The title complex salt, trans-anti-[CrBr2(Me2tn)2]ClO4 (where Me2tn = 2,2-dimethylpropane-1,3-diamine, C5H14N2), was prepared and its structure determined by single-crystal X-ray diffraction at 100 K. The asymmetric unit contains three conformationally similar complex cations and three perchlorate anions. In each complex cation, the CrIII centre is coordinated by four N atoms of two chelating Me2tn ligands in the equatorial plane and by two Br atoms in a trans-axial arrangement, to give a distorted octahedral geometry. Interionic contacts are dominated by extensive hydrogen bonding, involving the NH groups of the Me2tn ligand as donors and the anion O atoms or coordinated Br atoms as acceptors, resulting in two-dimensional layers in the bc plane. Ligand field analysis based on the angular overlap model, and IR and electronic spectroscopic properties, are also discussed.
Supporting information
CCDC reference: 1055916
Data collection: PAL ADSC Quantum-210 ADX (Arvai & Nielsen, 1983); cell refinement: HKL3000sm (Otwinowski & Minor, 1997); data reduction: HKL3000sm (Otwinowski & Minor, 1997); program(s) used to solve structure: SHELXS2013 (Sheldrick, 2015); program(s) used to refine structure: SHELXL2014/7 (Sheldrick, 2015); molecular graphics: DIAMOND (Brandenburg, 2014); software used to prepare material for publication: publCIF (Westrip, 2010) and PLATON (Spek, 2009).
trans-dibromidobis(2,2-dimethylpropane-1,3-diamine-
κ22N,N')chromium(III)
perchlorate
top
Crystal data top
[CrBr2(C5H14N2)2]ClO4 | Dx = 1.799 Mg m−3 |
Mr = 515.63 | Synchrotron radiation, λ = 0.62998 Å |
Orthorhombic, Pbca | Cell parameters from 352345 reflections |
a = 20.656 (4) Å | θ = 0.4–33.6° |
b = 17.666 (4) Å | µ = 3.60 mm−1 |
c = 31.305 (6) Å | T = 100 K |
V = 11423 (4) Å3 | Plate, green |
Z = 24 | 0.12 × 0.10 × 0.05 mm |
F(000) = 6216 | |
Data collection top
ADSC Q210 CCD area-detector diffractometer | 13691 reflections with I > 2σ(I) |
Radiation source: PLSII 2D bending magnet | Rint = 0.036 |
ω scans | θmax = 26.0°, θmin = 1.8° |
Absorption correction: empirical (using intensity measurements) (HKL3000sm SCALEPACK; Otwinowski & Minor, 1997) | h = −28→28 |
Tmin = 0.670, Tmax = 0.841 | k = −23→23 |
115348 measured reflections | l = −43→43 |
15666 independent reflections | |
Refinement top
Refinement on F2 | Hydrogen site location: inferred from neighbouring sites |
Least-squares matrix: full | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.031 | w = 1/[σ2(Fo2) + (0.0577P)2 + 5.702P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.086 | (Δ/σ)max = 0.003 |
S = 1.04 | Δρmax = 1.25 e Å−3 |
15666 reflections | Δρmin = −1.42 e Å−3 |
636 parameters | Extinction correction: SHELXL2014/7 (Sheldrick, 2015), Fc*=kFc[1+0.001xFc2λ3/sin(2θ)]-1/4 |
6 restraints | Extinction coefficient: 0.00083 (5) |
Crystal data top
[CrBr2(C5H14N2)2]ClO4 | V = 11423 (4) Å3 |
Mr = 515.63 | Z = 24 |
Orthorhombic, Pbca | Synchrotron radiation, λ = 0.62998 Å |
a = 20.656 (4) Å | µ = 3.60 mm−1 |
b = 17.666 (4) Å | T = 100 K |
c = 31.305 (6) Å | 0.12 × 0.10 × 0.05 mm |
Data collection top
ADSC Q210 CCD area-detector diffractometer | 15666 independent reflections |
Absorption correction: empirical (using intensity measurements) (HKL3000sm SCALEPACK; Otwinowski & Minor, 1997) | 13691 reflections with I > 2σ(I) |
Tmin = 0.670, Tmax = 0.841 | Rint = 0.036 |
115348 measured reflections | |
Refinement top
R[F2 > 2σ(F2)] = 0.031 | 6 restraints |
wR(F2) = 0.086 | H-atom parameters constrained |
S = 1.04 | Δρmax = 1.25 e Å−3 |
15666 reflections | Δρmin = −1.42 e Å−3 |
636 parameters | |
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. |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cr1A | 0.73021 (2) | 0.60628 (2) | 0.61679 (2) | 0.01368 (7) | |
Br1A | 0.69990 (2) | 0.61566 (2) | 0.69298 (2) | 0.02048 (5) | |
Br2A | 0.76227 (2) | 0.60157 (2) | 0.54027 (2) | 0.02102 (5) | |
N1A | 0.76335 (9) | 0.71878 (10) | 0.61996 (5) | 0.0179 (3) | |
H1A1 | 0.7377 | 0.7468 | 0.6024 | 0.022* | |
H1A2 | 0.7561 | 0.7354 | 0.6470 | 0.022* | |
N2A | 0.82196 (9) | 0.56954 (11) | 0.63681 (6) | 0.0235 (4) | |
H2A1 | 0.8222 | 0.5710 | 0.6659 | 0.028* | |
H2A2 | 0.8257 | 0.5200 | 0.6292 | 0.028* | |
N3A | 0.63830 (8) | 0.64035 (9) | 0.59742 (5) | 0.0171 (3) | |
H3A1 | 0.6349 | 0.6907 | 0.6031 | 0.021* | |
H3A2 | 0.6365 | 0.6351 | 0.5685 | 0.021* | |
N4A | 0.69737 (8) | 0.49462 (9) | 0.61381 (5) | 0.0164 (3) | |
H4A1 | 0.7004 | 0.4795 | 0.5861 | 0.020* | |
H4A2 | 0.7257 | 0.4658 | 0.6290 | 0.020* | |
C1A | 0.83200 (11) | 0.73755 (13) | 0.60917 (7) | 0.0242 (4) | |
H1A3 | 0.8391 | 0.7920 | 0.6150 | 0.029* | |
H1A4 | 0.8382 | 0.7296 | 0.5781 | 0.029* | |
C2A | 0.88357 (11) | 0.69270 (13) | 0.63286 (7) | 0.0226 (4) | |
C3A | 0.88151 (11) | 0.60849 (14) | 0.62206 (8) | 0.0259 (5) | |
H3A3 | 0.8851 | 0.6025 | 0.5907 | 0.031* | |
H3A4 | 0.9195 | 0.5835 | 0.6352 | 0.031* | |
C4A | 0.88047 (14) | 0.70619 (16) | 0.68088 (8) | 0.0351 (6) | |
H4A3 | 0.8383 | 0.6898 | 0.6917 | 0.053* | |
H4A4 | 0.8863 | 0.7602 | 0.6868 | 0.053* | |
H4A5 | 0.9148 | 0.6773 | 0.6950 | 0.053* | |
C5A | 0.94937 (13) | 0.72192 (17) | 0.61612 (9) | 0.0384 (6) | |
H5A1 | 0.9527 | 0.7765 | 0.6214 | 0.058* | |
H5A2 | 0.9526 | 0.7121 | 0.5854 | 0.058* | |
H5A3 | 0.9846 | 0.6957 | 0.6310 | 0.058* | |
C6A | 0.57964 (10) | 0.60288 (11) | 0.61545 (7) | 0.0184 (4) | |
H6A1 | 0.5407 | 0.6274 | 0.6033 | 0.022* | |
H6A2 | 0.5789 | 0.6112 | 0.6467 | 0.022* | |
C7A | 0.57586 (10) | 0.51758 (11) | 0.60673 (6) | 0.0163 (3) | |
C8A | 0.63097 (10) | 0.47504 (11) | 0.62882 (6) | 0.0172 (4) | |
H8A1 | 0.6284 | 0.4851 | 0.6599 | 0.021* | |
H8A2 | 0.6242 | 0.4201 | 0.6246 | 0.021* | |
C9A | 0.51254 (10) | 0.48940 (13) | 0.62657 (7) | 0.0225 (4) | |
H9A1 | 0.5116 | 0.5026 | 0.6570 | 0.034* | |
H9A2 | 0.5097 | 0.4343 | 0.6234 | 0.034* | |
H9A3 | 0.4758 | 0.5133 | 0.6120 | 0.034* | |
C10A | 0.57512 (11) | 0.50025 (12) | 0.55865 (6) | 0.0215 (4) | |
H10A | 0.5388 | 0.5268 | 0.5452 | 0.032* | |
H10B | 0.5703 | 0.4456 | 0.5543 | 0.032* | |
H10C | 0.6158 | 0.5173 | 0.5458 | 0.032* | |
Cr2B | 0.74038 (2) | 0.35435 (2) | 0.45410 (2) | 0.01221 (6) | |
Br1B | 0.71078 (2) | 0.36587 (2) | 0.53011 (2) | 0.01848 (5) | |
Br2B | 0.77134 (2) | 0.34418 (2) | 0.37785 (2) | 0.01968 (5) | |
N1B | 0.77384 (8) | 0.46610 (10) | 0.45463 (5) | 0.0171 (3) | |
H1B1 | 0.7475 | 0.4935 | 0.4372 | 0.021* | |
H1B2 | 0.7683 | 0.4844 | 0.4816 | 0.021* | |
N2B | 0.83098 (8) | 0.31690 (10) | 0.47411 (6) | 0.0183 (3) | |
H2B1 | 0.8318 | 0.3203 | 0.5031 | 0.022* | |
H2B2 | 0.8337 | 0.2668 | 0.4675 | 0.022* | |
N3B | 0.64815 (8) | 0.39030 (10) | 0.43512 (6) | 0.0177 (3) | |
H3B1 | 0.6448 | 0.4404 | 0.4416 | 0.021* | |
H3B2 | 0.6462 | 0.3863 | 0.4062 | 0.021* | |
N4B | 0.70788 (8) | 0.24197 (9) | 0.45332 (5) | 0.0161 (3) | |
H4B1 | 0.7123 | 0.2246 | 0.4261 | 0.019* | |
H4B2 | 0.7354 | 0.2145 | 0.4699 | 0.019* | |
C1B | 0.84187 (10) | 0.48221 (12) | 0.44183 (6) | 0.0200 (4) | |
H1B3 | 0.8500 | 0.5371 | 0.4455 | 0.024* | |
H1B4 | 0.8467 | 0.4705 | 0.4111 | 0.024* | |
C2B | 0.89352 (10) | 0.43872 (12) | 0.46642 (6) | 0.0190 (4) | |
C3B | 0.89071 (10) | 0.35377 (13) | 0.45785 (7) | 0.0215 (4) | |
H3B3 | 0.8937 | 0.3452 | 0.4267 | 0.026* | |
H3B4 | 0.9287 | 0.3294 | 0.4713 | 0.026* | |
C4B | 0.88902 (10) | 0.45569 (13) | 0.51443 (6) | 0.0222 (4) | |
H4B3 | 0.8943 | 0.5102 | 0.5192 | 0.033* | |
H4B4 | 0.9233 | 0.4282 | 0.5296 | 0.033* | |
H4B5 | 0.8467 | 0.4395 | 0.5252 | 0.033* | |
C5B | 0.95930 (11) | 0.46563 (15) | 0.44929 (7) | 0.0294 (5) | |
H5B1 | 0.9620 | 0.4549 | 0.4186 | 0.044* | |
H5B2 | 0.9941 | 0.4389 | 0.4643 | 0.044* | |
H5B3 | 0.9637 | 0.5202 | 0.4541 | 0.044* | |
C6B | 0.58999 (10) | 0.35189 (12) | 0.45285 (7) | 0.0193 (4) | |
H6B1 | 0.5509 | 0.3759 | 0.4406 | 0.023* | |
H6B2 | 0.5889 | 0.3601 | 0.4841 | 0.023* | |
C7B | 0.58704 (10) | 0.26653 (12) | 0.44415 (7) | 0.0193 (4) | |
C8B | 0.64089 (10) | 0.22375 (12) | 0.46736 (7) | 0.0188 (4) | |
H8B1 | 0.6374 | 0.2346 | 0.4983 | 0.023* | |
H8B2 | 0.6337 | 0.1688 | 0.4634 | 0.023* | |
C9B | 0.52314 (11) | 0.23787 (15) | 0.46299 (8) | 0.0308 (5) | |
H9B1 | 0.5196 | 0.1832 | 0.4583 | 0.046* | |
H9B2 | 0.4869 | 0.2636 | 0.4490 | 0.046* | |
H9B3 | 0.5221 | 0.2485 | 0.4937 | 0.046* | |
C10B | 0.58856 (11) | 0.25022 (14) | 0.39600 (7) | 0.0270 (5) | |
H10D | 0.6303 | 0.2663 | 0.3842 | 0.040* | |
H10E | 0.5536 | 0.2781 | 0.3819 | 0.040* | |
H10F | 0.5828 | 0.1958 | 0.3912 | 0.040* | |
Cr3C | 0.77123 (2) | 0.60947 (2) | 0.28850 (2) | 0.01335 (7) | |
Br1C | 0.77231 (2) | 0.60241 (2) | 0.36740 (2) | 0.02133 (5) | |
Br2C | 0.77070 (2) | 0.61867 (2) | 0.20966 (2) | 0.02258 (5) | |
N1C | 0.80290 (9) | 0.49676 (10) | 0.28534 (5) | 0.0184 (3) | |
H1C1 | 0.7714 | 0.4678 | 0.2974 | 0.022* | |
H1C2 | 0.8045 | 0.4840 | 0.2572 | 0.022* | |
N2C | 0.86765 (9) | 0.64642 (10) | 0.28850 (6) | 0.0218 (4) | |
H2C1 | 0.8793 | 0.6535 | 0.2608 | 0.026* | |
H2C2 | 0.8683 | 0.6928 | 0.3012 | 0.026* | |
N3C | 0.73779 (9) | 0.72025 (10) | 0.29261 (5) | 0.0191 (3) | |
H3C1 | 0.7340 | 0.7315 | 0.3209 | 0.023* | |
H3C2 | 0.7695 | 0.7507 | 0.2820 | 0.023* | |
N4C | 0.67622 (9) | 0.57112 (11) | 0.28831 (6) | 0.0224 (4) | |
H4C1 | 0.6764 | 0.5245 | 0.2759 | 0.027* | |
H4C2 | 0.6645 | 0.5643 | 0.3161 | 0.027* | |
C1C | 0.86550 (11) | 0.47276 (12) | 0.30467 (7) | 0.0216 (4) | |
H1C3 | 0.8736 | 0.4193 | 0.2968 | 0.026* | |
H1C4 | 0.8612 | 0.4749 | 0.3361 | 0.026* | |
C2C | 0.92458 (10) | 0.51994 (13) | 0.29155 (6) | 0.0204 (4) | |
C3C | 0.91985 (11) | 0.60027 (13) | 0.30895 (7) | 0.0250 (4) | |
H3C3 | 0.9117 | 0.5979 | 0.3401 | 0.030* | |
H3C4 | 0.9619 | 0.6260 | 0.3046 | 0.030* | |
C4C | 0.98386 (12) | 0.48336 (17) | 0.31252 (8) | 0.0332 (6) | |
H4C3 | 1.0228 | 0.5121 | 0.3050 | 0.050* | |
H4C4 | 0.9883 | 0.4311 | 0.3024 | 0.050* | |
H4C5 | 0.9784 | 0.4834 | 0.3436 | 0.050* | |
C5C | 0.93349 (11) | 0.51937 (14) | 0.24310 (6) | 0.0250 (4) | |
H5C1 | 0.8947 | 0.5402 | 0.2294 | 0.037* | |
H5C2 | 0.9403 | 0.4673 | 0.2333 | 0.037* | |
H5C3 | 0.9712 | 0.5503 | 0.2355 | 0.037* | |
C6C | 0.67599 (11) | 0.74305 (13) | 0.27164 (7) | 0.0249 (4) | |
H6C1 | 0.6817 | 0.7396 | 0.2403 | 0.030* | |
H6C2 | 0.6672 | 0.7967 | 0.2787 | 0.030* | |
C7C | 0.61710 (11) | 0.69604 (14) | 0.28422 (7) | 0.0250 (4) | |
C8C | 0.62341 (11) | 0.61555 (14) | 0.26747 (8) | 0.0271 (5) | |
H8C1 | 0.5818 | 0.5889 | 0.2719 | 0.033* | |
H8C2 | 0.6316 | 0.6175 | 0.2363 | 0.033* | |
C9C | 0.60537 (12) | 0.69717 (16) | 0.33251 (7) | 0.0312 (5) | |
H9C1 | 0.5658 | 0.6690 | 0.3391 | 0.047* | |
H9C2 | 0.6007 | 0.7496 | 0.3422 | 0.047* | |
H9C3 | 0.6422 | 0.6736 | 0.3471 | 0.047* | |
C10C | 0.55839 (14) | 0.73118 (18) | 0.26123 (9) | 0.0421 (7) | |
H10G | 0.5646 | 0.7277 | 0.2303 | 0.063* | |
H10H | 0.5542 | 0.7844 | 0.2695 | 0.063* | |
H10I | 0.5190 | 0.7037 | 0.2693 | 0.063* | |
Cl1P | 0.87873 (3) | 0.35173 (3) | 0.61703 (2) | 0.02205 (10) | |
O1P | 0.86864 (9) | 0.30699 (9) | 0.57889 (6) | 0.0307 (4) | |
O2P | 0.93932 (11) | 0.39045 (13) | 0.61403 (8) | 0.0492 (6) | |
O3P | 0.87621 (13) | 0.30179 (12) | 0.65299 (6) | 0.0492 (6) | |
O4P | 0.82714 (11) | 0.40598 (11) | 0.61975 (6) | 0.0399 (5) | |
Cl2Q | 0.60607 (3) | 0.62761 (3) | 0.45976 (2) | 0.02007 (10) | |
O1Q | 0.66222 (11) | 0.66244 (12) | 0.44072 (7) | 0.0461 (5) | |
O2Q | 0.61357 (15) | 0.54746 (11) | 0.45927 (7) | 0.0583 (7) | |
O3Q | 0.60013 (10) | 0.65500 (9) | 0.50285 (5) | 0.0306 (4) | |
O4Q | 0.55041 (12) | 0.64969 (15) | 0.43565 (7) | 0.0550 (6) | |
Cl3R | 0.61738 (3) | 0.38323 (3) | 0.29233 (2) | 0.02591 (11) | |
O1R | 0.62185 (12) | 0.41908 (12) | 0.33324 (7) | 0.0462 (5) | |
O2R | 0.6456 (3) | 0.30919 (16) | 0.28913 (16) | 0.0462 (13) | 0.529 (6) |
O3R | 0.6370 (3) | 0.4267 (2) | 0.25554 (9) | 0.070 (2) | 0.529 (6) |
O4R | 0.54967 (9) | 0.3750 (4) | 0.2822 (2) | 0.077 (2) | 0.529 (6) |
O5R | 0.68302 (11) | 0.3923 (3) | 0.27750 (15) | 0.0452 (15) | 0.471 (6) |
O6R | 0.5724 (3) | 0.4243 (3) | 0.26626 (14) | 0.0512 (16) | 0.471 (6) |
O7R | 0.6056 (4) | 0.30346 (10) | 0.29699 (17) | 0.0485 (15) | 0.471 (6) |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cr1A | 0.01807 (15) | 0.01021 (15) | 0.01276 (14) | 0.00180 (10) | 0.00074 (10) | 0.00106 (10) |
Br1A | 0.03104 (11) | 0.01724 (10) | 0.01315 (9) | 0.00004 (7) | 0.00137 (7) | 0.00075 (6) |
Br2A | 0.02793 (11) | 0.01914 (11) | 0.01598 (9) | −0.00214 (7) | 0.00514 (7) | −0.00147 (7) |
N1A | 0.0239 (9) | 0.0124 (8) | 0.0174 (8) | 0.0012 (6) | −0.0012 (6) | 0.0012 (6) |
N2A | 0.0214 (8) | 0.0176 (9) | 0.0314 (10) | 0.0045 (7) | −0.0016 (7) | 0.0055 (7) |
N3A | 0.0204 (8) | 0.0119 (8) | 0.0191 (8) | 0.0015 (6) | −0.0025 (6) | 0.0017 (6) |
N4A | 0.0213 (8) | 0.0120 (8) | 0.0159 (7) | 0.0021 (6) | 0.0021 (6) | 0.0006 (6) |
C1A | 0.0253 (10) | 0.0239 (11) | 0.0233 (10) | −0.0053 (8) | −0.0045 (8) | 0.0029 (8) |
C2A | 0.0220 (10) | 0.0242 (11) | 0.0216 (10) | −0.0016 (8) | −0.0062 (8) | 0.0001 (8) |
C3A | 0.0220 (10) | 0.0265 (12) | 0.0290 (11) | 0.0023 (8) | −0.0011 (8) | 0.0006 (8) |
C4A | 0.0422 (14) | 0.0379 (14) | 0.0252 (11) | 0.0054 (11) | −0.0116 (10) | −0.0048 (10) |
C5A | 0.0264 (12) | 0.0403 (16) | 0.0485 (16) | −0.0084 (11) | −0.0025 (11) | 0.0032 (12) |
C6A | 0.0186 (9) | 0.0169 (10) | 0.0198 (9) | 0.0033 (7) | 0.0004 (7) | −0.0008 (7) |
C7A | 0.0196 (9) | 0.0163 (9) | 0.0130 (8) | 0.0000 (7) | 0.0003 (7) | 0.0004 (6) |
C8A | 0.0214 (9) | 0.0147 (9) | 0.0156 (8) | 0.0003 (7) | 0.0004 (7) | 0.0019 (6) |
C9A | 0.0207 (9) | 0.0262 (11) | 0.0207 (9) | −0.0031 (8) | 0.0029 (7) | 0.0008 (8) |
C10A | 0.0273 (10) | 0.0228 (11) | 0.0142 (8) | 0.0004 (8) | −0.0014 (7) | −0.0007 (7) |
Cr2B | 0.01444 (14) | 0.01041 (15) | 0.01179 (13) | 0.00034 (10) | −0.00175 (10) | −0.00169 (10) |
Br1B | 0.02322 (10) | 0.01904 (10) | 0.01319 (9) | −0.00211 (7) | 0.00067 (7) | −0.00349 (6) |
Br2B | 0.02469 (10) | 0.02097 (11) | 0.01337 (9) | −0.00362 (7) | 0.00062 (7) | −0.00448 (7) |
N1B | 0.0213 (8) | 0.0130 (8) | 0.0170 (8) | −0.0017 (6) | −0.0038 (6) | −0.0008 (6) |
N2B | 0.0161 (7) | 0.0147 (8) | 0.0240 (8) | 0.0005 (6) | −0.0033 (6) | 0.0008 (6) |
N3B | 0.0186 (8) | 0.0153 (8) | 0.0192 (8) | 0.0030 (6) | −0.0049 (6) | −0.0026 (6) |
N4B | 0.0164 (7) | 0.0116 (8) | 0.0201 (8) | 0.0002 (6) | −0.0006 (6) | −0.0018 (6) |
C1B | 0.0243 (10) | 0.0209 (10) | 0.0149 (8) | −0.0074 (8) | −0.0031 (7) | 0.0025 (7) |
C2B | 0.0178 (9) | 0.0235 (10) | 0.0157 (8) | −0.0058 (7) | −0.0007 (7) | 0.0006 (7) |
C3B | 0.0152 (9) | 0.0267 (11) | 0.0227 (10) | −0.0008 (8) | −0.0001 (7) | −0.0016 (8) |
C4B | 0.0228 (10) | 0.0281 (11) | 0.0158 (9) | −0.0048 (8) | −0.0041 (7) | −0.0012 (8) |
C5B | 0.0234 (11) | 0.0407 (14) | 0.0242 (10) | −0.0126 (9) | 0.0014 (8) | −0.0002 (9) |
C6B | 0.0159 (9) | 0.0197 (10) | 0.0224 (9) | 0.0024 (7) | −0.0018 (7) | −0.0065 (7) |
C7B | 0.0166 (9) | 0.0178 (10) | 0.0236 (10) | −0.0001 (7) | −0.0025 (7) | −0.0059 (7) |
C8B | 0.0183 (9) | 0.0147 (9) | 0.0234 (9) | −0.0029 (7) | 0.0006 (7) | −0.0017 (7) |
C9B | 0.0187 (10) | 0.0311 (13) | 0.0426 (14) | −0.0048 (9) | 0.0015 (9) | −0.0068 (10) |
C10B | 0.0283 (11) | 0.0275 (12) | 0.0251 (10) | 0.0020 (9) | −0.0065 (9) | −0.0113 (8) |
Cr3C | 0.01761 (15) | 0.01122 (15) | 0.01120 (13) | 0.00002 (10) | 0.00117 (10) | −0.00110 (10) |
Br1C | 0.03008 (11) | 0.02170 (11) | 0.01220 (9) | 0.00659 (8) | 0.00108 (7) | −0.00062 (7) |
Br2C | 0.03001 (11) | 0.02544 (12) | 0.01229 (9) | 0.00771 (8) | 0.00140 (7) | −0.00137 (7) |
N1C | 0.0233 (8) | 0.0135 (8) | 0.0185 (8) | 0.0012 (6) | 0.0008 (6) | −0.0030 (6) |
N2C | 0.0225 (9) | 0.0168 (9) | 0.0260 (9) | −0.0030 (7) | 0.0011 (7) | −0.0053 (7) |
N3C | 0.0273 (9) | 0.0125 (8) | 0.0174 (8) | 0.0016 (6) | 0.0053 (6) | −0.0003 (6) |
N4C | 0.0208 (8) | 0.0187 (9) | 0.0277 (9) | −0.0024 (7) | 0.0004 (7) | 0.0027 (7) |
C1C | 0.0276 (10) | 0.0195 (10) | 0.0178 (9) | 0.0055 (8) | 0.0006 (8) | −0.0009 (7) |
C2C | 0.0202 (9) | 0.0267 (11) | 0.0143 (8) | 0.0058 (8) | −0.0004 (7) | −0.0045 (7) |
C3C | 0.0219 (10) | 0.0292 (12) | 0.0239 (10) | 0.0001 (8) | −0.0035 (8) | −0.0102 (8) |
C4C | 0.0280 (12) | 0.0474 (15) | 0.0244 (11) | 0.0142 (11) | −0.0063 (9) | −0.0070 (10) |
C5C | 0.0244 (10) | 0.0344 (12) | 0.0161 (9) | 0.0025 (9) | 0.0013 (8) | −0.0060 (8) |
C6C | 0.0346 (12) | 0.0206 (11) | 0.0195 (9) | 0.0114 (9) | 0.0048 (8) | 0.0051 (8) |
C7C | 0.0237 (10) | 0.0305 (12) | 0.0208 (10) | 0.0097 (9) | 0.0013 (8) | 0.0003 (8) |
C8C | 0.0211 (10) | 0.0319 (13) | 0.0284 (11) | 0.0026 (8) | −0.0030 (8) | −0.0011 (9) |
C9C | 0.0268 (11) | 0.0423 (15) | 0.0244 (11) | 0.0041 (10) | 0.0082 (9) | −0.0001 (10) |
C10C | 0.0372 (14) | 0.0519 (18) | 0.0374 (14) | 0.0235 (13) | −0.0056 (11) | −0.0024 (12) |
Cl1P | 0.0285 (2) | 0.0157 (2) | 0.0219 (2) | 0.00190 (18) | 0.00275 (18) | 0.00091 (17) |
O1P | 0.0421 (10) | 0.0175 (8) | 0.0323 (9) | 0.0008 (7) | 0.0004 (7) | −0.0055 (6) |
O2P | 0.0382 (11) | 0.0560 (14) | 0.0535 (13) | −0.0205 (10) | −0.0062 (10) | −0.0071 (10) |
O3P | 0.0796 (17) | 0.0371 (12) | 0.0308 (10) | 0.0115 (11) | 0.0024 (10) | 0.0155 (8) |
O4P | 0.0510 (12) | 0.0265 (10) | 0.0421 (11) | 0.0188 (9) | 0.0103 (9) | −0.0024 (8) |
Cl2Q | 0.0308 (3) | 0.0143 (2) | 0.0151 (2) | −0.00351 (18) | 0.00013 (17) | −0.00130 (15) |
O1Q | 0.0485 (12) | 0.0486 (13) | 0.0411 (11) | −0.0201 (10) | 0.0232 (9) | −0.0174 (9) |
O2Q | 0.127 (2) | 0.0115 (9) | 0.0362 (11) | 0.0078 (11) | 0.0110 (13) | −0.0033 (7) |
O3Q | 0.0501 (11) | 0.0256 (9) | 0.0161 (7) | 0.0085 (7) | 0.0024 (7) | −0.0026 (6) |
O4Q | 0.0487 (13) | 0.0718 (17) | 0.0446 (12) | 0.0006 (11) | −0.0225 (10) | −0.0051 (11) |
Cl3R | 0.0322 (3) | 0.0144 (2) | 0.0311 (3) | 0.00260 (19) | 0.0053 (2) | 0.00028 (18) |
O1R | 0.0581 (14) | 0.0355 (12) | 0.0450 (12) | 0.0125 (10) | −0.0116 (10) | −0.0162 (9) |
O2R | 0.061 (3) | 0.022 (2) | 0.056 (3) | 0.021 (2) | −0.010 (2) | −0.0047 (17) |
O3R | 0.147 (7) | 0.021 (2) | 0.042 (2) | −0.021 (3) | 0.017 (3) | −0.0061 (17) |
O4R | 0.049 (3) | 0.085 (5) | 0.098 (5) | 0.038 (3) | −0.032 (3) | −0.035 (4) |
O5R | 0.034 (2) | 0.064 (3) | 0.038 (3) | −0.012 (2) | 0.0173 (19) | −0.021 (2) |
O6R | 0.075 (4) | 0.038 (3) | 0.041 (3) | 0.024 (3) | −0.019 (3) | 0.003 (2) |
O7R | 0.086 (5) | 0.013 (2) | 0.047 (3) | −0.001 (2) | 0.006 (3) | 0.0009 (16) |
Geometric parameters (Å, º) top
Cr1A—N3A | 2.0819 (17) | C5B—H5B3 | 0.9800 |
Cr1A—N4A | 2.0881 (17) | C6B—C7B | 1.534 (3) |
Cr1A—N2A | 2.0990 (19) | C6B—H6B1 | 0.9900 |
Cr1A—N1A | 2.1044 (18) | C6B—H6B2 | 0.9900 |
Cr1A—Br1A | 2.4714 (6) | C7B—C8B | 1.529 (3) |
Cr1A—Br2A | 2.4867 (6) | C7B—C9B | 1.532 (3) |
N1A—C1A | 1.495 (3) | C7B—C10B | 1.535 (3) |
N1A—H1A1 | 0.9100 | C8B—H8B1 | 0.9900 |
N1A—H1A2 | 0.9100 | C8B—H8B2 | 0.9900 |
N2A—C3A | 1.483 (3) | C9B—H9B1 | 0.9800 |
N2A—H2A1 | 0.9100 | C9B—H9B2 | 0.9800 |
N2A—H2A2 | 0.9100 | C9B—H9B3 | 0.9800 |
N3A—C6A | 1.492 (3) | C10B—H10D | 0.9800 |
N3A—H3A1 | 0.9100 | C10B—H10E | 0.9800 |
N3A—H3A2 | 0.9100 | C10B—H10F | 0.9800 |
N4A—C8A | 1.490 (3) | Cr3C—N4C | 2.0761 (19) |
N4A—H4A1 | 0.9100 | Cr3C—N3C | 2.0794 (18) |
N4A—H4A2 | 0.9100 | Cr3C—N2C | 2.0958 (19) |
C1A—C2A | 1.521 (3) | Cr3C—N1C | 2.0982 (18) |
C1A—H1A3 | 0.9900 | Cr3C—Br1C | 2.4732 (6) |
C1A—H1A4 | 0.9900 | Cr3C—Br2C | 2.4735 (6) |
C2A—C4A | 1.523 (3) | N1C—C1C | 1.489 (3) |
C2A—C3A | 1.526 (3) | N1C—H1C1 | 0.9100 |
C2A—C5A | 1.546 (3) | N1C—H1C2 | 0.9100 |
C3A—H3A3 | 0.9900 | N2C—C3C | 1.496 (3) |
C3A—H3A4 | 0.9900 | N2C—H2C1 | 0.9100 |
C4A—H4A3 | 0.9800 | N2C—H2C2 | 0.9100 |
C4A—H4A4 | 0.9800 | N3C—C6C | 1.491 (3) |
C4A—H4A5 | 0.9800 | N3C—H3C1 | 0.9100 |
C5A—H5A1 | 0.9800 | N3C—H3C2 | 0.9100 |
C5A—H5A2 | 0.9800 | N4C—C8C | 1.494 (3) |
C5A—H5A3 | 0.9800 | N4C—H4C1 | 0.9100 |
C6A—C7A | 1.533 (3) | N4C—H4C2 | 0.9100 |
C6A—H6A1 | 0.9900 | C1C—C2C | 1.534 (3) |
C6A—H6A2 | 0.9900 | C1C—H1C3 | 0.9900 |
C7A—C8A | 1.529 (3) | C1C—H1C4 | 0.9900 |
C7A—C9A | 1.531 (3) | C2C—C3C | 1.523 (3) |
C7A—C10A | 1.536 (3) | C2C—C5C | 1.528 (3) |
C8A—H8A1 | 0.9900 | C2C—C4C | 1.532 (3) |
C8A—H8A2 | 0.9900 | C3C—H3C3 | 0.9900 |
C9A—H9A1 | 0.9800 | C3C—H3C4 | 0.9900 |
C9A—H9A2 | 0.9800 | C4C—H4C3 | 0.9800 |
C9A—H9A3 | 0.9800 | C4C—H4C4 | 0.9800 |
C10A—H10A | 0.9800 | C4C—H4C5 | 0.9800 |
C10A—H10B | 0.9800 | C5C—H5C1 | 0.9800 |
C10A—H10C | 0.9800 | C5C—H5C2 | 0.9800 |
Cr2B—N2B | 2.0816 (17) | C5C—H5C3 | 0.9800 |
Cr2B—N1B | 2.0917 (18) | C6C—C7C | 1.525 (3) |
Cr2B—N3B | 2.0941 (17) | C6C—H6C1 | 0.9900 |
Cr2B—N4B | 2.0959 (17) | C6C—H6C2 | 0.9900 |
Cr2B—Br1B | 2.4653 (6) | C7C—C8C | 1.521 (3) |
Cr2B—Br2B | 2.4778 (6) | C7C—C9C | 1.531 (3) |
N1B—C1B | 1.489 (3) | C7C—C10C | 1.541 (3) |
N1B—H1B1 | 0.9100 | C8C—H8C1 | 0.9900 |
N1B—H1B2 | 0.9100 | C8C—H8C2 | 0.9900 |
N2B—C3B | 1.485 (3) | C9C—H9C1 | 0.9800 |
N2B—H2B1 | 0.9100 | C9C—H9C2 | 0.9800 |
N2B—H2B2 | 0.9100 | C9C—H9C3 | 0.9800 |
N3B—C6B | 1.487 (3) | C10C—H10G | 0.9800 |
N3B—H3B1 | 0.9100 | C10C—H10H | 0.9800 |
N3B—H3B2 | 0.9100 | C10C—H10I | 0.9800 |
N4B—C8B | 1.487 (3) | Cl1P—O2P | 1.429 (2) |
N4B—H4B1 | 0.9100 | Cl1P—O3P | 1.4311 (19) |
N4B—H4B2 | 0.9100 | Cl1P—O4P | 1.4357 (19) |
C1B—C2B | 1.524 (3) | Cl1P—O1P | 1.4469 (17) |
C1B—H1B3 | 0.9900 | Cl2Q—O2Q | 1.4245 (19) |
C1B—H1B4 | 0.9900 | Cl2Q—O4Q | 1.430 (2) |
C2B—C3B | 1.526 (3) | Cl2Q—O3Q | 1.4384 (16) |
C2B—C4B | 1.535 (3) | Cl2Q—O1Q | 1.442 (2) |
C2B—C5B | 1.536 (3) | Cl3R—O1R | 1.432 (2) |
C3B—H3B3 | 0.9900 | Cl3R—O6R | 1.4335 (10) |
C3B—H3B4 | 0.9900 | Cl3R—O2R | 1.4357 (10) |
C4B—H4B3 | 0.9800 | Cl3R—O7R | 1.4377 (10) |
C4B—H4B4 | 0.9800 | Cl3R—O4R | 1.4414 (10) |
C4B—H4B5 | 0.9800 | Cl3R—O3R | 1.4422 (10) |
C5B—H5B1 | 0.9800 | Cl3R—O5R | 1.4423 (10) |
C5B—H5B2 | 0.9800 | | |
| | | |
N3A—Cr1A—N4A | 87.93 (7) | H4B4—C4B—H4B5 | 109.5 |
N3A—Cr1A—N2A | 178.67 (7) | C2B—C5B—H5B1 | 109.5 |
N4A—Cr1A—N2A | 90.83 (7) | C2B—C5B—H5B2 | 109.5 |
N3A—Cr1A—N1A | 92.14 (7) | H5B1—C5B—H5B2 | 109.5 |
N4A—Cr1A—N1A | 179.85 (7) | C2B—C5B—H5B3 | 109.5 |
N2A—Cr1A—N1A | 89.10 (7) | H5B1—C5B—H5B3 | 109.5 |
N3A—Cr1A—Br1A | 91.75 (5) | H5B2—C5B—H5B3 | 109.5 |
N4A—Cr1A—Br1A | 91.38 (5) | N3B—C6B—C7B | 114.48 (16) |
N2A—Cr1A—Br1A | 87.78 (6) | N3B—C6B—H6B1 | 108.6 |
N1A—Cr1A—Br1A | 88.48 (5) | C7B—C6B—H6B1 | 108.6 |
N3A—Cr1A—Br2A | 88.39 (5) | N3B—C6B—H6B2 | 108.6 |
N4A—Cr1A—Br2A | 90.68 (5) | C7B—C6B—H6B2 | 108.6 |
N2A—Cr1A—Br2A | 92.12 (6) | H6B1—C6B—H6B2 | 107.6 |
N1A—Cr1A—Br2A | 89.46 (5) | C8B—C7B—C9B | 106.30 (18) |
Br1A—Cr1A—Br2A | 177.938 (16) | C8B—C7B—C6B | 111.88 (16) |
C1A—N1A—Cr1A | 120.49 (14) | C9B—C7B—C6B | 106.91 (17) |
C1A—N1A—H1A1 | 107.2 | C8B—C7B—C10B | 111.05 (17) |
Cr1A—N1A—H1A1 | 107.2 | C9B—C7B—C10B | 109.49 (18) |
C1A—N1A—H1A2 | 107.2 | C6B—C7B—C10B | 110.99 (18) |
Cr1A—N1A—H1A2 | 107.2 | N4B—C8B—C7B | 115.44 (17) |
H1A1—N1A—H1A2 | 106.8 | N4B—C8B—H8B1 | 108.4 |
C3A—N2A—Cr1A | 120.82 (14) | C7B—C8B—H8B1 | 108.4 |
C3A—N2A—H2A1 | 107.1 | N4B—C8B—H8B2 | 108.4 |
Cr1A—N2A—H2A1 | 107.1 | C7B—C8B—H8B2 | 108.4 |
C3A—N2A—H2A2 | 107.1 | H8B1—C8B—H8B2 | 107.5 |
Cr1A—N2A—H2A2 | 107.1 | C7B—C9B—H9B1 | 109.5 |
H2A1—N2A—H2A2 | 106.8 | C7B—C9B—H9B2 | 109.5 |
C6A—N3A—Cr1A | 120.15 (12) | H9B1—C9B—H9B2 | 109.5 |
C6A—N3A—H3A1 | 107.3 | C7B—C9B—H9B3 | 109.5 |
Cr1A—N3A—H3A1 | 107.3 | H9B1—C9B—H9B3 | 109.5 |
C6A—N3A—H3A2 | 107.3 | H9B2—C9B—H9B3 | 109.5 |
Cr1A—N3A—H3A2 | 107.3 | C7B—C10B—H10D | 109.5 |
H3A1—N3A—H3A2 | 106.9 | C7B—C10B—H10E | 109.5 |
C8A—N4A—Cr1A | 120.28 (12) | H10D—C10B—H10E | 109.5 |
C8A—N4A—H4A1 | 107.3 | C7B—C10B—H10F | 109.5 |
Cr1A—N4A—H4A1 | 107.3 | H10D—C10B—H10F | 109.5 |
C8A—N4A—H4A2 | 107.3 | H10E—C10B—H10F | 109.5 |
Cr1A—N4A—H4A2 | 107.3 | N4C—Cr3C—N3C | 89.62 (8) |
H4A1—N4A—H4A2 | 106.9 | N4C—Cr3C—N2C | 179.09 (8) |
N1A—C1A—C2A | 116.01 (18) | N3C—Cr3C—N2C | 91.29 (7) |
N1A—C1A—H1A3 | 108.3 | N4C—Cr3C—N1C | 89.14 (7) |
C2A—C1A—H1A3 | 108.3 | N3C—Cr3C—N1C | 178.49 (7) |
N1A—C1A—H1A4 | 108.3 | N2C—Cr3C—N1C | 89.96 (7) |
C2A—C1A—H1A4 | 108.3 | N4C—Cr3C—Br1C | 89.71 (5) |
H1A3—C1A—H1A4 | 107.4 | N3C—Cr3C—Br1C | 89.35 (5) |
C1A—C2A—C4A | 111.7 (2) | N2C—Cr3C—Br1C | 90.41 (5) |
C1A—C2A—C3A | 112.35 (18) | N1C—Cr3C—Br1C | 89.80 (5) |
C4A—C2A—C3A | 111.7 (2) | N4C—Cr3C—Br2C | 90.83 (5) |
C1A—C2A—C5A | 106.05 (19) | N3C—Cr3C—Br2C | 89.91 (5) |
C4A—C2A—C5A | 108.6 (2) | N2C—Cr3C—Br2C | 89.07 (5) |
C3A—C2A—C5A | 106.0 (2) | N1C—Cr3C—Br2C | 90.95 (5) |
N2A—C3A—C2A | 113.97 (19) | Br1C—Cr3C—Br2C | 179.081 (17) |
N2A—C3A—H3A3 | 108.8 | C1C—N1C—Cr3C | 121.44 (13) |
C2A—C3A—H3A3 | 108.8 | C1C—N1C—H1C1 | 107.0 |
N2A—C3A—H3A4 | 108.8 | Cr3C—N1C—H1C1 | 107.0 |
C2A—C3A—H3A4 | 108.8 | C1C—N1C—H1C2 | 107.0 |
H3A3—C3A—H3A4 | 107.7 | Cr3C—N1C—H1C2 | 107.0 |
C2A—C4A—H4A3 | 109.5 | H1C1—N1C—H1C2 | 106.7 |
C2A—C4A—H4A4 | 109.5 | C3C—N2C—Cr3C | 121.02 (14) |
H4A3—C4A—H4A4 | 109.5 | C3C—N2C—H2C1 | 107.1 |
C2A—C4A—H4A5 | 109.5 | Cr3C—N2C—H2C1 | 107.1 |
H4A3—C4A—H4A5 | 109.5 | C3C—N2C—H2C2 | 107.1 |
H4A4—C4A—H4A5 | 109.5 | Cr3C—N2C—H2C2 | 107.1 |
C2A—C5A—H5A1 | 109.5 | H2C1—N2C—H2C2 | 106.8 |
C2A—C5A—H5A2 | 109.5 | C6C—N3C—Cr3C | 120.76 (14) |
H5A1—C5A—H5A2 | 109.5 | C6C—N3C—H3C1 | 107.1 |
C2A—C5A—H5A3 | 109.5 | Cr3C—N3C—H3C1 | 107.1 |
H5A1—C5A—H5A3 | 109.5 | C6C—N3C—H3C2 | 107.1 |
H5A2—C5A—H5A3 | 109.5 | Cr3C—N3C—H3C2 | 107.1 |
N3A—C6A—C7A | 114.22 (16) | H3C1—N3C—H3C2 | 106.8 |
N3A—C6A—H6A1 | 108.7 | C8C—N4C—Cr3C | 121.34 (14) |
C7A—C6A—H6A1 | 108.7 | C8C—N4C—H4C1 | 107.0 |
N3A—C6A—H6A2 | 108.7 | Cr3C—N4C—H4C1 | 107.0 |
C7A—C6A—H6A2 | 108.7 | C8C—N4C—H4C2 | 107.0 |
H6A1—C6A—H6A2 | 107.6 | Cr3C—N4C—H4C2 | 107.0 |
C8A—C7A—C9A | 107.02 (16) | H4C1—N4C—H4C2 | 106.7 |
C8A—C7A—C6A | 111.38 (16) | N1C—C1C—C2C | 115.29 (17) |
C9A—C7A—C6A | 106.91 (17) | N1C—C1C—H1C3 | 108.5 |
C8A—C7A—C10A | 110.64 (17) | C2C—C1C—H1C3 | 108.5 |
C9A—C7A—C10A | 108.91 (17) | N1C—C1C—H1C4 | 108.5 |
C6A—C7A—C10A | 111.76 (16) | C2C—C1C—H1C4 | 108.5 |
N4A—C8A—C7A | 115.36 (16) | H1C3—C1C—H1C4 | 107.5 |
N4A—C8A—H8A1 | 108.4 | C3C—C2C—C5C | 111.64 (19) |
C7A—C8A—H8A1 | 108.4 | C3C—C2C—C4C | 106.91 (19) |
N4A—C8A—H8A2 | 108.4 | C5C—C2C—C4C | 109.04 (18) |
C7A—C8A—H8A2 | 108.4 | C3C—C2C—C1C | 111.07 (17) |
H8A1—C8A—H8A2 | 107.5 | C5C—C2C—C1C | 110.99 (18) |
C7A—C9A—H9A1 | 109.5 | C4C—C2C—C1C | 106.97 (19) |
C7A—C9A—H9A2 | 109.5 | N2C—C3C—C2C | 113.63 (17) |
H9A1—C9A—H9A2 | 109.5 | N2C—C3C—H3C3 | 108.8 |
C7A—C9A—H9A3 | 109.5 | C2C—C3C—H3C3 | 108.8 |
H9A1—C9A—H9A3 | 109.5 | N2C—C3C—H3C4 | 108.8 |
H9A2—C9A—H9A3 | 109.5 | C2C—C3C—H3C4 | 108.8 |
C7A—C10A—H10A | 109.5 | H3C3—C3C—H3C4 | 107.7 |
C7A—C10A—H10B | 109.5 | C2C—C4C—H4C3 | 109.5 |
H10A—C10A—H10B | 109.5 | C2C—C4C—H4C4 | 109.5 |
C7A—C10A—H10C | 109.5 | H4C3—C4C—H4C4 | 109.5 |
H10A—C10A—H10C | 109.5 | C2C—C4C—H4C5 | 109.5 |
H10B—C10A—H10C | 109.5 | H4C3—C4C—H4C5 | 109.5 |
N2B—Cr2B—N1B | 90.03 (7) | H4C4—C4C—H4C5 | 109.5 |
N2B—Cr2B—N3B | 178.57 (7) | C2C—C5C—H5C1 | 109.5 |
N1B—Cr2B—N3B | 90.96 (7) | C2C—C5C—H5C2 | 109.5 |
N2B—Cr2B—N4B | 89.45 (7) | H5C1—C5C—H5C2 | 109.5 |
N1B—Cr2B—N4B | 179.35 (7) | C2C—C5C—H5C3 | 109.5 |
N3B—Cr2B—N4B | 89.57 (7) | H5C1—C5C—H5C3 | 109.5 |
N2B—Cr2B—Br1B | 87.63 (5) | H5C2—C5C—H5C3 | 109.5 |
N1B—Cr2B—Br1B | 89.80 (5) | N3C—C6C—C7C | 114.98 (17) |
N3B—Cr2B—Br1B | 91.33 (5) | N3C—C6C—H6C1 | 108.5 |
N4B—Cr2B—Br1B | 90.57 (5) | C7C—C6C—H6C1 | 108.5 |
N2B—Cr2B—Br2B | 92.00 (5) | N3C—C6C—H6C2 | 108.5 |
N1B—Cr2B—Br2B | 89.47 (5) | C7C—C6C—H6C2 | 108.5 |
N3B—Cr2B—Br2B | 89.05 (5) | H6C1—C6C—H6C2 | 107.5 |
N4B—Cr2B—Br2B | 90.15 (5) | C8C—C7C—C6C | 110.60 (18) |
Br1B—Cr2B—Br2B | 179.177 (16) | C8C—C7C—C9C | 111.5 (2) |
C1B—N1B—Cr2B | 119.36 (13) | C6C—C7C—C9C | 112.0 (2) |
C1B—N1B—H1B1 | 107.5 | C8C—C7C—C10C | 106.4 (2) |
Cr2B—N1B—H1B1 | 107.5 | C6C—C7C—C10C | 106.7 (2) |
C1B—N1B—H1B2 | 107.5 | C9C—C7C—C10C | 109.35 (19) |
Cr2B—N1B—H1B2 | 107.5 | N4C—C8C—C7C | 113.78 (19) |
H1B1—N1B—H1B2 | 107.0 | N4C—C8C—H8C1 | 108.8 |
C3B—N2B—Cr2B | 120.29 (13) | C7C—C8C—H8C1 | 108.8 |
C3B—N2B—H2B1 | 107.3 | N4C—C8C—H8C2 | 108.8 |
Cr2B—N2B—H2B1 | 107.3 | C7C—C8C—H8C2 | 108.8 |
C3B—N2B—H2B2 | 107.3 | H8C1—C8C—H8C2 | 107.7 |
Cr2B—N2B—H2B2 | 107.3 | C7C—C9C—H9C1 | 109.5 |
H2B1—N2B—H2B2 | 106.9 | C7C—C9C—H9C2 | 109.5 |
C6B—N3B—Cr2B | 119.38 (13) | H9C1—C9C—H9C2 | 109.5 |
C6B—N3B—H3B1 | 107.5 | C7C—C9C—H9C3 | 109.5 |
Cr2B—N3B—H3B1 | 107.5 | H9C1—C9C—H9C3 | 109.5 |
C6B—N3B—H3B2 | 107.5 | H9C2—C9C—H9C3 | 109.5 |
Cr2B—N3B—H3B2 | 107.5 | C7C—C10C—H10G | 109.5 |
H3B1—N3B—H3B2 | 107.0 | C7C—C10C—H10H | 109.5 |
C8B—N4B—Cr2B | 119.97 (12) | H10G—C10C—H10H | 109.5 |
C8B—N4B—H4B1 | 107.3 | C7C—C10C—H10I | 109.5 |
Cr2B—N4B—H4B1 | 107.3 | H10G—C10C—H10I | 109.5 |
C8B—N4B—H4B2 | 107.3 | H10H—C10C—H10I | 109.5 |
Cr2B—N4B—H4B2 | 107.3 | O2P—Cl1P—O3P | 112.24 (15) |
H4B1—N4B—H4B2 | 106.9 | O2P—Cl1P—O4P | 109.53 (14) |
N1B—C1B—C2B | 115.38 (16) | O3P—Cl1P—O4P | 109.75 (13) |
N1B—C1B—H1B3 | 108.4 | O2P—Cl1P—O1P | 109.47 (13) |
C2B—C1B—H1B3 | 108.4 | O3P—Cl1P—O1P | 107.89 (12) |
N1B—C1B—H1B4 | 108.4 | O4P—Cl1P—O1P | 107.86 (12) |
C2B—C1B—H1B4 | 108.4 | O2Q—Cl2Q—O4Q | 110.67 (16) |
H1B3—C1B—H1B4 | 107.5 | O2Q—Cl2Q—O3Q | 110.72 (11) |
C1B—C2B—C3B | 112.37 (17) | O4Q—Cl2Q—O3Q | 109.55 (13) |
C1B—C2B—C4B | 110.72 (18) | O2Q—Cl2Q—O1Q | 109.41 (15) |
C3B—C2B—C4B | 111.23 (17) | O4Q—Cl2Q—O1Q | 108.20 (15) |
C1B—C2B—C5B | 106.67 (18) | O3Q—Cl2Q—O1Q | 108.23 (12) |
C3B—C2B—C5B | 106.06 (18) | O1R—Cl3R—O6R | 109.1 (2) |
C4B—C2B—C5B | 109.56 (17) | O1R—Cl3R—O2R | 116.0 (2) |
N2B—C3B—C2B | 113.74 (17) | O1R—Cl3R—O7R | 110.7 (2) |
N2B—C3B—H3B3 | 108.8 | O6R—Cl3R—O7R | 116.4 (4) |
C2B—C3B—H3B3 | 108.8 | O1R—Cl3R—O4R | 107.7 (2) |
N2B—C3B—H3B4 | 108.8 | O2R—Cl3R—O4R | 106.7 (3) |
C2B—C3B—H3B4 | 108.8 | O1R—Cl3R—O3R | 117.4 (2) |
H3B3—C3B—H3B4 | 107.7 | O2R—Cl3R—O3R | 108.3 (3) |
C2B—C4B—H4B3 | 109.5 | O4R—Cl3R—O3R | 98.7 (4) |
C2B—C4B—H4B4 | 109.5 | O1R—Cl3R—O5R | 100.2 (2) |
H4B3—C4B—H4B4 | 109.5 | O6R—Cl3R—O5R | 111.7 (3) |
C2B—C4B—H4B5 | 109.5 | O7R—Cl3R—O5R | 107.5 (4) |
H4B3—C4B—H4B5 | 109.5 | | |
| | | |
Cr1A—N1A—C1A—C2A | −53.2 (2) | Cr2B—N3B—C6B—C7B | −58.5 (2) |
N1A—C1A—C2A—C4A | −62.1 (3) | N3B—C6B—C7B—C8B | 66.3 (2) |
N1A—C1A—C2A—C3A | 64.4 (3) | N3B—C6B—C7B—C9B | −177.70 (17) |
N1A—C1A—C2A—C5A | 179.7 (2) | N3B—C6B—C7B—C10B | −58.3 (2) |
Cr1A—N2A—C3A—C2A | 57.8 (2) | Cr2B—N4B—C8B—C7B | 55.4 (2) |
C1A—C2A—C3A—N2A | −66.1 (2) | C9B—C7B—C8B—N4B | 178.89 (17) |
C4A—C2A—C3A—N2A | 60.4 (3) | C6B—C7B—C8B—N4B | −64.8 (2) |
C5A—C2A—C3A—N2A | 178.48 (19) | C10B—C7B—C8B—N4B | 59.9 (2) |
Cr1A—N3A—C6A—C7A | −60.2 (2) | Cr3C—N1C—C1C—C2C | −51.7 (2) |
N3A—C6A—C7A—C8A | 64.5 (2) | N1C—C1C—C2C—C3C | 67.0 (2) |
N3A—C6A—C7A—C9A | −178.87 (16) | N1C—C1C—C2C—C5C | −57.8 (2) |
N3A—C6A—C7A—C10A | −59.8 (2) | N1C—C1C—C2C—C4C | −176.64 (17) |
Cr1A—N4A—C8A—C7A | 57.6 (2) | Cr3C—N2C—C3C—C2C | 56.3 (2) |
C9A—C7A—C8A—N4A | 179.95 (16) | C5C—C2C—C3C—N2C | 55.5 (2) |
C6A—C7A—C8A—N4A | −63.5 (2) | C4C—C2C—C3C—N2C | 174.68 (19) |
C10A—C7A—C8A—N4A | 61.4 (2) | C1C—C2C—C3C—N2C | −69.0 (2) |
Cr2B—N1B—C1B—C2B | −55.1 (2) | Cr3C—N3C—C6C—C7C | 54.9 (2) |
N1B—C1B—C2B—C3B | 66.0 (2) | N3C—C6C—C7C—C8C | −67.6 (2) |
N1B—C1B—C2B—C4B | −59.0 (2) | N3C—C6C—C7C—C9C | 57.3 (2) |
N1B—C1B—C2B—C5B | −178.17 (18) | N3C—C6C—C7C—C10C | 176.96 (19) |
Cr2B—N2B—C3B—C2B | 57.2 (2) | Cr3C—N4C—C8C—C7C | −56.2 (2) |
C1B—C2B—C3B—N2B | −66.3 (2) | C6C—C7C—C8C—N4C | 67.7 (2) |
C4B—C2B—C3B—N2B | 58.5 (2) | C9C—C7C—C8C—N4C | −57.6 (3) |
C5B—C2B—C3B—N2B | 177.53 (17) | C10C—C7C—C8C—N4C | −176.8 (2) |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2A—H2A2···O4P | 0.91 | 2.04 | 2.940 (3) | 172 |
N3A—H3A2···O3Q | 0.91 | 2.22 | 3.075 (2) | 157 |
N4A—H4A2···O4P | 0.91 | 2.36 | 3.110 (3) | 139 |
N2B—H2B1···O1P | 0.91 | 2.50 | 3.376 (3) | 161 |
N3B—H3B1···O2Q | 0.91 | 2.07 | 2.965 (3) | 166 |
N3B—H3B2···O1R | 0.91 | 2.41 | 3.275 (3) | 159 |
N1C—H1C1···O5R | 0.91 | 2.34 | 3.097 (3) | 140 |
N4C—H4C1···O3R | 0.91 | 2.01 | 2.867 (5) | 155 |
N4C—H4C1···O5R | 0.91 | 2.34 | 3.180 (5) | 153 |
N1A—H1A1···O1Pi | 0.91 | 2.55 | 3.393 (3) | 155 |
N3A—H3A1···O1Pi | 0.91 | 2.19 | 3.004 (2) | 149 |
N3A—H3A1···O3Pi | 0.91 | 2.52 | 3.354 (3) | 153 |
N2C—H2C2···O2Ri | 0.91 | 2.11 | 2.889 (4) | 143 |
N2C—H2C2···O7Ri | 0.91 | 2.03 | 2.841 (4) | 147 |
N3C—H3C2···O2Ri | 0.91 | 2.05 | 2.878 (4) | 151 |
N2B—H2B2···O1Qii | 0.91 | 2.03 | 2.925 (3) | 169 |
N4B—H4B2···O1Qii | 0.91 | 2.48 | 3.054 (3) | 121 |
N4A—H4A1···Br1B | 0.91 | 2.67 | 3.4808 (17) | 148 |
N1B—H1B2···Br2A | 0.91 | 2.77 | 3.6017 (18) | 152 |
N4B—H4B1···Br1Cii | 0.91 | 2.85 | 3.6715 (17) | 150 |
N1C—H1C2···Br1Aiii | 0.91 | 2.67 | 3.5081 (18) | 153 |
N3C—H3C1···Br2Bi | 0.91 | 2.68 | 3.4568 (18) | 145 |
N4A—H4A2···Br2Civ | 0.91 | 2.93 | 3.6665 (17) | 139 |
Symmetry codes: (i) −x+3/2, y+1/2, z; (ii) −x+3/2, y−1/2, z; (iii) −x+3/2, −y+1, z−1/2; (iv) −x+3/2, −y+1, z+1/2. |
Experimental details
Crystal data |
Chemical formula | [CrBr2(C5H14N2)2]ClO4 |
Mr | 515.63 |
Crystal system, space group | Orthorhombic, Pbca |
Temperature (K) | 100 |
a, b, c (Å) | 20.656 (4), 17.666 (4), 31.305 (6) |
V (Å3) | 11423 (4) |
Z | 24 |
Radiation type | Synchrotron, λ = 0.62998 Å |
µ (mm−1) | 3.60 |
Crystal size (mm) | 0.12 × 0.10 × 0.05 |
|
Data collection |
Diffractometer | ADSC Q210 CCD area-detector diffractometer |
Absorption correction | Empirical (using intensity measurements) (HKL3000sm SCALEPACK; Otwinowski & Minor, 1997) |
Tmin, Tmax | 0.670, 0.841 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 115348, 15666, 13691 |
Rint | 0.036 |
(sin θ/λ)max (Å−1) | 0.696 |
|
Refinement |
R[F2 > 2σ(F2)], wR(F2), S | 0.031, 0.086, 1.04 |
No. of reflections | 15666 |
No. of parameters | 636 |
No. of restraints | 6 |
H-atom treatment | H-atom parameters constrained |
Δρmax, Δρmin (e Å−3) | 1.25, −1.42 |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
N2A—H2A2···O4P | 0.91 | 2.04 | 2.940 (3) | 172.0 |
N3A—H3A2···O3Q | 0.91 | 2.22 | 3.075 (2) | 156.8 |
N4A—H4A2···O4P | 0.91 | 2.36 | 3.110 (3) | 139.1 |
N2B—H2B1···O1P | 0.91 | 2.50 | 3.376 (3) | 161.0 |
N3B—H3B1···O2Q | 0.91 | 2.07 | 2.965 (3) | 165.7 |
N3B—H3B2···O1R | 0.91 | 2.41 | 3.275 (3) | 159.3 |
N1C—H1C1···O5R | 0.91 | 2.34 | 3.097 (3) | 140.0 |
N4C—H4C1···O3R | 0.91 | 2.01 | 2.867 (5) | 155.4 |
N4C—H4C1···O5R | 0.91 | 2.34 | 3.180 (5) | 153.4 |
N1A—H1A1···O1Pi | 0.91 | 2.55 | 3.393 (3) | 154.6 |
N3A—H3A1···O1Pi | 0.91 | 2.19 | 3.004 (2) | 148.5 |
N3A—H3A1···O3Pi | 0.91 | 2.52 | 3.354 (3) | 152.8 |
N2C—H2C2···O2Ri | 0.91 | 2.11 | 2.889 (4) | 142.8 |
N2C—H2C2···O7Ri | 0.91 | 2.03 | 2.841 (4) | 147.2 |
N3C—H3C2···O2Ri | 0.91 | 2.05 | 2.878 (4) | 150.9 |
N2B—H2B2···O1Qii | 0.91 | 2.03 | 2.925 (3) | 168.6 |
N4B—H4B2···O1Qii | 0.91 | 2.48 | 3.054 (3) | 121.4 |
N4A—H4A1···Br1B | 0.91 | 2.67 | 3.4808 (17) | 148.3 |
N1B—H1B2···Br2A | 0.91 | 2.77 | 3.6017 (18) | 152.3 |
N4B—H4B1···Br1Cii | 0.91 | 2.85 | 3.6715 (17) | 150.4 |
N1C—H1C2···Br1Aiii | 0.91 | 2.67 | 3.5081 (18) | 152.8 |
N3C—H3C1···Br2Bi | 0.91 | 2.68 | 3.4568 (18) | 144.5 |
N4A—H4A2···Br2Civ | 0.91 | 2.93 | 3.6665 (17) | 138.7 |
Symmetry codes: (i) −x+3/2, y+1/2, z; (ii) −x+3/2, y−1/2, z; (iii) −x+3/2, −y+1, z−1/2; (iv) −x+3/2, −y+1, z+1/2. |