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The systematic twinning of three 2,6-diaminopyridine-based Fe-PNP complexes is interpreted using order–disorder (OD) theory. The monoclinic [Fe0(PNPEt-iPr)(CO)2] [P1121/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 p21a(b) symmetry. The a glide planes of adjacent layers do not overlap, leading to OD polytypism. trans-[FeII(PNP-Et)Br2(CO)] [P21/n, Z′ = 1] is systematically twinned via twofold rotation about [001]. It is made up of OD layers with idealized p2121(2) symmetry. OD polytypism is caused by the twofold rotation axes of adjacent layers which do not overlap. [FeII2P,N-PNP-iPr,TAD)Cl2]·THF [P1, Z^{\prime} = 2] is systematically twinned via a twofold rotation about [010]. It is made up of layers with idealized p121(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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2052520615015097/um5003sup1.cif
Contains datablocks global, Fe_PNP-HEt_CO2, Fe_PNP-Et_Br2_CO, Fe_PNP-TADDOL-iPr_Cl2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615015097/um5003Fe_PNP-HEt_CO2sup2.hkl
Contains datablock Fe_(PNP-HEt)_(CO)2

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615015097/um5003Fe_PNP-Et_Br2_COsup3.hkl
Contains datablock Fe_(PNP-Et)_Br2_CO

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2052520615015097/um5003Fe_PNP-TADDOL-iPr_Cl2sup4.hkl
Contains datablock Fe_(PNP-TADDOL-iPr)_Cl2

CCDC references: 1418467; 1418468; 1418469

Computing details top

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.

Figures top
[Figure 1]
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[Figure 11]
[Figure 12]
[Figure 13]
[Figure 14]
[Figure 15]
[Figure 16]
(Fe_PNP-HEt_CO2) top
Crystal data top
C23H41FeN3O2P2F(000) = 4352
Mr = 509.4Dx = 1.295 Mg m3
Monoclinic, P1121/bMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2zbcCell parameters from 9703 reflections
a = 31.781 (3) Åθ = 2.4–30.0°
b = 18.012 (5) ŵ = 0.72 mm1
c = 18.262 (3) ÅT = 100 K
β = 90°Block, dark red
V = 10454 (3) Å30.80 × 0.75 × 0.55 mm
Z = 16
Data collection top
Bruker KAPPA APEX II CCD
diffractometer
30818 independent reflections
Radiation source: X-ray tube25454 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.051
ω– and φ–scansθmax = 30.2°, θmin = 0.6°
Absorption correction: multi-scan
SADABS
h = 4444
Tmin = 0.57, Tmax = 0.67k = 2525
450669 measured reflectionsl = 2525
Refinement top
Refinement on F1017 constraints
R[F2 > 2σ(F2)] = 0.063H-atom parameters constrained
wR(F2) = 0.079Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
S = 3.87(Δ/σ)max = 0.031
30818 reflectionsΔρmax = 2.07 e Å3
815 parametersΔρmin = 0.87 e Å3
0 restraints
Crystal data top
C23H41FeN3O2P2V = 10454 (3) Å3
Mr = 509.4Z = 16
Monoclinic, P1121/bMo Kα radiation
a = 31.781 (3) ŵ = 0.72 mm1
b = 18.012 (5) ÅT = 100 K
c = 18.262 (3) Å0.80 × 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 = 0.67Rint = 0.051
450669 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0630 restraints
wR(F2) = 0.079H-atom parameters constrained
S = 3.87Δρmax = 2.07 e Å3
30818 reflectionsΔρmin = 0.87 e Å3
815 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Fe10.63784 (3)0.67589 (5)0.74296 (3)0.0166 (2)
P10.58272 (5)0.60210 (10)0.74442 (6)0.0187 (4)
P20.70338 (5)0.71444 (10)0.74529 (5)0.0161 (4)
O10.60617 (13)0.7750 (3)0.63415 (19)0.0675 (18)
O20.61918 (10)0.7285 (2)0.8828 (2)0.0444 (12)
N20.59862 (10)0.53019 (19)0.68778 (18)0.0193 (5)
N10.66433 (10)0.58654 (18)0.69107 (17)0.0167 (5)
N30.72946 (10)0.64589 (18)0.69873 (17)0.0186 (5)
C10.63985 (12)0.5292 (2)0.6663 (2)0.0163 (6)
C20.65581 (13)0.4756 (2)0.6200 (2)0.0211 (7)
C30.69801 (13)0.4789 (2)0.5984 (2)0.0210 (7)
C40.72356 (13)0.5343 (2)0.6244 (2)0.0205 (6)
C50.70572 (12)0.5884 (2)0.67018 (19)0.0152 (6)
C60.57153 (12)0.4666 (2)0.6708 (2)0.0211 (7)
C70.58217 (14)0.3944 (2)0.7130 (3)0.0292 (8)
C80.77533 (12)0.6480 (2)0.6861 (2)0.0254 (7)
C90.79942 (16)0.5945 (3)0.7362 (3)0.0312 (8)
C100.53142 (13)0.6307 (3)0.6226 (2)0.0249 (7)
C110.53103 (12)0.6304 (2)0.7043 (2)0.0204 (6)
C120.51882 (17)0.7085 (3)0.7372 (2)0.0265 (7)
C130.60371 (15)0.5215 (3)0.8653 (3)0.0375 (9)
C140.56576 (14)0.5507 (3)0.8252 (2)0.0289 (8)
C150.53528 (16)0.6012 (3)0.8770 (2)0.0394 (11)
C160.71978 (15)0.7860 (3)0.6111 (3)0.0268 (8)
C170.72087 (14)0.7999 (2)0.6949 (2)0.0258 (7)
C180.69358 (16)0.8684 (3)0.7161 (3)0.0340 (9)
C190.72534 (15)0.6483 (3)0.8757 (2)0.0344 (9)
C200.73332 (13)0.7196 (2)0.8314 (2)0.0259 (7)
C210.72384 (16)0.7883 (3)0.8780 (3)0.0311 (8)
C220.61914 (13)0.7353 (3)0.6708 (3)0.0258 (8)
C230.62760 (15)0.7061 (3)0.8289 (3)0.0305 (8)
Fe20.40299 (3)0.85264 (5)0.75093 (3)0.0130 (2)
P30.39556 (4)0.83737 (7)0.63337 (7)0.0159 (3)
P40.40285 (4)0.83730 (7)0.86930 (7)0.0156 (3)
O30.48504 (15)0.9239 (3)0.74327 (15)0.0298 (12)
O40.33607 (13)0.9601 (3)0.75961 (17)0.0255 (12)
N50.39999 (12)0.7411 (2)0.62381 (19)0.0124 (6)
N40.40365 (16)0.7366 (2)0.75086 (13)0.0082 (4)
N60.40653 (14)0.7413 (2)0.87854 (19)0.0161 (6)
C240.40474 (13)0.7012 (2)0.6869 (2)0.0108 (6)
C250.41223 (14)0.6241 (2)0.6842 (3)0.0162 (6)
C260.41671 (17)0.5877 (3)0.75015 (18)0.0168 (5)
C270.41598 (14)0.6240 (3)0.8158 (3)0.0164 (6)
C280.40856 (15)0.7012 (3)0.8146 (2)0.0141 (6)
C290.39823 (15)0.7041 (2)0.5522 (2)0.0222 (9)
C300.35750 (15)0.6619 (3)0.5399 (2)0.0291 (10)
C310.41028 (17)0.7031 (3)0.9497 (2)0.0254 (8)
C320.37076 (18)0.6578 (3)0.9697 (3)0.0380 (10)
C330.47683 (15)0.8340 (3)0.5704 (3)0.0291 (10)
C340.43430 (13)0.8738 (2)0.5652 (2)0.0163 (8)
C350.44242 (18)0.9588 (3)0.5783 (3)0.0319 (10)
C360.30817 (13)0.8176 (3)0.6280 (2)0.0247 (9)
C370.34587 (15)0.8557 (3)0.5845 (3)0.0270 (9)
C380.33621 (16)0.9339 (3)0.5665 (3)0.0345 (10)
C390.48833 (15)0.8318 (3)0.9099 (2)0.0285 (10)
C400.44627 (16)0.8714 (2)0.9289 (3)0.0249 (9)
C410.45098 (16)0.9563 (3)0.9225 (3)0.0286 (10)
C420.31657 (16)0.8236 (3)0.8940 (3)0.0310 (10)
C430.35658 (13)0.8646 (3)0.9237 (2)0.0208 (9)
C440.3574 (2)0.8641 (4)1.0053 (3)0.0304 (15)0.612 (8)
C450.45452 (18)0.8911 (3)0.74581 (17)0.0152 (5)
C460.36151 (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)
H210.6380550.4361780.6026960.0253*
H310.7090960.4423620.5653660.0252*
H410.7528540.5360640.6117010.0247*
H610.5426830.479680.6794260.0253*
H620.5723020.4569990.6190860.0253*
H710.56390.3551750.6969130.035*
H720.5783050.4024120.7645160.035*
H730.6108820.3807950.7036880.035*
H810.7811310.6360930.6358630.0305*
H820.7854620.6976610.693530.0305*
H910.828820.5959420.7242060.0374*
H920.7889290.5450120.7293950.0374*
H930.7955880.609110.7862990.0374*
H1010.5398060.5826460.6050990.0299*
H1020.5509460.6674330.6055230.0299*
H1030.5037620.642060.6047560.0299*
H1110.5100110.5944320.717220.0245*
H1210.5267960.7103480.7878570.0318*
H1220.4889920.7157280.732970.0318*
H1230.5332470.7468930.7107610.0318*
H1310.6281050.5261710.8346360.045*
H1320.5993880.4702480.8774090.045*
H1330.6078250.5496370.9093860.045*
H1410.5491150.5088330.8103930.0346*
H1510.5165190.6296540.8468760.0472*
H1520.5521620.6342040.9060480.0472*
H1530.5192160.5694820.9087220.0472*
H1610.7383950.7457830.5990590.0322*
H1620.7286170.8300250.5858050.0322*
H1630.6916460.7734190.5964270.0322*
H1710.7493190.810790.7089940.0309*
H1810.6922540.8725390.7684720.0408*
H1820.6656830.8623250.6968530.0408*
H1830.7059650.9125570.6960710.0408*
H1910.7183360.6085320.8429040.0413*
H1920.7024640.6563260.9091140.0413*
H1930.7502290.6355930.9027060.0413*
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H2110.7271310.8321180.8486080.0374*
H2120.7429740.7901840.9185940.0374*
H2130.695480.7856170.8958510.0374*
H2510.4141190.5981090.6384390.0194*
H2610.4204960.5348350.7499210.0201*
H2710.4203490.5979890.8610570.0197*
H2910.4216090.6706540.547520.0266*
H2920.4017990.7402340.5140410.0266*
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H3320.4849150.829760.6209030.0349*
H3330.4977230.8619780.5443360.0349*
H3410.4223060.8652190.5176580.0196*
H3510.4170420.9860860.5688710.0383*
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H3530.4509480.9665750.6281730.0383*
H3610.314250.7658690.6350280.0297*
H3620.282630.8226580.6003390.0297*
H3630.3048950.841260.674710.0297*
H3710.3495940.8338970.5369670.0324*
H3810.3528040.9492140.5252560.0414*
H3820.3426650.964840.6078390.0414*
H3830.306880.9385270.5547620.0414*
H3910.4915070.8292880.8576890.0342*
H3920.4880480.7824280.9297770.0342*
H3930.5113930.8590990.9305370.0342*
H4010.4392650.8598610.9787290.0299*
H4110.4241490.979430.9303890.0343*
H4120.4611070.9687250.8745270.0343*
H4130.4706130.9735830.9586240.0343*
H4210.3112690.8388050.84450.0372*
H4220.2927570.8358930.9240160.0372*
H4230.3211590.7709230.8953920.0372*
H4310.3563780.9172880.9157110.025*0.612 (8)
H4410.3329320.8890641.0237250.0364*0.612 (8)
H4420.3822510.8892081.0221760.0364*0.612 (8)
H4430.3576550.8137621.0225050.0364*0.612 (8)
H21'0.1383580.8079890.907780.0253*
H31'0.2096830.8033390.9390020.0252*
H41'0.2532960.7106620.8889370.0247*
H61'0.0430150.770340.8242640.0253*
H62'0.0721960.7887760.8867520.0253*
H71'0.0708270.8962010.8252290.035*
H72'0.0718740.8564580.7488810.035*
H73'0.1129060.8615660.796260.035*
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H82'0.2844830.5516740.7984920.0305*
H91'0.327850.6608610.7829560.0374*
H92'0.2863490.7059210.7696430.0374*
H93'0.2997330.643510.7145320.0374*
H101'0.0344460.6620050.8980280.0299*
H102'0.0521730.5809040.8937090.0299*
H103'0.0034470.5944420.8937020.0299*
H111'0.0100520.6549550.7796520.0245*
H121'0.0276810.5426540.7102280.0318*
H122'0.0103410.5358820.7645080.0318*
H123'0.0339960.5052840.7869720.0318*
H131'0.1217760.7643290.66950.045*
H132'0.0976280.7632280.5946550.045*
H133'0.122930.6931350.6201620.045*
H141'0.0497260.7450290.6930060.0346*
H151'0.00930.6638780.6451980.0472*
H152'0.0467280.6150310.6168290.0472*
H153'0.0363030.6906440.5783850.0472*
H161'0.2377470.4997190.8936780.0322*
H162'0.227670.4150480.9030360.0322*
H163'0.1909090.4724250.894470.0322*
H171'0.2488920.4424350.7816780.0309*
H181'0.1923560.3790290.7241950.0408*
H182'0.1668840.3860060.7973840.0408*
H183'0.2080770.3381970.7948940.0408*
H191'0.2322350.649590.6491420.0413*
H192'0.1946270.6107160.6089440.0413*
H193'0.2400560.6066150.5757450.0413*
H201'0.261770.5355340.6754770.031*
H211'0.2349310.4235460.6403230.0374*
H212'0.2352670.4720120.5690230.0374*
H213'0.1931680.4600160.6121680.0374*
H251'0.080460.3540010.364720.0194*
H261'0.0753760.2859280.2536620.0201*
H271'0.0877550.3486480.1424490.0197*
H291'0.0819230.4985640.4863060.0266*
H292'0.0643910.4304240.4507620.0266*
H301'0.1229540.4010320.523010.035*
H302'0.1513760.4499520.4720720.035*
H303'0.1309820.376920.4417190.035*
H311'0.073150.4220350.0514550.0305*
H313'0.0920980.4873160.0141010.0305*
H321'0.1348810.3911750.0160870.0456*
H322'0.1376130.3639290.0653020.0456*
H323'0.1613630.4361760.0411440.0456*
H331'0.0184140.5342430.415860.0349*
H332'0.0011970.5996040.3677440.0349*
H333'0.0063440.5996690.4525770.0349*
H341'0.0620650.6196540.4748740.0196*
H351'0.0713150.7382180.4309830.0383*
H352'0.0228320.7277930.4430020.0383*
H353'0.0418250.7224310.3639550.0383*
H361'0.174620.5262080.372140.0297*
H362'0.20390.5700520.4260180.0297*
H363'0.1921120.604390.3498540.0297*
H371'0.1401290.5877790.4697430.0324*
H381'0.128560.7149870.4615350.0414*
H382'0.1582630.7194150.393140.0414*
H383'0.1768210.6992610.4701510.0414*
H391'0.0251130.5353920.0756880.0342*
H392'0.0052630.6015520.03190.0342*
H393'0.0094380.6063110.1173050.0342*
H401'0.0736870.6078350.0169410.0299*
H411'0.0926240.7251460.0650110.0343*
H412'0.0515070.7228820.1123820.0343*
H413'0.0484710.7253820.0267370.0343*
H421'0.2164030.5842120.1128660.0372*
H422'0.187040.514560.1191060.0372*
H423'0.1867580.5750010.1808730.0372*
H431'0.1585460.659740.0976010.025*0.747 (8)
H441'0.1413470.6404150.0127960.0364*0.747 (8)
H442'0.1549410.5568380.009050.0364*0.747 (8)
H443'0.1889710.6196310.0038690.0364*0.747 (8)
C44b0.3495 (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)
H441b0.3697560.9538340.9817810.0288*0.388
H442b0.3216350.9445280.965290.0288*0.388
H443b0.3522130.9718020.9035330.0288*0.388
H441b'0.1782590.7143350.1073570.0288*0.2528
H442b'0.1365610.7136880.0615030.0288*0.2528
H443b'0.1793120.6919950.0244110.0288*0.2528
H431b0.3643460.8478620.9717470.025*0.388
H431b'0.1566010.5869340.0415420.025*0.2528
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0110 (3)0.0134 (4)0.0254 (3)0.0025 (3)0.0016 (2)0.0022 (2)
P10.0166 (7)0.0167 (7)0.0228 (6)0.0010 (6)0.0002 (4)0.0021 (4)
P20.0121 (7)0.0174 (7)0.0190 (6)0.0001 (6)0.0021 (4)0.0045 (4)
O10.042 (2)0.136 (5)0.0243 (18)0.042 (3)0.0038 (17)0.012 (2)
O20.0267 (19)0.055 (2)0.051 (2)0.0186 (17)0.0201 (16)0.0261 (19)
N20.0139 (9)0.0169 (9)0.0270 (10)0.0049 (7)0.0019 (8)0.0016 (7)
N10.0135 (9)0.0164 (9)0.0203 (9)0.0014 (7)0.0018 (7)0.0020 (7)
N30.0115 (9)0.0196 (9)0.0248 (10)0.0019 (7)0.0013 (7)0.0048 (8)
C10.0177 (11)0.0131 (9)0.0182 (10)0.0010 (8)0.0014 (9)0.0003 (8)
C20.0221 (12)0.0172 (11)0.0239 (12)0.0013 (9)0.0030 (9)0.0072 (9)
C30.0245 (12)0.0182 (11)0.0202 (11)0.0049 (9)0.0018 (9)0.0048 (9)
C40.0165 (11)0.0214 (11)0.0237 (11)0.0037 (9)0.0018 (9)0.0032 (9)
C50.0153 (10)0.0154 (10)0.0148 (9)0.0002 (8)0.0025 (8)0.0022 (7)
C60.0179 (11)0.0168 (10)0.0287 (12)0.0030 (9)0.0050 (9)0.0020 (9)
C70.0179 (12)0.0183 (12)0.0513 (17)0.0046 (9)0.0065 (12)0.0035 (11)
C80.0130 (11)0.0284 (13)0.0348 (14)0.0026 (9)0.0025 (10)0.0094 (10)
C90.0140 (11)0.0330 (13)0.0466 (17)0.0077 (9)0.0031 (11)0.0109 (11)
C100.0216 (12)0.0291 (13)0.0241 (12)0.0029 (10)0.0036 (10)0.0003 (10)
C110.0189 (12)0.0238 (11)0.0185 (10)0.0032 (9)0.0020 (9)0.0020 (9)
C120.0169 (11)0.0235 (11)0.0391 (15)0.0052 (9)0.0035 (10)0.0044 (10)
C130.0371 (16)0.0417 (17)0.0336 (15)0.0066 (13)0.0100 (12)0.0172 (13)
C140.0264 (14)0.0392 (15)0.0210 (12)0.0056 (11)0.0044 (10)0.0084 (10)
C150.0343 (16)0.072 (3)0.0116 (11)0.0115 (16)0.0019 (11)0.0025 (13)
C160.0264 (14)0.0267 (14)0.0274 (14)0.0042 (11)0.0052 (11)0.0055 (11)
C170.0224 (13)0.0175 (11)0.0374 (14)0.0039 (9)0.0027 (11)0.0012 (10)
C180.0284 (14)0.0186 (12)0.0551 (17)0.0006 (10)0.0012 (13)0.0034 (12)
C190.0296 (15)0.0445 (17)0.0292 (14)0.0004 (13)0.0075 (12)0.0028 (12)
C200.0236 (13)0.0312 (14)0.0227 (12)0.0032 (10)0.0015 (10)0.0053 (10)
C210.0264 (14)0.0359 (16)0.0311 (14)0.0049 (12)0.0009 (11)0.0162 (12)
C220.0103 (11)0.0201 (12)0.0469 (16)0.0069 (9)0.0116 (11)0.0089 (11)
C230.0233 (14)0.0305 (14)0.0378 (15)0.0117 (11)0.0033 (11)0.0032 (12)
Fe20.0161 (4)0.0049 (3)0.0181 (4)0.0030 (4)0.00081 (19)0.00054 (17)
P30.0181 (6)0.0103 (5)0.0193 (5)0.0036 (4)0.0001 (4)0.0016 (4)
P40.0182 (6)0.0102 (5)0.0183 (5)0.0009 (4)0.0007 (4)0.0000 (4)
O30.040 (2)0.026 (2)0.0232 (16)0.0103 (19)0.0004 (13)0.0030 (13)
O40.0194 (19)0.030 (2)0.0273 (17)0.0124 (18)0.0059 (12)0.0081 (14)
N50.0181 (13)0.0073 (9)0.0119 (8)0.0002 (9)0.0026 (8)0.0031 (7)
N40.0089 (8)0.0031 (8)0.0127 (7)0.0023 (6)0.0007 (7)0.0009 (6)
N60.0259 (12)0.0099 (8)0.0126 (8)0.0032 (8)0.0025 (8)0.0011 (7)
C240.0071 (11)0.0111 (10)0.0143 (9)0.0004 (8)0.0020 (8)0.0038 (7)
C250.0199 (13)0.0078 (10)0.0210 (11)0.0013 (9)0.0023 (9)0.0060 (8)
C260.0175 (10)0.0064 (7)0.0264 (10)0.0015 (7)0.0001 (10)0.0001 (10)
C270.0197 (12)0.0103 (10)0.0193 (11)0.0017 (9)0.0008 (9)0.0039 (8)
C280.0147 (11)0.0100 (10)0.0175 (10)0.0004 (8)0.0011 (8)0.0008 (8)
C290.038 (2)0.0150 (12)0.0139 (10)0.0015 (14)0.0055 (13)0.0064 (9)
C300.040 (2)0.0235 (14)0.0242 (15)0.0027 (15)0.0090 (14)0.0087 (11)
C310.045 (2)0.0163 (12)0.0155 (11)0.0043 (12)0.0007 (12)0.0047 (9)
C320.064 (2)0.0214 (13)0.0282 (14)0.0023 (14)0.0192 (15)0.0088 (10)
C330.0282 (19)0.0273 (15)0.0316 (18)0.0010 (14)0.0147 (14)0.0045 (13)
C340.0250 (18)0.0154 (12)0.0084 (11)0.0020 (12)0.0020 (11)0.0019 (9)
C350.054 (2)0.0188 (13)0.0230 (14)0.0039 (14)0.0142 (14)0.0028 (10)
C360.0114 (15)0.0268 (15)0.0359 (18)0.0023 (13)0.0062 (13)0.0016 (14)
C370.0355 (19)0.0239 (13)0.0216 (13)0.0109 (14)0.0138 (13)0.0011 (10)
C380.041 (2)0.0306 (16)0.0317 (15)0.0152 (15)0.0072 (14)0.0059 (12)
C390.032 (2)0.0274 (16)0.0257 (17)0.0001 (15)0.0116 (14)0.0029 (13)
C400.040 (2)0.0159 (12)0.0185 (12)0.0019 (13)0.0092 (13)0.0006 (10)
C410.048 (2)0.0168 (12)0.0207 (14)0.0049 (15)0.0073 (14)0.0038 (11)
C420.0286 (17)0.0313 (17)0.033 (2)0.0049 (14)0.0173 (15)0.0046 (16)
C430.0226 (18)0.0205 (14)0.0193 (14)0.0014 (13)0.0058 (12)0.0076 (11)
C440.047 (3)0.025 (2)0.019 (2)0.009 (2)0.019 (2)0.0012 (16)
C450.0235 (10)0.0112 (9)0.0108 (9)0.0027 (7)0.0023 (11)0.0025 (11)
C460.0178 (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—P12.1990 (19)P1'—C11'1.858 (4)
Fe1—P22.1962 (18)P1'—C14'1.865 (4)
Fe1—N12.049 (3)P2'—N3'1.733 (4)
Fe1—C221.798 (5)P2'—C17'1.857 (4)
Fe1—C231.692 (5)P2'—C20'1.870 (4)
P1—N21.733 (4)O1'—C22'1.071 (5)
P1—C111.870 (4)O2'—C23'1.106 (6)
P1—C141.823 (4)N2'—C1'1.378 (5)
P2—N31.713 (4)N2'—C6'1.465 (5)
P2—C171.877 (4)N1'—C1'1.369 (5)
P2—C201.841 (4)N1'—C5'1.364 (5)
O1—C221.064 (7)N3'—C5'1.365 (5)
O2—C231.097 (6)N3'—C8'1.477 (5)
N2—C11.368 (5)C1'—C2'1.396 (5)
N2—C61.467 (5)C2'—C3'1.377 (6)
N1—C11.370 (5)C2'—H21'0.96
N1—C51.370 (5)C3'—C4'1.384 (6)
N3—C51.383 (5)C3'—H31'0.96
N3—C81.476 (5)C4'—C5'1.412 (5)
C1—C21.380 (5)C4'—H41'0.96
C2—C31.399 (6)C6'—C7'1.524 (6)
C2—H210.96C6'—H61'0.96
C3—C41.372 (6)C6'—H62'0.96
C3—H310.96C7'—H71'0.96
C4—C51.403 (5)C7'—H72'0.96
C4—H410.96C7'—H73'0.96
C6—C71.549 (6)C8'—C9'1.540 (7)
C6—H610.96C8'—H81'0.96
C6—H620.96C8'—H82'0.96
C7—H710.96C9'—H91'0.96
C7—H720.96C9'—H92'0.96
C7—H730.96C9'—H93'0.96
C8—C91.534 (7)C10'—C11'1.541 (5)
C8—H810.96C10'—H101'0.96
C8—H820.96C10'—H102'0.96
C9—H910.96C10'—H103'0.96
C9—H920.96C11'—C12'1.512 (7)
C9—H930.96C11'—H111'0.96
C10—C111.491 (5)C12'—H121'0.96
C10—H1010.96C12'—H122'0.96
C10—H1020.96C12'—H123'0.96
C10—H1030.96C13'—C14'1.547 (7)
C11—H1110.96C13'—H131'0.96
C12—H1210.96C13'—H132'0.96
C12—H1220.96C13'—H133'0.96
C12—H1230.96C14'—C15'1.492 (6)
C13—C141.505 (6)C14'—H141'0.96
C13—H1310.96C15'—H151'0.96
C13—H1320.96C15'—H152'0.96
C13—H1330.96C15'—H153'0.96
C14—H1410.96C16'—C17'1.511 (6)
C15—H1510.96C16'—H161'0.96
C15—H1520.96C16'—H162'0.96
C15—H1530.96C16'—H163'0.96
C16—C171.553 (6)C17'—C18'1.531 (6)
C16—H1610.96C17'—H171'0.96
C16—H1620.96C18'—H181'0.96
C16—H1630.96C18'—H182'0.96
C17—C181.557 (6)C18'—H183'0.96
C17—H1710.96C19'—C20'1.522 (6)
C18—H1810.96C19'—H191'0.96
C18—H1820.96C19'—H192'0.96
C18—H1830.96C19'—H193'0.96
C19—C201.538 (6)C20'—C21'1.553 (7)
C19—H1910.96C20'—H201'0.96
C19—H1920.96C21'—H211'0.96
C19—H1930.96C21'—H212'0.96
C20—C211.531 (7)C21'—H213'0.96
C20—H2010.96Fe2'—P3'2.1701 (12)
C21—H2110.96Fe2'—P4'2.1728 (13)
C21—H2120.96Fe2'—N4'1.970 (4)
C21—H2130.96Fe2'—C45'1.752 (6)
Fe2—P32.1772 (14)Fe2'—C46'1.743 (6)
Fe2—P42.1793 (14)P3'—N5'1.701 (4)
Fe2—N42.091 (4)P3'—C34'1.855 (4)
Fe2—C451.781 (6)P3'—C37'1.870 (5)
Fe2—C461.721 (6)P4'—N6'1.696 (4)
P3—N51.749 (4)P4'—C40'1.853 (5)
P3—C341.870 (4)P4'—C43'1.863 (4)
P3—C371.843 (5)O3'—C45'1.166 (7)
P4—N61.740 (4)O4'—C46'1.167 (8)
P4—C401.862 (5)N5'—C24'1.386 (5)
P4—C431.842 (4)N5'—C29'1.478 (5)
O3—C451.136 (8)N4'—C24'1.396 (5)
O4—C461.163 (8)N4'—C28'1.387 (5)
N5—C241.365 (5)N6'—C28'1.404 (6)
N5—C291.470 (5)N6'—C31'1.477 (6)
N4—C241.331 (5)C24'—C25'1.379 (6)
N4—C281.336 (5)C25'—C26'1.397 (6)
N6—C281.374 (6)C25'—H251'0.96
N6—C311.476 (6)C26'—C27'1.385 (6)
C24—C251.410 (6)C26'—H261'0.96
C25—C261.379 (6)C27'—C28'1.381 (6)
C25—H2510.96C27'—H271'0.96
C26—C271.366 (6)C29'—C30'1.514 (7)
C26—H2610.96C29'—H291'0.96
C27—C281.411 (6)C29'—H292'0.96
C27—H2710.96C30'—H301'0.96
C29—C301.517 (7)C30'—H302'0.96
C29—H2910.96C30'—H303'0.96
C29—H2920.96C31'—C32'1.526 (8)
C30—H3010.96C31'—H311'0.96
C30—H3020.96C31'—H313'0.96
C30—H3030.96C32'—H321'0.96
C31—C321.541 (8)C32'—H322'0.96
C31—H3110.96C32'—H323'0.96
C31—H3130.96C33'—C34'1.494 (7)
C32—H3210.96C33'—H331'0.96
C32—H3220.96C33'—H332'0.96
C32—H3230.96C33'—H333'0.96
C33—C341.533 (6)C34'—C35'1.541 (6)
C33—H3310.96C34'—H341'0.96
C33—H3320.96C35'—H351'0.96
C33—H3330.96C35'—H352'0.96
C34—C351.572 (6)C35'—H353'0.96
C34—H3410.96C36'—C37'1.469 (7)
C35—H3510.96C36'—H361'0.96
C35—H3520.96C36'—H362'0.96
C35—H3530.96C36'—H363'0.96
C36—H3610.96C37'—C38'1.558 (7)
C36—H3620.96C37'—H371'0.96
C36—H3630.96C38'—H381'0.96
C37—C381.480 (7)C38'—H382'0.96
C37—H3710.96C38'—H383'0.96
C38—H3810.96C39'—C40'1.491 (7)
C38—H3820.96C39'—H391'0.96
C38—H3830.96C39'—H392'0.96
C39—C401.555 (7)C39'—H393'0.96
C39—H3910.96C40'—C41'1.516 (6)
C39—H3920.96C40'—H401'0.96
C39—H3930.96C41'—H411'0.96
C40—C411.540 (6)C41'—H412'0.96
C40—H4010.96C41'—H413'0.96
C41—H4110.96C42'—C43'1.476 (7)
C41—H4120.96C42'—H421'0.96
C41—H4130.96C42'—H422'0.96
C42—C431.568 (7)C42'—H423'0.96
C42—H4210.96C43'—C44'1.493 (6)
C42—H4220.96C43'—H431'0.96
C42—H4230.96C43'—C44b'1.554 (17)
C43—C441.490 (7)C43'—H431b'0.96
C43—H4310.96C44'—H441'0.96
C43—C44b1.430 (12)C44'—H442'0.96
C43—H431b0.96C44'—H443'0.96
C44—H4410.96C44'—H431b'0.7001
C44—H4420.96H431—C44b0.7121
C44—H4430.96H431'—C44b'0.7675
C44—H431b0.7135C44b—H441b0.96
Fe1'—P1'2.1801 (17)C44b—H442b0.96
Fe1'—P2'2.1922 (17)C44b—H443b0.96
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—P2161.16 (8)C17'—P2'—C20'103.4 (2)
P1—Fe1—N181.85 (10)P1'—N2'—C1'117.5 (3)
P1—Fe1—C2296.03 (15)P1'—N2'—C6'122.9 (3)
P1—Fe1—C2391.71 (17)C1'—N2'—C6'119.5 (3)
P2—Fe1—N182.38 (10)Fe1'—N1'—C1'120.2 (2)
P2—Fe1—C2298.03 (15)Fe1'—N1'—C5'121.2 (2)
P2—Fe1—C2393.59 (16)C1'—N1'—C5'118.0 (3)
N1—Fe1—C22105.31 (18)P2'—N3'—C5'117.8 (3)
N1—Fe1—C23139.51 (19)P2'—N3'—C8'121.9 (3)
C22—Fe1—C23115.1 (2)C5'—N3'—C8'120.1 (3)
Fe1—P1—N2102.25 (13)N2'—C1'—N1'115.6 (3)
Fe1—P1—C11122.03 (16)N2'—C1'—C2'122.7 (3)
Fe1—P1—C14123.51 (15)N1'—C1'—C2'121.8 (3)
N2—P1—C11103.06 (17)C1'—C2'—C3'119.3 (4)
N2—P1—C14100.9 (2)C1'—C2'—H21'120.36
C11—P1—C14101.3 (2)C3'—C2'—H21'120.36
Fe1—P2—N3102.79 (13)C2'—C3'—C4'120.5 (4)
Fe1—P2—C17122.04 (15)C2'—C3'—H31'119.78
Fe1—P2—C20121.52 (14)C4'—C3'—H31'119.77
N3—P2—C17101.82 (18)C3'—C4'—C5'118.1 (4)
N3—P2—C20102.15 (19)C3'—C4'—H41'120.96
C17—P2—C20103.0 (2)C5'—C4'—H41'120.96
P1—N2—C1117.4 (3)N1'—C5'—N3'115.8 (3)
P1—N2—C6122.6 (3)N1'—C5'—C4'122.2 (3)
C1—N2—C6119.4 (3)N3'—C5'—C4'122.0 (3)
Fe1—N1—C1120.8 (2)N2'—C6'—C7'114.9 (3)
Fe1—N1—C5120.3 (2)N2'—C6'—H61'109.47
C1—N1—C5118.2 (3)N2'—C6'—H62'109.47
P2—N3—C5117.5 (3)C7'—C6'—H61'109.47
P2—N3—C8122.5 (3)C7'—C6'—H62'109.47
C5—N3—C8120.0 (3)H61'—C6'—H62'103.47
N2—C1—N1116.1 (3)C6'—C7'—H71'109.47
N2—C1—C2122.5 (4)C6'—C7'—H72'109.47
N1—C1—C2121.4 (3)C6'—C7'—H73'109.47
C1—C2—C3119.7 (4)H71'—C7'—H72'109.47
C1—C2—H21120.17H71'—C7'—H73'109.47
C3—C2—H21120.17H72'—C7'—H73'109.47
C2—C3—C4120.1 (4)N3'—C8'—C9'112.7 (3)
C2—C3—H31119.96N3'—C8'—H81'109.47
C4—C3—H31119.97N3'—C8'—H82'109.47
C3—C4—C5118.2 (4)C9'—C8'—H81'109.47
C3—C4—H41120.9C9'—C8'—H82'109.47
C5—C4—H41120.91H81'—C8'—H82'106
N1—C5—N3116.0 (3)C8'—C9'—H91'109.47
N1—C5—C4122.4 (3)C8'—C9'—H92'109.47
N3—C5—C4121.6 (3)C8'—C9'—H93'109.47
N2—C6—C7115.0 (3)H91'—C9'—H92'109.47
N2—C6—H61109.47H91'—C9'—H93'109.47
N2—C6—H62109.47H92'—C9'—H93'109.47
C7—C6—H61109.47C11'—C10'—H101'109.47
C7—C6—H62109.47C11'—C10'—H102'109.47
H61—C6—H62103.31C11'—C10'—H103'109.47
C6—C7—H71109.47H101'—C10'—H102'109.47
C6—C7—H72109.47H101'—C10'—H103'109.47
C6—C7—H73109.47H102'—C10'—H103'109.47
H71—C7—H72109.47P1'—C11'—C10'112.4 (3)
H71—C7—H73109.47P1'—C11'—C12'109.2 (3)
H72—C7—H73109.47P1'—C11'—H111'107.77
N3—C8—C9112.5 (3)C10'—C11'—C12'109.9 (3)
N3—C8—H81109.47C10'—C11'—H111'107.11
N3—C8—H82109.47C12'—C11'—H111'110.42
C9—C8—H81109.47C11'—C12'—H121'109.47
C9—C8—H82109.47C11'—C12'—H122'109.47
H81—C8—H82106.21C11'—C12'—H123'109.47
C8—C9—H91109.47H121'—C12'—H122'109.47
C8—C9—H92109.47H121'—C12'—H123'109.47
C8—C9—H93109.47H122'—C12'—H123'109.47
H91—C9—H92109.47C14'—C13'—H131'109.47
H91—C9—H93109.47C14'—C13'—H132'109.47
H92—C9—H93109.47C14'—C13'—H133'109.47
C11—C10—H101109.47H131'—C13'—H132'109.47
C11—C10—H102109.47H131'—C13'—H133'109.47
C11—C10—H103109.47H132'—C13'—H133'109.47
H101—C10—H102109.47P1'—C14'—C13'109.4 (3)
H101—C10—H103109.47P1'—C14'—C15'114.7 (3)
H102—C10—H103109.47P1'—C14'—H141'106.96
P1—C11—C10112.7 (3)C13'—C14'—C15'112.5 (3)
P1—C11—H111109.31C13'—C14'—H141'109.44
C10—C11—H111104.73C15'—C14'—H141'103.44
H121—C12—H122109.47C14'—C15'—H151'109.47
H121—C12—H123109.47C14'—C15'—H152'109.47
H122—C12—H123109.47C14'—C15'—H153'109.47
C14—C13—H131109.47H151'—C15'—H152'109.47
C14—C13—H132109.47H151'—C15'—H153'109.47
C14—C13—H133109.47H152'—C15'—H153'109.47
H131—C13—H132109.47C17'—C16'—H161'109.47
H131—C13—H133109.47C17'—C16'—H162'109.47
H132—C13—H133109.47C17'—C16'—H163'109.47
P1—C14—C13109.5 (3)H161'—C16'—H162'109.47
P1—C14—H141109.49H161'—C16'—H163'109.47
C13—C14—H141107.74H162'—C16'—H163'109.47
H151—C15—H152109.47P2'—C17'—C16'110.4 (3)
H151—C15—H153109.47P2'—C17'—C18'112.4 (3)
H152—C15—H153109.47P2'—C17'—H171'106.67
C17—C16—H161109.47C16'—C17'—C18'109.1 (4)
C17—C16—H162109.47C16'—C17'—H171'110.14
C17—C16—H163109.47C18'—C17'—H171'108.05
H161—C16—H162109.47C17'—C18'—H181'109.47
H161—C16—H163109.47C17'—C18'—H182'109.47
H162—C16—H163109.47C17'—C18'—H183'109.47
P2—C17—C16110.1 (3)H181'—C18'—H182'109.47
P2—C17—C18111.3 (3)H181'—C18'—H183'109.47
P2—C17—H171108.37H182'—C18'—H183'109.47
C16—C17—C18111.2 (4)C20'—C19'—H191'109.47
C16—C17—H171108.52C20'—C19'—H192'109.47
C18—C17—H171107.26C20'—C19'—H193'109.47
C17—C18—H181109.47H191'—C19'—H192'109.47
C17—C18—H182109.47H191'—C19'—H193'109.47
C17—C18—H183109.47H192'—C19'—H193'109.47
H181—C18—H182109.47P2'—C20'—C19'110.9 (3)
H181—C18—H183109.47P2'—C20'—C21'111.3 (3)
H182—C18—H183109.47P2'—C20'—H201'107.94
C20—C19—H191109.47C19'—C20'—C21'111.5 (4)
C20—C19—H192109.47C19'—C20'—H201'107.75
C20—C19—H193109.47C21'—C20'—H201'107.22
H191—C19—H192109.47C20'—C21'—H211'109.47
H191—C19—H193109.47C20'—C21'—H212'109.47
H192—C19—H193109.47C20'—C21'—H213'109.47
P2—C20—C19108.8 (3)H211'—C21'—H212'109.47
P2—C20—C21114.4 (3)H211'—C21'—H213'109.47
P2—C20—H201106.91H212'—C21'—H213'109.47
C19—C20—C21110.5 (4)Fe1'—C22'—O1'171.8 (4)
C19—C20—H201111.11Fe1'—C23'—O2'174.1 (4)
C21—C20—H201105.03P3'—Fe2'—P4'164.48 (6)
C20—C21—H211109.47P3'—Fe2'—N4'83.40 (8)
C20—C21—H212109.47P3'—Fe2'—C45'96.51 (11)
C20—C21—H213109.47P3'—Fe2'—C46'92.38 (11)
H211—C21—H212109.47P4'—Fe2'—N4'82.78 (8)
H211—C21—H213109.47P4'—Fe2'—C45'95.32 (11)
H212—C21—H213109.47P4'—Fe2'—C46'91.37 (11)
Fe1—C22—O1171.9 (5)N4'—Fe2'—C45'112.8 (2)
Fe1—C23—O2175.7 (5)N4'—Fe2'—C46'131.0 (3)
P3—Fe2—P4164.12 (6)C45'—Fe2'—C46'116.2 (3)
P3—Fe2—N482.77 (8)Fe2'—P3'—N5'101.98 (12)
P3—Fe2—C4595.57 (11)Fe2'—P3'—C34'121.86 (13)
P3—Fe2—C4692.80 (12)Fe2'—P3'—C37'121.81 (16)
P4—Fe2—N482.75 (8)N5'—P3'—C34'102.49 (18)
P4—Fe2—C4595.92 (11)N5'—P3'—C37'100.9 (2)
P4—Fe2—C4691.63 (11)C34'—P3'—C37'103.9 (2)
N4—Fe2—C45112.3 (2)Fe2'—P4'—N6'102.90 (13)
N4—Fe2—C46130.4 (2)Fe2'—P4'—C40'121.78 (16)
C45—Fe2—C46117.3 (3)Fe2'—P4'—C43'118.12 (14)
Fe2—P3—N5102.42 (13)N6'—P4'—C40'103.1 (2)
Fe2—P3—C34122.76 (14)N6'—P4'—C43'103.8 (2)
Fe2—P3—C37123.20 (16)C40'—P4'—C43'104.6 (2)
N5—P3—C34103.18 (18)P3'—N5'—C24'118.8 (3)
N5—P3—C37101.4 (2)P3'—N5'—C29'122.8 (3)
C34—P3—C37100.3 (2)C24'—N5'—C29'118.3 (3)
Fe2—P4—N6102.82 (13)Fe2'—N4'—C24'122.4 (3)
Fe2—P4—C40122.44 (16)Fe2'—N4'—C28'123.2 (3)
Fe2—P4—C43120.19 (15)C24'—N4'—C28'114.1 (4)
N6—P4—C40102.8 (2)P4'—N6'—C28'117.7 (3)
N6—P4—C43105.5 (2)P4'—N6'—C31'124.7 (3)
C40—P4—C43100.8 (2)C28'—N6'—C31'117.4 (4)
P3—N5—C24116.5 (3)N5'—C24'—N4'112.9 (4)
P3—N5—C29122.4 (3)N5'—C24'—C25'122.7 (4)
C24—N5—C29121.1 (4)N4'—C24'—C25'124.4 (4)
Fe2—N4—C24118.6 (3)C24'—C25'—C26'119.2 (4)
Fe2—N4—C28118.5 (3)C24'—C25'—H251'120.41
C24—N4—C28122.3 (4)C26'—C25'—H251'120.41
P4—N6—C28116.3 (3)C25'—C26'—C27'118.3 (5)
P4—N6—C31123.7 (3)C25'—C26'—H261'120.84
C28—N6—C31119.9 (4)C27'—C26'—H261'120.84
N5—C24—N4119.1 (4)C26'—C27'—C28'120.1 (4)
N5—C24—C25120.5 (4)C26'—C27'—H271'119.93
N4—C24—C25120.4 (4)C28'—C27'—H271'119.93
C24—C25—C26117.1 (4)N4'—C28'—N6'113.0 (4)
C24—C25—H251121.44N4'—C28'—C27'123.8 (4)
C26—C25—H251121.44N6'—C28'—C27'123.2 (4)
C25—C26—C27122.5 (5)N5'—C29'—C30'115.7 (4)
C25—C26—H261118.75N5'—C29'—H291'109.47
C27—C26—H261118.75N5'—C29'—H292'109.47
C26—C27—C28117.5 (4)C30'—C29'—H291'109.47
C26—C27—H271121.27C30'—C29'—H292'109.47
C28—C27—H271121.27H291'—C29'—H292'102.37
N4—C28—N6119.0 (4)C29'—C30'—H301'109.47
N4—C28—C27120.2 (4)C29'—C30'—H302'109.47
N6—C28—C27120.9 (4)C29'—C30'—H303'109.47
N5—C29—C30113.0 (4)H301'—C30'—H302'109.47
N5—C29—H291109.47H301'—C30'—H303'109.47
N5—C29—H292109.47H302'—C30'—H303'109.47
C30—C29—H291109.47N6'—C31'—C32'116.4 (4)
C30—C29—H292109.47N6'—C31'—H311'109.47
H291—C29—H292105.67N6'—C31'—H313'109.47
C29—C30—H301109.47C32'—C31'—H311'109.47
C29—C30—H302109.47C32'—C31'—H313'109.47
C29—C30—H303109.47H311'—C31'—H313'101.49
H301—C30—H302109.47C31'—C32'—H321'109.47
H301—C30—H303109.47C31'—C32'—H322'109.47
H302—C30—H303109.47C31'—C32'—H323'109.47
N6—C31—C32113.0 (4)H321'—C32'—H322'109.47
N6—C31—H311109.47H321'—C32'—H323'109.47
N6—C31—H313109.47H322'—C32'—H323'109.47
C32—C31—H311109.47C34'—C33'—H331'109.47
C32—C31—H313109.47C34'—C33'—H332'109.47
H311—C31—H313105.73C34'—C33'—H333'109.47
C31—C32—H321109.47H331'—C33'—H332'109.47
C31—C32—H322109.47H331'—C33'—H333'109.47
C31—C32—H323109.47H332'—C33'—H333'109.47
H321—C32—H322109.47P3'—C34'—C33'112.8 (3)
H321—C32—H323109.47P3'—C34'—C35'112.1 (3)
H322—C32—H323109.47P3'—C34'—H341'105.72
C34—C33—H331109.47C33'—C34'—C35'110.8 (4)
C34—C33—H332109.47C33'—C34'—H341'107.15
C34—C33—H333109.47C35'—C34'—H341'107.96
H331—C33—H332109.47C34'—C35'—H351'109.47
H331—C33—H333109.47C34'—C35'—H352'109.47
H332—C33—H333109.47C34'—C35'—H353'109.47
P3—C34—C33112.0 (3)H351'—C35'—H352'109.47
P3—C34—C35110.3 (3)H351'—C35'—H353'109.47
P3—C34—H341106.51H352'—C35'—H353'109.47
C33—C34—C35107.5 (4)C37'—C36'—H361'109.47
C33—C34—H341109.38C37'—C36'—H362'109.47
C35—C34—H341111.09C37'—C36'—H363'109.47
C34—C35—H351109.47H361'—C36'—H362'109.47
C34—C35—H352109.47H361'—C36'—H363'109.47
C34—C35—H353109.47H362'—C36'—H363'109.47
H351—C35—H352109.47P3'—C37'—C36'111.2 (3)
H351—C35—H353109.47P3'—C37'—C38'113.6 (3)
H352—C35—H353109.47P3'—C37'—H371'106.07
H361—C36—H362109.47C36'—C37'—C38'111.6 (4)
H361—C36—H363109.47C36'—C37'—H371'108.36
H362—C36—H363109.47C38'—C37'—H371'105.57
P3—C37—C38117.1 (4)C37'—C38'—H381'109.47
P3—C37—H371105.03C37'—C38'—H382'109.47
C38—C37—H371102.34C37'—C38'—H383'109.47
C37—C38—H381109.47H381'—C38'—H382'109.47
C37—C38—H382109.47H381'—C38'—H383'109.47
C37—C38—H383109.47H382'—C38'—H383'109.47
H381—C38—H382109.47C40'—C39'—H391'109.47
H381—C38—H383109.47C40'—C39'—H392'109.47
H382—C38—H383109.47C40'—C39'—H393'109.47
C40—C39—H391109.47H391'—C39'—H392'109.47
C40—C39—H392109.47H391'—C39'—H393'109.47
C40—C39—H393109.47H392'—C39'—H393'109.47
H391—C39—H392109.47P4'—C40'—C39'113.1 (3)
H391—C39—H393109.47P4'—C40'—C41'109.7 (3)
H392—C39—H393109.47P4'—C40'—H401'108.25
P4—C40—C39110.8 (3)C39'—C40'—C41'113.5 (4)
P4—C40—C41110.8 (3)C39'—C40'—H401'103.98
P4—C40—H401108.1C41'—C40'—H401'107.85
C39—C40—C41110.8 (4)C40'—C41'—H411'109.47
C39—C40—H401108.1C40'—C41'—H412'109.47
C41—C40—H401108.06C40'—C41'—H413'109.47
C40—C41—H411109.47H411'—C41'—H412'109.47
C40—C41—H412109.47H411'—C41'—H413'109.47
C40—C41—H413109.47H412'—C41'—H413'109.47
H411—C41—H412109.47C43'—C42'—H421'109.47
H411—C41—H413109.47C43'—C42'—H422'109.47
H412—C41—H413109.47C43'—C42'—H423'109.47
C43—C42—H421109.47H421'—C42'—H422'109.47
C43—C42—H422109.47H421'—C42'—H423'109.47
C43—C42—H423109.47H422'—C42'—H423'109.47
H421—C42—H422109.47P4'—C43'—C42'110.4 (3)
H421—C42—H423109.47P4'—C43'—C44'119.8 (3)
H422—C42—H423109.47P4'—C43'—H431'102.5
P4—C43—C42109.6 (3)P4'—C43'—C44b'115.2 (7)
P4—C43—C44121.6 (4)P4'—C43'—H431b'109
P4—C43—H431100.81C42'—C43'—C44'113.4 (4)
P4—C43—C44b121.9 (5)C42'—C43'—H431'110.76
P4—C43—H431b101.77C42'—C43'—C44b'119.0 (7)
C42—C43—C44110.9 (4)C42'—C43'—H431b'103.93
C42—C43—H431114.06C44'—C43'—H431'98.46
C42—C43—C44b114.5 (6)C44'—C43'—C44b'75.5 (7)
C42—C43—H431b112.11C44'—C43'—H431b'21.87
C44—C43—H43199.09H431'—C43'—C44b'22.98
C44—C43—C44b74.5 (5)H431'—C43'—H431b'120.24
C44—C43—H431b23.04C44b'—C43'—H431b'97.35
H431—C43—C44b26.38C43'—C44'—H441'109.47
H431—C43—H431b116.83C43'—C44'—H442'109.47
C44b—C43—H431b94.93C43'—C44'—H443'109.47
C43—C44—H441109.47C43'—C44'—H431b'30.72
C43—C44—H442109.47H441'—C44'—H442'109.47
C43—C44—H443109.47H441'—C44'—H443'109.47
C43—C44—H431b31.77H441'—C44'—H431b'123.2
H441—C44—H442109.47H442'—C44'—H443'109.47
H441—C44—H443109.47H442'—C44'—H431b'78.78
H441—C44—H431b137.99H443'—C44'—H431b'120.44
H442—C44—H443109.47Fe2'—C45'—O3'173.2 (5)
H442—C44—H431b102.47Fe2'—C46'—O4'176.8 (5)
H443—C44—H431b83.76C43—H431—C44b116.83
Fe2—C45—O3171.6 (6)C43'—H431'—C44b'127.79
Fe2—C46—O4174.0 (5)C43—C44b—H43136.79
P1'—Fe1'—P2'160.50 (7)C43—C44b—H441b109.47
P1'—Fe1'—N1'82.38 (10)C43—C44b—H442b109.47
P1'—Fe1'—C22'97.82 (14)C43—C44b—H443b109.47
P1'—Fe1'—C23'90.34 (16)H431—C44b—H441b117.97
P2'—Fe1'—N1'82.15 (10)H431—C44b—H442b128.5
P2'—Fe1'—C22'97.90 (14)H431—C44b—H443b73.1
P2'—Fe1'—C23'92.68 (16)H441b—C44b—H442b109.47
N1'—Fe1'—C22'106.51 (17)H441b—C44b—H443b109.47
N1'—Fe1'—C23'136.30 (19)H442b—C44b—H443b109.47
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—C44125.19
N3'—P2'—C20'99.08 (18)C43'—H431b'—C44'127.4
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C15—H151···C120.962.463.245 (7)139.30
C35—H353···O30.962.493.362 (6)151.59
C41—H411···C44b0.962.493.267 (12)137.55
C43—H431···C44b0.960.711.430 (12)116.83
C44b—H431···P40.712.232.868 (11)149.59
C44b—H431···C420.712.152.522 (12)114.06
C44b—H431···C430.710.961.430 (12)116.83
C41—H411···C44b0.962.333.158 (18)143.58
C43—H431···C44b0.960.771.554 (17)127.79
C44b—H431···P40.772.272.890 (17)138.06
C44b—H431···C420.772.032.611 (17)133.05
C44b—H431···C430.770.961.554 (17)127.79
C44b—H442b···C410.962.303.158 (18)148.03
C43—H431b···C440.960.711.490 (7)125.19
C44—H431b···P40.712.242.913 (7)156.71
C44—H431b···C420.712.122.519 (8)115.97
C44—H431b···C430.710.961.490 (7)125.19
C43—H431b···C440.960.701.493 (6)127.40
C44—H431b···P40.702.362.909 (5)137.02
C44—H431b···C420.701.952.482 (7)133.84
C44—H431b···C430.700.961.493 (6)127.40
(Fe_PNP-Et_Br2_CO) top
Crystal data top
C14H25Br2FeN3OP2F(000) = 1056
Mr = 529Dx = 1.768 Mg m3
Monoclinic, P21/nMo Kα radiation, λ = 0.71069 Å
Hall symbol: -P 2yabcCell parameters from 5440 reflections
a = 9.2939 (16) Åθ = 2.3–27.1°
b = 11.7224 (18) ŵ = 4.95 mm1
c = 18.307 (3) ÅT = 100 K
β = 94.999 (10)°Tabular, translucent blue
V = 1986.9 (6) Å30.27 × 0.20 × 0.04 mm
Z = 4
Data collection top
Bruker KAPPA APEX II CCD
diffractometer
12579 independent reflections
Radiation source: X-ray tube6782 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.091
ω– and φ–scansθmax = 27.6°, θmin = 2.1°
Absorption correction: multi-scan
TWINABS
h = 1112
Tmin = 0.32, Tmax = 0.82k = 1414
13162 measured reflectionsl = 2323
Refinement top
Refinement on F120 constraints
R[F2 > 2σ(F2)] = 0.090H-atom parameters constrained
wR(F2) = 0.128Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
S = 1.61(Δ/σ)max = 0.036
12579 reflectionsΔρmax = 1.93 e Å3
99 parametersΔρmin = 2.09 e Å3
0 restraints
Crystal data top
C14H25Br2FeN3OP2V = 1986.9 (6) Å3
Mr = 529Z = 4
Monoclinic, P21/nMo Kα radiation
a = 9.2939 (16) ŵ = 4.95 mm1
b = 11.7224 (18) ÅT = 100 K
c = 18.307 (3) Å0.27 × 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 = 0.82Rint = 0.091
13162 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.0900 restraints
wR(F2) = 0.128H-atom parameters constrained
S = 1.61Δρmax = 1.93 e Å3
12579 reflectionsΔρmin = 2.09 e Å3
99 parameters
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.9744 (2)0.22645 (14)0.14457 (8)0.0141 (6)
Br10.75736 (19)0.34704 (10)0.14646 (7)0.0289 (4)
Br1'1.18939 (18)0.10544 (10)0.13766 (7)0.0289 (4)
P11.1156 (5)0.3834 (3)0.15824 (16)0.0204 (9)
P1'0.8470 (5)0.0687 (3)0.16106 (16)0.0204 (9)
N11.0079 (12)0.2210 (7)0.2544 (4)0.018 (2)*
N21.1307 (10)0.3938 (6)0.2500 (3)0.0173 (16)*
N2'0.8808 (10)0.0533 (6)0.2523 (3)0.0173 (16)*
C11.0881 (14)0.3095 (8)0.2949 (5)0.0147 (18)*
C21.1103 (13)0.3040 (8)0.3673 (5)0.0140 (19)*
C31.0718 (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)*
C41.0476 (14)0.5248 (8)0.1266 (5)0.026 (2)*
C51.1067 (14)0.6228 (8)0.1704 (5)0.028 (2)*
C61.2930 (13)0.3758 (8)0.1363 (5)0.0160 (19)*
C71.3222 (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)*
C80.9503 (15)0.2260 (9)0.0487 (5)0.0203 (16)*
O10.9312 (9)0.2299 (6)0.0123 (3)0.0203 (16)*
H1c21.158590.3676320.3915560.0168*
H1c31.0980950.2155750.4619330.0209*
H1c41.0655360.5353720.0761980.0308*
H2c40.9440580.525640.1249660.0308*
H1c51.0765450.6926280.1463250.0339*
H2c51.071790.6205370.2181980.0339*
H3c51.2103130.6188150.1750950.0339*
H1c61.3482390.4357050.1610620.0192*
H2c61.3397640.3116670.1607280.0192*
H1c71.4236010.3640920.0507110.0402*
H2c71.2694070.3130630.0303220.0402*
H3c71.2916550.4456250.0324510.0402*
H1c4'0.867640.0571990.0645870.0308*
H2c4'0.9858060.0793930.1205710.0308*
H1c5'0.8455940.2337260.1155440.0339*
H2c5'0.8257610.1771980.191620.0339*
H3c5'0.7074490.1608690.1260270.0339*
H1c6'0.6162530.0115940.1769770.0192*
H2c6'0.6212180.1322490.1818520.0192*
H1c7'0.470410.0879750.0785220.0402*
H2c7'0.6035530.1497660.0492930.0402*
H3c7'0.5916550.0164630.0454650.0402*
H1c2'0.9455510.0675920.3979020.0168*
H1n21.1674120.4558610.269890.0207*
H1n2'0.8445190.0047210.2738970.0207*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.0028 (11)0.0084 (9)0.0314 (8)0.0001 (8)0.0035 (10)0.0002 (7)
Br10.0308 (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)
P10.022 (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—Br12.465 (3)C2'—C1'1.400 (12)
Fe1—Br1'2.463 (3)C2'—H1c2'0.96
Fe1—P12.262 (4)C4—C51.479 (14)
Fe1—P1'2.230 (4)C4—H1c40.96
Fe1—N12.008 (7)C4—H2c40.96
Fe1—C81.749 (9)C5—H1c50.96
Br1—N13.272 (9)C5—H2c50.96
Br1—N2'i3.369 (8)C5—H3c50.96
Br1'—N13.143 (9)C6—C71.540 (13)
Br1'—N2ii3.547 (7)C6—H1c60.96
P1—N21.677 (7)C6—H2c60.96
P1—C41.849 (10)C7—H1c70.96
P1—C61.733 (13)C7—H2c70.96
P1'—N2'1.681 (7)C7—H3c70.96
P1'—C4'1.819 (10)C4'—C5'1.462 (15)
P1'—C6'1.783 (13)C4'—H1c4'0.96
N1—C11.444 (13)C4'—H2c4'0.96
N1—C1'1.338 (13)C5'—H1c5'0.96
N2—C11.366 (12)C5'—H2c5'0.96
N2—H1n20.87C5'—H3c5'0.96
N2'—C1'1.426 (13)C6'—C7'1.548 (13)
N2'—H1n2'0.87C6'—H1c6'0.96
C1—C21.324 (12)C6'—H2c6'0.96
C2—C31.345 (14)C7'—H1c7'0.96
C2—H1c20.96C7'—H2c7'0.96
C3—C2'1.457 (14)C7'—H3c7'0.96
C3—H1c30.96C8—O11.117 (11)
Br1—Fe1—Br1'177.85 (8)C3—C2—H1c2116.8
Br1—Fe1—P189.98 (13)C2—C3—C2'114.7 (8)
Br1—Fe1—P1'91.67 (14)C2—C3—H1c3122.64
Br1—Fe1—N193.4 (3)C2'—C3—H1c3122.64
Br1—Fe1—C889.0 (4)C3—C2'—C1'118.1 (9)
Br1'—Fe1—P190.48 (14)C3—C2'—H1c2'120.94
Br1'—Fe1—P1'88.39 (13)C1'—C2'—H1c2'120.94
Br1'—Fe1—N188.7 (3)N1—C1'—N2'112.0 (8)
Br1'—Fe1—C888.9 (4)N1—C1'—C2'124.8 (9)
P1—Fe1—P1'165.80 (13)N2'—C1'—C2'122.5 (9)
P1—Fe1—N182.9 (3)P1—C4—C5115.2 (7)
P1—Fe1—C897.8 (4)P1—C4—H1c4109.47
P1'—Fe1—N182.9 (3)P1—C4—H2c4109.47
P1'—Fe1—C896.3 (4)C5—C4—H1c4109.47
N1—Fe1—C8177.5 (5)C5—C4—H2c4109.47
Fe1—Br1—N137.78 (15)H1c4—C4—H2c4103.08
Fe1—Br1—N2'i140.42 (15)C4—C5—H1c5109.47
N1—Br1—N2'i106.09 (19)C4—C5—H2c5109.47
Fe1—Br1'—N139.71 (16)C4—C5—H3c5109.47
Fe1—Br1'—N2ii135.77 (15)H1c5—C5—H2c5109.47
N1—Br1'—N2ii99.26 (19)H1c5—C5—H3c5109.47
Fe1—P1—N299.6 (3)H2c5—C5—H3c5109.47
Fe1—P1—C4121.0 (4)P1—C6—C7118.5 (8)
Fe1—P1—C6119.2 (4)P1—C6—H1c6109.47
N2—P1—C4104.2 (4)P1—C6—H2c6109.47
N2—P1—C6103.8 (5)C7—C6—H1c6109.47
C4—P1—C6106.2 (5)C7—C6—H2c6109.47
Fe1—P1'—N2'99.7 (3)H1c6—C6—H2c698.65
Fe1—P1'—C4'122.5 (4)C6—C7—H1c7109.47
Fe1—P1'—C6'119.8 (3)C6—C7—H2c7109.47
N2'—P1'—C4'108.9 (4)C6—C7—H3c7109.47
N2'—P1'—C6'102.0 (5)H1c7—C7—H2c7109.47
C4'—P1'—C6'101.9 (5)H1c7—C7—H3c7109.47
Fe1—N1—Br148.8 (2)H2c7—C7—H3c7109.47
Fe1—N1—Br1'51.6 (2)P1'—C4'—C5'118.3 (8)
Fe1—N1—C1121.3 (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—C1107.1 (6)C5'—C4'—H2c4'109.47
Br1—N1—C1'117.6 (8)H1c4'—C4'—H2c4'98.89
Br1'—N1—C1112.0 (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—P1128.7 (4)H1c5'—C5'—H2c5'109.47
Br1'iii—N2—C1107.7 (5)H1c5'—C5'—H3c5'109.47
Br1'iii—N2—H1n212.66H2c5'—C5'—H3c5'109.47
P1—N2—C1123.2 (6)P1'—C6'—C7'120.8 (8)
P1—N2—H1n2118.42P1'—C6'—H1c6'109.47
C1—N2—H1n2118.42P1'—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'—H1n2'6.57H1c6'—C6'—H2c6'95.19
P1'—N2'—C1'121.3 (6)C6'—C7'—H1c7'109.47
P1'—N2'—H1n2'119.33C6'—C7'—H2c7'109.47
C1'—N2'—H1n2'119.33C6'—C7'—H3c7'109.47
N1—C1—N2112.0 (7)H1c7'—C7'—H2c7'109.47
N1—C1—C2120.5 (9)H1c7'—C7'—H3c7'109.47
N2—C1—C2127.6 (9)H2c7'—C7'—H3c7'109.47
C1—C2—C3126.4 (9)Fe1—C8—O1176.9 (11)
C1—C2—H1c2116.8
Symmetry codes: (i) x+3/2, y+1/2, z+1/2; (ii) x+5/2, y1/2, z+1/2; (iii) x+5/2, y+1/2, z+1/2; (iv) x+3/2, y1/2, z+1/2.
(Fe_PNP-TADDOL-iPr_Cl2) top
Crystal data top
C46H55Cl2FeN3O5P2Z = 2
Mr = 918.7F(000) = 964
Triclinic, P1Dx = 1.311 Mg m3
Hall symbol: P 1Mo Kα radiation, λ = 0.71069 Å
a = 9.3389 (7) ÅCell parameters from 9106 reflections
b = 10.3155 (8) Åθ = 2.3–25.8°
c = 24.3224 (18) ŵ = 0.55 mm1
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 tube35102 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.066
ω– and φ–scansθmax = 28.0°, θmin = 0.8°
Absorption correction: multi-scan
TWINABS
h = 1212
Tmin = 0.23, Tmax = 0.85k = 1212
40097 measured reflectionsl = 3232
Refinement top
Refinement on FH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.051Weighting scheme based on measured s.u.'s w = 1/(σ2(F) + 0.0001F2)
wR(F2) = 0.070(Δ/σ)max = 0.048
S = 1.76Δρmax = 0.84 e Å3
39775 reflectionsΔρmin = 0.70 e Å3
439 parametersAbsolute structure: 5587 of Friedel pairs used in the refinement
0 restraintsAbsolute structure parameter: 0.05 (2)
527 constraints
Crystal data top
C46H55Cl2FeN3O5P2γ = 90.009 (2)°
Mr = 918.7V = 2327.0 (3) Å3
Triclinic, P1Z = 2
a = 9.3389 (7) ÅMo Kα radiation
b = 10.3155 (8) ŵ = 0.55 mm1
c = 24.3224 (18) ÅT = 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 = 0.85Rint = 0.066
40097 measured reflections
Refinement top
R[F2 > 2σ(F2)] = 0.051H-atom parameters constrained
wR(F2) = 0.070Δρmax = 0.84 e Å3
S = 1.76Δρmin = 0.70 e Å3
39775 reflectionsAbsolute structure: 5587 of Friedel pairs used in the refinement
439 parametersAbsolute structure parameter: 0.05 (2)
0 restraints
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe10.5240510.8375720.4146410.01355 (9)
Cl10.6549 (2)0.8137 (2)0.33478 (8)0.02670 (17)
Cl20.5217 (2)0.6875 (2)0.47380 (9)0.02682 (19)
P10.4882 (2)1.0515 (2)0.46065 (8)0.01661 (16)
P20.27212 (19)0.5643 (2)0.28631 (8)0.01528 (17)
O10.2950 (5)0.6448 (5)0.23528 (18)0.0184 (4)*
O20.4265 (4)0.4918 (4)0.28390 (16)0.0155 (3)*
O30.3101 (4)0.4141 (4)0.10871 (15)0.0178 (4)*
O40.5092 (4)0.3382 (4)0.14502 (17)0.0155 (4)*
N10.3075 (5)0.8642 (5)0.3990 (2)0.0131 (4)*
N20.3056 (5)1.0442 (5)0.45992 (19)0.0175 (4)*
N30.3235 (5)0.6813 (5)0.33445 (19)0.0165 (4)*
C10.2308 (7)0.9550 (7)0.4264 (3)0.0150 (5)*
C20.0786 (6)0.9675 (6)0.4235 (2)0.0159 (5)*
C30.0111 (6)0.8653 (6)0.3938 (2)0.0144 (5)*
C40.0901 (7)0.7698 (7)0.3611 (3)0.0159 (4)*
C50.2379 (6)0.7718 (6)0.3680 (2)0.0142 (5)*
C60.5481 (7)1.1848 (6)0.4202 (3)0.0212 (5)*
C70.4910 (6)1.3147 (6)0.4467 (2)0.0268 (7)*
C80.7032 (7)1.1785 (7)0.4030 (3)0.0307 (6)*
C90.5227 (6)1.0911 (6)0.5333 (2)0.0195 (5)*
C100.4313 (7)1.0130 (7)0.5699 (3)0.0296 (7)*
C110.6775 (6)1.0861 (5)0.5444 (2)0.0263 (6)*
C120.2500 (6)0.6041 (6)0.1782 (2)0.0161 (5)*
C130.3065 (6)0.4551 (6)0.1666 (2)0.0155 (5)*
C140.4532 (6)0.4206 (6)0.1881 (2)0.0153 (5)*
C150.4621 (7)0.3737 (6)0.2434 (2)0.0161 (5)*
C160.0925 (7)0.6176 (7)0.1753 (3)0.0214 (5)*
C170.0170 (6)0.5336 (7)0.1409 (2)0.0295 (7)*
C180.1327 (8)0.5481 (8)0.1352 (3)0.0419 (8)*
C190.2011 (7)0.6452 (6)0.1617 (2)0.0338 (8)*
C200.1313 (6)0.7303 (7)0.1984 (2)0.0287 (7)*
C210.0271 (6)0.7264 (6)0.2064 (2)0.0221 (6)*
C220.3293 (6)0.6990 (6)0.1410 (2)0.0189 (5)*
C230.2895 (6)0.6973 (6)0.0892 (2)0.0261 (6)*
C240.3551 (6)0.7810 (6)0.0555 (2)0.0305 (8)*
C250.4691 (6)0.8678 (6)0.0753 (3)0.0282 (8)*
C260.5043 (7)0.8644 (7)0.1265 (3)0.0277 (7)*
C270.4376 (6)0.7790 (7)0.1620 (2)0.0225 (6)*
C280.3635 (6)0.2692 (7)0.2559 (3)0.0176 (5)*
C290.3334 (6)0.1624 (7)0.2140 (3)0.0206 (6)*
C300.2392 (7)0.0611 (8)0.2313 (3)0.0294 (6)*
C310.1911 (7)0.0524 (8)0.2817 (3)0.0262 (5)*
C320.2198 (6)0.1435 (6)0.3199 (3)0.0239 (6)*
C330.3063 (6)0.2469 (6)0.3110 (3)0.0206 (5)*
C340.6200 (6)0.3400 (6)0.2521 (2)0.0170 (5)*
C350.6753 (7)0.2178 (7)0.2431 (3)0.0259 (6)*
C360.8255 (6)0.2077 (6)0.2520 (2)0.0256 (7)*
C370.9115 (7)0.3081 (6)0.2669 (2)0.0269 (6)*
C380.8561 (8)0.4257 (8)0.2749 (3)0.0319 (6)*
C390.7117 (6)0.4527 (7)0.2678 (2)0.0270 (6)*
C400.4518 (6)0.3617 (6)0.0962 (2)0.0162 (6)*
C410.4288 (6)0.2249 (6)0.0588 (2)0.0236 (6)*
C420.5387 (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)*
C430.1177 (7)0.0541 (8)0.0750 (3)0.0526 (11)*
C440.0094 (8)0.0060 (9)0.1141 (3)0.0629 (13)*
C450.0113 (9)0.1277 (9)0.1074 (3)0.0475 (9)*
C460.1520 (8)0.1693 (9)0.0938 (3)0.0493 (9)*
O50.2196 (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)*
H1c20.0269091.0422870.4411290.019*
H1c30.0915460.8602340.3957570.0172*
H1c40.0459470.706380.335310.0191*
H1c60.5052541.1722930.3848340.0254*
H1c70.3914071.3222440.4391250.0321*
H2c70.5435861.3837150.4317830.0321*
H3c70.5015241.3207140.4859670.0321*
H1c80.7229511.0985960.3798010.0368*
H2c80.7595241.1816870.4352770.0368*
H3c80.7271481.2511410.3829260.0368*
H1c90.4942411.1803630.543010.0234*
H1c100.3400231.0552980.5776740.0355*
H2c100.478051.0068210.6039240.0355*
H3c100.4176040.9271370.5513910.0355*
H1c110.7287631.1455830.5231260.0315*
H2c110.7132850.9992260.5341560.0315*
H3c110.6907361.1104330.5830960.0315*
H1c130.2377910.4102140.1879370.0186*
H1c140.5069280.498640.1974680.0184*
H1c170.0664180.4618150.1197960.0355*
H1c180.1831150.4848860.1114360.0502*
H1c190.3008530.6580230.1556580.0405*
H1c200.1870470.7966390.2203440.0344*
H1c210.0775480.7901520.2299510.0265*
H1c240.3248710.7820090.0183210.0366*
H1c260.5782140.9217140.1408220.0332*
H1c270.4667780.7770930.1993310.0269*
H1c290.3735320.1590580.1768560.0247*
H1c300.2100350.0050980.2031940.0353*
H1c310.1348010.0212190.2902580.0314*
H1c320.1784990.1388360.3564440.0287*
H1c330.3305170.3071250.3421680.0247*
H1c350.6180170.1432260.2316280.0311*
H1c371.0116910.2941970.2716460.0323*
H1c380.9179840.4971480.2862550.0383*
H1c410.4043070.1586180.0822950.0283*
H2c410.5156460.2006790.0376460.0283*
H3c410.3527370.2340080.0340940.0283*
H1c2'0.5390640.5404310.5557540.019*
H1c4'0.5322750.2890110.6718930.0191*
H1c6'0.0818920.7297660.6229220.0254*
H1c7'0.149030.8594780.5517360.0321*
H2c7'0.0276990.92950.5905350.0321*
H3c7'0.0094580.8573360.5328160.0321*
H1c8'0.1621450.766370.6438540.0368*
H2c8'0.174920.6333340.6065490.0368*
H3c8'0.1964660.7650260.581250.0368*
H1c10'0.2193830.4715150.4492690.0355*
H2c10'0.1125710.4912740.4028150.0355*
H3c10'0.0716180.3993910.4482130.0355*
H1c11'0.1470130.6851080.4856930.0315*
H2c11'0.1579390.5336950.4865770.0315*
H3c11'0.1267780.5921160.4304590.0315*
H1c13'0.3484750.0679370.8219160.0186*
H1c18'0.7661460.1703520.8901910.0502*
H1c19'0.8730290.3378020.8392020.0405*
H1c20'0.727930.4648590.7868320.0344*
H1c21'0.4960650.4138140.7857570.0265*
H1c23'0.361870.3428820.9403090.0313*
H1c24'0.2346690.4918011.0028060.0366*
H1c25'0.073290.6299890.9726530.0338*
H1c26'0.0035240.5948840.878550.0332*
H1c30'0.3349620.3593110.8106170.0353*
H1c31'0.4517780.4046780.7199940.0314*
H1c32'0.3950660.2653440.6483730.0287*
H1c35'0.0293820.2146240.775190.0311*
H1c37'0.4353980.1201020.7430890.0323*
H1c38'0.3480970.0941890.7234290.0383*
H1c39'0.1024340.1390020.7271230.0323*
H1c41'0.1859980.0396020.9818060.0283*
H2c41'0.2190170.1240760.9251110.0283*
H3c41'0.0612110.1108570.9497370.0283*
H1c42'0.0647210.1707690.9861770.0268*
H2c42'0.0624920.1306890.9478960.0268*
H3c42'0.0485640.2349660.9312320.0268*
H1c420.6182350.3995110.0456180.0268*
H2c420.5738370.5192720.0882610.0268*
H3c420.4808920.4809030.0368270.0268*
H1c390.6744260.540110.2729820.0323*
H1c230.2162520.6387410.0753250.0313*
H1c250.5161890.9250310.0517840.0338*
H1c360.8677330.1221790.2468260.0307*
H1c9'0.09260.6751180.4684540.0234*
H1c14'0.067760.1731980.8248310.0184*
H1c17'0.5201230.1257920.883030.0355*
H1c33'0.2431110.0769860.6751570.0247*
H1c27'0.109460.4317730.8173960.0269*
H1c3'0.65720.4444670.6260690.0172*
H1n20.2567271.1009850.4822980.0211*
H1n30.4152210.6865210.3392290.0198*
H1n2'0.3099330.6422110.5382190.0211*
H1n3'0.1587640.2463710.6642440.0198*
H1c36'0.2743630.268320.7728280.0307*
H1c430.16770.1261020.0886410.0632*
H2c430.0713280.0864310.0401860.0632*
H1c440.0425660.018220.1510170.0755*
H2c440.0824180.0424450.1015760.0755*
H1c450.0571240.1447210.0785070.057*
H2c450.0166840.1771410.1409630.057*
H1c460.1426480.2327940.0677940.0591*
H2c460.2060920.1991360.1272110.0591*
H1c46'0.2672220.9347840.9546290.0591*
H2c46'0.220010.9128150.8913790.0591*
H1c43'0.324040.6973450.9882730.0632*
H2c43'0.2588740.5825790.9415150.0632*
H1c44'0.5152890.6688980.9301340.0755*
H2c44'0.4087730.6441120.8758880.0755*
H1c45'0.438770.855980.8692140.057*
H2c45'0.4890170.8849750.9345870.057*
H1c29'0.2163170.1683920.8307710.0247*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Fe10.00779 (12)0.01374 (17)0.01891 (15)0.00044 (14)0.00167 (10)0.00038 (15)
Cl10.0161 (2)0.0371 (4)0.0245 (2)0.0065 (3)0.00485 (18)0.0050 (3)
Cl20.0149 (2)0.0268 (4)0.0416 (3)0.0026 (3)0.0016 (2)0.0182 (3)
P10.0082 (2)0.0153 (3)0.0253 (3)0.0005 (2)0.0023 (2)0.0032 (2)
P20.0088 (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—Cl12.2416 (19)N1'—C1'1.403 (9)
Fe1—Cl22.225 (2)N1'—C5'1.377 (8)
Fe1—P12.380 (2)N2'—C1'1.395 (9)
Fe1—N12.097 (5)N2'—H1n2'0.87
Cl1—N33.383 (5)N3'—C5'1.350 (8)
Cl2—N2'3.301 (5)N3'—H1n3'0.87
P1—N21.707 (5)O3'—C13'1.423 (7)
P1—C61.849 (7)O3'—C40'1.472 (6)
P1—C91.813 (6)O4'—C14'1.483 (7)
P2—O11.575 (5)O4'—C40'1.452 (7)
P2—N31.672 (5)C1'—C2'1.370 (9)
O1—C121.484 (7)C2'—C3'1.399 (9)
O2—C151.508 (7)C2'—H1c2'0.96
O3—C131.423 (6)C3'—C4'1.373 (9)
O3—C401.437 (6)C3'—H1c3'0.96
O4—C141.362 (7)C4'—C5'1.388 (9)
O4—C401.367 (7)C4'—H1c4'0.96
N1—C11.288 (8)C6'—H1c6'0.96
N1—C51.336 (8)C7'—H1c7'0.96
N2—C11.372 (8)C7'—H2c7'0.96
N2—Cl2'i3.328 (5)C7'—H3c7'0.96
N2—H1n20.87C8'—H1c8'0.96
N3—C51.399 (7)C8'—H2c8'0.96
N3—H1n30.87C8'—H3c8'0.96
C1—C21.432 (9)C9'—C10'1.548 (9)
C2—C31.380 (8)C9'—C11'1.529 (8)
C2—H1c20.96C9'—H1c9'0.96
C3—C41.389 (8)C10'—H1c10'0.96
C3—H1c30.96C10'—H2c10'0.96
C4—C51.397 (9)C10'—H3c10'0.96
C4—H1c40.96C11'—H1c11'0.96
C6—C71.509 (8)C11'—H2c11'0.96
C6—C81.490 (9)C11'—H3c11'0.96
C6—H1c60.96C12'—C13'1.500 (9)
C7—H1c70.96C12'—C22'1.502 (8)
C7—H2c70.96C13'—C14'1.547 (8)
C7—H3c70.96C13'—H1c13'0.96
C8—H1c80.96C14'—H1c14'0.96
C8—H2c80.96C15'—C34'1.540 (9)
C8—H3c80.96C16'—C17'1.410 (9)
C9—C101.503 (9)C16'—C21'1.356 (9)
C9—C111.484 (8)C17'—C18'1.372 (9)
C9—H1c90.96C17'—H1c17'0.96
C10—H1c100.96C18'—C19'1.471 (10)
C10—H2c100.96C18'—H1c18'0.96
C10—H3c100.96C19'—C20'1.387 (9)
C11—H1c110.96C19'—H1c19'0.96
C11—H2c110.96C20'—C21'1.302 (8)
C11—H3c110.96C20'—H1c20'0.96
C12—C161.483 (9)C21'—H1c21'0.96
C12—C221.569 (9)C22'—C23'1.431 (8)
C13—C141.543 (8)C22'—C27'1.394 (9)
C13—H1c130.96C23'—C24'1.393 (8)
C14—C151.483 (9)C23'—H1c23'0.96
C14—H1c140.96C24'—C25'1.309 (8)
C15—C281.467 (9)C24'—H1c24'0.96
C15—C341.544 (9)C25'—C26'1.432 (8)
C16—C171.355 (9)C25'—H1c25'0.96
C16—C211.408 (9)C26'—C27'1.373 (9)
C17—C181.421 (9)C26'—H1c26'0.96
C17—H1c170.96C27'—H1c27'0.96
C18—C191.285 (9)C28'—C29'1.325 (10)
C18—H1c180.96C28'—C33'1.385 (8)
C19—C201.368 (9)C29'—C30'1.314 (10)
C19—H1c190.96C29'—H1c29'0.96
C20—C211.502 (8)C30'—C31'1.433 (9)
C20—H1c200.96C30'—H1c30'0.96
C21—H1c210.96C31'—C32'1.464 (10)
C22—C231.327 (8)C31'—H1c31'0.96
C22—C271.385 (8)C32'—C33'1.429 (8)
C23—C241.380 (9)C32'—H1c32'0.96
C23—H1c230.96C33'—H1c33'0.96
C24—C251.454 (8)C34'—C35'1.414 (10)
C24—H1c240.96C34'—C39'1.333 (9)
C25—C261.306 (9)C35'—C36'1.404 (9)
C25—H1c250.96C35'—H1c35'0.96
C26—C271.426 (9)C36'—C37'1.359 (9)
C26—H1c260.96C36'—H1c36'0.96
C27—H1c270.96C37'—C38'1.471 (10)
C28—C291.453 (9)C37'—H1c37'0.96
C28—C331.464 (9)C38'—C39'1.391 (9)
C29—C301.453 (10)C38'—H1c38'0.96
C29—H1c290.96C39'—H1c39'0.96
C30—C311.300 (10)C40'—C41'1.449 (8)
C30—H1c300.96C40'—C42'1.539 (8)
C31—C321.283 (9)C41'—H1c41'0.96
C31—H1c310.96C41'—H2c41'0.96
C32—C331.369 (9)C41'—H3c41'0.96
C32—H1c320.96C42'—H1c42'0.96
C33—H1c330.96C42'—H2c42'0.96
C34—C351.355 (10)C42'—H3c42'0.96
C34—C391.470 (9)C43—C441.467 (10)
C35—C361.433 (9)C43—O51.449 (10)
C35—H1c350.96C43—H1c430.96
C36—C371.338 (8)C43—H2c430.96
C36—H1c360.96C44—C451.407 (13)
C37—C381.310 (10)C44—H1c440.96
C37—H1c370.96C44—H2c440.96
C38—C391.399 (9)C45—C461.445 (12)
C38—H1c380.96C45—H1c450.96
C39—H1c390.96C45—H2c450.96
C40—C421.472 (8)C46—O51.514 (11)
C41—H1c410.96C46—H1c460.96
C41—H2c410.96C46—H2c460.96
C41—H3c410.96C46'—O5'1.386 (11)
C42—H1c420.96C46'—C45'1.556 (11)
C42—H2c420.96C46'—H1c46'0.96
C42—H3c420.96C46'—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—Cl2122.17 (8)C1'—N1'—C5'120.8 (5)
Cl1—Fe1—P1118.47 (8)Cl2—N2'—P1'134.1 (2)
Cl1—Fe1—N1110.01 (14)Cl2—N2'—C1'101.4 (3)
Cl2—Fe1—P1111.93 (7)Cl2—N2'—H1n2'25.88
Cl2—Fe1—N1104.34 (16)P1'—N2'—C1'120.4 (4)
P1—Fe1—N180.48 (15)P1'—N2'—H1n2'119.78
Fe1—Cl1—N362.76 (9)C1'—N2'—H1n2'119.78
Fe1—Cl2—N2'131.90 (12)P2'—N3'—C5'123.0 (4)
Fe1—P1—N294.50 (18)P2'—N3'—H1n3'118.48
Fe1—P1—C6114.9 (2)C5'—N3'—H1n3'118.48
Fe1—P1—C9122.0 (2)C13'—O3'—C40'112.9 (4)
N2—P1—C6108.0 (3)C14'—O4'—C40'105.4 (4)
N2—P1—C9103.5 (3)N1'—C1'—N2'119.8 (5)
C6—P1—C9110.8 (3)N1'—C1'—C2'119.0 (6)
O1—P2—N396.7 (3)N2'—C1'—C2'121.2 (6)
P2—O1—C12125.7 (4)C1'—C2'—C3'119.8 (6)
C13—O3—C40104.8 (4)C1'—C2'—H1c2'120.11
C14—O4—C40111.1 (4)C3'—C2'—H1c2'120.11
Fe1—N1—C1121.9 (4)C2'—C3'—C4'119.0 (6)
Fe1—N1—C5119.9 (4)C2'—C3'—H1c3'120.51
C1—N1—C5116.9 (5)C4'—C3'—H1c3'120.51
P1—N2—C1124.5 (4)C3'—C4'—C5'121.2 (6)
P1—N2—Cl2'i133.1 (2)C3'—C4'—H1c4'119.39
P1—N2—H1n2117.77C5'—C4'—H1c4'119.39
C1—N2—Cl2'i102.1 (3)N1'—C5'—N3'113.7 (5)
C1—N2—H1n2117.77N1'—C5'—C4'118.5 (5)
Cl2'i—N2—H1n216.49N3'—C5'—C4'127.3 (6)
Cl1—N3—P2123.5 (2)P1'—C6'—H1c6'102.28
Cl1—N3—C5104.8 (3)H1c7'—C7'—H2c7'109.47
Cl1—N3—H1n322.28H1c7'—C7'—H3c7'109.47
P2—N3—C5128.3 (4)H2c7'—C7'—H3c7'109.47
P2—N3—H1n3115.87H1c8'—C8'—H2c8'109.47
C5—N3—H1n3115.86H1c8'—C8'—H3c8'109.47
N1—C1—N2115.1 (6)H2c8'—C8'—H3c8'109.47
N1—C1—C2124.8 (6)P1'—C9'—C10'107.8 (4)
N2—C1—C2120.2 (5)P1'—C9'—C11'109.8 (4)
C1—C2—C3115.7 (5)P1'—C9'—H1c9'110.86
C1—C2—H1c2122.14C10'—C9'—C11'110.9 (5)
C3—C2—H1c2122.14C10'—C9'—H1c9'109.77
C2—C3—C4120.8 (6)C11'—C9'—H1c9'107.78
C2—C3—H1c3119.62C9'—C10'—H1c10'109.47
C4—C3—H1c3119.62C9'—C10'—H2c10'109.47
C3—C4—C5115.7 (6)C9'—C10'—H3c10'109.47
C3—C4—H1c4122.16H1c10'—C10'—H2c10'109.47
C5—C4—H1c4122.16H1c10'—C10'—H3c10'109.47
N1—C5—N3116.0 (5)H2c10'—C10'—H3c10'109.47
N1—C5—C4125.1 (5)C9'—C11'—H1c11'109.47
N3—C5—C4118.2 (5)C9'—C11'—H2c11'109.47
P1—C6—C7110.9 (4)C9'—C11'—H3c11'109.47
P1—C6—C8114.0 (5)H1c11'—C11'—H2c11'109.47
P1—C6—H1c6108.29H1c11'—C11'—H3c11'109.47
C7—C6—C8116.8 (5)H2c11'—C11'—H3c11'109.47
C7—C6—H1c6104.75O1'—C12'—C13'111.6 (5)
C8—C6—H1c6100.85O1'—C12'—C22'106.5 (5)
C6—C7—H1c7109.47C13'—C12'—C22'115.3 (5)
C6—C7—H2c7109.47O3'—C13'—C12'115.4 (5)
C6—C7—H3c7109.47O3'—C13'—C14'102.3 (4)
H1c7—C7—H2c7109.47O3'—C13'—H1c13'110.34
H1c7—C7—H3c7109.47C12'—C13'—C14'109.0 (5)
H2c7—C7—H3c7109.47C12'—C13'—H1c13'103.77
C6—C8—H1c8109.47C14'—C13'—H1c13'116.57
C6—C8—H2c8109.47O4'—C14'—C13'103.7 (4)
C6—C8—H3c8109.47O4'—C14'—H1c14'117.01
H1c8—C8—H2c8109.47C13'—C14'—H1c14'109.93
H1c8—C8—H3c8109.47O2'—C15'—C34'103.9 (5)
H2c8—C8—H3c8109.47C17'—C16'—C21'117.0 (6)
P1—C9—C10112.3 (4)C16'—C17'—C18'117.9 (6)
P1—C9—C11112.5 (4)C16'—C17'—H1c17'121.06
P1—C9—H1c9106.72C18'—C17'—H1c17'121.06
C10—C9—C11113.3 (5)C17'—C18'—C19'119.2 (6)
C10—C9—H1c9105.81C17'—C18'—H1c18'120.38
C11—C9—H1c9105.56C19'—C18'—H1c18'120.38
C9—C10—H1c10109.47C18'—C19'—C20'121.5 (6)
C9—C10—H2c10109.47C18'—C19'—H1c19'119.25
C9—C10—H3c10109.47C20'—C19'—H1c19'119.25
H1c10—C10—H2c10109.47C19'—C20'—C21'113.2 (6)
H1c10—C10—H3c10109.47C19'—C20'—H1c20'123.39
H2c10—C10—H3c10109.47C21'—C20'—H1c20'123.39
C9—C11—H1c11109.47C16'—C21'—C20'131.0 (6)
C9—C11—H2c11109.47C16'—C21'—H1c21'114.49
C9—C11—H3c11109.47C20'—C21'—H1c21'114.49
H1c11—C11—H2c11109.47C12'—C22'—C23'124.1 (5)
H1c11—C11—H3c11109.47C12'—C22'—C27'121.3 (5)
H2c11—C11—H3c11109.47C23'—C22'—C27'114.6 (5)
O1—C12—C16110.3 (5)C22'—C23'—C24'122.6 (6)
O1—C12—C22105.3 (5)C22'—C23'—H1c23'118.7
C16—C12—C22110.5 (5)C24'—C23'—H1c23'118.71
O3—C13—C14107.3 (4)C23'—C24'—C25'121.1 (5)
O3—C13—H1c13114.45C23'—C24'—H1c24'119.44
C14—C13—H1c13104.83C25'—C24'—H1c24'119.44
O4—C14—C13101.8 (4)C24'—C25'—C26'118.6 (5)
O4—C14—C15115.2 (5)C24'—C25'—H1c25'120.69
O4—C14—H1c14115.55C26'—C25'—H1c25'120.69
C13—C14—C15120.2 (5)C25'—C26'—C27'120.9 (6)
C13—C14—H1c14110C25'—C26'—H1c26'119.54
C15—C14—H1c1494.8C27'—C26'—H1c26'119.54
O2—C15—C14104.7 (5)C22'—C27'—C26'121.8 (6)
O2—C15—C28107.8 (5)C22'—C27'—H1c27'119.08
O2—C15—C34105.9 (4)C26'—C27'—H1c27'119.09
C14—C15—C28116.7 (5)C29'—C28'—C33'122.0 (6)
C14—C15—C34108.4 (5)C28'—C29'—C30'124.9 (7)
C28—C15—C34112.6 (5)C28'—C29'—H1c29'117.56
C12—C16—C17121.0 (6)C30'—C29'—H1c29'117.56
C12—C16—C21117.2 (6)C29'—C30'—C31'118.2 (7)
C17—C16—C21121.7 (6)C29'—C30'—H1c30'120.92
C16—C17—C18122.2 (6)C31'—C30'—H1c30'120.92
C16—C17—H1c17118.92C30'—C31'—C32'118.7 (6)
C18—C17—H1c17118.92C30'—C31'—H1c31'120.65
C17—C18—C19120.5 (6)C32'—C31'—H1c31'120.64
C17—C18—H1c18119.77C31'—C32'—C33'117.7 (5)
C19—C18—H1c18119.77C31'—C32'—H1c32'121.15
C18—C19—C20119.7 (6)C33'—C32'—H1c32'121.15
C18—C19—H1c19120.14C28'—C33'—C32'118.0 (6)
C20—C19—H1c19120.14C28'—C33'—H1c33'121.02
C19—C20—C21124.1 (5)C32'—C33'—H1c33'121.02
C19—C20—H1c20117.97C15'—C34'—C35'119.5 (6)
C21—C20—H1c20117.97C15'—C34'—C39'121.7 (6)
C16—C21—C20111.6 (5)C35'—C34'—C39'118.7 (6)
C16—C21—H1c21124.2C34'—C35'—C36'122.4 (6)
C20—C21—H1c21124.2C34'—C35'—H1c35'118.81
C12—C22—C23117.3 (5)C36'—C35'—H1c35'118.81
C12—C22—C27120.4 (5)C35'—C36'—C37'118.8 (6)
C23—C22—C27122.3 (6)C35'—C36'—H1c36'120.61
C22—C23—C24119.0 (6)C37'—C36'—H1c36'120.61
C22—C23—H1c23120.51C36'—C37'—C38'118.9 (6)
C24—C23—H1c23120.51C36'—C37'—H1c37'120.53
C23—C24—C25121.3 (5)C38'—C37'—H1c37'120.53
C23—C24—H1c24119.36C37'—C38'—C39'119.2 (6)
C25—C24—H1c24119.36C37'—C38'—H1c38'120.4
C24—C25—C26116.9 (6)C39'—C38'—H1c38'120.4
C24—C25—H1c25121.54C34'—C39'—C38'121.8 (7)
C26—C25—H1c25121.54C34'—C39'—H1c39'119.09
C25—C26—C27122.7 (6)C38'—C39'—H1c39'119.09
C25—C26—H1c26118.66O3'—C40'—O4'102.8 (4)
C27—C26—H1c26118.66O3'—C40'—C41'110.1 (4)
C22—C27—C26117.8 (6)O3'—C40'—C42'111.1 (4)
C22—C27—H1c27121.1O4'—C40'—C41'107.3 (4)
C26—C27—H1c27121.1O4'—C40'—C42'109.4 (4)
C15—C28—C29120.7 (5)C41'—C40'—C42'115.3 (5)
C15—C28—C33125.7 (5)C40'—C41'—H1c41'109.47
C29—C28—C33112.7 (6)C40'—C41'—H2c41'109.47
C28—C29—C30116.3 (6)C40'—C41'—H3c41'109.47
C28—C29—H1c29121.85H1c41'—C41'—H2c41'109.47
C30—C29—H1c29121.85H1c41'—C41'—H3c41'109.47
C29—C30—C31125.5 (7)H2c41'—C41'—H3c41'109.47
C29—C30—H1c30117.24C40'—C42'—H1c42'109.47
C31—C30—H1c30117.24C40'—C42'—H2c42'109.47
C30—C31—C32119.2 (7)C40'—C42'—H3c42'109.47
C30—C31—H1c31120.41H1c42'—C42'—H2c42'109.47
C32—C31—H1c31120.41H1c42'—C42'—H3c42'109.47
C31—C32—C33123.2 (6)H2c42'—C42'—H3c42'109.47
C31—C32—H1c32118.41C44—C43—O5111.8 (6)
C33—C32—H1c32118.41C44—C43—H1c43109.47
C28—C33—C32122.5 (5)C44—C43—H2c43109.47
C28—C33—H1c33118.74O5—C43—H1c43109.47
C32—C33—H1c33118.74O5—C43—H2c43109.47
C15—C34—C35123.9 (6)H1c43—C43—H2c43107.04
C15—C34—C39115.0 (5)C43—C44—C45100.3 (7)
C35—C34—C39121.0 (6)C43—C44—H1c44109.47
C34—C35—C36115.2 (6)C43—C44—H2c44109.47
C34—C35—H1c35122.4C45—C44—H1c44109.47
C36—C35—H1c35122.4C45—C44—H2c44109.47
C35—C36—C37125.2 (6)H1c44—C44—H2c44117.28
C35—C36—H1c36117.4C44—C45—C46111.2 (7)
C37—C36—H1c36117.4C44—C45—H1c45109.47
C36—C37—C38118.6 (6)C44—C45—H2c45109.47
C36—C37—H1c37120.69C46—C45—H1c45109.47
C38—C37—H1c37120.69C46—C45—H2c45109.47
C37—C38—C39123.5 (7)H1c45—C45—H2c45107.68
C37—C38—H1c38118.26C45—C46—O5104.3 (7)
C39—C38—H1c38118.26C45—C46—H1c46109.47
C34—C39—C38116.4 (6)C45—C46—H2c46109.47
C34—C39—H1c39121.79O5—C46—H1c46109.47
C38—C39—H1c39121.79O5—C46—H2c46109.47
O3—C40—O4107.8 (4)H1c46—C46—H2c46114.19
O3—C40—C42111.1 (5)C43—O5—C46103.0 (6)
O4—C40—C42114.2 (5)O5'—C46'—C45'108.7 (7)
H1c41—C41—H2c41109.47O5'—C46'—H1c46'109.47
H1c41—C41—H3c41109.47O5'—C46'—H2c46'109.47
H2c41—C41—H3c41109.47C45'—C46'—H1c46'109.47
C40—C42—H1c42109.47C45'—C46'—H2c46'109.47
C40—C42—H2c42109.47H1c46'—C46'—H2c46'110.2
C40—C42—H3c42109.47C46'—O5'—C43'110.4 (6)
H1c42—C42—H2c42109.47O5'—C43'—H1c43'109.47
H1c42—C42—H3c42109.47O5'—C43'—H2c43'109.47
H2c42—C42—H3c42109.47H1c43'—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, y1, z.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
C17—H1c17···O30.962.333.038 (7)130.43
C27—H1c27···O10.962.312.684 (8)102.21
C29—H1c29···O40.962.423.038 (8)121.96
C21—H1c21···O10.962.472.840 (7)102.69
C35—H1c35···C280.962.502.887 (9)104.30
C39—H1c39···O20.962.382.682 (7)97.82
C39—H1c39···O20.962.382.700 (7)98.92
C17—H1c17···O30.962.383.041 (7)125.43
C33—H1c33···O20.962.172.580 (7)104.57
C27—H1c27···O10.962.292.648 (7)100.97
C29—H1c29···O40.962.323.007 (8)128.08

Experimental details

(Fe_PNP-HEt_CO2)(Fe_PNP-Et_Br2_CO)(Fe_PNP-TADDOL-iPr_Cl2)
Crystal data
Chemical formulaC23H41FeN3O2P2C14H25Br2FeN3OP2C46H55Cl2FeN3O5P2
Mr509.4529918.7
Crystal system, space groupMonoclinic, P1121/bMonoclinic, P21/nTriclinic, P1
Temperature (K)100100100
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), 9096.277 (3), 92.393 (3), 90.009 (2)
V3)10454 (3)1986.9 (6)2327.0 (3)
Z1642
Radiation typeMo KαMo KαMo Kα
µ (mm1)0.724.950.55
Crystal size (mm)0.80 × 0.75 × 0.550.27 × 0.20 × 0.040.67 × 0.41 × 0.06
Data collection
DiffractometerBruker KAPPA APEX II CCD
diffractometer
Bruker KAPPA APEX II CCD
diffractometer
Bruker KAPPA APEX II CCD
diffractometer
Absorption correctionMulti-scan
SADABS
Multi-scan
TWINABS
Multi-scan
TWINABS
Tmin, Tmax0.57, 0.670.32, 0.820.23, 0.85
No. of measured, independent and
observed [I > 3σ(I)] reflections
450669, 30818, 25454 13162, 12579, 6782 40097, 39775, 35102
Rint0.0510.0910.066
(sin θ/λ)max1)0.7070.6520.659
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 reflections308181257939775
No. of parameters81599439
H-atom treatmentH-atom parameters constrainedH-atom parameters constrainedH-atom parameters constrained
Δρmax, Δρmin (e Å3)2.07, 0.871.93, 2.090.84, 0.70
Absolute structure??5587 of Friedel pairs used in the refinement
Absolute structure parameter??0.05 (2)

Computer programs: APEX 2 (Bruker, 2014), SAINT (Bruker, 2014), SUPERFLIP (Palatinus & Chapuis, 2007), JANA20006 (Petříček, M. Dušek & L. Palatinus, 2014).

 

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