catena-Poly[[(N,N-dimethyl­propane-1,3-diamine)thio­cyanato­nickel(II)]-μ-thio­cyanato]

The title compound, [Ni(NCS)₂(C₅H₁₄N₂)]_n, is a thio­cyanate-bridged polynuclear nickel(II) complex. The Ni atom is five-coordinated in a square-pyramidal geometry, with two N atoms of the N,N-dimethyl­propane-1,3-diamine ligand and two N atoms from two thio­cyanate ligands defining the basal plane, and one S atom of another thio­cyanate ligand occupying the apical position. The [Ni(NCS)₂(C₅H₁₄N₂)] units are linked by bridging thio­cyanate ligands, forming chains running along the b axis.

Key indicators

• Single-crystal X-ray study
• T = 298 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.029
• wR factor = 0.067
• Data-to-parameter ratio = 19.6

checkCIF/PLATON results

No syntax errors found



Alert level C
STRVA01_ALERT_4_C           Flack test results are ambiguous.
           From the CIF: _refine_ls_abs_structure_Flack    0.576
           From the CIF: _refine_ls_abs_structure_Flack_su    0.014
PLAT033_ALERT_2_C Flack Parameter Value Deviates from Zero .......       0.58
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         N3
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         C6

Alert level G
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           27.50
           From the CIF: _reflns_number_total               2542
           Count of symmetry unique reflns         1446
           Completeness (_total/calc)            175.80%
           TEST3: Check Friedels for noncentro structure
           Estimate of Friedel pairs measured      1096
           Fraction of Friedel pairs measured     0.758
           Are heavy atom types Z>Si present        yes

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

   0 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
   2 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Siemens, 1996); cell refinement: SAINT (Siemens, 1996); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997a); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997a); molecular graphics: SHELXTL (Sheldrick, 1997b); software used to prepare material for publication: SHELXTL.

catena-Poly[[(N,N-dimethylpropane-1,3-diamine)thiocyanatonickel(II)]-µ- thiocyanato]

Crystal data

[Ni(NCS)2(C5H14N2)]	F(000) = 288
Mr = 277.05	Dx = 1.574 Mg m^−3
Monoclinic, P21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: P 2yb	Cell parameters from 2235 reflections
a = 8.216 (1) Å	θ = 2.6–26.7°
b = 6.927 (1) Å	µ = 1.99 mm^−1
c = 10.987 (2) Å	T = 298 K
β = 110.819 (2)°	Plate, green
V = 584.47 (15) Å^3	0.35 × 0.11 × 0.04 mm
Z = 2

Data collection

Bruker SMART CCD area-detector diffractometer	2542 independent reflections
Radiation source: fine-focus sealed tube	2376 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.027
ω scans	θmax = 27.5°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→10
Tmin = 0.543, Tmax = 0.925	k = −9→9
4931 measured reflections	l = −14→13

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)] = 0.029	H-atom parameters constrained
wR(F^2) = 0.067	w = 1/[σ^2(Fo^2) + (0.0252P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.03	(Δ/σ)max < 0.001
2542 reflections	Δρmax = 0.31 e Å^−3
130 parameters	Δρmin = −0.25 e Å^−3
1 restraint	Absolute structure: Flack (1983), 1096 Friedel pairs?
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.576 (14)

Special details

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
Ni1	0.16574 (4)	0.30631 (5)	0.90877 (3)	0.03061 (10)
S1	0.50500 (12)	0.33321 (17)	1.35741 (8)	0.0601 (3)
S2	−0.23968 (10)	0.40932 (12)	1.11257 (8)	0.04139 (19)
N1	−0.0051 (3)	0.3098 (5)	0.7173 (2)	0.0362 (5)
N2	0.3585 (3)	0.4172 (4)	0.8608 (3)	0.0400 (6)
H2A	0.3392	0.5449	0.8491	0.048*
H2B	0.4577	0.4026	0.9298	0.048*
N3	0.3224 (3)	0.3130 (10)	1.0921 (2)	0.0568 (7)
N4	−0.0297 (3)	0.3072 (6)	0.9717 (2)	0.0473 (6)
C1	0.0758 (4)	0.2574 (5)	0.6198 (3)	0.0455 (8)
H1A	−0.0119	0.2715	0.5336	0.055*
H1B	0.1079	0.1220	0.6313	0.055*
C2	0.2351 (4)	0.3722 (5)	0.6243 (3)	0.0505 (9)
H2C	0.2659	0.3370	0.5498	0.061*
H2D	0.2056	0.5084	0.6166	0.061*
C3	0.3904 (4)	0.3422 (5)	0.7455 (3)	0.0451 (9)
H3A	0.4169	0.2054	0.7570	0.054*
H3B	0.4903	0.4075	0.7370	0.054*
C4	−0.0800 (5)	0.5071 (5)	0.6923 (4)	0.0533 (9)
H4A	−0.1599	0.5156	0.6040	0.080*
H4B	0.0119	0.5994	0.7058	0.080*
H4C	−0.1405	0.5339	0.7508	0.080*
C5	−0.1507 (4)	0.1711 (6)	0.6979 (4)	0.0496 (9)
H5A	−0.2052	0.1967	0.7603	0.074*
H5B	−0.1060	0.0417	0.7093	0.074*
H5C	−0.2347	0.1856	0.6115	0.074*
C6	0.3973 (3)	0.3231 (6)	1.2026 (3)	0.0384 (6)
C7	−0.1174 (4)	0.3493 (4)	1.0293 (3)	0.0340 (7)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Ni1	0.02630 (16)	0.03851 (18)	0.02669 (16)	−0.00061 (19)	0.00902 (12)	−0.0032 (2)
S1	0.0635 (5)	0.0681 (7)	0.0360 (4)	0.0095 (6)	0.0023 (4)	0.0009 (5)
S2	0.0373 (4)	0.0442 (4)	0.0487 (5)	0.0012 (3)	0.0227 (4)	−0.0027 (4)
N1	0.0352 (11)	0.0372 (11)	0.0329 (11)	−0.0018 (17)	0.0081 (9)	−0.0028 (18)
N2	0.0318 (13)	0.0419 (14)	0.0432 (15)	−0.0039 (12)	0.0096 (11)	−0.0010 (12)
N3	0.0458 (14)	0.084 (2)	0.0364 (13)	−0.002 (2)	0.0099 (11)	−0.005 (2)
N4	0.0435 (13)	0.0596 (14)	0.0431 (13)	0.0000 (19)	0.0205 (11)	−0.007 (2)
C1	0.0589 (19)	0.046 (2)	0.0310 (15)	−0.0063 (14)	0.0154 (14)	−0.0069 (12)
C2	0.061 (2)	0.056 (2)	0.0432 (19)	−0.0070 (16)	0.0283 (17)	0.0010 (14)
C3	0.0446 (16)	0.041 (2)	0.059 (2)	−0.0022 (14)	0.0302 (15)	0.0007 (15)
C4	0.052 (2)	0.044 (2)	0.052 (2)	0.0123 (17)	0.0031 (18)	0.0038 (16)
C5	0.0407 (19)	0.053 (2)	0.048 (2)	−0.0091 (16)	0.0077 (15)	−0.0060 (16)
C6	0.0350 (13)	0.0410 (17)	0.0398 (15)	0.0028 (17)	0.0140 (12)	−0.0016 (18)
C7	0.0323 (14)	0.0343 (19)	0.0318 (14)	−0.0013 (11)	0.0070 (11)	−0.0002 (11)

Geometric parameters (Å, º)

Ni1—N1	2.073 (3)	C1—C2	1.517 (4)
Ni1—N2	1.993 (3)	C1—H1A	0.9700
Ni1—N3	1.968 (3)	C1—H1B	0.9700
Ni1—N4	1.961 (3)	C2—C3	1.496 (5)
Ni1—S2^i	2.8439 (10)	C2—H2C	0.9700
S1—C6	1.616 (3)	C2—H2D	0.9700
S2—C7	1.635 (3)	C3—H3A	0.9700
N1—C4	1.484 (5)	C3—H3B	0.9700
N1—C5	1.489 (4)	C4—H4A	0.9600
N1—C1	1.493 (4)	C4—H4B	0.9600
N2—C3	1.476 (4)	C4—H4C	0.9600
N2—H2A	0.9000	C5—H5A	0.9600
N2—H2B	0.9000	C5—H5B	0.9600
N3—C6	1.152 (4)	C5—H5C	0.9600
N4—C7	1.153 (4)
N4—Ni1—N3	87.64 (12)	C2—C1—H1B	108.1
N4—Ni1—N2	156.87 (15)	H1A—C1—H1B	107.3
N3—Ni1—N2	88.24 (14)	C3—C2—C1	114.1 (3)
N4—Ni1—N1	90.78 (12)	C3—C2—H2C	108.7
N3—Ni1—N1	177.4 (2)	C1—C2—H2C	108.7
N2—Ni1—N1	92.44 (11)	C3—C2—H2D	108.7
N1—Ni1—S2^i	90.86 (11)	C1—C2—H2D	108.7
N2—Ni1—S2^i	97.92 (11)	H2C—C2—H2D	107.6
N3—Ni1—S2^i	91.49 (11)	N2—C3—C2	111.1 (3)
N4—Ni1—S2^i	104.93 (11)	N2—C3—H3A	109.4
C4—N1—C5	108.0 (3)	C2—C3—H3A	109.4
C4—N1—C1	110.6 (3)	N2—C3—H3B	109.4
C5—N1—C1	106.3 (3)	C2—C3—H3B	109.4
C4—N1—Ni1	106.6 (2)	H3A—C3—H3B	108.0
C5—N1—Ni1	111.0 (2)	N1—C4—H4A	109.5
C1—N1—Ni1	114.32 (19)	N1—C4—H4B	109.5
C3—N2—Ni1	119.4 (2)	H4A—C4—H4B	109.5
C3—N2—H2A	107.5	N1—C4—H4C	109.5
Ni1—N2—H2A	107.5	H4A—C4—H4C	109.5
C3—N2—H2B	107.5	H4B—C4—H4C	109.5
Ni1—N2—H2B	107.5	N1—C5—H5A	109.5
H2A—N2—H2B	107.0	N1—C5—H5B	109.5
C6—N3—Ni1	172.0 (3)	H5A—C5—H5B	109.5
C7—N4—Ni1	160.8 (3)	N1—C5—H5C	109.5
N1—C1—C2	116.6 (3)	H5A—C5—H5C	109.5
N1—C1—H1A	108.1	H5B—C5—H5C	109.5
C2—C1—H1A	108.1	N3—C6—S1	178.7 (4)
N1—C1—H1B	108.1	N4—C7—S2	179.3 (3)

Symmetry code: (i) −x, y−1/2, −z+2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
N2—H2B···S2^ii	0.90	2.58	3.473 (4)	171
N2—H2A···S2^iii	0.90	2.73	3.586 (4)	159

Symmetry codes: (ii) x+1, y, z; (iii) −x, y+1/2, −z+2.