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The eight-coordinate ZrIV atom in the title compound, (C3H12N2)[Zr(SO4)3(H2O)3], has an approximate square-anti­prismatic coordination geometry. In the dianion, one of the sulfate groups is unidentate whereas the other two chelate the metal atom. In the crystal strucure, cations and anions are linked into a three-dimensional network architecture by hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806047672/lh2241sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806047672/lh2241Isup2.hkl
Contains datablock I

CCDC reference: 630098

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](N-C) = 0.007 Å
  • Disorder in solvent or counterion
  • R factor = 0.038
  • wR factor = 0.122
  • Data-to-parameter ratio = 13.6

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT242_ALERT_2_C Check Low Ueq as Compared to Neighbors for S3 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C3 PLAT243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C3' PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N2 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 29.00 Perc. PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 16
Alert level G FORMU01_ALERT_1_G There is a discrepancy between the atom counts in the _chemical_formula_sum and _chemical_formula_moiety. This is usually due to the moiety formula being in the wrong format. Atom count from _chemical_formula_sum: C3 H18 N2 O15 S3 Zr1 Atom count from _chemical_formula_moiety:
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 1 ALERT level G = General alerts; check 2 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 0 ALERT type 3 Indicator that the structure quality may be low 5 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Bruker, 2003); cell refinement: SAINT (Bruker, 2003); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: X-SEED (Barbour, 2001); software used to prepare material for publication: publCIF (Westrip, 2006).

(I) top
Crystal data top
(C3H12N2)[Zr(SO4)3(H2O)3]F(000) = 1032
Mr = 509.59Dx = 2.160 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 3634 reflections
a = 7.9124 (5) Åθ = 2.4–28.4°
b = 20.464 (1) ŵ = 1.18 mm1
c = 10.4195 (7) ÅT = 295 K
β = 111.727 (1)°Block, colorless
V = 1567.26 (16) Å30.16 × 0.14 × 0.09 mm
Z = 4
Data collection top
Bruker APEX area-detector
diffractometer
3532 independent reflections
Radiation source: fine-focus sealed tube3079 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.034
φ and ω scansθmax = 27.5°, θmin = 2.0°
Absorption correction: multi-scan
SADABS (Sheldrick, 1996)
h = 910
Tmin = 0.833, Tmax = 0.901k = 2610
8512 measured reflectionsl = 1313
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.038Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.122H atoms treated by a mixture of independent and constrained refinement
S = 1.14 w = 1/[σ2(Fo2) + (0.0601P)2 + 2.5754P]
where P = (Fo2 + 2Fc2)/3
3532 reflections(Δ/σ)max = 0.001
260 parametersΔρmax = 0.77 e Å3
30 restraintsΔρmin = 0.63 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Zr10.38179 (5)0.452032 (18)0.22355 (4)0.01721 (14)
S10.42897 (14)0.33109 (5)0.36724 (11)0.0247 (2)
S20.77173 (13)0.46493 (5)0.30988 (10)0.0213 (2)
S30.33649 (14)0.61484 (5)0.12587 (10)0.0226 (2)
O10.3456 (4)0.34326 (15)0.2140 (3)0.0293 (7)
O20.4558 (4)0.40149 (15)0.4166 (3)0.0273 (7)
O30.6001 (5)0.29773 (17)0.4014 (4)0.0402 (8)
O40.3069 (5)0.29846 (17)0.4202 (4)0.0410 (8)
O50.6347 (4)0.42140 (15)0.2057 (3)0.0255 (6)
O60.6468 (4)0.50364 (14)0.3611 (3)0.0236 (6)
O70.9042 (5)0.42775 (17)0.4172 (4)0.0392 (8)
O80.8547 (4)0.50903 (16)0.2397 (3)0.0277 (7)
O90.3458 (5)0.54112 (14)0.1172 (3)0.0289 (7)
O100.4852 (5)0.64178 (17)0.0921 (4)0.0443 (9)
O110.1628 (5)0.63582 (17)0.0278 (4)0.0442 (9)
O120.3620 (5)0.63221 (17)0.2671 (3)0.0398 (8)
O1W0.3017 (4)0.42292 (16)0.0050 (3)0.0280 (7)
H1w10.268 (6)0.4560 (15)0.047 (4)0.034*
H1w20.386 (5)0.4030 (19)0.011 (5)0.034*
O2W0.2970 (4)0.51707 (15)0.3571 (3)0.0245 (6)
H2w10.314 (6)0.5098 (18)0.4408 (17)0.029*
H2w20.305 (7)0.5575 (7)0.343 (4)0.029*
O3W0.0879 (4)0.44305 (17)0.1527 (3)0.0310 (7)
H3w10.024 (5)0.466 (2)0.186 (4)0.037*
H3w20.017 (5)0.422 (2)0.083 (3)0.037*
N10.7089 (5)0.2301 (2)0.6655 (4)0.0364 (9)
H1n10.661 (6)0.2072 (18)0.713 (4)0.044*
H1n20.691 (7)0.2088 (18)0.590 (3)0.044*
H1n30.646 (6)0.2657 (13)0.643 (4)0.044*
N21.1902 (6)0.3570 (2)0.6203 (4)0.0390 (10)
H2n11.235 (6)0.338 (2)0.567 (4)0.047*
H2n21.272 (5)0.377 (2)0.683 (4)0.047*
H2n31.107 (5)0.3834 (19)0.572 (4)0.047*
C10.9053 (6)0.2396 (3)0.7371 (6)0.0496 (14)
H1a0.96640.19770.76030.059*
H1b0.92940.26400.82190.059*
C20.9747 (11)0.2779 (4)0.6385 (7)0.049 (2)0.66 (1)
H2a1.01830.24720.58670.059*0.66 (1)
H2b0.87470.30230.57310.059*0.66 (1)
C31.1217 (14)0.3231 (4)0.7135 (9)0.062 (3)0.66 (1)
H3a1.07700.35480.76250.074*0.66 (1)
H3b1.22010.29900.78110.074*0.66 (1)
C2'0.999 (2)0.3011 (6)0.7327 (15)0.049 (2)0.34 (1)
H2'c1.09250.30930.82250.059*0.34 (1)
H2'd0.91230.33680.71180.059*0.34 (1)
C3'1.083 (3)0.2983 (7)0.6255 (19)0.062 (3)0.34 (1)
H3'c1.16190.26030.64340.074*0.34 (1)
H3'd0.98720.29230.53570.074*0.34 (1)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Zr10.0185 (2)0.0181 (2)0.0156 (2)0.00142 (14)0.00705 (15)0.00090 (14)
S10.0306 (5)0.0215 (5)0.0227 (5)0.0024 (4)0.0106 (4)0.0016 (4)
S20.0184 (5)0.0249 (5)0.0207 (5)0.0030 (4)0.0076 (4)0.0018 (4)
S30.0267 (5)0.0206 (5)0.0194 (5)0.0033 (4)0.0072 (4)0.0005 (4)
O10.0378 (17)0.0236 (16)0.0217 (15)0.0016 (13)0.0054 (13)0.0001 (12)
O20.0360 (16)0.0248 (15)0.0184 (14)0.0041 (13)0.0071 (12)0.0011 (12)
O30.0435 (19)0.0370 (19)0.042 (2)0.0160 (16)0.0179 (16)0.0113 (16)
O40.051 (2)0.040 (2)0.040 (2)0.0134 (17)0.0250 (17)0.0009 (16)
O50.0215 (14)0.0325 (17)0.0202 (15)0.0022 (12)0.0051 (11)0.0080 (12)
O60.0240 (14)0.0250 (15)0.0256 (15)0.0002 (12)0.0134 (12)0.0034 (12)
O70.0313 (17)0.0399 (19)0.042 (2)0.0093 (16)0.0078 (15)0.0130 (17)
O80.0221 (14)0.0359 (18)0.0253 (15)0.0014 (13)0.0091 (12)0.0042 (13)
O90.0436 (19)0.0192 (15)0.0281 (16)0.0033 (13)0.0182 (14)0.0018 (12)
O100.053 (2)0.0282 (18)0.065 (2)0.0063 (17)0.038 (2)0.0060 (17)
O110.0398 (19)0.0334 (19)0.041 (2)0.0133 (16)0.0060 (16)0.0032 (16)
O120.069 (2)0.0280 (17)0.0233 (16)0.0068 (17)0.0184 (16)0.0007 (14)
O1w0.0332 (16)0.0279 (17)0.0249 (16)0.0081 (13)0.0130 (13)0.0017 (13)
O2w0.0299 (15)0.0252 (15)0.0204 (14)0.0006 (13)0.0115 (12)0.0013 (12)
O3w0.0183 (14)0.045 (2)0.0253 (16)0.0006 (13)0.0037 (12)0.0139 (14)
N10.041 (2)0.037 (2)0.034 (2)0.0071 (19)0.0166 (19)0.0014 (18)
N20.032 (2)0.044 (3)0.035 (2)0.0045 (19)0.0052 (18)0.003 (2)
C10.034 (3)0.060 (4)0.050 (3)0.002 (3)0.011 (3)0.002 (3)
C20.048 (4)0.066 (6)0.031 (4)0.022 (4)0.012 (3)0.004 (4)
C30.104 (8)0.041 (5)0.052 (5)0.016 (5)0.043 (6)0.000 (4)
C2'0.048 (4)0.066 (6)0.031 (4)0.022 (4)0.012 (3)0.004 (4)
C3'0.104 (8)0.041 (5)0.052 (5)0.016 (5)0.043 (6)0.000 (4)
Geometric parameters (Å, º) top
Zr1—O12.242 (3)O3w—H3w20.86 (3)
Zr1—O22.142 (3)N1—C11.467 (5)
Zr1—O52.170 (3)N1—H1n10.86 (2)
Zr1—O62.311 (3)N1—H1n20.86 (2)
Zr1—O92.097 (3)N1—H1n30.87 (2)
Zr1—O1w2.207 (3)N2—C31.452 (7)
Zr1—O2w2.202 (3)N2—C3'1.484 (8)
Zr1—O3w2.171 (3)N2—H2n10.86 (2)
S1—O31.438 (3)N2—H2n20.84 (2)
S1—O41.442 (3)N2—H2n30.86 (2)
S1—O11.505 (3)C1—C2'1.468 (9)
S1—O21.518 (3)C1—C21.546 (7)
S2—O71.435 (3)C1—H1A0.9700
S2—O81.462 (3)C1—H1B0.9700
S2—O51.509 (3)C2—C31.465 (8)
S2—O61.510 (3)C2—H2A0.9700
S3—O111.441 (3)C2—H2B0.9700
S3—O121.454 (3)C3—H3A0.9700
S3—O101.455 (4)C3—H3B0.9700
S3—O91.515 (3)C2'—C3'1.499 (9)
O1w—H1w10.85 (3)C2'—H2'C0.9700
O1w—H1w20.85 (3)C2'—H2'D0.9700
O2w—H2w10.85 (3)C3'—H3'C0.9700
O2w—H2w20.85 (3)C3'—H3'D0.9700
O3w—H3w10.85 (3)
O1—Zr1—O263.1 (1)Zr1—O1w—H1w2113 (3)
O1—Zr1—O579.4 (1)H1w1—O1w—H1w2110 (4)
O1—Zr1—O6123.6 (1)Zr1—O2w—H2w1125 (3)
O1—Zr1—O9148.2 (1)Zr1—O2w—H2w2115 (3)
O1—Zr1—O1w72.7 (1)H2w1—O2w—H2w2111 (4)
O1—Zr1—O2w124.4 (1)Zr1—O3w—H3w1122 (3)
O1—Zr1—O3w78.3 (1)Zr1—O3w—H3w2128 (3)
O2—Zr1—O590.1 (1)H3w1—O3w—H3w2109 (4)
O2—Zr1—O676.6 (1)C1—N1—H1n1113 (3)
O2—Zr1—O9148.5 (1)C1—N1—H1n2109 (3)
O2—Zr1—O1w135.5 (1)H1n1—N1—H1n2107 (2)
O2—Zr1—O2w74.9 (1)C1—N1—H1n3115 (3)
O2—Zr1—O3w99.5 (1)H1n1—N1—H1n3107 (2)
O5—Zr1—O662.1 (1)H1n2—N1—H1n3107 (2)
O5—Zr1—O998.9 (1)C3—N2—H2n1124 (4)
O5—Zr1—O1w75.8 (1)C3'—N2—H2n2131 (4)
O5—Zr1—O2w137.3 (1)H2n1—N2—H2n2110 (2)
O5—Zr1—O3w148.4 (1)C3—N2—H2n3107 (4)
O6—Zr1—O981.1 (1)C3'—N2—H2n3102 (4)
O6—Zr1—O1w127.7 (1)H2n1—N2—H2n3109 (2)
O6—Zr1—O2w75.6 (1)H2n2—N2—H2n3110 (2)
O6—Zr1—O3w149.4 (1)N1—C1—C2107.4 (5)
O9—Zr1—O1w76.0 (1)C2'—C1—H1A123.7
O9—Zr1—O2w78.2 (1)N1—C1—H1A110.2
O9—Zr1—O3w88.6 (1)C2—C1—H1A110.2
O1w—Zr1—O2w141.0 (1)N1—C1—H1B110.2
O1w—Zr1—O3w76.3 (1)C2—C1—H1B110.2
O2w—Zr1—O3w74.2 (1)H1A—C1—H1B108.5
O3—S1—O4112.8 (2)C3—C2—C1111.9 (5)
O3—S1—O1110.1 (2)C3—C2—H2A109.2
O4—S1—O1113.0 (2)C1—C2—H2A109.2
O3—S1—O2111.5 (2)C3—C2—H2B109.2
O4—S1—O2109.8 (2)C1—C2—H2B109.2
O1—S1—O298.85 (17)H2A—C2—H2B107.9
O7—S2—O8112.56 (19)N2—C3—C2111.4 (6)
O7—S2—O5111.8 (2)N2—C3—H3A109.3
O8—S2—O5109.93 (18)C2—C3—H3A109.3
O7—S2—O6112.77 (19)N2—C3—H3B109.3
O8—S2—O6109.10 (18)C2—C3—H3B109.3
O5—S2—O6100.01 (16)H3A—C3—H3B108.0
O11—S3—O12112.6 (2)C1—C2'—C3'111.0 (8)
O11—S3—O10111.1 (2)C1—C2'—H2'C109.4
O12—S3—O10109.3 (2)C3'—C2'—H2'C109.4
O11—S3—O9108.0 (2)C1—C2'—H2'D109.4
O12—S3—O9108.20 (18)C3'—C2'—H2'D109.4
O10—S3—O9107.5 (2)H2'C—C2'—H2'D108.0
S1—O1—Zr196.82 (15)N2—C3'—C2'114.5 (9)
S1—O2—Zr1100.64 (15)N2—C3'—H3'C108.6
S2—O5—Zr1101.99 (15)C2'—C3'—H3'C108.6
S2—O6—Zr195.93 (14)N2—C3'—H3'D108.6
S3—O9—Zr1146.54 (19)C2'—C3'—H3'D108.6
Zr1—O1w—H1w1111 (3)H3'C—C3'—H3'D107.6
O3—S1—O1—Zr1110.50 (19)O1—Zr1—O5—S2136.92 (17)
O4—S1—O1—Zr1122.35 (19)O6—Zr1—O5—S20.46 (13)
O2—S1—O1—Zr16.34 (18)O7—S2—O6—Zr1118.25 (18)
O9—Zr1—O1—S1179.63 (18)O8—S2—O6—Zr1115.89 (15)
O2—Zr1—O1—S14.97 (14)O5—S2—O6—Zr10.59 (16)
O3w—Zr1—O1—S1111.99 (18)O9—Zr1—O6—S2105.57 (15)
O5—Zr1—O1—S190.54 (16)O2—Zr1—O6—S296.86 (15)
O2w—Zr1—O1—S150.5 (2)O3w—Zr1—O6—S2177.20 (19)
O1w—Zr1—O1—S1168.86 (19)O5—Zr1—O6—S20.46 (13)
O6—Zr1—O1—S144.7 (2)O2w—Zr1—O6—S2174.44 (16)
O3—S1—O2—Zr1109.09 (19)O1w—Zr1—O6—S241.0 (2)
O4—S1—O2—Zr1125.11 (19)O1—Zr1—O6—S252.54 (18)
O1—S1—O2—Zr16.70 (19)S1—Zr1—O6—S274.51 (13)
O9—Zr1—O2—S1179.59 (18)O11—S3—O9—Zr1122.6 (4)
O3w—Zr1—O2—S176.67 (17)O12—S3—O9—Zr10.5 (5)
O5—Zr1—O2—S173.09 (16)O10—S3—O9—Zr1117.4 (4)
O2w—Zr1—O2—S1147.34 (18)O2—Zr1—O9—S310.1 (6)
O1w—Zr1—O2—S13.4 (3)O3w—Zr1—O9—S395.8 (4)
O1—Zr1—O2—S14.98 (14)O5—Zr1—O9—S3115.0 (4)
O6—Zr1—O2—S1134.28 (17)O2w—Zr1—O9—S321.6 (4)
O7—S2—O5—Zr1118.94 (19)O1w—Zr1—O9—S3172.1 (4)
O8—S2—O5—Zr1115.31 (17)O1—Zr1—O9—S3160.7 (3)
O6—S2—O5—Zr10.64 (18)O6—Zr1—O9—S355.4 (4)
O9—Zr1—O5—S275.35 (17)N1—C1—C2—C3145.1 (8)
O2—Zr1—O5—S274.31 (16)C1—C2—C3—N2177.9 (7)
O3w—Zr1—O5—S2177.31 (19)N1—C1—C2'—C3'97.3 (15)
O2w—Zr1—O5—S26.8 (3)C1—C2'—C3'—N2176.3 (13)
O1w—Zr1—O5—S2148.40 (18)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1w—H1w1···O8i0.85 (3)2.01 (3)2.763 (4)148 (5)
O1w—H1w2···O10i0.85 (3)1.80 (2)2.624 (5)164 (5)
O2w—H2w1···O6ii0.85 (2)1.99 (1)2.834 (4)178 (4)
O2w—H2w2···O120.85 (3)1.85 (2)2.656 (5)158 (4)
O3w—H3w1···O8iii0.85 (3)1.85 (4)2.700 (4)171 (4)
O3w—H3w2···O11iv0.85 (3)1.88 (2)2.705 (5)162 (5)
N1—H1n1···O3v0.86 (2)2.19 (3)2.945 (6)146 (4)
N1—H1n2···O10vi0.86 (2)2.34 (3)3.126 (6)152 (4)
N1—H1n3···O12ii0.87 (2)2.30 (3)3.007 (6)139 (4)
N2—H2n1···O4vii0.86 (2)1.99 (2)2.839 (6)172 (4)
N2—H2n2···O6viii0.84 (2)2.60 (5)3.106 (5)120 (4)
N2—H2n3···O70.86 (2)2.02 (2)2.855 (5)164 (4)
Symmetry codes: (i) x+1, y+1, z; (ii) x+1, y+1, z+1; (iii) x1, y, z; (iv) x, y+1, z; (v) x, y+1/2, z+1/2; (vi) x+1, y1/2, z+1/2; (vii) x+1, y, z; (viii) x+2, y+1, z+1.
 

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