
The crystal structures of [1,2-bis(2,6-diisopropylphenylimino)acenaphthene-N,N′]carbonylchlororhodium(I) (1) and [N,N′-ethylene-bis(3-methylsalicylideneiminato)-O,N,N′,O′](tetrahydrofurfuryl)-cobalt(II) (2) have been determined from high-resolution synchrotron X-ray powder diffraction data. Compound 1 is the first neutral Rh complex, in contrast with findings in the literature, containing a bidentate nitrogen ligand, and compound 2 is the first three-dimensional structure of a (five-coordinated) tetrahydrofurfurylcobalt(III) complex. Grid-search and Rietveld refinement have been used to determine and refine the structures, respectively. Crystals of 1 are orthorhombic, space group Pbca, Z = 8, with cell parameters a = 21.729 (2), b = 27.376 (3), c = 11.580 (1) Å. Crystals of 2 are monoclinic, space group P21/n, Z = 4, a = 16.6701 (6), b = 9.4170 (4), c = 13.7088 (7) Å and β = 96.520 (3)°. Chemical diagrams for the two compounds are given. Soft restraints were applied during Rietveld refinement; for 1 converging to Rp = 8.4%, Rw = 11.0%, GoF = 2.3, and for 2 converging to Rp = 8.5%, Rw = 11.4%, GoF = 7.6.
Supporting information
![]() | Crystallographic Information File (CIF) https://doi.org/10.1107/S0909049501013784/wl2002sup1.cif |
Computing details top
For both compounds, cell refinement: UnitCell; data reduction: MRIA; program(s) used to solve structure: MRIA; program(s) used to refine structure: MRIA; molecular graphics: CHEMDRAW and PLATON.
(Compound_1) chloro-CO-(bis(2,6-di-isoprpopylpheylimino)acenaphtene-N,N')-rhodium top
Crystal data top
C37H40ClN2ORh | V = 6888 (2) Å3 |
Mr = 667.07 | Z = 8 |
Orthorhombic, Pbca | Synchrotron radiation, λ = 0.65296 Å |
Hall symbol: -p 2ac 2ab | µ = 0.6 mm−1 |
a = 21.729 (2) Å | T = 293 K |
b = 27.376 (3) Å | cylinder, ? × 0.7 mm mm |
c = 11.579 (1) Å |
Data collection top
ESRF BM16 diffractometer | Data collection mode: transmission |
Radiation source: synchrotron | Scan method: continuous |
Specimen mounting: capillary | 2θmin = 2.500°, 2θmax = 25.00°, 2θstep = 0.005° |
Refinement top
Rp = 8.4 | 175 parameters |
Rwp = 11.1 | 38 restraints |
Rexp = ? | Calculated and kept fixed |
χ2 = 6.250 | |
4500 data points | Background function: polynomal |
Profile function: split-type pseudo-Voigt | Preferred orientation correction: 'Ahtee and Jarvinen' |
Crystal data top
C37H40ClN2ORh | V = 6888 (2) Å3 |
Mr = 667.07 | Z = 8 |
Orthorhombic, Pbca | Synchrotron radiation, λ = 0.65296 Å |
a = 21.729 (2) Å | µ = 0.6 mm−1 |
b = 27.376 (3) Å | T = 293 K |
c = 11.579 (1) Å | cylinder, ? × 0.7 mm mm |
Data collection top
ESRF BM16 diffractometer | Scan method: continuous |
Specimen mounting: capillary | 2θmin = 2.500°, 2θmax = 25.00°, 2θstep = 0.005° |
Data collection mode: transmission |
Refinement top
Rp = 8.4 | 4500 data points |
Rwp = 11.1 | 175 parameters |
Rexp = ? | 38 restraints |
χ2 = 6.250 | Calculated and kept fixed |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Biso*/Beq | ||
Rh1 | 0.5684 (6) | 0.3673 (4) | 0.5327 (10) | * | |
Cl1 | 0.4653 (12) | 0.3676 (9) | 0.5116 (18) | * | |
N1 | 0.6610 (10) | 0.3707 (8) | 0.5681 (19) | * | |
N2 | 0.5655 (10) | 0.3838 (8) | 0.705 (2) | * | |
C1 | 0.6703 (10) | 0.3808 (9) | 0.6734 (18) | * | |
C2 | 0.7244 (10) | 0.3815 (11) | 0.7402 (17) | * | |
C3 | 0.7880 (12) | 0.3750 (10) | 0.7166 (16) | * | |
C4 | 0.8308 (11) | 0.373 (2) | 0.817 (3) | * | |
C5 | 0.8095 (12) | 0.380 (3) | 0.928 (3) | * | |
C6 | 0.7467 (12) | 0.398 (4) | 0.946 (3) | * | |
C7 | 0.7179 (12) | 0.400 (3) | 1.056 (2) | * | |
C8 | 0.6529 (14) | 0.400 (2) | 1.067 (2) | * | |
C9 | 0.6151 (9) | 0.3976 (9) | 0.971 (2) | * | |
C10 | 0.6424 (9) | 0.3921 (10) | 0.862 (2) | * | |
C11 | 0.6204 (10) | 0.3875 (9) | 0.746 (2) | * | |
C12 | 0.7058 (9) | 0.3892 (14) | 0.854 (2) | * | |
C13 | 0.5804 (12) | 0.3525 (11) | 0.366 (3) | * | |
O13 | 0.5851 (13) | 0.3448 (11) | 0.278 (3) | * | |
C14 | 0.7077 (11) | 0.3555 (6) | 0.4867 (18) | * | |
C15 | 0.7234 (12) | 0.3054 (8) | 0.476 (2) | * | |
C16 | 0.7707 (13) | 0.2902 (8) | 0.400 (2) | * | |
C18 | 0.7842 (13) | 0.3743 (8) | 0.340 (2) | * | |
C19 | 0.7381 (12) | 0.3904 (8) | 0.417 (2) | * | |
C20 | 0.6896 (11) | 0.2656 (8) | 0.549 (2) | * | |
C21 | 0.7335 (12) | 0.2405 (8) | 0.630 (2) | * | |
C22 | 0.6568 (10) | 0.2288 (8) | 0.471 (2) | * | |
C23 | 0.7212 (12) | 0.4459 (9) | 0.425 (2) | * | |
C24 | 0.7764 (13) | 0.4753 (8) | 0.467 (2) | * | |
C25 | 0.6980 (11) | 0.4648 (8) | 0.311 (2) | * | |
C26 | 0.5108 (10) | 0.3813 (6) | 0.775 (2) | * | |
C27 | 0.4782 (12) | 0.4246 (8) | 0.802 (2) | * | |
C28 | 0.4273 (12) | 0.4218 (8) | 0.878 (3) | * | |
C29 | 0.4099 (14) | 0.3770 (8) | 0.929 (3) | * | |
C17 | 0.8011 (15) | 0.3254 (8) | 0.335 (3) | * | |
C30 | 0.4385 (12) | 0.3338 (8) | 0.894 (3) | * | |
C31 | 0.4897 (12) | 0.3352 (7) | 0.819 (2) | * | |
C32 | 0.4987 (12) | 0.4744 (9) | 0.752 (2) | * | |
C33 | 0.4493 (14) | 0.4978 (9) | 0.675 (2) | * | |
C34 | 0.5171 (11) | 0.5094 (8) | 0.852 (2) | * | |
C35 | 0.5223 (12) | 0.2876 (8) | 0.788 (2) | * | |
C36 | 0.4807 (12) | 0.2510 (8) | 0.726 (2) | * | |
C37 | 0.5498 (11) | 0.2642 (8) | 0.898 (2) | * | |
H1 | 0.80273 | 0.36977 | 0.63452 | * | |
H2 | 0.87553 | 0.37255 | 0.79426 | * | |
H3 | 0.83992 | 0.38567 | 0.98991 | * | |
H4 | 0.74619 | 0.39694 | 1.12774 | * | |
H5 | 0.63566 | 0.40459 | 1.14665 | * | |
H6 | 0.56971 | 0.40008 | 0.97761 | * | |
H7 | 0.77919 | 0.25485 | 0.38967 | * | |
H8 | 0.83211 | 0.31403 | 0.27445 | * | |
H9 | 0.80656 | 0.39862 | 0.28890 | * | |
H10 | 0.65634 | 0.28327 | 0.59441 | * | |
H11 | 0.76640 | 0.22461 | 0.58515 | * | |
H12 | 0.75116 | 0.26574 | 0.68351 | * | |
H13 | 0.71101 | 0.21551 | 0.67785 | * | |
H14 | 0.62441 | 0.24620 | 0.42087 | * | |
H15 | 0.68620 | 0.21209 | 0.41974 | * | |
H16 | 0.63330 | 0.20350 | 0.51744 | * | |
H17 | 0.68886 | 0.44885 | 0.48102 | * | |
H18 | 0.79058 | 0.46276 | 0.54411 | * | |
H19 | 0.81327 | 0.47030 | 0.41072 | * | |
H20 | 0.76802 | 0.51043 | 0.47085 | * | |
H21 | 0.73195 | 0.45969 | 0.24681 | * | |
H22 | 0.66150 | 0.44596 | 0.28395 | * | |
H23 | 0.68910 | 0.50012 | 0.31176 | * | |
H24 | 0.40127 | 0.45159 | 0.89068 | * | |
H25 | 0.36719 | 0.37442 | 0.96421 | * | |
H26 | 0.42220 | 0.30131 | 0.91827 | * | |
H27 | 0.53578 | 0.46870 | 0.70549 | * | |
H28 | 0.43986 | 0.47522 | 0.61058 | * | |
H29 | 0.41007 | 0.50198 | 0.72382 | * | |
H30 | 0.46204 | 0.52997 | 0.64681 | * | |
H31 | 0.47990 | 0.51334 | 0.90543 | * | |
H32 | 0.55086 | 0.49359 | 0.89863 | * | |
H33 | 0.52987 | 0.54112 | 0.82320 | * | |
H34 | 0.55903 | 0.29602 | 0.73582 | * | |
H35 | 0.44626 | 0.24312 | 0.77591 | * | |
H36 | 0.46760 | 0.26601 | 0.65177 | * | |
H37 | 0.50485 | 0.21997 | 0.70692 | * | |
H38 | 0.58117 | 0.28854 | 0.93443 | * | |
H39 | 0.51778 | 0.25752 | 0.95441 | * | |
H40 | 0.57413 | 0.23387 | 0.88007 | * |
Geometric parameters (Å, º) top
Rh1—C13 | 1.99 (3) | C21—H13 | 1.01 (2) |
Rh1—N2 | 2.04 (3) | C22—H15 | 0.99 (2) |
Rh1—N1 | 2.06 (2) | C22—H16 | 1.01 (2) |
Rh1—Cl1 | 2.26 (3) | C22—H14 | 1.03 (2) |
N1—C1 | 1.27 (3) | C23—H17 | 0.96 (3) |
N1—C14 | 1.45 (3) | C23—C25 | 1.50 (4) |
N2—C11 | 1.29 (3) | C23—C24 | 1.52 (4) |
N2—C26 | 1.44 (3) | C24—H20 | 0.98 (2) |
C1—C11 | 1.38 (3) | C24—H18 | 1.00 (2) |
C1—C2 | 1.41 (3) | C24—H19 | 1.04 (3) |
C2—C12 | 1.40 (3) | C25—H23 | 0.99 (2) |
C2—C3 | 1.42 (3) | C25—H22 | 1.00 (2) |
C3—H1 | 1.01 (2) | C25—H21 | 1.06 (3) |
C3—C4 | 1.49 (4) | C26—C27 | 1.41 (3) |
C4—H2 | 1.01 (3) | C26—C31 | 1.43 (3) |
C4—C5 | 1.38 (4) | C27—C28 | 1.41 (4) |
C5—H3 | 0.98 (3) | C27—C32 | 1.55 (3) |
C5—C6 | 1.46 (6) | C28—H24 | 1.00 (2) |
C6—C12 | 1.40 (4) | C28—C29 | 1.42 (4) |
C6—C7 | 1.43 (4) | C29—H25 | 1.01 (3) |
C7—H4 | 1.03 (3) | C29—C30 | 1.40 (3) |
C7—C8 | 1.42 (4) | C17—H8 | 1.02 (3) |
C8—H5 | 1.00 (3) | C30—H26 | 1.00 (2) |
C8—C9 | 1.39 (4) | C30—C31 | 1.41 (4) |
C9—H6 | 0.99 (2) | C31—C35 | 1.53 (3) |
C9—C10 | 1.40 (3) | C32—H27 | 0.98 (3) |
C10—C12 | 1.38 (3) | C32—C33 | 1.53 (4) |
C10—C11 | 1.44 (3) | C32—C34 | 1.55 (4) |
C13—O13 | 1.04 (4) | C33—H30 | 0.98 (2) |
C14—C19 | 1.41 (3) | C33—H28 | 0.99 (2) |
C14—C15 | 1.42 (3) | C33—H29 | 1.03 (3) |
C15—C16 | 1.42 (4) | C34—H33 | 0.97 (2) |
C15—C20 | 1.56 (3) | C34—H32 | 1.01 (2) |
C16—H7 | 0.99 (2) | C34—H31 | 1.02 (3) |
C16—C17 | 1.39 (4) | C35—H34 | 1.02 (3) |
C18—H9 | 1.02 (2) | C35—C36 | 1.52 (3) |
C18—C17 | 1.39 (3) | C35—C37 | 1.55 (4) |
C18—C19 | 1.41 (4) | C36—H35 | 0.97 (2) |
C19—C23 | 1.57 (3) | C36—H36 | 1.00 (2) |
C20—H10 | 1.01 (2) | C36—H37 | 1.02 (2) |
C20—C21 | 1.50 (3) | C37—H39 | 0.98 (2) |
C20—C22 | 1.53 (3) | C37—H40 | 1.00 (2) |
C21—H11 | 0.98 (2) | C37—H38 | 1.04 (2) |
C21—H12 | 1.01 (2) | ||
C37···H14i | 1.67 (2) | C14···C21 | 3.60 (3) |
C22···H38 | 1.76 (2) | C2···C9 | 3.60 (3) |
C25···H17 | 2.02 (3) | C6···C11 | 3.60 (4) |
C4···H3 | 2.04 (3) | C20···C37 | 3.60 (3) |
C24···H17 | 2.04 (3) | C26···C37 | 3.60 (3) |
C20···H12 | 2.05 (3) | O13···C14 | 3.61 (4) |
C20···H11 | 2.05 (2) | C14···C24 | 3.61 (3) |
C35···H35 | 2.06 (2) | C3···C10 | 3.62 (3) |
C35···H36 | 2.06 (3) | C26···C34 | 3.62 (3) |
C19···H17 | 2.06 (2) | C14···C25 | 3.62 (3) |
C22···H10 | 2.06 (2) | C13···C19 | 3.63 (4) |
C27···H27 | 2.07 (3) | C9···C27 | 3.64 (3) |
C34···H27 | 2.07 (3) | C22···C35 | 3.64 (3) |
C33···H27 | 2.07 (3) | C14···C22 | 3.64 (3) |
C7···H5 | 2.07 (3) | C26···C33 | 3.65 (3) |
C30···H25 | 2.07 (3) | C3···C15 | 3.65 (3) |
C32···H28 | 2.07 (3) | C3···C19 | 3.65 (3) |
C37···H34 | 2.08 (3) | C11···C14 | 3.66 (3) |
C17···H9 | 2.08 (2) | C7···C18 | 3.66 (4) |
C10···H6 | 2.08 (2) | C12···C22i | 3.66 (4) |
C20···H13 | 2.08 (2) | C1···C26 | 3.66 (3) |
C16···H8 | 2.08 (3) | C9···C31 | 3.67 (3) |
C31···H34 | 2.08 (2) | C26···C36 | 3.67 (3) |
C8···H6 | 2.08 (3) | C3···C11 | 3.67 (3) |
C31···H26 | 2.08 (3) | C1···C9 | 3.68 (3) |
C21···H10 | 2.09 (2) | C3···C30 | 3.69 (4) |
C23···H22 | 2.09 (3) | C2···C15 | 3.70 (3) |
C15···H10 | 2.09 (3) | C2···C7 | 3.70 (3) |
C17···H7 | 2.09 (2) | C10···C31 | 3.70 (3) |
C29···H26 | 2.09 (2) | Cl1···C31 | 3.70 (4) |
C9···H5 | 2.09 (2) | C8···C22i | 3.70 (6) |
C32···H29 | 2.09 (3) | Cl1···C27 | 3.72 (4) |
C23···H18 | 2.09 (3) | C5···C10 | 3.72 (3) |
C18···H8 | 2.10 (2) | C10···C27 | 3.74 (3) |
C28···H25 | 2.10 (3) | N2···C28 | 3.75 (4) |
C15···H7 | 2.10 (2) | C4···C27 | 3.76 (4) |
C27···H24 | 2.10 (3) | C2···C19 | 3.76 (3) |
C20···H15 | 2.10 (2) | N1···C18 | 3.76 (4) |
C23···H23 | 2.10 (2) | C4···C7 | 3.77 (4) |
C29···H24 | 2.10 (2) | N2···C30 | 3.78 (4) |
C35···H39 | 2.10 (3) | N1···C16 | 3.78 (3) |
C32···H30 | 2.10 (3) | C5···C8 | 3.80 (4) |
C36···H34 | 2.10 (2) | C8···C11 | 3.80 (3) |
C23···H20 | 2.11 (2) | Rh1···C35 | 3.80 (3) |
C3···H2 | 2.11 (2) | Cl1···O13 | 3.81 (4) |
C35···H37 | 2.11 (2) | N1···O13 | 3.81 (4) |
C6···H4 | 2.11 (3) | C18···C29 | 3.82 (4) |
C23···H21 | 2.11 (3) | Rh1···C15 | 3.83 (3) |
C32···H32 | 2.11 (3) | C29···C35 | 3.83 (4) |
C23···H19 | 2.11 (3) | Rh1···C31 | 3.83 (3) |
C32···H31 | 2.11 (3) | C20···C17 | 3.84 (4) |
C19···H9 | 2.12 (3) | Rh1···C20 | 3.84 (3) |
C32···H33 | 2.12 (2) | C28···C34 | 3.85 (4) |
C6···H3 | 2.12 (3) | C1···C4 | 3.87 (3) |
C20···H14 | 2.12 (3) | C23···C17 | 3.87 (3) |
C2···H1 | 2.12 (2) | C27···C35 | 3.87 (3) |
C5···H2 | 2.12 (3) | O13···C35 | 3.88 (4) |
C20···H16 | 2.13 (2) | C29···C17 | 3.88 (5) |
C35···H38 | 2.13 (3) | C29···C32 | 3.88 (4) |
C35···H40 | 2.14 (2) | C19···C20 | 3.89 (3) |
C8···H4 | 2.15 (3) | C15···C23 | 3.89 (3) |
C4···H1 | 2.20 (3) | C31···C32 | 3.89 (3) |
C11···C12 | 2.24 (3) | C9···O13 | 3.90 (4) |
C1···C12 | 2.24 (3) | C7···C22i | 3.90 (7) |
C2···C11 | 2.27 (3) | O13···C19 | 3.90 (4) |
N1···C11 | 2.29 (3) | C8···C24 | 3.91 (6) |
C1···C10 | 2.29 (3) | C13···C36 | 3.91 (4) |
C2···C10 | 2.29 (3) | O13···C15 | 3.93 (4) |
N2···C1 | 2.31 (3) | C4···C31 | 3.93 (4) |
C7···C12 | 2.37 (4) | C2···C20 | 3.94 (3) |
C8···C10 | 2.39 (3) | Rh1···C37 | 3.95 (2) |
C9···C12 | 2.40 (3) | C12···C24 | 3.95 (4) |
C1···C14 | 2.41 (3) | C7···C21i | 3.96 (7) |
C11···C26 | 2.41 (3) | N1···C21 | 3.96 (3) |
C15···C17 | 2.42 (4) | C13···C22 | 3.96 (4) |
C5···C12 | 2.42 (3) | C10···C35 | 3.97 (3) |
C16···C18 | 2.42 (3) | C13···C20 | 3.97 (4) |
C3···C12 | 2.43 (3) | Rh1···C19 | 3.97 (3) |
C28···C30 | 2.43 (3) | C9···C34 | 3.97 (3) |
C14···C18 | 2.43 (4) | N2···C34 | 3.98 (3) |
C26···C28 | 2.43 (3) | N2···C37 | 3.98 (3) |
N1···C2 | 2.44 (3) | N1···C24 | 3.98 (3) |
C19···C17 | 2.44 (4) | C3···C24 | 3.99 (3) |
C29···C31 | 2.44 (4) | C3···C21 | 4.00 (3) |
C7···C9 | 2.44 (3) | C6···C22i | 4.00 (10) |
C15···C19 | 2.45 (3) | Rh1···C27 | 4.00 (3) |
C4···C6 | 2.45 (5) | C9···C37 | 4.01 (3) |
C26···C30 | 2.46 (3) | N1···C25 | 4.01 (3) |
C14···C16 | 2.46 (3) | C24···C28 | 4.02 (4) |
C27···C29 | 2.47 (4) | C8···C13 | 4.02 (4) |
C27···C31 | 2.47 (3) | N2···C33 | 4.03 (3) |
C6···C10 | 2.47 (4) | N2···C13 | 4.03 (4) |
C2···C6 | 2.47 (4) | N1···C22 | 4.04 (3) |
N2···C27 | 2.47 (3) | C13···C23 | 4.05 (4) |
C6···C8 | 2.48 (4) | C13···C25 | 4.05 (4) |
N1···C19 | 2.48 (3) | Cl1···C33 | 4.05 (3) |
N1···C15 | 2.48 (3) | C2···C23 | 4.05 (3) |
C22···C37 | 2.48 (3) | C10···C32 | 4.06 (3) |
N2···C10 | 2.49 (3) | C4···C26 | 4.06 (3) |
C2···C4 | 2.49 (3) | C10···C37 | 4.06 (3) |
N2···C31 | 2.49 (3) | Cl1···C36 | 4.06 (3) |
C24···C25 | 2.50 (4) | N1···C26 | 4.06 (3) |
C21···C22 | 2.50 (3) | N2···C14 | 4.07 (3) |
C3···C5 | 2.50 (4) | Cl1···C35 | 4.07 (3) |
C36···C37 | 2.51 (3) | C2···C21 | 4.07 (4) |
C31···C37 | 2.51 (3) | N2···C36 | 4.08 (3) |
C15···C21 | 2.52 (3) | Cl1···C32 | 4.10 (3) |
C19···C25 | 2.53 (3) | C11···C37 | 4.10 (3) |
C30···C35 | 2.54 (4) | C1···C21 | 4.11 (3) |
C19···C24 | 2.54 (3) | C36···C37 | 4.12 (4) |
C27···C34 | 2.54 (3) | O13···C25 | 4.12 (4) |
C33···C34 | 2.54 (4) | C2···C8 | 4.13 (3) |
C5···C7 | 2.54 (4) | C18···C21 | 4.13 (3) |
C31···C36 | 2.55 (3) | C24···C29 | 4.13 (4) |
C15···C22 | 2.55 (3) | C1···C13 | 4.14 (4) |
C16···C20 | 2.55 (4) | C13···C35 | 4.14 (4) |
C27···C33 | 2.56 (3) | C19···C29 | 4.15 (4) |
C28···C32 | 2.57 (4) | C7···O13 | 4.15 (5) |
C26···C32 | 2.58 (3) | Rh1···C23 | 4.15 (3) |
C26···C35 | 2.58 (3) | C9···C32 | 4.15 (3) |
C18···C23 | 2.58 (3) | C3···C23 | 4.16 (3) |
C14···C20 | 2.59 (3) | C3···C20 | 4.16 (3) |
C14···C23 | 2.59 (3) | C4···C10 | 4.16 (3) |
C1···C3 | 2.61 (3) | Rh1···C32 | 4.16 (3) |
C9···C11 | 2.62 (3) | Rh1···C2 | 4.17 (2) |
N1···N2 | 2.64 (3) | C23···C33 | 4.18 (4) |
C8···C12 | 2.74 (4) | C13···C33 | 4.18 (4) |
Rh1···C11 | 2.77 (2) | O13···C22 | 4.19 (4) |
Rh1···C1 | 2.77 (2) | C7···C11 | 4.19 (3) |
C4···C12 | 2.78 (3) | C11···C22i | 4.19 (3) |
C7···C10 | 2.79 (3) | Rh1···C10 | 4.20 (3) |
C15···C18 | 2.79 (3) | C9···C35 | 4.20 (3) |
C14···C17 | 2.81 (4) | C9···C24 | 4.20 (3) |
C28···C31 | 2.81 (3) | C11···C34 | 4.20 (3) |
C26···C29 | 2.83 (4) | C1···C24 | 4.21 (3) |
C27···C30 | 2.84 (3) | C10···C34 | 4.21 (3) |
C16···C19 | 2.84 (3) | C7···C19 | 4.21 (4) |
C2···C5 | 2.86 (4) | C10···C24 | 4.21 (4) |
C3···C6 | 2.87 (4) | C15···C21 | 4.21 (3) |
C6···C9 | 2.87 (3) | C7···C17 | 4.22 (5) |
N2···C32 | 2.92 (3) | C1···C5 | 4.22 (4) |
N1···C20 | 2.95 (3) | C2···C24 | 4.23 (3) |
N1···C23 | 2.95 (3) | C6···C25 | 4.23 (10) |
N2···C35 | 2.95 (3) | N1···C17 | 4.26 (4) |
N1···C13 | 2.97 (4) | Cl1···C37 | 4.26 (3) |
Rh1···O13 | 3.03 (3) | N2···C29 | 4.27 (4) |
C2···C14 | 3.04 (3) | C4···C33 | 4.27 (5) |
Cl1···C13 | 3.05 (4) | C9···C28 | 4.27 (3) |
C10···C26 | 3.05 (3) | C3···C7 | 4.27 (3) |
C30···C37 | 3.08 (3) | C5···C9 | 4.28 (3) |
C16···C21 | 3.09 (4) | C2···C22i | 4.29 (3) |
Rh1···C14 | 3.09 (3) | C8···C21i | 4.29 (6) |
Rh1···C26 | 3.10 (3) | Cl1···N1 | 4.30 (3) |
C13···C14 | 3.10 (4) | Rh1···C22 | 4.31 (3) |
C16···C22 | 3.10 (3) | C9···C30 | 4.31 (3) |
C28···C34 | 3.11 (3) | C11···C20 | 4.31 (3) |
C30···C36 | 3.12 (4) | C1···C35 | 4.31 (3) |
C18···C25 | 3.12 (3) | C29···C34 | 4.32 (4) |
C18···C24 | 3.13 (3) | C8···C18 | 4.32 (4) |
C3···C29 | 3.14 (4) | C16···C29 | 4.32 (4) |
Cl1···N2 | 3.15 (3) | C15···C37 | 4.32 (3) |
C28···C33 | 3.17 (4) | C6···C23 | 4.33 (11) |
C3···C14 | 3.23 (3) | Rh1···C36 | 4.34 (3) |
C8···O13 | 3.23 (5) | O13···C21 | 4.34 (4) |
Cl1···C26 | 3.23 (3) | C28···C35 | 4.34 (3) |
C9···C26 | 3.24 (3) | C12···C26 | 4.34 (3) |
N1···C3 | 3.25 (3) | C17···C30 | 4.34 (4) |
C13···C37 | 3.28 (4) | C24···C25 | 4.35 (4) |
C1···C15 | 3.28 (3) | C29···C37 | 4.35 (3) |
N2···C9 | 3.29 (3) | C18···C20 | 4.35 (3) |
C11···C31 | 3.29 (3) | C3···C16 | 4.35 (3) |
C11···C27 | 3.32 (3) | C9···C34 | 4.35 (3) |
C1···C19 | 3.32 (3) | C3···C27 | 4.36 (4) |
C21···C17i | 3.32 (4) | C12···C14 | 4.36 (3) |
C4···C29 | 3.33 (5) | C3···C18 | 4.36 (3) |
C16···C21 | 3.34 (4) | Cl1···C11 | 4.36 (3) |
C4···C28 | 3.35 (4) | C6···C21i | 4.36 (10) |
C25···C33 | 3.36 (4) | C5···C21i | 4.37 (6) |
O13···C37 | 3.38 (4) | O13···C22 | 4.37 (4) |
C3···C28 | 3.46 (4) | C21···C22i | 4.38 (3) |
C7···C25 | 3.47 (5) | C21···C17 | 4.38 (4) |
Cl1···C5 | 3.47 (4) | C30···C32 | 4.39 (3) |
C8···C25 | 3.48 (5) | O13···C23 | 4.39 (4) |
N2···C2 | 3.48 (3) | C22···C17 | 4.40 (4) |
N1···C10 | 3.48 (3) | C5···C24 | 4.40 (7) |
C1···C20 | 3.49 (3) | C27···C34 | 4.40 (4) |
N1···C12 | 3.49 (3) | C29···C34 | 4.40 (3) |
C11···C35 | 3.50 (3) | C22···C31 | 4.40 (3) |
C6···C24 | 3.51 (11) | C16···C23 | 4.41 (3) |
N2···C12 | 3.51 (3) | O13···C33 | 4.41 (4) |
O13···C36 | 3.52 (4) | C24···C17 | 4.41 (3) |
Cl1···C4 | 3.54 (4) | Rh1···C33 | 4.42 (3) |
C34···C34 | 3.55 (4) | C25···C17 | 4.43 (3) |
C4···C30 | 3.55 (4) | Cl1···C30 | 4.56 (4) |
C10···C22i | 3.56 (4) | Cl1···C28 | 4.56 (4) |
C11···C32 | 3.56 (3) | Cl1···C36 | 4.64 (3) |
C1···C23 | 3.56 (3) | Rh1···C25 | 4.65 (3) |
C7···C24 | 3.57 (7) | Cl1···C33 | 4.66 (3) |
C9···C22i | 3.58 (3) | Rh1···C33 | 4.71 (3) |
C1···C6 | 3.59 (4) | Rh1···C12 | 4.81 (2) |
C13···C15 | 3.60 (4) | ||
C13—Rh1—N2 | 174.2 (12) | H16—C22—H14 | 106 (2) |
C13—Rh1—N1 | 94.3 (11) | H16—C22—C20 | 112 (2) |
C13—Rh1—Cl1 | 91.4 (10) | H14—C22—C20 | 110 (2) |
N2—Rh1—N1 | 80.0 (10) | H17—C23—C25 | 108 (2) |
N2—Rh1—Cl1 | 94.2 (9) | H17—C23—C24 | 108 (2) |
N1—Rh1—Cl1 | 174.0 (10) | H17—C23—C19 | 107 (2) |
C1—N1—C14 | 125 (2) | C25—C23—C24 | 111 (2) |
C1—N1—Rh1 | 111.0 (17) | C25—C23—C19 | 111 (2) |
C14—N1—Rh1 | 122.9 (16) | C24—C23—C19 | 110 (2) |
C11—N2—C26 | 124 (2) | H20—C24—H18 | 111 (2) |
C11—N2—Rh1 | 110.3 (17) | H20—C24—H19 | 107 (2) |
C26—N2—Rh1 | 124.6 (17) | H20—C24—C23 | 113 (2) |
N1—C1—C11 | 119 (2) | H18—C24—H19 | 106 (2) |
N1—C1—C2 | 132 (2) | H18—C24—C23 | 110 (2) |
C11—C1—C2 | 108.6 (19) | H19—C24—C23 | 110 (2) |
C12—C2—C1 | 106.3 (19) | H23—C25—H22 | 111 (2) |
C12—C2—C3 | 118.8 (18) | H23—C25—H21 | 106 (2) |
C1—C2—C3 | 134.8 (19) | H23—C25—C23 | 114 (2) |
H1—C3—C2 | 120 (2) | H22—C25—H21 | 105 (2) |
H1—C3—C4 | 122 (2) | H22—C25—C23 | 112 (2) |
C2—C3—C4 | 117.5 (18) | H21—C25—C23 | 110 (2) |
H2—C4—C5 | 125 (3) | C27—C26—C31 | 120 (2) |
H2—C4—C3 | 114 (3) | C27—C26—N2 | 119.6 (18) |
C5—C4—C3 | 121 (2) | C31—C26—N2 | 120.2 (18) |
H3—C5—C4 | 118 (3) | C28—C27—C26 | 119 (2) |
H3—C5—C6 | 118 (4) | C28—C27—C32 | 120 (2) |
C4—C5—C6 | 119 (3) | C26—C27—C32 | 121 (2) |
C12—C6—C7 | 114 (3) | H24—C28—C27 | 119 (2) |
C12—C6—C5 | 115 (5) | H24—C28—C29 | 119 (3) |
C7—C6—C5 | 123 (4) | C27—C28—C29 | 121 (2) |
H4—C7—C8 | 121 (2) | H25—C29—C30 | 118 (2) |
H4—C7—C6 | 117 (3) | H25—C29—C28 | 118 (2) |
C8—C7—C6 | 121 (2) | C30—C29—C28 | 119 (3) |
H5—C8—C9 | 122 (3) | H8—C17—C18 | 120 (3) |
H5—C8—C7 | 117 (3) | H8—C17—C16 | 118 (2) |
C9—C8—C7 | 121 (2) | C18—C17—C16 | 121 (3) |
H6—C9—C8 | 121 (2) | H26—C30—C29 | 121 (3) |
H6—C9—C10 | 120 (2) | H26—C30—C31 | 119 (2) |
C8—C9—C10 | 119 (2) | C29—C30—C31 | 121 (2) |
C12—C10—C9 | 119 (2) | C30—C31—C26 | 119 (2) |
C12—C10—C11 | 105.2 (19) | C30—C31—C35 | 119 (2) |
C9—C10—C11 | 135.5 (19) | C26—C31—C35 | 121 (2) |
N2—C11—C1 | 119 (2) | H27—C32—C33 | 109 (2) |
N2—C11—C10 | 131 (2) | H27—C32—C27 | 108 (2) |
C1—C11—C10 | 108.7 (18) | H27—C32—C34 | 107 (2) |
C10—C12—C2 | 111 (2) | C33—C32—C27 | 113 (2) |
C10—C12—C6 | 125 (2) | C33—C32—C34 | 111 (2) |
C2—C12—C6 | 124 (2) | C27—C32—C34 | 110 (2) |
O13—C13—Rh1 | 178 (3) | H30—C33—H28 | 112 (2) |
C19—C14—C15 | 120 (2) | H30—C33—H29 | 109 (2) |
C19—C14—N1 | 120.2 (17) | H30—C33—C32 | 112 (2) |
C15—C14—N1 | 120 (2) | H28—C33—H29 | 108 (3) |
C14—C15—C16 | 121 (2) | H28—C33—C32 | 109 (2) |
C14—C15—C20 | 121 (2) | H29—C33—C32 | 108 (2) |
C16—C15—C20 | 118.2 (19) | H33—C34—H32 | 111 (2) |
H7—C16—C17 | 121 (3) | H33—C34—H31 | 110 (2) |
H7—C16—C15 | 120 (2) | H33—C34—C32 | 112 (2) |
C17—C16—C15 | 119 (2) | H32—C34—H31 | 107 (2) |
H9—C18—C17 | 118 (3) | H32—C34—C32 | 109 (2) |
H9—C18—C19 | 120 (2) | H31—C34—C32 | 108 (2) |
C17—C18—C19 | 121 (2) | H34—C35—C36 | 110 (2) |
C18—C19—C14 | 119 (2) | H34—C35—C31 | 108 (2) |
C18—C19—C23 | 120 (2) | H34—C35—C37 | 106 (2) |
C14—C19—C23 | 121 (2) | C36—C35—C31 | 113 (2) |
H10—C20—C21 | 110 (2) | C36—C35—C37 | 109.8 (18) |
H10—C20—C22 | 107 (2) | C31—C35—C37 | 110 (2) |
H10—C20—C15 | 106.4 (18) | H35—C36—H36 | 113 (2) |
C21—C20—C22 | 111.1 (18) | H35—C36—H37 | 110 (2) |
C21—C20—C15 | 111 (2) | H35—C36—C35 | 109 (2) |
C22—C20—C15 | 111 (2) | H36—C36—H37 | 107 (2) |
H11—C21—H12 | 111 (2) | H36—C36—C35 | 108 (2) |
H11—C21—H13 | 110 (2) | H37—C36—C35 | 110 (2) |
H11—C21—C20 | 110 (2) | H39—C37—H40 | 111 (2) |
H12—C21—H13 | 108 (2) | H39—C37—H38 | 108 (2) |
H12—C21—C20 | 108.2 (19) | H39—C37—C35 | 111 (2) |
H13—C21—C20 | 110 (2) | H40—C37—H38 | 105 (2) |
H15—C22—H16 | 109 (2) | H40—C37—C35 | 112 (2) |
H15—C22—H14 | 108 (2) | H38—C37—C35 | 108.9 (19) |
H15—C22—C20 | 111 (2) | ||
Cl1—Rh1—N1—C1 | 16 (11) | H9—C18—C17—H8 | −6 (5) |
Cl1—Rh1—N1—C14 | −174 (9) | C14—C19—C23—C24 | 117 (3) |
N2—Rh1—N1—C1 | −0.0 (18) | C14—C19—C23—C25 | −119 (3) |
N2—Rh1—N1—C14 | 170.6 (18) | C14—C19—C23—H17 | 0 (3) |
C13—Rh1—N1—C1 | 179 (2) | C18—C19—C23—C24 | −63 (3) |
C13—Rh1—N1—C14 | −10 (2) | C18—C19—C23—C25 | 61 (3) |
Cl1—Rh1—N2—C11 | −178.7 (18) | C18—C19—C23—H17 | 179 (2) |
Cl1—Rh1—N2—C26 | 13.7 (19) | C15—C20—C21—H11 | −60 (3) |
N1—Rh1—N2—C11 | −0.3 (18) | C15—C20—C21—H12 | 61 (3) |
N1—Rh1—N2—C26 | −168.0 (19) | C15—C20—C21—H13 | 178 (2) |
C13—Rh1—N2—C11 | −9 (13) | C22—C20—C21—H11 | 64 (3) |
C13—Rh1—N2—C26 | −177 (12) | C22—C20—C21—H12 | −175 (2) |
Cl1—Rh1—C13—O13 | 6 (91) | C22—C20—C21—H13 | −57 (3) |
N1—Rh1—C13—O13 | −172 (91) | H10—C20—C21—H11 | −178 (2) |
N2—Rh1—C13—O13 | −163 (84) | H10—C20—C21—H12 | −57 (3) |
Rh1—N1—C1—C2 | 172 (3) | H10—C20—C21—H13 | 61 (3) |
Rh1—N1—C1—C11 | 0 (3) | C15—C20—C22—H14 | −60 (3) |
C14—N1—C1—C2 | 1 (4) | C15—C20—C22—H15 | 60 (3) |
C14—N1—C1—C11 | −170 (2) | C15—C20—C22—H16 | −178 (2) |
Rh1—N1—C14—C15 | −82 (3) | C21—C20—C22—H14 | 176 (2) |
Rh1—N1—C14—C19 | 98 (2) | C21—C20—C22—H15 | −64 (3) |
C1—N1—C14—C15 | 87 (3) | C21—C20—C22—H16 | 58 (3) |
C1—N1—C14—C19 | −93 (3) | H10—C20—C22—H14 | 55 (3) |
Rh1—N2—C11—C1 | 0 (3) | H10—C20—C22—H15 | 175 (2) |
Rh1—N2—C11—C10 | −171 (2) | H10—C20—C22—H16 | −62 (3) |
C26—N2—C11—C1 | 168 (2) | C19—C23—C24—H18 | −57 (3) |
C26—N2—C11—C10 | −3 (4) | C19—C23—C24—H19 | 59 (3) |
Rh1—N2—C26—C27 | −101 (2) | C19—C23—C24—H20 | 178 (2) |
Rh1—N2—C26—C31 | 80 (3) | C25—C23—C24—H18 | 178 (2) |
C11—N2—C26—C27 | 93 (3) | C25—C23—C24—H19 | −65 (3) |
C11—N2—C26—C31 | −87 (3) | C25—C23—C24—H20 | 54 (3) |
N1—C1—C2—C3 | 5 (6) | H17—C23—C24—H18 | 59 (3) |
N1—C1—C2—C12 | −172 (3) | H17—C23—C24—H19 | 175 (2) |
C11—C1—C2—C3 | 177 (3) | H17—C23—C24—H20 | −65 (3) |
C11—C1—C2—C12 | 0 (3) | C19—C23—C25—H21 | −59 (3) |
N1—C1—C11—N2 | 0 (4) | C19—C23—C25—H22 | 57 (3) |
N1—C1—C11—C10 | 173 (2) | C19—C23—C25—H23 | −177 (2) |
C2—C1—C11—N2 | −174 (2) | C24—C23—C25—H21 | 65 (3) |
C2—C1—C11—C10 | 0 (3) | C24—C23—C25—H22 | −179 (2) |
C1—C2—C3—C4 | −173 (4) | C24—C23—C25—H23 | −53 (3) |
C1—C2—C3—H1 | 3 (5) | H17—C23—C25—H21 | −176 (2) |
C12—C2—C3—C4 | 4 (5) | H17—C23—C25—H22 | −60 (3) |
C12—C2—C3—H1 | −179 (3) | H17—C23—C25—H23 | 66 (3) |
C1—C2—C12—C6 | −172 (6) | N2—C26—C27—C28 | −176 (2) |
C1—C2—C12—C10 | 1 (4) | N2—C26—C27—C32 | 3 (4) |
C3—C2—C12—C6 | 10 (7) | C31—C26—C27—C28 | 4 (4) |
C3—C2—C12—C10 | −177 (3) | C31—C26—C27—C32 | −177 (2) |
C2—C3—C4—C5 | −3 (7) | N2—C26—C31—C30 | 176 (2) |
C2—C3—C4—H2 | −173 (4) | N2—C26—C31—C35 | −3 (4) |
H1—C3—C4—C5 | −179 (5) | C27—C26—C31—C30 | −4 (4) |
H1—C3—C4—H2 | 10 (6) | C27—C26—C31—C35 | 178 (2) |
C3—C4—C5—C6 | −12 (*) | C26—C27—C28—C29 | 2 (4) |
C3—C4—C5—H3 | −167 (5) | C26—C27—C28—H24 | −174 (3) |
H2—C4—C5—C6 | 158 (7) | C32—C27—C28—C29 | −176 (3) |
H2—C4—C5—H3 | 2 (11) | C32—C27—C28—H24 | 8 (4) |
C4—C5—C6—C7 | 171 (7) | C26—C27—C32—C33 | 118 (3) |
C4—C5—C6—C12 | 24 (11) | C26—C27—C32—C34 | −118 (3) |
H3—C5—C6—C7 | −33 (13) | C26—C27—C32—H27 | −2 (4) |
H3—C5—C6—C12 | −180 (6) | C28—C27—C32—C33 | −63 (3) |
C5—C6—C7—C8 | −157 (7) | C28—C27—C32—C34 | 61 (3) |
C5—C6—C7—H4 | 16 (13) | C28—C27—C32—H27 | 177 (3) |
C12—C6—C7—C8 | −9 (12) | C27—C28—C29—C30 | −8 (5) |
C12—C6—C7—H4 | 163 (7) | C27—C28—C29—H25 | −163 (3) |
C5—C6—C12—C2 | −24 (10) | H24—C28—C29—C30 | 168 (3) |
C5—C6—C12—C10 | 164 (5) | H24—C28—C29—H25 | 13 (5) |
C7—C6—C12—C2 | −174 (6) | C28—C29—C30—C31 | 8 (5) |
C7—C6—C12—C10 | 14 (11) | C28—C29—C30—H26 | −169 (3) |
C6—C7—C8—C9 | 1 (10) | H25—C29—C30—C31 | 163 (3) |
C6—C7—C8—H5 | −175 (7) | H25—C29—C30—H26 | −14 (5) |
H4—C7—C8—C9 | −171 (6) | C29—C30—C31—C26 | −2 (4) |
H4—C7—C8—H5 | 13 (*) | C29—C30—C31—C35 | 176 (3) |
C7—C8—C9—C10 | 4 (7) | H26—C30—C31—C26 | 175 (3) |
C7—C8—C9—H6 | −176 (5) | H26—C30—C31—C35 | −6 (4) |
H5—C8—C9—C10 | 179 (4) | C26—C31—C35—C36 | −121 (3) |
H5—C8—C9—H6 | 0 (7) | C26—C31—C35—C37 | 116 (3) |
C8—C9—C10—C11 | 179 (4) | C26—C31—C35—H34 | 1 (4) |
C8—C9—C10—C12 | 0 (5) | C30—C31—C35—C36 | 61 (3) |
H6—C9—C10—C11 | −2 (5) | C30—C31—C35—C37 | −62 (3) |
H6—C9—C10—C12 | 180 (3) | C30—C31—C35—H34 | −177 (2) |
C9—C10—C11—N2 | −5 (5) | C27—C32—C33—H28 | −59 (3) |
C9—C10—C11—C1 | −177 (3) | C27—C32—C33—H29 | 58 (3) |
C12—C10—C11—N2 | 174 (3) | C27—C32—C33—H30 | 177 (2) |
C12—C10—C11—C1 | 1 (3) | C34—C32—C33—H28 | 178 (2) |
C9—C10—C12—C2 | 177 (3) | C34—C32—C33—H29 | −65 (3) |
C9—C10—C12—C6 | −10 (7) | C34—C32—C33—H30 | 54 (3) |
C11—C10—C12—C2 | −2 (4) | H27—C32—C33—H28 | 60 (3) |
C11—C10—C12—C6 | 171 (6) | H27—C32—C33—H29 | 177 (2) |
N1—C14—C15—C16 | −178 (2) | H27—C32—C33—H30 | −63 (3) |
N1—C14—C15—C20 | 2 (3) | C27—C32—C34—H31 | −59 (3) |
C19—C14—C15—C16 | 2 (4) | C27—C32—C34—H32 | 57 (3) |
C19—C14—C15—C20 | −178 (2) | C27—C32—C34—H33 | −180 (2) |
N1—C14—C19—C18 | 179 (2) | C33—C32—C34—H31 | 66 (3) |
N1—C14—C19—C23 | −1 (4) | C33—C32—C34—H32 | −178 (2) |
C15—C14—C19—C18 | 0 (4) | C33—C32—C34—H33 | −55 (3) |
C15—C14—C19—C23 | 179 (2) | H27—C32—C34—H31 | −175 (2) |
C14—C15—C16—C17 | 0 (4) | H27—C32—C34—H32 | −59 (3) |
C14—C15—C16—H7 | −176 (2) | H27—C32—C34—H33 | 64 (3) |
C20—C15—C16—C17 | 180 (3) | C31—C35—C36—H35 | −60 (3) |
C20—C15—C16—H7 | 5 (4) | C31—C35—C36—H36 | 63 (3) |
C14—C15—C20—C21 | −117 (2) | C31—C35—C36—H37 | 179 (2) |
C14—C15—C20—C22 | 119 (2) | C37—C35—C36—H35 | 64 (3) |
C14—C15—C20—H10 | 3 (3) | C37—C35—C36—H36 | −174 (2) |
C16—C15—C20—C21 | 63 (3) | C37—C35—C36—H37 | −57 (3) |
C16—C15—C20—C22 | −61 (3) | H34—C35—C36—H35 | 180 (2) |
C16—C15—C20—H10 | −177 (2) | H34—C35—C36—H36 | −58 (3) |
C15—C16—C17—C18 | −2 (4) | H34—C35—C36—H37 | 59 (3) |
C15—C16—C17—H8 | −174 (3) | C31—C35—C37—H38 | −60 (3) |
H7—C16—C17—C18 | 173 (3) | C31—C35—C37—H39 | 59 (3) |
H7—C16—C17—H8 | 0 (5) | C31—C35—C37—H40 | −176 (2) |
C17—C18—C19—C14 | −2 (4) | C36—C35—C37—H38 | 175 (2) |
C17—C18—C19—C23 | 178 (3) | C36—C35—C37—H39 | −66 (3) |
H9—C18—C19—C14 | 179 (2) | C36—C35—C37—H40 | 59 (3) |
H9—C18—C19—C23 | 0 (4) | H34—C35—C37—H38 | 57 (3) |
C19—C18—C17—C16 | 4 (5) | H34—C35—C37—H39 | 175 (2) |
C19—C18—C17—H8 | 176 (3) | H34—C35—C37—H40 | −60 (3) |
H9—C18—C17—C16 | −178 (3) |
Symmetry code: (i) x, −y+1/2, z+1/2. |
(Compound_2) tetrahydrofurfuryl-(N,N'-ethylene-bis(3-methyl-salicylideneiminato
–N,N',O,O')-cobalt top
Crystal data top
C23H27CoN2O3 | β = 96.520 (3)° |
Mr = 438.41 | V = 2138.1 (2) Å3 |
Monoclinic, P21/n | Z = 4 |
Hall symbol: -p 2yn | Synchrotron radiation, λ = 0.65051 Å |
a = 16.6701 (6) Å | µ = 0.8 mm−1 |
b = 9.4170 (4) Å | T = 293 K |
c = 13.7088 (7) Å | cylinder, ? × 0.7 mm mm |
Data collection top
ESRF BM16 diffractometer | Data collection mode: transmission |
Radiation source: synchrotron | Scan method: continuous |
Specimen mounting: capillary | 2θmin = 0.010°, 2θmax = 30.00°, 2θstep = 0.005° |
Refinement top
Rp = 8.5 | 142 parameters |
Rwp = 11.4 | Calculated and kept fixed |
Rexp = ? | |
χ2 = 57.760 | Background function: polynomal |
5999 data points | Preferred orientation correction: 'Ahtee and Jarvinen' |
Profile function: split-type pseudo-Voigt |
Crystal data top
C23H27CoN2O3 | V = 2138.1 (2) Å3 |
Mr = 438.41 | Z = 4 |
Monoclinic, P21/n | Synchrotron radiation, λ = 0.65051 Å |
a = 16.6701 (6) Å | µ = 0.8 mm−1 |
b = 9.4170 (4) Å | T = 293 K |
c = 13.7088 (7) Å | cylinder, ? × 0.7 mm mm |
β = 96.520 (3)° |
Data collection top
ESRF BM16 diffractometer | Scan method: continuous |
Specimen mounting: capillary | 2θmin = 0.010°, 2θmax = 30.00°, 2θstep = 0.005° |
Data collection mode: transmission |
Refinement top
Rp = 8.5 | 5999 data points |
Rwp = 11.4 | 142 parameters |
Rexp = ? | Calculated and kept fixed |
χ2 = 57.760 |
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
x | y | z | Biso*/Beq | ||
Co | 0.5091 (7) | 0.6512 (9) | 0.4239 (9) | * | |
O1 | 0.531 (3) | 0.551 (5) | 0.315 (3) | * | |
O2 | 0.395 (3) | 0.637 (5) | 0.377 (4) | * | |
O3 | 0.540 (4) | 0.932 (5) | 0.193 (3) | * | |
N1 | 0.616 (4) | 0.677 (5) | 0.475 (4) | * | |
N2 | 0.486 (4) | 0.750 (5) | 0.542 (5) | * | |
C1 | 0.599 (5) | 0.502 (8) | 0.294 (5) | * | |
C2 | 0.671 (4) | 0.526 (9) | 0.353 (5) | * | |
C3 | 0.676 (4) | 0.600 (7) | 0.448 (5) | * | |
C4 | 0.337 (4) | 0.724 (8) | 0.415 (5) | * | |
C5 | 0.349 (4) | 0.796 (7) | 0.504 (5) | * | |
C6 | 0.423 (4) | 0.802 (7) | 0.561 (5) | * | |
C7 | 0.562 (5) | 0.754 (7) | 0.615 (5) | * | |
C8 | 0.630 (5) | 0.764 (6) | 0.562 (5) | * | |
C9 | 0.603 (5) | 0.433 (8) | 0.203 (6) | * | |
C10 | 0.679 (5) | 0.383 (7) | 0.177 (5) | * | |
C11 | 0.748 (5) | 0.438 (8) | 0.238 (7) | * | |
C12 | 0.741 (5) | 0.496 (8) | 0.325 (5) | * | |
C13 | 0.534 (4) | 0.387 (7) | 0.138 (4) | * | |
C14 | 0.253 (5) | 0.698 (8) | 0.377 (5) | * | |
C15 | 0.190 (4) | 0.745 (7) | 0.424 (5) | * | |
C16 | 0.206 (4) | 0.827 (7) | 0.511 (5) | * | |
C17 | 0.285 (4) | 0.863 (7) | 0.543 (5) | * | |
C18 | 0.242 (5) | 0.623 (7) | 0.278 (6) | * | |
C19 | 0.504 (5) | 0.834 (6) | 0.343 (5) | * | |
C20 | 0.519 (5) | 0.801 (7) | 0.240 (4) | * | |
C21 | 0.508 (5) | 0.917 (6) | 0.097 (5) | * | |
C22 | 0.463 (4) | 0.783 (5) | 0.076 (5) | * | |
C23 | 0.449 (5) | 0.740 (6) | 0.179 (5) | * | |
H1 | 0.72884 | 0.61379 | 0.48906 | * | |
H2 | 0.43276 | 0.90214 | 0.60771 | * | |
H3 | 0.55768 | 0.84416 | 0.65820 | * | |
H4 | 0.56422 | 0.67196 | 0.65380 | * | |
H5 | 0.63725 | 0.87313 | 0.53487 | * | |
H6 | 0.68218 | 0.74487 | 0.60020 | * | |
H7 | 0.68471 | 0.34137 | 0.11580 | * | |
H8 | 0.80489 | 0.39637 | 0.22219 | * | |
H9 | 0.79623 | 0.51885 | 0.37329 | * | |
H10 | 0.49656 | 0.33205 | 0.17186 | * | |
H11 | 0.50302 | 0.48493 | 0.11774 | * | |
H12 | 0.53528 | 0.34401 | 0.07094 | * | |
H13 | 0.13313 | 0.73514 | 0.39212 | * | |
H14 | 0.15992 | 0.85422 | 0.54692 | * | |
H15 | 0.29630 | 0.90654 | 0.61220 | * | |
H16 | 0.26695 | 0.69110 | 0.22854 | * | |
H17 | 0.26302 | 0.53630 | 0.28082 | * | |
H18 | 0.18150 | 0.62065 | 0.24375 | * | |
H19 | 0.45160 | 0.86780 | 0.33850 | * | |
H20 | 0.54797 | 0.88792 | 0.37344 | * | |
H21 | 0.57209 | 0.73194 | 0.23607 | * | |
H22 | 0.47607 | 0.99620 | 0.06920 | * | |
H23 | 0.55818 | 0.91210 | 0.04944 | * | |
H24 | 0.40989 | 0.79650 | 0.03228 | * | |
H25 | 0.49384 | 0.70628 | 0.03658 | * | |
H26 | 0.40026 | 0.76273 | 0.19330 | * | |
H27 | 0.45486 | 0.62278 | 0.17759 | * |
Geometric parameters (Å, º) top
Co—O1 | 1.83 (5) | C10—C11 | 1.43 (11) |
Co—N1 | 1.86 (6) | C11—H8 | 1.08 (9) |
Co—N2 | 1.94 (6) | C11—C12 | 1.34 (12) |
Co—O2 | 1.95 (5) | C12—H9 | 1.09 (8) |
Co—C19 | 2.05 (6) | C13—H10 | 0.97 (7) |
O1—C1 | 1.30 (9) | C13—H12 | 1.00 (6) |
O2—C4 | 1.40 (9) | C13—H11 | 1.07 (6) |
O3—C21 | 1.36 (8) | C14—C15 | 1.37 (11) |
O3—C20 | 1.45 (8) | C14—C18 | 1.52 (10) |
N1—C3 | 1.31 (9) | C15—H13 | 1.01 (6) |
N1—C8 | 1.44 (9) | C15—C16 | 1.42 (9) |
N2—C6 | 1.22 (10) | C16—H14 | 0.99 (8) |
N2—C7 | 1.52 (9) | C16—C17 | 1.38 (10) |
C1—C2 | 1.38 (10) | C17—H15 | 1.03 (7) |
C1—C9 | 1.42 (11) | C18—H17 | 0.88 (7) |
C2—C12 | 1.31 (11) | C18—H16 | 1.05 (8) |
C2—C3 | 1.46 (10) | C18—H18 | 1.07 (8) |
C3—H1 | 1.00 (6) | C19—H19 | 0.93 (8) |
C4—C5 | 1.39 (10) | C19—H20 | 0.95 (7) |
C4—C14 | 1.46 (11) | C19—C20 | 1.49 (9) |
C5—C6 | 1.39 (9) | C20—H21 | 1.10 (8) |
C5—C17 | 1.40 (10) | C20—C23 | 1.48 (10) |
C6—H2 | 1.14 (7) | C21—H22 | 0.97 (7) |
C7—H4 | 0.94 (7) | C21—H23 | 1.12 (9) |
C7—H3 | 1.04 (7) | C21—C22 | 1.48 (9) |
C7—C8 | 1.42 (11) | C22—H24 | 1.01 (7) |
C8—H6 | 0.98 (7) | C22—H25 | 1.07 (6) |
C8—H5 | 1.10 (6) | C22—C23 | 1.52 (10) |
C9—C13 | 1.43 (10) | C23—H26 | 0.88 (8) |
C9—C10 | 1.44 (11) | C23—H27 | 1.11 (6) |
C10—H7 | 0.94 (7) | ||
N1···H1 | 1.95 (6) | C1···C19 | 3.60 (10) |
C20···H19 | 1.96 (7) | C5···C19 | 3.61 (11) |
N2···H2 | 1.96 (6) | C6···C16 | 3.61 (10) |
C8···H4 | 1.96 (8) | O2···N1 | 3.61 (7) |
C9···H11 | 1.98 (7) | C10···C16 | 3.61 (10) |
O3···H22 | 1.99 (5) | N1···C20 | 3.63 (8) |
C9···H10 | 2.01 (7) | O1···C10 | 3.65 (9) |
C20···H20 | 2.01 (6) | C2···C5 | 3.65 (10) |
C22···H22 | 2.02 (5) | N2···C1 | 3.67 (10) |
C22···H26 | 2.03 (7) | C13···C23 | 3.68 (9) |
O3···H21 | 2.03 (4) | C19···C22 | 3.68 (9) |
O3···H23 | 2.03 (5) | O2···C15 | 3.68 (8) |
C8···H3 | 2.03 (8) | C11···C13 | 3.70 (11) |
N2···H4 | 2.03 (6) | C6···C14 | 3.70 (10) |
C14···H17 | 2.03 (7) | C2···C6 | 3.71 (10) |
N1···H6 | 2.04 (6) | C5···C7 | 3.72 (10) |
N1···H5 | 2.04 (5) | C7···C18 | 3.73 (10) |
C7···H6 | 2.04 (8) | O3···C12 | 3.74 (10) |
C20···H26 | 2.05 (8) | O2···C17 | 3.74 (9) |
C16···H15 | 2.06 (7) | N1···C6 | 3.75 (10) |
C22···H23 | 2.07 (7) | C2···C8 | 3.75 (10) |
C14···H13 | 2.07 (8) | C21···C22 | 3.75 (9) |
C22···H27 | 2.07 (6) | O2···C7 | 3.76 (8) |
C14···H16 | 2.07 (7) | C2···C13 | 3.76 (9) |
C11···H7 | 2.08 (8) | C5···C18 | 3.76 (10) |
N2···H3 | 2.08 (6) | C3···C19 | 3.77 (9) |
C2···H9 | 2.08 (7) | O1···C6 | 3.77 (8) |
C15···H14 | 2.08 (7) | O1···N2 | 3.77 (8) |
C5···H15 | 2.09 (7) | C3···C9 | 3.79 (10) |
C12···H8 | 2.09 (8) | C9···C20 | 3.79 (10) |
C7···H5 | 2.09 (7) | C3···C14 | 3.79 (9) |
C11···H9 | 2.09 (9) | Co···N2 | 3.80 (5) |
C17···H14 | 2.09 (7) | O2···N1 | 3.81 (7) |
C9···H7 | 2.10 (8) | C11···C16 | 3.81 (11) |
C21···H24 | 2.10 (8) | C3···C5 | 3.82 (9) |
C16···H13 | 2.11 (7) | C2···C20 | 3.82 (10) |
C23···H24 | 2.11 (7) | C7···C19 | 3.82 (9) |
C23···H21 | 2.11 (7) | C12···C16 | 3.82 (10) |
C10···H8 | 2.12 (7) | N2···C3 | 3.82 (10) |
C20···H27 | 2.12 (7) | C6···C19 | 3.82 (9) |
C5···H2 | 2.13 (7) | C16···C18 | 3.83 (10) |
C21···H25 | 2.15 (6) | C9···C23 | 3.85 (10) |
C2···H1 | 2.16 (7) | C12···C17 | 3.88 (10) |
O1···H21 | 2.17 (5) | C10···C12 | 3.88 (11) |
C19···H21 | 2.17 (7) | O2···C8 | 3.90 (8) |
C9···H12 | 2.18 (7) | C4···C23 | 3.92 (11) |
C14···H18 | 2.19 (7) | C1···C7 | 3.92 (11) |
C23···H25 | 2.19 (7) | O2···C1 | 3.93 (9) |
C20···C21 | 2.23 (9) | O1···O3 | 3.97 (6) |
C21···C23 | 2.30 (10) | C2···C4 | 3.97 (10) |
C2···C11 | 2.31 (12) | C13···C15 | 3.97 (9) |
C3···C12 | 2.32 (11) | C13···C22 | 3.97 (8) |
N2···C5 | 2.33 (9) | C2···C17 | 3.97 (10) |
N1···C7 | 2.33 (10) | C1···C5 | 3.97 (10) |
O1···C9 | 2.34 (9) | C6···C9 | 3.98 (10) |
O1···C2 | 2.34 (9) | O1···C4 | 3.99 (9) |
C20···C22 | 2.35 (9) | O1···C22 | 4.00 (8) |
C1···C12 | 2.35 (11) | C18···C23 | 4.00 (12) |
O3···C23 | 2.35 (8) | C2···C19 | 4.00 (10) |
C6···C17 | 2.36 (10) | C9···C16 | 4.00 (11) |
N2···C8 | 2.38 (10) | Co···C7 | 4.01 (7) |
C3···C8 | 2.38 (10) | C5···C12 | 4.01 (10) |
C6···C7 | 2.39 (10) | O1···C11 | 4.02 (11) |
O3···C19 | 2.39 (8) | Co···O2 | 4.05 (5) |
O3···C22 | 2.39 (8) | N2···C2 | 4.06 (10) |
C5···C14 | 2.41 (10) | Co···N1 | 4.07 (6) |
C2···C9 | 2.41 (10) | C11···C20 | 4.07 (12) |
C9···C11 | 2.41 (11) | C7···C19 | 4.09 (9) |
C15···C17 | 2.41 (9) | C3···C10 | 4.10 (10) |
C14···C16 | 2.41 (10) | C3···C20 | 4.10 (9) |
C5···C16 | 2.41 (10) | N1···C4 | 4.11 (9) |
C10···C12 | 2.42 (10) | O1···C8 | 4.11 (8) |
O2···C14 | 2.42 (10) | C8···C17 | 4.11 (10) |
C10···C13 | 2.42 (10) | Co···C9 | 4.11 (8) |
C4···C17 | 2.43 (10) | C3···C6 | 4.12 (9) |
N1···C2 | 2.43 (10) | C7···C13 | 4.13 (10) |
C4···C6 | 2.44 (10) | C4···C20 | 4.15 (11) |
Co···H20 | 2.443 (9) | C6···C15 | 4.15 (9) |
C1···C10 | 2.47 (11) | C13···C20 | 4.16 (9) |
C4···C15 | 2.48 (10) | C12···C15 | 4.17 (9) |
O2···C5 | 2.48 (9) | Co···O1 | 4.17 (5) |
Co···H19 | 2.489 (10) | O2···C7 | 4.19 (8) |
C19···C23 | 2.49 (9) | C12···C13 | 4.19 (10) |
C4···C18 | 2.50 (10) | O3···C6 | 4.19 (8) |
C1···C3 | 2.51 (9) | Co···O3 | 4.20 (5) |
C1···C13 | 2.53 (9) | C11···C17 | 4.21 (11) |
C15···C18 | 2.54 (10) | C3···C15 | 4.21 (9) |
N1···N2 | 2.55 (9) | O3···C21 | 4.21 (8) |
O1···C20 | 2.57 (8) | O2···C16 | 4.21 (9) |
O1···O2 | 2.64 (8) | N2···C19 | 4.22 (8) |
O2···C19 | 2.68 (9) | C2···C16 | 4.22 (10) |
O1···C19 | 2.73 (7) | C12···C17 | 4.23 (10) |
O2···C18 | 2.74 (9) | C2···C10 | 4.24 (11) |
C1···C11 | 2.74 (12) | O2···N2 | 4.24 (7) |
O1···N1 | 2.74 (7) | C11···C16 | 4.24 (11) |
C9···C12 | 2.76 (10) | C3···C10 | 4.24 (10) |
C14···C17 | 2.76 (9) | C11···C12 | 4.25 (11) |
C2···C10 | 2.79 (10) | O2···C2 | 4.26 (9) |
O2···N2 | 2.79 (8) | Co···C14 | 4.26 (8) |
C5···C15 | 2.79 (9) | C5···C8 | 4.26 (9) |
Co···C3 | 2.80 (7) | C10···C22 | 4.26 (9) |
Co···C8 | 2.81 (7) | N2···C3 | 4.27 (9) |
O1···C23 | 2.81 (8) | N2···C20 | 4.27 (9) |
Co···C1 | 2.83 (8) | C12···C21 | 4.27 (12) |
Co···C7 | 2.83 (7) | C17···C18 | 4.27 (10) |
C4···C16 | 2.84 (11) | N2···C14 | 4.29 (10) |
N1···C19 | 2.86 (8) | C7···C9 | 4.29 (11) |
Co···C6 | 2.87 (7) | C9···C22 | 4.29 (9) |
N2···C4 | 2.87 (9) | C16···C21 | 4.30 (11) |
O1···C13 | 2.89 (8) | C13···C21 | 4.31 (9) |
O1···C3 | 2.89 (8) | N2···C9 | 4.31 (10) |
N2···C19 | 2.89 (9) | C13···C16 | 4.32 (10) |
Co···C20 | 2.91 (6) | C2···C14 | 4.32 (10) |
Co···C4 | 2.94 (7) | C6···C12 | 4.33 (11) |
O2···C6 | 2.96 (8) | C2···C11 | 4.34 (11) |
N1···C1 | 2.96 (9) | C15···C21 | 4.34 (11) |
C21···C21 | 3.07 (9) | C9···C22 | 4.35 (10) |
O2···C23 | 3.11 (9) | O3···C1 | 4.35 (9) |
C1···C20 | 3.16 (10) | O3···C13 | 4.35 (8) |
Co···C2 | 3.19 (8) | C3···C11 | 4.36 (11) |
C4···C19 | 3.23 (11) | N1···N2 | 4.36 (7) |
Co···C5 | 3.30 (7) | N1···C9 | 4.36 (9) |
O2···C20 | 3.33 (9) | C13···C13 | 4.36 (8) |
C13···C22 | 3.34 (9) | C16···C22 | 4.37 (11) |
C11···C17 | 3.37 (11) | C3···C18 | 4.38 (10) |
C6···C19 | 3.44 (10) | C9···C17 | 4.38 (11) |
O1···C7 | 3.45 (8) | C4···C7 | 4.38 (10) |
C3···C7 | 3.46 (10) | C1···C8 | 4.40 (10) |
C6···C8 | 3.46 (11) | Co···C3 | 4.40 (7) |
C19···C21 | 3.46 (10) | C3···C17 | 4.41 (10) |
O1···N2 | 3.48 (7) | Co···C6 | 4.41 (6) |
Co···C23 | 3.49 (7) | C1···C22 | 4.42 (9) |
C8···C18 | 3.50 (10) | C1···C17 | 4.42 (10) |
N1···C12 | 3.52 (10) | C2···C15 | 4.43 (9) |
C8···C19 | 3.52 (10) | C13···C16 | 4.43 (10) |
N2···C17 | 3.52 (10) | C4···C12 | 4.44 (11) |
C1···C6 | 3.53 (10) | C11···C21 | 4.44 (12) |
O1···C12 | 3.53 (10) | Co···C12 | 4.48 (9) |
Co···Co | 3.564 (14) | Co···C8 | 4.56 (7) |
O3···C11 | 3.57 (10) | Co···C18 | 4.67 (8) |
O2···C3 | 3.57 (9) | Co···C1 | 4.68 (8) |
C3···C11 | 3.58 (11) | Co···C17 | 4.70 (8) |
C1···C23 | 3.59 (10) | Co···C13 | 4.70 (6) |
C10···C17 | 3.59 (10) | Co···C4 | 4.76 (7) |
C3···C4 | 3.60 (10) | Co···C2 | 4.82 (8) |
O1—Co—N1 | 96 (3) | H9—C12—C2 | 120 (7) |
O1—Co—N2 | 178 (2) | H9—C12—C11 | 118 (8) |
O1—Co—O2 | 88 (2) | C2—C12—C11 | 121 (7) |
O1—Co—C19 | 89 (2) | H10—C13—H12 | 108 (6) |
N1—Co—N2 | 84 (3) | H10—C13—H11 | 105 (6) |
N1—Co—O2 | 175 (2) | H10—C13—C9 | 112 (6) |
N1—Co—C19 | 94 (3) | H12—C13—H11 | 100 (5) |
N2—Co—O2 | 92 (2) | H12—C13—C9 | 126 (7) |
N2—Co—C19 | 93 (2) | H11—C13—C9 | 103 (5) |
O2—Co—C19 | 84 (3) | C15—C14—C4 | 122 (6) |
C1—O1—Co | 129 (5) | C15—C14—C18 | 123 (7) |
C4—O2—Co | 121 (4) | C4—C14—C18 | 114 (7) |
C21—O3—C20 | 105 (5) | H13—C15—C14 | 120 (6) |
C3—N1—C8 | 120 (6) | H13—C15—C16 | 120 (6) |
C3—N1—Co | 123 (4) | C14—C15—C16 | 119 (6) |
C8—N1—Co | 116 (5) | H14—C16—C17 | 123 (7) |
C6—N2—C7 | 121 (6) | H14—C16—C15 | 118 (6) |
C6—N2—Co | 129 (5) | C17—C16—C15 | 119 (7) |
C7—N2—Co | 109 (5) | H15—C17—C16 | 118 (7) |
O1—C1—C2 | 122 (7) | H15—C17—C5 | 118 (6) |
O1—C1—C9 | 119 (6) | C16—C17—C5 | 120 (6) |
C2—C1—C9 | 119 (7) | H17—C18—H16 | 114 (9) |
C12—C2—C1 | 122 (7) | H17—C18—H18 | 110 (7) |
C12—C2—C3 | 114 (6) | H17—C18—C14 | 113 (7) |
C1—C2—C3 | 124 (7) | H16—C18—H18 | 98 (6) |
H1—C3—N1 | 114 (6) | H16—C18—C14 | 106 (6) |
H1—C3—C2 | 121 (7) | H18—C18—C14 | 115 (7) |
N1—C3—C2 | 123 (6) | H19—C19—H20 | 121 (7) |
C5—C4—O2 | 125 (6) | H19—C19—C20 | 106 (6) |
C5—C4—C14 | 116 (7) | H19—C19—Co | 108 (5) |
O2—C4—C14 | 116 (6) | H20—C19—C20 | 109 (7) |
C4—C5—C6 | 123 (7) | H20—C19—Co | 103 (5) |
C4—C5—C17 | 121 (6) | C20—C19—Co | 110 (4) |
C6—C5—C17 | 116 (6) | H21—C20—O3 | 105 (6) |
H2—C6—N2 | 113 (6) | H21—C20—C23 | 109 (5) |
H2—C6—C5 | 114 (6) | H21—C20—C19 | 113 (5) |
N2—C6—C5 | 127 (7) | O3—C20—C23 | 107 (5) |
H4—C7—H3 | 110 (7) | O3—C20—C19 | 109 (5) |
H4—C7—C8 | 111 (7) | C23—C20—C19 | 114 (7) |
H4—C7—N2 | 110 (6) | H22—C21—H23 | 102 (6) |
H3—C7—C8 | 110 (6) | H22—C21—O3 | 116 (6) |
H3—C7—N2 | 107 (6) | H22—C21—C22 | 110 (7) |
C8—C7—N2 | 109 (6) | H23—C21—O3 | 109 (7) |
H6—C8—H5 | 103 (6) | H23—C21—C22 | 104 (5) |
H6—C8—C7 | 115 (7) | O3—C21—C22 | 114 (5) |
H6—C8—N1 | 113 (6) | H24—C22—H25 | 103 (5) |
H5—C8—C7 | 111 (6) | H24—C22—C21 | 113 (5) |
H5—C8—N1 | 105 (6) | H24—C22—C23 | 112 (7) |
C7—C8—N1 | 109 (6) | H25—C22—C21 | 114 (7) |
C1—C9—C13 | 125 (7) | H25—C22—C23 | 115 (5) |
C1—C9—C10 | 119 (6) | C21—C22—C23 | 100 (5) |
C13—C9—C10 | 115 (6) | H26—C23—H27 | 110 (6) |
H7—C10—C11 | 122 (8) | H26—C23—C20 | 118 (6) |
H7—C10—C9 | 122 (7) | H26—C23—C22 | 112 (6) |
C11—C10—C9 | 114 (7) | H27—C23—C20 | 109 (6) |
H8—C11—C12 | 119 (8) | H27—C23—C22 | 103 (5) |
H8—C11—C10 | 115 (7) | C20—C23—C22 | 103 (6) |
C12—C11—C10 | 122 (8) | ||
O2—Co—O1—C1 | −174 (6) | C4—C5—C6—N2 | 2 (12) |
N1—Co—O1—C1 | 8 (6) | C4—C5—C6—H2 | 151 (7) |
N2—Co—O1—C1 | −82 (66) | C17—C5—C6—N2 | 179 (7) |
C19—Co—O1—C1 | 102 (6) | C17—C5—C6—H2 | −32 (9) |
O1—Co—O2—C4 | −164 (5) | C4—C5—C17—C16 | 19 (10) |
N1—Co—O2—C4 | −7 (32) | C4—C5—C17—H15 | 174 (6) |
N2—Co—O2—C4 | 18 (5) | C6—C5—C17—C16 | −159 (6) |
C19—Co—O2—C4 | −75 (5) | C6—C5—C17—H15 | −3 (*) |
O1—Co—N1—C3 | −19 (6) | N2—C7—C8—N1 | −38 (7) |
O1—Co—N1—C8 | 176 (4) | N2—C7—C8—H5 | 77 (7) |
O2—Co—N1—C3 | −176 (27) | N2—C7—C8—H6 | −166 (5) |
O2—Co—N1—C8 | 18 (32) | H3—C7—C8—N1 | −155 (5) |
N2—Co—N1—C3 | 159 (6) | H3—C7—C8—H5 | −40 (8) |
N2—Co—N1—C8 | −7 (4) | H3—C7—C8—H6 | 77 (7) |
C19—Co—N1—C3 | −108 (6) | H4—C7—C8—N1 | 82 (7) |
C19—Co—N1—C8 | 86 (5) | H4—C7—C8—H5 | −162 (6) |
O1—Co—N2—C6 | −103 (64) | H4—C7—C8—H6 | −46 (9) |
O1—Co—N2—C7 | 76 (65) | C1—C9—C10—C11 | −13 (10) |
O2—Co—N2—C6 | −12 (6) | C1—C9—C10—H7 | −176 (7) |
O2—Co—N2—C7 | 167 (4) | C13—C9—C10—C11 | 175 (6) |
N1—Co—N2—C6 | 166 (6) | C13—C9—C10—H7 | 12 (11) |
N1—Co—N2—C7 | −15 (4) | C1—C9—C13—H10 | −51 (*) |
C19—Co—N2—C6 | 72 (6) | C1—C9—C13—H11 | 62 (9) |
C19—Co—N2—C7 | −108 (4) | C1—C9—C13—H12 | 175 (7) |
O1—Co—C19—C20 | 0 (5) | C10—C9—C13—H10 | 120 (7) |
O1—Co—C19—H19 | 115 (5) | C10—C9—C13—H11 | −127 (6) |
O1—Co—C19—H20 | −116 (5) | C10—C9—C13—H12 | −14 (10) |
O2—Co—C19—C20 | −88 (5) | C9—C10—C11—C12 | 17 (11) |
O2—Co—C19—H19 | 26 (5) | C9—C10—C11—H8 | 176 (7) |
O2—Co—C19—H20 | 156 (5) | H7—C10—C11—C12 | −179 (7) |
N1—Co—C19—C20 | 96 (5) | H7—C10—C11—H8 | −21 (11) |
N1—Co—C19—H19 | −149 (5) | C10—C11—C12—C2 | −11 (12) |
N1—Co—C19—H20 | −20 (5) | C10—C11—C12—H9 | 170 (7) |
N2—Co—C19—C20 | −180 (5) | H8—C11—C12—C2 | −169 (8) |
N2—Co—C19—H19 | −65 (5) | H8—C11—C12—H9 | 12 (12) |
N2—Co—C19—H20 | 64 (5) | C4—C14—C15—C16 | 3 (10) |
Co—O1—C1—C2 | −3 (11) | C4—C14—C15—H13 | 173 (6) |
Co—O1—C1—C9 | −177 (5) | C18—C14—C15—C16 | −174 (6) |
Co—O2—C4—C5 | −19 (9) | C18—C14—C15—H13 | −4 (10) |
Co—O2—C4—C14 | −177 (5) | C4—C14—C18—H16 | −62 (8) |
C21—O3—C20—C19 | −146 (6) | C4—C14—C18—H17 | 64 (*) |
C21—O3—C20—C23 | −22 (8) | C4—C14—C18—H18 | −169 (6) |
C21—O3—C20—H21 | 93 (6) | C15—C14—C18—H16 | 115 (8) |
C20—O3—C21—C22 | 2 (9) | C15—C14—C18—H17 | −120 (9) |
C20—O3—C21—H22 | 131 (8) | C15—C14—C18—H18 | 8 (*) |
C20—O3—C21—H23 | −114 (6) | C14—C15—C16—C17 | 3 (*) |
Co—N1—C3—C2 | 24 (9) | C14—C15—C16—H14 | −176 (6) |
Co—N1—C3—H1 | −170 (5) | H13—C15—C16—C17 | −167 (6) |
C8—N1—C3—C2 | −170 (6) | H13—C15—C16—H14 | 14 (*) |
C8—N1—C3—H1 | −5 (9) | C15—C16—C17—C5 | −14 (*) |
Co—N1—C8—C7 | 28 (6) | C15—C16—C17—H15 | −169 (6) |
Co—N1—C8—H5 | −92 (6) | H14—C16—C17—C5 | 166 (6) |
Co—N1—C8—H6 | 157 (5) | H14—C16—C17—H15 | 10 (11) |
C3—N1—C8—C7 | −138 (6) | Co—C19—C20—O3 | −163 (5) |
C3—N1—C8—H5 | 102 (7) | Co—C19—C20—C23 | 78 (6) |
C3—N1—C8—H6 | −9 (9) | Co—C19—C20—H21 | −47 (7) |
Co—N2—C6—C5 | 4 (11) | H19—C19—C20—O3 | 81 (7) |
Co—N2—C6—H2 | −145 (5) | H19—C19—C20—C23 | −38 (7) |
C7—N2—C6—C5 | −175 (6) | H19—C19—C20—H21 | −163 (6) |
C7—N2—C6—H2 | 35 (9) | H20—C19—C20—O3 | −51 (8) |
Co—N2—C7—C8 | 33 (6) | H20—C19—C20—C23 | −170 (5) |
Co—N2—C7—H3 | 152 (5) | H20—C19—C20—H21 | 65 (7) |
Co—N2—C7—H4 | −88 (7) | O3—C20—C23—C22 | 33 (7) |
C6—N2—C7—C8 | −147 (6) | O3—C20—C23—H26 | −91 (8) |
C6—N2—C7—H3 | −28 (9) | O3—C20—C23—H27 | 142 (6) |
C6—N2—C7—H4 | 91 (8) | C19—C20—C23—C22 | 153 (5) |
O1—C1—C2—C3 | 4 (12) | C19—C20—C23—H26 | 29 (9) |
O1—C1—C2—C12 | −170 (7) | C19—C20—C23—H27 | −98 (7) |
C9—C1—C2—C3 | 179 (7) | H21—C20—C23—C22 | −79 (6) |
C9—C1—C2—C12 | 5 (12) | H21—C20—C23—H26 | 156 (6) |
O1—C1—C9—C10 | 178 (7) | H21—C20—C23—H27 | 30 (8) |
O1—C1—C9—C13 | −12 (11) | O3—C21—C22—C23 | 18 (8) |
C2—C1—C9—C10 | 3 (11) | O3—C21—C22—H24 | 136 (7) |
C2—C1—C9—C13 | 173 (7) | O3—C21—C22—H25 | −106 (7) |
C1—C2—C3—N1 | −16 (12) | H22—C21—C22—C23 | −115 (7) |
C1—C2—C3—H1 | 179 (7) | H22—C21—C22—H24 | 4 (*) |
C12—C2—C3—N1 | 158 (7) | H22—C21—C22—H25 | 122 (7) |
C12—C2—C3—H1 | −6 (11) | H23—C21—C22—C23 | 137 (6) |
C1—C2—C12—C11 | −1 (13) | H23—C21—C22—H24 | −105 (7) |
C1—C2—C12—H9 | 178 (7) | H23—C21—C22—H25 | 13 (8) |
C3—C2—C12—C11 | −176 (7) | C21—C22—C23—C20 | −30 (7) |
C3—C2—C12—H9 | 4 (11) | C21—C22—C23—H26 | 99 (7) |
O2—C4—C5—C6 | 7 (11) | C21—C22—C23—H27 | −143 (6) |
O2—C4—C5—C17 | −170 (7) | H24—C22—C23—C20 | −149 (5) |
C14—C4—C5—C6 | 165 (7) | H24—C22—C23—H26 | −21 (7) |
C14—C4—C5—C17 | −12 (*) | H24—C22—C23—H27 | 97 (6) |
O2—C4—C14—C15 | 162 (6) | H25—C22—C23—C20 | 93 (6) |
O2—C4—C14—C18 | −21 (9) | H25—C22—C23—H26 | −138 (6) |
C5—C4—C14—C15 | 2 (10) | H25—C22—C23—H27 | −20 (8) |
C5—C4—C14—C18 | 178 (6) |
Experimental details
(Compound_1) | (Compound_2) | |
Crystal data | ||
Chemical formula | C37H40ClN2ORh | C23H27CoN2O3 |
Mr | 667.07 | 438.41 |
Crystal system, space group | Orthorhombic, Pbca | Monoclinic, P21/n |
Temperature (K) | 293 | 293 |
a, b, c (Å) | 21.729 (2), 27.376 (3), 11.579 (1) | 16.6701 (6), 9.4170 (4), 13.7088 (7) |
α, β, γ (°) | 90, 90, 90 | 90, 96.520 (3), 90 |
V (Å3) | 6888 (2) | 2138.1 (2) |
Z | 8 | 4 |
Radiation type | Synchrotron, λ = 0.65296 Å | Synchrotron, λ = 0.65051 Å |
µ (mm−1) | 0.6 | 0.8 |
Specimen shape, size (mm) | Cylinder, ? × 0.7 mm | Cylinder, ? × 0.7 mm |
Data collection | ||
Data collection method | ESRF BM16 | ESRF BM16 |
Specimen mounting | Capillary | Capillary |
Data collection mode | Transmission | Transmission |
Scan method | Continuous | Continuous |
2θ values (°) | 2θmin = 2.500 2θmax = 25.00 2θstep = 0.005 | 2θmin = 0.010 2θmax = 30.00 2θstep = 0.005 |
Refinement | ||
R factors and goodness of fit | Rp = 8.4, Rwp = 11.1, Rexp = ?, χ2 = 6.250 | Rp = 8.5, Rwp = 11.4, Rexp = ?, χ2 = 57.760 |
No. of data points | 4500 | 5999 |
No. of parameters | 175 | 142 |
No. of restraints | 38 | ? |
H-atom treatment | Calculated and kept fixed | Calculated and kept fixed |
Computer programs: UnitCell, MRIA, CHEMDRAW and PLATON.