Identification code | mo_B0383_0m |
Empirical formula | C21H44Br2N2O5Zn3 |
Formula weight | 760.51 |
Temperature/K | 99.99 |
Crystal system | monoclinic |
Space group | P21/n |
a/Å | 12.1460(7) |
b/Å | 21.0763(13) |
c/Å | 12.5832(7) |
α/° | 90 |
β/° | 115.275(2) |
γ/° | 90 |
Volume/Å3 | 2912.8(3) |
Z | 4 |
ρcalcg/cm3 | 1.734 |
μ/mm‑1 | 5.225 |
F(000) | 1536.0 |
Crystal size/mm3 | 0.22 × 0.17 × 0.13 |
Radiation | MoKα (λ = 0.71073) |
2Θ range for data collection/° | 4.182 to 53.998 |
Index ranges | -15 ≤ h ≤ 15, -26 ≤ k ≤ 26, -16 ≤ l ≤ 16 |
Reflections collected | 60917 |
Independent reflections | 6355 [Rint = 0.0406, Rsigma = 0.0191] |
Data/restraints/parameters | 6355/0/323 |
Goodness-of-fit on F2 | 1.274 |
Final R indexes [I>=2σ (I)] | R1 = 0.0176, wR2 = 0.0522 |
Final R indexes [all data] | R1 = 0.0219, wR2 = 0.0702 |
Largest diff. peak/hole / e Å-3 | 0.92/-0.98 |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
Br1 | 7956.6(2) | 6100.2(2) | 5900.6(2) | 21.64(7) |
Br2 | 8056.6(2) | 3402.4(2) | 5399.7(2) | 21.98(7) |
Zn2 | 4521.0(2) | 4965.8(2) | 3274.4(2) | 11.88(7) |
Zn3 | 6134.5(2) | 3807.0(2) | 5136.1(2) | 11.85(6) |
Zn1 | 6215.9(2) | 6311.1(2) | 4111.6(2) | 13.33(7) |
O3 | 3716.0(14) | 5356.0(7) | 4123.0(13) | 16.2(3) |
O1 | 4866.7(13) | 6713.7(7) | 4321.5(13) | 15.8(3) |
O4 | 5035.5(13) | 4086.4(7) | 3558.7(12) | 13.1(3) |
O2 | 5687.7(14) | 5557.8(7) | 3175.6(14) | 17.7(3) |
N1 | 6357.3(16) | 7134.6(8) | 3232.4(16) | 16.0(3) |
O5 | 7621.0(17) | 5227.4(10) | 2500.6(19) | 37.2(4) |
N2 | 3270.1(15) | 4673.5(9) | 1554.4(14) | 15.1(3) |
C5 | 7642(2) | 7367.5(11) | 3705(2) | 21.8(5) |
C4 | 5644(2) | 7580.3(10) | 3613(2) | 19.4(4) |
C10 | 4656.8(18) | 3727(1) | 2503.1(18) | 14.5(4) |
C1 | 4507.5(19) | 7298.9(10) | 3689(2) | 18.2(4) |
C6 | 8421(2) | 6946.1(12) | 3323(2) | 25.9(5) |
C2 | 3426(2) | 7176.2(11) | 2502(2) | 24.1(5) |
C13 | 3386.3(19) | 3972.3(10) | 1664.2(18) | 16.6(4) |
C3 | 4149(2) | 7787.6(11) | 4385(2) | 26.2(5) |
C11 | 5624(2) | 3783.5(11) | 2035(2) | 21.2(5) |
C14 | 1994.2(19) | 4850.7(11) | 1300(2) | 21.0(4) |
C12 | 4502(2) | 3031.8(10) | 2750(2) | 20.4(4) |
C9 | 5852(2) | 7118.8(12) | 1922(2) | 22.8(5) |
C18 | 3549(2) | 4909.9(12) | 580(2) | 24.5(5) |
C15 | 1795(2) | 5562.4(12) | 1175(2) | 26.0(5) |
C7 | 7908(2) | 6910.7(13) | 1988(2) | 30.2(5) |
C21 | 9621(2) | 5269.3(13) | 2614(2) | 30.1(5) |
C17 | 3393(2) | 5624.1(13) | 429(2) | 29.5(5) |
C16 | 2109(2) | 5825.6(13) | 207(2) | 32.0(6) |
C8 | 6588(2) | 6697.0(12) | 1490(2) | 26.9(5) |
C19 | 8625(2) | 5035.8(15) | 2911(3) | 38.2(7) |
C20B | 8770(5) | 4278(4) | 3187(8) | 48(3) |
C20A | 9040(8) | 4762(6) | 4147(8) | 91(4) |
Atom | U11 | U22 | U33 | U23 | U13 | U12 |
---|---|---|---|---|---|---|
Br1 | 18.24(11) | 22.63(12) | 21.73(12) | 4.36(8) | 6.29(9) | 2.41(8) |
Br2 | 14.31(11) | 23.20(12) | 30.65(13) | 4.03(9) | 11.71(9) | 5.93(8) |
Zn2 | 12.43(12) | 9.61(12) | 14.46(12) | -1.48(8) | 6.57(9) | -0.81(8) |
Zn3 | 11.70(12) | 10.76(12) | 14.39(12) | 0.31(8) | 6.82(9) | 1.34(8) |
Zn1 | 13.25(12) | 9.42(12) | 19.37(13) | 0.94(8) | 8.92(10) | -0.03(8) |
O3 | 18.8(7) | 13.3(7) | 21.0(8) | -4.3(6) | 12.8(6) | -4.1(6) |
O1 | 16.2(7) | 9.7(7) | 24.8(8) | 4.7(6) | 12.0(6) | 3.0(5) |
O4 | 15.4(7) | 10.8(7) | 12.4(6) | -3.1(5) | 5.2(6) | -0.1(5) |
O2 | 16.9(7) | 13.1(7) | 28.1(8) | -3.1(6) | 14.3(7) | -2.2(6) |
N1 | 17.4(8) | 12.4(8) | 21.0(9) | 1.0(7) | 10.8(7) | -1.8(7) |
O5 | 31.9(10) | 37.0(11) | 52.8(12) | 2.7(9) | 27.9(9) | 4.8(8) |
N2 | 14.7(8) | 17.8(9) | 12.4(8) | 0.7(7) | 5.5(7) | -0.3(7) |
C5 | 19.6(10) | 17.7(11) | 30.3(12) | 0.2(9) | 12.8(9) | -6.2(9) |
C4 | 24.8(11) | 9.5(9) | 28.4(11) | 2.1(8) | 15.6(9) | 0.4(8) |
C10 | 16.1(9) | 12.8(10) | 15.3(10) | -6.3(7) | 7.3(8) | -2.6(7) |
C1 | 20.2(10) | 11.9(10) | 26.5(11) | 6.1(8) | 13.8(9) | 4.0(8) |
C6 | 19.5(10) | 26.5(12) | 36.0(13) | 4.9(10) | 15.8(10) | -1.0(9) |
C2 | 19.3(10) | 24.1(12) | 29.6(12) | 9.9(9) | 11.1(9) | 5.1(9) |
C13 | 17(1) | 16.7(10) | 15.0(9) | -4.6(8) | 5.7(8) | -3.3(8) |
C3 | 33.2(13) | 12.6(10) | 42.0(14) | 4.7(10) | 24.9(12) | 6.3(9) |
C11 | 21.6(11) | 25.3(12) | 21.4(11) | -4.2(9) | 13.6(9) | -0.3(9) |
C14 | 13.8(10) | 25.3(11) | 20.1(10) | 1.3(9) | 3.7(8) | 0.5(8) |
C12 | 22.5(10) | 12.3(10) | 26.7(11) | -6.2(8) | 10.8(9) | -2.9(8) |
C9 | 22.6(11) | 24.7(12) | 21.8(11) | 6.7(9) | 10.3(9) | 1.0(9) |
C18 | 29.5(12) | 31.2(13) | 16.3(10) | 4.0(9) | 13.1(10) | 1.7(10) |
C15 | 21.3(11) | 27.1(13) | 26.7(12) | 6.1(10) | 7.6(10) | 7.2(10) |
C7 | 31.9(13) | 32.0(14) | 38.0(14) | 5.2(11) | 25.7(12) | 1.1(11) |
C21 | 24.4(12) | 31.5(14) | 35.5(13) | 5.1(11) | 13.8(11) | -1.5(10) |
C17 | 35.6(13) | 32.8(14) | 23.2(12) | 11.7(10) | 15.4(11) | 2.0(11) |
C16 | 36.1(14) | 29.8(13) | 23.7(12) | 12(1) | 6.5(11) | 5.5(11) |
C8 | 32.6(13) | 29.2(13) | 24.0(12) | 0.8(10) | 16.9(10) | -0.5(10) |
C19 | 26.6(13) | 47.6(18) | 40.2(15) | 21.1(13) | 14.0(12) | 3.6(12) |
C20B | 19(3) | 48(4) | 74(6) | 37(4) | 17(3) | 4(3) |
C20A | 81(6) | 143(10) | 71(6) | 69(6) | 52(5) | 55(6) |
Atom | Atom | Length/Å | Atom | Atom | Length/Å | |
---|---|---|---|---|---|---|
Br1 | Zn1 | 2.3814(3) | N2 | C13 | 1.485(3) | |
Br2 | Zn3 | 2.3719(3) | N2 | C14 | 1.490(3) | |
Zn2 | O3 | 1.9143(15) | N2 | C18 | 1.491(3) | |
Zn2 | O4 | 1.9397(14) | C5 | C6 | 1.518(3) | |
Zn2 | O2 | 1.9314(15) | C4 | C1 | 1.542(3) | |
Zn2 | N2 | 2.1364(17) | C10 | C13 | 1.540(3) | |
Zn3 | O31 | 1.9672(15) | C10 | C11 | 1.527(3) | |
Zn3 | O11 | 1.9641(14) | C10 | C12 | 1.526(3) | |
Zn3 | O4 | 1.9508(14) | C1 | C2 | 1.532(3) | |
Zn1 | O1 | 1.9609(14) | C1 | C3 | 1.531(3) | |
Zn1 | O2 | 1.9168(15) | C6 | C7 | 1.523(4) | |
Zn1 | N1 | 2.1045(17) | C14 | C15 | 1.517(3) | |
O3 | Zn31 | 1.9672(15) | C9 | C8 | 1.517(3) | |
O1 | Zn31 | 1.9641(14) | C18 | C17 | 1.519(4) | |
O1 | C1 | 1.431(2) | C15 | C16 | 1.528(3) | |
O4 | C10 | 1.424(2) | C7 | C8 | 1.519(3) | |
N1 | C5 | 1.496(3) | C21 | C19 | 1.493(3) | |
N1 | C4 | 1.489(3) | C17 | C16 | 1.522(4) | |
N1 | C9 | 1.494(3) | C19 | C20B | 1.628(8) | |
O5 | C19 | 1.175(3) | C19 | C20A | 1.529(7) |
Atom | Atom | Atom | Angle/˚ | Atom | Atom | Atom | Angle/˚ | |
---|---|---|---|---|---|---|---|---|
O3 | Zn2 | O4 | 120.57(6) | C13 | N2 | C18 | 111.29(17) | |
O3 | Zn2 | O2 | 108.77(7) | C14 | N2 | Zn2 | 111.73(13) | |
O3 | Zn2 | N2 | 112.17(7) | C14 | N2 | C18 | 108.68(17) | |
O4 | Zn2 | N2 | 86.85(6) | C18 | N2 | Zn2 | 115.08(14) | |
O2 | Zn2 | O4 | 116.22(6) | N1 | C5 | C6 | 111.58(18) | |
O2 | Zn2 | N2 | 110.19(7) | N1 | C4 | C1 | 115.87(17) | |
O31 | Zn3 | Br2 | 111.71(5) | O4 | C10 | C13 | 106.90(16) | |
O11 | Zn3 | Br2 | 117.97(4) | O4 | C10 | C11 | 108.86(16) | |
O11 | Zn3 | O31 | 106.38(6) | O4 | C10 | C12 | 109.83(17) | |
O4 | Zn3 | Br2 | 117.12(4) | C11 | C10 | C13 | 114.83(18) | |
O4 | Zn3 | O31 | 95.51(6) | C12 | C10 | C13 | 106.70(17) | |
O4 | Zn3 | O11 | 105.43(6) | C12 | C10 | C11 | 109.63(17) | |
O1 | Zn1 | Br1 | 114.15(5) | O1 | C1 | C4 | 107.30(16) | |
O1 | Zn1 | N1 | 88.53(6) | O1 | C1 | C2 | 109.12(17) | |
O2 | Zn1 | Br1 | 110.82(5) | O1 | C1 | C3 | 110.80(18) | |
O2 | Zn1 | O1 | 111.19(7) | C2 | C1 | C4 | 114.97(18) | |
O2 | Zn1 | N1 | 116.18(7) | C3 | C1 | C4 | 104.92(18) | |
N1 | Zn1 | Br1 | 114.34(5) | C3 | C1 | C2 | 109.65(18) | |
Zn2 | O3 | Zn31 | 133.15(9) | C5 | C6 | C7 | 111.2(2) | |
Zn1 | O1 | Zn31 | 118.82(7) | N2 | C13 | C10 | 115.18(17) | |
C1 | O1 | Zn31 | 126.01(12) | N2 | C14 | C15 | 112.06(18) | |
C1 | O1 | Zn1 | 111.82(12) | N1 | C9 | C8 | 112.42(19) | |
Zn2 | O4 | Zn3 | 120.18(7) | N2 | C18 | C17 | 111.95(19) | |
C10 | O4 | Zn2 | 112.70(12) | C14 | C15 | C16 | 111.0(2) | |
C10 | O4 | Zn3 | 126.63(12) | C8 | C7 | C6 | 109.41(19) | |
Zn1 | O2 | Zn2 | 123.91(8) | C18 | C17 | C16 | 111.3(2) | |
C5 | N1 | Zn1 | 111.54(13) | C17 | C16 | C15 | 109.74(19) | |
C4 | N1 | Zn1 | 99.31(12) | C9 | C8 | C7 | 111.0(2) | |
C4 | N1 | C5 | 108.46(17) | O5 | C19 | C21 | 125.2(3) | |
C4 | N1 | C9 | 110.37(17) | O5 | C19 | C20B | 115.4(3) | |
C9 | N1 | Zn1 | 118.33(14) | O5 | C19 | C20A | 113.9(4) | |
C9 | N1 | C5 | 108.25(17) | C21 | C19 | C20B | 110.6(3) | |
C13 | N2 | Zn2 | 101.21(12) | C21 | C19 | C20A | 115.4(4) | |
C13 | N2 | C14 | 108.55(16) |
A | B | C | D | Angle/˚ | A | B | C | D | Angle/˚ | |
---|---|---|---|---|---|---|---|---|---|---|
Zn2 | O4 | C10 | C13 | -36.56(18) | N1 | C4 | C1 | C3 | 165.85(18) | |
Zn2 | O4 | C10 | C11 | 88.02(17) | N1 | C9 | C8 | C7 | -57.6(3) | |
Zn2 | O4 | C10 | C12 | -151.95(13) | N2 | C14 | C15 | C16 | 57.6(3) | |
Zn2 | N2 | C13 | C10 | -32.19(18) | N2 | C18 | C17 | C16 | -57.3(3) | |
Zn2 | N2 | C14 | C15 | 69.2(2) | C5 | N1 | C4 | C1 | -154.89(19) | |
Zn2 | N2 | C18 | C17 | -67.6(2) | C5 | N1 | C9 | C8 | 58.5(2) | |
Zn31 | O1 | C1 | C4 | 171.95(13) | C5 | C6 | C7 | C8 | -54.8(3) | |
Zn31 | O1 | C1 | C2 | -62.9(2) | C4 | N1 | C5 | C6 | -178.37(18) | |
Zn31 | O1 | C1 | C3 | 57.9(2) | C4 | N1 | C9 | C8 | 177.02(18) | |
Zn3 | O4 | C10 | C13 | 151.58(13) | C6 | C7 | C8 | C9 | 54.1(3) | |
Zn3 | O4 | C10 | C11 | -83.84(19) | C13 | N2 | C14 | C15 | 179.93(18) | |
Zn3 | O4 | C10 | C12 | 36.2(2) | C13 | N2 | C18 | C17 | 178.06(19) | |
Zn1 | O1 | C1 | C4 | -29.2(2) | C11 | C10 | C13 | N2 | -73.4(2) | |
Zn1 | O1 | C1 | C2 | 96.01(16) | C14 | N2 | C13 | C10 | -149.88(17) | |
Zn1 | O1 | C1 | C3 | -143.16(15) | C14 | N2 | C18 | C17 | 58.6(2) | |
Zn1 | N1 | C5 | C6 | 73.3(2) | C14 | C15 | C16 | C17 | -53.6(3) | |
Zn1 | N1 | C4 | C1 | -38.3(2) | C12 | C10 | C13 | N2 | 164.87(17) | |
Zn1 | N1 | C9 | C8 | -69.6(2) | C9 | N1 | C5 | C6 | -58.6(2) | |
O4 | C10 | C13 | N2 | 47.4(2) | C9 | N1 | C4 | C1 | 86.7(2) | |
N1 | C5 | C6 | C7 | 58.5(2) | C18 | N2 | C13 | C10 | 90.6(2) | |
N1 | C4 | C1 | O1 | 47.9(2) | C18 | N2 | C14 | C15 | -58.9(2) | |
N1 | C4 | C1 | C2 | -73.6(2) | C18 | C17 | C16 | C15 | 53.5(3) |
Atom | x | y | z | U(eq) |
---|---|---|---|---|
H5A | 7993 | 7378 | 4574 | 26 |
H5B | 7649 | 7805 | 3424 | 26 |
H4A | 5383 | 7942 | 3059 | 23 |
H4B | 6190 | 7750 | 4396 | 23 |
H6A | 8456 | 6514 | 3645 | 31 |
H6B | 9261 | 7116 | 3643 | 31 |
H2A | 3622 | 6825 | 2102 | 36 |
H2B | 3257 | 7559 | 2017 | 36 |
H2C | 2708 | 7066 | 2630 | 36 |
H13A | 3170 | 3791 | 874 | 20 |
H13B | 2787 | 3812 | 1940 | 20 |
H3A | 3436 | 7635 | 4483 | 39 |
H3B | 3952 | 8192 | 3959 | 39 |
H3C | 4828 | 7850 | 5159 | 39 |
H11A | 5778 | 4233 | 1948 | 32 |
H11B | 5335 | 3573 | 1269 | 32 |
H11C | 6378 | 3581 | 2587 | 32 |
H14A | 1801 | 4695 | 1943 | 25 |
H14B | 1431 | 4641 | 564 | 25 |
H12A | 5296 | 2853 | 3268 | 31 |
H12B | 4160 | 2795 | 2009 | 31 |
H12C | 3950 | 3001 | 3133 | 31 |
H9A | 5839 | 7555 | 1626 | 27 |
H9B | 5003 | 6963 | 1598 | 27 |
H18A | 3003 | 4699 | -162 | 29 |
H18B | 4398 | 4796 | 744 | 29 |
H15A | 2310 | 5771 | 1930 | 31 |
H15B | 933 | 5658 | 986 | 31 |
H7A | 7961 | 7333 | 1667 | 36 |
H7B | 8390 | 6607 | 1759 | 36 |
H21A | 9267 | 5462 | 1831 | 45 |
H21B | 10142 | 4913 | 2622 | 45 |
H21C | 10108 | 5586 | 3195 | 45 |
H17A | 3562 | 5760 | -241 | 35 |
H17B | 3987 | 5837 | 1145 | 35 |
H16A | 1521 | 5664 | -567 | 38 |
H16B | 2055 | 6294 | 194 | 38 |
H8A | 6233 | 6711 | 621 | 32 |
H8B | 6550 | 6253 | 1730 | 32 |
H20A | 8347 | 4165 | 3672 | 71 |
H20B | 9636 | 4171 | 3609 | 71 |
H20C | 8415 | 4041 | 2447 | 71 |
H20D | 9662 | 5039 | 4715 | 137 |
H20E | 9381 | 4338 | 4177 | 137 |
H20F | 8342 | 4735 | 4343 | 137 |
H3 | 3290(30) | 5135(13) | 4180(20) | 16(7) |
H2 | 6190(30) | 5419(16) | 3060(30) | 39(9) |
Atom | Occupancy | Atom | Occupancy | Atom | Occupancy | ||
---|---|---|---|---|---|---|---|
C20B | 0.446(9) | H20A | 0.446(9) | H20B | 0.446(9) | ||
H20C | 0.446(9) | C20A | 0.554(9) | H20D | 0.554(9) | ||
H20E | 0.554(9) | H20F | 0.554(9) |
Experimental
Single crystals of C21H44Br2N2O5Zn3 [mo_B0383_0m] were []. A suitable crystal was selected and [] on a Bruker D8 VENTURE area detector diffractometer. The crystal was kept at 99.99 K during data collection. Using Olex2 [1], the structure was solved with the SIR2004 [2] structure solution program using Direct Methods and refined with the XL [3] refinement package using Least Squares minimisation.
Crystal structure determination of [mo_B0383_0m]
Crystal Data for C21H44Br2N2O5Zn3 (M =760.51 g/mol): monoclinic, space group P21/n (no. 14), a = 12.1460(7) Å, b = 21.0763(13) Å, c = 12.5832(7) Å, β = 115.275(2)°, V = 2912.8(3) Å3, Z = 4, T = 99.99 K, μ(MoKα) = 5.225 mm-1, Dcalc = 1.734 g/cm3, 60917 reflections measured (4.182° ≤ 2Θ ≤ 53.998°), 6355 unique (Rint = 0.0406, Rsigma = 0.0191) which were used in all calculations. The final R1 was 0.0176 (I > 2σ(I)) and wR2 was 0.0702 (all data).
Refinement model description
Number of restraints - 0, number of constraints - unknown.
Details:
1. Fixed Uiso
At 1.2 times of:
All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Others
Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(H20C)=1-FVAR(1)
Sof(C20A)=Sof(H20D)=Sof(H20E)=Sof(H20F)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
C5(H5A,H5B), C4(H4A,H4B), C6(H6A,H6B), C13(H13A,H13B), C14(H14A,H14B), C9(H9A,
H9B), C18(H18A,H18B), C15(H15A,H15B), C7(H7A,H7B), C17(H17A,H17B), C16(H16A,
H16B), C8(H8A,H8B)
3.b Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
C21(H21A,H21B,H21C), C20B(H20A,H20B,H20C), C20A(H20D,H20E,H20F)
This report has been created with Olex2, compiled on 2016.02.19 svn.r3266 for OlexSys. Please let us know if there are any errors or if you would like to have additional features.