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The structure of the title compound, C16H40N4P+·Br·0.5H2O or [P{N(C2H5)2}4]Br·0.5H2O, at 130 K has Z′ = 4 and is ionic, with Br not bonded to P. The P atoms are tetrahedral, with P—N distances in the range 1.628 (2)–1.6400 (19) Å. The N atoms are approximately planar. The water mol­ecules form cyclic hydrogen-bonded [(H2O)2Br2]2− units about inversion centers, with O...Br distances in the range 3.425 (2)–3.611 (3) Å.

Supporting information

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0108270100010453/da1144sup1.cif
Contains datablocks global, III

hkl

Structure factor file (CIF format) https://doi.org/10.1107/S0108270100010453/da1144IIIsup2.hkl
Contains datablock III

CCDC reference: 153899

Computing details top

Data collection: please provide details; cell refinement: DENZO (Otwinowski & Minor, 1997); data reduction: DENZO; program(s) used to solve structure: SIR92 (Altomare et al., 1994); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPIII (Burnett & Johnson, 1996) and PLUTON (Spek, 1990); software used to prepare material for publication: maXus (Mackay et al., 1999).

Tetrakis(diethylamino)phosphonium bromide hemihydrate top
Crystal data top
C16H40N4P+·Br·0.5H2OF(000) = 1752
Mr = 408.4Dx = 1.229 Mg m3
Triclinic, P1Melting point: 412 K
a = 14.2475 (2) ÅMo Kα radiation, λ = 0.71073 Å
b = 14.9756 (3) ÅCell parameters from 43363 reflections
c = 20.7125 (5) Åθ = 1.0–27.5°
α = 92.144 (2)°µ = 1.94 mm1
β = 91.799 (2)°T = 130 K
γ = 90.246 (2)°Fragment, colorless
V = 4414.0 (3) Å30.27 × 0.25 × 0.22 mm
Z = 8
Data collection top
Nonius KappaCCD (with Oxford Cryostream)
diffractometer
20107 independent reflections
Radiation source: sealed tube11547 reflections with I > 2σ(I)
Graphite monochromatorRint = 0.064
ω scans with κ offsetsθmax = 27.5°
Absorption correction: multi-scan
(SORTAV; Blessing, 1995)
h = 1818
Tmin = 0.600, Tmax = 0.652k = 1919
43363 measured reflectionsl = 2626
Refinement top
Refinement on F2Secondary atom site location: difference Fourier map
Least-squares matrix: fullHydrogen site location: inferred from neighbouring sites
R[F2 > 2σ(F2)] = 0.036H atoms treated by a mixture of independent and constrained refinement
wR(F2) = 0.072 w = 1/[σ2(Fo2) + (0.0282P)2]
where P = (Fo2 + 2Fc2)/3
S = 0.89(Δ/σ)max = 0.005
20107 reflectionsΔρmax = 0.66 e Å3
860 parametersΔρmin = 0.45 e Å3
4 restraintsExtinction correction: SHELXL97 (Sheldrick, 1997), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4
Primary atom site location: structure-invariant direct methodsExtinction coefficient: 0.00103 (8)
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
Br10.441885 (16)0.960335 (17)0.121215 (14)0.03876 (8)
Br20.416410 (16)0.552451 (16)0.612750 (15)0.03875 (8)
Br30.041737 (16)0.931885 (17)0.678825 (14)0.03768 (8)
Br40.055817 (16)0.562574 (16)0.163999 (14)0.03490 (7)
P10.71720 (4)0.73037 (4)0.74630 (3)0.02191 (14)
P20.74148 (4)0.75833 (4)0.24715 (3)0.02454 (15)
P30.21208 (4)0.73480 (4)0.95525 (3)0.02184 (14)
P40.22316 (4)0.76662 (4)0.46884 (3)0.02345 (15)
O1W0.64136 (14)0.96203 (14)0.03319 (14)0.0462 (5)
H1W10.6258 (18)0.9800 (18)0.0008 (10)0.040 (10)*
H2W10.5949 (16)0.965 (2)0.0513 (15)0.073 (12)*
O2W0.36975 (15)0.44743 (15)0.46308 (14)0.0485 (5)
H1W20.378 (2)0.465 (2)0.4982 (10)0.059 (12)*
H2W20.4194 (14)0.448 (2)0.4473 (15)0.061 (11)*
N10.75389 (12)0.79770 (12)0.80588 (9)0.0246 (5)
N20.67685 (11)0.64224 (12)0.78105 (10)0.0240 (5)
N30.63572 (11)0.77663 (12)0.70119 (9)0.0237 (5)
N40.80090 (11)0.70463 (12)0.69685 (9)0.0235 (4)
N50.70919 (12)0.84118 (12)0.29533 (10)0.0265 (5)
N60.82603 (11)0.78767 (11)0.20071 (9)0.0227 (4)
N70.65565 (12)0.72608 (12)0.19724 (10)0.0267 (5)
N80.77422 (13)0.67922 (12)0.29534 (10)0.0293 (5)
N90.18732 (11)0.79858 (11)0.89479 (10)0.0236 (5)
N100.15641 (11)0.63922 (11)0.94707 (9)0.0213 (4)
N110.18254 (12)0.79277 (12)1.01980 (10)0.0254 (5)
N120.32350 (11)0.70817 (12)0.95775 (9)0.0236 (5)
N130.32796 (12)0.77972 (12)0.43991 (10)0.0257 (5)
N140.16977 (12)0.86095 (12)0.45595 (9)0.0233 (4)
N150.22793 (12)0.74419 (12)0.54517 (9)0.0250 (5)
N160.16729 (12)0.68243 (12)0.43298 (10)0.0262 (5)
C10.82807 (16)0.86499 (15)0.79559 (13)0.0322 (6)
H1A0.86520.84440.75840.039*
H1B0.87090.86820.83420.039*
C20.79219 (18)0.95828 (16)0.78315 (14)0.0471 (8)
H2A0.74810.95590.74580.071*
H2B0.84520.99740.77430.071*
H2C0.76010.98180.82130.071*
C30.69815 (15)0.81560 (16)0.86430 (12)0.0299 (6)
H3A0.64430.77350.86350.036*
H3B0.67260.87690.86290.036*
C40.75433 (17)0.80654 (18)0.92747 (13)0.0398 (7)
H4A0.77380.74430.93160.060*
H4B0.71530.82440.96380.060*
H4C0.81000.84520.92760.060*
C50.60547 (15)0.58446 (14)0.74692 (12)0.0284 (6)
H5A0.56730.62140.71750.034*
H5B0.56300.56070.77910.034*
C60.64532 (18)0.50710 (16)0.70814 (14)0.0426 (7)
H6A0.68870.52970.67670.064*
H6B0.59410.47400.68530.064*
H6C0.67910.46730.73720.064*
C70.72899 (15)0.59970 (16)0.83485 (12)0.0316 (6)
H7A0.77990.64050.85130.038*
H7B0.75840.54410.81810.038*
C80.66681 (18)0.57754 (19)0.89019 (14)0.0466 (7)
H8A0.63480.63170.90550.070*
H8B0.70540.55390.92560.070*
H8C0.62000.53260.87520.070*
C90.56698 (15)0.83806 (15)0.73130 (13)0.0311 (6)
H9A0.54650.88190.69920.037*
H9B0.59860.87160.76800.037*
C100.48023 (15)0.79119 (17)0.75581 (14)0.0418 (7)
H10A0.44840.75770.71990.063*
H10B0.43730.83590.77390.063*
H10C0.49940.75000.78940.063*
C110.60572 (16)0.73888 (15)0.63643 (12)0.0300 (6)
H11A0.54280.71120.63930.036*
H11B0.65000.69120.62340.036*
C120.60172 (18)0.80799 (17)0.58492 (13)0.0432 (7)
H12A0.55060.84990.59370.065*
H12B0.59050.77810.54250.065*
H12C0.66150.84070.58530.065*
C130.86781 (15)0.63232 (15)0.71162 (13)0.0312 (6)
H13A0.88530.60170.67060.037*
H13B0.83600.58800.73780.037*
C140.95656 (16)0.66442 (18)0.74779 (14)0.0447 (8)
H14A0.98810.70920.72260.067*
H14B0.99860.61370.75420.067*
H14C0.94040.69110.78990.067*
C150.83246 (16)0.76597 (15)0.64702 (12)0.0302 (6)
H15A0.89410.79210.66100.036*
H15B0.78700.81550.64330.036*
C160.84128 (18)0.71901 (18)0.58125 (13)0.0424 (7)
H16A0.89630.68000.58200.064*
H16B0.84850.76360.54830.064*
H16C0.78470.68310.57110.064*
C170.64252 (16)0.90836 (15)0.27030 (13)0.0328 (6)
H17A0.61060.93710.30740.039*
H17B0.59390.87690.24270.039*
C180.68609 (16)0.98087 (15)0.23148 (13)0.0346 (6)
H18A0.73081.01580.25920.052*
H18B0.63671.02020.21520.052*
H18C0.71890.95340.19500.052*
C190.76672 (17)0.87253 (16)0.35283 (12)0.0344 (6)
H19A0.79410.93160.34430.041*
H19B0.81920.83040.35950.041*
C200.71090 (19)0.88039 (17)0.41479 (14)0.0453 (7)
H20A0.65930.92260.40880.068*
H20B0.75240.90190.45070.068*
H20C0.68530.82170.42440.068*
C210.85254 (15)0.73387 (15)0.14237 (12)0.0281 (6)
H21A0.80390.68750.13260.034*
H21B0.91250.70310.15170.034*
C220.86326 (16)0.78994 (17)0.08349 (12)0.0361 (6)
H22A0.80900.82940.07900.054*
H22B0.86700.75060.04480.054*
H22C0.92070.82600.08870.054*
C230.89752 (14)0.85493 (14)0.22334 (12)0.0266 (6)
H23A0.86940.89580.25600.032*
H23B0.91480.89100.18640.032*
C240.98553 (15)0.81531 (17)0.25249 (14)0.0422 (7)
H24A0.96980.78250.29080.063*
H24B1.03020.86330.26490.063*
H24C1.01380.77440.22070.063*
C250.62954 (15)0.77433 (16)0.13856 (12)0.0301 (6)
H25A0.67840.81970.13130.036*
H25B0.56970.80610.14560.036*
C260.61833 (17)0.71331 (17)0.07840 (13)0.0395 (7)
H26A0.67710.68120.07130.059*
H26B0.60300.74920.04090.059*
H26C0.56760.67020.08430.059*
C270.58354 (16)0.66201 (17)0.21756 (14)0.0397 (7)
H27A0.60970.62830.25410.048*
H27B0.56940.61860.18130.048*
C280.49270 (18)0.7059 (2)0.23785 (17)0.0658 (10)
H28A0.50600.74940.27350.099*
H28B0.44930.66010.25200.099*
H28C0.46420.73640.20110.099*
C290.84066 (17)0.60997 (16)0.27267 (14)0.0386 (7)
H29A0.88000.59150.31000.046*
H29B0.88280.63670.24150.046*
C300.7945 (2)0.52746 (16)0.24082 (15)0.0478 (8)
H30A0.75550.49830.27210.072*
H30B0.84310.48600.22610.072*
H30C0.75520.54480.20370.072*
C310.72009 (18)0.65512 (17)0.35221 (13)0.0408 (7)
H31A0.68840.59690.34280.049*
H31B0.67080.70050.35950.049*
C320.7808 (2)0.64880 (19)0.41389 (14)0.0553 (8)
H32A0.82750.60160.40800.083*
H32B0.74100.63480.44990.083*
H32C0.81290.70600.42340.083*
C330.24661 (15)0.80021 (16)0.83800 (12)0.0289 (6)
H33A0.30870.77500.84970.035*
H33B0.25660.86320.82690.035*
C340.20733 (17)0.74938 (19)0.77877 (13)0.0458 (7)
H34A0.18910.68900.79040.069*
H34B0.25520.74550.74590.069*
H34C0.15220.78060.76160.069*
C350.09616 (15)0.84564 (15)0.88796 (13)0.0312 (6)
H35A0.06230.84160.92880.037*
H35B0.05750.81480.85330.037*
C360.10628 (17)0.94318 (15)0.87225 (14)0.0412 (7)
H36A0.15260.97200.90220.062*
H36B0.04560.97300.87650.062*
H36C0.12720.94760.82790.062*
C370.17664 (15)0.56269 (14)0.98884 (12)0.0245 (5)
H37A0.12540.55691.01960.029*
H37B0.23560.57491.01430.029*
C380.18627 (16)0.47475 (14)0.95001 (13)0.0305 (6)
H38A0.12740.46130.92580.046*
H38B0.20020.42660.97950.046*
H38C0.23740.47990.91980.046*
C390.06536 (13)0.63277 (15)0.91056 (12)0.0263 (6)
H39A0.05950.57260.88940.032*
H39B0.06480.67700.87620.032*
C400.01919 (15)0.64909 (18)0.95276 (14)0.0426 (7)
H40A0.01650.60880.98900.064*
H40B0.07710.63780.92690.064*
H40C0.01830.71120.96950.064*
C410.20365 (15)0.88949 (15)1.02915 (13)0.0342 (6)
H41A0.22760.91230.98850.041*
H41B0.25370.89801.06310.041*
C420.11735 (17)0.94371 (17)1.04860 (15)0.0483 (8)
H42A0.06540.93081.01740.072*
H42B0.13261.00761.04900.072*
H42C0.09880.92741.09180.072*
C430.16194 (16)0.74718 (16)1.08003 (12)0.0318 (6)
H43A0.13190.68881.06840.038*
H43B0.11610.78351.10440.038*
C440.24732 (18)0.73134 (19)1.12402 (14)0.0510 (8)
H44A0.29120.69161.10160.076*
H44B0.22730.70371.16350.076*
H44C0.27850.78851.13530.076*
C450.36211 (15)0.63720 (15)0.91508 (13)0.0294 (6)
H45A0.40120.66510.88260.035*
H45B0.30950.60540.89170.035*
C460.42124 (16)0.56969 (16)0.95124 (14)0.0411 (7)
H46A0.47700.59960.97090.062*
H46B0.44060.52190.92100.062*
H46C0.38410.54420.98510.062*
C470.39405 (14)0.76687 (15)0.99242 (12)0.0284 (6)
H47A0.43350.72991.02110.034*
H47B0.36070.81081.02020.034*
C480.45732 (16)0.81688 (17)0.94913 (14)0.0402 (7)
H48A0.49390.77410.92340.060*
H48B0.50000.85560.97560.060*
H48C0.41910.85340.92020.060*
C490.37856 (15)0.70406 (16)0.40904 (13)0.0322 (6)
H49A0.39390.72000.36460.039*
H49B0.33600.65150.40560.039*
C500.46832 (15)0.67780 (16)0.44442 (14)0.0379 (7)
H50A0.51370.72720.44420.057*
H50B0.49470.62470.42280.057*
H50C0.45460.66450.48910.057*
C510.38350 (15)0.86171 (16)0.45209 (13)0.0347 (7)
H51A0.43490.84960.48380.042*
H51B0.34290.90810.47170.042*
C520.42580 (18)0.89807 (18)0.39158 (16)0.0527 (8)
H52A0.47210.85570.37480.079*
H52B0.45660.95560.40240.079*
H52C0.37590.90630.35870.079*
C530.09380 (15)0.89241 (15)0.49813 (13)0.0342 (6)
H53A0.09700.95840.50270.041*
H53B0.10450.86840.54160.041*
C540.00418 (16)0.86509 (18)0.47309 (15)0.0484 (8)
H54A0.01730.89220.43150.073*
H54B0.05060.88560.50420.073*
H54C0.00770.79990.46750.073*
C550.17315 (16)0.90638 (15)0.39383 (12)0.0312 (6)
H55A0.11090.90110.37140.037*
H55B0.21950.87590.36610.037*
C560.19963 (18)1.00469 (15)0.40243 (14)0.0399 (7)
H56A0.14961.03690.42470.060*
H56B0.20791.02980.36000.060*
H56C0.25841.01070.42810.060*
C570.30818 (15)0.77441 (15)0.58728 (12)0.0303 (6)
H57A0.36570.77300.56170.036*
H57B0.31690.73190.62240.036*
C580.29668 (17)0.86813 (16)0.61713 (13)0.0399 (7)
H58A0.29130.91120.58270.060*
H58B0.35150.88330.64530.060*
H58C0.23990.87020.64260.060*
C590.14419 (15)0.71520 (15)0.57984 (13)0.0318 (6)
H59A0.09130.70550.54820.038*
H59B0.12620.76370.61070.038*
C600.15956 (18)0.62981 (16)0.61662 (14)0.0417 (7)
H60A0.17850.58160.58660.063*
H60B0.10110.61300.63680.063*
H60C0.20890.64000.65010.063*
C610.11546 (16)0.69341 (16)0.37080 (13)0.0366 (7)
H61A0.09060.75500.37000.044*
H61B0.06110.65190.36850.044*
C620.1733 (2)0.6766 (2)0.31164 (15)0.0655 (10)
H62A0.22120.72350.30960.098*
H62B0.13240.67700.27280.098*
H62C0.20400.61830.31420.098*
C630.18881 (16)0.58791 (15)0.44878 (14)0.0343 (6)
H63A0.23170.58760.48730.041*
H63B0.22140.55860.41220.041*
C640.10029 (18)0.53465 (17)0.46200 (15)0.0487 (8)
H64A0.06400.56700.49470.073*
H64B0.11790.47600.47780.073*
H64C0.06210.52670.42200.073*
Atomic displacement parameters (Å2) top
U11U22U33U12U13U23
Br10.03329 (14)0.03597 (15)0.0469 (2)0.00376 (11)0.00133 (13)0.00100 (13)
Br20.03246 (13)0.02973 (14)0.0539 (2)0.00266 (11)0.00206 (13)0.00097 (13)
Br30.03336 (13)0.03692 (15)0.04231 (19)0.00509 (11)0.00429 (12)0.00632 (13)
Br40.03144 (13)0.02819 (14)0.04470 (19)0.00239 (11)0.00227 (12)0.00003 (12)
P10.0211 (3)0.0226 (3)0.0220 (4)0.0002 (2)0.0005 (3)0.0022 (3)
P20.0300 (3)0.0210 (3)0.0227 (4)0.0024 (3)0.0018 (3)0.0013 (3)
P30.0196 (3)0.0215 (3)0.0245 (4)0.0015 (2)0.0006 (3)0.0018 (3)
P40.0230 (3)0.0230 (3)0.0242 (4)0.0014 (3)0.0001 (3)0.0001 (3)
O1W0.0343 (12)0.0511 (13)0.0536 (18)0.0018 (10)0.0046 (12)0.0058 (13)
O2W0.0363 (12)0.0594 (14)0.0491 (17)0.0009 (10)0.0015 (12)0.0065 (13)
N10.0261 (10)0.0276 (11)0.0200 (12)0.0003 (8)0.0005 (9)0.0020 (9)
N20.0213 (9)0.0245 (10)0.0265 (13)0.0007 (8)0.0002 (9)0.0052 (9)
N30.0243 (10)0.0248 (10)0.0218 (12)0.0006 (8)0.0048 (9)0.0019 (9)
N40.0240 (9)0.0241 (10)0.0225 (12)0.0002 (8)0.0002 (9)0.0026 (9)
N50.0329 (10)0.0232 (10)0.0234 (13)0.0045 (9)0.0062 (9)0.0020 (9)
N60.0250 (9)0.0200 (10)0.0230 (13)0.0013 (8)0.0013 (9)0.0004 (9)
N70.0292 (10)0.0258 (11)0.0252 (13)0.0062 (9)0.0009 (9)0.0025 (9)
N80.0424 (11)0.0224 (11)0.0233 (13)0.0016 (9)0.0004 (10)0.0047 (9)
N90.0222 (9)0.0225 (10)0.0265 (13)0.0023 (8)0.0026 (9)0.0070 (9)
N100.0190 (9)0.0193 (10)0.0257 (13)0.0004 (8)0.0003 (8)0.0025 (9)
N110.0256 (10)0.0215 (10)0.0288 (13)0.0053 (8)0.0034 (9)0.0027 (9)
N120.0194 (9)0.0245 (10)0.0268 (13)0.0017 (8)0.0007 (9)0.0005 (9)
N130.0246 (10)0.0257 (11)0.0268 (13)0.0011 (8)0.0018 (9)0.0006 (9)
N140.0258 (10)0.0236 (10)0.0208 (12)0.0026 (8)0.0048 (9)0.0008 (9)
N150.0280 (10)0.0271 (11)0.0201 (12)0.0002 (8)0.0028 (9)0.0037 (9)
N160.0263 (10)0.0203 (10)0.0315 (14)0.0038 (8)0.0029 (9)0.0015 (9)
C10.0328 (13)0.0367 (15)0.0263 (16)0.0087 (11)0.0005 (12)0.0058 (12)
C20.0619 (18)0.0351 (16)0.045 (2)0.0085 (14)0.0139 (15)0.0022 (14)
C30.0341 (13)0.0321 (14)0.0232 (16)0.0034 (11)0.0018 (12)0.0026 (12)
C40.0445 (15)0.0502 (17)0.0241 (17)0.0035 (13)0.0011 (13)0.0039 (13)
C50.0298 (12)0.0239 (13)0.0318 (17)0.0027 (10)0.0008 (12)0.0064 (12)
C60.0491 (16)0.0292 (15)0.049 (2)0.0034 (12)0.0038 (14)0.0036 (14)
C70.0286 (12)0.0358 (15)0.0308 (17)0.0044 (11)0.0015 (12)0.0100 (12)
C80.0473 (16)0.0576 (19)0.0364 (19)0.0004 (14)0.0005 (14)0.0206 (15)
C90.0326 (13)0.0275 (13)0.0333 (17)0.0106 (11)0.0014 (12)0.0040 (12)
C100.0286 (13)0.0477 (17)0.050 (2)0.0105 (12)0.0069 (13)0.0048 (15)
C110.0274 (12)0.0321 (14)0.0303 (17)0.0055 (11)0.0052 (11)0.0029 (12)
C120.0513 (16)0.0486 (17)0.0293 (18)0.0121 (14)0.0125 (14)0.0097 (14)
C130.0296 (12)0.0301 (14)0.0346 (17)0.0040 (11)0.0071 (12)0.0022 (12)
C140.0268 (13)0.0512 (18)0.057 (2)0.0041 (12)0.0046 (13)0.0112 (15)
C150.0305 (13)0.0307 (14)0.0300 (17)0.0049 (11)0.0033 (12)0.0072 (12)
C160.0498 (16)0.0486 (17)0.0288 (18)0.0107 (13)0.0090 (14)0.0032 (14)
C170.0335 (13)0.0270 (14)0.0383 (18)0.0019 (11)0.0096 (12)0.0004 (12)
C180.0384 (14)0.0251 (14)0.0405 (19)0.0024 (11)0.0053 (13)0.0033 (12)
C190.0462 (15)0.0283 (14)0.0285 (17)0.0061 (12)0.0036 (13)0.0041 (12)
C200.0646 (18)0.0372 (16)0.0341 (19)0.0102 (14)0.0117 (15)0.0074 (14)
C210.0273 (12)0.0302 (14)0.0264 (16)0.0021 (10)0.0007 (11)0.0051 (12)
C220.0380 (14)0.0485 (17)0.0217 (16)0.0030 (12)0.0038 (12)0.0023 (13)
C230.0275 (12)0.0237 (13)0.0286 (16)0.0049 (10)0.0002 (11)0.0017 (11)
C240.0348 (14)0.0422 (16)0.048 (2)0.0008 (13)0.0126 (14)0.0022 (14)
C250.0222 (12)0.0338 (14)0.0343 (17)0.0037 (11)0.0002 (11)0.0022 (12)
C260.0365 (14)0.0470 (17)0.0342 (18)0.0058 (12)0.0101 (13)0.0001 (14)
C270.0430 (15)0.0396 (16)0.0362 (19)0.0174 (13)0.0005 (13)0.0011 (13)
C280.0441 (17)0.073 (2)0.082 (3)0.0202 (16)0.0277 (18)0.006 (2)
C290.0491 (15)0.0294 (14)0.0373 (19)0.0063 (12)0.0066 (14)0.0063 (13)
C300.075 (2)0.0236 (14)0.044 (2)0.0042 (14)0.0037 (16)0.0016 (13)
C310.0632 (17)0.0305 (15)0.0293 (18)0.0106 (13)0.0057 (15)0.0039 (13)
C320.087 (2)0.0486 (18)0.030 (2)0.0087 (16)0.0014 (17)0.0072 (15)
C330.0262 (12)0.0324 (14)0.0289 (16)0.0017 (11)0.0042 (11)0.0095 (12)
C340.0389 (15)0.067 (2)0.0310 (19)0.0047 (14)0.0035 (13)0.0017 (15)
C350.0262 (12)0.0286 (14)0.0393 (18)0.0062 (10)0.0035 (12)0.0070 (12)
C360.0439 (15)0.0322 (15)0.049 (2)0.0113 (12)0.0073 (14)0.0140 (14)
C370.0254 (12)0.0248 (13)0.0235 (15)0.0006 (10)0.0006 (11)0.0048 (11)
C380.0334 (13)0.0241 (13)0.0340 (17)0.0006 (11)0.0008 (12)0.0024 (12)
C390.0220 (11)0.0264 (13)0.0300 (16)0.0042 (10)0.0063 (11)0.0025 (11)
C400.0222 (12)0.0523 (17)0.054 (2)0.0027 (12)0.0041 (13)0.0083 (15)
C410.0337 (13)0.0280 (14)0.0404 (19)0.0061 (11)0.0009 (12)0.0048 (12)
C420.0493 (16)0.0326 (15)0.062 (2)0.0080 (13)0.0057 (15)0.0108 (15)
C430.0338 (13)0.0353 (15)0.0263 (16)0.0044 (11)0.0062 (12)0.0039 (12)
C440.0530 (17)0.065 (2)0.035 (2)0.0175 (15)0.0082 (15)0.0101 (16)
C450.0245 (12)0.0299 (14)0.0340 (17)0.0036 (10)0.0050 (11)0.0002 (12)
C460.0291 (13)0.0373 (15)0.058 (2)0.0079 (12)0.0066 (13)0.0071 (14)
C470.0202 (11)0.0321 (14)0.0324 (17)0.0037 (10)0.0040 (11)0.0001 (12)
C480.0345 (14)0.0382 (16)0.047 (2)0.0129 (12)0.0012 (13)0.0049 (14)
C490.0311 (13)0.0353 (15)0.0301 (17)0.0038 (11)0.0061 (12)0.0047 (12)
C500.0319 (13)0.0352 (15)0.046 (2)0.0085 (11)0.0010 (13)0.0013 (13)
C510.0283 (13)0.0306 (14)0.046 (2)0.0039 (11)0.0043 (12)0.0055 (13)
C520.0429 (16)0.0435 (17)0.074 (3)0.0045 (13)0.0157 (16)0.0164 (17)
C530.0410 (14)0.0247 (13)0.0373 (18)0.0068 (11)0.0112 (13)0.0000 (12)
C540.0304 (14)0.0490 (18)0.067 (2)0.0113 (13)0.0110 (14)0.0060 (16)
C550.0350 (13)0.0304 (14)0.0283 (17)0.0042 (11)0.0004 (12)0.0044 (12)
C560.0522 (16)0.0290 (14)0.0391 (19)0.0022 (12)0.0032 (14)0.0094 (13)
C570.0355 (13)0.0310 (14)0.0242 (16)0.0018 (11)0.0031 (12)0.0014 (12)
C580.0464 (15)0.0363 (15)0.0357 (19)0.0010 (12)0.0050 (14)0.0083 (13)
C590.0339 (13)0.0304 (14)0.0317 (17)0.0007 (11)0.0060 (12)0.0051 (12)
C600.0489 (16)0.0401 (16)0.0373 (19)0.0015 (13)0.0093 (14)0.0114 (14)
C610.0343 (13)0.0313 (14)0.0427 (19)0.0068 (11)0.0119 (13)0.0087 (13)
C620.072 (2)0.089 (2)0.034 (2)0.0421 (19)0.0157 (17)0.0183 (18)
C630.0383 (14)0.0229 (13)0.0416 (19)0.0043 (11)0.0016 (13)0.0007 (12)
C640.0542 (17)0.0279 (15)0.064 (2)0.0098 (13)0.0041 (16)0.0022 (15)
Geometric parameters (Å, º) top
P1—N41.6343 (19)C24—H24B0.9800
P1—N11.6355 (19)C24—H24C0.9800
P1—N21.6371 (19)C25—C261.521 (3)
P1—N31.6395 (18)C25—H25A0.9900
P2—N61.6339 (19)C25—H25B0.9900
P2—N71.6357 (19)C26—H26A0.9800
P2—N81.637 (2)C26—H26B0.9800
P2—N51.6397 (19)C26—H26C0.9800
P3—N101.6338 (18)C27—C281.518 (3)
P3—N91.6340 (19)C27—H27A0.9900
P3—N111.6342 (19)C27—H27B0.9900
P3—N121.6382 (17)C28—H28A0.9800
P4—N151.628 (2)C28—H28B0.9800
P4—N161.6305 (18)C28—H28C0.9800
P4—N141.6343 (18)C29—C301.516 (3)
P4—N131.6400 (18)C29—H29A0.9900
O1W—H1W10.789 (16)C29—H29B0.9900
O1W—H2W10.773 (17)C30—H30A0.9800
O2W—H1W20.766 (17)C30—H30B0.9800
O2W—H2W20.790 (16)C30—H30C0.9800
N1—C11.483 (3)C31—C321.526 (4)
N1—C31.485 (3)C31—H31A0.9900
N2—C51.478 (3)C31—H31B0.9900
N2—C71.485 (3)C32—H32A0.9800
N3—C91.483 (3)C32—H32B0.9800
N3—C111.485 (3)C32—H32C0.9800
N4—C131.480 (3)C33—C341.510 (3)
N4—C151.486 (3)C33—H33A0.9900
N5—C171.483 (3)C33—H33B0.9900
N5—C191.485 (3)C34—H34A0.9800
N6—C231.483 (3)C34—H34B0.9800
N6—C211.486 (3)C34—H34C0.9800
N7—C251.476 (3)C35—C361.515 (3)
N7—C271.484 (3)C35—H35A0.9900
N8—C291.480 (3)C35—H35B0.9900
N8—C311.483 (3)C36—H36A0.9800
N9—C331.470 (3)C36—H36B0.9800
N9—C351.486 (3)C36—H36C0.9800
N10—C391.482 (3)C37—C381.527 (3)
N10—C371.485 (3)C37—H37A0.9900
N11—C431.481 (3)C37—H37B0.9900
N11—C411.483 (3)C38—H38A0.9800
N12—C451.476 (3)C38—H38B0.9800
N12—C471.483 (3)C38—H38C0.9800
N13—C511.468 (3)C39—C401.526 (3)
N13—C491.481 (3)C39—H39A0.9900
N14—C531.480 (3)C39—H39B0.9900
N14—C551.480 (3)C40—H40A0.9800
N15—C571.475 (3)C40—H40B0.9800
N15—C591.483 (3)C40—H40C0.9800
N16—C611.479 (3)C41—C421.532 (3)
N16—C631.496 (3)C41—H41A0.9900
C1—C21.518 (3)C41—H41B0.9900
C1—H1A0.9900C42—H42A0.9800
C1—H1B0.9900C42—H42B0.9800
C2—H2A0.9800C42—H42C0.9800
C2—H2B0.9800C43—C441.522 (3)
C2—H2C0.9800C43—H43A0.9900
C3—C41.523 (3)C43—H43B0.9900
C3—H3A0.9900C44—H44A0.9800
C3—H3B0.9900C44—H44B0.9800
C4—H4A0.9800C44—H44C0.9800
C4—H4B0.9800C45—C461.522 (3)
C4—H4C0.9800C45—H45A0.9900
C5—C61.508 (3)C45—H45B0.9900
C5—H5A0.9900C46—H46A0.9800
C5—H5B0.9900C46—H46B0.9800
C6—H6A0.9800C46—H46C0.9800
C6—H6B0.9800C47—C481.508 (3)
C6—H6C0.9800C47—H47A0.9900
C7—C81.516 (3)C47—H47B0.9900
C7—H7A0.9900C48—H48A0.9800
C7—H7B0.9900C48—H48B0.9800
C8—H8A0.9800C48—H48C0.9800
C8—H8B0.9800C49—C501.515 (3)
C8—H8C0.9800C49—H49A0.9900
C9—C101.528 (3)C49—H49B0.9900
C9—H9A0.9900C50—H50A0.9800
C9—H9B0.9900C50—H50B0.9800
C10—H10A0.9800C50—H50C0.9800
C10—H10B0.9800C51—C521.525 (4)
C10—H10C0.9800C51—H51A0.9900
C11—C121.514 (3)C51—H51B0.9900
C11—H11A0.9900C52—H52A0.9800
C11—H11B0.9900C52—H52B0.9800
C12—H12A0.9800C52—H52C0.9800
C12—H12B0.9800C53—C541.523 (3)
C12—H12C0.9800C53—H53A0.9900
C13—C141.517 (3)C53—H53B0.9900
C13—H13A0.9900C54—H54A0.9800
C13—H13B0.9900C54—H54B0.9800
C14—H14A0.9800C54—H54C0.9800
C14—H14B0.9800C55—C561.520 (3)
C14—H14C0.9800C55—H55A0.9900
C15—C161.518 (3)C55—H55B0.9900
C15—H15A0.9900C56—H56A0.9800
C15—H15B0.9900C56—H56B0.9800
C16—H16A0.9800C56—H56C0.9800
C16—H16B0.9800C57—C581.524 (3)
C16—H16C0.9800C57—H57A0.9900
C17—C181.517 (3)C57—H57B0.9900
C17—H17A0.9900C58—H58A0.9800
C17—H17B0.9900C58—H58B0.9800
C18—H18A0.9800C58—H58C0.9800
C18—H18B0.9800C59—C601.526 (3)
C18—H18C0.9800C59—H59A0.9900
C19—C201.532 (3)C59—H59B0.9900
C19—H19A0.9900C60—H60A0.9800
C19—H19B0.9900C60—H60B0.9800
C20—H20A0.9800C60—H60C0.9800
C20—H20B0.9800C61—C621.512 (4)
C20—H20C0.9800C61—H61A0.9900
C21—C221.517 (3)C61—H61B0.9900
C21—H21A0.9900C62—H62A0.9800
C21—H21B0.9900C62—H62B0.9800
C22—H22A0.9800C62—H62C0.9800
C22—H22B0.9800C63—C641.527 (3)
C22—H22C0.9800C63—H63A0.9900
C23—C241.508 (3)C63—H63B0.9900
C23—H23A0.9900C64—H64A0.9800
C23—H23B0.9900C64—H64B0.9800
C24—H24A0.9800C64—H64C0.9800
N4—P1—N1112.11 (9)H26B—C26—H26C109.5
N4—P1—N2111.82 (9)N7—C27—C28113.8 (2)
N1—P1—N2105.01 (10)N7—C27—H27A108.8
N4—P1—N3104.91 (10)C28—C27—H27A108.8
N1—P1—N3111.76 (9)N7—C27—H27B108.8
N2—P1—N3111.41 (9)C28—C27—H27B108.8
N6—P2—N7104.84 (10)H27A—C27—H27B107.7
N6—P2—N8111.86 (10)C27—C28—H28A109.5
N7—P2—N8112.16 (10)C27—C28—H28B109.5
N6—P2—N5111.86 (9)H28A—C28—H28B109.5
N7—P2—N5111.27 (10)C27—C28—H28C109.5
N8—P2—N5105.01 (11)H28A—C28—H28C109.5
N10—P3—N9111.26 (10)H28B—C28—H28C109.5
N10—P3—N11112.62 (10)N8—C29—C30114.6 (2)
N9—P3—N11105.23 (10)N8—C29—H29A108.6
N10—P3—N12104.70 (9)C30—C29—H29A108.6
N9—P3—N12111.25 (10)N8—C29—H29B108.6
N11—P3—N12111.93 (10)C30—C29—H29B108.6
N15—P4—N16105.28 (10)H29A—C29—H29B107.6
N15—P4—N14112.03 (10)C29—C30—H30A109.5
N16—P4—N14111.45 (9)C29—C30—H30B109.5
N15—P4—N13112.03 (10)H30A—C30—H30B109.5
N16—P4—N13111.64 (10)C29—C30—H30C109.5
N14—P4—N13104.58 (10)H30A—C30—H30C109.5
H1W1—O1W—H2W1102 (3)H30B—C30—H30C109.5
H1W2—O2W—H2W2106 (3)N8—C31—C32113.2 (2)
C1—N1—C3114.49 (18)N8—C31—H31A108.9
C1—N1—P1120.29 (16)C32—C31—H31A108.9
C3—N1—P1122.50 (15)N8—C31—H31B108.9
C5—N2—C7114.81 (18)C32—C31—H31B108.9
C5—N2—P1119.96 (16)H31A—C31—H31B107.7
C7—N2—P1122.16 (15)C31—C32—H32A109.5
C9—N3—C11114.46 (17)C31—C32—H32B109.5
C9—N3—P1119.85 (16)H32A—C32—H32B109.5
C11—N3—P1122.54 (15)C31—C32—H32C109.5
C13—N4—C15114.44 (18)H32A—C32—H32C109.5
C13—N4—P1120.56 (16)H32B—C32—H32C109.5
C15—N4—P1122.60 (14)N9—C33—C34114.87 (19)
C17—N5—C19114.44 (18)N9—C33—H33A108.6
C17—N5—P2119.14 (17)C34—C33—H33A108.6
C19—N5—P2122.55 (15)N9—C33—H33B108.6
C23—N6—C21114.06 (17)C34—C33—H33B108.6
C23—N6—P2121.15 (15)H33A—C33—H33B107.5
C21—N6—P2122.78 (14)C33—C34—H34A109.5
C25—N7—C27114.57 (18)C33—C34—H34B109.5
C25—N7—P2122.94 (15)H34A—C34—H34B109.5
C27—N7—P2120.47 (17)C33—C34—H34C109.5
C29—N8—C31114.72 (19)H34A—C34—H34C109.5
C29—N8—P2119.77 (17)H34B—C34—H34C109.5
C31—N8—P2122.72 (16)N9—C35—C36113.56 (19)
C33—N9—C35115.16 (19)N9—C35—H35A108.9
C33—N9—P3121.60 (14)C36—C35—H35A108.9
C35—N9—P3122.39 (16)N9—C35—H35B108.9
C39—N10—C37114.45 (17)C36—C35—H35B108.9
C39—N10—P3120.25 (14)H35A—C35—H35B107.7
C37—N10—P3123.09 (14)C35—C36—H36A109.5
C43—N11—C41114.34 (19)C35—C36—H36B109.5
C43—N11—P3120.30 (15)H36A—C36—H36B109.5
C41—N11—P3122.54 (16)C35—C36—H36C109.5
C45—N12—C47115.46 (16)H36A—C36—H36C109.5
C45—N12—P3122.28 (15)H36B—C36—H36C109.5
C47—N12—P3120.95 (14)N10—C37—C38112.5 (2)
C51—N13—C49115.39 (17)N10—C37—H37A109.1
C51—N13—P4122.46 (15)C38—C37—H37A109.1
C49—N13—P4121.42 (15)N10—C37—H37B109.1
C53—N14—C55114.18 (18)C38—C37—H37B109.1
C53—N14—P4120.70 (16)H37A—C37—H37B107.8
C55—N14—P4122.92 (15)C37—C38—H38A109.5
C57—N15—C59114.9 (2)C37—C38—H38B109.5
C57—N15—P4120.84 (15)H38A—C38—H38B109.5
C59—N15—P4122.31 (16)C37—C38—H38C109.5
C61—N16—C63115.04 (18)H38A—C38—H38C109.5
C61—N16—P4120.58 (16)H38B—C38—H38C109.5
C63—N16—P4121.81 (15)N10—C39—C40113.4 (2)
N1—C1—C2114.81 (19)N10—C39—H39A108.9
N1—C1—H1A108.6C40—C39—H39A108.9
C2—C1—H1A108.6N10—C39—H39B108.9
N1—C1—H1B108.6C40—C39—H39B108.9
C2—C1—H1B108.6H39A—C39—H39B107.7
H1A—C1—H1B107.5C39—C40—H40A109.5
C1—C2—H2A109.5C39—C40—H40B109.5
C1—C2—H2B109.5H40A—C40—H40B109.5
H2A—C2—H2B109.5C39—C40—H40C109.5
C1—C2—H2C109.5H40A—C40—H40C109.5
H2A—C2—H2C109.5H40B—C40—H40C109.5
H2B—C2—H2C109.5N11—C41—C42112.42 (19)
N1—C3—C4113.59 (18)N11—C41—H41A109.1
N1—C3—H3A108.8C42—C41—H41A109.1
C4—C3—H3A108.8N11—C41—H41B109.1
N1—C3—H3B108.8C42—C41—H41B109.1
C4—C3—H3B108.8H41A—C41—H41B107.9
H3A—C3—H3B107.7C41—C42—H42A109.5
C3—C4—H4A109.5C41—C42—H42B109.5
C3—C4—H4B109.5H42A—C42—H42B109.5
H4A—C4—H4B109.5C41—C42—H42C109.5
C3—C4—H4C109.5H42A—C42—H42C109.5
H4A—C4—H4C109.5H42B—C42—H42C109.5
H4B—C4—H4C109.5N11—C43—C44114.7 (2)
N2—C5—C6114.40 (18)N11—C43—H43A108.6
N2—C5—H5A108.7C44—C43—H43A108.6
C6—C5—H5A108.7N11—C43—H43B108.6
N2—C5—H5B108.7C44—C43—H43B108.6
C6—C5—H5B108.7H43A—C43—H43B107.6
H5A—C5—H5B107.6C43—C44—H44A109.5
C5—C6—H6A109.5C43—C44—H44B109.5
C5—C6—H6B109.5H44A—C44—H44B109.5
H6A—C6—H6B109.5C43—C44—H44C109.5
C5—C6—H6C109.5H44A—C44—H44C109.5
H6A—C6—H6C109.5H44B—C44—H44C109.5
H6B—C6—H6C109.5N12—C45—C46113.3 (2)
N2—C7—C8112.86 (18)N12—C45—H45A108.9
N2—C7—H7A109.0C46—C45—H45A108.9
C8—C7—H7A109.0N12—C45—H45B108.9
N2—C7—H7B109.0C46—C45—H45B108.9
C8—C7—H7B109.0H45A—C45—H45B107.7
H7A—C7—H7B107.8C45—C46—H46A109.5
C7—C8—H8A109.5C45—C46—H46B109.5
C7—C8—H8B109.5H46A—C46—H46B109.5
H8A—C8—H8B109.5C45—C46—H46C109.5
C7—C8—H8C109.5H46A—C46—H46C109.5
H8A—C8—H8C109.5H46B—C46—H46C109.5
H8B—C8—H8C109.5N12—C47—C48114.6 (2)
N3—C9—C10114.02 (19)N12—C47—H47A108.6
N3—C9—H9A108.7C48—C47—H47A108.6
C10—C9—H9A108.7N12—C47—H47B108.6
N3—C9—H9B108.7C48—C47—H47B108.6
C10—C9—H9B108.7H47A—C47—H47B107.6
H9A—C9—H9B107.6C47—C48—H48A109.5
C9—C10—H10A109.5C47—C48—H48B109.5
C9—C10—H10B109.5H48A—C48—H48B109.5
H10A—C10—H10B109.5C47—C48—H48C109.5
C9—C10—H10C109.5H48A—C48—H48C109.5
H10A—C10—H10C109.5H48B—C48—H48C109.5
H10B—C10—H10C109.5N13—C49—C50114.7 (2)
N3—C11—C12113.2 (2)N13—C49—H49A108.6
N3—C11—H11A108.9C50—C49—H49A108.6
C12—C11—H11A108.9N13—C49—H49B108.6
N3—C11—H11B108.9C50—C49—H49B108.6
C12—C11—H11B108.9H49A—C49—H49B107.6
H11A—C11—H11B107.8C49—C50—H50A109.5
C11—C12—H12A109.5C49—C50—H50B109.5
C11—C12—H12B109.5H50A—C50—H50B109.5
H12A—C12—H12B109.5C49—C50—H50C109.5
C11—C12—H12C109.5H50A—C50—H50C109.5
H12A—C12—H12C109.5H50B—C50—H50C109.5
H12B—C12—H12C109.5N13—C51—C52113.8 (2)
N4—C13—C14113.86 (19)N13—C51—H51A108.8
N4—C13—H13A108.8C52—C51—H51A108.8
C14—C13—H13A108.8N13—C51—H51B108.8
N4—C13—H13B108.8C52—C51—H51B108.8
C14—C13—H13B108.8H51A—C51—H51B107.7
H13A—C13—H13B107.7C51—C52—H52A109.5
C13—C14—H14A109.5C51—C52—H52B109.5
C13—C14—H14B109.5H52A—C52—H52B109.5
H14A—C14—H14B109.5C51—C52—H52C109.5
C13—C14—H14C109.5H52A—C52—H52C109.5
H14A—C14—H14C109.5H52B—C52—H52C109.5
H14B—C14—H14C109.5N14—C53—C54113.8 (2)
N4—C15—C16112.40 (19)N14—C53—H53A108.8
N4—C15—H15A109.1C54—C53—H53A108.8
C16—C15—H15A109.1N14—C53—H53B108.8
N4—C15—H15B109.1C54—C53—H53B108.8
C16—C15—H15B109.1H53A—C53—H53B107.7
H15A—C15—H15B107.9C53—C54—H54A109.5
C15—C16—H16A109.5C53—C54—H54B109.5
C15—C16—H16B109.5H54A—C54—H54B109.5
H16A—C16—H16B109.5C53—C54—H54C109.5
C15—C16—H16C109.5H54A—C54—H54C109.5
H16A—C16—H16C109.5H54B—C54—H54C109.5
H16B—C16—H16C109.5N14—C55—C56112.8 (2)
N5—C17—C18115.22 (18)N14—C55—H55A109.0
N5—C17—H17A108.5C56—C55—H55A109.0
C18—C17—H17A108.5N14—C55—H55B109.0
N5—C17—H17B108.5C56—C55—H55B109.0
C18—C17—H17B108.5H55A—C55—H55B107.8
H17A—C17—H17B107.5C55—C56—H56A109.5
C17—C18—H18A109.5C55—C56—H56B109.5
C17—C18—H18B109.5H56A—C56—H56B109.5
H18A—C18—H18B109.5C55—C56—H56C109.5
C17—C18—H18C109.5H56A—C56—H56C109.5
H18A—C18—H18C109.5H56B—C56—H56C109.5
H18B—C18—H18C109.5N15—C57—C58113.79 (18)
N5—C19—C20113.4 (2)N15—C57—H57A108.8
N5—C19—H19A108.9C58—C57—H57A108.8
C20—C19—H19A108.9N15—C57—H57B108.8
N5—C19—H19B108.9C58—C57—H57B108.8
C20—C19—H19B108.9H57A—C57—H57B107.7
H19A—C19—H19B107.7C57—C58—H58A109.5
C19—C20—H20A109.5C57—C58—H58B109.5
C19—C20—H20B109.5H58A—C58—H58B109.5
H20A—C20—H20B109.5C57—C58—H58C109.5
C19—C20—H20C109.5H58A—C58—H58C109.5
H20A—C20—H20C109.5H58B—C58—H58C109.5
H20B—C20—H20C109.5N15—C59—C60113.55 (19)
N6—C21—C22112.84 (19)N15—C59—H59A108.9
N6—C21—H21A109.0C60—C59—H59A108.9
C22—C21—H21A109.0N15—C59—H59B108.9
N6—C21—H21B109.0C60—C59—H59B108.9
C22—C21—H21B109.0H59A—C59—H59B107.7
H21A—C21—H21B107.8C59—C60—H60A109.5
C21—C22—H22A109.5C59—C60—H60B109.5
C21—C22—H22B109.5H60A—C60—H60B109.5
H22A—C22—H22B109.5C59—C60—H60C109.5
C21—C22—H22C109.5H60A—C60—H60C109.5
H22A—C22—H22C109.5H60B—C60—H60C109.5
H22B—C22—H22C109.5N16—C61—C62114.46 (19)
N6—C23—C24114.01 (18)N16—C61—H61A108.6
N6—C23—H23A108.8C62—C61—H61A108.6
C24—C23—H23A108.8N16—C61—H61B108.6
N6—C23—H23B108.8C62—C61—H61B108.6
C24—C23—H23B108.8H61A—C61—H61B107.6
H23A—C23—H23B107.6C61—C62—H62A109.5
C23—C24—H24A109.5C61—C62—H62B109.5
C23—C24—H24B109.5H62A—C62—H62B109.5
H24A—C24—H24B109.5C61—C62—H62C109.5
C23—C24—H24C109.5H62A—C62—H62C109.5
H24A—C24—H24C109.5H62B—C62—H62C109.5
H24B—C24—H24C109.5N16—C63—C64112.13 (19)
N7—C25—C26113.18 (19)N16—C63—H63A109.2
N7—C25—H25A108.9C64—C63—H63A109.2
C26—C25—H25A108.9N16—C63—H63B109.2
N7—C25—H25B108.9C64—C63—H63B109.2
C26—C25—H25B108.9H63A—C63—H63B107.9
H25A—C25—H25B107.8C63—C64—H64A109.5
C25—C26—H26A109.5C63—C64—H64B109.5
C25—C26—H26B109.5H64A—C64—H64B109.5
H26A—C26—H26B109.5C63—C64—H64C109.5
C25—C26—H26C109.5H64A—C64—H64C109.5
H26A—C26—H26C109.5H64B—C64—H64C109.5
N4—P1—N1—C133.09 (19)N13—P4—N14—C53152.67 (17)
N2—P1—N1—C1154.71 (16)N15—P4—N14—C55166.72 (16)
N3—P1—N1—C184.37 (18)N16—P4—N14—C5575.61 (19)
N4—P1—N1—C3166.65 (16)N13—P4—N14—C5545.15 (19)
N2—P1—N1—C345.03 (19)N16—P4—N15—C57148.26 (15)
N3—P1—N1—C375.89 (19)N14—P4—N15—C5790.45 (17)
N4—P1—N2—C582.73 (17)N13—P4—N15—C5726.73 (19)
N1—P1—N2—C5155.46 (15)N16—P4—N15—C5948.45 (19)
N3—P1—N2—C534.31 (18)N14—P4—N15—C5972.84 (19)
N4—P1—N2—C776.40 (19)N13—P4—N15—C59169.98 (16)
N1—P1—N2—C745.40 (19)N15—P4—N16—C61154.60 (17)
N3—P1—N2—C7166.56 (17)N14—P4—N16—C6132.9 (2)
N4—P1—N3—C9156.89 (16)N13—P4—N16—C6183.62 (18)
N1—P1—N3—C935.17 (19)N15—P4—N16—C6344.47 (19)
N2—P1—N3—C981.95 (18)N14—P4—N16—C63166.14 (17)
N4—P1—N3—C1144.29 (19)N13—P4—N16—C6377.3 (2)
N1—P1—N3—C11166.01 (17)C3—N1—C1—C263.9 (3)
N2—P1—N3—C1176.9 (2)P1—N1—C1—C297.9 (2)
N1—P1—N4—C1382.79 (18)C1—N1—C3—C467.7 (3)
N2—P1—N4—C1334.84 (19)P1—N1—C3—C4130.97 (19)
N3—P1—N4—C13155.73 (16)C7—N2—C5—C668.2 (3)
N1—P1—N4—C1578.64 (19)P1—N2—C5—C692.4 (2)
N2—P1—N4—C15163.74 (17)C5—N2—C7—C865.3 (3)
N3—P1—N4—C1542.84 (19)P1—N2—C7—C8134.58 (19)
N6—P2—N5—C1782.15 (17)C11—N3—C9—C1073.0 (3)
N7—P2—N5—C1734.75 (19)P1—N3—C9—C1087.4 (2)
N8—P2—N5—C17156.32 (16)C9—N3—C11—C1268.3 (3)
N6—P2—N5—C1974.5 (2)P1—N3—C11—C12131.86 (19)
N7—P2—N5—C19168.62 (18)C15—N4—C13—C1470.3 (3)
N8—P2—N5—C1947.0 (2)P1—N4—C13—C1492.6 (2)
N7—P2—N6—C23153.11 (16)C13—N4—C15—C1664.5 (3)
N8—P2—N6—C2385.10 (17)P1—N4—C15—C16133.02 (18)
N5—P2—N6—C2332.40 (19)C19—N5—C17—C1877.0 (3)
N7—P2—N6—C2143.95 (18)P2—N5—C17—C1881.4 (2)
N8—P2—N6—C2177.84 (19)C17—N5—C19—C2072.7 (3)
N5—P2—N6—C21164.66 (16)P2—N5—C19—C20129.67 (19)
N6—P2—N7—C2542.06 (19)C23—N6—C21—C2263.3 (2)
N8—P2—N7—C25163.66 (17)P2—N6—C21—C22132.64 (18)
N5—P2—N7—C2579.04 (19)C21—N6—C23—C2470.3 (3)
N6—P2—N7—C27155.01 (17)P2—N6—C23—C2494.0 (2)
N8—P2—N7—C2733.4 (2)C27—N7—C25—C2664.5 (3)
N5—P2—N7—C2783.90 (19)P2—N7—C25—C26131.64 (18)
N6—P2—N8—C2934.6 (2)C25—N7—C27—C2864.6 (3)
N7—P2—N8—C2982.85 (18)P2—N7—C27—C2899.7 (3)
N5—P2—N8—C29156.17 (16)C31—N8—C29—C3070.6 (3)
N6—P2—N8—C31165.31 (17)P2—N8—C29—C3090.9 (2)
N7—P2—N8—C3177.2 (2)C29—N8—C31—C3267.7 (3)
N5—P2—N8—C3143.8 (2)P2—N8—C31—C32131.4 (2)
N10—P3—N9—C3393.99 (18)C35—N9—C33—C3466.4 (3)
N11—P3—N9—C33143.75 (17)P3—N9—C33—C34103.3 (2)
N12—P3—N9—C3322.3 (2)C33—N9—C35—C3657.5 (3)
N10—P3—N9—C3574.90 (19)P3—N9—C35—C36132.9 (2)
N11—P3—N9—C3547.35 (19)C39—N10—C37—C3863.8 (2)
N12—P3—N9—C35168.76 (16)P3—N10—C37—C38133.02 (17)
N9—P3—N10—C3927.85 (19)C37—N10—C39—C4073.2 (2)
N11—P3—N10—C3990.02 (18)P3—N10—C39—C4090.5 (2)
N12—P3—N10—C39148.14 (17)C43—N11—C41—C4268.9 (3)
N9—P3—N10—C37169.95 (16)P3—N11—C41—C42130.1 (2)
N11—P3—N10—C3772.17 (18)C41—N11—C43—C4473.9 (3)
N12—P3—N10—C3749.67 (19)P3—N11—C43—C4487.5 (2)
N10—P3—N11—C4336.24 (19)C47—N12—C45—C4663.3 (3)
N9—P3—N11—C43157.62 (16)P3—N12—C45—C46129.63 (18)
N12—P3—N11—C4381.41 (17)C45—N12—C47—C4859.6 (3)
N10—P3—N11—C41163.84 (16)P3—N12—C47—C48107.6 (2)
N9—P3—N11—C4142.47 (19)C51—N13—C49—C5054.9 (3)
N12—P3—N11—C4178.50 (19)P4—N13—C49—C50115.5 (2)
N10—P3—N12—C4541.0 (2)C49—N13—C51—C5257.2 (3)
N9—P3—N12—C4579.3 (2)P4—N13—C51—C52132.47 (19)
N11—P3—N12—C45163.33 (18)C55—N14—C53—C5470.2 (3)
N10—P3—N12—C47152.64 (17)P4—N14—C53—C5493.4 (2)
N9—P3—N12—C4787.07 (19)C53—N14—C55—C5666.7 (2)
N11—P3—N12—C4730.3 (2)P4—N14—C55—C56130.06 (18)
N15—P4—N13—C5177.2 (2)C59—N15—C57—C5877.0 (3)
N16—P4—N13—C51164.97 (18)P4—N15—C57—C5887.4 (2)
N14—P4—N13—C5144.3 (2)C57—N15—C59—C6067.5 (3)
N15—P4—N13—C4992.53 (19)P4—N15—C59—C60128.2 (2)
N16—P4—N13—C4925.3 (2)C63—N16—C61—C6272.8 (3)
N14—P4—N13—C49145.91 (18)P4—N16—C61—C6289.3 (2)
N15—P4—N14—C5331.11 (19)C61—N16—C63—C6467.7 (3)
N16—P4—N14—C5386.57 (19)P4—N16—C63—C64130.4 (2)
Hydrogen-bond geometry (Å, º) top
D—H···AD—HH···AD···AD—H···A
O1W—H2W1···Br10.77 (2)2.66 (2)3.425 (2)174 (3)
O1W—H1W1···Br1i0.79 (2)2.82 (2)3.611 (3)176 (3)
O2W—H1W2···Br20.77 (2)2.71 (2)3.467 (3)169 (3)
O2W—H2W2···Br2ii0.79 (2)2.68 (2)3.471 (2)177 (3)
Symmetry codes: (i) x+1, y+2, z; (ii) x+1, y+1, z+1.
 

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