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In the title compound, di­aqua­bis(1,10-phenanthroline-κ2N,N′)­cadmium(II) fumarate tetrahydrate, [Cd(phen)2(H2O)2]L·4H2O where phen is 1,10-phenanthroline (C12H8N2) and L2− is the fumarate anion (C4H2O42−), the cadmium(II) cation is six-coordinated by two water mol­ecules and four N atoms derived from two phen mol­ecules. Each of the two independent L2− anions is located about an inversion centre and they do not coordinate to cadmium(II), acting rather as counter-ions. The water mol­ecules and L2− anions are linked through a complex hydrogen-bonding network to form a three-dimensional structure.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536803014624/tk6116sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536803014624/tk6116Isup2.hkl
Contains datablock I

CCDC reference: 221618

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.005 Å
  • R factor = 0.032
  • wR factor = 0.107
  • Data-to-parameter ratio = 15.6

checkCIF results

No syntax errors found

ADDSYM reports no extra symmetry


Red Alert Alert Level A:
DIFF_020 Alert A _diffrn_standards_interval_count and _diffrn_standards_interval_time are missing. Number of measurements between standards or time (min) between standards.
1 Alert Level A = Potentially serious problem
0 Alert Level B = Potential problem
0 Alert Level C = Please check

Computing details top

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.

(I) top
Crystal data top
[Cd(C12H8N2)2(H2O)2](C4H2O4)·4H2OZ = 2
Mr = 694.96F(000) = 708
Triclinic, P1Dx = 1.576 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.619 (2) ÅCell parameters from 6009 reflections
b = 10.630 (2) Åθ = 1.5–27.4°
c = 13.586 (3) ŵ = 0.81 mm1
α = 95.19 (3)°T = 293 K
β = 95.56 (3)°Block, colorless
γ = 104.94 (3)°0.28 × 0.24 × 0.17 mm
V = 1464.1 (6) Å3
Data collection top
Rigaku R-AXIS RAPID
diffractometer
6613 independent reflections
Radiation source: rotor-target5875 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.049
ω scansθmax = 27.4°, θmin = 1.5°
Absorption correction: multi-scan
(ABSCOR; Higashi, 1995)
h = 013
Tmin = 0.791, Tmax = 0.874k = 1313
14103 measured reflectionsl = 1717
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)] = 0.032Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.107H atoms treated by a mixture of independent and constrained refinement
S = 1.09 w = 1/[σ2(Fo2) + (0.0739P)2]
where P = (Fo2 + 2Fc2)/3
6613 reflections(Δ/σ)max = 0.001
424 parametersΔρmax = 0.65 e Å3
12 restraintsΔρmin = 1.06 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
Cd10.079686 (17)0.260181 (17)0.754618 (13)0.01854 (8)
C10.5191 (3)0.5283 (3)0.5461 (2)0.0242 (6)
H10.57420.61320.55600.029*
C20.4789 (3)0.4635 (3)0.6359 (2)0.0232 (6)
C30.3777 (3)0.0345 (3)0.8956 (2)0.0207 (5)
C40.4918 (3)0.0009 (3)0.9511 (2)0.0210 (5)
H40.55480.02000.91450.025*
C1010.1832 (3)0.4832 (3)0.6010 (2)0.0276 (6)
H1010.23020.53290.65920.033*
C1020.1982 (3)0.5359 (3)0.5101 (3)0.0329 (7)
H1020.25270.61950.50840.039*
C1030.1314 (3)0.4622 (3)0.4248 (2)0.0350 (7)
H1030.14210.49430.36380.042*
C1040.0464 (3)0.3378 (3)0.4284 (2)0.0288 (6)
C1050.0361 (3)0.2930 (3)0.5229 (2)0.0222 (5)
C1060.0316 (4)0.2577 (4)0.3420 (2)0.0389 (8)
H1060.02300.28620.27970.047*
C1070.1166 (4)0.1427 (4)0.3496 (2)0.0372 (8)
H1070.16780.09410.29250.045*
C1080.1305 (3)0.0928 (3)0.4435 (2)0.0272 (6)
C1090.0520 (3)0.1665 (3)0.53008 (19)0.0209 (5)
C1100.2151 (3)0.0282 (3)0.4538 (2)0.0324 (7)
H1100.26920.07870.39860.039*
C1110.2186 (3)0.0725 (3)0.5450 (2)0.0314 (7)
H1110.27460.15320.55260.038*
C1120.1364 (3)0.0053 (3)0.6271 (2)0.0269 (6)
H1120.13850.02590.68890.032*
C2010.2804 (3)0.5310 (3)0.8734 (2)0.0323 (7)
H2010.34440.48990.85730.039*
C2020.3204 (4)0.6601 (3)0.9207 (3)0.0409 (8)
H2020.40910.70370.93540.049*
C2030.2268 (4)0.7206 (3)0.9449 (2)0.0384 (8)
H2030.25150.80590.97700.046*
C2040.0932 (3)0.6539 (3)0.9211 (2)0.0290 (6)
C2050.0611 (3)0.5242 (3)0.87410 (19)0.0229 (6)
C2060.0099 (4)0.7128 (3)0.9424 (2)0.0384 (8)
H2060.01120.79840.97370.046*
C2070.1372 (4)0.6458 (3)0.9177 (3)0.0392 (8)
H2070.20240.68640.93130.047*
C2080.1739 (3)0.5126 (3)0.8706 (2)0.0301 (6)
C2090.0749 (3)0.4517 (3)0.8486 (2)0.0236 (6)
C2100.3042 (3)0.4402 (4)0.8441 (2)0.0390 (8)
H2100.37190.47820.85560.047*
C2110.3328 (3)0.3126 (4)0.8008 (3)0.0413 (8)
H2110.41940.26260.78480.050*
C2120.2283 (3)0.2591 (3)0.7813 (2)0.0320 (7)
H2120.24760.17310.75120.038*
N10.0560 (2)0.1215 (2)0.62059 (17)0.0210 (5)
N20.1046 (2)0.3650 (2)0.60719 (17)0.0218 (5)
N30.1548 (2)0.4650 (2)0.85068 (17)0.0237 (5)
N40.1032 (2)0.3266 (2)0.80411 (17)0.0232 (5)
O10.4886 (2)0.5359 (2)0.71547 (15)0.0300 (5)
O20.4342 (2)0.3398 (2)0.62490 (16)0.0293 (5)
O30.3849 (2)0.0495 (2)0.80548 (14)0.0264 (4)
O40.2830 (2)0.0464 (2)0.94031 (16)0.0311 (5)
OW10.2910 (2)0.2543 (2)0.76376 (16)0.0255 (4)
OW20.0633 (2)0.0931 (2)0.84848 (17)0.0301 (5)
OW30.5130 (3)0.9617 (2)0.65335 (19)0.0410 (6)
OW40.8238 (2)0.9608 (3)0.88344 (18)0.0375 (5)
OW50.6429 (3)0.7919 (3)0.7440 (2)0.0509 (7)
OW60.5821 (3)0.1794 (2)0.5449 (2)0.0405 (6)
H110.316 (4)0.181 (3)0.781 (3)0.061*
H120.338 (4)0.286 (4)0.714 (3)0.061*
H210.136 (3)0.076 (4)0.881 (3)0.061*
H220.015 (3)0.041 (4)0.861 (3)0.061*
H320.544 (4)1.035 (3)0.626 (3)0.061*
H310.467 (4)0.992 (4)0.700 (3)0.061*
H410.767 (4)0.898 (3)0.839 (3)0.061*
H420.795 (4)0.968 (4)0.944 (2)0.061*
H510.589 (4)0.841 (4)0.725 (3)0.061*
H520.589 (4)0.712 (3)0.749 (4)0.061*
H610.532 (4)0.231 (4)0.564 (3)0.061*
H620.560 (4)0.139 (4)0.4831 (18)0.061*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Cd10.01843 (12)0.01945 (11)0.01690 (11)0.00454 (7)0.00003 (7)0.00172 (7)
C10.0215 (13)0.0242 (13)0.0283 (14)0.0044 (11)0.0080 (11)0.0097 (11)
C20.0187 (13)0.0286 (14)0.0245 (14)0.0071 (11)0.0055 (11)0.0090 (11)
C30.0186 (12)0.0206 (12)0.0222 (13)0.0041 (10)0.0000 (10)0.0063 (10)
C40.0167 (12)0.0239 (13)0.0229 (13)0.0054 (10)0.0006 (10)0.0070 (10)
C1010.0209 (13)0.0277 (14)0.0350 (16)0.0057 (11)0.0032 (12)0.0113 (12)
C1020.0237 (15)0.0331 (16)0.0472 (19)0.0100 (12)0.0092 (13)0.0212 (14)
C1030.0368 (17)0.0465 (19)0.0327 (17)0.0210 (15)0.0133 (14)0.0236 (14)
C1040.0305 (15)0.0402 (17)0.0219 (14)0.0174 (13)0.0051 (12)0.0118 (12)
C1050.0194 (12)0.0310 (14)0.0202 (13)0.0131 (11)0.0018 (10)0.0063 (11)
C1060.048 (2)0.057 (2)0.0171 (14)0.0232 (17)0.0012 (13)0.0087 (13)
C1070.0444 (19)0.050 (2)0.0180 (14)0.0201 (16)0.0054 (13)0.0021 (13)
C1080.0246 (14)0.0369 (16)0.0204 (13)0.0138 (12)0.0024 (11)0.0048 (11)
C1090.0187 (12)0.0275 (13)0.0186 (12)0.0109 (11)0.0012 (10)0.0008 (10)
C1100.0243 (14)0.0369 (17)0.0309 (16)0.0084 (13)0.0061 (12)0.0136 (13)
C1110.0228 (14)0.0270 (15)0.0396 (17)0.0023 (12)0.0029 (13)0.0066 (13)
C1120.0256 (14)0.0261 (14)0.0277 (14)0.0046 (11)0.0060 (12)0.0004 (11)
C2010.0287 (15)0.0309 (16)0.0309 (16)0.0007 (12)0.0037 (13)0.0036 (12)
C2020.0399 (19)0.0320 (17)0.0385 (18)0.0100 (14)0.0065 (15)0.0044 (14)
C2030.056 (2)0.0218 (15)0.0297 (16)0.0039 (14)0.0077 (15)0.0000 (12)
C2040.0478 (19)0.0212 (14)0.0188 (13)0.0080 (13)0.0085 (13)0.0052 (10)
C2050.0345 (15)0.0201 (13)0.0156 (12)0.0080 (11)0.0061 (11)0.0050 (10)
C2060.064 (2)0.0248 (15)0.0319 (16)0.0191 (16)0.0129 (16)0.0048 (12)
C2070.059 (2)0.0391 (18)0.0341 (17)0.0329 (17)0.0149 (16)0.0110 (14)
C2080.0356 (16)0.0400 (17)0.0229 (14)0.0229 (14)0.0045 (12)0.0089 (12)
C2090.0316 (15)0.0269 (14)0.0167 (12)0.0128 (12)0.0064 (11)0.0078 (10)
C2100.0339 (17)0.064 (2)0.0296 (16)0.0308 (17)0.0029 (14)0.0081 (15)
C2110.0227 (15)0.065 (2)0.0360 (18)0.0149 (16)0.0025 (13)0.0034 (16)
C2120.0222 (14)0.0416 (18)0.0293 (15)0.0071 (13)0.0022 (12)0.0008 (13)
N10.0198 (11)0.0231 (11)0.0193 (11)0.0055 (9)0.0001 (9)0.0018 (9)
N20.0177 (11)0.0251 (12)0.0235 (11)0.0069 (9)0.0000 (9)0.0067 (9)
N30.0238 (12)0.0245 (12)0.0207 (11)0.0031 (9)0.0041 (9)0.0009 (9)
N40.0195 (11)0.0292 (12)0.0192 (11)0.0071 (9)0.0043 (9)0.0000 (9)
O10.0341 (11)0.0312 (11)0.0251 (10)0.0072 (9)0.0069 (9)0.0063 (8)
O20.0359 (12)0.0248 (10)0.0294 (11)0.0066 (9)0.0125 (9)0.0101 (8)
O30.0284 (10)0.0350 (11)0.0203 (10)0.0151 (9)0.0025 (8)0.0086 (8)
O40.0240 (10)0.0501 (13)0.0262 (11)0.0179 (10)0.0058 (9)0.0146 (9)
OW10.0225 (10)0.0282 (10)0.0307 (11)0.0097 (8)0.0099 (8)0.0133 (8)
OW20.0202 (10)0.0359 (12)0.0368 (12)0.0068 (9)0.0022 (9)0.0206 (9)
OW30.0578 (16)0.0380 (13)0.0361 (13)0.0220 (12)0.0190 (12)0.0096 (10)
OW40.0283 (12)0.0462 (14)0.0321 (12)0.0029 (10)0.0108 (10)0.0038 (10)
OW50.0523 (17)0.0349 (14)0.0564 (17)0.0044 (12)0.0149 (14)0.0031 (12)
OW60.0428 (14)0.0329 (13)0.0460 (14)0.0101 (11)0.0112 (12)0.0004 (11)
Geometric parameters (Å, º) top
Cd1—Ow12.252 (2)C112—N11.324 (4)
Cd1—Ow22.259 (2)C112—H1120.9300
Cd1—N12.340 (2)C201—N31.328 (4)
Cd1—N22.383 (2)C201—C2021.401 (4)
Cd1—N32.338 (2)C201—H2010.9300
Cd1—N42.365 (2)C202—C2031.365 (5)
C1—C1i1.317 (6)C202—H2020.9300
C1—C21.499 (4)C203—C2041.404 (5)
C1—H10.9300C203—H2030.9300
C2—O11.248 (4)C204—C2051.407 (4)
C2—O21.267 (3)C204—C2061.434 (5)
C3—O41.252 (3)C205—N31.355 (4)
C3—O31.256 (3)C205—C2091.443 (4)
C3—C41.503 (4)C206—C2071.349 (6)
C4—C4ii1.327 (5)C206—H2060.9300
C4—H40.9300C207—C2081.438 (5)
C101—N21.332 (4)C207—H2070.9300
C101—C1021.408 (4)C208—C2101.394 (5)
C101—H1010.9300C208—C2091.410 (4)
C102—C1031.361 (5)C209—N41.356 (4)
C102—H1020.9300C210—C2111.373 (5)
C103—C1041.404 (5)C210—H2100.9300
C103—H1030.9300C211—C2121.407 (5)
C104—C1051.414 (4)C211—H2110.9300
C104—C1061.433 (5)C212—N41.328 (4)
C105—N21.349 (4)C212—H2120.9300
C105—C1091.444 (4)OW1—H110.93 (4)
C106—C1071.339 (5)OW1—H120.91 (4)
C106—H1060.9300OW2—H210.92 (4)
C107—C1081.432 (4)OW2—H220.92 (4)
C107—H1070.9300OW3—H320.90 (4)
C108—C1101.394 (5)OW3—H310.92 (4)
C108—C1091.414 (4)OW4—H410.90 (4)
C109—N11.360 (3)OW4—H420.90 (4)
C110—C1111.366 (5)OW5—H510.90 (4)
C110—H1100.9300OW5—H520.91 (4)
C111—C1121.401 (4)OW6—H610.90 (4)
C111—H1110.9300OW6—H620.90 (4)
OW1—Cd1—OW282.59 (8)N1—C112—H112118.6
OW1—Cd1—N1113.70 (8)C111—C112—H112118.6
OW1—Cd1—N289.55 (8)N3—C201—C202122.7 (3)
OW1—Cd1—N387.18 (9)N3—C201—H201118.7
OW1—Cd1—N4156.45 (8)C202—C201—H201118.7
OW2—Cd1—N191.67 (8)C203—C202—C201118.9 (3)
OW2—Cd1—N2156.18 (9)C203—C202—H202120.6
OW2—Cd1—N3112.20 (9)C201—C202—H202120.6
OW2—Cd1—N496.85 (9)C202—C203—C204119.9 (3)
N1—Cd1—N270.94 (8)C202—C203—H203120.1
N1—Cd1—N3150.62 (9)C204—C203—H203120.1
N1—Cd1—N489.84 (8)C203—C204—C205117.8 (3)
N2—Cd1—N389.70 (9)C203—C204—C206122.7 (3)
N2—Cd1—N499.17 (8)C205—C204—C206119.5 (3)
N3—Cd1—N471.15 (9)N3—C205—C204121.8 (3)
C1i—C1—C2123.6 (3)N3—C205—C209118.5 (2)
C1i—C1—H1118.2C204—C205—C209119.7 (3)
C2—C1—H1118.2C207—C206—C204120.9 (3)
O1—C2—O2124.8 (3)C207—C206—H206119.6
O1—C2—C1117.5 (3)C204—C206—H206119.6
O2—C2—C1117.7 (3)C206—C207—C208121.2 (3)
O4—C3—O3124.1 (3)C206—C207—H207119.4
O4—C3—C4119.5 (2)C208—C207—H207119.4
O3—C3—C4116.5 (2)C210—C208—C209117.7 (3)
C4ii—C4—C3124.1 (3)C210—C208—C207122.9 (3)
C4ii—C4—H4117.9C209—C208—C207119.4 (3)
C3—C4—H4117.9N4—C209—C208122.2 (3)
N2—C101—C102122.7 (3)N4—C209—C205118.5 (2)
N2—C101—H101118.6C208—C209—C205119.3 (3)
C102—C101—H101118.6C211—C210—C208120.0 (3)
C103—C102—C101118.6 (3)C211—C210—H210120.0
C103—C102—H102120.7C208—C210—H210120.0
C101—C102—H102120.7C210—C211—C212118.7 (3)
C102—C103—C104120.3 (3)C210—C211—H211120.7
C102—C103—H103119.8C212—C211—H211120.7
C104—C103—H103119.8N4—C212—C211122.6 (3)
C103—C104—C105117.3 (3)N4—C212—H212118.7
C103—C104—C106123.2 (3)C211—C212—H212118.7
C105—C104—C106119.5 (3)C112—N1—C109118.6 (2)
N2—C105—C104122.3 (3)C112—N1—Cd1124.98 (19)
N2—C105—C109118.6 (2)C109—N1—Cd1116.44 (18)
C104—C105—C109119.1 (3)C101—N2—C105118.7 (3)
C107—C106—C104121.2 (3)C101—N2—Cd1125.9 (2)
C107—C106—H106119.4C105—N2—Cd1115.33 (18)
C104—C106—H106119.4C201—N3—C205119.0 (3)
C106—C107—C108121.5 (3)C201—N3—Cd1124.7 (2)
C106—C107—H107119.3C205—N3—Cd1115.92 (18)
C108—C107—H107119.3C212—N4—C209118.7 (3)
C110—C108—C109117.7 (3)C212—N4—Cd1125.8 (2)
C110—C108—C107123.1 (3)C209—N4—Cd1114.88 (18)
C109—C108—C107119.2 (3)Cd1—OW1—H11121 (3)
N1—C109—C108121.9 (3)Cd1—OW1—H12118 (3)
N1—C109—C105118.6 (2)H11—OW1—H12108 (4)
C108—C109—C105119.5 (3)Cd1—OW2—H21122 (3)
C111—C110—C108119.9 (3)Cd1—OW2—H22123 (3)
C111—C110—H110120.0H21—OW2—H22115 (4)
C108—C110—H110120.0H32—OW3—H31100 (4)
C110—C111—C112119.0 (3)H41—OW4—H42113 (4)
C110—C111—H111120.5H51—OW5—H52105 (4)
C112—C111—H111120.5H61—OW6—H62116 (4)
N1—C112—C111122.8 (3)
Symmetry codes: (i) x+1, y+1, z+1; (ii) x+1, y, z+2.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
OW2—H21···O40.92 (4)1.80 (2)2.718 (3)178 (4)
OW2—H22···OW4iii0.92 (4)1.77 (2)2.680 (3)171 (4)
OW1—H12···O20.91 (4)1.71 (2)2.618 (3)176 (5)
OW1—H11···O30.93 (4)1.78 (2)2.700 (3)171 (4)
OW3—H31···O3iv0.92 (4)1.89 (2)2.800 (3)174 (4)
OW3—H32···OW6iv0.90 (4)1.95 (2)2.832 (4)168 (4)
OW4—H42···O4v0.90 (4)1.85 (2)2.746 (3)170 (4)
OW4—H41···OW50.90 (4)1.83 (2)2.721 (4)171 (4)
OW5—H51···OW30.91 (4)1.96 (2)2.835 (4)162 (4)
OW5—H52···O10.91 (4)1.89 (2)2.762 (4)162 (4)
OW6—H61···O20.90 (4)1.93 (2)2.816 (3)172 (4)
OW6—H62···OW3i0.90 (4)2.03 (2)2.913 (4)173 (4)
Symmetry codes: (i) x+1, y+1, z+1; (iii) x1, y1, z; (iv) x, y+1, z; (v) x+1, y+1, z+2.
 

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