catena-Poly[[[aqua­(dipyrido[3,2-a:2′,3′-c]phenazine)cobalt(II)]-μ-succinato] monohydrate]

In the title compound, {[Co(C₄H₄O₄)(C₁₈H₁₀N₄)(H₂O)]·H₂O}_n, each Co^II atom is six-coordinated by two N atoms from one dipyrido[3,2-a:2′,3′-c]phenazine ligand, and by four O atoms from two succinate anions (one chelating bidentate and one monodentate) and one water mol­ecule in a distorted cis-CoN₂O₄ octa­hedral coordination. The Co^II atoms are bridged by the succinate ligands to generate a helical chain structure. The chain motif is consolidated into a layer structure by O—H...O hydrogen bonds involving the water mol­ecules and carboxyl­ate O atoms.

Key indicators

• Single-crystal X-ray study
• T = 292 K
• Mean [sigma](C-C) = 0.008 Å
• R factor = 0.074
• wR factor = 0.211
• Data-to-parameter ratio = 15.3

checkCIF/PLATON results

No syntax errors found



Alert level B
DIFMX01_ALERT_2_B  The maximum difference density is > 0.1*ZMAX*1.00
            _refine_diff_density_max given =      3.078
            Test value =      2.700
PLAT094_ALERT_2_B Ratio of Maximum / Minimum Residual Density ....       7.12
PLAT097_ALERT_2_B Maximum (Positive) Residual Density ............       3.08 e/A   

Alert level C
DIFMX02_ALERT_1_C  The maximum difference density is > 0.1*ZMAX*0.75
            The relevant atom site should be identified.
PLAT341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ...          7

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

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

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Computing details

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: PROCESS-AUTO; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL-Plus (Sheldrick, 1990); software used to prepare material for publication: SHELXL97.

catena-Poly[[[aqua(dipyrido[3,2 - a:2',3'-c]phenazine)cobalt(II)]-µ-succinato] monohydrate]

Crystal data

[Co(C4H4O4)(C18H10N4)(H2O)]·H2O	F(000) = 1012
Mr = 493.33	Dx = 1.569 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 12823 reflections
a = 8.6818 (17) Å	θ = 3.0–27.5°
b = 7.8022 (16) Å	µ = 0.87 mm^−1
c = 30.968 (6) Å	T = 292 K
β = 95.27 (3)°	Block, red
V = 2088.9 (7) Å^3	0.31 × 0.27 × 0.24 mm
Z = 4

Data collection

Rigaku R-AXIS RAPID diffractometer	4741 independent reflections
Radiation source: rotorating anode	3215 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.074
Detector resolution: 10.0 pixels mm^-1	θmax = 27.5°, θmin = 3.3°
ω scans	h = −11→11
Absorption correction: multi-scan (ABSCOR; Higashi, 1995)	k = −9→10
Tmin = 0.759, Tmax = 0.816	l = −40→37
18973 measured reflections

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.074	Hydrogen site location: difmap and geom
wR(F^2) = 0.211	H atoms treated by a mixture of independent and constrained refinement
S = 1.04	w = 1/[σ^2(Fo^2) + (0.11P)^2 + 1.9763P] where P = (Fo^2 + 2Fc^2)/3
4741 reflections	(Δ/σ)max = 0.001
310 parameters	Δρmax = 3.08 e Å^−3
5 restraints	Δρmin = −0.43 e Å^−3

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
C1	0.1687 (5)	0.2986 (6)	0.73657 (15)	0.0430 (10)
C2	0.1010 (5)	0.4481 (6)	0.71048 (15)	0.0475 (11)
H2A	−0.0087	0.4545	0.7140	0.057*
H2B	0.1119	0.4266	0.6801	0.057*
C3	0.1738 (6)	0.6196 (6)	0.72261 (15)	0.0472 (11)
H3A	0.1130	0.7095	0.7076	0.057*
H3B	0.1706	0.6376	0.7535	0.057*
C4	0.3369 (5)	0.6341 (5)	0.71182 (13)	0.0382 (9)
C5	0.2173 (6)	−0.0034 (6)	0.87933 (15)	0.0485 (11)
H5	0.2058	−0.0934	0.8596	0.058*
C6	0.1530 (7)	−0.0185 (7)	0.91811 (17)	0.0585 (13)
H6	0.0989	−0.1169	0.9244	0.070*
C7	0.1703 (7)	0.1159 (7)	0.94796 (16)	0.0578 (13)
H7	0.1284	0.1075	0.9745	0.069*
C8	0.2501 (6)	0.2615 (6)	0.93777 (14)	0.0465 (11)
C9	0.3133 (5)	0.2650 (5)	0.89771 (13)	0.0390 (9)
C10	0.4001 (5)	0.4130 (5)	0.88498 (12)	0.0380 (9)
C11	0.5328 (6)	0.5404 (6)	0.83269 (14)	0.0472 (11)
H11	0.5693	0.5377	0.8054	0.057*
C12	0.5603 (7)	0.6857 (6)	0.85834 (16)	0.0532 (13)
H12	0.6159	0.7774	0.8485	0.064*
C13	0.5053 (7)	0.6921 (6)	0.89786 (16)	0.0519 (12)
H13	0.5229	0.7886	0.9152	0.062*
C14	0.4228 (6)	0.5550 (6)	0.91247 (13)	0.0428 (10)
C15	0.3547 (6)	0.5556 (6)	0.95388 (13)	0.0452 (11)
C16	0.2701 (6)	0.4100 (7)	0.96631 (13)	0.0471 (11)
C17	0.2216 (7)	0.5495 (8)	1.02874 (15)	0.0628 (15)
C18	0.3077 (7)	0.6920 (7)	1.01627 (15)	0.0590 (14)
C19	0.3243 (8)	0.8376 (8)	1.04357 (17)	0.0727 (18)
H19	0.3806	0.9318	1.0354	0.087*
C20	0.2579 (9)	0.8397 (11)	1.0818 (2)	0.085 (2)
H20	0.2681	0.9356	1.0997	0.102*
C21	0.1750 (9)	0.6984 (12)	1.09397 (18)	0.090 (3)
H21	0.1315	0.7017	1.1203	0.108*
C22	0.1544 (8)	0.5541 (10)	1.06890 (16)	0.0733 (18)
H22	0.0980	0.4615	1.0779	0.088*
N1	0.4560 (4)	0.4050 (4)	0.84584 (11)	0.0394 (8)
N2	0.2953 (5)	0.1355 (5)	0.86886 (12)	0.0422 (8)
N3	0.2040 (5)	0.4069 (6)	1.00327 (12)	0.0573 (11)
N4	0.3752 (5)	0.6932 (5)	0.97869 (12)	0.0534 (11)
O1	0.2278 (4)	0.3294 (4)	0.77472 (10)	0.0508 (8)
O2	0.1612 (4)	0.1528 (4)	0.71977 (11)	0.0553 (9)
O1W	0.3003 (4)	−0.0376 (4)	0.78083 (10)	0.0480 (8)
O3	0.3794 (4)	0.5638 (4)	0.67832 (9)	0.0464 (8)
O2W	−0.0779 (8)	0.0431 (9)	0.65845 (14)	0.113 (2)
H22W	0.006 (7)	0.077 (13)	0.677 (2)	0.170*
H21W	−0.139 (9)	−0.017 (12)	0.676 (2)	0.170*
O4	0.4358 (4)	0.7225 (4)	0.73540 (10)	0.0468 (8)
Co1	0.39350 (7)	0.18197 (7)	0.809548 (17)	0.0385 (2)
H11W	0.230 (5)	0.002 (6)	0.7585 (13)	0.058*
H12W	0.349 (6)	−0.125 (5)	0.7674 (15)	0.058*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
C1	0.034 (2)	0.048 (2)	0.048 (2)	−0.0015 (19)	0.0039 (18)	−0.002 (2)
C2	0.032 (2)	0.059 (3)	0.051 (2)	−0.001 (2)	0.0002 (19)	−0.002 (2)
C3	0.046 (3)	0.045 (2)	0.051 (2)	0.009 (2)	0.011 (2)	0.006 (2)
C4	0.041 (2)	0.0334 (19)	0.041 (2)	0.0057 (18)	0.0063 (18)	0.0067 (17)
C5	0.046 (3)	0.045 (2)	0.054 (3)	0.000 (2)	0.001 (2)	0.004 (2)
C6	0.062 (4)	0.055 (3)	0.061 (3)	−0.007 (3)	0.013 (3)	0.015 (2)
C7	0.061 (4)	0.068 (3)	0.047 (2)	−0.003 (3)	0.014 (2)	0.014 (2)
C8	0.045 (3)	0.054 (3)	0.041 (2)	0.010 (2)	0.0051 (19)	0.010 (2)
C9	0.041 (2)	0.040 (2)	0.036 (2)	0.0066 (18)	0.0037 (17)	0.0032 (18)
C10	0.044 (3)	0.037 (2)	0.0330 (19)	0.0057 (18)	−0.0005 (17)	0.0003 (17)
C11	0.062 (3)	0.043 (2)	0.039 (2)	0.000 (2)	0.015 (2)	0.0013 (19)
C12	0.073 (4)	0.039 (2)	0.048 (3)	−0.008 (2)	0.013 (2)	0.001 (2)
C13	0.070 (4)	0.038 (2)	0.047 (2)	−0.002 (2)	0.001 (2)	−0.0068 (19)
C14	0.044 (3)	0.045 (2)	0.038 (2)	0.008 (2)	0.0016 (18)	0.0001 (19)
C15	0.049 (3)	0.052 (3)	0.0333 (19)	0.014 (2)	0.0003 (18)	−0.0022 (19)
C16	0.044 (3)	0.066 (3)	0.0307 (19)	0.012 (2)	0.0022 (18)	0.001 (2)
C17	0.060 (4)	0.093 (4)	0.035 (2)	0.030 (3)	0.001 (2)	−0.002 (3)
C18	0.062 (3)	0.077 (4)	0.036 (2)	0.023 (3)	−0.005 (2)	−0.008 (2)
C19	0.079 (5)	0.088 (4)	0.047 (3)	0.024 (3)	−0.010 (3)	−0.026 (3)
C20	0.092 (5)	0.114 (6)	0.047 (3)	0.037 (5)	0.000 (3)	−0.025 (3)
C21	0.086 (5)	0.147 (7)	0.037 (3)	0.044 (5)	0.009 (3)	−0.018 (4)
C22	0.066 (4)	0.112 (5)	0.043 (3)	0.018 (4)	0.011 (2)	−0.003 (3)
N1	0.040 (2)	0.0422 (19)	0.0360 (17)	0.0015 (16)	0.0046 (15)	0.0025 (15)
N2	0.042 (2)	0.0414 (18)	0.0436 (19)	0.0028 (16)	0.0071 (16)	0.0005 (16)
N3	0.055 (3)	0.080 (3)	0.0379 (19)	0.010 (2)	0.0106 (18)	0.003 (2)
N4	0.063 (3)	0.058 (2)	0.0384 (19)	0.015 (2)	−0.0003 (18)	−0.0111 (18)
O1	0.057 (2)	0.0472 (18)	0.0468 (17)	0.0088 (16)	−0.0031 (15)	−0.0103 (14)
O2	0.056 (2)	0.0508 (19)	0.0579 (19)	−0.0029 (16)	−0.0010 (16)	−0.0129 (16)
O1W	0.051 (2)	0.0415 (17)	0.0531 (18)	−0.0037 (15)	0.0120 (15)	−0.0127 (15)
O3	0.049 (2)	0.0514 (17)	0.0399 (15)	−0.0001 (15)	0.0092 (14)	−0.0075 (14)
O2W	0.095 (4)	0.177 (6)	0.065 (3)	−0.063 (4)	−0.004 (3)	−0.010 (3)
O4	0.052 (2)	0.0444 (16)	0.0451 (16)	−0.0013 (15)	0.0114 (15)	−0.0088 (14)
Co1	0.0426 (4)	0.0365 (3)	0.0369 (3)	−0.0002 (2)	0.0068 (2)	−0.0037 (2)

Geometric parameters (Å, º)

C1—O2	1.250 (5)	C12—H12	0.9300
C1—O1	1.267 (5)	C13—C14	1.386 (7)
C1—C2	1.507 (6)	C13—H13	0.9300
C2—C3	1.512 (7)	C14—C15	1.460 (6)
C2—H2A	0.9700	C15—N4	1.323 (6)
C2—H2B	0.9700	C15—C16	1.425 (7)
C3—C4	1.489 (7)	C16—N3	1.327 (6)
C3—H3A	0.9700	C17—N3	1.364 (7)
C3—H3B	0.9700	C17—C18	1.413 (9)
C4—O3	1.258 (5)	C17—C22	1.421 (7)
C4—O4	1.277 (6)	C18—N4	1.350 (7)
C4—Co1^i	2.518 (5)	C18—C19	1.415 (7)
C5—N2	1.334 (6)	C19—C20	1.365 (9)
C5—C6	1.375 (7)	C19—H19	0.9300
C5—H5	0.9300	C20—C21	1.388 (11)
C6—C7	1.397 (8)	C20—H20	0.9300
C6—H6	0.9300	C21—C22	1.370 (10)
C7—C8	1.382 (7)	C21—H21	0.9300
C7—H7	0.9300	C22—H22	0.9300
C8—C9	1.402 (6)	Co1—N1	2.115 (4)
C8—C16	1.458 (7)	Co1—N2	2.126 (4)
C9—N2	1.348 (6)	Co1—O1	2.067 (3)
C9—C10	1.453 (6)	Co1—O1W	2.061 (3)
C10—N1	1.348 (5)	Co1—O3^ii	2.177 (3)
C10—C14	1.400 (6)	Co1—O4^ii	2.147 (3)
C11—N1	1.332 (6)	O1W—H11W	0.93 (4)
C11—C12	1.392 (6)	O1W—H12W	0.92 (4)
C11—H11	0.9300	O2W—H22W	0.92 (7)
C12—C13	1.355 (7)	O2W—H21W	0.92 (7)
O2—C1—O1	124.2 (4)	C16—C15—C14	119.7 (4)
O2—C1—C2	118.6 (4)	N3—C16—C15	121.5 (4)
O1—C1—C2	117.2 (4)	N3—C16—C8	118.1 (5)
C1—C2—C3	114.7 (4)	C15—C16—C8	120.4 (4)
C1—C2—H2A	108.6	N3—C17—C18	121.1 (5)
C3—C2—H2A	108.6	N3—C17—C22	119.6 (6)
C1—C2—H2B	108.6	C18—C17—C22	119.3 (6)
C3—C2—H2B	108.6	N4—C18—C17	121.5 (5)
H2A—C2—H2B	107.6	N4—C18—C19	118.7 (6)
C4—C3—C2	113.3 (4)	C17—C18—C19	119.7 (5)
C4—C3—H3A	108.9	C20—C19—C18	120.0 (7)
C2—C3—H3A	108.9	C20—C19—H19	120.0
C4—C3—H3B	108.9	C18—C19—H19	120.0
C2—C3—H3B	108.9	C19—C20—C21	119.8 (6)
H3A—C3—H3B	107.7	C19—C20—H20	120.1
O3—C4—O4	118.3 (4)	C21—C20—H20	120.1
O3—C4—C3	120.6 (4)	C22—C21—C20	122.9 (6)
O4—C4—C3	121.1 (4)	C22—C21—H21	118.5
O3—C4—Co1^i	59.9 (2)	C20—C21—H21	118.5
O4—C4—Co1^i	58.5 (2)	C21—C22—C17	118.3 (7)
C3—C4—Co1^i	175.2 (3)	C21—C22—H22	120.9
N2—C5—C6	122.6 (5)	C17—C22—H22	120.9
N2—C5—H5	118.7	C11—N1—C10	118.0 (4)
C6—C5—H5	118.7	C11—N1—Co1	126.9 (3)
C5—C6—C7	119.1 (5)	C10—N1—Co1	114.8 (3)
C5—C6—H6	120.5	C5—N2—C9	118.5 (4)
C7—C6—H6	120.5	C5—N2—Co1	127.0 (3)
C8—C7—C6	119.4 (4)	C9—N2—Co1	114.5 (3)
C8—C7—H7	120.3	C16—N3—C17	116.7 (5)
C6—C7—H7	120.3	C15—N4—C18	116.7 (5)
C7—C8—C9	117.6 (5)	C1—O1—Co1	125.7 (3)
C7—C8—C16	123.3 (4)	Co1—O1W—H11W	104 (3)
C9—C8—C16	119.1 (4)	Co1—O1W—H12W	129 (4)
N2—C9—C8	122.8 (4)	H11W—O1W—H12W	102 (4)
N2—C9—C10	116.5 (4)	C4—O3—Co1^i	90.2 (3)
C8—C9—C10	120.7 (4)	H22W—O2W—H21W	104 (3)
N1—C10—C14	122.8 (4)	C4—O4—Co1^i	91.0 (3)
N1—C10—C9	116.5 (4)	O1W—Co1—O1	90.61 (14)
C14—C10—C9	120.8 (4)	O1W—Co1—N1	169.90 (14)
N1—C11—C12	122.4 (4)	O1—Co1—N1	87.24 (13)
N1—C11—H11	118.8	O1W—Co1—N2	93.36 (14)
C12—C11—H11	118.8	O1—Co1—N2	103.34 (15)
C13—C12—C11	119.2 (5)	N1—Co1—N2	77.57 (14)
C13—C12—H12	120.4	O1W—Co1—O4^ii	96.28 (13)
C11—C12—H12	120.4	O1—Co1—O4^ii	93.93 (14)
C12—C13—C14	120.2 (4)	N1—Co1—O4^ii	93.71 (13)
C12—C13—H13	119.9	N2—Co1—O4^ii	160.12 (15)
C14—C13—H13	119.9	O1W—Co1—O3^ii	92.05 (14)
C13—C14—C10	117.4 (4)	O1—Co1—O3^ii	154.36 (14)
C13—C14—C15	123.2 (4)	N1—Co1—O3^ii	94.16 (14)
C10—C14—C15	119.4 (4)	N2—Co1—O3^ii	101.96 (13)
N4—C15—C16	122.4 (4)	O4^ii—Co1—O3^ii	60.43 (12)
N4—C15—C14	118.0 (5)
C1—C2—C3—C4	67.6 (5)

Symmetry codes: (i) −x+1, y+1/2, −z+3/2; (ii) −x+1, y−1/2, −z+3/2.

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H11W···O2	0.93 (4)	1.75 (3)	2.612 (5)	154 (5)
O1W—H12W···O4^iii	0.92 (4)	1.76 (2)	2.678 (4)	172 (5)
O2W—H21W···O1^iv	0.92 (7)	2.14 (8)	3.041 (6)	165 (9)
O2W—H22W···O2	0.92 (7)	1.90 (6)	2.815 (6)	173 (10)

Symmetry codes: (iii) x, y−1, z; (iv) −x, y−1/2, −z+3/2.