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In the title compound, {[Mn(endc)(phen)(H2O)]·H2O}n [phen is 1,10-phenanthroline (C12H8N2) and endc is the endo-norbornene-cis-5,6-dicarboxyl­ate anion (C9H8O4)], each MnII ion is surrounded by two N atoms from a phen ligand, four O atoms from water mol­ecules and two carboxyl­ate groups of two endc anions, with one endc carboxyl­ate group coordinating in a monodentate fashion and the other in a chelating fashion, forming a distorted MnO4N2 octa­hedron. The endc anions act as bridges between MnII ions, resulting in a zigzag chain structure along the [010] axis.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805014017/bh6004sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805014017/bh6004Isup2.hkl
Contains datablock I

CCDC reference: 274330

Key indicators

  • Single-crystal X-ray study
  • T = 298 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.040
  • wR factor = 0.099
  • Data-to-parameter ratio = 12.9

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O6 - H6B ... ?
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 0 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 1 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

Computing details top

Data collection: SMART (Bruker, 2002); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2002); software used to prepare material for publication: SHELXL97.

catena-Poly[[[aqua(1,10-phenanthroline)manganese(II)]-µ-endo-norbornene- cis-5,6-dicarboxylato] monohydrate] top
Crystal data top
[Mn(C9H8O4)(C12H8N2)(H2O)]·H2OF(000) = 932
Mr = 451.33Dx = 1.542 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 4067 reflections
a = 10.941 (3) Åθ = 2.5–24.9°
b = 9.135 (2) ŵ = 0.72 mm1
c = 20.013 (4) ÅT = 298 K
β = 103.605 (4)°Block, pink
V = 1944.1 (8) Å30.27 × 0.23 × 0.21 mm
Z = 4
Data collection top
Bruker APEX CCD area-detector
diffractometer
3501 independent reflections
Radiation source: fine-focus sealed tube3002 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.020
φ and ω scansθmax = 25.3°, θmin = 1.9°
Absorption correction: multi-scan
(SADABS; Bruker, 2002)
h = 139
Tmin = 0.829, Tmax = 0.863k = 910
9928 measured reflectionsl = 2423
Refinement top
Refinement on F2Primary atom site location: structure-invariant direct methods
Least-squares matrix: fullSecondary atom site location: difference Fourier map
R[F2 > 2σ(F2)] = 0.040Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.099H-atom parameters constrained
S = 1.07 w = 1/[σ2(Fo2) + (0.0491P)2 + 0.9627P]
where P = (Fo2 + 2Fc2)/3
3501 reflections(Δ/σ)max < 0.001
271 parametersΔρmax = 0.32 e Å3
0 restraintsΔρmin = 0.25 e Å3
Special details top

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 (Å2) top
xyzUiso*/Ueq
Mn10.54328 (3)0.25324 (4)0.173606 (17)0.03121 (13)
O10.67961 (15)0.41325 (17)0.21165 (8)0.0351 (4)
O20.79614 (16)0.32338 (18)0.30950 (9)0.0427 (4)
O30.60661 (16)0.83219 (17)0.27767 (8)0.0368 (4)
O40.63046 (15)0.61386 (16)0.32313 (8)0.0361 (4)
O50.65970 (19)0.10364 (19)0.24268 (9)0.0565 (5)
H5A0.71030.14860.27230.068*
H5B0.63540.02550.25510.068*
O60.9932 (5)0.1852 (5)0.4001 (3)0.236 (3)
H6A0.95760.22130.36310.283*
H6B0.95650.19620.43100.283*
N10.42814 (18)0.3548 (2)0.07296 (9)0.0336 (4)
N20.60989 (18)0.1488 (2)0.08592 (9)0.0326 (4)
C10.9014 (3)0.7807 (3)0.33231 (16)0.0486 (7)
H10.89900.88780.33440.058*
C20.9013 (3)0.7027 (3)0.39818 (15)0.0520 (7)
H20.87480.74100.43550.062*
C30.9453 (2)0.5704 (3)0.39358 (14)0.0482 (7)
H30.95440.49780.42690.058*
C40.9785 (2)0.5565 (3)0.32502 (13)0.0426 (6)
H41.03990.48020.32190.051*
C50.8544 (2)0.5534 (2)0.26790 (12)0.0338 (5)
H50.88010.55470.22420.041*
C60.7968 (2)0.7077 (2)0.27458 (12)0.0347 (5)
H60.79130.76130.23150.042*
C71.0201 (3)0.7149 (3)0.31557 (17)0.0540 (7)
H7A1.09690.74230.34840.065*
H7B1.02700.73570.26910.065*
C80.7699 (2)0.4200 (2)0.26468 (11)0.0311 (5)
C90.6701 (2)0.7148 (2)0.29258 (11)0.0288 (5)
C100.3362 (2)0.4516 (3)0.06601 (13)0.0414 (6)
H100.31480.48570.10550.050*
C110.2696 (3)0.5054 (3)0.00287 (14)0.0467 (6)
H110.20440.57190.00060.056*
C120.3014 (3)0.4594 (3)0.05549 (13)0.0465 (7)
H120.25910.49570.09810.056*
C130.3983 (2)0.3567 (3)0.05095 (12)0.0391 (6)
C140.4386 (3)0.3027 (3)0.10956 (13)0.0492 (7)
H140.40070.33840.15300.059*
C150.5299 (3)0.2018 (3)0.10306 (13)0.0473 (7)
H150.55390.16840.14200.057*
C160.5906 (2)0.1450 (3)0.03712 (12)0.0383 (6)
C170.6855 (2)0.0385 (3)0.02794 (14)0.0457 (6)
H170.71190.00190.06560.055*
C180.7384 (2)0.0108 (3)0.03668 (14)0.0460 (6)
H180.80090.08200.04370.055*
C190.6976 (2)0.0470 (3)0.09217 (13)0.0409 (6)
H190.73410.01190.13590.049*
C200.5559 (2)0.1972 (2)0.02186 (11)0.0324 (5)
C210.4581 (2)0.3058 (2)0.01486 (11)0.0325 (5)
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0330 (2)0.0325 (2)0.0270 (2)0.00107 (15)0.00467 (15)0.00219 (14)
O10.0355 (9)0.0314 (8)0.0341 (9)0.0038 (7)0.0005 (7)0.0018 (7)
O20.0453 (10)0.0347 (9)0.0415 (10)0.0032 (8)0.0030 (8)0.0073 (8)
O30.0431 (10)0.0274 (8)0.0411 (9)0.0065 (7)0.0122 (7)0.0063 (7)
O40.0385 (9)0.0304 (8)0.0417 (9)0.0027 (7)0.0138 (7)0.0070 (7)
O50.0679 (13)0.0348 (10)0.0528 (11)0.0137 (9)0.0134 (10)0.0148 (8)
O60.237 (6)0.155 (4)0.233 (5)0.068 (4)0.113 (5)0.021 (4)
N10.0356 (11)0.0339 (10)0.0314 (10)0.0014 (9)0.0083 (8)0.0032 (8)
N20.0309 (10)0.0330 (10)0.0321 (10)0.0043 (8)0.0038 (8)0.0012 (8)
C10.0391 (15)0.0310 (13)0.0708 (19)0.0047 (11)0.0034 (13)0.0074 (12)
C20.0433 (16)0.0600 (17)0.0455 (16)0.0031 (13)0.0040 (12)0.0130 (14)
C30.0357 (14)0.0533 (17)0.0481 (16)0.0010 (12)0.0051 (12)0.0004 (13)
C40.0270 (12)0.0393 (14)0.0585 (16)0.0004 (10)0.0043 (11)0.0032 (12)
C50.0305 (12)0.0343 (12)0.0375 (13)0.0002 (10)0.0101 (10)0.0010 (10)
C60.0363 (13)0.0294 (12)0.0377 (13)0.0027 (10)0.0072 (10)0.0048 (10)
C70.0339 (15)0.0512 (16)0.074 (2)0.0115 (12)0.0065 (13)0.0001 (15)
C80.0332 (12)0.0291 (12)0.0318 (12)0.0034 (10)0.0091 (10)0.0012 (10)
C90.0349 (12)0.0267 (11)0.0234 (11)0.0001 (9)0.0041 (9)0.0002 (9)
C100.0438 (15)0.0408 (14)0.0414 (14)0.0023 (12)0.0135 (12)0.0044 (11)
C110.0409 (15)0.0402 (14)0.0562 (17)0.0037 (12)0.0056 (12)0.0111 (13)
C120.0530 (16)0.0404 (14)0.0385 (14)0.0052 (12)0.0046 (12)0.0087 (11)
C130.0503 (15)0.0315 (12)0.0315 (13)0.0101 (11)0.0018 (11)0.0036 (10)
C140.072 (2)0.0453 (15)0.0252 (13)0.0095 (14)0.0020 (12)0.0010 (11)
C150.0690 (19)0.0431 (14)0.0318 (13)0.0115 (14)0.0154 (13)0.0085 (11)
C160.0475 (15)0.0343 (13)0.0337 (13)0.0142 (11)0.0108 (11)0.0083 (10)
C170.0453 (15)0.0447 (15)0.0499 (16)0.0100 (12)0.0168 (13)0.0185 (12)
C180.0354 (14)0.0424 (15)0.0586 (17)0.0022 (12)0.0076 (12)0.0163 (13)
C190.0333 (13)0.0414 (14)0.0432 (14)0.0018 (11)0.0007 (11)0.0028 (11)
C200.0365 (13)0.0283 (11)0.0313 (12)0.0105 (10)0.0060 (10)0.0022 (9)
C210.0391 (13)0.0278 (11)0.0292 (12)0.0102 (10)0.0052 (10)0.0000 (9)
Geometric parameters (Å, º) top
Mn1—O12.0992 (16)C4—C51.556 (3)
Mn1—O52.1384 (18)C4—H40.9800
Mn1—O3i2.2165 (17)C5—C81.522 (3)
Mn1—N22.2633 (19)C5—C61.563 (3)
Mn1—O4i2.3015 (16)C5—H50.9800
Mn1—N12.3045 (19)C6—C91.513 (3)
Mn1—Mn1i5.6983 (10)C6—H60.9800
O1—C81.270 (3)C7—H7A0.9700
O2—C81.243 (3)C7—H7B0.9700
O3—C91.274 (3)C10—C111.391 (3)
O3—Mn1ii2.2165 (17)C10—H100.9300
O4—C91.240 (3)C11—C121.361 (4)
O4—Mn1ii2.3015 (16)C11—H110.9300
O5—H5A0.8200C12—C131.403 (4)
O5—H5B0.8200C12—H120.9300
O6—H6A0.8200C13—C211.404 (3)
O6—H6B0.8200C13—C141.434 (4)
N1—C101.323 (3)C14—C151.343 (4)
N1—C211.356 (3)C14—H140.9300
N2—C191.322 (3)C15—C161.428 (4)
N2—C201.354 (3)C15—H150.9300
C1—C21.499 (4)C16—C171.403 (4)
C1—C71.538 (4)C16—C201.406 (3)
C1—C61.571 (3)C17—C181.363 (4)
C1—H10.9800C17—H170.9300
C2—C31.312 (4)C18—C191.394 (4)
C2—H20.9300C18—H180.9300
C3—C41.505 (4)C19—H190.9300
C3—H30.9300C20—C211.441 (3)
C4—C71.542 (4)
O1—Mn1—O586.91 (7)C1—C6—H6108.5
O1—Mn1—O3i98.63 (6)C1—C7—C492.9 (2)
O5—Mn1—O3i108.27 (7)C1—C7—H7A113.1
O1—Mn1—N2104.11 (7)C4—C7—H7A113.1
O5—Mn1—N288.88 (8)C1—C7—H7B113.1
O3i—Mn1—N2152.23 (7)C4—C7—H7B113.1
O1—Mn1—O4i153.64 (6)H7A—C7—H7B110.5
O5—Mn1—O4i89.91 (7)O2—C8—O1124.8 (2)
O3i—Mn1—O4i57.73 (6)O2—C8—C5120.2 (2)
N2—Mn1—O4i101.98 (6)O1—C8—C5114.80 (19)
O1—Mn1—N1103.44 (6)O4—C9—O3120.5 (2)
O5—Mn1—N1160.44 (7)O4—C9—C6122.1 (2)
O3i—Mn1—N186.83 (7)O3—C9—C6117.35 (19)
N2—Mn1—N172.62 (7)N1—C10—C11123.7 (2)
O4i—Mn1—N187.83 (6)N1—C10—H10118.2
C10—N1—C21117.5 (2)C11—C10—H10118.2
C10—N1—Mn1127.39 (16)C12—C11—C10119.1 (3)
C21—N1—Mn1115.10 (15)C12—C11—H11120.5
C19—N2—C20117.7 (2)C10—C11—H11120.5
C19—N2—Mn1125.63 (16)C11—C12—C13119.5 (2)
C20—N2—Mn1116.63 (15)C11—C12—H12120.2
C2—C1—C7100.5 (2)C13—C12—H12120.2
C2—C1—C6107.1 (2)C12—C13—C21117.4 (2)
C7—C1—C6100.4 (2)C12—C13—C14123.4 (2)
C2—C1—H1115.6C21—C13—C14119.2 (2)
C7—C1—H1115.6C15—C14—C13121.4 (2)
C6—C1—H1115.6C15—C14—H14119.3
C3—C2—C1107.4 (3)C13—C14—H14119.3
C3—C2—H2126.3C14—C15—C16120.8 (2)
C1—C2—H2126.3C14—C15—H15119.6
C2—C3—C4108.3 (3)C16—C15—H15119.6
C2—C3—H3125.9C17—C16—C20117.6 (2)
C4—C3—H3125.9C17—C16—C15122.8 (2)
C3—C4—C7100.0 (2)C20—C16—C15119.6 (2)
C3—C4—C5108.4 (2)C18—C17—C16119.3 (2)
C7—C4—C599.2 (2)C18—C17—H17120.3
C3—C4—H4115.7C16—C17—H17120.3
C7—C4—H4115.7C17—C18—C19119.1 (2)
C5—C4—H4115.7C17—C18—H18120.5
C8—C5—C4117.55 (19)C19—C18—H18120.5
C8—C5—C6118.22 (18)N2—C19—C18123.5 (2)
C4—C5—C6102.72 (18)N2—C19—H19118.2
C8—C5—H5105.7C18—C19—H19118.2
C4—C5—H5105.7N2—C20—C16122.7 (2)
C6—C5—H5105.7N2—C20—C21117.8 (2)
C9—C6—C5117.98 (18)C16—C20—C21119.5 (2)
C9—C6—C1110.9 (2)N1—C21—C13122.8 (2)
C5—C6—C1101.96 (19)N1—C21—C20117.8 (2)
C9—C6—H6108.5C13—C21—C20119.3 (2)
C5—C6—H6108.5
Symmetry codes: (i) x+1, y1/2, z+1/2; (ii) x+1, y+1/2, z+1/2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H5A···O20.821.912.666 (2)152
O5—H5B···O3iii0.821.872.677 (2)169
O6—H6A···O20.822.062.773 (4)145
Symmetry code: (iii) x, y1, z.
 

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