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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

cif

Crystallographic Information File (CIF) https://doi.org/10.1107/S0909049501013784/wl2002sup1.cif
Contains datablocks global, Compound_1, Compound_2

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.

Figures top
[Figure 1]
[Figure 2]
[Figure 3]
[Figure 4]
[Figure 5]
[Figure 6]
[Figure 7]
(Compound_1) chloro-CO-(bis(2,6-di-isoprpopylpheylimino)acenaphtene-N,N')-rhodium top
Crystal data top
C37H40ClN2ORhV = 6888 (2) Å3
Mr = 667.07Z = 8
Orthorhombic, PbcaSynchrotron radiation, λ = 0.65296 Å
Hall symbol: -p 2ac 2abµ = 0.6 mm1
a = 21.729 (2) ÅT = 293 K
b = 27.376 (3) Åcylinder, ? × 0.7 mm mm
c = 11.579 (1) Å
Data collection top
ESRF BM16
diffractometer
Data collection mode: transmission
Radiation source: synchrotronScan method: continuous
Specimen mounting: capillary2θmin = 2.500°, 2θmax = 25.00°, 2θstep = 0.005°
Refinement top
Rp = 8.4175 parameters
Rwp = 11.138 restraints
Rexp = ?Calculated and kept fixed
χ2 = 6.250
4500 data pointsBackground function: polynomal
Profile function: split-type pseudo-VoigtPreferred orientation correction: 'Ahtee and Jarvinen'
Crystal data top
C37H40ClN2ORhV = 6888 (2) Å3
Mr = 667.07Z = 8
Orthorhombic, PbcaSynchrotron radiation, λ = 0.65296 Å
a = 21.729 (2) ŵ = 0.6 mm1
b = 27.376 (3) ÅT = 293 K
c = 11.579 (1) Åcylinder, ? × 0.7 mm mm
Data collection top
ESRF BM16
diffractometer
Scan method: continuous
Specimen mounting: capillary2θmin = 2.500°, 2θmax = 25.00°, 2θstep = 0.005°
Data collection mode: transmission
Refinement top
Rp = 8.44500 data points
Rwp = 11.1175 parameters
Rexp = ?38 restraints
χ2 = 6.250Calculated and kept fixed
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
Rh10.5684 (6)0.3673 (4)0.5327 (10)*
Cl10.4653 (12)0.3676 (9)0.5116 (18)*
N10.6610 (10)0.3707 (8)0.5681 (19)*
N20.5655 (10)0.3838 (8)0.705 (2)*
C10.6703 (10)0.3808 (9)0.6734 (18)*
C20.7244 (10)0.3815 (11)0.7402 (17)*
C30.7880 (12)0.3750 (10)0.7166 (16)*
C40.8308 (11)0.373 (2)0.817 (3)*
C50.8095 (12)0.380 (3)0.928 (3)*
C60.7467 (12)0.398 (4)0.946 (3)*
C70.7179 (12)0.400 (3)1.056 (2)*
C80.6529 (14)0.400 (2)1.067 (2)*
C90.6151 (9)0.3976 (9)0.971 (2)*
C100.6424 (9)0.3921 (10)0.862 (2)*
C110.6204 (10)0.3875 (9)0.746 (2)*
C120.7058 (9)0.3892 (14)0.854 (2)*
C130.5804 (12)0.3525 (11)0.366 (3)*
O130.5851 (13)0.3448 (11)0.278 (3)*
C140.7077 (11)0.3555 (6)0.4867 (18)*
C150.7234 (12)0.3054 (8)0.476 (2)*
C160.7707 (13)0.2902 (8)0.400 (2)*
C180.7842 (13)0.3743 (8)0.340 (2)*
C190.7381 (12)0.3904 (8)0.417 (2)*
C200.6896 (11)0.2656 (8)0.549 (2)*
C210.7335 (12)0.2405 (8)0.630 (2)*
C220.6568 (10)0.2288 (8)0.471 (2)*
C230.7212 (12)0.4459 (9)0.425 (2)*
C240.7764 (13)0.4753 (8)0.467 (2)*
C250.6980 (11)0.4648 (8)0.311 (2)*
C260.5108 (10)0.3813 (6)0.775 (2)*
C270.4782 (12)0.4246 (8)0.802 (2)*
C280.4273 (12)0.4218 (8)0.878 (3)*
C290.4099 (14)0.3770 (8)0.929 (3)*
C170.8011 (15)0.3254 (8)0.335 (3)*
C300.4385 (12)0.3338 (8)0.894 (3)*
C310.4897 (12)0.3352 (7)0.819 (2)*
C320.4987 (12)0.4744 (9)0.752 (2)*
C330.4493 (14)0.4978 (9)0.675 (2)*
C340.5171 (11)0.5094 (8)0.852 (2)*
C350.5223 (12)0.2876 (8)0.788 (2)*
C360.4807 (12)0.2510 (8)0.726 (2)*
C370.5498 (11)0.2642 (8)0.898 (2)*
H10.802730.369770.63452*
H20.875530.372550.79426*
H30.839920.385670.98991*
H40.746190.396941.12774*
H50.635660.404591.14665*
H60.569710.400080.97761*
H70.779190.254850.38967*
H80.832110.314030.27445*
H90.806560.398620.28890*
H100.656340.283270.59441*
H110.766400.224610.58515*
H120.751160.265740.68351*
H130.711010.215510.67785*
H140.624410.246200.42087*
H150.686200.212090.41974*
H160.633300.203500.51744*
H170.688860.448850.48102*
H180.790580.462760.54411*
H190.813270.470300.41072*
H200.768020.510430.47085*
H210.731950.459690.24681*
H220.661500.445960.28395*
H230.689100.500120.31176*
H240.401270.451590.89068*
H250.367190.374420.96421*
H260.422200.301310.91827*
H270.535780.468700.70549*
H280.439860.475220.61058*
H290.410070.501980.72382*
H300.462040.529970.64681*
H310.479900.513340.90543*
H320.550860.493590.89863*
H330.529870.541120.82320*
H340.559030.296020.73582*
H350.446260.243120.77591*
H360.467600.266010.65177*
H370.504850.219970.70692*
H380.581170.288540.93443*
H390.517780.257520.95441*
H400.574130.233870.88007*
Geometric parameters (Å, º) top
Rh1—C131.99 (3)C21—H131.01 (2)
Rh1—N22.04 (3)C22—H150.99 (2)
Rh1—N12.06 (2)C22—H161.01 (2)
Rh1—Cl12.26 (3)C22—H141.03 (2)
N1—C11.27 (3)C23—H170.96 (3)
N1—C141.45 (3)C23—C251.50 (4)
N2—C111.29 (3)C23—C241.52 (4)
N2—C261.44 (3)C24—H200.98 (2)
C1—C111.38 (3)C24—H181.00 (2)
C1—C21.41 (3)C24—H191.04 (3)
C2—C121.40 (3)C25—H230.99 (2)
C2—C31.42 (3)C25—H221.00 (2)
C3—H11.01 (2)C25—H211.06 (3)
C3—C41.49 (4)C26—C271.41 (3)
C4—H21.01 (3)C26—C311.43 (3)
C4—C51.38 (4)C27—C281.41 (4)
C5—H30.98 (3)C27—C321.55 (3)
C5—C61.46 (6)C28—H241.00 (2)
C6—C121.40 (4)C28—C291.42 (4)
C6—C71.43 (4)C29—H251.01 (3)
C7—H41.03 (3)C29—C301.40 (3)
C7—C81.42 (4)C17—H81.02 (3)
C8—H51.00 (3)C30—H261.00 (2)
C8—C91.39 (4)C30—C311.41 (4)
C9—H60.99 (2)C31—C351.53 (3)
C9—C101.40 (3)C32—H270.98 (3)
C10—C121.38 (3)C32—C331.53 (4)
C10—C111.44 (3)C32—C341.55 (4)
C13—O131.04 (4)C33—H300.98 (2)
C14—C191.41 (3)C33—H280.99 (2)
C14—C151.42 (3)C33—H291.03 (3)
C15—C161.42 (4)C34—H330.97 (2)
C15—C201.56 (3)C34—H321.01 (2)
C16—H70.99 (2)C34—H311.02 (3)
C16—C171.39 (4)C35—H341.02 (3)
C18—H91.02 (2)C35—C361.52 (3)
C18—C171.39 (3)C35—C371.55 (4)
C18—C191.41 (4)C36—H350.97 (2)
C19—C231.57 (3)C36—H361.00 (2)
C20—H101.01 (2)C36—H371.02 (2)
C20—C211.50 (3)C37—H390.98 (2)
C20—C221.53 (3)C37—H401.00 (2)
C21—H110.98 (2)C37—H381.04 (2)
C21—H121.01 (2)
C37···H14i1.67 (2)C14···C213.60 (3)
C22···H381.76 (2)C2···C93.60 (3)
C25···H172.02 (3)C6···C113.60 (4)
C4···H32.04 (3)C20···C373.60 (3)
C24···H172.04 (3)C26···C373.60 (3)
C20···H122.05 (3)O13···C143.61 (4)
C20···H112.05 (2)C14···C243.61 (3)
C35···H352.06 (2)C3···C103.62 (3)
C35···H362.06 (3)C26···C343.62 (3)
C19···H172.06 (2)C14···C253.62 (3)
C22···H102.06 (2)C13···C193.63 (4)
C27···H272.07 (3)C9···C273.64 (3)
C34···H272.07 (3)C22···C353.64 (3)
C33···H272.07 (3)C14···C223.64 (3)
C7···H52.07 (3)C26···C333.65 (3)
C30···H252.07 (3)C3···C153.65 (3)
C32···H282.07 (3)C3···C193.65 (3)
C37···H342.08 (3)C11···C143.66 (3)
C17···H92.08 (2)C7···C183.66 (4)
C10···H62.08 (2)C12···C22i3.66 (4)
C20···H132.08 (2)C1···C263.66 (3)
C16···H82.08 (3)C9···C313.67 (3)
C31···H342.08 (2)C26···C363.67 (3)
C8···H62.08 (3)C3···C113.67 (3)
C31···H262.08 (3)C1···C93.68 (3)
C21···H102.09 (2)C3···C303.69 (4)
C23···H222.09 (3)C2···C153.70 (3)
C15···H102.09 (3)C2···C73.70 (3)
C17···H72.09 (2)C10···C313.70 (3)
C29···H262.09 (2)Cl1···C313.70 (4)
C9···H52.09 (2)C8···C22i3.70 (6)
C32···H292.09 (3)Cl1···C273.72 (4)
C23···H182.09 (3)C5···C103.72 (3)
C18···H82.10 (2)C10···C273.74 (3)
C28···H252.10 (3)N2···C283.75 (4)
C15···H72.10 (2)C4···C273.76 (4)
C27···H242.10 (3)C2···C193.76 (3)
C20···H152.10 (2)N1···C183.76 (4)
C23···H232.10 (2)C4···C73.77 (4)
C29···H242.10 (2)N2···C303.78 (4)
C35···H392.10 (3)N1···C163.78 (3)
C32···H302.10 (3)C5···C83.80 (4)
C36···H342.10 (2)C8···C113.80 (3)
C23···H202.11 (2)Rh1···C353.80 (3)
C3···H22.11 (2)Cl1···O133.81 (4)
C35···H372.11 (2)N1···O133.81 (4)
C6···H42.11 (3)C18···C293.82 (4)
C23···H212.11 (3)Rh1···C153.83 (3)
C32···H322.11 (3)C29···C353.83 (4)
C23···H192.11 (3)Rh1···C313.83 (3)
C32···H312.11 (3)C20···C173.84 (4)
C19···H92.12 (3)Rh1···C203.84 (3)
C32···H332.12 (2)C28···C343.85 (4)
C6···H32.12 (3)C1···C43.87 (3)
C20···H142.12 (3)C23···C173.87 (3)
C2···H12.12 (2)C27···C353.87 (3)
C5···H22.12 (3)O13···C353.88 (4)
C20···H162.13 (2)C29···C173.88 (5)
C35···H382.13 (3)C29···C323.88 (4)
C35···H402.14 (2)C19···C203.89 (3)
C8···H42.15 (3)C15···C233.89 (3)
C4···H12.20 (3)C31···C323.89 (3)
C11···C122.24 (3)C9···O133.90 (4)
C1···C122.24 (3)C7···C22i3.90 (7)
C2···C112.27 (3)O13···C193.90 (4)
N1···C112.29 (3)C8···C243.91 (6)
C1···C102.29 (3)C13···C363.91 (4)
C2···C102.29 (3)O13···C153.93 (4)
N2···C12.31 (3)C4···C313.93 (4)
C7···C122.37 (4)C2···C203.94 (3)
C8···C102.39 (3)Rh1···C373.95 (2)
C9···C122.40 (3)C12···C243.95 (4)
C1···C142.41 (3)C7···C21i3.96 (7)
C11···C262.41 (3)N1···C213.96 (3)
C15···C172.42 (4)C13···C223.96 (4)
C5···C122.42 (3)C10···C353.97 (3)
C16···C182.42 (3)C13···C203.97 (4)
C3···C122.43 (3)Rh1···C193.97 (3)
C28···C302.43 (3)C9···C343.97 (3)
C14···C182.43 (4)N2···C343.98 (3)
C26···C282.43 (3)N2···C373.98 (3)
N1···C22.44 (3)N1···C243.98 (3)
C19···C172.44 (4)C3···C243.99 (3)
C29···C312.44 (4)C3···C214.00 (3)
C7···C92.44 (3)C6···C22i4.00 (10)
C15···C192.45 (3)Rh1···C274.00 (3)
C4···C62.45 (5)C9···C374.01 (3)
C26···C302.46 (3)N1···C254.01 (3)
C14···C162.46 (3)C24···C284.02 (4)
C27···C292.47 (4)C8···C134.02 (4)
C27···C312.47 (3)N2···C334.03 (3)
C6···C102.47 (4)N2···C134.03 (4)
C2···C62.47 (4)N1···C224.04 (3)
N2···C272.47 (3)C13···C234.05 (4)
C6···C82.48 (4)C13···C254.05 (4)
N1···C192.48 (3)Cl1···C334.05 (3)
N1···C152.48 (3)C2···C234.05 (3)
C22···C372.48 (3)C10···C324.06 (3)
N2···C102.49 (3)C4···C264.06 (3)
C2···C42.49 (3)C10···C374.06 (3)
N2···C312.49 (3)Cl1···C364.06 (3)
C24···C252.50 (4)N1···C264.06 (3)
C21···C222.50 (3)N2···C144.07 (3)
C3···C52.50 (4)Cl1···C354.07 (3)
C36···C372.51 (3)C2···C214.07 (4)
C31···C372.51 (3)N2···C364.08 (3)
C15···C212.52 (3)Cl1···C324.10 (3)
C19···C252.53 (3)C11···C374.10 (3)
C30···C352.54 (4)C1···C214.11 (3)
C19···C242.54 (3)C36···C374.12 (4)
C27···C342.54 (3)O13···C254.12 (4)
C33···C342.54 (4)C2···C84.13 (3)
C5···C72.54 (4)C18···C214.13 (3)
C31···C362.55 (3)C24···C294.13 (4)
C15···C222.55 (3)C1···C134.14 (4)
C16···C202.55 (4)C13···C354.14 (4)
C27···C332.56 (3)C19···C294.15 (4)
C28···C322.57 (4)C7···O134.15 (5)
C26···C322.58 (3)Rh1···C234.15 (3)
C26···C352.58 (3)C9···C324.15 (3)
C18···C232.58 (3)C3···C234.16 (3)
C14···C202.59 (3)C3···C204.16 (3)
C14···C232.59 (3)C4···C104.16 (3)
C1···C32.61 (3)Rh1···C324.16 (3)
C9···C112.62 (3)Rh1···C24.17 (2)
N1···N22.64 (3)C23···C334.18 (4)
C8···C122.74 (4)C13···C334.18 (4)
Rh1···C112.77 (2)O13···C224.19 (4)
Rh1···C12.77 (2)C7···C114.19 (3)
C4···C122.78 (3)C11···C22i4.19 (3)
C7···C102.79 (3)Rh1···C104.20 (3)
C15···C182.79 (3)C9···C354.20 (3)
C14···C172.81 (4)C9···C244.20 (3)
C28···C312.81 (3)C11···C344.20 (3)
C26···C292.83 (4)C1···C244.21 (3)
C27···C302.84 (3)C10···C344.21 (3)
C16···C192.84 (3)C7···C194.21 (4)
C2···C52.86 (4)C10···C244.21 (4)
C3···C62.87 (4)C15···C214.21 (3)
C6···C92.87 (3)C7···C174.22 (5)
N2···C322.92 (3)C1···C54.22 (4)
N1···C202.95 (3)C2···C244.23 (3)
N1···C232.95 (3)C6···C254.23 (10)
N2···C352.95 (3)N1···C174.26 (4)
N1···C132.97 (4)Cl1···C374.26 (3)
Rh1···O133.03 (3)N2···C294.27 (4)
C2···C143.04 (3)C4···C334.27 (5)
Cl1···C133.05 (4)C9···C284.27 (3)
C10···C263.05 (3)C3···C74.27 (3)
C30···C373.08 (3)C5···C94.28 (3)
C16···C213.09 (4)C2···C22i4.29 (3)
Rh1···C143.09 (3)C8···C21i4.29 (6)
Rh1···C263.10 (3)Cl1···N14.30 (3)
C13···C143.10 (4)Rh1···C224.31 (3)
C16···C223.10 (3)C9···C304.31 (3)
C28···C343.11 (3)C11···C204.31 (3)
C30···C363.12 (4)C1···C354.31 (3)
C18···C253.12 (3)C29···C344.32 (4)
C18···C243.13 (3)C8···C184.32 (4)
C3···C293.14 (4)C16···C294.32 (4)
Cl1···N23.15 (3)C15···C374.32 (3)
C28···C333.17 (4)C6···C234.33 (11)
C3···C143.23 (3)Rh1···C364.34 (3)
C8···O133.23 (5)O13···C214.34 (4)
Cl1···C263.23 (3)C28···C354.34 (3)
C9···C263.24 (3)C12···C264.34 (3)
N1···C33.25 (3)C17···C304.34 (4)
C13···C373.28 (4)C24···C254.35 (4)
C1···C153.28 (3)C29···C374.35 (3)
N2···C93.29 (3)C18···C204.35 (3)
C11···C313.29 (3)C3···C164.35 (3)
C11···C273.32 (3)C9···C344.35 (3)
C1···C193.32 (3)C3···C274.36 (4)
C21···C17i3.32 (4)C12···C144.36 (3)
C4···C293.33 (5)C3···C184.36 (3)
C16···C213.34 (4)Cl1···C114.36 (3)
C4···C283.35 (4)C6···C21i4.36 (10)
C25···C333.36 (4)C5···C21i4.37 (6)
O13···C373.38 (4)O13···C224.37 (4)
C3···C283.46 (4)C21···C22i4.38 (3)
C7···C253.47 (5)C21···C174.38 (4)
Cl1···C53.47 (4)C30···C324.39 (3)
C8···C253.48 (5)O13···C234.39 (4)
N2···C23.48 (3)C22···C174.40 (4)
N1···C103.48 (3)C5···C244.40 (7)
C1···C203.49 (3)C27···C344.40 (4)
N1···C123.49 (3)C29···C344.40 (3)
C11···C353.50 (3)C22···C314.40 (3)
C6···C243.51 (11)C16···C234.41 (3)
N2···C123.51 (3)O13···C334.41 (4)
O13···C363.52 (4)C24···C174.41 (3)
Cl1···C43.54 (4)Rh1···C334.42 (3)
C34···C343.55 (4)C25···C174.43 (3)
C4···C303.55 (4)Cl1···C304.56 (4)
C10···C22i3.56 (4)Cl1···C284.56 (4)
C11···C323.56 (3)Cl1···C364.64 (3)
C1···C233.56 (3)Rh1···C254.65 (3)
C7···C243.57 (7)Cl1···C334.66 (3)
C9···C22i3.58 (3)Rh1···C334.71 (3)
C1···C63.59 (4)Rh1···C124.81 (2)
C13···C153.60 (4)
C13—Rh1—N2174.2 (12)H16—C22—H14106 (2)
C13—Rh1—N194.3 (11)H16—C22—C20112 (2)
C13—Rh1—Cl191.4 (10)H14—C22—C20110 (2)
N2—Rh1—N180.0 (10)H17—C23—C25108 (2)
N2—Rh1—Cl194.2 (9)H17—C23—C24108 (2)
N1—Rh1—Cl1174.0 (10)H17—C23—C19107 (2)
C1—N1—C14125 (2)C25—C23—C24111 (2)
C1—N1—Rh1111.0 (17)C25—C23—C19111 (2)
C14—N1—Rh1122.9 (16)C24—C23—C19110 (2)
C11—N2—C26124 (2)H20—C24—H18111 (2)
C11—N2—Rh1110.3 (17)H20—C24—H19107 (2)
C26—N2—Rh1124.6 (17)H20—C24—C23113 (2)
N1—C1—C11119 (2)H18—C24—H19106 (2)
N1—C1—C2132 (2)H18—C24—C23110 (2)
C11—C1—C2108.6 (19)H19—C24—C23110 (2)
C12—C2—C1106.3 (19)H23—C25—H22111 (2)
C12—C2—C3118.8 (18)H23—C25—H21106 (2)
C1—C2—C3134.8 (19)H23—C25—C23114 (2)
H1—C3—C2120 (2)H22—C25—H21105 (2)
H1—C3—C4122 (2)H22—C25—C23112 (2)
C2—C3—C4117.5 (18)H21—C25—C23110 (2)
H2—C4—C5125 (3)C27—C26—C31120 (2)
H2—C4—C3114 (3)C27—C26—N2119.6 (18)
C5—C4—C3121 (2)C31—C26—N2120.2 (18)
H3—C5—C4118 (3)C28—C27—C26119 (2)
H3—C5—C6118 (4)C28—C27—C32120 (2)
C4—C5—C6119 (3)C26—C27—C32121 (2)
C12—C6—C7114 (3)H24—C28—C27119 (2)
C12—C6—C5115 (5)H24—C28—C29119 (3)
C7—C6—C5123 (4)C27—C28—C29121 (2)
H4—C7—C8121 (2)H25—C29—C30118 (2)
H4—C7—C6117 (3)H25—C29—C28118 (2)
C8—C7—C6121 (2)C30—C29—C28119 (3)
H5—C8—C9122 (3)H8—C17—C18120 (3)
H5—C8—C7117 (3)H8—C17—C16118 (2)
C9—C8—C7121 (2)C18—C17—C16121 (3)
H6—C9—C8121 (2)H26—C30—C29121 (3)
H6—C9—C10120 (2)H26—C30—C31119 (2)
C8—C9—C10119 (2)C29—C30—C31121 (2)
C12—C10—C9119 (2)C30—C31—C26119 (2)
C12—C10—C11105.2 (19)C30—C31—C35119 (2)
C9—C10—C11135.5 (19)C26—C31—C35121 (2)
N2—C11—C1119 (2)H27—C32—C33109 (2)
N2—C11—C10131 (2)H27—C32—C27108 (2)
C1—C11—C10108.7 (18)H27—C32—C34107 (2)
C10—C12—C2111 (2)C33—C32—C27113 (2)
C10—C12—C6125 (2)C33—C32—C34111 (2)
C2—C12—C6124 (2)C27—C32—C34110 (2)
O13—C13—Rh1178 (3)H30—C33—H28112 (2)
C19—C14—C15120 (2)H30—C33—H29109 (2)
C19—C14—N1120.2 (17)H30—C33—C32112 (2)
C15—C14—N1120 (2)H28—C33—H29108 (3)
C14—C15—C16121 (2)H28—C33—C32109 (2)
C14—C15—C20121 (2)H29—C33—C32108 (2)
C16—C15—C20118.2 (19)H33—C34—H32111 (2)
H7—C16—C17121 (3)H33—C34—H31110 (2)
H7—C16—C15120 (2)H33—C34—C32112 (2)
C17—C16—C15119 (2)H32—C34—H31107 (2)
H9—C18—C17118 (3)H32—C34—C32109 (2)
H9—C18—C19120 (2)H31—C34—C32108 (2)
C17—C18—C19121 (2)H34—C35—C36110 (2)
C18—C19—C14119 (2)H34—C35—C31108 (2)
C18—C19—C23120 (2)H34—C35—C37106 (2)
C14—C19—C23121 (2)C36—C35—C31113 (2)
H10—C20—C21110 (2)C36—C35—C37109.8 (18)
H10—C20—C22107 (2)C31—C35—C37110 (2)
H10—C20—C15106.4 (18)H35—C36—H36113 (2)
C21—C20—C22111.1 (18)H35—C36—H37110 (2)
C21—C20—C15111 (2)H35—C36—C35109 (2)
C22—C20—C15111 (2)H36—C36—H37107 (2)
H11—C21—H12111 (2)H36—C36—C35108 (2)
H11—C21—H13110 (2)H37—C36—C35110 (2)
H11—C21—C20110 (2)H39—C37—H40111 (2)
H12—C21—H13108 (2)H39—C37—H38108 (2)
H12—C21—C20108.2 (19)H39—C37—C35111 (2)
H13—C21—C20110 (2)H40—C37—H38105 (2)
H15—C22—H16109 (2)H40—C37—C35112 (2)
H15—C22—H14108 (2)H38—C37—C35108.9 (19)
H15—C22—C20111 (2)
Cl1—Rh1—N1—C116 (11)H9—C18—C17—H86 (5)
Cl1—Rh1—N1—C14174 (9)C14—C19—C23—C24117 (3)
N2—Rh1—N1—C10.0 (18)C14—C19—C23—C25119 (3)
N2—Rh1—N1—C14170.6 (18)C14—C19—C23—H170 (3)
C13—Rh1—N1—C1179 (2)C18—C19—C23—C2463 (3)
C13—Rh1—N1—C1410 (2)C18—C19—C23—C2561 (3)
Cl1—Rh1—N2—C11178.7 (18)C18—C19—C23—H17179 (2)
Cl1—Rh1—N2—C2613.7 (19)C15—C20—C21—H1160 (3)
N1—Rh1—N2—C110.3 (18)C15—C20—C21—H1261 (3)
N1—Rh1—N2—C26168.0 (19)C15—C20—C21—H13178 (2)
C13—Rh1—N2—C119 (13)C22—C20—C21—H1164 (3)
C13—Rh1—N2—C26177 (12)C22—C20—C21—H12175 (2)
Cl1—Rh1—C13—O136 (91)C22—C20—C21—H1357 (3)
N1—Rh1—C13—O13172 (91)H10—C20—C21—H11178 (2)
N2—Rh1—C13—O13163 (84)H10—C20—C21—H1257 (3)
Rh1—N1—C1—C2172 (3)H10—C20—C21—H1361 (3)
Rh1—N1—C1—C110 (3)C15—C20—C22—H1460 (3)
C14—N1—C1—C21 (4)C15—C20—C22—H1560 (3)
C14—N1—C1—C11170 (2)C15—C20—C22—H16178 (2)
Rh1—N1—C14—C1582 (3)C21—C20—C22—H14176 (2)
Rh1—N1—C14—C1998 (2)C21—C20—C22—H1564 (3)
C1—N1—C14—C1587 (3)C21—C20—C22—H1658 (3)
C1—N1—C14—C1993 (3)H10—C20—C22—H1455 (3)
Rh1—N2—C11—C10 (3)H10—C20—C22—H15175 (2)
Rh1—N2—C11—C10171 (2)H10—C20—C22—H1662 (3)
C26—N2—C11—C1168 (2)C19—C23—C24—H1857 (3)
C26—N2—C11—C103 (4)C19—C23—C24—H1959 (3)
Rh1—N2—C26—C27101 (2)C19—C23—C24—H20178 (2)
Rh1—N2—C26—C3180 (3)C25—C23—C24—H18178 (2)
C11—N2—C26—C2793 (3)C25—C23—C24—H1965 (3)
C11—N2—C26—C3187 (3)C25—C23—C24—H2054 (3)
N1—C1—C2—C35 (6)H17—C23—C24—H1859 (3)
N1—C1—C2—C12172 (3)H17—C23—C24—H19175 (2)
C11—C1—C2—C3177 (3)H17—C23—C24—H2065 (3)
C11—C1—C2—C120 (3)C19—C23—C25—H2159 (3)
N1—C1—C11—N20 (4)C19—C23—C25—H2257 (3)
N1—C1—C11—C10173 (2)C19—C23—C25—H23177 (2)
C2—C1—C11—N2174 (2)C24—C23—C25—H2165 (3)
C2—C1—C11—C100 (3)C24—C23—C25—H22179 (2)
C1—C2—C3—C4173 (4)C24—C23—C25—H2353 (3)
C1—C2—C3—H13 (5)H17—C23—C25—H21176 (2)
C12—C2—C3—C44 (5)H17—C23—C25—H2260 (3)
C12—C2—C3—H1179 (3)H17—C23—C25—H2366 (3)
C1—C2—C12—C6172 (6)N2—C26—C27—C28176 (2)
C1—C2—C12—C101 (4)N2—C26—C27—C323 (4)
C3—C2—C12—C610 (7)C31—C26—C27—C284 (4)
C3—C2—C12—C10177 (3)C31—C26—C27—C32177 (2)
C2—C3—C4—C53 (7)N2—C26—C31—C30176 (2)
C2—C3—C4—H2173 (4)N2—C26—C31—C353 (4)
H1—C3—C4—C5179 (5)C27—C26—C31—C304 (4)
H1—C3—C4—H210 (6)C27—C26—C31—C35178 (2)
C3—C4—C5—C612 (*)C26—C27—C28—C292 (4)
C3—C4—C5—H3167 (5)C26—C27—C28—H24174 (3)
H2—C4—C5—C6158 (7)C32—C27—C28—C29176 (3)
H2—C4—C5—H32 (11)C32—C27—C28—H248 (4)
C4—C5—C6—C7171 (7)C26—C27—C32—C33118 (3)
C4—C5—C6—C1224 (11)C26—C27—C32—C34118 (3)
H3—C5—C6—C733 (13)C26—C27—C32—H272 (4)
H3—C5—C6—C12180 (6)C28—C27—C32—C3363 (3)
C5—C6—C7—C8157 (7)C28—C27—C32—C3461 (3)
C5—C6—C7—H416 (13)C28—C27—C32—H27177 (3)
C12—C6—C7—C89 (12)C27—C28—C29—C308 (5)
C12—C6—C7—H4163 (7)C27—C28—C29—H25163 (3)
C5—C6—C12—C224 (10)H24—C28—C29—C30168 (3)
C5—C6—C12—C10164 (5)H24—C28—C29—H2513 (5)
C7—C6—C12—C2174 (6)C28—C29—C30—C318 (5)
C7—C6—C12—C1014 (11)C28—C29—C30—H26169 (3)
C6—C7—C8—C91 (10)H25—C29—C30—C31163 (3)
C6—C7—C8—H5175 (7)H25—C29—C30—H2614 (5)
H4—C7—C8—C9171 (6)C29—C30—C31—C262 (4)
H4—C7—C8—H513 (*)C29—C30—C31—C35176 (3)
C7—C8—C9—C104 (7)H26—C30—C31—C26175 (3)
C7—C8—C9—H6176 (5)H26—C30—C31—C356 (4)
H5—C8—C9—C10179 (4)C26—C31—C35—C36121 (3)
H5—C8—C9—H60 (7)C26—C31—C35—C37116 (3)
C8—C9—C10—C11179 (4)C26—C31—C35—H341 (4)
C8—C9—C10—C120 (5)C30—C31—C35—C3661 (3)
H6—C9—C10—C112 (5)C30—C31—C35—C3762 (3)
H6—C9—C10—C12180 (3)C30—C31—C35—H34177 (2)
C9—C10—C11—N25 (5)C27—C32—C33—H2859 (3)
C9—C10—C11—C1177 (3)C27—C32—C33—H2958 (3)
C12—C10—C11—N2174 (3)C27—C32—C33—H30177 (2)
C12—C10—C11—C11 (3)C34—C32—C33—H28178 (2)
C9—C10—C12—C2177 (3)C34—C32—C33—H2965 (3)
C9—C10—C12—C610 (7)C34—C32—C33—H3054 (3)
C11—C10—C12—C22 (4)H27—C32—C33—H2860 (3)
C11—C10—C12—C6171 (6)H27—C32—C33—H29177 (2)
N1—C14—C15—C16178 (2)H27—C32—C33—H3063 (3)
N1—C14—C15—C202 (3)C27—C32—C34—H3159 (3)
C19—C14—C15—C162 (4)C27—C32—C34—H3257 (3)
C19—C14—C15—C20178 (2)C27—C32—C34—H33180 (2)
N1—C14—C19—C18179 (2)C33—C32—C34—H3166 (3)
N1—C14—C19—C231 (4)C33—C32—C34—H32178 (2)
C15—C14—C19—C180 (4)C33—C32—C34—H3355 (3)
C15—C14—C19—C23179 (2)H27—C32—C34—H31175 (2)
C14—C15—C16—C170 (4)H27—C32—C34—H3259 (3)
C14—C15—C16—H7176 (2)H27—C32—C34—H3364 (3)
C20—C15—C16—C17180 (3)C31—C35—C36—H3560 (3)
C20—C15—C16—H75 (4)C31—C35—C36—H3663 (3)
C14—C15—C20—C21117 (2)C31—C35—C36—H37179 (2)
C14—C15—C20—C22119 (2)C37—C35—C36—H3564 (3)
C14—C15—C20—H103 (3)C37—C35—C36—H36174 (2)
C16—C15—C20—C2163 (3)C37—C35—C36—H3757 (3)
C16—C15—C20—C2261 (3)H34—C35—C36—H35180 (2)
C16—C15—C20—H10177 (2)H34—C35—C36—H3658 (3)
C15—C16—C17—C182 (4)H34—C35—C36—H3759 (3)
C15—C16—C17—H8174 (3)C31—C35—C37—H3860 (3)
H7—C16—C17—C18173 (3)C31—C35—C37—H3959 (3)
H7—C16—C17—H80 (5)C31—C35—C37—H40176 (2)
C17—C18—C19—C142 (4)C36—C35—C37—H38175 (2)
C17—C18—C19—C23178 (3)C36—C35—C37—H3966 (3)
H9—C18—C19—C14179 (2)C36—C35—C37—H4059 (3)
H9—C18—C19—C230 (4)H34—C35—C37—H3857 (3)
C19—C18—C17—C164 (5)H34—C35—C37—H39175 (2)
C19—C18—C17—H8176 (3)H34—C35—C37—H4060 (3)
H9—C18—C17—C16178 (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
C23H27CoN2O3β = 96.520 (3)°
Mr = 438.41V = 2138.1 (2) Å3
Monoclinic, P21/nZ = 4
Hall symbol: -p 2ynSynchrotron radiation, λ = 0.65051 Å
a = 16.6701 (6) ŵ = 0.8 mm1
b = 9.4170 (4) ÅT = 293 K
c = 13.7088 (7) Åcylinder, ? × 0.7 mm mm
Data collection top
ESRF BM16
diffractometer
Data collection mode: transmission
Radiation source: synchrotronScan method: continuous
Specimen mounting: capillary2θmin = 0.010°, 2θmax = 30.00°, 2θstep = 0.005°
Refinement top
Rp = 8.5142 parameters
Rwp = 11.4Calculated and kept fixed
Rexp = ?
χ2 = 57.760Background function: polynomal
5999 data pointsPreferred orientation correction: 'Ahtee and Jarvinen'
Profile function: split-type pseudo-Voigt
Crystal data top
C23H27CoN2O3V = 2138.1 (2) Å3
Mr = 438.41Z = 4
Monoclinic, P21/nSynchrotron radiation, λ = 0.65051 Å
a = 16.6701 (6) ŵ = 0.8 mm1
b = 9.4170 (4) ÅT = 293 K
c = 13.7088 (7) Åcylinder, ? × 0.7 mm mm
β = 96.520 (3)°
Data collection top
ESRF BM16
diffractometer
Scan method: continuous
Specimen mounting: capillary2θmin = 0.010°, 2θmax = 30.00°, 2θstep = 0.005°
Data collection mode: transmission
Refinement top
Rp = 8.55999 data points
Rwp = 11.4142 parameters
Rexp = ?Calculated and kept fixed
χ2 = 57.760
Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Å2) top
xyzBiso*/Beq
Co0.5091 (7)0.6512 (9)0.4239 (9)*
O10.531 (3)0.551 (5)0.315 (3)*
O20.395 (3)0.637 (5)0.377 (4)*
O30.540 (4)0.932 (5)0.193 (3)*
N10.616 (4)0.677 (5)0.475 (4)*
N20.486 (4)0.750 (5)0.542 (5)*
C10.599 (5)0.502 (8)0.294 (5)*
C20.671 (4)0.526 (9)0.353 (5)*
C30.676 (4)0.600 (7)0.448 (5)*
C40.337 (4)0.724 (8)0.415 (5)*
C50.349 (4)0.796 (7)0.504 (5)*
C60.423 (4)0.802 (7)0.561 (5)*
C70.562 (5)0.754 (7)0.615 (5)*
C80.630 (5)0.764 (6)0.562 (5)*
C90.603 (5)0.433 (8)0.203 (6)*
C100.679 (5)0.383 (7)0.177 (5)*
C110.748 (5)0.438 (8)0.238 (7)*
C120.741 (5)0.496 (8)0.325 (5)*
C130.534 (4)0.387 (7)0.138 (4)*
C140.253 (5)0.698 (8)0.377 (5)*
C150.190 (4)0.745 (7)0.424 (5)*
C160.206 (4)0.827 (7)0.511 (5)*
C170.285 (4)0.863 (7)0.543 (5)*
C180.242 (5)0.623 (7)0.278 (6)*
C190.504 (5)0.834 (6)0.343 (5)*
C200.519 (5)0.801 (7)0.240 (4)*
C210.508 (5)0.917 (6)0.097 (5)*
C220.463 (4)0.783 (5)0.076 (5)*
C230.449 (5)0.740 (6)0.179 (5)*
H10.728840.613790.48906*
H20.432760.902140.60771*
H30.557680.844160.65820*
H40.564220.671960.65380*
H50.637250.873130.53487*
H60.682180.744870.60020*
H70.684710.341370.11580*
H80.804890.396370.22219*
H90.796230.518850.37329*
H100.496560.332050.17186*
H110.503020.484930.11774*
H120.535280.344010.07094*
H130.133130.735140.39212*
H140.159920.854220.54692*
H150.296300.906540.61220*
H160.266950.691100.22854*
H170.263020.536300.28082*
H180.181500.620650.24375*
H190.451600.867800.33850*
H200.547970.887920.37344*
H210.572090.731940.23607*
H220.476070.996200.06920*
H230.558180.912100.04944*
H240.409890.796500.03228*
H250.493840.706280.03658*
H260.400260.762730.19330*
H270.454860.622780.17759*
Geometric parameters (Å, º) top
Co—O11.83 (5)C10—C111.43 (11)
Co—N11.86 (6)C11—H81.08 (9)
Co—N21.94 (6)C11—C121.34 (12)
Co—O21.95 (5)C12—H91.09 (8)
Co—C192.05 (6)C13—H100.97 (7)
O1—C11.30 (9)C13—H121.00 (6)
O2—C41.40 (9)C13—H111.07 (6)
O3—C211.36 (8)C14—C151.37 (11)
O3—C201.45 (8)C14—C181.52 (10)
N1—C31.31 (9)C15—H131.01 (6)
N1—C81.44 (9)C15—C161.42 (9)
N2—C61.22 (10)C16—H140.99 (8)
N2—C71.52 (9)C16—C171.38 (10)
C1—C21.38 (10)C17—H151.03 (7)
C1—C91.42 (11)C18—H170.88 (7)
C2—C121.31 (11)C18—H161.05 (8)
C2—C31.46 (10)C18—H181.07 (8)
C3—H11.00 (6)C19—H190.93 (8)
C4—C51.39 (10)C19—H200.95 (7)
C4—C141.46 (11)C19—C201.49 (9)
C5—C61.39 (9)C20—H211.10 (8)
C5—C171.40 (10)C20—C231.48 (10)
C6—H21.14 (7)C21—H220.97 (7)
C7—H40.94 (7)C21—H231.12 (9)
C7—H31.04 (7)C21—C221.48 (9)
C7—C81.42 (11)C22—H241.01 (7)
C8—H60.98 (7)C22—H251.07 (6)
C8—H51.10 (6)C22—C231.52 (10)
C9—C131.43 (10)C23—H260.88 (8)
C9—C101.44 (11)C23—H271.11 (6)
C10—H70.94 (7)
N1···H11.95 (6)C1···C193.60 (10)
C20···H191.96 (7)C5···C193.61 (11)
N2···H21.96 (6)C6···C163.61 (10)
C8···H41.96 (8)O2···N13.61 (7)
C9···H111.98 (7)C10···C163.61 (10)
O3···H221.99 (5)N1···C203.63 (8)
C9···H102.01 (7)O1···C103.65 (9)
C20···H202.01 (6)C2···C53.65 (10)
C22···H222.02 (5)N2···C13.67 (10)
C22···H262.03 (7)C13···C233.68 (9)
O3···H212.03 (4)C19···C223.68 (9)
O3···H232.03 (5)O2···C153.68 (8)
C8···H32.03 (8)C11···C133.70 (11)
N2···H42.03 (6)C6···C143.70 (10)
C14···H172.03 (7)C2···C63.71 (10)
N1···H62.04 (6)C5···C73.72 (10)
N1···H52.04 (5)C7···C183.73 (10)
C7···H62.04 (8)O3···C123.74 (10)
C20···H262.05 (8)O2···C173.74 (9)
C16···H152.06 (7)N1···C63.75 (10)
C22···H232.07 (7)C2···C83.75 (10)
C14···H132.07 (8)C21···C223.75 (9)
C22···H272.07 (6)O2···C73.76 (8)
C14···H162.07 (7)C2···C133.76 (9)
C11···H72.08 (8)C5···C183.76 (10)
N2···H32.08 (6)C3···C193.77 (9)
C2···H92.08 (7)O1···C63.77 (8)
C15···H142.08 (7)O1···N23.77 (8)
C5···H152.09 (7)C3···C93.79 (10)
C12···H82.09 (8)C9···C203.79 (10)
C7···H52.09 (7)C3···C143.79 (9)
C11···H92.09 (9)Co···N23.80 (5)
C17···H142.09 (7)O2···N13.81 (7)
C9···H72.10 (8)C11···C163.81 (11)
C21···H242.10 (8)C3···C53.82 (9)
C16···H132.11 (7)C2···C203.82 (10)
C23···H242.11 (7)C7···C193.82 (9)
C23···H212.11 (7)C12···C163.82 (10)
C10···H82.12 (7)N2···C33.82 (10)
C20···H272.12 (7)C6···C193.82 (9)
C5···H22.13 (7)C16···C183.83 (10)
C21···H252.15 (6)C9···C233.85 (10)
C2···H12.16 (7)C12···C173.88 (10)
O1···H212.17 (5)C10···C123.88 (11)
C19···H212.17 (7)O2···C83.90 (8)
C9···H122.18 (7)C4···C233.92 (11)
C14···H182.19 (7)C1···C73.92 (11)
C23···H252.19 (7)O2···C13.93 (9)
C20···C212.23 (9)O1···O33.97 (6)
C21···C232.30 (10)C2···C43.97 (10)
C2···C112.31 (12)C13···C153.97 (9)
C3···C122.32 (11)C13···C223.97 (8)
N2···C52.33 (9)C2···C173.97 (10)
N1···C72.33 (10)C1···C53.97 (10)
O1···C92.34 (9)C6···C93.98 (10)
O1···C22.34 (9)O1···C43.99 (9)
C20···C222.35 (9)O1···C224.00 (8)
C1···C122.35 (11)C18···C234.00 (12)
O3···C232.35 (8)C2···C194.00 (10)
C6···C172.36 (10)C9···C164.00 (11)
N2···C82.38 (10)Co···C74.01 (7)
C3···C82.38 (10)C5···C124.01 (10)
C6···C72.39 (10)O1···C114.02 (11)
O3···C192.39 (8)Co···O24.05 (5)
O3···C222.39 (8)N2···C24.06 (10)
C5···C142.41 (10)Co···N14.07 (6)
C2···C92.41 (10)C11···C204.07 (12)
C9···C112.41 (11)C7···C194.09 (9)
C15···C172.41 (9)C3···C104.10 (10)
C14···C162.41 (10)C3···C204.10 (9)
C5···C162.41 (10)N1···C44.11 (9)
C10···C122.42 (10)O1···C84.11 (8)
O2···C142.42 (10)C8···C174.11 (10)
C10···C132.42 (10)Co···C94.11 (8)
C4···C172.43 (10)C3···C64.12 (9)
N1···C22.43 (10)C7···C134.13 (10)
C4···C62.44 (10)C4···C204.15 (11)
Co···H202.443 (9)C6···C154.15 (9)
C1···C102.47 (11)C13···C204.16 (9)
C4···C152.48 (10)C12···C154.17 (9)
O2···C52.48 (9)Co···O14.17 (5)
Co···H192.489 (10)O2···C74.19 (8)
C19···C232.49 (9)C12···C134.19 (10)
C4···C182.50 (10)O3···C64.19 (8)
C1···C32.51 (9)Co···O34.20 (5)
C1···C132.53 (9)C11···C174.21 (11)
C15···C182.54 (10)C3···C154.21 (9)
N1···N22.55 (9)O3···C214.21 (8)
O1···C202.57 (8)O2···C164.21 (9)
O1···O22.64 (8)N2···C194.22 (8)
O2···C192.68 (9)C2···C164.22 (10)
O1···C192.73 (7)C12···C174.23 (10)
O2···C182.74 (9)C2···C104.24 (11)
C1···C112.74 (12)O2···N24.24 (7)
O1···N12.74 (7)C11···C164.24 (11)
C9···C122.76 (10)C3···C104.24 (10)
C14···C172.76 (9)C11···C124.25 (11)
C2···C102.79 (10)O2···C24.26 (9)
O2···N22.79 (8)Co···C144.26 (8)
C5···C152.79 (9)C5···C84.26 (9)
Co···C32.80 (7)C10···C224.26 (9)
Co···C82.81 (7)N2···C34.27 (9)
O1···C232.81 (8)N2···C204.27 (9)
Co···C12.83 (8)C12···C214.27 (12)
Co···C72.83 (7)C17···C184.27 (10)
C4···C162.84 (11)N2···C144.29 (10)
N1···C192.86 (8)C7···C94.29 (11)
Co···C62.87 (7)C9···C224.29 (9)
N2···C42.87 (9)C16···C214.30 (11)
O1···C132.89 (8)C13···C214.31 (9)
O1···C32.89 (8)N2···C94.31 (10)
N2···C192.89 (9)C13···C164.32 (10)
Co···C202.91 (6)C2···C144.32 (10)
Co···C42.94 (7)C6···C124.33 (11)
O2···C62.96 (8)C2···C114.34 (11)
N1···C12.96 (9)C15···C214.34 (11)
C21···C213.07 (9)C9···C224.35 (10)
O2···C233.11 (9)O3···C14.35 (9)
C1···C203.16 (10)O3···C134.35 (8)
Co···C23.19 (8)C3···C114.36 (11)
C4···C193.23 (11)N1···N24.36 (7)
Co···C53.30 (7)N1···C94.36 (9)
O2···C203.33 (9)C13···C134.36 (8)
C13···C223.34 (9)C16···C224.37 (11)
C11···C173.37 (11)C3···C184.38 (10)
C6···C193.44 (10)C9···C174.38 (11)
O1···C73.45 (8)C4···C74.38 (10)
C3···C73.46 (10)C1···C84.40 (10)
C6···C83.46 (11)Co···C34.40 (7)
C19···C213.46 (10)C3···C174.41 (10)
O1···N23.48 (7)Co···C64.41 (6)
Co···C233.49 (7)C1···C224.42 (9)
C8···C183.50 (10)C1···C174.42 (10)
N1···C123.52 (10)C2···C154.43 (9)
C8···C193.52 (10)C13···C164.43 (10)
N2···C173.52 (10)C4···C124.44 (11)
C1···C63.53 (10)C11···C214.44 (12)
O1···C123.53 (10)Co···C124.48 (9)
Co···Co3.564 (14)Co···C84.56 (7)
O3···C113.57 (10)Co···C184.67 (8)
O2···C33.57 (9)Co···C14.68 (8)
C3···C113.58 (11)Co···C174.70 (8)
C1···C233.59 (10)Co···C134.70 (6)
C10···C173.59 (10)Co···C44.76 (7)
C3···C43.60 (10)Co···C24.82 (8)
O1—Co—N196 (3)H9—C12—C2120 (7)
O1—Co—N2178 (2)H9—C12—C11118 (8)
O1—Co—O288 (2)C2—C12—C11121 (7)
O1—Co—C1989 (2)H10—C13—H12108 (6)
N1—Co—N284 (3)H10—C13—H11105 (6)
N1—Co—O2175 (2)H10—C13—C9112 (6)
N1—Co—C1994 (3)H12—C13—H11100 (5)
N2—Co—O292 (2)H12—C13—C9126 (7)
N2—Co—C1993 (2)H11—C13—C9103 (5)
O2—Co—C1984 (3)C15—C14—C4122 (6)
C1—O1—Co129 (5)C15—C14—C18123 (7)
C4—O2—Co121 (4)C4—C14—C18114 (7)
C21—O3—C20105 (5)H13—C15—C14120 (6)
C3—N1—C8120 (6)H13—C15—C16120 (6)
C3—N1—Co123 (4)C14—C15—C16119 (6)
C8—N1—Co116 (5)H14—C16—C17123 (7)
C6—N2—C7121 (6)H14—C16—C15118 (6)
C6—N2—Co129 (5)C17—C16—C15119 (7)
C7—N2—Co109 (5)H15—C17—C16118 (7)
O1—C1—C2122 (7)H15—C17—C5118 (6)
O1—C1—C9119 (6)C16—C17—C5120 (6)
C2—C1—C9119 (7)H17—C18—H16114 (9)
C12—C2—C1122 (7)H17—C18—H18110 (7)
C12—C2—C3114 (6)H17—C18—C14113 (7)
C1—C2—C3124 (7)H16—C18—H1898 (6)
H1—C3—N1114 (6)H16—C18—C14106 (6)
H1—C3—C2121 (7)H18—C18—C14115 (7)
N1—C3—C2123 (6)H19—C19—H20121 (7)
C5—C4—O2125 (6)H19—C19—C20106 (6)
C5—C4—C14116 (7)H19—C19—Co108 (5)
O2—C4—C14116 (6)H20—C19—C20109 (7)
C4—C5—C6123 (7)H20—C19—Co103 (5)
C4—C5—C17121 (6)C20—C19—Co110 (4)
C6—C5—C17116 (6)H21—C20—O3105 (6)
H2—C6—N2113 (6)H21—C20—C23109 (5)
H2—C6—C5114 (6)H21—C20—C19113 (5)
N2—C6—C5127 (7)O3—C20—C23107 (5)
H4—C7—H3110 (7)O3—C20—C19109 (5)
H4—C7—C8111 (7)C23—C20—C19114 (7)
H4—C7—N2110 (6)H22—C21—H23102 (6)
H3—C7—C8110 (6)H22—C21—O3116 (6)
H3—C7—N2107 (6)H22—C21—C22110 (7)
C8—C7—N2109 (6)H23—C21—O3109 (7)
H6—C8—H5103 (6)H23—C21—C22104 (5)
H6—C8—C7115 (7)O3—C21—C22114 (5)
H6—C8—N1113 (6)H24—C22—H25103 (5)
H5—C8—C7111 (6)H24—C22—C21113 (5)
H5—C8—N1105 (6)H24—C22—C23112 (7)
C7—C8—N1109 (6)H25—C22—C21114 (7)
C1—C9—C13125 (7)H25—C22—C23115 (5)
C1—C9—C10119 (6)C21—C22—C23100 (5)
C13—C9—C10115 (6)H26—C23—H27110 (6)
H7—C10—C11122 (8)H26—C23—C20118 (6)
H7—C10—C9122 (7)H26—C23—C22112 (6)
C11—C10—C9114 (7)H27—C23—C20109 (6)
H8—C11—C12119 (8)H27—C23—C22103 (5)
H8—C11—C10115 (7)C20—C23—C22103 (6)
C12—C11—C10122 (8)
O2—Co—O1—C1174 (6)C4—C5—C6—N22 (12)
N1—Co—O1—C18 (6)C4—C5—C6—H2151 (7)
N2—Co—O1—C182 (66)C17—C5—C6—N2179 (7)
C19—Co—O1—C1102 (6)C17—C5—C6—H232 (9)
O1—Co—O2—C4164 (5)C4—C5—C17—C1619 (10)
N1—Co—O2—C47 (32)C4—C5—C17—H15174 (6)
N2—Co—O2—C418 (5)C6—C5—C17—C16159 (6)
C19—Co—O2—C475 (5)C6—C5—C17—H153 (*)
O1—Co—N1—C319 (6)N2—C7—C8—N138 (7)
O1—Co—N1—C8176 (4)N2—C7—C8—H577 (7)
O2—Co—N1—C3176 (27)N2—C7—C8—H6166 (5)
O2—Co—N1—C818 (32)H3—C7—C8—N1155 (5)
N2—Co—N1—C3159 (6)H3—C7—C8—H540 (8)
N2—Co—N1—C87 (4)H3—C7—C8—H677 (7)
C19—Co—N1—C3108 (6)H4—C7—C8—N182 (7)
C19—Co—N1—C886 (5)H4—C7—C8—H5162 (6)
O1—Co—N2—C6103 (64)H4—C7—C8—H646 (9)
O1—Co—N2—C776 (65)C1—C9—C10—C1113 (10)
O2—Co—N2—C612 (6)C1—C9—C10—H7176 (7)
O2—Co—N2—C7167 (4)C13—C9—C10—C11175 (6)
N1—Co—N2—C6166 (6)C13—C9—C10—H712 (11)
N1—Co—N2—C715 (4)C1—C9—C13—H1051 (*)
C19—Co—N2—C672 (6)C1—C9—C13—H1162 (9)
C19—Co—N2—C7108 (4)C1—C9—C13—H12175 (7)
O1—Co—C19—C200 (5)C10—C9—C13—H10120 (7)
O1—Co—C19—H19115 (5)C10—C9—C13—H11127 (6)
O1—Co—C19—H20116 (5)C10—C9—C13—H1214 (10)
O2—Co—C19—C2088 (5)C9—C10—C11—C1217 (11)
O2—Co—C19—H1926 (5)C9—C10—C11—H8176 (7)
O2—Co—C19—H20156 (5)H7—C10—C11—C12179 (7)
N1—Co—C19—C2096 (5)H7—C10—C11—H821 (11)
N1—Co—C19—H19149 (5)C10—C11—C12—C211 (12)
N1—Co—C19—H2020 (5)C10—C11—C12—H9170 (7)
N2—Co—C19—C20180 (5)H8—C11—C12—C2169 (8)
N2—Co—C19—H1965 (5)H8—C11—C12—H912 (12)
N2—Co—C19—H2064 (5)C4—C14—C15—C163 (10)
Co—O1—C1—C23 (11)C4—C14—C15—H13173 (6)
Co—O1—C1—C9177 (5)C18—C14—C15—C16174 (6)
Co—O2—C4—C519 (9)C18—C14—C15—H134 (10)
Co—O2—C4—C14177 (5)C4—C14—C18—H1662 (8)
C21—O3—C20—C19146 (6)C4—C14—C18—H1764 (*)
C21—O3—C20—C2322 (8)C4—C14—C18—H18169 (6)
C21—O3—C20—H2193 (6)C15—C14—C18—H16115 (8)
C20—O3—C21—C222 (9)C15—C14—C18—H17120 (9)
C20—O3—C21—H22131 (8)C15—C14—C18—H188 (*)
C20—O3—C21—H23114 (6)C14—C15—C16—C173 (*)
Co—N1—C3—C224 (9)C14—C15—C16—H14176 (6)
Co—N1—C3—H1170 (5)H13—C15—C16—C17167 (6)
C8—N1—C3—C2170 (6)H13—C15—C16—H1414 (*)
C8—N1—C3—H15 (9)C15—C16—C17—C514 (*)
Co—N1—C8—C728 (6)C15—C16—C17—H15169 (6)
Co—N1—C8—H592 (6)H14—C16—C17—C5166 (6)
Co—N1—C8—H6157 (5)H14—C16—C17—H1510 (11)
C3—N1—C8—C7138 (6)Co—C19—C20—O3163 (5)
C3—N1—C8—H5102 (7)Co—C19—C20—C2378 (6)
C3—N1—C8—H69 (9)Co—C19—C20—H2147 (7)
Co—N2—C6—C54 (11)H19—C19—C20—O381 (7)
Co—N2—C6—H2145 (5)H19—C19—C20—C2338 (7)
C7—N2—C6—C5175 (6)H19—C19—C20—H21163 (6)
C7—N2—C6—H235 (9)H20—C19—C20—O351 (8)
Co—N2—C7—C833 (6)H20—C19—C20—C23170 (5)
Co—N2—C7—H3152 (5)H20—C19—C20—H2165 (7)
Co—N2—C7—H488 (7)O3—C20—C23—C2233 (7)
C6—N2—C7—C8147 (6)O3—C20—C23—H2691 (8)
C6—N2—C7—H328 (9)O3—C20—C23—H27142 (6)
C6—N2—C7—H491 (8)C19—C20—C23—C22153 (5)
O1—C1—C2—C34 (12)C19—C20—C23—H2629 (9)
O1—C1—C2—C12170 (7)C19—C20—C23—H2798 (7)
C9—C1—C2—C3179 (7)H21—C20—C23—C2279 (6)
C9—C1—C2—C125 (12)H21—C20—C23—H26156 (6)
O1—C1—C9—C10178 (7)H21—C20—C23—H2730 (8)
O1—C1—C9—C1312 (11)O3—C21—C22—C2318 (8)
C2—C1—C9—C103 (11)O3—C21—C22—H24136 (7)
C2—C1—C9—C13173 (7)O3—C21—C22—H25106 (7)
C1—C2—C3—N116 (12)H22—C21—C22—C23115 (7)
C1—C2—C3—H1179 (7)H22—C21—C22—H244 (*)
C12—C2—C3—N1158 (7)H22—C21—C22—H25122 (7)
C12—C2—C3—H16 (11)H23—C21—C22—C23137 (6)
C1—C2—C12—C111 (13)H23—C21—C22—H24105 (7)
C1—C2—C12—H9178 (7)H23—C21—C22—H2513 (8)
C3—C2—C12—C11176 (7)C21—C22—C23—C2030 (7)
C3—C2—C12—H94 (11)C21—C22—C23—H2699 (7)
O2—C4—C5—C67 (11)C21—C22—C23—H27143 (6)
O2—C4—C5—C17170 (7)H24—C22—C23—C20149 (5)
C14—C4—C5—C6165 (7)H24—C22—C23—H2621 (7)
C14—C4—C5—C1712 (*)H24—C22—C23—H2797 (6)
O2—C4—C14—C15162 (6)H25—C22—C23—C2093 (6)
O2—C4—C14—C1821 (9)H25—C22—C23—H26138 (6)
C5—C4—C14—C152 (10)H25—C22—C23—H2720 (8)
C5—C4—C14—C18178 (6)

Experimental details

(Compound_1)(Compound_2)
Crystal data
Chemical formulaC37H40ClN2ORhC23H27CoN2O3
Mr667.07438.41
Crystal system, space groupOrthorhombic, PbcaMonoclinic, P21/n
Temperature (K)293293
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, 9090, 96.520 (3), 90
V3)6888 (2)2138.1 (2)
Z84
Radiation typeSynchrotron, λ = 0.65296 ÅSynchrotron, λ = 0.65051 Å
µ (mm1)0.60.8
Specimen shape, size (mm)Cylinder, ? × 0.7 mmCylinder, ? × 0.7 mm
Data collection
Data collection methodESRF BM16ESRF BM16
Specimen mountingCapillaryCapillary
Data collection modeTransmissionTransmission
Scan methodContinuousContinuous
2θ values (°)2θmin = 2.500 2θmax = 25.00 2θstep = 0.0052θmin = 0.010 2θmax = 30.00 2θstep = 0.005
Refinement
R factors and goodness of fitRp = 8.4, Rwp = 11.1, Rexp = ?, χ2 = 6.250Rp = 8.5, Rwp = 11.4, Rexp = ?, χ2 = 57.760
No. of data points45005999
No. of parameters175142
No. of restraints38?
H-atom treatmentCalculated and kept fixedCalculated and kept fixed

Computer programs: UnitCell, MRIA, CHEMDRAW and PLATON.

 

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