Crystal structure of bis­[di­hydro­bis­(pyrazol-1-yl)borato-κ²N²,N^2′](1,10-phenanthroline-κ²N,N′)zinc(II)

In the crystal structure of the title compound, the Zn^II cation is octa­hedrally coordinated by the N atoms of a chelating phenanthroline ligand and the N atoms of two symmetry-related di­hydro­bis­(pyrazol-1-yl)borate ligands into discrete complexes.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.005 Å
• R factor = 0.039
• wR factor = 0.089
• Data-to-parameter ratio = 16.5

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT906_ALERT_3_C Large K Value in the Analysis of Variance ......      4.303 Check
PLAT911_ALERT_3_C Missing FCF Refl Between Thmin & STh/L=    0.600         11 Report

Alert level G
PLAT012_ALERT_1_G N.O.K.   _shelx_res_checksum Found in CIF ......     Please Check
PLAT128_ALERT_4_G Alternate Setting for Input Space Group     C2/c       I2/a Note
PLAT199_ALERT_1_G Reported _cell_measurement_temperature ..... (K)        293 Check
PLAT200_ALERT_1_G Reported   _diffrn_ambient_temperature ..... (K)        293 Check
PLAT794_ALERT_5_G Tentative Bond Valency for Zn1       (II)      .       1.76 Info
PLAT910_ALERT_3_G Missing # of FCF Reflection(s) Below Theta(Min).          1 Note
PLAT913_ALERT_3_G Missing # of Very Strong Reflections in FCF ....          3 Note
PLAT978_ALERT_2_G Number C-C Bonds with Positive Residual Density.          3 Info

   0 ALERT level A = Most likely a serious problem - resolve or explain
   0 ALERT level B = A potentially serious problem, consider carefully
   2 ALERT level C = Check. Ensure it is not caused by an omission or oversight
   8 ALERT level G = General information/check it is not something unexpected

   3 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
   4 ALERT type 3 Indicator that the structure quality may be low
   1 ALERT type 4 Improvement, methodology, query or suggestion
   1 ALERT type 5 Informative message, check

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Computing details

Data collection: X-AREA (Stoe & Cie, 2008); cell refinement: X-AREA (Stoe & Cie, 2008); data reduction: X-AREA (Stoe & Cie, 2008); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL2014 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 1999); software used to prepare material for publication: publCIF (Westrip, 2010).

Bis[dihydrobis(pyrazol-1-yl)borato-κ²N²,N^2'](1,10-\ phenanthroline-κ²N,N')zinc(II)

Crystal data

[Zn(C6H8BN4)2(C12H8N2)]	F(000) = 1112
Mr = 539.52	Dx = 1.410 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
a = 17.4591 (10) Å	Cell parameters from 10361 reflections
b = 16.0990 (7) Å	θ = 2.3–27.0°
c = 10.6076 (6) Å	µ = 1.00 mm^−1
β = 121.533 (4)°	T = 293 K
V = 2541.3 (3) Å^3	Block, colourless
Z = 4	0.13 × 0.10 × 0.06 mm

Data collection

Stoe IPDS-2 diffractometer	2359 reflections with I > 2σ(I)
ω scans	Rint = 0.031
Absorption correction: numerical (X-RED and X-SHAPE; Stoe & Cie, 2008)	θmax = 27.0°, θmin = 2.3°
Tmin = 0.805, Tmax = 0.911	h = −21→22
10361 measured reflections	k = −20→16
2765 independent reflections	l = −13→13

Refinement

Refinement on F^2	0 restraints
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.039	H-atom parameters constrained
wR(F^2) = 0.089	w = 1/[σ^2(Fo^2) + (0.0445P)^2 + 0.6977P] where P = (Fo^2 + 2Fc^2)/3
S = 1.08	(Δ/σ)max < 0.001
2765 reflections	Δρmax = 0.22 e Å^−3
168 parameters	Δρmin = −0.22 e Å^−3

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Zn1	0.5000	0.75993 (2)	0.7500	0.04673 (13)
N1	0.42976 (13)	0.86884 (12)	0.6097 (2)	0.0560 (5)
C1	0.36392 (18)	0.86814 (18)	0.4692 (3)	0.0689 (7)
H1	0.3393	0.8173	0.4246	0.083*
C2	0.3299 (2)	0.9403 (2)	0.3851 (4)	0.0835 (9)
H2	0.2851	0.9372	0.2855	0.100*
C3	0.3626 (2)	1.0144 (2)	0.4497 (4)	0.0912 (10)
H3	0.3399	1.0630	0.3950	0.109*
C4	0.4307 (2)	1.01866 (16)	0.5991 (4)	0.0762 (8)
C5	0.46363 (16)	0.94306 (13)	0.6741 (3)	0.0556 (5)
C6	0.4676 (3)	1.09407 (18)	0.6787 (5)	0.1086 (14)
H6	0.4458	1.1445	0.6300	0.130*
N11	0.43035 (14)	0.63487 (13)	0.4888 (2)	0.0595 (5)
N12	0.41630 (13)	0.66673 (11)	0.5937 (2)	0.0518 (4)
C11	0.37140 (18)	0.60880 (16)	0.6182 (3)	0.0642 (6)
H11	0.3534	0.6138	0.6863	0.077*
C12	0.3549 (2)	0.54065 (19)	0.5298 (4)	0.0870 (9)
H12	0.3241	0.4925	0.5248	0.104*
C13	0.3939 (2)	0.55958 (19)	0.4513 (4)	0.0830 (9)
H13	0.3950	0.5251	0.3819	0.100*
B1	0.4746 (2)	0.6851 (2)	0.4199 (3)	0.0690 (8)
H1A	0.4381	0.7334	0.3693	0.083*
H1B	0.4782	0.6511	0.3476	0.083*
N13	0.57014 (14)	0.71333 (13)	0.5411 (2)	0.0580 (5)
N14	0.58774 (13)	0.75821 (12)	0.6621 (2)	0.0546 (4)
C14	0.67425 (17)	0.78014 (16)	0.7300 (3)	0.0631 (6)
H24	0.7046	0.8106	0.8173	0.076*
C15	0.71221 (18)	0.75136 (19)	0.6524 (3)	0.0732 (7)
H15	0.7710	0.7589	0.6753	0.088*
C16	0.64476 (18)	0.70945 (19)	0.5346 (3)	0.0695 (7)
H16	0.6497	0.6825	0.4617	0.083*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0499 (2)	0.0432 (2)	0.04314 (19)	0.000	0.02155 (15)	0.000
N1	0.0552 (11)	0.0514 (11)	0.0531 (11)	0.0032 (9)	0.0225 (9)	0.0053 (8)
C1	0.0653 (16)	0.0721 (16)	0.0568 (15)	0.0089 (13)	0.0232 (13)	0.0111 (12)
C2	0.0744 (19)	0.099 (2)	0.0705 (18)	0.0207 (17)	0.0335 (16)	0.0335 (17)
C3	0.081 (2)	0.079 (2)	0.115 (3)	0.0242 (17)	0.052 (2)	0.051 (2)
C4	0.0742 (18)	0.0522 (14)	0.112 (2)	0.0121 (13)	0.0552 (18)	0.0250 (14)
C5	0.0550 (13)	0.0459 (12)	0.0735 (15)	0.0046 (10)	0.0390 (12)	0.0063 (10)
C6	0.104 (3)	0.0439 (14)	0.174 (4)	0.0090 (15)	0.070 (3)	0.0195 (17)
N11	0.0640 (12)	0.0682 (12)	0.0513 (11)	−0.0061 (10)	0.0338 (10)	−0.0125 (9)
N12	0.0583 (11)	0.0524 (10)	0.0486 (10)	−0.0039 (8)	0.0307 (9)	−0.0052 (8)
C11	0.0742 (17)	0.0613 (14)	0.0657 (15)	−0.0147 (12)	0.0425 (14)	−0.0092 (11)
C12	0.110 (3)	0.0628 (16)	0.108 (2)	−0.0286 (17)	0.070 (2)	−0.0235 (16)
C13	0.094 (2)	0.0747 (18)	0.088 (2)	−0.0200 (16)	0.0525 (19)	−0.0387 (16)
B1	0.0674 (18)	0.098 (2)	0.0443 (14)	−0.0064 (16)	0.0308 (14)	−0.0032 (14)
N13	0.0588 (11)	0.0716 (12)	0.0495 (10)	0.0034 (9)	0.0324 (9)	0.0081 (9)
N14	0.0524 (10)	0.0625 (11)	0.0484 (9)	−0.0004 (9)	0.0260 (8)	0.0083 (8)
C14	0.0559 (13)	0.0688 (15)	0.0584 (13)	−0.0027 (11)	0.0256 (12)	0.0166 (11)
C15	0.0540 (13)	0.095 (2)	0.0748 (16)	0.0067 (14)	0.0365 (13)	0.0276 (15)
C16	0.0663 (16)	0.0879 (18)	0.0663 (16)	0.0139 (14)	0.0430 (15)	0.0181 (13)

Geometric parameters (Å, º)

Zn1—N12	2.1454 (18)	N11—N12	1.358 (2)
Zn1—N12^i	2.1454 (18)	N11—B1	1.541 (4)
Zn1—N14	2.1704 (18)	N12—C11	1.328 (3)
Zn1—N14^i	2.1705 (18)	C11—C12	1.372 (4)
Zn1—N1	2.2101 (19)	C11—H11	0.9300
Zn1—N1^i	2.2101 (19)	C12—C13	1.356 (4)
N1—C1	1.323 (3)	C12—H12	0.9300
N1—C5	1.350 (3)	C13—H13	0.9300
C1—C2	1.394 (4)	B1—N13	1.549 (4)
C1—H1	0.9300	B1—H1A	0.9700
C2—C3	1.347 (5)	B1—H1B	0.9700
C2—H2	0.9300	N13—C16	1.341 (3)
C3—C4	1.399 (5)	N13—N14	1.361 (3)
C3—H3	0.9300	N14—C14	1.337 (3)
C4—C5	1.402 (3)	C14—C15	1.379 (4)
C4—C6	1.426 (5)	C14—H24	0.9300
C5—C5^i	1.438 (5)	C15—C16	1.365 (4)
C6—C6^i	1.334 (8)	C15—H15	0.9300
C6—H6	0.9300	C16—H16	0.9300
N11—C13	1.329 (3)
N12—Zn1—N12^i	91.24 (10)	C13—N11—N12	109.0 (2)
N12—Zn1—N14	90.43 (7)	C13—N11—B1	128.0 (2)
N12^i—Zn1—N14	88.55 (7)	N12—N11—B1	122.7 (2)
N12—Zn1—N14^i	88.55 (7)	C11—N12—N11	105.83 (19)
N12^i—Zn1—N14^i	90.43 (7)	C11—N12—Zn1	124.95 (15)
N14—Zn1—N14^i	178.54 (11)	N11—N12—Zn1	123.73 (14)
N12—Zn1—N1	96.92 (7)	N12—C11—C12	111.2 (2)
N12^i—Zn1—N1	171.59 (8)	N12—C11—H11	124.4
N14—Zn1—N1	89.34 (7)	C12—C11—H11	124.4
N14^i—Zn1—N1	91.83 (7)	C13—C12—C11	104.3 (2)
N12—Zn1—N1^i	171.59 (7)	C13—C12—H12	127.9
N12^i—Zn1—N1^i	96.92 (7)	C11—C12—H12	127.9
N14—Zn1—N1^i	91.83 (7)	N11—C13—C12	109.6 (2)
N14^i—Zn1—N1^i	89.34 (7)	N11—C13—H13	125.2
N1—Zn1—N1^i	75.01 (11)	C12—C13—H13	125.2
C1—N1—C5	118.1 (2)	N11—B1—N13	110.5 (2)
C1—N1—Zn1	126.95 (18)	N11—B1—H1A	109.6
C5—N1—Zn1	114.81 (16)	N13—B1—H1A	109.6
N1—C1—C2	122.8 (3)	N11—B1—H1B	109.6
N1—C1—H1	118.6	N13—B1—H1B	109.6
C2—C1—H1	118.6	H1A—B1—H1B	108.1
C3—C2—C1	119.2 (3)	C16—N13—N14	109.1 (2)
C3—C2—H2	120.4	C16—N13—B1	126.7 (2)
C1—C2—H2	120.4	N14—N13—B1	123.6 (2)
C2—C3—C4	120.2 (3)	C14—N14—N13	106.4 (2)
C2—C3—H3	119.9	C14—N14—Zn1	128.16 (17)
C4—C3—H3	119.9	N13—N14—Zn1	123.37 (14)
C3—C4—C5	117.0 (3)	N14—C14—C15	110.5 (2)
C3—C4—C6	124.4 (3)	N14—C14—H24	124.8
C5—C4—C6	118.6 (3)	C15—C14—H24	124.8
N1—C5—C4	122.7 (3)	C16—C15—C14	105.0 (2)
N1—C5—C5^i	117.61 (13)	C16—C15—H15	127.5
C4—C5—C5^i	119.68 (18)	C14—C15—H15	127.5
C6^i—C6—C4	121.61 (19)	N13—C16—C15	109.0 (2)
C6^i—C6—H6	119.2	N13—C16—H16	125.5
C4—C6—H6	119.2	C15—C16—H16	125.5

Symmetry code: (i) −x+1, y, −z+3/2.