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In the title organic–inorganic salt, [CrCl2(tn)2]2[Cr2O7] (tn is propane-1,3-di­amine), the CrIII ions are coordinated by four N atoms from two tn ligands and two chloride ions in a trans geometry, displaying a distorted octa­hedral arrangement. The crystal packing is stabilized by N—H...Cl and N—H...O hydrogen bonds.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S2056989016012755/wm5308sup1.cif
Contains datablock I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S2056989016012755/wm5308Isup2.hkl
Contains datablock I

CCDC reference: 1498083

Key indicators

  • Single-crystal synchrotron study
  • T = 253 K
  • Mean [sigma](C-C) = 0.004 Å
  • Disorder in main residue
  • R factor = 0.037
  • wR factor = 0.105
  • Data-to-parameter ratio = 17.9

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full value Low . 0.961 Note PLAT213_ALERT_2_C Atom O3SA has ADP max/min Ratio ..... 3.3 prolat PLAT242_ALERT_2_C Low 'MainMol' Ueq as Compared to Neighbors of Cr2 Check PLAT420_ALERT_2_C D-H Without Acceptor N2 -- H2B ... Please Check PLAT480_ALERT_4_C Long H...A H-Bond Reported H2B .. O2SB .. 2.63 Ang. PLAT911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 103 Report
Alert level G ABSMU01_ALERT_1_G Calculation of _exptl_absorpt_correction_mu not performed for this radiation type. PLAT003_ALERT_2_G Number of Uiso or Uij Restrained non-H Atoms ... 4 Report PLAT007_ALERT_5_G Number of Unrefined Donor-H Atoms .............. 8 Report PLAT042_ALERT_1_G Calc. and Reported MoietyFormula Strings Differ Please Check PLAT066_ALERT_1_G Predicted and Reported Tmin&Tmax Range Identical ? Check PLAT171_ALERT_4_G The CIF-Embedded .res File Contains EADP Records 1 Report PLAT186_ALERT_4_G The CIF-Embedded .res File Contains ISOR Records 2 Report PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Cr2 -- O2SB .. 14.0 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Cr2 -- O3SB .. 20.0 s.u. PLAT232_ALERT_2_G Hirshfeld Test Diff (M-X) Cr2 -- O4SB .. 13.5 s.u. PLAT300_ALERT_4_G Atom Site Occupancy of >O2SA is Constrained at 0.7 Check PLAT300_ALERT_4_G Atom Site Occupancy of >O3SA is Constrained at 0.7 Check PLAT300_ALERT_4_G Atom Site Occupancy of >O4SA is Constrained at 0.7 Check PLAT300_ALERT_4_G Atom Site Occupancy of <O1SA is Constrained at 0.35 Check PLAT300_ALERT_4_G Atom Site Occupancy of <O1SB is Constrained at 0.15 Check PLAT300_ALERT_4_G Atom Site Occupancy of <O2SB is Constrained at 0.3 Check PLAT300_ALERT_4_G Atom Site Occupancy of <O3SB is Constrained at 0.3 Check PLAT300_ALERT_4_G Atom Site Occupancy of <O4SB is Constrained at 0.3 Check PLAT301_ALERT_3_G Main Residue Disorder ............ Percentage = 31 Note PLAT720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 8 Note PLAT764_ALERT_4_G Overcomplete CIF Bond List Detected (Rep/Expd) . 1.17 Ratio PLAT860_ALERT_3_G Number of Least-Squares Restraints ............. 24 Note PLAT912_ALERT_4_G Missing # of FCF Reflections Above STh/L= 0.600 60 Note PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF .... 1 Note PLAT933_ALERT_2_G Number of OMIT records in Embedded RES ......... 3 Note PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density 2 Note
0 ALERT level A = Most likely a serious problem - resolve or explain 0 ALERT level B = A potentially serious problem, consider carefully 6 ALERT level C = Check. Ensure it is not caused by an omission or oversight 26 ALERT level G = General information/check it is not something unexpected 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 9 ALERT type 2 Indicator that the structure model may be wrong or deficient 5 ALERT type 3 Indicator that the structure quality may be low 14 ALERT type 4 Improvement, methodology, query or suggestion 1 ALERT type 5 Informative message, check

Computing details top

Data collection: PAL BL2D-SMDC Program (Shin et al., 2016); cell refinement: HKL3000sm (Otwinowski & Minor, 1997); data reduction: HKL3000sm (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXT2014 (Sheldrick, 2015a); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015b); molecular graphics: DIAMOND 4 (Putz & Brandenburg, 2014); software used to prepare material for publication: publCIF (Westrip, 2010).

Bis[trans-dichloridobis(propane-1,3-diamine-κ2N,N')chromium(III)]dichromate top
Crystal data top
[CrCl2(C3H10N2)2]2[Cr2O7]F(000) = 776
Mr = 758.32Dx = 1.738 Mg m3
Monoclinic, P21/cSynchrotron radiation, λ = 0.610 Å
a = 6.5240 (13) ÅCell parameters from 48108 reflections
b = 17.350 (4) Åθ = 0.4–33.7°
c = 12.901 (3) ŵ = 1.22 mm1
β = 97.18 (3)°T = 253 K
V = 1448.8 (5) Å3Plate, green
Z = 20.13 × 0.10 × 0.09 mm
Data collection top
ADSC Q210 CCD area detector
diffractometer
3059 reflections with I > 2σ(I)
Radiation source: PLSII 2D bending magnetRint = 0.019
ω scanθmax = 24.0°, θmin = 1.7°
Absorption correction: empirical (using intensity measurements)
(HKL3000sm SCALEPACK; Otwinowski & Minor, 1997)
h = 88
Tmin = 0.862, Tmax = 0.897k = 2323
13070 measured reflectionsl = 1616
3438 independent reflections
Refinement top
Refinement on F2Hydrogen site location: inferred from neighbouring sites
Least-squares matrix: fullH-atom parameters constrained
R[F2 > 2σ(F2)] = 0.037 w = 1/[σ2(Fo2) + (0.0617P)2 + 0.9892P]
where P = (Fo2 + 2Fc2)/3
wR(F2) = 0.105(Δ/σ)max = 0.001
S = 1.10Δρmax = 0.67 e Å3
3438 reflectionsΔρmin = 0.96 e Å3
192 parametersExtinction correction: SHELXL2014 (Sheldrick, 2015b), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
24 restraintsExtinction coefficient: 0.025 (3)
Special details top

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

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Cr10.49736 (4)0.22092 (2)0.64090 (2)0.01917 (12)
Cl10.74178 (8)0.17096 (3)0.54341 (5)0.03402 (16)
Cl20.26188 (9)0.27054 (4)0.74422 (5)0.04056 (18)
N10.4818 (3)0.11569 (11)0.71701 (16)0.0333 (4)
H1A0.60040.10940.75840.040*
H1B0.38270.11940.75830.040*
N20.2575 (3)0.18582 (11)0.52655 (15)0.0281 (4)
H2A0.13860.19680.55040.034*
H2B0.26390.21500.47040.034*
N30.5108 (4)0.32459 (11)0.56009 (17)0.0355 (4)
H3A0.59970.31800.51380.043*
H3B0.38710.33200.52380.043*
N40.7385 (3)0.25541 (12)0.75231 (14)0.0288 (4)
H4A0.72660.22930.81070.035*
H4B0.85590.24040.73010.035*
C10.4434 (4)0.04454 (13)0.6542 (2)0.0386 (5)
H1C0.43860.00090.70080.046*
H1D0.55710.03640.61370.046*
C20.2426 (4)0.04817 (15)0.5807 (2)0.0420 (6)
H2C0.21130.00290.55240.050*
H2D0.13190.06290.62040.050*
C30.2471 (4)0.10400 (14)0.4914 (2)0.0355 (5)
H3C0.36600.09280.45570.043*
H3D0.12410.09670.44180.043*
C40.5687 (5)0.39723 (14)0.6173 (2)0.0429 (6)
H4C0.46140.41100.65960.051*
H4D0.57990.43850.56760.051*
C50.7716 (4)0.38861 (15)0.6867 (2)0.0419 (6)
H5A0.87290.36740.64560.050*
H5B0.81940.43930.71040.050*
C60.7610 (4)0.33802 (15)0.78056 (19)0.0366 (5)
H6A0.88570.34490.82910.044*
H6B0.64460.35380.81560.044*
Cr21.00840 (7)0.57351 (2)0.59016 (4)0.03941 (15)
O1SA1.0285 (19)0.4915 (6)0.5165 (9)0.064 (2)0.35
O2SA0.7745 (6)0.5919 (3)0.6061 (3)0.0760 (12)0.7
O3SA1.1407 (11)0.6446 (3)0.5675 (4)0.099 (2)0.7
O4SA1.1024 (7)0.5391 (3)0.7046 (3)0.0930 (16)0.7
O1SB1.0285 (19)0.4915 (6)0.5165 (9)0.064 (2)0.15
O2SB0.937 (2)0.6545 (9)0.5161 (12)0.112 (4)0.3
O3SB0.932 (3)0.5716 (9)0.6899 (13)0.118 (4)0.3
O4SB1.239 (2)0.6098 (8)0.5919 (11)0.089 (4)0.3
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cr10.01447 (17)0.02308 (18)0.0206 (2)0.00022 (10)0.00483 (11)0.00014 (11)
Cl10.0215 (3)0.0465 (3)0.0364 (3)0.0014 (2)0.0128 (2)0.0111 (2)
Cl20.0256 (3)0.0509 (4)0.0486 (4)0.0003 (2)0.0181 (2)0.0147 (3)
N10.0381 (11)0.0329 (9)0.0292 (10)0.0018 (8)0.0055 (8)0.0069 (7)
N20.0188 (8)0.0314 (9)0.0331 (10)0.0013 (7)0.0005 (7)0.0009 (7)
N30.0473 (12)0.0274 (9)0.0316 (11)0.0024 (8)0.0036 (8)0.0026 (7)
N40.0233 (8)0.0405 (10)0.0225 (9)0.0040 (7)0.0022 (6)0.0018 (7)
C10.0441 (14)0.0248 (10)0.0466 (15)0.0000 (9)0.0042 (11)0.0077 (9)
C20.0361 (13)0.0321 (12)0.0574 (17)0.0112 (10)0.0040 (11)0.0004 (11)
C30.0301 (11)0.0350 (11)0.0392 (13)0.0029 (9)0.0040 (9)0.0075 (9)
C40.0559 (16)0.0247 (11)0.0493 (16)0.0052 (10)0.0117 (12)0.0018 (10)
C50.0447 (14)0.0348 (12)0.0488 (16)0.0144 (10)0.0165 (11)0.0086 (10)
C60.0339 (12)0.0461 (13)0.0306 (13)0.0121 (10)0.0081 (9)0.0142 (10)
Cr20.0402 (3)0.0366 (2)0.0431 (3)0.00926 (16)0.01182 (18)0.01372 (16)
O1SA0.072 (7)0.044 (5)0.074 (7)0.000 (3)0.000 (4)0.029 (4)
O2SA0.052 (2)0.108 (3)0.069 (3)0.031 (2)0.0139 (17)0.021 (2)
O3SA0.173 (5)0.062 (2)0.076 (3)0.078 (3)0.074 (3)0.033 (2)
O4SA0.077 (3)0.112 (4)0.078 (3)0.035 (3)0.039 (2)0.023 (3)
O1SB0.072 (7)0.044 (5)0.074 (7)0.000 (3)0.000 (4)0.029 (4)
O2SB0.112 (4)0.111 (4)0.112 (4)0.0009 (10)0.0136 (11)0.0006 (10)
O3SB0.118 (4)0.118 (4)0.118 (4)0.0005 (10)0.0163 (12)0.0006 (10)
O4SB0.088 (4)0.089 (4)0.089 (4)0.0013 (10)0.0110 (11)0.0013 (10)
Geometric parameters (Å, º) top
Cr1—N12.0814 (19)C3—H3C0.9700
Cr1—N42.0816 (19)C3—H3D0.9700
Cr1—N32.086 (2)C4—C51.509 (4)
Cr1—N22.1020 (19)C4—H4C0.9700
Cr1—Cl12.3189 (8)C4—H4D0.9700
Cr1—Cl22.3216 (8)C5—C61.504 (4)
N1—C11.481 (3)C5—H5A0.9700
N1—H1A0.8900C5—H5B0.9700
N1—H1B0.8900C6—H6A0.9700
N2—C31.489 (3)C6—H6B0.9700
N2—H2A0.8900Cr2—O3SB1.437 (16)
N2—H2B0.8900Cr2—O3SA1.554 (3)
N3—C41.486 (3)Cr2—O2SA1.597 (4)
N3—H3A0.8900Cr2—O4SB1.629 (14)
N3—H3B0.8900Cr2—O4SA1.639 (4)
N4—C61.482 (3)Cr2—O1SB1.725 (12)
N4—H4A0.8900Cr2—O1SA1.725 (12)
N4—H4B0.8900Cr2—O2SB1.729 (15)
C1—C21.519 (4)Cr2—O1SBi1.772 (12)
C1—H1C0.9700Cr2—O1SAi1.772 (12)
C1—H1D0.9700O1SA—O1SAi0.607 (12)
C2—C31.509 (4)O1SA—Cr2i1.772 (12)
C2—H2C0.9700O1SB—O1SBi0.607 (12)
C2—H2D0.9700O1SB—Cr2i1.772 (12)
N1—Cr1—N490.20 (8)N2—C3—C2112.6 (2)
N1—Cr1—N3178.19 (8)N2—C3—H3C109.1
N4—Cr1—N391.25 (8)C2—C3—H3C109.1
N1—Cr1—N290.07 (8)N2—C3—H3D109.1
N4—Cr1—N2179.02 (7)C2—C3—H3D109.1
N3—Cr1—N288.46 (8)H3C—C3—H3D107.8
N1—Cr1—Cl190.30 (6)N3—C4—C5111.1 (2)
N4—Cr1—Cl188.31 (6)N3—C4—H4C109.4
N3—Cr1—Cl188.66 (7)C5—C4—H4C109.4
N2—Cr1—Cl190.75 (6)N3—C4—H4D109.4
N1—Cr1—Cl288.84 (6)C5—C4—H4D109.4
N4—Cr1—Cl289.66 (6)H4C—C4—H4D108.0
N3—Cr1—Cl292.26 (7)C6—C5—C4114.2 (2)
N2—Cr1—Cl291.29 (6)C6—C5—H5A108.7
Cl1—Cr1—Cl2177.79 (3)C4—C5—H5A108.7
C1—N1—Cr1119.21 (15)C6—C5—H5B108.7
C1—N1—H1A107.5C4—C5—H5B108.7
Cr1—N1—H1A107.5H5A—C5—H5B107.6
C1—N1—H1B107.5N4—C6—C5112.30 (19)
Cr1—N1—H1B107.5N4—C6—H6A109.1
H1A—N1—H1B107.0C5—C6—H6A109.1
C3—N2—Cr1119.45 (14)N4—C6—H6B109.1
C3—N2—H2A107.5C5—C6—H6B109.1
Cr1—N2—H2A107.5H6A—C6—H6B107.9
C3—N2—H2B107.5O3SA—Cr2—O2SA115.3 (3)
Cr1—N2—H2B107.5O3SB—Cr2—O4SB114.8 (8)
H2A—N2—H2B107.0O3SA—Cr2—O4SA107.8 (3)
C4—N3—Cr1120.46 (17)O2SA—Cr2—O4SA102.3 (2)
C4—N3—H3A107.2O3SB—Cr2—O1SB122.2 (8)
Cr1—N3—H3A107.2O4SB—Cr2—O1SB101.1 (7)
C4—N3—H3B107.2O3SA—Cr2—O1SA118.0 (6)
Cr1—N3—H3B107.2O2SA—Cr2—O1SA112.0 (5)
H3A—N3—H3B106.8O4SA—Cr2—O1SA98.6 (3)
C6—N4—Cr1119.42 (15)O3SB—Cr2—O2SB114.5 (8)
C6—N4—H4A107.5O4SB—Cr2—O2SB82.9 (7)
Cr1—N4—H4A107.5O1SB—Cr2—O2SB113.6 (6)
C6—N4—H4B107.5O3SB—Cr2—O1SBi130.7 (8)
Cr1—N4—H4B107.5O4SB—Cr2—O1SBi107.0 (7)
H4A—N4—H4B107.0O1SB—Cr2—O1SBi19.9 (4)
N1—C1—C2112.4 (2)O2SB—Cr2—O1SBi95.0 (6)
N1—C1—H1C109.1O3SA—Cr2—O1SAi112.5 (5)
C2—C1—H1C109.1O2SA—Cr2—O1SAi100.8 (5)
N1—C1—H1D109.1O4SA—Cr2—O1SAi117.9 (3)
C2—C1—H1D109.1O1SA—Cr2—O1SAi19.9 (4)
H1C—C1—H1D107.9O1SAi—O1SA—Cr284 (2)
C3—C2—C1113.9 (2)O1SAi—O1SA—Cr2i76 (2)
C3—C2—H2C108.8Cr2—O1SA—Cr2i160.1 (4)
C1—C2—H2C108.8O1SBi—O1SB—Cr284 (2)
C3—C2—H2D108.8O1SBi—O1SB—Cr2i76 (2)
C1—C2—H2D108.8Cr2—O1SB—Cr2i160.1 (4)
H2C—C2—H2D107.7
Cr1—N1—C1—C258.0 (3)O3SA—Cr2—O1SA—Cr2i79 (3)
N1—C1—C2—C369.9 (3)O2SA—Cr2—O1SA—Cr2i59 (3)
Cr1—N2—C3—C255.6 (2)O4SA—Cr2—O1SA—Cr2i166 (3)
C1—C2—C3—N268.5 (3)O1SAi—Cr2—O1SA—Cr2i0.002 (7)
Cr1—N3—C4—C553.7 (3)O3SB—Cr2—O1SB—O1SBi122 (3)
N3—C4—C5—C671.0 (3)O4SB—Cr2—O1SB—O1SBi109 (3)
Cr1—N4—C6—C554.5 (2)O2SB—Cr2—O1SB—O1SBi22 (3)
C4—C5—C6—N472.2 (3)O3SB—Cr2—O1SB—Cr2i122 (3)
O3SA—Cr2—O1SA—O1SAi79 (3)O4SB—Cr2—O1SB—Cr2i109 (3)
O2SA—Cr2—O1SA—O1SAi59 (3)O2SB—Cr2—O1SB—Cr2i22 (3)
O4SA—Cr2—O1SA—O1SAi166 (3)O1SBi—Cr2—O1SB—Cr2i0.002 (7)
Symmetry code: (i) x+2, y+1, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N1—H1A···O4SAii0.892.293.076 (4)147
N1—H1A···O4SBii0.892.082.877 (14)149
N1—H1B···O2SAiii0.892.193.022 (4)156
N1—H1B···O3SBiii0.892.393.182 (16)149
N2—H2A···Cl1iv0.892.623.4085 (19)149
N2—H2B···O2SBv0.892.633.070 (15)111
N3—H3A···O3SAi0.892.203.017 (5)153
N3—H3A···O4SBi0.892.212.933 (14)138
N3—H3B···O2SAv0.892.283.027 (5)141
N3—H3B···O2SBv0.892.132.989 (16)162
N4—H4A···O3SAii0.892.253.044 (4)149
N4—H4A···O4SBii0.892.423.220 (14)150
N4—H4B···Cl2vi0.892.683.439 (2)143
Symmetry codes: (i) x+2, y+1, z+1; (ii) x+2, y1/2, z+3/2; (iii) x+1, y1/2, z+3/2; (iv) x1, y, z; (v) x+1, y+1, z+1; (vi) x+1, y, z.
 

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