Aqua­azido­bis(2,2′-bipyridine)mangan­ese(II) perchlorate

In the title complex, [Mn(N₃)(C₁₀H₈N₂)₂(H₂O)]ClO₄, each Mn atom is surrounded by one O atom from an aqua ligand, one N atom from an azide anion and four N atoms from 2,2′-bipyridine ligands to form a distorted octa­hedral geometry. In the complex, the perchlorate anion acts as a counter-ion to balance the charge.

Key indicators

• Single-crystal X-ray study
• T = 273 K
• Mean [sigma](C-C) = 0.004 Å
• R factor = 0.036
• wR factor = 0.099
• Data-to-parameter ratio = 12.9

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         N5
PLAT242_ALERT_2_C Check Low       Ueq as Compared to Neighbors for         N6
PLAT244_ALERT_4_C Low   'Solvent' Ueq as Compared to Neighbors for        Cl1
PLAT480_ALERT_4_C Long H...A H-Bond Reported H1WB   ..  CL1     ..       2.94 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........          2

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

   0 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
   2 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
   3 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: SMART (Bruker, 2000); cell refinement: SAINT (Bruker, 2000); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Sheldrick, 2000); software used to prepare material for publication: SHELXTL.

Aquaazidobis(2,2'-bipyridine)manganese(II) perchlorate

Crystal data

[Mn(N3)(C10H8N2)2(H2O)]ClO4	F(000) = 1076
Mr = 526.80	Dx = 1.537 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 4474 reflections
a = 9.0144 (3) Å	θ = 2.3–23.6°
b = 14.4325 (5) Å	µ = 0.75 mm^−1
c = 17.5808 (6) Å	T = 273 K
β = 95.570 (2)°	Stylolithic, yellow
V = 2276.47 (13) Å^3	0.20 × 0.18 × 0.12 mm
Z = 4

Data collection

Bruker SMART APEX CCD area-detector diffractometer	4032 independent reflections
Radiation source: fine-focus sealed tube	3086 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.030
ω scans	θmax = 25.1°, θmin = 2.3°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −10→10
Tmin = 0.865, Tmax = 0.916	k = −17→16
14158 measured reflections	l = −20→20

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)] = 0.036	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.099	w = 1/[σ^2(Fo^2) + (0.0454P)^2 + 0.628P] where P = (Fo^2 + 2Fc^2)/3
S = 1.07	(Δ/σ)max < 0.001
4032 reflections	Δρmax = 0.41 e Å^−3
313 parameters	Δρmin = −0.28 e Å^−3
0 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.0026 (6)

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
Mn1	0.55610 (4)	0.25299 (2)	0.17583 (2)	0.04906 (15)
Cl1	0.94740 (8)	0.26444 (5)	0.92632 (4)	0.0608 (2)
C1	0.3660 (3)	0.19050 (19)	0.01992 (17)	0.0645 (7)
H1	0.2897	0.2226	0.0404	0.077*
C2	0.3398 (3)	0.1552 (2)	−0.05286 (17)	0.0726 (8)
H2	0.2478	0.1635	−0.0809	0.087*
C3	0.4513 (4)	0.1076 (2)	−0.08319 (17)	0.0714 (8)
H3	0.4368	0.0833	−0.1323	0.086*
C4	0.5850 (3)	0.09635 (19)	−0.03979 (16)	0.0611 (7)
H4	0.6621	0.0642	−0.0594	0.073*
C5	0.6046 (3)	0.13283 (16)	0.03288 (14)	0.0492 (6)
C6	0.7463 (3)	0.12312 (16)	0.08311 (14)	0.0488 (6)
C7	0.8570 (3)	0.06078 (19)	0.06847 (17)	0.0636 (7)
H7	0.8445	0.0221	0.0260	0.076*
C8	0.9861 (3)	0.0568 (2)	0.11769 (18)	0.0707 (8)
H8	1.0612	0.0152	0.1087	0.085*
C9	1.0024 (3)	0.1137 (2)	0.17901 (18)	0.0683 (8)
H9	1.0895	0.1129	0.2120	0.082*
C10	0.8877 (3)	0.1729 (2)	0.19153 (17)	0.0655 (7)
H10	0.8987	0.2115	0.2341	0.079*
C11	0.7324 (3)	0.4036 (2)	0.08472 (16)	0.0631 (7)
H11	0.7987	0.3550	0.0804	0.076*
C12	0.7699 (4)	0.4899 (2)	0.06010 (16)	0.0723 (8)
H12	0.8603	0.4996	0.0400	0.087*
C13	0.6725 (4)	0.5613 (2)	0.06552 (16)	0.0713 (8)
H13	0.6964	0.6204	0.0496	0.086*
C14	0.5391 (3)	0.54523 (17)	0.09462 (15)	0.0608 (7)
H14	0.4709	0.5931	0.0980	0.073*
C15	0.5074 (3)	0.45679 (15)	0.11883 (13)	0.0474 (6)
C16	0.3681 (3)	0.43368 (16)	0.15270 (14)	0.0503 (6)
C17	0.2491 (3)	0.49481 (19)	0.15268 (18)	0.0692 (8)
H17	0.2540	0.5527	0.1298	0.083*
C18	0.1247 (4)	0.4697 (2)	0.1864 (2)	0.0841 (10)
H18	0.0435	0.5096	0.1856	0.101*
C19	0.1212 (4)	0.3853 (3)	0.2215 (2)	0.0868 (10)
H19	0.0392	0.3678	0.2465	0.104*
C20	0.2406 (3)	0.3270 (2)	0.21913 (19)	0.0748 (8)
H20	0.2374	0.2694	0.2426	0.090*
N1	0.4957 (2)	0.18071 (14)	0.06244 (12)	0.0513 (5)
N2	0.7609 (2)	0.17739 (14)	0.14533 (12)	0.0539 (5)
N3	0.6043 (2)	0.38656 (13)	0.11471 (11)	0.0497 (5)
N4	0.3616 (2)	0.34925 (14)	0.18448 (12)	0.0559 (5)
N5	0.4618 (3)	0.14550 (16)	0.23865 (14)	0.0741 (7)
N6	0.4035 (2)	0.07515 (15)	0.22114 (12)	0.0536 (5)
N7	0.3433 (3)	0.00583 (16)	0.20631 (15)	0.0773 (7)
O2	1.0251 (3)	0.3082 (2)	0.87097 (16)	0.1207 (10)
O3	0.7907 (2)	0.28416 (15)	0.91388 (13)	0.0816 (6)
O4	0.9638 (3)	0.16787 (17)	0.9165 (2)	0.1253 (10)
O5	1.0046 (3)	0.2904 (3)	0.99904 (15)	0.1282 (11)
O1W	0.6817 (3)	0.31373 (14)	0.27566 (14)	0.0700 (6)
H1WA	0.6716	0.3702	0.2746	0.105*
H1WB	0.703 (4)	0.296 (3)	0.314 (2)	0.097 (14)*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mn1	0.0554 (3)	0.0340 (2)	0.0573 (3)	0.00216 (16)	0.00324 (18)	0.00035 (16)
Cl1	0.0573 (4)	0.0543 (4)	0.0698 (5)	−0.0030 (3)	0.0016 (3)	0.0015 (3)
C1	0.0582 (17)	0.0578 (17)	0.076 (2)	0.0029 (13)	−0.0020 (14)	0.0002 (14)
C2	0.0669 (19)	0.076 (2)	0.070 (2)	−0.0037 (16)	−0.0154 (15)	0.0024 (16)
C3	0.075 (2)	0.078 (2)	0.0594 (18)	−0.0054 (16)	−0.0020 (15)	−0.0050 (15)
C4	0.0649 (18)	0.0601 (17)	0.0588 (17)	−0.0020 (13)	0.0089 (14)	−0.0036 (13)
C5	0.0553 (15)	0.0384 (12)	0.0536 (15)	−0.0054 (11)	0.0036 (12)	0.0023 (11)
C6	0.0527 (14)	0.0397 (13)	0.0545 (15)	−0.0001 (11)	0.0074 (11)	0.0024 (11)
C7	0.0661 (18)	0.0561 (16)	0.0694 (18)	0.0060 (14)	0.0104 (14)	−0.0085 (14)
C8	0.0623 (18)	0.0680 (19)	0.082 (2)	0.0187 (15)	0.0088 (16)	0.0012 (16)
C9	0.0536 (17)	0.0699 (19)	0.079 (2)	0.0098 (14)	−0.0045 (14)	−0.0023 (16)
C10	0.0648 (18)	0.0604 (17)	0.0689 (18)	0.0081 (14)	−0.0057 (14)	−0.0090 (14)
C11	0.0643 (18)	0.0601 (17)	0.0655 (18)	−0.0030 (13)	0.0095 (14)	0.0025 (14)
C12	0.073 (2)	0.078 (2)	0.0658 (19)	−0.0206 (17)	0.0081 (15)	0.0106 (16)
C13	0.094 (2)	0.0537 (17)	0.0637 (18)	−0.0221 (17)	−0.0058 (16)	0.0113 (14)
C14	0.083 (2)	0.0400 (14)	0.0566 (16)	−0.0003 (13)	−0.0089 (14)	−0.0006 (12)
C15	0.0602 (15)	0.0374 (12)	0.0424 (13)	−0.0008 (11)	−0.0063 (11)	−0.0030 (10)
C16	0.0583 (15)	0.0402 (13)	0.0506 (14)	0.0054 (11)	−0.0039 (11)	−0.0054 (11)
C17	0.073 (2)	0.0520 (16)	0.081 (2)	0.0178 (14)	−0.0004 (16)	−0.0045 (14)
C18	0.067 (2)	0.080 (2)	0.104 (3)	0.0230 (18)	0.0039 (18)	−0.017 (2)
C19	0.0576 (19)	0.090 (2)	0.116 (3)	0.0015 (18)	0.0245 (18)	−0.017 (2)
C20	0.0636 (19)	0.0636 (18)	0.099 (2)	−0.0054 (15)	0.0183 (17)	0.0033 (17)
N1	0.0526 (12)	0.0423 (11)	0.0585 (13)	0.0007 (9)	0.0019 (10)	0.0004 (9)
N2	0.0554 (13)	0.0436 (11)	0.0615 (13)	0.0043 (9)	−0.0016 (10)	−0.0047 (10)
N3	0.0562 (13)	0.0415 (11)	0.0514 (12)	−0.0001 (9)	0.0056 (10)	0.0015 (9)
N4	0.0540 (13)	0.0462 (12)	0.0680 (14)	0.0010 (10)	0.0086 (11)	0.0007 (10)
N5	0.109 (2)	0.0461 (13)	0.0678 (16)	−0.0167 (13)	0.0106 (14)	0.0064 (11)
N6	0.0661 (14)	0.0425 (13)	0.0522 (13)	0.0124 (11)	0.0046 (10)	0.0090 (10)
N7	0.102 (2)	0.0449 (14)	0.0814 (17)	−0.0060 (13)	−0.0107 (14)	0.0028 (12)
O2	0.0998 (19)	0.154 (3)	0.1075 (19)	−0.0437 (18)	0.0044 (15)	0.0412 (19)
O3	0.0583 (12)	0.0739 (13)	0.1093 (17)	0.0053 (10)	−0.0085 (11)	−0.0107 (12)
O4	0.1015 (19)	0.0608 (15)	0.216 (3)	0.0112 (13)	0.028 (2)	−0.0061 (17)
O5	0.0882 (18)	0.209 (3)	0.0836 (17)	0.0159 (19)	−0.0127 (13)	−0.045 (2)
O1W	0.0953 (16)	0.0469 (11)	0.0638 (14)	0.0108 (10)	−0.0130 (12)	−0.0064 (10)

Geometric parameters (Å, º)

Mn1—N5	2.129 (2)	C9—H9	0.9300
Mn1—O1W	2.179 (2)	C10—N2	1.338 (3)
Mn1—N4	2.254 (2)	C10—H10	0.9300
Mn1—N2	2.253 (2)	C11—N3	1.338 (3)
Mn1—N1	2.269 (2)	C11—C12	1.371 (4)
Mn1—N3	2.2695 (19)	C11—H11	0.9300
Cl1—O5	1.383 (3)	C12—C13	1.362 (4)
Cl1—O2	1.403 (2)	C12—H12	0.9300
Cl1—O4	1.414 (2)	C13—C14	1.372 (4)
Cl1—O3	1.437 (2)	C13—H13	0.9300
C1—N1	1.333 (3)	C14—C15	1.384 (3)
C1—C2	1.376 (4)	C14—H14	0.9300
C1—H1	0.9300	C15—N3	1.345 (3)
C2—C3	1.368 (4)	C15—C16	1.480 (3)
C2—H2	0.9300	C16—N4	1.344 (3)
C3—C4	1.372 (4)	C16—C17	1.389 (4)
C3—H3	0.9300	C17—C18	1.367 (4)
C4—C5	1.377 (4)	C17—H17	0.9300
C4—H4	0.9300	C18—C19	1.367 (5)
C5—N1	1.346 (3)	C18—H18	0.9300
C5—C6	1.487 (3)	C19—C20	1.370 (4)
C6—N2	1.342 (3)	C19—H19	0.9300
C6—C7	1.386 (3)	C20—N4	1.339 (3)
C7—C8	1.383 (4)	C20—H20	0.9300
C7—H7	0.9300	N5—N6	1.171 (3)
C8—C9	1.352 (4)	N6—N7	1.156 (3)
C8—H8	0.9300	O1W—H1WA	0.8200
C9—C10	1.375 (4)	O1W—H1WB	0.74 (4)
N5—Mn1—O1W	94.46 (10)	N2—C10—H10	118.5
N5—Mn1—N4	93.54 (9)	C9—C10—H10	118.5
O1W—Mn1—N4	92.55 (8)	N3—C11—C12	122.7 (3)
N5—Mn1—N2	98.52 (9)	N3—C11—H11	118.7
O1W—Mn1—N2	90.73 (8)	C12—C11—H11	118.7
N4—Mn1—N2	167.21 (8)	C13—C12—C11	119.0 (3)
N5—Mn1—N1	92.69 (9)	C13—C12—H12	120.5
O1W—Mn1—N1	162.65 (8)	C11—C12—H12	120.5
N4—Mn1—N1	102.76 (8)	C12—C13—C14	119.5 (3)
N2—Mn1—N1	72.57 (7)	C12—C13—H13	120.2
N5—Mn1—N3	165.74 (9)	C14—C13—H13	120.2
O1W—Mn1—N3	86.05 (8)	C13—C14—C15	119.0 (3)
N4—Mn1—N3	72.20 (8)	C13—C14—H14	120.5
N2—Mn1—N3	95.72 (7)	C15—C14—H14	120.5
N1—Mn1—N3	90.87 (7)	N3—C15—C14	121.6 (2)
O5—Cl1—O2	110.69 (19)	N3—C15—C16	115.7 (2)
O5—Cl1—O4	110.2 (2)	C14—C15—C16	122.7 (2)
O2—Cl1—O4	107.09 (19)	N4—C16—C17	120.8 (2)
O5—Cl1—O3	111.09 (15)	N4—C16—C15	116.4 (2)
O2—Cl1—O3	110.79 (16)	C17—C16—C15	122.9 (2)
O4—Cl1—O3	106.82 (15)	C18—C17—C16	119.8 (3)
N1—C1—C2	123.0 (3)	C18—C17—H17	120.1
N1—C1—H1	118.5	C16—C17—H17	120.1
C2—C1—H1	118.5	C19—C18—C17	119.2 (3)
C3—C2—C1	118.8 (3)	C19—C18—H18	120.4
C3—C2—H2	120.6	C17—C18—H18	120.4
C1—C2—H2	120.6	C18—C19—C20	118.7 (3)
C2—C3—C4	118.8 (3)	C18—C19—H19	120.6
C2—C3—H3	120.6	C20—C19—H19	120.6
C4—C3—H3	120.6	N4—C20—C19	123.0 (3)
C3—C4—C5	119.9 (3)	N4—C20—H20	118.5
C3—C4—H4	120.1	C19—C20—H20	118.5
C5—C4—H4	120.1	C1—N1—C5	118.1 (2)
N1—C5—C4	121.4 (2)	C1—N1—Mn1	124.51 (18)
N1—C5—C6	115.8 (2)	C5—N1—Mn1	116.97 (16)
C4—C5—C6	122.7 (2)	C10—N2—C6	118.5 (2)
N2—C6—C7	121.0 (2)	C10—N2—Mn1	123.40 (18)
N2—C6—C5	116.1 (2)	C6—N2—Mn1	117.31 (16)
C7—C6—C5	122.9 (2)	C11—N3—C15	118.2 (2)
C8—C7—C6	119.2 (3)	C11—N3—Mn1	123.73 (17)
C8—C7—H7	120.4	C15—N3—Mn1	117.36 (16)
C6—C7—H7	120.4	C20—N4—C16	118.4 (2)
C9—C8—C7	119.6 (3)	C20—N4—Mn1	123.83 (19)
C9—C8—H8	120.2	C16—N4—Mn1	117.74 (16)
C7—C8—H8	120.2	N6—N5—Mn1	133.4 (2)
C8—C9—C10	118.6 (3)	N7—N6—N5	177.4 (3)
C8—C9—H9	120.7	Mn1—O1W—H1WA	109.5
C10—C9—H9	120.7	Mn1—O1W—H1WB	132 (3)
N2—C10—C9	123.0 (3)	H1WA—O1W—H1WB	112.9

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H1WA···N7^i	0.82	1.99	2.802 (3)	169
O1W—H1WB···O3^ii	0.74 (4)	2.18 (4)	2.899 (3)	166 (4)
O1W—H1WB···Cl1^ii	0.74 (4)	2.94 (4)	3.577 (2)	146 (4)

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