The structure of the title compound, {[Mn2Mo(CN)8(C4H4N2)2(H2O)2]·3H2O}n, is built up of MoIV atoms in a square-antiprismatic coordination, which are linked to distorted octahedrally coordinated MnII atoms through cyanide bridges to form a three-dimensional structure. The MnII atoms are also bridged by the pyrimidine ligands.
Supporting information
CCDC reference: 647285
Key indicators
- Single-crystal X-ray study
- T = 90 K
- Mean (C-C) = 0.004 Å
- H-atom completeness 67%
- Disorder in solvent or counterion
- R factor = 0.032
- wR factor = 0.088
- Data-to-parameter ratio = 14.3
checkCIF/PLATON results
No syntax errors found
Alert level A
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O3
| Author Response: ...
see _publ_section_exptl_refinement
|
PLAT306_ALERT_2_A Isolated Oxygen Atom (H-atoms Missing ?) ....... O4
| Author Response: ...
see _publ_section_exptl_refinement
|
Alert level B
PLAT430_ALERT_2_B Short Inter D...A Contact O3 .. N4 .. 2.76 Ang.
PLAT430_ALERT_2_B Short Inter D...A Contact O4 .. N3 .. 2.79 Ang.
Alert level C
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)... ?
PLAT094_ALERT_2_C Ratio of Maximum / Minimum Residual Density .... 2.19
PLAT220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.09 Ratio
PLAT302_ALERT_4_C Anion/Solvent Disorder ......................... 25.00 Perc.
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... >O5A
PLAT311_ALERT_2_C Isolated Disordered Oxygen Atom (No H's ?) ..... <O5B
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:C16 H18 Mn2 Mo1 N12 O5
Atom count from the _atom_site data: C16 H12 Mn2 Mo1 N12 O5
CELLZ01_ALERT_1_G Difference between formula and atom_site contents detected.
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 C16 H18 Mn2 Mo N12 O5
TEST: Compare cell contents of formula and atom_site data
atom Z*formula cif sites diff
C 64.00 64.00 0.00
H 72.00 48.00 24.00
Mn 8.00 8.00 0.00
Mo 4.00 4.00 0.00
N 48.00 48.00 0.00
O 20.00 20.00 0.00
2 ALERT level A = In general: serious problem
2 ALERT level B = Potentially serious problem
8 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
9 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
1 ALERT type 4 Improvement, methodology, query or suggestion
0 ALERT type 5 Informative message, check
Data collection: PROCESS-AUTO (Rigaku, 1998); cell refinement: PROCESS-AUTO; data reduction: CrystalStructure (Rigaku, 2006); program(s) used to solve structure: SIR97 (Altomare et al., 1999); program(s) used to refine structure: CRYSTALS (Betteridge et al., 2003); molecular graphics: ORTEP-3 (Farrugia, 1997) and VESTA (Momma & Izumi, 2006); software used to prepare material for publication: CrystalStructure.
Poly[[diaquahexa-µ-cyanido-dicyanido-di-µ-pyrimidine-
dimanganese(II)molybdate(IV)] trihydrate]
top
Crystal data top
[Mn2Mo(CN)8(C4H4N2)2(H2O)2]·3H2O | F(000) = 1320.00 |
Mr = 664.21 | Dx = 1.756 Mg m−3 |
Monoclinic, P21/n | Mo Kα radiation, λ = 0.71075 Å |
Hall symbol: -P 2yn | Cell parameters from 21390 reflections |
a = 13.0160 (6) Å | θ = 3.1–27.5° |
b = 12.8648 (4) Å | µ = 1.53 mm−1 |
c = 15.1056 (6) Å | T = 90 K |
β = 96.7670 (19)° | Platelet, yellow |
V = 2511.77 (17) Å3 | 0.30 × 0.27 × 0.07 mm |
Z = 4 | |
Data collection top
Rigaku R-AXIS RAPID diffractometer | 4944 reflections with F2 > 2σ(F2) |
Detector resolution: 10.00 pixels mm-1 | Rint = 0.032 |
ω scans | θmax = 27.5° |
Absorption correction: multi-scan (ABSCOR; Higashi, 1995) | h = −16→16 |
Tmin = 0.696, Tmax = 0.898 | k = −16→16 |
24053 measured reflections | l = −19→19 |
5745 independent reflections | |
Refinement top
Refinement on F2 | H-atom parameters constrained |
R[F2 > 2σ(F2)] = 0.032 | w = 1/[0.001Fo2 + σ(Fo2)]/(4Fo2) |
wR(F2) = 0.088 | (Δ/σ)max < 0.001 |
S = 1.00 | Δρmax = 1.93 e Å−3 |
4944 reflections | Δρmin = −0.88 e Å−3 |
346 parameters | |
Special details top
Refinement. Refinement was performed using reflections with F2 > 2.0
σ(F2). The weighted R-factor (wR) and goodness of fit
(S) are based on F2. R-factor (gt) are based on
F. The threshold expression of F2 > 2.0 σ(F2) is
used only for calculating R-factor (gt). |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top | x | y | z | Uiso*/Ueq | Occ. (<1) |
Mo | 0.17385 (2) | 0.174320 (10) | 0.466030 (10) | 0.00740 (5) | |
Mn1 | 0.30204 (3) | 0.37146 (3) | 0.77718 (3) | 0.01089 (9) | |
Mn2 | 0.36871 (3) | 0.29698 (3) | 0.18649 (3) | 0.01058 (9) | |
O1 | 0.23734 (16) | 0.25104 (15) | 0.85617 (14) | 0.0201 (4) | |
O2 | 0.2582 (2) | 0.2176 (2) | 0.09342 (16) | 0.0349 (6) | |
O3 | 0.13513 (17) | 0.35762 (17) | 0.98064 (16) | 0.0265 (5) | |
O4 | 0.1277 (2) | 0.6160 (2) | 0.5527 (2) | 0.0767 (10) | |
O5A | 0.5331 (4) | 0.2936 (4) | 0.6228 (3) | 0.0508 (14) | 0.60 |
O5B | 0.6919 (6) | 0.4777 (5) | 0.6367 (4) | 0.052 (2) | 0.40 |
N1 | 0.27441 (18) | 0.27820 (17) | 0.65655 (15) | 0.0155 (5) | |
N2 | 0.27277 (19) | 0.26710 (18) | 0.29085 (15) | 0.0172 (5) | |
N3 | 0.1240 (2) | 0.4269 (2) | 0.46245 (19) | 0.0295 (7) | |
N4 | 0.4255 (2) | 0.1251 (2) | 0.49041 (18) | 0.0270 (6) | |
N5 | −0.03740 (19) | 0.18203 (17) | 0.32036 (16) | 0.0156 (5) | |
N6 | 0.18869 (18) | −0.02021 (17) | 0.60963 (15) | 0.0144 (5) | |
N7 | −0.02385 (18) | 0.18879 (17) | 0.58453 (15) | 0.0143 (5) | |
N8 | 0.18389 (19) | −0.04191 (17) | 0.34781 (16) | 0.0168 (5) | |
N9 | 0.13005 (18) | 0.42813 (17) | 0.75056 (15) | 0.0165 (5) | |
N10 | −0.04046 (18) | 0.35708 (18) | 0.72620 (16) | 0.0168 (5) | |
N11 | 0.49092 (18) | 0.37600 (16) | 0.29007 (15) | 0.0141 (5) | |
N12 | 0.62438 (18) | 0.50375 (17) | 0.30390 (14) | 0.0136 (5) | |
C1 | 0.2405 (2) | 0.24248 (19) | 0.58958 (17) | 0.0126 (5) | |
C2 | 0.2371 (2) | 0.23582 (19) | 0.35156 (17) | 0.0125 (5) | |
C3 | 0.1403 (2) | 0.3391 (2) | 0.46172 (18) | 0.0157 (6) | |
C4 | 0.3376 (2) | 0.1408 (2) | 0.48202 (18) | 0.0157 (6) | |
C5 | 0.0368 (2) | 0.17845 (18) | 0.36993 (17) | 0.0115 (5) | |
C6 | 0.1816 (2) | 0.04517 (19) | 0.55709 (17) | 0.0121 (5) | |
C7 | 0.0427 (2) | 0.18251 (19) | 0.54080 (18) | 0.0128 (5) | |
C8 | 0.1788 (2) | 0.0346 (2) | 0.38684 (17) | 0.0129 (5) | |
C9 | 0.0619 (2) | 0.3520 (2) | 0.72806 (18) | 0.0161 (6) | |
C10 | 0.0895 (2) | 0.5200 (2) | 0.7721 (2) | 0.0241 (7) | |
C11 | −0.0160 (2) | 0.5333 (2) | 0.7709 (2) | 0.0355 (9) | |
C12 | −0.0791 (2) | 0.4486 (2) | 0.7488 (2) | 0.0277 (8) | |
C13 | 0.5525 (2) | 0.44517 (19) | 0.25724 (17) | 0.0140 (6) | |
C14 | 0.5024 (2) | 0.3637 (2) | 0.37895 (18) | 0.0170 (6) | |
C15 | 0.5744 (2) | 0.4211 (2) | 0.43375 (18) | 0.0181 (6) | |
C16 | 0.6345 (2) | 0.4912 (2) | 0.39357 (18) | 0.0170 (6) | |
H9 | 0.0895 | 0.2874 | 0.7117 | 0.019* | |
H10 | 0.1345 | 0.5768 | 0.7883 | 0.029* | |
H11 | −0.0442 | 0.5985 | 0.7850 | 0.043* | |
H12 | −0.1517 | 0.4553 | 0.7495 | 0.033* | |
H13 | 0.5443 | 0.4538 | 0.1943 | 0.017* | |
H14 | 0.4602 | 0.3149 | 0.4049 | 0.020* | |
H15 | 0.5822 | 0.4123 | 0.4966 | 0.022* | |
H16 | 0.6841 | 0.5317 | 0.4297 | 0.020* | |
H1A | 0.2034 | 0.2859 | 0.9000 | 0.025* | |
H1B | 0.2885 | 0.2084 | 0.8882 | 0.025* | |
H2A | 0.2731 | 0.1734 | 0.0462 | 0.041* | |
H2B | 0.1987 | 0.2549 | 0.0685 | 0.041* | |
Atomic displacement parameters (Å2) top | U11 | U22 | U33 | U12 | U13 | U23 |
Mo | 0.00851 (12) | 0.00750 (11) | 0.00615 (12) | −0.00022 (7) | 0.00066 (8) | −0.00015 (7) |
Mn1 | 0.0113 (2) | 0.01120 (18) | 0.00972 (19) | −0.00153 (14) | −0.00063 (15) | −0.00185 (14) |
Mn2 | 0.0109 (2) | 0.01108 (18) | 0.00996 (19) | −0.00053 (14) | 0.00207 (15) | 0.00229 (15) |
O1 | 0.0220 (10) | 0.0180 (9) | 0.0205 (9) | −0.0021 (7) | 0.0038 (8) | 0.0038 (8) |
O2 | 0.0335 (13) | 0.0428 (13) | 0.0263 (11) | −0.0143 (11) | −0.0053 (10) | −0.0074 (10) |
O3 | 0.0172 (10) | 0.0259 (10) | 0.0364 (12) | −0.0010 (8) | 0.0030 (9) | −0.0007 (9) |
O4 | 0.0329 (15) | 0.0460 (16) | 0.141 (3) | 0.0164 (12) | −0.0328 (19) | −0.060 (2) |
O5A | 0.051 (3) | 0.060 (2) | 0.043 (2) | 0.009 (2) | 0.015 (2) | 0.015 (2) |
O5B | 0.059 (4) | 0.049 (4) | 0.042 (3) | 0.024 (3) | −0.013 (3) | −0.012 (3) |
N1 | 0.0158 (11) | 0.0165 (10) | 0.0139 (10) | −0.0015 (8) | 0.0002 (8) | −0.0028 (9) |
N2 | 0.0179 (11) | 0.0191 (10) | 0.0149 (11) | 0.0007 (9) | 0.0032 (9) | 0.0030 (9) |
N3 | 0.0372 (16) | 0.0167 (11) | 0.0319 (14) | 0.0046 (10) | −0.0074 (12) | −0.0037 (10) |
N4 | 0.0191 (13) | 0.0350 (14) | 0.0270 (13) | 0.0041 (10) | 0.0029 (10) | 0.0054 (11) |
N5 | 0.0158 (11) | 0.0153 (10) | 0.0153 (11) | 0.0003 (8) | −0.0002 (9) | −0.0027 (8) |
N6 | 0.0171 (11) | 0.0144 (10) | 0.0123 (10) | 0.0026 (8) | 0.0038 (8) | 0.0027 (8) |
N7 | 0.0144 (11) | 0.0164 (10) | 0.0124 (10) | 0.0004 (8) | 0.0022 (9) | −0.0018 (8) |
N8 | 0.0187 (12) | 0.0156 (10) | 0.0165 (11) | −0.0013 (8) | 0.0039 (9) | −0.0031 (9) |
N9 | 0.0183 (12) | 0.0146 (10) | 0.0159 (11) | −0.0012 (8) | −0.0011 (9) | −0.0014 (8) |
N10 | 0.0150 (11) | 0.0152 (10) | 0.0206 (11) | −0.0010 (8) | 0.0038 (9) | −0.0026 (9) |
N11 | 0.0155 (11) | 0.0124 (9) | 0.0144 (10) | −0.0009 (8) | 0.0022 (8) | 0.0006 (8) |
N12 | 0.0151 (11) | 0.0135 (9) | 0.0120 (10) | 0.0002 (8) | 0.0000 (8) | −0.0013 (8) |
C1 | 0.0129 (12) | 0.0120 (10) | 0.0131 (11) | −0.0005 (9) | 0.0020 (9) | 0.0004 (9) |
C2 | 0.0123 (12) | 0.0116 (10) | 0.0133 (11) | 0.0012 (9) | 0.0010 (9) | −0.0002 (9) |
C3 | 0.0165 (13) | 0.0156 (12) | 0.0141 (12) | 0.0013 (10) | −0.0017 (10) | −0.0023 (10) |
C4 | 0.0134 (13) | 0.0203 (12) | 0.0135 (12) | 0.0011 (10) | 0.0020 (10) | 0.0008 (10) |
C5 | 0.0135 (12) | 0.0113 (10) | 0.0102 (11) | 0.0003 (9) | 0.0034 (9) | −0.0001 (9) |
C6 | 0.0098 (11) | 0.0146 (11) | 0.0119 (11) | 0.0011 (9) | 0.0013 (9) | −0.0045 (10) |
C7 | 0.0132 (12) | 0.0114 (10) | 0.0130 (12) | −0.0006 (9) | −0.0021 (10) | 0.0001 (9) |
C8 | 0.0121 (12) | 0.0145 (11) | 0.0120 (11) | −0.0007 (9) | 0.0012 (9) | 0.0004 (9) |
C9 | 0.0184 (13) | 0.0152 (11) | 0.0144 (12) | −0.0018 (10) | 0.0004 (10) | −0.0035 (10) |
C10 | 0.0238 (15) | 0.0144 (12) | 0.0333 (16) | −0.0013 (10) | 0.0000 (13) | −0.0045 (12) |
C11 | 0.0268 (17) | 0.0176 (13) | 0.062 (2) | 0.0044 (12) | 0.0051 (16) | −0.0139 (15) |
C12 | 0.0196 (15) | 0.0204 (13) | 0.0433 (19) | 0.0021 (11) | 0.0047 (13) | −0.0073 (13) |
C13 | 0.0174 (13) | 0.0131 (11) | 0.0114 (11) | 0.0003 (9) | 0.0008 (10) | −0.0006 (9) |
C14 | 0.0198 (14) | 0.0154 (11) | 0.0159 (13) | −0.0004 (10) | 0.0028 (10) | 0.0028 (10) |
C15 | 0.0222 (14) | 0.0205 (12) | 0.0113 (12) | 0.0032 (11) | −0.0001 (10) | 0.0024 (10) |
C16 | 0.0193 (13) | 0.0146 (11) | 0.0162 (12) | 0.0018 (10) | −0.0015 (10) | −0.0022 (10) |
Geometric parameters (Å, º) top
Mo—C1 | 2.150 (2) | N7—C7 | 1.152 (3) |
Mo—C2 | 2.151 (2) | N8—C8 | 1.153 (3) |
Mo—C3 | 2.164 (2) | N9—C9 | 1.338 (3) |
Mo—C4 | 2.160 (2) | N9—C10 | 1.350 (3) |
Mo—C5 | 2.164 (2) | N10—C9 | 1.330 (3) |
Mo—C6 | 2.152 (2) | N10—C12 | 1.340 (3) |
Mo—C7 | 2.158 (2) | N11—C13 | 1.331 (3) |
Mo—C8 | 2.164 (2) | N11—C14 | 1.343 (3) |
Mn1—O1 | 2.184 (2) | N12—C13 | 1.336 (3) |
Mn1—N1 | 2.176 (2) | N12—C16 | 1.355 (3) |
Mn1—N5i | 2.224 (2) | C10—C11 | 1.381 (4) |
Mn1—N6ii | 2.198 (2) | C11—C12 | 1.382 (4) |
Mn1—N9 | 2.344 (2) | C14—C15 | 1.388 (3) |
Mn1—N12iii | 2.296 (2) | C15—C16 | 1.380 (4) |
Mn2—O2 | 2.148 (2) | O1—H1A | 0.950 |
Mn2—N2 | 2.158 (2) | O1—H1B | 0.950 |
Mn2—N7iv | 2.207 (2) | O2—H2A | 0.950 |
Mn2—N8v | 2.225 (2) | O2—H2B | 0.950 |
Mn2—N10iv | 2.349 (2) | C9—H9 | 0.950 |
Mn2—N11 | 2.329 (2) | C10—H10 | 0.950 |
N1—C1 | 1.151 (3) | C11—H11 | 0.950 |
N2—C2 | 1.149 (3) | C12—H12 | 0.950 |
N3—C3 | 1.148 (3) | C13—H13 | 0.950 |
N4—C4 | 1.154 (3) | C14—H14 | 0.950 |
N5—C5 | 1.151 (3) | C15—H15 | 0.950 |
N6—C6 | 1.153 (3) | C16—H16 | 0.950 |
| | | |
Mn1···C9 | 3.137 (2) | O5B···H14iii | 3.338 |
Mn1···C10 | 3.356 (3) | O5B···H15 | 2.552 |
Mn1···C13iii | 3.107 (2) | O5B···H16 | 3.193 |
Mn1···C16iii | 3.310 (2) | O5B···H2Ai | 2.665 |
Mn2···C9iv | 3.165 (2) | O5B···H2Bi | 3.170 |
Mn2···C12iv | 3.343 (3) | N1···H9 | 2.640 |
Mn2···C13 | 3.145 (2) | N1···H9 | 2.641 |
Mn2···C14 | 3.320 (2) | N1···H10vii | 2.929 |
O1···O2vi | 3.588 (3) | N1···H16iii | 2.852 |
O1···O3 | 2.788 (3) | N2···H11xii | 3.514 |
O1···O4vii | 2.726 (3) | N2···H12iv | 3.113 |
O1···N9 | 3.027 (2) | N2···H14 | 2.882 |
O1···C9 | 3.100 (3) | N3···H12xii | 3.599 |
O1···C14viii | 3.449 (3) | N3···H16iii | 2.867 |
O1···C15viii | 3.370 (3) | N4···H10vii | 3.576 |
O1···C16viii | 3.465 (3) | N4···H11vii | 3.575 |
O2···O1ix | 3.588 (3) | N4···H14 | 2.822 |
O2···O3ix | 2.840 (3) | N5···H11xii | 3.469 |
O2···O4x | 3.093 (4) | N5···H13x | 2.945 |
O2···O5Axi | 3.018 (6) | N6···H10vii | 2.898 |
O2···O5Bxi | 2.760 (7) | N6···H13viii | 2.542 |
O2···N10iv | 3.252 (3) | N7···H9 | 2.609 |
O3···O1 | 2.788 (3) | N7···H13viii | 2.561 |
O3···O2vi | 2.840 (3) | N8···H12iv | 2.962 |
O3···O5Aviii | 3.291 (5) | N8···H13x | 2.964 |
O3···N4ii | 3.569 (3) | N9···H1A | 2.975 |
O3···N4viii | 2.759 (3) | N10···H14viii | 3.490 |
O3···N6ii | 3.213 (3) | N10···H2Aviii | 3.447 |
O3···N8ii | 3.535 (3) | N11···H9iv | 2.798 |
O3···N9 | 3.585 (3) | N1···H9 | 2.641 |
O3···C6ii | 3.487 (3) | N1···H10vii | 2.929 |
O3···C14viii | 3.582 (3) | N1···H16iii | 2.852 |
O4···O1ii | 2.726 (3) | N2···H11xii | 3.514 |
O4···O2v | 3.093 (4) | N2···H12iv | 3.113 |
O4···N3 | 2.787 (4) | N2···H14 | 2.882 |
O4···N3xii | 3.303 (4) | N3···H12xii | 3.599 |
O4···N5xii | 3.513 (4) | N3···H16iii | 2.867 |
O4···N7xii | 3.431 (4) | N4···H10vii | 3.576 |
O4···C3xii | 3.516 (4) | N4···H11vii | 3.575 |
O4···C7xii | 3.591 (3) | N4···H14 | 2.822 |
O4···C16iii | 3.399 (4) | N5···H11xii | 3.469 |
O5A···O2i | 3.018 (6) | N5···H13x | 2.945 |
O5A···O3iv | 3.291 (5) | N6···H10vii | 2.898 |
O5A···O5B | 3.136 (9) | N6···H13viii | 2.542 |
O5A···N1 | 3.470 (5) | N7···H9 | 2.609 |
O5A···N4 | 3.161 (5) | N7···H13viii | 2.561 |
O5A···N5i | 3.239 (5) | N8···H12iv | 2.962 |
O5A···N12iii | 3.572 (5) | N8···H13x | 2.964 |
O5A···C15 | 3.391 (5) | N9···H1A | 2.975 |
O5A···C16iii | 3.515 (5) | N10···H14viii | 3.490 |
O5B···O2i | 2.760 (7) | N10···H2Aviii | 3.447 |
O5B···O5A | 3.136 (9) | N11···H9iv | 2.798 |
O5B···N2iii | 3.474 (7) | C1···H9 | 2.907 |
O5B···N3iii | 3.214 (8) | C1···H10vii | 3.145 |
O5B···N8i | 3.308 (7) | C1···H16iii | 3.091 |
O5B···N11iii | 3.324 (8) | C2···H12iv | 3.323 |
O5B···C12xiii | 3.271 (7) | C2···H14 | 3.093 |
O5B···C14iii | 3.236 (8) | C3···H16iii | 3.130 |
O5B···C15 | 3.341 (7) | C4···H10vii | 3.543 |
N1···O5A | 3.470 (5) | C4···H14 | 3.058 |
N1···N9 | 3.146 (3) | C5···H13x | 3.189 |
N1···N12iii | 3.127 (3) | C6···H10vii | 3.168 |
N1···C9 | 3.229 (3) | C6···H13viii | 2.892 |
N1···C16iii | 3.315 (3) | C7···H9 | 2.913 |
N2···O5Biii | 3.474 (7) | C7···H13viii | 2.906 |
N2···N10iv | 3.158 (3) | C8···H12iv | 3.203 |
N2···N11 | 3.168 (3) | C8···H13x | 3.191 |
N2···C12iv | 3.479 (3) | C9···H1A | 3.121 |
N2···C14 | 3.363 (3) | C13···H9iv | 3.121 |
N3···O4 | 2.787 (4) | C14···H9iv | 3.482 |
N3···O4xii | 3.303 (4) | C14···H1Aiv | 3.234 |
N3···O5Biii | 3.214 (8) | C15···H1Aiv | 3.220 |
N3···C12xii | 3.557 (4) | C15···H1Biv | 3.385 |
N4···O3vii | 3.569 (3) | C15···H2Ai | 3.164 |
N4···O3iv | 2.759 (3) | C15···H2Bi | 3.333 |
N4···O5A | 3.161 (5) | C16···H1Biv | 3.265 |
N5···O4xii | 3.513 (4) | C16···H2Ai | 3.475 |
N5···O5Axi | 3.239 (5) | H9···Mn1 | 3.026 |
N5···N6xiv | 3.134 (3) | H9···Mn2viii | 3.053 |
N5···N12x | 3.093 (3) | H9···O1 | 2.774 |
N5···C13x | 3.262 (3) | H9···N1 | 2.641 |
N6···O3vii | 3.213 (3) | H9···N7 | 2.609 |
N6···N5xiv | 3.134 (3) | H9···N11viii | 2.798 |
N6···N9vii | 3.049 (3) | H9···C1 | 2.907 |
N6···N12viii | 3.152 (3) | H9···C7 | 2.913 |
N6···C10vii | 3.253 (3) | H9···C13viii | 3.121 |
N6···C13viii | 3.159 (3) | H9···C14viii | 3.482 |
N7···O4xii | 3.431 (4) | H9···H13viii | 3.164 |
N7···N8xiv | 3.075 (3) | H9···H1A | 3.049 |
N7···N10 | 3.070 (3) | H10···Mn1 | 3.443 |
N7···N11viii | 3.199 (3) | H10···O4 | 3.584 |
N7···C8xiv | 3.567 (3) | H10···N1ii | 2.929 |
N7···C9 | 3.128 (3) | H10···N4ii | 3.576 |
N7···C13viii | 3.186 (3) | H10···N6ii | 2.898 |
N8···O3vii | 3.535 (3) | H10···C1ii | 3.145 |
N8···O5Bxi | 3.308 (7) | H10···C4ii | 3.543 |
N8···N7xiv | 3.075 (3) | H10···C6ii | 3.168 |
N8···N11x | 3.084 (3) | H10···H1Bii | 3.407 |
N8···C13x | 3.295 (3) | H11···O5Aii | 2.866 |
N9···O1 | 3.027 (2) | H11···N2xii | 3.514 |
N9···O3 | 3.585 (3) | H11···N4ii | 3.575 |
N9···N1 | 3.146 (3) | H11···N5xii | 3.469 |
N9···N6ii | 3.049 (3) | H12···Mn2viii | 3.402 |
N9···N12iii | 3.504 (3) | H12···O2viii | 3.352 |
N10···O2viii | 3.252 (3) | H12···O5Bxv | 2.512 |
N10···N2viii | 3.158 (3) | H12···N2viii | 3.113 |
N10···N7 | 3.070 (3) | H12···N3xii | 3.599 |
N10···N11viii | 3.162 (3) | H12···N8viii | 2.962 |
N11···O5Biii | 3.324 (8) | H12···C2viii | 3.323 |
N11···N2 | 3.168 (3) | H12···C8viii | 3.203 |
N11···N7iv | 3.199 (3) | H12···H2Aviii | 3.524 |
N11···N8v | 3.084 (3) | H13···Mn1iii | 3.006 |
N11···N10iv | 3.162 (3) | H13···Mn2 | 3.041 |
N11···C9iv | 3.247 (3) | H13···N5v | 2.945 |
N12···O5Aiii | 3.572 (5) | H13···N6iv | 2.542 |
N12···N1iii | 3.127 (3) | H13···N7iv | 2.561 |
N12···N5v | 3.093 (3) | H13···N8v | 2.964 |
N12···N6iv | 3.152 (3) | H13···C5v | 3.189 |
N12···N9iii | 3.504 (3) | H13···C6iv | 2.892 |
C1···C9 | 3.594 (3) | H13···C7iv | 2.906 |
C3···O4xii | 3.516 (4) | H13···C8v | 3.191 |
C6···O3vii | 3.487 (3) | H13···H9iv | 3.164 |
C7···O4xii | 3.591 (3) | H14···Mn2 | 3.381 |
C7···C9 | 3.557 (3) | H14···O3iv | 3.287 |
C8···N7xiv | 3.567 (3) | H14···O5A | 3.327 |
C9···Mn1 | 3.137 (2) | H14···O5Biii | 3.338 |
C9···Mn2viii | 3.165 (2) | H14···N2 | 2.882 |
C9···O1 | 3.100 (3) | H14···N4 | 2.822 |
C9···N1 | 3.229 (3) | H14···N10iv | 3.490 |
C9···N7 | 3.128 (3) | H14···C2 | 3.093 |
C9···N11viii | 3.247 (3) | H14···C4 | 3.058 |
C9···C1 | 3.594 (3) | H14···H1Aiv | 3.430 |
C9···C7 | 3.557 (3) | H15···O2i | 3.064 |
C10···Mn1 | 3.356 (3) | H15···O3iv | 3.554 |
C10···N6ii | 3.253 (3) | H15···O5A | 2.581 |
C12···Mn2viii | 3.343 (3) | H15···O5B | 2.552 |
C12···O5Bxv | 3.271 (7) | H15···H1Aiv | 3.415 |
C12···N2viii | 3.479 (3) | H15···H2Ai | 2.740 |
C12···N3xii | 3.557 (4) | H15···H2Bi | 2.779 |
C13···Mn1iii | 3.107 (2) | H16···Mn1iii | 3.389 |
C13···Mn2 | 3.145 (2) | H16···O4iii | 3.087 |
C13···N5v | 3.262 (3) | H16···O5B | 3.193 |
C13···N6iv | 3.159 (3) | H16···N1iii | 2.852 |
C13···N7iv | 3.186 (3) | H16···N3iii | 2.867 |
C13···N8v | 3.295 (3) | H16···C1iii | 3.091 |
C14···Mn2 | 3.320 (2) | H16···C3iii | 3.130 |
C14···O1iv | 3.449 (3) | H16···H1Biv | 3.461 |
C14···O3iv | 3.582 (3) | H16···H2Ai | 3.304 |
C14···O5Biii | 3.236 (8) | H1A···O2vi | 3.054 |
C14···N2 | 3.363 (3) | H1A···O3 | 1.839 |
C15···O1iv | 3.370 (3) | H1A···O4vii | 3.122 |
C15···O5A | 3.391 (5) | H1A···N9 | 2.975 |
C15···O5B | 3.341 (7) | H1A···C9 | 3.121 |
C16···Mn1iii | 3.310 (2) | H1A···C14viii | 3.234 |
C16···O1iv | 3.465 (3) | H1A···C15viii | 3.220 |
C16···O4iii | 3.399 (4) | H1A···H9 | 3.049 |
C16···O5Aiii | 3.515 (5) | H1A···H14viii | 3.430 |
C16···N1iii | 3.315 (3) | H1A···H15viii | 3.415 |
Mn1···H9 | 3.026 | H1A···H2Avi | 2.706 |
Mn1···H10 | 3.443 | H1A···H2Bvi | 2.584 |
Mn1···H13iii | 3.006 | H1B···O2vi | 3.172 |
Mn1···H16iii | 3.389 | H1B···O3 | 3.205 |
Mn2···H9iv | 3.053 | H1B···O4vii | 1.781 |
Mn2···H12iv | 3.402 | H1B···C15viii | 3.385 |
Mn2···H13 | 3.041 | H1B···C16viii | 3.265 |
Mn2···H14 | 3.381 | H1B···H10vii | 3.407 |
O1···H9 | 2.774 | H1B···H16viii | 3.461 |
O1···H2Avi | 3.024 | H1B···H2Avi | 2.460 |
O1···H2Bvi | 3.305 | H1B···H2Bvi | 3.145 |
O2···H12iv | 3.352 | H2A···O1ix | 3.024 |
O2···H15xi | 3.064 | H2A···O3ix | 3.067 |
O2···H1Aix | 3.054 | H2A···O4x | 2.214 |
O2···H1Bix | 3.172 | H2A···O5Axi | 3.483 |
O3···H14viii | 3.287 | H2A···O5Bxi | 2.665 |
O3···H15viii | 3.554 | H2A···N10iv | 3.447 |
O3···H1A | 1.839 | H2A···C15xi | 3.164 |
O3···H1B | 3.205 | H2A···C16xi | 3.475 |
O3···H2Avi | 3.067 | H2A···H12iv | 3.524 |
O3···H2Bvi | 1.983 | H2A···H15xi | 2.740 |
O4···H10 | 3.584 | H2A···H16xi | 3.304 |
O4···H16iii | 3.087 | H2A···H1Aix | 2.706 |
O4···H1Aii | 3.122 | H2A···H1Bix | 2.460 |
O4···H1Bii | 1.781 | H2B···O1ix | 3.305 |
O4···H2Av | 2.214 | H2B···O3ix | 1.983 |
O4···H2Bv | 3.554 | H2B···O4x | 3.554 |
O5A···H11vii | 2.866 | H2B···O5Axi | 2.475 |
O5A···H14 | 3.327 | H2B···O5Bxi | 3.170 |
O5A···H15 | 2.581 | H2B···C15xi | 3.333 |
O5A···H2Ai | 3.483 | H2B···H15xi | 2.779 |
O5A···H2Bi | 2.475 | H2B···H1Aix | 2.584 |
O5B···H12xiii | 2.512 | H2B···H1Bix | 3.145 |
| | | |
C1—Mo—C2 | 113.23 (9) | Mn1—N1—C1 | 164.7 (2) |
C1—Mo—C3 | 71.70 (9) | Mn2—N2—C2 | 165.7 (2) |
C1—Mo—C4 | 72.10 (10) | Mn1—N5i—C5i | 150.0 (2) |
C1—Mo—C5 | 142.05 (9) | Mn1—N6ii—C6ii | 172.2 (2) |
C1—Mo—C6 | 77.07 (9) | Mn2—N7iv—C7iv | 170.7 (2) |
C1—Mo—C7 | 77.81 (9) | Mn2—N8v—C8v | 151.6 (2) |
C1—Mo—C8 | 141.55 (9) | C9—N9—C10 | 115.8 (2) |
C2—Mo—C3 | 73.18 (10) | C9—N10—C12 | 116.3 (2) |
C2—Mo—C4 | 72.40 (9) | C13—N11—C14 | 116.7 (2) |
C2—Mo—C5 | 79.33 (9) | Mn1iii—N12—C13 | 115.05 (16) |
C2—Mo—C6 | 143.54 (9) | Mn1iii—N12—C16 | 128.24 (17) |
C2—Mo—C7 | 143.50 (9) | C13—N12—C16 | 116.1 (2) |
C2—Mo—C8 | 79.74 (9) | Mo—C1—N1 | 178.6 (2) |
C3—Mo—C4 | 113.09 (10) | Mo—C2—N2 | 178.4 (2) |
C3—Mo—C5 | 78.93 (9) | Mo—C3—N3 | 177.6 (2) |
C3—Mo—C6 | 140.33 (10) | Mo—C4—N4 | 178.5 (2) |
C3—Mo—C7 | 78.37 (10) | Mo—C5—N5 | 178.3 (2) |
C3—Mo—C8 | 144.69 (9) | Mo—C6—N6 | 176.0 (2) |
C4—Mo—C5 | 143.57 (10) | Mo—C7—N7 | 176.3 (2) |
C4—Mo—C6 | 78.64 (10) | Mo—C8—N8 | 177.0 (2) |
C4—Mo—C7 | 141.48 (9) | N9—C9—N10 | 127.0 (2) |
C4—Mo—C8 | 78.61 (9) | N9—C10—C11 | 121.4 (2) |
C5—Mo—C6 | 114.87 (9) | C10—C11—C12 | 117.9 (3) |
C5—Mo—C7 | 73.09 (10) | N10—C12—C11 | 121.6 (3) |
C5—Mo—C8 | 74.08 (9) | N11—C13—N12 | 126.5 (2) |
C6—Mo—C7 | 71.55 (9) | N11—C14—C15 | 121.4 (2) |
C6—Mo—C8 | 73.13 (9) | C14—C15—C16 | 117.6 (2) |
C7—Mo—C8 | 114.01 (9) | N12—C16—C15 | 121.6 (2) |
O1—Mn1—N1 | 91.72 (8) | Mn1—O1—H1A | 106.7 |
O1—Mn1—N5i | 91.71 (8) | Mn1—O1—H1B | 113.3 |
O1—Mn1—N6ii | 90.81 (8) | H1A—O1—H1B | 105.8 |
O1—Mn1—N9 | 83.82 (7) | Mn2—O2—H2A | 126.6 |
O1—Mn1—N12iii | 178.04 (7) | Mn2—O2—H2B | 118.1 |
N1—Mn1—N5i | 97.58 (8) | H2A—O2—H2B | 103.6 |
N1—Mn1—N6ii | 171.69 (8) | N9—C9—H9 | 116.5 |
N1—Mn1—N9 | 88.14 (8) | N10—C9—H9 | 116.5 |
N1—Mn1—N12iii | 88.68 (8) | N9—C10—H10 | 119.3 |
N5i—Mn1—N6ii | 90.26 (8) | C11—C10—H10 | 119.3 |
N5i—Mn1—N12iii | 86.34 (8) | C10—C11—H11 | 121.1 |
N6ii—Mn1—N12iii | 89.05 (8) | C12—C11—H11 | 121.0 |
O2—Mn2—N2 | 89.59 (9) | N10—C12—H12 | 119.2 |
O2—Mn2—N7iv | 90.77 (9) | C11—C12—H12 | 119.3 |
O2—Mn2—N8v | 97.26 (9) | N11—C13—H13 | 116.7 |
O2—Mn2—N10iv | 92.54 (8) | N12—C13—H13 | 116.7 |
O2—Mn2—N11 | 177.48 (8) | N11—C14—H14 | 119.3 |
N2—Mn2—N7iv | 173.53 (8) | C15—C14—H14 | 119.2 |
N2—Mn2—N8v | 98.48 (9) | C14—C15—H15 | 121.2 |
N2—Mn2—N10iv | 88.87 (8) | C16—C15—H15 | 121.2 |
N2—Mn2—N11 | 89.72 (8) | N12—C16—H16 | 119.2 |
N7iv—Mn2—N8v | 87.89 (8) | C15—C16—H16 | 119.2 |
Symmetry codes: (i) x+1/2, −y+1/2, z+1/2; (ii) −x+1/2, y+1/2, −z+3/2; (iii) −x+1, −y+1, −z+1; (iv) x+1/2, −y+1/2, z−1/2; (v) −x+1/2, y+1/2, −z+1/2; (vi) x, y, z+1; (vii) −x+1/2, y−1/2, −z+3/2; (viii) x−1/2, −y+1/2, z+1/2; (ix) x, y, z−1; (x) −x+1/2, y−1/2, −z+1/2; (xi) x−1/2, −y+1/2, z−1/2; (xii) −x, −y+1, −z+1; (xiii) x+1, y, z; (xiv) −x, −y, −z+1; (xv) x−1, y, z. |