Synthesis, structural, characterization and Hirshfeld analysis of a bis­selenide and a zinc com­plex of a new hemilabile ferrocenylbisphos­phane, [Fe{C₅H₄P(C₆H₄CH₂NMe₂-o)₂}₂]

The novel hemilabile ferrocenylbisphosphane 1,1′-bis­(bis­{2-[(di­methyl­amino)­meth­yl]phen­yl}phosphan­yl)ferrocene, [Fe{C₅H₄P(C₆H₄CH₂NMe₂-o)₂}₂] (1), was synthesized by reacting bis­(di­chloro­phosphan­yl)ferrocene, [Fe{C₅H₄(PCl₂)}₂] with LiC₆H₄CH₂NMe₂-o. Treatment of 1 with gray selenium and anhydrous ZnCl₂ yielded, respectively, the bis­selenide (ferrocene-1,1′-di­yl)bis­(bis­{2-[(di­methyl­amino)­meth­yl]phen­yl}phosphine selenide), [Fe(C₂₃H₂₈N₂PSe)₂] (2), and the dizinc com­plex [μ-1,1′-bis­(bis­{2-[(di­methyl­amino)­meth­yl]phen­yl}phosphan­yl)ferrocene-κ²N,P:κ²N′,P′]bis­[di­chlorido­zinc(II)] di­chloro­methane monosolvate, [FeZn₂Cl₄(C₂₃H₂₈N₂P)₂]·CH₂Cl₂ (3), and both have been structurally characterized. Both com­pounds crystallized with the asymmetric unit containing half a mol­ecule and with the Fe atom on an inversion centre. A Hirshfeld surface analysis indicated that the most significant contributions to the crystal packing of 2 are from H...H (76.7%), C...H/H...C (13.2%) and Se...H/H...Se (7.1%) contacts, while those for 3 are from H...H (62.3%), Cl...H/H...Cl (24.4%) and C...H/H...C (10.9%) contacts.

Computing details

Data collection: APEX2 (Bruker, 2015) for Compound_2; APEX3 (Bruker, 2016) for Compound_3. Cell refinement: SAINT (Bruker, 2015) for Compound_2; SAINT (Bruker, 2016) for Compound_3. Data reduction: SAINT (Bruker, 2015) for Compound_2; SAINT (Bruker, 2016) for Compound_3. Program(s) used to solve structure: SHELXT (Sheldrick, 2015a) for Compound_2; SHELXT (Sheldrick, 2015a) for Compound_3. Program(s) used to refine structure: SHELXL (Sheldrick, 2015b) for Compound_2; SHELXL2014 (Sheldrick, 2015b) for Compound_3. For both structures, molecular graphics: DIAMOND (Brandenburg & Putz, 2012). Software used to prepare material for publication: SHELXTL (Bruker, 2015) and CELL_NOW (Sheldrick, 2008) for Compound_2; SHELXTL (Bruker, 2016) for Compound_3.

(Ferrocene-1,1'-diyl)bis(bis{2-[(dimethylamino)methyl]phenyl}phosphine selenide) (Compound_2)

Crystal data

[Fe(C23H28N2PSe)2]	Z = 1
Mr = 940.65	F(000) = 484
Triclinic, P1	Dx = 1.491 Mg m^−3
a = 9.244 (4) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.465 (5) Å	Cell parameters from 9535 reflections
c = 10.998 (5) Å	θ = 2.6–28.4°
α = 93.969 (5)°	µ = 2.21 mm^−1
β = 97.973 (5)°	T = 100 K
γ = 94.312 (5)°	Column, gold
V = 1047.3 (8) Å^3	0.23 × 0.06 × 0.04 mm

Data collection

Bruker SMART APEX CCD diffractometer	4853 independent reflections
Radiation source: fine-focus sealed tube	4250 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.049
Detector resolution: 8.3660 pixels mm^-1	θmax = 28.4°, θmin = 1.9°
φ and ω scans	h = −11→12
Absorption correction: multi-scan (SADABS; Bruker, 2015)	k = −12→12
Tmin = 0.63, Tmax = 0.91	l = −12→14
17800 measured reflections

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)] = 0.058	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.170	H-atom parameters constrained
S = 1.05	w = 1/[σ^2(Fo^2) + (0.1155P)^2 + 0.5035P] where P = (Fo^2 + 2Fc^2)/3
4853 reflections	(Δ/σ)max = 0.001
254 parameters	Δρmax = 1.63 e Å^−3
0 restraints	Δρmin = −1.84 e Å^−3

Special details

Experimental. The diffraction data were collected in three sets of 606 frames (0.3° width in ω) at φ = 0, 120 and 240°. A scan time of 60 sec/frame was used. Analysis of 1333 reflections having I/σ(I) > 15 and chosen from the full data set with CELL_NOW (Sheldrick, 2008) showed the crystal to belong to the triclinic system and to consist of 2 components rotated by 3° about c*. The raw data were processed using the multi-component version of SAINT under control of the two-component orientation file generated by CELL_NOW.

Geometry. All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds 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 > 2sigma(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. H-atoms attached to carbon were placed in calculated positions (C—H = 0.95 - 0.99 Å). All were included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached atoms. Trial refinements with the single-component reflection file extracted from the full data set with TWINABS and with the full two-component reflection file indicated the former refinement to be superior.

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

	x	y	z	Uiso*/Ueq
Se1	0.58085 (4)	−0.03032 (3)	0.79310 (3)	0.01609 (15)
Fe1	1.0000	0.0000	1.0000	0.01219 (19)
P1	0.73340 (10)	0.13251 (8)	0.80505 (8)	0.0104 (2)
N1	0.8698 (3)	0.5733 (3)	0.8098 (3)	0.0158 (6)
N2	0.3408 (3)	0.2702 (3)	0.5700 (3)	0.0178 (7)
C1	0.9188 (4)	0.0974 (3)	0.8535 (3)	0.0124 (7)
C2	0.9808 (4)	−0.0162 (4)	0.8118 (4)	0.0181 (7)
H2	0.9299	−0.0860	0.7593	0.022*
C3	1.1312 (5)	−0.0067 (4)	0.8622 (4)	0.0243 (9)
H3	1.1986	−0.0685	0.8484	0.029*
C4	1.1644 (4)	0.1118 (4)	0.9374 (4)	0.0230 (9)
H4	1.2572	0.1423	0.9824	0.028*
C5	1.0332 (4)	0.1761 (4)	0.9328 (4)	0.0153 (7)
H5	1.0232	0.2567	0.9746	0.018*
C6	0.7016 (4)	0.2650 (3)	0.9129 (3)	0.0119 (7)
C7	0.7644 (4)	0.3932 (3)	0.9159 (3)	0.0123 (7)
C8	0.7250 (4)	0.4836 (3)	1.0030 (4)	0.0158 (7)
H8	0.7640	0.5706	1.0057	0.019*
C9	0.6306 (4)	0.4495 (4)	1.0851 (4)	0.0186 (8)
H9	0.6058	0.5129	1.1430	0.022*
C10	0.5722 (4)	0.3229 (4)	1.0830 (4)	0.0166 (7)
H10	0.5090	0.2990	1.1403	0.020*
C11	0.6071 (4)	0.2317 (3)	0.9964 (3)	0.0136 (7)
H11	0.5660	0.1455	0.9940	0.016*
C12	0.8757 (4)	0.4383 (3)	0.8365 (3)	0.0138 (7)
H12A	0.9750	0.4263	0.8785	0.017*
H12B	0.8594	0.3839	0.7578	0.017*
C13	0.7362 (4)	0.5912 (4)	0.7259 (4)	0.0241 (9)
H13A	0.7321	0.6826	0.7131	0.036*
H13B	0.6501	0.5604	0.7619	0.036*
H13C	0.7372	0.5424	0.6467	0.036*
C14	0.9982 (4)	0.6147 (4)	0.7550 (4)	0.0220 (8)
H14A	0.9986	0.5627	0.6774	0.033*
H14B	1.0871	0.6037	0.8118	0.033*
H14C	0.9954	0.7054	0.7389	0.033*
C15	0.7295 (4)	0.1888 (3)	0.6512 (3)	0.0126 (7)
C16	0.6071 (4)	0.2444 (4)	0.5922 (3)	0.0137 (7)
C17	0.6082 (4)	0.2749 (4)	0.4701 (4)	0.0185 (8)
H17	0.5270	0.3131	0.4291	0.022*
C18	0.7252 (4)	0.2504 (4)	0.4079 (4)	0.0201 (8)
H18	0.7232	0.2717	0.3252	0.024*
C19	0.8438 (4)	0.1956 (4)	0.4656 (4)	0.0196 (8)
H19	0.9233	0.1782	0.4226	0.023*
C20	0.8473 (4)	0.1655 (3)	0.5882 (3)	0.0144 (7)
H20	0.9301	0.1290	0.6286	0.017*
C21	0.4773 (4)	0.2777 (4)	0.6550 (3)	0.0160 (7)
H21A	0.4659	0.2181	0.7197	0.019*
H21B	0.4973	0.3659	0.6955	0.019*
C22	0.2849 (4)	0.1365 (4)	0.5382 (4)	0.0235 (9)
H22A	0.3601	0.0891	0.5049	0.035*
H22B	0.1973	0.1323	0.4762	0.035*
H22C	0.2596	0.0979	0.6121	0.035*
C23	0.2313 (4)	0.3412 (4)	0.6227 (4)	0.0242 (9)
H23A	0.1400	0.3331	0.5646	0.036*
H23B	0.2674	0.4321	0.6389	0.036*
H23C	0.2129	0.3060	0.6999	0.036*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Se1	0.0173 (2)	0.0129 (2)	0.0176 (2)	−0.00440 (14)	0.00329 (15)	0.00255 (14)
Fe1	0.0123 (4)	0.0128 (4)	0.0136 (4)	0.0041 (3)	0.0052 (3)	0.0060 (3)
P1	0.0109 (4)	0.0099 (4)	0.0110 (4)	0.0001 (3)	0.0031 (3)	0.0025 (3)
N1	0.0162 (15)	0.0105 (14)	0.0221 (17)	0.0010 (11)	0.0057 (13)	0.0049 (12)
N2	0.0106 (14)	0.0236 (17)	0.0195 (17)	0.0054 (12)	0.0008 (12)	0.0024 (13)
C1	0.0123 (16)	0.0144 (16)	0.0125 (17)	0.0037 (13)	0.0042 (13)	0.0068 (12)
C2	0.0225 (19)	0.0185 (18)	0.0165 (19)	0.0086 (15)	0.0083 (15)	0.0056 (14)
C3	0.025 (2)	0.034 (2)	0.021 (2)	0.0173 (18)	0.0170 (17)	0.0144 (17)
C4	0.0119 (17)	0.034 (2)	0.027 (2)	0.0007 (15)	0.0048 (15)	0.0232 (18)
C5	0.0142 (17)	0.0143 (16)	0.0188 (19)	0.0000 (13)	0.0039 (14)	0.0090 (14)
C6	0.0104 (15)	0.0149 (16)	0.0109 (16)	0.0025 (12)	0.0015 (12)	0.0031 (12)
C7	0.0115 (15)	0.0145 (16)	0.0114 (17)	0.0018 (12)	0.0029 (12)	0.0027 (12)
C8	0.0157 (17)	0.0117 (16)	0.0196 (19)	−0.0013 (13)	0.0033 (14)	−0.0003 (13)
C9	0.0181 (18)	0.0192 (18)	0.0179 (19)	0.0057 (14)	0.0009 (14)	−0.0024 (14)
C10	0.0140 (17)	0.0233 (19)	0.0143 (18)	0.0021 (14)	0.0067 (13)	0.0036 (14)
C11	0.0134 (16)	0.0158 (17)	0.0126 (17)	0.0003 (13)	0.0038 (13)	0.0055 (13)
C12	0.0144 (16)	0.0103 (16)	0.0175 (18)	0.0012 (12)	0.0035 (13)	0.0048 (13)
C13	0.0174 (19)	0.031 (2)	0.026 (2)	0.0043 (16)	0.0025 (16)	0.0133 (17)
C14	0.0197 (19)	0.0176 (18)	0.031 (2)	−0.0010 (14)	0.0089 (16)	0.0088 (16)
C15	0.0148 (16)	0.0116 (15)	0.0112 (17)	−0.0017 (12)	0.0020 (13)	0.0022 (12)
C16	0.0101 (15)	0.0178 (17)	0.0130 (17)	−0.0014 (13)	0.0021 (13)	0.0028 (13)
C17	0.0145 (17)	0.025 (2)	0.0152 (19)	0.0008 (14)	−0.0016 (14)	0.0060 (14)
C18	0.0205 (19)	0.027 (2)	0.0129 (18)	−0.0037 (15)	0.0031 (14)	0.0061 (15)
C19	0.0193 (18)	0.025 (2)	0.0154 (19)	−0.0020 (15)	0.0082 (14)	0.0013 (15)
C20	0.0147 (17)	0.0141 (16)	0.0148 (18)	−0.0014 (13)	0.0028 (13)	0.0050 (13)
C21	0.0140 (17)	0.0211 (18)	0.0129 (18)	0.0032 (13)	0.0005 (13)	0.0016 (13)
C22	0.0155 (18)	0.027 (2)	0.026 (2)	0.0018 (15)	−0.0006 (16)	−0.0039 (17)
C23	0.0146 (18)	0.029 (2)	0.029 (2)	0.0075 (15)	0.0037 (16)	−0.0010 (17)

Geometric parameters (Å, º)

Se1—P1	2.1132 (11)	C8—H8	0.9500
Fe1—C2^i	2.047 (4)	C9—C10	1.390 (5)
Fe1—C2	2.047 (4)	C9—H9	0.9500
Fe1—C5	2.050 (4)	C10—C11	1.388 (5)
Fe1—C5^i	2.050 (4)	C10—H10	0.9500
Fe1—C1^i	2.050 (4)	C11—H11	0.9500
Fe1—C1	2.050 (4)	C12—H12A	0.9900
Fe1—C3^i	2.069 (4)	C12—H12B	0.9900
Fe1—C3	2.069 (4)	C13—H13A	0.9800
Fe1—C4^i	2.071 (4)	C13—H13B	0.9800
Fe1—C4	2.071 (4)	C13—H13C	0.9800
P1—C1	1.796 (4)	C14—H14A	0.9800
P1—C15	1.826 (4)	C14—H14B	0.9800
P1—C6	1.829 (4)	C14—H14C	0.9800
N1—C14	1.455 (5)	C15—C20	1.396 (5)
N1—C12	1.466 (4)	C15—C16	1.410 (5)
N1—C13	1.468 (5)	C16—C17	1.403 (5)
N2—C21	1.456 (5)	C16—C21	1.516 (5)
N2—C22	1.457 (5)	C17—C18	1.387 (5)
N2—C23	1.458 (5)	C17—H17	0.9500
C1—C2	1.433 (5)	C18—C19	1.373 (6)
C1—C5	1.439 (5)	C18—H18	0.9500
C2—C3	1.417 (6)	C19—C20	1.402 (5)
C2—H2	0.9500	C19—H19	0.9500
C3—C4	1.431 (7)	C20—H20	0.9500
C3—H3	0.9500	C21—H21A	0.9900
C4—C5	1.427 (5)	C21—H21B	0.9900
C4—H4	0.9500	C22—H22A	0.9800
C5—H5	0.9500	C22—H22B	0.9800
C6—C11	1.397 (5)	C22—H22C	0.9800
C6—C7	1.418 (5)	C23—H23A	0.9800
C7—C8	1.403 (5)	C23—H23B	0.9800
C7—C12	1.508 (5)	C23—H23C	0.9800
C8—C9	1.386 (6)
C2^i—Fe1—C2	180.0	Fe1—C4—H4	126.8
C2^i—Fe1—C5	111.19 (16)	C4—C5—C1	108.0 (3)
C2—Fe1—C5	68.81 (16)	C4—C5—Fe1	70.5 (2)
C2^i—Fe1—C5^i	68.81 (16)	C1—C5—Fe1	69.5 (2)
C2—Fe1—C5^i	111.19 (16)	C4—C5—H5	126.0
C5—Fe1—C5^i	180.0	C1—C5—H5	126.0
C2^i—Fe1—C1^i	40.95 (14)	Fe1—C5—H5	125.6
C2—Fe1—C1^i	139.05 (14)	C11—C6—C7	120.1 (3)
C5—Fe1—C1^i	138.92 (14)	C11—C6—P1	114.8 (3)
C5^i—Fe1—C1^i	41.08 (14)	C7—C6—P1	125.1 (3)
C2^i—Fe1—C1	139.05 (14)	C8—C7—C6	117.5 (3)
C2—Fe1—C1	40.95 (14)	C8—C7—C12	117.6 (3)
C5—Fe1—C1	41.08 (14)	C6—C7—C12	124.9 (3)
C5^i—Fe1—C1	138.92 (14)	C9—C8—C7	121.8 (3)
C1^i—Fe1—C1	180.0	C9—C8—H8	119.1
C2^i—Fe1—C3^i	40.27 (17)	C7—C8—H8	119.1
C2—Fe1—C3^i	139.73 (17)	C8—C9—C10	120.2 (3)
C5—Fe1—C3^i	111.82 (16)	C8—C9—H9	119.9
C5^i—Fe1—C3^i	68.18 (16)	C10—C9—H9	119.9
C1^i—Fe1—C3^i	68.21 (15)	C11—C10—C9	119.4 (3)
C1—Fe1—C3^i	111.79 (15)	C11—C10—H10	120.3
C2^i—Fe1—C3	139.73 (17)	C9—C10—H10	120.3
C2—Fe1—C3	40.27 (17)	C10—C11—C6	121.0 (3)
C5—Fe1—C3	68.18 (16)	C10—C11—H11	119.5
C5^i—Fe1—C3	111.82 (16)	C6—C11—H11	119.5
C1^i—Fe1—C3	111.79 (15)	N1—C12—C7	113.8 (3)
C1—Fe1—C3	68.21 (15)	N1—C12—H12A	108.8
C3^i—Fe1—C3	180.0	C7—C12—H12A	108.8
C2^i—Fe1—C4^i	68.24 (17)	N1—C12—H12B	108.8
C2—Fe1—C4^i	111.76 (17)	C7—C12—H12B	108.8
C5—Fe1—C4^i	139.49 (15)	H12A—C12—H12B	107.7
C5^i—Fe1—C4^i	40.51 (15)	N1—C13—H13A	109.5
C1^i—Fe1—C4^i	68.47 (15)	N1—C13—H13B	109.5
C1—Fe1—C4^i	111.53 (15)	H13A—C13—H13B	109.5
C3^i—Fe1—C4^i	40.43 (19)	N1—C13—H13C	109.5
C3—Fe1—C4^i	139.57 (19)	H13A—C13—H13C	109.5
C2^i—Fe1—C4	111.76 (17)	H13B—C13—H13C	109.5
C2—Fe1—C4	68.24 (17)	N1—C14—H14A	109.5
C5—Fe1—C4	40.51 (15)	N1—C14—H14B	109.5
C5^i—Fe1—C4	139.49 (15)	H14A—C14—H14B	109.5
C1^i—Fe1—C4	111.53 (15)	N1—C14—H14C	109.5
C1—Fe1—C4	68.47 (15)	H14A—C14—H14C	109.5
C3^i—Fe1—C4	139.57 (19)	H14B—C14—H14C	109.5
C3—Fe1—C4	40.43 (19)	C20—C15—C16	120.1 (3)
C4^i—Fe1—C4	180.0	C20—C15—P1	117.9 (3)
C1—P1—C15	106.22 (16)	C16—C15—P1	121.8 (3)
C1—P1—C6	104.97 (17)	C17—C16—C15	118.1 (3)
C15—P1—C6	109.45 (16)	C17—C16—C21	118.2 (3)
C1—P1—Se1	113.04 (12)	C15—C16—C21	123.6 (3)
C15—P1—Se1	108.10 (12)	C18—C17—C16	121.4 (4)
C6—P1—Se1	114.70 (12)	C18—C17—H17	119.3
C14—N1—C12	109.5 (3)	C16—C17—H17	119.3
C14—N1—C13	109.7 (3)	C19—C18—C17	120.2 (4)
C12—N1—C13	111.0 (3)	C19—C18—H18	119.9
C21—N2—C22	110.2 (3)	C17—C18—H18	119.9
C21—N2—C23	111.1 (3)	C18—C19—C20	119.9 (4)
C22—N2—C23	110.1 (3)	C18—C19—H19	120.1
C2—C1—C5	107.4 (3)	C20—C19—H19	120.1
C2—C1—P1	124.1 (3)	C15—C20—C19	120.3 (3)
C5—C1—P1	128.4 (3)	C15—C20—H20	119.8
C2—C1—Fe1	69.4 (2)	C19—C20—H20	119.8
C5—C1—Fe1	69.4 (2)	N2—C21—C16	113.0 (3)
P1—C1—Fe1	128.89 (19)	N2—C21—H21A	109.0
C3—C2—C1	108.3 (4)	C16—C21—H21A	109.0
C3—C2—Fe1	70.7 (2)	N2—C21—H21B	109.0
C1—C2—Fe1	69.7 (2)	C16—C21—H21B	109.0
C3—C2—H2	125.9	H21A—C21—H21B	107.8
C1—C2—H2	125.9	N2—C22—H22A	109.5
Fe1—C2—H2	125.4	N2—C22—H22B	109.5
C2—C3—C4	108.4 (3)	H22A—C22—H22B	109.5
C2—C3—Fe1	69.0 (2)	N2—C22—H22C	109.5
C4—C3—Fe1	69.8 (2)	H22A—C22—H22C	109.5
C2—C3—H3	125.8	H22B—C22—H22C	109.5
C4—C3—H3	125.8	N2—C23—H23A	109.5
Fe1—C3—H3	126.9	N2—C23—H23B	109.5
C5—C4—C3	107.8 (4)	H23A—C23—H23B	109.5
C5—C4—Fe1	69.0 (2)	N2—C23—H23C	109.5
C3—C4—Fe1	69.7 (2)	H23A—C23—H23C	109.5
C5—C4—H4	126.1	H23B—C23—H23C	109.5
C3—C4—H4	126.1

Symmetry code: (i) −x+2, −y, −z+2.

[µ-1,1'-Bis(bis{2-[(dimethylamino)methyl]phenyl}phosphanyl)ferrocene-κ²N,P:κ²N',P']bis[dichloridozinc(II)] dichloromethane monosolvate (Compound_3)

Crystal data

[FeZn2Cl4(C23H28N2P)2]·CH2Cl2	Z = 2
Mr = 1140.20	F(000) = 1172
Triclinic, P1	Dx = 1.477 Mg m^−3
a = 10.1150 (13) Å	Mo Kα radiation, λ = 0.71073 Å
b = 10.7515 (14) Å	Cell parameters from 9979 reflections
c = 26.637 (3) Å	θ = 2.3–28.7°
α = 96.791 (2)°	µ = 1.62 mm^−1
β = 91.486 (2)°	T = 100 K
γ = 116.491 (2)°	Plate, orange
V = 2564.4 (6) Å^3	0.18 × 0.14 × 0.03 mm

Data collection

Bruker SMART APEX CCD diffractometer	48081 independent reflections
Radiation source: fine-focus sealed tube	41125 reflections with I > 2σ(I)
Graphite monochromator	Rint = 0.061
Detector resolution: 8.3660 pixels mm^-1	θmax = 28.7°, θmin = 2.1°
φ and ω scans	h = −13→13
Absorption correction: multi-scan (TWINABS; Sheldrick, 2009)	k = −14→14
Tmin = 0.76, Tmax = 0.96	l = −36→35
48081 measured reflections

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)] = 0.055	Hydrogen site location: inferred from neighbouring sites
wR(F^2) = 0.128	H-atom parameters constrained
S = 1.03	w = 1/[σ^2(Fo^2) + (0.0197P)^2 + 4.4933P] where P = (Fo^2 + 2Fc^2)/3
48081 reflections	(Δ/σ)max = 0.001
571 parameters	Δρmax = 1.04 e Å^−3
294 restraints	Δρmin = −0.63 e Å^−3

Special details

Experimental. The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5° in ω, colllected at φ = 0.00, 90.00 and 180.00° and 2 sets of 800 frames, each of width 0.45° in φ, collected at ω = –30.00 and 210.00°. The scan time was 25 sec/frame. Analysis of 1762 reflections having I/σ(I) > 15 and chosen from the full data set with CELL_NOW (Sheldrick, 2008) showed the crystal to belong to the triclinic system and to be twinned by a 180° rotation about the c* axis. The raw data were processed using the multi- component version of SAINT under control of the two-component orientation file generated by CELL_NOW.

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

Refinement. The diffraction data were obtained from 3 sets of 400 frames, each of width 0.5° in ω, colllected at φ = 0.00, 90.00 and 180.00° and 2 sets of 800 frames, each of width 0.45° in φ, collected at ω = –30.00 and 210.00°. The scan time was sec/frame. H-atoms attached to carbon were placed in calculated positions (C—H = 0.95 - 0.98 Å). All were included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached atoms. Refined as a 2-component twin.

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

	x	y	z	Uiso*/Ueq
Zn1	0.89247 (7)	0.52716 (6)	0.33790 (2)	0.01183 (13)
Fe1	1.0000	0.5000	0.5000	0.0289 (3)
Cl1	0.89074 (17)	0.32452 (14)	0.30938 (5)	0.0232 (3)
Cl2	0.67841 (14)	0.51622 (15)	0.36164 (6)	0.0222 (3)
P1	1.06349 (15)	0.69801 (13)	0.40472 (5)	0.0105 (3)
N1	0.9693 (5)	0.6567 (4)	0.28065 (16)	0.0137 (9)
N2	1.4674 (6)	1.1336 (5)	0.4311 (2)	0.0374 (15)
C1	1.0345 (6)	0.6777 (5)	0.4698 (2)	0.0160 (12)
C2	1.1441 (8)	0.7096 (6)	0.5111 (2)	0.0325 (16)
H2	1.2538	0.7515	0.5090	0.039*
C3	1.0707 (10)	0.6729 (7)	0.5550 (3)	0.0441 (19)
H3	1.1191	0.6831	0.5894	0.053*
C4	0.9192 (10)	0.6185 (7)	0.5424 (3)	0.0450 (19)
H4	0.8408	0.5829	0.5665	0.054*
C5	0.8928 (7)	0.6178 (6)	0.4892 (2)	0.0266 (14)
H5	0.7944	0.5851	0.4698	0.032*
C6	1.0211 (5)	0.8407 (5)	0.39269 (19)	0.0102 (10)
C7	0.9723 (6)	0.9077 (5)	0.4299 (2)	0.0139 (11)
H7	0.9680	0.8842	0.4633	0.017*
C8	0.9298 (6)	1.0083 (5)	0.4193 (2)	0.0149 (11)
H8	0.8978	1.0544	0.4452	0.018*
C9	0.9343 (6)	1.0412 (5)	0.3705 (2)	0.0174 (12)
H9	0.9064	1.1109	0.3630	0.021*
C10	0.9791 (5)	0.9732 (5)	0.3326 (2)	0.0152 (11)
H10	0.9791	0.9948	0.2991	0.018*
C11	1.0247 (5)	0.8723 (5)	0.34307 (19)	0.0116 (10)
C12	1.0772 (5)	0.8049 (5)	0.30110 (19)	0.0128 (11)
H12A	1.1709	0.8065	0.3137	0.015*
H12B	1.0992	0.8618	0.2730	0.015*
C13	1.0451 (6)	0.6017 (6)	0.2442 (2)	0.0238 (13)
H13A	0.9752	0.5071	0.2280	0.036*
H13B	1.1288	0.5980	0.2622	0.036*
H13C	1.0817	0.6636	0.2182	0.036*
C14	0.8396 (6)	0.6552 (6)	0.2529 (2)	0.0223 (13)
H14A	0.8727	0.7103	0.2249	0.034*
H14B	0.7912	0.6961	0.2761	0.034*
H14C	0.7693	0.5581	0.2394	0.034*
C15	1.2584 (6)	0.7470 (5)	0.3987 (2)	0.0139 (11)
C16	1.2831 (6)	0.6377 (6)	0.3736 (2)	0.0167 (12)
H16	1.2005	0.5504	0.3610	0.020*
C17	1.4233 (6)	0.6540 (6)	0.3667 (2)	0.0241 (13)
H17	1.4373	0.5781	0.3501	0.029*
C18	1.5440 (7)	0.7809 (6)	0.3839 (3)	0.0299 (15)
H18	1.6415	0.7925	0.3795	0.036*
C19	1.5224 (7)	0.8925 (7)	0.4079 (3)	0.0319 (15)
H19	1.6058	0.9808	0.4186	0.038*
C20	1.3799 (6)	0.8766 (6)	0.4165 (2)	0.0220 (13)
C21	1.3671 (6)	0.9990 (6)	0.4464 (3)	0.0272 (15)
H21A	1.2638	0.9849	0.4414	0.033*
H21B	1.3899	1.0015	0.4830	0.033*
C22	1.4622 (8)	1.2479 (7)	0.4654 (3)	0.048 (2)
H22A	1.5392	1.3382	0.4583	0.072*
H22B	1.4794	1.2369	0.5006	0.072*
H22C	1.3647	1.2453	0.4603	0.072*
C23	1.4264 (9)	1.1407 (8)	0.3790 (3)	0.060 (2)
H23A	1.4154	1.0564	0.3569	0.089*
H23B	1.5040	1.2242	0.3677	0.089*
H23C	1.3323	1.1462	0.3774	0.089*
Zn2	0.22774 (7)	0.14799 (6)	0.15950 (2)	0.01370 (14)
Fe2	0.0000	0.0000	0.0000	0.0259 (3)
Cl3	0.42342 (15)	0.12336 (15)	0.13325 (6)	0.0275 (3)
Cl4	0.04783 (15)	−0.03463 (14)	0.18613 (5)	0.0232 (3)
P2	0.18477 (14)	0.26880 (14)	0.09560 (5)	0.0119 (3)
N3	0.3048 (5)	0.3205 (5)	0.21884 (17)	0.0177 (10)
N4	0.1988 (5)	0.6836 (5)	0.0650 (2)	0.0267 (12)
C24	0.1611 (6)	0.1958 (5)	0.0298 (2)	0.0178 (12)
C25	0.2274 (6)	0.1119 (6)	0.0088 (2)	0.0271 (15)
H25	0.2974	0.0869	0.0273	0.032*
C26	0.1774 (8)	0.0717 (7)	−0.0438 (3)	0.0440 (19)
H26	0.2050	0.0115	−0.0685	0.053*
C27	0.0806 (8)	0.1272 (7)	−0.0549 (2)	0.0427 (19)
H27	0.0282	0.1140	−0.0889	0.051*
C28	0.0685 (6)	0.2047 (6)	−0.0102 (2)	0.0281 (15)
H28	0.0081	0.2573	−0.0070	0.034*
C29	0.3671 (5)	0.4205 (5)	0.1068 (2)	0.0117 (11)
C30	0.4642 (6)	0.4584 (5)	0.0689 (2)	0.0157 (11)
H30	0.4343	0.4057	0.0359	0.019*
C31	0.6045 (6)	0.5728 (5)	0.0788 (2)	0.0166 (12)
H31	0.6697	0.5985	0.0527	0.020*
C32	0.6478 (6)	0.6486 (5)	0.1273 (2)	0.0172 (12)
H32	0.7417	0.7290	0.1341	0.021*
C33	0.5554 (6)	0.6080 (5)	0.1657 (2)	0.0167 (12)
H33	0.5875	0.6593	0.1989	0.020*
C34	0.4156 (6)	0.4927 (5)	0.1566 (2)	0.0134 (11)
C35	0.3193 (6)	0.4513 (5)	0.2002 (2)	0.0176 (12)
H35A	0.3610	0.5295	0.2287	0.021*
H35B	0.2190	0.4382	0.1892	0.021*
C36	0.4495 (6)	0.3435 (6)	0.2416 (2)	0.0262 (14)
H36A	0.5207	0.3654	0.2158	0.039*
H36B	0.4388	0.2584	0.2547	0.039*
H36C	0.4851	0.4220	0.2695	0.039*
C37	0.1993 (7)	0.2899 (6)	0.2581 (2)	0.0295 (15)
H37A	0.1021	0.2725	0.2431	0.044*
H37B	0.2352	0.3702	0.2853	0.044*
H37C	0.1904	0.2065	0.2722	0.044*
C38	0.0444 (5)	0.3304 (5)	0.1042 (2)	0.0143 (11)
C39	0.0405 (6)	0.4452 (6)	0.0849 (2)	0.0181 (12)
C40	−0.0773 (6)	0.4753 (6)	0.0956 (2)	0.0237 (13)
H40	−0.0801	0.5539	0.0836	0.028*
C41	−0.1899 (6)	0.3939 (6)	0.1231 (2)	0.0246 (14)
H41	−0.2701	0.4155	0.1290	0.030*
C42	−0.1863 (6)	0.2805 (6)	0.1421 (2)	0.0218 (13)
H42	−0.2635	0.2243	0.1610	0.026*
C43	−0.0685 (6)	0.2506 (6)	0.1330 (2)	0.0175 (12)
H43	−0.0644	0.1745	0.1467	0.021*
C44	0.1542 (6)	0.5341 (6)	0.0512 (2)	0.0210 (13)
H44A	0.2428	0.5177	0.0541	0.025*
H44B	0.1117	0.5044	0.0154	0.025*
C45	0.2798 (7)	0.7350 (6)	0.1152 (3)	0.0389 (17)
H45A	0.3749	0.7316	0.1140	0.058*
H45B	0.2213	0.6758	0.1396	0.058*
H45C	0.2976	0.8321	0.1257	0.058*
C46	0.2947 (7)	0.7627 (7)	0.0278 (3)	0.0383 (18)
H46A	0.2391	0.7335	−0.0057	0.057*
H46B	0.3810	0.7439	0.0261	0.057*
H46C	0.3281	0.8634	0.0381	0.057*
Cl5	−0.26632 (17)	−0.01531 (16)	0.21729 (7)	0.0332 (4)
Cl6	−0.5516 (2)	−0.1373 (2)	0.25951 (9)	0.0626 (6)
C47	−0.4170 (7)	0.0106 (7)	0.2389 (3)	0.0373 (17)
H47A	−0.3800	0.0899	0.2671	0.045*
H47B	−0.4621	0.0364	0.2110	0.045*

Atomic displacement parameters (Ų)

	U^11	U^22	U^33	U^12	U^13	U^23
Zn1	0.0125 (3)	0.0101 (3)	0.0123 (3)	0.0046 (2)	0.0005 (3)	0.0018 (2)
Fe1	0.0727 (10)	0.0166 (6)	0.0095 (6)	0.0304 (7)	0.0066 (6)	0.0044 (5)
Cl1	0.0387 (9)	0.0133 (7)	0.0187 (7)	0.0132 (6)	0.0038 (6)	0.0001 (5)
Cl2	0.0119 (7)	0.0309 (8)	0.0252 (8)	0.0097 (6)	0.0037 (6)	0.0090 (6)
P1	0.0133 (7)	0.0093 (6)	0.0103 (7)	0.0063 (5)	−0.0006 (5)	0.0015 (5)
N1	0.016 (2)	0.013 (2)	0.009 (2)	0.0042 (19)	0.0014 (18)	0.0015 (18)
N2	0.030 (3)	0.014 (3)	0.057 (4)	0.003 (2)	−0.017 (3)	−0.003 (3)
C1	0.028 (3)	0.009 (2)	0.014 (3)	0.013 (2)	−0.001 (2)	0.000 (2)
C2	0.060 (4)	0.020 (3)	0.023 (3)	0.026 (3)	−0.013 (3)	−0.003 (2)
C3	0.102 (5)	0.023 (3)	0.017 (3)	0.038 (4)	−0.002 (3)	0.000 (3)
C4	0.100 (5)	0.023 (3)	0.030 (3)	0.040 (4)	0.033 (4)	0.013 (3)
C5	0.051 (4)	0.017 (3)	0.027 (3)	0.025 (3)	0.020 (3)	0.013 (2)
C6	0.010 (2)	0.008 (2)	0.012 (2)	0.0039 (19)	0.002 (2)	0.0021 (19)
C7	0.016 (3)	0.013 (3)	0.011 (2)	0.006 (2)	−0.002 (2)	0.000 (2)
C8	0.016 (3)	0.011 (2)	0.019 (3)	0.008 (2)	0.000 (2)	0.000 (2)
C9	0.020 (3)	0.010 (2)	0.023 (3)	0.008 (2)	−0.005 (2)	0.002 (2)
C10	0.016 (3)	0.014 (2)	0.014 (3)	0.005 (2)	−0.002 (2)	0.006 (2)
C11	0.009 (2)	0.010 (2)	0.013 (2)	0.0013 (19)	−0.001 (2)	0.003 (2)
C12	0.011 (2)	0.014 (2)	0.014 (3)	0.005 (2)	0.001 (2)	0.006 (2)
C13	0.027 (3)	0.024 (3)	0.017 (3)	0.009 (3)	0.006 (3)	0.001 (2)
C14	0.019 (3)	0.021 (3)	0.021 (3)	0.004 (2)	−0.007 (2)	0.008 (2)
C15	0.014 (3)	0.010 (2)	0.017 (3)	0.007 (2)	−0.004 (2)	−0.001 (2)
C16	0.014 (3)	0.017 (3)	0.019 (3)	0.007 (2)	−0.005 (2)	0.001 (2)
C17	0.020 (3)	0.026 (3)	0.032 (3)	0.016 (2)	0.000 (2)	0.000 (3)
C18	0.014 (3)	0.033 (3)	0.046 (4)	0.013 (3)	0.003 (3)	0.007 (3)
C19	0.016 (3)	0.024 (3)	0.051 (4)	0.007 (2)	−0.007 (3)	0.002 (3)
C20	0.016 (3)	0.015 (3)	0.034 (3)	0.008 (2)	−0.008 (2)	0.000 (2)
C21	0.020 (3)	0.016 (3)	0.043 (4)	0.009 (2)	−0.014 (3)	−0.005 (3)
C22	0.052 (5)	0.018 (3)	0.066 (5)	0.013 (3)	−0.023 (4)	−0.006 (3)
C23	0.073 (6)	0.029 (4)	0.067 (6)	0.015 (4)	−0.018 (5)	0.007 (4)
Zn2	0.0120 (3)	0.0121 (3)	0.0153 (3)	0.0036 (3)	0.0005 (3)	0.0037 (3)
Fe2	0.0258 (7)	0.0164 (6)	0.0114 (6)	−0.0111 (5)	0.0045 (5)	−0.0018 (5)
Cl3	0.0166 (7)	0.0249 (8)	0.0427 (10)	0.0122 (6)	0.0021 (7)	−0.0002 (7)
Cl4	0.0250 (8)	0.0183 (7)	0.0164 (7)	−0.0003 (6)	0.0012 (6)	0.0076 (6)
P2	0.0094 (7)	0.0097 (6)	0.0128 (7)	0.0011 (5)	−0.0004 (5)	0.0016 (5)
N3	0.015 (2)	0.017 (2)	0.013 (2)	0.000 (2)	0.0019 (19)	0.0001 (19)
N4	0.024 (3)	0.019 (3)	0.035 (3)	0.006 (2)	0.000 (2)	0.012 (2)
C24	0.014 (3)	0.014 (3)	0.014 (3)	−0.004 (2)	0.002 (2)	0.003 (2)
C25	0.018 (3)	0.017 (3)	0.030 (3)	−0.006 (2)	0.012 (2)	−0.004 (3)
C26	0.041 (4)	0.027 (3)	0.029 (3)	−0.014 (3)	0.024 (3)	−0.009 (3)
C27	0.038 (4)	0.033 (3)	0.014 (3)	−0.023 (3)	0.002 (3)	0.005 (3)
C28	0.025 (3)	0.024 (3)	0.016 (3)	−0.007 (2)	−0.004 (2)	0.007 (2)
C29	0.011 (2)	0.008 (2)	0.016 (3)	0.004 (2)	−0.002 (2)	0.003 (2)
C30	0.017 (3)	0.015 (3)	0.014 (3)	0.007 (2)	−0.004 (2)	0.003 (2)
C31	0.012 (3)	0.018 (3)	0.017 (3)	0.002 (2)	0.003 (2)	0.009 (2)
C32	0.013 (3)	0.014 (3)	0.020 (3)	0.001 (2)	−0.001 (2)	0.007 (2)
C33	0.016 (3)	0.013 (2)	0.016 (3)	0.003 (2)	−0.002 (2)	0.002 (2)
C34	0.014 (3)	0.010 (2)	0.015 (3)	0.005 (2)	−0.001 (2)	0.001 (2)
C35	0.015 (3)	0.017 (3)	0.018 (3)	0.005 (2)	0.002 (2)	−0.001 (2)
C36	0.029 (3)	0.022 (3)	0.023 (3)	0.007 (3)	−0.004 (3)	0.009 (3)
C37	0.032 (4)	0.026 (3)	0.016 (3)	0.001 (3)	0.007 (3)	0.000 (3)
C38	0.011 (2)	0.013 (2)	0.017 (3)	0.004 (2)	−0.001 (2)	0.002 (2)
C39	0.013 (3)	0.018 (3)	0.022 (3)	0.006 (2)	−0.001 (2)	0.003 (2)
C40	0.024 (3)	0.024 (3)	0.028 (3)	0.014 (2)	−0.001 (2)	0.008 (3)
C41	0.018 (3)	0.028 (3)	0.033 (3)	0.015 (2)	0.002 (2)	0.002 (3)
C42	0.015 (3)	0.024 (3)	0.027 (3)	0.009 (2)	0.003 (2)	0.003 (2)
C43	0.019 (3)	0.016 (3)	0.018 (3)	0.008 (2)	−0.003 (2)	0.001 (2)
C44	0.018 (3)	0.023 (3)	0.024 (3)	0.008 (2)	0.000 (2)	0.010 (2)
C45	0.046 (4)	0.021 (3)	0.040 (4)	0.007 (3)	0.001 (3)	0.007 (3)
C46	0.037 (4)	0.026 (3)	0.044 (4)	0.003 (3)	−0.004 (3)	0.022 (3)
Cl5	0.0269 (9)	0.0240 (8)	0.0455 (10)	0.0082 (7)	0.0086 (8)	0.0055 (7)
Cl6	0.0536 (13)	0.0430 (12)	0.0818 (17)	0.0104 (10)	0.0416 (12)	0.0143 (11)
C47	0.031 (4)	0.033 (3)	0.050 (4)	0.016 (3)	0.008 (3)	0.007 (3)

Geometric parameters (Å, º)

Zn1—N1	2.114 (4)	Zn2—Cl3	2.2299 (15)
Zn1—Cl1	2.2131 (14)	Zn2—P2	2.4002 (15)
Zn1—Cl2	2.2278 (15)	Fe2—C28	2.047 (6)
Zn1—P1	2.4015 (15)	Fe2—C28^ii	2.047 (6)
Fe1—C5	2.038 (5)	Fe2—C24^ii	2.048 (5)
Fe1—C5^i	2.038 (5)	Fe2—C24	2.048 (5)
Fe1—C2	2.045 (6)	Fe2—C27^ii	2.053 (6)
Fe1—C2^i	2.045 (6)	Fe2—C27	2.053 (6)
Fe1—C1	2.050 (5)	Fe2—C25^ii	2.057 (5)
Fe1—C1^i	2.050 (5)	Fe2—C25	2.057 (5)
Fe1—C4^i	2.050 (6)	Fe2—C26	2.064 (6)
Fe1—C4	2.050 (6)	Fe2—C26^ii	2.064 (6)
Fe1—C3	2.056 (6)	P2—C24	1.798 (6)
Fe1—C3^i	2.056 (6)	P2—C29	1.823 (5)
P1—C1	1.789 (6)	P2—C38	1.825 (5)
P1—C15	1.816 (5)	N3—C36	1.471 (7)
P1—C6	1.826 (5)	N3—C37	1.472 (7)
N1—C13	1.479 (6)	N3—C35	1.494 (7)
N1—C14	1.482 (6)	N4—C44	1.458 (7)
N1—C12	1.497 (6)	N4—C45	1.460 (8)
N2—C23	1.458 (9)	N4—C46	1.469 (8)
N2—C21	1.463 (7)	C24—C25	1.420 (8)
N2—C22	1.465 (8)	C24—C28	1.440 (8)
C1—C5	1.425 (8)	C25—C26	1.424 (9)
C1—C2	1.437 (8)	C25—H25	1.0000
C2—C3	1.401 (9)	C26—C27	1.396 (10)
C2—H2	1.0000	C26—H26	1.0000
C3—C4	1.389 (10)	C27—C28	1.411 (9)
C3—H3	1.0000	C27—H27	1.0000
C4—C5	1.433 (9)	C28—H28	1.0000
C4—H4	1.0000	C29—C30	1.391 (7)
C5—H5	1.0000	C29—C34	1.409 (7)
C6—C7	1.386 (7)	C30—C31	1.394 (7)
C6—C11	1.400 (7)	C30—H30	0.9500
C7—C8	1.385 (7)	C31—C32	1.388 (7)
C7—H7	0.9500	C31—H31	0.9500
C8—C9	1.383 (7)	C32—C33	1.379 (7)
C8—H8	0.9500	C32—H32	0.9500
C9—C10	1.378 (7)	C33—C34	1.393 (7)
C9—H9	0.9500	C33—H33	0.9500
C10—C11	1.407 (6)	C34—C35	1.513 (7)
C10—H10	0.9500	C35—H35A	0.9900
C11—C12	1.496 (7)	C35—H35B	0.9900
C12—H12A	0.9900	C36—H36A	0.9800
C12—H12B	0.9900	C36—H36B	0.9800
C13—H13A	0.9800	C36—H36C	0.9800
C13—H13B	0.9800	C37—H37A	0.9800
C13—H13C	0.9800	C37—H37B	0.9800
C14—H14A	0.9800	C37—H37C	0.9800
C14—H14B	0.9800	C38—C43	1.399 (7)
C14—H14C	0.9800	C38—C39	1.408 (7)
C15—C20	1.401 (7)	C39—C40	1.395 (7)
C15—C16	1.406 (7)	C39—C44	1.521 (7)
C16—C17	1.369 (7)	C40—C41	1.381 (8)
C16—H16	0.9500	C40—H40	0.9500
C17—C18	1.378 (8)	C41—C42	1.389 (7)
C17—H17	0.9500	C41—H41	0.9500
C18—C19	1.399 (8)	C42—C43	1.385 (7)
C18—H18	0.9500	C42—H42	0.9500
C19—C20	1.402 (8)	C43—H43	0.9500
C19—H19	0.9500	C44—H44A	0.9900
C20—C21	1.513 (8)	C44—H44B	0.9900
C21—H21A	0.9900	C45—H45A	0.9800
C21—H21B	0.9900	C45—H45B	0.9800
C22—H22A	0.9800	C45—H45C	0.9800
C22—H22B	0.9800	C46—H46A	0.9800
C22—H22C	0.9800	C46—H46B	0.9800
C23—H23A	0.9800	C46—H46C	0.9800
C23—H23B	0.9800	Cl5—C47	1.766 (6)
C23—H23C	0.9800	Cl6—C47	1.732 (6)
Zn2—N3	2.121 (4)	C47—H47A	0.9900
Zn2—Cl4	2.2087 (14)	C47—H47B	0.9900
N1—Zn1—Cl1	107.09 (12)	N3—Zn2—P2	95.97 (13)
N1—Zn1—Cl2	110.51 (12)	Cl4—Zn2—P2	122.77 (6)
Cl1—Zn1—Cl2	116.26 (6)	Cl3—Zn2—P2	101.62 (6)
N1—Zn1—P1	95.11 (12)	C28—Fe2—C28^ii	180.0
Cl1—Zn1—P1	124.77 (6)	C28—Fe2—C24^ii	138.8 (2)
Cl2—Zn1—P1	100.91 (5)	C28^ii—Fe2—C24^ii	41.2 (2)
C5—Fe1—C5^i	180.0	C28—Fe2—C24	41.2 (2)
C5—Fe1—C2	68.8 (3)	C28^ii—Fe2—C24	138.8 (2)
C5^i—Fe1—C2	111.2 (3)	C24^ii—Fe2—C24	180.0
C5—Fe1—C2^i	111.2 (3)	C28—Fe2—C27^ii	139.7 (2)
C5^i—Fe1—C2^i	68.8 (3)	C28^ii—Fe2—C27^ii	40.3 (2)
C2—Fe1—C2^i	180.0	C24^ii—Fe2—C27^ii	68.1 (2)
C5—Fe1—C1	40.8 (2)	C24—Fe2—C27^ii	111.9 (2)
C5^i—Fe1—C1	139.2 (2)	C28—Fe2—C27	40.3 (2)
C2—Fe1—C1	41.1 (2)	C28^ii—Fe2—C27	139.7 (2)
C2^i—Fe1—C1	138.9 (2)	C24^ii—Fe2—C27	111.9 (2)
C5—Fe1—C1^i	139.2 (2)	C24—Fe2—C27	68.1 (2)
C5^i—Fe1—C1^i	40.8 (2)	C27^ii—Fe2—C27	180.0
C2—Fe1—C1^i	138.9 (2)	C28—Fe2—C25^ii	111.4 (2)
C2^i—Fe1—C1^i	41.1 (2)	C28^ii—Fe2—C25^ii	68.6 (2)
C1—Fe1—C1^i	180.0	C24^ii—Fe2—C25^ii	40.5 (2)
C5—Fe1—C4^i	139.0 (2)	C24—Fe2—C25^ii	139.5 (2)
C5^i—Fe1—C4^i	41.0 (2)	C27^ii—Fe2—C25^ii	67.9 (3)
C2—Fe1—C4^i	112.8 (3)	C27—Fe2—C25^ii	112.1 (3)
C2^i—Fe1—C4^i	67.2 (3)	C28—Fe2—C25	68.6 (2)
C1—Fe1—C4^i	112.1 (2)	C28^ii—Fe2—C25	111.4 (2)
C1^i—Fe1—C4^i	67.9 (2)	C24^ii—Fe2—C25	139.5 (2)
C5—Fe1—C4	41.0 (2)	C24—Fe2—C25	40.5 (2)
C5^i—Fe1—C4	139.0 (2)	C27^ii—Fe2—C25	112.1 (3)
C2—Fe1—C4	67.2 (3)	C27—Fe2—C25	67.9 (3)
C2^i—Fe1—C4	112.8 (3)	C25^ii—Fe2—C25	180.0
C1—Fe1—C4	67.9 (2)	C28—Fe2—C26	67.5 (3)
C1^i—Fe1—C4	112.1 (2)	C28^ii—Fe2—C26	112.5 (3)
C4^i—Fe1—C4	180.0	C24^ii—Fe2—C26	112.3 (2)
C5—Fe1—C3	68.4 (3)	C24—Fe2—C26	67.7 (2)
C5^i—Fe1—C3	111.6 (3)	C27^ii—Fe2—C26	140.3 (3)
C2—Fe1—C3	40.0 (3)	C27—Fe2—C26	39.7 (3)
C2^i—Fe1—C3	140.0 (3)	C25^ii—Fe2—C26	139.6 (2)
C1—Fe1—C3	68.1 (2)	C25—Fe2—C26	40.4 (2)
C1^i—Fe1—C3	111.9 (2)	C28—Fe2—C26^ii	112.5 (3)
C4^i—Fe1—C3	140.5 (3)	C28^ii—Fe2—C26^ii	67.5 (3)
C4—Fe1—C3	39.5 (3)	C24^ii—Fe2—C26^ii	67.7 (2)
C5—Fe1—C3^i	111.6 (3)	C24—Fe2—C26^ii	112.3 (2)
C5^i—Fe1—C3^i	68.4 (3)	C27^ii—Fe2—C26^ii	39.7 (3)
C2—Fe1—C3^i	140.0 (3)	C27—Fe2—C26^ii	140.3 (3)
C2^i—Fe1—C3^i	40.0 (3)	C25^ii—Fe2—C26^ii	40.4 (2)
C1—Fe1—C3^i	111.9 (2)	C25—Fe2—C26^ii	139.6 (2)
C1^i—Fe1—C3^i	68.1 (2)	C26—Fe2—C26^ii	180.0 (3)
C4^i—Fe1—C3^i	39.5 (3)	C24—P2—C29	107.2 (2)
C4—Fe1—C3^i	140.5 (3)	C24—P2—C38	106.2 (3)
C3—Fe1—C3^i	180.0	C29—P2—C38	108.4 (2)
C1—P1—C15	106.3 (3)	C24—P2—Zn2	119.65 (19)
C1—P1—C6	106.2 (2)	C29—P2—Zn2	95.59 (16)
C15—P1—C6	110.7 (2)	C38—P2—Zn2	118.31 (18)
C1—P1—Zn1	120.68 (19)	C36—N3—C37	109.0 (5)
C15—P1—Zn1	116.00 (17)	C36—N3—C35	109.8 (4)
C6—P1—Zn1	95.94 (16)	C37—N3—C35	107.5 (4)
C13—N1—C14	108.4 (4)	C36—N3—Zn2	108.9 (3)
C13—N1—C12	107.2 (4)	C37—N3—Zn2	109.9 (3)
C14—N1—C12	109.5 (4)	C35—N3—Zn2	111.8 (3)
C13—N1—Zn1	110.3 (3)	C44—N4—C45	110.6 (5)
C14—N1—Zn1	108.4 (3)	C44—N4—C46	109.9 (5)
C12—N1—Zn1	113.0 (3)	C45—N4—C46	108.8 (5)
C23—N2—C21	110.9 (5)	C25—C24—C28	107.8 (5)
C23—N2—C22	109.8 (6)	C25—C24—P2	124.8 (4)
C21—N2—C22	109.3 (6)	C28—C24—P2	127.3 (5)
C5—C1—C2	107.5 (5)	C25—C24—Fe2	70.1 (3)
C5—C1—P1	124.6 (4)	C28—C24—Fe2	69.4 (3)
C2—C1—P1	127.9 (5)	P2—C24—Fe2	123.8 (3)
C5—C1—Fe1	69.2 (3)	C24—C25—C26	107.2 (6)
C2—C1—Fe1	69.3 (3)	C24—C25—Fe2	69.4 (3)
P1—C1—Fe1	124.3 (3)	C26—C25—Fe2	70.1 (3)
C3—C2—C1	108.1 (6)	C24—C25—H25	126.4
C3—C2—Fe1	70.5 (4)	C26—C25—H25	126.4
C1—C2—Fe1	69.6 (3)	Fe2—C25—H25	126.4
C3—C2—H2	125.9	C27—C26—C25	108.8 (6)
C1—C2—H2	125.9	C27—C26—Fe2	69.7 (4)
Fe1—C2—H2	125.9	C25—C26—Fe2	69.5 (3)
C4—C3—C2	108.6 (6)	C27—C26—H26	125.6
C4—C3—Fe1	70.0 (4)	C25—C26—H26	125.6
C2—C3—Fe1	69.6 (4)	Fe2—C26—H26	125.6
C4—C3—H3	125.7	C26—C27—C28	108.8 (6)
C2—C3—H3	125.7	C26—C27—Fe2	70.6 (4)
Fe1—C3—H3	125.7	C28—C27—Fe2	69.6 (3)
C3—C4—C5	109.2 (6)	C26—C27—H27	125.6
C3—C4—Fe1	70.5 (4)	C28—C27—H27	125.6
C5—C4—Fe1	69.0 (3)	Fe2—C27—H27	125.6
C3—C4—H4	125.4	C27—C28—C24	107.3 (6)
C5—C4—H4	125.4	C27—C28—Fe2	70.1 (4)
Fe1—C4—H4	125.4	C24—C28—Fe2	69.5 (3)
C1—C5—C4	106.6 (6)	C27—C28—H28	126.4
C1—C5—Fe1	70.0 (3)	C24—C28—H28	126.4
C4—C5—Fe1	69.9 (4)	Fe2—C28—H28	126.4
C1—C5—H5	126.7	C30—C29—C34	119.3 (5)
C4—C5—H5	126.7	C30—C29—P2	122.1 (4)
Fe1—C5—H5	126.7	C34—C29—P2	118.3 (4)
C7—C6—C11	119.9 (5)	C29—C30—C31	120.9 (5)
C7—C6—P1	121.7 (4)	C29—C30—H30	119.5
C11—C6—P1	118.2 (4)	C31—C30—H30	119.5
C8—C7—C6	121.1 (5)	C32—C31—C30	119.2 (5)
C8—C7—H7	119.5	C32—C31—H31	120.4
C6—C7—H7	119.5	C30—C31—H31	120.4
C9—C8—C7	119.4 (5)	C33—C32—C31	120.4 (5)
C9—C8—H8	120.3	C33—C32—H32	119.8
C7—C8—H8	120.3	C31—C32—H32	119.8
C10—C9—C8	120.3 (5)	C32—C33—C34	121.0 (5)
C10—C9—H9	119.8	C32—C33—H33	119.5
C8—C9—H9	119.8	C34—C33—H33	119.5
C9—C10—C11	120.9 (5)	C33—C34—C29	118.9 (5)
C9—C10—H10	119.6	C33—C34—C35	119.0 (5)
C11—C10—H10	119.6	C29—C34—C35	122.1 (5)
C6—C11—C10	118.4 (5)	N3—C35—C34	114.7 (4)
C6—C11—C12	122.8 (4)	N3—C35—H35A	108.6
C10—C11—C12	118.9 (5)	C34—C35—H35A	108.6
C11—C12—N1	114.5 (4)	N3—C35—H35B	108.6
C11—C12—H12A	108.6	C34—C35—H35B	108.6
N1—C12—H12A	108.6	H35A—C35—H35B	107.6
C11—C12—H12B	108.6	N3—C36—H36A	109.5
N1—C12—H12B	108.6	N3—C36—H36B	109.5
H12A—C12—H12B	107.6	H36A—C36—H36B	109.5
N1—C13—H13A	109.5	N3—C36—H36C	109.5
N1—C13—H13B	109.5	H36A—C36—H36C	109.5
H13A—C13—H13B	109.5	H36B—C36—H36C	109.5
N1—C13—H13C	109.5	N3—C37—H37A	109.5
H13A—C13—H13C	109.5	N3—C37—H37B	109.5
H13B—C13—H13C	109.5	H37A—C37—H37B	109.5
N1—C14—H14A	109.5	N3—C37—H37C	109.5
N1—C14—H14B	109.5	H37A—C37—H37C	109.5
H14A—C14—H14B	109.5	H37B—C37—H37C	109.5
N1—C14—H14C	109.5	C43—C38—C39	119.7 (5)
H14A—C14—H14C	109.5	C43—C38—P2	113.6 (4)
H14B—C14—H14C	109.5	C39—C38—P2	126.7 (4)
C20—C15—C16	119.3 (5)	C40—C39—C38	118.0 (5)
C20—C15—P1	127.3 (4)	C40—C39—C44	118.4 (5)
C16—C15—P1	113.3 (4)	C38—C39—C44	123.6 (5)
C17—C16—C15	121.6 (5)	C41—C40—C39	121.8 (5)
C17—C16—H16	119.2	C41—C40—H40	119.1
C15—C16—H16	119.2	C39—C40—H40	119.1
C16—C17—C18	119.8 (5)	C40—C41—C42	120.1 (5)
C16—C17—H17	120.1	C40—C41—H41	119.9
C18—C17—H17	120.1	C42—C41—H41	119.9
C17—C18—C19	119.7 (6)	C43—C42—C41	119.1 (5)
C17—C18—H18	120.1	C43—C42—H42	120.4
C19—C18—H18	120.1	C41—C42—H42	120.4
C18—C19—C20	121.2 (6)	C42—C43—C38	121.1 (5)
C18—C19—H19	119.4	C42—C43—H43	119.4
C20—C19—H19	119.4	C38—C43—H43	119.4
C15—C20—C19	118.2 (5)	N4—C44—C39	112.2 (5)
C15—C20—C21	123.9 (5)	N4—C44—H44A	109.2
C19—C20—C21	117.8 (5)	C39—C44—H44A	109.2
N2—C21—C20	112.3 (5)	N4—C44—H44B	109.2
N2—C21—H21A	109.1	C39—C44—H44B	109.2
C20—C21—H21A	109.1	H44A—C44—H44B	107.9
N2—C21—H21B	109.1	N4—C45—H45A	109.5
C20—C21—H21B	109.1	N4—C45—H45B	109.5
H21A—C21—H21B	107.9	H45A—C45—H45B	109.5
N2—C22—H22A	109.5	N4—C45—H45C	109.5
N2—C22—H22B	109.5	H45A—C45—H45C	109.5
H22A—C22—H22B	109.5	H45B—C45—H45C	109.5
N2—C22—H22C	109.5	N4—C46—H46A	109.5
H22A—C22—H22C	109.5	N4—C46—H46B	109.5
H22B—C22—H22C	109.5	H46A—C46—H46B	109.5
N2—C23—H23A	109.5	N4—C46—H46C	109.5
N2—C23—H23B	109.5	H46A—C46—H46C	109.5
H23A—C23—H23B	109.5	H46B—C46—H46C	109.5
N2—C23—H23C	109.5	Cl6—C47—Cl5	112.4 (3)
H23A—C23—H23C	109.5	Cl6—C47—H47A	109.1
H23B—C23—H23C	109.5	Cl5—C47—H47A	109.1
N3—Zn2—Cl4	108.40 (13)	Cl6—C47—H47B	109.1
N3—Zn2—Cl3	108.01 (13)	Cl5—C47—H47B	109.1
Cl4—Zn2—Cl3	117.43 (6)	H47A—C47—H47B	107.9
C15—P1—C1—C5	−169.2 (4)	C29—P2—C24—C25	77.1 (5)
C6—P1—C1—C5	72.8 (5)	C38—P2—C24—C25	−167.2 (4)
Zn1—P1—C1—C5	−34.5 (5)	Zn2—P2—C24—C25	−30.0 (5)
C15—P1—C1—C2	7.0 (5)	C29—P2—C24—C28	−106.1 (5)
C6—P1—C1—C2	−110.9 (5)	C38—P2—C24—C28	9.6 (5)
Zn1—P1—C1—C2	141.8 (4)	Zn2—P2—C24—C28	146.8 (4)
C15—P1—C1—Fe1	−82.2 (4)	C29—P2—C24—Fe2	165.2 (3)
C6—P1—C1—Fe1	159.8 (3)	C38—P2—C24—Fe2	−79.1 (4)
Zn1—P1—C1—Fe1	52.5 (4)	Zn2—P2—C24—Fe2	58.1 (4)
C5—C1—C2—C3	−1.4 (6)	C28—C24—C25—C26	0.8 (6)
P1—C1—C2—C3	−178.1 (4)	P2—C24—C25—C26	178.2 (4)
Fe1—C1—C2—C3	−60.2 (4)	Fe2—C24—C25—C26	60.2 (4)
C5—C1—C2—Fe1	58.8 (4)	C28—C24—C25—Fe2	−59.3 (4)
P1—C1—C2—Fe1	−117.9 (4)	P2—C24—C25—Fe2	118.0 (4)
C1—C2—C3—C4	0.4 (7)	C24—C25—C26—C27	−1.0 (7)
Fe1—C2—C3—C4	−59.3 (4)	Fe2—C25—C26—C27	58.8 (4)
C1—C2—C3—Fe1	59.7 (4)	C24—C25—C26—Fe2	−59.7 (4)
C2—C3—C4—C5	0.8 (7)	C25—C26—C27—C28	0.7 (7)
Fe1—C3—C4—C5	−58.3 (4)	Fe2—C26—C27—C28	59.4 (4)
C2—C3—C4—Fe1	59.1 (4)	C25—C26—C27—Fe2	−58.6 (4)
C2—C1—C5—C4	1.8 (6)	C26—C27—C28—C24	−0.2 (6)
P1—C1—C5—C4	178.7 (4)	Fe2—C27—C28—C24	59.8 (4)
Fe1—C1—C5—C4	60.7 (4)	C26—C27—C28—Fe2	−60.0 (4)
C2—C1—C5—Fe1	−58.9 (4)	C25—C24—C28—C27	−0.4 (6)
P1—C1—C5—Fe1	118.0 (4)	P2—C24—C28—C27	−177.6 (4)
C3—C4—C5—C1	−1.6 (6)	Fe2—C24—C28—C27	−60.2 (4)
Fe1—C4—C5—C1	−60.8 (4)	C25—C24—C28—Fe2	59.8 (4)
C3—C4—C5—Fe1	59.2 (4)	P2—C24—C28—Fe2	−117.5 (4)
C1—P1—C6—C7	−1.8 (5)	C24—P2—C29—C30	−3.1 (5)
C15—P1—C6—C7	−116.8 (4)	C38—P2—C29—C30	−117.3 (4)
Zn1—P1—C6—C7	122.5 (4)	Zn2—P2—C29—C30	120.4 (4)
C1—P1—C6—C11	−175.6 (4)	C24—P2—C29—C34	−176.9 (4)
C15—P1—C6—C11	69.5 (4)	C38—P2—C29—C34	68.9 (4)
Zn1—P1—C6—C11	−51.2 (4)	Zn2—P2—C29—C34	−53.5 (4)
C11—C6—C7—C8	−1.4 (8)	C34—C29—C30—C31	−4.5 (7)
P1—C6—C7—C8	−175.0 (4)	P2—C29—C30—C31	−178.3 (4)
C6—C7—C8—C9	0.8 (8)	C29—C30—C31—C32	0.6 (8)
C7—C8—C9—C10	0.8 (8)	C30—C31—C32—C33	2.5 (8)
C8—C9—C10—C11	−1.7 (8)	C31—C32—C33—C34	−1.7 (8)
C7—C6—C11—C10	0.5 (7)	C32—C33—C34—C29	−2.3 (8)
P1—C6—C11—C10	174.3 (4)	C32—C33—C34—C35	179.2 (5)
C7—C6—C11—C12	179.5 (5)	C30—C29—C34—C33	5.3 (7)
P1—C6—C11—C12	−6.7 (7)	P2—C29—C34—C33	179.3 (4)
C9—C10—C11—C6	1.1 (7)	C30—C29—C34—C35	−176.2 (5)
C9—C10—C11—C12	−178.0 (5)	P2—C29—C34—C35	−2.2 (7)
C6—C11—C12—N1	75.4 (6)	C36—N3—C35—C34	65.9 (6)
C10—C11—C12—N1	−105.6 (5)	C37—N3—C35—C34	−175.7 (4)
C13—N1—C12—C11	−173.5 (4)	Zn2—N3—C35—C34	−55.1 (5)
C14—N1—C12—C11	69.1 (5)	C33—C34—C35—N3	−107.2 (5)
Zn1—N1—C12—C11	−51.7 (5)	C29—C34—C35—N3	74.3 (6)
C1—P1—C15—C20	−73.0 (5)	C24—P2—C38—C43	110.2 (4)
C6—P1—C15—C20	41.9 (6)	C29—P2—C38—C43	−134.9 (4)
Zn1—P1—C15—C20	149.8 (5)	Zn2—P2—C38—C43	−27.7 (5)
C1—P1—C15—C16	106.3 (4)	C24—P2—C38—C39	−69.4 (5)
C6—P1—C15—C16	−138.7 (4)	C29—P2—C38—C39	45.6 (5)
Zn1—P1—C15—C16	−30.8 (4)	Zn2—P2—C38—C39	152.8 (4)
C20—C15—C16—C17	1.1 (8)	C43—C38—C39—C40	0.2 (8)
P1—C15—C16—C17	−178.3 (4)	P2—C38—C39—C40	179.7 (4)
C15—C16—C17—C18	−1.2 (9)	C43—C38—C39—C44	−177.2 (5)
C16—C17—C18—C19	−0.6 (9)	P2—C38—C39—C44	2.4 (8)
C17—C18—C19—C20	2.4 (10)	C38—C39—C40—C41	−1.7 (9)
C16—C15—C20—C19	0.6 (8)	C44—C39—C40—C41	175.8 (5)
P1—C15—C20—C19	179.9 (5)	C39—C40—C41—C42	1.6 (9)
C16—C15—C20—C21	−176.8 (5)	C40—C41—C42—C43	0.0 (9)
P1—C15—C20—C21	2.5 (9)	C41—C42—C43—C38	−1.5 (8)
C18—C19—C20—C15	−2.3 (9)	C39—C38—C43—C42	1.4 (8)
C18—C19—C20—C21	175.2 (6)	P2—C38—C43—C42	−178.2 (4)
C23—N2—C21—C20	65.5 (7)	C45—N4—C44—C39	66.4 (6)
C22—N2—C21—C20	−173.2 (5)	C46—N4—C44—C39	−173.4 (5)
C15—C20—C21—N2	−139.6 (6)	C40—C39—C44—N4	44.6 (7)
C19—C20—C21—N2	43.0 (8)	C38—C39—C44—N4	−138.1 (5)

Symmetry codes: (i) −x+2, −y+1, −z+1; (ii) −x, −y, −z.