(18-Crown-6)potassium di-tert-butyl­phospanylbisborohydride

The structure of the title compound, [K(C₁₂H₂₄O₆)](C₈H₂₄B₂P), is composed of di-tert-butyl­phosphanylbisborohydride anions and K cations which are coordinated by a crown ether mol­ecule.

Key indicators

• Single-crystal X-ray study
• T = 173 K
• Mean [sigma](C-C) = 0.003 Å
• R factor = 0.027
• wR factor = 0.049
• Data-to-parameter ratio = 18.6

checkCIF/PLATON results

No syntax errors found



Alert level C
PLAT029_ALERT_3_C _diffrn_measured_fraction_theta_full Low .......       0.96
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT241_ALERT_2_C Check High      Ueq as Compared to Neighbors for         B1

   0 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   3 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
   1 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
   0 ALERT type 4 Improvement, methodology, query or suggestion
   0 ALERT type 5 Informative message, check

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Computing details

Data collection: X-AREA (Stoe & Cie, 2001); cell refinement: X-AREA; data reduction: X-AREA; program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: XP in SHELXTL-Plus (Sheldrick, 1991); software used to prepare material for publication: SHELXL97.

(18-Crown-6)potassium di-tert-butylphospanylbisborohydride

Crystal data

[K(C12H24O6)](C8H24B2P)	F(000) = 1040
Mr = 476.27	Dx = 1.137 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 9632 reflections
a = 9.5690 (13) Å	θ = 3.6–25.8°
b = 15.8008 (15) Å	µ = 0.28 mm^−1
c = 18.850 (2) Å	T = 173 K
β = 102.585 (11)°	Block, colourless
V = 2781.6 (6) Å^3	0.48 × 0.43 × 0.37 mm
Z = 4

Data collection

Stow IPDS-II two-circle diffractometer	5075 independent reflections
Radiation source: fine-focus sealed tube	3446 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.031
ω scans	θmax = 25.8°, θmin = 3.8°
Absorption correction: multi-scan (MULABS; Spek, 2003; Blessing, 1995)	h = −11→10
Tmin = 0.878, Tmax = 0.904	k = −19→19
12395 measured reflections	l = −17→22

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.028	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.049	H-atom parameters constrained
S = 1.02	w = 1/[σ^2(Fo^2) + (0.01P)^2] where P = (Fo^2 + 2Fc^2)/3
5075 reflections	(Δ/σ)max = 0.001
273 parameters	Δρmax = 0.19 e Å^−3
0 restraints	Δρmin = −0.16 e Å^−3

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
K1	0.21591 (4)	0.459423 (19)	0.70243 (2)	0.02810 (9)
O1	−0.07433 (13)	0.43704 (6)	0.71942 (7)	0.0408 (3)
C2	−0.1763 (2)	0.44810 (12)	0.65252 (11)	0.0501 (5)
H2A	−0.2745	0.4460	0.6613	0.060*
H2B	−0.1662	0.4020	0.6184	0.060*
C3	−0.1509 (2)	0.53155 (12)	0.62058 (11)	0.0481 (5)
H3A	−0.2269	0.5430	0.5768	0.058*
H3B	−0.1524	0.5773	0.6563	0.058*
O4	−0.01617 (13)	0.52858 (6)	0.60185 (7)	0.0375 (3)
C5	0.0127 (2)	0.60426 (10)	0.56653 (11)	0.0482 (5)
H5A	0.0055	0.6538	0.5977	0.058*
H5B	−0.0584	0.6112	0.5201	0.058*
C6	0.1582 (2)	0.59915 (10)	0.55244 (10)	0.0447 (5)
H6A	0.1693	0.5458	0.5267	0.054*
H6B	0.1745	0.6471	0.5214	0.054*
O7	0.25982 (13)	0.60203 (6)	0.62028 (6)	0.0340 (3)
C8	0.4028 (2)	0.60226 (10)	0.61101 (10)	0.0404 (5)
H8A	0.4193	0.6523	0.5823	0.049*
H8B	0.4213	0.5507	0.5847	0.049*
C9	0.50084 (19)	0.60484 (9)	0.68440 (10)	0.0375 (4)
H9A	0.6008	0.6140	0.6797	0.045*
H9B	0.4735	0.6517	0.7135	0.045*
O10	0.48848 (12)	0.52601 (6)	0.71857 (6)	0.0340 (3)
C11	0.5904 (2)	0.51424 (10)	0.78490 (10)	0.0362 (4)
H11A	0.5748	0.5562	0.8214	0.043*
H11B	0.6886	0.5215	0.7771	0.043*
C12	0.5709 (2)	0.42663 (10)	0.81086 (10)	0.0385 (4)
H12A	0.5790	0.3851	0.7726	0.046*
H12B	0.6462	0.4139	0.8546	0.046*
O13	0.43407 (13)	0.42064 (6)	0.82765 (6)	0.0350 (3)
C14	0.4076 (2)	0.33694 (9)	0.85039 (10)	0.0417 (5)
H14A	0.4835	0.3202	0.8927	0.050*
H14B	0.4082	0.2963	0.8105	0.050*
C15	0.2674 (2)	0.33578 (10)	0.87023 (10)	0.0452 (5)
H15A	0.2525	0.2804	0.8920	0.054*
H15B	0.2637	0.3805	0.9066	0.054*
O16	0.15780 (13)	0.34979 (7)	0.80671 (7)	0.0393 (3)
C17	0.0204 (2)	0.35096 (10)	0.82225 (12)	0.0449 (5)
H17A	0.0113	0.4001	0.8535	0.054*
H17B	0.0048	0.2987	0.8484	0.054*
C18	−0.0876 (2)	0.35695 (10)	0.75255 (12)	0.0495 (5)
H18A	−0.0724	0.3108	0.7196	0.059*
H18B	−0.1851	0.3509	0.7618	0.059*
P1	0.36027 (5)	0.22344 (2)	0.56502 (2)	0.02450 (9)
B1	0.3564 (3)	0.33193 (11)	0.61270 (13)	0.0434 (6)
H1A	0.2700	0.3630	0.5893	0.065*
H1B	0.4413	0.3647	0.6089	0.065*
H1C	0.3558	0.3229	0.6641	0.065*
B2	0.3139 (2)	0.22855 (12)	0.45964 (10)	0.0330 (4)
H2C	0.3417	0.1753	0.4399	0.050*
H2D	0.3659	0.2756	0.4434	0.050*
H2E	0.2107	0.2373	0.4425	0.050*
C20	0.2276 (2)	0.15140 (10)	0.59414 (10)	0.0384 (4)
C21	0.0889 (2)	0.20256 (13)	0.58557 (13)	0.0565 (6)
H21A	0.0579	0.2213	0.5350	0.085*
H21B	0.1058	0.2520	0.6177	0.085*
H21C	0.0143	0.1671	0.5985	0.085*
C22	0.2731 (2)	0.12358 (13)	0.67385 (11)	0.0561 (6)
H22A	0.2939	0.1737	0.7050	0.084*
H22B	0.3591	0.0882	0.6801	0.084*
H22C	0.1956	0.0911	0.6873	0.084*
C23	0.1944 (2)	0.07373 (10)	0.54419 (12)	0.0549 (6)
H23A	0.1657	0.0924	0.4935	0.082*
H23B	0.1164	0.0412	0.5571	0.082*
H23C	0.2800	0.0381	0.5501	0.082*
C30	0.54635 (18)	0.18079 (9)	0.59595 (9)	0.0306 (4)
C31	0.5596 (2)	0.08738 (9)	0.57657 (11)	0.0469 (5)
H31A	0.5211	0.0792	0.5244	0.070*
H31B	0.5054	0.0526	0.6042	0.070*
H31C	0.6606	0.0706	0.5887	0.070*
C32	0.6386 (2)	0.23176 (11)	0.55419 (11)	0.0447 (5)
H32A	0.6019	0.2243	0.5018	0.067*
H32B	0.7378	0.2118	0.5675	0.067*
H32C	0.6351	0.2919	0.5666	0.067*
C33	0.6068 (2)	0.19390 (10)	0.67754 (10)	0.0427 (5)
H33A	0.5986	0.2537	0.6897	0.064*
H33B	0.7077	0.1770	0.6896	0.064*
H33C	0.5526	0.1593	0.7054	0.064*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0265 (2)	0.02755 (15)	0.03042 (19)	0.00041 (15)	0.00663 (16)	0.00102 (15)
O1	0.0297 (7)	0.0402 (6)	0.0525 (9)	−0.0066 (5)	0.0092 (7)	−0.0066 (5)
C2	0.0249 (10)	0.0661 (12)	0.0598 (14)	−0.0071 (9)	0.0105 (10)	−0.0193 (10)
C3	0.0306 (11)	0.0593 (11)	0.0495 (12)	0.0115 (9)	−0.0020 (10)	−0.0119 (10)
O4	0.0295 (7)	0.0352 (6)	0.0446 (7)	0.0053 (5)	0.0012 (6)	0.0009 (5)
C5	0.0486 (14)	0.0366 (9)	0.0480 (12)	0.0037 (8)	−0.0143 (11)	0.0059 (8)
C6	0.0577 (15)	0.0391 (9)	0.0306 (10)	−0.0090 (8)	−0.0051 (10)	0.0086 (8)
O7	0.0361 (8)	0.0346 (5)	0.0291 (7)	−0.0030 (5)	0.0026 (6)	0.0037 (5)
C8	0.0446 (13)	0.0389 (9)	0.0415 (11)	−0.0039 (8)	0.0173 (10)	0.0079 (8)
C9	0.0323 (11)	0.0348 (8)	0.0477 (11)	−0.0068 (7)	0.0140 (9)	0.0011 (8)
O10	0.0311 (7)	0.0316 (5)	0.0364 (7)	−0.0051 (5)	0.0014 (6)	0.0028 (5)
C11	0.0234 (10)	0.0458 (9)	0.0374 (10)	−0.0030 (7)	0.0024 (8)	−0.0089 (8)
C12	0.0296 (11)	0.0466 (9)	0.0353 (11)	0.0099 (7)	−0.0018 (9)	0.0010 (7)
O13	0.0367 (7)	0.0323 (5)	0.0357 (7)	0.0045 (5)	0.0073 (6)	0.0048 (5)
C14	0.0498 (13)	0.0336 (8)	0.0367 (11)	0.0045 (8)	−0.0015 (10)	0.0076 (7)
C15	0.0640 (15)	0.0364 (8)	0.0347 (11)	−0.0053 (9)	0.0095 (11)	0.0089 (8)
O16	0.0409 (8)	0.0424 (6)	0.0391 (8)	−0.0005 (5)	0.0183 (6)	0.0071 (5)
C17	0.0508 (13)	0.0345 (9)	0.0591 (14)	−0.0031 (8)	0.0334 (11)	0.0020 (8)
C18	0.0355 (12)	0.0381 (9)	0.0826 (17)	−0.0095 (8)	0.0296 (12)	−0.0089 (9)
P1	0.0243 (2)	0.02426 (17)	0.0248 (2)	0.00058 (17)	0.00502 (18)	0.00032 (17)
B1	0.0523 (15)	0.0358 (10)	0.0382 (13)	0.0136 (9)	0.0014 (11)	−0.0078 (9)
B2	0.0321 (11)	0.0401 (9)	0.0265 (10)	−0.0020 (9)	0.0056 (9)	0.0007 (8)
C20	0.0324 (11)	0.0456 (9)	0.0380 (11)	−0.0038 (8)	0.0096 (9)	0.0117 (8)
C21	0.0316 (12)	0.0801 (14)	0.0616 (15)	0.0022 (10)	0.0181 (11)	0.0203 (11)
C22	0.0453 (13)	0.0757 (13)	0.0495 (13)	−0.0046 (10)	0.0151 (11)	0.0272 (11)
C23	0.0486 (13)	0.0441 (10)	0.0678 (15)	−0.0224 (9)	0.0036 (11)	0.0097 (10)
C30	0.0293 (10)	0.0280 (7)	0.0324 (10)	0.0010 (7)	0.0022 (8)	−0.0015 (7)
C31	0.0435 (13)	0.0352 (9)	0.0577 (13)	0.0111 (8)	0.0016 (10)	−0.0060 (8)
C32	0.0263 (11)	0.0534 (10)	0.0545 (13)	−0.0025 (8)	0.0091 (9)	0.0065 (9)
C33	0.0348 (12)	0.0475 (9)	0.0390 (11)	0.0041 (8)	−0.0065 (9)	0.0002 (8)

Geometric parameters (Å, º)

K1—O16	2.7659 (12)	C15—H15B	0.9900
K1—O10	2.7671 (12)	O16—C17	1.408 (2)
K1—O4	2.8082 (12)	C17—C18	1.488 (3)
K1—O7	2.8170 (11)	C17—H17A	0.9900
K1—O13	2.8562 (12)	C17—H17B	0.9900
K1—O1	2.8860 (14)	C18—H18A	0.9900
K1—C22^i	3.4744 (19)	C18—H18B	0.9900
K1—C6	3.5345 (18)	P1—C20	1.8742 (18)
O1—C2	1.427 (2)	P1—C30	1.8741 (17)
O1—C18	1.429 (2)	P1—B1	1.9397 (18)
C2—C3	1.491 (3)	P1—B2	1.940 (2)
C2—H2A	0.9900	B1—H1A	0.9800
C2—H2B	0.9900	B1—H1B	0.9800
C3—O4	1.410 (2)	B1—H1C	0.9800
C3—H3A	0.9900	B2—H2C	0.9800
C3—H3B	0.9900	B2—H2D	0.9800
O4—C5	1.425 (2)	B2—H2E	0.9800
C5—C6	1.476 (3)	C20—C23	1.537 (3)
C5—H5A	0.9900	C20—C21	1.532 (3)
C5—H5B	0.9900	C20—C22	1.535 (3)
C6—O7	1.429 (2)	C21—H21A	0.9800
C6—H6A	0.9900	C21—H21B	0.9800
C6—H6B	0.9900	C21—H21C	0.9800
O7—C8	1.417 (2)	C22—K1^ii	3.4744 (19)
C8—C9	1.493 (3)	C22—H22A	0.9800
C8—H8A	0.9900	C22—H22B	0.9800
C8—H8B	0.9900	C22—H22C	0.9800
C9—O10	1.4190 (18)	C23—H23A	0.9800
C9—H9A	0.9900	C23—H23B	0.9800
C9—H9B	0.9900	C23—H23C	0.9800
O10—C11	1.420 (2)	C30—C31	1.532 (2)
C11—C12	1.493 (2)	C30—C32	1.533 (3)
C11—H11A	0.9900	C30—C33	1.535 (2)
C11—H11B	0.9900	C31—H31A	0.9800
C12—O13	1.416 (2)	C31—H31B	0.9800
C12—H12A	0.9900	C31—H31C	0.9800
C12—H12B	0.9900	C32—H32A	0.9800
O13—C14	1.4297 (18)	C32—H32B	0.9800
C14—C15	1.470 (3)	C32—H32C	0.9800
C14—H14A	0.9900	C33—H33A	0.9800
C14—H14B	0.9900	C33—H33B	0.9800
C15—O16	1.427 (2)	C33—H33C	0.9800
C15—H15A	0.9900
O16—K1—O10	119.38 (4)	O13—C14—H14A	110.0
O16—K1—O4	118.14 (4)	C15—C14—H14A	110.0
O10—K1—O4	120.94 (4)	O13—C14—H14B	110.0
O16—K1—O7	165.65 (4)	C15—C14—H14B	110.0
O10—K1—O7	60.42 (3)	H14A—C14—H14B	108.4
O4—K1—O7	60.55 (4)	O16—C15—C14	109.24 (16)
O16—K1—O13	60.15 (4)	O16—C15—H15A	109.8
O10—K1—O13	59.27 (3)	C14—C15—H15A	109.8
O4—K1—O13	165.82 (4)	O16—C15—H15B	109.8
O7—K1—O13	117.14 (3)	C14—C15—H15B	109.8
O16—K1—O1	59.80 (4)	H15A—C15—H15B	108.3
O10—K1—O1	160.26 (3)	C17—O16—C15	112.11 (16)
O4—K1—O1	58.93 (4)	C17—O16—K1	118.76 (10)
O7—K1—O1	114.92 (4)	C15—O16—K1	117.95 (10)
O13—K1—O1	115.45 (4)	O16—C17—C18	108.54 (17)
O16—K1—C22^i	88.39 (5)	O16—C17—H17A	110.0
O10—K1—C22^i	75.67 (5)	C18—C17—H17A	110.0
O4—K1—C22^i	93.81 (4)	O16—C17—H17B	110.0
O7—K1—C22^i	77.62 (5)	C18—C17—H17B	110.0
O13—K1—C22^i	72.29 (4)	H17A—C17—H17B	108.4
O1—K1—C22^i	84.60 (5)	O1—C18—C17	109.35 (14)
O16—K1—C6	159.90 (5)	O1—C18—H18A	109.8
O10—K1—C6	80.20 (4)	C17—C18—H18A	109.8
O4—K1—C6	41.76 (4)	O1—C18—H18B	109.8
O7—K1—C6	22.58 (4)	C17—C18—H18B	109.8
O13—K1—C6	138.92 (4)	H18A—C18—H18B	108.3
O1—K1—C6	100.30 (5)	C20—P1—C30	110.41 (7)
C22^i—K1—C6	92.71 (5)	C20—P1—B1	108.57 (10)
C2—O1—C18	112.70 (14)	C30—P1—B1	106.65 (9)
C2—O1—K1	112.08 (11)	C20—P1—B2	107.86 (9)
C18—O1—K1	109.66 (10)	C30—P1—B2	108.86 (9)
O1—C2—C3	108.98 (14)	B1—P1—B2	114.48 (9)
O1—C2—H2A	109.9	P1—B1—H1A	109.5
C3—C2—H2A	109.9	P1—B1—H1B	109.5
O1—C2—H2B	109.9	H1A—B1—H1B	109.5
C3—C2—H2B	109.9	P1—B1—H1C	109.5
H2A—C2—H2B	108.3	H1A—B1—H1C	109.5
O4—C3—C2	108.05 (14)	H1B—B1—H1C	109.5
O4—C3—H3A	110.1	P1—B2—H2C	109.5
C2—C3—H3A	110.1	P1—B2—H2D	109.5
O4—C3—H3B	110.1	H2C—B2—H2D	109.5
C2—C3—H3B	110.1	P1—B2—H2E	109.5
H3A—C3—H3B	108.4	H2C—B2—H2E	109.5
C3—O4—C5	111.71 (14)	H2D—B2—H2E	109.5
C3—O4—K1	118.41 (11)	C23—C20—C21	107.34 (16)
C5—O4—K1	115.91 (10)	C23—C20—C22	110.34 (15)
O4—C5—C6	108.95 (14)	C21—C20—C22	108.01 (18)
O4—C5—H5A	109.9	C23—C20—P1	111.60 (14)
C6—C5—H5A	109.9	C21—C20—P1	105.97 (12)
O4—C5—H5B	109.9	C22—C20—P1	113.24 (13)
C6—C5—H5B	109.9	C20—C21—H21A	109.5
H5A—C5—H5B	108.3	C20—C21—H21B	109.5
O7—C6—C5	108.80 (17)	H21A—C21—H21B	109.5
O7—C6—K1	49.21 (7)	C20—C21—H21C	109.5
C5—C6—K1	83.07 (11)	H21A—C21—H21C	109.5
O7—C6—H6A	109.9	H21B—C21—H21C	109.5
C5—C6—H6A	109.9	C20—C22—K1^ii	146.26 (13)
K1—C6—H6A	81.1	C20—C22—H22A	109.5
O7—C6—H6B	109.9	K1^ii—C22—H22A	103.1
C5—C6—H6B	109.9	C20—C22—H22B	109.5
K1—C6—H6B	159.0	K1^ii—C22—H22B	65.9
H6A—C6—H6B	108.3	H22A—C22—H22B	109.5
C8—O7—C6	112.15 (15)	C20—C22—H22C	109.5
C8—O7—K1	109.49 (9)	K1^ii—C22—H22C	49.4
C6—O7—K1	108.21 (9)	H22A—C22—H22C	109.5
O7—C8—C9	108.32 (16)	H22B—C22—H22C	109.5
O7—C8—H8A	110.0	C20—C23—H23A	109.5
C9—C8—H8A	110.0	C20—C23—H23B	109.5
O7—C8—H8B	110.0	H23A—C23—H23B	109.5
C9—C8—H8B	110.0	C20—C23—H23C	109.5
H8A—C8—H8B	108.4	H23A—C23—H23C	109.5
O10—C9—C8	107.39 (13)	H23B—C23—H23C	109.5
O10—C9—H9A	110.2	C31—C30—C32	107.27 (16)
C8—C9—H9A	110.2	C31—C30—C33	109.65 (14)
O10—C9—H9B	110.2	C32—C30—C33	108.07 (15)
C8—C9—H9B	110.2	C31—C30—P1	113.22 (11)
H9A—C9—H9B	108.5	C32—C30—P1	105.42 (11)
C11—O10—C9	113.92 (12)	C33—C30—P1	112.84 (13)
C11—O10—K1	119.78 (10)	C30—C31—H31A	109.5
C9—O10—K1	116.98 (9)	C30—C31—H31B	109.5
O10—C11—C12	107.42 (13)	H31A—C31—H31B	109.5
O10—C11—H11A	110.2	C30—C31—H31C	109.5
C12—C11—H11A	110.2	H31A—C31—H31C	109.5
O10—C11—H11B	110.2	H31B—C31—H31C	109.5
C12—C11—H11B	110.2	C30—C32—H32A	109.5
H11A—C11—H11B	108.5	C30—C32—H32B	109.5
O13—C12—C11	108.80 (13)	H32A—C32—H32B	109.5
O13—C12—H12A	109.9	C30—C32—H32C	109.5
C11—C12—H12A	109.9	H32A—C32—H32C	109.5
O13—C12—H12B	109.9	H32B—C32—H32C	109.5
C11—C12—H12B	109.9	C30—C33—H33A	109.5
H12A—C12—H12B	108.3	C30—C33—H33B	109.5
C12—O13—C14	111.19 (13)	H33A—C33—H33B	109.5
C12—O13—K1	110.24 (10)	C30—C33—H33C	109.5
C14—O13—K1	107.52 (9)	H33A—C33—H33C	109.5
O13—C14—C15	108.59 (14)	H33B—C33—H33C	109.5
O16—K1—O1—C2	−149.39 (11)	O1—K1—O10—C11	72.38 (15)
O10—K1—O1—C2	117.22 (13)	C22^i—K1—O10—C11	70.21 (11)
O4—K1—O1—C2	21.59 (10)	C6—K1—O10—C11	165.58 (11)
O7—K1—O1—C2	45.68 (11)	O16—K1—O10—C9	−154.23 (10)
O13—K1—O1—C2	−173.21 (10)	O4—K1—O10—C9	11.36 (12)
C22^i—K1—O1—C2	119.33 (11)	O7—K1—O10—C9	9.27 (10)
C6—K1—O1—C2	27.55 (10)	O13—K1—O10—C9	−152.11 (12)
O16—K1—O1—C18	−23.44 (11)	O1—K1—O10—C9	−72.27 (16)
O10—K1—O1—C18	−116.82 (13)	C22^i—K1—O10—C9	−74.44 (11)
O4—K1—O1—C18	147.54 (12)	C6—K1—O10—C9	20.93 (11)
O7—K1—O1—C18	171.63 (11)	C9—O10—C11—C12	−175.69 (15)
O13—K1—O1—C18	−47.26 (12)	K1—O10—C11—C12	38.65 (17)
C22^i—K1—O1—C18	−114.71 (12)	O10—C11—C12—O13	−64.99 (18)
C6—K1—O1—C18	153.51 (11)	C11—C12—O13—C14	177.92 (14)
C18—O1—C2—C3	−177.84 (16)	C11—C12—O13—K1	58.77 (14)
K1—O1—C2—C3	−53.56 (17)	O16—K1—O13—C12	151.03 (10)
O1—C2—C3—O4	65.71 (19)	O10—K1—O13—C12	−26.84 (9)
C2—C3—O4—C5	176.24 (14)	O4—K1—O13—C12	−121.94 (16)
C2—C3—O4—K1	−45.15 (17)	O7—K1—O13—C12	−45.02 (10)
O16—K1—O4—C3	22.22 (12)	O1—K1—O13—C12	174.76 (8)
O10—K1—O4—C3	−143.54 (10)	C22^i—K1—O13—C12	−110.39 (10)
O7—K1—O4—C3	−141.46 (12)	C6—K1—O13—C12	−37.31 (11)
O13—K1—O4—C3	−57.0 (2)	O16—K1—O13—C14	29.67 (11)
O1—K1—O4—C3	13.39 (10)	O10—K1—O13—C14	−148.20 (12)
C22^i—K1—O4—C3	−67.98 (11)	O4—K1—O13—C14	116.71 (16)
C6—K1—O4—C3	−157.78 (13)	O7—K1—O13—C14	−166.38 (11)
O16—K1—O4—C5	159.15 (12)	O1—K1—O13—C14	53.40 (11)
O10—K1—O4—C5	−6.62 (13)	C22^i—K1—O13—C14	128.26 (12)
O7—K1—O4—C5	−4.53 (12)	C6—K1—O13—C14	−158.66 (11)
O13—K1—O4—C5	80.0 (2)	C12—O13—C14—C15	177.39 (15)
O1—K1—O4—C5	150.31 (13)	K1—O13—C14—C15	−61.85 (15)
C22^i—K1—O4—C5	68.94 (13)	O13—C14—C15—O16	66.66 (18)
C6—K1—O4—C5	−20.86 (12)	C14—C15—O16—C17	−178.93 (13)
C3—O4—C5—C6	176.63 (15)	C14—C15—O16—K1	−35.46 (16)
K1—O4—C5—C6	36.91 (18)	O10—K1—O16—C17	146.44 (11)
O4—C5—C6—O7	−68.18 (17)	O4—K1—O16—C17	−19.55 (13)
O4—C5—C6—K1	−25.62 (13)	O7—K1—O16—C17	61.3 (2)
O16—K1—C6—O7	140.41 (11)	O13—K1—O16—C17	144.34 (13)
O10—K1—C6—O7	−27.24 (11)	O1—K1—O16—C17	−10.79 (11)
O4—K1—C6—O7	140.40 (14)	C22^i—K1—O16—C17	73.90 (12)
O13—K1—C6—O7	−18.12 (15)	C6—K1—O16—C17	−19.56 (19)
O1—K1—C6—O7	132.72 (11)	O10—K1—O16—C15	5.43 (13)
C22^i—K1—C6—O7	47.71 (12)	O4—K1—O16—C15	−160.57 (11)
O16—K1—C6—C5	18.16 (19)	O7—K1—O16—C15	−79.7 (2)
O10—K1—C6—C5	−149.49 (11)	O13—K1—O16—C15	3.33 (11)
O4—K1—C6—C5	18.15 (9)	O1—K1—O16—C15	−151.81 (13)
O7—K1—C6—C5	−122.25 (17)	C22^i—K1—O16—C15	−67.11 (12)
O13—K1—C6—C5	−140.38 (9)	C6—K1—O16—C15	−160.58 (13)
O1—K1—C6—C5	10.47 (11)	C15—O16—C17—C18	−174.26 (13)
C22^i—K1—C6—C5	−74.54 (11)	K1—O16—C17—C18	42.60 (16)
C5—C6—O7—C8	−176.65 (12)	C2—O1—C18—C17	−179.13 (15)
K1—C6—O7—C8	120.87 (12)	K1—O1—C18—C17	55.26 (17)
C5—C6—O7—K1	62.48 (14)	O16—C17—C18—O1	−66.22 (18)
O16—K1—O7—C8	119.55 (17)	C30—P1—C20—C23	−78.78 (14)
O10—K1—O7—C8	26.25 (10)	B1—P1—C20—C23	164.63 (13)
O4—K1—O7—C8	−151.69 (11)	B2—P1—C20—C23	40.06 (15)
O13—K1—O7—C8	44.21 (11)	C30—P1—C20—C21	164.68 (13)
O1—K1—O7—C8	−175.37 (10)	B1—P1—C20—C21	48.10 (15)
C22^i—K1—O7—C8	106.65 (11)	B2—P1—C20—C21	−76.48 (15)
C6—K1—O7—C8	−122.51 (16)	C30—P1—C20—C22	46.46 (17)
O16—K1—O7—C6	−117.94 (18)	B1—P1—C20—C22	−70.13 (16)
O10—K1—O7—C6	148.76 (12)	B2—P1—C20—C22	165.30 (15)
O4—K1—O7—C6	−29.18 (11)	C23—C20—C22—K1^ii	−15.4 (3)
O13—K1—O7—C6	166.72 (11)	C21—C20—C22—K1^ii	101.6 (3)
O1—K1—O7—C6	−52.85 (12)	P1—C20—C22—K1^ii	−141.35 (18)
C22^i—K1—O7—C6	−130.84 (12)	C20—P1—C30—C31	49.75 (16)
C6—O7—C8—C9	−179.69 (12)	B1—P1—C30—C31	167.53 (15)
K1—O7—C8—C9	−59.56 (13)	B2—P1—C30—C31	−68.47 (15)
O7—C8—C9—O10	68.61 (17)	C20—P1—C30—C32	166.72 (11)
C8—C9—O10—C11	171.58 (15)	B1—P1—C30—C32	−75.51 (14)
C8—C9—O10—K1	−41.74 (17)	B2—P1—C30—C32	48.50 (13)
O16—K1—O10—C11	−9.58 (11)	C20—P1—C30—C33	−75.55 (13)
O4—K1—O10—C11	156.01 (10)	B1—P1—C30—C33	42.22 (14)
O7—K1—O10—C11	153.92 (11)	B2—P1—C30—C33	166.23 (12)
O13—K1—O10—C11	−7.46 (10)

Symmetry codes: (i) −x+1/2, y+1/2, −z+3/2; (ii) −x+1/2, y−1/2, −z+3/2.