c20 | 117.97 | C15'—C34'—C35' | 119.5 (6) |
C21—C20—H1c20 | 117.97 | C15'—C34'—C39' | 121.7 (6) |
C16—C21—C20 | 111.6 (5) | C35'—C34'—C39' | 118.7 (6) |
C16—C21—H1c21 | 124.2 | C34'—C35'—C36' | 122.4 (6) |
C20—C21—H1c21 | 124.2 | C34'—C35'—H1c35' | 118.81 |
C12—C22—C23 | 117.3 (5) | C36'—C35'—H1c35' | 118.81 |
C12—C22—C27 | 120.4 (5) | C35'—C36'—C37' | 118.8 (6) |
C23—C22—C27 | 122.3 (6) | C35'—C36'—H1c36' | 120.61 |
C22—C23—C24 | 119.0 (6) | C37'—C36'—H1c36' | 120.61 |
C22—C23—H1c23 | 120.51 | C36'—C37'—C38' | 118.9 (6) |
C24—C23—H1c23 | 120.51 | C36'—C37'—H1c37' | 120.53 |
C23—C24—C25 | 121.3 (5) | C38'—C37'—H1c37' | 120.53 |
C23—C24—H1c24 | 119.36 | C37'—C38'—C39' | 119.2 (6) |
C25—C24—H1c24 | 119.36 | C37'—C38'—H1c38' | 120.4 |
C24—C25—C26 | 116.9 (6) | C39'—C38'—H1c38' | 120.4 |
C24—C25—H1c25 | 121.54 | C34'—C39'—C38' | 121.8 (7) |
C26—C25—H1c25 | 121.54 | C34'—C39'—H1c39' | 119.09 |
C25—C26—C27 | 122.7 (6) | C38'—C39'—H1c39' | 119.09 |
C25—C26—H1c26 | 118.66 | O3'—C40'—O4' | 102.8 (4) |
C27—C26—H1c26 | 118.66 | O3'—C40'—C41' | 110.1 (4) |
C22—C27—C26 | 117.8 (6) | O3'—C40'—C42' | 111.1 (4) |
C22—C27—H1c27 | 121.1 | O4'—C40'—C41' | 107.3 (4) |
C26—C27—H1c27 | 121.1 | O4'—C40'—C42' | 109.4 (4) |
C15—C28—C29 | 120.7 (5) | C41'—C40'—C42' | 115.3 (5) |
C15—C28—C33 | 125.7 (5) | C40'—C41'—H1c41' | 109.47 |
C29—C28—C33 | 112.7 (6) | C40'—C41'—H2c41' | 109.47 |
C28—C29—C30 | 116.3 (6) | C40'—C41'—H3c41' | 109.47 |
C28—C29—H1c29 | 121.85 | H1c41'—C41'—H2c41' | 109.47 |
C30—C29—H1c29 | 121.85 | H1c41'—C41'—H3c41' | 109.47 |
C29—C30—C31 | 125.5 (7) | H2c41'—C41'—H3c41' | 109.47 |
C29—C30—H1c30 | 117.24 | C40'—C42'—H1c42' | 109.47 |
C31—C30—H1c30 | 117.24 | C40'—C42'—H2c42' | 109.47 |
C30—C31—C32 | 119.2 (7) | C40'—C42'—H3c42' | 109.47 |
C30—C31—H1c31 | 120.41 | H1c42'—C42'—H2c42' | 109.47 |
C32—C31—H1c31 | 120.41 | H1c42'—C42'—H3c42' | 109.47 |
C31—C32—C33 | 123.2 (6) | H2c42'—C42'—H3c42' | 109.47 |
C31—C32—H1c32 | 118.41 | C44—C43—O5 | 111.8 (6) |
C33—C32—H1c32 | 118.41 | C44—C43—H1c43 | 109.47 |
C28—C33—C32 | 122.5 (5) | C44—C43—H2c43 | 109.47 |
C28—C33—H1c33 | 118.74 | O5—C43—H1c43 | 109.47 |
C32—C33—H1c33 | 118.74 | O5—C43—H2c43 | 109.47 |
C15—C34—C35 | 123.9 (6) | H1c43—C43—H2c43 | 107.04 |
C15—C34—C39 | 115.0 (5) | C43—C44—C45 | 100.3 (7) |
C35—C34—C39 | 121.0 (6) | C43—C44—H1c44 | 109.47 |
C34—C35—C36 | 115.2 (6) | C43—C44—H2c44 | 109.47 |
C34—C35—H1c35 | 122.4 | C45—C44—H1c44 | 109.47 |
C36—C35—H1c35 | 122.4 | C45—C44—H2c44 | 109.47 |
C35—C36—C37 | 125.2 (6) | H1c44—C44—H2c44 | 117.28 |
C35—C36—H1c36 | 117.4 | C44—C45—C46 | 111.2 (7) |
C37—C36—H1c36 | 117.4 | C44—C45—H1c45 | 109.47 |
C36—C37—C38 | 118.6 (6) | C44—C45—H2c45 | 109.47 |
C36—C37—H1c37 | 120.69 | C46—C45—H1c45 | 109.47 |
C38—C37—H1c37 | 120.69 | C46—C45—H2c45 | 109.47 |
C37—C38—C39 | 123.5 (7) | H1c45—C45—H2c45 | 107.68 |
C37—C38—H1c38 | 118.26 | C45—C46—O5 | 104.3 (7) |
C39—C38—H1c38 | 118.26 | C45—C46—H1c46 | 109.47 |
C34—C39—C38 | 116.4 (6) | C45—C46—H2c46 | 109.47 |
C34—C39—H1c39 | 121.79 | O5—C46—H1c46 | 109.47 |
C38—C39—H1c39 | 121.79 | O5—C46—H2c46 | 109.47 |
O3—C40—O4 | 107.8 (4) | H1c46—C46—H2c46 | 114.19 |
O3—C40—C42 | 111.1 (5) | C43—O5—C46 | 103.0 (6) |
O4—C40—C42 | 114.2 (5) | O5'—C46'—C45' | 108.7 (7) |
H1c41—C41—H2c41 | 109.47 | O5'—C46'—H1c46' | 109.47 |
H1c41—C41—H3c41 | 109.47 | O5'—C46'—H2c46' | 109.47 |
H2c41—C41—H3c41 | 109.47 | C45'—C46'—H1c46' | 109.47 |
C40—C42—H1c42 | 109.47 | C45'—C46'—H2c46' | 109.47 |
C40—C42—H2c42 | 109.47 | H1c46'—C46'—H2c46' | 110.2 |
C40—C42—H3c42 | 109.47 | C46'—O5'—C43' | 110.4 (6) |
H1c42—C42—H2c42 | 109.47 | O5'—C43'—H1c43' | 109.47 |
H1c42—C42—H3c42 | 109.47 | O5'—C43'—H2c43' | 109.47 |
H2c42—C42—H3c42 | 109.47 | H1c43'—C43'—H2c43' | 118.15 |
Cl1'—Fe1'—Cl2' | 121.70 (10) | C45'—C44'—H1c44' | 109.47 |
Cl1'—Fe1'—P1' | 118.41 (10) | C45'—C44'—H2c44' | 109.47 |
Cl2'—Fe1'—P1' | 113.23 (8) | H1c44'—C44'—H2c44' | 114.66 |
N2ii—Cl2'—Fe1' | 132.11 (11) | C46'—C45'—C44' | 101.1 (7) |
Fe1'—P1'—N2' | 99.3 (2) | C46'—C45'—H1c45' | 109.47 |
Fe1'—P1'—C6' | 114.9 (2) | C46'—C45'—H2c45' | 109.47 |
Fe1'—P1'—C9' | 128.0 (2) | C44'—C45'—H1c45' | 109.47 |
N2'—P1'—C6' | 101.7 (3) | C44'—C45'—H2c45' | 109.47 |
N2'—P1'—C9' | 103.3 (3) | H1c45'—C45'—H2c45' | 116.7 |
C6'—P1'—C9' | 105.3 (3) | | |
Symmetry codes: (i) x, y+1, z; (ii) x, y−1, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
C17—H1c17···O3 | 0.96 | 2.33 | 3.038 (7) | 130.43 |
C27—H1c27···O1 | 0.96 | 2.31 | 2.684 (8) | 102.21 |
C29—H1c29···O4 | 0.96 | 2.42 | 3.038 (8) | 121.96 |
C21′—H1c21′···O1′ | 0.96 | 2.47 | 2.840 (7) | 102.69 |
C35′—H1c35′···C28′ | 0.96 | 2.50 | 2.887 (9) | 104.30 |
C39′—H1c39′···O2′ | 0.96 | 2.38 | 2.682 (7) | 97.82 |
C39—H1c39···O2 | 0.96 | 2.38 | 2.700 (7) | 98.92 |
C17′—H1c17′···O3′ | 0.96 | 2.38 | 3.041 (7) | 125.43 |
C33′—H1c33′···O2′ | 0.96 | 2.17 | 2.580 (7) | 104.57 |
C27′—H1c27′···O1′ | 0.96 | 2.29 | 2.648 (7) | 100.97 |
C29′—H1c29′···O4′ | 0.96 | 2.32 | 3.007 (8) | 128.08 |
Experimental details
| (Fe_PNP-HEt_CO2) | (Fe_PNP-Et_Br2_CO) | (Fe_PNP-TADDOL-iPr_Cl2) |
Crystal data |
Chemical formula | C23H41FeN3O2P2 | C14H25Br2FeN3OP2 | C46H55Cl2FeN3O5P2 |
Mr | 509.4 | 529 | 918.7 |
Crystal system, space group | Monoclinic, P1121/b | Monoclinic, P21/n | Triclinic, P1 |
Temperature (K) | 100 | 100 | 100 |
a, b, c (Å) | 31.781 (3), 18.012 (5), 18.262 (3) | 9.2939 (16), 11.7224 (18), 18.307 (3) | 9.3389 (7), 10.3155 (8), 24.3224 (18) |
α, β, γ (°) | 90, 90, 90.004 (2) | 90, 94.999 (10), 90 | 96.277 (3), 92.393 (3), 90.009 (2) |
V (Å3) | 10454 (3) | 1986.9 (6) | 2327.0 (3) |
Z | 16 | 4 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 0.72 | 4.95 | 0.55 |
Crystal size (mm) | 0.80 × 0.75 × 0.55 | 0.27 × 0.20 × 0.04 | 0.67 × 0.41 × 0.06 |
|
Data collection |
Diffractometer | Bruker KAPPA APEX II CCD diffractometer | Bruker KAPPA APEX II CCD diffractometer | Bruker KAPPA APEX II CCD diffractometer |
Absorption correction | Multi-scan SADABS | Multi-scan TWINABS | Multi-scan TWINABS |
Tmin, Tmax | 0.57, 0.67 | 0.32, 0.82 | 0.23, 0.85 |
No. of measured, independent and observed [I > 3σ(I)] reflections | 450669, 30818, 25454 | 13162, 12579, 6782 | 40097, 39775, 35102 |
Rint | 0.051 | 0.091 | 0.066 |
(sin θ/λ)max (Å−1) | 0.707 | 0.652 | 0.659 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.063, 0.079, 3.87 | 0.090, 0.128, 1.61 | 0.051, 0.070, 1.76 |
No. of reflections | 30818 | 12579 | 39775 |
No. of parameters | 815 | 99 | 439 |
H-atom treatment | H-atom parameters constrained | H-atom parameters constrained | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 2.07, −0.87 | 1.93, −2.09 | 0.84, −0.70 |
Absolute structure | ? | ? | 5587 of Friedel pairs used in the refinement |
Absolute structure parameter | ? | ? | 0.05 (2) |