Poly[μ₄-isonicotinato-μ₃-nitrato-barium(II)]

The title compound, [Ba(C₆H₄NO₂)(NO₃)]_n, was formed by the hydro­thermal reaction of Ba(NO₃)₂, isonicotinamide and KOH with release of ammonia. The Ba ion is ten-coordinated by nine O atoms and one N atom. Five of these O atoms derive from one monodentate and two bidentate nitrate anions. The other O atoms derive from one bidentate and two monodentate carboxyl­ate groups of the isonicotinate anions. The coordination is completed by an N atom of the isonicotinate anion. These units are connected to form a three-dimensional framework structure.

Key indicators

• Single-crystal X-ray study
• T = 295 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.031
• wR factor = 0.074
• Data-to-parameter ratio = 22.7

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.98
PLAT063_ALERT_3_C Crystal Probably too Large for Beam Size .......       0.70 mm
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for        O22

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 ALERT level C = Check and explain
   0 ALERT level G = General alerts; check

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   1 ALERT type 2 Indicator that the structure model may be wrong or deficient
   2 ALERT type 3 Indicator that the structure quality may be low
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SIR92 (Altomare et al., 1993); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg, 2004); software used to prepare material for publication: SHELXL97.

Poly[µ₄-isonicotinato-µ₃-nitrato-barium(II)]

Crystal data

[Ba(C6H4NO2)(NO3)]	Z = 2
Mr = 321.45	F(000) = 300
Triclinic, P1	Dx = 2.523 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 5.6416 (10) Å	Cell parameters from 6816 reflections
b = 8.0487 (15) Å	θ = 2.1–32.2°
c = 9.7998 (18) Å	µ = 4.69 mm^−1
α = 93.525 (15)°	T = 295 K
β = 106.058 (14)°	Column, colourless
γ = 96.254 (15)°	0.7 × 0.3 × 0.2 mm
V = 423.12 (13) Å^3

Data collection

Stoe IPDS-II diffractometer	2928 independent reflections
Radiation source: fine-focus sealed tube	2604 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.040
ω and φ scans	θmax = 32.2°, θmin = 2.2°
Absorption correction: numerical [X-RED32 (Stoe & Cie, 2001) after optimizing the crystal shape using X-SHAPE (Stoe & Cie, 1999)	h = −7→8
Tmin = 0.367, Tmax = 0.670	k = −12→11
6949 measured reflections	l = −14→14

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.031	H-atom parameters constrained
wR(F^2) = 0.074	w = 1/[σ^2(Fo^2) + (0.0237P)^2 + 1.55P] where P = (Fo^2 + 2Fc^2)/3
S = 1.12	(Δ/σ)max = 0.001
2928 reflections	Δρmax = 1.81 e Å^−3
129 parameters	Δρmin = −1.34 e Å^−3
0 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.080 (3)

Special details

Experimental. A suitable single-crystal was carefully selected under a polarizing microscope and mounted in a glass capillary. The scattering intensities were collected on an imaging plate diffractometer (IPDS II, Stoe & Cie) equipped with a fine focus sealed tube X-ray source (Mo Kα, λ = 0.71073 Å) operating at 50 kV and 40 mA.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

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

	x	y	z	Uiso*/Ueq
Ba1	0.31305 (4)	0.21683 (3)	0.05085 (2)	0.02090 (9)
O11	−0.4910 (6)	0.1001 (4)	−0.1503 (3)	0.0304 (6)
O12	−0.1046 (5)	0.0703 (4)	−0.1524 (3)	0.0272 (6)
C1	−0.3143 (7)	0.1165 (5)	−0.2062 (4)	0.0223 (6)
C2	−0.3644 (7)	0.1824 (5)	−0.3511 (4)	0.0215 (6)
C6	−0.5678 (8)	0.2636 (6)	−0.4066 (4)	0.0280 (8)
H6	−0.6694	0.2920	−0.3509	0.034 (7)*
C4	−0.2805 (8)	0.1869 (6)	−0.5777 (4)	0.0308 (8)
H4	−0.1801	0.1616	−0.6350	0.034 (7)*
C3	−0.2142 (7)	0.1470 (6)	−0.4371 (4)	0.0265 (7)
H3	−0.0712	0.0972	−0.4012	0.034 (7)*
C5	−0.6179 (8)	0.3021 (6)	−0.5468 (4)	0.0312 (8)
H5	−0.7523	0.3602	−0.5823	0.034 (7)*
N1	−0.4837 (7)	0.2604 (5)	−0.6342 (4)	0.0305 (7)
N2	−0.1035 (6)	0.4325 (4)	0.1387 (3)	0.0241 (6)
O21	−0.2884 (6)	0.5109 (4)	0.1280 (4)	0.0357 (7)
O23	−0.1332 (6)	0.2758 (4)	0.1359 (4)	0.0326 (6)
O22	0.1083 (6)	0.5084 (5)	0.1506 (4)	0.0386 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ba1	0.02277 (12)	0.02352 (12)	0.01804 (12)	0.00532 (7)	0.00710 (7)	0.00460 (7)
O11	0.0343 (15)	0.0373 (16)	0.0250 (13)	0.0068 (12)	0.0157 (12)	0.0064 (12)
O12	0.0262 (13)	0.0304 (14)	0.0230 (12)	0.0043 (11)	0.0030 (10)	0.0056 (11)
C1	0.0278 (17)	0.0226 (16)	0.0168 (14)	0.0027 (13)	0.0068 (13)	0.0030 (12)
C2	0.0254 (16)	0.0211 (15)	0.0172 (14)	0.0006 (12)	0.0052 (12)	0.0029 (12)
C6	0.0301 (19)	0.032 (2)	0.0231 (17)	0.0081 (15)	0.0081 (14)	0.0044 (14)
C4	0.033 (2)	0.041 (2)	0.0203 (16)	0.0034 (17)	0.0103 (15)	0.0070 (15)
C3	0.0259 (17)	0.035 (2)	0.0197 (15)	0.0064 (15)	0.0067 (13)	0.0059 (14)
C5	0.034 (2)	0.033 (2)	0.0241 (18)	0.0081 (17)	0.0025 (16)	0.0071 (15)
N1	0.0348 (18)	0.0328 (18)	0.0210 (15)	0.0007 (14)	0.0044 (13)	0.0049 (13)
N2	0.0268 (15)	0.0278 (15)	0.0180 (13)	0.0074 (12)	0.0054 (11)	0.0040 (11)
O21	0.0378 (17)	0.0366 (17)	0.0398 (17)	0.0184 (14)	0.0157 (14)	0.0129 (14)
O23	0.0387 (16)	0.0240 (14)	0.0383 (16)	0.0066 (12)	0.0146 (14)	0.0064 (12)
O22	0.0313 (16)	0.0370 (17)	0.0455 (19)	−0.0032 (13)	0.0114 (14)	−0.0003 (14)

Geometric parameters (Å, º)

Ba1—O11^i	2.682 (3)	C1—C2	1.511 (5)
Ba1—O12	2.724 (3)	C2—C6	1.379 (5)
Ba1—O12^ii	2.838 (3)	C2—C3	1.388 (5)
Ba1—O21^iii	2.881 (3)	C6—C5	1.386 (6)
Ba1—O23	2.938 (3)	C6—H6	0.9300
Ba1—O22	2.954 (4)	C4—N1	1.344 (6)
Ba1—O11^ii	2.964 (3)	C4—C3	1.391 (5)
Ba1—N1^iv	2.964 (4)	C4—H4	0.9300
Ba1—O23^i	2.978 (3)	C3—H3	0.9300
Ba1—O21^i	2.985 (4)	C5—N1	1.341 (6)
Ba1—C1^ii	3.164 (4)	C5—H5	0.9300
Ba1—N2	3.332 (3)	N2—O23	1.251 (5)
O11—C1	1.262 (5)	N2—O22	1.253 (5)
O12—C1	1.261 (5)	N2—O21	1.260 (4)
O11^i—Ba1—O12	78.98 (10)	O11^i—Ba1—N2	149.01 (9)
O11^i—Ba1—O12^ii	106.02 (9)	O12—Ba1—N2	80.74 (9)
O12—Ba1—O12^ii	70.67 (9)	O12^ii—Ba1—N2	88.89 (8)
O11^i—Ba1—O21^iii	78.15 (9)	O21^iii—Ba1—N2	76.91 (8)
O12—Ba1—O21^iii	84.86 (10)	O23—Ba1—N2	21.88 (8)
O12^ii—Ba1—O21^iii	153.49 (9)	O22—Ba1—N2	21.95 (9)
O11^i—Ba1—O23	148.36 (10)	O11^ii—Ba1—N2	130.13 (8)
O12—Ba1—O23	69.63 (9)	N1^iv—Ba1—N2	79.32 (10)
O12^ii—Ba1—O23	67.63 (8)	O23^i—Ba1—N2	131.59 (9)
O21^iii—Ba1—O23	94.82 (9)	O21^i—Ba1—N2	93.43 (9)
O11^i—Ba1—O22	143.83 (10)	C1^ii—Ba1—N2	107.00 (9)
O12—Ba1—O22	98.43 (10)	C1—O11—Ba1^v	147.0 (3)
O12^ii—Ba1—O22	107.00 (9)	C1—O11—Ba1^ii	87.2 (2)
O21^iii—Ba1—O22	65.71 (10)	Ba1^v—O11—Ba1^ii	104.52 (9)
O23—Ba1—O22	43.09 (9)	C1—O12—Ba1	133.3 (3)
O11^i—Ba1—O11^ii	75.48 (9)	C1—O12—Ba1^ii	93.0 (2)
O12—Ba1—O11^ii	96.24 (9)	Ba1—O12—Ba1^ii	109.33 (9)
O12^ii—Ba1—O11^ii	45.02 (8)	O12—C1—O11	123.7 (3)
O21^iii—Ba1—O11^ii	152.85 (8)	O12—C1—C2	118.3 (3)
O23—Ba1—O11^ii	111.06 (8)	O11—C1—C2	117.9 (3)
O22—Ba1—O11^ii	140.09 (9)	O12—C1—Ba1^ii	63.6 (2)
O11^i—Ba1—N1^iv	130.54 (10)	O11—C1—Ba1^ii	69.3 (2)
O12—Ba1—N1^iv	139.25 (10)	C2—C1—Ba1^ii	143.3 (2)
O12^ii—Ba1—N1^iv	73.76 (10)	C6—C2—C3	118.5 (3)
O21^iii—Ba1—N1^iv	123.98 (11)	C6—C2—C1	122.2 (3)
O23—Ba1—N1^iv	78.97 (10)	C3—C2—C1	119.0 (3)
O22—Ba1—N1^iv	73.58 (11)	C2—C6—C5	118.8 (4)
O11^ii—Ba1—N1^iv	71.13 (10)	C2—C6—H6	120.6
O11^i—Ba1—O23^i	66.52 (10)	C5—C6—H6	120.6
O12—Ba1—O23^i	145.37 (9)	N1—C4—C3	122.8 (4)
O12^ii—Ba1—O23^i	115.17 (8)	N1—C4—H4	118.6
O21^iii—Ba1—O23^i	90.72 (9)	C3—C4—H4	118.6
O23—Ba1—O23^i	144.99 (13)	C2—C3—C4	119.1 (4)
O22—Ba1—O23^i	110.95 (9)	C2—C3—H3	120.5
O11^ii—Ba1—O23^i	72.99 (9)	C4—C3—H3	120.5
N1^iv—Ba1—O23^i	69.42 (10)	N1—C5—C6	123.7 (4)
O11^i—Ba1—O21^i	89.70 (10)	N1—C5—H5	118.2
O12—Ba1—O21^i	144.55 (9)	C6—C5—H5	118.2
O12^ii—Ba1—O21^i	144.57 (9)	C5—N1—C4	117.0 (3)
O21^iii—Ba1—O21^i	59.85 (12)	C5—N1—Ba1^vi	123.1 (3)
O23—Ba1—O21^i	113.59 (9)	C4—N1—Ba1^vi	116.7 (3)
O22—Ba1—O21^i	71.48 (9)	O23—N2—O22	119.5 (3)
O11^ii—Ba1—O21^i	113.41 (9)	O23—N2—O21	119.2 (4)
N1^iv—Ba1—O21^i	71.98 (10)	O22—N2—O21	121.2 (4)
O23^i—Ba1—O21^i	42.61 (8)	O23—N2—Ba1	61.0 (2)
O11^i—Ba1—C1^ii	95.72 (10)	O22—N2—Ba1	61.8 (2)
O12—Ba1—C1^ii	88.64 (9)	O21—N2—Ba1	161.1 (3)
O12^ii—Ba1—C1^ii	23.45 (9)	N2—O21—Ba1^iii	115.2 (2)
O21^iii—Ba1—C1^ii	171.80 (10)	N2—O21—Ba1^v	98.4 (2)
O23—Ba1—C1^ii	87.59 (9)	Ba1^iii—O21—Ba1^v	120.15 (12)
O22—Ba1—C1^ii	120.38 (10)	N2—O23—Ba1	97.1 (2)
O11^ii—Ba1—C1^ii	23.48 (9)	N2—O23—Ba1^v	98.9 (2)
N1^iv—Ba1—C1^ii	64.16 (10)	Ba1—O23—Ba1^v	144.99 (13)
O23^i—Ba1—C1^ii	91.79 (9)	N2—O22—Ba1	96.2 (2)
O21^i—Ba1—C1^ii	126.14 (9)
O11^i—Ba1—O12—C1	−134.6 (3)	O23—Ba1—N2—O22	159.4 (4)
O12^ii—Ba1—O12—C1	113.9 (4)	O11^ii—Ba1—N2—O22	126.3 (2)
O21^iii—Ba1—O12—C1	−55.7 (3)	N1^iv—Ba1—N2—O22	72.4 (2)
O23—Ba1—O12—C1	41.4 (3)	O23^i—Ba1—N2—O22	22.7 (3)
O22—Ba1—O12—C1	8.8 (3)	O21^i—Ba1—N2—O22	1.5 (2)
O11^ii—Ba1—O12—C1	151.6 (3)	C1^ii—Ba1—N2—O22	131.0 (2)
N1^iv—Ba1—O12—C1	83.4 (4)	O11^i—Ba1—N2—O21	10.9 (9)
O23^i—Ba1—O12—C1	−139.5 (3)	O12—Ba1—N2—O21	−38.8 (8)
O21^i—Ba1—O12—C1	−61.0 (4)	O12^ii—Ba1—N2—O21	−109.4 (8)
C1^ii—Ba1—O12—C1	129.3 (3)	O21^iii—Ba1—N2—O21	48.1 (9)
N2—Ba1—O12—C1	21.8 (3)	O23—Ba1—N2—O21	−96.1 (9)
O11^i—Ba1—O12—Ba1^ii	111.48 (12)	O22—Ba1—N2—O21	104.5 (9)
O12^ii—Ba1—O12—Ba1^ii	0.0	O11^ii—Ba1—N2—O21	−129.2 (8)
O21^iii—Ba1—O12—Ba1^ii	−169.62 (11)	N1^iv—Ba1—N2—O21	176.9 (9)
O23—Ba1—O12—Ba1^ii	−72.54 (10)	O23^i—Ba1—N2—O21	127.2 (8)
O22—Ba1—O12—Ba1^ii	−105.14 (11)	O21^i—Ba1—N2—O21	106.0 (8)
O11^ii—Ba1—O12—Ba1^ii	37.64 (11)	C1^ii—Ba1—N2—O21	−124.5 (8)
N1^iv—Ba1—O12—Ba1^ii	−30.6 (2)	O23—N2—O21—Ba1^iii	−138.6 (3)
O23^i—Ba1—O12—Ba1^ii	106.57 (15)	O22—N2—O21—Ba1^iii	40.6 (5)
O21^i—Ba1—O12—Ba1^ii	−174.94 (11)	Ba1—N2—O21—Ba1^iii	−53.2 (9)
C1^ii—Ba1—O12—Ba1^ii	15.39 (11)	O23—N2—O21—Ba1^v	−9.6 (4)
N2—Ba1—O12—Ba1^ii	−92.08 (11)	O22—N2—O21—Ba1^v	169.6 (3)
Ba1—O12—C1—O11	−83.8 (5)	Ba1—N2—O21—Ba1^v	75.9 (8)
Ba1^ii—O12—C1—O11	36.4 (4)	O22—N2—O23—Ba1	−20.9 (4)
Ba1—O12—C1—C2	101.2 (4)	O21—N2—O23—Ba1	158.4 (3)
Ba1^ii—O12—C1—C2	−138.5 (3)	O22—N2—O23—Ba1^v	−169.6 (3)
Ba1—O12—C1—Ba1^ii	−120.3 (3)	O21—N2—O23—Ba1^v	9.6 (4)
Ba1^v—O11—C1—O12	78.0 (6)	Ba1—N2—O23—Ba1^v	−148.76 (18)
Ba1^ii—O11—C1—O12	−34.6 (4)	O11^i—Ba1—O23—N2	−110.1 (3)
Ba1^v—O11—C1—C2	−107.0 (5)	O12—Ba1—O23—N2	−117.6 (2)
Ba1^ii—O11—C1—C2	140.3 (3)	O12^ii—Ba1—O23—N2	165.6 (3)
Ba1^v—O11—C1—Ba1^ii	112.7 (4)	O21^iii—Ba1—O23—N2	−34.9 (2)
O12—C1—C2—C6	−167.9 (4)	O22—Ba1—O23—N2	11.1 (2)
O11—C1—C2—C6	16.9 (6)	O11^ii—Ba1—O23—N2	153.4 (2)
Ba1^ii—C1—C2—C6	109.2 (5)	N1^iv—Ba1—O23—N2	88.8 (2)
O12—C1—C2—C3	18.2 (6)	O23^i—Ba1—O23—N2	63.2 (3)
O11—C1—C2—C3	−157.1 (4)	O21^i—Ba1—O23—N2	24.2 (3)
Ba1^ii—C1—C2—C3	−64.7 (6)	C1^ii—Ba1—O23—N2	152.9 (2)
C3—C2—C6—C5	1.8 (6)	O11^i—Ba1—O23—Ba1^v	6.7 (3)
C1—C2—C6—C5	−172.2 (4)	O12—Ba1—O23—Ba1^v	−0.88 (18)
C6—C2—C3—C4	−3.1 (6)	O12^ii—Ba1—O23—Ba1^v	−77.65 (19)
C1—C2—C3—C4	171.1 (4)	O21^iii—Ba1—O23—Ba1^v	81.8 (2)
N1—C4—C3—C2	0.7 (7)	O22—Ba1—O23—Ba1^v	127.8 (3)
C2—C6—C5—N1	2.1 (7)	O11^ii—Ba1—O23—Ba1^v	−89.8 (2)
C6—C5—N1—C4	−4.4 (7)	N1^iv—Ba1—O23—Ba1^v	−154.5 (2)
C6—C5—N1—Ba1^vi	154.9 (4)	O23^i—Ba1—O23—Ba1^v	180.0
C3—C4—N1—C5	3.0 (7)	O21^i—Ba1—O23—Ba1^v	140.93 (18)
C3—C4—N1—Ba1^vi	−157.6 (4)	C1^ii—Ba1—O23—Ba1^v	−90.3 (2)
O11^i—Ba1—N2—O23	106.9 (3)	N2—Ba1—O23—Ba1^v	116.8 (3)
O12—Ba1—N2—O23	57.3 (2)	O23—N2—O22—Ba1	20.7 (4)
O12^ii—Ba1—N2—O23	−13.3 (2)	O21—N2—O22—Ba1	−158.5 (3)
O21^iii—Ba1—N2—O23	144.1 (2)	O11^i—Ba1—O22—N2	119.4 (2)
O22—Ba1—N2—O23	−159.4 (4)	O12—Ba1—O22—N2	36.6 (2)
O11^ii—Ba1—N2—O23	−33.1 (3)	O12^ii—Ba1—O22—N2	−35.7 (3)
N1^iv—Ba1—N2—O23	−87.0 (2)	O21^iii—Ba1—O22—N2	117.1 (3)
O23^i—Ba1—N2—O23	−136.8 (3)	O23—Ba1—O22—N2	−11.1 (2)
O21^i—Ba1—N2—O23	−157.9 (2)	O11^ii—Ba1—O22—N2	−73.8 (3)
C1^ii—Ba1—N2—O23	−28.4 (2)	N1^iv—Ba1—O22—N2	−102.4 (2)
O11^i—Ba1—N2—O22	−93.6 (3)	O23^i—Ba1—O22—N2	−162.0 (2)
O12—Ba1—N2—O22	−143.3 (2)	O21^i—Ba1—O22—N2	−178.4 (3)
O12^ii—Ba1—N2—O22	146.1 (2)	C1^ii—Ba1—O22—N2	−56.8 (3)
O21^iii—Ba1—N2—O22	−56.5 (2)

Symmetry codes: (i) x+1, y, z; (ii) −x, −y, −z; (iii) −x, −y+1, −z; (iv) x+1, y, z+1; (v) x−1, y, z; (vi) x−1, y, z−1.