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The crystal structure of the title compound, {[Cu2(C10H8O6)2(C5H5N)4(H2O)2]·4H2O}n, consists of linear chains built from Cu(C10H8O6)(C5H5N)2(H2O) units (where the CuB atom lies on a general position) bridged through the dicarboxylate dianion to two other Cu(C10H8O6)(C5H5N)2(H2O) units (the CuA and CuC atoms lie on different inversion centers). The CuA and CuC atoms of the two units at the inversion centers are disordered over two sites, and the disorder is such that these atoms are five-coordinate in one component as both are coordinated by water molecules, whereas the CuA′ and CuC′ component atoms are only four-coordinate, as the metal–water distance exceeds 3 Å. The compound is formally a co-crystal, namely catena-poly[[[aquabis(pyridine-κN)copper(II)]-μ-1,3-phenylenedioxydiacetato-κ2-O:O′] dihydrate]–catena-poly[[[bis<(pyridine-κN)copper(II)]-μ-1,3-phenylenedioxydiacetato-κ2-O:O′] trihydrate] (1.5/0.5).
Supporting information
CCDC reference: 252786
Key indicators
- Single-crystal X-ray study
- T = 295 K
- Mean (C-C) = 0.006 Å
- R factor = 0.058
- wR factor = 0.135
- Data-to-parameter ratio = 16.1
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT242_ALERT_2_A Check Low U(eq) as Compared to Neighbors for Cu1
| Author Response: The Cu1/Cu1' and Cu3/Cu3' atoms are disordered. The disorder is
described in the refinement section.
|
Alert level B
ABSTM02_ALERT_3_B The ratio of expected to reported Tmax/Tmin(RR') is < 0.75
Tmin and Tmax reported: 0.432 0.827
Tmin' and Tmax expected: 0.668 0.820
RR' = 0.642
Please check that your absorption correction is appropriate.
PLAT061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.63
PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors for O1
PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors for O3W
PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors for O11
PLAT241_ALERT_2_B Check High U(eq) as Compared to Neighbors for O12
PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors for Cu1'
| Author Response: The Cu1/Cu1' and Cu3/Cu3' atoms are disordered. The disorder is
described in the refinement section.
|
PLAT242_ALERT_2_B Check Low U(eq) as Compared to Neighbors for Cu3
| Author Response: The Cu1/Cu1' and Cu3/Cu3' atoms are disordered. The disorder is
described in the refinement section.
|
PLAT420_ALERT_2_B D-H Without Acceptor O3W - H3W1 ... ?
PLAT420_ALERT_2_B D-H Without Acceptor O3W - H3W2 ... ?
Alert level C
PLAT042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ?
PLAT076_ALERT_1_C Occupancy 0.50 less than 1.0 for Sp.pos . Cu3'
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.53
PLAT152_ALERT_1_C Supplied and Calc Volume s.u. Inconsistent ..... ?
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.76 Ratio
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for O3
PLAT241_ALERT_2_C Check High U(eq) as Compared to Neighbors for N1
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for Cu3'
| Author Response: The Cu1/Cu1' and Cu3/Cu3' atoms are disordered. The disorder is
described in the refinement section.
|
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for C6
| Author Response: The Cu1/Cu1' and Cu3/Cu3' atoms are disordered. The disorder is
described in the refinement section.
|
PLAT242_ALERT_2_C Check Low U(eq) as Compared to Neighbors for C35
| Author Response: The Cu1/Cu1' and Cu3/Cu3' atoms are disordered. The disorder is
described in the refinement section.
|
PLAT301_ALERT_3_C Main Residue Disorder ......................... 2.00 Perc.
PLAT417_ALERT_2_C Short Inter D-H..H-D H2W1 .. H4W1 .. 2.14 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H2# .. O12 .. 2.83 Ang.
PLAT480_ALERT_4_C Long H...A H-Bond Reported H6# .. O3 .. 2.67 Ang.
PLAT720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 12
PLAT731_ALERT_1_C Bond Calc 0.83(4), Rep 0.840(10) ...... 4.00 su-Rat
O1W -H1W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H1W2 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O2W -H2W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O2W -H2W2 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.86(4), Rep 0.860(10) ...... 4.00 su-Rat
O3W -H3W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O3W -H3W2 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.86(4), Rep 0.860(10) ...... 4.00 su-Rat
O4W -H4W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.860(10) ...... 3.00 su-Rat
O4W -H4W2 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.860(10) ...... 3.00 su-Rat
O5W -H5W1 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.85(3), Rep 0.860(10) ...... 3.00 su-Rat
O5W -H5W2 1.555 1.555
PLAT731_ALERT_1_C Bond Calc 0.86(3), Rep 0.860(10) ...... 3.00 su-Rat
O6W -H6W2 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 111(5), Rep 110.6(18) ...... 2.78 su-Rat
H1W1 -O1W -H1W2 1.555 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 109(4), Rep 108.4(17) ...... 2.35 su-Rat
H3W1 -O3W -H3W2 1.555 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 108(4), Rep 108.0(17) ...... 2.35 su-Rat
H4W1 -O4W -H4W2 1.555 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 108(4), Rep 107.7(16) ...... 2.50 su-Rat
H5W1 -O5W -H5W2 1.555 1.555 1.555
PLAT732_ALERT_1_C Angle Calc 108(5), Rep 107.7(17) ...... 2.94 su-Rat
H6W1 -O6W -H6W2 1.555 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H2# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O1W -H2# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O2W -H4# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O2W -H3# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.850(10) ...... 3.00 su-Rat
O3W -H6# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.86(4), Rep 0.860(10) ...... 4.00 su-Rat
O3W -H5# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.86(3), Rep 0.860(10) ...... 3.00 su-Rat
O4W -H8# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.86(4), Rep 0.860(10) ...... 4.00 su-Rat
O4W -H7# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.86(3), Rep 0.860(10) ...... 3.00 su-Rat
O5W -H9# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.85(3), Rep 0.860(10) ...... 3.00 su-Rat
O5W -H10# 1.555 1.555
PLAT735_ALERT_1_C D-H Calc 0.86(3), Rep 0.860(10) ...... 3.00 su-Rat
O6W -H12# 1.555 1.555
PLAT736_ALERT_1_C H...A Calc 1.90(3), Rep 1.900(10) ...... 3.00 su-Rat
H3# -O4W 1.555 1.555
PLAT779_ALERT_2_C Suspect or Irrelevant (Bond) Angle in CIF ...... 30.85 Deg.
CU1 -O1 -CU1 1.555 1.555 2.575
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
PLAT804_ALERT_4_C ARU-Pack Problem in PLATON Analysis ............ !
1 ALERT level A = In general: serious problem
10 ALERT level B = Potentially serious problem
53 ALERT level C = Check and explain
0 ALERT level G = General alerts; check
31 ALERT type 1 CIF construction/syntax error, inconsistent or missing data
18 ALERT type 2 Indicator that the structure model may be wrong or deficient
3 ALERT type 3 Indicator that the structure quality may be low
12 ALERT type 4 Improvement, methodology, query or suggestion
Data collection: RAPID-AUTO (Rigaku, 1998); cell refinement: RAPID-AUTO; data reduction: CrystalStructure (Rigaku/MSC, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 1997); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997); molecular graphics: ORTEPII (Johnson, 1976); software used to prepare material for publication: SHELXL97.
catena-poly[[[aquabis(pyridine-
κN)copper(II)]-µ-1,3-phenylenedioxydiacetato-
κ2-O:
O']
dihydrate]–
catena-poly[[[bis(pyridine-
κN)copper(II)]-
µ-1,3-phenylenedioxydiacetato-
κ2-O:
O'] trihydrate] (1.5/0.5)
top
Crystal data top
[Cu2(C10H8O6)2(C5H5N)4(H2O)2]·4H2O | Z = 2 |
Mr = 999.90 | F(000) = 1036 |
Triclinic, P1 | Dx = 1.503 Mg m−3 |
Hall symbol: -P 1 | Mo Kα radiation, λ = 0.71073 Å |
a = 9.046 (2) Å | Cell parameters from 20300 reflections |
b = 14.626 (3) Å | θ = 3.2–27.4° |
c = 17.588 (4) Å | µ = 1.04 mm−1 |
α = 104.40 (2)° | T = 295 K |
β = 100.20 (2)° | Prism, blue |
γ = 92.47 (2)° | 0.38 × 0.25 × 0.19 mm |
V = 2209.1 (8) Å3 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 10073 independent reflections |
Radiation source: fine-focus sealed tube | 6123 reflections with I > 2σ(I) |
Graphite monochromator | Rint = 0.049 |
ω scans | θmax = 27.5°, θmin = 3.0° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −11→11 |
Tmin = 0.432, Tmax = 0.827 | k = −18→18 |
21663 measured reflections | l = −21→22 |
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)] = 0.058 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.135 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | w = 1/[σ2(Fo2) + (0.066P)2] where P = (Fo2 + 2Fc2)/3 |
10073 reflections | (Δ/σ)max = 0.001 |
624 parameters | Δρmax = 0.67 e Å−3 |
21 restraints | Δρmin = −0.26 e Å−3 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Cu1 | 0.0359 (3) | 1.03097 (15) | 0.02012 (13) | 0.0257 (6) | 0.2944 (14) |
Cu1' | 0.0000 | 1.0000 | 0.0000 | 0.0257 (6) | 0.41 |
Cu2 | 0.73956 (4) | 0.76487 (3) | 0.50556 (2) | 0.03527 (12) | |
Cu3 | 1.5346 (9) | 0.5295 (5) | 1.0166 (5) | 0.0318 (13) | 0.2496 (13) |
Cu3' | 1.5000 | 0.5000 | 1.0000 | 0.0318 (13) | 0.50 |
O1 | −0.0216 (3) | 0.9895 (2) | 0.10598 (17) | 0.0752 (10) | |
O2 | −0.1104 (4) | 0.8376 (3) | 0.06199 (17) | 0.0923 (12) | |
O3 | −0.1204 (3) | 0.8296 (2) | 0.21538 (16) | 0.0597 (7) | |
O4 | 0.4061 (2) | 0.79625 (18) | 0.23361 (13) | 0.0476 (6) | |
O5 | 0.6880 (2) | 0.75538 (17) | 0.38923 (12) | 0.0428 (6) | |
O6 | 0.5102 (3) | 0.85690 (19) | 0.39188 (14) | 0.0614 (7) | |
O7 | 0.8020 (2) | 0.75248 (16) | 0.61678 (12) | 0.0398 (5) | |
O8 | 0.9409 (3) | 0.63632 (17) | 0.57204 (14) | 0.0539 (7) | |
O9 | 1.0598 (2) | 0.63179 (17) | 0.72620 (15) | 0.0502 (6) | |
O10 | 1.5950 (3) | 0.64209 (19) | 0.76289 (15) | 0.0542 (7) | |
O11 | 1.5282 (3) | 0.5023 (2) | 0.89303 (16) | 0.0740 (10) | |
O12 | 1.5998 (4) | 0.6575 (3) | 0.91951 (16) | 0.0831 (10) | |
O1w | 0.1700 (4) | 1.1870 (2) | 0.1035 (2) | 0.0839 (10) | |
H1w1 | 0.246 (3) | 1.158 (3) | 0.112 (3) | 0.126* | |
H1w2 | 0.163 (6) | 1.201 (3) | 0.0591 (15) | 0.126* | |
O2w | 0.6276 (3) | 0.8977 (2) | 0.54763 (16) | 0.0600 (7) | |
H2w1 | 0.597 (4) | 0.921 (3) | 0.5907 (11) | 0.090* | |
H2w2 | 0.564 (4) | 0.905 (3) | 0.5081 (11) | 0.090* | |
O3w | 1.6454 (4) | 0.6794 (2) | 1.0805 (2) | 0.0809 (9) | |
H3w1 | 1.647 (5) | 0.704 (3) | 1.0413 (17) | 0.121* | |
H3w2 | 1.736 (2) | 0.678 (3) | 1.104 (3) | 0.121* | |
O4w | 0.5383 (4) | 0.9892 (2) | 0.6857 (2) | 0.0755 (9) | |
H4w1 | 0.615 (4) | 0.978 (3) | 0.717 (2) | 0.113* | |
H4w2 | 0.555 (5) | 1.0450 (17) | 0.680 (3) | 0.113* | |
O5w | 0.8019 (4) | 0.9138 (2) | 0.74496 (17) | 0.0708 (8) | |
H5w1 | 0.847 (5) | 0.908 (3) | 0.7904 (11) | 0.106* | |
H5w2 | 0.820 (5) | 0.867 (2) | 0.7088 (16) | 0.106* | |
O6w | 0.8937 (4) | 0.5522 (3) | 0.40163 (19) | 0.0830 (9) | |
H6w1 | 0.922 (6) | 0.582 (3) | 0.4511 (11) | 0.125* | |
H6w2 | 0.918 (6) | 0.4954 (14) | 0.396 (3) | 0.125* | |
N1 | 0.1965 (4) | 0.9413 (3) | 0.0096 (2) | 0.0712 (11) | |
N2 | 0.9379 (3) | 0.8374 (2) | 0.51565 (15) | 0.0408 (6) | |
N3 | 0.5557 (3) | 0.6756 (2) | 0.49020 (15) | 0.0383 (6) | |
N4 | 1.7005 (4) | 0.4472 (2) | 1.01872 (18) | 0.0573 (9) | |
C1 | 0.2237 (5) | 0.8724 (4) | −0.0501 (3) | 0.0780 (14) | |
H1 | 0.1487 | 0.8505 | −0.0956 | 0.094* | |
C2 | 0.3586 (6) | 0.8324 (4) | −0.0472 (3) | 0.0849 (16) | |
H2 | 0.3747 | 0.7847 | −0.0903 | 0.102* | |
C3 | 0.4671 (6) | 0.8629 (4) | 0.0187 (3) | 0.0865 (16) | |
H3 | 0.5600 | 0.8377 | 0.0215 | 0.104* | |
C4 | 0.4384 (6) | 0.9315 (4) | 0.0814 (3) | 0.102 (2) | |
H4 | 0.5102 | 0.9526 | 0.1284 | 0.123* | |
C5 | 0.3018 (6) | 0.9685 (4) | 0.0738 (3) | 0.0921 (18) | |
H5 | 0.2830 | 1.0155 | 0.1166 | 0.111* | |
C6 | −0.0751 (4) | 0.9122 (3) | 0.1137 (2) | 0.0513 (10) | |
C7 | −0.1009 (4) | 0.9181 (3) | 0.19792 (19) | 0.0447 (8) | |
H7a | −0.0155 | 0.9554 | 0.2360 | 0.054* | |
H7b | −0.1896 | 0.9515 | 0.2056 | 0.054* | |
C8 | 0.0073 (3) | 0.7831 (3) | 0.23268 (19) | 0.0424 (8) | |
C9 | −0.0168 (4) | 0.7035 (3) | 0.2594 (2) | 0.0504 (9) | |
H9 | −0.1132 | 0.6828 | 0.2631 | 0.061* | |
C10 | 0.1055 (4) | 0.6554 (3) | 0.2804 (2) | 0.0541 (9) | |
H10 | 0.0905 | 0.6023 | 0.2991 | 0.065* | |
C11 | 0.2500 (4) | 0.6842 (3) | 0.2743 (2) | 0.0489 (9) | |
H11 | 0.3313 | 0.6514 | 0.2892 | 0.059* | |
C12 | 0.2704 (3) | 0.7620 (2) | 0.24592 (18) | 0.0389 (7) | |
C13 | 0.1492 (4) | 0.8127 (3) | 0.22524 (18) | 0.0419 (8) | |
H13 | 0.1642 | 0.8660 | 0.2066 | 0.050* | |
C14 | 0.5403 (3) | 0.7599 (3) | 0.26649 (18) | 0.0457 (9) | |
H14a | 0.6234 | 0.7790 | 0.2441 | 0.055* | |
H14b | 0.5263 | 0.6912 | 0.2511 | 0.055* | |
C15 | 0.5805 (3) | 0.7944 (2) | 0.35696 (19) | 0.0395 (7) | |
C16 | 1.0282 (4) | 0.8067 (3) | 0.4643 (2) | 0.0508 (9) | |
H16 | 0.9964 | 0.7520 | 0.4231 | 0.061* | |
C17 | 1.1674 (4) | 0.8533 (3) | 0.4701 (3) | 0.0619 (11) | |
H17 | 1.2282 | 0.8300 | 0.4335 | 0.074* | |
C18 | 1.2147 (4) | 0.9336 (3) | 0.5299 (3) | 0.0619 (11) | |
H18 | 1.3080 | 0.9661 | 0.5347 | 0.074* | |
C19 | 1.1223 (4) | 0.9657 (3) | 0.5829 (2) | 0.0581 (10) | |
H19 | 1.1522 | 1.0204 | 0.6244 | 0.070* | |
C20 | 0.9850 (4) | 0.9161 (3) | 0.5741 (2) | 0.0483 (9) | |
H20 | 0.9227 | 0.9383 | 0.6101 | 0.058* | |
C21 | 0.4518 (4) | 0.6984 (3) | 0.5353 (2) | 0.0493 (9) | |
H21 | 0.4698 | 0.7542 | 0.5762 | 0.059* | |
C22 | 0.3199 (4) | 0.6429 (3) | 0.5237 (2) | 0.0586 (10) | |
H22 | 0.2487 | 0.6617 | 0.5553 | 0.070* | |
C23 | 0.2938 (4) | 0.5599 (3) | 0.4654 (2) | 0.0594 (10) | |
H23 | 0.2049 | 0.5211 | 0.4564 | 0.071* | |
C24 | 0.4020 (4) | 0.5349 (3) | 0.4202 (2) | 0.0518 (9) | |
H24 | 0.3878 | 0.4780 | 0.3806 | 0.062* | |
C25 | 0.5306 (4) | 0.5938 (2) | 0.43369 (19) | 0.0431 (8) | |
H25 | 0.6027 | 0.5763 | 0.4025 | 0.052* | |
C26 | 0.8897 (3) | 0.6877 (2) | 0.62555 (18) | 0.0370 (7) | |
C27 | 0.9246 (3) | 0.6759 (3) | 0.70985 (19) | 0.0461 (9) | |
H27a | 0.9335 | 0.7378 | 0.7475 | 0.055* | |
H27b | 0.8411 | 0.6382 | 0.7182 | 0.055* | |
C28 | 1.1927 (3) | 0.6844 (2) | 0.73252 (18) | 0.0389 (7) | |
C29 | 1.2032 (4) | 0.7764 (2) | 0.7240 (2) | 0.0479 (9) | |
H29 | 1.1172 | 0.8078 | 0.7149 | 0.057* | |
C30 | 1.3440 (4) | 0.8198 (3) | 0.7295 (2) | 0.0527 (9) | |
H30 | 1.3526 | 0.8811 | 0.7236 | 0.063* | |
C31 | 1.4727 (4) | 0.7746 (3) | 0.7436 (2) | 0.0508 (9) | |
H31 | 1.5670 | 0.8054 | 0.7476 | 0.061* | |
C32 | 1.4606 (3) | 0.6829 (3) | 0.75173 (18) | 0.0406 (8) | |
C33 | 1.3215 (4) | 0.6377 (2) | 0.74692 (18) | 0.0399 (8) | |
H33 | 1.3136 | 0.5765 | 0.7532 | 0.048* | |
C34 | 1.5926 (4) | 0.5583 (3) | 0.79006 (19) | 0.0468 (9) | |
H34a | 1.6866 | 0.5298 | 0.7853 | 0.056* | |
H34b | 1.5113 | 0.5133 | 0.7558 | 0.056* | |
C35 | 1.5717 (4) | 0.5760 (3) | 0.8760 (2) | 0.0510 (10) | |
C36 | 1.7369 (5) | 0.3768 (3) | 0.9637 (2) | 0.0700 (13) | |
H36 | 1.6669 | 0.3501 | 0.9169 | 0.084* | |
C37 | 1.8770 (5) | 0.3421 (4) | 0.9741 (3) | 0.0813 (15) | |
H37 | 1.9002 | 0.2928 | 0.9345 | 0.098* | |
C38 | 1.9794 (5) | 0.3793 (4) | 1.0413 (3) | 0.0848 (16) | |
H38 | 2.0744 | 0.3572 | 1.0486 | 0.102* | |
C39 | 1.9404 (6) | 0.4508 (4) | 1.0989 (3) | 0.0919 (17) | |
H39 | 2.0082 | 0.4780 | 1.1464 | 0.110* | |
C40 | 1.7993 (6) | 0.4816 (3) | 1.0851 (3) | 0.0765 (14) | |
H40 | 1.7726 | 0.5293 | 1.1249 | 0.092* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Cu1 | 0.0299 (13) | 0.0211 (16) | 0.0174 (12) | −0.0029 (10) | −0.0035 (9) | −0.0045 (9) |
Cu1' | 0.0299 (13) | 0.0211 (16) | 0.0174 (12) | −0.0029 (10) | −0.0035 (9) | −0.0045 (9) |
Cu2 | 0.02741 (19) | 0.0477 (3) | 0.0304 (2) | −0.00092 (17) | 0.00153 (14) | 0.01325 (17) |
Cu3 | 0.035 (3) | 0.032 (4) | 0.025 (3) | 0.002 (2) | 0.003 (2) | 0.004 (2) |
Cu3' | 0.035 (3) | 0.032 (4) | 0.025 (3) | 0.002 (2) | 0.003 (2) | 0.004 (2) |
O1 | 0.088 (2) | 0.096 (2) | 0.079 (2) | 0.053 (2) | 0.0506 (18) | 0.0611 (18) |
O2 | 0.072 (2) | 0.134 (3) | 0.0454 (16) | 0.015 (2) | −0.0023 (15) | −0.0153 (19) |
O3 | 0.0328 (13) | 0.0810 (19) | 0.0800 (18) | 0.0083 (13) | 0.0115 (13) | 0.0471 (16) |
O4 | 0.0320 (12) | 0.0739 (17) | 0.0430 (13) | 0.0092 (12) | 0.0034 (10) | 0.0287 (12) |
O5 | 0.0313 (11) | 0.0643 (15) | 0.0370 (12) | 0.0074 (11) | 0.0045 (10) | 0.0218 (11) |
O6 | 0.0663 (17) | 0.0664 (17) | 0.0455 (14) | 0.0227 (15) | −0.0009 (13) | 0.0087 (13) |
O7 | 0.0320 (11) | 0.0544 (14) | 0.0325 (11) | 0.0055 (11) | 0.0015 (9) | 0.0136 (10) |
O8 | 0.0627 (17) | 0.0526 (15) | 0.0433 (14) | 0.0068 (13) | 0.0147 (12) | 0.0037 (12) |
O9 | 0.0320 (12) | 0.0624 (16) | 0.0646 (16) | 0.0060 (12) | 0.0037 (11) | 0.0358 (13) |
O10 | 0.0357 (13) | 0.0742 (18) | 0.0670 (16) | 0.0168 (13) | 0.0191 (12) | 0.0360 (14) |
O11 | 0.093 (2) | 0.099 (2) | 0.0636 (18) | 0.055 (2) | 0.0461 (17) | 0.0535 (17) |
O12 | 0.087 (2) | 0.102 (3) | 0.0440 (16) | 0.018 (2) | 0.0020 (15) | −0.0036 (17) |
O1w | 0.094 (2) | 0.075 (2) | 0.093 (2) | 0.0174 (19) | 0.031 (2) | 0.0304 (19) |
O2w | 0.0564 (16) | 0.0701 (18) | 0.0531 (15) | 0.0181 (14) | 0.0073 (13) | 0.0157 (14) |
O3w | 0.093 (2) | 0.078 (2) | 0.077 (2) | 0.0084 (19) | 0.0158 (19) | 0.0305 (17) |
O4w | 0.086 (2) | 0.0553 (18) | 0.083 (2) | 0.0062 (17) | 0.0139 (18) | 0.0159 (16) |
O5w | 0.077 (2) | 0.0650 (19) | 0.0593 (17) | 0.0053 (16) | 0.0046 (16) | 0.0013 (15) |
O6w | 0.081 (2) | 0.086 (2) | 0.077 (2) | 0.012 (2) | 0.0169 (18) | 0.0100 (17) |
N1 | 0.082 (3) | 0.099 (3) | 0.065 (2) | 0.056 (2) | 0.042 (2) | 0.053 (2) |
N2 | 0.0324 (14) | 0.0523 (18) | 0.0381 (15) | −0.0012 (13) | 0.0025 (12) | 0.0163 (13) |
N3 | 0.0309 (13) | 0.0496 (17) | 0.0344 (14) | −0.0040 (13) | 0.0020 (11) | 0.0153 (13) |
N4 | 0.069 (2) | 0.068 (2) | 0.0475 (18) | 0.0333 (19) | 0.0225 (16) | 0.0254 (16) |
C1 | 0.066 (3) | 0.109 (4) | 0.069 (3) | 0.040 (3) | 0.021 (2) | 0.030 (3) |
C2 | 0.083 (3) | 0.101 (4) | 0.077 (3) | 0.053 (3) | 0.027 (3) | 0.019 (3) |
C3 | 0.075 (3) | 0.103 (4) | 0.098 (4) | 0.052 (3) | 0.031 (3) | 0.038 (3) |
C4 | 0.093 (4) | 0.127 (5) | 0.081 (3) | 0.052 (4) | 0.009 (3) | 0.014 (3) |
C5 | 0.116 (4) | 0.107 (4) | 0.072 (3) | 0.065 (4) | 0.041 (3) | 0.031 (3) |
C6 | 0.0399 (19) | 0.083 (3) | 0.0363 (19) | 0.029 (2) | 0.0066 (16) | 0.022 (2) |
C7 | 0.0392 (18) | 0.059 (2) | 0.0408 (18) | 0.0136 (17) | 0.0125 (15) | 0.0180 (16) |
C8 | 0.0307 (16) | 0.059 (2) | 0.0382 (17) | 0.0033 (16) | 0.0019 (14) | 0.0163 (16) |
C9 | 0.044 (2) | 0.058 (2) | 0.052 (2) | −0.0055 (18) | 0.0078 (17) | 0.0200 (18) |
C10 | 0.061 (2) | 0.048 (2) | 0.056 (2) | 0.0012 (19) | 0.0080 (19) | 0.0228 (18) |
C11 | 0.049 (2) | 0.050 (2) | 0.049 (2) | 0.0100 (18) | 0.0034 (17) | 0.0174 (17) |
C12 | 0.0342 (17) | 0.053 (2) | 0.0278 (15) | 0.0028 (15) | 0.0008 (13) | 0.0112 (14) |
C13 | 0.0381 (18) | 0.057 (2) | 0.0364 (17) | 0.0048 (16) | 0.0038 (14) | 0.0250 (16) |
C14 | 0.0313 (16) | 0.070 (2) | 0.0364 (17) | 0.0094 (17) | 0.0024 (14) | 0.0179 (17) |
C15 | 0.0292 (16) | 0.048 (2) | 0.0427 (18) | 0.0022 (15) | 0.0055 (14) | 0.0160 (16) |
C16 | 0.0415 (19) | 0.056 (2) | 0.058 (2) | 0.0005 (18) | 0.0171 (17) | 0.0153 (18) |
C17 | 0.042 (2) | 0.074 (3) | 0.079 (3) | 0.006 (2) | 0.027 (2) | 0.026 (2) |
C18 | 0.0348 (19) | 0.075 (3) | 0.082 (3) | −0.011 (2) | 0.005 (2) | 0.039 (3) |
C19 | 0.050 (2) | 0.063 (3) | 0.052 (2) | −0.020 (2) | −0.0057 (18) | 0.0132 (19) |
C20 | 0.046 (2) | 0.057 (2) | 0.0379 (18) | −0.0061 (18) | 0.0037 (15) | 0.0087 (17) |
C21 | 0.048 (2) | 0.055 (2) | 0.046 (2) | −0.0041 (18) | 0.0148 (16) | 0.0135 (17) |
C22 | 0.045 (2) | 0.069 (3) | 0.070 (3) | 0.000 (2) | 0.0221 (19) | 0.026 (2) |
C23 | 0.041 (2) | 0.069 (3) | 0.069 (3) | −0.013 (2) | 0.0013 (19) | 0.030 (2) |
C24 | 0.056 (2) | 0.049 (2) | 0.043 (2) | −0.0127 (19) | −0.0030 (17) | 0.0110 (17) |
C25 | 0.0427 (19) | 0.052 (2) | 0.0349 (17) | −0.0019 (17) | 0.0041 (15) | 0.0147 (16) |
C26 | 0.0286 (15) | 0.0448 (19) | 0.0357 (17) | −0.0053 (15) | 0.0029 (13) | 0.0106 (15) |
C27 | 0.0293 (16) | 0.072 (2) | 0.0446 (19) | 0.0087 (17) | 0.0084 (15) | 0.0267 (18) |
C28 | 0.0312 (16) | 0.052 (2) | 0.0354 (17) | 0.0021 (15) | 0.0024 (13) | 0.0173 (15) |
C29 | 0.0403 (19) | 0.050 (2) | 0.053 (2) | 0.0104 (17) | 0.0014 (16) | 0.0173 (17) |
C30 | 0.050 (2) | 0.042 (2) | 0.064 (2) | −0.0021 (17) | −0.0007 (18) | 0.0184 (18) |
C31 | 0.0409 (19) | 0.056 (2) | 0.056 (2) | −0.0043 (18) | 0.0066 (17) | 0.0182 (19) |
C32 | 0.0311 (16) | 0.057 (2) | 0.0382 (17) | 0.0089 (16) | 0.0094 (14) | 0.0187 (16) |
C33 | 0.0400 (18) | 0.0449 (19) | 0.0415 (18) | 0.0091 (16) | 0.0103 (14) | 0.0210 (15) |
C34 | 0.0389 (18) | 0.068 (2) | 0.0431 (19) | 0.0240 (18) | 0.0157 (15) | 0.0240 (17) |
C35 | 0.0410 (19) | 0.079 (3) | 0.0365 (19) | 0.030 (2) | 0.0076 (15) | 0.017 (2) |
C36 | 0.064 (3) | 0.089 (3) | 0.054 (2) | 0.033 (3) | 0.011 (2) | 0.008 (2) |
C37 | 0.073 (3) | 0.090 (3) | 0.070 (3) | 0.038 (3) | 0.010 (2) | −0.002 (3) |
C38 | 0.064 (3) | 0.090 (4) | 0.091 (3) | 0.036 (3) | 0.001 (3) | 0.010 (3) |
C39 | 0.082 (3) | 0.098 (4) | 0.074 (3) | 0.031 (3) | −0.014 (3) | 0.000 (3) |
C40 | 0.096 (4) | 0.077 (3) | 0.055 (3) | 0.035 (3) | 0.017 (3) | 0.008 (2) |
Geometric parameters (Å, º) top
Cu1—O1 | 1.905 (4) | C2—H2 | 0.9300 |
Cu1—O1i | 2.143 (4) | C3—C4 | 1.365 (7) |
Cu1—N1 | 2.001 (4) | C3—H3 | 0.9300 |
Cu1—N1i | 2.156 (4) | C4—C5 | 1.369 (6) |
Cu1—O1w | 2.509 (4) | C4—H4 | 0.9300 |
Cu1'—O1 | 1.951 (3) | C5—H5 | 0.9300 |
Cu1'—O1i | 1.951 (3) | C6—C7 | 1.522 (5) |
Cu1'—N1 | 2.006 (3) | C7—H7a | 0.9700 |
Cu1'—N1i | 2.006 (3) | C7—H7b | 0.9700 |
Cu2—O5 | 1.985 (2) | C8—C13 | 1.376 (4) |
Cu2—O7 | 1.993 (2) | C8—C9 | 1.381 (5) |
Cu2—N2 | 2.001 (3) | C9—C10 | 1.381 (5) |
Cu2—N3 | 2.006 (3) | C9—H9 | 0.9300 |
Cu2—O2w | 2.251 (2) | C10—C11 | 1.386 (5) |
Cu3—O11 | 2.100 (9) | C10—H10 | 0.9300 |
Cu3—O11ii | 1.931 (9) | C11—C12 | 1.370 (5) |
Cu3—N4 | 1.966 (9) | C11—H11 | 0.9300 |
Cu3—N4ii | 2.173 (9) | C12—C13 | 1.396 (4) |
Cu3—O3w | 2.293 (7) | C13—H13 | 0.9300 |
Cu3'—O11 | 1.951 (2) | C14—C15 | 1.516 (4) |
Cu3'—O11ii | 1.951 (2) | C14—H14a | 0.9700 |
Cu3'—N4 | 2.008 (3) | C14—H14b | 0.9700 |
Cu3'—N4ii | 2.008 (3) | C16—C17 | 1.380 (5) |
O1—C6 | 1.258 (5) | C16—H16 | 0.9300 |
O1—Cu1i | 2.143 (4) | C17—C18 | 1.361 (6) |
O2—C6 | 1.222 (5) | C17—H17 | 0.9300 |
O3—C8 | 1.392 (4) | C18—C19 | 1.372 (5) |
O3—C7 | 1.413 (4) | C18—H18 | 0.9300 |
O4—C12 | 1.378 (4) | C19—C20 | 1.375 (5) |
O4—C14 | 1.432 (3) | C19—H19 | 0.9300 |
O5—C15 | 1.268 (3) | C20—H20 | 0.9300 |
O6—C15 | 1.235 (4) | C21—C22 | 1.368 (5) |
O7—C26 | 1.283 (4) | C21—H21 | 0.9300 |
O8—C26 | 1.223 (3) | C22—C23 | 1.361 (6) |
O9—C28 | 1.371 (4) | C22—H22 | 0.9300 |
O9—C27 | 1.425 (3) | C23—C24 | 1.373 (5) |
O10—C32 | 1.382 (3) | C23—H23 | 0.9300 |
O10—C34 | 1.423 (4) | C24—C25 | 1.366 (5) |
O11—C35 | 1.254 (5) | C24—H24 | 0.9300 |
O11—Cu3ii | 1.931 (10) | C25—H25 | 0.9300 |
O12—C35 | 1.233 (5) | C26—C27 | 1.514 (4) |
O1w—H1w1 | 0.84 (1) | C27—H27a | 0.9700 |
O1w—H1w2 | 0.85 (1) | C27—H27b | 0.9700 |
O2w—H2w1 | 0.85 (1) | C28—C33 | 1.393 (4) |
O2w—H2w2 | 0.85 (1) | C28—C29 | 1.391 (5) |
O3w—H3w1 | 0.86 (1) | C29—C30 | 1.375 (5) |
O3w—H3w2 | 0.85 (1) | C29—H29 | 0.9300 |
O4w—H4w1 | 0.86 (1) | C30—C31 | 1.378 (5) |
O4w—H4w2 | 0.86 (1) | C30—H30 | 0.9300 |
O5w—H5w1 | 0.86 (1) | C31—C32 | 1.386 (5) |
O5w—H5w2 | 0.86 (1) | C31—H31 | 0.9300 |
O6w—H6w1 | 0.86 (1) | C32—C33 | 1.374 (5) |
O6w—H6w2 | 0.86 (1) | C33—H33 | 0.9300 |
N1—C5 | 1.306 (6) | C34—C35 | 1.515 (4) |
N1—C1 | 1.328 (5) | C34—H34a | 0.9700 |
N1—Cu1i | 2.156 (4) | C34—H34b | 0.9700 |
N2—C20 | 1.333 (4) | C36—C37 | 1.385 (5) |
N2—C16 | 1.333 (4) | C36—H36 | 0.9300 |
N3—C25 | 1.332 (4) | C37—C38 | 1.342 (6) |
N3—C21 | 1.336 (4) | C37—H37 | 0.9300 |
N4—C40 | 1.310 (5) | C38—C39 | 1.369 (6) |
N4—C36 | 1.323 (5) | C38—H38 | 0.9300 |
N4—Cu3ii | 2.173 (9) | C39—C40 | 1.373 (6) |
C1—C2 | 1.375 (5) | C39—H39 | 0.9300 |
C1—H1 | 0.9300 | C40—H40 | 0.9300 |
C2—C3 | 1.345 (7) | | |
| | | |
O1—Cu1—O1i | 149.2 (1) | H7a—C7—H7b | 107.6 |
O1—Cu1—O1w | 96.6 (2) | C13—C8—C9 | 120.9 (3) |
O1—Cu1—N1 | 92.6 (2) | C13—C8—O3 | 123.9 (3) |
O1—Cu1—N1i | 85.9 (2) | C9—C8—O3 | 115.2 (3) |
O1i—Cu1—N1 | 83.9 (1) | C10—C9—C8 | 118.6 (3) |
O1i—Cu1—N1i | 82.1 (1) | C10—C9—H9 | 120.7 |
O1i—Cu1—O1w | 114.0 (2) | C8—C9—H9 | 120.7 |
O1w—Cu1—N1 | 105.4 (2) | C9—C10—C11 | 121.8 (3) |
O1w—Cu1—N1i | 105.0 (2) | C9—C10—H10 | 119.1 |
N1—Cu1—N1i | 149.6 (1) | C11—C10—H10 | 119.1 |
O1—Cu1'—O1i | 180 | C12—C11—C10 | 118.5 (3) |
O1—Cu1'—N1 | 91.1 (1) | C12—C11—H11 | 120.7 |
O1—Cu1'—N1i | 88.9 (1) | C10—C11—H11 | 120.7 |
O1i—Cu1'—N1 | 88.9 (1) | C11—C12—O4 | 124.9 (3) |
O1i—Cu1'—N1i | 91.1 (1) | C11—C12—C13 | 120.9 (3) |
N1—Cu1'—N1i | 180 | O4—C12—C13 | 114.2 (3) |
O5—Cu2—O7 | 170.4 (1) | C8—C13—C12 | 119.2 (3) |
O5—Cu2—N2 | 91.5 (1) | C8—C13—H13 | 120.4 |
O5—Cu2—N3 | 87.5 (1) | C12—C13—H13 | 120.4 |
O5—Cu2—O2w | 97.3 (1) | O4—C14—C15 | 112.6 (2) |
O7—Cu2—N2 | 89.9 (1) | O4—C14—H14a | 109.1 |
O7—Cu2—N3 | 89.8 (1) | C15—C14—H14a | 109.1 |
O7—Cu2—O2w | 92.2 (1) | O4—C14—H14b | 109.1 |
O2w—Cu2—N2 | 92.7 (1) | C15—C14—H14b | 109.1 |
O2w—Cu2—N3 | 95.5 (1) | H14a—C14—H14b | 107.8 |
N2—Cu2—N3 | 171.8 (1) | O6—C15—O5 | 126.4 (3) |
O11—Cu3—O11ii | 150.9 (3) | O6—C15—C14 | 119.0 (3) |
O11—Cu3—O3w | 110.1 (4) | O5—C15—C14 | 114.6 (3) |
O11—Cu3—N4 | 86.3 (3) | N2—C16—C17 | 122.3 (4) |
O11—Cu3—N4ii | 82.4 (3) | N2—C16—H16 | 118.9 |
O11ii—Cu3—N4 | 92.5 (4) | C17—C16—H16 | 118.9 |
O11ii—Cu3—N4ii | 85.2 (4) | C18—C17—C16 | 119.3 (4) |
O11ii—Cu3—O3w | 98.3 (3) | C18—C17—H17 | 120.3 |
O3w—Cu3—N4 | 105.1 (3) | C16—C17—H17 | 120.3 |
O3w—Cu3—N4ii | 103.0 (3) | C17—C18—C19 | 118.8 (4) |
N4—Cu3—N4ii | 151.9 (3) | C17—C18—H18 | 120.6 |
O11—Cu3'—O11ii | 180 | C19—C18—H18 | 120.6 |
O11—Cu3'—N4 | 89.3 (1) | C18—C19—C20 | 119.2 (4) |
O11—Cu3'—N4ii | 90.7 (1) | C18—C19—H19 | 120.4 |
O11ii—Cu3'—N4 | 90.7 (1) | C20—C19—H19 | 120.4 |
O11ii—Cu3'—N4ii | 89.3 (1) | N2—C20—C19 | 122.4 (3) |
N4—Cu3'—N4ii | 180 | N2—C20—H20 | 118.8 |
C6—O1—Cu1 | 134.9 (3) | C19—C20—H20 | 118.8 |
C6—O1—Cu1' | 119.3 (3) | N3—C21—C22 | 122.5 (4) |
C6—O1—Cu1i | 105.3 (3) | N3—C21—H21 | 118.7 |
Cu1—O1—Cu1i | 30.85 (11) | C22—C21—H21 | 118.7 |
C8—O3—C7 | 118.1 (3) | C23—C22—C21 | 119.3 (4) |
C12—O4—C14 | 117.8 (3) | C23—C22—H22 | 120.3 |
C15—O5—Cu2 | 124.2 (2) | C21—C22—H22 | 120.3 |
C26—O7—Cu2 | 116.21 (18) | C22—C23—C24 | 118.3 (4) |
C28—O9—C27 | 116.6 (3) | C22—C23—H23 | 120.8 |
C32—O10—C34 | 117.0 (3) | C24—C23—H23 | 120.8 |
C35—O11—Cu3ii | 137.0 (3) | C25—C24—C23 | 119.8 (4) |
C35—O11—Cu3' | 123.2 (3) | C25—C24—H24 | 120.1 |
C35—O11—Cu3 | 110.3 (3) | C23—C24—H24 | 120.1 |
Cu1—O1w—H1w1 | 87 (3) | N3—C25—C24 | 122.0 (3) |
Cu1—O1w—H1w2 | 84 (3) | N3—C25—H25 | 119.0 |
H1w1—O1w—H1w2 | 110.6 (18) | C24—C25—H25 | 119.0 |
Cu2—O2w—H2w1 | 132 (2) | O8—C26—O7 | 125.2 (3) |
Cu2—O2w—H2w2 | 108 (2) | O8—C26—C27 | 120.5 (3) |
H2w1—O2w—H2w2 | 109.1 (17) | O7—C26—C27 | 114.3 (3) |
Cu3—O3w—H3w1 | 102 (3) | O9—C27—C26 | 113.3 (2) |
Cu3—O3w—H3w2 | 111 (3) | O9—C27—H27a | 108.9 |
H3w1—O3w—H3w2 | 108.4 (17) | C26—C27—H27a | 108.9 |
H4w1—O4w—H4w2 | 108.0 (17) | O9—C27—H27b | 108.9 |
H5w1—O5w—H5w2 | 107.7 (16) | C26—C27—H27b | 108.9 |
H6w1—O6w—H6w2 | 107.7 (17) | H27a—C27—H27b | 107.7 |
C5—N1—C1 | 117.5 (3) | O9—C28—C33 | 114.6 (3) |
C5—N1—Cu1 | 108.0 (3) | O9—C28—C29 | 124.6 (3) |
C1—N1—Cu1 | 133.8 (3) | C33—C28—C29 | 120.9 (3) |
C5—N1—Cu1' | 122.0 (3) | C30—C29—C28 | 118.3 (3) |
C1—N1—Cu1' | 120.5 (3) | C30—C29—H29 | 120.8 |
C5—N1—Cu1i | 134.3 (3) | C28—C29—H29 | 120.8 |
C1—N1—Cu1i | 107.6 (3) | C29—C30—C31 | 121.6 (3) |
C20—N2—C16 | 118.1 (3) | C29—C30—H30 | 119.2 |
C20—N2—Cu2 | 121.6 (2) | C31—C30—H30 | 119.2 |
C16—N2—Cu2 | 120.3 (3) | C30—C31—C32 | 119.4 (3) |
C25—N3—C21 | 118.0 (3) | C30—C31—H31 | 120.3 |
C25—N3—Cu2 | 121.7 (2) | C32—C31—H31 | 120.3 |
C21—N3—Cu2 | 120.3 (2) | C33—C32—O10 | 124.2 (3) |
C40—N4—C36 | 118.1 (3) | C33—C32—C31 | 120.3 (3) |
C40—N4—Cu3 | 108.6 (3) | O10—C32—C31 | 115.4 (3) |
C36—N4—Cu3 | 132.5 (3) | C32—C33—C28 | 119.4 (3) |
C40—N4—Cu3' | 121.2 (2) | C32—C33—H33 | 120.3 |
C36—N4—Cu3' | 120.7 (3) | C28—C33—H33 | 120.3 |
C40—N4—Cu3ii | 132.0 (3) | O10—C34—C35 | 113.2 (3) |
C36—N4—Cu3ii | 109.4 (3) | O10—C34—H34a | 108.9 |
N1—C1—C2 | 122.5 (5) | C35—C34—H34a | 108.9 |
N1—C1—H1 | 118.8 | O10—C34—H34b | 108.9 |
C2—C1—H1 | 118.8 | C35—C34—H34b | 108.9 |
C3—C2—C1 | 119.2 (4) | H34a—C34—H34b | 107.8 |
C3—C2—H2 | 120.4 | O12—C35—O11 | 128.6 (4) |
C1—C2—H2 | 120.4 | O12—C35—C34 | 118.3 (4) |
C2—C3—C4 | 118.8 (4) | O11—C35—C34 | 113.1 (4) |
C2—C3—H3 | 120.6 | N4—C36—C37 | 121.5 (4) |
C4—C3—H3 | 120.6 | N4—C36—H36 | 119.3 |
C5—C4—C3 | 118.7 (5) | C37—C36—H36 | 119.3 |
C5—C4—H4 | 120.7 | C38—C37—C36 | 120.2 (4) |
C3—C4—H4 | 120.7 | C38—C37—H37 | 119.9 |
N1—C5—C4 | 123.4 (4) | C36—C37—H37 | 119.9 |
N1—C5—H5 | 118.3 | C37—C38—C39 | 118.3 (4) |
C4—C5—H5 | 118.3 | C37—C38—H38 | 120.9 |
O2—C6—O1 | 127.6 (4) | C39—C38—H38 | 120.9 |
O2—C6—C7 | 119.3 (4) | C38—C39—C40 | 118.7 (4) |
O1—C6—C7 | 113.1 (4) | C38—C39—H39 | 120.6 |
O3—C7—C6 | 114.8 (3) | C40—C39—H39 | 120.6 |
O3—C7—H7a | 108.6 | N4—C40—C39 | 123.2 (4) |
C6—C7—H7a | 108.6 | N4—C40—H40 | 118.4 |
O3—C7—H7b | 108.6 | C39—C40—H40 | 118.4 |
C6—C7—H7b | 108.6 | | |
| | | |
N1—Cu1—O1—C6 | −62.6 (4) | O11—Cu3'—N4—Cu3 | 100.2 (11) |
O1i—Cu1—O1—C6 | 19.9 (5) | O11ii—Cu3'—N4—Cu3ii | 100.2 (10) |
N1i—Cu1—O1—C6 | 87.0 (4) | O11—Cu3'—N4—Cu3ii | −79.8 (10) |
O1w—Cu1—O1—C6 | −168.4 (3) | C5—N1—C1—C2 | −2.3 (7) |
N1—Cu1—O1—Cu1' | −82.4 (3) | Cu1—N1—C1—C2 | 167.0 (4) |
O1i—Cu1—O1—Cu1' | 0.000 (1) | Cu1'—N1—C1—C2 | 177.8 (4) |
N1i—Cu1—O1—Cu1' | 67.1 (3) | Cu1i—N1—C1—C2 | −174.7 (4) |
O1w—Cu1—O1—Cu1' | 171.7 (3) | N1—C1—C2—C3 | 0.7 (8) |
N1—Cu1—O1—Cu1i | −82.4 (3) | C1—C2—C3—C4 | 1.4 (9) |
O1i—Cu1—O1—Cu1i | 0.0 | C2—C3—C4—C5 | −1.9 (9) |
N1i—Cu1—O1—Cu1i | 67.1 (3) | C1—N1—C5—C4 | 1.7 (8) |
O1w—Cu1—O1—Cu1i | 171.7 (3) | Cu1—N1—C5—C4 | −170.2 (5) |
N1—Cu1'—O1—C6 | −82.8 (3) | Cu1'—N1—C5—C4 | −178.4 (4) |
N1i—Cu1'—O1—C6 | 97.2 (3) | Cu1i—N1—C5—C4 | 171.5 (4) |
N1—Cu1'—O1—Cu1 | 81.1 (3) | C3—C4—C5—N1 | 0.4 (9) |
N1i—Cu1'—O1—Cu1 | −98.9 (3) | Cu1—O1—C6—O2 | −2.2 (6) |
N1—Cu1'—O1—Cu1i | −98.9 (3) | Cu1'—O1—C6—O2 | 4.1 (5) |
N1i—Cu1'—O1—Cu1i | 81.1 (3) | Cu1i—O1—C6—O2 | 8.2 (4) |
N2—Cu2—O5—C15 | −114.4 (3) | Cu1—O1—C6—C7 | 180.0 (2) |
N3—Cu2—O5—C15 | 73.7 (3) | Cu1'—O1—C6—C7 | −173.72 (19) |
O2w—Cu2—O5—C15 | −21.4 (3) | Cu1i—O1—C6—C7 | −169.6 (2) |
N2—Cu2—O7—C26 | −79.8 (2) | C8—O3—C7—C6 | 78.0 (4) |
N3—Cu2—O7—C26 | 92.0 (2) | O2—C6—C7—O3 | 18.7 (4) |
O2w—Cu2—O7—C26 | −172.5 (2) | O1—C6—C7—O3 | −163.3 (3) |
N4—Cu3'—O11—C35 | −100.3 (3) | C7—O3—C8—C13 | −7.5 (5) |
N4ii—Cu3'—O11—C35 | 79.7 (3) | C7—O3—C8—C9 | 171.9 (3) |
N4—Cu3'—O11—Cu3ii | 102.3 (10) | C13—C8—C9—C10 | 1.6 (5) |
N4ii—Cu3'—O11—Cu3ii | −77.7 (10) | O3—C8—C9—C10 | −177.8 (3) |
N4—Cu3'—O11—Cu3 | −77.7 (10) | C8—C9—C10—C11 | −0.9 (5) |
N4ii—Cu3'—O11—Cu3 | 102.3 (10) | C9—C10—C11—C12 | −0.6 (5) |
O11ii—Cu3—O11—C35 | 159.9 (9) | C10—C11—C12—O4 | −177.2 (3) |
N4—Cu3—O11—C35 | −111.5 (3) | C10—C11—C12—C13 | 1.5 (5) |
N4ii—Cu3—O11—C35 | 94.4 (3) | C14—O4—C12—C11 | −12.4 (5) |
O3w—Cu3—O11—C35 | −6.7 (5) | C14—O4—C12—C13 | 168.8 (3) |
O11ii—Cu3—O11—Cu3ii | 0.000 (3) | C9—C8—C13—C12 | −0.8 (5) |
N4—Cu3—O11—Cu3ii | 88.6 (10) | O3—C8—C13—C12 | 178.6 (3) |
N4ii—Cu3—O11—Cu3ii | −65.5 (9) | C11—C12—C13—C8 | −0.8 (5) |
O3w—Cu3—O11—Cu3ii | −166.6 (13) | O4—C12—C13—C8 | 178.0 (3) |
O11ii—Cu3—O11—Cu3' | 0.000 (2) | C12—O4—C14—C15 | −71.0 (4) |
N4—Cu3—O11—Cu3' | 88.6 (10) | Cu2—O5—C15—O6 | 14.2 (5) |
N4ii—Cu3—O11—Cu3' | −65.5 (9) | Cu2—O5—C15—C14 | −166.9 (2) |
O3w—Cu3—O11—Cu3' | −166.6 (13) | O4—C14—C15—O6 | −8.8 (5) |
O1—Cu1—N1—C5 | −67.4 (4) | O4—C14—C15—O5 | 172.1 (3) |
O1i—Cu1—N1—C5 | 143.3 (4) | C20—N2—C16—C17 | 0.3 (5) |
N1i—Cu1—N1—C5 | −153.6 (4) | Cu2—N2—C16—C17 | −178.5 (3) |
O1w—Cu1—N1—C5 | 30.1 (4) | N2—C16—C17—C18 | −0.3 (6) |
O1—Cu1—N1—C1 | 122.6 (5) | C16—C17—C18—C19 | 0.2 (6) |
O1i—Cu1—N1—C1 | −26.6 (5) | C17—C18—C19—C20 | −0.1 (6) |
N1i—Cu1—N1—C1 | 36.4 (6) | C16—N2—C20—C19 | −0.2 (5) |
O1w—Cu1—N1—C1 | −139.9 (5) | Cu2—N2—C20—C19 | 178.6 (3) |
O1—Cu1—N1—Cu1' | 86.2 (3) | C18—C19—C20—N2 | 0.2 (6) |
O1i—Cu1—N1—Cu1' | −63.0 (3) | C25—N3—C21—C22 | −2.3 (5) |
N1i—Cu1—N1—Cu1' | 0.0 | Cu2—N3—C21—C22 | 175.6 (3) |
O1w—Cu1—N1—Cu1' | −176.3 (4) | N3—C21—C22—C23 | 1.7 (6) |
O1—Cu1—N1—Cu1i | 86.2 (3) | C21—C22—C23—C24 | 0.1 (6) |
O1i—Cu1—N1—Cu1i | −63.0 (3) | C22—C23—C24—C25 | −1.1 (6) |
N1i—Cu1—N1—Cu1i | 0.0 | C21—N3—C25—C24 | 1.2 (5) |
O1w—Cu1—N1—Cu1i | −176.3 (4) | Cu2—N3—C25—C24 | −176.6 (2) |
O1i—Cu1'—N1—C5 | 133.1 (4) | C23—C24—C25—N3 | 0.4 (5) |
O1—Cu1'—N1—C5 | −46.9 (4) | Cu2—O7—C26—O8 | 2.7 (4) |
O1i—Cu1'—N1—C1 | −46.9 (4) | Cu2—O7—C26—C27 | −175.6 (2) |
O1—Cu1'—N1—C1 | 133.1 (4) | C28—O9—C27—C26 | 70.9 (4) |
O1i—Cu1'—N1—Cu1 | 103.3 (3) | O8—C26—C27—O9 | 23.5 (5) |
O1—Cu1'—N1—Cu1 | −76.7 (3) | O7—C26—C27—O9 | −158.1 (3) |
O1i—Cu1'—N1—Cu1i | −76.7 (3) | C27—O9—C28—C33 | −178.8 (3) |
O1—Cu1'—N1—Cu1i | 103.3 (3) | C27—O9—C28—C29 | −0.1 (5) |
O5—Cu2—N2—C20 | 133.0 (3) | O9—C28—C29—C30 | −178.1 (3) |
O7—Cu2—N2—C20 | −56.5 (3) | C33—C28—C29—C30 | 0.6 (5) |
O2w—Cu2—N2—C20 | 35.6 (3) | C28—C29—C30—C31 | −0.4 (6) |
O5—Cu2—N2—C16 | −48.2 (3) | C29—C30—C31—C32 | 0.6 (6) |
O7—Cu2—N2—C16 | 122.3 (3) | C34—O10—C32—C33 | −15.8 (5) |
O2w—Cu2—N2—C16 | −145.6 (3) | C34—O10—C32—C31 | 165.6 (3) |
O5—Cu2—N3—C25 | 51.1 (2) | C30—C31—C32—C33 | −0.9 (5) |
O7—Cu2—N3—C25 | −119.6 (2) | C30—C31—C32—O10 | 177.8 (3) |
O2w—Cu2—N3—C25 | 148.2 (2) | O10—C32—C33—C28 | −177.6 (3) |
O5—Cu2—N3—C21 | −126.7 (2) | C31—C32—C33—C28 | 1.0 (5) |
O7—Cu2—N3—C21 | 62.5 (2) | O9—C28—C33—C32 | 177.9 (3) |
O2w—Cu2—N3—C21 | −29.6 (3) | C29—C28—C33—C32 | −0.9 (5) |
O11ii—Cu3—N4—C40 | −65.8 (4) | C32—O10—C34—C35 | −69.9 (4) |
O11—Cu3—N4—C40 | 143.3 (4) | Cu3ii—O11—C35—O12 | 6.3 (7) |
N4ii—Cu3—N4—C40 | −150.3 (10) | Cu3'—O11—C35—O12 | −2.2 (5) |
O3w—Cu3—N4—C40 | 33.5 (5) | Cu3—O11—C35—O12 | −7.9 (5) |
O11ii—Cu3—N4—C36 | 125.1 (5) | Cu3ii—O11—C35—C34 | −174.6 (4) |
O11—Cu3—N4—C36 | −25.8 (6) | Cu3'—O11—C35—C34 | 176.9 (2) |
N4ii—Cu3—N4—C36 | 40.6 (13) | Cu3—O11—C35—C34 | 171.3 (3) |
O3w—Cu3—N4—C36 | −135.6 (4) | O10—C34—C35—O12 | −19.4 (5) |
O11ii—Cu3—N4—Cu3' | 84.5 (10) | O10—C34—C35—O11 | 161.4 (3) |
O11—Cu3—N4—Cu3' | −66.4 (9) | C40—N4—C36—C37 | −2.1 (7) |
N4ii—Cu3—N4—Cu3' | 0.000 (3) | Cu3—N4—C36—C37 | 166.2 (5) |
O3w—Cu3—N4—Cu3' | −176.2 (13) | Cu3'—N4—C36—C37 | 177.3 (4) |
O11ii—Cu3—N4—Cu3ii | 84.5 (10) | Cu3ii—N4—C36—C37 | −174.8 (5) |
O11—Cu3—N4—Cu3ii | −66.4 (9) | N4—C36—C37—C38 | 0.3 (8) |
N4ii—Cu3—N4—Cu3ii | 0.000 (2) | C36—C37—C38—C39 | 1.0 (9) |
O3w—Cu3—N4—Cu3ii | −176.2 (13) | C37—C38—C39—C40 | −0.5 (9) |
O11ii—Cu3'—N4—C40 | −46.5 (4) | C36—N4—C40—C39 | 2.6 (8) |
O11—Cu3'—N4—C40 | 133.5 (4) | Cu3—N4—C40—C39 | −168.3 (5) |
O11ii—Cu3'—N4—C36 | 134.1 (3) | Cu3'—N4—C40—C39 | −176.8 (4) |
O11—Cu3'—N4—C36 | −45.9 (3) | Cu3ii—N4—C40—C39 | 173.4 (5) |
O11ii—Cu3'—N4—Cu3 | −79.8 (11) | C38—C39—C40—N4 | −1.3 (9) |
Symmetry codes: (i) −x, −y+2, −z; (ii) −x+3, −y+1, −z+2. |
Hydrogen-bond geometry (Å, º) top
D—H···A | D—H | H···A | D···A | D—H···A |
O1w—H1w2···O2i | 0.85 (1) | 2.02 (3) | 2.792 (5) | 151 (5) |
O1w—H1w2···O12iii | 0.85 (1) | 2.83 (5) | 3.166 (5) | 106 (4) |
O2w—H2w2···O6 | 0.85 (1) | 1.95 (2) | 2.663 (4) | 140 (3) |
O2w—H2w1···O4w | 0.85 (1) | 1.90 (1) | 2.741 (4) | 172 (5) |
O3w—H3w2···O3iv | 0.85 (1) | 2.67 (4) | 3.189 (5) | 121 (4) |
O3w—H3w1···O12 | 0.86 (1) | 2.04 (3) | 2.722 (4) | 136 (4) |
O4w—H4w2···O6v | 0.86 (1) | 2.17 (2) | 2.919 (4) | 146 (4) |
O4w—H4w1···O5w | 0.86 (1) | 2.02 (2) | 2.812 (4) | 154 (5) |
O5w—H5w1···O1v | 0.86 (1) | 2.34 (4) | 2.982 (5) | 132 (4) |
O5w—H5w2···O7 | 0.86 (1) | 1.99 (2) | 2.830 (3) | 165 (5) |
O6w—H6w1···O8 | 0.86 (1) | 2.05 (2) | 2.889 (4) | 165 (6) |
O6w—H6w2···O9vi | 0.86 (1) | 2.52 (3) | 3.146 (4) | 131 (4) |
Symmetry codes: (i) −x, −y+2, −z; (iii) −x+2, −y+2, −z+1; (iv) x+2, y, z+1; (v) −x+1, −y+2, −z+1; (vi) −x+2, −y+1, −z+1. |
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