Crystal structure determination and analysis have been carried out for the two spin-crossover compounds [Fe(teeX)6](BF4)2 (teeX is haloethyltetrazole; X = I: teei; X = Br: teeb), in both their high-spin (near 300 K) and their low-spin states (T = 90 K), using high-resolution powder-diffraction data collected at the ESRF (Grenoble, France) and SPring8 (Japan) synchrotron radiation facilities. The structures of teei have been solved using various direct-space structure determination techniques (grid search, genetic algorithm and parallel tempering) and refined with the Rietveld method using geometrical restraints. In the case of teeb, a structural model was found but a full refinement was not successful because of the presence of a significant amount of an amorphous component. Analysis of the structures (space group P21/c, Z = 2) and diffraction data, and the absence of phase transitions, show the overall structural similarity of these compounds and lead to the conclusion that the gradual spin-crossovers are likely to be accompanied by small structural changes only.
Supporting information
CCDC references: 255081; 255082; 255083; 255084
Program(s) used to refine structure: GSAS for LAST_publ, TEEB90RR3TEXT4_publ. Software used to prepare material for publication: Xtal BONDLA CIFIO for feteei.
Crystal data top
C18H30FeI6N24·2(BF4) | β = 90.3080 (11)° |
Mr = 1573.50 | V = 2427.96 (6) Å3 |
Monoclinic, P21/c | Z = 2 |
Hall symbol: -p 2ybc | Dx = 2.152 Mg m−3 |
a = 12.64250 (19) Å | Synchrotron radiation, λ = 0.75003 Å |
b = 18.0349 (3) Å | T = 293 K |
c = 10.64881 (15) Å | × × mm |
Crystal data top
C18H30FeI6N24·2(BF4) | β = 90.3080 (11)° |
Mr = 1573.50 | V = 2427.96 (6) Å3 |
Monoclinic, P21/c | Z = 2 |
a = 12.64250 (19) Å | Synchrotron radiation, λ = 0.75003 Å |
b = 18.0349 (3) Å | T = 293 K |
c = 10.64881 (15) Å | × × mm |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe | 0.00000 | 0.00000 | 0.00000 | 0.02533* | |
I1 | 0.4112 (5) | −0.1985 (3) | −0.0652 (5) | 0.0871 (13)* | |
I3 | 0.4192 (4) | 0.1155 (3) | −0.2359 (5) | 0.08713* | |
I2 | 0.4120 (5) | 0.0715 (3) | 0.3214 (4) | 0.08713* | |
N4A | 0.0964 (14) | −0.0687 (7) | −0.1261 (13) | 0.055 (6)* | |
N3A | 0.150 (2) | −0.0426 (7) | −0.2308 (12) | 0.05482* | |
N2A | 0.208 (2) | −0.0935 (9) | −0.2790 (18) | 0.05482* | |
N1A | 0.188 (2) | −0.1528 (10) | −0.2158 (17) | 0.05482* | |
N4C | 0.1014 (16) | 0.0975 (7) | −0.0382 (13) | 0.05482* | |
N4B | 0.1031 (16) | −0.0310 (9) | 0.1609 (11) | 0.05482* | |
N3C | 0.1517 (18) | 0.1402 (7) | 0.0502 (13) | 0.05482* | |
N3B | 0.1491 (18) | −0.0955 (8) | 0.1785 (12) | 0.05482* | |
N2C | 0.208 (2) | 0.1900 (9) | −0.0006 (16) | 0.05482* | |
N1C | 0.192 (2) | 0.1827 (9) | −0.1220 (19) | 0.05482* | |
N2B | 0.212 (2) | −0.0967 (9) | 0.2759 (15) | 0.05482* | |
N1B | 0.196 (2) | −0.0307 (11) | 0.3261 (14) | 0.05482* | |
C1A | 0.1199 (18) | −0.1376 (8) | −0.1200 (15) | 0.05482* | |
C2A | 0.235 (2) | −0.2259 (13) | −0.249 (2) | 0.08 (2)* | |
C3A | 0.353 (2) | −0.2217 (18) | −0.250 (2) | 0.07596* | |
C1C | 0.126 (2) | 0.1258 (8) | −0.1448 (16) | 0.05482* | |
C1B | 0.1308 (19) | 0.0110 (10) | 0.2541 (12) | 0.05482* | |
C2C | 0.235 (2) | 0.2362 (12) | −0.217 (3) | 0.12 (2)* | |
C2B | 0.244 (2) | −0.0049 (16) | 0.4512 (18) | 0.06 (2)* | |
C3C | 0.356 (2) | 0.2254 (11) | −0.224 (3) | 0.11794* | |
C3B | 0.3630 (18) | −0.0088 (16) | 0.443 (2) | 0.05796* | |
H1A | 0.094 (2) | −0.1758 (8) | −0.0479 (18) | 0.05066* | |
H21A | 0.206 (3) | −0.2688 (10) | −0.184 (3) | 0.05066* | |
H22A | 0.206 (3) | −0.2417 (17) | −0.341 (3) | 0.05066* | |
H31A | 0.385 (3) | −0.182 (2) | −0.303 (6) | 0.05066* | |
H32A | 0.382 (3) | −0.279 (2) | −0.271 (6) | 0.05066* | |
H1C | 0.103 (2) | 0.1047 (9) | −0.2365 (16) | 0.05066* | |
H1B | 0.111 (2) | 0.0681 (11) | 0.2694 (13) | 0.05066* | |
H21C | 0.203 (3) | 0.2258 (12) | −0.308 (2) | 0.05066* | |
H22C | 0.226 (3) | 0.2907 (13) | −0.186 (4) | 0.05066* | |
H21B | 0.217 (3) | 0.0457 (16) | 0.4782 (17) | 0.05066* | |
H22B | 0.226 (3) | −0.050 (2) | 0.519 (2) | 0.05066* | |
H31C | 0.396 (2) | 0.232 (3) | −0.140 (4) | 0.05066* | |
H32C | 0.386 (3) | 0.260 (3) | −0.301 (4) | 0.05066* | |
H31B | 0.396 (2) | −0.054 (3) | 0.400 (4) | 0.05066* | |
H32B | 0.400 (3) | 0.010 (3) | 0.526 (4) | 0.05066* | |
B | 0.0046 (19) | 0.1569 (13) | 0.489 (2) | 0.05066* | |
F1 | 0.1100 (18) | 0.1703 (17) | 0.492 (3) | 0.10132* | |
F2 | −0.022 (3) | 0.1682 (16) | 0.368 (2) | 0.10132* | |
F3 | −0.017 (3) | 0.0907 (13) | 0.542 (3) | 0.10132* | |
F4 | −0.038 (2) | 0.2053 (15) | 0.570 (2) | 0.10132* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
? | ? | ? | ? | ? | ? | ? |
Geometric parameters (Å, º) top
Fe—N4A | 2.200 (14) | N1B—C1B | 1.35 (3) |
Fe—N4C | 2.215 (16) | N1B—C2B | 1.53 (3) |
Fe—N4B | 2.219 (15) | C1A—H1A | 1.08 (2) |
Fe—N4A | 2.200 (14) | C2A—C3A | 1.50 (4) |
Fe—N4C | 2.215 (16) | C2A—H21A | 1.10 (4) |
Fe—N4B | 2.219 (15) | C2A—H22A | 1.08 (4) |
I1—C3A | 2.14 (2) | C3A—H31A | 1.00 (6) |
I3—C3C | 2.14 (2) | C3A—H32A | 1.12 (5) |
I2—C3B | 2.04 (3) | C1C—H1C | 1.09 (2) |
N4A—N3A | 1.39 (2) | C1B—H1B | 1.07 (3) |
N4A—C1A | 1.279 (19) | C2C—C3C | 1.54 (4) |
N3A—N2A | 1.28 (3) | C2C—H21C | 1.06 (4) |
N2A—N1A | 1.29 (2) | C2C—H22C | 1.04 (3) |
N1A—C1A | 1.37 (3) | C2B—C3B | 1.51 (4) |
N1A—C2A | 1.49 (3) | C2B—H21B | 1.02 (4) |
N4C—N3C | 1.37 (2) | C2B—H22B | 1.11 (4) |
N4C—C1C | 1.29 (2) | C3C—H31C | 1.03 (5) |
N4B—N3B | 1.31 (2) | C3C—H32C | 1.10 (6) |
N4B—C1B | 1.30 (2) | C3B—H31B | 1.03 (6) |
N3C—N2C | 1.27 (3) | C3B—H32B | 1.05 (5) |
N3B—N2B | 1.31 (3) | B—F1 | 1.35 (3) |
N2C—N1C | 1.32 (3) | B—F2 | 1.35 (3) |
N1C—C1C | 1.34 (3) | B—F3 | 1.35 (3) |
N1C—C2C | 1.50 (3) | B—F4 | 1.34 (4) |
N2B—N1B | 1.32 (3) | | |
| | | |
N4A—Fe—N4C | 90.7 (5) | C3A—C2A—H21A | 112 (3) |
N4A—Fe—N4B | 90.2 (6) | C3A—C2A—H22A | 110 (3) |
N4A—Fe—N4A | 180.0000 | H21A—C2A—H22A | 106 (3) |
N4A—Fe—N4C | 89.3 (5) | I1—C3A—C2A | 109.9 (16) |
N4A—Fe—N4B | 89.8 (6) | I1—C3A—H31A | 104 (4) |
N4C—Fe—N4B | 90.2 (6) | I1—C3A—H32A | 105 (4) |
N4C—Fe—N4A | 89.3 (5) | C2A—C3A—H31A | 117 (3) |
N4C—Fe—N4C | 180.0000 | C2A—C3A—H32A | 106 (3) |
N4C—Fe—N4B | 89.8 (6) | H31A—C3A—H32A | 115 (4) |
N4B—Fe—N4A | 89.8 (6) | N4C—C1C—N1C | 107.3 (16) |
N4B—Fe—N4C | 89.8 (6) | N4C—C1C—H1C | 126 (2) |
N4B—Fe—N4B | 180.0000 | N1C—C1C—H1C | 127 (2) |
N4A—Fe—N4C | 90.7 (5) | N4B—C1B—N1B | 105.7 (17) |
N4A—Fe—N4B | 90.2 (6) | N4B—C1B—H1B | 128 (2) |
N4C—Fe—N4B | 90.2 (6) | N1B—C1B—H1B | 126 (2) |
Fe—N4A—N3A | 125.0 (9) | N1C—C2C—C3C | 108 (2) |
Fe—N4A—C1A | 130.2 (12) | N1C—C2C—H21C | 111 (3) |
N3A—N4A—C1A | 104.8 (14) | N1C—C2C—H22C | 110 (3) |
N4A—N3A—N2A | 111.2 (13) | C3C—C2C—H21C | 108 (3) |
N3A—N2A—N1A | 106 (2) | C3C—C2C—H22C | 104 (3) |
N2A—N1A—C1A | 110.5 (18) | H21C—C2C—H22C | 114 (3) |
N2A—N1A—C2A | 122 (2) | N1B—C2B—C3B | 109 (2) |
C1A—N1A—C2A | 127.5 (18) | N1B—C2B—H21B | 113 (3) |
Fe—N4C—N3C | 125.9 (11) | N1B—C2B—H22B | 105 (3) |
Fe—N4C—C1C | 128.5 (12) | C3B—C2B—H21B | 113 (3) |
N3C—N4C—C1C | 105.6 (15) | C3B—C2B—H22B | 102 (3) |
Fe—N4B—N3B | 126.3 (11) | H21B—C2B—H22B | 114 (3) |
Fe—N4B—C1B | 126.8 (13) | I3—C3C—C2C | 119.5 (15) |
N3B—N4B—C1B | 106.9 (15) | I3—C3C—H31C | 89 (3) |
N4C—N3C—N2C | 111.5 (14) | I3—C3C—H32C | 110 (3) |
N4B—N3B—N2B | 113.3 (14) | C2C—C3C—H31C | 115 (3) |
N3C—N2C—N1C | 105.1 (18) | C2C—C3C—H32C | 108 (3) |
N2C—N1C—C1C | 110.5 (18) | H31C—C3C—H32C | 114 (4) |
N2C—N1C—C2C | 123 (2) | I2—C3B—C2B | 108.0 (17) |
C1C—N1C—C2C | 126 (2) | I2—C3B—H31B | 99 (3) |
N3B—N2B—N1B | 102.2 (18) | I2—C3B—H32B | 99 (3) |
N2B—N1B—C1B | 111.5 (17) | C2B—C3B—H31B | 118 (3) |
N2B—N1B—C2B | 124 (2) | C2B—C3B—H32B | 112 (3) |
C1B—N1B—C2B | 124.2 (19) | H31B—C3B—H32B | 117 (4) |
N4A—C1A—N1A | 107.7 (15) | F1—B—F2 | 104 (2) |
N4A—C1A—H1A | 126 (2) | F1—B—F3 | 111 (2) |
N1A—C1A—H1A | 126.7 (18) | F1—B—F4 | 105 (2) |
N1A—C2A—C3A | 111 (2) | F2—B—F3 | 119 (2) |
N1A—C2A—H21A | 110 (3) | F2—B—F4 | 115 (2) |
N1A—C2A—H22A | 109 (3) | F3—B—F4 | 103 (2) |
(TEEI90RRLAST_overall)
top
Crystal data top
? | β = ?° |
Mr = ? | γ = ?° |
?, ? | V = ? Å3 |
a = ? Å | Z = ? |
b = ? Å | ? radiation, λ = 0.999995 Å |
c = ? Å | ?, ? × ? × ? mm |
α = ?° | |
Data collection top
2θmin = 0.010°, 2θmax = 1.800°, 2θstep = 0.01° | |
Refinement top
Least-squares matrix: full | 180 data points |
Rp = 0.025 | Profile function: CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 48.559 #2(GV) = -12.839 #3(GW) = 1.726
#4(GP) = 1.788 #5(LX) = 0.000 #6(LY) = 35.036
#7(S/L) = 0.0051 #8(H/L) = 0.0053
#9(trns) = 1.71 #10(shft)= -0.0935
#11(stec)= -5.24 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0010 times the peak
Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 566.328 #2(GV) = -259.656 #3(GW) = 16.214
#4(GP) = 21.727 #5(LX) = 0.000 #6(LY) = 14.182
#7(S/L) = 0.0005 #8(H/L) = 0.0005
#9(trns) = 0.10 #10(shft)= 0.5088
#11(stec)= 9.76 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0010 times the peak
Aniso. broadening axis 0.0 0.0 1.0 |
Rwp = 0.037 | 212 parameters |
Rexp = 0.012 | 139 restraints |
R(F2) = 0.09479 | (Δ/σ)max = 0.73 |
χ2 = 10.368 | Background function: GSAS Background function number 1 with 14 terms.
Shifted Chebyshev function of 1st kind
1: 5355.24 2: -1049.87 3: -648.428 4: 844.728
5: -156.605 6: -613.953 7: 516.877 8: 102.555
9: -478.794 10: 194.480 11: 99.4550 12: -253.881
13: 23.9897 14: 104.895 |
Crystal data top
? | β = ?° |
Mr = ? | γ = ?° |
?, ? | V = ? Å3 |
a = ? Å | Z = ? |
b = ? Å | ? radiation, λ = 0.999995 Å |
c = ? Å | ?, ? × ? × ? mm |
α = ?° | |
Data collection top
2θmin = 0.010°, 2θmax = 1.800°, 2θstep = 0.01° | |
Refinement top
Rp = 0.025 | 180 data points |
Rwp = 0.037 | 212 parameters |
Rexp = 0.012 | 139 restraints |
R(F2) = 0.09479 | (Δ/σ)max = 0.73 |
χ2 = 10.368 | |
(TEEI90RRLAST_phase_1)
top
Crystal data top
C18H30B2F8FeI6N24 | β = 90.5991 (17)° |
Mr = 1573.50 | V = 2279.25 Å3 |
Monoclinic, P21/c | Z = 2 |
a = 12.3177 (3) Å | ? radiation, λ = 0.999995 Å |
b = 17.6766 (4) Å | ?, ? × ? × ? mm |
c = 10.4685 (3) Å | |
Data collection top
2θmin = 0.010°, 2θmax = 1.800°, 2θstep = 0.01° | |
Refinement top
Least-squares matrix: full | Profile function: CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 48.559 #2(GV) = -12.839 #3(GW) = 1.726
#4(GP) = 1.788 #5(LX) = 0.000 #6(LY) = 35.036
#7(S/L) = 0.0051 #8(H/L) = 0.0053
#9(trns) = 1.71 #10(shft)= -0.0935
#11(stec)= -5.24 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0010 times the peak
Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 566.328 #2(GV) = -259.656 #3(GW) = 16.214
#4(GP) = 21.727 #5(LX) = 0.000 #6(LY) = 14.182
#7(S/L) = 0.0005 #8(H/L) = 0.0005
#9(trns) = 0.10 #10(shft)= 0.5088
#11(stec)= 9.76 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0010 times the peak
Aniso. broadening axis 0.0 0.0 1.0 |
Rp = 0.025 | 212 parameters |
Rwp = 0.037 | 139 restraints |
Rexp = 0.012 | (Δ/σ)max = 0.73 |
R(F2) = 0.09479 | Background function: GSAS Background function number 1 with 14 terms.
Shifted Chebyshev function of 1st kind
1: 5355.24 2: -1049.87 3: -648.428 4: 844.728
5: -156.605 6: -613.953 7: 516.877 8: 102.555
9: -478.794 10: 194.480 11: 99.4550 12: -253.881
13: 23.9897 14: 104.895 |
χ2 = 10.368 | Preferred orientation correction: Spherical Harmonic ODF
PHASE 8 spherical harmonic order= 12
The sample symmetry is: cylindrical (fiber texture)
Index = 2 0 -2 Coeff= 0.1561
Index = 2 0 0 Coeff= -0.0949
Index = 2 0 2 Coeff= 0.1086
Index = 4 0 -4 Coeff= 0.1750
Index = 4 0 -2 Coeff= 0.2929
Index = 4 0 0 Coeff= -0.1704
Index = 4 0 2 Coeff= 0.0519
Index = 4 0 4 Coeff= 0.1589
Index = 6 0 -6 Coeff= -0.2985
Index = 6 0 -4 Coeff= 0.0680
Index = 6 0 -2 Coeff= 0.4817
Index = 6 0 0 Coeff= -0.4129
Index = 6 0 2 Coeff= 0.0545
Index = 6 0 4 Coeff= 0.0866
Index = 6 0 6 Coeff= 0.1516
Index = 8 0 -8 Coeff= -0.1592
Index = 8 0 -6 Coeff= 0.2818
Index = 8 0 -4 Coeff= -0.1597
Index = 8 0 -2 Coeff= 0.2573
Index = 8 0 0 Coeff= 0.2362
Index = 8 0 2 Coeff= 0.4805
Index = 8 0 4 Coeff= -0.2841
Index = 8 0 6 Coeff= 0.1408
Index = 8 0 8 Coeff= -0.2015
Index = 10 0-10 Coeff= 0.2043
Index = 10 0 -8 Coeff= 0.8930
Index = 10 0 -6 Coeff= -0.6192
Index = 10 0 -4 Coeff= -0.8047
Index = 10 0 -2 Coeff= 0.2301
Index = 10 0 0 Coeff= -1.0667
Index = 10 0 2 Coeff= 0.2810
Index = 10 0 4 Coeff= 0.0277
Index = 10 0 6 Coeff= -0.1352
Index = 10 0 8 Coeff= -0.1009
Index = 10 0 10 Coeff= -0.0845
Index = 12 0-12 Coeff= -0.4362
Index = 12 0-10 Coeff= -1.1188
Index = 12 0 -8 Coeff= 0.5807
Index = 12 0 -6 Coeff= -0.1400
Index = 12 0 -4 Coeff= -1.2841
Index = 12 0 -2 Coeff= 0.3818
Index = 12 0 0 Coeff= -0.1003
Index = 12 0 2 Coeff= -0.5853
Index = 12 0 4 Coeff= 0.5849
Index = 12 0 6 Coeff= 0.1246
Index = 12 0 8 Coeff= 0.5909
Index = 12 0 10 Coeff= 0.1549
Index = 12 0 12 Coeff= -0.9864 |
180 data points | |
Crystal data top
C18H30B2F8FeI6N24 | β = 90.5991 (17)° |
Mr = 1573.50 | V = 2279.25 Å3 |
Monoclinic, P21/c | Z = 2 |
a = 12.3177 (3) Å | ? radiation, λ = 0.999995 Å |
b = 17.6766 (4) Å | ?, ? × ? × ? mm |
c = 10.4685 (3) Å | |
Data collection top
2θmin = 0.010°, 2θmax = 1.800°, 2θstep = 0.01° | |
Refinement top
Rp = 0.025 | 180 data points |
Rwp = 0.037 | 212 parameters |
Rexp = 0.012 | 139 restraints |
R(F2) = 0.09479 | (Δ/σ)max = 0.73 |
χ2 = 10.368 | |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe | 0.0 | 0.0 | 0.0 | 0.020 (5)* | |
I1 | −0.4190 (4) | 0.1953 (2) | 0.0763 (5) | 0.0365 (6)* | |
I2 | −0.4107 (4) | −0.0756 (2) | −0.3263 (4) | 0.0365 (6)* | |
I3 | −0.4210 (3) | −0.1132 (2) | 0.2382 (4) | 0.0365 (6)* | |
N4A | −0.0973 (14) | 0.0633 (12) | 0.1157 (16) | 0.025* | |
N3A | −0.1658 (18) | 0.0417 (14) | 0.200 (2) | 0.025* | |
N2A | −0.2198 (17) | 0.0936 (14) | 0.253 (2) | 0.025* | |
N1A | −0.1842 (14) | 0.1519 (13) | 0.1987 (18) | 0.025* | |
N4B | −0.0941 (14) | 0.0279 (10) | −0.1459 (17) | 0.025* | |
N4C | −0.0897 (14) | −0.0834 (10) | 0.0309 (15) | 0.025* | |
N3B | −0.1492 (18) | 0.0894 (15) | −0.141 (3) | 0.025* | |
N3C | −0.1433 (16) | −0.1211 (11) | −0.047 (2) | 0.025* | |
N2B | −0.2128 (19) | 0.0997 (16) | −0.245 (3) | 0.025* | |
N1B | −0.1889 (16) | 0.0375 (14) | −0.307 (2) | 0.025* | |
N2C | −0.1975 (15) | −0.1701 (11) | 0.006 (2) | 0.025* | |
N1C | −0.1811 (14) | −0.1647 (11) | 0.123 (2) | 0.025* | |
C1A | −0.1105 (15) | 0.1320 (13) | 0.1104 (17) | 0.025* | |
C2A | −0.222 (2) | 0.2271 (17) | 0.225 (3) | 0.025* | |
C3A | −0.328 (3) | 0.222 (2) | 0.248 (3) | 0.025* | |
C1B | −0.1171 (17) | −0.0071 (13) | −0.247 (2) | 0.025* | |
C1C | −0.1142 (14) | −0.1103 (10) | 0.1357 (17) | 0.025* | |
C2B | −0.2369 (17) | 0.0177 (15) | −0.423 (3) | 0.025* | |
C2C | −0.2233 (17) | −0.2047 (14) | 0.232 (3) | 0.025* | |
C3B | −0.356 (2) | 0.0334 (15) | −0.389 (3) | 0.025* | |
C3C | −0.3389 (19) | −0.2026 (15) | 0.188 (3) | 0.025* | |
H1A | −0.063 (3) | 0.167 (3) | 0.043 (4) | 0.025* | |
H2A2 | −0.176 (6) | 0.249 (5) | 0.311 (6) | 0.025* | |
H2A1 | −0.215 (6) | 0.263 (4) | 0.146 (6) | 0.025* | |
H3A2 | −0.349 (6) | 0.271 (4) | 0.293 (7) | 0.025* | |
H3A1 | −0.342 (7) | 0.172 (4) | 0.314 (7) | 0.025* | |
H1B | −0.085 (3) | −0.061 (3) | −0.275 (5) | 0.025* | |
H1C | −0.084 (3) | −0.088 (3) | 0.224 (5) | 0.025* | |
H2B2 | −0.215 (6) | 0.054 (4) | −0.495 (6) | 0.025* | |
H2B1 | −0.232 (6) | −0.038 (3) | −0.445 (7) | 0.025* | |
H2C2 | −0.198 (6) | −0.260 (3) | 0.226 (7) | 0.025* | |
H2C1 | −0.221 (6) | −0.177 (4) | 0.318 (5) | 0.025* | |
H3B2 | −0.395 (6) | 0.046 (4) | −0.478 (6) | 0.025* | |
H3B1 | −0.362 (6) | 0.075 (4) | −0.318 (7) | 0.025* | |
H3C2 | −0.370 (6) | −0.253 (4) | 0.242 (8) | 0.025* | |
H3C1 | −0.339 (6) | −0.219 (5) | 0.090 (5) | 0.025* | |
B | 0.0071 (18) | 0.1617 (13) | 0.502 (2) | 0.025* | |
F1 | 0.045 (2) | 0.2189 (12) | 0.577 (3) | 0.025* | |
F2 | −0.0946 (18) | 0.1830 (14) | 0.494 (2) | 0.025* | |
F3 | 0.0704 (18) | 0.1593 (13) | 0.400 (2) | 0.025* | |
F4 | 0.020 (2) | 0.1028 (12) | 0.572 (2) | 0.025* | |
Geometric parameters (Å, º) top
Fe—N4A | 2.05 (2) | N1C—C2C | 1.44 (3) |
Fe—N4B | 1.97 (2) | C1A—H1A | 1.11 (5) |
Fe—N4C | 1.873 (19) | C2A—C3A | 1.33 (3) |
I1—C3A | 2.16 (3) | C2A—H2A2 | 1.12 (5) |
I2—C3B | 2.14 (3) | C2A—H2A1 | 1.05 (5) |
I3—C3C | 1.95 (3) | C3A—H3A2 | 1.02 (5) |
N4A—N3A | 1.29 (3) | C3A—H3A1 | 1.13 (5) |
N4A—C1A | 1.23 (2) | C1B—H1B | 1.07 (4) |
N3A—N2A | 1.26 (2) | C1C—H1C | 1.06 (5) |
N2A—N1A | 1.26 (2) | C2B—C3B | 1.54 (2) |
N1A—C1A | 1.350 (17) | C2B—H2B2 | 1.02 (5) |
N1A—C2A | 1.44 (3) | C2B—H2B1 | 1.01 (5) |
N4B—N3B | 1.28 (3) | C2C—C3C | 1.49 (2) |
N4B—C1B | 1.26 (2) | C2C—H2C2 | 1.03 (5) |
N3B—N2B | 1.35 (3) | C2C—H2C1 | 1.03 (5) |
N2B—N1B | 1.31 (3) | C3B—H3B2 | 1.07 (5) |
N1B—C1B | 1.33 (3) | C3B—H3B1 | 1.04 (5) |
N1B—C2B | 1.39 (3) | C3C—H3C2 | 1.12 (5) |
N4C—N3C | 1.24 (3) | C3C—H3C1 | 1.06 (5) |
N4C—C1C | 1.236 (14) | B—F1 | 1.36 (2) |
N3C—N2C | 1.229 (15) | B—F2 | 1.31 (2) |
N2C—N1C | 1.24 (2) | B—F3 | 1.33 (2) |
N1C—C1C | 1.27 (2) | B—F4 | 1.29 (2) |
| | | |
N4A—Fe—N4Ai | 180.0 | I1—C3A—C2A | 111 (2) |
N4A—Fe—N4B | 88.7 (5) | I1—C3A—H3A2 | 116 (4) |
N4A—Fe—N4Bi | 91.3 (5) | I1—C3A—H3A1 | 104 (4) |
N4A—Fe—N4C | 88.7 (7) | C2A—C3A—H3A2 | 106 (4) |
N4A—Fe—N4Ci | 91.3 (7) | C2A—C3A—H3A1 | 109 (4) |
N4Ai—Fe—N4B | 91.3 (5) | H3A2—C3A—H3A1 | 110 (4) |
N4Ai—Fe—N4Bi | 88.7 (5) | N4B—C1B—N1B | 104 (2) |
N4Ai—Fe—N4C | 91.3 (7) | N4B—C1B—H1B | 126 (3) |
N4Ai—Fe—N4Ci | 88.7 (7) | N1B—C1B—H1B | 130 (3) |
N4B—Fe—N4Bi | 180.0 | N4C—C1C—N1C | 111.4 (17) |
N4B—Fe—N4C | 89.3 (6) | N4C—C1C—H1C | 123 (3) |
N4B—Fe—N4Ci | 90.7 (6) | N1C—C1C—H1C | 126 (3) |
N4Bi—Fe—N4C | 90.7 (6) | N1B—C2B—C3B | 98.7 (17) |
N4Bi—Fe—N4Ci | 89.3 (6) | N1B—C2B—H2B2 | 112 (4) |
N4C—Fe—N4Ci | 180.0 | N1B—C2B—H2B1 | 115 (4) |
N3A—N4A—C1A | 103.8 (19) | C3B—C2B—H2B2 | 108 (4) |
N4A—N3A—N2A | 116 (2) | C3B—C2B—H2B1 | 107 (4) |
N3A—N2A—N1A | 102 (2) | H2B2—C2B—H2B1 | 115 (4) |
N2A—N1A—C1A | 110 (2) | N1C—C2C—C3C | 95.7 (17) |
N2A—N1A—C2A | 124 (2) | N1C—C2C—H2C2 | 108 (4) |
C1A—N1A—C2A | 127 (2) | N1C—C2C—H2C1 | 117 (4) |
N3B—N4B—C1B | 110 (2) | C3C—C2C—H2C2 | 107 (4) |
N3C—N4C—C1C | 103.9 (17) | C3C—C2C—H2C1 | 106 (4) |
N4B—N3B—N2B | 113 (2) | H2C2—C2C—H2C1 | 120 (4) |
N4C—N3C—N2C | 112 (2) | I2—C3B—C2B | 102.1 (14) |
N3B—N2B—N1B | 99 (2) | I2—C3B—H3B2 | 108 (4) |
N2B—N1B—C1B | 115 (2) | I2—C3B—H3B1 | 113 (4) |
N2B—N1B—C2B | 123 (2) | C2B—C3B—H3B2 | 105 (4) |
C1B—N1B—C2B | 122 (2) | C2B—C3B—H3B1 | 111 (4) |
N3C—N2C—N1C | 108 (2) | H3B2—C3B—H3B1 | 117 (4) |
N2C—N1C—C1C | 104.9 (19) | I3—C3C—C2C | 115.7 (16) |
N2C—N1C—C2C | 133 (2) | I3—C3C—H3C2 | 109 (4) |
C1C—N1C—C2C | 122.1 (19) | I3—C3C—H3C1 | 119 (4) |
N4A—C1A—N1A | 108.5 (19) | C2C—C3C—H3C2 | 99 (4) |
N4A—C1A—H1A | 121 (3) | C2C—C3C—H3C1 | 106 (4) |
N1A—C1A—H1A | 130 (3) | H3C2—C3C—H3C1 | 105 (4) |
N1A—C2A—C3A | 107 (2) | F1—B—F2 | 98 (2) |
N1A—C2A—H2A2 | 108 (4) | F1—B—F3 | 107 (2) |
N1A—C2A—H2A1 | 113 (4) | F1—B—F4 | 103 (2) |
C3A—C2A—H2A2 | 112 (4) | F2—B—F3 | 121.7 (18) |
C3A—C2A—H2A1 | 106 (4) | F2—B—F4 | 113 (2) |
H2A2—C2A—H2A1 | 112 (4) | F3—B—F4 | 111 (2) |
Symmetry code: (i) −x, −y, −z. |
Crystal data top
? | β = ?° |
Mr = ? | γ = ?° |
?, ? | V = ? Å3 |
a = ? Å | Z = ? |
b = ? Å | ? radiation, λ = 0.999995 Å |
c = ? Å | ?, ? × ? × ? mm |
α = ?° | |
Data collection top
2θmin = 0.010°, 2θmax = 1.800°, 2θstep = 0.01° | |
Refinement top
Rp = 0.025 | 180 data points |
Rwp = 0.037 | Profile function: CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 48.559 #2(GV) = -12.839 #3(GW) = 1.726
#4(GP) = 1.788 #5(LX) = 0.000 #6(LY) = 35.036
#7(S/L) = 0.0051 #8(H/L) = 0.0053
#9(trns) = 1.71 #10(shft)= -0.0935
#11(stec)= -5.24 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0010 times the peak
Aniso. broadening axis 0.0 0.0 1.0, CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 566.328 #2(GV) = -259.656 #3(GW) = 16.214
#4(GP) = 21.727 #5(LX) = 0.000 #6(LY) = 14.182
#7(S/L) = 0.0005 #8(H/L) = 0.0005
#9(trns) = 0.10 #10(shft)= 0.5088
#11(stec)= 9.76 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0010 times the peak
Aniso. broadening axis 0.0 0.0 1.0 |
Rexp = 0.012 | |
R(F2) = 0.09479 | Background function: GSAS Background function number 1 with 14 terms.
Shifted Chebyshev function of 1st kind
1: 5355.24 2: -1049.87 3: -648.428 4: 844.728
5: -156.605 6: -613.953 7: 516.877 8: 102.555
9: -478.794 10: 194.480 11: 99.4550 12: -253.881
13: 23.9897 14: 104.895 |
χ2 = NOT FOUND | |
Crystal data top
? | β = ?° |
Mr = ? | γ = ?° |
?, ? | V = ? Å3 |
a = ? Å | Z = ? |
b = ? Å | ? radiation, λ = 0.999995 Å |
c = ? Å | ?, ? × ? × ? mm |
α = ?° | |
Data collection top
2θmin = 0.010°, 2θmax = 1.800°, 2θstep = 0.01° | |
Refinement top
Rp = 0.025 | R(F2) = 0.09479 |
Rwp = 0.037 | χ2 = NOT FOUND |
Rexp = 0.012 | 180 data points |
Crystal data top
C18H30B2Br6F8FeN24 | V = 2325.45 Å3 |
Mr = 1291.53 | Z = 2 |
Monoclinic, P21/c | Synchrotron radiation, λ = 0.999995 Å |
a = 12.2832 (6) Å | T = 300 K K |
b = 18.0705 (15) Å | white |
c = 10.4767 (3) Å | ?, ? × ? × ? mm |
β = 90.106 (3)° | |
Data collection top
Debye Scherrer diffractometer | 2θmin = 0.010°, 2θmax = 1.800°, 2θstep = 0.01° |
Refinement top
Least-squares matrix: full | Profile function: CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 645.207 #2(GV) = -69.966 #3(GW) = 3.518
#4(GP) = 4.107 #5(LX) = 1.393 #6(LY) = 17.492
#7(S/L) = 0.0079 #8(H/L) = 0.0083
#9(trns) = 1.19 #10(shft)= -0.3822
#11(stec)= -14.81 #12(ptec)= -0.97 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0010 times the peak
Aniso. broadening axis 0.0 0.0 1.0 |
Rp = 0.046 | 184 parameters |
Rwp = 0.065 | 145 restraints |
Rexp = 0.011 | (Δ/σ)max = 0.64 |
χ2 = 40.704 | Background function: GSAS Background function number 1 with 14 terms.
Shifted Chebyshev function of 1st kind
1: 6463.90 2: 534.229 3: -2434.12 4: 1153.68
5: 82.1130 6: -855.145 7: 913.714 8: -212.529
9: -555.454 10: 605.683 11: 41.4069 12: -404.910
13: 340.430 14: 3.29907 |
180 data points | Preferred orientation correction: Spherical Harmonic ODF
Spherical harmonic order= 6
The sample symmetry is: cylindrical (fiber texture)
Index = 2 0 -2 Coeff= 0.3053
Index = 2 0 0 Coeff= 0.9590
Index = 2 0 2 Coeff= -0.4154
Index = 4 0 -4 Coeff= 1.0675
Index = 4 0 -2 Coeff= -0.3934
Index = 4 0 0 Coeff= -0.3008
Index = 4 0 2 Coeff= -1.2874
Index = 4 0 4 Coeff= -1.2947
Index = 6 0 -6 Coeff= 0.6688
Index = 6 0 -4 Coeff= -3.3617
Index = 6 0 -2 Coeff= 2.4541
Index = 6 0 0 Coeff= 1.1464
Index = 6 0 2 Coeff= -3.9732
Index = 6 0 4 Coeff= -2.1103
Index = 6 0 6 Coeff= 4.1837
Prefered orientation correction range: Min= -1.18333, Max= 4.64248 |
Crystal data top
C18H30B2Br6F8FeN24 | β = 90.106 (3)° |
Mr = 1291.53 | V = 2325.45 Å3 |
Monoclinic, P21/c | Z = 2 |
a = 12.2832 (6) Å | Synchrotron radiation, λ = 0.999995 Å |
b = 18.0705 (15) Å | T = 300 K K |
c = 10.4767 (3) Å | ?, ? × ? × ? mm |
Data collection top
Debye Scherrer diffractometer | 2θmin = 0.010°, 2θmax = 1.800°, 2θstep = 0.01° |
Refinement top
Rp = 0.046 | 180 data points |
Rwp = 0.065 | 184 parameters |
Rexp = 0.011 | 145 restraints |
χ2 = 40.704 | (Δ/σ)max = 0.64 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe | 0.0 | 0.0 | 0.0 | 0.034 (4)* | |
Br3 | −0.4035 (7) | −0.1466 (5) | 0.3202 (8) | 0.158 (2)* | |
Br1 | −0.3890 (7) | 0.1402 (5) | 0.3135 (8) | 0.158 (2)* | |
Br2 | −0.4123 (7) | −0.0580 (5) | −0.3075 (7) | 0.158 (2)* | |
N4c | −0.1078 (6) | −0.0882 (3) | 0.0757 (9) | 0.093 (7)* | |
N3c | −0.0918 (12) | −0.1291 (8) | 0.1834 (13) | 0.093 (7)* | |
N2c | −0.1744 (12) | −0.1722 (8) | 0.2011 (14) | 0.093 (7)* | |
N1c | −0.2452 (9) | −0.1624 (7) | 0.1118 (12) | 0.093 (7)* | |
N4a | −0.1144 (5) | 0.0828 (4) | 0.0810 (9) | 0.093 (7)* | |
N4b | −0.0960 (6) | 0.0056 (6) | −0.1802 (4) | 0.093 (7)* | |
N3a | −0.1666 (12) | 0.0759 (8) | 0.1972 (13) | 0.093 (7)* | |
N3b | −0.0782 (12) | −0.0339 (8) | −0.2868 (11) | 0.093 (7)* | |
N2a | −0.2312 (12) | 0.1302 (9) | 0.2224 (14) | 0.093 (7)* | |
N1a | −0.2324 (10) | 0.1715 (7) | 0.1190 (12) | 0.093 (7)* | |
N2b | −0.1459 (12) | −0.0182 (9) | −0.3804 (12) | 0.093 (7)* | |
N1b | −0.2095 (9) | 0.0318 (7) | −0.3387 (11) | 0.093 (7)* | |
C1c | −0.2043 (9) | −0.1088 (7) | 0.0370 (12) | 0.065 (9)* | |
C2c | −0.3513 (10) | −0.2043 (7) | 0.0957 (13) | 0.065 (9)* | |
C3c | −0.4407 (11) | −0.1611 (9) | 0.1552 (15) | 0.065 (9)* | |
C1a | −0.1649 (10) | 0.1427 (7) | 0.0312 (11) | 0.065 (9)* | |
C1b | −0.1816 (9) | 0.0475 (7) | −0.2162 (11) | 0.065 (9)* | |
C2a | −0.3032 (10) | 0.2383 (7) | 0.1174 (13) | 0.065 (9)* | |
C2b | −0.2954 (10) | 0.0596 (7) | −0.4221 (12) | 0.065 (9)* | |
C3a | −0.3640 (12) | 0.2426 (9) | 0.2480 (14) | 0.065 (9)* | |
C3b | −0.3998 (12) | 0.0451 (9) | −0.3419 (15) | 0.065 (9)* | |
H1c | −0.2429 (19) | −0.0866 (13) | −0.0491 (17) | 0.025* | |
H2c2 | −0.368 (2) | −0.214 (2) | −0.0082 (18) | 0.025* | |
H2c1 | −0.344 (2) | −0.2589 (11) | 0.138 (3) | 0.025* | |
H3c2 | −0.5163 (16) | −0.1889 (18) | 0.142 (3) | 0.025* | |
H3c1 | −0.443 (3) | −0.1071 (12) | 0.107 (3) | 0.025* | |
H1a | −0.1488 (19) | 0.1653 (13) | −0.0617 (17) | 0.025* | |
H1b | −0.2225 (18) | 0.0883 (11) | −0.158 (2) | 0.025* | |
H2a1 | −0.254 (2) | 0.2869 (11) | 0.104 (3) | 0.025* | |
H2a2 | −0.3642 (19) | 0.2337 (19) | 0.044 (2) | 0.025* | |
H2b2 | −0.286 (3) | 0.1181 (10) | −0.438 (3) | 0.025* | |
H2b1 | −0.296 (2) | 0.0294 (16) | −0.5100 (19) | 0.025* | |
H3a1 | −0.4349 (18) | 0.2735 (15) | 0.238 (3) | 0.025* | |
H3a2 | −0.307 (2) | 0.2703 (16) | 0.316 (2) | 0.025* | |
H3b2 | −0.4679 (18) | 0.0689 (16) | −0.394 (3) | 0.025* | |
H3b1 | −0.390 (3) | 0.0783 (15) | −0.254 (2) | 0.025* | |
B | 0.0269 (9) | 0.1867 (7) | 0.4989 (12) | 0.01 (3)* | |
F1 | 0.0254 (18) | 0.2593 (7) | 0.540 (2) | 0.226 (13)* | |
F2 | 0.0716 (15) | 0.1525 (10) | 0.5947 (14) | 0.226 (13)* | |
F3 | −0.0769 (9) | 0.1737 (12) | 0.481 (2) | 0.226 (13)* | |
F4 | 0.0852 (14) | 0.1893 (14) | 0.3943 (13) | 0.226 (13)* | |
Geometric parameters (Å, º) top
Fe—N4c | 2.219 (3) | C1a—H1a | 1.075 (14) |
Fe—N4ci | 2.219 (3) | C1b—N4b | 1.349 (9) |
Fe—N4a | 2.223 (3) | C1b—N3b | 2.080 (15) |
Fe—N4ai | 2.223 (3) | C1b—N2b | 2.136 (15) |
Fe—N4b | 2.227 (3) | C1b—N1b | 1.357 (12) |
Fe—N4bi | 2.227 (3) | C1b—H1b | 1.081 (15) |
Br3—C2c | 2.653 (14) | C2a—Br1 | 2.913 (15) |
Br3—C3c | 1.806 (16) | C2a—N1a | 1.487 (12) |
Br3—H3c2 | 2.45 (3) | C2a—C3a | 1.562 (13) |
Br3—H3c1 | 2.40 (3) | C2a—H2a1 | 1.074 (15) |
Br3—H3a1ii | 2.53 (2) | C2a—H2a2 | 1.080 (15) |
Br3—H3b2iii | 2.25 (3) | C2b—Br2 | 2.834 (15) |
Br1—Br2iii | 2.857 (12) | C2b—N1b | 1.459 (12) |
Br1—N2a | 2.170 (16) | C2b—C3b | 1.556 (13) |
Br1—N1a | 2.862 (15) | C2b—H2b2 | 1.077 (15) |
Br1—C2a | 2.913 (15) | C2b—H2b1 | 1.070 (15) |
Br1—C3a | 1.998 (16) | C3a—Br1 | 1.998 (16) |
Br1—H3a1 | 2.60 (3) | C3a—C2a | 1.562 (13) |
Br1—H3a2 | 2.56 (3) | C3a—H3a1 | 1.040 (16) |
Br2—Br1iii | 2.857 (12) | C3a—H3a2 | 1.112 (17) |
Br2—C2b | 2.834 (15) | C3b—Br2 | 1.904 (17) |
Br2—C3b | 1.904 (17) | C3b—C2b | 1.556 (13) |
Br2—H3b2 | 2.56 (3) | C3b—H3b2 | 1.088 (16) |
Br2—H3b1 | 2.54 (3) | C3b—H3b1 | 1.109 (16) |
N4c—Fe | 2.219 (3) | H1c—C1c | 1.094 (15) |
N4c—N3c | 1.363 (12) | H2c2—C2c | 1.118 (15) |
N4c—C1c | 1.306 (11) | H2c2—H2c1 | 1.76 (3) |
N3c—N4c | 1.363 (12) | H2c1—C2c | 1.085 (15) |
N3c—N2c | 1.292 (13) | H2c1—H2c2 | 1.76 (3) |
N3c—N1c | 2.115 (16) | H3c2—Br3 | 2.45 (3) |
N3c—C1c | 2.094 (16) | H3c2—C3c | 1.065 (16) |
N3c—F2iv | 2.376 (19) | H3c2—H3c1 | 1.77 (3) |
N2c—N3c | 1.292 (13) | H3c2—H3a1ii | 1.55 (4) |
N2c—N1c | 1.289 (13) | H3c1—Br3 | 2.40 (3) |
N2c—C1c | 2.097 (16) | H3c1—C2c | 2.09 (2) |
N1c—N3c | 2.115 (16) | H3c1—C3c | 1.099 (16) |
N1c—N2c | 1.289 (13) | H3c1—H3c2 | 1.77 (3) |
N1c—C1c | 1.343 (12) | H1a—C1a | 1.075 (14) |
N1c—C2c | 1.516 (12) | H1a—H1b | 1.94 (3) |
N4a—Fe | 2.223 (3) | H1b—C1b | 1.081 (15) |
N4a—N3a | 1.383 (12) | H1b—H1a | 1.94 (3) |
N4a—C1a | 1.351 (11) | H2a1—C2a | 1.074 (15) |
N4b—Fe | 2.227 (3) | H2a1—H2a2 | 1.78 (2) |
N4b—N3b | 1.343 (9) | H2a1—H2b2v | 1.82 (3) |
N4b—C1b | 1.349 (9) | H2a2—C2a | 1.080 (15) |
N3a—N4a | 1.383 (12) | H2a2—H2a1 | 1.78 (2) |
N3a—N2a | 1.289 (14) | H2b2—C2b | 1.077 (15) |
N3a—N1a | 2.076 (16) | H2b2—H2a1vi | 1.82 (3) |
N3a—C1a | 2.117 (16) | H2b2—H2b1 | 1.77 (2) |
N3b—N4b | 1.343 (9) | H2b1—C2b | 1.070 (15) |
N3b—N2b | 1.316 (13) | H2b1—H2b2 | 1.77 (2) |
N3b—N1b | 2.075 (15) | H3a1—Br3vii | 2.53 (2) |
N3b—C1b | 2.080 (15) | H3a1—Br1 | 2.60 (3) |
N2a—Br1 | 2.170 (16) | H3a1—C3a | 1.040 (16) |
N2a—N3a | 1.289 (14) | H3a1—H3c2vii | 1.55 (4) |
N2a—N1a | 1.317 (13) | H3a1—H3a2 | 1.77 (2) |
N2a—C1a | 2.175 (16) | H3a2—Br1 | 2.56 (3) |
N1a—Br1 | 2.862 (15) | H3a2—C3a | 1.112 (17) |
N1a—N3a | 2.076 (16) | H3a2—H3a1 | 1.77 (2) |
N1a—N2a | 1.317 (13) | H3b2—Br3iii | 2.25 (3) |
N1a—C1a | 1.344 (12) | H3b2—Br2 | 2.56 (3) |
N1a—C2a | 1.487 (12) | H3b2—C3b | 1.088 (16) |
N2b—N3b | 1.316 (13) | H3b2—H3b1 | 1.77 (3) |
N2b—N1b | 1.273 (13) | H3b1—Br2 | 2.54 (3) |
N2b—C1b | 2.136 (15) | H3b1—C3b | 1.109 (16) |
N1b—N3b | 2.075 (15) | H3b1—H3b2 | 1.77 (3) |
N1b—N2b | 1.273 (13) | B—F1 | 1.381 (12) |
N1b—C1b | 1.357 (12) | B—F2 | 1.299 (12) |
N1b—C2b | 1.459 (12) | B—F3 | 1.310 (11) |
C1c—N4c | 1.306 (11) | B—F4 | 1.311 (11) |
C1c—N3c | 2.094 (16) | F1—B | 1.381 (12) |
C1c—N2c | 2.097 (16) | F1—F2 | 2.093 (13) |
C1c—N1c | 1.343 (12) | F1—F3 | 2.085 (14) |
C1c—H1c | 1.094 (15) | F1—F4 | 2.113 (14) |
C2c—Br3 | 2.653 (14) | F2—N3civ | 2.376 (19) |
C2c—N1c | 1.516 (12) | F2—B | 1.299 (12) |
C2c—C3c | 1.486 (13) | F2—F1 | 2.093 (13) |
C2c—H2c2 | 1.118 (15) | F2—F3 | 2.210 (13) |
C2c—H2c1 | 1.085 (15) | F2—F4 | 2.209 (13) |
C2c—H3c1 | 2.09 (2) | F3—B | 1.310 (11) |
C3c—Br3 | 1.806 (16) | F3—F1 | 2.085 (14) |
C3c—C2c | 1.486 (13) | F3—F2 | 2.210 (13) |
C3c—H3c2 | 1.065 (16) | F3—F4 | 2.208 (13) |
C3c—H3c1 | 1.099 (16) | F4—B | 1.311 (11) |
C1a—N4a | 1.351 (11) | F4—F1 | 2.113 (14) |
C1a—N3a | 2.117 (16) | F4—F2 | 2.209 (13) |
C1a—N2a | 2.175 (16) | F4—F3 | 2.208 (13) |
C1a—N1a | 1.344 (12) | | |
| | | |
C3c—Br3—H3b2iii | 104.0 (9) | N4b—C1b—H1b | 126.1 (13) |
Br2iii—Br1—N2a | 135.3 (6) | N1b—C1b—H1b | 123.9 (12) |
Br2iii—Br1—C3a | 127.3 (6) | N1a—C2a—C3a | 108.2 (9) |
N2a—Br1—C3a | 77.7 (6) | N1a—C2a—H2a1 | 109.6 (14) |
Br1iii—Br2—C3b | 125.0 (6) | N1a—C2a—H2a2 | 110.5 (15) |
N3c—N4c—C1c | 103.4 (8) | C3a—C2a—H2a1 | 110.0 (15) |
N4c—N3c—N2c | 109.5 (10) | C3a—C2a—H2a2 | 107.4 (14) |
N3c—N2c—N1c | 110.0 (11) | H2a1—C2a—H2a2 | 111.0 (17) |
N2c—N1c—C1c | 105.6 (9) | N1b—C2b—C3b | 102.3 (9) |
N2c—N1c—C2c | 126.2 (10) | N1b—C2b—H2b2 | 110.8 (15) |
C1c—N1c—C2c | 128.1 (10) | N1b—C2b—H2b1 | 109.9 (15) |
N3a—N4a—C1a | 101.5 (8) | C3b—C2b—H2b2 | 109.9 (15) |
N3b—N4b—C1b | 101.2 (7) | C3b—C2b—H2b1 | 112.2 (15) |
N4a—N3a—N2a | 113.5 (10) | H2b2—C2b—H2b1 | 111.4 (16) |
N4b—N3b—N2b | 113.7 (10) | Br1—C3a—C2a | 109.2 (9) |
Br1—N2a—N3a | 134.8 (12) | Br1—C3a—H3a1 | 113.8 (14) |
Br1—N2a—N1a | 107.8 (10) | Br1—C3a—H3a2 | 107.2 (15) |
N3a—N2a—N1a | 105.6 (10) | C2a—C3a—H3a1 | 109.8 (15) |
N2a—N1a—C1a | 109.7 (9) | C2a—C3a—H3a2 | 106.2 (15) |
N2a—N1a—C2a | 118.4 (10) | H3a1—C3a—H3a2 | 110.4 (17) |
C1a—N1a—C2a | 132.0 (10) | Br2—C3b—C2b | 109.5 (9) |
N3b—N2b—N1b | 106.5 (10) | Br2—C3b—H3b2 | 114.8 (15) |
N2b—N1b—C1b | 108.6 (9) | Br2—C3b—H3b1 | 112.5 (14) |
N2b—N1b—C2b | 118.9 (10) | C2b—C3b—H3b2 | 107.1 (15) |
C1b—N1b—C2b | 132.5 (10) | C2b—C3b—H3b1 | 105.4 (16) |
N4c—C1c—N1c | 111.4 (8) | H3b2—C3b—H3b1 | 106.9 (17) |
N4c—C1c—H1c | 122.9 (13) | C3c—H3c2—H3a1ii | 116 (2) |
N1c—C1c—H1c | 125.6 (13) | C3a—H3a1—H3c2vii | 119 (2) |
N1c—C2c—C3c | 109.0 (9) | Br3iii—H3b2—C3b | 128 (2) |
N1c—C2c—H2c2 | 109.6 (15) | F1—B—F2 | 102.6 (10) |
N1c—C2c—H2c1 | 109.8 (15) | F1—B—F3 | 101.6 (10) |
C3c—C2c—H2c2 | 110.8 (15) | F1—B—F4 | 103.4 (10) |
C3c—C2c—H2c1 | 111.6 (15) | F2—B—F3 | 115.8 (10) |
H2c2—C2c—H2c1 | 106.0 (17) | F2—B—F4 | 115.7 (10) |
Br3—C3c—C2c | 107.0 (9) | F3—B—F4 | 114.8 (10) |
Br3—C3c—H3c2 | 114.4 (15) | B—F1—F2 | 37.3 (5) |
Br3—C3c—H3c1 | 108.5 (15) | B—F1—F3 | 38.0 (5) |
C2c—C3c—H3c2 | 110.0 (15) | B—F1—F4 | 37.1 (6) |
C2c—C3c—H3c1 | 107.0 (15) | F2—F1—F3 | 63.9 (5) |
H3c2—C3c—H3c1 | 109.6 (17) | F2—F1—F4 | 63.4 (5) |
N4a—C1a—N1a | 109.3 (8) | F3—F1—F4 | 63.4 (5) |
N4a—C1a—H1a | 124.7 (13) | B—F2—F1 | 40.1 (6) |
N1a—C1a—H1a | 125.9 (13) | B—F3—F1 | 40.4 (6) |
N4b—C1b—N1b | 110.0 (8) | B—F4—F1 | 39.5 (6) |
Symmetry codes: (i) −x, −y, −z; (ii) −x−1, y−1/2, −z+1/2; (iii) −x−1, −y, −z; (iv) −x, −y, −z+1; (v) x, −y+3/2, z+3/2; (vi) x, −y+3/2, z+1/2; (vii) −x−1, y+1/2, −z+1/2. |
(TEEB90RR3TEXT4_publ)
top
Crystal data top
C18H30B2Br6F8FeN24 | V = 2186.60 Å3 |
Mr = 1291.53 | Z = 2 |
Monoclinic, P21/c | Synchrotron radiation, λ = 0.999995 Å |
a = 11.9297 (7) Å | T = 300 K K |
b = 17.8169 (8) Å | white |
c = 10.2874 (3) Å | ?, ? × ? × ? mm |
β = 89.992 (2)° | |
Data collection top
Debye- Scherrer diffractometer | 2θmin = 0.010°, 2θmax = 1.800°, 2θstep = 0.01° |
Refinement top
Least-squares matrix: full | Profile function: CW Profile function number 3 with 19 terms
Pseudovoigt profile coefficients as parameterized in
P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
J. Appl. Cryst.,27,892-900.
#1(GU) = 124.334 #2(GV) = 103.923 #3(GW) = -1.733
#4(GP) = 0.584 #5(LX) = 0.020 #6(LY) = 30.831
#7(S/L) = 0.0006 #8(H/L) = 0.0100
#9(trns) = 0.85 #10(shft)= -0.1308
#11(stec)= -18.15 #12(ptec)= 0.00 #13(sfec)= 0.00
#14(L11) = 0.000 #15(L22) = 0.000 #16(L33) = 0.000
#17(L12) = 0.000 #18(L13) = 0.000 #19(L23) = 0.000
Peak tails are ignored where the intensity is below 0.0010 times the peak
Aniso. broadening axis 0.0 0.0 1.0 |
Rp = 0.051 | 181 parameters |
Rwp = 0.070 | 145 restraints |
Rexp = 0.011 | (Δ/σ)max = 3.95 |
χ2 = 43.824 | Background function: GSAS Background function number 1 with 16 terms.
Shifted Chebyshev function of 1st kind
1: 5952.42 2: -959.633 3: -1488.20 4: 1242.80
5: -333.815 6: -285.293 7: 759.718 8: -650.135
9: 65.4643 10: 456.653 11: -546.059 12: 167.687
13: 375.110 14: -372.413 15: 169.035 16: 43.4613 |
180 data points | Preferred orientation correction: Spherical Harmonic ODF
Spherical harmonic order= 6
The sample symmetry is: cylindrical (fiber texture)
Index = 2 0 -2 Coeff= -0.5709
Index = 2 0 0 Coeff= 0.7813
Index = 2 0 2 Coeff= 0.2983
Index = 4 0 -4 Coeff= 1.8830
Index = 4 0 -2 Coeff= 1.9726
Index = 4 0 0 Coeff= 0.8217
Index = 4 0 2 Coeff= -4.0098
Index = 4 0 4 Coeff= -2.6660
Index = 6 0 -6 Coeff= -3.7631
Index = 6 0 -4 Coeff= -2.2971
Index = 6 0 -2 Coeff= -3.2169
Index = 6 0 0 Coeff= 0.0774
Index = 6 0 2 Coeff= 1.5200
Index = 6 0 4 Coeff= 2.7549
Index = 6 0 6 Coeff= 5.8226
Prefered orientation correction range: Min= -2.17089, Max= 4.29201 |
Crystal data top
C18H30B2Br6F8FeN24 | β = 89.992 (2)° |
Mr = 1291.53 | V = 2186.60 Å3 |
Monoclinic, P21/c | Z = 2 |
a = 11.9297 (7) Å | Synchrotron radiation, λ = 0.999995 Å |
b = 17.8169 (8) Å | T = 300 K K |
c = 10.2874 (3) Å | ?, ? × ? × ? mm |
Data collection top
Debye- Scherrer diffractometer | 2θmin = 0.010°, 2θmax = 1.800°, 2θstep = 0.01° |
Refinement top
Rp = 0.051 | 180 data points |
Rwp = 0.070 | 181 parameters |
Rexp = 0.011 | 145 restraints |
χ2 = 43.824 | (Δ/σ)max = 3.95 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | |
Fe | 0.0 | 0.0 | 0.0 | 0.015* | |
Br1 | 0.4044 (7) | −0.1409 (5) | 0.2893 (7) | 0.1361 (18)* | |
Br2 | −0.3931 (8) | −0.0582 (4) | 0.3470 (6) | 0.1361 (18)* | |
Br3 | −0.4058 (7) | −0.1336 (4) | −0.2772 (7) | 0.1361 (18)* | |
N4a | 0.13142 (14) | −0.07101 (9) | 0.0570 (12) | 0.009 (3)* | |
N3a | 0.1980 (13) | −0.05606 (6) | 0.1529 (14) | 0.009 (3)* | |
N2a | 0.2716 (11) | −0.1087 (7) | 0.1706 (13) | 0.009 (3)* | |
N1a | 0.2659 (8) | −0.1563 (5) | 0.0733 (10) | 0.009 (3)* | |
N4b | −0.0694 (5) | 0.0009 (4) | 0.1738 (9) | 0.009 (3)* | |
N4c | −0.1142 (8) | −0.0845 (5) | −0.0435 (9) | 0.009 (3)* | |
N3b | −0.0391 (9) | −0.0448 (6) | 0.2731 (12) | 0.009 (3)* | |
N3c | −0.1072 (11) | −0.1357 (7) | −0.1335 (12) | 0.009 (3)* | |
N2b | −0.1001 (11) | −0.0290 (7) | 0.3716 (10) | 0.009 (3)* | |
N1b | −0.1722 (8) | 0.0253 (6) | 0.3396 (5) | 0.009 (3)* | |
N2c | −0.1946 (12) | −0.1798 (7) | −0.1375 (13) | 0.009 (3)* | |
N1c | −0.2578 (10) | −0.1556 (6) | −0.0465 (11) | 0.009 (3)* | |
C1a | 0.1793 (9) | −0.1318 (6) | 0.0005 (11) | 0.025* | |
C2a | 0.3410 (10) | −0.2235 (6) | 0.0549 (12) | 0.025* | |
C3a | 0.4024 (15) | −0.2302 (8) | 0.1817 (15) | 0.025* | |
C1b | −0.1524 (5) | 0.0430 (4) | 0.2172 (6) | 0.025* | |
C1c | −0.2132 (10) | −0.0970 (7) | 0.0116 (11) | 0.025* | |
C2b | −0.2536 (10) | 0.0571 (8) | 0.4382 (14) | 0.025* | |
C2c | −0.3664 (12) | −0.1929 (8) | −0.0216 (13) | 0.025* | |
C3b | −0.3755 (11) | 0.0294 (8) | 0.4494 (15) | 0.025* | |
C3c | −0.4410 (14) | −0.1350 (10) | −0.0968 (12) | 0.025* | |
H1a | 0.1485 (4) | −0.1587 (16) | −0.088 (2) | 0.025* | |
H2a2 | 0.291 (3) | −0.2756 (13) | 0.039 (4) | 0.025* | |
H2a1 | 0.397 (3) | −0.217 (2) | −0.027 (3) | 0.025* | |
H3a2 | 0.484 (2) | −0.252 (2) | 0.159 (4) | 0.025* | |
H3a1 | 0.356 (3) | −0.2740 (16) | 0.235 (3) | 0.025* | |
H1b | −0.1954 (15) | 0.0860 (9) | 0.1648 (19) | 0.025* | |
H1c | −0.2508 (19) | −0.0664 (11) | 0.0906 (16) | 0.025* | |
H2b1 | −0.217 (3) | 0.050 (3) | 0.533 (2) | 0.025* | |
H2b2 | −0.261 (3) | 0.1161 (11) | 0.418 (5) | 0.025* | |
H2c2 | −0.369 (3) | −0.2478 (12) | −0.066 (4) | 0.025* | |
H2c1 | −0.386 (3) | −0.193 (2) | 0.080 (2) | 0.025* | |
H3b1 | −0.429 (2) | 0.0726 (15) | 0.425 (4) | 0.025* | |
H3b2 | −0.385 (4) | 0.013 (2) | 0.553 (2) | 0.025* | |
H3c2 | −0.430 (4) | −0.0808 (13) | −0.048 (3) | 0.025* | |
H3c1 | −0.5280 (19) | −0.154 (3) | −0.076 (4) | 0.025* | |
B41 | −0.0038 (13) | 0.3016 (9) | 0.9834 (14) | 0.025* | |
F42 | −0.0163 (19) | 0.2499 (9) | 1.0878 (15) | 0.025* | |
F43 | 0.0206 (18) | 0.2645 (10) | 0.8761 (14) | 0.025* | |
F44 | −0.1003 (14) | 0.3346 (13) | 0.9819 (14) | 0.025* | |
F45 | 0.0788 (15) | 0.3404 (12) | 1.0275 (16) | 0.025* | |
Geometric parameters (Å, º) top
Fe—N4a | 2.098 (4) | C1b—N1b | 1.319 (4) |
Fe—N4ai | 2.098 (4) | C1b—H1b | 1.068 (15) |
Fe—N4b | 1.970 (9) | C1c—N4c | 1.329 (13) |
Fe—N4bi | 1.970 (9) | C1c—N3c | 2.074 (17) |
Fe—N4c | 2.079 (10) | C1c—N2c | 2.140 (17) |
Fe—N4ci | 2.079 (10) | C1c—N1c | 1.316 (13) |
Br1—Br2ii | 2.891 (12) | C1c—H1c | 1.077 (16) |
Br1—N2a | 2.081 (16) | C2b—Br2 | 2.806 (12) |
Br1—N1a | 2.783 (13) | C2b—N1b | 1.515 (13) |
Br1—C3a | 1.939 (13) | C2b—C3b | 1.539 (13) |
Br1—H3a2 | 2.56 (3) | C2b—H2b1 | 1.075 (17) |
Br1—H3a1 | 2.50 (3) | C2b—H2b2 | 1.075 (17) |
Br2—Br1iii | 2.891 (12) | C2c—Br3 | 2.873 (13) |
Br2—C2b | 2.806 (12) | C2c—N1c | 1.478 (14) |
Br2—C3b | 1.895 (12) | C2c—C3c | 1.567 (14) |
Br2—H3b1 | 2.50 (3) | C2c—H2c2 | 1.081 (17) |
Br2—H3b2 | 2.48 (3) | C2c—H2c1 | 1.068 (17) |
Br3—C2c | 2.873 (13) | C3b—Br2 | 1.895 (12) |
Br3—C3c | 1.903 (12) | C3b—C2b | 1.539 (13) |
Br3—H3a2iv | 2.52 (4) | C3b—H2b2 | 2.08 (3) |
Br3—H3b1v | 2.71 (3) | C3b—H3b1 | 1.034 (18) |
Br3—H3c2 | 2.56 (3) | C3b—H3b2 | 1.113 (17) |
Br3—H3c1 | 2.56 (3) | C3c—Br3 | 1.903 (12) |
N4a—Fe | 2.098 (4) | C3c—C2c | 1.567 (14) |
N4a—N3a | 1.295 (13) | C3c—H3c2 | 1.096 (18) |
N4a—N2a | 2.148 (15) | C3c—H3c1 | 1.111 (18) |
N4a—C1a | 1.355 (11) | H1a—C1a | 1.096 (16) |
N3a—N4a | 1.295 (13) | H1a—H1bi | 1.62 (3) |
N3a—N2a | 1.297 (13) | H1a—F42vi | 2.27 (3) |
N3a—N1a | 2.125 (13) | H2a2—C2a | 1.118 (17) |
N3a—C1a | 2.080 (15) | H2a2—H2a1 | 1.78 (3) |
N2a—Br1 | 2.081 (16) | H2a1—C2a | 1.082 (18) |
N2a—N4a | 2.148 (15) | H2a1—H2a2 | 1.78 (3) |
N2a—N3a | 1.297 (13) | H2a1—H3c1ii | 1.52 (5) |
N2a—N1a | 1.314 (13) | H3a2—Br1 | 2.56 (3) |
N2a—C1a | 2.107 (17) | H3a2—Br3vii | 2.52 (4) |
N1a—Br1 | 2.783 (13) | H3a2—C2a | 2.08 (3) |
N1a—N3a | 2.125 (13) | H3a2—C3a | 1.072 (18) |
N1a—N2a | 1.314 (13) | H3a2—H3a1 | 1.76 (3) |
N1a—C1a | 1.348 (12) | H3a1—Br1 | 2.50 (3) |
N1a—C2a | 1.507 (9) | H3a1—C2a | 2.07 (3) |
N4b—Fe | 1.970 (9) | H3a1—C3a | 1.103 (19) |
N4b—N3b | 1.356 (12) | H3a1—H3a2 | 1.76 (3) |
N4b—N2b | 2.135 (12) | H1b—C1ai | 1.90 (2) |
N4b—N1b | 2.145 (10) | H1b—C1b | 1.068 (15) |
N4b—C1b | 1.320 (4) | H1b—H1ai | 1.62 (3) |
N4c—Fe | 2.079 (10) | H1c—C1c | 1.077 (16) |
N4c—N3c | 1.302 (13) | H2b1—C2b | 1.075 (17) |
N4c—N1c | 2.132 (14) | H2b1—H2b2 | 1.75 (3) |
N4c—C1c | 1.329 (13) | H2b2—C2b | 1.075 (17) |
N3b—N4b | 1.356 (12) | H2b2—C3b | 2.08 (3) |
N3b—N2b | 1.278 (13) | H2b2—H2b1 | 1.75 (3) |
N3b—N1b | 2.132 (13) | H2b2—F44viii | 2.21 (4) |
N3b—C1b | 2.145 (11) | H2c2—C2c | 1.081 (17) |
N3c—N4c | 1.302 (13) | H2c2—H2c1 | 1.80 (3) |
N3c—N2c | 1.307 (14) | H2c1—C2c | 1.068 (17) |
N3c—N1c | 2.039 (16) | H2c1—H2c2 | 1.80 (3) |
N3c—C1c | 2.074 (17) | H3b1—Br2 | 2.50 (3) |
N2b—N4b | 2.135 (12) | H3b1—Br3v | 2.71 (3) |
N2b—N3b | 1.278 (13) | H3b1—C3b | 1.034 (18) |
N2b—N1b | 1.336 (13) | H3b1—H3b2 | 1.78 (3) |
N2b—C1b | 2.135 (11) | H3b2—Br2 | 2.48 (3) |
N1b—N4b | 2.145 (10) | H3b2—C3b | 1.113 (17) |
N1b—N3b | 2.132 (13) | H3b2—H3b1 | 1.78 (3) |
N1b—N2b | 1.336 (13) | H3c2—Br3 | 2.56 (3) |
N1b—C1b | 1.319 (4) | H3c2—C3c | 1.096 (18) |
N1b—C2b | 1.515 (13) | H3c2—H3c1 | 1.77 (3) |
N2c—N3c | 1.307 (14) | H3c1—Br3 | 2.56 (3) |
N2c—N1c | 1.277 (14) | H3c1—C3c | 1.111 (18) |
N2c—C1c | 2.140 (17) | H3c1—H2a1iii | 1.52 (5) |
N1c—N4c | 2.132 (14) | H3c1—H3c2 | 1.77 (3) |
N1c—N3c | 2.039 (16) | B41—F42 | 1.423 (14) |
N1c—N2c | 1.277 (14) | B41—F43 | 1.320 (14) |
N1c—C1c | 1.316 (13) | B41—F44 | 1.293 (15) |
N1c—C2c | 1.478 (14) | B41—F45 | 1.286 (15) |
C1a—N4a | 1.355 (11) | F42—H1avi | 2.27 (3) |
C1a—N3a | 2.080 (15) | F42—B41 | 1.423 (14) |
C1a—N2a | 2.107 (17) | F42—F43 | 2.237 (18) |
C1a—N1a | 1.348 (12) | F42—F44 | 2.113 (19) |
C1a—H1a | 1.096 (16) | F42—F45 | 2.067 (19) |
C1a—H1bi | 1.90 (2) | F43—B41 | 1.320 (14) |
C2a—N1a | 1.507 (9) | F43—F42 | 2.237 (18) |
C2a—C3a | 1.501 (14) | F43—F44 | 2.197 (19) |
C2a—H2a2 | 1.118 (17) | F43—F45 | 2.177 (18) |
C2a—H2a1 | 1.082 (18) | F44—H2b2ix | 2.21 (4) |
C2a—H3a2 | 2.08 (3) | F44—B41 | 1.293 (15) |
C2a—H3a1 | 2.07 (3) | F44—F42 | 2.113 (19) |
C3a—Br1 | 1.939 (13) | F44—F43 | 2.197 (19) |
C3a—C2a | 1.501 (14) | F44—F45 | 2.191 (18) |
C3a—H3a2 | 1.072 (18) | F45—B41 | 1.286 (15) |
C3a—H3a1 | 1.103 (19) | F45—F42 | 2.067 (19) |
C1b—N4b | 1.320 (4) | F45—F43 | 2.177 (18) |
C1b—N3b | 2.145 (11) | F45—F44 | 2.191 (18) |
C1b—N2b | 2.135 (11) | | |
| | | |
N4a—Fe—N4ai | 180.0 | C2a—C3a—H3a1 | 104.2 (19) |
N4a—Fe—N4b | 93.8 (4) | H3a2—C3a—H3a1 | 108 (2) |
N4a—Fe—N4bi | 86.2 (4) | N4b—C1b—N1b | 108.7 (7) |
N4a—Fe—N4c | 96.5 (2) | N4b—C1b—H1b | 126.6 (13) |
N4a—Fe—N4ci | 83.5 (2) | N1b—C1b—H1b | 124.6 (13) |
N4ai—Fe—N4b | 86.2 (4) | N4c—C1c—N1c | 107.4 (10) |
N4ai—Fe—N4bi | 93.8 (4) | N4c—C1c—H1c | 127.4 (15) |
N4ai—Fe—N4c | 83.5 (2) | N1c—C1c—H1c | 125.2 (14) |
N4ai—Fe—N4ci | 96.5 (2) | N1b—C2b—C3b | 122.4 (8) |
N4b—Fe—N4bi | 179.9802 | N1b—C2b—H2b1 | 107.3 (18) |
N4b—Fe—N4c | 85.8 (3) | N1b—C2b—H2b2 | 107 (2) |
N4b—Fe—N4ci | 94.2 (3) | C3b—C2b—H2b1 | 106.0 (19) |
N4bi—Fe—N4c | 94.2 (3) | C3b—C2b—H2b2 | 104 (2) |
N4bi—Fe—N4ci | 85.8 (3) | H2b1—C2b—H2b2 | 109 (2) |
N4c—Fe—N4ci | 180.0 | N1c—C2c—C3c | 96.7 (10) |
Br2ii—Br1—N2a | 128.0 (5) | N1c—C2c—H2c2 | 111 (2) |
Br2ii—Br1—C3a | 123.1 (7) | N1c—C2c—H2c1 | 111 (2) |
N2a—Br1—C3a | 83.2 (7) | C3c—C2c—H2c2 | 111.9 (19) |
Br1iii—Br2—C3b | 128.8 (6) | C3c—C2c—H2c1 | 111 (2) |
Fe—N4a—N3a | 123.2 (5) | H2c2—C2c—H2c1 | 114 (2) |
Fe—N4a—C1a | 132.6 (8) | Br2—C3b—C2b | 109.1 (7) |
N3a—N4a—C1a | 103.4 (7) | Br2—C3b—H3b1 | 114.1 (19) |
N4a—N3a—N2a | 111.9 (8) | Br2—C3b—H3b2 | 108.0 (19) |
Br1—N2a—N3a | 142.8 (11) | C2b—C3b—H3b1 | 109.2 (18) |
Br1—N2a—N1a | 108.0 (9) | C2b—C3b—H3b2 | 104 (2) |
N3a—N2a—N1a | 109.0 (11) | H3b1—C3b—H3b2 | 112 (2) |
N2a—N1a—C1a | 104.7 (9) | Br3—C3c—C2c | 111.4 (10) |
N2a—N1a—C2a | 125.3 (9) | Br3—C3c—H3c2 | 114.3 (18) |
C1a—N1a—C2a | 130.0 (8) | Br3—C3c—H3c1 | 113.2 (19) |
Fe—N4b—N3b | 124.5 (6) | C2c—C3c—H3c2 | 106.5 (19) |
Fe—N4b—C1b | 128.8 (6) | C2c—C3c—H3c1 | 104 (2) |
N3b—N4b—C1b | 106.6 (7) | H3c2—C3c—H3c1 | 107 (2) |
Fe—N4c—N3c | 128.2 (7) | C2a—H2a1—H3c1ii | 135 (4) |
Fe—N4c—C1c | 127.7 (8) | C3c—H3c1—H2a1iii | 147 (4) |
N3c—N4c—C1c | 104.0 (9) | F42—B41—F43 | 109.2 (12) |
N4b—N3b—N2b | 108.3 (7) | F42—B41—F44 | 102.1 (13) |
N4c—N3c—N2c | 113.1 (11) | F42—B41—F45 | 99.3 (12) |
N3b—N2b—N1b | 109.3 (7) | F43—B41—F44 | 114.5 (13) |
N2b—N1b—C1b | 107.1 (7) | F43—B41—F45 | 113.3 (13) |
N2b—N1b—C2b | 121.3 (9) | F44—B41—F45 | 116.3 (14) |
C1b—N1b—C2b | 131.6 (10) | B41—F42—F44 | 36.7 (7) |
N3c—N2c—N1c | 104.2 (11) | B41—F42—F45 | 37.9 (7) |
N2c—N1c—C1c | 111.2 (11) | F44—F42—F45 | 63.2 (7) |
N2c—N1c—C2c | 119.6 (11) | B41—F43—F44 | 32.4 (7) |
C1c—N1c—C2c | 129.2 (11) | B41—F43—F45 | 32.8 (7) |
N4a—C1a—N1a | 110.1 (9) | F44—F43—F45 | 60.1 (6) |
N4a—C1a—H1a | 124.4 (13) | B41—F44—F42 | 41.2 (8) |
N1a—C1a—H1a | 125.3 (12) | B41—F44—F43 | 33.1 (7) |
N1a—C2a—C3a | 104.2 (9) | B41—F44—F45 | 31.8 (7) |
N1a—C2a—H2a2 | 111.1 (18) | F42—F44—F43 | 62.5 (7) |
N1a—C2a—H2a1 | 112 (2) | F42—F44—F45 | 57.4 (7) |
C3a—C2a—H2a2 | 109.0 (19) | F43—F44—F45 | 59.5 (7) |
C3a—C2a—H2a1 | 112.7 (18) | B41—F45—F42 | 42.8 (8) |
H2a2—C2a—H2a1 | 108 (2) | B41—F45—F43 | 33.8 (7) |
Br1—C3a—C2a | 115.9 (10) | B41—F45—F44 | 31.9 (8) |
Br1—C3a—H3a2 | 113.6 (19) | F42—F45—F43 | 63.6 (7) |
Br1—C3a—H3a1 | 107.5 (18) | F42—F45—F44 | 59.4 (7) |
C2a—C3a—H3a2 | 107 (2) | F43—F45—F44 | 60.4 (7) |
Symmetry codes: (i) −x, −y, −z; (ii) x+1, y, z; (iii) x−1, y, z; (iv) x−1, −y+1/2, z+1/2; (v) −x−1, −y, −z; (vi) −x, −y, −z+1; (vii) x+1, −y+1/2, z+3/2; (viii) x, −y+3/2, z+1/2; (ix) x, −y+3/2, z+3/2. |
Experimental details
| (feteei) | (TEEI90RRLAST_overall) | (TEEI90RRLAST_phase_1) | (TEEI90RRLAST_p_01) |
Crystal data |
Chemical formula | C18H30FeI6N24·2(BF4) | ? | C18H30B2F8FeI6N24 | ? |
Mr | 1573.50 | ? | 1573.50 | ? |
Crystal system, space group | Monoclinic, P21/c | ?, ? | Monoclinic, P21/c | ?, ? |
Temperature (K) | 293 | ? | ? | ? |
a, b, c (Å) | 12.64250 (19), 18.0349 (3), 10.64881 (15) | ?, ?, ? | 12.3177 (3), 17.6766 (4), 10.4685 (3) | ?, ?, ? |
β (°) | 90, 90.3080 (11), 90 | ?, ?, ? | 90, 90.5991 (17), 90 | ?, ?, ? |
V (Å3) | 2427.96 (6) | ? | 2279.25 | ? |
Z | 2 | ? | 2 | ? |
Radiation type | Synchrotron, λ = 0.75003 Å | ?, λ = 0.999995 Å | ?, λ = 0.999995 Å | ?, λ = 0.999995 Å |
µ (mm−1) | ? | – | – | – |
Specimen shape, size (mm) | × × | ?, ? × ? × ? | ?, ? × ? × ? | ?, ? × ? × ? |
|
Data collection |
Diffractometer | ? | ? | ? | ? |
Specimen mounting | – | ? | ? | ? |
Data collection mode | – | ? | ? | ? |
Data collection method | ? | ? | ? | ? |
Absorption correction | ? | – | – | – |
No. of measured, independent and observed (?) reflections | ?, ?, ? | – | – | – |
Rint | ? | – | – | – |
θ values (°) | θmax = ? | 2θmin = 0.010 2θmax = 1.800 2θstep = 0.01 | 2θmin = 0.010 2θmax = 1.800 2θstep = 0.01 | 2θmin = 0.010 2θmax = 1.800 2θstep = 0.01 |
|
Refinement |
R factors and goodness of fit | R[F2 > 2σ(F2)] = ?, wR(F2) = ?, S = ? | Rp = 0.025, Rwp = 0.037, Rexp = 0.012, R(F2) = 0.09479, χ2 = 10.368 | Rp = 0.025, Rwp = 0.037, Rexp = 0.012, R(F2) = 0.09479, χ2 = 10.368 | Rp = 0.025, Rwp = 0.037, Rexp = 0.012, R(F2) = 0.09479, χ2 = NOT FOUND |
No. of reflections/data points | ? | 180 | 180 | 180 |
No. of parameters | ? | 212 | 212 | ? |
No. of restraints | ? | 139 | 139 | ? |
(Δ/σ)max | ? | 0.73 | 0.73 | ? |
Δρmax, Δρmin (e Å−3) | ?, ? | – | – | – |
| (LAST_publ) | (TEEB90RR3TEXT4_publ) |
Crystal data |
Chemical formula | C18H30B2Br6F8FeN24 | C18H30B2Br6F8FeN24 |
Mr | 1291.53 | 1291.53 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 300 K | 300 K |
a, b, c (Å) | 12.2832 (6), 18.0705 (15), 10.4767 (3) | 11.9297 (7), 17.8169 (8), 10.2874 (3) |
β (°) | 90, 90.106 (3), 90 | 90, 89.992 (2), 90 |
V (Å3) | 2325.45 | 2186.60 |
Z | 2 | 2 |
Radiation type | Synchrotron, λ = 0.999995 Å | Synchrotron, λ = 0.999995 Å |
µ (mm−1) | – | – |
Specimen shape, size (mm) | ?, ? × ? × ? | ?, ? × ? × ? |
|
Data collection |
Diffractometer | Debye Scherrer diffractometer | Debye- Scherrer diffractometer |
Specimen mounting | ? | ? |
Data collection mode | ? | ? |
Data collection method | ? | ? |
Absorption correction | – | – |
No. of measured, independent and observed (?) reflections | – | – |
Rint | – | – |
θ values (°) | 2θmin = 0.010 2θmax = 1.800 2θstep = 0.01 | 2θmin = 0.010 2θmax = 1.800 2θstep = 0.01 |
|
Refinement |
R factors and goodness of fit | Rp = 0.046, Rwp = 0.065, Rexp = 0.011, χ2 = 40.704 | Rp = 0.051, Rwp = 0.070, Rexp = 0.011, χ2 = 43.824 |
No. of reflections/data points | 180 | 180 |
No. of parameters | 184 | 181 |
No. of restraints | 145 | 145 |
(Δ/σ)max | 0.64 | 3.95 |
Δρmax, Δρmin (e Å−3) | – | – |