The solid-state structure of [{(C24H25)P(H)}Rb(C4H6N2)]2 or [Rb2(C24H26P)2(C4H6N2)2], a novel base adduct of tetrameric [DmpP(H)Rb]4 (Dmp = 2,6-dimesitylphenyl), is reported. It exhibits a dimeric centrosymmetric arrangement.
Supporting information
CCDC reference: 226668
Key indicators
- Single-crystal X-ray study
- T = 198 K
- Mean
(C-C) = 0.004 Å
- R factor = 0.038
- wR factor = 0.109
- Data-to-parameter ratio = 14.8
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.96
| Author Response: Parameter settings for data collection were less than
required for a hemisphere in two theta. Hence, data fraction at
50 degrees is two theta is 96 percent rather than 100 percent. The
data fraction at 55 degrees in two theta is 88 percent. The uniqueness of
this structure may warrant consideration for publication of this structue
eventhough the data collection is less than 100 percent.
|
Alert level C
PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings Differ .... ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio
PLAT764_ALERT_4_C Overcomplete CIF Bond list Detected (Rep/Expd) . 1.43 Ratio
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 21.00 Deg.
RB1 -P1 -H1A 2.666 1.555 1.555
1 ALERT level A = In general: serious problem
0 ALERT level B = Potentially serious problem
5 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
3 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
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
1 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: SMART (Bruker, 2001); cell refinement: SMART; data reduction: SAINT (Bruker, 2001); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.
Bis(µ-2,2'-4,4'-6,6'-hexamethyl-µ-terphenyl-2'-
phosphanido)bis[(
N-methylimidazole)rubidium(I)]
top
Crystal data top
[Rb2(C24H26P)2(C4H6N2)2] | Z = 1 |
Mr = 1026.00 | F(000) = 532 |
Triclinic, P1 | Dx = 1.306 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 8.6940 (3) Å | Cell parameters from 3500 reflections |
b = 12.3225 (4) Å | θ = 2.0–25.0° |
c = 13.6724 (5) Å | µ = 1.98 mm−1 |
α = 67.228 (1)° | T = 198 K |
β = 75.138 (1)° | Block, orange |
γ = 85.917 (1)° | 0.50 × 0.40 × 0.40 mm |
V = 1304.75 (8) Å3 | |
Data collection top
Siemens Bruker P4 1K CCD detector diffractometer | 4422 independent reflections |
Radiation source: fine-focus sealed tube | 3920 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.025 |
ω scans | θmax = 25.0°, θmin = 1.7° |
Absorption correction: multi-scan (SADABS; Bruker, 2001) | h = −9→10 |
Tmin = 0.393, Tmax = 0.454 | k = −14→14 |
7167 measured reflections | l = −14→16 |
Refinement top
Refinement on F2 | Primary atom site location: structure-invariant direct methods |
Least-squares matrix: full | Secondary atom site location: difference Fourier map |
R[F2 > 2σ(F2)] = 0.039 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.110 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.0741P)2 + 0.1125P] where P = (Fo2 + 2Fc2)/3 |
4422 reflections | (Δ/σ)max = 0.001 |
299 parameters | Δρmax = 0.91 e Å−3 |
0 restraints | Δρmin = −0.86 e Å−3 |
Special details top
Experimental. A crystal of approximately 0.40 x 0.40 x 0.50 mm3 on an edge was
handled under a nitrogen atomosphere and mounted on a glass fiber with
Paratone-N oil and then cooled to 198 K. The data were collected on a Siemens
Bruker 1 K P4/CCD diffractometer with Mo radiation (Bruker,2001). The strucure
was solved by direct methods and completed from subsequent difference Fourier
syntheses. Diffraction symmetry indiated a triclinic crystal system and the
solution successfully solved in P-1 space group. All non-hydrogen atoms were
refined with anisotropic thermal parameters. |
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 | x | y | z | Uiso*/Ueq | |
Rb1 | 0.74970 (3) | 0.55673 (2) | 0.28931 (2) | 0.03288 (12) | |
P1 | 0.42706 (9) | 0.65670 (6) | 0.41498 (7) | 0.0364 (2) | |
N1 | 0.5913 (3) | 0.4171 (2) | 0.2103 (2) | 0.0413 (6) | |
N2 | 0.4434 (3) | 0.2520 (2) | 0.2906 (2) | 0.0337 (5) | |
C1 | 0.5788 (3) | 0.7800 (2) | 0.1120 (2) | 0.0265 (6) | |
C2 | 0.7296 (3) | 0.7633 (2) | 0.0521 (2) | 0.0300 (6) | |
H2A | 0.7351 | 0.7392 | −0.0106 | 0.036* | |
C3 | 0.8683 (3) | 0.8042 (2) | 0.0600 (2) | 0.0298 (6) | |
C4 | 0.8552 (3) | 0.8605 (2) | 0.1333 (2) | 0.0305 (6) | |
H4A | 0.9536 | 0.8936 | 0.1380 | 0.037* | |
C5 | 0.7071 (3) | 0.8796 (2) | 0.1937 (2) | 0.0276 (6) | |
C6 | 0.5671 (3) | 0.8401 (2) | 0.1823 (2) | 0.0231 (5) | |
C7 | 0.4061 (3) | 0.8671 (2) | 0.2413 (2) | 0.0234 (5) | |
C8 | 0.3345 (3) | 0.9694 (2) | 0.1850 (2) | 0.0302 (6) | |
H8A | 0.3863 | 1.0176 | 0.1118 | 0.036* | |
C9 | 0.1872 (3) | 1.0014 (2) | 0.2353 (2) | 0.0337 (6) | |
H9A | 0.1387 | 1.0712 | 0.1974 | 0.040* | |
C10 | 0.1132 (3) | 0.9290 (2) | 0.3419 (2) | 0.0305 (6) | |
H10A | 0.0136 | 0.9507 | 0.3767 | 0.037* | |
C11 | 0.1804 (3) | 0.8258 (2) | 0.3991 (2) | 0.0242 (5) | |
C12 | 0.3304 (3) | 0.7907 (2) | 0.3493 (2) | 0.0230 (5) | |
C13 | 0.0925 (3) | 0.7529 (2) | 0.5145 (2) | 0.0236 (5) | |
C14 | 0.1240 (3) | 0.7697 (2) | 0.6036 (2) | 0.0249 (5) | |
C15 | 0.0430 (3) | 0.7007 (2) | 0.7101 (2) | 0.0299 (6) | |
H15A | 0.0655 | 0.7128 | 0.7696 | 0.036* | |
C16 | −0.0704 (3) | 0.6142 (2) | 0.7318 (2) | 0.0308 (6) | |
C17 | −0.1021 (3) | 0.5983 (2) | 0.6432 (2) | 0.0318 (6) | |
H17A | −0.1787 | 0.5397 | 0.6564 | 0.038* | |
C18 | −0.0238 (3) | 0.6665 (2) | 0.5356 (2) | 0.0275 (6) | |
C19 | 0.4302 (4) | 0.7330 (3) | 0.1009 (3) | 0.0421 (7) | |
H19A | 0.3533 | 0.7029 | 0.1725 | 0.063* | |
H19B | 0.4584 | 0.6692 | 0.0742 | 0.063* | |
H19C | 0.3828 | 0.7965 | 0.0490 | 0.063* | |
C20 | 1.0293 (4) | 0.7896 (3) | −0.0078 (3) | 0.0438 (8) | |
H20A | 1.0995 | 0.7502 | 0.0405 | 0.066* | |
H20B | 1.0758 | 0.8671 | −0.0593 | 0.066* | |
H20C | 1.0172 | 0.7419 | −0.0487 | 0.066* | |
C21 | 0.6980 (4) | 0.9425 (3) | 0.2701 (3) | 0.0401 (7) | |
H21A | 0.6319 | 0.8954 | 0.3427 | 0.060* | |
H21B | 0.6508 | 1.0195 | 0.2414 | 0.060* | |
H21C | 0.8053 | 0.9535 | 0.2759 | 0.060* | |
C22 | 0.2461 (3) | 0.8623 (2) | 0.5839 (3) | 0.0337 (6) | |
H22A | 0.3453 | 0.8527 | 0.5346 | 0.051* | |
H22B | 0.2667 | 0.8533 | 0.6538 | 0.051* | |
H22C | 0.2055 | 0.9408 | 0.5506 | 0.051* | |
C23 | −0.1578 (4) | 0.5403 (3) | 0.8484 (3) | 0.0494 (9) | |
H23A | −0.0986 | 0.5442 | 0.8992 | 0.074* | |
H23B | −0.1667 | 0.4583 | 0.8563 | 0.074* | |
H23C | −0.2645 | 0.5706 | 0.8652 | 0.074* | |
C24 | −0.0651 (4) | 0.6489 (3) | 0.4423 (3) | 0.0394 (7) | |
H24A | −0.1301 | 0.5763 | 0.4708 | 0.059* | |
H24B | 0.0329 | 0.6429 | 0.3901 | 0.059* | |
H24C | −0.1251 | 0.7159 | 0.4053 | 0.059* | |
C25 | 0.4988 (3) | 0.3453 (3) | 0.3020 (2) | 0.0361 (7) | |
H25A | 0.4736 | 0.3574 | 0.3688 | 0.043* | |
C26 | 0.5041 (4) | 0.2648 (3) | 0.1848 (3) | 0.0419 (7) | |
H26A | 0.4865 | 0.2135 | 0.1515 | 0.050* | |
C27 | 0.5949 (4) | 0.3656 (3) | 0.1360 (3) | 0.0464 (8) | |
H27A | 0.6527 | 0.3965 | 0.0614 | 0.056* | |
C28 | 0.3406 (4) | 0.1539 (3) | 0.3776 (3) | 0.0452 (8) | |
H28A | 0.3182 | 0.0984 | 0.3471 | 0.068* | |
H28B | 0.2404 | 0.1847 | 0.4075 | 0.068* | |
H28C | 0.3948 | 0.1134 | 0.4360 | 0.068* | |
H1A | 0.339 (4) | 0.614 (3) | 0.492 (3) | 0.053 (10)* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Rb1 | 0.03266 (18) | 0.03651 (18) | 0.03025 (18) | 0.00743 (11) | −0.00708 (12) | −0.01514 (13) |
P1 | 0.0366 (4) | 0.0297 (4) | 0.0310 (4) | 0.0136 (3) | −0.0047 (3) | −0.0035 (3) |
N1 | 0.0409 (15) | 0.0432 (14) | 0.0391 (15) | −0.0034 (11) | −0.0071 (12) | −0.0162 (12) |
N2 | 0.0333 (13) | 0.0329 (12) | 0.0309 (13) | 0.0016 (10) | −0.0066 (10) | −0.0089 (10) |
C1 | 0.0269 (14) | 0.0300 (13) | 0.0213 (13) | 0.0008 (10) | −0.0085 (11) | −0.0069 (11) |
C2 | 0.0372 (15) | 0.0338 (14) | 0.0174 (13) | 0.0059 (11) | −0.0051 (11) | −0.0101 (11) |
C3 | 0.0276 (14) | 0.0297 (14) | 0.0239 (14) | 0.0058 (10) | −0.0026 (11) | −0.0046 (11) |
C4 | 0.0227 (13) | 0.0306 (14) | 0.0334 (15) | −0.0007 (10) | −0.0050 (11) | −0.0081 (12) |
C5 | 0.0280 (14) | 0.0248 (13) | 0.0267 (14) | 0.0013 (10) | −0.0060 (11) | −0.0071 (11) |
C6 | 0.0236 (13) | 0.0219 (12) | 0.0179 (12) | 0.0009 (9) | −0.0026 (10) | −0.0028 (10) |
C7 | 0.0219 (13) | 0.0256 (12) | 0.0239 (13) | 0.0029 (10) | −0.0080 (10) | −0.0095 (11) |
C8 | 0.0304 (14) | 0.0287 (13) | 0.0247 (14) | 0.0013 (11) | −0.0054 (11) | −0.0038 (11) |
C9 | 0.0326 (15) | 0.0303 (14) | 0.0326 (16) | 0.0131 (11) | −0.0129 (13) | −0.0051 (12) |
C10 | 0.0257 (14) | 0.0321 (14) | 0.0344 (15) | 0.0092 (11) | −0.0079 (12) | −0.0146 (12) |
C11 | 0.0228 (12) | 0.0267 (13) | 0.0243 (13) | 0.0023 (10) | −0.0058 (10) | −0.0114 (11) |
C12 | 0.0243 (13) | 0.0240 (12) | 0.0215 (13) | 0.0033 (10) | −0.0066 (10) | −0.0094 (10) |
C13 | 0.0192 (12) | 0.0240 (12) | 0.0280 (14) | 0.0065 (9) | −0.0044 (10) | −0.0122 (11) |
C14 | 0.0231 (13) | 0.0251 (13) | 0.0266 (14) | 0.0043 (10) | −0.0042 (11) | −0.0120 (11) |
C15 | 0.0335 (15) | 0.0307 (14) | 0.0261 (14) | 0.0079 (11) | −0.0051 (12) | −0.0143 (12) |
C16 | 0.0297 (14) | 0.0261 (13) | 0.0274 (15) | 0.0071 (11) | 0.0011 (12) | −0.0067 (11) |
C17 | 0.0239 (13) | 0.0229 (13) | 0.0434 (17) | 0.0027 (10) | −0.0026 (12) | −0.0112 (12) |
C18 | 0.0235 (13) | 0.0272 (13) | 0.0345 (15) | 0.0050 (10) | −0.0061 (11) | −0.0160 (12) |
C19 | 0.0349 (16) | 0.059 (2) | 0.0409 (18) | −0.0063 (14) | −0.0084 (14) | −0.0274 (16) |
C20 | 0.0314 (16) | 0.0532 (19) | 0.0383 (18) | 0.0101 (14) | −0.0024 (14) | −0.0141 (15) |
C21 | 0.0350 (16) | 0.0448 (17) | 0.053 (2) | 0.0026 (13) | −0.0141 (15) | −0.0302 (16) |
C22 | 0.0355 (15) | 0.0329 (14) | 0.0378 (16) | −0.0009 (12) | −0.0105 (13) | −0.0176 (13) |
C23 | 0.053 (2) | 0.0425 (18) | 0.0340 (18) | −0.0021 (15) | 0.0043 (15) | −0.0037 (15) |
C24 | 0.0439 (17) | 0.0381 (16) | 0.0424 (18) | −0.0021 (13) | −0.0152 (14) | −0.0188 (14) |
C25 | 0.0354 (16) | 0.0430 (16) | 0.0322 (16) | −0.0003 (13) | −0.0070 (13) | −0.0174 (13) |
C26 | 0.0509 (19) | 0.0427 (17) | 0.0365 (17) | 0.0006 (14) | −0.0100 (15) | −0.0203 (14) |
C27 | 0.054 (2) | 0.0489 (19) | 0.0286 (17) | −0.0057 (15) | 0.0024 (15) | −0.0133 (14) |
C28 | 0.0395 (17) | 0.0378 (16) | 0.047 (2) | −0.0034 (13) | −0.0037 (15) | −0.0083 (15) |
Geometric parameters (Å, º) top
Rb1—N1 | 2.927 (3) | C11—C12 | 1.429 (4) |
Rb1—C2 | 3.297 (3) | C11—C13 | 1.504 (4) |
Rb1—P1 | 3.3185 (8) | C13—C14 | 1.406 (4) |
Rb1—C16i | 3.393 (3) | C13—C18 | 1.416 (3) |
Rb1—C3 | 3.403 (3) | C14—C15 | 1.393 (4) |
Rb1—C1 | 3.429 (3) | C14—C22 | 1.513 (3) |
Rb1—C25 | 3.441 (3) | C15—C16 | 1.397 (4) |
Rb1—C24ii | 3.476 (3) | C15—Rb1i | 3.533 (3) |
Rb1—C15i | 3.533 (3) | C15—H15A | 0.9500 |
Rb1—C4 | 3.565 (3) | C16—C17 | 1.394 (4) |
Rb1—C17i | 3.625 (3) | C16—C23 | 1.518 (4) |
Rb1—C6 | 3.647 (2) | C16—Rb1i | 3.393 (3) |
Rb1—C5 | 3.700 (3) | C17—C18 | 1.395 (4) |
P1—C12 | 1.811 (3) | C17—Rb1i | 3.625 (3) |
P1—Rb1i | 3.8448 (8) | C17—H17A | 0.9500 |
P1—H1A | 1.09 (4) | C18—C24 | 1.504 (4) |
N1—C25 | 1.315 (4) | C19—H19A | 0.9800 |
N1—C27 | 1.383 (4) | C19—H19B | 0.9800 |
N2—C25 | 1.354 (4) | C19—H19C | 0.9800 |
N2—C26 | 1.356 (4) | C20—H20A | 0.9800 |
N2—C28 | 1.473 (4) | C20—H20B | 0.9800 |
C1—C6 | 1.404 (4) | C20—H20C | 0.9800 |
C1—C2 | 1.405 (4) | C21—H21A | 0.9800 |
C1—C19 | 1.517 (4) | C21—H21B | 0.9800 |
C2—C3 | 1.384 (4) | C21—H21C | 0.9800 |
C2—H2A | 1.0000 | C22—H22A | 0.9800 |
C3—C4 | 1.403 (4) | C22—H22B | 0.9800 |
C3—C20 | 1.510 (4) | C22—H22C | 0.9800 |
C4—C5 | 1.399 (4) | C23—H23A | 0.9800 |
C4—H4A | 1.0000 | C23—H23B | 0.9800 |
C5—C6 | 1.408 (4) | C23—H23C | 0.9800 |
C5—C21 | 1.508 (4) | C24—H24A | 0.9800 |
C6—C7 | 1.511 (3) | C24—H24B | 0.9800 |
C7—C8 | 1.397 (4) | C24—H24C | 0.9800 |
C7—C12 | 1.419 (4) | C25—H25A | 0.9500 |
C8—C9 | 1.398 (4) | C26—C27 | 1.356 (4) |
C8—H8A | 0.9500 | C26—H26A | 0.9500 |
C9—C10 | 1.388 (4) | C27—H27A | 0.9500 |
C9—H9A | 0.9500 | C28—H28A | 0.9800 |
C10—C11 | 1.389 (4) | C28—H28B | 0.9800 |
C10—H10A | 0.9500 | C28—H28C | 0.9800 |
| | | |
N1—Rb1—C2 | 81.50 (7) | C7—C6—Rb1 | 121.97 (15) |
N1—Rb1—P1 | 98.17 (6) | C8—C7—C12 | 121.5 (2) |
C2—Rb1—P1 | 90.35 (5) | C8—C7—C6 | 117.4 (2) |
N1—Rb1—C16i | 87.90 (7) | C12—C7—C6 | 121.1 (2) |
C2—Rb1—C16i | 112.77 (7) | C7—C8—C9 | 120.5 (2) |
P1—Rb1—C16i | 156.77 (5) | C7—C8—H8A | 119.7 |
N1—Rb1—C3 | 102.00 (7) | C9—C8—H8A | 119.7 |
C2—Rb1—C3 | 23.77 (7) | C10—C9—C8 | 118.7 (2) |
P1—Rb1—C3 | 99.16 (5) | C10—C9—H9A | 120.7 |
C16i—Rb1—C3 | 101.48 (6) | C8—C9—H9A | 120.7 |
N1—Rb1—C1 | 80.97 (7) | C9—C10—C11 | 122.0 (2) |
C2—Rb1—C1 | 24.02 (7) | C9—C10—H10A | 119.0 |
P1—Rb1—C1 | 66.83 (5) | C11—C10—H10A | 119.0 |
C16i—Rb1—C1 | 136.40 (7) | C10—C11—C12 | 120.5 (2) |
C3—Rb1—C1 | 41.85 (6) | C10—C11—C13 | 118.5 (2) |
N1—Rb1—C25 | 21.98 (7) | C12—C11—C13 | 121.0 (2) |
C2—Rb1—C25 | 99.79 (7) | C7—C12—C11 | 116.7 (2) |
P1—Rb1—C25 | 85.98 (5) | C7—C12—P1 | 118.96 (18) |
C16i—Rb1—C25 | 91.96 (7) | C11—C12—P1 | 124.30 (19) |
C3—Rb1—C25 | 122.18 (7) | C14—C13—C18 | 118.7 (2) |
C1—Rb1—C25 | 92.82 (7) | C14—C13—C11 | 120.5 (2) |
N1—Rb1—C24ii | 164.28 (7) | C18—C13—C11 | 120.8 (2) |
C2—Rb1—C24ii | 114.19 (7) | C15—C14—C13 | 119.9 (2) |
P1—Rb1—C24ii | 83.28 (6) | C15—C14—C22 | 120.0 (2) |
C16i—Rb1—C24ii | 85.02 (8) | C13—C14—C22 | 120.1 (2) |
C3—Rb1—C24ii | 93.17 (7) | C14—C15—C16 | 121.7 (3) |
C1—Rb1—C24ii | 113.65 (7) | C14—C15—Rb1i | 94.31 (15) |
C25—Rb1—C24ii | 144.29 (7) | C16—C15—Rb1i | 72.80 (15) |
N1—Rb1—C15i | 67.97 (7) | C14—C15—H15A | 119.1 |
C2—Rb1—C15i | 118.51 (7) | C16—C15—H15A | 119.1 |
P1—Rb1—C15i | 143.91 (5) | Rb1i—C15—H15A | 103.1 |
C16i—Rb1—C15i | 23.15 (7) | C17—C16—C15 | 118.2 (2) |
C3—Rb1—C15i | 116.00 (6) | C17—C16—C23 | 120.9 (3) |
C1—Rb1—C15i | 137.10 (7) | C15—C16—C23 | 120.9 (3) |
C25—Rb1—C15i | 69.05 (7) | C17—C16—Rb1i | 88.07 (16) |
C24ii—Rb1—C15i | 101.73 (7) | C15—C16—Rb1i | 84.05 (16) |
N1—Rb1—C4 | 121.98 (7) | C23—C16—Rb1i | 98.13 (18) |
C2—Rb1—C4 | 40.48 (7) | C16—C17—C18 | 121.4 (2) |
P1—Rb1—C4 | 84.57 (5) | C16—C17—Rb1i | 69.33 (15) |
C16i—Rb1—C4 | 111.23 (6) | C18—C17—Rb1i | 94.48 (16) |
C3—Rb1—C4 | 23.08 (7) | C16—C17—H17A | 119.3 |
C1—Rb1—C4 | 46.92 (6) | C18—C17—H17A | 119.3 |
C25—Rb1—C4 | 138.87 (7) | Rb1i—C17—H17A | 106.3 |
C24ii—Rb1—C4 | 73.73 (7) | C17—C18—C13 | 120.0 (3) |
C15i—Rb1—C4 | 131.34 (6) | C17—C18—C24 | 119.7 (2) |
N1—Rb1—C17i | 107.03 (7) | C13—C18—C24 | 120.3 (2) |
C2—Rb1—C17i | 126.43 (7) | C1—C19—H19A | 109.5 |
P1—Rb1—C17i | 137.40 (5) | C1—C19—H19B | 109.5 |
C16i—Rb1—C17i | 22.61 (7) | H19A—C19—H19B | 109.5 |
C3—Rb1—C17i | 108.18 (6) | C1—C19—H19C | 109.5 |
C1—Rb1—C17i | 149.65 (6) | H19A—C19—H19C | 109.5 |
C25—Rb1—C17i | 105.13 (7) | H19B—C19—H19C | 109.5 |
C24ii—Rb1—C17i | 63.58 (7) | C3—C20—H20A | 109.5 |
C15i—Rb1—C17i | 39.06 (6) | C3—C20—H20B | 109.5 |
C4—Rb1—C17i | 108.80 (6) | H20A—C20—H20B | 109.5 |
N1—Rb1—C6 | 100.37 (7) | C3—C20—H20C | 109.5 |
C2—Rb1—C6 | 40.51 (6) | H20A—C20—H20C | 109.5 |
P1—Rb1—C6 | 52.41 (4) | H20B—C20—H20C | 109.5 |
C16i—Rb1—C6 | 148.52 (6) | C5—C21—H21A | 109.5 |
C3—Rb1—C6 | 47.18 (6) | C5—C21—H21B | 109.5 |
C1—Rb1—C6 | 22.63 (6) | H21A—C21—H21B | 109.5 |
C25—Rb1—C6 | 107.05 (6) | C5—C21—H21C | 109.5 |
C24ii—Rb1—C6 | 92.94 (7) | H21A—C21—H21C | 109.5 |
C15i—Rb1—C6 | 158.81 (6) | H21B—C21—H21C | 109.5 |
C4—Rb1—C6 | 39.28 (6) | C14—C22—H22A | 109.5 |
C17i—Rb1—C6 | 147.13 (6) | C14—C22—H22B | 109.5 |
C12—P1—Rb1 | 124.35 (9) | H22A—C22—H22B | 109.5 |
C12—P1—Rb1i | 122.32 (9) | C14—C22—H22C | 109.5 |
Rb1—P1—Rb1i | 113.08 (2) | H22A—C22—H22C | 109.5 |
C12—P1—H1A | 102.3 (19) | H22B—C22—H22C | 109.5 |
Rb1—P1—H1A | 131.8 (19) | C16—C23—H23A | 109.5 |
Rb1i—P1—H1A | 21.0 (19) | C16—C23—H23B | 109.5 |
C25—N1—C27 | 104.1 (2) | H23A—C23—H23B | 109.5 |
C25—N1—Rb1 | 101.61 (19) | C16—C23—H23C | 109.5 |
C27—N1—Rb1 | 149.7 (2) | H23A—C23—H23C | 109.5 |
C25—N2—C26 | 106.9 (2) | H23B—C23—H23C | 109.5 |
C25—N2—C28 | 126.3 (3) | C18—C24—H24A | 109.5 |
C26—N2—C28 | 126.8 (3) | C18—C24—H24B | 109.5 |
C6—C1—C2 | 119.4 (2) | H24A—C24—H24B | 109.5 |
C6—C1—C19 | 120.5 (2) | C18—C24—H24C | 109.5 |
C2—C1—C19 | 120.1 (3) | H24A—C24—H24C | 109.5 |
C6—C1—Rb1 | 87.46 (15) | H24B—C24—H24C | 109.5 |
C2—C1—Rb1 | 72.72 (15) | N1—C25—N2 | 112.3 (3) |
C19—C1—Rb1 | 109.60 (18) | N1—C25—Rb1 | 56.41 (15) |
C3—C2—C1 | 122.1 (3) | N2—C25—Rb1 | 162.0 (2) |
C3—C2—Rb1 | 82.43 (16) | N1—C25—H25A | 123.8 |
C1—C2—Rb1 | 83.26 (15) | N2—C25—H25A | 123.8 |
C3—C2—H2A | 118.1 | Rb1—C25—H25A | 69.1 |
C1—C2—H2A | 118.1 | C27—C26—N2 | 106.2 (3) |
Rb1—C2—H2A | 118.1 | C27—C26—H26A | 126.9 |
C2—C3—C4 | 117.9 (2) | N2—C26—H26A | 126.9 |
C2—C3—C20 | 121.6 (3) | C26—C27—N1 | 110.4 (3) |
C4—C3—C20 | 120.5 (3) | C26—C27—H27A | 124.8 |
C2—C3—Rb1 | 73.80 (15) | N1—C27—H27A | 124.8 |
C4—C3—Rb1 | 84.95 (16) | N2—C28—H28A | 109.5 |
C20—C3—Rb1 | 111.04 (18) | N2—C28—H28B | 109.5 |
C5—C4—C3 | 121.7 (2) | H28A—C28—H28B | 109.5 |
C5—C4—Rb1 | 84.41 (15) | N2—C28—H28C | 109.5 |
C3—C4—Rb1 | 71.98 (15) | H28A—C28—H28C | 109.5 |
C5—C4—H4A | 119.1 | H28B—C28—H28C | 109.5 |
C3—C4—H4A | 119.1 | C5—Rb1—C1 | 39.59 (6) |
Rb1—C4—H4A | 119.1 | C5—Rb1—C2 | 46.47 (7) |
C4—C5—C6 | 119.6 (2) | C5—Rb1—C3 | 40.01 (6) |
C4—C5—C21 | 120.0 (2) | C5—Rb1—C4 | 22.10 (6) |
C6—C5—C21 | 120.4 (2) | C5—Rb1—C6 | 22.08 (6) |
C4—C5—Rb1 | 73.49 (15) | C5—Rb1—P1 | 62.51 (4) |
C6—C5—Rb1 | 76.83 (14) | C5—Rb1—N1 | 120.51 (7) |
C21—C5—Rb1 | 120.67 (18) | C5—Rb1—C25 | 129.12 (7) |
C1—C6—C5 | 119.3 (2) | C5—Rb1—C15i | 153.43 (6) |
C1—C6—C7 | 120.5 (2) | C5—Rb1—C16i | 132.47 (6) |
C5—C6—C7 | 120.1 (2) | C5—Rb1—C17i | 125.31 (6) |
C1—C6—Rb1 | 69.92 (15) | P1—Rb1—P1i | 66.92 (2) |
C5—C6—Rb1 | 81.09 (15) | | |
Symmetry codes: (i) −x+1, −y+1, −z+1; (ii) x+1, y, z. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
P1—H1A···Rb1i | 1.09 (4) | 2.85 (4) | 3.8448 (8) | 151 (3) |
Symmetry code: (i) −x+1, −y+1, −z+1. |