Supporting information
Crystallographic Information File (CIF) https://doi.org/10.1107/S0108768112043996/gp5056sup1.cif | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768112043996/gp50561asup2.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768112043996/gp50561bsup3.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768112043996/gp50561csup4.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768112043996/gp50562asup5.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768112043996/gp50562bsup6.hkl | |
Structure factor file (CIF format) https://doi.org/10.1107/S0108768112043996/gp50562csup7.hkl | |
Portable Document Format (PDF) file https://doi.org/10.1107/S0108768112043996/gp5056sup8.pdf |
CCDC references: 914848; 914849; 914850; 914851; 914852; 914853
For all compounds, program(s) used to solve structure: SHELXS97 (Sheldrick, 1990); program(s) used to refine structure: SHELXL97 (Sheldrick, 1997).
C5H9Cl2MnNO2·H2O | F(000) = 524 |
Mr = 258.99 | Dx = 1.829 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 1584 reflections |
a = 7.0862 (6) Å | θ = 2.6–21.4° |
b = 10.0235 (8) Å | µ = 1.94 mm−1 |
c = 13.2437 (11) Å | T = 100 K |
V = 940.68 (13) Å3 | 0.14 × 0.06 × 0.05 mm |
Z = 4 |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 2039 independent reflections |
Radiation source: microsource | 1797 reflections with I > 2σ(I) |
Multi layer optics monochromator | Rint = 0.058 |
ω scans | θmax = 27.1°, θmin = 2.6° |
Absorption correction: multi-scan SADABS | h = −8→8 |
Tmin = 0.773, Tmax = 0.909 | k = −12→12 |
11373 measured reflections | l = −16→16 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.032 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.074 | w = 1/[σ2(Fo2) + (0.035P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.06 | (Δ/σ)max = 0.001 |
2039 reflections | Δρmax = 0.52 e Å−3 |
121 parameters | Δρmin = −0.33 e Å−3 |
4 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.02 (4) |
C5H9Cl2MnNO2·H2O | V = 940.68 (13) Å3 |
Mr = 258.99 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 7.0862 (6) Å | µ = 1.94 mm−1 |
b = 10.0235 (8) Å | T = 100 K |
c = 13.2437 (11) Å | 0.14 × 0.06 × 0.05 mm |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 2039 independent reflections |
Absorption correction: multi-scan SADABS | 1797 reflections with I > 2σ(I) |
Tmin = 0.773, Tmax = 0.909 | Rint = 0.058 |
11373 measured reflections |
R[F2 > 2σ(F2)] = 0.032 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.074 | Δρmax = 0.52 e Å−3 |
S = 1.06 | Δρmin = −0.33 e Å−3 |
2039 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
121 parameters | Absolute structure parameter: −0.02 (4) |
4 restraints |
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, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Mn1 | 0.32439 (6) | 0.24773 (5) | 0.50034 (4) | 0.01702 (13) | |
Cl1 | 0.57461 (12) | 0.36706 (8) | 0.60399 (6) | 0.02109 (18) | |
Cl2 | 0.57519 (12) | 0.06994 (7) | 0.46770 (5) | 0.01899 (17) | |
O1 | 0.4195 (3) | 0.3579 (2) | 0.37232 (15) | 0.0220 (5) | |
O2 | 0.7347 (3) | 0.3581 (2) | 0.36705 (16) | 0.0207 (5) | |
C1 | 0.5733 (5) | 0.4069 (3) | 0.3492 (2) | 0.0176 (6) | |
C2 | 0.5742 (5) | 0.5406 (3) | 0.2945 (2) | 0.0249 (7) | |
H2 | 0.6477 | 0.5351 | 0.2302 | 0.030* | |
C3 | 0.6488 (6) | 0.6513 (4) | 0.3617 (4) | 0.0408 (11) | |
H3A | 0.7552 | 0.6194 | 0.4037 | 0.049* | |
H3B | 0.6914 | 0.7285 | 0.3211 | 0.049* | |
C4 | 0.4804 (6) | 0.6881 (4) | 0.4268 (3) | 0.0464 (12) | |
H4A | 0.4938 | 0.7796 | 0.4539 | 0.056* | |
H4B | 0.4667 | 0.6250 | 0.4839 | 0.056* | |
C5 | 0.3123 (6) | 0.6788 (4) | 0.3561 (3) | 0.0342 (10) | |
H5A | 0.1997 | 0.6452 | 0.3922 | 0.041* | |
H5B | 0.2826 | 0.7672 | 0.3267 | 0.041* | |
N1 | 0.3728 (4) | 0.5818 (3) | 0.2746 (2) | 0.0230 (7) | |
H1A | 0.285 (4) | 0.516 (3) | 0.281 (3) | 0.028* | |
H1B | 0.363 (5) | 0.619 (3) | 0.2126 (17) | 0.028* | |
O3 | 0.0825 (4) | 0.4035 (3) | 0.2380 (2) | 0.0392 (7) | |
H1O | 0.015 (5) | 0.377 (4) | 0.290 (2) | 0.047* | |
H2O | 0.006 (5) | 0.452 (4) | 0.199 (3) | 0.047* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0132 (2) | 0.0212 (2) | 0.0166 (2) | −0.00012 (18) | 0.00084 (17) | 0.0030 (2) |
Cl1 | 0.0158 (4) | 0.0258 (4) | 0.0217 (4) | 0.0012 (4) | −0.0014 (4) | −0.0042 (3) |
Cl2 | 0.0160 (4) | 0.0192 (3) | 0.0218 (4) | 0.0001 (4) | −0.0001 (4) | 0.0008 (3) |
O1 | 0.0185 (12) | 0.0269 (12) | 0.0207 (12) | −0.0026 (12) | 0.0009 (12) | 0.0105 (10) |
O2 | 0.0149 (12) | 0.0285 (13) | 0.0186 (13) | 0.0022 (11) | 0.0011 (10) | 0.0067 (11) |
C1 | 0.0194 (16) | 0.0213 (16) | 0.0119 (14) | −0.0011 (16) | −0.0010 (15) | −0.0002 (12) |
C2 | 0.0173 (16) | 0.0300 (18) | 0.0274 (18) | 0.0032 (18) | 0.0007 (17) | 0.0114 (14) |
C3 | 0.038 (2) | 0.027 (2) | 0.058 (3) | −0.0076 (18) | −0.014 (2) | 0.007 (2) |
C4 | 0.078 (4) | 0.024 (2) | 0.037 (2) | 0.001 (2) | −0.013 (2) | −0.0044 (18) |
C5 | 0.047 (3) | 0.027 (2) | 0.028 (2) | 0.0081 (19) | 0.0118 (19) | 0.0036 (17) |
N1 | 0.0246 (17) | 0.0249 (16) | 0.0193 (15) | 0.0049 (13) | −0.0008 (12) | 0.0058 (13) |
O3 | 0.0346 (16) | 0.0481 (17) | 0.0349 (15) | −0.0014 (17) | −0.0006 (15) | 0.0179 (13) |
Mn1—O1 | 2.133 (2) | C2—H2 | 1.0000 |
Mn1—O2i | 2.148 (2) | C3—C4 | 1.517 (6) |
Mn1—Cl1i | 2.5231 (9) | C3—H3A | 0.9900 |
Mn1—Cl1 | 2.5414 (10) | C3—H3B | 0.9900 |
Mn1—Cl2 | 2.5536 (9) | C4—C5 | 1.518 (5) |
Mn1—Cl2i | 2.5764 (9) | C4—H4A | 0.9900 |
Cl1—Mn1ii | 2.5231 (9) | C4—H4B | 0.9900 |
Cl2—Mn1ii | 2.5764 (9) | C5—N1 | 1.514 (5) |
O1—C1 | 1.234 (4) | C5—H5A | 0.9900 |
O2—C1 | 1.266 (4) | C5—H5B | 0.9900 |
O2—Mn1ii | 2.148 (2) | N1—H1A | 0.906 (18) |
C1—C2 | 1.523 (4) | N1—H1B | 0.906 (18) |
C2—N1 | 1.509 (4) | O3—H1O | 0.878 (19) |
C2—C3 | 1.517 (5) | O3—H2O | 0.890 (18) |
O1—Mn1—O2i | 177.78 (10) | C1—C2—H2 | 111.0 |
O1—Mn1—Cl1i | 91.29 (7) | C4—C3—C2 | 103.7 (3) |
O2i—Mn1—Cl1i | 90.87 (6) | C4—C3—H3A | 111.0 |
O1—Mn1—Cl1 | 88.00 (7) | C2—C3—H3A | 111.0 |
O2i—Mn1—Cl1 | 89.83 (7) | C4—C3—H3B | 111.0 |
Cl1i—Mn1—Cl1 | 179.03 (3) | C2—C3—H3B | 111.0 |
O1—Mn1—Cl2 | 90.39 (7) | H3A—C3—H3B | 109.0 |
O2i—Mn1—Cl2 | 89.99 (7) | C3—C4—C5 | 104.6 (3) |
Cl1i—Mn1—Cl2 | 94.43 (3) | C3—C4—H4A | 110.8 |
Cl1—Mn1—Cl2 | 86.23 (3) | C5—C4—H4A | 110.8 |
O1—Mn1—Cl2i | 88.84 (7) | C3—C4—H4B | 110.8 |
O2i—Mn1—Cl2i | 90.75 (7) | C5—C4—H4B | 110.8 |
Cl1i—Mn1—Cl2i | 86.13 (3) | H4A—C4—H4B | 108.9 |
Cl1—Mn1—Cl2i | 93.19 (3) | N1—C5—C4 | 104.9 (3) |
Cl2—Mn1—Cl2i | 179.06 (3) | N1—C5—H5A | 110.8 |
Mn1ii—Cl1—Mn1 | 88.80 (2) | C4—C5—H5A | 110.8 |
Mn1—Cl2—Mn1ii | 87.37 (2) | N1—C5—H5B | 110.8 |
C1—O1—Mn1 | 133.0 (2) | C4—C5—H5B | 110.8 |
C1—O2—Mn1ii | 127.6 (2) | H5A—C5—H5B | 108.8 |
O1—C1—O2 | 126.7 (3) | C2—N1—C5 | 108.6 (3) |
O1—C1—C2 | 118.1 (3) | C2—N1—H1A | 116 (3) |
O2—C1—C2 | 115.2 (3) | C5—N1—H1A | 102 (3) |
N1—C2—C3 | 103.4 (3) | C2—N1—H1B | 110 (2) |
N1—C2—C1 | 108.7 (3) | C5—N1—H1B | 111 (2) |
C3—C2—C1 | 111.5 (3) | H1A—N1—H1B | 109 (3) |
N1—C2—H2 | 111.0 | H1O—O3—H2O | 106 (4) |
C3—C2—H2 | 111.0 |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1; (ii) x+1/2, −y+1/2, −z+1. |
C7H17Br2MnNO4 | F(000) = 386 |
Mr = 393.98 | Dx = 2.039 Mg m−3 |
Monoclinic, P21 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2yb | Cell parameters from 1044 reflections |
a = 8.286 (2) Å | θ = 2.5–22.3° |
b = 8.256 (2) Å | µ = 7.25 mm−1 |
c = 9.387 (3) Å | T = 100 K |
β = 92.172 (4)° | Needle, colorless |
V = 641.7 (3) Å3 | 0.27 × 0.08 × 0.08 mm |
Z = 2 |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 2665 independent reflections |
Radiation source: microsource | 2440 reflections with I > 2σ(I) |
Multi layer optics monochromator | Rint = 0.061 |
ω scans | θmax = 26.5°, θmin = 2.2° |
Absorption correction: multi-scan SADABS | h = −10→10 |
Tmin = 0.245, Tmax = 0.595 | k = −10→10 |
7642 measured reflections | l = −11→11 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.035 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.064 | w = 1/[σ2(Fo2) + (0.P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.00 | (Δ/σ)max = 0.001 |
2665 reflections | Δρmax = 0.61 e Å−3 |
152 parameters | Δρmin = −0.48 e Å−3 |
4 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: 0.015 (12) |
C7H17Br2MnNO4 | V = 641.7 (3) Å3 |
Mr = 393.98 | Z = 2 |
Monoclinic, P21 | Mo Kα radiation |
a = 8.286 (2) Å | µ = 7.25 mm−1 |
b = 8.256 (2) Å | T = 100 K |
c = 9.387 (3) Å | 0.27 × 0.08 × 0.08 mm |
β = 92.172 (4)° |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 2665 independent reflections |
Absorption correction: multi-scan SADABS | 2440 reflections with I > 2σ(I) |
Tmin = 0.245, Tmax = 0.595 | Rint = 0.061 |
7642 measured reflections |
R[F2 > 2σ(F2)] = 0.035 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.064 | Δρmax = 0.61 e Å−3 |
S = 1.00 | Δρmin = −0.48 e Å−3 |
2665 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
152 parameters | Absolute structure parameter: 0.015 (12) |
4 restraints |
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, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Mn1 | −0.00733 (9) | 0.82303 (10) | 0.66340 (8) | 0.01330 (18) | |
Br1 | 0.10226 (6) | 0.84859 (6) | 0.92578 (5) | 0.01619 (13) | |
Br2 | −0.26334 (6) | 0.65186 (7) | 0.71320 (6) | 0.01977 (14) | |
O1 | −0.0888 (4) | 0.8426 (5) | 0.4355 (3) | 0.0164 (8) | |
O2 | −0.1196 (4) | 1.1077 (4) | 0.4017 (4) | 0.0154 (8) | |
C1 | −0.1209 (6) | 0.9616 (7) | 0.3596 (5) | 0.0144 (12) | |
C2 | −0.1742 (7) | 0.9361 (6) | 0.2035 (5) | 0.0136 (12) | |
H2 | −0.1017 | 0.9986 | 0.1409 | 0.016* | |
C3 | −0.3499 (7) | 0.9880 (7) | 0.1733 (6) | 0.0210 (13) | |
H3A | −0.4103 | 0.9912 | 0.2623 | 0.025* | |
H3B | −0.3553 | 1.0961 | 0.1277 | 0.025* | |
C4 | −0.4172 (6) | 0.8570 (7) | 0.0721 (5) | 0.0175 (11) | |
H4A | −0.5362 | 0.8497 | 0.0756 | 0.021* | |
H4B | −0.3872 | 0.8780 | −0.0273 | 0.021* | |
C5 | −0.3379 (7) | 0.7068 (7) | 0.1296 (6) | 0.0229 (14) | |
H5A | −0.3406 | 0.6195 | 0.0572 | 0.028* | |
H5B | −0.3915 | 0.6680 | 0.2157 | 0.028* | |
N1 | −0.1682 (6) | 0.7588 (5) | 0.1651 (5) | 0.0134 (10) | |
H1A | −0.105 (5) | 0.756 (7) | 0.085 (4) | 0.016* | |
H1B | −0.117 (5) | 0.702 (6) | 0.238 (4) | 0.016* | |
O3 | 0.2121 (5) | 0.9575 (5) | 0.5868 (4) | 0.0207 (9) | |
H3 | 0.207 (7) | 0.997 (7) | 0.508 (5) | 0.027 (19)* | |
C6 | 0.3698 (6) | 0.8857 (7) | 0.5969 (6) | 0.0220 (14) | |
H7A | 0.3953 | 0.8549 | 0.6960 | 0.033* | |
H7B | 0.4499 | 0.9639 | 0.5653 | 0.033* | |
H7C | 0.3718 | 0.7892 | 0.5362 | 0.033* | |
O4 | −0.0991 (5) | 1.0725 (5) | 0.6809 (4) | 0.0174 (9) | |
H4 | −0.111 (7) | 1.085 (8) | 0.595 (5) | 0.026 (19)* | |
C7 | −0.2383 (6) | 1.1217 (8) | 0.7557 (6) | 0.0230 (14) | |
H6A | −0.3328 | 1.0606 | 0.7199 | 0.035* | |
H6B | −0.2571 | 1.2378 | 0.7407 | 0.035* | |
H6C | −0.2204 | 1.1004 | 0.8578 | 0.035* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0166 (4) | 0.0108 (5) | 0.0124 (4) | −0.0003 (4) | 0.0001 (3) | 0.0000 (3) |
Br1 | 0.0215 (3) | 0.0145 (3) | 0.0124 (2) | −0.0014 (3) | −0.0001 (2) | −0.0005 (2) |
Br2 | 0.0182 (3) | 0.0191 (3) | 0.0224 (3) | −0.0047 (3) | 0.0047 (2) | −0.0030 (3) |
O1 | 0.0213 (19) | 0.0117 (19) | 0.0162 (17) | −0.0005 (19) | 0.0013 (14) | −0.0020 (19) |
O2 | 0.023 (2) | 0.008 (2) | 0.0156 (19) | −0.0021 (16) | 0.0014 (16) | −0.0005 (15) |
C1 | 0.012 (3) | 0.018 (3) | 0.014 (3) | −0.002 (2) | 0.004 (2) | 0.000 (2) |
C2 | 0.018 (3) | 0.008 (3) | 0.014 (3) | 0.003 (2) | −0.003 (2) | 0.003 (2) |
C3 | 0.020 (3) | 0.018 (3) | 0.024 (3) | 0.007 (3) | −0.005 (2) | −0.003 (3) |
C4 | 0.015 (3) | 0.018 (3) | 0.019 (3) | 0.003 (3) | −0.003 (2) | 0.004 (3) |
C5 | 0.016 (3) | 0.021 (3) | 0.032 (3) | −0.006 (2) | −0.003 (3) | 0.001 (3) |
N1 | 0.016 (3) | 0.010 (2) | 0.015 (2) | 0.0000 (19) | 0.0022 (19) | −0.0027 (19) |
O3 | 0.019 (2) | 0.021 (2) | 0.023 (2) | 0.0008 (18) | 0.0029 (18) | 0.0104 (19) |
C6 | 0.013 (3) | 0.025 (4) | 0.028 (3) | −0.002 (2) | 0.001 (2) | 0.002 (3) |
O4 | 0.024 (2) | 0.014 (2) | 0.013 (2) | 0.0039 (17) | 0.0045 (17) | −0.0018 (17) |
C7 | 0.021 (3) | 0.024 (4) | 0.024 (3) | 0.003 (3) | 0.006 (2) | −0.003 (3) |
Mn1—O2i | 2.165 (3) | C4—H4A | 0.9900 |
Mn1—O4 | 2.204 (4) | C4—H4B | 0.9900 |
Mn1—O1 | 2.225 (3) | C5—N1 | 1.496 (7) |
Mn1—O3 | 2.270 (4) | C5—H5A | 0.9900 |
Mn1—Br1 | 2.6011 (11) | C5—H5B | 0.9900 |
Mn1—Br2 | 2.6060 (11) | N1—H1A | 0.931 (19) |
O1—C1 | 1.237 (6) | N1—H1B | 0.924 (19) |
O2—C1 | 1.269 (6) | O3—C6 | 1.435 (6) |
O2—Mn1ii | 2.165 (3) | O3—H3 | 0.81 (4) |
C1—C2 | 1.529 (7) | C6—H7A | 0.9800 |
C2—N1 | 1.509 (6) | C6—H7B | 0.9800 |
C2—C3 | 1.534 (7) | C6—H7C | 0.9800 |
C2—H2 | 1.0000 | O4—C7 | 1.432 (6) |
C3—C4 | 1.531 (8) | O4—H4 | 0.82 (4) |
C3—H3A | 0.9900 | C7—H6A | 0.9800 |
C3—H3B | 0.9900 | C7—H6B | 0.9800 |
C4—C5 | 1.494 (8) | C7—H6C | 0.9800 |
O2i—Mn1—O4 | 163.94 (14) | C3—C4—H4A | 111.3 |
O2i—Mn1—O1 | 85.49 (14) | C5—C4—H4B | 111.3 |
O4—Mn1—O1 | 84.87 (14) | C3—C4—H4B | 111.3 |
O2i—Mn1—O3 | 84.76 (14) | H4A—C4—H4B | 109.2 |
O4—Mn1—O3 | 81.34 (14) | C4—C5—N1 | 103.8 (4) |
O1—Mn1—O3 | 82.96 (14) | C4—C5—H5A | 111.0 |
O2i—Mn1—Br1 | 100.25 (10) | N1—C5—H5A | 111.0 |
O4—Mn1—Br1 | 87.86 (10) | C4—C5—H5B | 111.0 |
O1—Mn1—Br1 | 170.74 (11) | N1—C5—H5B | 111.0 |
O3—Mn1—Br1 | 90.29 (11) | H5A—C5—H5B | 109.0 |
O2i—Mn1—Br2 | 90.73 (10) | C5—N1—C2 | 107.0 (4) |
O4—Mn1—Br2 | 102.00 (11) | C5—N1—H1A | 112 (3) |
O1—Mn1—Br2 | 89.57 (10) | C2—N1—H1A | 104 (3) |
O3—Mn1—Br2 | 171.54 (11) | C5—N1—H1B | 115 (3) |
Br1—Mn1—Br2 | 97.56 (3) | C2—N1—H1B | 110 (3) |
C1—O1—Mn1 | 131.5 (3) | H1A—N1—H1B | 109 (4) |
C1—O2—Mn1ii | 133.7 (3) | C6—O3—Mn1 | 121.0 (3) |
O1—C1—O2 | 125.2 (5) | C6—O3—H3 | 104 (4) |
O1—C1—C2 | 119.4 (5) | Mn1—O3—H3 | 118 (4) |
O2—C1—C2 | 115.4 (5) | O3—C6—H7A | 109.5 |
N1—C2—C1 | 110.6 (4) | O3—C6—H7B | 109.5 |
N1—C2—C3 | 105.5 (4) | H7A—C6—H7B | 109.5 |
C1—C2—C3 | 112.1 (4) | O3—C6—H7C | 109.5 |
N1—C2—H2 | 109.5 | H7A—C6—H7C | 109.5 |
C1—C2—H2 | 109.5 | H7B—C6—H7C | 109.5 |
C3—C2—H2 | 109.5 | C7—O4—Mn1 | 126.1 (3) |
C4—C3—C2 | 103.8 (4) | C7—O4—H4 | 112 (4) |
C4—C3—H3A | 111.0 | Mn1—O4—H4 | 94 (4) |
C2—C3—H3A | 111.0 | O4—C7—H6A | 109.5 |
C4—C3—H3B | 111.0 | O4—C7—H6B | 109.5 |
C2—C3—H3B | 111.0 | H6A—C7—H6B | 109.5 |
H3A—C3—H3B | 109.0 | O4—C7—H6C | 109.5 |
C5—C4—C3 | 102.6 (4) | H6A—C7—H6C | 109.5 |
C5—C4—H4A | 111.3 | H6B—C7—H6C | 109.5 |
Symmetry codes: (i) −x, y−1/2, −z+1; (ii) −x, y+1/2, −z+1. |
C5H15IMnNO5·I | F(000) = 892 |
Mr = 477.92 | Dx = 2.398 Mg m−3 |
Orthorhombic, P212121 | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: P 2ac 2ab | Cell parameters from 1755 reflections |
a = 8.1264 (18) Å | θ = 2.3–25.5° |
b = 11.867 (3) Å | µ = 5.66 mm−1 |
c = 13.727 (3) Å | T = 100 K |
V = 1323.8 (5) Å3 | Needle, orange |
Z = 4 | 0.14 × 0.08 × 0.08 mm |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 2690 independent reflections |
Radiation source: microsource | 2412 reflections with I > 2σ(I) |
Multi layer optics monochromator | Rint = 0.086 |
ω scans | θmax = 26.4°, θmin = 2.3° |
Absorption correction: multi-scan SADABS | h = −10→10 |
Tmin = 0.505, Tmax = 0.660 | k = −14→14 |
15709 measured reflections | l = −17→17 |
Refinement on F2 | Secondary atom site location: difference Fourier map |
Least-squares matrix: full | Hydrogen site location: inferred from neighbouring sites |
R[F2 > 2σ(F2)] = 0.033 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.078 | w = 1/[σ2(Fo2) + (0.030P)2] where P = (Fo2 + 2Fc2)/3 |
S = 1.03 | (Δ/σ)max = 0.001 |
2690 reflections | Δρmax = 1.13 e Å−3 |
151 parameters | Δρmin = −1.09 e Å−3 |
21 restraints | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
Primary atom site location: structure-invariant direct methods | Absolute structure parameter: −0.05 (5) |
C5H15IMnNO5·I | V = 1323.8 (5) Å3 |
Mr = 477.92 | Z = 4 |
Orthorhombic, P212121 | Mo Kα radiation |
a = 8.1264 (18) Å | µ = 5.66 mm−1 |
b = 11.867 (3) Å | T = 100 K |
c = 13.727 (3) Å | 0.14 × 0.08 × 0.08 mm |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 2690 independent reflections |
Absorption correction: multi-scan SADABS | 2412 reflections with I > 2σ(I) |
Tmin = 0.505, Tmax = 0.660 | Rint = 0.086 |
15709 measured reflections |
R[F2 > 2σ(F2)] = 0.033 | H atoms treated by a mixture of independent and constrained refinement |
wR(F2) = 0.078 | Δρmax = 1.13 e Å−3 |
S = 1.03 | Δρmin = −1.09 e Å−3 |
2690 reflections | Absolute structure: Flack H D (1983), Acta Cryst. A39, 876-881 |
151 parameters | Absolute structure parameter: −0.05 (5) |
21 restraints |
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, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Mn1 | 0.46947 (13) | 0.16430 (8) | 0.57996 (7) | 0.0135 (2) | |
I1 | 0.47616 (5) | −0.03518 (3) | 0.69319 (3) | 0.01778 (12) | |
O1 | 0.4834 (6) | 0.3317 (3) | 0.5121 (3) | 0.0158 (10) | |
O2 | 0.7527 (6) | 0.3675 (4) | 0.5025 (3) | 0.0164 (11) | |
C1 | 0.6035 (8) | 0.3912 (6) | 0.4892 (4) | 0.0095 (12) | |
C2 | 0.5693 (8) | 0.5042 (5) | 0.4401 (5) | 0.0147 (12) | |
H2 | 0.6258 | 0.5075 | 0.3754 | 0.018* | |
C3 | 0.6178 (9) | 0.6069 (6) | 0.5021 (5) | 0.0187 (13) | |
H3A | 0.6990 | 0.5854 | 0.5525 | 0.022* | |
H3B | 0.6658 | 0.6669 | 0.4608 | 0.022* | |
C4 | 0.4586 (9) | 0.6466 (6) | 0.5486 (5) | 0.0212 (14) | |
H4A | 0.4653 | 0.7271 | 0.5671 | 0.025* | |
H4B | 0.4318 | 0.6014 | 0.6070 | 0.025* | |
C5 | 0.3327 (9) | 0.6283 (6) | 0.4685 (6) | 0.0198 (14) | |
H5A | 0.2197 | 0.6242 | 0.4953 | 0.024* | |
H5B | 0.3378 | 0.6889 | 0.4191 | 0.024* | |
N1 | 0.3856 (7) | 0.5171 (5) | 0.4267 (4) | 0.0156 (11) | |
H1A | 0.348 (8) | 0.517 (7) | 0.363 (2) | 0.019* | |
H1B | 0.331 (8) | 0.465 (5) | 0.463 (4) | 0.019* | |
O3 | 0.6187 (6) | 0.1028 (4) | 0.4573 (4) | 0.0183 (11) | |
H6A | 0.572 (8) | 0.056 (5) | 0.420 (4) | 0.022* | |
H6B | 0.661 (9) | 0.148 (5) | 0.417 (4) | 0.022* | |
O4 | 0.6893 (7) | 0.2186 (5) | 0.6499 (4) | 0.0206 (12) | |
H7A | 0.733 (9) | 0.270 (5) | 0.618 (5) | 0.025* | |
H7B | 0.740 (8) | 0.198 (6) | 0.700 (3) | 0.025* | |
O5 | 0.2999 (6) | 0.2602 (4) | 0.6791 (4) | 0.0156 (10) | |
H8A | 0.317 (9) | 0.312 (4) | 0.720 (4) | 0.019* | |
H8B | 0.236 (7) | 0.226 (6) | 0.717 (4) | 0.019* | |
I2 | 1.01186 (5) | 0.61933 (3) | 0.69342 (3) | 0.01725 (12) |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0126 (5) | 0.0105 (5) | 0.0174 (5) | 0.0006 (4) | −0.0010 (4) | 0.0009 (4) |
I1 | 0.0179 (2) | 0.0130 (2) | 0.0224 (2) | 0.00079 (17) | −0.0012 (2) | 0.00490 (18) |
O1 | 0.014 (2) | 0.010 (2) | 0.024 (2) | 0.002 (2) | −0.002 (2) | 0.0058 (18) |
O2 | 0.013 (2) | 0.015 (3) | 0.022 (3) | 0.002 (2) | −0.001 (2) | −0.001 (2) |
C1 | 0.014 (3) | 0.007 (2) | 0.008 (3) | −0.001 (2) | 0.002 (2) | −0.004 (2) |
C2 | 0.015 (2) | 0.011 (2) | 0.018 (3) | 0.000 (2) | −0.002 (3) | 0.0017 (17) |
C3 | 0.021 (2) | 0.005 (2) | 0.029 (4) | 0.003 (2) | −0.006 (2) | 0.001 (3) |
C4 | 0.026 (3) | 0.010 (3) | 0.027 (4) | 0.004 (3) | −0.003 (2) | −0.002 (2) |
C5 | 0.021 (3) | 0.008 (3) | 0.031 (4) | 0.004 (2) | −0.003 (3) | 0.004 (3) |
N1 | 0.015 (2) | 0.012 (3) | 0.020 (3) | 0.0007 (19) | 0.001 (2) | 0.002 (2) |
O3 | 0.021 (3) | 0.012 (3) | 0.022 (3) | −0.005 (2) | 0.001 (2) | −0.003 (2) |
O4 | 0.021 (3) | 0.018 (3) | 0.022 (3) | −0.002 (2) | −0.005 (2) | 0.008 (2) |
O5 | 0.021 (3) | 0.009 (3) | 0.017 (3) | −0.002 (2) | 0.004 (2) | 0.001 (2) |
I2 | 0.0165 (2) | 0.0185 (2) | 0.0167 (2) | 0.00217 (18) | −0.0009 (2) | −0.00241 (18) |
Mn1—O2i | 2.127 (5) | C3—H3B | 0.9900 |
Mn1—O4 | 2.128 (6) | C4—C5 | 1.517 (10) |
Mn1—O1 | 2.197 (4) | C4—H4A | 0.9900 |
Mn1—O3 | 2.200 (5) | C4—H4B | 0.9900 |
Mn1—O5 | 2.246 (5) | C5—N1 | 1.502 (9) |
Mn1—I1 | 2.8323 (11) | C5—H5A | 0.9900 |
O1—C1 | 1.245 (7) | C5—H5B | 0.9900 |
O2—C1 | 1.258 (8) | N1—H1A | 0.92 (2) |
O2—Mn1ii | 2.127 (5) | N1—H1B | 0.91 (2) |
C1—C2 | 1.527 (9) | O3—H6A | 0.84 (2) |
C2—N1 | 1.512 (9) | O3—H6B | 0.84 (2) |
C2—C3 | 1.538 (9) | O4—H7A | 0.83 (2) |
C2—H2 | 1.0000 | O4—H7B | 0.84 (2) |
C3—C4 | 1.517 (10) | O5—H8A | 0.84 (2) |
C3—H3A | 0.9900 | O5—H8B | 0.84 (2) |
O2i—Mn1—O4 | 171.42 (19) | C2—C3—H3B | 110.7 |
O2i—Mn1—O1 | 88.70 (18) | H3A—C3—H3B | 108.8 |
O4—Mn1—O1 | 82.79 (18) | C3—C4—C5 | 103.1 (6) |
O2i—Mn1—O3 | 89.47 (19) | C3—C4—H4A | 111.2 |
O4—Mn1—O3 | 89.0 (2) | C5—C4—H4A | 111.2 |
O1—Mn1—O3 | 86.97 (18) | C3—C4—H4B | 111.2 |
O2i—Mn1—O5 | 84.48 (18) | C5—C4—H4B | 111.2 |
O4—Mn1—O5 | 95.1 (2) | H4A—C4—H4B | 109.1 |
O1—Mn1—O5 | 80.24 (17) | N1—C5—C4 | 102.1 (5) |
O3—Mn1—O5 | 165.95 (19) | N1—C5—H5A | 111.3 |
O2i—Mn1—I1 | 99.19 (13) | C4—C5—H5A | 111.3 |
O4—Mn1—I1 | 89.38 (14) | N1—C5—H5B | 111.3 |
O1—Mn1—I1 | 170.89 (12) | C4—C5—H5B | 111.3 |
O3—Mn1—I1 | 97.59 (14) | H5A—C5—H5B | 109.2 |
O5—Mn1—I1 | 95.90 (13) | C5—N1—C2 | 109.0 (6) |
C1—O1—Mn1 | 131.3 (4) | C5—N1—H1A | 105 (5) |
C1—O2—Mn1ii | 139.5 (4) | C2—N1—H1A | 116 (5) |
O1—C1—O2 | 126.3 (6) | C5—N1—H1B | 104 (5) |
O1—C1—C2 | 117.9 (6) | C2—N1—H1B | 110 (5) |
O2—C1—C2 | 115.8 (6) | H1A—N1—H1B | 111 (7) |
N1—C2—C1 | 108.8 (5) | Mn1—O3—H6A | 116 (5) |
N1—C2—C3 | 103.9 (6) | Mn1—O3—H6B | 121 (5) |
C1—C2—C3 | 113.9 (5) | H6A—O3—H6B | 102 (7) |
N1—C2—H2 | 110.0 | Mn1—O4—H7A | 110 (6) |
C1—C2—H2 | 110.0 | Mn1—O4—H7B | 134 (5) |
C3—C2—H2 | 110.0 | H7A—O4—H7B | 116 (8) |
C4—C3—C2 | 105.1 (6) | Mn1—O5—H8A | 132 (5) |
C4—C3—H3A | 110.7 | Mn1—O5—H8B | 120 (5) |
C2—C3—H3A | 110.7 | H8A—O5—H8B | 92 (7) |
C4—C3—H3B | 110.7 |
Symmetry codes: (i) x−1/2, −y+1/2, −z+1; (ii) x+1/2, −y+1/2, −z+1. |
C10H22Cl2MnN2O6 | F(000) = 406 |
Mr = 392.14 | Dx = 1.659 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 2761 reflections |
a = 9.124 (3) Å | θ = 2.3–26.4° |
b = 9.034 (3) Å | µ = 1.21 mm−1 |
c = 10.001 (3) Å | T = 100 K |
β = 107.704 (4)° | Block, colorless |
V = 785.2 (4) Å3 | 0.30 × 0.20 × 0.20 mm |
Z = 2 |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 1630 independent reflections |
Radiation source: microsource | 1445 reflections with I > 2σ(I) |
Multi layer optics monochromator | Rint = 0.045 |
ω scans | θmax = 26.5°, θmin = 2.3° |
Absorption correction: multi-scan SADABS | h = −11→11 |
Tmin = 0.713, Tmax = 0.794 | k = −11→11 |
8789 measured reflections | l = −12→12 |
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)] = 0.028 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.071 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | w = 1/[σ2(Fo2) + (0.037P)2 + 0.3P] where P = (Fo2 + 2Fc2)/3 |
1630 reflections | (Δ/σ)max = 0.001 |
139 parameters | Δρmax = 0.54 e Å−3 |
3 restraints | Δρmin = −0.22 e Å−3 |
C10H22Cl2MnN2O6 | V = 785.2 (4) Å3 |
Mr = 392.14 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 9.124 (3) Å | µ = 1.21 mm−1 |
b = 9.034 (3) Å | T = 100 K |
c = 10.001 (3) Å | 0.30 × 0.20 × 0.20 mm |
β = 107.704 (4)° |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 1630 independent reflections |
Absorption correction: multi-scan SADABS | 1445 reflections with I > 2σ(I) |
Tmin = 0.713, Tmax = 0.794 | Rint = 0.045 |
8789 measured reflections |
R[F2 > 2σ(F2)] = 0.028 | 3 restraints |
wR(F2) = 0.071 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.03 | Δρmax = 0.54 e Å−3 |
1630 reflections | Δρmin = −0.22 e Å−3 |
139 parameters |
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, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | Occ. (<1) | |
Mn1 | 0.0000 | 0.5000 | 0.5000 | 0.01557 (13) | |
Cl1 | 0.20028 (5) | 0.33207 (5) | 0.44130 (5) | 0.01996 (14) | |
O3 | 0.07612 (17) | 0.42942 (16) | 0.71773 (15) | 0.0219 (3) | |
H5A | 0.100 (3) | 0.352 (2) | 0.750 (3) | 0.034 (7)* | |
H5B | 0.103 (3) | 0.488 (3) | 0.776 (3) | 0.044 (9)* | |
O1 | 0.16308 (15) | 0.68153 (14) | 0.57041 (13) | 0.0200 (3) | |
O2 | 0.12745 (18) | 0.84199 (15) | 0.39323 (14) | 0.0288 (3) | |
C1 | 0.1641 (2) | 0.8090 (2) | 0.52060 (19) | 0.0175 (4) | |
C2 | 0.2192 (2) | 0.9373 (2) | 0.62190 (19) | 0.0196 (4) | |
H2 | 0.1368 | 1.0146 | 0.5991 | 0.024* | |
C3A | 0.3612 (13) | 1.0081 (13) | 0.6280 (14) | 0.0231 (19) | 0.510 (8) |
H3AA | 0.3682 | 1.1074 | 0.6715 | 0.028* | 0.510 (8) |
H3BA | 0.3728 | 1.0182 | 0.5332 | 0.028* | 0.510 (8) |
C4A | 0.4827 (4) | 0.9032 (6) | 0.7194 (5) | 0.0268 (14) | 0.510 (8) |
H4AA | 0.5782 | 0.9575 | 0.7684 | 0.032* | 0.510 (8) |
H4BA | 0.5076 | 0.8233 | 0.6621 | 0.032* | 0.510 (8) |
C5A | 0.4064 (17) | 0.8404 (12) | 0.8244 (14) | 0.0243 (19) | 0.510 (8) |
H5AA | 0.4129 | 0.7309 | 0.8277 | 0.029* | 0.510 (8) |
H5BA | 0.4559 | 0.8800 | 0.9198 | 0.029* | 0.510 (8) |
C3B | 0.3940 (13) | 0.9766 (13) | 0.6176 (15) | 0.0215 (19) | 0.490 (8) |
H3AB | 0.4370 | 0.8942 | 0.5760 | 0.026* | 0.490 (8) |
H3BB | 0.3944 | 1.0679 | 0.5629 | 0.026* | 0.490 (8) |
C4B | 0.4841 (5) | 0.9982 (6) | 0.7710 (5) | 0.0262 (14) | 0.490 (8) |
H4AB | 0.5954 | 0.9815 | 0.7871 | 0.031* | 0.490 (8) |
H4BB | 0.4688 | 1.0992 | 0.8029 | 0.031* | 0.490 (8) |
C5B | 0.4183 (18) | 0.8840 (12) | 0.8449 (15) | 0.025 (2) | 0.490 (8) |
H5AB | 0.4415 | 0.9084 | 0.9457 | 0.030* | 0.490 (8) |
H5BB | 0.4603 | 0.7847 | 0.8359 | 0.030* | 0.490 (8) |
N1 | 0.24476 (19) | 0.88961 (19) | 0.77046 (16) | 0.0189 (3) | |
H1A | 0.219 (2) | 0.965 (2) | 0.818 (2) | 0.023* | |
H1B | 0.185 (2) | 0.812 (2) | 0.773 (2) | 0.023* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0189 (2) | 0.0116 (2) | 0.0147 (2) | −0.00210 (15) | 0.00279 (16) | −0.00012 (15) |
Cl1 | 0.0235 (3) | 0.0145 (2) | 0.0197 (2) | 0.00172 (17) | 0.00328 (18) | −0.00027 (17) |
O3 | 0.0335 (8) | 0.0120 (7) | 0.0165 (7) | 0.0004 (6) | 0.0020 (6) | 0.0001 (6) |
O1 | 0.0239 (7) | 0.0131 (7) | 0.0201 (7) | −0.0044 (5) | 0.0025 (5) | 0.0012 (5) |
O2 | 0.0500 (10) | 0.0160 (7) | 0.0180 (7) | −0.0009 (7) | 0.0070 (7) | 0.0008 (6) |
C1 | 0.0181 (9) | 0.0146 (9) | 0.0194 (9) | −0.0005 (7) | 0.0050 (7) | −0.0010 (7) |
C2 | 0.0242 (10) | 0.0135 (9) | 0.0180 (9) | 0.0015 (8) | 0.0017 (8) | 0.0008 (7) |
C3A | 0.021 (5) | 0.022 (4) | 0.025 (3) | −0.002 (3) | 0.007 (3) | 0.004 (3) |
C4A | 0.014 (2) | 0.031 (3) | 0.032 (3) | −0.0008 (17) | 0.0020 (17) | 0.002 (2) |
C5A | 0.022 (4) | 0.026 (5) | 0.022 (4) | −0.001 (4) | 0.002 (3) | 0.003 (4) |
C3B | 0.015 (5) | 0.023 (5) | 0.027 (3) | −0.009 (3) | 0.008 (3) | −0.002 (3) |
C4B | 0.020 (2) | 0.028 (3) | 0.026 (2) | −0.0072 (18) | 0.0017 (17) | 0.000 (2) |
C5B | 0.016 (3) | 0.029 (6) | 0.022 (4) | −0.003 (4) | −0.006 (3) | 0.002 (4) |
N1 | 0.0217 (8) | 0.0173 (8) | 0.0169 (8) | 0.0006 (7) | 0.0048 (7) | −0.0024 (7) |
Mn1—O3i | 2.1704 (15) | C4A—C5A | 1.535 (15) |
Mn1—O3 | 2.1704 (15) | C4A—H4AA | 0.9900 |
Mn1—O1 | 2.1820 (13) | C4A—H4BA | 0.9900 |
Mn1—O1i | 2.1820 (13) | C5A—N1 | 1.476 (15) |
Mn1—Cl1i | 2.5763 (7) | C5A—H5AA | 0.9900 |
Mn1—Cl1 | 2.5763 (7) | C5A—H5BA | 0.9900 |
O3—H5A | 0.774 (19) | C3B—C4B | 1.516 (15) |
O3—H5B | 0.77 (2) | C3B—H3AB | 0.9900 |
O1—C1 | 1.256 (2) | C3B—H3BB | 0.9900 |
O2—C1 | 1.251 (2) | C4B—C5B | 1.496 (15) |
C1—C2 | 1.521 (3) | C4B—H4AB | 0.9900 |
C2—C3A | 1.429 (13) | C4B—H4BB | 0.9900 |
C2—N1 | 1.496 (2) | C5B—N1 | 1.532 (15) |
C2—C3B | 1.647 (12) | C5B—H5AB | 0.9900 |
C2—H2 | 1.0000 | C5B—H5BB | 0.9900 |
C3A—C4A | 1.532 (13) | N1—H1A | 0.903 (16) |
C3A—H3AA | 0.9900 | N1—H1B | 0.890 (16) |
C3A—H3BA | 0.9900 | ||
O3i—Mn1—O3 | 180.0 | C3A—C4A—H4AA | 111.0 |
O3i—Mn1—O1 | 94.69 (5) | C5A—C4A—H4AA | 111.0 |
O3—Mn1—O1 | 85.31 (5) | C3A—C4A—H4BA | 111.0 |
O3i—Mn1—O1i | 85.30 (5) | C5A—C4A—H4BA | 111.0 |
O3—Mn1—O1i | 94.69 (5) | H4AA—C4A—H4BA | 109.0 |
O1—Mn1—O1i | 180.0 | N1—C5A—C4A | 104.4 (9) |
O3i—Mn1—Cl1i | 91.31 (4) | N1—C5A—H5AA | 110.9 |
O3—Mn1—Cl1i | 88.69 (4) | C4A—C5A—H5AA | 110.9 |
O1—Mn1—Cl1i | 86.87 (4) | N1—C5A—H5BA | 110.9 |
O1i—Mn1—Cl1i | 93.13 (4) | C4A—C5A—H5BA | 110.9 |
O3i—Mn1—Cl1 | 88.69 (4) | H5AA—C5A—H5BA | 108.9 |
O3—Mn1—Cl1 | 91.31 (4) | C4B—C3B—C2 | 103.4 (7) |
O1—Mn1—Cl1 | 93.13 (4) | C4B—C3B—H3AB | 111.1 |
O1i—Mn1—Cl1 | 86.87 (4) | C2—C3B—H3AB | 111.1 |
Cl1i—Mn1—Cl1 | 179.9990 (10) | C4B—C3B—H3BB | 111.1 |
Mn1—O3—H5A | 130.8 (19) | C2—C3B—H3BB | 111.1 |
Mn1—O3—H5B | 120 (2) | H3AB—C3B—H3BB | 109.0 |
H5A—O3—H5B | 108 (3) | C5B—C4B—C3B | 103.6 (7) |
C1—O1—Mn1 | 130.38 (12) | C5B—C4B—H4AB | 111.0 |
O2—C1—O1 | 126.18 (17) | C3B—C4B—H4AB | 111.0 |
O2—C1—C2 | 115.41 (16) | C5B—C4B—H4BB | 111.0 |
O1—C1—C2 | 118.39 (16) | C3B—C4B—H4BB | 111.0 |
C3A—C2—N1 | 102.8 (6) | H4AB—C4B—H4BB | 109.0 |
C3A—C2—C1 | 118.7 (4) | C4B—C5B—N1 | 104.4 (9) |
N1—C2—C1 | 111.24 (15) | C4B—C5B—H5AB | 110.9 |
C3A—C2—C3B | 14.6 (6) | N1—C5B—H5AB | 110.9 |
N1—C2—C3B | 103.2 (5) | C4B—C5B—H5BB | 110.9 |
C1—C2—C3B | 105.8 (4) | N1—C5B—H5BB | 110.9 |
C3A—C2—H2 | 107.9 | H5AB—C5B—H5BB | 108.9 |
N1—C2—H2 | 107.9 | C5A—N1—C2 | 106.7 (6) |
C1—C2—H2 | 107.9 | C5A—N1—C5B | 16.8 (5) |
C3B—C2—H2 | 120.7 | C2—N1—C5B | 108.5 (6) |
C2—C3A—C4A | 103.4 (8) | C5A—N1—H1A | 115.4 (15) |
C2—C3A—H3AA | 111.1 | C2—N1—H1A | 108.6 (14) |
C4A—C3A—H3AA | 111.1 | C5B—N1—H1A | 99.7 (15) |
C2—C3A—H3BA | 111.1 | C5A—N1—H1B | 107.6 (15) |
C4A—C3A—H3BA | 111.1 | C2—N1—H1B | 109.9 (14) |
H3AA—C3A—H3BA | 109.1 | C5B—N1—H1B | 120.6 (15) |
C3A—C4A—C5A | 103.9 (8) | H1A—N1—H1B | 109 (2) |
Symmetry code: (i) −x, −y+1, −z+1. |
C10H22Br2MnN2O6 | F(000) = 478 |
Mr = 481.06 | Dx = 1.951 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 1326 reflections |
a = 9.3156 (12) Å | θ = 3.1–22.4° |
b = 9.1319 (12) Å | µ = 5.71 mm−1 |
c = 10.0593 (13) Å | T = 100 K |
β = 106.904 (2)° | Block, colorless |
V = 818.76 (18) Å3 | 0.14 × 0.08 × 0.04 mm |
Z = 2 |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 2421 independent reflections |
Radiation source: microsource | 1997 reflections with I > 2σ(I) |
Multi layer optics monochromator | Rint = 0.066 |
ω scans | θmax = 30.9°, θmin = 3.1° |
Absorption correction: multi-scan SADABS | h = −13→13 |
Tmin = 0.502, Tmax = 0.804 | k = −12→12 |
12113 measured reflections | l = −13→13 |
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)] = 0.046 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.088 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | w = 1/[σ2(Fo2) + (0.020P)2 + 3.P] where P = (Fo2 + 2Fc2)/3 |
2421 reflections | (Δ/σ)max < 0.001 |
111 parameters | Δρmax = 0.90 e Å−3 |
3 restraints | Δρmin = −0.66 e Å−3 |
C10H22Br2MnN2O6 | V = 818.76 (18) Å3 |
Mr = 481.06 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 9.3156 (12) Å | µ = 5.71 mm−1 |
b = 9.1319 (12) Å | T = 100 K |
c = 10.0593 (13) Å | 0.14 × 0.08 × 0.04 mm |
β = 106.904 (2)° |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 2421 independent reflections |
Absorption correction: multi-scan SADABS | 1997 reflections with I > 2σ(I) |
Tmin = 0.502, Tmax = 0.804 | Rint = 0.066 |
12113 measured reflections |
R[F2 > 2σ(F2)] = 0.046 | 3 restraints |
wR(F2) = 0.088 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.05 | Δρmax = 0.90 e Å−3 |
2421 reflections | Δρmin = −0.66 e Å−3 |
111 parameters |
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, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Mn1 | 0.0000 | 0.5000 | 0.5000 | 0.01456 (17) | |
Br1 | 0.21256 (4) | 0.31959 (4) | 0.44867 (4) | 0.01881 (11) | |
O3 | 0.0633 (4) | 0.4400 (3) | 0.7173 (3) | 0.0217 (6) | |
H1O | 0.103 (5) | 0.371 (5) | 0.757 (5) | 0.031 (14)* | |
H2O | 0.090 (7) | 0.502 (6) | 0.771 (6) | 0.07 (2)* | |
O1 | 0.1559 (3) | 0.6797 (3) | 0.5675 (3) | 0.0198 (6) | |
O2 | 0.1237 (4) | 0.8344 (3) | 0.3892 (3) | 0.0260 (7) | |
C1 | 0.1613 (4) | 0.8040 (4) | 0.5158 (4) | 0.0155 (7) | |
C2 | 0.2273 (4) | 0.9295 (4) | 0.6141 (4) | 0.0167 (7) | |
H2 | 0.1630 | 1.0186 | 0.5873 | 0.020* | |
C3 | 0.3882 (5) | 0.9634 (5) | 0.6109 (4) | 0.0251 (9) | |
H3A | 0.4298 | 0.8807 | 0.5702 | 0.030* | |
H3B | 0.3903 | 1.0528 | 0.5558 | 0.030* | |
C4 | 0.4764 (5) | 0.9861 (6) | 0.7621 (5) | 0.0334 (11) | |
H4A | 0.5846 | 0.9666 | 0.7778 | 0.040* | |
H4B | 0.4635 | 1.0869 | 0.7933 | 0.040* | |
C5 | 0.4064 (5) | 0.8742 (5) | 0.8356 (4) | 0.0277 (9) | |
H5A | 0.4422 | 0.7740 | 0.8248 | 0.033* | |
H5B | 0.4284 | 0.8969 | 0.9357 | 0.033* | |
N1 | 0.2429 (4) | 0.8901 (4) | 0.7621 (3) | 0.0179 (7) | |
H1A | 0.212 (5) | 0.970 (3) | 0.802 (4) | 0.022* | |
H1B | 0.188 (4) | 0.810 (3) | 0.770 (5) | 0.022* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0198 (4) | 0.0120 (4) | 0.0110 (4) | −0.0033 (3) | 0.0032 (3) | 0.0000 (3) |
Br1 | 0.0230 (2) | 0.01310 (17) | 0.01790 (18) | 0.00011 (15) | 0.00207 (14) | −0.00006 (15) |
O3 | 0.0352 (18) | 0.0120 (13) | 0.0140 (14) | 0.0007 (12) | 0.0010 (12) | 0.0013 (11) |
O1 | 0.0215 (14) | 0.0137 (12) | 0.0210 (13) | −0.0028 (11) | 0.0013 (11) | 0.0030 (11) |
O2 | 0.0458 (19) | 0.0175 (14) | 0.0130 (13) | 0.0022 (13) | 0.0061 (12) | 0.0017 (11) |
C1 | 0.0178 (18) | 0.0142 (17) | 0.0162 (17) | 0.0014 (14) | 0.0075 (14) | −0.0012 (13) |
C2 | 0.0192 (19) | 0.0165 (17) | 0.0142 (17) | −0.0008 (14) | 0.0047 (14) | 0.0002 (14) |
C3 | 0.025 (2) | 0.030 (2) | 0.022 (2) | −0.0077 (18) | 0.0110 (17) | 0.0015 (17) |
C4 | 0.024 (2) | 0.039 (3) | 0.036 (3) | −0.008 (2) | 0.0065 (19) | 0.004 (2) |
C5 | 0.025 (2) | 0.035 (2) | 0.021 (2) | −0.0010 (19) | 0.0021 (17) | 0.0088 (18) |
N1 | 0.0236 (18) | 0.0176 (16) | 0.0142 (15) | −0.0018 (13) | 0.0079 (13) | −0.0006 (12) |
Mn1—O3 | 2.162 (3) | C2—H2 | 1.0000 |
Mn1—O3i | 2.162 (3) | C3—C4 | 1.519 (6) |
Mn1—O1i | 2.166 (3) | C3—H3A | 0.9900 |
Mn1—O1 | 2.166 (3) | C3—H3B | 0.9900 |
Mn1—Br1i | 2.7379 (5) | C4—C5 | 1.516 (6) |
Mn1—Br1 | 2.7379 (5) | C4—H4A | 0.9900 |
O3—H1O | 0.78 (4) | C4—H4B | 0.9900 |
O3—H2O | 0.77 (4) | C5—N1 | 1.494 (5) |
O1—C1 | 1.255 (4) | C5—H5A | 0.9900 |
O2—C1 | 1.249 (4) | C5—H5B | 0.9900 |
C1—C2 | 1.522 (5) | N1—H1A | 0.922 (19) |
C2—N1 | 1.498 (5) | N1—H1B | 0.913 (19) |
C2—C3 | 1.540 (5) | ||
O3—Mn1—O3i | 180.0 | C1—C2—H2 | 109.9 |
O3—Mn1—O1i | 94.90 (11) | C3—C2—H2 | 109.9 |
O3i—Mn1—O1i | 85.10 (11) | C4—C3—C2 | 104.6 (3) |
O3—Mn1—O1 | 85.09 (11) | C4—C3—H3A | 110.8 |
O3i—Mn1—O1 | 94.90 (11) | C2—C3—H3A | 110.8 |
O1i—Mn1—O1 | 180.0 | C4—C3—H3B | 110.8 |
O3—Mn1—Br1i | 87.79 (8) | C2—C3—H3B | 110.8 |
O3i—Mn1—Br1i | 92.21 (8) | H3A—C3—H3B | 108.9 |
O1i—Mn1—Br1i | 93.40 (8) | C5—C4—C3 | 102.2 (4) |
O1—Mn1—Br1i | 86.60 (8) | C5—C4—H4A | 111.3 |
O3—Mn1—Br1 | 92.21 (8) | C3—C4—H4A | 111.3 |
O3i—Mn1—Br1 | 87.79 (8) | C5—C4—H4B | 111.3 |
O1i—Mn1—Br1 | 86.60 (8) | C3—C4—H4B | 111.3 |
O1—Mn1—Br1 | 93.40 (8) | H4A—C4—H4B | 109.2 |
Br1i—Mn1—Br1 | 180.0 | N1—C5—C4 | 102.4 (3) |
Mn1—O3—H1O | 132 (4) | N1—C5—H5A | 111.3 |
Mn1—O3—H2O | 117 (5) | C4—C5—H5A | 111.3 |
H1O—O3—H2O | 103 (6) | N1—C5—H5B | 111.3 |
C1—O1—Mn1 | 131.2 (2) | C4—C5—H5B | 111.3 |
O2—C1—O1 | 126.2 (3) | H5A—C5—H5B | 109.2 |
O2—C1—C2 | 115.8 (3) | C5—N1—C2 | 107.8 (3) |
O1—C1—C2 | 117.9 (3) | C5—N1—H1A | 106 (3) |
N1—C2—C1 | 111.7 (3) | C2—N1—H1A | 107 (3) |
N1—C2—C3 | 104.8 (3) | C5—N1—H1B | 114 (3) |
C1—C2—C3 | 110.5 (3) | C2—N1—H1B | 113 (3) |
N1—C2—H2 | 109.9 | H1A—N1—H1B | 110 (4) |
Symmetry code: (i) −x, −y+1, −z+1. |
C10H22I2MnN2O6 | F(000) = 550 |
Mr = 575.04 | Dx = 2.165 Mg m−3 |
Monoclinic, P21/c | Mo Kα radiation, λ = 0.71073 Å |
Hall symbol: -P 2ybc | Cell parameters from 1525 reflections |
a = 9.664 (1) Å | θ = 3.0–24.4° |
b = 9.4026 (10) Å | µ = 4.27 mm−1 |
c = 10.0228 (11) Å | T = 100 K |
β = 104.454 (2)° | Block, yellow |
V = 881.91 (16) Å3 | 0.09 × 0.09 × 0.09 mm |
Z = 2 |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 2622 independent reflections |
Radiation source: microsource | 2151 reflections with I > 2σ(I) |
Multi layer optics monochromator | Rint = 0.064 |
ω scans | θmax = 30.6°, θmin = 3.0° |
Absorption correction: multi-scan SADABS | h = −13→13 |
Tmin = 0.700, Tmax = 0.700 | k = −13→12 |
13020 measured reflections | l = −14→14 |
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)] = 0.031 | Hydrogen site location: inferred from neighbouring sites |
wR(F2) = 0.061 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | w = 1/[σ2(Fo2) + (0.020P)2] where P = (Fo2 + 2Fc2)/3 |
2622 reflections | (Δ/σ)max = 0.001 |
111 parameters | Δρmax = 0.88 e Å−3 |
3 restraints | Δρmin = −0.68 e Å−3 |
C10H22I2MnN2O6 | V = 881.91 (16) Å3 |
Mr = 575.04 | Z = 2 |
Monoclinic, P21/c | Mo Kα radiation |
a = 9.664 (1) Å | µ = 4.27 mm−1 |
b = 9.4026 (10) Å | T = 100 K |
c = 10.0228 (11) Å | 0.09 × 0.09 × 0.09 mm |
β = 104.454 (2)° |
Bruker D8 goniometer with SMART APEX CCD detector diffractometer | 2622 independent reflections |
Absorption correction: multi-scan SADABS | 2151 reflections with I > 2σ(I) |
Tmin = 0.700, Tmax = 0.700 | Rint = 0.064 |
13020 measured reflections |
R[F2 > 2σ(F2)] = 0.031 | 3 restraints |
wR(F2) = 0.061 | H atoms treated by a mixture of independent and constrained refinement |
S = 1.01 | Δρmax = 0.88 e Å−3 |
2622 reflections | Δρmin = −0.68 e Å−3 |
111 parameters |
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, conventional R-factors R are based on F, with F set to zero for negative F2. The threshold expression of F2 > σ(F2) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F2 are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. |
x | y | z | Uiso*/Ueq | ||
Mn1 | 0.0000 | 0.5000 | 0.5000 | 0.01263 (15) | |
I1 | 0.23227 (2) | 0.31229 (2) | 0.45619 (2) | 0.01552 (7) | |
O3 | 0.0472 (3) | 0.4497 (3) | 0.7170 (2) | 0.0155 (5) | |
H1O | 0.083 (4) | 0.379 (4) | 0.751 (4) | 0.035 (13)* | |
H2O | 0.077 (5) | 0.509 (4) | 0.771 (4) | 0.039 (14)* | |
O1 | 0.1415 (2) | 0.6779 (2) | 0.5618 (2) | 0.0164 (5) | |
O2 | 0.1140 (3) | 0.8249 (2) | 0.3812 (2) | 0.0199 (5) | |
C1 | 0.1515 (3) | 0.7969 (3) | 0.5069 (3) | 0.0147 (6) | |
C2 | 0.2231 (3) | 0.9162 (3) | 0.5998 (3) | 0.0143 (6) | |
H2 | 0.1668 | 1.0058 | 0.5749 | 0.017* | |
C3 | 0.3765 (3) | 0.9394 (4) | 0.5866 (3) | 0.0184 (7) | |
H3A | 0.4121 | 0.8540 | 0.5479 | 0.022* | |
H3B | 0.3812 | 1.0218 | 0.5264 | 0.022* | |
C4 | 0.4636 (4) | 0.9672 (4) | 0.7331 (4) | 0.0235 (8) | |
H4A | 0.4557 | 1.0677 | 0.7597 | 0.028* | |
H4B | 0.5656 | 0.9433 | 0.7439 | 0.028* | |
C5 | 0.3942 (3) | 0.8676 (4) | 0.8174 (4) | 0.0200 (7) | |
H5A | 0.4264 | 0.7683 | 0.8119 | 0.024* | |
H5B | 0.4160 | 0.8972 | 0.9152 | 0.024* | |
N1 | 0.2390 (3) | 0.8832 (3) | 0.7499 (3) | 0.0149 (6) | |
H1A | 0.206 (3) | 0.958 (3) | 0.792 (3) | 0.018* | |
H1B | 0.188 (3) | 0.802 (3) | 0.752 (4) | 0.018* |
U11 | U22 | U33 | U12 | U13 | U23 | |
Mn1 | 0.0170 (4) | 0.0111 (3) | 0.0093 (3) | −0.0029 (3) | 0.0022 (3) | −0.0002 (3) |
I1 | 0.01752 (11) | 0.01175 (11) | 0.01572 (11) | 0.00074 (8) | 0.00119 (8) | 0.00082 (8) |
O3 | 0.0216 (13) | 0.0121 (12) | 0.0106 (12) | 0.0010 (10) | −0.0002 (10) | −0.0002 (10) |
O1 | 0.0206 (12) | 0.0101 (11) | 0.0170 (12) | −0.0027 (9) | 0.0019 (10) | 0.0024 (9) |
O2 | 0.0308 (14) | 0.0162 (12) | 0.0117 (11) | 0.0026 (10) | 0.0035 (10) | 0.0017 (9) |
C1 | 0.0149 (16) | 0.0147 (16) | 0.0164 (16) | −0.0007 (13) | 0.0075 (13) | −0.0015 (13) |
C2 | 0.0153 (16) | 0.0133 (16) | 0.0143 (15) | 0.0014 (12) | 0.0040 (13) | 0.0009 (12) |
C3 | 0.0198 (17) | 0.0176 (17) | 0.0197 (17) | −0.0003 (14) | 0.0082 (14) | 0.0006 (14) |
C4 | 0.0186 (18) | 0.029 (2) | 0.0222 (19) | −0.0049 (15) | 0.0039 (15) | 0.0006 (15) |
C5 | 0.0165 (17) | 0.0252 (18) | 0.0172 (16) | 0.0011 (14) | 0.0023 (13) | 0.0016 (15) |
N1 | 0.0160 (14) | 0.0153 (14) | 0.0146 (13) | −0.0010 (11) | 0.0059 (11) | −0.0025 (11) |
Mn1—O1i | 2.151 (2) | C2—H2 | 1.0000 |
Mn1—O1 | 2.151 (2) | C3—C4 | 1.521 (5) |
Mn1—O3i | 2.160 (2) | C3—H3A | 0.9900 |
Mn1—O3 | 2.160 (2) | C3—H3B | 0.9900 |
Mn1—I1i | 2.9729 (3) | C4—C5 | 1.524 (5) |
Mn1—I1 | 2.9730 (3) | C4—H4A | 0.9900 |
O3—H1O | 0.79 (3) | C4—H4B | 0.9900 |
O3—H2O | 0.78 (3) | C5—N1 | 1.491 (4) |
O1—C1 | 1.261 (3) | C5—H5A | 0.9900 |
O2—C1 | 1.249 (4) | C5—H5B | 0.9900 |
C1—C2 | 1.511 (4) | N1—H1A | 0.921 (18) |
C2—N1 | 1.507 (4) | N1—H1B | 0.910 (18) |
C2—C3 | 1.536 (4) | ||
O1i—Mn1—O1 | 180.00 (10) | C1—C2—H2 | 109.6 |
O1i—Mn1—O3i | 85.49 (9) | C3—C2—H2 | 109.6 |
O1—Mn1—O3i | 94.51 (9) | C4—C3—C2 | 104.8 (3) |
O1i—Mn1—O3 | 94.51 (9) | C4—C3—H3A | 110.8 |
O1—Mn1—O3 | 85.50 (9) | C2—C3—H3A | 110.8 |
O3i—Mn1—O3 | 180.00 (13) | C4—C3—H3B | 110.8 |
O1i—Mn1—I1i | 93.15 (6) | C2—C3—H3B | 110.8 |
O1—Mn1—I1i | 86.85 (6) | H3A—C3—H3B | 108.9 |
O3i—Mn1—I1i | 92.36 (7) | C3—C4—C5 | 102.4 (3) |
O3—Mn1—I1i | 87.64 (7) | C3—C4—H4A | 111.3 |
O1i—Mn1—I1 | 86.85 (6) | C5—C4—H4A | 111.3 |
O1—Mn1—I1 | 93.15 (6) | C3—C4—H4B | 111.3 |
O3i—Mn1—I1 | 87.64 (7) | C5—C4—H4B | 111.3 |
O3—Mn1—I1 | 92.36 (7) | H4A—C4—H4B | 109.2 |
I1i—Mn1—I1 | 180.0 | N1—C5—C4 | 102.7 (3) |
Mn1—O3—H1O | 126 (3) | N1—C5—H5A | 111.2 |
Mn1—O3—H2O | 120 (3) | C4—C5—H5A | 111.2 |
H1O—O3—H2O | 104 (4) | N1—C5—H5B | 111.2 |
C1—O1—Mn1 | 132.6 (2) | C4—C5—H5B | 111.2 |
O2—C1—O1 | 126.3 (3) | H5A—C5—H5B | 109.1 |
O2—C1—C2 | 116.0 (3) | C5—N1—C2 | 108.3 (2) |
O1—C1—C2 | 117.6 (3) | C5—N1—H1A | 107 (2) |
N1—C2—C1 | 112.3 (3) | C2—N1—H1A | 110 (2) |
N1—C2—C3 | 104.8 (2) | C5—N1—H1B | 113 (2) |
C1—C2—C3 | 110.8 (3) | C2—N1—H1B | 106 (2) |
N1—C2—H2 | 109.6 | H1A—N1—H1B | 113 (3) |
Symmetry code: (i) −x, −y+1, −z+1. |
Experimental details
(1a) | (1b) | (1c) | (2a) | |
Crystal data | ||||
Chemical formula | C5H9Cl2MnNO2·H2O | C7H17Br2MnNO4 | C5H15IMnNO5·I | C10H22Cl2MnN2O6 |
Mr | 258.99 | 393.98 | 477.92 | 392.14 |
Crystal system, space group | Orthorhombic, P212121 | Monoclinic, P21 | Orthorhombic, P212121 | Monoclinic, P21/c |
Temperature (K) | 100 | 100 | 100 | 100 |
a, b, c (Å) | 7.0862 (6), 10.0235 (8), 13.2437 (11) | 8.286 (2), 8.256 (2), 9.387 (3) | 8.1264 (18), 11.867 (3), 13.727 (3) | 9.124 (3), 9.034 (3), 10.001 (3) |
α, β, γ (°) | 90, 90, 90 | 90, 92.172 (4), 90 | 90, 90, 90 | 90, 107.704 (4), 90 |
V (Å3) | 940.68 (13) | 641.7 (3) | 1323.8 (5) | 785.2 (4) |
Z | 4 | 2 | 4 | 2 |
Radiation type | Mo Kα | Mo Kα | Mo Kα | Mo Kα |
µ (mm−1) | 1.94 | 7.25 | 5.66 | 1.21 |
Crystal size (mm) | 0.14 × 0.06 × 0.05 | 0.27 × 0.08 × 0.08 | 0.14 × 0.08 × 0.08 | 0.30 × 0.20 × 0.20 |
Data collection | ||||
Diffractometer | Bruker D8 goniometer with SMART APEX CCD detector diffractometer | Bruker D8 goniometer with SMART APEX CCD detector diffractometer | Bruker D8 goniometer with SMART APEX CCD detector diffractometer | Bruker D8 goniometer with SMART APEX CCD detector diffractometer |
Absorption correction | Multi-scan SADABS | Multi-scan SADABS | Multi-scan SADABS | Multi-scan SADABS |
Tmin, Tmax | 0.773, 0.909 | 0.245, 0.595 | 0.505, 0.660 | 0.713, 0.794 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 11373, 2039, 1797 | 7642, 2665, 2440 | 15709, 2690, 2412 | 8789, 1630, 1445 |
Rint | 0.058 | 0.061 | 0.086 | 0.045 |
(sin θ/λ)max (Å−1) | 0.641 | 0.628 | 0.625 | 0.628 |
Refinement | ||||
R[F2 > 2σ(F2)], wR(F2), S | 0.032, 0.074, 1.06 | 0.035, 0.064, 1.00 | 0.033, 0.078, 1.03 | 0.028, 0.071, 1.03 |
No. of reflections | 2039 | 2665 | 2690 | 1630 |
No. of parameters | 121 | 152 | 151 | 139 |
No. of restraints | 4 | 4 | 21 | 3 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.52, −0.33 | 0.61, −0.48 | 1.13, −1.09 | 0.54, −0.22 |
Absolute structure | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 | Flack H D (1983), Acta Cryst. A39, 876-881 | ? |
Absolute structure parameter | −0.02 (4) | 0.015 (12) | −0.05 (5) | ? |
(2b) | (2c) | |
Crystal data | ||
Chemical formula | C10H22Br2MnN2O6 | C10H22I2MnN2O6 |
Mr | 481.06 | 575.04 |
Crystal system, space group | Monoclinic, P21/c | Monoclinic, P21/c |
Temperature (K) | 100 | 100 |
a, b, c (Å) | 9.3156 (12), 9.1319 (12), 10.0593 (13) | 9.664 (1), 9.4026 (10), 10.0228 (11) |
α, β, γ (°) | 90, 106.904 (2), 90 | 90, 104.454 (2), 90 |
V (Å3) | 818.76 (18) | 881.91 (16) |
Z | 2 | 2 |
Radiation type | Mo Kα | Mo Kα |
µ (mm−1) | 5.71 | 4.27 |
Crystal size (mm) | 0.14 × 0.08 × 0.04 | 0.09 × 0.09 × 0.09 |
Data collection | ||
Diffractometer | Bruker D8 goniometer with SMART APEX CCD detector diffractometer | Bruker D8 goniometer with SMART APEX CCD detector diffractometer |
Absorption correction | Multi-scan SADABS | Multi-scan SADABS |
Tmin, Tmax | 0.502, 0.804 | 0.700, 0.700 |
No. of measured, independent and observed [I > 2σ(I)] reflections | 12113, 2421, 1997 | 13020, 2622, 2151 |
Rint | 0.066 | 0.064 |
(sin θ/λ)max (Å−1) | 0.723 | 0.715 |
Refinement | ||
R[F2 > 2σ(F2)], wR(F2), S | 0.046, 0.088, 1.05 | 0.031, 0.061, 1.01 |
No. of reflections | 2421 | 2622 |
No. of parameters | 111 | 111 |
No. of restraints | 3 | 3 |
H-atom treatment | H atoms treated by a mixture of independent and constrained refinement | H atoms treated by a mixture of independent and constrained refinement |
Δρmax, Δρmin (e Å−3) | 0.90, −0.66 | 0.88, −0.68 |
Absolute structure | ? | ? |
Absolute structure parameter | ? | ? |
Computer programs: SHELXS97 (Sheldrick, 1990), SHELXL97 (Sheldrick, 1997).
Subscribe to Acta Crystallographica Section B: Structural Science, Crystal Engineering and Materials
The full text of this article is available to subscribers to the journal.
- Information on subscribing
- Sample issue
- Purchase subscription
- Reduced-price subscriptions
- If you have already subscribed, you may need to register