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The title compound, [Mn(C31H31N7)](ClO4)2.0.435H2O, contains a high-spin MnII atom which is coordinated by seven N atoms at the corners of a distorted penta­gonal bipyramid.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806056169/bi2132sup1.cif
Contains datablocks global, I

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536806056169/bi2132Isup2.hkl
Contains datablock I

CCDC reference: 636147

Key indicators

  • Single-crystal X-ray study
  • T = 100 K
  • Mean [sigma](C-C) = 0.002 Å
  • Disorder in solvent or counterion
  • R factor = 0.035
  • wR factor = 0.037
  • Data-to-parameter ratio = 17.5

checkCIF/PLATON results

No syntax errors found



Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ? PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ? PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl1 PLAT244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for Cl2 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 4.00 Perc.
0 ALERT level A = In general: serious problem 0 ALERT level B = Potentially serious problem 7 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 0 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 3 ALERT type 4 Improvement, methodology, query or suggestion 0 ALERT type 5 Informative message, check

Computing details top

Data collection: SMART (Siemens, 1995); cell refinement: SAINT (Siemens, 1995); data reduction: SAINT; program(s) used to solve structure: SIR97 (Altomare et al., 1997); program(s) used to refine structure: KRYSTAL (Hazell, 1995); molecular graphics: ORTEPIII (Burnett & Johnson, 1996); software used to prepare material for publication: KRYSTAL.

{2,6-Bis[bis(2-pyridylmethyl)amino]methylpyridine}manganese(II) bis(perchlorate) 0.435-hydrate top
Crystal data top
[Mn(C31H31N7)](ClO4)2·0.435H2OF(000) = 1573.4
Mr = 763.34Dx = 1.556 Mg m3
Monoclinic, P21/cMo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybcCell parameters from 7479 reflections
a = 14.9038 (9) Åθ = 2.0–29.8°
b = 12.3825 (8) ŵ = 0.63 mm1
c = 18.647 (1) ÅT = 100 K
β = 108.733 (1)°Block, colourless
V = 3258.9 (4) Å30.42 × 0.34 × 0.32 mm
Z = 4
Data collection top
Siemens SMART CCD area-detector
diffractometer
9357 independent reflections
Radiation source: x-ray tube7918 reflections with I > 3σ(I)
Graphite monochromatorRint = 0.038
ω scansθmax = 29.8°, θmin = 2.0°
Absorption correction: integration
(XPREP; Siemens, 1995)
h = 2020
Tmin = 0.757, Tmax = 0.844k = 1617
35942 measured reflectionsl = 2523
Refinement top
Refinement on F0 restraints
Least-squares matrix: full2 constraints
R[F2 > 2σ(F2)] = 0.035H-atom parameters constrained
wR(F2) = 0.037 w = 1/{[σcs(F2 + B) + (1 + A)F2]1/2 - |F|}2,
where A = 0.03 and B = 2.0
S = 1.04(Δ/σ)max < 0.001
7918 reflectionsΔρmax = 0.60 e Å3
452 parametersΔρmin = 0.39 e Å3
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzUiso*/UeqOcc. (<1)
Mn10.25822 (2)0.11743 (2)0.10541 (1)0.0157 (1)
N10.12773 (9)0.15297 (10)0.15069 (7)0.0170 (6)
N90.28618 (9)0.04742 (10)0.00609 (7)0.0174 (6)
N100.12317 (9)0.12066 (10)0.00267 (7)0.0178 (6)
N110.31198 (9)0.11560 (11)0.23599 (7)0.0200 (7)
N210.21718 (10)0.30761 (10)0.08544 (7)0.0197 (7)
N310.27447 (9)0.07101 (11)0.11836 (8)0.0203 (7)
N410.39863 (9)0.18661 (10)0.10240 (8)0.0202 (7)
C20.0381 (1)0.1197 (1)0.09249 (9)0.0189 (7)
C30.0406 (1)0.1445 (1)0.01384 (8)0.0172 (7)
C40.0356 (1)0.1858 (1)0.04379 (9)0.0204 (8)
C50.0267 (1)0.1996 (1)0.11536 (9)0.0235 (8)
C60.0581 (1)0.1726 (1)0.12701 (9)0.0223 (8)
C70.1328 (1)0.1354 (1)0.06587 (9)0.0184 (8)
C80.2304 (1)0.1132 (1)0.07108 (9)0.0201 (8)
C120.4035 (1)0.1196 (1)0.27873 (9)0.0238 (8)
C130.4331 (1)0.1146 (1)0.35708 (9)0.0267 (9)
C140.3655 (1)0.1041 (1)0.39294 (9)0.0270 (9)
C150.2705 (1)0.0994 (1)0.34958 (9)0.0237 (9)
C160.2464 (1)0.1044 (1)0.27131 (9)0.0195 (8)
C170.1448 (1)0.0906 (1)0.22120 (9)0.0204 (8)
C220.2422 (1)0.3740 (1)0.03815 (9)0.0241 (9)
C230.2009 (1)0.4741 (1)0.01588 (9)0.0266 (9)
C240.1301 (1)0.5080 (1)0.04369 (10)0.0283 (9)
C250.1032 (1)0.4410 (1)0.09282 (10)0.0249 (9)
C260.1484 (1)0.3418 (1)0.11235 (9)0.0189 (8)
C270.1268 (1)0.2695 (1)0.16942 (9)0.0192 (8)
C320.2890 (1)0.1269 (1)0.18307 (9)0.0245 (9)
C330.3081 (1)0.2369 (1)0.19005 (10)0.0273 (9)
C340.3146 (1)0.2921 (1)0.12750 (11)0.0271 (9)
C350.3006 (1)0.2361 (1)0.06042 (10)0.0238 (9)
C360.2794 (1)0.1262 (1)0.05738 (9)0.0196 (8)
C370.2545 (1)0.0661 (1)0.01691 (9)0.0198 (8)
C420.4388 (1)0.2732 (1)0.14411 (10)0.0247 (9)
C430.5122 (1)0.3303 (1)0.13210 (10)0.0273 (9)
C440.5445 (1)0.2992 (1)0.07334 (11)0.0270 (9)
C450.5025 (1)0.2114 (1)0.02885 (9)0.0220 (8)
C460.4311 (1)0.1555 (1)0.04599 (9)0.0184 (7)
C470.3888 (1)0.0538 (1)0.00509 (9)0.0193 (8)
Cl10.39701 (3)0.45990 (3)0.29317 (2)0.0211 (2)
Cl20.13747 (3)0.82115 (4)0.34488 (2)0.0256 (2)
O10.3283 (1)0.3758 (1)0.2808 (1)0.051 (1)
O20.4056 (1)0.4922 (1)0.2220 (1)0.052 (1)
O30.4851 (1)0.4186 (2)0.3411 (1)0.065 (1)
O40.3689 (1)0.5508 (1)0.3291 (1)0.042 (1)
O50.0961 (1)0.7310 (1)0.2967 (1)0.058 (1)
O60.2341 (1)0.8373 (2)0.3508 (1)0.065 (1)
O70.0841 (1)0.9165 (1)0.3157 (1)0.059 (1)
O80.1309 (1)0.8003 (1)0.4188 (1)0.039 (1)
O90.1459 (3)0.5238 (3)0.2684 (2)0.056 (3)0.435 (5)
H9A0.13080.58770.27720.0680.435
H9B0.20610.53130.28480.0680.435
H2A0.01320.15760.10070.023
H2B0.02930.04430.09670.023
H40.09290.20440.03460.024
H50.07810.22720.15590.028
H60.06490.17950.17570.027
H8A0.22430.07540.11670.024
H8B0.26200.17980.07100.024
H120.45010.12620.25420.029
H130.49850.11830.38560.032
H140.38390.10010.44660.032
H150.22280.09290.37310.028
H17A0.13280.01630.20920.025
H17B0.10350.11560.24730.025
H220.29090.35110.01890.029
H230.22090.51840.01770.032
H240.10030.57600.02930.034
H250.05480.46250.11280.030
H27A0.17280.28170.21750.023
H27B0.06570.28740.17170.023
H320.28590.08880.22650.029
H330.31650.27320.23660.033
H340.32840.36720.13040.033
H350.30540.27230.01690.029
H37A0.28430.10090.04870.024
H37B0.18780.06770.04030.024
H420.41560.29600.18350.030
H430.54020.38970.16360.033
H440.59460.33750.06360.032
H450.52230.18980.01260.026
H47A0.39820.05270.04290.023
H47B0.41950.00670.03400.023*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Mn10.0154 (1)0.0167 (1)0.0154 (1)0.0004 (1)0.0055 (1)0.0000 (1)
N10.0181 (6)0.0168 (6)0.0160 (6)0.0015 (5)0.0055 (5)0.0004 (5)
N90.0156 (6)0.0167 (6)0.0196 (6)0.0004 (4)0.0051 (5)0.0007 (5)
N100.0173 (6)0.0181 (6)0.0177 (6)0.0006 (5)0.0053 (5)0.0008 (5)
N110.0204 (6)0.0207 (6)0.0186 (6)0.0007 (5)0.0060 (5)0.0001 (5)
N210.0234 (7)0.0171 (6)0.0199 (6)0.0003 (5)0.0089 (5)0.0001 (5)
N310.0184 (6)0.0185 (6)0.0229 (7)0.0004 (5)0.0053 (5)0.0013 (5)
N410.0195 (6)0.0194 (6)0.0224 (6)0.0009 (5)0.0077 (5)0.0019 (5)
C20.0163 (7)0.0208 (7)0.0200 (7)0.0017 (6)0.0065 (5)0.0017 (6)
C30.0170 (7)0.0159 (6)0.0185 (7)0.0013 (5)0.0056 (6)0.0028 (5)
C40.0161 (7)0.0206 (7)0.0231 (7)0.0004 (5)0.0045 (6)0.0014 (6)
C50.0190 (7)0.0256 (8)0.0216 (8)0.0015 (6)0.0006 (6)0.0012 (6)
C60.0235 (8)0.0253 (8)0.0169 (7)0.0006 (6)0.0049 (6)0.0005 (6)
C70.0195 (7)0.0174 (7)0.0182 (7)0.0000 (5)0.0057 (6)0.0017 (5)
C80.0198 (7)0.0235 (7)0.0175 (7)0.0021 (6)0.0067 (6)0.0017 (6)
C120.0224 (7)0.0264 (8)0.0224 (7)0.0004 (6)0.0068 (6)0.0002 (6)
C130.0230 (8)0.0312 (8)0.0224 (8)0.0009 (7)0.0022 (6)0.0021 (7)
C140.0313 (9)0.0307 (9)0.0167 (7)0.0008 (7)0.0047 (6)0.0020 (6)
C150.0271 (8)0.0258 (8)0.0193 (7)0.0002 (6)0.0091 (6)0.0009 (6)
C160.0223 (7)0.0179 (7)0.0187 (7)0.0005 (6)0.0069 (6)0.0009 (5)
C170.0218 (7)0.0225 (7)0.0182 (7)0.0026 (6)0.0081 (6)0.0027 (6)
C220.0310 (8)0.0214 (7)0.0230 (8)0.0028 (6)0.0131 (7)0.0011 (6)
C230.0382 (10)0.0188 (7)0.0228 (8)0.0039 (7)0.0098 (7)0.0023 (6)
C240.0347 (9)0.0180 (7)0.0302 (9)0.0029 (6)0.0078 (7)0.0022 (6)
C250.0257 (8)0.0204 (7)0.0284 (8)0.0025 (6)0.0085 (7)0.0018 (6)
C260.0199 (7)0.0177 (7)0.0186 (7)0.0020 (5)0.0055 (6)0.0020 (5)
C270.0209 (7)0.0189 (7)0.0192 (7)0.0002 (6)0.0084 (6)0.0022 (6)
C320.0248 (8)0.0221 (7)0.0248 (8)0.0015 (6)0.0055 (6)0.0022 (6)
C330.0257 (8)0.0220 (8)0.0306 (9)0.0007 (6)0.0042 (7)0.0067 (7)
C340.0211 (8)0.0171 (7)0.0399 (10)0.0001 (6)0.0052 (7)0.0013 (7)
C350.0189 (7)0.0181 (7)0.0334 (9)0.0002 (6)0.0071 (6)0.0033 (6)
C360.0137 (6)0.0187 (7)0.0253 (7)0.0007 (5)0.0045 (6)0.0006 (6)
C370.0191 (7)0.0178 (7)0.0226 (7)0.0008 (6)0.0066 (6)0.0030 (6)
C420.0259 (8)0.0237 (8)0.0246 (8)0.0023 (6)0.0086 (6)0.0042 (6)
C430.0262 (8)0.0226 (8)0.0300 (9)0.0050 (6)0.0048 (7)0.0033 (7)
C440.0213 (8)0.0249 (8)0.0350 (9)0.0042 (6)0.0091 (7)0.0018 (7)
C450.0194 (7)0.0226 (7)0.0255 (8)0.0017 (6)0.0093 (6)0.0025 (6)
C460.0167 (7)0.0174 (6)0.0202 (7)0.0024 (5)0.0049 (6)0.0013 (5)
C470.0179 (7)0.0188 (7)0.0231 (7)0.0014 (5)0.0091 (6)0.0024 (6)
Cl10.0245 (2)0.0193 (2)0.0190 (2)0.0025 (1)0.0064 (1)0.0018 (1)
Cl20.0225 (2)0.0311 (2)0.0230 (2)0.0034 (2)0.0072 (1)0.0044 (2)
O10.050 (1)0.041 (1)0.071 (1)0.024 (1)0.031 (1)0.019 (1)
O20.095 (1)0.035 (1)0.044 (1)0.010 (1)0.046 (1)0.010 (1)
O30.041 (1)0.078 (1)0.056 (1)0.021 (1)0.015 (1)0.012 (1)
O40.070 (1)0.025 (1)0.036 (1)0.007 (1)0.024 (1)0.006 (1)
O50.076 (1)0.067 (1)0.036 (1)0.030 (1)0.025 (1)0.026 (1)
O60.030 (1)0.066 (1)0.107 (2)0.007 (1)0.033 (1)0.004 (1)
O70.042 (1)0.053 (1)0.078 (1)0.007 (1)0.015 (1)0.045 (1)
O80.059 (1)0.032 (1)0.021 (1)0.013 (1)0.007 (1)0.001 (1)
O90.052 (2)0.058 (3)0.049 (2)0.011 (2)0.006 (2)0.002 (2)
Geometric parameters (Å, º) top
Mn1—N12.397 (1)C43—C441.384 (3)
Mn1—N92.409 (1)C44—C451.389 (2)
Mn1—N102.290 (1)C45—C461.390 (2)
Mn1—N112.306 (1)C46—C471.502 (2)
Mn1—N212.431 (1)Cl1—O11.426 (1)
Mn1—N312.350 (1)Cl1—O21.430 (1)
Mn1—N412.279 (1)Cl1—O31.425 (2)
N1—C21.484 (2)Cl1—O41.440 (1)
N1—C171.475 (2)Cl2—O51.442 (2)
N1—C271.486 (2)Cl2—O61.423 (2)
N9—C81.475 (2)Cl2—O71.430 (2)
N9—C371.476 (2)Cl2—O81.436 (1)
N9—C471.478 (2)C2—H2A0.950
N10—C31.345 (2)C2—H2B0.950
N10—C71.343 (2)C4—H40.950
N11—C121.342 (2)C5—H50.950
N11—C161.350 (2)C6—H60.950
N21—C221.343 (2)C8—H8A0.950
N21—C261.346 (2)C8—H8B0.950
N31—C321.347 (2)C12—H120.950
N31—C361.349 (2)C13—H130.950
N41—C421.347 (2)C14—H140.950
N41—C461.347 (2)C15—H150.950
C2—C31.510 (2)C17—H17A0.950
C3—C41.387 (2)C17—H17B0.950
C4—C51.394 (2)C22—H220.950
C5—C61.390 (2)C23—H230.950
C6—C71.391 (2)C24—H240.950
C7—C81.514 (2)C25—H250.950
C12—C131.385 (2)C27—H27A0.950
C13—C141.382 (2)C27—H27B0.950
C14—C151.388 (2)C32—H320.950
C15—C161.388 (2)C33—H330.950
C16—C171.512 (2)C34—H340.950
C22—C231.387 (2)C35—H350.950
C23—C241.383 (3)C37—H37A0.950
C24—C251.387 (2)C37—H37B0.950
C25—C261.392 (2)C42—H420.950
C26—C271.503 (2)C43—H430.950
C32—C331.389 (2)C44—H440.950
C33—C341.382 (3)C45—H450.950
C34—C351.386 (2)C47—H47A0.950
C35—C361.393 (2)C47—H47B0.950
C36—C371.510 (2)O9—H9A0.852
C42—C431.380 (2)O9—H9B0.854
N1—Mn1—N9139.02 (4)C44—C45—C46118.9 (2)
N1—Mn1—N1072.36 (4)N41—C46—C45122.1 (1)
N1—Mn1—N1171.09 (5)N41—C46—C47116.0 (1)
N1—Mn1—N2171.55 (4)C45—C46—C47121.8 (1)
N1—Mn1—N31102.39 (4)N9—C47—C46111.3 (1)
N1—Mn1—N41142.68 (4)O1—Cl1—O2109.1 (1)
N9—Mn1—N1068.50 (4)O1—Cl1—O3107.9 (1)
N9—Mn1—N11144.08 (5)O1—Cl1—O4110.2 (1)
N9—Mn1—N21108.73 (4)O2—Cl1—O3110.1 (1)
N9—Mn1—N3171.99 (5)O2—Cl1—O4109.8 (1)
N9—Mn1—N4172.50 (5)O3—Cl1—O4109.6 (1)
N10—Mn1—N11142.87 (5)O5—Cl2—O6112.1 (1)
N10—Mn1—N2175.21 (5)O5—Cl2—O7109.1 (1)
N10—Mn1—N3197.88 (4)O5—Cl2—O8108.2 (1)
N10—Mn1—N41122.70 (5)O6—Cl2—O7109.8 (1)
N11—Mn1—N2198.99 (5)O6—Cl2—O8109.3 (1)
N11—Mn1—N3183.82 (5)O7—Cl2—O8108.2 (1)
N11—Mn1—N4191.10 (5)H2A—C2—H2B109.5
N21—Mn1—N31171.82 (5)N1—C2—H2A109.1
N21—Mn1—N4179.63 (5)C3—C2—H2A109.1
N31—Mn1—N41108.10 (5)N1—C2—H2B109.1
Mn1—N1—C2109.48 (9)C3—C2—H2B109.1
Mn1—N1—C17106.91 (9)C3—C4—H4120.6
Mn1—N1—C27109.35 (9)C5—C4—H4120.6
Mn1—N9—C8107.57 (9)C6—C5—H5120.3
Mn1—N9—C37108.94 (9)C4—C5—H5120.3
Mn1—N9—C47108.48 (9)C5—C6—H6120.7
Mn1—N10—C3118.4 (1)C7—C6—H6120.7
Mn1—N10—C7117.7 (1)H8A—C8—H8B109.5
Mn1—N11—C12124.7 (1)N9—C8—H8A109.3
Mn1—N11—C16117.1 (1)C7—C8—H8A109.3
Mn1—N21—C22125.7 (1)N9—C8—H8B109.3
Mn1—N21—C26115.6 (1)C7—C8—H8B109.3
Mn1—N31—C32125.7 (1)N11—C12—H12118.6
Mn1—N31—C36116.6 (1)C13—C12—H12118.6
Mn1—N41—C42121.8 (1)C14—C13—H13120.6
Mn1—N41—C46118.3 (1)C12—C13—H13120.6
C2—N1—C17111.3 (1)C13—C14—H14120.4
C2—N1—C27111.5 (1)C15—C14—H14120.4
C17—N1—C27108.1 (1)C16—C15—H15120.6
C8—N9—C37110.0 (1)C14—C15—H15120.6
C8—N9—C47111.8 (1)H17A—C17—H17B109.5
C37—N9—C47109.9 (1)N1—C17—H17A109.3
C3—N10—C7120.0 (1)C16—C17—H17A109.3
C12—N11—C16118.1 (1)N1—C17—H17B109.3
C22—N21—C26117.2 (1)C16—C17—H17B109.3
C32—N31—C36117.3 (1)N21—C22—H22118.2
C42—N41—C46118.3 (1)C23—C22—H22118.2
N1—C2—C3110.9 (1)C24—C23—H23120.7
N10—C3—C4121.6 (1)C22—C23—H23120.7
N10—C3—C2114.5 (1)C23—C24—H24120.5
C2—C3—C4123.9 (1)C25—C24—H24120.6
C3—C4—C5118.7 (1)C24—C25—H25120.6
C4—C5—C6119.4 (1)C26—C25—H25120.6
C5—C6—C7118.7 (1)H27A—C27—H27B109.5
N10—C7—C6121.5 (1)N1—C27—H27A108.6
N10—C7—C8115.8 (1)C26—C27—H27A108.6
C6—C7—C8122.7 (1)N1—C27—H27B108.6
N9—C8—C7110.3 (1)C26—C27—H27B108.6
N11—C12—C13122.9 (2)N31—C32—H32118.1
C12—C13—C14118.7 (2)C33—C32—H32118.1
C13—C14—C15119.2 (2)C34—C33—H33120.9
C14—C15—C16118.8 (2)C32—C33—H33120.9
N11—C16—C15122.3 (1)C33—C34—H34120.6
N11—C16—C17116.6 (1)C35—C34—H34120.6
C15—C16—C17121.0 (1)C34—C35—H35120.3
N1—C17—C16110.1 (1)C36—C35—H35120.3
N21—C22—C23123.6 (2)H37A—C37—H37B109.5
C22—C23—C24118.5 (2)N9—C37—H37A108.9
C23—C24—C25118.9 (2)C36—C37—H37A108.9
C24—C25—C26118.9 (2)N9—C37—H37B108.9
N21—C26—C25122.9 (1)C36—C37—H37B108.9
N21—C26—C27116.0 (1)N41—C42—H42118.6
C25—C26—C27121.0 (1)C43—C42—H42118.6
N1—C27—C26113.1 (1)C42—C43—H43120.6
N31—C32—C33123.8 (2)C44—C43—H43120.6
C32—C33—C34118.3 (2)C43—C44—H44120.5
C33—C34—C35118.9 (2)C45—C44—H44120.5
C34—C35—C36119.5 (2)C44—C45—H45120.6
N31—C36—C35122.2 (2)C46—C45—H45120.6
N31—C36—C37117.4 (1)H47A—C47—H47B109.5
C35—C36—C37120.3 (1)N9—C47—H47A109.0
N9—C37—C36111.7 (1)C46—C47—H47A109.0
N41—C42—C43122.8 (2)N9—C47—H47B109.0
C42—C43—C44118.8 (2)C46—C47—H47B109.0
C43—C44—C45119.1 (2)H9A—O9—H9B98.2
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O9—H9A···O50.851.922.768 (4)180
O9—H9B···O40.852.313.165 (4)180
 

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