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In the crystal structure of the title compound, [Mn(C10H14O4)(C12H8N2)(H2O)2]·3H2O, the MnII atom is in a distorted octahedral geometry, being coordinated by two N atoms of one 1,10-phenanthroline ligand, two O atoms from two carboxyl­ate groups of the chelating cyclo­hexane-1,1′-di­acetate dianion and two O atoms of two trans water mol­ecules. The complex mol­ecules are linked to form a three-dimensional network by hydrogen-bonding interactions between coordinated water mol­ecules, non-coordinated water mol­ecules and carboxyl­ate groups of neighbouring mol­ecules, and by aromatic π–π stacking interactions of the phenthroline rings.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536805019665/ci6595sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536805019665/ci6595Isup2.hkl
Contains datablock I

CCDC reference: 229796

Key indicators

  • Single-crystal X-ray study
  • T = 297 K
  • Mean [sigma](C-C) = 0.004 Å
  • R factor = 0.035
  • wR factor = 0.075
  • Data-to-parameter ratio = 18.2

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.98 Ratio PLAT232_ALERT_2_C Hirshfeld Test Diff (M-X) Mn1 - N2 .. 6.24 su PLAT241_ALERT_2_C Check High Ueq as Compared to Neighbors for C18
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 2 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

Computing details top

Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2004); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: ORTEP-3 for Windows (Farrugia, 1997); software used to prepare material for publication: CrystalStructure.

Diaqua(cyclohexane-1,1-diacetato-κ2O,O')(phenanthroline- κ2N,N')manganese(II) trihydrate top
Crystal data top
[Mn(C12H8N2)(C10H14O4)(H2O)2]·3H2OF(000) = 1100.00
Mr = 523.44Dx = 1.414 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.7107 Å
Hall symbol: -P 2ybcCell parameters from 14069 reflections
a = 7.8763 (3) Åθ = 2.3–27.4°
b = 25.0242 (7) ŵ = 0.59 mm1
c = 12.7232 (3) ÅT = 297 K
β = 101.275 (1)°Block, yellow
V = 2459.3 (1) Å30.21 × 0.18 × 0.17 mm
Z = 4
Data collection top
Rigaku R-AXIS RAPID
diffractometer
3284 reflections with F2 > 2σ(F2)
Detector resolution: 10.00 pixels mm-1Rint = 0.045
ω scansθmax = 27.5°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 1010
Tmin = 0.801, Tmax = 0.905k = 3232
23941 measured reflectionsl = 1416
5611 independent reflections
Refinement top
Refinement on F2 w = 1/[0.0003Fo2 + σ(Fo2)]/(4Fo2)
R[F2 > 2σ(F2)] = 0.035(Δ/σ)max < 0.001
wR(F2) = 0.075Δρmax = 0.45 e Å3
S = 1.02Δρmin = 0.42 e Å3
5611 reflectionsExtinction correction: Larson (1970)
308 parametersExtinction coefficient: 11.4 (7)
H-atom parameters constrained
Special details top

Geometry. ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY

Refinement. Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F2. R-factor (gt) are based on F. The threshold expression of F2 > 2.0 σ(F2) is used only for calculating R-factor (gt).

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/Ueq
Mn10.24115 (4)0.33149 (1)0.52464 (2)0.03614 (8)
O10.3845 (2)0.28331 (5)0.6454 (1)0.0459 (4)
O20.4695 (2)0.22033 (6)0.7633 (1)0.0480 (4)
O30.1056 (2)0.27555 (5)0.4160 (1)0.0436 (4)
O40.0319 (2)0.20698 (5)0.3091 (1)0.0467 (4)
O50.4683 (2)0.33129 (5)0.4469 (1)0.0439 (4)
O60.0181 (2)0.33448 (5)0.6079 (1)0.0465 (4)
O70.7465 (2)0.26586 (6)0.5309 (1)0.0661 (5)
O80.7989 (2)0.20491 (6)0.7141 (1)0.0697 (6)
O90.6930 (2)0.30735 (6)0.8579 (1)0.0702 (6)
N10.3556 (2)0.40671 (6)0.6129 (1)0.0409 (5)
N20.1320 (2)0.40264 (6)0.4215 (1)0.0410 (5)
C10.4674 (3)0.40789 (9)0.7061 (2)0.0559 (7)
C20.5382 (4)0.4551 (1)0.7520 (2)0.0737 (9)
C30.4928 (4)0.5021 (1)0.7013 (2)0.073 (1)
C40.3752 (3)0.50306 (8)0.6029 (2)0.0573 (8)
C50.3182 (4)0.55073 (9)0.5448 (3)0.078 (1)
C60.2052 (4)0.54872 (9)0.4517 (3)0.079 (1)
C70.1361 (3)0.49916 (8)0.4058 (2)0.0588 (8)
C80.0178 (4)0.4947 (1)0.3085 (2)0.077 (1)
C90.0388 (4)0.4462 (1)0.2707 (2)0.076 (1)
C100.0203 (3)0.4007 (1)0.3289 (2)0.0574 (7)
C110.1899 (3)0.45127 (7)0.4603 (2)0.0420 (6)
C120.3103 (3)0.45317 (7)0.5614 (2)0.0420 (6)
C130.3639 (3)0.23813 (7)0.6845 (1)0.0333 (5)
C140.2111 (3)0.20394 (7)0.6352 (1)0.0333 (5)
C150.2431 (3)0.16524 (7)0.5460 (1)0.0348 (5)
C160.3976 (3)0.12878 (8)0.5897 (1)0.0521 (7)
C170.4172 (4)0.08185 (9)0.5171 (2)0.081 (1)
C180.2520 (5)0.04928 (9)0.4889 (2)0.099 (1)
C190.0988 (4)0.08463 (9)0.4403 (2)0.0750 (9)
C200.0807 (3)0.13036 (8)0.5163 (2)0.0500 (6)
C210.2815 (3)0.19643 (7)0.4480 (1)0.0340 (5)
C220.1303 (3)0.22845 (7)0.3866 (1)0.0333 (5)
H10.50080.37420.74380.067*
H20.62030.45470.82060.089*
H30.54180.53570.73330.092*
H40.36350.58540.57340.102*
H50.16720.58210.41400.104*
H60.02310.52700.26800.097*
H70.12120.44320.20250.091*
H80.02250.36580.30080.069*
H90.17940.18250.69200.040*
H100.11580.22740.60540.039*
H110.50270.15000.59870.060*
H120.38360.11500.65870.061*
H130.44680.09540.45160.094*
H140.50940.05880.55330.093*
H150.26730.02210.43720.112*
H160.22870.03230.55310.112*
H170.11740.09920.37290.086*
H180.00620.06330.42780.086*
H190.05530.11530.58170.058*
H200.01500.15270.48230.058*
H210.37640.22080.47310.040*
H220.31600.17080.39890.041*
H230.56870.31050.47550.054*
H240.45370.31850.37750.054*
H250.04670.32260.67540.057*
H260.07330.31360.57040.057*
H270.75260.24100.48090.079*
H280.75260.24900.58990.079*
H290.88610.22350.75130.083*
H300.70610.21250.74730.082*
H310.79390.30450.82720.083*
H320.60690.28260.81720.084*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0396 (2)0.0267 (1)0.0420 (2)0.0003 (1)0.0075 (1)0.0007 (1)
O10.044 (1)0.0364 (7)0.0525 (8)0.0049 (7)0.0016 (7)0.0066 (6)
O20.042 (1)0.0635 (9)0.0337 (7)0.0056 (7)0.0052 (7)0.0124 (6)
O30.042 (1)0.0347 (7)0.0497 (8)0.0056 (6)0.0019 (7)0.0017 (6)
O40.044 (1)0.0583 (8)0.0333 (7)0.0009 (7)0.0027 (7)0.0091 (6)
O50.0443 (9)0.0416 (7)0.0477 (8)0.0017 (7)0.0139 (7)0.0099 (6)
O60.048 (1)0.0469 (8)0.0464 (8)0.0064 (7)0.0130 (7)0.0108 (6)
O70.046 (1)0.093 (1)0.0570 (9)0.002 (1)0.0063 (8)0.0035 (9)
O80.044 (1)0.087 (1)0.074 (1)0.0051 (9)0.0013 (9)0.0219 (9)
O90.049 (1)0.084 (1)0.074 (1)0.0077 (9)0.0033 (9)0.0201 (9)
N10.048 (1)0.0354 (8)0.0409 (9)0.0042 (8)0.0135 (8)0.0019 (7)
N20.045 (1)0.0401 (9)0.0408 (9)0.0078 (8)0.0140 (8)0.0023 (7)
C10.062 (2)0.064 (1)0.042 (1)0.012 (1)0.009 (1)0.006 (1)
C20.076 (2)0.089 (2)0.058 (2)0.030 (2)0.016 (1)0.028 (1)
C30.081 (2)0.064 (2)0.086 (2)0.035 (2)0.043 (2)0.040 (1)
C40.066 (2)0.038 (1)0.082 (2)0.012 (1)0.046 (2)0.014 (1)
C50.102 (3)0.029 (1)0.124 (2)0.008 (1)0.071 (2)0.010 (1)
C60.109 (3)0.033 (1)0.119 (2)0.019 (1)0.076 (2)0.023 (1)
C70.069 (2)0.045 (1)0.075 (2)0.024 (1)0.047 (1)0.023 (1)
C80.084 (2)0.084 (2)0.073 (2)0.049 (2)0.041 (2)0.041 (2)
C90.071 (2)0.107 (2)0.049 (1)0.039 (2)0.014 (1)0.020 (1)
C100.053 (2)0.072 (2)0.047 (1)0.018 (1)0.008 (1)0.001 (1)
C110.048 (1)0.034 (1)0.052 (1)0.0108 (9)0.030 (1)0.0100 (9)
C120.049 (1)0.031 (1)0.055 (1)0.0013 (9)0.030 (1)0.0039 (9)
C130.031 (1)0.040 (1)0.029 (1)0.0018 (8)0.0067 (9)0.0018 (8)
C140.032 (1)0.0347 (9)0.0328 (9)0.0003 (8)0.0060 (8)0.0034 (8)
C150.037 (1)0.0303 (9)0.034 (1)0.0022 (9)0.0014 (9)0.0012 (8)
C160.062 (2)0.045 (1)0.045 (1)0.019 (1)0.001 (1)0.0028 (9)
C170.108 (3)0.054 (1)0.072 (2)0.044 (2)0.004 (2)0.005 (1)
C180.158 (3)0.037 (1)0.086 (2)0.014 (2)0.012 (2)0.014 (1)
C190.108 (3)0.044 (1)0.063 (2)0.020 (1)0.007 (2)0.005 (1)
C200.059 (2)0.041 (1)0.045 (1)0.014 (1)0.003 (1)0.0035 (9)
C210.033 (1)0.035 (1)0.033 (1)0.0036 (9)0.0044 (9)0.0035 (8)
C220.033 (1)0.038 (1)0.0291 (9)0.0022 (9)0.0078 (9)0.0025 (8)
Geometric parameters (Å, º) top
Mn1—O12.101 (1)C19—C201.522 (3)
Mn1—O32.105 (1)C21—C221.518 (2)
Mn1—O52.207 (2)O5—H230.96
Mn1—O62.224 (2)O5—H240.92
Mn1—N12.285 (2)O6—H250.89
Mn1—N22.278 (2)O6—H260.94
O1—C131.258 (2)O7—H270.90
O2—C131.252 (2)O7—H280.85
O3—C221.263 (2)O8—H290.88
O4—C221.250 (2)O8—H300.93
N1—C11.332 (2)O9—H310.95
N1—C121.348 (2)O9—H320.99
N2—C101.326 (3)C1—H10.98
N2—C111.358 (2)C2—H20.98
C1—C21.386 (3)C3—H30.98
C2—C31.355 (4)C5—H40.98
C3—C41.404 (4)C6—H50.98
C4—C51.429 (3)C8—H60.98
C4—C121.412 (3)C9—H70.98
C5—C61.337 (4)C10—H80.98
C6—C71.432 (3)C14—H90.97
C7—C81.401 (3)C14—H100.97
C7—C111.408 (3)C16—H110.97
C8—C91.348 (4)C16—H120.97
C9—C101.388 (4)C17—H130.97
C11—C121.442 (3)C17—H140.97
C13—C141.509 (3)C18—H150.97
C14—C151.549 (3)C18—H160.97
C15—C161.536 (3)C19—H170.97
C15—C201.534 (3)C19—H180.97
C15—C211.551 (3)C20—H190.97
C16—C171.520 (3)C20—H200.97
C17—C181.518 (4)C21—H210.97
C18—C191.526 (4)C21—H220.97
O3—Mn1—O1103.27 (5)C18—C19—C20110.1 (2)
O5—Mn1—O187.70 (5)Mn1—O5—H23120.7998
O6—Mn1—O191.86 (5)Mn1—O5—H24117.9140
N1—Mn1—O190.53 (5)Mn1—O6—H25111.7801
N2—Mn1—O1163.41 (5)Mn1—O6—H26109.6342
Mn1—O1—C13135.4 (1)H24—O5—H2396.5329
O5—Mn1—O393.19 (5)H26—O6—H25109.0152
O6—Mn1—O389.35 (5)H28—O7—H27106.2602
N1—Mn1—O3166.19 (5)H30—O8—H29104.3199
N2—Mn1—O393.20 (5)H32—O9—H31106.2397
Mn1—O3—C22136.7 (1)N1—C1—H1119.0086
O6—Mn1—O5177.46 (5)N2—C10—H8118.5474
N1—Mn1—O586.90 (6)H1—C1—C2118.6156
N2—Mn1—O589.48 (6)C1—C2—H2120.4165
N1—Mn1—O690.60 (6)H2—C2—C3120.0720
N2—Mn1—O690.23 (6)C2—C3—H3120.0424
N2—Mn1—N172.99 (5)H3—C3—C4119.6191
Mn1—N1—C1125.8 (1)C4—C5—H4119.4711
Mn1—N1—C12115.5 (1)H4—C5—C6119.5376
Mn1—N2—C10126.4 (1)C5—C6—H5119.2493
Mn1—N2—C11115.4 (1)H5—C6—C7118.8923
O1—C13—C14120.0 (1)C7—C8—H6119.4795
O1—C13—O2121.3 (2)C8—C9—H7119.9976
O2—C13—C14118.8 (2)H6—C8—C9120.2512
O3—C22—C21119.4 (1)C9—C10—H8118.7761
O3—C22—O4121.8 (2)H7—C9—C10120.3864
O4—C22—C21118.8 (2)C13—C14—H10108.2065
C12—N1—C1118.7 (2)C13—C14—H9107.7132
N1—C1—C2122.4 (2)H10—C14—C15108.4206
N1—C12—C11118.1 (2)H9—C14—C15107.6152
N1—C12—C4122.6 (2)H10—C14—H9109.4601
C11—N2—C10118.2 (2)C15—C16—H11108.4016
N2—C10—C9122.7 (2)C15—C16—H12108.4530
N2—C11—C12118.0 (2)C15—C20—H20108.6699
N2—C11—C7122.4 (2)C15—C20—H19108.1222
C1—C2—C3119.5 (2)C15—C21—H21108.1019
C2—C3—C4120.3 (2)C15—C21—H22107.9410
C3—C4—C12116.5 (2)H11—C16—C17107.9648
C3—C4—C5124.1 (2)H12—C16—C17108.4893
C12—C4—C5119.4 (2)C16—C17—H13108.7582
C4—C5—C6121.0 (2)C16—C17—H14109.0202
C4—C12—C11119.3 (2)H12—C16—H11109.4618
C5—C6—C7121.9 (2)H13—C17—C18108.8615
C6—C7—C11118.9 (2)H14—C17—C18108.7138
C6—C7—C8124.3 (2)C17—C18—H16109.3031
C11—C7—C8116.8 (2)C17—C18—H15108.8268
C7—C8—C9120.3 (2)H14—C17—H13109.4602
C7—C11—C12119.6 (2)C18—C19—H17109.3628
C8—C9—C10119.6 (2)H16—C18—C19109.2431
C13—C14—C15115.3 (2)C18—C19—H18109.1880
C14—C15—C21111.1 (1)H15—C18—C19109.0036
C14—C15—C16109.7 (1)H16—C18—H15109.4558
C14—C15—C20106.8 (2)C19—C20—H20108.1559
C21—C15—C16108.9 (2)H17—C19—C20109.1567
C20—C15—C16108.4 (2)C19—C20—H19108.3184
C15—C16—C17114.0 (2)H18—C19—C20109.5670
C21—C15—C20111.8 (1)H18—C19—H17109.4575
C15—C20—C19114.1 (2)H20—C20—H19109.4561
C15—C21—C22115.0 (2)H21—C21—C22108.2712
C16—C17—C18112.0 (3)H22—C21—C22107.9616
C17—C18—C19111.0 (2)H22—C21—H21109.4666
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O5—H23···O70.961.822.776 (2)175
O5—H24···O2i0.931.772.671 (2)163
O6—H25···O4ii0.901.882.744 (2)162
O6—H26···O7iii0.941.852.769 (2)165
O7—H27···O9i0.901.962.831 (2)163
O7—H28···O80.851.902.748 (2)170
O8—H29···O3iv0.892.443.201 (2)144
O8—H29···O4iv0.892.132.970 (2)157
O8—H30···O20.931.922.812 (2)158
O9—H31···O4iv0.951.952.879 (2)163
O9—H32···O10.992.523.318 (2)138
O9—H32···O20.991.942.909 (2)165
Symmetry codes: (i) x, y+1/2, z1/2; (ii) x, y+1/2, z+1/2; (iii) x1, y, z; (iv) x+1, y+1/2, z+1/2.
 

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