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The crystal structure of the title compound, (C6H5CH2NH3)4[Cu(NO3)4](NO3)2, consists of alternating organic and inorganic layers. The aromatic groups constitute the organic layer, while the nitrate ions, ammonium groups and [Cu(NO3)4]2− anions form the inorganic layer; the complex anions lie on twofold rotation axes. Strong classical N—H...O hydrogen bonds in the inorganic layer result in a complex two-dimensional hydrogen-bonding network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806000201/is2001sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806000201/is2001Isup2.hkl
Contains datablock I

CCDC reference: 298470

Key indicators

  • Single-crystal X-ray study
  • T = 295 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.043
  • wR factor = 0.127
  • Data-to-parameter ratio = 23.0

checkCIF/PLATON results

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Alert level A DIFF019_ALERT_1_A _diffrn_standards_number is missing Number of standards used in measurement. DIFF020_ALERT_1_A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards.
Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Cu1 - O4 .. 6.72 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O2 PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for O5 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N5 PLAT480_ALERT_4_C Long H...A H-Bond Reported H1B .. N5 .. 2.66 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H1C .. N5 .. 2.65 Ang. PLAT480_ALERT_4_C Long H...A H-Bond Reported H2C .. O3 .. 2.65 Ang. PLAT790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C7 H10 N
2 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 9 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 3 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

Computing details top

Data collection: CrysAlis CCD (Oxford Diffraction, 2003); cell refinement: CrysAlis CCD; data reduction: CrysAlis RED (Oxford Diffraction, 2003); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2003); software used to prepare material for publication: PLATON (Spek, 2003) and WinGX (Farrugia, 1999).

Tetrakis(benzylammonium) tetranitratocuprate(II) dinitrate top
Crystal data top
(C7H10N)4[Cu(NO4)3](NO3)2F(000) = 1804
Mr = 868.24Dx = 1.545 Mg m3
Monoclinic, C2/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2ycCell parameters from 476 reflections
a = 30.79 (3) Åθ = 2–31°
b = 5.749 (9) ŵ = 0.68 mm1
c = 21.293 (14) ÅT = 295 K
β = 97.93 (7)°Block, blue
V = 3733 (7) Å30.50 × 0.50 × 0.50 mm
Z = 4
Data collection top
Oxford Excalibur2
diffractometer
5929 independent reflections
Radiation source: fine-focus sealed tube4603 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.031
ω/2θ scansθmax = 32.0°, θmin = 4.4°
Absorption correction: multi-scan
(Blessing, 1995)
h = 4445
Tmin = 0.714, Tmax = 0.714k = 85
17698 measured reflectionsl = 3031
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)] = 0.043Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.127H-atom parameters constrained
S = 1.08 w = 1/[σ2(Fo2) + (0.071P)2 + 0.4182P]
where P = (Fo2 + 2Fc2)/3
5929 reflections(Δ/σ)max = 0.001
258 parametersΔρmax = 0.44 e Å3
0 restraintsΔρmin = 0.74 e Å3
Special details top

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 (Å2) top
xyzUiso*/Ueq
O10.00078 (4)0.51036 (19)0.84279 (5)0.0355 (3)
O40.06425 (4)0.4501 (2)0.73340 (6)0.0375 (3)
C70.22386 (7)0.0182 (3)0.69590 (10)0.0456 (4)
H70.21950.11290.71980.055*
N40.08162 (5)0.6563 (3)0.73080 (6)0.0351 (3)
O60.12115 (4)0.6739 (3)0.71617 (7)0.0534 (4)
O50.05672 (5)0.8235 (2)0.74217 (7)0.0485 (3)
C60.26161 (7)0.0378 (4)0.66773 (11)0.0548 (5)
H60.28250.08020.67290.066*
C90.11423 (5)0.0697 (3)0.55755 (8)0.0365 (3)
N10.11133 (5)0.1578 (3)0.68094 (8)0.0439 (3)
H1A0.08940.15020.70400.066*
H1B0.11170.02910.65780.066*
H1C0.10760.28100.65540.066*
C20.19256 (5)0.1928 (3)0.68870 (8)0.0361 (3)
C30.19970 (6)0.3858 (3)0.65233 (10)0.0463 (4)
H30.17890.50420.64690.056*
C140.11807 (6)0.1150 (4)0.59834 (9)0.0425 (4)
H140.09810.13040.63510.051*
C130.15124 (7)0.2761 (4)0.58474 (11)0.0515 (5)
H130.15360.39930.61240.062*
C10.15359 (6)0.1795 (4)0.72360 (9)0.0462 (4)
H1D0.15700.04670.75200.055*
H1E0.15270.31830.74930.055*
C40.23723 (7)0.4035 (4)0.62421 (11)0.0542 (5)
H40.24150.53310.59970.065*
N20.04000 (4)0.1950 (3)0.53864 (7)0.0360 (3)
H2A0.01920.30090.54950.054*
H2B0.02940.05400.54880.054*
H2C0.04870.20200.49700.054*
C80.07757 (6)0.2415 (4)0.57272 (10)0.0489 (5)
H8A0.06760.23810.61800.059*
H8B0.08860.39650.56200.059*
C50.26852 (7)0.2301 (4)0.63217 (11)0.0547 (5)
H50.29400.24330.61360.066*
O30.01356 (4)0.2967 (2)0.92662 (6)0.0437 (3)
N30.00426 (4)0.3077 (2)0.86831 (6)0.0314 (3)
O20.00023 (5)0.1350 (2)0.83423 (7)0.0555 (4)
C100.14412 (7)0.0906 (4)0.50340 (10)0.0503 (5)
H100.14210.21480.47600.060*
C120.18063 (7)0.2548 (4)0.53067 (12)0.0587 (5)
H120.20300.36350.52160.070*
C110.17716 (7)0.0723 (5)0.48965 (11)0.0628 (6)
H110.19700.05870.45270.075*
O70.10816 (5)0.6966 (3)0.63794 (7)0.0547 (4)
N50.08195 (5)0.6599 (3)0.58950 (7)0.0379 (3)
O80.05945 (5)0.8189 (3)0.56389 (8)0.0698 (5)
O90.07946 (7)0.4542 (3)0.57094 (10)0.0735 (5)
Cu10.00000.48583 (5)0.75000.03026 (9)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
O10.0433 (6)0.0361 (6)0.0272 (5)0.0026 (5)0.0054 (4)0.0024 (4)
O40.0309 (6)0.0406 (6)0.0409 (6)0.0003 (5)0.0050 (5)0.0015 (5)
C70.0494 (10)0.0420 (10)0.0444 (10)0.0084 (8)0.0034 (8)0.0041 (7)
N40.0327 (6)0.0432 (8)0.0294 (6)0.0018 (6)0.0049 (5)0.0023 (5)
O60.0312 (6)0.0639 (9)0.0634 (9)0.0088 (6)0.0002 (6)0.0047 (7)
O50.0476 (7)0.0444 (7)0.0540 (8)0.0098 (6)0.0089 (6)0.0001 (6)
C60.0444 (10)0.0609 (12)0.0582 (12)0.0221 (9)0.0043 (9)0.0006 (10)
C90.0320 (7)0.0415 (8)0.0374 (8)0.0034 (7)0.0100 (6)0.0067 (7)
N10.0336 (7)0.0491 (9)0.0498 (9)0.0013 (6)0.0091 (6)0.0082 (7)
C20.0328 (8)0.0366 (8)0.0376 (8)0.0001 (6)0.0001 (6)0.0054 (6)
C30.0373 (9)0.0365 (9)0.0652 (12)0.0074 (7)0.0073 (8)0.0056 (8)
C140.0357 (8)0.0550 (11)0.0373 (9)0.0023 (8)0.0066 (6)0.0052 (8)
C130.0469 (10)0.0485 (11)0.0625 (13)0.0004 (9)0.0196 (9)0.0119 (9)
C10.0402 (9)0.0573 (11)0.0414 (9)0.0031 (8)0.0061 (7)0.0079 (8)
C40.0483 (11)0.0510 (11)0.0648 (13)0.0024 (9)0.0135 (9)0.0113 (10)
N20.0326 (7)0.0380 (7)0.0378 (7)0.0039 (5)0.0057 (5)0.0002 (6)
C80.0434 (9)0.0536 (11)0.0533 (11)0.0120 (8)0.0197 (8)0.0215 (9)
C50.0384 (9)0.0713 (14)0.0557 (12)0.0047 (9)0.0115 (8)0.0014 (10)
O30.0514 (7)0.0517 (7)0.0266 (6)0.0010 (6)0.0005 (5)0.0058 (5)
N30.0271 (6)0.0369 (7)0.0298 (6)0.0019 (5)0.0033 (5)0.0006 (5)
O20.0792 (10)0.0375 (7)0.0477 (8)0.0040 (7)0.0016 (7)0.0110 (6)
C100.0479 (10)0.0572 (11)0.0445 (10)0.0062 (9)0.0012 (8)0.0116 (9)
C120.0422 (10)0.0636 (13)0.0709 (14)0.0184 (10)0.0101 (9)0.0058 (11)
C110.0461 (11)0.0876 (16)0.0505 (12)0.0155 (12)0.0082 (9)0.0040 (12)
O70.0492 (8)0.0581 (8)0.0510 (8)0.0108 (6)0.0132 (6)0.0128 (7)
N50.0321 (7)0.0490 (8)0.0329 (7)0.0028 (6)0.0051 (5)0.0028 (6)
O80.0501 (9)0.0942 (13)0.0633 (10)0.0146 (8)0.0017 (7)0.0354 (9)
O90.0771 (12)0.0688 (10)0.0764 (12)0.0181 (9)0.0165 (9)0.0363 (9)
Cu10.02681 (14)0.03910 (17)0.02504 (14)0.0000.00415 (9)0.000
Geometric parameters (Å, º) top
O1—N31.286 (2)C13—H130.9300
O1—Cu11.9841 (18)C1—H1D0.9700
O4—N41.299 (2)C1—H1E0.9700
O4—Cu11.972 (2)C4—C51.380 (3)
C7—C61.384 (3)C4—H40.9300
C7—C21.385 (3)N2—C81.472 (2)
C7—H70.9300N2—H2A0.8900
N4—O61.218 (2)N2—H2B0.8900
N4—O51.233 (2)N2—H2C0.8900
C6—C51.373 (4)C8—H8A0.9700
C6—H60.9300C8—H8B0.9700
C9—C101.378 (3)C5—H50.9300
C9—C141.387 (3)O3—N31.2366 (19)
C9—C81.501 (3)N3—O21.226 (2)
N1—C11.486 (3)C10—C111.384 (3)
N1—H1A0.8900C10—H100.9300
N1—H1B0.8900C12—C111.378 (4)
N1—H1C0.8900C12—H120.9300
C2—C31.388 (3)C11—H110.9300
C2—C11.498 (3)O7—N51.237 (2)
C3—C41.377 (3)N5—O81.228 (2)
C3—H30.9300N5—O91.246 (3)
C14—C131.379 (3)Cu1—O4i1.972 (2)
C14—H140.9300Cu1—O1i1.9842 (17)
C13—C121.368 (3)
N3—O1—Cu1109.82 (10)C3—C4—H4119.8
N4—O4—Cu1108.04 (11)C5—C4—H4119.8
C6—C7—C2120.41 (19)C8—N2—H2A109.5
C6—C7—H7119.8C8—N2—H2B109.5
C2—C7—H7119.8H2A—N2—H2B109.5
O6—N4—O5123.92 (17)C8—N2—H2C109.5
O6—N4—O4118.53 (15)H2A—N2—H2C109.5
O5—N4—O4117.53 (16)H2B—N2—H2C109.5
C5—C6—C7120.49 (18)N2—C8—C9113.14 (15)
C5—C6—H6119.8N2—C8—H8A109.0
C7—C6—H6119.8C9—C8—H8A109.0
C10—C9—C14119.09 (17)N2—C8—H8B109.0
C10—C9—C8121.21 (19)C9—C8—H8B109.0
C14—C9—C8119.70 (18)H8A—C8—H8B107.8
C1—N1—H1A109.5C6—C5—C4119.4 (2)
C1—N1—H1B109.5C6—C5—H5120.3
H1A—N1—H1B109.5C4—C5—H5120.3
C1—N1—H1C109.5O2—N3—O3122.94 (15)
H1A—N1—H1C109.5O2—N3—O1119.15 (15)
H1B—N1—H1C109.5O3—N3—O1117.91 (14)
C7—C2—C3118.66 (19)C9—C10—C11120.3 (2)
C7—C2—C1120.05 (18)C9—C10—H10119.9
C3—C2—C1121.14 (17)C11—C10—H10119.9
C4—C3—C2120.58 (18)C13—C12—C11120.1 (2)
C4—C3—H3119.7C13—C12—H12120.0
C2—C3—H3119.7C11—C12—H12120.0
C13—C14—C9120.46 (19)C12—C11—C10120.0 (2)
C13—C14—H14119.8C12—C11—H11120.0
C9—C14—H14119.8C10—C11—H11120.0
C12—C13—C14120.1 (2)O8—N5—O7120.45 (18)
C12—C13—H13120.0O8—N5—O9124.0 (2)
C14—C13—H13120.0O7—N5—O9115.50 (17)
N1—C1—C2113.24 (16)O4—Cu1—O4i168.04 (8)
N1—C1—H1D108.9O4—Cu1—O192.07 (8)
C2—C1—H1D108.9O4i—Cu1—O188.77 (8)
N1—C1—H1E108.9O4—Cu1—O1i88.77 (8)
C2—C1—H1E108.9O4i—Cu1—O1i92.07 (8)
H1D—C1—H1E107.7O1—Cu1—O1i171.85 (7)
C3—C4—C5120.4 (2)
Cu1—O4—N4—O6174.55 (12)C7—C6—C5—C40.6 (4)
Cu1—O4—N4—O54.01 (16)C3—C4—C5—C60.9 (4)
C2—C7—C6—C50.1 (3)Cu1—O1—N3—O213.76 (18)
C6—C7—C2—C30.5 (3)Cu1—O1—N3—O3165.38 (11)
C6—C7—C2—C1175.03 (19)C14—C9—C10—C110.8 (3)
C7—C2—C3—C40.2 (3)C8—C9—C10—C11178.7 (2)
C1—C2—C3—C4175.28 (19)C14—C13—C12—C110.0 (3)
C10—C9—C14—C130.3 (3)C13—C12—C11—C100.5 (4)
C8—C9—C14—C13179.22 (17)C9—C10—C11—C120.9 (4)
C9—C14—C13—C120.1 (3)N4—O4—Cu1—O4i178.14 (10)
C7—C2—C1—N1115.8 (2)N4—O4—Cu1—O184.25 (10)
C3—C2—C1—N168.7 (2)N4—O4—Cu1—O1i87.64 (10)
C2—C3—C4—C50.5 (3)N3—O1—Cu1—O491.75 (10)
C10—C9—C8—N281.2 (3)N3—O1—Cu1—O4i76.32 (10)
C14—C9—C8—N298.3 (2)
Symmetry code: (i) x, y, z+3/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O4i0.892.372.997 (3)127
N1—H1A···O5ii0.892.483.156 (3)133
N1—H1B···O7iii0.891.962.803 (4)158
N1—H1B···N5iii0.892.663.509 (4)159
N1—H1C···O90.892.132.953 (4)153
N1—H1C···O70.892.423.228 (5)151
N1—H1C···N50.892.653.530 (4)169
N2—H2A···O3ii0.892.373.096 (5)139
N2—H2A···O8iii0.892.503.036 (4)120
N2—H2A···O1ii0.892.543.154 (3)127
N2—H2B···O3i0.892.123.006 (4)172
N2—H2C···O9iv0.892.172.891 (3)138
N2—H2C···O8v0.892.553.072 (3)118
N2—H2C···O3vi0.892.653.136 (3)116
Symmetry codes: (i) x, y, z+3/2; (ii) x, y1, z+3/2; (iii) x, y1, z; (iv) x, y, z+1; (v) x, y+1, z+1; (vi) x, y, z1/2.
 

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