Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S1600536806051403/ng2165sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S1600536806051403/ng2165Isup2.hkl |
CCDC reference: 633964
Key indicators
- Single-crystal X-ray study
- T = 100 K
- Mean (C-C) = 0.003 Å
- R factor = 0.023
- wR factor = 0.051
- Data-to-parameter ratio = 19.0
checkCIF/PLATON results
No syntax errors found
Alert level B PLAT420_ALERT_2_B D-H Without Acceptor O1 - H1B ... ?
Alert level C PLAT153_ALERT_1_C The su's on the Cell Axes are Equal (x 100000) . 90 Ang.
0 ALERT level A = In general: serious problem 1 ALERT level B = Potentially serious problem 1 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 0 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
Data collection: APEXII (Bruker, 2004); cell refinement: SAINT-Plus (Bruker, 2004); data reduction: SAINT-Plus and XPREP (Bruker, 2004); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: DIAMOND (Brandenburg & Putz, 2005); software used to prepare material for publication: WinGX (Farrugia, 1999).
(C24H20P)2[Re(CN)4N(H2O)]·5H2O | F(000) = 2208 |
Mr = 1091.14 | Dx = 1.478 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2yn | Cell parameters from 8131 reflections |
a = 15.1335 (9) Å | θ = 2.5–28.3° |
b = 19.7216 (9) Å | µ = 2.59 mm−1 |
c = 16.7754 (9) Å | T = 100 K |
β = 101.576 (2)° | Cuboid, yellow |
V = 4904.9 (5) Å3 | 0.25 × 0.22 × 0.19 mm |
Z = 4 |
Bruker X8 APEXII 4K KappaCCD diffractometer | 10389 reflections with I > 2σ(I) |
ω and φ scans | Rint = 0.039 |
Absorption correction: multi-scan (SADABS; Bruker, 2004) | θmax = 28.3°, θmin = 2.0° |
Tmin = 0.541, Tmax = 0.613 | h = −20→20 |
49525 measured reflections | k = −25→26 |
12210 independent reflections | l = −22→22 |
Refinement on F2 | 18 restraints |
Least-squares matrix: full | H atoms treated by a mixture of independent and constrained refinement |
R[F2 > 2σ(F2)] = 0.023 | w = 1/[σ2(Fo2) + (0.0207P)2 + 1.3302P] where P = (Fo2 + 2Fc2)/3 |
wR(F2) = 0.051 | (Δ/σ)max = 0.006 |
S = 1.03 | Δρmax = 0.80 e Å−3 |
12210 reflections | Δρmin = −0.62 e Å−3 |
643 parameters |
Experimental. The intensity data was collected on a Bruker X8 Apex II 4 K Kappa CCD diffractometer using an exposure time of 3 s/frame. A total of 1865 frames were collected with a frame width of 0.5° covering up to θ = 28.28° with 99.6% completeness accomplished. |
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. |
x | y | z | Uiso*/Ueq | ||
Re1 | 0.470066 (5) | 0.329995 (4) | 0.736867 (5) | 0.01001 (3) | |
P2 | 0.44053 (4) | 0.30952 (3) | 0.10599 (3) | 0.01092 (11) | |
P1 | 0.55915 (4) | 0.06006 (3) | 0.32801 (3) | 0.01240 (11) | |
C3 | 0.49860 (14) | 0.22564 (11) | 0.73617 (12) | 0.0126 (4) | |
C55 | 0.34830 (19) | 0.29128 (11) | 0.31744 (15) | 0.0260 (6) | |
H55 | 0.3712 | 0.2847 | 0.3726 | 0.031* | |
C36 | 0.53514 (16) | 0.16125 (12) | 0.43556 (15) | 0.0221 (5) | |
H36 | 0.4872 | 0.1351 | 0.4451 | 0.027* | |
C16 | 0.63164 (15) | 0.00203 (12) | 0.47777 (13) | 0.0178 (5) | |
H16 | 0.6252 | 0.0444 | 0.5003 | 0.021* | |
C21 | 0.60426 (15) | 0.05656 (10) | 0.23692 (13) | 0.0133 (4) | |
C15 | 0.66623 (15) | −0.05210 (13) | 0.52705 (13) | 0.0218 (5) | |
H15 | 0.684 | −0.0457 | 0.5829 | 0.026* | |
C43 | 0.30385 (15) | −0.01368 (11) | 0.26613 (13) | 0.0184 (5) | |
H43 | 0.2758 | −0.0559 | 0.2601 | 0.022* | |
C14 | 0.67457 (15) | −0.11527 (12) | 0.49415 (14) | 0.0209 (5) | |
H14 | 0.6976 | −0.1512 | 0.5279 | 0.025* | |
C65 | 0.38329 (15) | 0.50661 (11) | 0.05640 (14) | 0.0193 (5) | |
H65 | 0.3753 | 0.5451 | 0.0861 | 0.023* | |
C72 | 0.45564 (14) | 0.22768 (11) | −0.02525 (13) | 0.0142 (4) | |
H72 | 0.4965 | 0.2598 | −0.0364 | 0.017* | |
C22 | 0.54794 (16) | 0.06414 (11) | 0.16073 (13) | 0.0172 (5) | |
H22 | 0.4861 | 0.0694 | 0.1564 | 0.021* | |
C31 | 0.58662 (15) | 0.13924 (11) | 0.37982 (13) | 0.0150 (4) | |
C41 | 0.43877 (14) | 0.05306 (10) | 0.30038 (12) | 0.0128 (4) | |
C75 | 0.33625 (16) | 0.12991 (11) | 0.01001 (14) | 0.0193 (5) | |
H75 | 0.2973 | 0.0967 | 0.022 | 0.023* | |
C82 | 0.59355 (15) | 0.36451 (11) | 0.20166 (13) | 0.0172 (5) | |
H82 | 0.5576 | 0.4018 | 0.2069 | 0.021* | |
C24 | 0.67712 (17) | 0.05668 (11) | 0.09779 (14) | 0.0206 (5) | |
H24 | 0.7016 | 0.0573 | 0.0512 | 0.025* | |
C26 | 0.69694 (15) | 0.04810 (11) | 0.24328 (14) | 0.0181 (5) | |
H26 | 0.7343 | 0.0422 | 0.294 | 0.022* | |
C61 | 0.41196 (14) | 0.38690 (10) | 0.05005 (13) | 0.0128 (4) | |
C74 | 0.37468 (16) | 0.12340 (11) | −0.05769 (14) | 0.0197 (5) | |
H74 | 0.3603 | 0.0862 | −0.0918 | 0.024* | |
C32 | 0.65950 (16) | 0.17783 (11) | 0.36705 (13) | 0.0187 (5) | |
H32 | 0.6943 | 0.1633 | 0.3306 | 0.022* | |
C12 | 0.61620 (15) | −0.07120 (11) | 0.36045 (14) | 0.0182 (5) | |
H12 | 0.6009 | −0.0774 | 0.3044 | 0.022* | |
C46 | 0.38687 (15) | 0.11145 (11) | 0.28209 (14) | 0.0180 (5) | |
H46 | 0.4149 | 0.1537 | 0.2866 | 0.022* | |
C71 | 0.41532 (14) | 0.23574 (10) | 0.04212 (12) | 0.0120 (4) | |
C23 | 0.58506 (17) | 0.06384 (11) | 0.09139 (14) | 0.0199 (5) | |
H23 | 0.5478 | 0.0685 | 0.0404 | 0.024* | |
C63 | 0.39045 (15) | 0.45435 (11) | −0.07166 (14) | 0.0189 (5) | |
H63 | 0.3877 | 0.458 | −0.1274 | 0.023* | |
C76 | 0.35612 (15) | 0.18641 (10) | 0.06029 (13) | 0.0149 (4) | |
H76 | 0.3301 | 0.1912 | 0.1057 | 0.018* | |
C11 | 0.60661 (14) | −0.00793 (10) | 0.39393 (12) | 0.0130 (4) | |
C83 | 0.68278 (16) | 0.36334 (12) | 0.24065 (13) | 0.0196 (5) | |
H83 | 0.7069 | 0.4001 | 0.2724 | 0.024* | |
C56 | 0.40724 (17) | 0.29598 (11) | 0.26351 (13) | 0.0185 (5) | |
H56 | 0.4692 | 0.2921 | 0.2822 | 0.022* | |
C66 | 0.39985 (15) | 0.44500 (11) | 0.09526 (13) | 0.0161 (4) | |
H66 | 0.403 | 0.4419 | 0.1511 | 0.019* | |
C25 | 0.73305 (16) | 0.04862 (11) | 0.17345 (14) | 0.0204 (5) | |
H25 | 0.7949 | 0.0435 | 0.1775 | 0.024* | |
C86 | 0.61182 (15) | 0.25334 (11) | 0.14673 (13) | 0.0153 (4) | |
H86 | 0.5878 | 0.2162 | 0.1156 | 0.018* | |
C81 | 0.55749 (14) | 0.30914 (11) | 0.15415 (12) | 0.0122 (4) | |
C64 | 0.37848 (15) | 0.51143 (12) | −0.02696 (14) | 0.0201 (5) | |
H64 | 0.3672 | 0.5531 | −0.0528 | 0.024* | |
C52 | 0.27867 (16) | 0.31334 (11) | 0.15391 (15) | 0.0194 (5) | |
H52 | 0.2553 | 0.3214 | 0.0991 | 0.023* | |
C84 | 0.73709 (16) | 0.30790 (12) | 0.23312 (13) | 0.0196 (5) | |
H84 | 0.7972 | 0.3075 | 0.2598 | 0.024* | |
C54 | 0.25645 (19) | 0.29631 (12) | 0.28967 (16) | 0.0281 (6) | |
H54 | 0.2177 | 0.2918 | 0.3259 | 0.034* | |
C33 | 0.67980 (17) | 0.23827 (12) | 0.40919 (14) | 0.0231 (5) | |
H33 | 0.729 | 0.2639 | 0.4014 | 0.028* | |
C44 | 0.25233 (15) | 0.04450 (11) | 0.24888 (13) | 0.0168 (5) | |
H44 | 0.1901 | 0.0415 | 0.2318 | 0.02* | |
C34 | 0.62755 (17) | 0.26057 (12) | 0.46250 (14) | 0.0235 (5) | |
H34 | 0.6407 | 0.3018 | 0.4892 | 0.028* | |
C73 | 0.43456 (15) | 0.17184 (10) | −0.07533 (13) | 0.0168 (4) | |
H73 | 0.4605 | 0.1667 | −0.1208 | 0.02* | |
C85 | 0.70121 (15) | 0.25335 (11) | 0.18564 (13) | 0.0185 (5) | |
H85 | 0.7376 | 0.2164 | 0.1799 | 0.022* | |
C62 | 0.40653 (14) | 0.39177 (11) | −0.03366 (13) | 0.0145 (4) | |
H62 | 0.4136 | 0.3533 | −0.0639 | 0.017* | |
C13 | 0.64880 (16) | −0.12537 (12) | 0.41110 (14) | 0.0207 (5) | |
H13 | 0.6532 | −0.1682 | 0.3892 | 0.025* | |
C42 | 0.39678 (15) | −0.00987 (10) | 0.29231 (13) | 0.0144 (4) | |
H42 | 0.4307 | −0.0492 | 0.3044 | 0.017* | |
C51 | 0.37190 (15) | 0.30655 (11) | 0.18135 (13) | 0.0146 (4) | |
C45 | 0.29437 (15) | 0.10739 (11) | 0.25727 (13) | 0.0191 (5) | |
H45 | 0.2603 | 0.1467 | 0.2462 | 0.023* | |
C35 | 0.55567 (17) | 0.22204 (12) | 0.47648 (15) | 0.0267 (6) | |
H35 | 0.5213 | 0.2369 | 0.5132 | 0.032* | |
C53 | 0.22153 (17) | 0.30808 (11) | 0.20793 (16) | 0.0247 (5) | |
H53 | 0.1596 | 0.3124 | 0.1896 | 0.03* | |
N3 | 0.51991 (13) | 0.16936 (9) | 0.74369 (12) | 0.0183 (4) | |
N5 | 0.38241 (13) | 0.32756 (9) | 0.78220 (11) | 0.0156 (4) | |
C2 | 0.39959 (15) | 0.32801 (10) | 0.61493 (13) | 0.0148 (4) | |
N2 | 0.36210 (14) | 0.32770 (10) | 0.54814 (12) | 0.0226 (4) | |
N1 | 0.48946 (14) | 0.49344 (10) | 0.72099 (11) | 0.0212 (4) | |
C1 | 0.48262 (14) | 0.43580 (11) | 0.72677 (12) | 0.0143 (4) | |
N4 | 0.63075 (14) | 0.32536 (9) | 0.89768 (12) | 0.0217 (4) | |
C4 | 0.57456 (15) | 0.32991 (10) | 0.84059 (13) | 0.0141 (4) | |
O1 | 0.59570 (11) | 0.33544 (8) | 0.66560 (9) | 0.0160 (3) | |
O6 | 0.67527 (11) | 0.20144 (8) | 0.98364 (10) | 0.0214 (4) | |
O2 | 0.61895 (12) | 0.42035 (8) | 0.54890 (10) | 0.0212 (4) | |
O4 | 0.31590 (12) | 0.44249 (8) | 0.43400 (11) | 0.0235 (4) | |
O3 | 0.50331 (12) | 0.58864 (9) | 0.59496 (11) | 0.0251 (4) | |
O5 | 0.62989 (12) | 0.08939 (8) | 0.88803 (11) | 0.0247 (4) | |
H6A | 0.7304 (8) | 0.1967 (11) | 1.0040 (15) | 0.029 (8)* | |
H6B | 0.6648 (15) | 0.2403 (7) | 0.9630 (15) | 0.030 (8)* | |
H5A | 0.637 (2) | 0.1236 (10) | 0.9193 (12) | 0.054 (10)* | |
H5B | 0.6041 (19) | 0.1022 (13) | 0.8405 (8) | 0.049 (10)* | |
H4A | 0.3286 (16) | 0.4130 (11) | 0.4717 (12) | 0.036 (8)* | |
H3A | 0.5560 (9) | 0.5798 (13) | 0.5894 (16) | 0.038 (9)* | |
H4B | 0.2614 (9) | 0.4366 (13) | 0.4098 (15) | 0.043 (9)* | |
H3B | 0.4896 (17) | 0.5664 (13) | 0.6336 (13) | 0.051 (10)* | |
H2A | 0.6408 (19) | 0.4598 (8) | 0.5539 (17) | 0.058 (11)* | |
H2B | 0.5782 (17) | 0.4176 (14) | 0.5065 (13) | 0.063 (11)* | |
H1A | 0.600 (2) | 0.3653 (9) | 0.6298 (13) | 0.043 (9)* | |
H1B | 0.6164 (19) | 0.2982 (7) | 0.6521 (15) | 0.042 (9)* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Re1 | 0.00901 (4) | 0.00980 (5) | 0.01063 (4) | −0.00031 (3) | 0.00055 (3) | −0.00040 (3) |
P2 | 0.0105 (3) | 0.0106 (3) | 0.0122 (2) | 0.0000 (2) | 0.0035 (2) | −0.0014 (2) |
P1 | 0.0114 (3) | 0.0113 (3) | 0.0138 (3) | −0.0004 (2) | 0.0009 (2) | −0.0013 (2) |
C3 | 0.0087 (10) | 0.0172 (12) | 0.0122 (10) | −0.0031 (8) | 0.0026 (8) | −0.0014 (8) |
C55 | 0.0500 (18) | 0.0116 (12) | 0.0214 (12) | −0.0007 (11) | 0.0190 (12) | 0.0001 (9) |
C36 | 0.0144 (11) | 0.0228 (13) | 0.0294 (13) | −0.0029 (9) | 0.0052 (10) | −0.0090 (10) |
C16 | 0.0147 (11) | 0.0234 (13) | 0.0161 (11) | 0.0006 (9) | 0.0050 (9) | −0.0035 (9) |
C21 | 0.0139 (11) | 0.0099 (10) | 0.0163 (10) | −0.0014 (8) | 0.0030 (8) | −0.0004 (8) |
C15 | 0.0158 (12) | 0.0381 (15) | 0.0107 (10) | 0.0000 (10) | 0.0007 (9) | 0.0037 (10) |
C43 | 0.0177 (11) | 0.0158 (11) | 0.0211 (11) | −0.0054 (9) | 0.0025 (9) | −0.0043 (9) |
C14 | 0.0140 (11) | 0.0271 (13) | 0.0219 (12) | 0.0057 (10) | 0.0044 (9) | 0.0116 (10) |
C65 | 0.0172 (11) | 0.0130 (11) | 0.0269 (12) | −0.0001 (9) | 0.0021 (10) | −0.0041 (9) |
C72 | 0.0116 (10) | 0.0135 (11) | 0.0176 (11) | 0.0013 (8) | 0.0032 (9) | 0.0004 (8) |
C22 | 0.0171 (12) | 0.0148 (11) | 0.0192 (11) | 0.0013 (9) | 0.0027 (9) | 0.0011 (9) |
C31 | 0.0139 (11) | 0.0114 (11) | 0.0182 (11) | −0.0007 (8) | −0.0003 (9) | −0.0025 (8) |
C41 | 0.0123 (10) | 0.0144 (11) | 0.0109 (10) | 0.0010 (8) | 0.0005 (8) | −0.0004 (8) |
C75 | 0.0174 (12) | 0.0131 (11) | 0.0265 (12) | −0.0014 (9) | 0.0019 (10) | 0.0012 (9) |
C82 | 0.0183 (12) | 0.0131 (11) | 0.0198 (11) | 0.0011 (9) | 0.0031 (9) | −0.0012 (9) |
C24 | 0.0274 (13) | 0.0158 (12) | 0.0211 (12) | −0.0016 (10) | 0.0109 (10) | 0.0018 (9) |
C26 | 0.0143 (11) | 0.0190 (12) | 0.0198 (11) | −0.0018 (9) | 0.0003 (9) | −0.0003 (9) |
C61 | 0.0115 (10) | 0.0096 (10) | 0.0169 (10) | −0.0001 (8) | 0.0019 (8) | 0.0008 (8) |
C74 | 0.0200 (12) | 0.0127 (11) | 0.0234 (12) | 0.0026 (9) | −0.0031 (10) | −0.0052 (9) |
C32 | 0.0216 (12) | 0.0175 (12) | 0.0169 (11) | −0.0034 (9) | 0.0034 (9) | −0.0007 (9) |
C12 | 0.0183 (12) | 0.0187 (12) | 0.0161 (11) | 0.0023 (9) | 0.0002 (9) | −0.0010 (9) |
C46 | 0.0173 (12) | 0.0117 (11) | 0.0240 (12) | −0.0011 (9) | 0.0017 (9) | 0.0039 (9) |
C71 | 0.0113 (10) | 0.0096 (10) | 0.0143 (10) | 0.0018 (8) | 0.0009 (8) | 0.0001 (8) |
C23 | 0.0258 (13) | 0.0174 (12) | 0.0159 (11) | 0.0032 (10) | 0.0026 (10) | 0.0039 (9) |
C63 | 0.0146 (11) | 0.0209 (12) | 0.0200 (11) | 0.0009 (9) | 0.0003 (9) | 0.0041 (9) |
C76 | 0.0139 (11) | 0.0131 (11) | 0.0181 (11) | 0.0023 (8) | 0.0044 (9) | 0.0017 (8) |
C11 | 0.0103 (10) | 0.0143 (11) | 0.0137 (10) | 0.0004 (8) | 0.0010 (8) | 0.0009 (8) |
C83 | 0.0189 (12) | 0.0178 (12) | 0.0201 (11) | −0.0048 (9) | −0.0011 (9) | −0.0019 (9) |
C56 | 0.0263 (13) | 0.0107 (11) | 0.0208 (11) | 0.0004 (9) | 0.0101 (10) | −0.0026 (9) |
C66 | 0.0146 (11) | 0.0153 (11) | 0.0181 (11) | 0.0005 (9) | 0.0026 (9) | −0.0025 (9) |
C25 | 0.0153 (12) | 0.0178 (12) | 0.0296 (13) | −0.0018 (9) | 0.0080 (10) | −0.0012 (10) |
C86 | 0.0169 (11) | 0.0149 (11) | 0.0145 (10) | −0.0016 (9) | 0.0042 (9) | −0.0015 (8) |
C81 | 0.0117 (10) | 0.0134 (10) | 0.0115 (10) | −0.0006 (8) | 0.0020 (8) | 0.0001 (8) |
C64 | 0.0121 (11) | 0.0164 (12) | 0.0308 (13) | 0.0008 (9) | 0.0022 (9) | 0.0083 (10) |
C52 | 0.0165 (12) | 0.0161 (12) | 0.0272 (12) | −0.0011 (9) | 0.0081 (10) | −0.0041 (9) |
C84 | 0.0139 (11) | 0.0263 (13) | 0.0171 (11) | −0.0013 (9) | −0.0007 (9) | 0.0034 (9) |
C54 | 0.0401 (16) | 0.0127 (12) | 0.0406 (15) | −0.0044 (11) | 0.0294 (13) | −0.0043 (10) |
C33 | 0.0297 (14) | 0.0193 (12) | 0.0186 (11) | −0.0096 (10) | 0.0011 (10) | 0.0007 (9) |
C44 | 0.0138 (11) | 0.0210 (12) | 0.0151 (10) | 0.0000 (9) | 0.0014 (9) | 0.0004 (9) |
C34 | 0.0280 (14) | 0.0144 (12) | 0.0242 (12) | −0.0006 (10) | −0.0044 (10) | −0.0054 (9) |
C73 | 0.0187 (11) | 0.0160 (11) | 0.0154 (10) | 0.0065 (9) | 0.0027 (9) | −0.0026 (8) |
C85 | 0.0172 (12) | 0.0210 (12) | 0.0177 (11) | 0.0065 (9) | 0.0048 (9) | 0.0012 (9) |
C62 | 0.0122 (11) | 0.0152 (11) | 0.0153 (10) | 0.0016 (8) | 0.0012 (8) | −0.0022 (8) |
C13 | 0.0217 (12) | 0.0152 (12) | 0.0252 (12) | 0.0030 (9) | 0.0048 (10) | 0.0014 (9) |
C42 | 0.0158 (11) | 0.0088 (10) | 0.0188 (11) | 0.0015 (8) | 0.0036 (9) | −0.0014 (8) |
C51 | 0.0177 (11) | 0.0099 (10) | 0.0185 (11) | −0.0021 (8) | 0.0091 (9) | −0.0046 (8) |
C45 | 0.0164 (12) | 0.0182 (12) | 0.0215 (12) | 0.0045 (9) | 0.0008 (9) | 0.0034 (9) |
C35 | 0.0232 (13) | 0.0271 (14) | 0.0289 (13) | 0.0021 (11) | 0.0030 (11) | −0.0145 (11) |
C53 | 0.0231 (13) | 0.0141 (12) | 0.0413 (15) | −0.0036 (10) | 0.0167 (12) | −0.0067 (10) |
N3 | 0.0147 (10) | 0.0171 (11) | 0.0236 (10) | −0.0013 (8) | 0.0049 (8) | −0.0008 (8) |
N5 | 0.0152 (9) | 0.0155 (10) | 0.0150 (9) | 0.0003 (7) | 0.0008 (7) | −0.0022 (7) |
C2 | 0.0118 (10) | 0.0129 (11) | 0.0198 (11) | −0.0025 (8) | 0.0032 (9) | −0.0011 (8) |
N2 | 0.0209 (11) | 0.0288 (12) | 0.0168 (10) | −0.0036 (9) | 0.0004 (8) | 0.0000 (8) |
N1 | 0.0267 (11) | 0.0165 (11) | 0.0203 (10) | 0.0001 (8) | 0.0042 (8) | −0.0004 (8) |
C1 | 0.0131 (11) | 0.0165 (12) | 0.0122 (10) | 0.0004 (8) | −0.0003 (8) | −0.0017 (8) |
N4 | 0.0195 (10) | 0.0175 (10) | 0.0238 (10) | 0.0004 (8) | −0.0056 (8) | 0.0002 (8) |
C4 | 0.0168 (11) | 0.0094 (10) | 0.0163 (10) | −0.0008 (8) | 0.0035 (9) | −0.0008 (8) |
O1 | 0.0152 (8) | 0.0143 (8) | 0.0196 (8) | 0.0008 (7) | 0.0062 (6) | 0.0033 (7) |
O6 | 0.0185 (9) | 0.0215 (10) | 0.0223 (9) | 0.0044 (7) | −0.0007 (7) | 0.0022 (7) |
O2 | 0.0269 (10) | 0.0161 (9) | 0.0203 (9) | −0.0015 (7) | 0.0038 (8) | 0.0013 (7) |
O4 | 0.0223 (10) | 0.0222 (10) | 0.0247 (9) | −0.0048 (7) | 0.0017 (8) | 0.0058 (7) |
O3 | 0.0249 (10) | 0.0269 (10) | 0.0242 (9) | −0.0010 (8) | 0.0065 (8) | 0.0057 (7) |
O5 | 0.0256 (10) | 0.0248 (10) | 0.0226 (9) | 0.0043 (8) | 0.0023 (8) | −0.0026 (8) |
Re1—N5 | 1.6570 (19) | C32—C33 | 1.388 (3) |
Re1—O1 | 2.4429 (15) | C32—H32 | 0.93 |
Re1—C1 | 2.105 (2) | C12—C11 | 1.388 (3) |
Re1—C2 | 2.109 (2) | C12—C13 | 1.392 (3) |
Re1—C3 | 2.103 (2) | C12—H12 | 0.93 |
Re1—C4 | 2.103 (2) | C46—C45 | 1.380 (3) |
P2—C51 | 1.791 (2) | C46—H46 | 0.93 |
P2—C81 | 1.792 (2) | C71—C76 | 1.397 (3) |
P2—C61 | 1.798 (2) | C23—H23 | 0.93 |
P2—C71 | 1.802 (2) | C63—C64 | 1.384 (3) |
P1—C41 | 1.793 (2) | C63—C62 | 1.388 (3) |
P1—C11 | 1.794 (2) | C63—H63 | 0.93 |
P1—C31 | 1.795 (2) | C76—H76 | 0.93 |
P1—C21 | 1.796 (2) | C83—C84 | 1.389 (3) |
C3—N3 | 1.156 (3) | C83—H83 | 0.93 |
C55—C54 | 1.378 (4) | C56—C51 | 1.390 (3) |
C55—C56 | 1.395 (3) | C56—H56 | 0.93 |
C55—H55 | 0.93 | C66—H66 | 0.93 |
C36—C35 | 1.385 (3) | C25—H25 | 0.93 |
C36—C31 | 1.401 (3) | C86—C85 | 1.379 (3) |
C36—H36 | 0.93 | C86—C81 | 1.394 (3) |
C16—C15 | 1.387 (3) | C86—H86 | 0.93 |
C16—C11 | 1.395 (3) | C64—H64 | 0.93 |
C16—H16 | 0.93 | C52—C53 | 1.376 (3) |
C21—C22 | 1.395 (3) | C52—C51 | 1.400 (3) |
C21—C26 | 1.395 (3) | C52—H52 | 0.93 |
C15—C14 | 1.379 (3) | C84—C85 | 1.383 (3) |
C15—H15 | 0.93 | C84—H84 | 0.93 |
C43—C44 | 1.385 (3) | C54—C53 | 1.387 (4) |
C43—C42 | 1.389 (3) | C54—H54 | 0.93 |
C43—H43 | 0.93 | C33—C34 | 1.379 (3) |
C14—C13 | 1.384 (3) | C33—H33 | 0.93 |
C14—H14 | 0.93 | C44—C45 | 1.388 (3) |
C65—C66 | 1.378 (3) | C44—H44 | 0.93 |
C65—C64 | 1.389 (3) | C34—C35 | 1.385 (3) |
C65—H65 | 0.93 | C34—H34 | 0.93 |
C72—C73 | 1.383 (3) | C73—H73 | 0.93 |
C72—C71 | 1.397 (3) | C85—H85 | 0.93 |
C72—H72 | 0.93 | C62—H62 | 0.93 |
C22—C23 | 1.390 (3) | C13—H13 | 0.93 |
C22—H22 | 0.93 | C42—H42 | 0.93 |
C31—C32 | 1.392 (3) | C45—H45 | 0.93 |
C41—C42 | 1.389 (3) | C35—H35 | 0.93 |
C41—C46 | 1.393 (3) | C53—H53 | 0.93 |
C75—C74 | 1.382 (3) | C2—N2 | 1.150 (3) |
C75—C76 | 1.393 (3) | N1—C1 | 1.147 (3) |
C75—H75 | 0.93 | N4—C4 | 1.150 (3) |
C82—C83 | 1.377 (3) | O1—H1A | 0.85 (2) |
C82—C81 | 1.397 (3) | O1—H1B | 0.847 (19) |
C82—H82 | 0.93 | O6—H6A | 0.841 (9) |
C24—C23 | 1.383 (3) | O6—H6B | 0.843 (9) |
C24—C25 | 1.386 (3) | O2—H2A | 0.843 (19) |
C24—H24 | 0.93 | O2—H2B | 0.844 (10) |
C26—C25 | 1.389 (3) | O4—H4A | 0.85 (2) |
C26—H26 | 0.93 | O4—H4B | 0.851 (9) |
C61—C62 | 1.393 (3) | O3—H3A | 0.840 (9) |
C61—C66 | 1.406 (3) | O3—H3B | 0.84 (2) |
C74—C73 | 1.389 (3) | O5—H5A | 0.85 (2) |
C74—H74 | 0.93 | O5—H5B | 0.85 (2) |
N5—Re1—C4 | 99.12 (8) | C72—C71—P2 | 119.89 (16) |
N5—Re1—C3 | 99.11 (8) | C76—C71—P2 | 120.08 (16) |
C1—Re1—O1 | 79.94 (7) | C24—C23—C22 | 120.4 (2) |
C2—Re1—O1 | 79.51 (7) | C24—C23—H23 | 119.8 |
C3—Re1—O1 | 81.93 (7) | C22—C23—H23 | 119.8 |
C4—Re1—O1 | 82.83 (7) | C64—C63—C62 | 120.3 (2) |
N5—Re1—O1 | 177.87 (7) | C64—C63—H63 | 119.9 |
C1—Re1—C2 | 88.66 (8) | C62—C63—H63 | 119.9 |
C3—Re1—C2 | 92.34 (8) | C75—C76—C71 | 119.7 (2) |
C4—Re1—C3 | 83.26 (8) | C75—C76—H76 | 120.2 |
N5—Re1—C1 | 99.15 (8) | C71—C76—H76 | 120.2 |
C3—Re1—C1 | 161.34 (8) | C12—C11—C16 | 120.3 (2) |
C4—Re1—C1 | 90.14 (8) | C12—C11—P1 | 118.95 (16) |
N5—Re1—C2 | 98.57 (9) | C16—C11—P1 | 120.69 (16) |
C4—Re1—C2 | 162.23 (8) | C82—C83—C84 | 120.8 (2) |
C51—P2—C81 | 109.99 (10) | C82—C83—H83 | 119.6 |
C51—P2—C61 | 106.46 (10) | C84—C83—H83 | 119.6 |
C81—P2—C61 | 110.55 (10) | C51—C56—C55 | 118.9 (2) |
C51—P2—C71 | 108.05 (10) | C51—C56—H56 | 120.5 |
C81—P2—C71 | 109.68 (10) | C55—C56—H56 | 120.5 |
C61—P2—C71 | 112.02 (10) | C65—C66—C61 | 119.6 (2) |
C41—P1—C11 | 111.24 (10) | C65—C66—H66 | 120.2 |
C41—P1—C31 | 108.47 (10) | C61—C66—H66 | 120.2 |
C11—P1—C31 | 109.06 (10) | C24—C25—C26 | 120.1 (2) |
C41—P1—C21 | 108.49 (10) | C24—C25—H25 | 119.9 |
C11—P1—C21 | 108.80 (10) | C26—C25—H25 | 119.9 |
C31—P1—C21 | 110.78 (10) | C85—C86—C81 | 119.9 (2) |
N3—C3—Re1 | 172.85 (19) | C85—C86—H86 | 120.1 |
C54—C55—C56 | 120.6 (2) | C81—C86—H86 | 120.1 |
C54—C55—H55 | 119.7 | C86—C81—C82 | 119.9 (2) |
C56—C55—H55 | 119.7 | C86—C81—P2 | 120.66 (16) |
C35—C36—C31 | 120.0 (2) | C82—C81—P2 | 119.44 (16) |
C35—C36—H36 | 120 | C63—C64—C65 | 120.2 (2) |
C31—C36—H36 | 120 | C63—C64—H64 | 119.9 |
C15—C16—C11 | 119.1 (2) | C65—C64—H64 | 119.9 |
C15—C16—H16 | 120.5 | C53—C52—C51 | 120.1 (2) |
C11—C16—H16 | 120.5 | C53—C52—H52 | 120 |
C22—C21—C26 | 120.2 (2) | C51—C52—H52 | 120 |
C22—C21—P1 | 120.59 (17) | C85—C84—C83 | 119.6 (2) |
C26—C21—P1 | 119.17 (17) | C85—C84—H84 | 120.2 |
C14—C15—C16 | 120.7 (2) | C83—C84—H84 | 120.2 |
C14—C15—H15 | 119.6 | C55—C54—C53 | 120.3 (2) |
C16—C15—H15 | 119.6 | C55—C54—H54 | 119.8 |
C44—C43—C42 | 120.9 (2) | C53—C54—H54 | 119.8 |
C44—C43—H43 | 119.6 | C34—C33—C32 | 120.5 (2) |
C42—C43—H43 | 119.6 | C34—C33—H33 | 119.8 |
C15—C14—C13 | 120.2 (2) | C32—C33—H33 | 119.8 |
C15—C14—H14 | 119.9 | C43—C44—C45 | 119.5 (2) |
C13—C14—H14 | 119.9 | C43—C44—H44 | 120.3 |
C66—C65—C64 | 120.3 (2) | C45—C44—H44 | 120.3 |
C66—C65—H65 | 119.9 | C33—C34—C35 | 120.5 (2) |
C64—C65—H65 | 119.9 | C33—C34—H34 | 119.8 |
C73—C72—C71 | 119.8 (2) | C35—C34—H34 | 119.8 |
C73—C72—H72 | 120.1 | C72—C73—C74 | 119.9 (2) |
C71—C72—H72 | 120.1 | C72—C73—H73 | 120 |
C23—C22—C21 | 119.4 (2) | C74—C73—H73 | 120 |
C23—C22—H22 | 120.3 | C86—C85—C84 | 120.5 (2) |
C21—C22—H22 | 120.3 | C86—C85—H85 | 119.8 |
C32—C31—C36 | 119.8 (2) | C84—C85—H85 | 119.8 |
C32—C31—P1 | 121.00 (17) | C63—C62—C61 | 119.6 (2) |
C36—C31—P1 | 119.15 (17) | C63—C62—H62 | 120.2 |
C42—C41—C46 | 119.4 (2) | C61—C62—H62 | 120.2 |
C42—C41—P1 | 121.03 (16) | C14—C13—C12 | 119.8 (2) |
C46—C41—P1 | 119.48 (17) | C14—C13—H13 | 120.1 |
C74—C75—C76 | 119.8 (2) | C12—C13—H13 | 120.1 |
C74—C75—H75 | 120.1 | C41—C42—C43 | 119.6 (2) |
C76—C75—H75 | 120.1 | C41—C42—H42 | 120.2 |
C83—C82—C81 | 119.4 (2) | C43—C42—H42 | 120.2 |
C83—C82—H82 | 120.3 | C56—C51—C52 | 120.1 (2) |
C81—C82—H82 | 120.3 | C56—C51—P2 | 122.85 (18) |
C23—C24—C25 | 120.2 (2) | C52—C51—P2 | 116.98 (17) |
C23—C24—H24 | 119.9 | C46—C45—C44 | 119.9 (2) |
C25—C24—H24 | 119.9 | C46—C45—H45 | 120 |
C25—C26—C21 | 119.6 (2) | C44—C45—H45 | 120 |
C25—C26—H26 | 120.2 | C34—C35—C36 | 119.8 (2) |
C21—C26—H26 | 120.2 | C34—C35—H35 | 120.1 |
C62—C61—C66 | 119.98 (19) | C36—C35—H35 | 120.1 |
C62—C61—P2 | 122.94 (16) | C52—C53—C54 | 119.9 (2) |
C66—C61—P2 | 116.99 (16) | C52—C53—H53 | 120 |
C75—C74—C73 | 120.8 (2) | C54—C53—H53 | 120 |
C75—C74—H74 | 119.6 | N2—C2—Re1 | 178.9 (2) |
C73—C74—H74 | 119.6 | N1—C1—Re1 | 179.77 (19) |
C33—C32—C31 | 119.5 (2) | N4—C4—Re1 | 175.50 (18) |
C33—C32—H32 | 120.2 | Re1—O1—H1A | 123.7 (18) |
C31—C32—H32 | 120.2 | Re1—O1—H1B | 117.3 (17) |
C11—C12—C13 | 119.7 (2) | H1A—O1—H1B | 108.9 (15) |
C11—C12—H12 | 120.1 | H6A—O6—H6B | 110.9 (15) |
C13—C12—H12 | 120.1 | H2A—O2—H2B | 110.5 (15) |
C45—C46—C41 | 120.7 (2) | H4A—O4—H4B | 108.3 (15) |
C45—C46—H46 | 119.6 | H3A—O3—H3B | 111.3 (16) |
C41—C46—H46 | 119.6 | H5A—O5—H5B | 108.8 (15) |
C72—C71—C76 | 120.04 (19) |
D—H···A | D—H | H···A | D···A | D—H···A |
O1—H1A···O2 | 0.85 (2) | 1.80 (1) | 2.653 (2) | 172 (2) |
O5—H5A···O6 | 0.85 (2) | 1.90 (1) | 2.736 (2) | 169 (3) |
O5—H5B···N3 | 0.85 (1) | 2.28 (2) | 3.083 (3) | 158 (2) |
O3—H3B···N1 | 0.84 (2) | 2.05 (1) | 2.866 (3) | 162 (2) |
O4—H4A···N2 | 0.85 (2) | 2.11 (1) | 2.957 (3) | 170 (3) |
O6—H6B···N4 | 0.84 (1) | 2.01 (1) | 2.849 (2) | 171 (2) |
C34—H34···O2 | 0.93 | 2.59 | 3.482 (3) | 161 |
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