Tetrakis­(diethyl­amino)­phospho­nium bromide hemihydrate

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.

Computing details

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

Crystal data

C16H40N4P^+·Br^−·0.5H2O	F(000) = 1752
Mr = 408.4	Dx = 1.229 Mg m^−3
Triclinic, P1	Melting point: 412 K
a = 14.2475 (2) Å	Mo Kα radiation, λ = 0.71073 Å
b = 14.9756 (3) Å	Cell parameters from 43363 reflections
c = 20.7125 (5) Å	θ = 1.0–27.5°
α = 92.144 (2)°	µ = 1.94 mm^−1
β = 91.799 (2)°	T = 130 K
γ = 90.246 (2)°	Fragment, colorless
V = 4414.0 (3) Å^3	0.27 × 0.25 × 0.22 mm
Z = 8

Data collection

Nonius KappaCCD (with Oxford Cryostream) diffractometer	20107 independent reflections
Radiation source: sealed tube	11547 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.064
ω scans with κ offsets	θmax = 27.5°
Absorption correction: multi-scan (SORTAV; Blessing, 1995)	h = −18→18
Tmin = 0.600, Tmax = 0.652	k = −19→19
43363 measured reflections	l = −26→26

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.036	H atoms treated by a mixture of independent and constrained refinement
wR(F^2) = 0.072	w = 1/[σ^2(Fo^2) + (0.0282P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 0.89	(Δ/σ)max = 0.005
20107 reflections	Δρmax = 0.66 e Å^−3
860 parameters	Δρmin = −0.45 e Å^−3
4 restraints	Extinction correction: SHELXL97 (Sheldrick, 1997), Fc^*=kFc[1+0.001xFc^2λ^3/sin(2θ)]^-1/4
Primary atom site location: structure-invariant direct methods	Extinction coefficient: 0.00103 (8)

Special details

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 (Ų)

	x	y	z	Uiso*/Ueq
Br1	0.441885 (16)	0.960335 (17)	0.121215 (14)	0.03876 (8)
Br2	0.416410 (16)	0.552451 (16)	0.612750 (15)	0.03875 (8)
Br3	0.041737 (16)	0.931885 (17)	0.678825 (14)	0.03768 (8)
Br4	0.055817 (16)	0.562574 (16)	0.163999 (14)	0.03490 (7)
P1	0.71720 (4)	0.73037 (4)	0.74630 (3)	0.02191 (14)
P2	0.74148 (4)	0.75833 (4)	0.24715 (3)	0.02454 (15)
P3	0.21208 (4)	0.73480 (4)	0.95525 (3)	0.02184 (14)
P4	0.22316 (4)	0.76662 (4)	0.46884 (3)	0.02345 (15)
O1W	0.64136 (14)	0.96203 (14)	0.03319 (14)	0.0462 (5)
H1W1	0.6258 (18)	0.9800 (18)	−0.0008 (10)	0.040 (10)*
H2W1	0.5949 (16)	0.965 (2)	0.0513 (15)	0.073 (12)*
O2W	0.36975 (15)	0.44743 (15)	0.46308 (14)	0.0485 (5)
H1W2	0.378 (2)	0.465 (2)	0.4982 (10)	0.059 (12)*
H2W2	0.4194 (14)	0.448 (2)	0.4473 (15)	0.061 (11)*
N1	0.75389 (12)	0.79770 (12)	0.80588 (9)	0.0246 (5)
N2	0.67685 (11)	0.64224 (12)	0.78105 (10)	0.0240 (5)
N3	0.63572 (11)	0.77663 (12)	0.70119 (9)	0.0237 (5)
N4	0.80090 (11)	0.70463 (12)	0.69685 (9)	0.0235 (4)
N5	0.70919 (12)	0.84118 (12)	0.29533 (10)	0.0265 (5)
N6	0.82603 (11)	0.78767 (11)	0.20071 (9)	0.0227 (4)
N7	0.65565 (12)	0.72608 (12)	0.19724 (10)	0.0267 (5)
N8	0.77422 (13)	0.67922 (12)	0.29534 (10)	0.0293 (5)
N9	0.18732 (11)	0.79858 (11)	0.89479 (10)	0.0236 (5)
N10	0.15641 (11)	0.63922 (11)	0.94707 (9)	0.0213 (4)
N11	0.18254 (12)	0.79277 (12)	1.01980 (10)	0.0254 (5)
N12	0.32350 (11)	0.70817 (12)	0.95775 (9)	0.0236 (5)
N13	0.32796 (12)	0.77972 (12)	0.43991 (10)	0.0257 (5)
N14	0.16977 (12)	0.86095 (12)	0.45595 (9)	0.0233 (4)
N15	0.22793 (12)	0.74419 (12)	0.54517 (9)	0.0250 (5)
N16	0.16729 (12)	0.68243 (12)	0.43298 (10)	0.0262 (5)
C1	0.82807 (16)	0.86499 (15)	0.79559 (13)	0.0322 (6)
H1A	0.8652	0.8444	0.7584	0.039*
H1B	0.8709	0.8682	0.8342	0.039*
C2	0.79219 (18)	0.95828 (16)	0.78315 (14)	0.0471 (8)
H2A	0.7481	0.9559	0.7458	0.071*
H2B	0.8452	0.9974	0.7743	0.071*
H2C	0.7601	0.9818	0.8213	0.071*
C3	0.69815 (15)	0.81560 (16)	0.86430 (12)	0.0299 (6)
H3A	0.6443	0.7735	0.8635	0.036*
H3B	0.6726	0.8769	0.8629	0.036*
C4	0.75433 (17)	0.80654 (18)	0.92747 (13)	0.0398 (7)
H4A	0.7738	0.7443	0.9316	0.060*
H4B	0.7153	0.8244	0.9638	0.060*
H4C	0.8100	0.8452	0.9276	0.060*
C5	0.60547 (15)	0.58446 (14)	0.74692 (12)	0.0284 (6)
H5A	0.5673	0.6214	0.7175	0.034*
H5B	0.5630	0.5607	0.7791	0.034*
C6	0.64532 (18)	0.50710 (16)	0.70814 (14)	0.0426 (7)
H6A	0.6887	0.5297	0.6767	0.064*
H6B	0.5941	0.4740	0.6853	0.064*
H6C	0.6791	0.4673	0.7372	0.064*
C7	0.72899 (15)	0.59970 (16)	0.83485 (12)	0.0316 (6)
H7A	0.7799	0.6405	0.8513	0.038*
H7B	0.7584	0.5441	0.8181	0.038*
C8	0.66681 (18)	0.57754 (19)	0.89019 (14)	0.0466 (7)
H8A	0.6348	0.6317	0.9055	0.070*
H8B	0.7054	0.5539	0.9256	0.070*
H8C	0.6200	0.5326	0.8752	0.070*
C9	0.56698 (15)	0.83806 (15)	0.73130 (13)	0.0311 (6)
H9A	0.5465	0.8819	0.6992	0.037*
H9B	0.5986	0.8716	0.7680	0.037*
C10	0.48023 (15)	0.79119 (17)	0.75581 (14)	0.0418 (7)
H10A	0.4484	0.7577	0.7199	0.063*
H10B	0.4373	0.8359	0.7739	0.063*
H10C	0.4994	0.7500	0.7894	0.063*
C11	0.60572 (16)	0.73888 (15)	0.63643 (12)	0.0300 (6)
H11A	0.5428	0.7112	0.6393	0.036*
H11B	0.6500	0.6912	0.6234	0.036*
C12	0.60172 (18)	0.80799 (17)	0.58492 (13)	0.0432 (7)
H12A	0.5506	0.8499	0.5937	0.065*
H12B	0.5905	0.7781	0.5425	0.065*
H12C	0.6615	0.8407	0.5853	0.065*
C13	0.86781 (15)	0.63232 (15)	0.71162 (13)	0.0312 (6)
H13A	0.8853	0.6017	0.6706	0.037*
H13B	0.8360	0.5880	0.7378	0.037*
C14	0.95656 (16)	0.66442 (18)	0.74779 (14)	0.0447 (8)
H14A	0.9881	0.7092	0.7226	0.067*
H14B	0.9986	0.6137	0.7542	0.067*
H14C	0.9404	0.6911	0.7899	0.067*
C15	0.83246 (16)	0.76597 (15)	0.64702 (12)	0.0302 (6)
H15A	0.8941	0.7921	0.6610	0.036*
H15B	0.7870	0.8155	0.6433	0.036*
C16	0.84128 (18)	0.71901 (18)	0.58125 (13)	0.0424 (7)
H16A	0.8963	0.6800	0.5820	0.064*
H16B	0.8485	0.7636	0.5483	0.064*
H16C	0.7847	0.6831	0.5711	0.064*
C17	0.64252 (16)	0.90836 (15)	0.27030 (13)	0.0328 (6)
H17A	0.6106	0.9371	0.3074	0.039*
H17B	0.5939	0.8769	0.2427	0.039*
C18	0.68609 (16)	0.98087 (15)	0.23148 (13)	0.0346 (6)
H18A	0.7308	1.0158	0.2592	0.052*
H18B	0.6367	1.0202	0.2152	0.052*
H18C	0.7189	0.9534	0.1950	0.052*
C19	0.76672 (17)	0.87253 (16)	0.35283 (12)	0.0344 (6)
H19A	0.7941	0.9316	0.3443	0.041*
H19B	0.8192	0.8304	0.3595	0.041*
C20	0.71090 (19)	0.88039 (17)	0.41479 (14)	0.0453 (7)
H20A	0.6593	0.9226	0.4088	0.068*
H20B	0.7524	0.9019	0.4507	0.068*
H20C	0.6853	0.8217	0.4244	0.068*
C21	0.85254 (15)	0.73387 (15)	0.14237 (12)	0.0281 (6)
H21A	0.8039	0.6875	0.1326	0.034*
H21B	0.9125	0.7031	0.1517	0.034*
C22	0.86326 (16)	0.78994 (17)	0.08349 (12)	0.0361 (6)
H22A	0.8090	0.8294	0.0790	0.054*
H22B	0.8670	0.7506	0.0448	0.054*
H22C	0.9207	0.8260	0.0887	0.054*
C23	0.89752 (14)	0.85493 (14)	0.22334 (12)	0.0266 (6)
H23A	0.8694	0.8958	0.2560	0.032*
H23B	0.9148	0.8910	0.1864	0.032*
C24	0.98553 (15)	0.81531 (17)	0.25249 (14)	0.0422 (7)
H24A	0.9698	0.7825	0.2908	0.063*
H24B	1.0302	0.8633	0.2649	0.063*
H24C	1.0138	0.7744	0.2207	0.063*
C25	0.62954 (15)	0.77433 (16)	0.13856 (12)	0.0301 (6)
H25A	0.6784	0.8197	0.1313	0.036*
H25B	0.5697	0.8061	0.1456	0.036*
C26	0.61833 (17)	0.71331 (17)	0.07840 (13)	0.0395 (7)
H26A	0.6771	0.6812	0.0713	0.059*
H26B	0.6030	0.7492	0.0409	0.059*
H26C	0.5676	0.6702	0.0843	0.059*
C27	0.58354 (16)	0.66201 (17)	0.21756 (14)	0.0397 (7)
H27A	0.6097	0.6283	0.2541	0.048*
H27B	0.5694	0.6186	0.1813	0.048*
C28	0.49270 (18)	0.7059 (2)	0.23785 (17)	0.0658 (10)
H28A	0.5060	0.7494	0.2735	0.099*
H28B	0.4493	0.6601	0.2520	0.099*
H28C	0.4642	0.7364	0.2011	0.099*
C29	0.84066 (17)	0.60997 (16)	0.27267 (14)	0.0386 (7)
H29A	0.8800	0.5915	0.3100	0.046*
H29B	0.8828	0.6367	0.2415	0.046*
C30	0.7945 (2)	0.52746 (16)	0.24082 (15)	0.0478 (8)
H30A	0.7555	0.4983	0.2721	0.072*
H30B	0.8431	0.4860	0.2261	0.072*
H30C	0.7552	0.5448	0.2037	0.072*
C31	0.72009 (18)	0.65512 (17)	0.35221 (13)	0.0408 (7)
H31A	0.6884	0.5969	0.3428	0.049*
H31B	0.6708	0.7005	0.3595	0.049*
C32	0.7808 (2)	0.64880 (19)	0.41389 (14)	0.0553 (8)
H32A	0.8275	0.6016	0.4080	0.083*
H32B	0.7410	0.6348	0.4499	0.083*
H32C	0.8129	0.7060	0.4234	0.083*
C33	0.24661 (15)	0.80021 (16)	0.83800 (12)	0.0289 (6)
H33A	0.3087	0.7750	0.8497	0.035*
H33B	0.2566	0.8632	0.8269	0.035*
C34	0.20733 (17)	0.74938 (19)	0.77877 (13)	0.0458 (7)
H34A	0.1891	0.6890	0.7904	0.069*
H34B	0.2552	0.7455	0.7459	0.069*
H34C	0.1522	0.7806	0.7616	0.069*
C35	0.09616 (15)	0.84564 (15)	0.88796 (13)	0.0312 (6)
H35A	0.0623	0.8416	0.9288	0.037*
H35B	0.0575	0.8148	0.8533	0.037*
C36	0.10628 (17)	0.94318 (15)	0.87225 (14)	0.0412 (7)
H36A	0.1526	0.9720	0.9022	0.062*
H36B	0.0456	0.9730	0.8765	0.062*
H36C	0.1272	0.9476	0.8279	0.062*
C37	0.17664 (15)	0.56269 (14)	0.98884 (12)	0.0245 (5)
H37A	0.1254	0.5569	1.0196	0.029*
H37B	0.2356	0.5749	1.0143	0.029*
C38	0.18627 (16)	0.47475 (14)	0.95001 (13)	0.0305 (6)
H38A	0.1274	0.4613	0.9258	0.046*
H38B	0.2002	0.4266	0.9795	0.046*
H38C	0.2374	0.4799	0.9198	0.046*
C39	0.06536 (13)	0.63277 (15)	0.91056 (12)	0.0263 (6)
H39A	0.0595	0.5726	0.8894	0.032*
H39B	0.0648	0.6770	0.8762	0.032*
C40	−0.01919 (15)	0.64909 (18)	0.95276 (14)	0.0426 (7)
H40A	−0.0165	0.6088	0.9890	0.064*
H40B	−0.0771	0.6378	0.9269	0.064*
H40C	−0.0183	0.7112	0.9695	0.064*
C41	0.20365 (15)	0.88949 (15)	1.02915 (13)	0.0342 (6)
H41A	0.2276	0.9123	0.9885	0.041*
H41B	0.2537	0.8980	1.0631	0.041*
C42	0.11735 (17)	0.94371 (17)	1.04860 (15)	0.0483 (8)
H42A	0.0654	0.9308	1.0174	0.072*
H42B	0.1326	1.0076	1.0490	0.072*
H42C	0.0988	0.9274	1.0918	0.072*
C43	0.16194 (16)	0.74718 (16)	1.08003 (12)	0.0318 (6)
H43A	0.1319	0.6888	1.0684	0.038*
H43B	0.1161	0.7835	1.1044	0.038*
C44	0.24732 (18)	0.73134 (19)	1.12402 (14)	0.0510 (8)
H44A	0.2912	0.6916	1.1016	0.076*
H44B	0.2273	0.7037	1.1635	0.076*
H44C	0.2785	0.7885	1.1353	0.076*
C45	0.36211 (15)	0.63720 (15)	0.91508 (13)	0.0294 (6)
H45A	0.4012	0.6651	0.8826	0.035*
H45B	0.3095	0.6054	0.8917	0.035*
C46	0.42124 (16)	0.56969 (16)	0.95124 (14)	0.0411 (7)
H46A	0.4770	0.5996	0.9709	0.062*
H46B	0.4406	0.5219	0.9210	0.062*
H46C	0.3841	0.5442	0.9851	0.062*
C47	0.39405 (14)	0.76687 (15)	0.99242 (12)	0.0284 (6)
H47A	0.4335	0.7299	1.0211	0.034*
H47B	0.3607	0.8108	1.0202	0.034*
C48	0.45732 (16)	0.81688 (17)	0.94913 (14)	0.0402 (7)
H48A	0.4939	0.7741	0.9234	0.060*
H48B	0.5000	0.8556	0.9756	0.060*
H48C	0.4191	0.8534	0.9202	0.060*
C49	0.37856 (15)	0.70406 (16)	0.40904 (13)	0.0322 (6)
H49A	0.3939	0.7200	0.3646	0.039*
H49B	0.3360	0.6515	0.4056	0.039*
C50	0.46832 (15)	0.67780 (16)	0.44442 (14)	0.0379 (7)
H50A	0.5137	0.7272	0.4442	0.057*
H50B	0.4947	0.6247	0.4228	0.057*
H50C	0.4546	0.6645	0.4891	0.057*
C51	0.38350 (15)	0.86171 (16)	0.45209 (13)	0.0347 (7)
H51A	0.4349	0.8496	0.4838	0.042*
H51B	0.3429	0.9081	0.4717	0.042*
C52	0.42580 (18)	0.89807 (18)	0.39158 (16)	0.0527 (8)
H52A	0.4721	0.8557	0.3748	0.079*
H52B	0.4566	0.9556	0.4024	0.079*
H52C	0.3759	0.9063	0.3587	0.079*
C53	0.09380 (15)	0.89241 (15)	0.49813 (13)	0.0342 (6)
H53A	0.0970	0.9584	0.5027	0.041*
H53B	0.1045	0.8684	0.5416	0.041*
C54	−0.00418 (16)	0.86509 (18)	0.47309 (15)	0.0484 (8)
H54A	−0.0173	0.8922	0.4315	0.073*
H54B	−0.0506	0.8856	0.5042	0.073*
H54C	−0.0077	0.7999	0.4675	0.073*
C55	0.17315 (16)	0.90638 (15)	0.39383 (12)	0.0312 (6)
H55A	0.1109	0.9011	0.3714	0.037*
H55B	0.2195	0.8759	0.3661	0.037*
C56	0.19963 (18)	1.00469 (15)	0.40243 (14)	0.0399 (7)
H56A	0.1496	1.0369	0.4247	0.060*
H56B	0.2079	1.0298	0.3600	0.060*
H56C	0.2584	1.0107	0.4281	0.060*
C57	0.30818 (15)	0.77441 (15)	0.58728 (12)	0.0303 (6)
H57A	0.3657	0.7730	0.5617	0.036*
H57B	0.3169	0.7319	0.6224	0.036*
C58	0.29668 (17)	0.86813 (16)	0.61713 (13)	0.0399 (7)
H58A	0.2913	0.9112	0.5827	0.060*
H58B	0.3515	0.8833	0.6453	0.060*
H58C	0.2399	0.8702	0.6426	0.060*
C59	0.14419 (15)	0.71520 (15)	0.57984 (13)	0.0318 (6)
H59A	0.0913	0.7055	0.5482	0.038*
H59B	0.1262	0.7637	0.6107	0.038*
C60	0.15956 (18)	0.62981 (16)	0.61662 (14)	0.0417 (7)
H60A	0.1785	0.5816	0.5866	0.063*
H60B	0.1011	0.6130	0.6368	0.063*
H60C	0.2089	0.6400	0.6501	0.063*
C61	0.11546 (16)	0.69341 (16)	0.37080 (13)	0.0366 (7)
H61A	0.0906	0.7550	0.3700	0.044*
H61B	0.0611	0.6519	0.3685	0.044*
C62	0.1733 (2)	0.6766 (2)	0.31164 (15)	0.0655 (10)
H62A	0.2212	0.7235	0.3096	0.098*
H62B	0.1324	0.6770	0.2728	0.098*
H62C	0.2040	0.6183	0.3142	0.098*
C63	0.18881 (16)	0.58791 (15)	0.44878 (14)	0.0343 (6)
H63A	0.2317	0.5876	0.4873	0.041*
H63B	0.2214	0.5586	0.4122	0.041*
C64	0.10029 (18)	0.53465 (17)	0.46200 (15)	0.0487 (8)
H64A	0.0640	0.5670	0.4947	0.073*
H64B	0.1179	0.4760	0.4778	0.073*
H64C	0.0621	0.5267	0.4220	0.073*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Br1	0.03329 (14)	0.03597 (15)	0.0469 (2)	0.00376 (11)	0.00133 (13)	−0.00100 (13)
Br2	0.03246 (13)	0.02973 (14)	0.0539 (2)	−0.00266 (11)	0.00206 (13)	−0.00097 (13)
Br3	0.03336 (13)	0.03692 (15)	0.04231 (19)	−0.00509 (11)	0.00429 (12)	−0.00632 (13)
Br4	0.03144 (13)	0.02819 (14)	0.04470 (19)	−0.00239 (11)	−0.00227 (12)	−0.00003 (12)
P1	0.0211 (3)	0.0226 (3)	0.0220 (4)	0.0002 (2)	−0.0005 (3)	0.0022 (3)
P2	0.0300 (3)	0.0210 (3)	0.0227 (4)	−0.0024 (3)	0.0018 (3)	0.0013 (3)
P3	0.0196 (3)	0.0215 (3)	0.0245 (4)	−0.0015 (2)	0.0006 (3)	0.0018 (3)
P4	0.0230 (3)	0.0230 (3)	0.0242 (4)	0.0014 (3)	−0.0001 (3)	−0.0001 (3)
O1W	0.0343 (12)	0.0511 (13)	0.0536 (18)	0.0018 (10)	0.0046 (12)	0.0058 (13)
O2W	0.0363 (12)	0.0594 (14)	0.0491 (17)	−0.0009 (10)	−0.0015 (12)	−0.0065 (13)
N1	0.0261 (10)	0.0276 (11)	0.0200 (12)	0.0003 (8)	0.0005 (9)	−0.0020 (9)
N2	0.0213 (9)	0.0245 (10)	0.0265 (13)	0.0007 (8)	0.0002 (9)	0.0052 (9)
N3	0.0243 (10)	0.0248 (10)	0.0218 (12)	0.0006 (8)	−0.0048 (9)	0.0019 (9)
N4	0.0240 (9)	0.0241 (10)	0.0225 (12)	−0.0002 (8)	−0.0002 (9)	0.0026 (9)
N5	0.0329 (10)	0.0232 (10)	0.0234 (13)	−0.0045 (9)	0.0062 (9)	−0.0020 (9)
N6	0.0250 (9)	0.0200 (10)	0.0230 (13)	−0.0013 (8)	0.0013 (9)	0.0004 (9)
N7	0.0292 (10)	0.0258 (11)	0.0252 (13)	−0.0062 (9)	0.0009 (9)	0.0025 (9)
N8	0.0424 (11)	0.0224 (11)	0.0233 (13)	−0.0016 (9)	0.0004 (10)	0.0047 (9)
N9	0.0222 (9)	0.0225 (10)	0.0265 (13)	0.0023 (8)	0.0026 (9)	0.0070 (9)
N10	0.0190 (9)	0.0193 (10)	0.0257 (13)	−0.0004 (8)	−0.0003 (8)	0.0025 (9)
N11	0.0256 (10)	0.0215 (10)	0.0288 (13)	−0.0053 (8)	0.0034 (9)	−0.0027 (9)
N12	0.0194 (9)	0.0245 (10)	0.0268 (13)	−0.0017 (8)	0.0007 (9)	−0.0005 (9)
N13	0.0246 (10)	0.0257 (11)	0.0268 (13)	0.0011 (8)	0.0018 (9)	0.0006 (9)
N14	0.0258 (10)	0.0236 (10)	0.0208 (12)	0.0026 (8)	0.0048 (9)	0.0008 (9)
N15	0.0280 (10)	0.0271 (11)	0.0201 (12)	0.0002 (8)	0.0028 (9)	0.0037 (9)
N16	0.0263 (10)	0.0203 (10)	0.0315 (14)	0.0038 (8)	−0.0029 (9)	−0.0015 (9)
C1	0.0328 (13)	0.0367 (15)	0.0263 (16)	−0.0087 (11)	0.0005 (12)	−0.0058 (12)
C2	0.0619 (18)	0.0351 (16)	0.045 (2)	−0.0085 (14)	0.0139 (15)	0.0022 (14)
C3	0.0341 (13)	0.0321 (14)	0.0232 (16)	0.0034 (11)	0.0018 (12)	−0.0026 (12)
C4	0.0445 (15)	0.0502 (17)	0.0241 (17)	0.0035 (13)	−0.0011 (13)	−0.0039 (13)
C5	0.0298 (12)	0.0239 (13)	0.0318 (17)	−0.0027 (10)	−0.0008 (12)	0.0064 (12)
C6	0.0491 (16)	0.0292 (15)	0.049 (2)	0.0034 (12)	−0.0038 (14)	−0.0036 (14)
C7	0.0286 (12)	0.0358 (15)	0.0308 (17)	0.0044 (11)	−0.0015 (12)	0.0100 (12)
C8	0.0473 (16)	0.0576 (19)	0.0364 (19)	−0.0004 (14)	−0.0005 (14)	0.0206 (15)
C9	0.0326 (13)	0.0275 (13)	0.0333 (17)	0.0106 (11)	−0.0014 (12)	0.0040 (12)
C10	0.0286 (13)	0.0477 (17)	0.050 (2)	0.0105 (12)	0.0069 (13)	0.0048 (15)
C11	0.0274 (12)	0.0321 (14)	0.0303 (17)	−0.0055 (11)	−0.0052 (11)	0.0029 (12)
C12	0.0513 (16)	0.0486 (17)	0.0293 (18)	−0.0121 (14)	−0.0125 (14)	0.0097 (14)
C13	0.0296 (12)	0.0301 (14)	0.0346 (17)	0.0040 (11)	0.0071 (12)	0.0022 (12)
C14	0.0268 (13)	0.0512 (18)	0.057 (2)	0.0041 (12)	−0.0046 (13)	0.0112 (15)
C15	0.0305 (13)	0.0307 (14)	0.0300 (17)	−0.0049 (11)	0.0033 (12)	0.0072 (12)
C16	0.0498 (16)	0.0486 (17)	0.0288 (18)	−0.0107 (13)	0.0090 (14)	−0.0032 (14)
C17	0.0335 (13)	0.0270 (14)	0.0383 (18)	0.0019 (11)	0.0096 (12)	−0.0004 (12)
C18	0.0384 (14)	0.0251 (14)	0.0405 (19)	0.0024 (11)	0.0053 (13)	0.0033 (12)
C19	0.0462 (15)	0.0283 (14)	0.0285 (17)	−0.0061 (12)	0.0036 (13)	−0.0041 (12)
C20	0.0646 (18)	0.0372 (16)	0.0341 (19)	−0.0102 (14)	0.0117 (15)	−0.0074 (14)
C21	0.0273 (12)	0.0302 (14)	0.0264 (16)	0.0021 (10)	0.0007 (11)	−0.0051 (12)
C22	0.0380 (14)	0.0485 (17)	0.0217 (16)	0.0030 (12)	0.0038 (12)	−0.0023 (13)
C23	0.0275 (12)	0.0237 (13)	0.0286 (16)	−0.0049 (10)	0.0002 (11)	0.0017 (11)
C24	0.0348 (14)	0.0422 (16)	0.048 (2)	0.0008 (13)	−0.0126 (14)	−0.0022 (14)
C25	0.0222 (12)	0.0338 (14)	0.0343 (17)	0.0037 (11)	−0.0002 (11)	0.0022 (12)
C26	0.0365 (14)	0.0470 (17)	0.0342 (18)	0.0058 (12)	−0.0101 (13)	0.0001 (14)
C27	0.0430 (15)	0.0396 (16)	0.0362 (19)	−0.0174 (13)	0.0005 (13)	−0.0011 (13)
C28	0.0441 (17)	0.073 (2)	0.082 (3)	−0.0202 (16)	0.0277 (18)	0.006 (2)
C29	0.0491 (15)	0.0294 (14)	0.0373 (19)	0.0063 (12)	−0.0066 (14)	0.0063 (13)
C30	0.075 (2)	0.0236 (14)	0.044 (2)	0.0042 (14)	0.0037 (16)	−0.0016 (13)
C31	0.0632 (17)	0.0305 (15)	0.0293 (18)	−0.0106 (13)	0.0057 (15)	0.0039 (13)
C32	0.087 (2)	0.0486 (18)	0.030 (2)	−0.0087 (16)	−0.0014 (17)	0.0072 (15)
C33	0.0262 (12)	0.0324 (14)	0.0289 (16)	0.0017 (11)	0.0042 (11)	0.0095 (12)
C34	0.0389 (15)	0.067 (2)	0.0310 (19)	−0.0047 (14)	0.0035 (13)	−0.0017 (15)
C35	0.0262 (12)	0.0286 (14)	0.0393 (18)	0.0062 (10)	0.0035 (12)	0.0070 (12)
C36	0.0439 (15)	0.0322 (15)	0.049 (2)	0.0113 (12)	0.0073 (14)	0.0140 (14)
C37	0.0254 (12)	0.0248 (13)	0.0235 (15)	−0.0006 (10)	−0.0006 (11)	0.0048 (11)
C38	0.0334 (13)	0.0241 (13)	0.0340 (17)	−0.0006 (11)	0.0008 (12)	0.0024 (12)
C39	0.0220 (11)	0.0264 (13)	0.0300 (16)	−0.0042 (10)	−0.0063 (11)	0.0025 (11)
C40	0.0222 (12)	0.0523 (17)	0.054 (2)	−0.0027 (12)	0.0041 (13)	0.0083 (15)
C41	0.0337 (13)	0.0280 (14)	0.0404 (19)	−0.0061 (11)	−0.0009 (12)	−0.0048 (12)
C42	0.0493 (16)	0.0326 (15)	0.062 (2)	0.0080 (13)	0.0057 (15)	−0.0108 (15)
C43	0.0338 (13)	0.0353 (15)	0.0263 (16)	−0.0044 (11)	0.0062 (12)	−0.0039 (12)
C44	0.0530 (17)	0.065 (2)	0.035 (2)	−0.0175 (15)	−0.0082 (15)	0.0101 (16)
C45	0.0245 (12)	0.0299 (14)	0.0340 (17)	−0.0036 (10)	0.0050 (11)	−0.0002 (12)
C46	0.0291 (13)	0.0373 (15)	0.058 (2)	0.0079 (12)	0.0066 (13)	0.0071 (14)
C47	0.0202 (11)	0.0321 (14)	0.0324 (17)	−0.0037 (10)	−0.0040 (11)	0.0001 (12)
C48	0.0345 (14)	0.0382 (16)	0.047 (2)	−0.0129 (12)	0.0012 (13)	−0.0049 (14)
C49	0.0311 (13)	0.0353 (15)	0.0301 (17)	0.0038 (11)	0.0061 (12)	−0.0047 (12)
C50	0.0319 (13)	0.0352 (15)	0.046 (2)	0.0085 (11)	0.0010 (13)	−0.0013 (13)
C51	0.0283 (13)	0.0306 (14)	0.046 (2)	−0.0039 (11)	0.0043 (12)	0.0055 (13)
C52	0.0429 (16)	0.0435 (17)	0.074 (3)	−0.0045 (13)	0.0157 (16)	0.0164 (17)
C53	0.0410 (14)	0.0247 (13)	0.0373 (18)	0.0068 (11)	0.0112 (13)	0.0000 (12)
C54	0.0304 (14)	0.0490 (18)	0.067 (2)	0.0113 (13)	0.0110 (14)	0.0060 (16)
C55	0.0350 (13)	0.0304 (14)	0.0283 (17)	0.0042 (11)	0.0004 (12)	0.0044 (12)
C56	0.0522 (16)	0.0290 (14)	0.0391 (19)	0.0022 (12)	0.0032 (14)	0.0094 (13)
C57	0.0355 (13)	0.0310 (14)	0.0242 (16)	0.0018 (11)	−0.0031 (12)	0.0014 (12)
C58	0.0464 (15)	0.0363 (15)	0.0357 (19)	−0.0010 (12)	−0.0050 (14)	−0.0083 (13)
C59	0.0339 (13)	0.0304 (14)	0.0317 (17)	0.0007 (11)	0.0060 (12)	0.0051 (12)
C60	0.0489 (16)	0.0401 (16)	0.0373 (19)	−0.0015 (13)	0.0093 (14)	0.0114 (14)
C61	0.0343 (13)	0.0313 (14)	0.0427 (19)	0.0068 (11)	−0.0119 (13)	−0.0087 (13)
C62	0.072 (2)	0.089 (2)	0.034 (2)	0.0421 (19)	−0.0157 (17)	−0.0183 (18)
C63	0.0383 (14)	0.0229 (13)	0.0416 (19)	0.0043 (11)	0.0016 (13)	−0.0007 (12)
C64	0.0542 (17)	0.0279 (15)	0.064 (2)	−0.0098 (13)	0.0041 (16)	−0.0022 (15)

Geometric parameters (Å, º)

P1—N4	1.6343 (19)	C24—H24B	0.9800
P1—N1	1.6355 (19)	C24—H24C	0.9800
P1—N2	1.6371 (19)	C25—C26	1.521 (3)
P1—N3	1.6395 (18)	C25—H25A	0.9900
P2—N6	1.6339 (19)	C25—H25B	0.9900
P2—N7	1.6357 (19)	C26—H26A	0.9800
P2—N8	1.637 (2)	C26—H26B	0.9800
P2—N5	1.6397 (19)	C26—H26C	0.9800
P3—N10	1.6338 (18)	C27—C28	1.518 (3)
P3—N9	1.6340 (19)	C27—H27A	0.9900
P3—N11	1.6342 (19)	C27—H27B	0.9900
P3—N12	1.6382 (17)	C28—H28A	0.9800
P4—N15	1.628 (2)	C28—H28B	0.9800
P4—N16	1.6305 (18)	C28—H28C	0.9800
P4—N14	1.6343 (18)	C29—C30	1.516 (3)
P4—N13	1.6400 (18)	C29—H29A	0.9900
O1W—H1W1	0.789 (16)	C29—H29B	0.9900
O1W—H2W1	0.773 (17)	C30—H30A	0.9800
O2W—H1W2	0.766 (17)	C30—H30B	0.9800
O2W—H2W2	0.790 (16)	C30—H30C	0.9800
N1—C1	1.483 (3)	C31—C32	1.526 (4)
N1—C3	1.485 (3)	C31—H31A	0.9900
N2—C5	1.478 (3)	C31—H31B	0.9900
N2—C7	1.485 (3)	C32—H32A	0.9800
N3—C9	1.483 (3)	C32—H32B	0.9800
N3—C11	1.485 (3)	C32—H32C	0.9800
N4—C13	1.480 (3)	C33—C34	1.510 (3)
N4—C15	1.486 (3)	C33—H33A	0.9900
N5—C17	1.483 (3)	C33—H33B	0.9900
N5—C19	1.485 (3)	C34—H34A	0.9800
N6—C23	1.483 (3)	C34—H34B	0.9800
N6—C21	1.486 (3)	C34—H34C	0.9800
N7—C25	1.476 (3)	C35—C36	1.515 (3)
N7—C27	1.484 (3)	C35—H35A	0.9900
N8—C29	1.480 (3)	C35—H35B	0.9900
N8—C31	1.483 (3)	C36—H36A	0.9800
N9—C33	1.470 (3)	C36—H36B	0.9800
N9—C35	1.486 (3)	C36—H36C	0.9800
N10—C39	1.482 (3)	C37—C38	1.527 (3)
N10—C37	1.485 (3)	C37—H37A	0.9900
N11—C43	1.481 (3)	C37—H37B	0.9900
N11—C41	1.483 (3)	C38—H38A	0.9800
N12—C45	1.476 (3)	C38—H38B	0.9800
N12—C47	1.483 (3)	C38—H38C	0.9800
N13—C51	1.468 (3)	C39—C40	1.526 (3)
N13—C49	1.481 (3)	C39—H39A	0.9900
N14—C53	1.480 (3)	C39—H39B	0.9900
N14—C55	1.480 (3)	C40—H40A	0.9800
N15—C57	1.475 (3)	C40—H40B	0.9800
N15—C59	1.483 (3)	C40—H40C	0.9800
N16—C61	1.479 (3)	C41—C42	1.532 (3)
N16—C63	1.496 (3)	C41—H41A	0.9900
C1—C2	1.518 (3)	C41—H41B	0.9900
C1—H1A	0.9900	C42—H42A	0.9800
C1—H1B	0.9900	C42—H42B	0.9800
C2—H2A	0.9800	C42—H42C	0.9800
C2—H2B	0.9800	C43—C44	1.522 (3)
C2—H2C	0.9800	C43—H43A	0.9900
C3—C4	1.523 (3)	C43—H43B	0.9900
C3—H3A	0.9900	C44—H44A	0.9800
C3—H3B	0.9900	C44—H44B	0.9800
C4—H4A	0.9800	C44—H44C	0.9800
C4—H4B	0.9800	C45—C46	1.522 (3)
C4—H4C	0.9800	C45—H45A	0.9900
C5—C6	1.508 (3)	C45—H45B	0.9900
C5—H5A	0.9900	C46—H46A	0.9800
C5—H5B	0.9900	C46—H46B	0.9800
C6—H6A	0.9800	C46—H46C	0.9800
C6—H6B	0.9800	C47—C48	1.508 (3)
C6—H6C	0.9800	C47—H47A	0.9900
C7—C8	1.516 (3)	C47—H47B	0.9900
C7—H7A	0.9900	C48—H48A	0.9800
C7—H7B	0.9900	C48—H48B	0.9800
C8—H8A	0.9800	C48—H48C	0.9800
C8—H8B	0.9800	C49—C50	1.515 (3)
C8—H8C	0.9800	C49—H49A	0.9900
C9—C10	1.528 (3)	C49—H49B	0.9900
C9—H9A	0.9900	C50—H50A	0.9800
C9—H9B	0.9900	C50—H50B	0.9800
C10—H10A	0.9800	C50—H50C	0.9800
C10—H10B	0.9800	C51—C52	1.525 (4)
C10—H10C	0.9800	C51—H51A	0.9900
C11—C12	1.514 (3)	C51—H51B	0.9900
C11—H11A	0.9900	C52—H52A	0.9800
C11—H11B	0.9900	C52—H52B	0.9800
C12—H12A	0.9800	C52—H52C	0.9800
C12—H12B	0.9800	C53—C54	1.523 (3)
C12—H12C	0.9800	C53—H53A	0.9900
C13—C14	1.517 (3)	C53—H53B	0.9900
C13—H13A	0.9900	C54—H54A	0.9800
C13—H13B	0.9900	C54—H54B	0.9800
C14—H14A	0.9800	C54—H54C	0.9800
C14—H14B	0.9800	C55—C56	1.520 (3)
C14—H14C	0.9800	C55—H55A	0.9900
C15—C16	1.518 (3)	C55—H55B	0.9900
C15—H15A	0.9900	C56—H56A	0.9800
C15—H15B	0.9900	C56—H56B	0.9800
C16—H16A	0.9800	C56—H56C	0.9800
C16—H16B	0.9800	C57—C58	1.524 (3)
C16—H16C	0.9800	C57—H57A	0.9900
C17—C18	1.517 (3)	C57—H57B	0.9900
C17—H17A	0.9900	C58—H58A	0.9800
C17—H17B	0.9900	C58—H58B	0.9800
C18—H18A	0.9800	C58—H58C	0.9800
C18—H18B	0.9800	C59—C60	1.526 (3)
C18—H18C	0.9800	C59—H59A	0.9900
C19—C20	1.532 (3)	C59—H59B	0.9900
C19—H19A	0.9900	C60—H60A	0.9800
C19—H19B	0.9900	C60—H60B	0.9800
C20—H20A	0.9800	C60—H60C	0.9800
C20—H20B	0.9800	C61—C62	1.512 (4)
C20—H20C	0.9800	C61—H61A	0.9900
C21—C22	1.517 (3)	C61—H61B	0.9900
C21—H21A	0.9900	C62—H62A	0.9800
C21—H21B	0.9900	C62—H62B	0.9800
C22—H22A	0.9800	C62—H62C	0.9800
C22—H22B	0.9800	C63—C64	1.527 (3)
C22—H22C	0.9800	C63—H63A	0.9900
C23—C24	1.508 (3)	C63—H63B	0.9900
C23—H23A	0.9900	C64—H64A	0.9800
C23—H23B	0.9900	C64—H64B	0.9800
C24—H24A	0.9800	C64—H64C	0.9800
N4—P1—N1	112.11 (9)	H26B—C26—H26C	109.5
N4—P1—N2	111.82 (9)	N7—C27—C28	113.8 (2)
N1—P1—N2	105.01 (10)	N7—C27—H27A	108.8
N4—P1—N3	104.91 (10)	C28—C27—H27A	108.8
N1—P1—N3	111.76 (9)	N7—C27—H27B	108.8
N2—P1—N3	111.41 (9)	C28—C27—H27B	108.8
N6—P2—N7	104.84 (10)	H27A—C27—H27B	107.7
N6—P2—N8	111.86 (10)	C27—C28—H28A	109.5
N7—P2—N8	112.16 (10)	C27—C28—H28B	109.5
N6—P2—N5	111.86 (9)	H28A—C28—H28B	109.5
N7—P2—N5	111.27 (10)	C27—C28—H28C	109.5
N8—P2—N5	105.01 (11)	H28A—C28—H28C	109.5
N10—P3—N9	111.26 (10)	H28B—C28—H28C	109.5
N10—P3—N11	112.62 (10)	N8—C29—C30	114.6 (2)
N9—P3—N11	105.23 (10)	N8—C29—H29A	108.6
N10—P3—N12	104.70 (9)	C30—C29—H29A	108.6
N9—P3—N12	111.25 (10)	N8—C29—H29B	108.6
N11—P3—N12	111.93 (10)	C30—C29—H29B	108.6
N15—P4—N16	105.28 (10)	H29A—C29—H29B	107.6
N15—P4—N14	112.03 (10)	C29—C30—H30A	109.5
N16—P4—N14	111.45 (9)	C29—C30—H30B	109.5
N15—P4—N13	112.03 (10)	H30A—C30—H30B	109.5
N16—P4—N13	111.64 (10)	C29—C30—H30C	109.5
N14—P4—N13	104.58 (10)	H30A—C30—H30C	109.5
H1W1—O1W—H2W1	102 (3)	H30B—C30—H30C	109.5
H1W2—O2W—H2W2	106 (3)	N8—C31—C32	113.2 (2)
C1—N1—C3	114.49 (18)	N8—C31—H31A	108.9
C1—N1—P1	120.29 (16)	C32—C31—H31A	108.9
C3—N1—P1	122.50 (15)	N8—C31—H31B	108.9
C5—N2—C7	114.81 (18)	C32—C31—H31B	108.9
C5—N2—P1	119.96 (16)	H31A—C31—H31B	107.7
C7—N2—P1	122.16 (15)	C31—C32—H32A	109.5
C9—N3—C11	114.46 (17)	C31—C32—H32B	109.5
C9—N3—P1	119.85 (16)	H32A—C32—H32B	109.5
C11—N3—P1	122.54 (15)	C31—C32—H32C	109.5
C13—N4—C15	114.44 (18)	H32A—C32—H32C	109.5
C13—N4—P1	120.56 (16)	H32B—C32—H32C	109.5
C15—N4—P1	122.60 (14)	N9—C33—C34	114.87 (19)
C17—N5—C19	114.44 (18)	N9—C33—H33A	108.6
C17—N5—P2	119.14 (17)	C34—C33—H33A	108.6
C19—N5—P2	122.55 (15)	N9—C33—H33B	108.6
C23—N6—C21	114.06 (17)	C34—C33—H33B	108.6
C23—N6—P2	121.15 (15)	H33A—C33—H33B	107.5
C21—N6—P2	122.78 (14)	C33—C34—H34A	109.5
C25—N7—C27	114.57 (18)	C33—C34—H34B	109.5
C25—N7—P2	122.94 (15)	H34A—C34—H34B	109.5
C27—N7—P2	120.47 (17)	C33—C34—H34C	109.5
C29—N8—C31	114.72 (19)	H34A—C34—H34C	109.5
C29—N8—P2	119.77 (17)	H34B—C34—H34C	109.5
C31—N8—P2	122.72 (16)	N9—C35—C36	113.56 (19)
C33—N9—C35	115.16 (19)	N9—C35—H35A	108.9
C33—N9—P3	121.60 (14)	C36—C35—H35A	108.9
C35—N9—P3	122.39 (16)	N9—C35—H35B	108.9
C39—N10—C37	114.45 (17)	C36—C35—H35B	108.9
C39—N10—P3	120.25 (14)	H35A—C35—H35B	107.7
C37—N10—P3	123.09 (14)	C35—C36—H36A	109.5
C43—N11—C41	114.34 (19)	C35—C36—H36B	109.5
C43—N11—P3	120.30 (15)	H36A—C36—H36B	109.5
C41—N11—P3	122.54 (16)	C35—C36—H36C	109.5
C45—N12—C47	115.46 (16)	H36A—C36—H36C	109.5
C45—N12—P3	122.28 (15)	H36B—C36—H36C	109.5
C47—N12—P3	120.95 (14)	N10—C37—C38	112.5 (2)
C51—N13—C49	115.39 (17)	N10—C37—H37A	109.1
C51—N13—P4	122.46 (15)	C38—C37—H37A	109.1
C49—N13—P4	121.42 (15)	N10—C37—H37B	109.1
C53—N14—C55	114.18 (18)	C38—C37—H37B	109.1
C53—N14—P4	120.70 (16)	H37A—C37—H37B	107.8
C55—N14—P4	122.92 (15)	C37—C38—H38A	109.5
C57—N15—C59	114.9 (2)	C37—C38—H38B	109.5
C57—N15—P4	120.84 (15)	H38A—C38—H38B	109.5
C59—N15—P4	122.31 (16)	C37—C38—H38C	109.5
C61—N16—C63	115.04 (18)	H38A—C38—H38C	109.5
C61—N16—P4	120.58 (16)	H38B—C38—H38C	109.5
C63—N16—P4	121.81 (15)	N10—C39—C40	113.4 (2)
N1—C1—C2	114.81 (19)	N10—C39—H39A	108.9
N1—C1—H1A	108.6	C40—C39—H39A	108.9
C2—C1—H1A	108.6	N10—C39—H39B	108.9
N1—C1—H1B	108.6	C40—C39—H39B	108.9
C2—C1—H1B	108.6	H39A—C39—H39B	107.7
H1A—C1—H1B	107.5	C39—C40—H40A	109.5
C1—C2—H2A	109.5	C39—C40—H40B	109.5
C1—C2—H2B	109.5	H40A—C40—H40B	109.5
H2A—C2—H2B	109.5	C39—C40—H40C	109.5
C1—C2—H2C	109.5	H40A—C40—H40C	109.5
H2A—C2—H2C	109.5	H40B—C40—H40C	109.5
H2B—C2—H2C	109.5	N11—C41—C42	112.42 (19)
N1—C3—C4	113.59 (18)	N11—C41—H41A	109.1
N1—C3—H3A	108.8	C42—C41—H41A	109.1
C4—C3—H3A	108.8	N11—C41—H41B	109.1
N1—C3—H3B	108.8	C42—C41—H41B	109.1
C4—C3—H3B	108.8	H41A—C41—H41B	107.9
H3A—C3—H3B	107.7	C41—C42—H42A	109.5
C3—C4—H4A	109.5	C41—C42—H42B	109.5
C3—C4—H4B	109.5	H42A—C42—H42B	109.5
H4A—C4—H4B	109.5	C41—C42—H42C	109.5
C3—C4—H4C	109.5	H42A—C42—H42C	109.5
H4A—C4—H4C	109.5	H42B—C42—H42C	109.5
H4B—C4—H4C	109.5	N11—C43—C44	114.7 (2)
N2—C5—C6	114.40 (18)	N11—C43—H43A	108.6
N2—C5—H5A	108.7	C44—C43—H43A	108.6
C6—C5—H5A	108.7	N11—C43—H43B	108.6
N2—C5—H5B	108.7	C44—C43—H43B	108.6
C6—C5—H5B	108.7	H43A—C43—H43B	107.6
H5A—C5—H5B	107.6	C43—C44—H44A	109.5
C5—C6—H6A	109.5	C43—C44—H44B	109.5
C5—C6—H6B	109.5	H44A—C44—H44B	109.5
H6A—C6—H6B	109.5	C43—C44—H44C	109.5
C5—C6—H6C	109.5	H44A—C44—H44C	109.5
H6A—C6—H6C	109.5	H44B—C44—H44C	109.5
H6B—C6—H6C	109.5	N12—C45—C46	113.3 (2)
N2—C7—C8	112.86 (18)	N12—C45—H45A	108.9
N2—C7—H7A	109.0	C46—C45—H45A	108.9
C8—C7—H7A	109.0	N12—C45—H45B	108.9
N2—C7—H7B	109.0	C46—C45—H45B	108.9
C8—C7—H7B	109.0	H45A—C45—H45B	107.7
H7A—C7—H7B	107.8	C45—C46—H46A	109.5
C7—C8—H8A	109.5	C45—C46—H46B	109.5
C7—C8—H8B	109.5	H46A—C46—H46B	109.5
H8A—C8—H8B	109.5	C45—C46—H46C	109.5
C7—C8—H8C	109.5	H46A—C46—H46C	109.5
H8A—C8—H8C	109.5	H46B—C46—H46C	109.5
H8B—C8—H8C	109.5	N12—C47—C48	114.6 (2)
N3—C9—C10	114.02 (19)	N12—C47—H47A	108.6
N3—C9—H9A	108.7	C48—C47—H47A	108.6
C10—C9—H9A	108.7	N12—C47—H47B	108.6
N3—C9—H9B	108.7	C48—C47—H47B	108.6
C10—C9—H9B	108.7	H47A—C47—H47B	107.6
H9A—C9—H9B	107.6	C47—C48—H48A	109.5
C9—C10—H10A	109.5	C47—C48—H48B	109.5
C9—C10—H10B	109.5	H48A—C48—H48B	109.5
H10A—C10—H10B	109.5	C47—C48—H48C	109.5
C9—C10—H10C	109.5	H48A—C48—H48C	109.5
H10A—C10—H10C	109.5	H48B—C48—H48C	109.5
H10B—C10—H10C	109.5	N13—C49—C50	114.7 (2)
N3—C11—C12	113.2 (2)	N13—C49—H49A	108.6
N3—C11—H11A	108.9	C50—C49—H49A	108.6
C12—C11—H11A	108.9	N13—C49—H49B	108.6
N3—C11—H11B	108.9	C50—C49—H49B	108.6
C12—C11—H11B	108.9	H49A—C49—H49B	107.6
H11A—C11—H11B	107.8	C49—C50—H50A	109.5
C11—C12—H12A	109.5	C49—C50—H50B	109.5
C11—C12—H12B	109.5	H50A—C50—H50B	109.5
H12A—C12—H12B	109.5	C49—C50—H50C	109.5
C11—C12—H12C	109.5	H50A—C50—H50C	109.5
H12A—C12—H12C	109.5	H50B—C50—H50C	109.5
H12B—C12—H12C	109.5	N13—C51—C52	113.8 (2)
N4—C13—C14	113.86 (19)	N13—C51—H51A	108.8
N4—C13—H13A	108.8	C52—C51—H51A	108.8
C14—C13—H13A	108.8	N13—C51—H51B	108.8
N4—C13—H13B	108.8	C52—C51—H51B	108.8
C14—C13—H13B	108.8	H51A—C51—H51B	107.7
H13A—C13—H13B	107.7	C51—C52—H52A	109.5
C13—C14—H14A	109.5	C51—C52—H52B	109.5
C13—C14—H14B	109.5	H52A—C52—H52B	109.5
H14A—C14—H14B	109.5	C51—C52—H52C	109.5
C13—C14—H14C	109.5	H52A—C52—H52C	109.5
H14A—C14—H14C	109.5	H52B—C52—H52C	109.5
H14B—C14—H14C	109.5	N14—C53—C54	113.8 (2)
N4—C15—C16	112.40 (19)	N14—C53—H53A	108.8
N4—C15—H15A	109.1	C54—C53—H53A	108.8
C16—C15—H15A	109.1	N14—C53—H53B	108.8
N4—C15—H15B	109.1	C54—C53—H53B	108.8
C16—C15—H15B	109.1	H53A—C53—H53B	107.7
H15A—C15—H15B	107.9	C53—C54—H54A	109.5
C15—C16—H16A	109.5	C53—C54—H54B	109.5
C15—C16—H16B	109.5	H54A—C54—H54B	109.5
H16A—C16—H16B	109.5	C53—C54—H54C	109.5
C15—C16—H16C	109.5	H54A—C54—H54C	109.5
H16A—C16—H16C	109.5	H54B—C54—H54C	109.5
H16B—C16—H16C	109.5	N14—C55—C56	112.8 (2)
N5—C17—C18	115.22 (18)	N14—C55—H55A	109.0
N5—C17—H17A	108.5	C56—C55—H55A	109.0
C18—C17—H17A	108.5	N14—C55—H55B	109.0
N5—C17—H17B	108.5	C56—C55—H55B	109.0
C18—C17—H17B	108.5	H55A—C55—H55B	107.8
H17A—C17—H17B	107.5	C55—C56—H56A	109.5
C17—C18—H18A	109.5	C55—C56—H56B	109.5
C17—C18—H18B	109.5	H56A—C56—H56B	109.5
H18A—C18—H18B	109.5	C55—C56—H56C	109.5
C17—C18—H18C	109.5	H56A—C56—H56C	109.5
H18A—C18—H18C	109.5	H56B—C56—H56C	109.5
H18B—C18—H18C	109.5	N15—C57—C58	113.79 (18)
N5—C19—C20	113.4 (2)	N15—C57—H57A	108.8
N5—C19—H19A	108.9	C58—C57—H57A	108.8
C20—C19—H19A	108.9	N15—C57—H57B	108.8
N5—C19—H19B	108.9	C58—C57—H57B	108.8
C20—C19—H19B	108.9	H57A—C57—H57B	107.7
H19A—C19—H19B	107.7	C57—C58—H58A	109.5
C19—C20—H20A	109.5	C57—C58—H58B	109.5
C19—C20—H20B	109.5	H58A—C58—H58B	109.5
H20A—C20—H20B	109.5	C57—C58—H58C	109.5
C19—C20—H20C	109.5	H58A—C58—H58C	109.5
H20A—C20—H20C	109.5	H58B—C58—H58C	109.5
H20B—C20—H20C	109.5	N15—C59—C60	113.55 (19)
N6—C21—C22	112.84 (19)	N15—C59—H59A	108.9
N6—C21—H21A	109.0	C60—C59—H59A	108.9
C22—C21—H21A	109.0	N15—C59—H59B	108.9
N6—C21—H21B	109.0	C60—C59—H59B	108.9
C22—C21—H21B	109.0	H59A—C59—H59B	107.7
H21A—C21—H21B	107.8	C59—C60—H60A	109.5
C21—C22—H22A	109.5	C59—C60—H60B	109.5
C21—C22—H22B	109.5	H60A—C60—H60B	109.5
H22A—C22—H22B	109.5	C59—C60—H60C	109.5
C21—C22—H22C	109.5	H60A—C60—H60C	109.5
H22A—C22—H22C	109.5	H60B—C60—H60C	109.5
H22B—C22—H22C	109.5	N16—C61—C62	114.46 (19)
N6—C23—C24	114.01 (18)	N16—C61—H61A	108.6
N6—C23—H23A	108.8	C62—C61—H61A	108.6
C24—C23—H23A	108.8	N16—C61—H61B	108.6
N6—C23—H23B	108.8	C62—C61—H61B	108.6
C24—C23—H23B	108.8	H61A—C61—H61B	107.6
H23A—C23—H23B	107.6	C61—C62—H62A	109.5
C23—C24—H24A	109.5	C61—C62—H62B	109.5
C23—C24—H24B	109.5	H62A—C62—H62B	109.5
H24A—C24—H24B	109.5	C61—C62—H62C	109.5
C23—C24—H24C	109.5	H62A—C62—H62C	109.5
H24A—C24—H24C	109.5	H62B—C62—H62C	109.5
H24B—C24—H24C	109.5	N16—C63—C64	112.13 (19)
N7—C25—C26	113.18 (19)	N16—C63—H63A	109.2
N7—C25—H25A	108.9	C64—C63—H63A	109.2
C26—C25—H25A	108.9	N16—C63—H63B	109.2
N7—C25—H25B	108.9	C64—C63—H63B	109.2
C26—C25—H25B	108.9	H63A—C63—H63B	107.9
H25A—C25—H25B	107.8	C63—C64—H64A	109.5
C25—C26—H26A	109.5	C63—C64—H64B	109.5
C25—C26—H26B	109.5	H64A—C64—H64B	109.5
H26A—C26—H26B	109.5	C63—C64—H64C	109.5
C25—C26—H26C	109.5	H64A—C64—H64C	109.5
H26A—C26—H26C	109.5	H64B—C64—H64C	109.5
N4—P1—N1—C1	33.09 (19)	N13—P4—N14—C53	−152.67 (17)
N2—P1—N1—C1	154.71 (16)	N15—P4—N14—C55	166.72 (16)
N3—P1—N1—C1	−84.37 (18)	N16—P4—N14—C55	−75.61 (19)
N4—P1—N1—C3	−166.65 (16)	N13—P4—N14—C55	45.15 (19)
N2—P1—N1—C3	−45.03 (19)	N16—P4—N15—C57	148.26 (15)
N3—P1—N1—C3	75.89 (19)	N14—P4—N15—C57	−90.45 (17)
N4—P1—N2—C5	−82.73 (17)	N13—P4—N15—C57	26.73 (19)
N1—P1—N2—C5	155.46 (15)	N16—P4—N15—C59	−48.45 (19)
N3—P1—N2—C5	34.31 (18)	N14—P4—N15—C59	72.84 (19)
N4—P1—N2—C7	76.40 (19)	N13—P4—N15—C59	−169.98 (16)
N1—P1—N2—C7	−45.40 (19)	N15—P4—N16—C61	154.60 (17)
N3—P1—N2—C7	−166.56 (17)	N14—P4—N16—C61	32.9 (2)
N4—P1—N3—C9	−156.89 (16)	N13—P4—N16—C61	−83.62 (18)
N1—P1—N3—C9	−35.17 (19)	N15—P4—N16—C63	−44.47 (19)
N2—P1—N3—C9	81.95 (18)	N14—P4—N16—C63	−166.14 (17)
N4—P1—N3—C11	44.29 (19)	N13—P4—N16—C63	77.3 (2)
N1—P1—N3—C11	166.01 (17)	C3—N1—C1—C2	−63.9 (3)
N2—P1—N3—C11	−76.9 (2)	P1—N1—C1—C2	97.9 (2)
N1—P1—N4—C13	82.79 (18)	C1—N1—C3—C4	−67.7 (3)
N2—P1—N4—C13	−34.84 (19)	P1—N1—C3—C4	130.97 (19)
N3—P1—N4—C13	−155.73 (16)	C7—N2—C5—C6	−68.2 (3)
N1—P1—N4—C15	−78.64 (19)	P1—N2—C5—C6	92.4 (2)
N2—P1—N4—C15	163.74 (17)	C5—N2—C7—C8	−65.3 (3)
N3—P1—N4—C15	42.84 (19)	P1—N2—C7—C8	134.58 (19)
N6—P2—N5—C17	82.15 (17)	C11—N3—C9—C10	73.0 (3)
N7—P2—N5—C17	−34.75 (19)	P1—N3—C9—C10	−87.4 (2)
N8—P2—N5—C17	−156.32 (16)	C9—N3—C11—C12	68.3 (3)
N6—P2—N5—C19	−74.5 (2)	P1—N3—C11—C12	−131.86 (19)
N7—P2—N5—C19	168.62 (18)	C15—N4—C13—C14	70.3 (3)
N8—P2—N5—C19	47.0 (2)	P1—N4—C13—C14	−92.6 (2)
N7—P2—N6—C23	153.11 (16)	C13—N4—C15—C16	64.5 (3)
N8—P2—N6—C23	−85.10 (17)	P1—N4—C15—C16	−133.02 (18)
N5—P2—N6—C23	32.40 (19)	C19—N5—C17—C18	77.0 (3)
N7—P2—N6—C21	−43.95 (18)	P2—N5—C17—C18	−81.4 (2)
N8—P2—N6—C21	77.84 (19)	C17—N5—C19—C20	72.7 (3)
N5—P2—N6—C21	−164.66 (16)	P2—N5—C19—C20	−129.67 (19)
N6—P2—N7—C25	−42.06 (19)	C23—N6—C21—C22	−63.3 (2)
N8—P2—N7—C25	−163.66 (17)	P2—N6—C21—C22	132.64 (18)
N5—P2—N7—C25	79.04 (19)	C21—N6—C23—C24	−70.3 (3)
N6—P2—N7—C27	155.01 (17)	P2—N6—C23—C24	94.0 (2)
N8—P2—N7—C27	33.4 (2)	C27—N7—C25—C26	−64.5 (3)
N5—P2—N7—C27	−83.90 (19)	P2—N7—C25—C26	131.64 (18)
N6—P2—N8—C29	−34.6 (2)	C25—N7—C27—C28	−64.6 (3)
N7—P2—N8—C29	82.85 (18)	P2—N7—C27—C28	99.7 (3)
N5—P2—N8—C29	−156.17 (16)	C31—N8—C29—C30	70.6 (3)
N6—P2—N8—C31	165.31 (17)	P2—N8—C29—C30	−90.9 (2)
N7—P2—N8—C31	−77.2 (2)	C29—N8—C31—C32	67.7 (3)
N5—P2—N8—C31	43.8 (2)	P2—N8—C31—C32	−131.4 (2)
N10—P3—N9—C33	−93.99 (18)	C35—N9—C33—C34	−66.4 (3)
N11—P3—N9—C33	143.75 (17)	P3—N9—C33—C34	103.3 (2)
N12—P3—N9—C33	22.3 (2)	C33—N9—C35—C36	−57.5 (3)
N10—P3—N9—C35	74.90 (19)	P3—N9—C35—C36	132.9 (2)
N11—P3—N9—C35	−47.35 (19)	C39—N10—C37—C38	63.8 (2)
N12—P3—N9—C35	−168.76 (16)	P3—N10—C37—C38	−133.02 (17)
N9—P3—N10—C39	−27.85 (19)	C37—N10—C39—C40	73.2 (2)
N11—P3—N10—C39	90.02 (18)	P3—N10—C39—C40	−90.5 (2)
N12—P3—N10—C39	−148.14 (17)	C43—N11—C41—C42	−68.9 (3)
N9—P3—N10—C37	169.95 (16)	P3—N11—C41—C42	130.1 (2)
N11—P3—N10—C37	−72.17 (18)	C41—N11—C43—C44	−73.9 (3)
N12—P3—N10—C37	49.67 (19)	P3—N11—C43—C44	87.5 (2)
N10—P3—N11—C43	36.24 (19)	C47—N12—C45—C46	63.3 (3)
N9—P3—N11—C43	157.62 (16)	P3—N12—C45—C46	−129.63 (18)
N12—P3—N11—C43	−81.41 (17)	C45—N12—C47—C48	59.6 (3)
N10—P3—N11—C41	−163.84 (16)	P3—N12—C47—C48	−107.6 (2)
N9—P3—N11—C41	−42.47 (19)	C51—N13—C49—C50	54.9 (3)
N12—P3—N11—C41	78.50 (19)	P4—N13—C49—C50	−115.5 (2)
N10—P3—N12—C45	41.0 (2)	C49—N13—C51—C52	57.2 (3)
N9—P3—N12—C45	−79.3 (2)	P4—N13—C51—C52	−132.47 (19)
N11—P3—N12—C45	163.33 (18)	C55—N14—C53—C54	70.2 (3)
N10—P3—N12—C47	−152.64 (17)	P4—N14—C53—C54	−93.4 (2)
N9—P3—N12—C47	87.07 (19)	C53—N14—C55—C56	66.7 (2)
N11—P3—N12—C47	−30.3 (2)	P4—N14—C55—C56	−130.06 (18)
N15—P4—N13—C51	−77.2 (2)	C59—N15—C57—C58	−77.0 (3)
N16—P4—N13—C51	164.97 (18)	P4—N15—C57—C58	87.4 (2)
N14—P4—N13—C51	44.3 (2)	C57—N15—C59—C60	−67.5 (3)
N15—P4—N13—C49	92.53 (19)	P4—N15—C59—C60	128.2 (2)
N16—P4—N13—C49	−25.3 (2)	C63—N16—C61—C62	−72.8 (3)
N14—P4—N13—C49	−145.91 (18)	P4—N16—C61—C62	89.3 (2)
N15—P4—N14—C53	−31.11 (19)	C61—N16—C63—C64	−67.7 (3)
N16—P4—N14—C53	86.57 (19)	P4—N16—C63—C64	130.4 (2)

Hydrogen-bond geometry (Å, º)

D—H···A	D—H	H···A	D···A	D—H···A
O1W—H2W1···Br1	0.77 (2)	2.66 (2)	3.425 (2)	174 (3)
O1W—H1W1···Br1^i	0.79 (2)	2.82 (2)	3.611 (3)	176 (3)
O2W—H1W2···Br2	0.77 (2)	2.71 (2)	3.467 (3)	169 (3)
O2W—H2W2···Br2^ii	0.79 (2)	2.68 (2)	3.471 (2)	177 (3)

Symmetry codes: (i) −x+1, −y+2, −z; (ii) −x+1, −y+1, −z+1.