Penta­aqua­disodium bis­(triphenyl­cyano­borate) (caesignost)

In the crystal structure of the title compound, [Na₂(H₂O)₅](C₁₉H₁₅BN)₂, the Na atom is octa­hedrally coordinated by three water mol­ecules and three N atoms of triphenyl­cyano­borate anions. The basic structural unit is composed of two octa­hedra sharing a common face, and this unit is connected by a common edge with the next unit, forming an infinite chain along the crystallographic c axis.

Key indicators

• Single-crystal X-ray study
• T = 293 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.048
• wR factor = 0.140
• Data-to-parameter ratio = 16.6

checkCIF/PLATON results

No syntax errors found



Alert level B
PLAT420_ALERT_2_B D-H Without Acceptor       O1     -   H1B    ...          ?
PLAT420_ALERT_2_B D-H Without Acceptor       O3     -   H3A    ...          ?
PLAT420_ALERT_2_B D-H Without Acceptor       O3     -   H3B    ...          ?

Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT199_ALERT_1_C Check the Reported _cell_measurement_temperature        293 K
PLAT200_ALERT_1_C Check the Reported _diffrn_ambient_temperature .        293 K

   0 ALERT level A = In general: serious problem
   3 ALERT level B = Potentially serious problem
   3 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
   0 ALERT type 4 Improvement, methodology, query or suggestion

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Computing details

Data collection: MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991)'; cell refinement: MSC/AFC Diffractometer Control Software; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: SHELXL97 and PLATON (Spek, 2003).

pentaaquadisodium bis(triphenylcyanoborate)

Crystal data

[Na2(H2O)5](C19H15BN)2	F(000) = 1416
Mr = 672.32	Dx = 1.219 Mg m^−3
Monoclinic, C2/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -C 2yc	Cell parameters from 25 reflections
a = 26.200 (5) Å	θ = 30–35°
b = 14.719 (3) Å	µ = 0.10 mm^−1
c = 9.5537 (19) Å	T = 293 K
β = 96.12 (3)°	Prism, colorless
V = 3663.4 (13) Å^3	0.50 × 0.30 × 0.25 mm
Z = 4

Data collection

Rigaku AFC-7S diffractometer	3134 reflections with I > 2σ(I)
Radiation source: fine-focus sealed tube	Rint = 0.03
Graphite monochromator	θmax = 27.5°, θmin = 2.6°
ω scans	h = 0→34
Absorption correction: ψ scan (TEXSAN; Molecular Structure Corporation, 1999)	k = −19→19
Tmin = 0.95, Tmax = 0.98	l = −12→12
4207 measured reflections	3 standard reflections every 150 reflections
4206 independent reflections	intensity decay: none

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)] = 0.048	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.140	w = 1/[σ^2(Fo^2) + (0.0735P)^2 + 0.6203P] where P = (Fo^2 + 2Fc^2)/3
S = 1.02	(Δ/σ)max < 0.001
4206 reflections	Δρmax = 0.25 e Å^−3
253 parameters	Δρmin = −0.18 e Å^−3
10 restraints	Extinction correction: SHELXL97, Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0052 (8)

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
Na	0.54657 (3)	0.51076 (5)	0.38663 (7)	0.0543 (2)
O1	0.57881 (7)	0.62044 (12)	0.54529 (17)	0.0818 (5)
H1A	0.5982 (10)	0.604 (2)	0.618 (2)	0.106*
H1B	0.5877 (12)	0.6712 (14)	0.519 (3)	0.106*
O2	0.5000	0.39618 (14)	0.2500	0.0637 (5)
H2	0.5170 (9)	0.3691 (16)	0.196 (2)	0.083*
O3	0.62024 (5)	0.43952 (10)	0.31851 (15)	0.0609 (4)
H3A	0.6444 (8)	0.4705 (15)	0.301 (3)	0.079*
H3B	0.6302 (9)	0.3955 (14)	0.367 (2)	0.079*
N1	0.45849 (5)	0.58515 (10)	0.37393 (14)	0.0456 (3)
B	0.37856 (7)	0.70975 (12)	0.33522 (19)	0.0413 (4)
C1	0.42604 (6)	0.63772 (10)	0.35529 (16)	0.0393 (3)
C11	0.39511 (6)	0.79668 (11)	0.24525 (17)	0.0446 (4)
C12	0.36442 (8)	0.87511 (13)	0.2401 (2)	0.0605 (5)
H12A	0.3329	0.87620	0.2949	0.073*
C13	0.37547 (10)	0.95112 (14)	0.1630 (3)	0.0717 (6)
H13A	0.3529	1.0045	0.1606	0.086*
C14	0.41763 (10)	0.95192 (15)	0.0905 (2)	0.0745 (7)
H14A	0.4250	1.0020	0.0404	0.089*
C15	0.44886 (9)	0.87701 (16)	0.0937 (2)	0.0701 (6)
H15A	0.4779	0.87737	0.0449	0.084*
C16	0.43725 (7)	0.80056 (13)	0.16957 (18)	0.0531 (4)
H16A	0.4588	0.7496	0.16950	0.064*
C21	0.32999 (6)	0.65421 (10)	0.25368 (16)	0.0413 (4)
C22	0.30832 (7)	0.67741 (12)	0.11941 (17)	0.0482 (4)
H22A	0.3214	0.7265	0.0754	0.058*
C23	0.26772 (7)	0.62951 (14)	0.0487 (2)	0.0570 (5)
H23A	0.2536	0.6485	−0.044	0.068*
C24	0.24756 (7)	0.55537 (13)	0.1104 (2)	0.0577 (5)
H24A	0.2194	0.5210	0.0606	0.069*
C25	0.26780 (7)	0.53036 (14)	0.2439 (2)	0.0567 (5)
H25A	0.2540	0.4788	0.2886	0.068*
C26	0.30793 (7)	0.57903 (12)	0.31406 (18)	0.0494 (4)
H26A	0.3211	0.5605	0.4080	0.059*
C31	0.37017 (6)	0.74256 (11)	0.49482 (17)	0.0437 (4)
C32	0.32293 (7)	0.74403 (14)	0.5486 (2)	0.0562 (5)
H32A	0.2929	0.7223	0.4906	0.067*
C33	0.31747 (8)	0.77597 (15)	0.6840 (2)	0.0643 (5)
H33A	0.2824	0.77641	0.7193	0.077*
C34	0.35913 (9)	0.80657 (14)	0.7689 (2)	0.0632 (5)
H34A	0.35542	0.8278	0.8610	0.076*
C35	0.40667 (9)	0.80637 (13)	0.7192 (2)	0.0603 (5)
H35A	0.4367	0.8286	0.7786	0.072*
C36	0.41173 (7)	0.77461 (12)	0.58494 (18)	0.0511 (4)
H36A	0.4445	0.77462	0.5531	0.061*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Na	0.0497 (4)	0.0626 (5)	0.0498 (4)	0.0055 (3)	0.0020 (3)	−0.0005 (3)
O1	0.1003 (12)	0.0779 (11)	0.0641 (9)	−0.0356 (10)	−0.0054 (8)	0.0085 (8)
O2	0.0541 (11)	0.0504 (11)	0.0877 (15)	0.000	0.0126 (10)	0.000
O3	0.0530 (8)	0.0613 (8)	0.0683 (9)	0.0020 (6)	0.0053 (6)	0.0208 (7)
N1	0.0431 (7)	0.0438 (7)	0.0498 (8)	0.0072 (6)	0.0042 (6)	−0.0008 (6)
B	0.0408 (9)	0.0402 (9)	0.0428 (9)	0.0103 (7)	0.0042 (7)	−0.0011 (7)
C1	0.0397 (8)	0.0397 (8)	0.0388 (8)	0.0021 (6)	0.0052 (6)	−0.0020 (6)
C11	0.0478 (9)	0.0415 (8)	0.0431 (8)	0.0038 (7)	−0.0025 (7)	−0.0017 (7)
C12	0.0638 (11)	0.0441 (10)	0.0731 (12)	0.0095 (8)	0.0053 (10)	0.0029 (9)
C13	0.0867 (15)	0.0411 (10)	0.0837 (15)	0.0055 (10)	−0.0076 (12)	0.0048 (10)
C14	0.0979 (18)	0.0489 (11)	0.0740 (14)	−0.0147 (11)	−0.0031 (13)	0.0132 (10)
C15	0.0758 (13)	0.0682 (14)	0.0678 (13)	−0.0115 (11)	0.0151 (11)	0.0068 (10)
C16	0.0562 (10)	0.0514 (10)	0.0515 (10)	0.0029 (8)	0.0057 (8)	0.0018 (8)
C21	0.0396 (8)	0.0425 (8)	0.0422 (8)	0.0107 (6)	0.0058 (6)	−0.0023 (6)
C22	0.0560 (10)	0.0452 (9)	0.0428 (8)	0.0069 (7)	0.0026 (7)	0.0002 (7)
C23	0.0626 (11)	0.0611 (11)	0.0442 (9)	0.0081 (9)	−0.0082 (8)	−0.0047 (8)
C24	0.0524 (10)	0.0595 (11)	0.0595 (11)	0.0004 (9)	−0.0018 (8)	−0.0118 (9)
C25	0.0553 (10)	0.0561 (10)	0.0588 (11)	−0.0059 (9)	0.0073 (8)	0.0009 (9)
C26	0.0507 (9)	0.0522 (10)	0.0444 (9)	0.0033 (7)	0.0012 (7)	0.0035 (7)
C31	0.0494 (9)	0.0380 (8)	0.0436 (8)	0.0106 (7)	0.0036 (7)	0.0004 (6)
C32	0.0487 (10)	0.0661 (12)	0.0536 (10)	0.0157 (8)	0.0043 (8)	−0.0093 (9)
C33	0.0639 (12)	0.0733 (13)	0.0578 (11)	0.0188 (10)	0.0153 (9)	−0.0093 (10)
C34	0.0861 (14)	0.0569 (11)	0.0471 (10)	0.0164 (10)	0.0100 (10)	−0.0084 (8)
C35	0.0742 (13)	0.0523 (11)	0.0520 (10)	−0.0013 (9)	−0.0039 (9)	−0.0061 (8)
C36	0.0549 (10)	0.0477 (9)	0.0508 (9)	0.0000 (8)	0.0052 (8)	−0.0029 (8)

Geometric parameters (Å, º)

Na—O1	2.3118 (18)	C15—C16	1.390 (3)
Na—O3	2.3488 (16)	C15—H15A	0.9331
Na—O2	2.3869 (17)	C16—H16A	0.9389
Na—N1	2.5455 (15)	C21—C22	1.389 (2)
Na—N1^i	2.7034 (16)	C21—C26	1.401 (2)
Na—N1^ii	2.7097 (16)	C22—C23	1.390 (3)
O1—H1A	0.851 (17)	C22—H22A	0.9204
O1—H1B	0.828 (17)	C23—C24	1.372 (3)
O2—Na^ii	2.3869 (17)	C23—H23A	0.9657
O2—H2	0.823 (16)	C24—C25	1.379 (3)
O3—H3A	0.812 (16)	C24—H24A	0.9744
O3—H3B	0.823 (16)	C25—C26	1.385 (3)
N1—C1	1.1492 (19)	C25—H25A	0.9611
B—C11	1.626 (2)	C26—H26A	0.9628
B—C1	1.630 (2)	C31—C32	1.390 (2)
B—C31	1.637 (2)	C31—C36	1.396 (2)
B—C21	1.638 (2)	C32—C33	1.398 (3)
C11—C16	1.384 (3)	C32—H32A	0.9663
C11—C12	1.405 (2)	C33—C34	1.365 (3)
C12—C13	1.387 (3)	C33—H33A	1.0114
C12—H12A	1.0233	C34—C35	1.379 (3)
C13—C14	1.365 (3)	C34—H34A	0.9502
C13—H13A	0.9822	C35—C36	1.385 (3)
C14—C15	1.372 (3)	C35—H35A	0.9765
C14—H14A	0.9105	C36—H36A	0.9418
O1—Na—O3	103.87 (7)	C12—C13—H13A	119.9
O1—Na—O2	169.03 (6)	C13—C14—C15	119.7 (2)
O3—Na—O2	85.43 (5)	C13—C14—H14A	120.2
O1—Na—N1	89.83 (7)	C15—C14—H14A	120.2
O3—Na—N1	161.17 (6)	C14—C15—C16	119.9 (2)
O2—Na—N1	82.52 (5)	C14—C15—H15A	120.0
O1—Na—N1^i	81.79 (6)	C16—C15—H15A	120.0
O3—Na—N1^i	96.73 (5)	C11—C16—C15	122.48 (19)
O2—Na—N1^i	91.46 (5)	C11—C16—H16A	118.8
N1—Na—N1^i	97.99 (5)	C15—C16—H16A	118.8
O1—Na—N1^ii	107.39 (6)	C22—C21—C26	115.37 (16)
O3—Na—N1^ii	83.51 (5)	C22—C21—B	122.47 (15)
O2—Na—N1^ii	79.11 (5)	C26—C21—B	122.15 (14)
N1—Na—N1^ii	80.05 (6)	C21—C22—C23	122.71 (18)
N1^i—Na—N1^ii	170.53 (5)	C21—C22—H22A	118.6
Na—O1—H1A	119 (2)	C23—C22—H22A	118.6
Na—O1—H1B	122 (2)	C24—C23—C22	120.31 (18)
H1A—O1—H1B	110 (3)	C24—C23—H23A	119.8
Na—O2—Na^ii	90.09 (8)	C22—C23—H23A	119.8
Na—O2—H2	114.1 (18)	C23—C24—C25	118.80 (18)
Na^ii—O2—H2	106.1 (19)	C23—C24—H24A	120.6
Na—O3—H3A	119.2 (18)	C25—C24—H24A	120.6
Na—O3—H3B	114.6 (17)	C24—C25—C26	120.48 (19)
H3A—O3—H3B	110 (2)	C24—C25—H25A	119.8
C1—N1—Na	161.59 (13)	C26—C25—H25A	119.8
Na—N1—Na^i	82.01 (5)	C25—C26—C21	122.32 (17)
C1—N1—Na^ii	99.60 (11)	C25—C26—H26A	118.8
Na—N1—Na^ii	79.94 (5)	C21—C26—H26A	118.8
Na^i—N1—Na^ii	124.36 (5)	C32—C31—C36	115.69 (16)
C11—B—C1	109.32 (13)	C32—C31—B	124.22 (15)
C11—B—C31	109.28 (13)	C36—C31—B	120.06 (15)
C1—B—C31	105.01 (12)	C31—C32—C33	122.02 (19)
C11—B—C21	112.26 (13)	C31—C32—H32A	119.0
C1—B—C21	106.01 (13)	C33—C32—H32A	119.0
C31—B—C21	114.57 (13)	C34—C33—C32	120.4 (2)
N1—C1—B	177.04 (16)	C34—C33—H33A	119.8
N1—C1—Na^ii	59.06 (10)	C32—C33—H33A	119.8
B—C1—Na^ii	122.42 (10)	C33—C34—C35	119.27 (18)
C16—C11—C12	115.68 (17)	C33—C34—H34A	120.4
C16—C11—B	125.54 (14)	C35—C34—H34A	120.4
C12—C11—B	118.78 (16)	C34—C35—C36	119.9 (2)
C13—C12—C11	122.0 (2)	C34—C35—H35A	120.0
C13—C12—H12A	119.0	C36—C35—H35A	120.0
C11—C12—H12A	119.0	C35—C36—C31	122.67 (19)
C14—C13—C12	120.2 (2)	C35—C36—H36A	118.7
C14—C13—H13A	119.9	C31—C36—H36A	118.7
O1—Na—O2—Na^ii	88.0 (4)	C12—C11—C16—C15	0.3 (3)
O3—Na—O2—Na^ii	−123.58 (4)	B—C11—C16—C15	179.33 (17)
N1—Na—O2—Na^ii	41.92 (4)	C14—C15—C16—C11	−0.8 (3)
N1^i—Na—O2—Na^ii	139.78 (4)	C11—B—C21—C22	3.6 (2)
N1^ii—Na—O2—Na^ii	−39.32 (3)	C1—B—C21—C22	−115.74 (16)
O1—Na—N1—C1	61.0 (4)	C31—B—C21—C22	128.96 (16)
O3—Na—N1—C1	−76.2 (5)	C11—B—C21—C26	−177.41 (14)
O2—Na—N1—C1	−126.9 (4)	C1—B—C21—C26	63.29 (18)
N1^i—Na—N1—C1	142.7 (4)	C31—B—C21—C26	−52.01 (19)
N1^ii—Na—N1—C1	−46.7 (4)	C26—C21—C22—C23	−0.3 (2)
O1—Na—N1—Na^i	−81.69 (5)	B—C21—C22—C23	178.79 (15)
O3—Na—N1—Na^i	141.08 (18)	C21—C22—C23—C24	−0.6 (3)
O2—Na—N1—Na^i	90.43 (5)	C22—C23—C24—C25	0.9 (3)
O1—Na—N1—Na^ii	151.18 (5)	C23—C24—C25—C26	−0.3 (3)
O3—Na—N1—Na^ii	13.9 (2)	C24—C25—C26—C21	−0.7 (3)
O2—Na—N1—Na^ii	−36.70 (4)	C22—C21—C26—C25	0.9 (2)
N1^i—Na—N1—Na^ii	−127.14 (5)	B—C21—C26—C25	−178.16 (16)
N1^ii—Na—N1—Na^ii	43.48 (5)	C11—B—C31—C32	112.26 (18)
Na—N1—C1—Na^ii	87.0 (4)	C1—B—C31—C32	−130.57 (17)
Na^i—N1—C1—Na^ii	−133.52 (10)	C21—B—C31—C32	−14.7 (2)
C1—B—C11—C16	13.9 (2)	C11—B—C31—C36	−65.44 (18)
C31—B—C11—C16	128.35 (17)	C1—B—C31—C36	51.73 (19)
C21—B—C11—C16	−103.41 (18)	C21—B—C31—C36	167.62 (14)
C1—B—C11—C12	−167.06 (15)	C36—C31—C32—C33	0.3 (3)
C31—B—C11—C12	−52.6 (2)	B—C31—C32—C33	−177.50 (17)
C21—B—C11—C12	75.60 (19)	C31—C32—C33—C34	−0.4 (3)
C16—C11—C12—C13	0.6 (3)	C32—C33—C34—C35	0.5 (3)
B—C11—C12—C13	−178.54 (18)	C33—C34—C35—C36	−0.5 (3)
C11—C12—C13—C14	−0.9 (3)	C34—C35—C36—C31	0.4 (3)
C12—C13—C14—C15	0.4 (3)	C32—C31—C36—C35	−0.3 (3)
C13—C14—C15—C16	0.5 (3)	B—C31—C36—C35	177.60 (16)

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

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1—H1A···O3^iii	0.85 (2)	2.04 (2)	2.858 (2)	160 (2)
O1—H1B···C16^ii	0.83 (2)	2.65 (3)	3.352 (3)	143 (2)
O2—H2···O1^iv	0.82 (2)	2.28 (2)	3.001 (2)	146 (2)
O3—H3A···C26^ii	0.81 (2)	2.37 (2)	3.142 (2)	159 (2)
O3—H3B···C31^i	0.82 (2)	2.42 (2)	3.214 (2)	161 (2)

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