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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768104015356/na5021sup1.cif
Contains datablocks global, TEEI90RRLAST_publ, LAST_publ, TEEB90RR3TEXT4_publ, feteei, TEEI90RRLAST_phase_1, TEEI90RRLAST_p_01, TEEI90RRLAST_overall

CCDC references: 255081; 255082; 255083; 255084

Computing details top

Program(s) used to refine structure: GSAS for LAST_publ, TEEB90RR3TEXT4_publ. Software used to prepare material for publication: Xtal BONDLA CIFIO for feteei.

Figures top
[Figure 1]
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[Figure 5]
[Figure 6]
[Figure 7]
[Figure 8]
[Figure 9]
[Figure 10]
(feteei) top
Crystal data top
C18H30FeI6N24·2(BF4)β = 90.3080 (11)°
Mr = 1573.50V = 2427.96 (6) Å3
Monoclinic, P21/cZ = 2
Hall symbol: -p 2ybcDx = 2.152 Mg m3
a = 12.64250 (19) ÅSynchrotron radiation, λ = 0.75003 Å
b = 18.0349 (3) ÅT = 293 K
c = 10.64881 (15) Å × × mm
Data collection top
h = ??l = ??
k = ??
Refinement top
Crystal data top
C18H30FeI6N24·2(BF4)β = 90.3080 (11)°
Mr = 1573.50V = 2427.96 (6) Å3
Monoclinic, P21/cZ = 2
a = 12.64250 (19) ÅSynchrotron radiation, λ = 0.75003 Å
b = 18.0349 (3) ÅT = 293 K
c = 10.64881 (15) Å × × mm
Data collection top
Refinement top
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe0.000000.000000.000000.02533*
I10.4112 (5)0.1985 (3)0.0652 (5)0.0871 (13)*
I30.4192 (4)0.1155 (3)0.2359 (5)0.08713*
I20.4120 (5)0.0715 (3)0.3214 (4)0.08713*
N4A0.0964 (14)0.0687 (7)0.1261 (13)0.055 (6)*
N3A0.150 (2)0.0426 (7)0.2308 (12)0.05482*
N2A0.208 (2)0.0935 (9)0.2790 (18)0.05482*
N1A0.188 (2)0.1528 (10)0.2158 (17)0.05482*
N4C0.1014 (16)0.0975 (7)0.0382 (13)0.05482*
N4B0.1031 (16)0.0310 (9)0.1609 (11)0.05482*
N3C0.1517 (18)0.1402 (7)0.0502 (13)0.05482*
N3B0.1491 (18)0.0955 (8)0.1785 (12)0.05482*
N2C0.208 (2)0.1900 (9)0.0006 (16)0.05482*
N1C0.192 (2)0.1827 (9)0.1220 (19)0.05482*
N2B0.212 (2)0.0967 (9)0.2759 (15)0.05482*
N1B0.196 (2)0.0307 (11)0.3261 (14)0.05482*
C1A0.1199 (18)0.1376 (8)0.1200 (15)0.05482*
C2A0.235 (2)0.2259 (13)0.249 (2)0.08 (2)*
C3A0.353 (2)0.2217 (18)0.250 (2)0.07596*
C1C0.126 (2)0.1258 (8)0.1448 (16)0.05482*
C1B0.1308 (19)0.0110 (10)0.2541 (12)0.05482*
C2C0.235 (2)0.2362 (12)0.217 (3)0.12 (2)*
C2B0.244 (2)0.0049 (16)0.4512 (18)0.06 (2)*
C3C0.356 (2)0.2254 (11)0.224 (3)0.11794*
C3B0.3630 (18)0.0088 (16)0.443 (2)0.05796*
H1A0.094 (2)0.1758 (8)0.0479 (18)0.05066*
H21A0.206 (3)0.2688 (10)0.184 (3)0.05066*
H22A0.206 (3)0.2417 (17)0.341 (3)0.05066*
H31A0.385 (3)0.182 (2)0.303 (6)0.05066*
H32A0.382 (3)0.279 (2)0.271 (6)0.05066*
H1C0.103 (2)0.1047 (9)0.2365 (16)0.05066*
H1B0.111 (2)0.0681 (11)0.2694 (13)0.05066*
H21C0.203 (3)0.2258 (12)0.308 (2)0.05066*
H22C0.226 (3)0.2907 (13)0.186 (4)0.05066*
H21B0.217 (3)0.0457 (16)0.4782 (17)0.05066*
H22B0.226 (3)0.050 (2)0.519 (2)0.05066*
H31C0.396 (2)0.232 (3)0.140 (4)0.05066*
H32C0.386 (3)0.260 (3)0.301 (4)0.05066*
H31B0.396 (2)0.054 (3)0.400 (4)0.05066*
H32B0.400 (3)0.010 (3)0.526 (4)0.05066*
B0.0046 (19)0.1569 (13)0.489 (2)0.05066*
F10.1100 (18)0.1703 (17)0.492 (3)0.10132*
F20.022 (3)0.1682 (16)0.368 (2)0.10132*
F30.017 (3)0.0907 (13)0.542 (3)0.10132*
F40.038 (2)0.2053 (15)0.570 (2)0.10132*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
???????
Geometric parameters (Å, º) top
Fe—N4A2.200 (14)N1B—C1B1.35 (3)
Fe—N4C2.215 (16)N1B—C2B1.53 (3)
Fe—N4B2.219 (15)C1A—H1A1.08 (2)
Fe—N4A2.200 (14)C2A—C3A1.50 (4)
Fe—N4C2.215 (16)C2A—H21A1.10 (4)
Fe—N4B2.219 (15)C2A—H22A1.08 (4)
I1—C3A2.14 (2)C3A—H31A1.00 (6)
I3—C3C2.14 (2)C3A—H32A1.12 (5)
I2—C3B2.04 (3)C1C—H1C1.09 (2)
N4A—N3A1.39 (2)C1B—H1B1.07 (3)
N4A—C1A1.279 (19)C2C—C3C1.54 (4)
N3A—N2A1.28 (3)C2C—H21C1.06 (4)
N2A—N1A1.29 (2)C2C—H22C1.04 (3)
N1A—C1A1.37 (3)C2B—C3B1.51 (4)
N1A—C2A1.49 (3)C2B—H21B1.02 (4)
N4C—N3C1.37 (2)C2B—H22B1.11 (4)
N4C—C1C1.29 (2)C3C—H31C1.03 (5)
N4B—N3B1.31 (2)C3C—H32C1.10 (6)
N4B—C1B1.30 (2)C3B—H31B1.03 (6)
N3C—N2C1.27 (3)C3B—H32B1.05 (5)
N3B—N2B1.31 (3)B—F11.35 (3)
N2C—N1C1.32 (3)B—F21.35 (3)
N1C—C1C1.34 (3)B—F31.35 (3)
N1C—C2C1.50 (3)B—F41.34 (4)
N2B—N1B1.32 (3)
N4A—Fe—N4C90.7 (5)C3A—C2A—H21A112 (3)
N4A—Fe—N4B90.2 (6)C3A—C2A—H22A110 (3)
N4A—Fe—N4A180.0000H21A—C2A—H22A106 (3)
N4A—Fe—N4C89.3 (5)I1—C3A—C2A109.9 (16)
N4A—Fe—N4B89.8 (6)I1—C3A—H31A104 (4)
N4C—Fe—N4B90.2 (6)I1—C3A—H32A105 (4)
N4C—Fe—N4A89.3 (5)C2A—C3A—H31A117 (3)
N4C—Fe—N4C180.0000C2A—C3A—H32A106 (3)
N4C—Fe—N4B89.8 (6)H31A—C3A—H32A115 (4)
N4B—Fe—N4A89.8 (6)N4C—C1C—N1C107.3 (16)
N4B—Fe—N4C89.8 (6)N4C—C1C—H1C126 (2)
N4B—Fe—N4B180.0000N1C—C1C—H1C127 (2)
N4A—Fe—N4C90.7 (5)N4B—C1B—N1B105.7 (17)
N4A—Fe—N4B90.2 (6)N4B—C1B—H1B128 (2)
N4C—Fe—N4B90.2 (6)N1B—C1B—H1B126 (2)
Fe—N4A—N3A125.0 (9)N1C—C2C—C3C108 (2)
Fe—N4A—C1A130.2 (12)N1C—C2C—H21C111 (3)
N3A—N4A—C1A104.8 (14)N1C—C2C—H22C110 (3)
N4A—N3A—N2A111.2 (13)C3C—C2C—H21C108 (3)
N3A—N2A—N1A106 (2)C3C—C2C—H22C104 (3)
N2A—N1A—C1A110.5 (18)H21C—C2C—H22C114 (3)
N2A—N1A—C2A122 (2)N1B—C2B—C3B109 (2)
C1A—N1A—C2A127.5 (18)N1B—C2B—H21B113 (3)
Fe—N4C—N3C125.9 (11)N1B—C2B—H22B105 (3)
Fe—N4C—C1C128.5 (12)C3B—C2B—H21B113 (3)
N3C—N4C—C1C105.6 (15)C3B—C2B—H22B102 (3)
Fe—N4B—N3B126.3 (11)H21B—C2B—H22B114 (3)
Fe—N4B—C1B126.8 (13)I3—C3C—C2C119.5 (15)
N3B—N4B—C1B106.9 (15)I3—C3C—H31C89 (3)
N4C—N3C—N2C111.5 (14)I3—C3C—H32C110 (3)
N4B—N3B—N2B113.3 (14)C2C—C3C—H31C115 (3)
N3C—N2C—N1C105.1 (18)C2C—C3C—H32C108 (3)
N2C—N1C—C1C110.5 (18)H31C—C3C—H32C114 (4)
N2C—N1C—C2C123 (2)I2—C3B—C2B108.0 (17)
C1C—N1C—C2C126 (2)I2—C3B—H31B99 (3)
N3B—N2B—N1B102.2 (18)I2—C3B—H32B99 (3)
N2B—N1B—C1B111.5 (17)C2B—C3B—H31B118 (3)
N2B—N1B—C2B124 (2)C2B—C3B—H32B112 (3)
C1B—N1B—C2B124.2 (19)H31B—C3B—H32B117 (4)
N4A—C1A—N1A107.7 (15)F1—B—F2104 (2)
N4A—C1A—H1A126 (2)F1—B—F3111 (2)
N1A—C1A—H1A126.7 (18)F1—B—F4105 (2)
N1A—C2A—C3A111 (2)F2—B—F3119 (2)
N1A—C2A—H21A110 (3)F2—B—F4115 (2)
N1A—C2A—H22A109 (3)F3—B—F4103 (2)
(TEEI90RRLAST_overall) top
Crystal data top
?β = ?°
Mr = ?γ = ?°
?, ?V = ? Å3
a = ? ÅZ = ?
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: full180 data points
Rp = 0.025Profile 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 = 0.037212 parameters
Rexp = 0.012139 restraints
R(F2) = 0.09479(Δ/σ)max = 0.73
χ2 = 10.368Background 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 = ? ÅZ = ?
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 = 0.025180 data points
Rwp = 0.037212 parameters
Rexp = 0.012139 restraints
R(F2) = 0.09479(Δ/σ)max = 0.73
χ2 = 10.368
(TEEI90RRLAST_phase_1) top
Crystal data top
C18H30B2F8FeI6N24β = 90.5991 (17)°
Mr = 1573.50V = 2279.25 Å3
Monoclinic, P21/cZ = 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: fullProfile 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 = 0.025212 parameters
Rwp = 0.037139 restraints
Rexp = 0.012(Δ/σ)max = 0.73
R(F2) = 0.09479Background 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 = 10.368Preferred 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
C18H30B2F8FeI6N24β = 90.5991 (17)°
Mr = 1573.50V = 2279.25 Å3
Monoclinic, P21/cZ = 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 = 0.025180 data points
Rwp = 0.037212 parameters
Rexp = 0.012139 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
xyzUiso*/Ueq
Fe0.00.00.00.020 (5)*
I10.4190 (4)0.1953 (2)0.0763 (5)0.0365 (6)*
I20.4107 (4)0.0756 (2)0.3263 (4)0.0365 (6)*
I30.4210 (3)0.1132 (2)0.2382 (4)0.0365 (6)*
N4A0.0973 (14)0.0633 (12)0.1157 (16)0.025*
N3A0.1658 (18)0.0417 (14)0.200 (2)0.025*
N2A0.2198 (17)0.0936 (14)0.253 (2)0.025*
N1A0.1842 (14)0.1519 (13)0.1987 (18)0.025*
N4B0.0941 (14)0.0279 (10)0.1459 (17)0.025*
N4C0.0897 (14)0.0834 (10)0.0309 (15)0.025*
N3B0.1492 (18)0.0894 (15)0.141 (3)0.025*
N3C0.1433 (16)0.1211 (11)0.047 (2)0.025*
N2B0.2128 (19)0.0997 (16)0.245 (3)0.025*
N1B0.1889 (16)0.0375 (14)0.307 (2)0.025*
N2C0.1975 (15)0.1701 (11)0.006 (2)0.025*
N1C0.1811 (14)0.1647 (11)0.123 (2)0.025*
C1A0.1105 (15)0.1320 (13)0.1104 (17)0.025*
C2A0.222 (2)0.2271 (17)0.225 (3)0.025*
C3A0.328 (3)0.222 (2)0.248 (3)0.025*
C1B0.1171 (17)0.0071 (13)0.247 (2)0.025*
C1C0.1142 (14)0.1103 (10)0.1357 (17)0.025*
C2B0.2369 (17)0.0177 (15)0.423 (3)0.025*
C2C0.2233 (17)0.2047 (14)0.232 (3)0.025*
C3B0.356 (2)0.0334 (15)0.389 (3)0.025*
C3C0.3389 (19)0.2026 (15)0.188 (3)0.025*
H1A0.063 (3)0.167 (3)0.043 (4)0.025*
H2A20.176 (6)0.249 (5)0.311 (6)0.025*
H2A10.215 (6)0.263 (4)0.146 (6)0.025*
H3A20.349 (6)0.271 (4)0.293 (7)0.025*
H3A10.342 (7)0.172 (4)0.314 (7)0.025*
H1B0.085 (3)0.061 (3)0.275 (5)0.025*
H1C0.084 (3)0.088 (3)0.224 (5)0.025*
H2B20.215 (6)0.054 (4)0.495 (6)0.025*
H2B10.232 (6)0.038 (3)0.445 (7)0.025*
H2C20.198 (6)0.260 (3)0.226 (7)0.025*
H2C10.221 (6)0.177 (4)0.318 (5)0.025*
H3B20.395 (6)0.046 (4)0.478 (6)0.025*
H3B10.362 (6)0.075 (4)0.318 (7)0.025*
H3C20.370 (6)0.253 (4)0.242 (8)0.025*
H3C10.339 (6)0.219 (5)0.090 (5)0.025*
B0.0071 (18)0.1617 (13)0.502 (2)0.025*
F10.045 (2)0.2189 (12)0.577 (3)0.025*
F20.0946 (18)0.1830 (14)0.494 (2)0.025*
F30.0704 (18)0.1593 (13)0.400 (2)0.025*
F40.020 (2)0.1028 (12)0.572 (2)0.025*
Geometric parameters (Å, º) top
Fe—N4A2.05 (2)N1C—C2C1.44 (3)
Fe—N4B1.97 (2)C1A—H1A1.11 (5)
Fe—N4C1.873 (19)C2A—C3A1.33 (3)
I1—C3A2.16 (3)C2A—H2A21.12 (5)
I2—C3B2.14 (3)C2A—H2A11.05 (5)
I3—C3C1.95 (3)C3A—H3A21.02 (5)
N4A—N3A1.29 (3)C3A—H3A11.13 (5)
N4A—C1A1.23 (2)C1B—H1B1.07 (4)
N3A—N2A1.26 (2)C1C—H1C1.06 (5)
N2A—N1A1.26 (2)C2B—C3B1.54 (2)
N1A—C1A1.350 (17)C2B—H2B21.02 (5)
N1A—C2A1.44 (3)C2B—H2B11.01 (5)
N4B—N3B1.28 (3)C2C—C3C1.49 (2)
N4B—C1B1.26 (2)C2C—H2C21.03 (5)
N3B—N2B1.35 (3)C2C—H2C11.03 (5)
N2B—N1B1.31 (3)C3B—H3B21.07 (5)
N1B—C1B1.33 (3)C3B—H3B11.04 (5)
N1B—C2B1.39 (3)C3C—H3C21.12 (5)
N4C—N3C1.24 (3)C3C—H3C11.06 (5)
N4C—C1C1.236 (14)B—F11.36 (2)
N3C—N2C1.229 (15)B—F21.31 (2)
N2C—N1C1.24 (2)B—F31.33 (2)
N1C—C1C1.27 (2)B—F41.29 (2)
N4A—Fe—N4Ai180.0I1—C3A—C2A111 (2)
N4A—Fe—N4B88.7 (5)I1—C3A—H3A2116 (4)
N4A—Fe—N4Bi91.3 (5)I1—C3A—H3A1104 (4)
N4A—Fe—N4C88.7 (7)C2A—C3A—H3A2106 (4)
N4A—Fe—N4Ci91.3 (7)C2A—C3A—H3A1109 (4)
N4Ai—Fe—N4B91.3 (5)H3A2—C3A—H3A1110 (4)
N4Ai—Fe—N4Bi88.7 (5)N4B—C1B—N1B104 (2)
N4Ai—Fe—N4C91.3 (7)N4B—C1B—H1B126 (3)
N4Ai—Fe—N4Ci88.7 (7)N1B—C1B—H1B130 (3)
N4B—Fe—N4Bi180.0N4C—C1C—N1C111.4 (17)
N4B—Fe—N4C89.3 (6)N4C—C1C—H1C123 (3)
N4B—Fe—N4Ci90.7 (6)N1C—C1C—H1C126 (3)
N4Bi—Fe—N4C90.7 (6)N1B—C2B—C3B98.7 (17)
N4Bi—Fe—N4Ci89.3 (6)N1B—C2B—H2B2112 (4)
N4C—Fe—N4Ci180.0N1B—C2B—H2B1115 (4)
N3A—N4A—C1A103.8 (19)C3B—C2B—H2B2108 (4)
N4A—N3A—N2A116 (2)C3B—C2B—H2B1107 (4)
N3A—N2A—N1A102 (2)H2B2—C2B—H2B1115 (4)
N2A—N1A—C1A110 (2)N1C—C2C—C3C95.7 (17)
N2A—N1A—C2A124 (2)N1C—C2C—H2C2108 (4)
C1A—N1A—C2A127 (2)N1C—C2C—H2C1117 (4)
N3B—N4B—C1B110 (2)C3C—C2C—H2C2107 (4)
N3C—N4C—C1C103.9 (17)C3C—C2C—H2C1106 (4)
N4B—N3B—N2B113 (2)H2C2—C2C—H2C1120 (4)
N4C—N3C—N2C112 (2)I2—C3B—C2B102.1 (14)
N3B—N2B—N1B99 (2)I2—C3B—H3B2108 (4)
N2B—N1B—C1B115 (2)I2—C3B—H3B1113 (4)
N2B—N1B—C2B123 (2)C2B—C3B—H3B2105 (4)
C1B—N1B—C2B122 (2)C2B—C3B—H3B1111 (4)
N3C—N2C—N1C108 (2)H3B2—C3B—H3B1117 (4)
N2C—N1C—C1C104.9 (19)I3—C3C—C2C115.7 (16)
N2C—N1C—C2C133 (2)I3—C3C—H3C2109 (4)
C1C—N1C—C2C122.1 (19)I3—C3C—H3C1119 (4)
N4A—C1A—N1A108.5 (19)C2C—C3C—H3C299 (4)
N4A—C1A—H1A121 (3)C2C—C3C—H3C1106 (4)
N1A—C1A—H1A130 (3)H3C2—C3C—H3C1105 (4)
N1A—C2A—C3A107 (2)F1—B—F298 (2)
N1A—C2A—H2A2108 (4)F1—B—F3107 (2)
N1A—C2A—H2A1113 (4)F1—B—F4103 (2)
C3A—C2A—H2A2112 (4)F2—B—F3121.7 (18)
C3A—C2A—H2A1106 (4)F2—B—F4113 (2)
H2A2—C2A—H2A1112 (4)F3—B—F4111 (2)
Symmetry code: (i) x, y, z.
(TEEI90RRLAST_p_01) top
Crystal data top
?β = ?°
Mr = ?γ = ?°
?, ?V = ? Å3
a = ? ÅZ = ?
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 = 0.025180 data points
Rwp = 0.037Profile 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) = 0.09479Background 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 = ? ÅZ = ?
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 = 0.025R(F2) = 0.09479
Rwp = 0.037χ2 = NOT FOUND
Rexp = 0.012180 data points
(LAST_publ) top
Crystal data top
C18H30B2Br6F8FeN24V = 2325.45 Å3
Mr = 1291.53Z = 2
Monoclinic, P21/cSynchrotron radiation, λ = 0.999995 Å
a = 12.2832 (6) ÅT = 300 K K
b = 18.0705 (15) Åwhite
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: fullProfile 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 = 0.046184 parameters
Rwp = 0.065145 restraints
Rexp = 0.011(Δ/σ)max = 0.64
χ2 = 40.704Background 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 pointsPreferred 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
C18H30B2Br6F8FeN24β = 90.106 (3)°
Mr = 1291.53V = 2325.45 Å3
Monoclinic, P21/cZ = 2
a = 12.2832 (6) ÅSynchrotron radiation, λ = 0.999995 Å
b = 18.0705 (15) ÅT = 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 = 0.046180 data points
Rwp = 0.065184 parameters
Rexp = 0.011145 restraints
χ2 = 40.704(Δ/σ)max = 0.64
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe0.00.00.00.034 (4)*
Br30.4035 (7)0.1466 (5)0.3202 (8)0.158 (2)*
Br10.3890 (7)0.1402 (5)0.3135 (8)0.158 (2)*
Br20.4123 (7)0.0580 (5)0.3075 (7)0.158 (2)*
N4c0.1078 (6)0.0882 (3)0.0757 (9)0.093 (7)*
N3c0.0918 (12)0.1291 (8)0.1834 (13)0.093 (7)*
N2c0.1744 (12)0.1722 (8)0.2011 (14)0.093 (7)*
N1c0.2452 (9)0.1624 (7)0.1118 (12)0.093 (7)*
N4a0.1144 (5)0.0828 (4)0.0810 (9)0.093 (7)*
N4b0.0960 (6)0.0056 (6)0.1802 (4)0.093 (7)*
N3a0.1666 (12)0.0759 (8)0.1972 (13)0.093 (7)*
N3b0.0782 (12)0.0339 (8)0.2868 (11)0.093 (7)*
N2a0.2312 (12)0.1302 (9)0.2224 (14)0.093 (7)*
N1a0.2324 (10)0.1715 (7)0.1190 (12)0.093 (7)*
N2b0.1459 (12)0.0182 (9)0.3804 (12)0.093 (7)*
N1b0.2095 (9)0.0318 (7)0.3387 (11)0.093 (7)*
C1c0.2043 (9)0.1088 (7)0.0370 (12)0.065 (9)*
C2c0.3513 (10)0.2043 (7)0.0957 (13)0.065 (9)*
C3c0.4407 (11)0.1611 (9)0.1552 (15)0.065 (9)*
C1a0.1649 (10)0.1427 (7)0.0312 (11)0.065 (9)*
C1b0.1816 (9)0.0475 (7)0.2162 (11)0.065 (9)*
C2a0.3032 (10)0.2383 (7)0.1174 (13)0.065 (9)*
C2b0.2954 (10)0.0596 (7)0.4221 (12)0.065 (9)*
C3a0.3640 (12)0.2426 (9)0.2480 (14)0.065 (9)*
C3b0.3998 (12)0.0451 (9)0.3419 (15)0.065 (9)*
H1c0.2429 (19)0.0866 (13)0.0491 (17)0.025*
H2c20.368 (2)0.214 (2)0.0082 (18)0.025*
H2c10.344 (2)0.2589 (11)0.138 (3)0.025*
H3c20.5163 (16)0.1889 (18)0.142 (3)0.025*
H3c10.443 (3)0.1071 (12)0.107 (3)0.025*
H1a0.1488 (19)0.1653 (13)0.0617 (17)0.025*
H1b0.2225 (18)0.0883 (11)0.158 (2)0.025*
H2a10.254 (2)0.2869 (11)0.104 (3)0.025*
H2a20.3642 (19)0.2337 (19)0.044 (2)0.025*
H2b20.286 (3)0.1181 (10)0.438 (3)0.025*
H2b10.296 (2)0.0294 (16)0.5100 (19)0.025*
H3a10.4349 (18)0.2735 (15)0.238 (3)0.025*
H3a20.307 (2)0.2703 (16)0.316 (2)0.025*
H3b20.4679 (18)0.0689 (16)0.394 (3)0.025*
H3b10.390 (3)0.0783 (15)0.254 (2)0.025*
B0.0269 (9)0.1867 (7)0.4989 (12)0.01 (3)*
F10.0254 (18)0.2593 (7)0.540 (2)0.226 (13)*
F20.0716 (15)0.1525 (10)0.5947 (14)0.226 (13)*
F30.0769 (9)0.1737 (12)0.481 (2)0.226 (13)*
F40.0852 (14)0.1893 (14)0.3943 (13)0.226 (13)*
Geometric parameters (Å, º) top
Fe—N4c2.219 (3)C1a—H1a1.075 (14)
Fe—N4ci2.219 (3)C1b—N4b1.349 (9)
Fe—N4a2.223 (3)C1b—N3b2.080 (15)
Fe—N4ai2.223 (3)C1b—N2b2.136 (15)
Fe—N4b2.227 (3)C1b—N1b1.357 (12)
Fe—N4bi2.227 (3)C1b—H1b1.081 (15)
Br3—C2c2.653 (14)C2a—Br12.913 (15)
Br3—C3c1.806 (16)C2a—N1a1.487 (12)
Br3—H3c22.45 (3)C2a—C3a1.562 (13)
Br3—H3c12.40 (3)C2a—H2a11.074 (15)
Br3—H3a1ii2.53 (2)C2a—H2a21.080 (15)
Br3—H3b2iii2.25 (3)C2b—Br22.834 (15)
Br1—Br2iii2.857 (12)C2b—N1b1.459 (12)
Br1—N2a2.170 (16)C2b—C3b1.556 (13)
Br1—N1a2.862 (15)C2b—H2b21.077 (15)
Br1—C2a2.913 (15)C2b—H2b11.070 (15)
Br1—C3a1.998 (16)C3a—Br11.998 (16)
Br1—H3a12.60 (3)C3a—C2a1.562 (13)
Br1—H3a22.56 (3)C3a—H3a11.040 (16)
Br2—Br1iii2.857 (12)C3a—H3a21.112 (17)
Br2—C2b2.834 (15)C3b—Br21.904 (17)
Br2—C3b1.904 (17)C3b—C2b1.556 (13)
Br2—H3b22.56 (3)C3b—H3b21.088 (16)
Br2—H3b12.54 (3)C3b—H3b11.109 (16)
N4c—Fe2.219 (3)H1c—C1c1.094 (15)
N4c—N3c1.363 (12)H2c2—C2c1.118 (15)
N4c—C1c1.306 (11)H2c2—H2c11.76 (3)
N3c—N4c1.363 (12)H2c1—C2c1.085 (15)
N3c—N2c1.292 (13)H2c1—H2c21.76 (3)
N3c—N1c2.115 (16)H3c2—Br32.45 (3)
N3c—C1c2.094 (16)H3c2—C3c1.065 (16)
N3c—F2iv2.376 (19)H3c2—H3c11.77 (3)
N2c—N3c1.292 (13)H3c2—H3a1ii1.55 (4)
N2c—N1c1.289 (13)H3c1—Br32.40 (3)
N2c—C1c2.097 (16)H3c1—C2c2.09 (2)
N1c—N3c2.115 (16)H3c1—C3c1.099 (16)
N1c—N2c1.289 (13)H3c1—H3c21.77 (3)
N1c—C1c1.343 (12)H1a—C1a1.075 (14)
N1c—C2c1.516 (12)H1a—H1b1.94 (3)
N4a—Fe2.223 (3)H1b—C1b1.081 (15)
N4a—N3a1.383 (12)H1b—H1a1.94 (3)
N4a—C1a1.351 (11)H2a1—C2a1.074 (15)
N4b—Fe2.227 (3)H2a1—H2a21.78 (2)
N4b—N3b1.343 (9)H2a1—H2b2v1.82 (3)
N4b—C1b1.349 (9)H2a2—C2a1.080 (15)
N3a—N4a1.383 (12)H2a2—H2a11.78 (2)
N3a—N2a1.289 (14)H2b2—C2b1.077 (15)
N3a—N1a2.076 (16)H2b2—H2a1vi1.82 (3)
N3a—C1a2.117 (16)H2b2—H2b11.77 (2)
N3b—N4b1.343 (9)H2b1—C2b1.070 (15)
N3b—N2b1.316 (13)H2b1—H2b21.77 (2)
N3b—N1b2.075 (15)H3a1—Br3vii2.53 (2)
N3b—C1b2.080 (15)H3a1—Br12.60 (3)
N2a—Br12.170 (16)H3a1—C3a1.040 (16)
N2a—N3a1.289 (14)H3a1—H3c2vii1.55 (4)
N2a—N1a1.317 (13)H3a1—H3a21.77 (2)
N2a—C1a2.175 (16)H3a2—Br12.56 (3)
N1a—Br12.862 (15)H3a2—C3a1.112 (17)
N1a—N3a2.076 (16)H3a2—H3a11.77 (2)
N1a—N2a1.317 (13)H3b2—Br3iii2.25 (3)
N1a—C1a1.344 (12)H3b2—Br22.56 (3)
N1a—C2a1.487 (12)H3b2—C3b1.088 (16)
N2b—N3b1.316 (13)H3b2—H3b11.77 (3)
N2b—N1b1.273 (13)H3b1—Br22.54 (3)
N2b—C1b2.136 (15)H3b1—C3b1.109 (16)
N1b—N3b2.075 (15)H3b1—H3b21.77 (3)
N1b—N2b1.273 (13)B—F11.381 (12)
N1b—C1b1.357 (12)B—F21.299 (12)
N1b—C2b1.459 (12)B—F31.310 (11)
C1c—N4c1.306 (11)B—F41.311 (11)
C1c—N3c2.094 (16)F1—B1.381 (12)
C1c—N2c2.097 (16)F1—F22.093 (13)
C1c—N1c1.343 (12)F1—F32.085 (14)
C1c—H1c1.094 (15)F1—F42.113 (14)
C2c—Br32.653 (14)F2—N3civ2.376 (19)
C2c—N1c1.516 (12)F2—B1.299 (12)
C2c—C3c1.486 (13)F2—F12.093 (13)
C2c—H2c21.118 (15)F2—F32.210 (13)
C2c—H2c11.085 (15)F2—F42.209 (13)
C2c—H3c12.09 (2)F3—B1.310 (11)
C3c—Br31.806 (16)F3—F12.085 (14)
C3c—C2c1.486 (13)F3—F22.210 (13)
C3c—H3c21.065 (16)F3—F42.208 (13)
C3c—H3c11.099 (16)F4—B1.311 (11)
C1a—N4a1.351 (11)F4—F12.113 (14)
C1a—N3a2.117 (16)F4—F22.209 (13)
C1a—N2a2.175 (16)F4—F32.208 (13)
C1a—N1a1.344 (12)
C3c—Br3—H3b2iii104.0 (9)N4b—C1b—H1b126.1 (13)
Br2iii—Br1—N2a135.3 (6)N1b—C1b—H1b123.9 (12)
Br2iii—Br1—C3a127.3 (6)N1a—C2a—C3a108.2 (9)
N2a—Br1—C3a77.7 (6)N1a—C2a—H2a1109.6 (14)
Br1iii—Br2—C3b125.0 (6)N1a—C2a—H2a2110.5 (15)
N3c—N4c—C1c103.4 (8)C3a—C2a—H2a1110.0 (15)
N4c—N3c—N2c109.5 (10)C3a—C2a—H2a2107.4 (14)
N3c—N2c—N1c110.0 (11)H2a1—C2a—H2a2111.0 (17)
N2c—N1c—C1c105.6 (9)N1b—C2b—C3b102.3 (9)
N2c—N1c—C2c126.2 (10)N1b—C2b—H2b2110.8 (15)
C1c—N1c—C2c128.1 (10)N1b—C2b—H2b1109.9 (15)
N3a—N4a—C1a101.5 (8)C3b—C2b—H2b2109.9 (15)
N3b—N4b—C1b101.2 (7)C3b—C2b—H2b1112.2 (15)
N4a—N3a—N2a113.5 (10)H2b2—C2b—H2b1111.4 (16)
N4b—N3b—N2b113.7 (10)Br1—C3a—C2a109.2 (9)
Br1—N2a—N3a134.8 (12)Br1—C3a—H3a1113.8 (14)
Br1—N2a—N1a107.8 (10)Br1—C3a—H3a2107.2 (15)
N3a—N2a—N1a105.6 (10)C2a—C3a—H3a1109.8 (15)
N2a—N1a—C1a109.7 (9)C2a—C3a—H3a2106.2 (15)
N2a—N1a—C2a118.4 (10)H3a1—C3a—H3a2110.4 (17)
C1a—N1a—C2a132.0 (10)Br2—C3b—C2b109.5 (9)
N3b—N2b—N1b106.5 (10)Br2—C3b—H3b2114.8 (15)
N2b—N1b—C1b108.6 (9)Br2—C3b—H3b1112.5 (14)
N2b—N1b—C2b118.9 (10)C2b—C3b—H3b2107.1 (15)
C1b—N1b—C2b132.5 (10)C2b—C3b—H3b1105.4 (16)
N4c—C1c—N1c111.4 (8)H3b2—C3b—H3b1106.9 (17)
N4c—C1c—H1c122.9 (13)C3c—H3c2—H3a1ii116 (2)
N1c—C1c—H1c125.6 (13)C3a—H3a1—H3c2vii119 (2)
N1c—C2c—C3c109.0 (9)Br3iii—H3b2—C3b128 (2)
N1c—C2c—H2c2109.6 (15)F1—B—F2102.6 (10)
N1c—C2c—H2c1109.8 (15)F1—B—F3101.6 (10)
C3c—C2c—H2c2110.8 (15)F1—B—F4103.4 (10)
C3c—C2c—H2c1111.6 (15)F2—B—F3115.8 (10)
H2c2—C2c—H2c1106.0 (17)F2—B—F4115.7 (10)
Br3—C3c—C2c107.0 (9)F3—B—F4114.8 (10)
Br3—C3c—H3c2114.4 (15)B—F1—F237.3 (5)
Br3—C3c—H3c1108.5 (15)B—F1—F338.0 (5)
C2c—C3c—H3c2110.0 (15)B—F1—F437.1 (6)
C2c—C3c—H3c1107.0 (15)F2—F1—F363.9 (5)
H3c2—C3c—H3c1109.6 (17)F2—F1—F463.4 (5)
N4a—C1a—N1a109.3 (8)F3—F1—F463.4 (5)
N4a—C1a—H1a124.7 (13)B—F2—F140.1 (6)
N1a—C1a—H1a125.9 (13)B—F3—F140.4 (6)
N4b—C1b—N1b110.0 (8)B—F4—F139.5 (6)
Symmetry codes: (i) x, y, z; (ii) x1, y1/2, z+1/2; (iii) x1, y, z; (iv) x, y, z+1; (v) x, y+3/2, z+3/2; (vi) x, y+3/2, z+1/2; (vii) x1, y+1/2, z+1/2.
(TEEB90RR3TEXT4_publ) top
Crystal data top
C18H30B2Br6F8FeN24V = 2186.60 Å3
Mr = 1291.53Z = 2
Monoclinic, P21/cSynchrotron radiation, λ = 0.999995 Å
a = 11.9297 (7) ÅT = 300 K K
b = 17.8169 (8) Åwhite
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: fullProfile 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 = 0.051181 parameters
Rwp = 0.070145 restraints
Rexp = 0.011(Δ/σ)max = 3.95
χ2 = 43.824Background 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 pointsPreferred 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
C18H30B2Br6F8FeN24β = 89.992 (2)°
Mr = 1291.53V = 2186.60 Å3
Monoclinic, P21/cZ = 2
a = 11.9297 (7) ÅSynchrotron radiation, λ = 0.999995 Å
b = 17.8169 (8) ÅT = 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 = 0.051180 data points
Rwp = 0.070181 parameters
Rexp = 0.011145 restraints
χ2 = 43.824(Δ/σ)max = 3.95
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Fe0.00.00.00.015*
Br10.4044 (7)0.1409 (5)0.2893 (7)0.1361 (18)*
Br20.3931 (8)0.0582 (4)0.3470 (6)0.1361 (18)*
Br30.4058 (7)0.1336 (4)0.2772 (7)0.1361 (18)*
N4a0.13142 (14)0.07101 (9)0.0570 (12)0.009 (3)*
N3a0.1980 (13)0.05606 (6)0.1529 (14)0.009 (3)*
N2a0.2716 (11)0.1087 (7)0.1706 (13)0.009 (3)*
N1a0.2659 (8)0.1563 (5)0.0733 (10)0.009 (3)*
N4b0.0694 (5)0.0009 (4)0.1738 (9)0.009 (3)*
N4c0.1142 (8)0.0845 (5)0.0435 (9)0.009 (3)*
N3b0.0391 (9)0.0448 (6)0.2731 (12)0.009 (3)*
N3c0.1072 (11)0.1357 (7)0.1335 (12)0.009 (3)*
N2b0.1001 (11)0.0290 (7)0.3716 (10)0.009 (3)*
N1b0.1722 (8)0.0253 (6)0.3396 (5)0.009 (3)*
N2c0.1946 (12)0.1798 (7)0.1375 (13)0.009 (3)*
N1c0.2578 (10)0.1556 (6)0.0465 (11)0.009 (3)*
C1a0.1793 (9)0.1318 (6)0.0005 (11)0.025*
C2a0.3410 (10)0.2235 (6)0.0549 (12)0.025*
C3a0.4024 (15)0.2302 (8)0.1817 (15)0.025*
C1b0.1524 (5)0.0430 (4)0.2172 (6)0.025*
C1c0.2132 (10)0.0970 (7)0.0116 (11)0.025*
C2b0.2536 (10)0.0571 (8)0.4382 (14)0.025*
C2c0.3664 (12)0.1929 (8)0.0216 (13)0.025*
C3b0.3755 (11)0.0294 (8)0.4494 (15)0.025*
C3c0.4410 (14)0.1350 (10)0.0968 (12)0.025*
H1a0.1485 (4)0.1587 (16)0.088 (2)0.025*
H2a20.291 (3)0.2756 (13)0.039 (4)0.025*
H2a10.397 (3)0.217 (2)0.027 (3)0.025*
H3a20.484 (2)0.252 (2)0.159 (4)0.025*
H3a10.356 (3)0.2740 (16)0.235 (3)0.025*
H1b0.1954 (15)0.0860 (9)0.1648 (19)0.025*
H1c0.2508 (19)0.0664 (11)0.0906 (16)0.025*
H2b10.217 (3)0.050 (3)0.533 (2)0.025*
H2b20.261 (3)0.1161 (11)0.418 (5)0.025*
H2c20.369 (3)0.2478 (12)0.066 (4)0.025*
H2c10.386 (3)0.193 (2)0.080 (2)0.025*
H3b10.429 (2)0.0726 (15)0.425 (4)0.025*
H3b20.385 (4)0.013 (2)0.553 (2)0.025*
H3c20.430 (4)0.0808 (13)0.048 (3)0.025*
H3c10.5280 (19)0.154 (3)0.076 (4)0.025*
B410.0038 (13)0.3016 (9)0.9834 (14)0.025*
F420.0163 (19)0.2499 (9)1.0878 (15)0.025*
F430.0206 (18)0.2645 (10)0.8761 (14)0.025*
F440.1003 (14)0.3346 (13)0.9819 (14)0.025*
F450.0788 (15)0.3404 (12)1.0275 (16)0.025*
Geometric parameters (Å, º) top
Fe—N4a2.098 (4)C1b—N1b1.319 (4)
Fe—N4ai2.098 (4)C1b—H1b1.068 (15)
Fe—N4b1.970 (9)C1c—N4c1.329 (13)
Fe—N4bi1.970 (9)C1c—N3c2.074 (17)
Fe—N4c2.079 (10)C1c—N2c2.140 (17)
Fe—N4ci2.079 (10)C1c—N1c1.316 (13)
Br1—Br2ii2.891 (12)C1c—H1c1.077 (16)
Br1—N2a2.081 (16)C2b—Br22.806 (12)
Br1—N1a2.783 (13)C2b—N1b1.515 (13)
Br1—C3a1.939 (13)C2b—C3b1.539 (13)
Br1—H3a22.56 (3)C2b—H2b11.075 (17)
Br1—H3a12.50 (3)C2b—H2b21.075 (17)
Br2—Br1iii2.891 (12)C2c—Br32.873 (13)
Br2—C2b2.806 (12)C2c—N1c1.478 (14)
Br2—C3b1.895 (12)C2c—C3c1.567 (14)
Br2—H3b12.50 (3)C2c—H2c21.081 (17)
Br2—H3b22.48 (3)C2c—H2c11.068 (17)
Br3—C2c2.873 (13)C3b—Br21.895 (12)
Br3—C3c1.903 (12)C3b—C2b1.539 (13)
Br3—H3a2iv2.52 (4)C3b—H2b22.08 (3)
Br3—H3b1v2.71 (3)C3b—H3b11.034 (18)
Br3—H3c22.56 (3)C3b—H3b21.113 (17)
Br3—H3c12.56 (3)C3c—Br31.903 (12)
N4a—Fe2.098 (4)C3c—C2c1.567 (14)
N4a—N3a1.295 (13)C3c—H3c21.096 (18)
N4a—N2a2.148 (15)C3c—H3c11.111 (18)
N4a—C1a1.355 (11)H1a—C1a1.096 (16)
N3a—N4a1.295 (13)H1a—H1bi1.62 (3)
N3a—N2a1.297 (13)H1a—F42vi2.27 (3)
N3a—N1a2.125 (13)H2a2—C2a1.118 (17)
N3a—C1a2.080 (15)H2a2—H2a11.78 (3)
N2a—Br12.081 (16)H2a1—C2a1.082 (18)
N2a—N4a2.148 (15)H2a1—H2a21.78 (3)
N2a—N3a1.297 (13)H2a1—H3c1ii1.52 (5)
N2a—N1a1.314 (13)H3a2—Br12.56 (3)
N2a—C1a2.107 (17)H3a2—Br3vii2.52 (4)
N1a—Br12.783 (13)H3a2—C2a2.08 (3)
N1a—N3a2.125 (13)H3a2—C3a1.072 (18)
N1a—N2a1.314 (13)H3a2—H3a11.76 (3)
N1a—C1a1.348 (12)H3a1—Br12.50 (3)
N1a—C2a1.507 (9)H3a1—C2a2.07 (3)
N4b—Fe1.970 (9)H3a1—C3a1.103 (19)
N4b—N3b1.356 (12)H3a1—H3a21.76 (3)
N4b—N2b2.135 (12)H1b—C1ai1.90 (2)
N4b—N1b2.145 (10)H1b—C1b1.068 (15)
N4b—C1b1.320 (4)H1b—H1ai1.62 (3)
N4c—Fe2.079 (10)H1c—C1c1.077 (16)
N4c—N3c1.302 (13)H2b1—C2b1.075 (17)
N4c—N1c2.132 (14)H2b1—H2b21.75 (3)
N4c—C1c1.329 (13)H2b2—C2b1.075 (17)
N3b—N4b1.356 (12)H2b2—C3b2.08 (3)
N3b—N2b1.278 (13)H2b2—H2b11.75 (3)
N3b—N1b2.132 (13)H2b2—F44viii2.21 (4)
N3b—C1b2.145 (11)H2c2—C2c1.081 (17)
N3c—N4c1.302 (13)H2c2—H2c11.80 (3)
N3c—N2c1.307 (14)H2c1—C2c1.068 (17)
N3c—N1c2.039 (16)H2c1—H2c21.80 (3)
N3c—C1c2.074 (17)H3b1—Br22.50 (3)
N2b—N4b2.135 (12)H3b1—Br3v2.71 (3)
N2b—N3b1.278 (13)H3b1—C3b1.034 (18)
N2b—N1b1.336 (13)H3b1—H3b21.78 (3)
N2b—C1b2.135 (11)H3b2—Br22.48 (3)
N1b—N4b2.145 (10)H3b2—C3b1.113 (17)
N1b—N3b2.132 (13)H3b2—H3b11.78 (3)
N1b—N2b1.336 (13)H3c2—Br32.56 (3)
N1b—C1b1.319 (4)H3c2—C3c1.096 (18)
N1b—C2b1.515 (13)H3c2—H3c11.77 (3)
N2c—N3c1.307 (14)H3c1—Br32.56 (3)
N2c—N1c1.277 (14)H3c1—C3c1.111 (18)
N2c—C1c2.140 (17)H3c1—H2a1iii1.52 (5)
N1c—N4c2.132 (14)H3c1—H3c21.77 (3)
N1c—N3c2.039 (16)B41—F421.423 (14)
N1c—N2c1.277 (14)B41—F431.320 (14)
N1c—C1c1.316 (13)B41—F441.293 (15)
N1c—C2c1.478 (14)B41—F451.286 (15)
C1a—N4a1.355 (11)F42—H1avi2.27 (3)
C1a—N3a2.080 (15)F42—B411.423 (14)
C1a—N2a2.107 (17)F42—F432.237 (18)
C1a—N1a1.348 (12)F42—F442.113 (19)
C1a—H1a1.096 (16)F42—F452.067 (19)
C1a—H1bi1.90 (2)F43—B411.320 (14)
C2a—N1a1.507 (9)F43—F422.237 (18)
C2a—C3a1.501 (14)F43—F442.197 (19)
C2a—H2a21.118 (17)F43—F452.177 (18)
C2a—H2a11.082 (18)F44—H2b2ix2.21 (4)
C2a—H3a22.08 (3)F44—B411.293 (15)
C2a—H3a12.07 (3)F44—F422.113 (19)
C3a—Br11.939 (13)F44—F432.197 (19)
C3a—C2a1.501 (14)F44—F452.191 (18)
C3a—H3a21.072 (18)F45—B411.286 (15)
C3a—H3a11.103 (19)F45—F422.067 (19)
C1b—N4b1.320 (4)F45—F432.177 (18)
C1b—N3b2.145 (11)F45—F442.191 (18)
C1b—N2b2.135 (11)
N4a—Fe—N4ai180.0C2a—C3a—H3a1104.2 (19)
N4a—Fe—N4b93.8 (4)H3a2—C3a—H3a1108 (2)
N4a—Fe—N4bi86.2 (4)N4b—C1b—N1b108.7 (7)
N4a—Fe—N4c96.5 (2)N4b—C1b—H1b126.6 (13)
N4a—Fe—N4ci83.5 (2)N1b—C1b—H1b124.6 (13)
N4ai—Fe—N4b86.2 (4)N4c—C1c—N1c107.4 (10)
N4ai—Fe—N4bi93.8 (4)N4c—C1c—H1c127.4 (15)
N4ai—Fe—N4c83.5 (2)N1c—C1c—H1c125.2 (14)
N4ai—Fe—N4ci96.5 (2)N1b—C2b—C3b122.4 (8)
N4b—Fe—N4bi179.9802N1b—C2b—H2b1107.3 (18)
N4b—Fe—N4c85.8 (3)N1b—C2b—H2b2107 (2)
N4b—Fe—N4ci94.2 (3)C3b—C2b—H2b1106.0 (19)
N4bi—Fe—N4c94.2 (3)C3b—C2b—H2b2104 (2)
N4bi—Fe—N4ci85.8 (3)H2b1—C2b—H2b2109 (2)
N4c—Fe—N4ci180.0N1c—C2c—C3c96.7 (10)
Br2ii—Br1—N2a128.0 (5)N1c—C2c—H2c2111 (2)
Br2ii—Br1—C3a123.1 (7)N1c—C2c—H2c1111 (2)
N2a—Br1—C3a83.2 (7)C3c—C2c—H2c2111.9 (19)
Br1iii—Br2—C3b128.8 (6)C3c—C2c—H2c1111 (2)
Fe—N4a—N3a123.2 (5)H2c2—C2c—H2c1114 (2)
Fe—N4a—C1a132.6 (8)Br2—C3b—C2b109.1 (7)
N3a—N4a—C1a103.4 (7)Br2—C3b—H3b1114.1 (19)
N4a—N3a—N2a111.9 (8)Br2—C3b—H3b2108.0 (19)
Br1—N2a—N3a142.8 (11)C2b—C3b—H3b1109.2 (18)
Br1—N2a—N1a108.0 (9)C2b—C3b—H3b2104 (2)
N3a—N2a—N1a109.0 (11)H3b1—C3b—H3b2112 (2)
N2a—N1a—C1a104.7 (9)Br3—C3c—C2c111.4 (10)
N2a—N1a—C2a125.3 (9)Br3—C3c—H3c2114.3 (18)
C1a—N1a—C2a130.0 (8)Br3—C3c—H3c1113.2 (19)
Fe—N4b—N3b124.5 (6)C2c—C3c—H3c2106.5 (19)
Fe—N4b—C1b128.8 (6)C2c—C3c—H3c1104 (2)
N3b—N4b—C1b106.6 (7)H3c2—C3c—H3c1107 (2)
Fe—N4c—N3c128.2 (7)C2a—H2a1—H3c1ii135 (4)
Fe—N4c—C1c127.7 (8)C3c—H3c1—H2a1iii147 (4)
N3c—N4c—C1c104.0 (9)F42—B41—F43109.2 (12)
N4b—N3b—N2b108.3 (7)F42—B41—F44102.1 (13)
N4c—N3c—N2c113.1 (11)F42—B41—F4599.3 (12)
N3b—N2b—N1b109.3 (7)F43—B41—F44114.5 (13)
N2b—N1b—C1b107.1 (7)F43—B41—F45113.3 (13)
N2b—N1b—C2b121.3 (9)F44—B41—F45116.3 (14)
C1b—N1b—C2b131.6 (10)B41—F42—F4436.7 (7)
N3c—N2c—N1c104.2 (11)B41—F42—F4537.9 (7)
N2c—N1c—C1c111.2 (11)F44—F42—F4563.2 (7)
N2c—N1c—C2c119.6 (11)B41—F43—F4432.4 (7)
C1c—N1c—C2c129.2 (11)B41—F43—F4532.8 (7)
N4a—C1a—N1a110.1 (9)F44—F43—F4560.1 (6)
N4a—C1a—H1a124.4 (13)B41—F44—F4241.2 (8)
N1a—C1a—H1a125.3 (12)B41—F44—F4333.1 (7)
N1a—C2a—C3a104.2 (9)B41—F44—F4531.8 (7)
N1a—C2a—H2a2111.1 (18)F42—F44—F4362.5 (7)
N1a—C2a—H2a1112 (2)F42—F44—F4557.4 (7)
C3a—C2a—H2a2109.0 (19)F43—F44—F4559.5 (7)
C3a—C2a—H2a1112.7 (18)B41—F45—F4242.8 (8)
H2a2—C2a—H2a1108 (2)B41—F45—F4333.8 (7)
Br1—C3a—C2a115.9 (10)B41—F45—F4431.9 (8)
Br1—C3a—H3a2113.6 (19)F42—F45—F4363.6 (7)
Br1—C3a—H3a1107.5 (18)F42—F45—F4459.4 (7)
C2a—C3a—H3a2107 (2)F43—F45—F4460.4 (7)
Symmetry codes: (i) x, y, z; (ii) x+1, y, z; (iii) x1, y, z; (iv) x1, y+1/2, z+1/2; (v) x1, 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 formulaC18H30FeI6N24·2(BF4)?C18H30B2F8FeI6N24?
Mr1573.50?1573.50?
Crystal system, space groupMonoclinic, 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?, ?, ?
V3)2427.96 (6)?2279.25?
Z2?2?
Radiation typeSynchrotron, λ = 0.75003 Å?, λ = 0.999995 Å?, λ = 0.999995 Å?, λ = 0.999995 Å
µ (mm1)?
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 = 0.012θmin = 0.010 2θmax = 1.800 2θstep = 0.012θmin = 0.010 2θmax = 1.800 2θstep = 0.01
Refinement
R factors and goodness of fitR[F2 > 2σ(F2)] = ?, wR(F2) = ?, S = ?Rp = 0.025, Rwp = 0.037, Rexp = 0.012, R(F2) = 0.09479, χ2 = 10.368Rp = 0.025, Rwp = 0.037, Rexp = 0.012, R(F2) = 0.09479, χ2 = 10.368Rp = 0.025, Rwp = 0.037, Rexp = 0.012, R(F2) = 0.09479, χ2 = NOT FOUND
No. of reflections/data points?180180180
No. of parameters?212212?
No. of restraints?139139?
(Δ/σ)max?0.730.73?
Δρmax, Δρmin (e Å3)?, ?


(LAST_publ)(TEEB90RR3TEXT4_publ)
Crystal data
Chemical formulaC18H30B2Br6F8FeN24C18H30B2Br6F8FeN24
Mr1291.531291.53
Crystal system, space groupMonoclinic, P21/cMonoclinic, P21/c
Temperature (K)300 K300 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), 9090, 89.992 (2), 90
V3)2325.452186.60
Z22
Radiation typeSynchrotron, λ = 0.999995 ÅSynchrotron, λ = 0.999995 Å
µ (mm1)
Specimen shape, size (mm)?, ? × ? × ??, ? × ? × ?
Data collection
DiffractometerDebye 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 = 0.012θmin = 0.010 2θmax = 1.800 2θstep = 0.01
Refinement
R factors and goodness of fitRp = 0.046, Rwp = 0.065, Rexp = 0.011, χ2 = 40.704Rp = 0.051, Rwp = 0.070, Rexp = 0.011, χ2 = 43.824
No. of reflections/data points180180
No. of parameters184181
No. of restraints145145
(Δ/σ)max0.643.95
Δρmax, Δρmin (e Å3)

Computer programs: GSAS, Xtal BONDLA CIFIO.

 

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