μ-Hydro­xo-bis[(4,4′-di­methyl-2,2′-bi­pyridine)tri­carbonylrhenium(I)] perrhenate acetone hemisolvate

The title compound, [Re₂(OH)(C₁₂H₁₂N₂)₂(CO)₆][ReO₄]·0.5C₃H₆O, is the first crystal structure reported for a hydro­xo-bridged binuclear rhenium complex containing bi­pyridine or substituted bi­pyridine ligands. The cation has distorted octahedral coord­ination about both rhenium centers, resulting from geometric constraints imposed by the chelating 4,4′-di­methyl-2,2′-bi­pyridine ligands, which are involved in an intermolecular π–π stacking interaction. The distance between the rhenium atoms is 4.0185 (3) Å, with no metal–metal bond. The H atom of the bridging hydro­xo ligand was directly located in the crystallographic analysis, and is hydrogen-bonded to the perrhenate. The acetone solvent molecule is disordered.

Key indicators

• Single-crystal X-ray study
• T = 110 K
• Mean [sigma](C-C) = 0.007 Å
• H-atom completeness 90%
• Disorder in solvent or counterion
• R factor = 0.027
• wR factor = 0.076
• Data-to-parameter ratio = 17.5

checkCIF/PLATON results

No syntax errors found



Alert level A
PLAT029_ALERT_3_A _diffrn_measured_fraction_theta_full Low .......       0.93

Alert level C
REFLT03_ALERT_3_C  Reflection count < 95% complete
           From the CIF: _diffrn_reflns_theta_max           28.30
           From the CIF: _diffrn_reflns_theta_full           0.00
           From the CIF: _reflns_number_total               7989
           TEST2: Reflns within _diffrn_reflns_theta_max
           Count of symmetry unique reflns         8581
           Completeness (_total/calc)             93.10%

Author Response: Completeness of data is 99.81% for 25.07 theta max

PLAT041_ALERT_1_C Calc. and Rep. SumFormula Strings    Differ ....          ?
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ ....          ?
PLAT068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)...          ?
PLAT244_ALERT_4_C Low Solvent  U(eq) as Compared to Neighbors ....        Re3
PLAT244_ALERT_4_C Low Solvent  U(eq) as Compared to Neighbors ....        C60
PLAT302_ALERT_4_C Anion/Solvent Disorder .........................      22.00 Perc.

Author Response: A disordered acetone solvate (atoms O60, C60, C61, C62 and O60#1 , C60#1, C61#1, C62#1 generated by -x, -y, -z+2) is located at each corner of the unit cell; see _publ_section_exptl_refinement

Alert level G
FORMU01_ALERT_2_G  There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
            Atom count from _chemical_formula_sum:C31.5 H28 N4 O11.5 Re3
            Atom count from the _atom_site data:  C31.5 H25 N4 O11.5 Re3

Author Response: Three H atoms on each of the half-occupancy methyl carbons (C61 and C62) in the disordered acetone solvate are not included in the model thus accounting for the discrepancy between the atom counts in the _chemical_formula_sum and the formula from the _atom_site* data.

CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.

Author Response: Yes, this is intentional.

            Three H atoms on each of the half-occupancy methyl carbons
            (C61 and C62) in the disordered acetone solvate are not
            included in the model thus accounting for the discrepancy
            between the atom counts in the _chemical_formula_sum and
            the formula from the _atom_site* data which results in a
            difference of 12 H atoms between Z*formula and cif sites.

CELLZ01_ALERT_1_G WARNING: H atoms missing from atom site list. Is this intentional?
           From the CIF: _cell_formula_units_Z    4
           From the CIF: _chemical_formula_sum  C31.50 H28 N4 O11.50 Re3
           TEST: Compare cell contents of formula and atom_site data

           atom    Z*formula  cif sites diff
           C        126.00    126.00    0.00
           H        112.00    100.00   12.00
           N         16.00     16.00    0.00
           O         46.00     46.00    0.00
           Re        12.00     12.00    0.00

Author Response: Yes, this is intentional.

            Three H atoms on each of the half-occupancy methyl carbons
            (C61 and C62) in the disordered acetone solvate are not
            included in the model thus accounting for the discrepancy
            between the atom counts in the _chemical_formula_sum and
            the formula from the _atom_site* data which results in a
            difference of 12 H atoms between Z*formula and cif sites.


   1 ALERT level A = In general: serious problem
   0 ALERT level B = Potentially serious problem
   7 ALERT level C = Check and explain
   3 ALERT level G = General alerts; check

   5 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
   2 ALERT type 3 Indicator that the structure quality may be low
   3 ALERT type 4 Improvement, methodology, query or suggestion

---

Computing details

Data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2001); data reduction: SAINT; program(s) used to solve structure: SHELXS (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: SHELXTL (Bruker, 2001); software used to prepare material for publication: SHELXTL.

µ-Hydroxo bis-[Tricarbonyl(4,4'-dimethyl-2,2'-bipyridine) rhenium(I)] perrhenate acetone solvate

Crystal data

[Re2(C12H12N2)2(Co)6(OH)]ReO4·0.5C3H6O	F(000) = 2248
Mr = 1205.16	Dx = 2.320 Mg m^−3
Monoclinic, P21/c	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2ybc	Cell parameters from 8716 reflections
a = 10.6841 (7) Å	θ = 2.4–28.1°
b = 31.649 (2) Å	µ = 10.56 mm^−1
c = 10.5758 (7) Å	T = 110 K
β = 105.222 (1)°	Rect-plate, yellow
V = 3450.7 (4) Å^3	0.29 × 0.14 × 0.01 mm
Z = 4

Data collection

SMART APEX CCD diffractometer	7989 independent reflections
Radiation source: normal-focus sealed tube	7184 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.042
ω scans	θmax = 28.3°, θmin = 2.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 2001)	h = −13→14
Tmin = 0.180, Tmax = 0.900	k = −41→42
29838 measured reflections	l = −14→14

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)] = 0.027	Hydrogen site location: mixed
wR(F^2) = 0.076	H atoms treated by a mixture of independent and constrained refinement
S = 1.07	w = 1/[σ^2(Fo^2) + (0.039P)^2 + 1.9625P] where P = (Fo^2 + 2Fc^2)/3
7989 reflections	(Δ/σ)max = 0.003
457 parameters	Δρmax = 3.70 e Å^−3
0 restraints	Δρmin = −1.94 e Å^−3

Special details

Experimental. Data were collected with a Bruker SMART APEX CCD-based diffractometer using /w-scans of width 0.3 °. and 25 s duration at a crystal-to-detector distance of 4.908 cm. Intensity decay over the course of the data collection was evaluated by recollecting the first 50 frames of data at the end of the experiment. No significant decay was noted.

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.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Re1	0.77598 (2)	0.07054 (1)	0.27710 (2)	0.01529 (6)
Re2	0.69927 (2)	0.19502 (1)	0.26189 (2)	0.01525 (6)
O1	0.6890 (3)	0.04395 (10)	−0.0131 (3)	0.0286 (7)
O2	1.0227 (3)	0.11192 (11)	0.2342 (3)	0.0304 (8)
O3	0.9234 (3)	−0.01352 (10)	0.3404 (3)	0.0305 (8)
O4	0.9016 (4)	0.20196 (11)	0.1017 (4)	0.0336 (8)
O5	0.9319 (3)	0.19761 (11)	0.5047 (4)	0.0298 (8)
O6	0.7178 (3)	0.29158 (10)	0.2805 (3)	0.0254 (7)
O7	0.6672 (3)	0.12867 (9)	0.2469 (3)	0.0184 (6)
H7O	0.614 (6)	0.121 (2)	0.189 (6)	0.044 (19)*
N1	0.8064 (4)	0.08676 (11)	0.4823 (3)	0.0171 (7)
N2	0.6004 (3)	0.04996 (11)	0.3286 (3)	0.0165 (7)
N3	0.5453 (4)	0.18840 (11)	0.3602 (3)	0.0176 (7)
N4	0.5166 (4)	0.19858 (10)	0.1072 (3)	0.0174 (8)
C1	0.7228 (4)	0.05406 (13)	0.0945 (4)	0.0194 (9)
C2	0.9284 (5)	0.09566 (14)	0.2488 (4)	0.0213 (9)
C3	0.8673 (4)	0.01789 (14)	0.3160 (4)	0.0212 (9)
C4	0.8243 (5)	0.19801 (15)	0.1602 (5)	0.0265 (10)
C5	0.8444 (5)	0.19465 (13)	0.4134 (5)	0.0207 (9)
C6	0.7109 (4)	0.25487 (14)	0.2736 (4)	0.0189 (9)
C7	0.9200 (4)	0.10058 (14)	0.5611 (4)	0.0216 (9)
H7	0.9934	0.1027	0.5265	0.026*
C8	0.9333 (5)	0.11177 (14)	0.6907 (5)	0.0247 (10)
H8	1.0150	0.1209	0.7435	0.030*
C9	0.8272 (5)	0.10965 (14)	0.7436 (4)	0.0224 (10)
C10	0.7113 (5)	0.09372 (13)	0.6632 (4)	0.0208 (9)
H10	0.6377	0.0903	0.6967	0.025*
C11	0.7042 (4)	0.08296 (13)	0.5340 (4)	0.0186 (9)
C12	0.5853 (4)	0.06361 (12)	0.4462 (4)	0.0165 (8)
C13	0.4713 (4)	0.05874 (13)	0.4805 (4)	0.0196 (9)
H13	0.4638	0.0694	0.5621	0.024*
C14	0.3660 (4)	0.03823 (13)	0.3971 (4)	0.0211 (9)
C15	0.3837 (4)	0.02307 (14)	0.2792 (4)	0.0214 (9)
H15	0.3158	0.0081	0.2202	0.026*
C16	0.5008 (4)	0.02982 (13)	0.2476 (4)	0.0196 (9)
H16	0.5103	0.0198	0.1659	0.024*
C17	0.8394 (5)	0.12219 (16)	0.8835 (4)	0.0295 (11)
H17A	0.8822	0.0995	0.9421	0.044*
H17B	0.7529	0.1272	0.8959	0.044*
H17C	0.8911	0.1481	0.9037	0.044*
C18	0.2399 (5)	0.03322 (16)	0.4316 (5)	0.0307 (11)
H18A	0.1786	0.0547	0.3857	0.046*
H18B	0.2538	0.0366	0.5264	0.046*
H18C	0.2045	0.0050	0.4053	0.046*
C19	0.5664 (4)	0.18187 (13)	0.4905 (4)	0.0165 (8)
H19	0.6523	0.1841	0.5450	0.020*
C20	0.4668 (4)	0.17210 (13)	0.5469 (4)	0.0196 (9)
H20	0.4851	0.1682	0.6390	0.023*
C21	0.3409 (5)	0.16804 (14)	0.4704 (4)	0.0209 (9)
C22	0.3195 (4)	0.17544 (14)	0.3365 (4)	0.0212 (9)
H22	0.2341	0.1733	0.2806	0.025*
C23	0.4216 (4)	0.18593 (12)	0.2842 (4)	0.0172 (8)
C24	0.4054 (5)	0.19548 (12)	0.1429 (4)	0.0187 (9)
C25	0.2854 (5)	0.20235 (14)	0.0566 (4)	0.0215 (9)
H25	0.2091	0.2004	0.0863	0.026*
C26	0.2759 (5)	0.21226 (13)	−0.0749 (4)	0.0232 (10)
C27	0.3910 (5)	0.21361 (13)	−0.1110 (4)	0.0261 (11)
H27	0.3888	0.2192	−0.1999	0.031*
C28	0.5084 (5)	0.20709 (13)	−0.0219 (4)	0.0225 (10)
H28	0.5856	0.2085	−0.0503	0.027*
C29	0.2305 (5)	0.15688 (18)	0.5268 (5)	0.0335 (12)
H29A	0.1837	0.1826	0.5383	0.050*
H29B	0.2642	0.1431	0.6119	0.050*
H29C	0.1712	0.1376	0.4671	0.050*
C30	0.1456 (6)	0.22050 (16)	−0.1696 (5)	0.0339 (12)
H30A	0.1569	0.2387	−0.2408	0.051*
H30B	0.0886	0.2345	−0.1235	0.051*
H30C	0.1067	0.1936	−0.2060	0.051*
Re3	0.37483 (2)	0.09301 (1)	0.89115 (2)	0.02158 (6)
O8	0.4668 (5)	0.10920 (15)	0.7886 (5)	0.0611 (14)
O9	0.2276 (3)	0.11873 (12)	0.8469 (4)	0.0397 (9)
O10	0.3519 (4)	0.03912 (12)	0.8818 (5)	0.0542 (13)
O11	0.4516 (4)	0.10585 (11)	1.0507 (3)	0.0361 (9)
O60	−0.0967 (9)	0.0157 (3)	0.8430 (8)	0.050 (2)*	0.50
C60	−0.0244 (13)	0.0084 (4)	0.9482 (11)	0.041 (3)*	0.50
C61	0.0916 (18)	0.0397 (6)	0.9980 (16)	0.055 (4)*	0.50
C62	−0.050 (2)	−0.0297 (7)	1.014 (2)	0.078 (6)*	0.50

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Re1	0.01409 (10)	0.01218 (9)	0.01857 (10)	0.00078 (6)	0.00249 (7)	−0.00059 (6)
Re2	0.01703 (10)	0.01150 (9)	0.01687 (9)	−0.00034 (6)	0.00385 (7)	−0.00073 (6)
O1	0.033 (2)	0.0266 (17)	0.0254 (18)	0.0035 (15)	0.0063 (15)	−0.0036 (14)
O2	0.0199 (18)	0.0326 (19)	0.0384 (19)	−0.0043 (15)	0.0070 (15)	0.0031 (15)
O3	0.031 (2)	0.0228 (17)	0.0370 (19)	0.0150 (15)	0.0073 (16)	0.0043 (14)
O4	0.040 (2)	0.0302 (18)	0.039 (2)	−0.0081 (16)	0.0259 (18)	−0.0063 (15)
O5	0.0192 (19)	0.0274 (18)	0.036 (2)	0.0004 (14)	−0.0059 (16)	−0.0003 (14)
O6	0.036 (2)	0.0143 (16)	0.0237 (16)	−0.0036 (14)	0.0049 (14)	−0.0019 (12)
O7	0.0188 (17)	0.0132 (15)	0.0199 (16)	0.0009 (13)	−0.0010 (13)	−0.0018 (12)
N1	0.0155 (19)	0.0141 (17)	0.0196 (18)	0.0005 (14)	0.0005 (15)	0.0003 (13)
N2	0.0132 (18)	0.0158 (17)	0.0196 (17)	0.0015 (14)	0.0028 (14)	−0.0007 (13)
N3	0.0162 (19)	0.0185 (17)	0.0187 (18)	0.0013 (15)	0.0052 (15)	0.0005 (14)
N4	0.025 (2)	0.0046 (15)	0.0208 (18)	−0.0007 (14)	0.0027 (16)	0.0000 (12)
C1	0.017 (2)	0.015 (2)	0.027 (2)	0.0017 (17)	0.0064 (18)	−0.0012 (17)
C2	0.019 (2)	0.020 (2)	0.024 (2)	0.0025 (18)	0.0028 (19)	−0.0008 (17)
C3	0.017 (2)	0.020 (2)	0.026 (2)	−0.0021 (18)	0.0065 (19)	−0.0028 (17)
C4	0.027 (3)	0.025 (2)	0.028 (2)	−0.001 (2)	0.009 (2)	−0.0038 (18)
C5	0.023 (3)	0.014 (2)	0.025 (2)	0.0005 (17)	0.009 (2)	−0.0003 (16)
C6	0.018 (2)	0.022 (2)	0.015 (2)	0.0014 (17)	0.0012 (17)	0.0010 (16)
C7	0.015 (2)	0.020 (2)	0.026 (2)	0.0003 (17)	−0.0019 (18)	0.0011 (17)
C8	0.021 (2)	0.022 (2)	0.026 (2)	−0.0006 (19)	−0.0036 (19)	−0.0006 (18)
C9	0.030 (3)	0.016 (2)	0.016 (2)	0.0003 (19)	−0.0027 (18)	−0.0004 (16)
C10	0.022 (2)	0.017 (2)	0.022 (2)	0.0018 (17)	0.0042 (19)	0.0016 (16)
C11	0.024 (2)	0.0085 (18)	0.021 (2)	0.0027 (17)	0.0023 (18)	0.0021 (15)
C12	0.020 (2)	0.0089 (18)	0.019 (2)	0.0019 (16)	0.0024 (17)	0.0013 (15)
C13	0.021 (2)	0.013 (2)	0.022 (2)	0.0038 (17)	0.0016 (18)	0.0018 (16)
C14	0.017 (2)	0.013 (2)	0.032 (2)	0.0021 (17)	0.0032 (19)	0.0052 (17)
C15	0.017 (2)	0.018 (2)	0.027 (2)	−0.0013 (17)	0.0000 (18)	−0.0011 (17)
C16	0.022 (2)	0.0109 (19)	0.022 (2)	0.0014 (17)	−0.0006 (18)	−0.0010 (16)
C17	0.037 (3)	0.028 (2)	0.018 (2)	0.001 (2)	−0.002 (2)	−0.0012 (18)
C18	0.019 (3)	0.029 (3)	0.041 (3)	0.000 (2)	0.003 (2)	0.005 (2)
C19	0.016 (2)	0.015 (2)	0.0155 (19)	0.0005 (16)	−0.0007 (16)	−0.0002 (15)
C20	0.023 (2)	0.018 (2)	0.018 (2)	0.0015 (18)	0.0050 (18)	0.0019 (16)
C21	0.020 (2)	0.017 (2)	0.026 (2)	−0.0012 (18)	0.0073 (19)	−0.0013 (17)
C22	0.014 (2)	0.022 (2)	0.027 (2)	0.0011 (17)	0.0031 (18)	−0.0009 (17)
C23	0.020 (2)	0.0088 (18)	0.020 (2)	0.0035 (16)	0.0005 (17)	−0.0022 (15)
C24	0.023 (2)	0.0084 (19)	0.023 (2)	0.0013 (16)	0.0028 (18)	−0.0008 (15)
C25	0.021 (2)	0.018 (2)	0.022 (2)	0.0023 (18)	−0.0004 (18)	−0.0017 (17)
C26	0.028 (3)	0.010 (2)	0.023 (2)	−0.0010 (18)	−0.0068 (19)	−0.0014 (16)
C27	0.046 (3)	0.012 (2)	0.017 (2)	−0.001 (2)	0.001 (2)	0.0005 (15)
C28	0.034 (3)	0.0116 (19)	0.023 (2)	−0.0038 (19)	0.008 (2)	−0.0011 (16)
C29	0.022 (3)	0.052 (3)	0.029 (3)	−0.006 (2)	0.010 (2)	0.000 (2)
C30	0.041 (3)	0.024 (2)	0.027 (3)	0.002 (2)	−0.009 (2)	0.0015 (19)
Re3	0.01847 (11)	0.01695 (10)	0.02495 (10)	0.00191 (7)	−0.00206 (8)	−0.00318 (6)
O8	0.066 (3)	0.068 (3)	0.063 (3)	0.041 (3)	0.041 (3)	0.038 (2)
O9	0.0165 (18)	0.0292 (19)	0.065 (3)	0.0063 (15)	−0.0047 (17)	−0.0052 (18)
O10	0.040 (3)	0.0207 (19)	0.090 (3)	−0.0010 (17)	−0.004 (2)	−0.019 (2)
O11	0.038 (2)	0.0299 (19)	0.0320 (19)	0.0043 (17)	−0.0066 (16)	−0.0031 (15)

Geometric parameters (Å, º)

Re1—C1	1.936 (4)	C14—C18	1.494 (7)
Re1—C2	1.905 (5)	C15—C16	1.393 (6)
Re1—C3	1.920 (5)	C15—H15	0.95
Re1—N1	2.169 (4)	C16—H16	0.95
Re1—N2	2.186 (4)	C17—H17A	0.98
Re1—O7	2.155 (3)	C17—H17B	0.98
Re2—C4	1.925 (5)	C17—H17C	0.98
Re2—C5	1.915 (5)	C18—H18A	0.98
Re2—C6	1.900 (5)	C18—H18B	0.98
Re2—N3	2.175 (4)	C18—H18C	0.98
Re2—N4	2.196 (4)	C19—C20	1.385 (6)
Re2—O7	2.127 (3)	C19—H19	0.95
O1—C1	1.145 (5)	C20—C21	1.381 (7)
O2—C2	1.177 (6)	C20—H20	0.95
O3—C3	1.154 (6)	C21—C22	1.393 (6)
O4—C4	1.162 (6)	C21—C29	1.498 (6)
O5—C5	1.158 (6)	C22—C23	1.387 (6)
O6—C6	1.165 (5)	C22—H22	0.95
O7—H7O	0.76 (7)	C23—C24	1.490 (6)
N1—C7	1.352 (6)	C24—C25	1.382 (6)
N1—C11	1.349 (6)	C25—C26	1.402 (6)
N2—C16	1.339 (5)	C25—H25	0.95
N2—C12	1.366 (5)	C26—C27	1.380 (7)
N3—C19	1.353 (5)	C26—C30	1.509 (7)
N3—C23	1.357 (6)	C27—C28	1.372 (7)
N4—C24	1.341 (6)	C27—H27	0.95
N4—C28	1.372 (6)	C28—H28	0.95
C7—C8	1.386 (6)	C29—H29A	0.98
C7—H7	0.95	C29—H29B	0.98
C8—C9	1.391 (7)	C29—H29C	0.98
C8—H8	0.95	C30—H30A	0.98
C9—C10	1.399 (6)	C30—H30B	0.98
C9—C17	1.505 (6)	C30—H30C	0.98
C10—C11	1.391 (6)	Re3—O11	1.720 (3)
C10—H10	0.95	Re3—O10	1.722 (4)
C11—C12	1.493 (6)	Re3—O9	1.724 (3)
C12—C13	1.368 (6)	Re3—O8	1.722 (4)
C13—C14	1.395 (6)	O60—C60	1.199 (15)
C13—H13	0.95	C60—C62	1.45 (3)
C14—C15	1.395 (6)	C60—C61	1.56 (2)
C2—Re1—C3	89.35 (19)	C13—C14—C18	121.6 (4)
C2—Re1—C1	89.70 (19)	C15—C14—C18	121.6 (4)
C3—Re1—C1	88.81 (18)	C16—C15—C14	120.2 (4)
C2—Re1—O7	94.05 (16)	C16—C15—H15	119.9
C3—Re1—O7	175.33 (15)	C14—C15—H15	119.9
C1—Re1—O7	94.41 (15)	N2—C16—C15	122.2 (4)
C2—Re1—N1	98.54 (16)	N2—C16—H16	118.9
C3—Re1—N1	93.26 (16)	C15—C16—H16	118.9
C1—Re1—N1	171.52 (16)	C9—C17—H17A	109.5
O7—Re1—N1	83.08 (12)	C9—C17—H17B	109.5
C2—Re1—N2	171.33 (16)	H17A—C17—H17B	109.5
C3—Re1—N2	96.26 (16)	C9—C17—H17C	109.5
C1—Re1—N2	97.00 (16)	H17A—C17—H17C	109.5
O7—Re1—N2	80.00 (12)	H17B—C17—H17C	109.5
N1—Re1—N2	74.60 (13)	C14—C18—H18A	109.5
C6—Re2—C5	85.80 (18)	C14—C18—H18B	109.5
C6—Re2—C4	86.80 (19)	H18A—C18—H18B	109.5
C5—Re2—C4	86.6 (2)	C14—C18—H18C	109.5
C6—Re2—O7	174.61 (16)	H18A—C18—H18C	109.5
C5—Re2—O7	97.78 (15)	H18B—C18—H18C	109.5
C4—Re2—O7	97.41 (16)	N3—C19—C20	122.1 (4)
C6—Re2—N3	96.30 (16)	N3—C19—H19	118.9
C5—Re2—N3	98.47 (17)	C20—C19—H19	118.9
C4—Re2—N3	174.26 (17)	C19—C20—C21	120.5 (4)
O7—Re2—N3	79.22 (13)	C19—C20—H20	119.7
C6—Re2—N4	91.58 (15)	C21—C20—H20	119.7
C5—Re2—N4	171.76 (16)	C20—C21—C22	117.1 (4)
C4—Re2—N4	101.11 (18)	C20—C21—C29	122.4 (4)
O7—Re2—N4	84.32 (12)	C22—C21—C29	120.5 (4)
N3—Re2—N4	74.03 (14)	C21—C22—C23	120.6 (4)
Re2—O7—Re1	139.63 (17)	C21—C22—H22	119.7
Re2—O7—H7O	116 (5)	C23—C22—H22	119.7
Re1—O7—H7O	96 (5)	N3—C23—C22	121.6 (4)
C7—N1—C11	118.0 (4)	N3—C23—C24	114.9 (4)
C7—N1—Re1	124.6 (3)	C22—C23—C24	123.5 (4)
C11—N1—Re1	117.4 (3)	N4—C24—C25	122.6 (4)
C16—N2—C12	118.0 (4)	N4—C24—C23	114.8 (4)
C16—N2—Re1	124.9 (3)	C25—C24—C23	122.6 (4)
C12—N2—Re1	116.5 (3)	C24—C25—C26	120.2 (4)
C19—N3—C23	118.1 (4)	C24—C25—H25	119.9
C19—N3—Re2	123.8 (3)	C26—C25—H25	119.9
C23—N3—Re2	117.7 (3)	C27—C26—C25	116.4 (4)
C24—N4—C28	117.7 (4)	C27—C26—C30	123.0 (4)
C24—N4—Re2	117.8 (3)	C25—C26—C30	120.7 (5)
C28—N4—Re2	124.3 (3)	C28—C27—C26	121.7 (4)
O1—C1—Re1	178.5 (4)	C28—C27—H27	119.2
O2—C2—Re1	178.1 (4)	C26—C27—H27	119.2
O3—C3—Re1	179.2 (5)	N4—C28—C27	121.4 (4)
O4—C4—Re2	176.3 (4)	N4—C28—H28	119.3
O5—C5—Re2	175.0 (4)	C27—C28—H28	119.3
O6—C6—Re2	179.8 (5)	C21—C29—H29A	109.5
N1—C7—C8	122.3 (4)	C21—C29—H29B	109.5
N1—C7—H7	118.8	H29A—C29—H29B	109.5
C8—C7—H7	118.8	C21—C29—H29C	109.5
C7—C8—C9	120.2 (4)	H29A—C29—H29C	109.5
C7—C8—H8	119.9	H29B—C29—H29C	109.5
C9—C8—H8	119.9	C26—C30—H30A	109.5
C8—C9—C10	117.2 (4)	C26—C30—H30B	109.5
C8—C9—C17	120.9 (4)	H30A—C30—H30B	109.5
C10—C9—C17	121.8 (4)	C26—C30—H30C	109.5
C11—C10—C9	119.8 (4)	H30A—C30—H30C	109.5
C11—C10—H10	120.1	H30B—C30—H30C	109.5
C9—C10—H10	120.1	O11—Re3—O10	108.3 (2)
N1—C11—C10	122.3 (4)	O11—Re3—O9	108.71 (19)
N1—C11—C12	115.6 (4)	O10—Re3—O9	110.23 (19)
C10—C11—C12	122.0 (4)	O11—Re3—O8	110.1 (2)
N2—C12—C13	122.1 (4)	O10—Re3—O8	110.8 (2)
N2—C12—C11	114.3 (4)	O9—Re3—O8	108.6 (2)
C13—C12—C11	123.5 (4)	C62^i—C60—O60	118.4 (18)
C12—C13—C14	120.8 (4)	O60—C60—C62	116.6 (17)
C12—C13—H13	119.6	O60—C60—C61	116.8 (11)
C14—C13—H13	119.6	C62—C60—C61	126.6 (16)
C13—C14—C15	116.7 (4)

Symmetry code: (i) −x, −y, −z+2.