Structure determination of the [Fe(teec)₆](BF₄)₂ metal complex from laboratory and synchrotron X-­ray powder diffraction data with grid-search techniques

The structure of the coordination compound [Fe(teec)₆](BF₄)₂, hexa[1-(2-chloroethyl)tetrazole]iron(II) di(borotetrafluoride), has been determined using the grid-search techniques of the program suite MRIA. A Guinier-camera data set was used to determine the unit cell, the space group and to position the initial model. A high-resolution synchrotron powder data set was used to position a more detailed model using torsion-angle variation and to refine the structure leading to Rp = 0.0689, Rw = 0.0805 and GoF = 1.38. The crystal structure at room temperature shows the existence of two symmetry-equivalent iron(II) ions in the high-spin state.

Computing details

Software used to prepare material for publication: PLATON (Spek, 1990).

Figures

View of the title compound with the atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 50% probability level.

(stassen)

Crystal data

C18H30Cl6FeN24·2(BF4)	V = 2315.5 (3) Å^3
Mr = 1024.83	Z = 2
Monoclinic, P21/c	F(000) = 1032
Hall symbol: -P 2ybc	Dx = 1.470 Mg m^−3
a = 12.1966 (11) Å	?? Kα radiation, λ = 0.99542 Å
b = 17.9677 (13) Å	T = 0 K
c = 10.5667 (8) Å	× × mm
β = 90.555 (5)°

Data collection

h = ?→?	l = ?→?
k = ?→?

Refinement

0 restraints
See text

Special details

Geometry. Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All e.s.d.'s are estimated from the variances of the (full) variance-covariance matrix. The cell e.s.d.'s are taken into account in the estimation of distances, angles and torsion angles

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Fe	0.00000	0.50000	0.50000	0.049 (8)*
Cl1	0.3742 (16)	0.7360 (11)	0.4318 (17)	0.135 (8)*
Cl2	0.3820 (17)	0.4423 (11)	0.8872 (18)	0.1354*
Cl3	0.3944 (16)	0.3536 (10)	0.224 (2)	0.1354*
N1A	0.188 (2)	0.6619 (9)	0.2947 (18)	0.0507*
N1B	0.179 (2)	0.5307 (12)	0.8490 (13)	0.0507*
N1C	0.194 (2)	0.3143 (9)	0.375 (2)	0.0507*
N2A	0.224 (2)	0.6015 (8)	0.2437 (17)	0.0507*
N2B	0.212 (2)	0.5873 (10)	0.7853 (13)	0.0507*
N2C	0.231 (2)	0.3198 (9)	0.4948 (16)	0.0507*
N3A	0.175 (2)	0.5467 (7)	0.2963 (14)	0.0507*
N3B	0.167 (2)	0.5857 (8)	0.6761 (11)	0.0507*
N3C	0.177 (2)	0.3732 (7)	0.5466 (13)	0.0507*
N4A	0.1038 (17)	0.5725 (7)	0.3836 (14)	0.0507*
N4B	0.1021 (17)	0.5274 (9)	0.6687 (12)	0.0507*
N4C	0.1065 (17)	0.4038 (8)	0.4604 (15)	0.0507*
C1A	0.1112 (19)	0.6440 (9)	0.3786 (17)	0.0507*
C1B	0.1075 (19)	0.4932 (11)	0.7773 (12)	0.0507*
C1C	0.1174 (18)	0.3651 (8)	0.3553 (18)	0.0507*
C2A	0.221 (2)	0.7373 (13)	0.249 (3)	0.0507*
C2B	0.208 (2)	0.5173 (18)	0.9849 (17)	0.0507*
C2C	0.233 (2)	0.2547 (11)	0.290 (3)	0.0507*
C3A	0.341 (2)	0.7496 (15)	0.270 (3)	0.0507*
C3B	0.335 (2)	0.5073 (19)	0.994 (2)	0.0507*
C3C	0.358 (2)	0.2599 (15)	0.277 (3)	0.0507*
F1	0.10593	0.15933	0.55844	0.0507*
F2	0.04371	0.17048	0.37391	0.0507*
F3	−0.02864	0.09152	0.51076	0.0507*
F4	−0.04674	0.21288	0.53886	0.0507*
B	0.00913	0.15841	0.48901	0.0507*
H1A	0.0608 (17)	0.6823 (8)	0.4334 (19)	0.0507*
H1B	0.0625 (18)	0.4439 (12)	0.8046 (12)	0.0507*
H1C	0.0736 (18)	0.3746 (9)	0.2687 (17)	0.0507*
H21A	0.172 (2)	0.7799 (10)	0.302 (3)	0.0507*
H21B	0.170 (3)	0.466 (2)	1.0170 (17)	0.0507*
H21C	0.194 (3)	0.2609 (15)	0.199 (3)	0.0507*
H22A	0.198 (3)	0.7435 (17)	0.150 (3)	0.0507*
H22B	0.182 (3)	0.563 (2)	1.042 (2)	0.0507*
H22C	0.214 (3)	0.2011 (11)	0.330 (4)	0.0507*
H31A	0.385 (2)	0.7146 (19)	0.207 (4)	0.0507*
H31B	0.370 (3)	0.563 (2)	0.982 (3)	0.0507*
H31C	0.397 (2)	0.245 (2)	0.361 (3)	0.0507*
H32A	0.357 (3)	0.8085 (16)	0.247 (5)	0.0507*
H32B	0.351 (3)	0.491 (3)	1.094 (3)	0.0507*
H32C	0.380 (3)	0.221 (2)	0.199 (4)	0.0507*

Geometric parameters (Å, º)

Fe—N4A	2.201 (16)	N3B—N4B	1.31 (3)
Fe—N4B	2.220 (16)	N3C—N4C	1.36 (3)
Fe—N4C	2.205 (17)	N4A—C1A	1.29 (2)
Cl1—C3A	1.77 (4)	N4B—C1B	1.30 (2)
Cl2—C3B	1.73 (3)	N4C—C1C	1.32 (2)
Cl3—C3C	1.83 (3)	C2A—C3A	1.49 (3)
F1—B	1.3841	C2B—C3B	1.56 (3)
F2—B	1.3092	C2C—C3C	1.53 (3)
F3—B	1.3082	C1A—H1A	1.09 (3)
F4—B	1.3064	C1B—H1B	1.08 (3)
N1A—N2A	1.29 (2)	C1C—H1C	1.07 (3)
N1A—C2A	1.49 (3)	C2A—H22A	1.09 (4)
N1A—C1A	1.34 (3)	C2A—H21A	1.12 (4)
N1B—N2B	1.29 (3)	C2B—H22B	1.07 (4)
N1B—C1B	1.33 (3)	C2B—H21B	1.09 (5)
N1B—C2B	1.50 (2)	C2C—H21C	1.07 (4)
N1C—C2C	1.48 (3)	C2C—H22C	1.08 (3)
N1C—C1C	1.32 (3)	C3A—H31A	1.06 (5)
N1C—N2C	1.34 (3)	C3A—H32A	1.10 (4)
N2A—N3A	1.28 (2)	C3B—H32B	1.11 (4)
N2B—N3B	1.27 (2)	C3B—H31B	1.10 (5)
N2C—N3C	1.29 (3)	C3C—H31C	1.04 (4)
N3A—N4A	1.35 (3)	C3C—H32C	1.12 (5)
Cl1···N1A	2.99 (3)	N2C···H31C	2.82 (4)
Cl1···C1A	3.65 (3)	N3A···H22B^ii	2.71 (3)
Cl1···C3A^i	3.61 (4)	N3B···H21A^i	2.76 (3)
Cl2···C1B	3.65 (3)	N3C···H21C^iii	2.90 (3)
Cl2···N1B	2.97 (3)	N4A···H1B^vii	2.84 (3)
Cl2···N2B	3.49 (3)	N4B···H1C^vii	2.86 (3)
Cl3···N1C	3.02 (3)	N4C···H1A^vii	2.80 (3)
Cl1···H31A^i	3.04 (5)	C1A···F2^ix	3.2890
Cl3···H32B^ii	2.87 (5)	C1A···F4^vii	2.8293
F1···C2C^iii	3.2713	C1A···N3B	3.38 (2)
F1···C1C^iii	3.1691	C1A···Cl1	3.65 (3)
F2···C2C	2.9062	C1B···F3^viii	3.0171
F2···N1C	3.1682	C1B···Cl2	3.65 (3)
F2···C1B^iv	3.2112	C1B···N3C	3.37 (2)
F2···C1A^v	3.2890	C1B···F3^iii	3.3525
F3···N1B^vi	2.6088	C1B···F2^iii	3.2112
F3···C2B^vi	2.5628	C1C···N3A	3.40 (2)
F3···N2B^vi	3.1216	C1C···F1^iv	3.1691
F3···C1B^vi	3.0171	C2A···N2B^x	3.18 (3)
F3···C1B^iv	3.3525	C2A···N3B^x	3.34 (3)
F4···C2A^vii	3.2305	C2A···F4^vii	3.2305
F4···C1A^vii	2.8293	C2B···F3^viii	2.5628
F1···H21C^iii	2.3201	C2B···N3A^xi	3.36 (2)
F1···H21B^iv	2.4250	C2B···N2A^xi	3.13 (3)
F1···H1C^iii	2.3410	C2C···F2	2.9062
F1···H22C	2.8617	C2C···N2C^iv	3.39 (3)
F2···H1B^iv	2.1944	C2C···F1^iv	3.2713
F2···H22C	2.2023	C3A···N2B^x	3.33 (3)
F3···H21B^vi	2.8522	C3A···Cl1^x	3.61 (4)
F3···H1B^iv	2.5364	C3B···N2A^xi	3.42 (3)
F3···H21B^iv	2.6342	B···H21B^iv	2.9871
F3···H22B^vi	2.0130	B···H22B^vi	2.9095
F4···H22A^v	2.7600	B···H1B^iv	2.7612
F4···H21A^vii	2.2866	H1A···F4^vii	1.9140
F4···H1A^vii	1.9140	H1A···N4C^vii	2.80 (3)
N1A···Cl1	2.99 (3)	H1B···N4A^vii	2.84 (3)
N1B···Cl2	2.97 (3)	H1B···F2^iii	2.1944
N1B···F3^viii	2.6088	H1B···B^iii	2.7612
N1C···F2	3.1682	H1B···F3^iii	2.5364
N1C···Cl3	3.02 (3)	H1C···F1^iv	2.3410
N2A···C3B^ii	3.42 (3)	H1C···N4B^vii	2.86 (3)
N2A···C2B^ii	3.13 (3)	H21A···N2B^x	2.44 (3)
N2B···Cl2	3.49 (3)	H21A···N3B^x	2.76 (3)
N2B···F3^viii	3.1216	H21A···F4^vii	2.2866
N2B···C2A^i	3.18 (3)	H21B···B^iii	2.9871
N2B···C3A^i	3.33 (3)	H21B···F3^iii	2.6342
N2C···C2C^iii	3.39 (3)	H21B···F3^viii	2.8522
N3A···N4C	3.21 (2)	H21B···F1^iii	2.4250
N3A···C2B^ii	3.36 (2)	H21C···F1^iv	2.3201
N3A···C1C	3.40 (2)	H21C···N3C^iv	2.90 (3)
N3B···C2A^i	3.34 (3)	H21C···N2C^iv	2.64 (3)
N3B···C1A	3.38 (2)	H22A···F4^ix	2.7600
N3B···N4A	3.19 (2)	H22B···F3^viii	2.0130
N3C···N4B	3.19 (2)	H22B···B^viii	2.9095
N3C···C1B	3.37 (2)	H22B···N2A^xi	2.29 (3)
N4A···N3B	3.19 (2)	H22B···N3A^xi	2.71 (3)
N4B···N3C	3.19 (2)	H22C···F2	2.2023
N4C···N3A	3.21 (2)	H22C···F1	2.8617
N2A···H31A	2.85 (4)	H31A···N2A	2.85 (4)
N2A···H22B^ii	2.29 (3)	H31A···Cl1^x	3.04 (5)
N2B···H21A^i	2.44 (3)	H31B···N2B	2.85 (4)
N2B···H32A^i	2.61 (4)	H31C···N2C	2.82 (4)
N2B···H31B	2.85 (4)	H32A···N2B^x	2.61 (4)
N2C···H21C^iii	2.64 (3)	H32B···Cl3^xi	2.87 (5)
N2C···H32C^iii	2.90 (4)	H32C···N2C^iv	2.90 (4)
N4A—Fe—N4B	89.8 (6)	Cl1—C3A—C2A	110 (2)
N4A—Fe—N4C	90.8 (6)	Cl2—C3B—C2B	111.9 (19)
N4A—Fe—N4A^vii	180.00	Cl3—C3C—C2C	109.1 (18)
N4A—Fe—N4B^vii	90.2 (6)	N1A—C1A—H1A	127.0 (18)
N4A—Fe—N4C^vii	89.2 (6)	N4A—C1A—H1A	124 (2)
N4B—Fe—N4C	90.0 (6)	N1B—C1B—H1B	126.4 (16)
N4A^vii—Fe—N4B	90.2 (6)	N4B—C1B—H1B	126.8 (19)
N4B—Fe—N4B^vii	180.00	N1C—C1C—H1C	126 (2)
N4B—Fe—N4C^vii	90.0 (6)	N4C—C1C—H1C	126 (2)
N4A^vii—Fe—N4C	89.2 (6)	N1A—C2A—H21A	108 (2)
N4B^vii—Fe—N4C	90.0 (6)	N1A—C2A—H22A	110 (3)
N4C—Fe—N4C^vii	180.00	C3A—C2A—H21A	110 (3)
N4A^vii—Fe—N4B^vii	89.8 (6)	C3A—C2A—H22A	112 (3)
N4A^vii—Fe—N4C^vii	90.8 (6)	H21A—C2A—H22A	106 (3)
N4B^vii—Fe—N4C^vii	90.0 (6)	N1B—C2B—H21B	110 (2)
N2A—N1A—C1A	108.6 (17)	N1B—C2B—H22B	110 (3)
N2A—N1A—C2A	122 (2)	C3B—C2B—H21B	108 (3)
C1A—N1A—C2A	128.7 (19)	C3B—C2B—H22B	111 (3)
N2B—N1B—C1B	108.0 (15)	H21B—C2B—H22B	110 (3)
N2B—N1B—C2B	124 (2)	N1C—C2C—H21C	109 (2)
C1B—N1B—C2B	128 (2)	N1C—C2C—H22C	110 (3)
N2C—N1C—C1C	109.2 (18)	C3C—C2C—H21C	110 (3)
N2C—N1C—C2C	121 (2)	C3C—C2C—H22C	108 (3)
C1C—N1C—C2C	129 (2)	H21C—C2C—H22C	110 (3)
N1A—N2A—N3A	107.6 (19)	Cl1—C3A—H31A	114 (3)
N1B—N2B—N3B	108.8 (19)	Cl1—C3A—H32A	108 (3)
N1C—N2C—N3C	106.7 (18)	C2A—C3A—H31A	109 (3)
N2A—N3A—N4A	109.7 (14)	C2A—C3A—H32A	107 (3)
N2B—N3B—N4B	109.0 (14)	H31A—C3A—H32A	110 (4)
N2C—N3C—N4C	109.8 (15)	Cl2—C3B—H31B	114 (2)
Fe—N4A—N3A	123.6 (10)	Cl2—C3B—H32B	113 (3)
Fe—N4A—C1A	130.8 (15)	C2B—C3B—H31B	106 (3)
N3A—N4A—C1A	105.5 (16)	C2B—C3B—H32B	105 (3)
Fe—N4B—N3B	123.9 (10)	H31B—C3B—H32B	107 (4)
Fe—N4B—C1B	128.7 (15)	Cl3—C3C—H31C	113 (3)
N3B—N4B—C1B	107.3 (15)	Cl3—C3C—H32C	107 (3)
Fe—N4C—N3C	124.0 (11)	C2C—C3C—H31C	111 (3)
Fe—N4C—C1C	129.6 (14)	C2C—C3C—H32C	106 (3)
N3C—N4C—C1C	106.4 (16)	H31C—C3C—H32C	111 (4)
N1A—C1A—N4A	108.5 (17)	F1—B—F2	102.10
N1B—C1B—N4B	106.8 (18)	F1—B—F3	102.59
N1C—C1C—N4C	108.0 (18)	F1—B—F4	102.87
N1A—C2A—C3A	111 (2)	F2—B—F3	115.63
N1B—C2B—C3B	107.6 (18)	F2—B—F4	115.11
N1C—C2C—C3C	110 (2)	F3—B—F4	115.57
N4B—Fe—N4A—N3A	108.7 (17)	C1B—N1B—N2B—N3B	−2 (3)
N4B—Fe—N4A—C1A	−73 (2)	C2B—N1B—N2B—N3B	−175 (2)
N4C—Fe—N4A—N3A	18.7 (17)	N2B—N1B—C1B—N4B	2 (3)
N4C—Fe—N4A—C1A	−162.7 (19)	C2B—N1B—C1B—N4B	175 (2)
N4B^vii—Fe—N4A—N3A	−71.3 (17)	N2B—N1B—C2B—C3B	−63 (3)
N4B^vii—Fe—N4A—C1A	107 (2)	C1B—N1B—C2B—C3B	125 (3)
N4C^vii—Fe—N4A—N3A	−161.3 (17)	C1C—N1C—N2C—N3C	0 (3)
N4C^vii—Fe—N4A—C1A	17.3 (19)	C2C—N1C—N2C—N3C	−176 (2)
N4A—Fe—N4B—N3B	18.9 (17)	N2C—N1C—C1C—N4C	1 (2)
N4A—Fe—N4B—C1B	−163.9 (19)	C2C—N1C—C1C—N4C	177 (2)
N4C—Fe—N4B—N3B	109.8 (17)	N2C—N1C—C2C—C3C	−59 (3)
N4C—Fe—N4B—C1B	−73.1 (19)	C1C—N1C—C2C—C3C	126 (3)
N4A^vii—Fe—N4B—N3B	−161.1 (17)	N1A—N2A—N3A—N4A	1 (3)
N4A^vii—Fe—N4B—C1B	16.1 (19)	N1B—N2B—N3B—N4B	1 (3)
N4C^vii—Fe—N4B—N3B	−70.2 (17)	N1C—N2C—N3C—N4C	−1 (2)
N4C^vii—Fe—N4B—C1B	106.9 (19)	N2A—N3A—N4A—Fe	−179.9 (15)
N4A—Fe—N4C—N3C	106.9 (16)	N2A—N3A—N4A—C1A	1 (2)
N4A—Fe—N4C—C1C	−72.5 (18)	N2B—N3B—N4B—Fe	178.2 (15)
N4B—Fe—N4C—N3C	17.1 (16)	N2B—N3B—N4B—C1B	1 (3)
N4B—Fe—N4C—C1C	−162.3 (18)	N2C—N3C—N4C—Fe	−177.5 (14)
N4A^vii—Fe—N4C—N3C	−73.1 (16)	N2C—N3C—N4C—C1C	2 (2)
N4A^vii—Fe—N4C—C1C	107.5 (18)	Fe—N4A—C1A—N1A	178.7 (15)
N4B^vii—Fe—N4C—N3C	−162.9 (16)	N3A—N4A—C1A—N1A	−3 (2)
N4B^vii—Fe—N4C—C1C	17.7 (18)	Fe—N4B—C1B—N1B	−179.2 (15)
C1A—N1A—N2A—N3A	−2 (3)	N3B—N4B—C1B—N1B	−2 (2)
C2A—N1A—N2A—N3A	−175 (2)	Fe—N4C—C1C—N1C	177.6 (15)
N2A—N1A—C1A—N4A	3 (3)	N3C—N4C—C1C—N1C	−2 (2)
C2A—N1A—C1A—N4A	175 (2)	N1A—C2A—C3A—Cl1	−56 (3)
N2A—N1A—C2A—C3A	−65 (3)	N1B—C2B—C3B—Cl2	−51 (3)
C1A—N1A—C2A—C3A	124 (3)	N1C—C2C—C3C—Cl3	−55 (3)

Symmetry codes: (i) x, −y+3/2, z+1/2; (ii) x, y, z−1; (iii) x, −y+1/2, z+1/2; (iv) x, −y+1/2, z−1/2; (v) −x, y−1/2, −z+1/2; (vi) −x, y−1/2, −z+3/2; (vii) −x, −y+1, −z+1; (viii) −x, y+1/2, −z+3/2; (ix) −x, y+1/2, −z+1/2; (x) x, −y+3/2, z−1/2; (xi) x, y, z+1.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
C1A—H1A···F4^vii	1.09 (3)	1.9140	2.8293	138.82
C1B—H1B···F2^iii	1.08 (3)	2.1944	3.2112	155.50
C1B—H1B···F3^iii	1.08 (3)	2.5364	3.3525	131.43
C1C—H1C···F1^iv	1.07 (3)	2.3410	3.1691	133.12
C2A—H21A···F4^vii	1.12 (4)	2.2866	3.2305	140.12
C2A—H21A···N2B^x	1.12 (4)	2.44 (3)	3.18 (3)	121 (2)
C2B—H21B···F1^iii	1.09 (5)	2.4250	3.4993	169.28
C2C—H21C···F1^iv	1.07 (4)	2.3201	3.2713	146.63
C2B—H22B···N2A^xi	1.07 (4)	2.29 (3)	3.13 (3)	134 (3)
C2B—H22B···F3^viii	1.07 (4)	2.0130	2.5628	108.61
C2C—H22C···F2	1.08 (3)	2.2023	2.9062	120.84
C3A—H32A···N2B^x	1.10 (4)	2.61 (4)	3.33 (3)	122 (3)

Symmetry codes: (iii) x, −y+1/2, z+1/2; (iv) x, −y+1/2, z−1/2; (vii) −x, −y+1, −z+1; (viii) −x, y+1/2, −z+3/2; (x) x, −y+3/2, z−1/2; (xi) x, y, z+1.