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The title compound, hexaamminechromium(III) diaquatetrachlorosodium(I), [Cr(NH3)6][NaCl4(H2O)2], is composed of discrete [Cr(NH3)6]3+ cations and [NaCl4(H2O)2]3- anions. The Cr and Na ions are octahedrally coordinated. The crystal packing is characterized by an alternating arrangement of anions and cations and is stabilized by numerous hydrogen bonds.
Supporting information
Key indicators
- Single-crystal X-ray study
- T = 173 K
- Mean (Cr-N) = 0.004 Å
- R factor = 0.037
- wR factor = 0.073
- Data-to-parameter ratio = 15.2
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93
Alert level B
CHEMS01_ALERT_1_B The sum formula contains elements in the wrong order.
H precedes Cl
Sequence must be C, H, then alphabetical.
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT420_ALERT_2_C D-H Without Acceptor N6 - H6C ... ?
PLAT731_ALERT_1_C Bond Calc 0.88(3), Rep 0.881(10) ...... 3.00 su-Rat
N1 -H1A 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.88(4), Rep 0.873(10) ...... 4.00 su-Rat
N2 -H2B 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.88(3), Rep 0.875(10) ...... 3.00 su-Rat
N2 -H2C 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.88(3), Rep 0.877(10) ...... 3.00 su-Rat
N3 -H3A 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.88(3), Rep 0.875(10) ...... 3.00 su-Rat
N4 -H4A 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.87(3), Rep 0.877(10) ...... 3.00 su-Rat
N5 -H5C 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.87(3), Rep 0.874(10) ...... 3.00 su-Rat
N6 -H6C 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.837(10) ...... 3.00 su-Rat
O1 -H1E 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.84(3), Rep 0.836(10) ...... 3.00 su-Rat
O2 -H2E 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.88(3), Rep 0.881(10) ...... 3.00 su-Rat
N1 -H1A 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.88(4), Rep 0.873(10) ...... 4.00 su-Rat
N2 -H2B 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.88(3), Rep 0.875(10) ...... 3.00 su-Rat
N2 -H2C 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.88(3), Rep 0.875(10) ...... 3.00 su-Rat
N2 -H2C 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.88(3), Rep 0.877(10) ...... 3.00 su-Rat
N3 -H3A 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.88(3), Rep 0.875(10) ...... 3.00 su-Rat
N4 -H4A 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.87(3), Rep 0.877(10) ...... 3.00 su-Rat
N5 -H5C 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.87(3), Rep 0.874(10) ...... 3.00 su-Rat
N6 -H6C 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.837(10) ...... 3.00 su-Rat
O1 -H1E 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.84(3), Rep 0.836(10) ...... 3.00 su-Rat
O2 -H2E 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 2.43(4), Rep 2.426(14) ...... 2.86 su-Rat
H2B -CL1 1.555 4.466
PLAT736_ALERT_1_C H...A Calc 2.49(3), Rep 2.487(14) ...... 2.14 su-Rat
H3B -CL2 1.555 2.665
Alert level G
REFLT03_ALERT_1_G ALERT: Expected hkl max differ from CIF values
From the CIF: _diffrn_reflns_theta_max 27.12
From the CIF: _reflns_number_total 2941
From the CIF: _diffrn_reflns_limit_ max hkl 8. 10. 27.
From the CIF: _diffrn_reflns_limit_ min hkl -9. -10. -27.
TEST1: Expected hkl limits for theta max
Calculated maximum hkl 9. 11. 29.
Calculated minimum hkl -9. -11. -29.
REFLT03_ALERT_4_G Please check that the estimate of the number of Friedel pairs is
correct. If it is not, please give the correct count in the
_publ_section_exptl_refinement section of the submitted CIF.
From the CIF: _diffrn_reflns_theta_max 27.12
From the CIF: _reflns_number_total 2941
Count of symmetry unique reflns 1880
Completeness (_total/calc) 156.44%
TEST3: Check Friedels for noncentro structure
Estimate of Friedel pairs measured 1061
Fraction of Friedel pairs measured 0.564
Are heavy atom types Z>Si present yes
1 ALERT level A = In general: serious problem
1 ALERT level B = Potentially serious problem
24 ALERT level C = Check and explain
2 ALERT level G = General alerts; check
25 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
1 ALERT type 3 Indicator that the structure quality may be low
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Siemens, 1995); cell refinement: SMART; data reduction: SAINT (Siemens, 1995); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97.
Hexaamminechromium(III) diaquatetrachlorosodium(I)
top
Crystal data top
H18CrN63+·H4Cl4NaO23− | F(000) = 732 |
Mr = 355.03 | Dx = 1.612 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 5893 reflections |
a = 7.0596 (3) Å | θ = 1–25° |
b = 9.1575 (4) Å | µ = 1.53 mm−1 |
c = 22.631 (1) Å | T = 173 K |
V = 1463.06 (11) Å3 | Plate, orange |
Z = 4 | 0.34 × 0.12 × 0.06 mm |
Data collection top
Siemens CCD three-circle diffractometer | 2941 independent reflections |
Radiation source: fine-focus sealed tube | 2340 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.062 |
ω scans | θmax = 27.1°, θmin = 1.8° |
Absorption correction: empirical (SADABS; Sheldrick, 1996) | h = −9→8 |
Tmin = 0.624, Tmax = 0.914 | k = −10→10 |
14937 measured reflections | l = −27→27 |
Refinement top
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.037 | Only H-atom coordinates refined |
wR(F2) = 0.073 | w = 1/[σ2(Fo2) + (0.0304P)2 + 0.4093P] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
2941 reflections | Δρmax = 0.41 e Å−3 |
194 parameters | Δρmin = −0.43 e Å−3 |
22 restraints | Absolute structure: Flack (1983), 0000 Friedel pairs |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.18 (3) |
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 | x | y | z | Uiso*/Ueq | |
Cr1 | 0.59753 (10) | 0.59589 (6) | 0.87758 (2) | 0.01310 (14) | |
N1 | 0.8049 (5) | 0.5294 (4) | 0.93629 (16) | 0.0201 (8) | |
H1A | 0.894 (4) | 0.595 (3) | 0.9420 (18) | 0.030* | |
H1B | 0.859 (5) | 0.445 (2) | 0.9312 (17) | 0.030* | |
H1C | 0.775 (7) | 0.526 (4) | 0.9739 (7) | 0.030* | |
N2 | 0.3845 (6) | 0.5288 (4) | 0.93486 (16) | 0.0203 (7) | |
H2A | 0.420 (6) | 0.511 (4) | 0.9714 (8) | 0.030* | |
H2B | 0.298 (5) | 0.596 (4) | 0.9401 (18) | 0.030* | |
H2C | 0.329 (5) | 0.451 (3) | 0.9204 (17) | 0.030* | |
N3 | 0.3916 (6) | 0.6643 (4) | 0.81852 (14) | 0.0186 (7) | |
H3A | 0.286 (3) | 0.616 (4) | 0.8247 (17) | 0.028* | |
H3B | 0.427 (6) | 0.636 (4) | 0.7833 (8) | 0.028* | |
H3C | 0.371 (6) | 0.7582 (14) | 0.8190 (17) | 0.028* | |
N4 | 0.8059 (5) | 0.6616 (4) | 0.81882 (16) | 0.0193 (8) | |
H4A | 0.902 (4) | 0.601 (4) | 0.8191 (17) | 0.029* | |
H4B | 0.778 (6) | 0.670 (5) | 0.7812 (7) | 0.029* | |
H4C | 0.847 (6) | 0.749 (2) | 0.8273 (17) | 0.029* | |
N5 | 0.5928 (6) | 0.3919 (3) | 0.83651 (14) | 0.0187 (7) | |
H5A | 0.624 (6) | 0.412 (4) | 0.8000 (7) | 0.028* | |
H5B | 0.475 (2) | 0.361 (4) | 0.8379 (17) | 0.028* | |
H5C | 0.666 (4) | 0.328 (3) | 0.8539 (15) | 0.028* | |
N6 | 0.5999 (6) | 0.7992 (3) | 0.91872 (14) | 0.0206 (7) | |
H6A | 0.595 (7) | 0.792 (4) | 0.9576 (5) | 0.031* | |
H6B | 0.717 (2) | 0.830 (4) | 0.9181 (18) | 0.031* | |
H6C | 0.512 (4) | 0.860 (4) | 0.9072 (17) | 0.031* | |
Na1 | 0.6003 (3) | 0.40765 (16) | 0.12594 (6) | 0.0228 (3) | |
Cl1 | 0.60018 (16) | 0.68763 (10) | 0.06311 (4) | 0.0213 (2) | |
Cl3 | 0.59675 (17) | 0.11893 (10) | 0.17514 (4) | 0.0234 (2) | |
Cl2 | 0.91942 (16) | 0.47705 (10) | 0.19570 (4) | 0.0205 (2) | |
Cl4 | 0.27215 (15) | 0.34262 (11) | 0.06183 (4) | 0.0228 (2) | |
O1 | 0.8203 (4) | 0.3253 (5) | 0.05777 (16) | 0.0373 (9) | |
H1D | 0.9384 (16) | 0.332 (6) | 0.058 (2) | 0.056* | |
H1E | 0.787 (7) | 0.282 (5) | 0.0269 (13) | 0.056* | |
O2 | 0.3804 (5) | 0.5098 (3) | 0.19172 (13) | 0.0292 (7) | |
H2D | 0.397 (7) | 0.526 (5) | 0.2279 (7) | 0.044* | |
H2E | 0.273 (3) | 0.477 (5) | 0.183 (2) | 0.044* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cr1 | 0.0146 (3) | 0.0105 (3) | 0.0141 (3) | −0.0003 (3) | −0.0001 (3) | −0.0002 (2) |
N1 | 0.026 (2) | 0.0143 (18) | 0.0202 (18) | 0.0029 (15) | −0.0074 (18) | −0.0029 (18) |
N2 | 0.022 (2) | 0.0172 (18) | 0.0216 (17) | 0.0005 (17) | 0.000 (2) | 0.0016 (16) |
N3 | 0.0194 (19) | 0.0155 (17) | 0.0210 (17) | 0.003 (2) | −0.0016 (19) | 0.0025 (15) |
N4 | 0.022 (2) | 0.0156 (18) | 0.0200 (18) | 0.0014 (17) | 0.0021 (17) | 0.0002 (17) |
N5 | 0.0223 (19) | 0.0146 (17) | 0.0192 (16) | 0.0001 (19) | −0.0047 (18) | 0.0003 (14) |
N6 | 0.024 (2) | 0.0160 (17) | 0.0218 (17) | 0.0028 (19) | −0.0067 (19) | −0.0034 (14) |
Na1 | 0.0227 (7) | 0.0218 (7) | 0.0240 (7) | 0.0010 (8) | 0.0005 (8) | −0.0012 (6) |
Cl1 | 0.0213 (5) | 0.0190 (5) | 0.0235 (5) | −0.0009 (5) | −0.0010 (5) | 0.0023 (4) |
Cl3 | 0.0217 (5) | 0.0199 (5) | 0.0285 (5) | 0.0005 (5) | −0.0004 (5) | 0.0051 (4) |
Cl2 | 0.0236 (6) | 0.0196 (5) | 0.0183 (5) | −0.0027 (5) | −0.0011 (5) | 0.0012 (4) |
Cl4 | 0.0269 (6) | 0.0193 (5) | 0.0221 (5) | −0.0023 (5) | −0.0008 (5) | 0.0005 (4) |
O1 | 0.0286 (18) | 0.050 (2) | 0.0329 (19) | −0.0022 (18) | 0.0029 (18) | −0.0169 (17) |
O2 | 0.0263 (18) | 0.0393 (18) | 0.0222 (16) | 0.0022 (17) | −0.0041 (16) | −0.0038 (14) |
Geometric parameters (Å, º) top
Cr1—N1 | 2.069 (4) | N4—H4C | 0.876 (10) |
Cr1—N3 | 2.072 (4) | N5—H5A | 0.875 (10) |
Cr1—N4 | 2.072 (4) | N5—H5B | 0.880 (10) |
Cr1—N2 | 2.079 (4) | N5—H5C | 0.877 (10) |
Cr1—N6 | 2.082 (3) | N6—H6A | 0.883 (10) |
Cr1—N5 | 2.087 (3) | N6—H6B | 0.876 (10) |
N1—H1A | 0.881 (10) | N6—H6C | 0.874 (10) |
N1—H1B | 0.874 (10) | Na1—O1 | 2.316 (4) |
N1—H1C | 0.878 (10) | Na1—O2 | 2.345 (4) |
N2—H2A | 0.878 (10) | Na1—Cl4 | 2.797 (2) |
N2—H2B | 0.873 (10) | Na1—Cl2 | 2.824 (2) |
N2—H2C | 0.875 (10) | Na1—Cl3 | 2.8690 (17) |
N3—H3A | 0.877 (10) | Na1—Cl1 | 2.9318 (17) |
N3—H3B | 0.873 (10) | O1—H1D | 0.836 (10) |
N3—H3C | 0.872 (10) | O1—H1E | 0.837 (10) |
N4—H4A | 0.875 (10) | O2—H2D | 0.840 (10) |
N4—H4B | 0.877 (10) | O2—H2E | 0.836 (10) |
| | | |
N1—Cr1—N3 | 179.40 (17) | Cr1—N4—H4C | 111 (3) |
N1—Cr1—N4 | 89.72 (16) | H4A—N4—H4C | 109 (4) |
N3—Cr1—N4 | 89.79 (13) | H4B—N4—H4C | 102 (4) |
N1—Cr1—N2 | 91.41 (13) | Cr1—N5—H5A | 103 (3) |
N3—Cr1—N2 | 89.08 (16) | Cr1—N5—H5B | 107 (3) |
N4—Cr1—N2 | 178.66 (16) | H5A—N5—H5B | 110 (4) |
N1—Cr1—N6 | 88.30 (14) | Cr1—N5—H5C | 113 (3) |
N3—Cr1—N6 | 91.37 (14) | H5A—N5—H5C | 114 (4) |
N4—Cr1—N6 | 91.25 (15) | H5B—N5—H5C | 109 (4) |
N2—Cr1—N6 | 89.49 (15) | Cr1—N6—H6A | 112 (3) |
N1—Cr1—N5 | 91.94 (14) | Cr1—N6—H6B | 107 (3) |
N3—Cr1—N5 | 88.39 (14) | H6A—N6—H6B | 95 (4) |
N4—Cr1—N5 | 89.16 (14) | Cr1—N6—H6C | 116 (3) |
N2—Cr1—N5 | 90.09 (14) | H6A—N6—H6C | 108 (4) |
N6—Cr1—N5 | 179.52 (19) | H6B—N6—H6C | 118 (4) |
Cr1—N1—H1A | 114 (3) | O1—Na1—O2 | 175.42 (15) |
Cr1—N1—H1B | 119 (3) | O1—Na1—Cl4 | 98.07 (10) |
H1A—N1—H1B | 108 (4) | O2—Na1—Cl4 | 82.30 (10) |
Cr1—N1—H1C | 118 (3) | O1—Na1—Cl2 | 84.88 (10) |
H1A—N1—H1C | 93 (4) | O2—Na1—Cl2 | 94.79 (9) |
H1B—N1—H1C | 102 (4) | Cl4—Na1—Cl2 | 177.03 (7) |
Cr1—N2—H2A | 116 (3) | O1—Na1—Cl3 | 87.94 (12) |
Cr1—N2—H2B | 112 (3) | O2—Na1—Cl3 | 96.63 (9) |
H2A—N2—H2B | 102 (4) | Cl4—Na1—Cl3 | 89.88 (5) |
Cr1—N2—H2C | 109 (3) | Cl2—Na1—Cl3 | 89.85 (5) |
H2A—N2—H2C | 109 (4) | O1—Na1—Cl1 | 87.82 (12) |
H2B—N2—H2C | 108 (4) | O2—Na1—Cl1 | 87.65 (9) |
Cr1—N3—H3A | 110 (3) | Cl4—Na1—Cl1 | 86.24 (5) |
Cr1—N3—H3B | 107 (3) | Cl2—Na1—Cl1 | 94.28 (5) |
H3A—N3—H3B | 104 (4) | Cl3—Na1—Cl1 | 173.80 (6) |
Cr1—N3—H3C | 114 (3) | Na1—O1—H1D | 130 (4) |
H3A—N3—H3C | 111 (4) | Na1—O1—H1E | 122 (4) |
H3B—N3—H3C | 110 (4) | H1D—O1—H1E | 108 (5) |
Cr1—N4—H4A | 111 (3) | Na1—O2—H2D | 127 (4) |
Cr1—N4—H4B | 119 (3) | Na1—O2—H2E | 108 (3) |
H4A—N4—H4B | 103 (4) | H2D—O2—H2E | 114 (5) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N1—H1A···Cl1i | 0.88 (1) | 2.47 (2) | 3.325 (4) | 165 (4) |
N1—H1B···Cl4ii | 0.87 (1) | 2.71 (3) | 3.415 (4) | 139 (3) |
N1—H1C···O1iii | 0.88 (1) | 2.66 (3) | 3.326 (6) | 133 (3) |
N1—H1C···Cl1iii | 0.88 (1) | 2.79 (3) | 3.525 (4) | 142 (3) |
N2—H2A···Cl1iii | 0.88 (1) | 2.92 (3) | 3.586 (4) | 134 (3) |
N2—H2A···Cl4iii | 0.88 (1) | 2.77 (3) | 3.434 (4) | 134 (4) |
N2—H2B···Cl1iv | 0.87 (1) | 2.43 (1) | 3.282 (4) | 167 (4) |
N2—H2C···Cl3v | 0.88 (1) | 2.79 (3) | 3.486 (4) | 138 (3) |
N2—H2C···O1v | 0.88 (1) | 2.58 (3) | 3.278 (5) | 137 (3) |
N3—H3A···Cl3v | 0.88 (1) | 2.53 (2) | 3.329 (4) | 151 (4) |
N3—H3B···Cl2vi | 0.87 (1) | 2.49 (1) | 3.344 (4) | 167 (4) |
N3—H3C···Cl2iv | 0.87 (1) | 2.47 (2) | 3.306 (3) | 161 (4) |
N4—H4A···Cl3ii | 0.88 (1) | 2.44 (2) | 3.291 (4) | 164 (4) |
N4—H4B···Cl2vi | 0.88 (1) | 2.74 (3) | 3.450 (4) | 139 (4) |
N4—H4C···O2i | 0.88 (1) | 2.26 (2) | 3.064 (5) | 153 (4) |
N5—H5B···Cl3v | 0.88 (1) | 2.69 (2) | 3.513 (4) | 156 (4) |
N5—H5A···Cl2vi | 0.88 (1) | 2.59 (2) | 3.406 (3) | 156 (4) |
N5—H5C···Cl4ii | 0.88 (1) | 2.58 (2) | 3.392 (3) | 156 (3) |
N6—H6A···Cl1iii | 0.88 (1) | 2.57 (2) | 3.424 (3) | 162 (3) |
N6—H6B···Cl1i | 0.88 (1) | 2.74 (2) | 3.558 (4) | 156 (4) |
N6—H6C···Cl2iv | 0.87 (1) | 2.84 (3) | 3.539 (3) | 138 (3) |
O1—H1D···Cl4vii | 0.84 (1) | 2.36 (1) | 3.195 (3) | 177 (6) |
O1—H1E···Cl4viii | 0.84 (1) | 2.31 (2) | 3.131 (4) | 167 (5) |
O2—H2D···Cl3ix | 0.84 (1) | 2.35 (2) | 3.179 (3) | 167 (4) |
O2—H2E···Cl2x | 0.84 (1) | 2.51 (3) | 3.269 (4) | 151 (4) |
Symmetry codes: (i) x+1/2, −y+3/2, −z+1; (ii) x+1/2, −y+1/2, −z+1; (iii) x, y, z+1; (iv) x−1/2, −y+3/2, −z+1; (v) x−1/2, −y+1/2, −z+1; (vi) −x+3/2, −y+1, z+1/2; (vii) x+1, y, z; (viii) x+1/2, −y+1/2, −z; (ix) −x+1, y+1/2, −z+1/2; (x) x−1, y, z. |
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