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The asymmetric unit of the title compound, (C2H10N2)2[Ti4O4(C6H6NO6)4], consists of halves of two centrosymmetric tetrameric [Ti4O4{N(CH2COO)3}4]4− anions, two [H3N(CH2)2NH3]2+ cations and a disordered mol­ecule of water of crystallization. In the [Ti4O4{N(CH2COO)3}4]4− tetramer, each Ti atom is coord­inated by one nitrilo­tri­acetate ligand and two μ-oxo ligands, so that four titanium and four μ-O atoms form an eight-membered ring. The tetramers are connected by hydrogen bonds with [H3N(CH2)2NH3]2+ cations and with water mol­ecules, leading to an intricate three-dimensional network.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536804016186/dn6144sup1.cif
Contains datablocks I, global

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S1600536804016186/dn6144Isup2.hkl
Contains datablock I

CCDC reference: 248722

Key indicators

  • Single-crystal X-ray study
  • T = 293 K
  • Mean [sigma](C-C) = 0.006 Å
  • Disorder in solvent or counterion
  • R factor = 0.050
  • wR factor = 0.124
  • Data-to-parameter ratio = 15.7

checkCIF/PLATON results

No syntax errors found



Alert level B PLAT432_ALERT_2_B Short Inter X...Y Contact C4 .. O300 .. 2.74 Ang. PLAT432_ALERT_2_B Short Inter X...Y Contact C26 .. O100 .. 2.88 Ang.
Alert level C PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low ....... 0.98 PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? PLAT213_ALERT_2_C Atom O15 has ADP max/min Ratio ............. 3.40 prolat PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 2.61 Ratio PLAT220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.38 Ratio PLAT243_ALERT_4_C High Solvent U(eq) as Compared to Neighbors .... C26 PLAT244_ALERT_4_C Low Solvent U(eq) as Compared to Neighbors .... C25 PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 9.00 Perc.
0 ALERT level A = In general: serious problem 2 ALERT level B = Potentially serious problem 8 ALERT level C = Check and explain 0 ALERT level G = General alerts; check 1 ALERT type 1 CIF construction/syntax error, inconsistent or missing data 5 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

Computing details top

Data collection: TEXRAY (Molecular Structure Corporation, 1999); cell refinement: TEXRAY; data reduction: TEXSAN (Molecular Structure Corporation, 1999); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEX (McArdle, 1995) and CAMERON (Watkin et al., 1993); software used to prepare material for publication: SHELXL97.

Bis(ethylenediammonium) tetra-µ-oxo-tetrakis[(nitrilotriacetato)titanate] monohydrate top
Crystal data top
(C2H10N2)2[Ti4O4(C6H6NO6)4]·H2OZ = 2
Mr = 1150.33F(000) = 1180
Triclinic, P1Dx = 1.697 Mg m3
Hall symbol: -P 1Mo Kα radiation, λ = 0.71073 Å
a = 10.8082 (10) ÅCell parameters from 25 reflections
b = 10.9099 (11) Åθ = 12–18°
c = 19.6832 (15) ŵ = 0.79 mm1
α = 91.483 (5)°T = 293 K
β = 90.796 (3)°Block, colourless
γ = 104.374 (5)°0.46 × 0.42 × 0.40 mm
V = 2247.1 (4) Å3
Data collection top
Rigaku Weissenberg IP
diffractometer
7090 reflections with I > 2σ(I)
Radiation source: rotor targetRint = 0.039
Graphite monochromatorθmax = 27.5°, θmin = 1.9°
scintillation counter scansh = 1413
20995 measured reflectionsk = 014
10124 independent reflectionsl = 2525
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)] = 0.050Hydrogen site location: inferred from neighbouring sites
wR(F2) = 0.124H-atom parameters constrained
S = 1.01 w = 1/[σ2(Fo2) + (0.0528P)2 + 2.7799P]
where P = (Fo2 + 2Fc2)/3
10120 reflections(Δ/σ)max = 0.002
644 parametersΔρmax = 0.91 e Å3
0 restraintsΔρmin = 0.55 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*/UeqOcc. (<1)
Ti10.36201 (6)0.28848 (5)0.95177 (3)0.02277 (13)
Ti20.43714 (5)0.42907 (5)1.11896 (3)0.02071 (13)
Ti30.13032 (5)0.85902 (5)0.54886 (3)0.02267 (13)
Ti40.05249 (5)1.06278 (5)0.62183 (3)0.02150 (13)
O10.1049 (3)0.4002 (3)0.83621 (17)0.0659 (10)
O20.2076 (2)0.3368 (3)0.92170 (13)0.0386 (6)
O30.1484 (3)0.0781 (3)0.93518 (15)0.0560 (9)
O40.2496 (3)0.1163 (2)0.97213 (12)0.0405 (7)
O50.6363 (3)0.1516 (3)0.86376 (15)0.0460 (7)
O60.5013 (2)0.2019 (2)0.93719 (12)0.0344 (6)
O70.0586 (3)0.3843 (3)1.1196 (2)0.0753 (11)
O80.2675 (2)0.4628 (2)1.12545 (13)0.0345 (6)
O90.5938 (3)0.1390 (4)1.1639 (2)0.0869 (14)
O100.5581 (2)0.3228 (2)1.13637 (14)0.0375 (6)
O110.4501 (4)0.4362 (3)1.32604 (13)0.0751 (12)
O120.4694 (2)0.4851 (2)1.21778 (11)0.0333 (6)
O130.3711 (3)1.1282 (3)0.66016 (18)0.0657 (10)
O140.2848 (2)0.9933 (2)0.57538 (13)0.0374 (6)
O150.3808 (5)0.6378 (5)0.55212 (19)0.1084 (18)
O160.2434 (3)0.7473 (3)0.52373 (13)0.0451 (7)
O170.1318 (3)0.6111 (3)0.6489 (2)0.0650 (10)
O180.0044 (3)0.7086 (2)0.56898 (14)0.0412 (6)
O190.4316 (3)0.9373 (3)0.6544 (3)0.0865 (14)
O200.2278 (2)0.9564 (2)0.63282 (13)0.0358 (6)
O210.1197 (3)1.4351 (3)0.6334 (2)0.0642 (10)
O220.0766 (2)1.2263 (2)0.63284 (13)0.0322 (5)
O230.0584 (3)1.0870 (3)0.82981 (12)0.0455 (7)
O240.0268 (2)1.0397 (2)0.72245 (11)0.0331 (6)
O250.3827 (2)0.3353 (2)1.03778 (11)0.0344 (6)
O260.4629 (2)0.4301 (2)0.90892 (11)0.0335 (6)
O270.0351 (2)0.9545 (2)0.59874 (11)0.0330 (6)
O280.1008 (2)0.8887 (2)0.46404 (11)0.0349 (6)
N10.3199 (2)0.1971 (2)0.84546 (13)0.0219 (5)
N20.3177 (2)0.2590 (2)1.17354 (13)0.0235 (5)
N30.1933 (3)0.8014 (3)0.65276 (14)0.0287 (6)
N40.1600 (2)1.1977 (2)0.67040 (13)0.0238 (6)
N50.3320 (4)0.2798 (4)0.43429 (19)0.0676 (12)
H5A0.31890.34960.41620.101*
H5B0.28560.21210.41140.101*
H5C0.41440.28070.43200.101*
N60.3594 (3)0.3660 (3)0.61761 (18)0.0484 (9)
H6A0.28450.38570.62050.073*
H6B0.41930.42520.63940.073*
H6C0.35410.29150.63640.073*
N70.1948 (3)0.6737 (3)0.91657 (16)0.0397 (7)
H7A0.12040.63080.89820.060*
H7B0.25840.65810.89240.060*
H7C0.19890.75620.91660.060*
N80.1440 (3)0.8023 (3)1.05629 (15)0.0392 (8)
H8A0.22280.82321.07420.059*
H8B0.08910.81551.08730.059*
H8C0.14010.84961.02050.059*
C10.2556 (3)0.2809 (3)0.80863 (16)0.0283 (7)
H1A0.19770.23170.77420.034*
H1B0.31870.34500.78600.034*
C20.1812 (4)0.3443 (4)0.8574 (2)0.0367 (8)
C30.2375 (3)0.0683 (3)0.85269 (16)0.0267 (7)
H3A0.27850.00810.83120.032*
H3B0.15730.06220.82850.032*
C40.2094 (4)0.0313 (3)0.92524 (18)0.0352 (8)
C50.4471 (3)0.1948 (3)0.81881 (17)0.0289 (7)
H5D0.48290.27290.79580.035*
H5E0.43790.12510.78600.035*
C60.5365 (3)0.1798 (3)0.87612 (18)0.0313 (7)
C70.1871 (3)0.2425 (3)1.14460 (18)0.0321 (8)
H7D0.12460.20051.17680.039*
H7E0.17690.19041.10320.039*
C80.1661 (4)0.3713 (4)1.1292 (2)0.0388 (9)
C90.3770 (4)0.1540 (3)1.1573 (2)0.0370 (9)
H9A0.34340.11371.11410.044*
H9B0.35710.09111.19210.044*
C100.5202 (4)0.2050 (4)1.1537 (2)0.0441 (10)
C110.3246 (4)0.2908 (4)1.24682 (17)0.0342 (8)
H11A0.34540.22211.27110.041*
H11B0.24120.29781.26140.041*
C120.4224 (4)0.4128 (4)1.26608 (17)0.0371 (9)
C130.2506 (4)0.9235 (4)0.68858 (18)0.0401 (9)
H13A0.31610.91280.72050.048*
H13B0.18540.95030.71420.048*
C140.3086 (4)1.0240 (4)0.6393 (2)0.0390 (9)
C150.2877 (4)0.7254 (3)0.64089 (19)0.0349 (8)
H15A0.25920.64510.66300.042*
H15B0.36890.76960.66170.042*
C160.3069 (4)0.7007 (4)0.5675 (2)0.0494 (11)
C170.0749 (4)0.7292 (4)0.6838 (2)0.0481 (10)
H17A0.04490.78410.71570.058*
H17B0.09320.66020.70890.058*
C180.0296 (4)0.6758 (3)0.6310 (2)0.0413 (9)
C190.2953 (3)1.1470 (3)0.64885 (19)0.0319 (8)
H19A0.31001.17810.60450.038*
H19B0.35071.17490.68090.038*
C200.3251 (3)1.0036 (4)0.6459 (2)0.0407 (9)
C210.0984 (3)1.3218 (3)0.64294 (19)0.0312 (7)
H21A0.11231.38890.67290.037*
H21B0.13551.33020.59870.037*
C220.0434 (4)1.3331 (3)0.6367 (2)0.0365 (8)
C230.1423 (4)1.1962 (4)0.74541 (17)0.0355 (8)
H23A0.22551.17810.76610.043*
H23B0.09531.27970.76150.043*
C240.0723 (3)1.1005 (3)0.76866 (16)0.0291 (7)
C250.2947 (4)0.2750 (4)0.5043 (2)0.0526 (11)
H25A0.28090.18870.51930.063*
H25B0.21460.29940.50800.063*
C260.3913 (6)0.3588 (6)0.5492 (3)0.0787 (18)
H26A0.46950.33060.54690.094*
H26B0.40930.44350.53150.094*
C270.2060 (4)0.6337 (4)0.9878 (2)0.0404 (9)
H27A0.29140.67281.00530.048*
H27B0.19500.54270.98750.048*
C280.1108 (4)0.6676 (4)1.0347 (2)0.0441 (9)
H28A0.02770.64731.01200.053*
H28B0.10450.61641.07460.053*
O1000.3410 (11)0.5492 (12)0.4179 (5)0.082 (4)0.35
H10A0.30750.58010.45050.050*0.35
H10B0.32260.58220.38130.050*0.35
O2000.4848 (10)0.0809 (11)0.4897 (6)0.077 (3)0.35
H20A0.44730.10890.52350.050*0.35
H20B0.54990.14180.48160.050*0.35
O3000.6040 (14)0.0751 (15)1.0255 (8)0.098 (5)0.30
H30A0.66420.03771.01350.050*0.30
H30B0.59450.11910.99160.050*0.30
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Ti10.0276 (3)0.0201 (3)0.0183 (3)0.0016 (2)0.0021 (2)0.0021 (2)
Ti20.0240 (3)0.0194 (3)0.0176 (3)0.0032 (2)0.0014 (2)0.0009 (2)
Ti30.0255 (3)0.0243 (3)0.0196 (3)0.0091 (2)0.0005 (2)0.0014 (2)
Ti40.0235 (3)0.0228 (3)0.0190 (3)0.0077 (2)0.0005 (2)0.0028 (2)
O10.072 (2)0.079 (2)0.065 (2)0.055 (2)0.0148 (18)0.0091 (18)
O20.0362 (14)0.0457 (16)0.0372 (14)0.0174 (12)0.0004 (12)0.0098 (12)
O30.083 (2)0.0258 (14)0.0450 (16)0.0139 (15)0.0071 (16)0.0011 (12)
O40.0576 (17)0.0270 (13)0.0268 (12)0.0088 (12)0.0068 (12)0.0018 (10)
O50.0305 (14)0.0612 (19)0.0507 (17)0.0207 (13)0.0008 (13)0.0083 (14)
O60.0383 (14)0.0409 (15)0.0274 (12)0.0172 (12)0.0050 (11)0.0028 (10)
O70.0304 (16)0.066 (2)0.134 (3)0.0205 (16)0.0176 (19)0.009 (2)
O80.0337 (13)0.0293 (13)0.0430 (14)0.0125 (11)0.0010 (11)0.0033 (11)
O90.052 (2)0.065 (2)0.160 (4)0.0401 (19)0.025 (2)0.042 (2)
O100.0272 (13)0.0355 (14)0.0522 (16)0.0112 (11)0.0095 (12)0.0105 (12)
O110.085 (2)0.084 (2)0.0221 (14)0.045 (2)0.0118 (15)0.0073 (14)
O120.0379 (14)0.0337 (14)0.0206 (11)0.0056 (11)0.0000 (10)0.0009 (9)
O130.083 (2)0.0288 (15)0.077 (2)0.0011 (16)0.0449 (19)0.0064 (15)
O140.0344 (14)0.0358 (14)0.0360 (14)0.0027 (11)0.0056 (11)0.0056 (11)
O150.137 (4)0.180 (5)0.062 (2)0.141 (4)0.001 (2)0.005 (3)
O160.0572 (18)0.0621 (19)0.0294 (13)0.0408 (15)0.0016 (13)0.0044 (12)
O170.0487 (18)0.0420 (18)0.101 (3)0.0023 (15)0.0320 (18)0.0082 (17)
O180.0368 (14)0.0323 (14)0.0494 (16)0.0005 (12)0.0019 (13)0.0029 (12)
O190.0285 (16)0.046 (2)0.178 (4)0.0048 (14)0.019 (2)0.009 (2)
O200.0309 (13)0.0250 (13)0.0482 (15)0.0012 (10)0.0005 (12)0.0038 (11)
O210.0428 (17)0.0282 (15)0.114 (3)0.0055 (13)0.0178 (18)0.0041 (17)
O220.0236 (12)0.0288 (13)0.0431 (14)0.0046 (10)0.0041 (11)0.0032 (10)
O230.0570 (18)0.068 (2)0.0189 (12)0.0305 (16)0.0021 (12)0.0013 (12)
O240.0423 (14)0.0413 (15)0.0218 (11)0.0221 (12)0.0019 (10)0.0000 (10)
O250.0472 (15)0.0298 (13)0.0207 (11)0.0009 (11)0.0036 (11)0.0021 (9)
O260.0424 (14)0.0237 (12)0.0275 (12)0.0050 (10)0.0031 (11)0.0019 (9)
O270.0423 (14)0.0351 (14)0.0272 (12)0.0203 (12)0.0023 (11)0.0037 (10)
O280.0427 (15)0.0424 (15)0.0240 (12)0.0192 (12)0.0023 (11)0.0021 (10)
N10.0215 (13)0.0218 (13)0.0216 (12)0.0041 (10)0.0008 (10)0.0027 (10)
N20.0219 (13)0.0235 (14)0.0246 (13)0.0045 (11)0.0022 (11)0.0017 (10)
N30.0371 (16)0.0270 (15)0.0239 (13)0.0112 (12)0.0016 (12)0.0016 (11)
N40.0220 (13)0.0226 (13)0.0260 (13)0.0045 (11)0.0007 (11)0.0006 (10)
N50.078 (3)0.062 (3)0.046 (2)0.014 (2)0.010 (2)0.0033 (19)
N60.0413 (19)0.041 (2)0.058 (2)0.0011 (16)0.0025 (17)0.0016 (16)
N70.0280 (16)0.049 (2)0.0415 (18)0.0092 (14)0.0062 (14)0.0011 (15)
N80.0404 (18)0.055 (2)0.0269 (15)0.0215 (16)0.0010 (14)0.0034 (14)
C10.0296 (17)0.0286 (17)0.0269 (16)0.0075 (14)0.0042 (14)0.0021 (13)
C20.0327 (19)0.035 (2)0.044 (2)0.0137 (16)0.0092 (17)0.0067 (16)
C30.0283 (17)0.0221 (16)0.0270 (16)0.0021 (13)0.0048 (14)0.0032 (12)
C40.045 (2)0.0214 (17)0.0348 (19)0.0005 (15)0.0020 (16)0.0019 (14)
C50.0250 (16)0.0356 (19)0.0259 (16)0.0075 (14)0.0031 (13)0.0040 (14)
C60.0279 (17)0.0296 (18)0.0353 (19)0.0060 (14)0.0010 (15)0.0044 (14)
C70.0205 (16)0.0345 (19)0.0370 (19)0.0011 (14)0.0033 (14)0.0000 (15)
C80.0290 (19)0.040 (2)0.049 (2)0.0122 (16)0.0076 (17)0.0018 (17)
C90.040 (2)0.0236 (18)0.052 (2)0.0140 (16)0.0127 (18)0.0093 (16)
C100.038 (2)0.038 (2)0.062 (3)0.0192 (18)0.0111 (19)0.0122 (19)
C110.0349 (19)0.037 (2)0.0250 (17)0.0026 (16)0.0025 (15)0.0056 (14)
C120.0343 (19)0.046 (2)0.0228 (17)0.0044 (17)0.0028 (15)0.0018 (15)
C130.061 (3)0.036 (2)0.0272 (17)0.0203 (19)0.0135 (18)0.0070 (15)
C140.044 (2)0.030 (2)0.042 (2)0.0116 (17)0.0178 (18)0.0018 (16)
C150.037 (2)0.0295 (19)0.041 (2)0.0128 (16)0.0059 (16)0.0026 (15)
C160.054 (3)0.064 (3)0.044 (2)0.041 (2)0.003 (2)0.005 (2)
C170.051 (2)0.058 (3)0.039 (2)0.017 (2)0.0174 (19)0.0172 (19)
C180.039 (2)0.0230 (18)0.064 (3)0.0093 (16)0.015 (2)0.0059 (17)
C190.0209 (16)0.0329 (19)0.043 (2)0.0084 (14)0.0005 (15)0.0016 (15)
C200.0253 (18)0.036 (2)0.059 (3)0.0037 (16)0.0019 (18)0.0030 (18)
C210.0304 (18)0.0225 (17)0.042 (2)0.0093 (14)0.0034 (15)0.0000 (14)
C220.0340 (19)0.0274 (19)0.046 (2)0.0034 (15)0.0047 (17)0.0030 (15)
C230.043 (2)0.044 (2)0.0261 (17)0.0236 (18)0.0012 (15)0.0050 (15)
C240.0275 (17)0.0381 (19)0.0235 (16)0.0112 (15)0.0043 (14)0.0011 (14)
C250.055 (3)0.047 (3)0.048 (2)0.002 (2)0.014 (2)0.006 (2)
C260.075 (4)0.078 (4)0.063 (3)0.018 (3)0.018 (3)0.006 (3)
C270.042 (2)0.037 (2)0.045 (2)0.0145 (17)0.0049 (18)0.0035 (17)
C280.043 (2)0.046 (2)0.041 (2)0.0060 (19)0.0055 (18)0.0076 (18)
O1000.086 (8)0.127 (10)0.049 (6)0.062 (8)0.006 (5)0.024 (6)
O2000.065 (6)0.095 (8)0.078 (7)0.027 (6)0.038 (6)0.028 (6)
O3000.084 (10)0.109 (12)0.108 (11)0.034 (9)0.023 (9)0.040 (9)
Geometric parameters (Å, º) top
Ti1—O251.751 (2)N5—H5C0.8900
Ti1—O261.882 (2)N6—C261.399 (6)
Ti1—O21.959 (3)N6—H6A0.8900
Ti1—O61.986 (2)N6—H6B0.8900
Ti1—O42.021 (3)N6—H6C0.8900
Ti1—N12.285 (2)N7—C271.491 (5)
Ti2—O26i1.751 (2)N7—H7A0.8900
Ti2—O251.881 (2)N7—H7B0.8900
Ti2—O81.962 (2)N7—H7C0.8900
Ti2—O101.983 (3)N8—C281.473 (5)
Ti2—O122.023 (2)N8—H8A0.8900
Ti2—N22.284 (3)N8—H8B0.8900
Ti3—O281.749 (2)N8—H8C0.8900
Ti3—O271.902 (2)C1—C21.520 (5)
Ti3—O181.958 (3)C1—H1A0.9700
Ti3—O141.982 (3)C1—H1B0.9700
Ti3—O161.988 (3)C3—C41.509 (5)
Ti3—N32.298 (3)C3—H3A0.9700
Ti4—O271.742 (2)C3—H3B0.9700
Ti4—O28ii1.889 (2)C5—C61.514 (5)
Ti4—O221.978 (2)C5—H5D0.9700
Ti4—O201.979 (3)C5—H5E0.9700
Ti4—O242.027 (2)C7—C81.516 (5)
Ti4—N42.289 (3)C7—H7D0.9700
O1—C21.216 (4)C7—H7E0.9700
O2—C21.302 (4)C9—C101.513 (5)
O3—C41.233 (4)C9—H9A0.9700
O4—C41.283 (4)C9—H9B0.9700
O5—C61.219 (4)C11—C121.516 (5)
O6—C61.300 (4)C11—H11A0.9700
O7—C81.218 (5)C11—H11B0.9700
O8—C81.291 (5)C13—C141.505 (6)
O9—C101.215 (5)C13—H13A0.9700
O10—C101.304 (5)C13—H13B0.9700
O11—C121.218 (4)C15—C161.490 (5)
O12—C121.280 (4)C15—H15A0.9700
O13—C141.226 (4)C15—H15B0.9700
O14—C141.299 (4)C17—C181.518 (6)
O15—C161.212 (5)C17—H17A0.9700
O16—C161.284 (5)C17—H17B0.9700
O17—C181.216 (5)C19—C201.516 (5)
O18—C181.294 (5)C19—H19A0.9700
O19—C201.214 (5)C19—H19B0.9700
O20—C201.307 (4)C21—C221.514 (5)
O21—C221.213 (4)C21—H21A0.9700
O22—C221.303 (4)C21—H21B0.9700
O23—C241.228 (4)C23—C241.510 (5)
O24—C241.285 (4)C23—H23A0.9700
O26—Ti2i1.751 (2)C23—H23B0.9700
O28—Ti4ii1.889 (2)C25—C261.471 (6)
N1—C11.476 (4)C25—H25A0.9700
N1—C31.477 (4)C25—H25B0.9700
N1—C51.483 (4)C26—H26A0.9700
N2—C111.471 (4)C26—H26B0.9700
N2—C91.475 (4)C27—C281.498 (5)
N2—C71.482 (4)C27—H27A0.9700
N3—C171.475 (5)C27—H27B0.9700
N3—C131.478 (4)C28—H28A0.9700
N3—C151.483 (4)C28—H28B0.9700
N4—C211.473 (4)O100—H10A0.8440
N4—C191.481 (4)O100—H10B0.8557
N4—C231.487 (4)O200—H20A0.8721
N5—C251.440 (5)O200—H20B0.8594
N5—H5A0.8900O300—H30A0.8808
N5—H5B0.8900O300—H30B0.8519
O25—Ti1—O26102.25 (11)O1—C2—O2123.7 (4)
O25—Ti1—O2105.18 (12)O1—C2—C1120.8 (4)
O26—Ti1—O289.75 (12)O2—C2—C1115.5 (3)
O25—Ti1—O6102.62 (11)N1—C3—C4114.3 (3)
O26—Ti1—O688.24 (11)N1—C3—H3A108.7
O2—Ti1—O6151.92 (10)C4—C3—H3A108.7
O25—Ti1—O493.07 (11)N1—C3—H3B108.7
O26—Ti1—O4164.58 (10)C4—C3—H3B108.7
O2—Ti1—O487.87 (12)H3A—C3—H3B107.6
O6—Ti1—O486.72 (12)O3—C4—O4124.7 (3)
O25—Ti1—N1171.11 (11)O3—C4—C3117.7 (3)
O26—Ti1—N186.51 (10)O4—C4—C3117.6 (3)
O2—Ti1—N176.04 (10)N1—C5—C6110.5 (3)
O6—Ti1—N175.88 (9)N1—C5—H5D109.6
O4—Ti1—N178.13 (10)C6—C5—H5D109.6
O26i—Ti2—O25103.42 (11)N1—C5—H5E109.6
O26i—Ti2—O8105.21 (12)C6—C5—H5E109.6
O25—Ti2—O888.98 (11)H5D—C5—H5E108.1
O26i—Ti2—O10102.80 (12)O5—C6—O6123.7 (3)
O25—Ti2—O1089.62 (12)O5—C6—C5120.3 (3)
O8—Ti2—O10151.50 (11)O6—C6—C5116.0 (3)
O26i—Ti2—O1292.31 (10)N2—C7—C8109.1 (3)
O25—Ti2—O12164.18 (10)N2—C7—H7D109.9
O8—Ti2—O1288.42 (11)C8—C7—H7D109.9
O10—Ti2—O1285.27 (11)N2—C7—H7E109.9
O26i—Ti2—N2170.20 (10)C8—C7—H7E109.9
O25—Ti2—N286.33 (10)H7D—C7—H7E108.3
O8—Ti2—N275.52 (10)O7—C8—O8123.3 (4)
O10—Ti2—N275.97 (10)O7—C8—C7120.5 (4)
O12—Ti2—N277.92 (10)O8—C8—C7116.2 (3)
O28—Ti3—O27103.75 (11)N2—C9—C10109.3 (3)
O28—Ti3—O18104.31 (12)N2—C9—H9A109.8
O27—Ti3—O1887.05 (12)C10—C9—H9A109.8
O28—Ti3—O14104.18 (12)N2—C9—H9B109.8
O27—Ti3—O1487.02 (11)C10—C9—H9B109.8
O18—Ti3—O14151.50 (11)H9A—C9—H9B108.3
O28—Ti3—O1692.91 (11)O9—C10—O10122.8 (4)
O27—Ti3—O16163.34 (11)O9—C10—C9122.0 (4)
O18—Ti3—O1689.16 (13)O10—C10—C9115.1 (3)
O14—Ti3—O1688.62 (12)N2—C11—C12113.7 (3)
O28—Ti3—N3170.08 (11)N2—C11—H11A108.8
O27—Ti3—N386.13 (10)C12—C11—H11A108.8
O18—Ti3—N376.75 (11)N2—C11—H11B108.8
O14—Ti3—N375.05 (10)C12—C11—H11B108.8
O16—Ti3—N377.22 (10)H11A—C11—H11B107.7
O27—Ti4—O28ii101.47 (11)O11—C12—O12124.4 (3)
O27—Ti4—O22104.46 (11)O11—C12—C11118.3 (3)
O28ii—Ti4—O2289.88 (11)O12—C12—C11117.3 (3)
O27—Ti4—O20103.84 (12)N3—C13—C14111.2 (3)
O28ii—Ti4—O2089.85 (11)N3—C13—H13A109.4
O22—Ti4—O20151.17 (10)C14—C13—H13A109.4
O27—Ti4—O2492.70 (10)N3—C13—H13B109.4
O28ii—Ti4—O24165.82 (10)C14—C13—H13B109.4
O22—Ti4—O2487.10 (11)H13A—C13—H13B108.0
O20—Ti4—O2486.17 (11)O13—C14—O14123.9 (4)
O27—Ti4—N4170.45 (11)O13—C14—C13120.4 (4)
O28ii—Ti4—N488.08 (10)O14—C14—C13115.7 (3)
O22—Ti4—N475.31 (9)N3—C15—C16113.2 (3)
O20—Ti4—N475.87 (10)N3—C15—H15A108.9
O24—Ti4—N477.75 (9)C16—C15—H15A108.9
C2—O2—Ti1121.3 (2)N3—C15—H15B108.9
C4—O4—Ti1121.9 (2)C16—C15—H15B108.9
C6—O6—Ti1120.8 (2)H15A—C15—H15B107.7
C8—O8—Ti2121.0 (2)O15—C16—O16123.5 (4)
C10—O10—Ti2122.5 (2)O15—C16—C15118.6 (4)
C12—O12—Ti2121.9 (2)O16—C16—C15117.9 (3)
C14—O14—Ti3119.4 (2)N3—C17—C18112.1 (3)
C16—O16—Ti3123.4 (2)N3—C17—H17A109.2
C18—O18—Ti3121.1 (2)C18—C17—H17A109.2
C20—O20—Ti4122.9 (2)N3—C17—H17B109.2
C22—O22—Ti4121.3 (2)C18—C17—H17B109.2
C24—O24—Ti4122.6 (2)H17A—C17—H17B107.9
Ti1—O25—Ti2162.66 (15)O17—C18—O18124.2 (4)
Ti2i—O26—Ti1171.64 (14)O17—C18—C17119.5 (4)
Ti4—O27—Ti3163.35 (15)O18—C18—C17116.2 (3)
Ti3—O28—Ti4ii170.80 (15)N4—C19—C20108.9 (3)
C1—N1—C3112.8 (3)N4—C19—H19A109.9
C1—N1—C5114.1 (3)C20—C19—H19A109.9
C3—N1—C5111.9 (3)N4—C19—H19B109.9
C1—N1—Ti1104.76 (18)C20—C19—H19B109.9
C3—N1—Ti1107.80 (18)H19A—C19—H19B108.3
C5—N1—Ti1104.65 (18)O19—C20—O20122.3 (4)
C11—N2—C9111.9 (3)O19—C20—C19122.7 (4)
C11—N2—C7112.2 (3)O20—C20—C19115.1 (3)
C9—N2—C7114.6 (3)N4—C21—C22109.3 (3)
C11—N2—Ti2108.01 (19)N4—C21—H21A109.8
C9—N2—Ti2105.2 (2)C22—C21—H21A109.8
C7—N2—Ti2104.1 (2)N4—C21—H21B109.8
C17—N3—C13113.4 (3)C22—C21—H21B109.8
C17—N3—C15113.2 (3)H21A—C21—H21B108.3
C13—N3—C15112.3 (3)O21—C22—O22122.8 (4)
C17—N3—Ti3105.2 (2)O21—C22—C21121.7 (3)
C13—N3—Ti3103.9 (2)O22—C22—C21115.4 (3)
C15—N3—Ti3108.0 (2)N4—C23—C24114.0 (3)
C21—N4—C19114.7 (3)N4—C23—H23A108.7
C21—N4—C23112.0 (3)C24—C23—H23A108.7
C19—N4—C23112.0 (3)N4—C23—H23B108.7
C21—N4—Ti4104.06 (19)C24—C23—H23B108.7
C19—N4—Ti4105.34 (19)H23A—C23—H23B107.6
C23—N4—Ti4108.03 (19)O23—C24—O24123.4 (3)
C25—N5—H5A109.5O23—C24—C23119.2 (3)
C25—N5—H5B109.5O24—C24—C23117.3 (3)
H5A—N5—H5B109.5N5—C25—C26112.4 (4)
C25—N5—H5C109.5N5—C25—H25A109.1
H5A—N5—H5C109.5C26—C25—H25A109.1
H5B—N5—H5C109.5N5—C25—H25B109.1
C26—N6—H6A109.5C26—C25—H25B109.1
C26—N6—H6B109.5H25A—C25—H25B107.9
H6A—N6—H6B109.5N6—C26—C25116.2 (4)
C26—N6—H6C109.5N6—C26—H26A108.2
H6A—N6—H6C109.5C25—C26—H26A108.2
H6B—N6—H6C109.5N6—C26—H26B108.2
C27—N7—H7A109.5C25—C26—H26B108.2
C27—N7—H7B109.5H26A—C26—H26B107.4
H7A—N7—H7B109.5N7—C27—C28113.8 (3)
C27—N7—H7C109.5N7—C27—H27A108.8
H7A—N7—H7C109.5C28—C27—H27A108.8
H7B—N7—H7C109.5N7—C27—H27B108.8
C28—N8—H8A109.5C28—C27—H27B108.8
C28—N8—H8B109.5H27A—C27—H27B107.7
H8A—N8—H8B109.5N8—C28—C27113.3 (3)
C28—N8—H8C109.5N8—C28—H28A108.9
H8A—N8—H8C109.5C27—C28—H28A108.9
H8B—N8—H8C109.5N8—C28—H28B108.9
N1—C1—C2110.6 (3)C27—C28—H28B108.9
N1—C1—H1A109.5H28A—C28—H28B107.7
C2—C1—H1A109.5H10A—O100—H10B107.7
N1—C1—H1B109.5H20A—O200—H20B104.9
C2—C1—H1B109.5H30A—O300—H30B104.8
H1A—C1—H1B108.1
Symmetry codes: (i) x+1, y+1, z+2; (ii) x, y+2, z+1.
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
N5—H5A···O1000.892.132.942 (13)151
N5—H5A···O11iii0.892.352.875 (5)117
N5—H5A···O17iv0.892.513.172 (6)132
N5—H5B···O20iv0.891.962.827 (5)163
N5—H5C···O15v0.892.193.016 (7)155
N6—H6A···O21vi0.892.002.891 (5)176
N6—H6A···O22vi0.892.503.080 (4)124
N6—H6B···O11i0.891.902.781 (4)172
N6—H6C···O13vi0.891.912.778 (5)166
N7—H7A···O7vii0.891.932.733 (4)150
N7—H7B···O10i0.892.032.872 (4)157
N7—H7C···O3viii0.892.042.889 (5)159
N8—H8A···O5i0.891.902.762 (4)163
N8—H8B···O23ix0.892.002.795 (4)148
N8—H8C···O3viii0.891.872.743 (4)167
O100—H10A···O150.842.162.781 (10)130
O100—H10A···O160.842.533.329 (10)158
O200—H20A···O14vi0.872.182.755 (10)124
O200—H20B···O16v0.862.273.087 (11)160
O200—H20B···O15v0.862.453.187 (12)145
O300—H30A···O4x0.882.142.917 (15)147
O300—H30A···O3x0.882.192.767 (14)123
O300—H30B···O60.851.862.647 (13)153
O300—H30B···O50.852.583.314 (15)145
Symmetry codes: (i) x+1, y+1, z+2; (iii) x, y, z1; (iv) x, y+1, z+1; (v) x+1, y+1, z+1; (vi) x, y1, z; (vii) x, y+1, z+2; (viii) x, y+1, z; (ix) x, y+2, z+2; (x) x+1, y, z+2.
 

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