Polymeric [dihydrobis(pyrazol-1-yl)borato]potassium(I) and three dihydrobis(pyrazol-1-yl)borate–magnesium(I) compounds obtained by disproportionation of the Grignard reagent

Reaction of the Grignard reagent with polydentate nitro­gen-donor ligands yields new species with rare magnesium coordination and possible catalytic activity. In the first of the title compounds, poly[[μ₄-dihydrobis(pyrazol-1-yl)borato-κ²N,N′]potassium(I)], [K(C₆H₈BN₄)]_n, (I), polymeric chains form a two-dimensional network in the [100] plane. Each potassium ion is coordinated by four N atoms of pyrazolyl ligands, while weak (μ-BH)...K⁺ inter­actions additionally stabilize the structure. The K and B atoms both lie on a mirror plane. In three new structures obtained by disproportionation of the Grignard reagent, each Mg atom is bound to a κ²N,N′-type ligand, forming the basal plane, and tetra­hydro­furan mol­ecules occupy the axial positions. Di-μ-chlorido-bis­[dihydrido­bis(pyrazol-1-yl)borato]tris­(tetra­hydro­furan)­dimagnesium(II), [Mg₂(C₆H₈BN₄)₂Cl₂(C₄H₈O)₃], (II), adopts a dimeric structure with μ-Cl—Mg inter­actions. One of the Mg atoms has an octa­hedral coordination, while the other has a distorted square-pyramidal environment. However, in the bis-chelate compounds bis­[dihydridobis(pyrazol-1-yl)borato-κ²N,N′](tetra­hydro­furan-κO)magnesium(II), [Mg(C₆H₈BN₄)₂(C₄H₈O)], (III), and bis­[dihydridobis(pyrazol-1-yl)borato-κ²N,N′]bis­(tetra­hydro­furan-κO)magnesium(II), [Mg(C₆H₈BN₄)₂(C₄H₈O)₂], (IV), the Mg atoms have square-pyramidal and octa­hedral environments, respectively. The Mg atom in (IV) lies on an inversion centre.

S1. Comment

The geometric characteristics of dihydrobis(pyrazol-1-yl)borate ligands are very similar to β-diketonate ions, though Cp or Cp* ligands are comparable to hydrotris(pyrazol-1-yl)borate ligands, according to Trofimenko (1993). Although pyrazol ligands have been considered widely, their solid-state structures have not been well studied. There is a lack of structural information on dihydrobis(pyrazol-1-yl)borate and hydrotris(1-pyrazoly)borate ligands with a Cp behaviour. Dias et al. (1995) have reported an interaction of σ-bonding type between potassium ions and highly fluorinated bis(pyrazol-1-yl)borate ligands, while (µ-BH)···K interactions have been observed only for dihydrobis(pyrazol-1-yl)borate ligands. Hu & Gorun (2001), however, have reported that hydrotris(pyrazol-1-yl)borate ligands may function not only as σ-donors but also as Cp-like π-donors.

The search for new species with catalytic activity has led to increased attention being paid to studies of reactivity between Grignard reagents and polydentate nitrogen-donor ligands. Reports on this area, dealing with magnesium halides and magnesium alkyls with different solvents, have been published (Ashby & Arnott, 1968), but little information about their chemical and physical properties is available (Gibson et al., 2000; Bailey et al., 2003).

The present paper reports the structure of ligand (I) in its polymeric form, representing the first example with (η⁵-pyrazole)-, k²N,N'- and (µ-BH)-binding modes. Several side products, (II)–(IV), can be obtained by reaction of the corresponding tetrahydrofuran (THF) solution of complex (I) (Trofimenko, 1966, 1993) and a THF solution of MeMgCl at room temperature.

In the polymeric molecular structure of (I) (Fig. 1), each monomer ligand has a butterfly arrangement of three condensed rings: two pyrazole rings and a boat-shaped central BN₄K moiety. The K and B atoms lie on a mirror plane. Selected bond lengths are listed in Table 1. The short B—N bond distances in the H₂BN₂ group [1.561 (2) Å] are comparable with similar values for pyrazolyl groups (1.562 Å) retrieved from the Cambridge Structural Database (Version of May 2005; Allen, 2002). The acute dihedral angle of 58.78 (16)° (at atom B1) suggests a deeper boat conformation than in similar pyrazabole complexes [35.5 (1) and 33.4 (3)°; Hanecker et al., 1985]. In (I), the (η⁵-pyrazole)—K⁺ distances range from 3.025 (2) to 3.473 (2) Å [with a K⁺···centroid distance of 3.035 (2) Å]. Comparison of the (η⁵-pyrazole)—K⁺ contacts in highly fluorinated bis(pyrazol-1-yl)borate ligands [3.355 (2) Å] and (η⁵-indol)—K⁺ contacts [3.640 (2) Å] (Hu & Gorun, 2001; Dunbar, 1998; Dias & Gorden, 1996) with the (η⁵-pyrazole)—K⁺ distances in (I) suggests that there is a strong π bond with the potassium ion in the latter. In addition, the (η⁵-pyrazolecentroid)···K⁺ distances are longer than the corresponding Cp···K interactions (2.699 Å; Forbes et al., 2002). The pyrazol rings in (I) are located on opposite sides of the K atom, with a corresponding angle between the ring centroids of 92.2 (2)°. The σ-N bonding interactions with the potassium ion (the average K—N bond distance is 2.787 Å) are similar to those found in {[HB{3,5-(CF₃)₂Pz}₃]K(DMAC)}₂ [2.885 (7) Å] and {[HB{3-(CF₃),5-(CH₃)Pz}₃]K(DMAC)}₂ [2.827 (4) Å] (Dias & Gorden, 1996). The (µ-BH)···K contacts (2.88 Å) are shorter than π interactions and can be described as s-block agostic interactions (a donor–acceptor interaction type), providing an extra stability to the polymeric complex. The intra-chain K···K(x, y - 1, z) separation is equal to the b unit-cell dimension, i.e. 5.843 (3) Å, while the inter-chain separation is equal to half of the a unit-cell dimension [8.584 (3) Å]. Several Csp²—H···π interactions (average distance 2.88 Å) are strong enough to direct the crystal packing through inter-polymeric chain interactions between equivalent planes ([100] and [200]; Fig. 2).

The formation of the by-product complexes (II)–(IV) is explained by a disproportionation of the Grignard reagent known as the Schlenk equilibrium. Complex (II) suggests solvation and association, by which MgCl₂ is also formed in solution, and associations by µ-bridging halide atoms predominate. In addition, in complexes (III) and (IV) a large solvent effect is present during the reaction, especially when a strong donor solvent such as THF is used. In general, in complexes (II)–(IV), the ligand (I) coordinates in a κ²N,N' fashion, with boat-shaped central BN₄Mg units. The B—N bond distances in the H₂BN₂ group for compounds (II)–(IV) (average 1.551 Å) are not significantly different from those in pyrazolyl groups (average 1.562 Å; Allen, 2002). The average Mg—N bond distances for complexes (II) and (III) (2.138 Å) are shorter than the average distance for complex (IV) (2.186 Å). All these Mg—N bond distances are typical σ-bonding distances of similar magnesium complexes (Takahashi et al., 1998; Malbosc et al., 1999; Viebrock & Weiss, 1994; Bailey et al., 2000, 2003).

In the asymmetric molecular structure (II) (Fig. 3), two Mg atoms are bridged by two Cl atoms, forming a square Mg₂Cl₂ core in which the Mg—Cl—Mg angles are 94.05 (3) and 94.55 (3)°, while the Cl—Mg—Cl angles are 84.08 (3) and 85.99 (3)°. An octahedral environment is observed for atom Mg1, while a rare distorted square-pyramidal environment is adopted by atom Mg2. The boat conformation of the ring containing atom Mg1 is characterized by dihedral angles at atoms B1 and Mg1 of 46.48 (17) and 13.92 (15)°, respectively, which results in a boat slightly flatter than that in (I). In the case of the six-coordinated atom Mg1, both disordered THF molecules are in the axial positions, with Mg1—O1 and Mg1—O2 bond distances of 2.0920 (15) and 2.1477 (15) Å, respectively. It should be noted that the Mg1—O1 and Mg1—O2 bonds are both almost perpendicular to the Cl1/Cl2/N1/N3 plane [with angles of 93.07 (4) and 87.49 (4)°, respectively]. The boat conformation of the Mg2-containing ring is characterized by dihedral angles at atoms B2 and Mg2 of 47.59 (15) and 27.80 (16)°, respectively. In addition, the distorted square-pyramidal environment of atom Mg2 involves a rather short Mg2—O3 bond distance [2.0201 (15) Å], with atom Mg2 atom lying 0.40 (3) Å out of the N5/N7/Cl1/Cl2 plane. Finally, two chlorine atoms bridge Mg atoms, forming a square Mg₂Cl₂ core, where Mg—Cl—Mg angles are 94.05 (3) and 94.55 (3)°, while the Cl—Mg—Cl angles are 84.08 (3) and 85.99 (3)°, respectively. Selected bond lengths and angles are listed in Table 2.

The X-ray structure of compound (III) (Fig. 4), reveals a bis-chelate complex, with a square-pyramidal geometry around the two Mg atoms in the asymmetric unit. The short Mg—O interactions [2.0397 (16) and 2.0233 (17) Å] agree well with previously reported values (Takahashi et al., 1998; Malbosc et al., 1999; Viebrock & Weiss, 1994; Bailey et al., 2000, 2003). Selected bond lengths and angles for (III) are listed in Table 3. The boat conformation of the B1-containing ring is characterized by dihedral angles at atoms B1 and Mg1 of 48.43 (15) and 23.52 (17)°, respectively. However, a more pronounced boat conformation, with dihedral angles of 53.81 (15) and 41.29 (16)° for atoms B2 and Mg1, is observed for the other chelate ring; this conformation could be related to a weak pseudoaxial B—H···Mg interaction (distance 2.69 Å) (Takahashi et al., 1998; Malbosc et al., 1999). Moreover, the observed strong Mg—O interaction induces the Mg atom to be located 0.39 (3) Å out of the N1/N3/N5/N7 plane.

The X-ray crystal structure of (IV) (Fig. 5), one the other hand, also reveals a bis-chelate complex, but with an octahedral environment for the Mg atoms. The two Mg atoms in the asymmetric unit are located on inversion centers, while the average σ-N—Mg bond distance (2.186 Å) is a little longer than the corresponding distance in complex (III). The axial positions are occupied by two disordered THF molecules, with Mg—O bond lengths [2.1735 (10) and 2.1989 (10) Å] longer than those in complex (III). As a result, the boat conformation in complex (IV) is flatter than that in complex (III), with dihedral angles at atoms B2 and Mg1 of 45.60 (17) and 18.44 (18)°, respectively. Selected bond lengths and angles for (IV) are listed in Table 4, and more information about the dihedral angles for all complexes is given in Table 5.

S2. Experimental

All solvents and reagents were used as received from Aldrich and Fisher. The starting material (I) was prepared as described by Trofimenko (1966). Colourless needle-shaped crystals were grown from a concentrated THF solution at room temperature. A suitable crystal was selected from the resulting batch. A solution of (I) (1.000 g, 5.358 mmol) in THF (5 ml) was treated with MeMgCl (1.8 ml, 3.0 M in THF, 5.358 mmol) at room temperature. After three hours, the solvent and volatile components were removed under vacuum, diethyl ether was added (10 ml) and the suspension was filtered under nitrogen atmosphere through Ceolite 521. The final solution was concentrated (5 ml) and left at room temperature for 2 d to give colourless block-shaped [plate according to CIF] crystals of (II) (1.69 mmol, yield 63%). Colourless block-shaped crystals for complexes (III) and (IV) were obtained in a similar manner as (II), but the reaction time was 10 and 24 h, respectively [(III): 1.82 mmol, yield 68%; (IV): 1.91 mmol, yield 72%]. Suitable crystals were selected from the resulting batch. Owing to the air- and moisture-sensitive nature of the final product, reliable microanalysis was not possible.

S3. Refinement

The H atoms were included in the refinement at calculated positions, in the riding-model approximation, with C—H distances of 0.93–0.99 Å and B—H distances of 1.11 Å. The U_iso(H) values were set equal to 1.2U_eq(C,B). The refinement of positional disorder in complexes (II) and (IV) was resolved with two components and the use of similarity restraints. The THF molecules in complex (II) are disordered, and the pairs of atoms C15 and C15A, C18 and C18A, and C23 and C23A have occupancy ratios of 80:20, 79:21 and 86:14% occupancies, respectively. One disordered THF molecule is also found in the asymmetric unit of complex (IV). Atoms C7, C7A, C8, C8A, C9 and C9A have an coccupancy ratio of 82:18%.

Computing details

For all compounds, data collection: SMART (Bruker, 2001); cell refinement: SAINT (Bruker, 2002); data reduction: SAINT (Bruker, 2002); program(s) used to solve structure: SHELXS97 (Sheldrick, 2008); program(s) used to refine structure: SHELXL97 (Sheldrick, 2008). Molecular graphics: SHELXTL (Version 5.03; Sheldrick, 2008) and WinGX2003 (Farrugia, 1999) for (I); SHELXTL (Version 5.03; Sheldrick, 2008) for (II), (III), (IV). For all compounds, software used to prepare material for publication: SHELXL97 (Sheldrick, 2008).

Figures

	Fig. 1. The asymmetric unit of (I) and some symmetry-related atoms. Displacement ellipsoids are drawn at the 50% probability level. [Symmetry codes: (i) -x + 1, y, z; (ii) -x + 1, -y + 1, z + 1/2; (iii) -x + 1, -y, z + 1/2; (iv) x, y - 1, z.] DON'T MATCH TABLE
	Fig. 2. Part of the crystal packing of (I), showing Csp^2—H···π interactions between chains. [Symmetry codes: (i) -x + 1, y, z; (ii) -x + 1, -y + 1, z + 1/2; (v) x, -y + 1, z + 1/2; (vi) -x + 1/2, y - 1/2, z; (vii) -x + 1/2, -y + 1/2, z + 1/2; (viii) x + 1/2, y - 1/2, z; (ix) x + 1/2, -y + 1/2, z + 1/2.]
	Fig. 3. The major disorder component of (II), with displacement ellipsoids shown at the 50% probability level.
	Fig. 4. The molecular structure of (III). Displacement ellipsoids are drawn at the 50% probability level. The dashed line indicates a pseudoaxial B—H···Mg interaction.
	Fig. 5. The major disorder component of (IV), with displacement ellipsoids shown at the 50% probability level. [Symmetry code: (i) -x, -y + 1, -z + 1.]

(I) Poly[[µ₄-dihydrobis(pyrazol-1-yl)borato-κ²N,N']potassium(I)]

Crystal data

[K(C6H8BN4)]	Dx = 1.408 Mg m^−3
Mr = 186.07	Melting point: 444 K
Orthorhombic, Cmc21	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: C 2c -2	Cell parameters from 409 reflections
a = 17.167 (3) Å	θ = 2.5–27.5°
b = 5.843 (4) Å	µ = 0.55 mm^−1
c = 8.754 (3) Å	T = 150 K
V = 878.1 (7) Å^3	Needle, colourless
Z = 4	0.32 × 0.06 × 0.06 mm
F(000) = 384

Data collection

Bruker SMART APEX CCD area-detector diffractometer	926 independent reflections
Radiation source: normal-focus sealed tube	893 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.020
ϕ and ω scans	θmax = 27.5°, θmin = 2.4°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −22→19
Tmin = 0.958, Tmax = 0.965	k = −6→7
2664 measured reflections	l = −8→11

Refinement

Refinement on F^2	Secondary atom site location: difference Fourier map
Least-squares matrix: full	Hydrogen site location: inferred from neighbouring sites
R[F^2 > 2σ(F^2)] = 0.024	H-atom parameters constrained
wR(F^2) = 0.056	w = 1/[σ^2(Fo^2) + (0.0354P)^2] where P = (Fo^2 + 2Fc^2)/3
S = 1.00	(Δ/σ)max < 0.001
926 reflections	Δρmax = 0.27 e Å^−3
64 parameters	Δρmin = −0.17 e Å^−3
1 restraint	Absolute structure: Flack (1983), 373 Friedel pairs
Primary atom site location: structure-invariant direct methods	Absolute structure parameter: 0.10 (5)

Special details

Experimental. 1H and 13C were obtained using a Bruker AC300 spectrometer at room temperature.

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Reflections after merge 555 R(merge) 0.014939 (FRIEDEL MERGED) Reflections after merge 928 R(merge) 0.020369 (FRIEDEL NOT MERGED)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
K1	0.5000	0.53814 (7)	0.33974 (5)	0.02430 (13)
N1	0.59509 (8)	0.6783 (2)	0.62593 (17)	0.0260 (3)
N2	0.57477 (8)	0.8776 (2)	0.55564 (16)	0.0211 (3)
B1	0.5000	1.0107 (6)	0.6045 (4)	0.0223 (5)
H111	0.5000	1.0344	0.7303	0.027*
H112	0.5000	1.1826	0.5505	0.027*
C1	0.65960 (10)	0.6074 (3)	0.5547 (2)	0.0287 (4)
H1	0.6866	0.4744	0.5794	0.034*
C2	0.68114 (10)	0.7569 (3)	0.4394 (2)	0.0287 (4)
H2	0.7234	0.7444	0.3735	0.034*
C3	0.62618 (10)	0.9279 (3)	0.4439 (2)	0.0253 (4)
H3	0.6247	1.0559	0.3809	0.030*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
K1	0.0313 (2)	0.0222 (2)	0.0194 (2)	0.000	0.000	−0.0023 (3)
N1	0.0294 (7)	0.0230 (7)	0.0258 (8)	0.0031 (6)	0.0001 (6)	0.0027 (6)
N2	0.0227 (6)	0.0213 (7)	0.0192 (7)	−0.0010 (5)	−0.0016 (5)	0.0004 (6)
B1	0.0249 (11)	0.0190 (12)	0.0229 (15)	0.000	0.000	−0.0035 (10)
C1	0.0255 (8)	0.0284 (9)	0.0324 (10)	0.0044 (7)	−0.0023 (7)	−0.0012 (8)
C2	0.0207 (8)	0.0388 (10)	0.0267 (9)	−0.0008 (7)	0.0024 (7)	−0.0041 (8)
C3	0.0226 (8)	0.0297 (9)	0.0236 (9)	−0.0060 (6)	−0.0013 (7)	0.0026 (7)

Geometric parameters (Å, º)

K1—N1^i	2.7870 (15)	N2—C3	1.350 (2)
K1—N1^ii	2.7870 (15)	N2—B1	1.561 (2)
K1—N2	3.0252 (14)	B1—H111	1.1100
K1—N1	3.1003 (15)	B1—H112	1.1100
K1—C1	3.3481 (18)	C1—C2	1.385 (3)
K1—C2	3.4734 (18)	C1—H1	0.9300
K1—C3	3.2721 (17)	C2—C3	1.375 (3)
N1—C1	1.337 (2)	C2—H2	0.9300
N1—N2	1.3621 (18)	C3—H3	0.9300
K1···H111^iii	2.6700	K1···H111^v	2.6700
K1···H112^iii	3.0100	K1···H112^v	3.0100
K1···H112^iv	2.7800	C2···H1^vi	2.8800
K1···H111^i	3.4800	H1···C2^vii	2.8800
N1^i—K1—N1^ii	71.71 (6)	B1^iii—K1—C1^viii	104.52 (5)
N1^i—K1—N2	164.91 (4)	C1—K1—C1^viii	109.83 (7)
N1^ii—K1—N2	117.94 (4)	N1^i—K1—C2	149.31 (4)
N1^i—K1—N2^viii	117.94 (4)	N1^ii—K1—C2	79.12 (4)
N1^ii—K1—N2^viii	164.91 (4)	N2—K1—C2	38.93 (4)
N2—K1—N2^viii	50.21 (5)	N2^viii—K1—C2	88.96 (4)
N1^i—K1—N1	166.16 (4)	N1—K1—C2	39.51 (4)
N1^ii—K1—N1	110.74 (4)	N1^viii—K1—C2	99.86 (4)
N2—K1—N1	25.66 (3)	C3—K1—C2	23.27 (4)
N2^viii—K1—N1	62.96 (4)	C3^viii—K1—C2	105.47 (4)
N1^i—K1—N1^viii	110.74 (4)	B1^iii—K1—C2	82.22 (4)
N1^ii—K1—N1^viii	166.16 (4)	C1—K1—C2	23.34 (4)
N2—K1—N1^viii	62.96 (4)	C1^viii—K1—C2	123.17 (5)
N2^viii—K1—N1^viii	25.66 (3)	C1—N1—N2	105.45 (14)
N1—K1—N1^viii	63.54 (5)	C1—N1—K1^ix	131.13 (11)
N1^i—K1—C3	152.95 (5)	N2—N1—K1^ix	122.76 (9)
N1^ii—K1—C3	96.61 (4)	C1—N1—K1	88.69 (11)
N2—K1—C3	24.35 (4)	N2—N1—K1	74.09 (8)
N2^viii—K1—C3	69.55 (4)	K1^ix—N1—K1	96.57 (4)
N1—K1—C3	40.76 (4)	C3—N2—N1	110.24 (13)
N1^viii—K1—C3	86.54 (4)	C3—N2—B1	128.89 (19)
N1^i—K1—C3^viii	96.61 (4)	N1—N2—B1	120.85 (18)
N1^ii—K1—C3^viii	152.95 (5)	C3—N2—K1	88.12 (10)
N2—K1—C3^viii	69.55 (4)	N1—N2—K1	80.25 (8)
N2^viii—K1—C3^viii	24.35 (4)	B1—N2—K1	98.58 (12)
N1—K1—C3^viii	86.54 (4)	N2^viii—B1—N2	110.6 (2)
N1^viii—K1—C3^viii	40.76 (4)	N2^viii—B1—K1^x	124.17 (11)
C3—K1—C3^viii	82.90 (6)	N2—B1—K1^x	124.17 (12)
N1^i—K1—B1^iii	86.80 (6)	N2^viii—B1—H111	109.5
N1^ii—K1—B1^iii	86.80 (6)	N2—B1—H111	109.5
N2—K1—B1^iii	82.42 (7)	N2^viii—B1—H112	109.5
N2^viii—K1—B1^iii	82.42 (7)	N2—B1—H112	109.5
N1—K1—B1^iii	106.82 (6)	K1^x—B1—H112	63.2
N1^viii—K1—B1^iii	106.82 (6)	H111—B1—H112	108.1
C3—K1—B1^iii	67.86 (6)	N1—C1—C2	111.45 (16)
C3^viii—K1—B1^iii	67.86 (6)	N1—C1—K1	67.78 (10)
N1^i—K1—C1	155.71 (4)	C2—C1—K1	83.41 (11)
N1^ii—K1—C1	87.30 (4)	N1—C1—H1	124.3
N2—K1—C1	38.97 (4)	C2—C1—H1	124.3
N2^viii—K1—C1	85.24 (4)	K1—C1—H1	115.9
N1—K1—C1	23.53 (4)	C3—C2—C1	104.71 (16)
N1^viii—K1—C1	86.84 (4)	C3—C2—K1	70.12 (10)
C3—K1—C1	38.53 (5)	C1—C2—K1	73.25 (10)
C3^viii—K1—C1	107.52 (4)	C3—C2—H2	127.6
B1^iii—K1—C1	104.52 (5)	C1—C2—H2	127.6
N1^i—K1—C1^viii	87.30 (4)	K1—C2—H2	121.0
N1^ii—K1—C1^viii	155.71 (4)	N2—C3—C2	108.15 (15)
N2—K1—C1^viii	85.24 (4)	N2—C3—K1	67.52 (8)
N2^viii—K1—C1^viii	38.97 (4)	C2—C3—K1	86.61 (10)
N1—K1—C1^viii	86.84 (4)	N2—C3—H3	125.9
N1^viii—K1—C1^viii	23.53 (4)	C2—C3—H3	125.9
C3—K1—C1^viii	107.52 (4)	K1—C3—H3	112.1
C3^viii—K1—C1^viii	38.53 (5)
N1^i—K1—N1—C1	102.87 (15)	N2—N1—C1—C2	−0.17 (19)
N1^ii—K1—N1—C1	5.16 (10)	K1^ix—N1—C1—C2	170.50 (12)
N2—K1—N1—C1	−106.47 (13)	K1—N1—C1—C2	72.92 (14)
N2^viii—K1—N1—C1	−159.82 (11)	N2—N1—C1—K1	−73.09 (9)
N1^viii—K1—N1—C1	171.39 (9)	K1^ix—N1—C1—K1	97.58 (12)
C3—K1—N1—C1	−70.31 (11)	N1^i—K1—C1—N1	−145.45 (10)
C3^viii—K1—N1—C1	−153.45 (10)	N1^ii—K1—C1—N1	−175.17 (9)
B1^iii—K1—N1—C1	−87.83 (10)	N2—K1—C1—N1	41.32 (9)
C1^viii—K1—N1—C1	167.95 (13)	N2^viii—K1—C1—N1	17.96 (10)
C2—K1—N1—C1	−33.90 (10)	N1^viii—K1—C1—N1	−7.72 (8)
N1^i—K1—N1—N2	−150.66 (11)	C3—K1—C1—N1	80.69 (11)
N1^ii—K1—N1—N2	111.63 (7)	C3^viii—K1—C1—N1	27.89 (11)
N2^viii—K1—N1—N2	−53.35 (8)	B1^iii—K1—C1—N1	98.84 (11)
N1^viii—K1—N1—N2	−82.14 (8)	C1^viii—K1—C1—N1	−12.80 (13)
C3—K1—N1—N2	36.16 (8)	C2—K1—C1—N1	116.41 (15)
C3^viii—K1—N1—N2	−46.98 (9)	N1^i—K1—C1—C2	98.14 (14)
B1^iii—K1—N1—N2	18.65 (9)	N1^ii—K1—C1—C2	68.42 (10)
C1—K1—N1—N2	106.47 (13)	N2—K1—C1—C2	−75.09 (11)
C1^viii—K1—N1—N2	−85.57 (8)	N2^viii—K1—C1—C2	−98.45 (11)
C2—K1—N1—N2	72.57 (9)	N1—K1—C1—C2	−116.41 (15)
N1^i—K1—N1—K1^ix	−28.41 (10)	N1^viii—K1—C1—C2	−124.13 (10)
N1^ii—K1—N1—K1^ix	−126.12 (6)	C3—K1—C1—C2	−35.72 (10)
N2—K1—N1—K1^ix	122.25 (9)	C3^viii—K1—C1—C2	−88.51 (11)
N2^viii—K1—N1—K1^ix	68.90 (4)	B1^iii—K1—C1—C2	−17.57 (12)
N1^viii—K1—N1—K1^ix	40.11 (4)	C1^viii—K1—C1—C2	−129.21 (9)
C3—K1—N1—K1^ix	158.41 (8)	N1—C1—C2—C3	0.5 (2)
C3^viii—K1—N1—K1^ix	75.27 (4)	K1—C1—C2—C3	63.50 (13)
B1^iii—K1—N1—K1^ix	140.90 (5)	N1—C1—C2—K1	−62.98 (13)
C1—K1—N1—K1^ix	−131.28 (11)	N1^i—K1—C2—C3	119.92 (12)
C1^viii—K1—N1—K1^ix	36.68 (4)	N1^ii—K1—C2—C3	138.06 (12)
C2—K1—N1—K1^ix	−165.17 (8)	N2—K1—C2—C3	−37.71 (10)
C1—N1—N2—C3	−0.27 (17)	N2^viii—K1—C2—C3	−32.65 (11)
K1^ix—N1—N2—C3	−171.93 (11)	N1—K1—C2—C3	−78.81 (12)
K1—N1—N2—C3	−84.33 (11)	N1^viii—K1—C2—C3	−55.98 (12)
C1—N1—N2—B1	178.29 (18)	C3^viii—K1—C2—C3	−14.54 (10)
K1^ix—N1—N2—B1	6.6 (2)	B1^iii—K1—C2—C3	49.84 (13)
K1—N1—N2—B1	94.22 (16)	C1—K1—C2—C3	−113.01 (16)
C1—N1—N2—K1	84.06 (12)	C1^viii—K1—C2—C3	−52.46 (13)
K1^ix—N1—N2—K1	−87.59 (8)	N1^i—K1—C2—C1	−127.08 (11)
N1^i—K1—N2—C3	−95.86 (18)	N1^ii—K1—C2—C1	−108.93 (11)
N1^ii—K1—N2—C3	31.17 (11)	N2—K1—C2—C1	75.30 (11)
N2^viii—K1—N2—C3	−137.54 (9)	N2^viii—K1—C2—C1	80.36 (11)
N1—K1—N2—C3	110.90 (13)	N1—K1—C2—C1	34.19 (9)
N1^viii—K1—N2—C3	−164.42 (10)	N1^viii—K1—C2—C1	57.03 (11)
C3^viii—K1—N2—C3	−120.25 (12)	C3—K1—C2—C1	113.01 (16)
B1^iii—K1—N2—C3	−51.11 (10)	C3^viii—K1—C2—C1	98.47 (11)
C1—K1—N2—C3	73.41 (11)	B1^iii—K1—C2—C1	162.85 (12)
C1^viii—K1—N2—C3	−156.48 (10)	C1^viii—K1—C2—C1	60.55 (11)
C2—K1—N2—C3	35.87 (10)	N1—N2—C3—C2	0.61 (19)
N1^i—K1—N2—N1	153.24 (16)	B1—N2—C3—C2	−177.80 (19)
N1^ii—K1—N2—N1	−79.74 (8)	K1—N2—C3—C2	−78.29 (13)
N2^viii—K1—N2—N1	111.56 (8)	N1—N2—C3—K1	78.89 (10)
N1^viii—K1—N2—N1	84.68 (9)	B1—N2—C3—K1	−99.52 (19)
C3—K1—N2—N1	−110.90 (13)	C1—C2—C3—N2	−0.67 (19)
C3^viii—K1—N2—N1	128.84 (9)	K1—C2—C3—N2	65.01 (11)
B1^iii—K1—N2—N1	−162.02 (9)	C1—C2—C3—K1	−65.68 (13)
C1—K1—N2—N1	−37.49 (8)	N1^i—K1—C3—N2	145.29 (10)
C1^viii—K1—N2—N1	92.62 (9)	N1^ii—K1—C3—N2	−152.60 (10)
C2—K1—N2—N1	−75.03 (9)	N2^viii—K1—C3—N2	33.62 (8)
N1^i—K1—N2—B1	33.2 (3)	N1—K1—C3—N2	−38.29 (9)
N1^ii—K1—N2—B1	160.24 (15)	N1^viii—K1—C3—N2	13.87 (9)
N2^viii—K1—N2—B1	−8.46 (16)	C3^viii—K1—C3—N2	54.65 (11)
N1—K1—N2—B1	−120.02 (18)	B1^iii—K1—C3—N2	123.59 (11)
N1^viii—K1—N2—B1	−35.34 (15)	C1—K1—C3—N2	−75.40 (11)
C3—K1—N2—B1	129.08 (19)	C1^viii—K1—C3—N2	24.65 (10)
C3^viii—K1—N2—B1	8.83 (16)	C2—K1—C3—N2	−111.24 (16)
B1^iii—K1—N2—B1	77.97 (13)	N1^i—K1—C3—C2	−103.47 (13)
C1—K1—N2—B1	−157.51 (17)	N1^ii—K1—C3—C2	−41.36 (11)
C1^viii—K1—N2—B1	−27.40 (16)	N2—K1—C3—C2	111.24 (16)
C2—K1—N2—B1	164.95 (18)	N2^viii—K1—C3—C2	144.86 (12)
C3—N2—B1—N2^viii	108.1 (2)	N1—K1—C3—C2	72.95 (11)
N1—N2—B1—N2^viii	−70.2 (3)	N1^viii—K1—C3—C2	125.11 (11)
K1—N2—B1—N2^viii	13.5 (3)	C3^viii—K1—C3—C2	165.89 (9)
C3—N2—B1—K1^x	−83.1 (3)	B1^iii—K1—C3—C2	−125.17 (13)
N1—N2—B1—K1^x	98.7 (2)	C1—K1—C3—C2	35.84 (10)
K1—N2—B1—K1^x	−177.59 (16)	C1^viii—K1—C3—C2	135.89 (11)

Symmetry codes: (i) −x+1, −y+1, z−1/2; (ii) x, −y+1, z−1/2; (iii) −x+1, −y+2, z−1/2; (iv) x, y−1, z; (v) x, −y+2, z−1/2; (vi) −x+3/2, y+1/2, z; (vii) −x+3/2, y−1/2, z; (viii) −x+1, y, z; (ix) −x+1, −y+1, z+1/2; (x) −x+1, −y+2, z+1/2.

(II) di-µ-chlorido-bis[dihydridobis(pyrazol-1-yl)borato]- 1κ²N,N';2κ²N,N'-tris(tetrahydrofuran)- 1κ²O,2κO-dimagnesium(II)

Crystal data

[Mg2(C6H8BN4)2Cl2(C4H8O)3]	F(000) = 1328
Mr = 629.78	Dx = 1.309 Mg m^−3
Monoclinic, P21/n	Mo Kα radiation, λ = 0.71073 Å
Hall symbol: -P 2yn	Cell parameters from 4830 reflections
a = 15.119 (3) Å	θ = 2.5–27.5°
b = 13.862 (2) Å	µ = 0.28 mm^−1
c = 15.453 (3) Å	T = 150 K
β = 99.319 (3)°	Plate, colourless
V = 3195.9 (10) Å^3	0.48 × 0.32 × 0.18 mm
Z = 4

Data collection

Bruker SMART APEX CCD area-detector diffractometer	8068 independent reflections
Radiation source: normal-focus sealed tube	6406 reflections with I > 2s(I)
Graphite monochromator	Rint = 0.051
ϕ and ω scans	θmax = 28.9°, θmin = 1.8°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −19→20
Tmin = 0.894, Tmax = 0.951	k = −18→18
38733 measured reflections	l = −20→20

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.054	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.133	H-atom parameters constrained
S = 1.08	w = 1/[σ^2(Fo^2) + (0.0756P)^2] where P = (Fo^2 + 2Fc^2)/3
7868 reflections	(Δ/σ)max < 0.001
400 parameters	Δρmax = 0.54 e Å^−3
114 restraints	Δρmin = −0.32 e Å^−3

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

The SHELX manual (pages 5-7 ff.) gives an example for the refinement of thf disorders.

The refinement of positional disorder in complex (II) was resolved with two components and the use of similarity restraints. The THF molecules in complex (II) are disordered, and the pairs of atoms C15, C15A; C18, C18A; C23, C23A have the ratio of 80:20, 79:21 and 86:14 % occupancies, respectively.

According to the SHELX manual:

Disorder for C15, FOR EXAMPLE:

SIMU C15 C15A ANIS O1 > C15A

FVAR ···.. 0.6 ···. SAME O1 C13 C14 C15A C16 O1 4 ···.. ···.. ···.. C13 1 ···.. ···.. ···.. AFIX 23 H13A 2 ···.. ···.. ···.. H13B 2 ···.. ···.. ···.. AFIX 0 C14 1 ···.. ···.. ···.. PART 1 AFIX 23 H14A 2 ···.. ···.. ···.. 21 H14B 2 ···.. ···.. ···.. 21 PART 2 AFIX 23 H14C 2 ···.. ···.. ···.. -21 H14D 2 ···.. ···.. ···.. -21 AFIX 0 PART 1 C15 1 ···.. ···.. ···.. 21 AFIX 23 H15A 2 ···.. ···.. ···.. 21 H15B 2 ···.. ···.. ···.. 21 AFIX 0 PART 2 C15A 1 ···.. ···.. ···.. -21 AFIX 23 H15C 2 ···.. ···.. ···.. -21 H15D 2 ···.. ···.. ···.. -21 AFIX 0 PART 0 C16 1 ···.. ···.. ···.. PART 1 AFIX 23 H16A 2 ···.. ···.. ···.. 21 H16B 2 ···.. ···.. ···.. 21 PART 2 AFIX 23 H16C 2 ···.. ···.. ···.. -21 H16D 2 ···.. ···.. ···.. -21 AFIX 0 (···)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Cl1	0.45177 (3)	0.70159 (3)	0.14688 (3)	0.02543 (12)
Cl2	0.35786 (3)	0.92175 (3)	0.12664 (3)	0.02501 (12)
Mg1	0.38203 (4)	0.80575 (5)	0.25155 (4)	0.02232 (15)
Mg2	0.40389 (4)	0.80710 (5)	0.02011 (4)	0.02209 (15)
N1	0.31222 (11)	0.89537 (13)	0.33040 (11)	0.0267 (4)
N2	0.31351 (11)	0.87908 (14)	0.41779 (11)	0.0298 (4)
N3	0.40288 (11)	0.70041 (12)	0.35317 (10)	0.0264 (4)
N4	0.39801 (11)	0.72008 (14)	0.43885 (11)	0.0303 (4)
N5	0.40663 (11)	0.68834 (12)	−0.06699 (10)	0.0260 (3)
N6	0.38825 (11)	0.69998 (12)	−0.15602 (11)	0.0287 (4)
N7	0.29654 (11)	0.86410 (12)	−0.07311 (10)	0.0261 (3)
N8	0.29095 (11)	0.84723 (12)	−0.16100 (10)	0.0276 (4)
B1	0.39234 (16)	0.8244 (2)	0.47440 (15)	0.0340 (5)
H111	0.4562	0.8630	0.4720	0.041*
H112	0.3815	0.8220	0.5437	0.041*
B2	0.37013 (17)	0.80094 (19)	−0.19826 (16)	0.0329 (5)
H121	0.3531	0.7941	−0.2706	0.039*
H122	0.4308	0.8468	−0.1827	0.039*
C1	0.23967 (14)	0.94929 (16)	0.30366 (14)	0.0312 (4)
H1	0.2218	0.9713	0.2452	0.037*
C2	0.19393 (15)	0.96896 (18)	0.37255 (15)	0.0396 (5)
H2	0.1407	1.0057	0.3711	0.048*
C3	0.24320 (15)	0.92314 (18)	0.44346 (14)	0.0370 (5)
H3	0.2296	0.9228	0.5013	0.044*
C4	0.41280 (13)	0.60511 (16)	0.34741 (15)	0.0314 (5)
H4	0.4175	0.5716	0.2948	0.038*
C5	0.41531 (15)	0.56162 (19)	0.42854 (17)	0.0418 (6)
H5	0.4221	0.4950	0.4424	0.050*
C6	0.40572 (14)	0.63640 (19)	0.48410 (15)	0.0403 (6)
H6	0.4047	0.6303	0.5452	0.048*
C7	0.42405 (14)	0.59428 (15)	−0.05321 (14)	0.0307 (4)
H7	0.4386	0.5654	0.0030	0.037*
C8	0.41806 (15)	0.54477 (17)	−0.13175 (15)	0.0382 (5)
H8	0.4279	0.4780	−0.1402	0.046*
C9	0.39467 (16)	0.61433 (17)	−0.19487 (15)	0.0385 (5)
H9	0.3846	0.6034	−0.2564	0.046*
C10	0.22047 (13)	0.90849 (15)	−0.06323 (14)	0.0296 (4)
H10	0.2058	0.9287	−0.0085	0.036*
C11	0.16553 (14)	0.92126 (16)	−0.14369 (15)	0.0335 (5)
H11	0.1081	0.9508	−0.1548	0.040*
C12	0.21297 (14)	0.88158 (16)	−0.20341 (14)	0.0336 (5)
H12	0.1936	0.8789	−0.2650	0.040*
O1	0.50584 (9)	0.86991 (10)	0.29814 (9)	0.0262 (3)
C13	0.58566 (13)	0.81622 (16)	0.33491 (15)	0.0342 (5)
H13A	0.6097	0.7804	0.2883	0.041*
H13B	0.5719	0.7696	0.3794	0.041*
C14	0.65237 (17)	0.8904 (2)	0.3763 (2)	0.0539 (7)
H14A	0.6504	0.8967	0.4398	0.065*	0.796 (13)
H14B	0.7140	0.8725	0.3685	0.065*	0.796 (13)
H14C	0.6764	0.8721	0.4376	0.065*	0.204 (13)
H14D	0.7030	0.8953	0.3432	0.065*	0.204 (13)
C15	0.6240 (2)	0.9822 (2)	0.3293 (3)	0.0370 (10)	0.796 (13)
H15A	0.6474	0.9868	0.2732	0.044*	0.796 (13)
H15B	0.6439	1.0392	0.3659	0.044*	0.796 (13)
C15A	0.6083 (10)	0.9758 (11)	0.3745 (16)	0.047 (5)	0.204 (13)
H15C	0.6461	1.0274	0.3554	0.057*	0.204 (13)
H15D	0.5973	0.9918	0.4343	0.057*	0.204 (13)
C16	0.52168 (15)	0.97222 (15)	0.31410 (15)	0.0338 (5)
H16A	0.4967	0.9936	0.3663	0.041*	0.796 (13)
H16B	0.4942	1.0109	0.2629	0.041*	0.796 (13)
H16C	0.4732	1.0013	0.3415	0.041*	0.204 (13)
H16D	0.5256	1.0068	0.2588	0.041*	0.204 (13)
O2	0.25636 (9)	0.73569 (11)	0.20624 (8)	0.0294 (3)
C17	0.21266 (15)	0.72134 (19)	0.11669 (13)	0.0374 (5)
H17A	0.2471	0.6749	0.0866	0.045*	0.785 (13)
H17B	0.2088	0.7832	0.0843	0.045*	0.785 (13)
H17C	0.2196	0.6540	0.0975	0.045*	0.215 (13)
H17D	0.2369	0.7657	0.0761	0.045*	0.215 (13)
C18	0.1217 (3)	0.6833 (5)	0.1199 (2)	0.0460 (13)	0.785 (13)
H18A	0.1209	0.6119	0.1185	0.055*	0.785 (13)
H18B	0.0775	0.7084	0.0707	0.055*	0.785 (13)
C18A	0.1132 (10)	0.745 (2)	0.1214 (10)	0.056 (5)	0.215 (13)
H18C	0.1001	0.8136	0.1082	0.068*	0.215 (13)
H18D	0.0726	0.7046	0.0793	0.068*	0.215 (13)
C19	0.10307 (16)	0.7224 (2)	0.20963 (18)	0.0523 (7)
H19A	0.0855	0.7913	0.2060	0.063*	0.785 (13)
H19B	0.0563	0.6843	0.2322	0.063*	0.785 (13)
H19C	0.0670	0.6630	0.2106	0.063*	0.215 (13)
H19D	0.0713	0.7757	0.2342	0.063*	0.215 (13)
C20	0.19356 (14)	0.70828 (18)	0.26415 (14)	0.0353 (5)
H20A	0.2009	0.7499	0.3169	0.042*
H20B	0.2024	0.6402	0.2828	0.042*
O3	0.52684 (9)	0.86067 (10)	0.01330 (9)	0.0276 (3)
C21	0.57941 (14)	0.90979 (17)	0.08799 (15)	0.0347 (5)
H21A	0.5514	0.9022	0.1412	0.042*
H21B	0.5849	0.9794	0.0757	0.042*
C22	0.66936 (15)	0.8616 (2)	0.09959 (16)	0.0443 (6)
H22A	0.6693	0.8010	0.1335	0.053*	0.856 (9)
H22B	0.7170	0.9047	0.1293	0.053*	0.856 (9)
H22C	0.7163	0.9087	0.0909	0.053*	0.144 (9)
H22D	0.6843	0.8344	0.1594	0.053*	0.144 (9)
C23	0.68137 (18)	0.8416 (3)	0.0051 (2)	0.0389 (9)	0.856 (9)
H23A	0.7050	0.8991	−0.0216	0.047*	0.856 (9)
H23B	0.7225	0.7867	0.0019	0.047*	0.856 (9)
C23A	0.6646 (12)	0.787 (2)	0.0365 (16)	0.057 (7)	0.144 (9)
H23C	0.6499	0.7249	0.0620	0.069*	0.144 (9)
H23D	0.7223	0.7807	0.0147	0.069*	0.144 (9)
C24	0.58876 (16)	0.8181 (3)	−0.03893 (19)	0.0577 (8)
H24A	0.5780	0.8450	−0.0991	0.069*	0.856 (9)
H24B	0.5803	0.7473	−0.0427	0.069*	0.856 (9)
H24C	0.6100	0.8659	−0.0785	0.069*	0.144 (9)
H24D	0.5621	0.7621	−0.0734	0.069*	0.144 (9)

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Cl1	0.0278 (2)	0.0223 (2)	0.0261 (2)	0.00429 (18)	0.00397 (17)	0.00150 (17)
Cl2	0.0264 (2)	0.0234 (2)	0.0249 (2)	0.00516 (18)	0.00304 (17)	0.00213 (17)
Mg1	0.0204 (3)	0.0231 (3)	0.0228 (3)	0.0014 (3)	0.0012 (2)	0.0017 (2)
Mg2	0.0203 (3)	0.0218 (3)	0.0236 (3)	0.0004 (3)	0.0018 (2)	0.0003 (2)
N1	0.0246 (8)	0.0302 (9)	0.0245 (8)	0.0011 (7)	0.0014 (6)	−0.0007 (7)
N2	0.0256 (8)	0.0379 (10)	0.0251 (8)	0.0017 (7)	0.0020 (6)	−0.0033 (7)
N3	0.0223 (8)	0.0298 (9)	0.0257 (8)	−0.0007 (7)	−0.0002 (6)	0.0046 (7)
N4	0.0214 (8)	0.0422 (11)	0.0266 (8)	0.0031 (7)	0.0014 (6)	0.0093 (7)
N5	0.0245 (8)	0.0261 (9)	0.0262 (8)	0.0003 (7)	0.0003 (6)	−0.0009 (7)
N6	0.0304 (9)	0.0300 (9)	0.0247 (8)	0.0021 (7)	0.0010 (7)	−0.0039 (7)
N7	0.0247 (8)	0.0261 (9)	0.0267 (8)	−0.0002 (7)	0.0014 (6)	0.0015 (7)
N8	0.0302 (9)	0.0265 (9)	0.0246 (8)	−0.0017 (7)	0.0001 (6)	0.0034 (7)
B1	0.0289 (12)	0.0485 (15)	0.0226 (10)	0.0032 (11)	−0.0013 (9)	0.0001 (10)
B2	0.0359 (13)	0.0362 (14)	0.0270 (11)	0.0033 (11)	0.0063 (9)	0.0033 (10)
C1	0.0299 (10)	0.0298 (11)	0.0327 (10)	0.0067 (9)	0.0009 (8)	−0.0008 (8)
C2	0.0327 (11)	0.0431 (14)	0.0430 (12)	0.0121 (10)	0.0059 (9)	−0.0057 (10)
C3	0.0337 (11)	0.0467 (14)	0.0317 (11)	0.0033 (10)	0.0088 (9)	−0.0085 (10)
C4	0.0227 (9)	0.0291 (11)	0.0410 (12)	−0.0016 (8)	0.0006 (8)	0.0077 (9)
C5	0.0290 (11)	0.0406 (13)	0.0554 (14)	0.0040 (10)	0.0054 (10)	0.0227 (12)
C6	0.0278 (10)	0.0561 (16)	0.0367 (12)	0.0047 (11)	0.0044 (9)	0.0221 (11)
C7	0.0299 (10)	0.0253 (10)	0.0347 (11)	0.0014 (8)	−0.0015 (8)	−0.0011 (8)
C8	0.0400 (12)	0.0279 (11)	0.0429 (12)	0.0054 (10)	−0.0049 (10)	−0.0096 (10)
C9	0.0398 (12)	0.0397 (13)	0.0334 (11)	0.0062 (10)	−0.0016 (9)	−0.0127 (10)
C10	0.0248 (9)	0.0265 (10)	0.0368 (11)	0.0016 (8)	0.0029 (8)	0.0044 (8)
C11	0.0246 (10)	0.0281 (11)	0.0447 (12)	−0.0006 (9)	−0.0039 (9)	0.0093 (9)
C12	0.0324 (11)	0.0293 (11)	0.0345 (11)	−0.0040 (9)	−0.0089 (9)	0.0065 (9)
O1	0.0218 (6)	0.0202 (7)	0.0344 (7)	0.0021 (5)	−0.0020 (5)	0.0001 (6)
C13	0.0231 (10)	0.0311 (11)	0.0457 (12)	0.0051 (9)	−0.0025 (9)	0.0034 (9)
C14	0.0294 (12)	0.0519 (16)	0.0747 (19)	−0.0083 (12)	−0.0092 (12)	0.0080 (14)
C15	0.0347 (17)	0.0368 (17)	0.037 (2)	−0.0108 (13)	−0.0025 (14)	−0.0030 (15)
C15A	0.041 (7)	0.045 (7)	0.056 (11)	−0.021 (6)	0.008 (7)	−0.017 (7)
C16	0.0356 (11)	0.0221 (10)	0.0411 (12)	−0.0023 (9)	−0.0019 (9)	−0.0046 (9)
O2	0.0237 (7)	0.0411 (9)	0.0228 (7)	−0.0074 (6)	0.0018 (5)	0.0015 (6)
C17	0.0338 (11)	0.0482 (14)	0.0270 (10)	−0.0112 (10)	−0.0044 (8)	0.0004 (10)
C18	0.0293 (17)	0.064 (3)	0.0418 (18)	−0.017 (2)	−0.0017 (13)	−0.005 (2)
C18A	0.037 (7)	0.083 (13)	0.044 (7)	0.003 (8)	−0.009 (5)	0.003 (8)
C19	0.0280 (12)	0.075 (2)	0.0540 (15)	−0.0124 (13)	0.0076 (11)	−0.0013 (14)
C20	0.0312 (11)	0.0423 (13)	0.0344 (11)	−0.0085 (10)	0.0111 (9)	0.0016 (10)
O3	0.0218 (6)	0.0322 (8)	0.0290 (7)	−0.0028 (6)	0.0049 (5)	−0.0051 (6)
C21	0.0271 (10)	0.0388 (12)	0.0371 (11)	−0.0091 (9)	0.0021 (8)	−0.0086 (9)
C22	0.0288 (11)	0.0563 (16)	0.0448 (13)	−0.0035 (11)	−0.0030 (10)	0.0060 (12)
C23	0.0214 (12)	0.0427 (19)	0.0539 (18)	−0.0005 (12)	0.0100 (11)	−0.0022 (14)
C23A	0.028 (8)	0.070 (14)	0.082 (13)	0.013 (9)	0.032 (8)	−0.011 (11)
C24	0.0275 (12)	0.076 (2)	0.0627 (17)	−0.0078 (13)	0.0177 (11)	−0.0268 (16)

Geometric parameters (Å, º)

Cl1—Mg1	2.5229 (8)	C14—C15	1.493 (5)
Cl1—Mg2	2.4579 (8)	C14—H14A	0.9900
Cl2—Mg1	2.4932 (8)	C14—H14B	0.9900
Cl2—Mg2	2.4681 (8)	C14—H14C	0.9900
Mg1—O1	2.0920 (15)	C14—H14D	0.9900
Mg1—N1	2.1352 (18)	C15—C16	1.533 (4)
Mg1—N3	2.1301 (17)	C15—H15A	0.9900
Mg1—O2	2.1477 (15)	C15—H15B	0.9900
Mg2—O3	2.0201 (15)	C15A—C16	1.480 (15)
Mg2—N5	2.1310 (18)	C15A—H15C	0.9900
Mg2—N7	2.1393 (17)	C15A—H15D	0.9900
N1—C1	1.336 (3)	C16—H16A	0.9900
N1—N2	1.366 (2)	C16—H16B	0.9900
N2—C3	1.340 (3)	C16—H16C	0.9900
B1—N2	1.556 (3)	C16—H16D	0.9900
N3—C4	1.334 (3)	O2—C17	1.447 (2)
N3—N4	1.365 (2)	O2—C20	1.457 (2)
N4—C6	1.350 (3)	C17—C18	1.481 (4)
B1—N4	1.554 (3)	C17—C18A	1.551 (16)
N5—C7	1.340 (3)	C17—H17A	0.9900
N5—N6	1.368 (2)	C17—H17B	0.9900
N6—C9	1.341 (3)	C17—H17C	0.9900
B2—N6	1.550 (3)	C17—H17D	0.9900
N7—C10	1.335 (3)	C18—C19	1.557 (5)
N7—N8	1.367 (2)	C18—H18A	0.9900
N8—C12	1.340 (3)	C18—H18B	0.9900
B2—N8	1.549 (3)	C18A—C19	1.430 (16)
B1—H111	1.1100	C18A—H18C	0.9900
B1—H112	1.1100	C18A—H18D	0.9900
B2—H121	1.1100	C19—C20	1.499 (3)
B2—H122	1.1100	C19—H19A	0.9900
C1—C2	1.387 (3)	C19—H19B	0.9900
C1—H1	0.9500	C19—H19C	0.9900
C2—C3	1.376 (3)	C19—H19D	0.9900
C2—H2	0.9500	C20—H20A	0.9900
C3—H3	0.9500	C20—H20B	0.9900
C4—C5	1.386 (3)	O3—C24	1.456 (3)
C4—H4	0.9500	O3—C21	1.460 (2)
C5—C6	1.369 (4)	C21—C22	1.500 (3)
C5—H5	0.9500	C21—H21A	0.9900
C6—H6	0.9500	C21—H21B	0.9900
C7—C8	1.384 (3)	C22—C23A	1.41 (2)
C7—H7	0.9500	C22—C23	1.525 (4)
C8—C9	1.376 (3)	C22—H22A	0.9900
C8—H8	0.9500	C22—H22B	0.9900
C9—H9	0.9500	C22—H22C	0.9900
C10—C11	1.390 (3)	C22—H22D	0.9900
C10—H10	0.9500	C23—C24	1.490 (4)
C11—C12	1.372 (3)	C23—H23A	0.9900
C11—H11	0.9500	C23—H23B	0.9900
C12—H12	0.9500	C23A—C24	1.56 (2)
O1—C13	1.453 (2)	C23A—H23C	0.9900
O1—C16	1.453 (2)	C23A—H23D	0.9900
C13—C14	1.509 (3)	C24—H24A	0.9900
C13—H13A	0.9900	C24—H24B	0.9900
C13—H13B	0.9900	C24—H24C	0.9900
C14—C15A	1.357 (15)	C24—H24D	0.9900
Mg2—Cl1—Mg1	94.05 (3)	C16—C15—H15B	111.5
Mg2—Cl2—Mg1	94.55 (3)	H15A—C15—H15B	109.3
O1—Mg1—N3	91.17 (6)	C14—C15A—C16	111.4 (9)
O1—Mg1—N1	93.08 (6)	C14—C15A—H15C	109.3
N1—Mg1—N3	90.34 (7)	C16—C15A—H15C	109.3
O1—Mg1—O2	178.09 (6)	C14—C15A—H15D	109.3
N3—Mg1—O2	87.01 (6)	C16—C15A—H15D	109.3
N1—Mg1—O2	87.49 (6)	H15C—C15A—H15D	108.0
O1—Mg1—Cl2	90.18 (4)	O1—C16—C15A	104.2 (6)
N3—Mg1—Cl2	176.84 (6)	O1—C16—C15	104.4 (2)
N1—Mg1—Cl2	92.44 (5)	O1—C16—H16A	110.9
O2—Mg1—Cl2	91.62 (4)	C15A—C16—H16A	83.7
O1—Mg1—Cl1	91.17 (5)	C15—C16—H16A	110.9
N3—Mg1—Cl1	93.04 (5)	O1—C16—H16B	110.9
N1—Mg1—Cl1	174.52 (5)	C15A—C16—H16B	134.4
O2—Mg1—Cl1	88.38 (5)	C15—C16—H16B	110.9
Cl2—Mg1—Cl1	84.08 (3)	H16A—C16—H16B	108.9
O1—Mg1—Mg2	96.73 (4)	O1—C16—H16C	110.9
N3—Mg1—Mg2	134.49 (5)	C15A—C16—H16C	110.9
N1—Mg1—Mg2	133.54 (5)	C15—C16—H16C	134.1
O2—Mg1—Mg2	84.17 (4)	H16B—C16—H16C	83.0
Cl2—Mg1—Mg2	42.459 (18)	O1—C16—H16D	110.9
Cl1—Mg1—Mg2	42.278 (18)	C15A—C16—H16D	110.9
O3—Mg2—N5	97.99 (6)	C15—C16—H16D	83.6
O3—Mg2—N7	115.68 (7)	H16A—C16—H16D	130.0
N5—Mg2—N7	87.15 (7)	H16C—C16—H16D	108.9
O3—Mg2—Cl1	96.06 (5)	C17—O2—C20	108.03 (15)
N5—Mg2—Cl1	90.59 (5)	C17—O2—Mg1	128.07 (12)
N7—Mg2—Cl1	148.20 (5)	C20—O2—Mg1	123.22 (12)
O3—Mg2—Cl2	99.16 (5)	O2—C17—C18	107.4 (2)
N5—Mg2—Cl2	162.77 (5)	O2—C17—C18A	102.8 (6)
N7—Mg2—Cl2	86.92 (5)	O2—C17—H17A	110.2
Cl1—Mg2—Cl2	85.99 (3)	C18—C17—H17A	110.2
O3—Mg2—Mg1	106.46 (4)	C18A—C17—H17A	138.1
N5—Mg2—Mg1	129.04 (5)	O2—C17—H17B	110.2
N7—Mg2—Mg1	118.89 (5)	C18—C17—H17B	110.2
Cl1—Mg2—Mg1	43.669 (19)	C18A—C17—H17B	82.2
Cl2—Mg2—Mg1	42.994 (18)	H17A—C17—H17B	108.5
C1—N1—N2	106.13 (16)	O2—C17—H17C	111.2
C1—N1—Mg1	127.29 (14)	C18—C17—H17C	79.6
N2—N1—Mg1	122.59 (13)	C18A—C17—H17C	111.2
C3—N2—N1	109.39 (17)	H17B—C17—H17C	131.7
C3—N2—B1	128.85 (18)	O2—C17—H17D	111.2
N1—N2—B1	121.55 (16)	C18—C17—H17D	133.1
C4—N3—N4	106.66 (17)	C18A—C17—H17D	111.2
C4—N3—Mg1	129.38 (14)	H17A—C17—H17D	80.2
N4—N3—Mg1	123.58 (13)	H17C—C17—H17D	109.1
C6—N4—N3	108.48 (19)	C17—C18—C19	102.0 (3)
C6—N4—B1	128.44 (19)	C17—C18—H18A	111.4
N3—N4—B1	122.90 (16)	C19—C18—H18A	111.4
C7—N5—N6	106.09 (16)	C17—C18—H18B	111.4
C7—N5—Mg2	132.42 (14)	C19—C18—H18B	111.4
N6—N5—Mg2	121.49 (13)	H18A—C18—H18B	109.2
C9—N6—N5	109.15 (17)	C19—C18A—C17	104.7 (9)
C9—N6—B2	129.18 (18)	C19—C18A—H18C	110.8
N5—N6—B2	121.55 (16)	C17—C18A—H18C	110.8
C10—N7—N8	106.06 (16)	C19—C18A—H18D	110.8
C10—N7—Mg2	131.84 (14)	C17—C18A—H18D	110.8
N8—N7—Mg2	121.60 (12)	H18C—C18A—H18D	108.9
C12—N8—N7	109.45 (17)	C18A—C19—C20	109.6 (6)
C12—N8—B2	129.57 (18)	C20—C19—C18	100.1 (2)
N7—N8—B2	120.85 (16)	C18A—C19—H19A	78.9
N4—B1—N2	109.60 (17)	C20—C19—H19A	111.8
N4—B1—H111	109.8	C18—C19—H19A	111.8
N2—B1—H111	109.8	C18A—C19—H19B	130.1
N4—B1—H112	109.8	C20—C19—H19B	111.8
N2—B1—H112	109.8	C18—C19—H19B	111.8
H111—B1—H112	108.2	H19A—C19—H19B	109.5
N6—B2—N8	108.19 (17)	C18A—C19—H19C	109.8
N6—B2—H121	110.1	C20—C19—H19C	109.8
N8—B2—H121	110.1	C18—C19—H19C	84.4
N6—B2—H122	110.1	H19A—C19—H19C	131.3
N8—B2—H122	110.1	C18A—C19—H19D	109.8
H121—B2—H122	108.4	C20—C19—H19D	109.8
N1—C1—C2	111.03 (19)	C18—C19—H19D	140.4
N1—C1—H1	124.5	H19B—C19—H19D	81.1
C2—C1—H1	124.5	H19C—C19—H19D	108.2
C3—C2—C1	104.33 (19)	O2—C20—C19	104.30 (18)
C3—C2—H2	127.8	O2—C20—H20A	110.9
C1—C2—H2	127.8	C19—C20—H20A	110.9
N2—C3—C2	109.12 (19)	O2—C20—H20B	110.9
N2—C3—H3	125.4	C19—C20—H20B	110.9
C2—C3—H3	125.4	H20A—C20—H20B	108.9
N3—C4—C5	110.9 (2)	C24—O3—C21	108.09 (15)
N3—C4—H4	124.5	C24—O3—Mg2	124.03 (14)
C5—C4—H4	124.5	C21—O3—Mg2	121.21 (12)
C6—C5—C4	104.3 (2)	O3—C21—C22	104.69 (18)
C6—C5—H5	127.8	O3—C21—H21A	110.8
C4—C5—H5	127.8	C22—C21—H21A	110.8
N4—C6—C5	109.6 (2)	O3—C21—H21B	110.8
N4—C6—H6	125.2	C22—C21—H21B	110.8
C5—C6—H6	125.2	H21A—C21—H21B	108.9
N5—C7—C8	111.08 (19)	C23A—C22—C21	107.4 (8)
N5—C7—H7	124.5	C21—C22—C23	102.27 (19)
C8—C7—H7	124.5	C23A—C22—H22A	75.1
C9—C8—C7	104.3 (2)	C21—C22—H22A	111.3
C9—C8—H8	127.9	C23—C22—H22A	111.3
C7—C8—H8	127.9	C23A—C22—H22B	135.5
N6—C9—C8	109.39 (19)	C21—C22—H22B	111.3
N6—C9—H9	125.3	C23—C22—H22B	111.3
C8—C9—H9	125.3	H22A—C22—H22B	109.2
N7—C10—C11	110.94 (19)	C23A—C22—H22C	110.2
N7—C10—H10	124.5	C21—C22—H22C	110.2
C11—C10—H10	124.5	C23—C22—H22C	77.9
C12—C11—C10	104.41 (19)	H22A—C22—H22C	133.9
C12—C11—H11	127.8	C23A—C22—H22D	110.2
C10—C11—H11	127.8	C21—C22—H22D	110.2
N8—C12—C11	109.13 (19)	C23—C22—H22D	141.3
N8—C12—H12	125.4	H22B—C22—H22D	76.0
C11—C12—H12	125.4	H22C—C22—H22D	108.5
C13—O1—C16	109.27 (15)	C24—C23—C22	103.2 (2)
C13—O1—Mg1	123.85 (12)	C24—C23—H23A	111.1
C16—O1—Mg1	125.96 (12)	C22—C23—H23A	111.1
O1—C13—C14	105.83 (18)	C24—C23—H23B	111.1
O1—C13—H13A	110.6	C22—C23—H23B	111.1
C14—C13—H13A	110.6	H23A—C23—H23B	109.1
O1—C13—H13B	110.6	C22—C23A—C24	105.4 (14)
C14—C13—H13B	110.6	C22—C23A—H23C	110.7
H13A—C13—H13B	108.7	C24—C23A—H23C	110.7
C15A—C14—C13	107.0 (6)	C22—C23A—H23D	110.7
C15—C14—C13	104.8 (2)	C24—C23A—H23D	110.7
C15A—C14—H14A	81.4	H23C—C23A—H23D	108.8
C15—C14—H14A	110.8	O3—C24—C23	107.4 (2)
C13—C14—H14A	110.8	O3—C24—C23A	99.1 (7)
C15A—C14—H14B	133.2	O3—C24—H24A	110.2
C15—C14—H14B	110.8	C23—C24—H24A	110.2
C13—C14—H14B	110.8	C23A—C24—H24A	142.7
H14A—C14—H14B	108.9	O3—C24—H24B	110.2
C15A—C14—H14C	110.3	C23—C24—H24B	110.2
C15—C14—H14C	135.7	C23A—C24—H24B	81.0
C13—C14—H14C	110.3	H24A—C24—H24B	108.5
H14B—C14—H14C	81.2	O3—C24—H24C	112.0
C15A—C14—H14D	110.3	C23—C24—H24C	76.2
C15—C14—H14D	82.8	C23A—C24—H24C	112.0
C13—C14—H14D	110.3	H24B—C24—H24C	132.7
H14A—C14—H14D	131.1	O3—C24—H24D	112.0
H14C—C14—H14D	108.6	C23—C24—H24D	133.5
C14—C15—C16	101.6 (3)	C23A—C24—H24D	112.0
C14—C15—H15A	111.5	H24A—C24—H24D	78.4
C16—C15—H15A	111.5	H24C—C24—H24D	109.6
C14—C15—H15B	111.5
Mg2—Cl2—Mg1—O1	99.81 (5)	N5—N6—B2—N8	−56.7 (2)
Mg2—Cl2—Mg1—N1	−167.10 (5)	C12—N8—B2—N6	−124.0 (2)
Mg2—Cl2—Mg1—O2	−79.55 (5)	N7—N8—B2—N6	60.4 (2)
Mg2—Cl2—Mg1—Cl1	8.65 (3)	N2—N1—C1—C2	0.4 (2)
Mg2—Cl1—Mg1—O1	−98.74 (4)	Mg1—N1—C1—C2	158.07 (16)
Mg2—Cl1—Mg1—N3	170.03 (5)	N1—C1—C2—C3	−0.2 (3)
Mg2—Cl1—Mg1—O2	83.11 (5)	N1—N2—C3—C2	0.4 (3)
Mg2—Cl1—Mg1—Cl2	−8.68 (3)	B1—N2—C3—C2	175.1 (2)
Mg1—Cl1—Mg2—O3	107.55 (5)	C1—C2—C3—N2	−0.1 (3)
Mg1—Cl1—Mg2—N5	−154.35 (5)	N4—N3—C4—C5	−0.5 (2)
Mg1—Cl1—Mg2—N7	−68.81 (11)	Mg1—N3—C4—C5	−173.57 (14)
Mg1—Cl1—Mg2—Cl2	8.75 (3)	N3—C4—C5—C6	0.4 (2)
Mg1—Cl2—Mg2—O3	−104.35 (5)	N3—N4—C6—C5	−0.2 (2)
Mg1—Cl2—Mg2—N5	70.13 (19)	B1—N4—C6—C5	−175.5 (2)
Mg1—Cl2—Mg2—N7	140.12 (5)	C4—C5—C6—N4	−0.1 (2)
Mg1—Cl2—Mg2—Cl1	−8.86 (3)	N6—N5—C7—C8	0.5 (2)
O1—Mg1—Mg2—O3	2.94 (6)	Mg2—N5—C7—C8	−179.56 (15)
N3—Mg1—Mg2—O3	−95.38 (8)	N5—C7—C8—C9	−0.7 (3)
N1—Mg1—Mg2—O3	103.71 (8)	N5—N6—C9—C8	−0.4 (3)
O2—Mg1—Mg2—O3	−175.37 (7)	B2—N6—C9—C8	175.5 (2)
Cl2—Mg1—Mg2—O3	85.79 (5)	C7—C8—C9—N6	0.7 (3)
Cl1—Mg1—Mg2—O3	−81.36 (5)	N8—N7—C10—C11	−0.3 (2)
O1—Mg1—Mg2—N5	118.17 (7)	Mg2—N7—C10—C11	−172.05 (14)
N3—Mg1—Mg2—N5	19.85 (10)	N7—C10—C11—C12	0.1 (2)
N1—Mg1—Mg2—N5	−141.06 (9)	N7—N8—C12—C11	−0.4 (2)
O2—Mg1—Mg2—N5	−60.14 (8)	B2—N8—C12—C11	−176.3 (2)
Cl2—Mg1—Mg2—N5	−158.98 (7)	C10—C11—C12—N8	0.2 (2)
Cl1—Mg1—Mg2—N5	33.87 (6)	N3—Mg1—O1—C13	36.76 (16)
O1—Mg1—Mg2—N7	−129.84 (7)	N1—Mg1—O1—C13	127.16 (15)
N3—Mg1—Mg2—N7	131.83 (9)	Cl2—Mg1—O1—C13	−140.38 (15)
N1—Mg1—Mg2—N7	−29.08 (9)	Cl1—Mg1—O1—C13	−56.30 (15)
O2—Mg1—Mg2—N7	51.84 (7)	Mg2—Mg1—O1—C13	−98.33 (15)
Cl2—Mg1—Mg2—N7	−46.99 (6)	N3—Mg1—O1—C16	−131.05 (16)
Cl1—Mg1—Mg2—N7	145.86 (6)	N1—Mg1—O1—C16	−40.65 (16)
O1—Mg1—Mg2—Cl1	84.30 (5)	Cl2—Mg1—O1—C16	51.81 (15)
N3—Mg1—Mg2—Cl1	−14.03 (7)	Cl1—Mg1—O1—C16	135.89 (15)
N1—Mg1—Mg2—Cl1	−174.93 (8)	Mg2—Mg1—O1—C16	93.86 (15)
O2—Mg1—Mg2—Cl1	−94.01 (5)	C16—O1—C13—C14	0.9 (2)
Cl2—Mg1—Mg2—Cl1	167.15 (4)	Mg1—O1—C13—C14	−168.68 (16)
O1—Mg1—Mg2—Cl2	−82.85 (5)	O1—C13—C14—C15A	8.6 (12)
N3—Mg1—Mg2—Cl2	178.83 (8)	O1—C13—C14—C15	−23.8 (3)
N1—Mg1—Mg2—Cl2	17.92 (7)	C15A—C14—C15—C16	−62.7 (11)
O2—Mg1—Mg2—Cl2	98.84 (5)	C13—C14—C15—C16	36.0 (4)
Cl1—Mg1—Mg2—Cl2	−167.15 (4)	C15—C14—C15A—C16	75.6 (17)
O1—Mg1—N1—C1	127.17 (18)	C13—C14—C15A—C16	−14.9 (19)
N3—Mg1—N1—C1	−141.65 (18)	C13—O1—C16—C15A	−9.1 (10)
O2—Mg1—N1—C1	−54.66 (18)	Mg1—O1—C16—C15A	160.2 (10)
Cl2—Mg1—N1—C1	36.86 (18)	C13—O1—C16—C15	21.7 (3)
Mg2—Mg1—N1—C1	24.9 (2)	Mg1—O1—C16—C15	−169.0 (2)
O1—Mg1—N1—N2	−78.51 (15)	C14—C15A—C16—O1	15.3 (18)
N3—Mg1—N1—N2	12.68 (15)	C14—C15A—C16—C15	−79.1 (17)
O2—Mg1—N1—N2	99.67 (15)	C14—C15—C16—O1	−35.5 (4)
Cl2—Mg1—N1—N2	−168.81 (14)	C14—C15—C16—C15A	58.0 (12)
Mg2—Mg1—N1—N2	179.19 (11)	N3—Mg1—O2—C17	−143.62 (18)
C1—N1—N2—C3	−0.5 (2)	N1—Mg1—O2—C17	125.91 (18)
Mg1—N1—N2—C3	−159.44 (15)	Cl2—Mg1—O2—C17	33.54 (18)
C1—N1—N2—B1	−175.6 (2)	Cl1—Mg1—O2—C17	−50.50 (18)
Mg1—N1—N2—B1	25.4 (2)	Mg2—Mg1—O2—C17	−8.32 (17)
O1—Mg1—N3—C4	−115.03 (17)	N3—Mg1—O2—C20	47.01 (16)
N1—Mg1—N3—C4	151.88 (17)	N1—Mg1—O2—C20	−43.47 (16)
O2—Mg1—N3—C4	64.42 (17)	Cl2—Mg1—O2—C20	−135.84 (15)
Cl1—Mg1—N3—C4	−23.80 (17)	Cl1—Mg1—O2—C20	140.13 (15)
Mg2—Mg1—N3—C4	−14.4 (2)	Mg2—Mg1—O2—C20	−177.70 (16)
O1—Mg1—N3—N4	72.95 (15)	C20—O2—C17—C18	−0.7 (4)
N1—Mg1—N3—N4	−20.14 (15)	Mg1—O2—C17—C18	−171.3 (3)
O2—Mg1—N3—N4	−107.60 (15)	C20—O2—C17—C18A	33.1 (11)
Cl1—Mg1—N3—N4	164.18 (14)	Mg1—O2—C17—C18A	−137.6 (11)
Mg2—Mg1—N3—N4	173.58 (11)	O2—C17—C18—C19	25.6 (5)
C4—N3—N4—C6	0.4 (2)	C18A—C17—C18—C19	−61.2 (11)
Mg1—N3—N4—C6	174.01 (14)	O2—C17—C18A—C19	−27.6 (18)
C4—N3—N4—B1	176.01 (18)	C18—C17—C18A—C19	74.7 (16)
Mg1—N3—N4—B1	−10.4 (2)	C17—C18A—C19—C20	12.5 (19)
O3—Mg2—N5—C7	98.92 (19)	C17—C18A—C19—C18	−65.6 (13)
N7—Mg2—N5—C7	−145.54 (19)	C17—C18—C19—C18A	70.6 (11)
Cl1—Mg2—N5—C7	2.72 (19)	C17—C18—C19—C20	−39.9 (4)
Cl2—Mg2—N5—C7	−75.6 (3)	C17—O2—C20—C19	−25.8 (3)
Mg1—Mg2—N5—C7	−19.9 (2)	Mg1—O2—C20—C19	145.44 (17)
O3—Mg2—N5—N6	−81.18 (15)	C18A—C19—C20—O2	7.2 (13)
N7—Mg2—N5—N6	34.36 (14)	C18—C19—C20—O2	40.1 (3)
Cl1—Mg2—N5—N6	−177.38 (14)	N5—Mg2—O3—C24	−0.8 (2)
Cl2—Mg2—N5—N6	104.3 (2)	N7—Mg2—O3—C24	−91.5 (2)
Mg1—Mg2—N5—N6	159.99 (11)	Cl1—Mg2—O3—C24	90.63 (19)
C7—N5—N6—C9	−0.1 (2)	Cl2—Mg2—O3—C24	177.52 (19)
Mg2—N5—N6—C9	180.00 (14)	Mg1—Mg2—O3—C24	133.98 (19)
C7—N5—N6—B2	−176.33 (18)	N5—Mg2—O3—C21	−148.74 (15)
Mg2—N5—N6—B2	3.7 (2)	N7—Mg2—O3—C21	120.59 (15)
O3—Mg2—N7—C10	−122.89 (18)	Cl1—Mg2—O3—C21	−57.28 (15)
N5—Mg2—N7—C10	139.62 (19)	Cl2—Mg2—O3—C21	29.61 (15)
Cl1—Mg2—N7—C10	53.1 (2)	Mg1—Mg2—O3—C21	−13.93 (15)
Cl2—Mg2—N7—C10	−24.20 (18)	C24—O3—C21—C22	−23.2 (3)
Mg1—Mg2—N7—C10	5.8 (2)	Mg2—O3—C21—C22	129.18 (16)
O3—Mg2—N7—N8	66.46 (16)	O3—C21—C22—C23A	−2.3 (14)
N5—Mg2—N7—N8	−31.03 (14)	O3—C21—C22—C23	36.4 (3)
Cl1—Mg2—N7—N8	−117.55 (14)	C23A—C22—C23—C24	66.9 (12)
Cl2—Mg2—N7—N8	165.15 (14)	C21—C22—C23—C24	−35.7 (3)
Mg1—Mg2—N7—N8	−164.89 (12)	C21—C22—C23A—C24	24.9 (18)
C10—N7—N8—C12	0.4 (2)	C23—C22—C23A—C24	−62.8 (16)
Mg2—N7—N8—C12	173.20 (14)	C21—O3—C24—C23	0.2 (3)
C10—N7—N8—B2	176.80 (18)	Mg2—O3—C24—C23	−151.3 (2)
Mg2—N7—N8—B2	−10.4 (2)	C21—O3—C24—C23A	36.6 (12)
C6—N4—B1—N2	−132.1 (2)	Mg2—O3—C24—C23A	−114.8 (11)
N3—N4—B1—N2	53.2 (2)	C22—C23—C24—O3	22.4 (4)
C3—N2—B1—N4	124.0 (2)	C22—C23—C24—C23A	−59.1 (12)
N1—N2—B1—N4	−61.9 (2)	C22—C23A—C24—O3	−37.6 (16)
C9—N6—B2—N8	127.9 (2)	C22—C23A—C24—C23	69.5 (17)

(III) bis[dihydridobis(pyrazol-1-yl)borato-κ²N,N'](tetrahydrofuran- κO)magnesium(II)

Crystal data

[Mg(C6H8BN4)2(C4H8O)]	Z = 4
Mr = 390.36	F(000) = 824
Triclinic, P1	Dx = 1.253 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.951 (3) Å	Cell parameters from 5780 reflections
b = 10.741 (2) Å	θ = 2.5–27.5°
c = 20.996 (3) Å	µ = 0.11 mm^−1
α = 99.137 (5)°	T = 150 K
β = 97.410 (4)°	Plate, colourless
γ = 107.909 (3)°	0.42 × 0.26 × 0.12 mm
V = 2070.2 (8) Å^3

Data collection

Bruker SMART APEX CCD area-detector diffractometer	8386 independent reflections
Radiation source: normal-focus sealed tube	5502 reflections with I > 2s(I)
Graphite monochromator	Rint = 0.031
ϕ and ω scans	θmax = 26.4°, θmin = 1.0°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→12
Tmin = 0.982, Tmax = 0.997	k = −13→13
17263 measured reflections	l = −26→25

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.049	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.115	H-atom parameters constrained
S = 1.00	w = 1/[σ^2(Fo^2) + (0.0515P)^2] where P = (Fo^2 + 2Fc^2)/3
8386 reflections	(Δ/σ)max < 0.001
537 parameters	Δρmax = 0.25 e Å^−3
0 restraints	Δρmin = −0.21 e Å^−3

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq
Mg1	0.74052 (7)	0.65043 (7)	0.35931 (3)	0.0329 (2)
O1	0.71567 (15)	0.62904 (14)	0.25978 (7)	0.0394 (5)
N1	0.61381 (19)	0.76865 (18)	0.38742 (8)	0.0380 (6)
N2	0.65006 (19)	0.90132 (18)	0.38551 (9)	0.0404 (6)
N3	0.92576 (19)	0.82932 (17)	0.38829 (9)	0.0385 (6)
N4	0.9151 (2)	0.95317 (17)	0.38732 (9)	0.0401 (6)
N5	0.56005 (19)	0.47474 (18)	0.35870 (9)	0.0387 (6)
N6	0.57788 (19)	0.41402 (18)	0.40983 (9)	0.0402 (6)
N7	0.87463 (18)	0.53422 (17)	0.37699 (9)	0.0371 (6)
N8	0.84278 (18)	0.45861 (17)	0.42249 (8)	0.0367 (6)
B1	0.7760 (3)	0.9687 (3)	0.35276 (14)	0.0443 (10)
H111	0.7532	0.9218	0.3000	0.053*
H112	0.7900	1.0768	0.3576	0.053*
B2	0.7216 (3)	0.4713 (3)	0.45998 (14)	0.0485 (10)
H121	0.7421	0.5780	0.4820	0.058*
H122	0.7174	0.4146	0.4998	0.058*
C1	0.4997 (2)	0.7411 (3)	0.41701 (11)	0.0463 (8)
H1	0.4525	0.6575	0.4251	0.056*
C2	0.4618 (3)	0.8530 (3)	0.43380 (12)	0.0573 (10)
H2	0.3870	0.8603	0.4548	0.069*
C3	0.5591 (3)	0.9514 (3)	0.41269 (11)	0.0504 (9)
H3	0.5611	1.0395	0.4167	0.061*
C4	1.0590 (2)	0.8517 (2)	0.41978 (12)	0.0462 (8)
H4	1.0961	0.7848	0.4275	0.055*
C5	1.1347 (3)	0.9869 (2)	0.43938 (13)	0.0536 (9)
H5	1.2289	1.0280	0.4621	0.064*
C6	1.0400 (3)	1.0469 (2)	0.41787 (12)	0.0495 (8)
H6	1.0593	1.1388	0.4236	0.059*
C7	0.4289 (2)	0.4029 (2)	0.32357 (12)	0.0446 (8)
H7	0.3880	0.4212	0.2853	0.053*
C8	0.3626 (2)	0.2983 (2)	0.35153 (12)	0.0491 (8)
H8	0.2714	0.2347	0.3367	0.059*
C9	0.4600 (2)	0.3085 (2)	0.40570 (12)	0.0479 (9)
H9	0.4468	0.2514	0.4351	0.058*
C10	0.9823 (2)	0.5057 (2)	0.35368 (12)	0.0445 (8)
H10	1.0262	0.5436	0.3216	0.053*
C11	1.0204 (3)	0.4125 (2)	0.38331 (12)	0.0505 (9)
H11	1.0918	0.3761	0.3756	0.061*
C12	0.9294 (3)	0.3861 (2)	0.42646 (12)	0.0471 (8)
H12	0.9280	0.3267	0.4543	0.056*
C13	0.8338 (3)	0.6598 (3)	0.22530 (12)	0.0644 (10)
H13A	0.8777	0.5905	0.2235	0.077*
H13B	0.9063	0.7445	0.2476	0.077*
C14	0.7750 (4)	0.6673 (4)	0.15853 (15)	0.0940 (15)
H14A	0.8394	0.7415	0.1445	0.113*
H14B	0.7612	0.5851	0.1275	0.113*
C15	0.6381 (5)	0.6871 (4)	0.16272 (16)	0.0694 (8)
H15A	0.5700	0.6450	0.1217	0.131*
H15B	0.6504	0.7817	0.1724	0.131*
C16	0.5870 (3)	0.6234 (3)	0.21702 (12)	0.0629 (10)
H16A	0.5342	0.6719	0.2404	0.075*
H16B	0.5249	0.5314	0.2001	0.075*
Mg2	0.30052 (7)	0.94379 (7)	0.13000 (3)	0.03199 (18)
O2	0.50324 (15)	1.06065 (14)	0.17408 (7)	0.0387 (4)
N9	0.24418 (17)	1.02465 (17)	0.04886 (8)	0.0338 (4)
N10	0.22177 (18)	1.14510 (17)	0.05584 (9)	0.0358 (4)
N11	0.18564 (18)	1.04967 (17)	0.18365 (8)	0.0347 (4)
N12	0.17176 (18)	1.16618 (17)	0.17030 (9)	0.0371 (4)
N13	0.35332 (18)	0.79829 (17)	0.06321 (8)	0.0355 (4)
N14	0.2555 (2)	0.67255 (18)	0.05076 (9)	0.0417 (5)
N15	0.2613 (2)	0.80215 (17)	0.19274 (8)	0.0392 (4)
N16	0.18466 (19)	0.67506 (17)	0.16040 (9)	0.0394 (4)
B3	0.2609 (3)	1.2407 (3)	0.12382 (14)	0.0416 (6)
H131	0.2353	1.3330	0.1195	0.050*
H132	0.3776	1.2697	0.1438	0.050*
B4	0.1259 (3)	0.6489 (3)	0.08607 (15)	0.0529 (8)
H141	0.0666	0.7180	0.0760	0.064*
H142	0.0515	0.5446	0.0685	0.064*
C17	0.1937 (2)	0.9652 (2)	−0.01456 (10)	0.0392 (5)
H17	0.1937	0.8806	−0.0331	0.047*
C18	0.1417 (2)	1.0454 (2)	−0.04878 (11)	0.0446 (6)
H18	0.1028	1.0275	−0.0933	0.054*
C19	0.1604 (2)	1.1577 (2)	−0.00225 (11)	0.0434 (6)
H19	0.1345	1.2309	−0.0099	0.052*
C20	0.0950 (2)	1.0121 (2)	0.22433 (10)	0.0397 (5)
H20	0.0825	0.9357	0.2416	0.048*
C21	0.0227 (2)	1.1007 (2)	0.23731 (12)	0.0477 (6)
H21	−0.0459	1.0965	0.2639	0.057*
C22	0.0743 (2)	1.1963 (2)	0.20234 (12)	0.0454 (6)
H22	0.0460	1.2708	0.2010	0.054*
C23	0.4538 (2)	0.7905 (2)	0.02772 (11)	0.0413 (5)
H23	0.5343	0.8622	0.0269	0.050*
C24	0.4222 (3)	0.6621 (2)	−0.00748 (12)	0.0504 (6)
H24	0.4745	0.6309	−0.0359	0.061*
C25	0.2968 (3)	0.5907 (2)	0.00871 (12)	0.0552 (7)
H25	0.2478	0.4997	−0.0070	0.066*
C26	0.3026 (3)	0.7955 (3)	0.25470 (11)	0.0468 (6)
H26	0.3574	0.8687	0.2878	0.061*
C27	0.2532 (3)	0.6657 (3)	0.26312 (13)	0.0518 (7)
H27	0.2667	0.6346	0.3015	0.062*
C28	0.1800 (3)	0.5931 (3)	0.20231 (14)	0.0528 (7)
H28	0.1341	0.5009	0.1917	0.063*
C29	0.5495 (3)	1.1229 (3)	0.24300 (11)	0.0568 (7)
H29A	0.5702	1.0603	0.2680	0.068*
H29B	0.4749	1.1517	0.2595	0.068*
C30	0.6819 (3)	1.2404 (3)	0.24905 (15)	0.0723 (9)
H30A	0.6713	1.3211	0.2727	0.087*
H30B	0.7649	1.2263	0.2723	0.087*
C31	0.6986 (3)	1.2519 (3)	0.18144 (16)	0.0779 (9)
H31A	0.6593	1.3177	0.1678	0.093*
H31B	0.7992	1.2777	0.1778	0.093*
C32	0.6176 (3)	1.1171 (3)	0.14106 (13)	0.0619 (8)
H32A	0.5793	1.1228	0.0972	0.074*
H32B	0.6793	1.0627	0.1378	0.074*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mg1	0.0325 (4)	0.0316 (4)	0.0349 (4)	0.0115 (3)	0.0066 (3)	0.0062 (3)
O1	0.0373 (9)	0.0460 (9)	0.0353 (8)	0.0136 (7)	0.0079 (7)	0.0099 (7)
N1	0.0396 (11)	0.0400 (11)	0.0355 (10)	0.0169 (9)	0.0076 (8)	0.0039 (8)
N2	0.0457 (11)	0.0402 (11)	0.0369 (10)	0.0230 (10)	0.0006 (9)	0.0012 (9)
N3	0.0385 (11)	0.0328 (10)	0.0438 (11)	0.0134 (9)	0.0037 (9)	0.0073 (9)
N4	0.0454 (11)	0.0301 (10)	0.0437 (11)	0.0120 (9)	0.0071 (9)	0.0068 (9)
N5	0.0335 (10)	0.0392 (11)	0.0422 (11)	0.0117 (9)	0.0059 (9)	0.0071 (9)
N6	0.0350 (10)	0.0454 (12)	0.0385 (11)	0.0089 (9)	0.0104 (9)	0.0107 (9)
N7	0.0314 (10)	0.0352 (10)	0.0466 (11)	0.0112 (8)	0.0099 (9)	0.0118 (9)
N8	0.0342 (10)	0.0351 (10)	0.0376 (10)	0.0087 (9)	0.0010 (8)	0.0091 (8)
B1	0.0553 (18)	0.0337 (15)	0.0453 (17)	0.0187 (14)	0.0027 (14)	0.0102 (13)
B2	0.0424 (16)	0.061 (2)	0.0362 (15)	0.0103 (15)	0.0055 (13)	0.0093 (15)
C1	0.0399 (13)	0.0599 (16)	0.0383 (13)	0.0172 (12)	0.0118 (11)	0.0035 (12)
C2	0.0504 (16)	0.081 (2)	0.0457 (15)	0.0369 (16)	0.0108 (12)	−0.0034 (14)
C3	0.0579 (16)	0.0561 (16)	0.0420 (14)	0.0380 (15)	−0.0016 (12)	−0.0053 (12)
C4	0.0368 (13)	0.0423 (14)	0.0573 (16)	0.0136 (11)	0.0005 (11)	0.0106 (12)
C5	0.0363 (14)	0.0465 (16)	0.0650 (17)	0.0022 (12)	−0.0010 (12)	0.0068 (13)
C6	0.0514 (15)	0.0312 (13)	0.0568 (16)	0.0046 (12)	0.0068 (13)	0.0050 (11)
C7	0.0342 (13)	0.0493 (15)	0.0463 (14)	0.0143 (12)	0.0003 (11)	0.0044 (12)
C8	0.0309 (13)	0.0445 (15)	0.0614 (16)	0.0026 (11)	0.0102 (12)	0.0004 (13)
C9	0.0428 (14)	0.0443 (15)	0.0542 (16)	0.0053 (12)	0.0185 (12)	0.0144 (12)
C10	0.0350 (13)	0.0459 (14)	0.0543 (15)	0.0140 (11)	0.0125 (11)	0.0112 (12)
C11	0.0430 (14)	0.0489 (15)	0.0622 (17)	0.0258 (13)	0.0033 (13)	0.0032 (13)
C12	0.0485 (15)	0.0384 (14)	0.0529 (15)	0.0169 (12)	−0.0049 (12)	0.0128 (12)
C13	0.0542 (17)	0.085 (2)	0.0513 (16)	0.0122 (15)	0.0240 (14)	0.0181 (15)
C14	0.099 (3)	0.121 (3)	0.0520 (19)	0.014 (2)	0.0218 (19)	0.0293 (19)
C15	0.123 (4)	0.123 (4)	0.0519 (12)	0.059 (3)	0.0148 (12)	0.0351 (12)
C16	0.0526 (16)	0.092 (2)	0.0431 (15)	0.0314 (16)	−0.0045 (13)	0.0086 (15)
Mg2	0.0341 (4)	0.0295 (4)	0.0309 (4)	0.0091 (3)	0.0042 (3)	0.0066 (3)
O2	0.0354 (8)	0.0402 (9)	0.0338 (8)	0.0069 (7)	0.0052 (7)	0.0009 (7)
N9	0.0339 (10)	0.0350 (10)	0.0333 (10)	0.0107 (8)	0.0078 (8)	0.0092 (8)
N10	0.0336 (10)	0.0340 (10)	0.0418 (11)	0.0102 (8)	0.0074 (8)	0.0154 (8)
N11	0.0357 (10)	0.0327 (10)	0.0346 (10)	0.0100 (8)	0.0070 (8)	0.0067 (8)
N12	0.0388 (11)	0.0302 (10)	0.0424 (11)	0.0130 (9)	0.0071 (9)	0.0057 (8)
N13	0.0370 (10)	0.0332 (10)	0.0351 (10)	0.0106 (9)	0.0058 (8)	0.0069 (8)
N14	0.0449 (11)	0.0346 (11)	0.0367 (11)	0.0057 (9)	0.0072 (9)	−0.0015 (9)
N15	0.0495 (12)	0.0309 (10)	0.0362 (11)	0.0122 (9)	0.0073 (9)	0.0073 (8)
N16	0.0419 (11)	0.0326 (11)	0.0452 (11)	0.0101 (9)	0.0164 (9)	0.0108 (9)
B3	0.0426 (16)	0.0327 (15)	0.0505 (17)	0.0130 (13)	0.0089 (13)	0.0104 (13)
B4	0.0458 (17)	0.0516 (19)	0.0467 (17)	0.0015 (15)	0.0073 (14)	0.0001 (15)
C17	0.0340 (12)	0.0460 (14)	0.0325 (12)	0.0072 (11)	0.0058 (10)	0.0070 (10)
C18	0.0345 (13)	0.0606 (16)	0.0356 (13)	0.0086 (12)	0.0032 (10)	0.0190 (12)
C19	0.0340 (12)	0.0518 (15)	0.0514 (15)	0.0143 (11)	0.0095 (11)	0.0292 (13)
C20	0.0378 (13)	0.0415 (13)	0.0361 (12)	0.0075 (11)	0.0071 (10)	0.0093 (10)
C21	0.0402 (14)	0.0561 (16)	0.0480 (14)	0.0156 (12)	0.0176 (11)	0.0080 (12)
C22	0.0438 (14)	0.0407 (14)	0.0549 (15)	0.0208 (12)	0.0113 (12)	0.0042 (12)
C23	0.0403 (13)	0.0431 (14)	0.0406 (13)	0.0122 (11)	0.0101 (11)	0.0108 (11)
C24	0.0582 (16)	0.0535 (16)	0.0430 (14)	0.0240 (14)	0.0169 (12)	0.0033 (12)
C25	0.0721 (19)	0.0356 (14)	0.0476 (15)	0.0091 (13)	0.0147 (14)	−0.0057 (12)
C26	0.0459 (14)	0.0556 (16)	0.0382 (13)	0.0138 (12)	0.0068 (11)	0.0156 (12)
C27	0.0463 (15)	0.0694 (18)	0.0546 (16)	0.0251 (14)	0.0188 (13)	0.0366 (14)
C28	0.0548 (16)	0.0414 (14)	0.0750 (19)	0.0234 (13)	0.0186 (15)	0.0272 (14)
C29	0.0510 (16)	0.0688 (18)	0.0356 (13)	0.0104 (14)	−0.0015 (12)	−0.0042 (13)
C30	0.0594 (18)	0.0569 (18)	0.074 (2)	0.0028 (15)	−0.0020 (16)	−0.0156 (16)
C31	0.0484 (17)	0.064 (2)	0.104 (3)	−0.0037 (15)	0.0067 (17)	0.0196 (18)
C32	0.0468 (15)	0.074 (2)	0.0520 (16)	0.0031 (14)	0.0155 (13)	0.0067 (14)

Geometric parameters (Å, º)

Mg1—O1	2.0397 (16)	Mg2—O2	2.0233 (17)
Mg1—N1	2.119 (2)	Mg2—N9	2.1199 (19)
Mg1—N3	2.150 (2)	Mg2—N11	2.1434 (19)
Mg1—N5	2.165 (2)	Mg2—N13	2.1642 (19)
Mg1—N7	2.126 (2)	Mg2—N15	2.1462 (19)
Mg1—H121	2.8100	O2—C32	1.434 (3)
O1—C13	1.439 (3)	O2—C29	1.444 (3)
O1—C16	1.445 (3)	N9—C17	1.339 (3)
N1—C1	1.340 (3)	N9—N10	1.368 (2)
N1—N2	1.367 (2)	N10—C19	1.338 (3)
N2—C3	1.330 (3)	B3—N10	1.545 (3)
B1—N2	1.546 (3)	N11—C20	1.338 (3)
N3—C4	1.334 (3)	N11—N12	1.368 (2)
N3—N4	1.369 (2)	N12—C22	1.338 (3)
N4—C6	1.338 (3)	B3—N12	1.554 (3)
B1—N4	1.547 (3)	B3—H131	1.1100
B1—H111	1.1100	B3—H132	1.1100
B1—H112	1.1100	N13—C23	1.336 (3)
N5—C7	1.340 (3)	N13—N14	1.361 (2)
N5—N6	1.361 (2)	N14—C25	1.337 (3)
N6—C9	1.339 (3)	B4—N14	1.543 (3)
B2—N6	1.549 (3)	N15—C26	1.333 (3)
N7—C10	1.331 (3)	N15—N16	1.356 (2)
N7—N8	1.356 (2)	N16—C28	1.335 (3)
N8—C12	1.331 (3)	B4—N16	1.543 (3)
B2—N8	1.550 (3)	B4—H141	1.1100
B2—H122	1.1100	B4—H142	1.1100
B2—H121	1.1100	C17—C18	1.378 (3)
C1—C2	1.374 (3)	C17—H17	0.9300
C1—H1	0.9300	C18—C19	1.373 (3)
C2—C3	1.371 (4)	C18—H18	0.9300
C2—H2	0.9300	C19—H19	0.9300
C3—H3	0.9300	C20—C21	1.373 (3)
C4—C5	1.380 (3)	C20—H20	0.9300
C4—H4	0.9300	C21—C22	1.367 (3)
C5—C6	1.365 (3)	C21—H21	0.9300
C5—H5	0.9300	C22—H22	0.9300
C6—H6	0.9300	C23—C24	1.377 (3)
C7—C8	1.376 (3)	C23—H23	0.9300
C7—H7	0.9300	C24—C25	1.365 (3)
C8—C9	1.362 (3)	C24—H24	0.9300
C8—H8	0.9300	C25—H25	0.9300
C9—H9	0.9300	C26—C27	1.376 (3)
C10—C11	1.379 (3)	C26—H26	0.9300
C10—H10	0.9300	C27—C28	1.365 (3)
C11—C12	1.363 (3)	C27—H27	0.9300
C11—H11	0.9300	C28—H28	0.9300
C12—H12	0.9300	C29—C30	1.492 (3)
C13—C14	1.472 (4)	C29—H29A	0.9700
C13—H13A	0.9700	C29—H29B	0.9700
C13—H13B	0.9700	C30—C31	1.470 (4)
C14—C15	1.454 (5)	C30—H30A	0.9700
C14—H14A	0.9700	C30—H30B	0.9700
C14—H14B	0.9700	C31—C32	1.476 (4)
C15—C16	1.486 (4)	C31—H31A	0.9700
C15—H15A	0.9700	C31—H31B	0.9700
C15—H15B	0.9700	C32—H32A	0.9700
C16—H16A	0.9700	C32—H32B	0.9700
C16—H16B	0.9700
O1—Mg1—N1	104.53 (7)	N7—C10—H10	124.00
O1—Mg1—N3	99.40 (7)	C10—C11—H11	128.00
O1—Mg1—N5	96.20 (7)	C12—C11—H11	128.00
O1—Mg1—N7	101.29 (7)	C11—C12—H12	125.00
N1—Mg1—N3	88.04 (8)	N8—C12—H12	125.00
N1—Mg1—N5	88.20 (8)	O1—C13—H13A	110.00
N1—Mg1—N7	154.11 (7)	C14—C13—H13B	110.00
N3—Mg1—N5	164.39 (8)	O1—C13—H13B	110.00
N3—Mg1—N7	89.74 (8)	H13A—C13—H13B	109.00
N5—Mg1—N7	87.06 (8)	C14—C13—H13A	110.00
N9—Mg2—N11	87.56 (7)	C13—C14—H14B	111.00
N11—Mg2—N15	88.92 (7)	C13—C14—H14A	111.00
N11—Mg2—B4	110.85 (8)	H14A—C14—H14B	109.00
N13—Mg2—N15	87.39 (7)	C15—C14—H14B	111.00
N13—Mg2—B4	54.35 (8)	C15—C14—H14A	111.00
N15—Mg2—B4	54.48 (8)	C16—C15—H15A	111.00
O2—Mg2—N9	106.50 (7)	C16—C15—H15B	111.00
O2—Mg2—N11	98.60 (7)	C14—C15—H15B	111.00
O2—Mg2—N13	98.16 (7)	C14—C15—H15A	111.00
O2—Mg2—N15	99.52 (7)	H15A—C15—H15B	109.00
O2—Mg2—B4	138.67 (8)	O1—C16—H16A	111.00
N9—Mg2—N13	88.60 (7)	O1—C16—H16B	111.00
N9—Mg2—N15	153.98 (8)	C15—C16—H16B	111.00
N9—Mg2—B4	103.19 (8)	H16A—C16—H16B	109.00
N11—Mg2—N13	163.21 (8)	C15—C16—H16A	111.00
Mg1—O1—C13	123.76 (14)	N9—C17—C18	111.34 (19)
Mg1—O1—C16	124.87 (14)	C17—C18—C19	104.38 (19)
C13—O1—C16	108.69 (18)	N10—C19—C18	109.21 (19)
Mg2—O2—C32	125.71 (14)	N11—C20—C21	111.44 (19)
C29—O2—C32	107.74 (19)	C20—C21—C22	104.33 (19)
Mg2—O2—C29	125.51 (16)	N12—C22—C21	109.58 (19)
Mg1—N1—N2	123.14 (15)	N13—C23—C24	111.0 (2)
Mg1—N1—C1	130.42 (18)	C23—C24—C25	104.6 (2)
N2—N1—C1	105.9 (2)	N14—C25—C24	109.2 (2)
C3—N2—B1	130.0 (2)	N15—C26—C27	111.0 (2)
N1—N2—B1	120.75 (19)	C26—C27—C28	104.3 (2)
N1—N2—C3	109.2 (2)	N16—C28—C27	109.4 (3)
Mg1—N3—N4	121.71 (15)	O2—C29—C30	106.9 (2)
Mg1—N3—C4	131.55 (15)	C29—C30—C31	105.9 (2)
N4—N3—C4	105.72 (17)	C30—C31—C32	104.8 (3)
N3—N4—C6	109.07 (19)	O2—C32—C31	105.8 (2)
C6—N4—B1	129.8 (2)	N9—C17—H17	124.00
N3—N4—B1	121.14 (19)	C18—C17—H17	124.00
Mg1—N5—C7	140.26 (16)	C19—C18—H18	128.00
Mg1—N5—N6	114.24 (14)	C17—C18—H18	128.00
N6—N5—C7	105.49 (18)	C18—C19—H19	125.00
N5—N6—B2	118.88 (19)	N10—C19—H19	125.00
N5—N6—C9	109.65 (19)	N11—C20—H20	124.00
C9—N6—B2	131.5 (2)	C21—C20—H20	124.00
Mg1—N7—C10	138.57 (15)	C22—C21—H21	128.00
N8—N7—C10	105.73 (18)	C20—C21—H21	128.00
Mg1—N7—N8	115.58 (14)	N12—C22—H22	125.00
N7—N8—B2	118.31 (19)	C21—C22—H22	125.00
N7—N8—C12	109.57 (18)	N13—C23—H23	124.00
C12—N8—B2	132.1 (2)	C24—C23—H23	124.00
N10—N9—C17	105.63 (17)	C25—C24—H24	128.00
Mg2—N9—N10	122.86 (13)	C23—C24—H24	128.00
Mg2—N9—C17	129.98 (15)	C24—C25—H25	125.00
C19—N10—B3	129.7 (2)	N14—C25—H25	125.00
N9—N10—B3	120.82 (18)	C27—C26—H26	125.00
N9—N10—C19	109.43 (17)	N15—C26—H26	125.00
Mg2—N11—N12	122.12 (13)	C28—C27—H27	128.00
Mg2—N11—C20	131.04 (15)	C26—C27—H27	128.00
N12—N11—C20	105.69 (17)	C27—C28—H28	125.00
N11—N12—C22	108.97 (17)	N16—C28—H28	125.00
N11—N12—B3	120.84 (19)	O2—C29—H29A	110.00
C22—N12—B3	130.2 (2)	C30—C29—H29B	110.00
Mg2—N13—N14	113.87 (14)	O2—C29—H29B	110.00
N14—N13—C23	105.90 (17)	C30—C29—H29A	110.00
Mg2—N13—C23	140.23 (15)	H29A—C29—H29B	109.00
N13—N14—C25	109.32 (19)	C31—C30—H30A	111.00
C25—N14—B4	132.5 (2)	C29—C30—H30A	111.00
N13—N14—B4	118.14 (19)	C31—C30—H30B	111.00
N16—N15—C26	106.24 (19)	H30A—C30—H30B	109.00
Mg2—N15—C26	139.37 (18)	C29—C30—H30B	111.00
Mg2—N15—N16	113.85 (12)	C30—C31—H31A	111.00
C28—N16—B4	132.2 (2)	C32—C31—H31B	111.00
N15—N16—C28	109.09 (19)	C32—C31—H31A	111.00
N15—N16—B4	118.70 (18)	H31A—C31—H31B	109.00
N1—C1—C2	110.9 (3)	C30—C31—H31B	111.00
C1—C2—C3	104.5 (3)	O2—C32—H32A	111.00
N2—C3—C2	109.5 (3)	H32A—C32—H32B	109.00
N3—C4—C5	111.3 (2)	C31—C32—H32A	111.00
C4—C5—C6	104.4 (2)	O2—C32—H32B	111.00
N4—C6—C5	109.5 (2)	C31—C32—H32B	111.00
N5—C7—C8	111.1 (2)	N2—B1—N4	108.9 (2)
C7—C8—C9	104.78 (19)	N6—B2—N8	107.6 (2)
N6—C9—C8	109.0 (2)	N2—B1—H111	110.00
N7—C10—C11	111.2 (2)	N2—B1—H112	110.00
C10—C11—C12	104.1 (2)	H111—B1—H112	109.00
N8—C12—C11	109.4 (2)	N4—B1—H112	110.00
O1—C13—C14	107.2 (3)	N4—B1—H111	110.00
C13—C14—C15	105.4 (3)	N8—B2—H122	110.00
C14—C15—C16	105.3 (3)	N8—B2—H121	110.00
O1—C16—C15	105.3 (3)	N6—B2—H121	110.00
C2—C1—H1	125.00	H122—B2—H121	109.00
N1—C1—H1	125.00	N6—B2—H122	110.00
C3—C2—H2	128.00	N10—B3—N12	107.9 (2)
C1—C2—H2	128.00	N14—B4—N16	107.7 (2)
N2—C3—H3	125.00	Mg2—B4—N16	72.82 (13)
C2—C3—H3	125.00	Mg2—B4—N14	73.62 (14)
C5—C4—H4	124.00	N10—B3—H131	110.00
N3—C4—H4	124.00	N10—B3—H132	110.00
C6—C5—H5	128.00	N12—B3—H131	110.00
C4—C5—H5	128.00	N12—B3—H132	110.00
N4—C6—H6	125.00	H131—B3—H132	108.00
C5—C6—H6	125.00	Mg2—B4—H141	65.00
C8—C7—H7	124.00	Mg2—B4—H142	174.00
N5—C7—H7	124.00	N14—B4—H141	110.00
C7—C8—H8	128.00	N14—B4—H142	110.00
C9—C8—H8	128.00	N16—B4—H141	110.00
C8—C9—H9	126.00	N16—B4—H142	110.00
N6—C9—H9	125.00	H141—B4—H142	109.00
C11—C10—H10	124.00
N1—Mg1—O1—C13	127.32 (18)	C1—N1—N2—B1	−178.3 (2)
N1—Mg1—O1—C16	−32.0 (2)	Mg1—N1—C1—C2	172.13 (16)
N3—Mg1—O1—C13	36.91 (19)	N2—N1—C1—C2	0.3 (2)
N3—Mg1—O1—C16	−122.43 (19)	B1—N2—C3—C2	178.2 (2)
N5—Mg1—O1—C13	−142.94 (18)	N1—N2—B1—N4	−58.5 (3)
N5—Mg1—O1—C16	57.72 (19)	C3—N2—B1—N4	124.3 (3)
N7—Mg1—O1—C13	−54.71 (19)	N1—N2—C3—C2	0.7 (3)
N7—Mg1—O1—C16	145.95 (18)	N4—N3—C4—C5	0.2 (3)
O1—Mg1—N1—N2	−70.60 (16)	Mg1—N3—N4—B1	−12.2 (3)
O1—Mg1—N1—C1	118.76 (19)	C4—N3—N4—C6	−0.1 (3)
N3—Mg1—N1—N2	28.61 (16)	Mg1—N3—N4—C6	169.57 (16)
N3—Mg1—N1—C1	−142.03 (19)	Mg1—N3—C4—C5	−168.08 (17)
N5—Mg1—N1—N2	−166.54 (16)	C4—N3—N4—B1	178.2 (2)
N5—Mg1—N1—C1	22.82 (19)	N3—N4—B1—N2	60.2 (3)
N7—Mg1—N1—N2	114.0 (2)	B1—N4—C6—C5	−178.1 (2)
N7—Mg1—N1—C1	−56.7 (3)	N3—N4—C6—C5	0.0 (3)
O1—Mg1—N3—N4	77.48 (16)	C6—N4—B1—N2	−121.9 (3)
O1—Mg1—N3—C4	−115.8 (2)	Mg1—N5—C7—C8	−178.34 (18)
N1—Mg1—N3—N4	−26.92 (16)	N6—N5—C7—C8	0.4 (2)
N1—Mg1—N3—C4	139.8 (2)	C7—N5—N6—B2	178.9 (2)
N7—Mg1—N3—N4	178.88 (16)	Mg1—N5—N6—C9	178.86 (14)
N7—Mg1—N3—C4	−14.4 (2)	Mg1—N5—N6—B2	−2.0 (2)
O1—Mg1—N5—N6	148.51 (15)	C7—N5—N6—C9	−0.3 (2)
O1—Mg1—N5—C7	−32.8 (3)	N5—N6—C9—C8	0.0 (3)
N1—Mg1—N5—N6	−107.08 (15)	B2—N6—C9—C8	−179.0 (2)
N1—Mg1—N5—C7	71.6 (2)	N5—N6—B2—N8	−62.7 (3)
N7—Mg1—N5—N6	47.46 (15)	C9—N6—B2—N8	116.2 (3)
N7—Mg1—N5—C7	−133.9 (2)	C10—N7—N8—C12	0.0 (2)
O1—Mg1—N7—N8	−139.90 (14)	C10—N7—N8—B2	178.9 (2)
O1—Mg1—N7—C10	35.6 (2)	Mg1—N7—N8—B2	−4.2 (2)
N1—Mg1—N7—N8	35.6 (3)	Mg1—N7—N8—C12	176.87 (15)
N1—Mg1—N7—C10	−148.9 (2)	Mg1—N7—C10—C11	−175.61 (18)
N3—Mg1—N7—N8	120.56 (14)	N8—N7—C10—C11	0.1 (3)
N3—Mg1—N7—C10	−64.0 (2)	N7—N8—C12—C11	−0.1 (3)
N5—Mg1—N7—N8	−44.16 (14)	N7—N8—B2—N6	67.3 (3)
N5—Mg1—N7—C10	131.3 (2)	C12—N8—B2—N6	−114.0 (3)
B4—Mg2—O2—C29	−98.2 (2)	B2—N8—C12—C11	−178.9 (2)
B4—Mg2—O2—C32	95.0 (2)	C17—N9—N10—C19	−0.5 (2)
O2—Mg2—N9—N10	−69.28 (17)	Mg2—N9—N10—C19	−167.65 (14)
O2—Mg2—N9—C17	126.97 (18)	Mg2—N9—N10—B3	10.3 (3)
N11—Mg2—N9—N10	28.97 (16)	N10—N9—C17—C18	1.1 (2)
N11—Mg2—N9—C17	−134.78 (19)	C17—N9—N10—B3	177.4 (2)
N13—Mg2—N9—N10	−167.38 (16)	Mg2—N9—C17—C18	166.93 (15)
N13—Mg2—N9—C17	28.87 (19)	B3—N10—C19—C18	−177.9 (2)
N15—Mg2—N9—N10	111.5 (2)	N9—N10—B3—N12	−60.0 (3)
N15—Mg2—N9—C17	−52.3 (3)	C19—N10—B3—N12	117.4 (2)
B4—Mg2—N9—N10	139.82 (16)	N9—N10—C19—C18	−0.2 (2)
B4—Mg2—N9—C17	−23.9 (2)	Mg2—N11—N12—C22	168.73 (15)
O2—Mg2—N11—N12	77.76 (16)	N12—N11—C20—C21	0.3 (2)
O2—Mg2—N11—C20	−116.37 (19)	C20—N11—N12—C22	−0.2 (2)
N9—Mg2—N11—N12	−28.55 (16)	C20—N11—N12—B3	−179.74 (19)
N9—Mg2—N11—C20	137.31 (19)	Mg2—N11—N12—B3	−10.8 (3)
N15—Mg2—N11—N12	177.23 (16)	Mg2—N11—C20—C21	−167.32 (16)
N15—Mg2—N11—C20	−16.90 (19)	N11—N12—C22—C21	0.1 (3)
B4—Mg2—N11—N12	−131.75 (15)	B3—N12—C22—C21	179.6 (2)
B4—Mg2—N11—C20	34.1 (2)	N11—N12—B3—N10	60.2 (3)
O2—Mg2—N13—N14	147.13 (14)	C22—N12—B3—N10	−119.2 (3)
O2—Mg2—N13—C23	−34.1 (2)	C23—N13—N14—B4	179.1 (2)
N9—Mg2—N13—N14	−106.41 (14)	Mg2—N13—N14—C25	179.41 (15)
N9—Mg2—N13—C23	72.4 (2)	Mg2—N13—C23—C24	−178.72 (18)
N15—Mg2—N13—N14	47.87 (14)	N14—N13—C23—C24	0.2 (2)
N15—Mg2—N13—C23	−133.3 (2)	Mg2—N13—N14—B4	−1.7 (2)
B4—Mg2—N13—N14	0.96 (13)	C23—N13—N14—C25	0.2 (2)
B4—Mg2—N13—C23	179.8 (3)	N13—N14—C25—C24	−0.5 (3)
O2—Mg2—N15—N16	−142.09 (15)	N13—N14—B4—Mg2	1.18 (16)
O2—Mg2—N15—C26	27.8 (3)	N13—N14—B4—N16	−64.2 (3)
N9—Mg2—N15—N16	37.2 (3)	B4—N14—C25—C24	−179.1 (2)
N9—Mg2—N15—C26	−152.9 (3)	C25—N14—B4—N16	114.3 (3)
N11—Mg2—N15—N16	119.37 (16)	C25—N14—B4—Mg2	179.7 (3)
N11—Mg2—N15—C26	−70.7 (3)	Mg2—N15—N16—B4	−4.7 (3)
N13—Mg2—N15—N16	−44.25 (16)	Mg2—N15—N16—C28	173.15 (18)
N13—Mg2—N15—C26	125.7 (3)	N16—N15—C26—C27	−0.3 (3)
B4—Mg2—N15—N16	2.57 (14)	C26—N15—N16—C28	0.0 (3)
B4—Mg2—N15—C26	172.5 (3)	C26—N15—N16—B4	−177.9 (2)
O2—Mg2—B4—N14	−57.36 (18)	Mg2—N15—C26—C27	−170.7 (2)
O2—Mg2—B4—N16	57.58 (18)	B4—N16—C28—C27	177.8 (3)
N9—Mg2—B4—N14	77.72 (14)	N15—N16—B4—Mg2	3.18 (18)
N9—Mg2—B4—N16	−167.34 (13)	N15—N16—B4—N14	69.1 (3)
N11—Mg2—B4—N14	170.15 (12)	N15—N16—C28—C27	0.3 (3)
N11—Mg2—B4—N16	−74.91 (15)	C28—N16—B4—Mg2	−174.1 (3)
N13—Mg2—B4—N14	−0.80 (11)	C28—N16—B4—N14	−108.2 (3)
N13—Mg2—B4—N16	114.14 (16)	N1—C1—C2—C3	0.1 (3)
N15—Mg2—B4—N14	−117.11 (16)	C1—C2—C3—N2	−0.5 (3)
N15—Mg2—B4—N16	−2.17 (12)	N3—C4—C5—C6	−0.2 (3)
N9—Mg2—O2—C29	127.62 (19)	C4—C5—C6—N4	0.1 (3)
N9—Mg2—O2—C32	−39.2 (2)	N5—C7—C8—C9	−0.4 (3)
N11—Mg2—O2—C29	37.63 (19)	C7—C8—C9—N6	0.2 (3)
N11—Mg2—O2—C32	−129.21 (19)	N7—C10—C11—C12	−0.2 (3)
N13—Mg2—O2—C29	−141.42 (19)	C10—C11—C12—N8	0.2 (3)
N13—Mg2—O2—C32	51.7 (2)	O1—C13—C14—C15	19.3 (4)
N15—Mg2—O2—C29	−52.71 (19)	C13—C14—C15—C16	−28.2 (4)
N15—Mg2—O2—C32	140.45 (19)	C14—C15—C16—O1	26.7 (3)
C16—O1—C13—C14	−2.6 (3)	N9—C17—C18—C19	−1.2 (2)
Mg1—O1—C16—C15	147.2 (2)	C17—C18—C19—N10	0.8 (2)
C13—O1—C16—C15	−14.8 (3)	N11—C20—C21—C22	−0.2 (3)
Mg1—O1—C13—C14	−164.8 (2)	C20—C21—C22—N12	0.1 (3)
Mg2—O2—C29—C30	−156.45 (18)	N13—C23—C24—C25	−0.4 (3)
C32—O2—C29—C30	12.4 (3)	C23—C24—C25—N14	0.6 (3)
C29—O2—C32—C31	−26.5 (3)	N15—C26—C27—C28	0.5 (4)
Mg2—O2—C32—C31	142.24 (18)	C26—C27—C28—N16	−0.5 (3)
Mg1—N1—N2—B1	9.1 (3)	O2—C29—C30—C31	6.6 (3)
C1—N1—N2—C3	−0.6 (2)	C29—C30—C31—C32	−22.4 (3)
Mg1—N1—N2—C3	−173.18 (15)	C30—C31—C32—O2	30.2 (3)

(IV) bis[dihydridobis(pyrazol-1-yl)borato- κ²N,N']bis(tetrahydrofuran-κO)magnesium(II)

Crystal data

[Mg(C6H8BN4)2(C4H8O)2]	Z = 2
Mr = 462.47	F(000) = 492
Triclinic, P1	Dx = 1.281 Mg m^−3
Hall symbol: -P 1	Mo Kα radiation, λ = 0.71073 Å
a = 9.4171 (19) Å	Cell parameters from 3579 reflections
b = 10.936 (2) Å	θ = 2.8–27.4°
c = 13.013 (3) Å	µ = 0.11 mm^−1
α = 94.069 (3)°	T = 150 K
β = 109.329 (3)°	Plate, colourless
γ = 105.568 (3)°	0.40 × 0.26 × 0.12 mm
V = 1199.3 (4) Å^3

Data collection

Bruker SMART APEX CCD area-detector diffractometer	6335 independent reflections
Radiation source: normal-focus sealed tube	4305 reflections with I > 2s(I)
Graphite monochromator	Rint = 0.022
ϕ and ω scans	θmax = 29.0°, θmin = 1.7°
Absorption correction: multi-scan (SADABS; Sheldrick, 1996)	h = −12→12
Tmin = 0.962, Tmax = 0.984	k = −14→14
10757 measured reflections	l = −17→16

Refinement

Refinement on F^2	Primary atom site location: structure-invariant direct methods
Least-squares matrix: full	Secondary atom site location: difference Fourier map
R[F^2 > 2σ(F^2)] = 0.043	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.109	H-atom parameters constrained
S = 1.01	w = 1/[σ^2(Fo^2) + (0.0564P)^2] where P = (Fo^2 + 2Fc^2)/3
5640 reflections	(Δ/σ)max < 0.001
329 parameters	Δρmax = 0.29 e Å^−3
48 restraints	Δρmin = −0.32 e Å^−3

Special details

Geometry. All e.s.d.'s (except the e.s.d. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell e.s.d.'s are taken into account individually in the estimation of e.s.d.'s in distances, angles and torsion angles; correlations between e.s.d.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell e.s.d.'s is used for estimating e.s.d.'s involving l.s. planes.

Refinement. Refinement of F² against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F², conventional R-factors R are based on F, with F set to zero for negative F². The threshold expression of F² > σ(F²) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F² are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.

The SHELX manual (pages 5-7 ff.) gives an example for the refinement of thf disorders.

The refinement of positional disorder in complex (IV) was resolved with two components and the use of similarity restraints. One disordered THF molecule is found in the asymmetric unit of complex (IV). All atoms of C7, C7A; C8, C8A; C9, C9A have a ratio of 82:18% occupancies.

According to the SHELX manual: the disordered THF was treated like in (II)

Fractional atomic coordinates and isotropic or equivalent isotropic displacement parameters (Ų)

	x	y	z	Uiso*/Ueq	Occ. (<1)
Mg1	0.0000	0.5000	0.5000	0.02050 (15)
B1	−0.04629 (19)	0.73840 (15)	0.34207 (13)	0.0248 (3)
H111	−0.0603	0.6625	0.2749	0.030*
H112	−0.0579	0.8260	0.3064	0.030*
N1	−0.18912 (13)	0.58921 (10)	0.44551 (9)	0.0224 (2)
N2	−0.17655 (13)	0.69135 (11)	0.39097 (9)	0.0229 (3)
N3	0.16663 (13)	0.68072 (11)	0.49479 (9)	0.0235 (3)
N4	0.11879 (13)	0.76930 (11)	0.43409 (9)	0.0235 (3)
C1	−0.32337 (16)	0.57231 (13)	0.46512 (11)	0.0251 (3)
H1	−0.3621	0.5078	0.5029	0.030*
C2	−0.39872 (17)	0.66062 (15)	0.42337 (12)	0.0300 (3)
H2	−0.4956	0.6684	0.4259	0.036*
C3	−0.30116 (16)	0.73438 (14)	0.37741 (12)	0.0284 (3)
H3	−0.3191	0.8046	0.3417	0.034*
C4	0.31938 (16)	0.73858 (14)	0.55675 (12)	0.0262 (3)
H4	0.3837	0.6997	0.6079	0.031*
C5	0.37184 (17)	0.86250 (14)	0.53678 (12)	0.0294 (3)
H5	0.4750	0.9229	0.5694	0.035*
C6	0.24047 (17)	0.87809 (14)	0.45896 (12)	0.0282 (3)
H6	0.2365	0.9537	0.4278	0.034*
O1	−0.04678 (11)	0.42908 (9)	0.32798 (8)	0.0264 (2)
C7	−0.2080 (8)	0.3834 (6)	0.2429 (4)	0.0280 (10)	0.822 (8)
H7A	−0.2748	0.4331	0.2581	0.034*	0.822 (8)
H7B	−0.2588	0.2908	0.2403	0.034*	0.822 (8)
C8	−0.1838 (3)	0.4059 (3)	0.13425 (17)	0.0343 (7)	0.822 (8)
H8A	−0.1802	0.4946	0.1213	0.041*	0.822 (8)
H8B	−0.2685	0.3434	0.0705	0.041*	0.822 (8)
C9	−0.0232 (4)	0.3844 (4)	0.1541 (3)	0.0351 (7)	0.822 (8)
H9A	0.0279	0.4273	0.1053	0.042*	0.822 (8)
H9B	−0.0343	0.2913	0.1421	0.042*	0.822 (8)
C7A	−0.181 (4)	0.391 (3)	0.239 (2)	0.035 (6)	0.178 (8)
H7C	−0.2263	0.4633	0.2271	0.042*	0.178 (8)
H7D	−0.2587	0.3183	0.2506	0.042*	0.178 (8)
C8A	−0.1486 (16)	0.3518 (14)	0.1400 (8)	0.039 (3)	0.178 (8)
H8C	−0.1427	0.2626	0.1359	0.047*	0.178 (8)
H8D	−0.2304	0.3580	0.0712	0.047*	0.178 (8)
C9A	−0.003 (2)	0.4409 (16)	0.1583 (13)	0.036 (3)	0.178 (8)
H9C	−0.0126	0.5253	0.1399	0.044*	0.178 (8)
H9D	0.0552	0.4092	0.1166	0.044*	0.178 (8)
C10	0.07112 (18)	0.44706 (15)	0.27670 (12)	0.0321 (3)
H10A	0.1508	0.4043	0.3114	0.039*	0.822 (8)
H10B	0.1258	0.5399	0.2836	0.039*	0.822 (8)
H10C	0.1233	0.3792	0.2903	0.039*	0.178 (8)
H10D	0.1531	0.5318	0.3100	0.039*	0.178 (8)
Mg2	0.0000	0.0000	0.0000	0.02217 (16)
B2	0.2528 (2)	0.16144 (18)	0.25980 (14)	0.0306 (4)
H121	0.3001	0.0790	0.2571	0.037*
H122	0.3230	0.2261	0.3409	0.037*
N5	0.19556 (13)	0.18107 (11)	0.05523 (9)	0.0261 (3)
N6	0.26897 (13)	0.23649 (11)	0.16452 (10)	0.0276 (3)
N7	−0.03770 (13)	0.03360 (11)	0.15384 (9)	0.0248 (3)
N8	0.07719 (14)	0.11116 (11)	0.24755 (9)	0.0267 (3)
C11	0.24899 (17)	0.26960 (14)	−0.00065 (13)	0.0318 (3)
H11	0.2182	0.2575	−0.0789	0.038*
C12	0.35513 (18)	0.38112 (15)	0.07095 (14)	0.0379 (4)
H12	0.4098	0.4577	0.0526	0.045*
C13	0.36348 (17)	0.35593 (15)	0.17444 (14)	0.0356 (4)
H13	0.4263	0.4140	0.2421	0.043*
C14	−0.17223 (17)	0.00927 (14)	0.17360 (12)	0.0284 (3)
H14	−0.2726	−0.0428	0.1224	0.034*
C15	−0.14670 (19)	0.06956 (14)	0.27820 (12)	0.0318 (3)
H15	−0.2226	0.0676	0.3118	0.038*
C16	0.01282 (19)	0.13276 (14)	0.32233 (12)	0.0309 (3)
H16	0.0688	0.1836	0.3941	0.037*
O2	0.16676 (11)	−0.10620 (10)	0.07066 (8)	0.0278 (2)
C17	0.14011 (18)	−0.19947 (16)	0.14101 (13)	0.0356 (4)
H17A	0.0446	−0.2734	0.0996	0.043*
H17B	0.1249	−0.1596	0.2057	0.043*
C18	0.2846 (2)	−0.24368 (18)	0.17809 (15)	0.0439 (4)
H18A	0.3088	−0.2608	0.2547	0.053*
H18B	0.2698	−0.3227	0.1285	0.053*
C19	0.41319 (19)	−0.13236 (17)	0.17139 (15)	0.0429 (4)
H19A	0.4958	−0.1622	0.1562	0.052*
H19B	0.4628	−0.0687	0.2411	0.052*
C20	0.32851 (17)	−0.07517 (15)	0.07656 (13)	0.0319 (3)
H20A	0.3780	0.0194	0.0900	0.038*
H20B	0.3329	−0.1126	0.0065	0.038*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Mg1	0.0190 (3)	0.0198 (3)	0.0248 (3)	0.0089 (3)	0.0079 (3)	0.0068 (3)
B1	0.0265 (8)	0.0256 (8)	0.0257 (8)	0.0110 (7)	0.0101 (7)	0.0106 (6)
N1	0.0225 (6)	0.0221 (6)	0.0247 (6)	0.0098 (5)	0.0084 (5)	0.0074 (5)
N2	0.0229 (6)	0.0225 (6)	0.0250 (6)	0.0107 (5)	0.0072 (5)	0.0077 (5)
N3	0.0227 (6)	0.0237 (6)	0.0285 (6)	0.0116 (5)	0.0103 (5)	0.0098 (5)
N4	0.0246 (6)	0.0220 (6)	0.0281 (6)	0.0102 (5)	0.0117 (5)	0.0092 (5)
C1	0.0223 (7)	0.0273 (7)	0.0271 (7)	0.0093 (6)	0.0092 (6)	0.0060 (6)
C2	0.0233 (7)	0.0375 (9)	0.0342 (8)	0.0166 (6)	0.0105 (6)	0.0091 (7)
C3	0.0258 (7)	0.0321 (8)	0.0312 (8)	0.0175 (6)	0.0075 (6)	0.0100 (6)
C4	0.0217 (7)	0.0285 (8)	0.0303 (8)	0.0103 (6)	0.0093 (6)	0.0073 (6)
C5	0.0238 (7)	0.0273 (8)	0.0345 (8)	0.0030 (6)	0.0113 (6)	0.0055 (6)
C6	0.0298 (8)	0.0225 (7)	0.0341 (8)	0.0066 (6)	0.0144 (6)	0.0085 (6)
O1	0.0271 (5)	0.0290 (5)	0.0258 (5)	0.0117 (4)	0.0103 (4)	0.0064 (4)
C7	0.022 (2)	0.0348 (19)	0.0215 (15)	0.0047 (15)	0.0037 (13)	0.0024 (11)
C8	0.0412 (13)	0.0355 (14)	0.0259 (11)	0.0185 (11)	0.0067 (9)	0.0046 (9)
C9	0.0422 (15)	0.0397 (18)	0.0305 (12)	0.0209 (17)	0.0151 (10)	0.0086 (16)
C7A	0.025 (9)	0.015 (7)	0.073 (12)	0.003 (6)	0.029 (7)	0.008 (6)
C8A	0.062 (8)	0.041 (7)	0.023 (5)	0.031 (6)	0.013 (5)	0.004 (4)
C9A	0.063 (8)	0.035 (7)	0.030 (5)	0.032 (8)	0.026 (5)	0.013 (7)
C10	0.0358 (9)	0.0383 (9)	0.0329 (8)	0.0194 (7)	0.0187 (7)	0.0108 (7)
Mg2	0.0218 (3)	0.0246 (3)	0.0203 (3)	0.0088 (3)	0.0067 (3)	0.0039 (3)
B2	0.0296 (9)	0.0371 (10)	0.0232 (8)	0.0144 (7)	0.0045 (7)	0.0019 (7)
N5	0.0247 (6)	0.0280 (7)	0.0244 (6)	0.0088 (5)	0.0073 (5)	0.0036 (5)
N6	0.0221 (6)	0.0296 (7)	0.0277 (6)	0.0093 (5)	0.0046 (5)	0.0005 (5)
N7	0.0257 (6)	0.0273 (6)	0.0219 (6)	0.0110 (5)	0.0070 (5)	0.0050 (5)
N8	0.0325 (7)	0.0275 (6)	0.0207 (6)	0.0139 (5)	0.0071 (5)	0.0037 (5)
C11	0.0295 (8)	0.0332 (8)	0.0356 (8)	0.0109 (7)	0.0138 (7)	0.0096 (7)
C12	0.0296 (8)	0.0302 (8)	0.0515 (10)	0.0045 (7)	0.0151 (7)	0.0092 (7)
C13	0.0250 (8)	0.0331 (9)	0.0409 (9)	0.0053 (6)	0.0071 (7)	−0.0034 (7)
C14	0.0297 (8)	0.0294 (8)	0.0303 (8)	0.0128 (6)	0.0125 (6)	0.0094 (6)
C15	0.0433 (9)	0.0297 (8)	0.0360 (8)	0.0192 (7)	0.0241 (7)	0.0119 (6)
C16	0.0451 (9)	0.0279 (8)	0.0251 (7)	0.0169 (7)	0.0148 (7)	0.0054 (6)
O2	0.0256 (5)	0.0340 (6)	0.0281 (5)	0.0138 (4)	0.0102 (4)	0.0126 (4)
C17	0.0338 (8)	0.0403 (9)	0.0377 (9)	0.0154 (7)	0.0136 (7)	0.0194 (7)
C18	0.0407 (10)	0.0557 (11)	0.0483 (10)	0.0274 (9)	0.0188 (8)	0.0284 (9)
C19	0.0311 (9)	0.0542 (11)	0.0484 (10)	0.0216 (8)	0.0115 (8)	0.0210 (8)
C20	0.0290 (8)	0.0368 (9)	0.0370 (9)	0.0157 (7)	0.0156 (7)	0.0126 (7)

Geometric parameters (Å, º)

Mg1—O1^i	2.1735 (10)	C9A—H9C	0.9900
Mg1—O1	2.1735 (10)	C9A—H9D	0.9900
Mg1—N1	2.1958 (11)	C10—H10A	0.9900
Mg1—N1^i	2.1958 (11)	C10—H10B	0.9900
Mg1—N3	2.1904 (11)	C10—H10C	0.9900
Mg1—N3^i	2.1904 (12)	C10—H10D	0.9900
B1—N2	1.5487 (19)	Mg2—N5	2.1894 (12)
B1—N4	1.5470 (19)	Mg2—N5^ii	2.1894 (12)
B1—H111	1.1100	Mg2—N7	2.1690 (12)
B1—H112	1.1100	Mg2—N7^ii	2.1690 (12)
N1—C1	1.3388 (17)	Mg2—O2^ii	2.1989 (10)
N1—N2	1.3648 (15)	Mg2—O2	2.1989 (10)
N2—C3	1.3419 (17)	B2—N6	1.561 (2)
N3—C4	1.3382 (17)	B2—N8	1.545 (2)
N3—N4	1.3684 (15)	B2—H121	1.1100
N4—C6	1.3421 (18)	B2—H122	1.1100
C1—C2	1.3850 (19)	N5—C11	1.3416 (18)
C1—H1	0.9500	N5—N6	1.3673 (16)
C2—C3	1.374 (2)	N6—C13	1.3382 (19)
C2—H2	0.9500	N7—C14	1.3365 (18)
C3—H3	0.9500	N7—N8	1.3654 (16)
C4—C5	1.387 (2)	N8—C16	1.3434 (18)
C4—H4	0.9500	C11—C12	1.387 (2)
C5—C6	1.376 (2)	C11—H11	0.9500
C5—H5	0.9500	C12—C13	1.375 (2)
C6—H6	0.9500	C12—H12	0.9500
O1—C7A	1.34 (3)	C13—H13	0.9500
O1—C10	1.4521 (16)	C14—C15	1.384 (2)
O1—C7	1.477 (6)	C14—H14	0.9500
C7—C8	1.531 (6)	C15—C16	1.371 (2)
C7—H7A	0.9900	C15—H15	0.9500
C7—H7B	0.9900	C16—H16	0.9500
C8—C9	1.533 (5)	O2—C20	1.4431 (17)
C8—H8A	0.9900	O2—C17	1.4451 (17)
C8—H8B	0.9900	C17—C18	1.506 (2)
C9—C10	1.544 (4)	C17—H17A	0.9900
C9—H9A	0.9900	C17—H17B	0.9900
C9—H9B	0.9900	C18—C19	1.500 (2)
C7A—C8A	1.48 (3)	C18—H18A	0.9900
C7A—H7C	0.9900	C18—H18B	0.9900
C7A—H7D	0.9900	C19—C20	1.509 (2)
C8A—C9A	1.39 (2)	C19—H19A	0.9900
C8A—H8C	0.9900	C19—H19B	0.9900
C8A—H8D	0.9900	C20—H20A	0.9900
C9A—C10	1.454 (16)	C20—H20B	0.9900
O1^i—Mg1—O1	180.0	O1—C10—H10A	110.8
O1^i—Mg1—N3	89.41 (4)	C9A—C10—H10A	124.8
O1—Mg1—N3	90.59 (4)	C9—C10—H10A	110.8
O1^i—Mg1—N3^i	90.59 (4)	O1—C10—H10B	110.8
O1—Mg1—N3^i	89.41 (4)	C9A—C10—H10B	88.8
N3—Mg1—N3^i	180.0	C9—C10—H10B	110.8
O1^i—Mg1—N1	90.63 (4)	H10A—C10—H10B	108.9
O1—Mg1—N1	89.37 (4)	O1—C10—H10C	109.6
N1—Mg1—N3	88.24 (4)	C9A—C10—H10C	109.6
N1^i—Mg1—N3	91.76 (4)	C9—C10—H10C	92.3
O1^i—Mg1—N1^i	89.37 (4)	H10B—C10—H10C	125.4
O1—Mg1—N1^i	90.63 (4)	O1—C10—H10D	109.6
N3—Mg1—N1^i	91.76 (4)	C9A—C10—H10D	109.6
N3^i—Mg1—N1^i	88.24 (4)	C9—C10—H10D	130.3
N1—Mg1—N1^i	180.000 (1)	H10A—C10—H10D	89.2
N4—B1—N2	109.65 (11)	H10C—C10—H10D	108.1
N4—B1—H111	109.7	N5—Mg2—N7	88.99 (4)
N2—B1—H111	109.7	N5^ii—Mg2—N7	91.01 (4)
N4—B1—H112	109.7	N7—Mg2—N7^ii	180.00 (6)
N2—B1—H112	109.7	N7—Mg2—N5^ii	91.01 (4)
H111—B1—H112	108.2	N7^ii—Mg2—N5^ii	88.99 (4)
C1—N1—N2	105.52 (11)	N5—Mg2—N5^ii	180.0
C1—N1—Mg1	131.81 (9)	N7—Mg2—O2^ii	87.59 (4)
N2—N1—Mg1	122.27 (8)	N7^ii—Mg2—O2^ii	92.41 (4)
C3—N2—N1	109.71 (11)	N5—Mg2—O2^ii	89.86 (4)
C3—N2—B1	126.14 (12)	N5^ii—Mg2—O2^ii	90.14 (4)
N1—N2—B1	123.83 (11)	N7—Mg2—O2	92.41 (4)
C4—N3—N4	105.62 (11)	N7^ii—Mg2—O2	87.59 (4)
C4—N3—Mg1	131.10 (9)	N5—Mg2—O2	90.14 (4)
N4—N3—Mg1	122.44 (8)	N5^ii—Mg2—O2	89.86 (4)
C6—N4—N3	109.69 (11)	O2^ii—Mg2—O2	180.00 (4)
C6—N4—B1	126.71 (12)	N8—B2—N6	110.08 (12)
N3—N4—B1	123.24 (11)	N8—B2—H121	109.6
N1—C1—C2	111.53 (13)	N6—B2—H121	109.6
N1—C1—H1	124.2	N8—B2—H122	109.6
C2—C1—H1	124.2	N6—B2—H122	109.6
C3—C2—C1	104.13 (12)	H121—B2—H122	108.2
C3—C2—H2	127.9	C11—N5—N6	105.74 (12)
C1—C2—H2	127.9	C11—N5—Mg2	131.64 (10)
N2—C3—C2	109.11 (13)	N6—N5—Mg2	121.55 (9)
N2—C3—H3	125.4	C13—N6—N5	109.73 (12)
C2—C3—H3	125.4	C13—N6—B2	127.24 (13)
N3—C4—C5	111.41 (13)	N5—N6—B2	122.76 (11)
N3—C4—H4	124.3	C14—N7—N8	105.59 (11)
C5—C4—H4	124.3	C14—N7—Mg2	130.10 (10)
C6—C5—C4	104.26 (13)	N8—N7—Mg2	123.09 (9)
C6—C5—H5	127.9	C16—N8—N7	109.68 (12)
C4—C5—H5	127.9	C16—N8—B2	127.87 (12)
N4—C6—C5	109.02 (13)	N7—N8—B2	122.45 (11)
N4—C6—H6	125.5	N5—C11—C12	110.99 (14)
C5—C6—H6	125.5	N5—C11—H11	124.5
C7A—O1—C10	101.0 (14)	C12—C11—H11	124.5
C10—O1—C7	110.5 (3)	C13—C12—C11	104.50 (14)
C7A—O1—Mg1	131.5 (14)	C13—C12—H12	127.7
C10—O1—Mg1	125.35 (8)	C11—C12—H12	127.7
C7—O1—Mg1	122.7 (3)	N6—C13—C12	109.04 (14)
O1—C7—C8	104.6 (4)	N6—C13—H13	125.5
O1—C7—H7A	110.8	C12—C13—H13	125.5
C8—C7—H7A	110.8	N7—C14—C15	111.41 (13)
O1—C7—H7B	110.8	N7—C14—H14	124.3
C8—C7—H7B	110.8	C15—C14—H14	124.3
H7A—C7—H7B	108.9	C16—C15—C14	104.40 (13)
C7—C8—C9	102.2 (3)	C16—C15—H15	127.8
C7—C8—H8A	111.3	C14—C15—H15	127.8
C9—C8—H8A	111.3	N8—C16—C15	108.92 (13)
C7—C8—H8B	111.3	N8—C16—H16	125.5
C9—C8—H8B	111.3	C15—C16—H16	125.5
H8A—C8—H8B	109.2	C20—O2—C17	109.32 (10)
C8—C9—C10	102.5 (2)	C20—O2—Mg2	126.35 (8)
C8—C9—H9A	111.3	C17—O2—Mg2	122.91 (8)
C10—C9—H9A	111.3	O2—C17—C18	106.75 (12)
C8—C9—H9B	111.3	O2—C17—H17A	110.4
C10—C9—H9B	111.3	C18—C17—H17A	110.4
H9A—C9—H9B	109.2	O2—C17—H17B	110.4
O1—C7A—C8A	110 (2)	C18—C17—H17B	110.4
O1—C7A—H7C	109.6	H17A—C17—H17B	108.6
C8A—C7A—H7C	109.6	C19—C18—C17	103.59 (13)
O1—C7A—H7D	109.6	C19—C18—H18A	111.0
C8A—C7A—H7D	109.6	C17—C18—H18A	111.0
H7C—C7A—H7D	108.1	C19—C18—H18B	111.0
C9A—C8A—C7A	102.0 (16)	C17—C18—H18B	111.0
C9A—C8A—H8C	111.4	H18A—C18—H18B	109.0
C7A—C8A—H8C	111.4	C18—C19—C20	103.87 (13)
C9A—C8A—H8D	111.4	C18—C19—H19A	111.0
C7A—C8A—H8D	111.4	C20—C19—H19A	111.0
H8C—C8A—H8D	109.2	C18—C19—H19B	111.0
C8A—C9A—C10	99.0 (12)	C20—C19—H19B	111.0
C8A—C9A—H9C	112.0	H19A—C19—H19B	109.0
C10—C9A—H9C	112.0	O2—C20—C19	106.31 (12)
C8A—C9A—H9D	112.0	O2—C20—H20A	110.5
C10—C9A—H9D	112.0	C19—C20—H20A	110.5
H9C—C9A—H9D	109.6	O2—C20—H20B	110.5
O1—C10—C9A	110.3 (7)	C19—C20—H20B	110.5
O1—C10—C9	104.84 (17)	H20A—C20—H20B	108.7
O1^i—Mg1—N1—C1	−59.76 (12)	Mg1—O1—C10—C9A	−154.8 (7)
O1—Mg1—N1—C1	120.24 (12)	C7A—O1—C10—C9	−12.4 (13)
N3—Mg1—N1—C1	−149.14 (12)	C7—O1—C10—C9	−11.0 (3)
N3^i—Mg1—N1—C1	30.86 (12)	Mg1—O1—C10—C9	−177.59 (15)
O1^i—Mg1—N1—N2	111.81 (9)	C8A—C9A—C10—O1	−33.1 (14)
O1—Mg1—N1—N2	−68.19 (9)	C8A—C9A—C10—C9	46.5 (18)
N3—Mg1—N1—N2	22.42 (10)	C8—C9—C10—O1	31.1 (3)
N3^i—Mg1—N1—N2	−157.58 (10)	C8—C9—C10—C9A	−76.3 (19)
C1—N1—N2—C3	−0.42 (15)	N7—Mg2—N5—C11	−146.23 (13)
Mg1—N1—N2—C3	−173.90 (9)	N7^ii—Mg2—N5—C11	33.77 (13)
C1—N1—N2—B1	−174.34 (12)	O2^ii—Mg2—N5—C11	−58.64 (13)
Mg1—N1—N2—B1	12.18 (16)	O2—Mg2—N5—C11	121.36 (13)
N4—B1—N2—C3	130.94 (14)	N7—Mg2—N5—N6	20.16 (10)
N4—B1—N2—N1	−56.15 (16)	N7^ii—Mg2—N5—N6	−159.84 (10)
O1^i—Mg1—N3—C4	56.58 (12)	O2^ii—Mg2—N5—N6	107.75 (10)
O1—Mg1—N3—C4	−123.42 (12)	O2—Mg2—N5—N6	−72.25 (10)
N1—Mg1—N3—C4	147.23 (12)	C11—N5—N6—C13	0.48 (15)
N1^i—Mg1—N3—C4	−32.77 (12)	Mg2—N5—N6—C13	−168.99 (9)
O1^i—Mg1—N3—N4	−111.35 (10)	C11—N5—N6—B2	−173.97 (13)
O1—Mg1—N3—N4	68.65 (10)	Mg2—N5—N6—B2	16.56 (16)
N1—Mg1—N3—N4	−20.70 (10)	N8—B2—N6—C13	127.09 (15)
N1^i—Mg1—N3—N4	159.30 (10)	N8—B2—N6—N5	−59.48 (17)
C4—N3—N4—C6	0.12 (14)	N5—Mg2—N7—C14	142.75 (12)
Mg1—N3—N4—C6	170.70 (9)	N5^ii—Mg2—N7—C14	−37.25 (12)
C4—N3—N4—B1	173.70 (12)	O2^ii—Mg2—N7—C14	52.85 (12)
Mg1—N3—N4—B1	−15.72 (16)	O2—Mg2—N7—C14	−127.15 (12)
N2—B1—N4—C6	−129.39 (14)	N5—Mg2—N7—N8	−22.70 (10)
N2—B1—N4—N3	58.15 (16)	N5^ii—Mg2—N7—N8	157.30 (10)
N2—N1—C1—C2	0.62 (15)	O2^ii—Mg2—N7—N8	−112.60 (10)
Mg1—N1—C1—C2	173.23 (10)	O2—Mg2—N7—N8	67.40 (10)
N1—C1—C2—C3	−0.58 (16)	C14—N7—N8—C16	0.14 (15)
N1—N2—C3—C2	0.07 (16)	Mg2—N7—N8—C16	168.63 (9)
B1—N2—C3—C2	173.82 (13)	C14—N7—N8—B2	179.54 (12)
C1—C2—C3—N2	0.30 (16)	Mg2—N7—N8—B2	−11.97 (17)
N4—N3—C4—C5	−0.49 (15)	N6—B2—N8—C16	−124.14 (15)
Mg1—N3—C4—C5	−169.93 (10)	N6—B2—N8—N7	56.57 (17)
N3—C4—C5—C6	0.66 (17)	N6—N5—C11—C12	−0.20 (16)
N3—N4—C6—C5	0.29 (16)	Mg2—N5—C11—C12	167.78 (10)
B1—N4—C6—C5	−173.01 (13)	N5—C11—C12—C13	−0.14 (18)
C4—C5—C6—N4	−0.56 (16)	N5—N6—C13—C12	−0.58 (17)
N3—Mg1—O1—C7A	−120.6 (17)	B2—N6—C13—C12	173.55 (14)
N3^i—Mg1—O1—C7A	59.4 (17)	C11—C12—C13—N6	0.44 (17)
N1—Mg1—O1—C7A	−32.3 (17)	N8—N7—C14—C15	0.02 (16)
N1^i—Mg1—O1—C7A	147.7 (17)	Mg2—N7—C14—C15	−167.36 (10)
N3—Mg1—O1—C10	39.92 (10)	N7—C14—C15—C16	−0.16 (16)
N3^i—Mg1—O1—C10	−140.08 (10)	N7—N8—C16—C15	−0.24 (16)
N1—Mg1—O1—C10	128.15 (10)	B2—N8—C16—C15	−179.60 (13)
N1^i—Mg1—O1—C10	−51.85 (10)	C14—C15—C16—N8	0.24 (16)
N3—Mg1—O1—C7	−125.1 (3)	N7—Mg2—O2—C20	−122.48 (11)
N3^i—Mg1—O1—C7	54.9 (3)	N7^ii—Mg2—O2—C20	57.52 (11)
N1—Mg1—O1—C7	−36.9 (3)	N5—Mg2—O2—C20	−33.49 (11)
N1^i—Mg1—O1—C7	143.1 (3)	N5^ii—Mg2—O2—C20	146.51 (11)
C7A—O1—C7—C8	−6 (9)	N7—Mg2—O2—C17	42.42 (11)
C10—O1—C7—C8	−13.7 (5)	N7^ii—Mg2—O2—C17	−137.58 (11)
Mg1—O1—C7—C8	153.3 (2)	N5—Mg2—O2—C17	131.42 (11)
O1—C7—C8—C9	32.6 (5)	N5^ii—Mg2—O2—C17	−48.58 (11)
C7—C8—C9—C10	−38.9 (4)	C20—O2—C17—C18	−9.14 (17)
C10—O1—C7A—C8A	16 (2)	Mg2—O2—C17—C18	−176.30 (10)
C7—O1—C7A—C8A	−156 (10)	O2—C17—C18—C19	25.68 (18)
Mg1—O1—C7A—C8A	179.7 (9)	C17—C18—C19—C20	−31.76 (18)
O1—C7A—C8A—C9A	−38 (2)	C17—O2—C20—C19	−11.19 (16)
C7A—C8A—C9A—C10	39.5 (18)	Mg2—O2—C20—C19	155.42 (10)
C7A—O1—C10—C9A	10.5 (14)	C18—C19—C20—O2	26.97 (17)
C7—O1—C10—C9A	11.8 (7)

Symmetry codes: (i) −x, −y+1, −z+1; (ii) −x, −y, −z.